TY - CONF A1 - Völker, Christoph T1 - Integration von Forschungsdaten im Bereich zerstörungsfreien Prüfung (ZfP) im Bauwesen N2 - Der Vortrag gibt einen Überblick zu Fragestellungen, Herausforderungen und Nutzen von semantischer Datenintegration im Forschungsbereich der zerstörungsfreien Prüfung im Bauwesen. T2 - 1. KDA Kolloquium der BAM CY - Berlin, Germany DA - 29.03.2019 KW - Digitalisierung KW - Ontology KW - ZfP KW - Beton KW - Datenanalyse PY - 2019 AN - OPUS4-50026 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reimold, W. U. A1 - Crosta, A. P. A1 - Hasch, M. A1 - Kowitz, Astrid A1 - Hauser, N. A1 - Sanchez, J. P. A1 - Simoes, L. S. A. A1 - de Sanchez, G. J. A1 - Zaag, P. T. T1 - Shock deformation confirms the impact origin for the Cerro do Jarau, Rio Grande do Sul, Brazil, structure N2 - Cerro do Jarau is a conspicuous, circular morpho‐structural feature in Rio Grande do Sul State (Brazil), with a central elevated core in the otherwise flat “Pampas” terrain typical for the border regions between Brazil and Uruguay. The structure has a diameter of approximately 13.5 km. It is centered at 30o12′S and 56o32′W and was formed on basaltic flows of the Cretaceous Serra Geral Formation, which is part of the Paraná‐Etendeka Large Igneous Province (LIP), and in sandstones of the Botucatu and Guará formations. The structure was first spotted on aerial photographs in the 1960s. Ever since, its origin has been debated, sometimes in terms of an endogenous (igneous) origin, sometimes as the result of an exogenous (meteorite impact) event. In recent years, a number of studies have been conducted in order to investigate its nature and origin. Although the results have indicated a possible impact origin, no conclusive evidence could be produced. The interpretation of an impact origin was mostly based on the morphological characteristics of the structure; geophysical data; as well as the occurrence of different breccia types; extensive deformation/silicification of the rocks within the structure, in particular the sandstones; and also on the widespread occurrence of low‐pressure deformation features, including some planar fractures (PFs). A detailed optical microscopic analysis of samples collected during a number of field campaigns since 2007 resulted in the disclosure of a large number of quartz grains from sandstone and monomict arenite breccia from the central part of the structure with PFs and feather features (FFs), as well as a number of quartz grains exhibiting planar deformation features (PDFs). While most of these latter grains only carry a single set of PDFs, we have observed several with two sets, and one grain with three sets of PDFs. Consequently, we here propose Cerro do Jarau as the seventh confirmed impact structure in Brazil. Cerro do Jarau, together with Vargeão Dome (Santa Catalina state) and Vista Alegre (Paraná State), is one of very few impact structures on Earth formed in basaltic rocks. KW - Serra da cangalha KW - Recovery experiments KW - Piaui state KW - Santa-marta KW - Features KW - Pressure KW - GPA KW - Sandstone KW - Geology PY - 2018 DO - https://doi.org/10.1111/maps.13233 SN - 1086-9379 VL - 54 IS - 10 SP - 2384 EP - 2394 PB - Wiley AN - OPUS4-50029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Hufschläger, Daniel A1 - Bente, Klaas T1 - Advances in air-coupled ultrasonic transducers for non-destructive testing N2 - Commercially available air-coupled transducers applied in non-destructive testing consist of a piezocomposite material and matching layers to reduce the impedance mismatch between the transducer and air. This contribution is an overview of innovative approaches using new piezoelectric materials and other physical principles to transmit and receive an ultrasonic pulse in air. Capacitive and piezoelectric micromachined ultrasonic transducers (CMUTs and PMUTs) produce high pressure levels, but they exhibit a very narrow bandwidth. Optical laser-based methods for transmitting and receiving ultrasound promise a higher bandwidth, but do not achieve the same sensitivity as conventional air-coupled transducers. Ferroelectrets are charged cellular polymers exhibiting piezoelectric properties, having a very small acoustic impedance well matched to air. Ferroelectret transducers achieve about the same bandwidth as the most broadband conventional air-coupled transducers, having a higher sensitivity. Thermoacoustic transducers use heat to initiate an acoustic wave, acting as transmitters in ultrasonic range. Thermoacoustic transducers enable excitation of extremely broadband pulses while producing high pressure levels, which opens new possibilities for advanced signal processing. The newest member of the family of air-coupled ultrasonic transmitters is the plasma-based transducer, using both the thermoacoustic effect and the movements of the ions (so called ionic wind) to create acoustic waves. T2 - International Congress on Ultrasonics CY - Bruges, Belgium DA - 03.09.2019 KW - Air-coupled transducers KW - Ferroelectret KW - Thermoacoustics KW - Plasma acoustics KW - Non-destructive testing PY - 2019 DO - https://doi.org/10.1121/2.0001072 SN - 1939-800X N1 - Geburtsname von Hufschläger, Daniel: Kotschate, D. - Birth name of Hufschläger, Daniel: Kotschate, D. VL - 38 IS - 1 SP - 030003-1 EP - 030003-7 PB - American Institute of Physics CY - Lancaster, Pa. AN - OPUS4-50103 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dominguez-Macaya, A. A1 - Gaal, Mate A1 - Gómez Álvarez-Arenas, T. E A1 - Aurrekoetxea, J. A1 - Iturrospe, A. T1 - Air-coupled ultrasonic testing with Lamb waves for straight and curved GFRP plates N2 - The use of composite materials has been steadily growing during the last decades, as well as the requirements on quality, mechanical properties and geometries of the parts. Some processes, like the 3D UV pultrusion process, manufacture parts that are long and thin, whilst having a varying curvature radius along the same part or even no curvature at all. Studying their mechanical properties along the main fiber direction, which is of foremost interest, is not an easy task nor efficient with most nondestructive methods. The use of air-coupled ultrasonics to evaluate the properties of composite materials has been widely proved by several authors, mainly using guided waves that provide information on the orthotropic properties of this kind of materials. Most of this work has focused on analyzing straight plate-like geometries, due to the simplicity to generate desired Lamb modes in the plate and analyze the behavior of guided waves inside the plate. In our contribution, the differences in the propagation of Lamb waves for straight and curved geometry glass fiber reinforced polymers (GFRP) have been analyzed. A GFRP test sample cured with UV light with one straight and one curved area has been evaluated. The responses of the generated Lamb wave modes for the straight and curved geometries have been compared, accounting for variations in the transducer characteristics, e.g. resonance behavior and focusing. T2 - International Congress on Ultrasonics CY - Bruges, Begium DA - 03.09.2019 KW - Air-coupled KW - Guided waves KW - Composites PY - 2019 DO - https://doi.org/10.1121/2.0001072 VL - 38 SP - 045005 AN - OPUS4-50104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Ferroelektret-Wandler für Luftultraschall N2 - Es wird ein Überblick über die Forschung an Ferroelektret-Wandlern für luftgekoppelte Ultraschallprüfung gegeben. T2 - Innovative ZFP mit bildgebender Ultraschallprüftechnik CY - Braunschweig, Germany DA - 29.11.2019 KW - Luftultraschall KW - Ferroelektret KW - Wandler PY - 2019 AN - OPUS4-50107 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian A1 - Emmerling, Franziska T1 - Insights into the mechanochemical Knoevenagel condensation N2 - Mechanochemistry paves the way to simple, fast, and green syntheses, but there is a lack in understanding of the underlying mechanisms. Here, we present a universal strategy for simultaneous real-time in situ analysis, combining X-ray diffraction, Raman spectroscopy, and thermography. T2 - Bessy User Meeting 2019 CY - Berlin, Germany DA - 05.12.2019 KW - Mechanochemistry PY - 2019 AN - OPUS4-50122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Mechanochemistrry - a time resolved perspective on unconventional crystallization N2 - Green chemsistry apporoach for the synthesis of metal organic frameworks. T2 - IFW BAM Workshop CY - Berlin, Germany DA - 25.11.2019 KW - Mechanochemistry KW - XRD KW - Metal-organic-frameworks PY - 2019 AN - OPUS4-50110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Colini, Claudia T1 - Chinese paper in Persian manuscript: Preliminary results of a of a codicological, technological and scientific study N2 - In the 15th century, Persian manuscripts underwent significant and lasting changes. Possibly as a response to the import of tinted and gold-decorated paper from China, which was used for manuscript production in Greater Iran, Persian papers were also tinted and embellished with gold-decorated and marbled margins or frames. In a joint project between CSMC and the University of St Andrews, we aim to analyse papers and their decorations in Persian The analyses aim to determine the consistencies of papers, pigments and metals and the techniques used for their production and application. The support will be first described in its codicological characteristics such as dimensions, thickness, colour (expressed in colour coordinates), pattern left from the sieve (observed in transmitted light). The plant used as raw material in paper production will be studied by fibres analysis, while the sizing agents, the pigments, dyes and metals will be analysed by the application of several methods: in particular Reflectography, X-Ray Fluorescence and InfraRed, Raman and Visible Reflectance Spectroscopy. The results of the analyses will form an important resource for the material aspects of Persian manuscripts and be a starting point for establishing a first chronology of the materials and techniques used in Persian manuscript production. An example of the application of the techniques on the analysis of a fragment from a 15th c. Persian Manuscript will be provided. T2 - The Second International Seminar on Traditional Writing and Printing Materials (Fudan University) CY - Shanghai, Republic of China DA - 12.11.2019 KW - Persian manuscript KW - Chinese paper KW - Paper tinting KW - UV-VIS reflectance spectroscopy KW - XRF KW - ATR PY - 2019 AN - OPUS4-50131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Ein Blick in die Welt der Mechanochemie N2 - Perhaps due in no small part to its historical mystique, mechanochemistry has been shrowded in relative obscurity for quite some time. The successes of mechanochemistry in organic synthesis have often been curtailed by a fundamentally limited mechanistic understanding. Lately, however, the community has made great strides towards understanding the fundamentals, as well as large steps forward regarding industrially significant scale-up via twin-screw extrusion. A variety of recent work has traded in some of mechanochemistry’s mystique for simple, straight-forward chemical guidelines. T2 - Seminar Anorganische Chemie Universität Kiel CY - Kiel, Germany DA - 22.10.19 KW - Mechanochemistry KW - XRD PY - 2019 AN - OPUS4-50134 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Shaken or levitated? A time resolved perspective on unconventional crystallization N2 - This Outlook provides a brief overview of the recent achievements and opportunities created by acoustic levitation and mechanochemistry, including access to materials, molecular targets, and synthetic strategies that are difficult to access by conventional means. T2 - Vortragsreihe Analytik Merck CY - Darmstadt, Germany DA - 18.11.19 KW - Levitation KW - Acoustic levitation KW - X-ray and electron diffraction PY - 2019 AN - OPUS4-50135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - May the force be with you - in situ investigation of mechanochemical reactions N2 - The past decade has seen a reawakening of solid-state to chemical synthesis, driven by the search for new, cleaner synthetic methodologies. Mechanochemistry has advanced to a widely applicable technique. T2 - SALSA's "Make and Measure 2019 CY - Berlin, Germany DA - 25.10.2019 KW - Mechanochemistry KW - Metal–organic frameworks PY - 2019 AN - OPUS4-50138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Colini, Claudia T1 - Fifty shades of black: Typologies and terminology of black inks in the light of new discoveries N2 - The identification of the materials constituting an artefact is the basis of any correct conservation project. For this reason (among others) in the last 50 years analytical techniques have been applied to the study of manuscripts. Unfortunately, the scientific investigation of Arabic books is still uncommon, focusing mainly on single case studies of illuminated manuscripts where the black media used to write the text is largely overlooked. This lack of knowledge prompted a recent research in which black ink recipes have been collected from written Arabic sources, their feasibility has been assessed, and some of them have been reproduced. These samples were artificially aged and analysed through an array of analytical techniques, mostly non-invasive and non-destructive, in order to build a database of Arabic inks and their ingredients and to verify the detection limits of the equipment employed. Finally, the results were compared to the data collected from historical manuscripts. In this talk I will focus on the ink typologies and the terminology (ancient and modern) used to describe them. In particular I will highlight how even the modern classification fails to capture the variety encountered in both recipes and manuscripts, particularly in the light of recent discoveries. I will address especially the terminological and conceptual issues of mixed inks – in the form of carbon inks and tannins, of carbon and iron gall inks, and of carbon and metallic salts –, iron gall inks made without vitriol and iron gall inks made with sources of tannins different from gall nuts. T2 - First International Conference Oriental Manuscripts: Codicology and Conservation issues CY - Saint Petersburg, Russia DA - 04.12.2019 KW - Ink terminology KW - Codicology KW - Non destructive analytical techniques PY - 2019 AN - OPUS4-50159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Colini, Claudia T1 - Ink recipes from the islamic era: Texts, manuscripts, ink reproductions and scientific analyses N2 - Ink recipes can often be found in Arabic manuscripts. They may be included in treatises of diverse subjects – from handbooks for secretaries or calligraphers to books on arts and crafts, to alchemical and astrological essays. Recipes can also appear, with or without relation to the main text in the manuscript, in the form of lists or collections or even added in empty spaces as single entries. Why were these recipes written down? Were they used by the many professionals dealing with inks in their every-day work? Or were they part of the literary genre of adab with little or no practical application? To answer these questions a research project was set up: ink recipes have been collected from written Arabic sources, their feasibility has been assessed and some of them have been reproduced. These samples were artificially aged and analysed through an array of analytical techniques, most non-invasive and non-destructive, and the results compared to the data obtained by the application of the same analyses on concrete manuscripts. The codicological characteristics of the manuscripts have also been studied. My aim in this talk is to show how such an interdisciplinary approach could be beneficial for the study of material culture. T2 - Broadening Horizons 6 CY - Berlin, Germany DA - 24.06.2019 KW - Inks KW - Arabic Recipes KW - Non destructive analytical techniques PY - 2019 AN - OPUS4-50160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Colini, Claudia T1 - Analyses of decorated papers: Potential and preliminary results on persianate manuscripts from 15th – 17th centuries N2 - This talk will be divided into two parts. In the first part I will present the analytical techniques and the equipment used by the Centre for the Study of Manuscript Cultures that can be applied for the study of decorated papers. The analyses aim to determine the constituent materials of papers, pigments, dyes and metals and the techniques used for their production. I will focus in particular on the kind of information these techniques allow us to gather: through optical microscopy we conduct fibre analysis in order to identify the plant used as raw material in paper production while Reflectography, X-Ray Fluorescence and InfraRed, Raman and Visible Reflectance Spectroscopy are used to study the sizing agents, the pigments, dyes and metals. In the second part I will show some results obtained by the application of these techniques on a few Persianate manuscripts, dating between the 15th and 17th centuries, belonging to the corpus of Ilse Sturkenboom. T2 - Symposium Decorated Paper in Early Modern Islamic Cultures CY - Istanbul, Turkey DA - 23.11.2019 KW - XRF KW - UV-VIS Reflectance spectroscopy KW - Fibre analysis KW - Persian manuscripts KW - Chinese Paper KW - FTIR spectroscopy PY - 2019 AN - OPUS4-50161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Colini, Claudia A1 - Sturkenboom, I. T1 - Analyses of paper, tinting and illumination in persian manuscripts held in the Golestan Palace library N2 - In the 15th century, Persian manuscripts underwent significant and lasting changes. Possibly as a response to the import of tinted and gold-decorated paper from China, which was used for manuscript production in Greater Iran, Persian papers were also tinted and embellished with gold-decorated and marbled margins or frames. In a joint project between CSMC and the University of St Andrews, and in co-operation with the Golestan Palace Museum, we aim to analyse papers and their decorations in manuscripts in the holdings of the Golestan Palace Library. The analyses aim to determine the consistencies of papers, pigments and metals and the techniques used for their production and application. The support will be first described in its codicological characteristics such as dimensions, thickness, colour (expressed in colour coordinates), pattern left from the sieve (observed in transmitted light). The plant used as raw material in paper production will be studied by fibres analysis, while the sizing agents, the pigments, dyes and metals will be analysed by the application of several methods: in particular Reflectography, X-Ray Fluorescence and InfraRed, Raman and Visible Reflectance Spectroscopy. The results of the analyses will be published in an online database that will form an important resource for the material aspects of Persian manuscripts and be a starting point for establishing a first chronology of the materials and techniques used in Persian manuscript production. T2 - DFG workshop at Golestan Palace CY - Tehran, Iran DA - 07.04.2019 KW - Persian manuscripts KW - Chinese paper KW - Non destructive analytical techniques KW - Tinting KW - Gold PY - 2019 AN - OPUS4-50164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona A1 - Pohlisch, Jakob A1 - Blind, K. T1 - International Diffusion of the Information Security Management System Standard ISO/IEC 27001: Exploring the Role of Culture N2 - In the wake of digitalization, organizations are increasingly exposed to risks associated with security breaches and must take measures to preserve the confidentiality, integrity, and availability of information, and to ensure business continuity. The international standard ISO/IEC 27001 assists organizations in setting up, maintaining and continuously improving their information security management systems. However, despite high growth rates, its international diffusion rates are quite heterogeneous. This paper explores why the diffusion of the international management system standard ISO/IEC 27001 differs across countries. We classify the adoption of ISO/IEC 27001 as a ‘preventive organizational innovation’ and draw from diffusion studies of other management system standards and information security research to develop a set of hypotheses. These relate to the impact of cultural dimensions and national ICT development. We use a negative binomial regression model with panel data covering 57 countries over a 12-year period from 2006 to 2017 to test our hypotheses. We find that the cultural dimensions future orientation, power distance, and institutional collectivism as well as high ICT development are driving factors for the diffusion of ISO/IEC 27001. We derive policy recommendations and avenues for future research. T2 - Twenty-Eighth European Conference on Information Systems (ECIS2020) – A Virtual AIS Conference CY - Online meeting DA - 15.06.2020 KW - Information security KW - International diffusion KW - Standards KW - Management system standards KW - ISO/IEC 27001 KW - Preventive innovations KW - Culture KW - GLOBE KW - ICT development index PY - 2020 SP - RP 88 AN - OPUS4-50919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona T1 - International Diffusion of the Information Security Management System Standard ISO/IEC 27001: Exploring the role of culture N2 - In the wake of digitalization, organizations are increasingly exposed to risks associated with security breaches and must take measures to preserve the confidentiality, integrity, and availability of information, and to ensure business continuity. The international standard ISO/IEC 27001 assists organizations in setting up, maintaining and continuously improving their information security management systems. However, despite high growth rates, its international diffusion rates are quite heterogeneous. This paper explores why the diffusion of the international management system standard ISO/IEC 27001 differs across countries. We classify the adoption of ISO/IEC 27001 as a ‘preventive organizational innovation’ and draw from diffusion studies of other management system standards and information security research to develop a set of hypotheses. These relate to the impact of cultural dimensions and national ICT development. We use a negative binomial regression model with panel data covering 57 countries over a 12-year period from 2006 to 2017 to test our hypotheses. We find that the cultural dimensions future orientation, power distance, and institutional collectivism as well as high ICT development are driving factors for the diffusion of ISO/IEC 27001. We derive policy recommendations and avenues for future research. T2 - Twenty-Eighth European Conference on Information Systems (ECIS2020) – A Virtual AIS Conference CY - Online meeting DA - 15.06.2020 KW - Information security KW - International diffusion KW - Standards KW - Management system standards KW - ISO/IEC 27001 KW - Preventive innovations KW - Culture KW - GLOBE KW - ICT development index PY - 2020 AN - OPUS4-50921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Faßbender, Sebastian T1 - On-line species-specific isotopic analysis of sulfur by hyphenation of capillary electrophoresis with MC-ICP-MS N2 - In many scientific fields, isotopic analysis can offer valuable information. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement. Whereas some works hyphenating GC and IC with MC-ICP-MS have already been reported, LC and CE hyphenations are still inadequately represented based on the capabilities of these separation techniques. In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species using a multiple-injection approach for instrumental mass bias correction by standard-sample bracketing. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared to data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was promising regarding the differentiation of the river systems by the isotopic signature of river water sulfate. The great potential of this method is based on the versatility of the applied separation technique, not only in the environmental field but also for, e.g., biomolecules, as sulfur is the only covalently bound constituent of proteins that can be analyzed by MC-ICP-MS. T2 - Virtual Goldschmidt 2020 CY - Online meeting DA - 21.06.2020 KW - Isotopic analysis KW - Hyphenated techniques KW - Capillary electrophoresis KW - Multicollector-ICP-MS KW - Speciation analysis PY - 2020 AN - OPUS4-50922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim A1 - Thiel, Erik A1 - Karagianni, Christina A1 - Hirsch, Philipp Daniel A1 - Burgholzer, P. A1 - Mayr, G. A1 - Jung, P. A1 - Caire, G. A1 - Ziegler, Mathias T1 - Photothermal super resolution image reconstruction using structured 1D laser illumination N2 - The separation of two closely spaced defects in fields of Thermographic NDE is very challenging. The diffusive nature of thermal waves leads to a fundamental limitation in spatial resolution. Therefore, super resolution image reconstruction can be used. A new concerted ansatz based on spatially structured heating and joint sparsity of the signal ensemble allows for an improved reconstruction of closely spaced defects. This new technique has been studied using a 1D laser array with randomly chosen illumination pattern. This paper presents the results after applying super resolution algorithms, such as the iterative joint sparsity (IJOSP) algorithm, to our processed measurement data. Different data processing techniques before applying the IJOSP algorithm as well as the influence of regularization parameters in the data processing techniques are discussed. Moreover, the degradation of super resolution reconstruction goodness by the choice of experimental parameters such as laser line width or number of measurements is shown. The application of the super resolution results in a spatial resolution enhancement of approximately a factor of four which leads to a better separation of two closely spaced defects. T2 - Quantitative Nondestructive Evaluation Conference 2019 CY - Portland, OR, USA DA - 14.07.2019 KW - Super resolution KW - Photothermal KW - Thermography KW - Laser PY - 2019 SP - Paper 8593, 1 PB - ASME AN - OPUS4-50924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. A1 - Kim, K. J. T1 - Analysis of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by electron probe microanalysis and micro-focus X-ray fluorescence N2 - The present study reports on results of analysis of the elemental composition of thin films by electron probe microanalysis with energy dispersive (ED-EPMA) X-ray spectrometry in conjunction with the dedicated thin-film analysis software package Stratagem and by X-ray fluorescence in its version with a micro-focus X-ray fluorescence (μ-XRF) source attached to a scanning electron microscope (SEM). Two thin-film systems have been analyzed: Fe1-xNix on silicon wafer and Si1-xGex on Al2O3 substrate, in both cases the layers being grown to a thickness of about 200 nm by ion beam sputter deposition. Samples of five different atomic fractions have been produced and analyzed for each thin-film system. Moreover, reference samples with certified elemental composition and thickness have been also available. This study is part of an interlaboratory comparison organized in the frame of standardization technical committee ISO/TC 201 “Surface chemical analysis.” Two laboratories have been analyzed by ED-EPMA (one laboratory standardless and one laboratory using both standardless and with standards variants) and one laboratory by μ-XRF (standardless and with standards). All the elemental compositions obtained with different methods are in very good agreement for the complete two sets of five samples each. KW - Thin films KW - Elemental composition KW - FeNi KW - SiGe KW - Electron probe microanalysis KW - X-ray Fluorescence PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509262 DO - https://doi.org/10.1002/sia.6834 SN - 0142-2421 VL - 52 IS - 12 SP - 929 EP - 932 PB - John Wiley & Sons Ltd AN - OPUS4-50926 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuhring, M. A1 - Doellinger, J. A1 - Nitsche, A. A1 - Muth, Thilo A1 - Renard, B. Y. T1 - TaxIt: An Iterative Computational Pipeline for Untargeted Strain-Level Identification Using MS/MS Spectra from Pathogenic Single-Organism Samples N2 - Untargeted accurate strain-level classification of a priori unidentified organisms using tandem mass spectrometry is a challenging task. Reference databases often lack taxonomic depth, limiting peptide assignments to the species level. However, the extension with detailed strain information increases runtime and decreases statistical power. In addition, larger databases contain a higher number of similar proteomes. We present TaxIt, an iterative workflow to address the increasing search space required for MS/MS-based strain-level classification of samples with unknown taxonomic origin. TaxIt first applies reference sequence data for initial identification of species candidates, followed by automated acquisition of relevant strain sequences for low level classification. Furthermore, proteome similarities resulting in ambiguous taxonomic assignments are addressed with an abundance weighting strategy to increase the confidence in candidate taxa. For benchmarking the performance of our method, we apply our iterative workflow on several samples of bacterial and viral origin. In comparison to noniterative approaches using unique peptides or advanced abundance correction, TaxIt identifies microbial strains correctly in all examples presented (with one tie), thereby demonstrating the potential for untargeted and deeper taxonomic classification. TaxIt makes extensive use of public, unrestricted, and continuously growing sequence resources such as the NCBI databases and is available under open-source BSD license at https://gitlab.com/rki_bioinformatics/TaxIt. KW - Bioinformatics KW - Mass spectrometry KW - Microbial proteomics KW - Strain identification KW - MS/MS PY - 2020 DO - https://doi.org/10.1021/acs.jproteome.9b00714 VL - 19 IS - 6 SP - 2501 EP - 2510 PB - ACS AN - OPUS4-50942 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Sennikov, P. A1 - Kornev, R. A1 - Ermakov, A. A1 - Shkrunin, V. T1 - Laser Induced Dielectric Breakdown for Chemical Vapor Deposition by Hydrogen Reduction of Volatile Boron Halides BCl3 and  BF3 N2 - A possibility of deposition from laser-induced plasma is investigated in search for an economic and simple method for obtaining isotopic compounds from enriched gaseous precursors although no isotopic compounds are used in this the proof-of-principle work. A breakdown in mixtures of BCl3 and BCl3 with hydrogen, argon, and methane are studied both theoretically and experimentally. Equilibrium chemistry calculations show the deposition of boron, boron carbide, and carbon is thermodynamically favorable in BCl3 systems and only carbon in BF3 systems. Dynamic calculation of expanding plasma is performed using fluid dynamics coupled with equilibrium chemistry. Condensed phases of boron, boron carbide, and graphite are predicted with maximum concentrations in peripheral zones of the plasma. In experiment, plasma is induced in mixtures BCl3, H2 + BCl3, H2 + Ar + BCl3, H2 + BCl3 + CH4, BF3, H2 + BF3, H2 + Ar + BF3, and H2 + Ar + BF3. The gases are analyzed before, during, and after laser irradiation by optical and mass spectrometry methods. The results show the composition of reaction products close to that predicted theoretically. The conversion of precursor gases BCl3 and BF3 into gaseous and condensed products is 100% for BCl3 and 80% for BF3. Solid deposits of up to 30 mg are obtained from all reaction mixtures. Due to technical reasons only FTIR characterization of the BCl3 + H2 + CH4 deposit is done. It points to presence of condensed boron and boron carbide predicted by the model. Overall, the calculations and preliminary experimental results imply the chemical vapor deposition with laser induced plasma is promising for conversion of gaseous enriched precursors into elemental isotopes and their isotopic compounds. KW - Boron halides KW - Chemical vapor deposition KW - Laser induced dielectric breakdown, Hydrogen reduction PY - 2020 DO - https://doi.org/10.1007/s11090-020-10096-w VL - 40 IS - 5 SP - 1145 EP - 1162 PB - Springer AN - OPUS4-50968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Challenges in Intelligent Computing for Non destructive testing in civil engineering – today and tomorrow N2 - A large amount of data and information is collected in the field of non-destructive testing (NDT) in civil engineering. The weakly structured data are usually evaluated with regard to specific testing tasks (e.g. geometry determination, damage localization, quality assurance). While the data offers great economic potential, i.e. to support construction planning, monitoring and maintenance processes, the evaluation is manual and case-by-case and therefore too inefficient for broader applications. We present recent visions and approaches how these large amounts of data need to be handled in the future and how we aim to make the acquired knowledge accessible to our stakeholders. Building on initiatives in materials research, we stress the importance of further research in the field of semantic data integration particularly motivate why an ontology is needed for the area of NDT in civil engineering. T2 - EG-ICE 2020 CY - Online meeting DA - 01.07.2020 KW - Data analysis KW - Non destructive testing KW - Computational engineering KW - AI PY - 2020 AN - OPUS4-50971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donskyi, Ievgen A1 - Chen, Y. A1 - Nickl, Philip A1 - Guday, G. A1 - Qiao, H. A1 - Achasi, K. A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Böttcher, C. A1 - Chen, W. A1 - Adeli, M. A1 - Haag, R. T1 - Self-degrading graphene sheets for tumor therapy N2 - Low biodegradability of graphene derivatives and related health risks are the main limiting factors for their in vivo biomedical applications. Here, we present the synthesis of enzyme-functionalized graphene sheets with self-degrading properties under physiological conditions and their applications in Tumor therapy. The synergistic enzyme cascade glucose oxidase and myeloperoxidase are covalently conjugated to the surface of graphene sheets and two-dimensional (2D) platforms are obtained that can produce sodium hypochlorite from glucose. The enzyme-functionalized graphene sheets with up to 289 nm average size are degraded into small pieces (≤40 nm) by incubation under physiological conditions for 24 h. Biodegradable graphene sheets are further loaded with doxorubicin and their ability for Tumor therapy is evaluated in vitro and in vivo. The laser-triggered release of doxorubicin in combination with the enzymatic activity of the functionalized graphene sheets results in a synergistic antitumor activity. Taking advantage of their neutrophil-like activity, fast biodegradability, high photo- and chemotherapeutic effects, the novel two-dimensional nanoplatforms can be used for tumor therapeutic applications. KW - Graphene KW - Self-degrading KW - Thumor therapy KW - XPS KW - NEXAFS PY - 2020 DO - https://doi.org/10.1039/d0nr02159h SP - 1 EP - 12 PB - The Royal Society of Chemistry AN - OPUS4-50978 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmadi, Samim A1 - Burgholzer, P. A1 - Jung, P. A1 - Caire, G. A1 - Ziegler, Mathias T1 - Super resolution laser line scanning thermography N2 - In this paper we propose super resolution measurement and post-processing strategies that can be applied in thermography using laser line scanning. The implementation of these techniques facilitates the separation of two closely spaced defects and avoids the expected deterioration of spatial resolution due to heat diffusion. The experimental studies were performed using a high-power laser as heat source in combination with pulsed thermography measurements (step scanning) or with continuous heating measurements (continuous scanning). Our work shows that laser line step scanning as well as continuous scanning both can be used within our developed super resolution (SR) techniques. Our SR techniques make use of a compressed sensing based algorithm in post- processing, the so-called iterative joint sparsity (IJOSP) approach. The IJOSP method benefits from both - the sparse nature of defects in space as well as from the similarity of each measurement. In addition, we show further methods to improve the reconstruction quality e.g. by simple manipulations in thermal image processing such as by considering the effect of the scanning motion or by using different optimization algorithms within the IJOSP approach. These super resolution image processing methods are discussed so that the advantages and disadvantages of each method can be extracted. Our contribution thus provides new approaches for the implementation of super resolution techniques in laser line scanning thermography and informs about which experimental and post-processing parameters should be chosen to better separate two closely spaced defects. KW - Super resolution KW - Laser thermography KW - Compressed sensing KW - Laser scanning KW - Joint sparsity PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509796 DO - https://doi.org/10.1016/j.optlaseng.2020.106279 SN - 0143-8166 VL - 134 SP - 106279 PB - Elsevier Ltd. AN - OPUS4-50979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rus, J. A1 - Gustschin, A. A1 - Mooshofer, H. A1 - Grager, J.-C. A1 - Bente, Klaas A1 - Gaal, Mate A1 - Pfeiffer, F. A1 - Grosse, C. U. T1 - Qualitative comparison of non-destructive methods for inspection of carbon fiber-reinforced polymer laminates N2 - In the rapidly expanding composite industry, novel inspection methods have been developed in recent years. Particularly promising for air-coupled testing are cellular polypropylene transducers which offer better impedance matching to air than piezoelectric transducers. Furthermore, broadband transmitters (laser-induced ultrasound and thermoacoustic emitters) and receivers (optical microphones) have opened a completely new chapter for advanced contact-free ultra-sound inspection. X-ray dark-field radiography offers a different approach to detect porosity and microcracks, employing small angle X-ray scattering. These innovative ultrasonic and radiographic alternatives were evaluated in comparison with well-established inspection techniques. We applied thirteen different non-destructive methods to inspect the same specimen (a carbon fiber-reinforced polymer laminate with induced impact damage): air-coupled ultrasound testing (using piezoelectric transducers, broadband optical microphones, cellular polypropylene transducers, and a thermoa- coustic emitter), laser-induced ultrasound testing, ultrasonic immersion testing, phased array ultrasonic testing, optically excited lock-in thermography, and X-ray radiography (projectional absorption and dark-field, tomosynthesis, and micro-computed tomography). The inspection methods were qualitatively characterized by comparing the scan results. The conclusions are advantageous for a decision on the optimal method for certain testing constraints. KW - Carbon fiber-reinforced polymer KW - Air-coupled ultrasound KW - Optically excited lock-in thermography KW - X-ray micro-computed tomography KW - X-ray dark-field radiography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509473 DO - https://doi.org/10.1177/0021998320931162 SN - 0021-9983 VL - 54 IS - 27 SP - 4325 EP - 4337 PB - SAGE AN - OPUS4-50947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tiitta, M. A1 - Tiitta, V. A1 - Gaal, Mate A1 - Heikkinen, J. A1 - Lappalainen, R. A1 - Tomppo, L. T1 - Air-coupled ultrasound detection of natural defects in wood using ferroelectret and piezoelectric sensors N2 - Air-coupled ultrasound was used for assessing natural defects in wood boards by through-transmission scanning measurements. Gas matrix piezoelectric (GMP) and ferroelectret (FE) transducers were studied. The study also included tests with additional bias voltage with the ferroelectret receivers. Signal analyses, analyses of the measurement dynamics and statistical analyses of the signal parameters were conducted. After the measurement series, the samples were cut from the measurement regions and the defects were analyzed visually from the cross sections. The ultrasound responses were compared with the results of the visual examination of the cross sections. With the additional bias voltage, the ferroelectret measurement showed increased signal-to-noise ratio, which is especially important for air-coupled measurement of high-attenuation materials like wood. When comparing the defect response of GMP and FE sensors, it was found that FE sensors had more sensitive dynamic range, resulting from better s/n ratio and short response pulse. Classification test was made to test the possibility of detecting defects in sound wood. Machine learning methods including decision trees, k-nearest neighbor and support vector machine were used. The classification accuracy varied between 72 and 77% in the tests. All the tested machine learning methods could be used efficiently for the classification. KW - Air-coupled transducers KW - Wood KW - Ultrasound KW - Ultrasonic imaging KW - Ferroelectret KW - Machine learning PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509503 DO - https://doi.org/10.1007/s00226-020-01189-y SP - 1 EP - 14 PB - Springer AN - OPUS4-50950 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Haas, Marko ED - Hirsch, B ED - Weber, J ED - Schäfer, F ED - Schmid, J T1 - Das Risikomanagementsystem in der Bundesanstalt für Materialforschung und -prüfung (BAM) N2 - Im Rahmen des Bandes Management von Risiken in Behörden beschreibt der Praxisbeitrag das Risikomanagementsystem der BAM. KW - Risiko KW - Risikomanagement KW - Controlling KW - Management KW - Steuerung PY - 2020 SN - 978-3-503-19150-5 SP - 90 EP - 100 PB - Erich Schmidt Verlag CY - Berlin AN - OPUS4-50915 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Aerial Robot Olfaction - A Summary and Survey from BAM Perspective N2 - This presentation gives an introduction to the gas-sensitive aerial robots developed at BAM, including various application examples in the field of mobile robot olfaction: gas source localization and gas distribution mapping. T2 - Harvard University School of Engineering and Applied Sciences (SEAS)/Earth and Planetary Sciences (EPS) - Martin Group Seminar CY - Online meeting DA - 11.06.2020 KW - Mobile Robot Olfaction KW - Localization of gas sources KW - UAV KW - Tomographic reconstruction of gas plumes KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) PY - 2020 AN - OPUS4-50916 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Solomun, Tihomir A1 - Hahn, Marc Benjamin A1 - Smiatek, J. T1 - Raman spectroscopic signature of ectoine conformations in bulk solution and crystalline state N2 - Recent crystallographic results revealed conformational changes of zwitterionic ectoine upon hydration. By means of confocal Raman spectroscopy and density functional theory calculations, we present a detailed study of this transformation process as part of a Fermi resonance analysis. The corresponding findings highlight that all resonant couplings are lifted upon exposure to water vapor as a consequence of molecular binding processes. The importance of the involved molecular groups for water binding and conformational changes upon hydration is discussed. Our approach further Shows that the underlying rapid process can be reversed by carbon dioxide saturated atmospheres. For the first time, we also confirm that the conformational state of ectoine in aqueous bulk solution coincides with crystalline ectoine in its dihydrate state, thereby highlighting the important role of a few bound water molecules. KW - Fermi resonance KW - Ectoine hydration KW - DFT calculations of Raman spectra KW - Position of carboxylate group PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509855 DO - https://doi.org/10.1002/cphc.202000457 SN - 1439-4235 SN - 1439-7641 VL - 21 IS - 17 SP - 1945 EP - 1950 PB - Wiley-VCH CY - Weinheim AN - OPUS4-50985 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. A1 - Sennikov, P. T1 - Laser Induced Plasma for Chemical Vapor Deposition: Theory and Experiment N2 - A possibility of deposition from laser-induced plasma (LIP) is investigated in search for an economic and simple method to obtain isotopic compounds from enriched gaseous precursors. A breakdown in mixtures of BCl3 and BCl3 with hydrogen, argon, and methane are studied both theoretically and experimentally. Calculations of expanding plasma of different composition are performed with the use of the fluid dynamic code coupled to the equilibrium chemistry solver. Condensed phases of boron, boron carbide, and graphite are predicted showing maximum concentrations in peripheral zones of the plasma. In experiment LIP is induced in mixtures BCl3, Н2+BCl3, H2+Ar+BCl3, H2+BCl3+CH4, BF3, Н2+BF3, H2+Ar+BF3, and H2+Ar+BF3. The gases are analyzed before, during, and after laser irradiation by optical and mass spectroscopic methods. The composition of reaction products is found to be close to that predicted theoretically. The conversion of precursor gases BCl3 and BF3 into gaseous and condensed products is 100% for BCl3 and 80% for BF3. Solid deposits of up to 30 mg are obtained from all the reaction mixtures. FTIR analysis of BCl3+H2+CH4 deposits points to a presence of condensed boron and boron carbide that are also predicted by the model. Both calculations and preliminary experimental results suggest the chemical vapor deposition by LIP is promising for conversion of gaseous enriched precursors into elemental isotopes and their isotopic compounds. T2 - International Online Meeting on Laser Induced Breakdown Spectroscopy (IIOMLIBS) CY - Online meeting DA - 06.07.2020 KW - Chemical vapor deposition KW - Laser induced plasma PY - 2020 AN - OPUS4-50994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Faßbender, Sebastian A1 - Rodiouchkina, K. A1 - Vanhaecke, F. A1 - Meermann, Björn T1 - Method development for on-line species-specific sulfur isotopic analysis by means of capillary electrophoresis/multicollector ICP-mass spectrometry N2 - In this work, a method for species-specific isotopic analysis of sulfur via capillary electrophoresis hyphenated on-line with multicollector ICP-MS (CE/MC-ICP-MS) was developed. Correction for the mass bias caused by instrumental mass discrimination was realized via external correction with multiple-injection sample-standard bracketing. By comparing the isotope ratio measurement results obtained using the newly developed on-line CE/MC-ICP-MS method with those obtained via traditional MC-ICP-MS measurement after analyte/matrix separation by anion exchange chromatography for isotopic reference materials and an in-house bracketing standard, the most suitable data evaluation method could be identified. The repeatability for the sulfate-δ34S value (calculated from 18 measurements of a standard conducted over seven measurement sessions) was 0.57‰ (2SD) and thereby only twice that obtained with off-line measurements (0.30‰, n = 68). As a proof of concept for analysis of samples with a real matrix, the determination of the sulfur isotopic composition of naturally present sulfate was performed for different river systems. The CE/MC-ICP-MS results thus obtained agreed with the corresponding off-line MC-ICP-MS results within the 2SD ranges, and the repeatability of consecutive δ34S measurements (n = 3) was between 0.3‰ and 1.3‰ (2SD). Finally, the isotopic analysis of two different S-species in a river water sample spiked with 2-pyridinesulfonic acid (PSA) was also accomplished. KW - River water sulfate KW - Environmental speciation KW - Sulfur isotopes KW - On-line CE/MC-ICP-MS KW - Multiple-injection sample-standard bracketing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509549 DO - https://doi.org/10.1007/s00216-020-02781-8 SN - 1618-2642 VL - 412 IS - 23 SP - 5637 EP - 5646 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-50954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmed, R. A1 - Vaishampayan, A. A1 - Cuellar-Camacho, J. L. A1 - Wight, D. J. A1 - Donskyi, Ievgen A1 - Unger, Wolfgang A1 - Grohmann, E. A1 - Haag, R. A1 - Wagner, O. T1 - Multivalent Bacteria Binding by Flexible Polycationic Microsheets Matching Their Surface Charge Density N2 - Aiming at the overall negative surface charge of bacteria, a new strategy of antibacterial agents based on large polymer-modified graphene oxide (GO) sheets is assessed. The presented flexible, polycationic Sheets match the size and charge density of the Escherichia coli surface charge density (2 × 1014 cm−2). These matching parameters create an unspecific but very strong bacteria adsorber by multivalent, electrostatic attraction. Their interaction with bacteria is visualized via atomic force and confocal microscopy and shows that they effectively bind and wrap around E. coli cells, and thereby immobilize them. The incubation of Gram-negative and -positive bacteria (E. coli and methicillin-resistant Staphylococcus aureus, MRSA) with these polycationic sheets leads to the inhibition of proliferation and a reduction of the colony forming bacteria over time. This new type of antibacterial agent acts in a different mode of Action than classical biocides and could potentially be employed in medicinal, technical, or agriculture applications. The presented microsheets and their unspecific binding of cell interfaces could further be employed as adsorber material for bacterial filtration or immobilization for imaging, analysis, or sensor technologies. KW - Surface charge KW - Bacteria KW - Graphene oxide KW - Escherichia coli KW - XPS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509651 DO - https://doi.org/10.1002/admi.201902066 VL - 7 IS - 15 SP - 1902066 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - Damage Quantification in Aluminium-CFRP Composite Structures using Guided Wave Wavenumber Mapping N2 - The use of composite materials is associated not only with the advantages of weight reduction and improved structural performance but also with the risk of barely visible impacts or manufacturing damages. One of the promising techniques for the detection and characterisation of such damages is based on ultrasonic guided wave propagation and analysis. However, the multimodal nature and dispersive behaviour of these waves make their analysis difficult. Various signal processing techniques have been proposed for easier interpretation of guided wave signals and extraction of the necessary information about the damage. One of them is the wavenumber mapping which consists of creating a cartography of the wavenumber of a propagating mode over an inspected area, using a dense wavefield acquisition measured for example with a scanning laser Doppler vibrometer. This technique allows both the quantification of the in-plane size and the depth of damage, for example, impact-induced delamination in composite laminates. In this contribution, wavenumber mapping is applied to a delaminated aluminium-CFRP composite structure which corresponds to composite-overwrapped pressure vessels used for storing gases in aerospace and automotive industries. The analysis of experimental data obtained from measurements of guided waves propagating in an aluminium-CFRP composite plate with impact-induced damage is performed. The output of the imaging is a three-dimensional representation of the delamination induced by the impact. Good agreement between conventional ultrasonic testing and guided wave damage mapping can be found. T2 - 11th International Symposium on NDT in Aerospace CY - Paris Saclay, France DA - 13.11.2019 KW - Damage assessment KW - Lamb waves KW - Multilayered structures KW - Wavefield analysis KW - Impact damage PY - 2019 AN - OPUS4-49662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya A1 - Mesnil, Olivier A1 - Bulling, Jannis A1 - Prager, Jens A1 - Boller, C. T1 - Damage Quantification in Aluminium-CFRP Composite Structures using Guided Wave Wavenumber Mapping N2 - The use of composite materials is associated not only with the advantages of weight reduction and improved structural performance but also with the risk of barely visible impacts or manufacturing damages. One of the promising techniques for the detection and characterisation of such damages is based on ultrasonic guided wave propagation and analysis. However, the multimodal nature and dispersive behaviour of these waves make their analysis difficult. Various signal processing techniques have been proposed for easier interpretation of guided wave signals and extraction of the necessary information about the damage. One of them is the wavenumber mapping which consists of creating a cartography of the wavenumber of a propagating mode over an inspected area, using a dense wavefield acquisition measured for example with a scanning laser Doppler vibrometer. This technique allows both the quantification of the in-plane size and the depth of damage, for example, impact-induced delamination in composite laminates. In this contribution, wavenumber mapping is applied to a delaminated aluminium-CFRP composite structure which corresponds to composite-overwrapped pressure vessels used for storing gases in aerospace and automotive industries. The analysis of experimental data obtained from measurements of guided waves propagating in an aluminium-CFRP composite plate with impact-induced damage is performed. The output of the imaging is a three-dimensional representation of the delamination induced by the impact. Good agreement between conventional ultrasonic testing and guided wave damage mapping can be found. T2 - 11th International Symposium on NDT in Aerospace CY - Paris Saclay, France DA - 13.11.2019 KW - Damage assessment KW - Lamb waves KW - Multilayered structures KW - Wavefield analysis KW - Impact damage PY - 2019 SP - 33 AN - OPUS4-49663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Trainingsworkshop Datenanalyse N2 - Wir laden zum Trainingsworkshop Datenanalyse ein. Angetrieben durch die Digitalisierung und die sogenannte Industrie 4.0 steigt die Erwartungshaltung gegenüber der Nutzung von Daten. Die Unsicherheit, Widersprüchlichkeit und Redundanz separat verarbeiteter einzelner Quellen soll durch die synergetische Zusammenführung heterogener Datensätze überwunden werden. Dabei steht der zunehmenden Aufgabenkomplexität eine ebenso zunehmende Verfügbarkeit an Daten und Analyseverfahren gegenüber. Der Workshop vermittelt ein konzeptionelles Verständnis für moderne Datenanalyseverfahren (Machine Learning (ML), Multivariate Statistik) und soll durch ein anschließendes Hands-On Training mit Python (https://www.python.org) einen einfachen Einstieg in die Thematik ermöglichen. Der Kurs richtet sich an den wissenschaftlichen Nachwuchs. T2 - Trainingsworkshop KDA: Schwerpunkt Machine Learning und Python CY - Berlin, Germany DA - 03.06.2019 KW - KDA Training KW - Data Analysis KW - Machine Learning PY - 2019 AN - OPUS4-49860 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kepes, E. T1 - Tomography of asymmetrical laser-induced plasmas N2 - Asymmetrical laser-induced plasmas were investigated by a tomography approach based on the inverse Radon transform. Two distinct sources of asymmetricity were investigated: double-pulsed laser-induced plasmas in the orthogonal configuration and single-pulsed laser-induced plasmas under an inclined incidence angle. Both cases were observed at various delay times. The optical thinness of the laser-induced plasmas was achieved by appropriately adjusting the pulse energies. High temporal resolution is achieved by a gated intensified charge-coupled-device camera. The asymmetrical laser-induced plasmas are investigated in terms of their total emissivity, spectrally resolved emissivity, and temperature. The latter is obtained by the Saha–Boltzmann plot method. The images required for the inverse Radon transform technique were obtained with a high angular accuracy and reproducibility provided by mounting the spectrometer on a high-precision nano-positioning rotary stage. The plasmas were induced in the center of rotation of the stage. This arrangement allows the reconstruction of emissivity, which is integrated over a full spectral range (200-800 nm) or over a desired spectral range selected by a bandpass filter (~10 nm). It also allows for the reconstruction of spectrally-resolved emissivity in each cross sectional plasma slice by scanning the plasma across a spectrometer slit. The 3D maps of temperature and electron density are thus obtained for different types of asymmetric plasmas. T2 - 10th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy CY - Brno, Czech Republic DA - 08.09.2019 KW - Plasma diagnostics KW - Laser induced plasma KW - LIBS PY - 2019 AN - OPUS4-49834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas A1 - Wack, Y. A1 - Mook, G. T1 - Simulation of an instrumented ultrasonic test run with a rail inspection train N2 - Rail inspection performed by ultrasonic rail inspection trains is a complex and challenging process. A large number of variables and parameters given by the environment, the track and the testing-system have an influence on the overall performance of the inspection and the inspection result. Typically the parameter vary in a combination depending on the track condition. To evaluate the individual influence of each relevant variable, simulation tools can be used. Therefore the entire inspection process has to be transferred into a model using combined modelling techniques. The goal of this work is to model an instrumented ultrasonic test run with a rail inspection train with the parameters varied by a script over a virtually driven distance. T2 - 46th Annual Review of Progress in Quantitative Nondestructive Evaluation- QNDE 2019 CY - Portland, OR, USA DA - 14.07.2019 KW - Ultrasound KW - Rail inspection KW - Modelling KW - Simulation PY - 2019 VL - 2019 SP - 1 EP - 3 AN - OPUS4-49839 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhattacharya, Biswajit A1 - Das, S. A1 - Lal, G. A1 - Soni, S. R. A1 - Ghosh, A. A1 - Reddy, C. M. A1 - Ghosh, S. T1 - Screening, crystal structures and solubility studies of a series of multidrug salt hydrates and cocrystals of fenamic acids with trimethoprim and sulfamethazine N2 - Multidrug solids have a potential use to efficiently treat and control a superfluity of medical conditions. To address the current drawbacks of drug development in R&D, it was targeted to achieve new pharmaceutical solid forms of fenamic acids having improved solubility and thermal stability. Subsequently, five new multicomponent solids consisting of three salt hydrates of trimethoprim (TMP) with mefenamic acid (TMP-MFA-H2O), tolfenamic acid (TMP-TFA-H2O) and flufenamic acid (TMP-FFA-H2O), and two cocrystals of sulfamethazine (SFZ) with flufenamic acid (SFZ-FFA) and niflumic acid (SFZ-NFA) were prepared by liquid assisted grinding. Looking at the structures of active pharmaceutical ingredient (API) molecules, it was quite expected that a wide range of supramolecular synthons would lead to cocrystallization. New forms were characterized thoroughly by various solid-state techniques, including single crystal X-ray diffraction (SCXRD), which provided details of hydrogen bonding, molecular packing and interactions between drug and coformer. Kinetic solubility at pH 7.4 buffer study has been carried out and a comparison is made with respect to the parent drugs. A significant enhancement of NSAIDs solubility was observed in all salt hydrate systems of TMP. Thus with increasing physicochemical properties such as improved solubility further leads to the enhancement of bioavailability, which has implications to overcoming the formulation related problems of active pharmaceutical ingredients (APIs). KW - Cocrystals KW - Crystal engineering KW - Solubility PY - 2020 DO - https://doi.org/10.1016/j.molstruc.2019.127028 SN - 0022-2860 VL - 1199 SP - 127028 PB - Elsevier B.V. AN - OPUS4-49873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bhattacharya, Biswajit A1 - Michalchuk, Adam A1 - Emmerling, Franziska T1 - Revealing Mechanical Plastic Bending in Coordination Polymer Crystals N2 - Crystalline molecular materials with mechanical flexibility are promising for technological development. This is particularly true for the development of advanced materials with optoelectronic and biomedical applications. While a growing number of mechanically flexible crystalline molecular materials are being reported,1 they remain scarce. At present, most discoveries are serendipitous, as limited design strategies are currently known. Amongst these strategies Desiraju et. al. suggested that elastic materials must contain herringbone structures.2 For plastic crystals, the so-called ‘shape-synthon’ strategy has been developed, in which weak non-covalent interactions are introduced into structures to facilitate mobility of molecules.3 This includes formation of slip planes. Generally, these models have performed very well at predicting and rationalizing the mechanical properties of new materials. Recently, however, a family of one-dimensional covalent networks (coordination polymers; CPs) has been described, which show mechanical elasticity. With drastically different structural chemistry, these systems do not seem to adhere to the currently established rules. Herein, we present the first such system: a plastically bendable crystal of a 1D CP, [Zn(-Cl)2(3,5-Cl2Py)2]n (where 3,5-Cl2Py = 3,5-dichloro pyridine). This CP crystallizes in a tetragonal, and can therefore be bent over two major faces to acute angles without fracturing. We conducted bending and indentation experiments to quantify the mechanical properties of the CP crystal. This was complimented by Vibrational (Raman and Terahertz) spectroscopy and theoretical calculations for deeper understanding of molecular level structural deformation. T2 - 32nd European Crystallographic Meeting (ECM32) CY - University of Vienna, Vienna, Austria DA - 18.08.2019 KW - Mechanical Flexiblity KW - Crystal engineering KW - Coordination Polymers PY - 2019 AN - OPUS4-49875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Combining Broadband Dielectric Spectroscopy with advanced calorimetry to reveal the multiple glass transitions in discotic liquid crystals N2 - Broadband dielectric spectroscopy and advanced calorimetry were combined to investigate the molecular dynamics of discotic liquid crystals T2 - Flash DSC Conference CY - Zurich, Switzerland DA - 24.11.2019 KW - Discotic Liquid Crystals PY - 2019 AN - OPUS4-49879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Air-coupled ultrasonic sensors N2 - We present an overview of air-coupled ultrasonic transducers. T2 - Workshop BAM-IWF CY - Berlin, Germany DA - 25.11.2019 KW - Air-coupled transducers KW - Ferroelectret KW - Thermoacoustics KW - Plasma PY - 2019 AN - OPUS4-49806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hirsch, Philipp Daniel T1 - Verbesserung der Tiefenreichweite der Impuls-Thermografie mithilfe von Hochleistungs-Laser-Array, kHz-Kamera und Virtual-Wave-Konzept N2 - Im weitverbreiteten Fall der thermografischen ZfP sollen Defekte im Probeninneren detektiert werden. Da diese eine Inhomogenität darstellen, genügt jegliche Mess- und Datenverarbeitungstechnik, die diese Inhomogenität als Kontrast in der transienten Temperaturverteilung herausarbeitet. Ein üblicher Ansatz ist eine extrem kurze und intensive Blitzlampenbeleuchtung zusammen mit einer nachträglichen Fourier-Transformation zu verwenden. Für die zusätzliche Tiefenbestimmung werden entweder rein phänomenologische Ansätze, semi-analytische Ansätze mit Kalibrationsmessungen oder Fits an analytische bzw. numerische Modelle verwendet. Ein üblicher semi-analytischer Ansatz ist z.B. die Analyse des Abknickens der transienten Abkühlkurve. Problematisch ist das schnelle Abklingen der Amplitude auf Rauschniveau und damit die inhärente Beschränkung der Tiefenreichweite. Eine äquivalente Beschreibung der Wärmeleitung ist über sehr stark gedämpfte thermische Diffusionswellen möglich. Die Eindringtiefe ist dann gleich der thermischen Diffusionslänge. Der semi-analytische Ansatz über normales Least-Squares-Fitting funktioniert für 1D-Schicht-Systeme sehr gut, versagt aber für höherdimensionale Messprobleme. Genau hier setzt eine seit Kurzem bekannte Transformation der diffusen Temperaturentwicklung (bzw. des Realteils der Diffusionswelle) in eine propagierende virtuelle Temperaturwelle an. Dieses sog. Virtual-Wave-Konzept stellt sich selbst als ein weiteres inverses Problem dar. Der Nutzen dieser in einer linearen virtuellen Zeitdomäne propagierenden Welle überkompensiert den numerischen Mehraufwand jedoch deutlich. Zusammen mit neuen Technologien in der Erwärmung durch Hochleistungs-Laser-Arrays und in der Datenakquisition durch kHz-Kameras erlaubt dieser Ansatz eine signifikante Verbesserung der Tiefenreichweite in der Impuls-Thermografie. Im Beitrag werden experimentelle Ergebnisse an einer additiv hergestellten Metallprobe mit überdeckten Schlitzen vorgestellt, die eine Detektion dieser Defekte bis zu einem Seitenverhältnis von Defektbreite/Defekttiefe ~ 0,25 erlauben, also ca. 4 mal tiefer als die übliche Faustformel. T2 - Thermografie Kolloquium CY - Halle, Germany DA - 19.09.2019 KW - Laserthermografie KW - Virtuelle Welle KW - VCSEL PY - 2019 AN - OPUS4-49809 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meermann, Björn A1 - Faßbender, Sebastian T1 - Antifoulingmittel im Wasser N2 - Für das Biozid Zink-Pyrithion, das in Schiffsanstrichen weit verbreitet ist, fehlten bisher die analytischen Methoden, um den Komplex und seine Abbauprodukte in der Umwelt nachzuweisen. Kapillarelektrophorese, gekoppelt mit komplementärer Massenspektrometrie könnte dieses Problem lösen. KW - Antifouling-Biozide KW - Kapillarelektrophorese-Massenspektrometrie KW - Komplementäre Massenspektrometrie KW - Umwelt-Speziation PY - 2019 DO - https://doi.org/10.1002/nadc.20194088793 SN - 1439-9598 SN - 1868-0054 VL - 67 IS - 12 SP - 56 EP - 58 PB - Wiley-VCH CY - Weinheim AN - OPUS4-49789 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Boehm, Rainer T1 - Phased Array und Imaging, zwei raumzeitliche Interferenzverfahren N2 - Phased-Array-Technik und Bildgebung mit Ultraschallwellen sind nach langer Entwicklungszeit inzwischen auf dem Weg zu allgemeiner Verbreitung. Daher bietet sich an, die verschiedenen Techniken und deren Begriffe wie z.B. Phased-Array, SAFT, TFM, FMC und Sparse-Array zusammenfassend in Beziehung zu setzen. All diesen Techniken liegt dieselbe Idee zu Grunde, nämlich durch gezielte Überlagerung von Ultraschallsignalen den gewünschten Effekt zu erreichen. Die verschiedenen Techniken werden kurz charakterisiert und neben den Unterschieden wird beschreiben, auf welche Weise bei all diesen Techniken das Phänomen der konstruktiven Interferenz jeweils genutzt wird. T2 - Ultraschall-Array-Technologien und ihre Anwendungen, Seminar des FA Ultraschallprüfung der DGZfP CY - Berlin, Germany DA - 04.11.2019 KW - Phased Array KW - Imaging KW - Synthetic Aperture Focusing Technique KW - Total Focusing Methode KW - Full Matrix Capture PY - 2019 UR - https://www.dgzfp.de/seminar/ultraschall# AN - OPUS4-49791 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bulling, Jannis A1 - Gravenkamp, H. T1 - Comparison of different models for stress singularities in higher order finite element methods for elastic waves N2 - In this contribution, we present three models to capture singularities in combination with the Spectral Element Method. The first model, the continued-fraction-based Scaled Boundary Finite Element Method, the second model, a new approach based on enrichment with static modes, and the third model, which uses an hp-refinement near the singularity, are compared among each other and evaluated in terms of their respective efficiency and accuracy. T2 - GAMM 2019 CY - Wien, Austria DA - 18.02.2019 KW - Enriched finite element method KW - Scaled boundary finite element method PY - 2019 DO - https://doi.org/10.1002/pamm.201900095 VL - 19 IS - 1 SP - 1 EP - 2 PB - Wiley-VHC AN - OPUS4-49794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Identification of Transformation Products of Warfarin N2 - Warfarin, also known as Coumadin is one of the most popular anticoagulant drugs used as a therapeutic in humans to prevent thrombosis, atrial fibrosis, and fibrillation since the 1950s. Because of its ability to hinder blood from clotting by blocking vitamin K-depending carboxylation of blood clotting precursors, it is also used as a rodenticide worldwide. Until today it has been partially substituted by far more potent anticoagulant rodenticides (ARs), so-called superwarfarins. There are numerous references confirming secondary and tertiary poisoning in non-target-animals and wildlife like mammals, birds, and fish associated with ARs. Up to now relatively little is known about persistence and toxicity of transformation products of those AR in the environment and food chain. Herein, warfarin was chosen as a model compound to determine andelucidate TPs which are generated technically and under environment-like conditions. Such as the simulation of the oxidative phase I metabolism by implementing electrochemical flow cells coupled to mass spectrometry (MS). Obtained results are being compared to TPs generated by UVB-irradiation and ozonation. Analysis and separation of degradation products and TPs were achieved by a variety of gas- and liquid chromatographic techniques coupled to (high resolution) MS. T2 - Goldschmidt 2019 CY - Barcelona, Spain DA - 18.08.2019 KW - GC-MS KW - Warfarin KW - Transformations products PY - 2019 AN - OPUS4-49795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis T1 - Simulation von Wechselwirkungen von geführten Wellen mit Fehlstellen N2 - In der Zerstörungsfreien Prüfung und der Zustandsüberwachung sind geführte Wellen von großem Interesse, um Fehlstellen zu finden und zu charakterisieren. Die Interaktion der Wellen mit den Fehlstellen kann dabei aufgrund ihrer Komplexität häufig nicht analytisch beschrieben werden. Dies macht numerische Programme neben Experimenten unabdingbar. Aufgrund der kleinen Wellenlänge im Verhältnis zur Bauteilgröße ist jedoch eine effiziente Simulation noch immer Teil der aktiven Forschung. Um die Effizienz der Simulationsalgorithmen zu steigern, ist es möglich, analytische Annahmen in die Finite Elemente Methode (FEM) zu integrieren. Beispiele für solche Methoden sind die Scaled Boundary Finite Element Method als ein semi-analytisches Verfahren und eXtended Finite Element Method. Diese beiden Möglichkeiten erlauben es, die Wechselwirkungen effizient zu simulieren. In diesem Beitrag werden verschiedene Wechselwirkungen und Auswertungsmöglichkeiten von geführten Wellen mit Fehlstellen vorgestellt. Hierbei liegt der Fokus auf linearen und nicht-linearen Effekten. Zunächst wird auf Modenkonversion eingegangen und der Frage nachgegangen, ob diese ausreicht, um einen Riss zu charakterisieren. Diese Untersuchungen motivieren dann ein inverses Verfahren, mit dem einige Parameter eines simulierten Risses in einer Folge von Simulationen wieder rekonstruiert werden. Ein zweiter Teil beschäftigt sich mit nicht-linearen Risseffekten. Diese Risseffekte erzeugen im allgemeinen höhere harmonische Wellen. Hier werden Ergebnisse und Filtermethoden zur Auswertung vorgestellt. T2 - Doktorandenseminar "Geführte Wellen" CY - Delbrück, Germany DA - 21.10.2019 KW - Singular stress KW - Enriched finite element method KW - Scaled boundary finite element method; Stress intensity factors PY - 2019 AN - OPUS4-49798 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Beschreibung des Verhaltens von organischen Schadstoffen unter umweltrelevanten Bedingungen N2 - Zu den letzten beiden Jahrestagungen der GUS wurden Verfahren und Methoden vorgestellt, die es gestatten, den Transfer von Schadstoffen aus Materialien und Produkten in die Umwelt unter umweltrelevanten Bedingungen beschreiben zu können. Dabei lag der Fokus auf den Materialien und der eingesetzten Umweltsimulationen. In einem sich anschließenden Schritt soll nun das Verhalten der freigesetzten organischen Schadstoffe unter den Bedingungen von realen und simulierten Umwelteinflüssen charakterisiert und beschrieben werden. Hier werden im Detail drei potentielle Schadstoffe betrachtet, die Inhaltsstoffe bzw. Additive in den jeweils eingesetzten Materialien sind. Im Falle von Polypropylen (PP) und Polystyrol (PS) handelt es sich um polybromierte Flammschutzmittel BDE 209 (Decabrom-diphenylether, als Einzelsubstanz) und HBCD (Hexabromcyclododecan, als technische Formulierung). Für das eingesetzte Polycarbonat ist BPA (Bisphenol A) als Schadstoff zu definieren, welcher unter umweltrelevanten Bedingungen freigesetzt wird. Im Rahmen der durchzuführenden Arbeiten sollen die aufgeführten prioritären Schadstoffe hinsichtlich möglicher Transformationsprozesse in Umwelt und Klärwerk charakterisiert werden. Die unter den Bedingungen der Ozonung, Chlorierung und UV-Bestrahlung erhaltenen Transformationsprodukte (TPs) sollen im Sinne einer Non-Target-Analytik identifiziert und eindeutig charakterisiert werden. Die Ergebnisse sollen mittels vorhandener Analysenverfahren, wie GC-EI-MS, HPLC-ESI-IT-MSn bzw. LC-MS/MS erzeugt bzw. abgesichert werden. Anhand der in der Struktur eindeutig zu beschreibenden Transformationsprodukte und der Charakterisierung von potentiellen Intermediaten sollen belastbare Reaktionswege und –mechanismen abgeleitet werden. T2 - 48. Jahrestagung der GUS CY - Blankenloch-Stutensee, Germany DA - 27.03.2019 KW - Transformationsprodukte KW - Schadstoffe KW - Umweltverhalten PY - 2019 AN - OPUS4-49799 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schönhals, Andreas ED - Zorn, R. T1 - Quasi-elastic scattering of high free volume polymers by neutron time-of-flight spectroscopy N2 - Neutron backscattering experiments have been carried out on a polymer of intrinsic microporosity KW - Polymers of Intrinsic Microporosity PY - 2019 SP - 1 EP - 2 CY - Garching AN - OPUS4-49852 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haller, T. A1 - Völker, Christoph A1 - Hartmann, T. T1 - Machine learning based multi-sensor fusion for the nondestructive testing of corrosion in concrete N2 - Half-cell potential mapping (HP) is the most popular non-destructive testing method (NDT) for locating corrosion damage in concrete. It is generally accepted that HP is susceptible to environmental factors caused by salt-related deterioration, such as different moisture and chloride gradients. Additional NDT methods are able to identify distinctive areas but are not yet used to estimate more accurate test results. We present a Supervised Machine Learning (SML) based approach to data fusion of seven different signal features to obtain higher quality information. SMLs are methods that explore (or learn) relationships between different (sensor) data from predefined data labels. To obtain a representative, labelled data set we conducted a comprehensive experiment simulating the deterioration cycle of a chloride exposed device in the laboratory. Our data set consists of 18 measurement campaigns, each containing HP, Ground Penetrating- Radar, Microwave Moisture and Wenner resistivity data. We compare the performance of different ML approaches. Many outperform the best single method, HP. We describe the intrinsic challenges posed by a data-driven approach in NDT and show how future work can help overcome them. T2 - SMAR2019 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures CY - Potsdam, Germany DA - 27.08.2019 KW - Machine Learning KW - NDT KW - Half-Cell Potential Mapping KW - Corrosion KW - Reinforced Concrete KW - Data Fusion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498563 UR - http://www.ndt.net/?id=24890 VL - 25 IS - 1 SP - 24890-1 EP - 24890-8 PB - NDT.net CY - Kirchwald AN - OPUS4-49856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Genath, A. A1 - Hofmann, Michael A1 - Tiebe, Carlo A1 - Einspanier, R. T1 - Auf dem Weg zum Monitoring der Ameisensäurekonzentration in der Bienenstock-Luft mit einem Multigassensorsystem N2 - Die Varroose gilt weltweit als eine der bedeutendsten Erkrankungen der westlichen Honigbiene, Apis mellifera. Verursacht wird sie durch den Ektoparasiten Varroa destructor, der durch Saugen der Hämolymphe und Virenübertragung sowohl die Bienenbrut als auch die adulten Individuen schädigt. Ohne imkerliche Unterstützung gehen betroffene Bienenvölker in der Regel innerhalb von drei Jahren ein. Als bewährte, häufige Behandlung wird flächendeckend 60%ige Ameisensäure (AS) - im Bienenstock appliziert über verschiedene Verdampfungssysteme - eingesetzt. Sie wirkt als einziger zugelassener Stoff gegen die Varroamilbe auch in die verdeckelte Brut hinein und birgt kein Risiko der Resistenzentwicklung. Allerdings ist das therapeutische Fenster, der Bereich zwischen Milbenabtötung und Bienenschädigung, relativ schmal und die tatsächliche AS-Konzentration im Bienenstock stark abhängig von äußeren Einflussfaktoren, wie Temperatur, Luftfeuchte oder Applikationsart. Eine Bestimmung der exakten AS-Konzentration im Bienenstock ist also notwendig, um einerseits das Wirkungsoptimum zu bestimmen und andererseits bei Übersteigen der Maximalkonzentrationen mit Folge-Schädigung der Bienen, ein rechtzeitiges Eingreifen der Imker zu ermöglichen. T2 - 6. HSN-Fachsymposium „Innovative Sensorik, verteilte Sensorsysteme, neue Technologien und Anwendungsfelder“ CY - Karlsruhe, Germany DA - 06.11.2019 KW - Biene KW - Apis mellifera KW - Varroa destructor KW - Ameisensäure KW - Multigassensorik PY - 2019 AN - OPUS4-49606 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frunza, S. A1 - Frunza, L. A1 - Ganea, C. P. A1 - Zgura, I. A1 - Schönhals, Andreas T1 - Density of adsorbed surface species for cyanophemyl benzoates confined to Aerosil 380: Development of the evaluating algorithm for Attachment by two types of bonds N2 - We found previously how to estimate the density of the adsorbed surface species in the case of the molecules interacting to the oxide support surface by one type of bond. Here this algorithm is developed for the case of the molecules which can be bonded to the support surface by two types of bonds. The adsorption assumptions are similar to those considered in the case of only one type of bond. The calculation is exemplified for some composites of cyanophenyl alkylbenzoates (CPnBs) (n is the number of carbon atoms in the alkyl chain) interacting with Aerosil A380. The interaction takes place by hydrogen bonding between the –OH groups or the support and the functional groups of the CPnB molecules. The estimated values of the total surface density of CPnBs agree well with those found for the composites containing related but simpler molecules. KW - Surface species PY - 2019 SN - 1223-7027 VL - 81 IS - 4 SP - 232 EP - 236 PB - University Politehnica of Bucharest CY - Bucharest AN - OPUS4-49615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - X-ray fluorescence imaging with coded apertures N2 - Our aim is to develop a new simple and inexpensive method for full field X-ray fluorescence imaging . We combine an energy dispersive array detector with a coded aperture to obtain high resolution images . To obtain the information from the recorded image a reconstruction step is necessary . The reconstruction methods we have developed , were tested on simulated data and then applied to experimental data . The first tests were carried out at the BAM line @ BESSY II. This method enables the simultaneous detection of multiple elements , which is important e.g. in the field of catalysis. T2 - Adlershofer Forschungsforum CY - Berlin, Germany DA - 11.11.2019 KW - X-ray KW - Fluorescence KW - Imaging KW - Spectroscopy KW - Coded aperture PY - 2019 AN - OPUS4-49695 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska T1 - Acoustic Emission Monitoring of materials, production processes, infrastructures N2 - Acoustic Emission testing is a usable tool for failure Analysis of materials as well as to monitor infrastructurs or production processes. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures CY - Potsdam, Germany DA - 27.08.2019 KW - Acoustic Emission (AE) KW - Laser Metal Deposition (LMD) KW - Pipeline KW - NDT Monitoring PY - 2019 AN - OPUS4-49696 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - An automated single algae-ICP-ToF-MS Approach for the Investigation of Metal Uptake in Diatoms N2 - Entwicklung neuer ökotoxikologischer Bewertungsmethoden auf der Basis der automatisierten single cell-ICP-ToF-MS T2 - CANAS CY - Freiberg, Germany DA - 23.09.2019 KW - Automated single cell-ICP-ToF-MS KW - Diatoms KW - Ecotoxicological Assessment PY - 2019 AN - OPUS4-49744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - HR-CS-GFMAS als leistungsstarkes Werkzeug zur Analyse von organisch gebundenem Fluor (EOF) in Oberflächengewässern N2 - Entwicklung einer off-line SPE HR-CS-GFMAS basierten Methode zur Analyse von extrahierbar organisch gebundenem Fluor (EOF) in Oberflächengewässern T2 - Analytik Jena Forum CY - Berlin, Germany DA - 24.10.2019 KW - HR-CS-GFMAS KW - Extrahierbar organisch gebundenes Fluor (EOF) KW - Oberflächengewässer PY - 2019 AN - OPUS4-49745 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - An automated single algae-ICP-ToF-MS approach for the Investigation of Metal Uptake in Diatoms N2 - Entwicklung einer automatisierten single cell-ICP-ToF-MS Methode zur Analyse von metallexponierten Diatomen. T2 - CANAS CY - Freiberg, Germany DA - 23.09.2019 KW - Single cell-ICP-ToF-MS KW - Multivariate Datenauswertung KW - Diatom PY - 2019 AN - OPUS4-49748 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Borovinskaya, O. A1 - Büchel, C. A1 - Meermann, Björn T1 - Der Fingerabdruck der Kieselalge N2 - Elementanalytische Verfahren werden heute zu mehr eingesetzt als bloß zur Bestimmung von Metallgesamtgehalten in diversen Probenmatrizes. Sie stellen heute ein wichtiges Werkzeug zur Beantwortung lebenswissenschaftlicher Fragen aus Umwelt, Medizin und Biologie dar. In der vorliegenden Arbeit kommt die single-cell-ICP-Flugzeitmassenspektrometrie (single-cell-ICP-TOF-MS) zur Multielementanalytik in einzelnen Kieselalgen (Diatomeen) zum Einsatz und wird zukünftig ein wichtiges Werkzeug z.B. bei der Beantwortung ökotoxikologischer Fragestellung sein. KW - Diatomeenanalytik KW - Single cell-ICP-ToF-MS KW - Multielementanalytik in kurzen transienten Signalen PY - 2019 UR - https://q-more.chemie.de/q-more-artikel/299/der-fingerabdruck-der-kieselalge.html SP - 1 EP - 3 PB - LUMITOS AN - OPUS4-49749 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Meermann, Björn T1 - Screening von Organofluorverbindungen im Oberflächenwasser N2 - Organofluorverbindungen kommen in vielen Bereichen zum Einsatz und gelangen in die aquatische Umwelt. Die Belastungssituation der Gewässer ist bisher wenig untersucht – hier kommt die HR-CS GF MAS als leistungsstarkes Screeningtool zum Einsatz. KW - HR-CS-GFMAS KW - Extrahierbar organisch gebundenes Fluor (EOF) KW - Oberflächengewässer PY - 2019 UR - https://analytik.news/Fachartikel/Volltext/bam5.pdf SP - 1 EP - 3 PB - Dr. Beyer Internet-Beratung AN - OPUS4-49750 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas A1 - Bertovic, Marija A1 - Rosenthal, Martina A1 - Pavlovic, M. A1 - Bartsch, L. A1 - Muhs, V. A1 - Holstein, R. T1 - Zuverlässigkeitsbetrachtungen bei der Ultraschallprüfung von Radsatzwellen im Ausbildungsbetrieb N2 - Im Rahmen der UT1-M1 Ausbildung im Ausbildungszentrum Wittenberge der DGZfP wurden statistische Untersuchungen am Beispiel der Radsatzwellenprüfung mit Testradsatzwellen durchgeführt. Diese Untersuchungen hatten zum Ziel, die wesentlichen Einflussparameter bei der Prüfung auf das Prüfergebnis zu evaluieren. Dabei wurde unter anderem die intrinsische Fähigkeit des Prüfverfahrens zum Auffinden verschiedener Reflektorgeometrien ermittelt. Die Ergebnisse der Handprüfung wurden mit Ergebnissen mechanisierter Prüfungen verglichen. Im Rahmen der Zuverlässigkeitsbetrachtung wurden die Probability of Detection (POD) und die Nachweisgrenzen ermittelt. Ziel dieser Arbeit war es auch, menschliche und organisatorische Einflussfaktoren auf die Ultraschall-Handprüfung von Radsatzwellen zu identifizieren, um Empfehlungen zur Optimierung der Ausbildung auszuarbeiten. Dazu wurden prüfungsbezogene Risiken in der Praxis mittels Fehlzustandsart- und –auswirkungsanalyse (FMEA) analysiert sowie von den Prüfern empfundene Probleme während der Ausbildung und in der Praxis mittels Fragebogen identifiziert. Die Ergebnisse der FMEA haben gezeigt, dass während des gesamten Prozesses Fehler auftreten können, für die Gegenmaßnahmen getroffen und implementiert werden sollten. Aus den Hinweisen und Erkenntnissen wurden einige Empfehlungen zur Optimierung der Ausbildung erarbeitet. T2 - DGZfP DACH Tagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Zuverlässigkeit KW - Wellenprüfung KW - Ultraschall PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496783 VL - 2019 SP - 1 EP - 11 AN - OPUS4-49678 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Berthold, J. A1 - Vrana, J. A1 - Heckel, Thomas A1 - Kanzler, D. A1 - Jatzlau, P. A1 - Große, C. T1 - Modellgestützte Bestimmung der Auffindwahrscheinlichkeit (POD) von Reflektoren bei der Ultraschallprüfung großer Schmiedeteile N2 - Bruchmechanische Untersuchungen werden zur Vorhersage der Lebensdauer und der Wartungszyklen benutzt. Dabei wird davon ausgegangen, dass auch Objekte ohne detektierte Anzeigen Materialfehler mit einer Reflektivität kleiner der Nachweisgrenze aufweisen können. Keine detektierte Anzeige bedeutet daher für Bauteilauslegung, dass sie eine konservative Annahme machen müssen: es wird angenommen, dass das Bauteil Materialfehler in Größe der Nachweisgrenze enthält. Dies macht die Nachweisgrenze zu dem die Lebensdauer limitierenden Faktor. Bei probabilistischen Methoden wird zusätzliches Wissen, wie Zuverlässigkeit und Fehlerauffindwahrscheinlichkeiten bei der zerstörungsfreien Prüfung mit in die Berechnung einbezogen, um zu konservative Annahmen zu vermeiden. Ziel ist es eine Model-Assisted-POD aufzubauen mit der die reale volumetrische Ultraschallprüfung großer Schmiedeteile nachgebildet werden kann. Die resultierende POD soll im Weiteren in bruchmechanischen Betrachtungen Verwendung finden. In vorangegangenen Arbeiten [Preißel2015] wurde dazu der Einfluss des Prüfrasters nach der DGZfP-Richtlinie US 07:2014 auf die Fehlerauffindwahrscheinlichkeit (parametrisch) simulativ betrachtet und die Simulationstechnik experimentell validiert. In diesem Paper werden die Ergebnisse von Preißel überprüft und um eine Prüfraster-Summen-POD, die das Szenario der realen Bauteilprüfung beschreibt, erweitert. Zudem wird eine experimentell validierte, simulative, nicht-parametrische POD für schrägliegende Defekte aufgebaut. Schließlich werden erste Untersuchungen zur Defektmorphologie vorgestellt. Diese Arbeit ist im Rahmen eines Studenten-Stipendiums der DGZfP entstanden. T2 - DGZfP DACH Tagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Schmiedeteile KW - POD KW - Ultraschall KW - Zerstörungsfreie Prüfung PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496796 UR - http://www.ndt.net/?id=24529 VL - 24 IS - 8 SP - 1 EP - 12 PB - NDT.net CY - Kirchwald AN - OPUS4-49679 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas A1 - Boehm, Rainer A1 - Mook, G. T1 - Ultrasonic rail inspection with array probes N2 - For more than 60 years ultrasonic rail inspection is used as non-destructive testing method to ensure the safe operation of rail tracks. Constantly increasing traffic density and heavy loads have been the motor for the development of new test equipment from handheld devices to rail inspection trains. (Krull 2003)Up to the present most of the system solutions feature conventional ultrasonic transducers housed in wheel-type and slide-type probes. Different tasks have to be carried out during an in-service inspection for flaws in the rail head, rail web and rail foot as well as rolling contact fatigue (Heckel 2018). The more tasks the inspection system has to perform, the more probes are needed. Compared against standard ultrasonic testing methods the application of array probes offers advantages and flexibility by the electronic steering possibilities to control the transmitted and received sound fields. This allows to increase functionality by software while decreasing the number of probes needed in hardware in parallel. One drawback in application of phased array probes is that the repetition frequency of the subsequent measurements will be reduced by the number of virtual probe functions each phased array probe has to perform. This may limit the range of use for phased array probes in high speed applications. To overcome these limits special designs for array probes and signal processing are necessary. T2 - Railway Engineering 2019 CY - Edinburgh, UK DA - 03.07.2019 KW - High speed KW - Ultrasound KW - Rail inspection KW - Phased array probes PY - 2019 VL - 2019 SP - 1 EP - 3 AN - OPUS4-49680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Ultrasonic Rail inspection with array Probes N2 - For more than 60 years ultrasonic rail inspection is used as non-destructive testing method to ensure the safe operation of rail tracks. Constantly increasing traffic density and heavy loads have been the motor for the development of new test equipment from handheld devices to rail inspection trains. (Krull 2003)Up to the present most of the system solutions feature conventional ultrasonic transducers housed in wheel-type and slide-type probes. Different tasks have to be carried out during an in-service inspection for flaws in the rail head, rail web and rail foot as well as rolling contact fatigue (Heckel 2018). The more tasks the inspection system has to perform, the more probes are needed. Compared against standard ultrasonic testing methods the application of array probes offers advantages and flexibility by the electronic steering possibilities to control the transmitted and received sound fields. This allows to increase functionality by software while decreasing the number of probes needed in hardware in parallel. One drawback in application of phased array probes is that the repetition frequency of the subsequent measurements will be reduced by the number of virtual probe functions each phased array probe has to perform. This may limit the range of use for phased array probes in high speed applications. To overcome these limits special designs for array probes and signal processing are necessary. T2 - Railway Engineering 2019 CY - Edinburgh, UK DA - 03.07.2019 KW - High speed KW - Ultrasound KW - Rail inspection KW - Phased array probes PY - 2019 AN - OPUS4-49681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - Human-Related Risks in the Non-Destructive Testing (NDT) of Hollow Railway Axles: Implications for the Education and Training of the NDT Personnel N2 - Non-destructive testing (NDT) is a major contributor to the safe railway operation. Even though NDT reliability in railway maintenance is affected by human factors, there are only just a few studies published in this field so far. Education and training of the NDT personnel are some of the most important drivers of safe and reliable NDT. Continuously improving current practices and tools used for educational purposes can be achieved not only through technical con¬tent, but also through the attention to human factors. The aim of this study was to deepen the understanding of possible human-related risks in the manual ultrasonic inspection of the hollow railway axles and to suggest measures to improve the education and training of the NDT person¬nel. This was achieved by means of Failure Modes and Effects Analysis (FMEA) carried out with eight NDT experts and by a survey of 27 experienced inspectors. The results show that failures can happen throughout the entire NDT process. Prevention of those failures could be improved through the optimization of the organization, technology, documentation and regulations, working conditions and the general process, and through the optimization of the formal education and training. Specialized training of the executives, extended training of the supervisors and the inspectors and improvement of the inspection documentation have been suggested. The study also showed potential for the improvements of the inspection in the field. T2 - 29th European Safety and Reliability Conference CY - Hannover, Germany DA - 22.09.2019 KW - Human Factors KW - Non-Destructive Testing KW - NDT KW - Education KW - Training KW - Failure Modes and Effects Analysis KW - Railway KW - Axle Inspection KW - Ultrasonic Testing KW - Reliability PY - 2019 SN - 978-981-11-2724-3 DO - https://doi.org/10.3850/978-981-11-2724-3_1058-cd SP - 294 EP - 300 PB - Research Publishing CY - Singapore AN - OPUS4-49733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul A1 - Bulling, Jannis A1 - Gravenkamp, H. A1 - Prager, Jens T1 - Acoustic-structure interaction in the Scaled Boundary Finite Element Method for primsatic geometries N2 - Due to the short wavelength compared to the dimensions of the structure, the simulation of ultrasonic waves is still a challenging task. A numerical method well suited for this purpose is the semi-analytical Scaled Boundary Finite Element Method (SBFEM). When applying this method, only the boundary of a computational domain is discretized using finite elements, while the interior is described by an analytical ansatz. Hence, the number of degrees of freedom is reduced significantly compared to the classical Finite Element Method (FEM). In recent years, a particular formulation of the SBFEM for the simulation of ultrasonic guided waves was developed. The method constitutes an efficient algorithm for prismatic structures of arbitrary length, such as plates, pipes, or beams. Wave propagation phenomena in such structures can be modeled for isotropic and anisotropic inhomogeneous waveguides. Even though the method is an efficient tool for the simulation of guided waves in solid media, a reliable model for the simulation of acoustic wave propagation in fluids as well as acoustic-structure interaction in terms of SBFEM is still missing. In principle, the fluid can be described by a displacement-based formulation and thus be implemented in existing SBFEM algorithms for solid bodies. However, due to the discretization with classical finite elements, spurious modes occur, which cannot be separated from the physical modes straightforwardly. The spurious modes can be suppressed using a penalty parameter. Although very accurate results were achieved for some problems, this procedure has been proven unreliable for certain cases. For this reason, we propose a different approach in this contribution. We employ a pressure model to simulate the acoustic behavior of fluids. The implementation of the pressure model results in a higher effort due to the necessity of incorporating coupling terms, but it presents a stable alternative without spurious modes. The accuracy of the method is demonstrated in comparison with analytical solutions and results obtained using the FEM. T2 - GACM 2019 CY - Kassel, Germany DA - 28.08.2019 KW - Scaled Boundary Finite Element Method KW - Guided Waves KW - Ultrasound KW - Acoustic-Structure Interaction PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-497364 UR - https://www.upress.uni-kassel.de/katalog/abstract.php?978-3-7376-5093-9 SN - 978-3-86219-5093-9 DO - https://doi.org/10.19211/KUP9783737650939 SP - 347 EP - 350 AN - OPUS4-49736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lardy-Fontan, S. T1 - A project to deliver reliable measurements of estrogens for better monitoring survey and risks assessments N2 - Monitoring programs should generate high-quality data on the concentrations of substances and other pollutants in the aquatic environment to enable reliable risk assessment. Furthermore, the need for comparability over space and time is critical for analysis of trends and evaluation of restoration of natural environment. Additionally, research work and exercises at the European level have highlighted that reliable measurements of estrogenic substances at the PNEC level are still challenging to achieve. The project EDC-WFD “Metrology for monitoring endocrine disrupting compounds under the EU Water Framework Directive” aims to develop traceable analytical methods for determining endocrine disrupting compounds and their effects, with a specific focus on three estrogens of the first watch list (17-beta-estradiol (17βE2), 17-alpha-ethinylestradiol (EE2), and estrone (E1)). Estrogens 17-alpha-estradiol (17aE2) and estriol (E3) will be included to demonstrate the reliability of the developed methods - Mass Spectrometry based method and effect-based methods (EBM) - and to support the requirements of Directive 2013/39/EC, Directive 2009/90/EC and Commission Implementation Decision (EU) 2018/840, hence improving the comparability and compatibility of measurement results within Europe. During the EDC-WFD project four EBM will be deeply investigated in order to improve their rationale use and their support in water quality assessment. T2 - Eurachem Workshop - Uncertainty from sampling and analysis for accredited laboratories CY - Berlin, Germany DA - 19.11.2019 KW - MS based method KW - Estrogens KW - Reliable measurements KW - Comparability KW - Effect based Method PY - 2019 AN - OPUS4-49738 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lardy-Fontan, S. T1 - A project to deliver reliable measurements of estrogens for better monitoring survey and risks assessments N2 - Monitoring programs should generate high-quality data on the concentrations of substances and other pollutants in the aquatic environment to enable reliable risk assessment. Furthermore, the need for comparability over space and time is critical for analysis of trends and evaluation of restoration of natural environment. Additionally, research work and exercises at the European level have highlighted that reliable measurements of estrogenic substances at the PNEC level are still challenging to achieve. The project EDC-WFD “Metrology for monitoring endocrine disrupting compounds under the EU Water Framework Directive” aims to develop traceable analytical methods for determining endocrine disrupting compounds and their effects, with a specific focus on three estrogens of the first watch list (17-beta-estradiol (17βE2), 17-alpha-ethinylestradiol (EE2), and estrone (E1)). Estrogens 17-alpha-estradiol (17aE2) and estriol (E3) will be included to demonstrate the reliability of the developed methods - Mass Spectrometry based method and effect-based methods (EBM) - and to support the requirements of Directive 2013/39/EC, Directive 2009/90/EC and Commission Implementation Decision (EU) 2018/840, hence improving the comparability and compatibility of measurement results within Europe. During the EDC-WFD project four EBM will be deeply investigated in order to improve their rationale use and their support in water quality assessment. T2 - ICRAPHE - Second International Conference on Risk Assessment of Pharmaceuticals in the Environment CY - Barcelona, Spanien DA - 28.11.2019 KW - Estrogens KW - Effect based Method KW - Comparability KW - Reliable measurements KW - MS based method PY - 2019 AN - OPUS4-49739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Kick-off meeting “18NRM01-EDC-WFD” N2 - Monitoring programs should generate high-quality data on the concentrations of substances and other pollutants in the aquatic environment to enable reliable risk assessment. Furthermore, the need for comparability over space and time is critical for analysis of trends and evaluation of restoration of natural environment. Additionally, research work and exercises at the European level have highlighted that reliable measurements of estrogenic substances at the PNEC level are still challenging to achieve. The project EDC-WFD “Metrology for monitoring endocrine disrupting compounds under the EU Water Framework Directive” aims to develop traceable analytical methods for determining endocrine disrupting compounds and their effects, with a specific focus on three estrogens of the first watch list (17-beta-estradiol (17βE2), 17-alpha-ethinylestradiol (EE2), and estrone (E1)). Estrogens 17-alpha-estradiol (17aE2) and estriol (E3) will be included to demonstrate the reliability of the developed methods - Mass Spectrometry based method and effect-based methods (EBM) - and to support the requirements of Directive 2013/39/EC, Directive 2009/90/EC and Commission Implementation Decision (EU) 2018/840, hence improving the comparability and compatibility of measurement results within Europe. During the EDC-WFD project four EBM will be deeply investigated in order to improve their rationale use and their support in water quality assessment. T2 - EMPIR Kick-off meeting EDC-WFD CY - Paris, France DA - 07.10.2019 KW - Estrogens KW - Reliable measurements KW - Effect based Method KW - Comparability KW - MS based method PY - 2019 AN - OPUS4-49741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kastania, Eleni T1 - Spectro-Electrochemical Investigation of the Effects of Flavin Electron Transporters in Artificial and Bacterial Biofilms N2 - Bacterial biofilms have the capacity to develop and thrive in virtually all circumstances and surfaces, even in the most challenging environmental conditions. The pervasive and recalcitrant existence of biofilms renders them to be a significant safety risk and economical encumbrance in a wide array of industries and technologies, and therefore is a priority area of research. It is essential to develop an improved understanding of the mechanisms implicated during biofilm formation, such as in the case of the diffusion of bacterial-secreted extracellular electron transporters, which are purported to play an important role during biocorrosion by exoelectrogenic bacteria. Hence, a fundamental understanding of electron transfer mechanisms between bacteria and extracellular electron acceptors will contribute insight to our understanding of charge transport and chemistry at the biofilm – external insoluble electron acceptor interface. In the present work, Attenuated Total Reflection - Fourier transform-infrared (ATR-FTIR) spectroscopy has been coupled to electrochemical techniques for the nondestructive, in situ spectro-electrochemical monitoring of biofilms in real-time. Shewanella sp. have been selected for this investigation due to their adaptable exoelectrogenic respiratory capacities and their notable ability to reduce metals via several different mechanisms of extracellular electron transfer mechanisms, including self-secreted flavin shuttles. Gold-thin film model substrates have been used due to their inert nature and for their ability to permit precise manipulation of the substrate surface polarization. Additionally, hydrogels comprised of calcium cross-linked alginate have been used to mimic the architectural features of extracellular polymeric substances which are integral to a bacterial biofilm, to allow the study of electron-transporting flavin molecules in an artificial biofilm. The results will demonstrate patterns of diffusion, akin to how flavins would diffuse in a naturally occurring biofilm, and how polarization affects this process. Furthermore, insight will be gained on how the redox behavior of flavins can influence the development and evolution of a biofilm. This interdisciplinary approach should shed light on bacterial electron transfer mechanisms which could contribute towards emerging technologies which seek to better understand such mechanisms for novel antifouling strategies, renewable energies, and bioremediation. T2 - ECEE 2019 Electrochemical Conference on Energy and the Environment: Bioelectrochemistry and Energy Storage CY - Scottish Events Campus (SEC), Glasgow, Scotland DA - 21.07.2019 KW - Biofilms KW - Raman Spectroscopy KW - Electrochemistry KW - Biocorrosion KW - Fourier Transform Infra Red Spectroscopy KW - Spectroelectrochemical Techniques KW - Surface Enhanced Raman Spectroscopy PY - 2019 UR - http://ma.ecsdl.org/content/MA2019-04/8/397.abstract AN - OPUS4-49766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völzke, Jule L. T1 - Immunoprecipitation with Nanodiamonds for the Enrichment of Ceruloplasmin from Human Serum N2 - In this study, we developed a new immunoprecipitation method based on protein-coated nanodiamonds. Performing SDS-PAGE and using the SDS-PAGE buffer as an eluent showed that CER could be successfully enriched from human serum. Based on the copper determination with ICP-MS, the amount of bound CER on the nanodiamonds can be calculated. We could show the fulfilled mass balance of bound CER and CER in the supernatant after incubation with a known amount of CER. For isotope ratio analysis this method can be applied to compare ratios of the total copper content in human serum to copper ratios from CER enrichment. T2 - ReMiND 2019 CY - Braunschweig, Germany DA - 26.06.2019 KW - Metalloprotein KW - Copper KW - Affinity enrichment KW - Immunoaffinity KW - Protein g KW - Blood KW - Serum KW - Plasma KW - SDS-PAGE KW - ICP-MS PY - 2019 UR - https://www.ptb.de/empir/remind-conference.html AN - OPUS4-49728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - Human-related risks in the nondestructivetesting (NDT) of hollow railway axles: implications for the education and training of the NDT personnel N2 - Non-destructive testing (NDT) is a major contributor to the safe railway operation. Even though NDT reliability in railway maintenance is affected by human factors, there are only just a few studies published in this field so far. Education and training of the NDT personnel are some of the most important drivers of safe and reliable NDT. Continuously improving current practices and tools used for educational purposes can be achieved not only through technical content, but also through the attention to human factors. The aim of this study was to deepen the understanding of possible human-related risks in the manual ultrasonic inspection of the hollow railway axles and to suggest measures to improve the education and training of the NDT personnel. This was achieved by means of Failure Modes and Effects Analysis (FMEA) carried out with eight NDT experts and by a survey of 27 experienced inspectors. The results show that failures can happen throughout the entire NDT process. Prevention of those failures could be improved through the optimization of the organization, technology, documentation and regulations, working conditions and the general process, and through the optimization of the formal education and training. Specialized training of the executives, extended training of the supervisors and the inspectors and improvement of the inspection documentation have been suggested. The study also showed potential for the improvements of the inspection in the field. T2 - 29th European Safety and Reliability Conference CY - Hannover, Germany DA - 22.09.2019 KW - Human Factors KW - Non-Destructive Testing KW - NDT KW - Education KW - Training KW - Failure Modes and Effects Analysis KW - Railway KW - Axle Inspection KW - Ultrasonic Testing KW - Reliability PY - 2019 AN - OPUS4-49729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Simulation von mechanisierten Eisenbahnschienenprüfungen mit Ultraschall N2 - Bei der mechanisierten Prüfung von verlegten Eisenbahnschienen mit Schienenprüfzügen werden große Prüfdatenmengen mit einer komplexen Prüfkopfanordnung in kurzer Zeit bei hohen Prüfgeschwindigkeiten aufgenommen. Der Typ und der Zustand des Gleises kann während der Prüfung in schnellem Wechsel streckenabhängig variieren, z.B. unterschiedliche Schienentypen oder Abnutzung sowie beim Durchfahren von Weichenstraßen. Der logistische Aufwand diese Prüfung insgesamt durchzuführen ist dabei sehr hoch und eine Wiederholung der Prüfung in einem kurzen Zeitintervall nicht möglich. Es werden während der Prüfdatenaufnahme bereits Datenreduktionsverfahren, Rekonstruktionsverfahren und Online-Parametervariationen eingesetzt, um die Ergebnisdaten zum einen in Ihrer Menge zu begrenzen zum anderen auf die lokalen Geometrie- und Zustandsänderungen des Prüfobjektes Schiene zu reagieren. Im Regelwerk EN 16729-1 „Zerstörungsfreie Prüfung an Schienen im Gleis -Teil 1: Anforderungen an Ultraschallprüfungen und Bewertungsgrundlagen“ werden Bezugsreflektoren definiert, um die Leistung automatisierter Ultraschallsysteme für die Schienenprüfung zu verifizieren. Um die Einflüsse der komplexen Randbedingungen der mechanisierten Schienenprüfung auf das Prüfergebnis evaluieren zu können, wurde ein Softwarewerkzeug erarbeitet, mit dem eine Prüffahrt auf einer Schiene simuliert werden kann. Basierend auf der Datenaufnahme mit dem Glassy-Rail-Diagramm können alle relevanten Prüfparameter und Artefakte in Schienen sowie Störeinflüsse bei der Simulation berücksichtigt werden. T2 - DGZfP DACH Tagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Eisenbahnschienen KW - Simulation KW - Zerstörungsfreie Prüfung KW - Ultraschall PY - 2019 AN - OPUS4-49682 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Simulation of an instrumented ultrasonic test run with a rail inspection train N2 - Rail inspection performed by ultrasonic rail inspection trains is a complex and challenging process. A large number of variables and parameters given by the environment, the track and the testing-system have an influence on the overall performance of the inspection and the inspection result. Typically the parameter vary in a combination depending on the track condition. To evaluate the individual influence of each relevant variable, simulation tools can be used. Therefore the entire inspection process has to be transferred into a model using combined modelling techniques. The goal of this work is to model an instrumented ultrasonic test run with a rail inspection train with the parameters varied by a script over a virtually driven distance. T2 - 46th Annual Review of Progress in Quantitative Nondestructive Evaluation- QNDE 2019 CY - Portland, OR, USA DA - 14.07.2019 KW - Simulation KW - Ultrasound KW - Rail inspection KW - Modelling PY - 2019 AN - OPUS4-49684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vahlsing, Thorsten T1 - Fe-simulation of eddy current signals produced from basic model cracks for running surface rail defects N2 - Non-destructive testing for surface crack detection and head check depth quantification at the gauge cor-ner of railway tracks can be achieved using eddy current methods. With the extension of the tested zone to the running surface, rail defect signal types other than head checks can be measured. Due to their most-ly irregular shape, a quantitation based on a calibration against regular test cracks of varying depth may not be linear. Estimates of the expected influence of more complex crack patterns may be obtained by a finite element simulation of sufficiently simple limiting cases, like two displaced or intersecting cracks or a simply branched or flexed crack. As a first step, a 3D finite element model of the HC10 eddy current probe distributed by Prüftechnik Linke und Rühe (PLR), Germany was built and verified against meas-ured results from an (easily fabricated) reference block with isolated long cracks. T2 - Railway Engineering 2019 CY - Edinburgh, UK DA - 03.07.2019 KW - Finite element analysis KW - Eddy current testing KW - Rail inspection PY - 2019 AN - OPUS4-49686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Akustische und elektromagnetische Prüfverfahren für verlegte Eisenbahnschienen N2 - In diesem Vortrag werden die aktuellen Techniken für die angewandte mechanisierte Schienenprüfung dargestellt und Perspektiven für die Zukunft der handgeführten und fahrzeuggeführten Prüftechnik aufgezeigt. Insbesondere wird hier die bildhafte Darstellung, der zusätzliche Nutzen von Arraysensoren sowie die Möglichkeiten der Simulation von Schienenfehlern vorgestellt. T2 - ZfP-Prüfertag 2019 im RB Südost CY - Halle, Germany DA - 13.11.2019 KW - Arraysensoren KW - Mechanisierte Schienenprüfung KW - Ultraschall KW - Wirbelstrom KW - Simulation PY - 2019 AN - OPUS4-49687 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - TFM und FMC für die bildgebende Ultraschallprüfung mit Arrays N2 - Im Rahmen des Vortrages wird das Verfahren zur Total Focussing Methode (TFM) auf Basis des Full Matrix Captures (FMC) für Ultraschallarrayprüfköpfe erläutert und die Möglichkeiten der Anwendung für die Prüfung von Gussteilen diskutiert. Der Stand der Normung im Bereich Guss wird diskutiert. T2 - Sitzung des Fachausschusses Eisenguss des BDG CY - Berlin, Germany DA - 12.09.2019 KW - Standardisierung KW - Array KW - Ultraschall KW - TFM KW - MFC KW - Guss PY - 2019 AN - OPUS4-49688 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian A1 - Emmerling, Franziska T1 - Insights into mechanochemical Knoevenagel condensations N2 - Mechanochemistry paves the way to simple, fast, and green syntheses. Despite considerable effort, there is a lack in understanding of the underlying mechanisms. In situ investigations help to understand these mechanisms, which occur during a mechanochemical reaction. Here we present a universal strategy for simultaneous real-time in situ analysis, combining X-ray diffraction, Raman spectroscopy, and thermography. The potential of of our approach is shown for diffrent model reactions. T2 - Adlershofer Forschungsforum 2019 CY - Berlin, Germany DA - 11.11.2019 KW - Mechanochemistry KW - In situ KW - Knoevenagel condensation PY - 2019 AN - OPUS4-49694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen A1 - Scheliga, F. T1 - Synthesis of cyclic polymers and flaws of the Jacobson–Stockmayer theory N2 - Cyclic poly(L-lactide)s were prepared by ring-opening polymerization combined with simultaneous polycondensation (ROPPOC) in bulk at 160 ° with dibutyltin bis(4-cyanophenoxide) as catalyst. It is demonstrated by MALDI TOF mass spectrometry and 1H NMR end group analyses that cycles are formed by endto-end cyclization in addition to “back-biting” transesterification. Formation of high molar mass cyclic poly L-lactide)s by means of several more reactive ROPPOC catalysts presented previously and in new experiments is discussed. These experimental results, together with theoretical arguments, prove that part of the Jacobson–Stockmayer theory is wrong. The critical monomer concentration, above which end-toend cyclization is seemingly impossible, does not exist and reversible like irreversible polycondensations can theoretically proceed up to 100% conversion, so that finally all reaction products will necessarily adopt a cyclic architecture. KW - Polylactide KW - MALDI-TOF MS KW - Cyclization PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506419 DO - https://doi.org/10.1039/d0py00226g VL - 11 IS - 14 SP - 2595 EP - 2604 PB - Royal Society for Chemistry AN - OPUS4-50641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - Metal based pollutant assessment via diatoms - new possibilities via automated single cell-ICP-ToF-MS N2 - Diatoms are located at the bottom of the food chain. Toxicological relevant metals can possibly accumulate within the food web and cause harmful effects. Diatoms are a test system in ecotoxicology. Toxicological effects weaken the growth of algae which is by default investigated by means of fluorescence detection. On basis of the expose concentration as well as obtained fluorescence data potential threshold exceedance in e.g. surface waters is assessed. However, this approach does not allow for the determination of “real” accumulated metal concentration in diatoms. Common approaches are based on bulk analysis via e.g. ICP-MS, ICP-OES or AAS. But, biological variability is completely disregarded. To tackle this problem, alternative approaches are highly needed. Within the last years, sp-ICP-MS for nanoparticle as well as single cell analysis turned out as a powerful technique to analyze metal contents as well as size distributions on broad size range. But, common ICP-MS systems do not allow for multi-element detection within single particle/cell events. Thus, simultaneous MS detection devices are needed - just recently, ICP-ToF-MS experienced a revival. Within our previous work, we developed an automated sample introduction system based on a HPLC system on-line with single particle-ICP-MS, which allowed for ionic background separation and single algae analysis. However, for unambiguous tracing several fingerprint elements and multielement analysis in single algae (diatoms) is needed. Thus, we coupled our previous setup on-line to ICP-ToF-MS. Test diatom species were exposed to test substances (Zn) as well as nanoparticles (FeNPs). The developed setup allowed for a fast, automated and multielement analysis in single diatoms. Furthermore, we combined our approach with multivariate data assessment - multielement detection of characteristic fingerprint elements allowed for an unambiguous diatom tracing. Clustering of diatoms according to metal exposure concentration levels was enabled. Our approach is a new potential tool in ecotoxicological testing. T2 - 53. DGMS & 27th ICP-MS user meeting CY - Münster, Germany DA - 01.03.2020 KW - Single cell-ICP-ToF-MS KW - Diatoms KW - New ecotoxicological testing tools PY - 2020 AN - OPUS4-50644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Meyer, A. A1 - Kricheldorf, H. R. T1 - Ring–Ring Equilibration in Solid, Even-Numbered Cyclic Poly(l-lactide)s and their Stereocomplexes N2 - Even-numbered cyclic poly(d-lactide) and poly(l-lactide) are prepared by ringexpansion polymerization. The cyclic pol(l-lactide) is annealed either at 120 or at 160 °C for several days. The progress of transesterification in the solid state is monitored by the formation of odd-numbered cycles via matrix-assisted laser desorption/ionization-time of flight mass spectrometry. The changes of the crystallinity are monitored by differential scanning calorimetry, wideand small-angle x-ray scattering (WAXS and SAXS) measurements. Despite total even-odd equilibration at 160 °C, the crystallinity of poly(l-lactide) is not reduced. Furthermore, the crystallinity of the stereocomplexes of both cyclic polylactides do not decrease or vanish, as expected, when a blocky or random stereosequence is formed by transesterification. This conclusion is confirmed by 13C NMR spectroscopy. These measurements demonstrate that transesterification is a ring–ring equilibration involving the loops on the surfaces of the lamellar crystallites thereby improving crystallinity and 3D packing of crystallites without significant broadening of the molecular weight distribution. KW - Polylactide KW - MALDI-TOF MS KW - Cyclization PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506458 DO - https://doi.org/10.1002/macp.202000012 VL - 221 IS - 9 SP - 2000012 PB - Wiley-VCH Verlag AN - OPUS4-50645 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Calibration of Mg isotope amount ratios and delta values N2 - In the past, δ26/24Mg measurements were referenced to NIST SRM 980, the initial zero of the δ26/24Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. To solve this problem a suite of magnesium isotope reference materials, ERM-AE143, -AE144 and -AE145, has been certified in a first study by applying an ab initio calibration for absolute Mg isotope ratios without any a priori assumptions, a procedure which fulfils all requirements of a primary method of measurement. We could achieve for the first time measurement uncertainties for isotope amount ratios close to the typical precision of magnesium delta values, δ26/24Mg, which are at the 0.1 ‰ level (2SD). In addition, it was demonstrated that commonly used fractionation laws are invalid for correcting Mg isotope ratios in multi-collector ICPMS as they result in a bias which is not covered by its associated uncertainty. Depending on their type, fractionation laws create a bias up to several per mil, with the exponential law showing the smallest bias between 0.1 ‰ to 0.7 ‰. With these isotope reference materials, it is possible to establish SI-traceability for magnesium delta measurements. To realize this, we organized a second study within which five expert laboratories participated to cross-calibrate all available magnesium isotope standards, which are NIST SRM 980, IRMM-009, ERM-AE143, ERM-AE144, ERM-AE145 and the standards DSM3 and Cambridge-1. The mean δ26/24Mg values for the individual iRMs, calculated from the laboratory means show 2 SD reproducibilities varying between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for δ26/24Mg determinations (2SD). Thus, SI traceability for magnesium isotope amount ratios and delta values is demonstrated to be established. T2 - 53rd annual conference of the DGMS including 27th ICP-MS User's Meeting CY - Münster, Germany DA - 01.03.2020 KW - Isotope ratio KW - Delta value KW - Metrology KW - Magnesium KW - Magnesium isotope ratios PY - 2020 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. AN - OPUS4-50549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Becker, S. A1 - Beckmann, Jörg A1 - Braun, M.-T. A1 - Cojocari, O. A1 - Feige, V. A1 - Fischer, B. A1 - Friederich, F. A1 - Globisch, B. A1 - Hechtfischer, G. A1 - Hens, K. A1 - Hübers, H.-W. A1 - Jelonnek, J. A1 - Jonuscheit, J. A1 - Keil, A. A1 - Kleine-Ostmann, T. A1 - Marquardt, E. A1 - Mayr, M. A1 - Nickel, H.-U. A1 - Nüßler, D. A1 - Peichl, M. A1 - Peters, O. A1 - Schür, J. A1 - Sprenger, T. A1 - Steiger, A. A1 - van Frank, S. A1 - Vieweg, N. A1 - Wilk, R. ED - Jonuscheit, J. ED - Marquardt, E. T1 - Terahertzsysteme und Anwendungsfelder N2 - Der Frequenzbereich der Terahertzwellen liegt im elektromagnetischen Spektrum zwischen den Mikrowellen und dem infraroten Licht – also etwa im Bereich von 0,1 bis 10 Terahertz (THz). Der VDI-Statusreport „Terahertzsysteme und Anwendungen“ stellt die unterschiedlichen Konzepte für Terahertzsysteme vor und zeigt Anwendungsbeispiele, bei denen die Terahertztechnik erfolgreich eingesetzt wird. Umfangreiche Literaturangaben ermöglichen eine intensivere Beschäftigung mit allen Themen des VDI-Statusreports. KW - Terahertzsysteme PY - 2020 UR - https://www.vdi.de/ueber-uns/presse/publikationen/details/terahertzsysteme-und-anwendungsfelder SP - 1 EP - 44 PB - Verein Deutscher Ingenieure (VDI) CY - Düsseldorf AN - OPUS4-50556 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beyranvand, S. A1 - Pourghobadi, Z. A1 - Sattari, S. A1 - Soleymani, K. A1 - Donskyi, Ievgen A1 - Gharabaghi, M. A1 - Unger, Wolfgang A1 - Farjanikish, G. A1 - Nayebzadeh, H. A1 - Adeli, M. T1 - Boronic acid functionalized graphene platforms for diabetic wound N2 - While noncovalent interactions between graphene derivatives and biosystems are extensively studied, less knowledge about their covalent multivalent interactions at biointerfaces is available. Due to the affinity of boronic acids towards cis-diol bearing biosystems, graphene sheets with this functionality were synthesized and their covalent interactions with the bacteria and nematode were investigated. As expected, graphene platforms with boronic acid functionality were able to wrap bacteria and destroy it in a short time. Surprisingly, body of nematodes was ruptured and their viability decreased to 30% after 24 h incubation with the functionalized graphene sheets. Because of their antibacterial and antiparasitic activities as well as their ability for wound dressing, graphene platforms with the boronic acid functionality were further investigated for diabetic wound healing. In vivo experiments showed that graphene platforms are more efficient than the commercially available drug, phenytoin, and restore both infected and non-infected diabetic wounds in ten days. Taking advantage of their straightforward synthesis, strong interactions with different biosystems as well as their ability to heal diabetic wounds, the boronic Acid functionalized graphene sheets are promising candidates for a broad range of future biomedical applications. KW - Graphene KW - Boronic acid KW - Functionalized graphene KW - XPS PY - 2020 UR - https://www.sciencedirect.com/science/article/abs/pii/S0008622319310954 DO - https://doi.org/doi.org/10.1016/j.carbon.2019.10.077 VL - 158 SP - 327 EP - 336 PB - Elsevier Ltd. AN - OPUS4-50559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Alfeld, M. A1 - Eckhardt, H.-S. A1 - Kraft, J. A1 - Maiwald, Michael A1 - Meermann, Björn A1 - Merz, K. A1 - Prikler, S. A1 - Richert, J. A1 - Steiner, G. A1 - von Tümpling, W. T1 - Trendbericht Analytische Chemie N2 - Zusätzlich zu Methodenentwicklung, Miniaturisierung und Kopplungsverfahren zeigen sich die Hyperspektroskopie zusammen mit Imaging‐Verfahren, der Einzelmolekülnachweis und der Einsatz von 3‐D‐Druckern als neue Schwerpunkte. Hinzu kommen künstliche Intelligenz bei Sensoren, Bildgebungsverfahren und Prozesssteuerung sowie die Vernetzung von Analyse‐ und Laborgeräten. Trends und Forschungsthemen aus der analytischen Chemie, zusammengestellt von elf Autoren, koordiniert von Günter Gauglitz. KW - Multielementanalytik KW - Multimodale Analytik KW - Kristallolgraphie KW - Prozessanalytik KW - Prozessindustrie KW - Industrielle Analytik KW - Chemometrik KW - Chemometrie PY - 2020 DO - https://doi.org/10.1002/nadc.20204095786 SN - 1868-0054 VL - 68 IS - 4 SP - 52 EP - 60 PB - Wiley CY - Weinheim AN - OPUS4-50609 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Millar, Steven A1 - Gottlieb, Cassian A1 - Wilsch, Gerd A1 - Günther, Tobias A1 - Völker, Tobias T1 - Chemische Zustandsanalyse von Stahlbetonbauwerken mit der laserinduzierten Plasmaspektroskopie (LIBS) N2 - Die chemische Analyse von Beton gehört bei der Ermittlung des Ist-Zustandes von Stahl- und Spannbetonbauwerken zu den grundlegenden Untersuchungen bei der Zustandserfassung. Der tiefenabhängige Chloridgehalt sowie der Karbonatisierungsfortschritt müssen bei der Bewertung des Ist-Zustandes, beim Instandsetzungsbedarf und ggf. bei der Planung eines erforderlichen Instandsetzungskonzeptes mit einbezogen werden. Seit Mitte der 1990er Jahre wird an der Bundesanstalt für Materialforschung und -prüfung die laserinduzierte Plasmaspektroskopie (engl. Laser-induced Breakdown Spectroscopy) – kurz LIBS – stetig für die chemische Analyse von Beton weiterentwickelt. In diesem Beitrag wird der aktuelle Stand der Forschung/ Technik und der Normungsarbeit präsentiert, sowie zukünftig mögliche Anwendungen vorgestellt. Mit den aktuellen LIBS-Systemen (mobiles LIBS-System sowie kommerziell erhältliche Laborsysteme) ist es möglich den Chloridgehalt ortsaufgelöst in wenigen Minuten zu quantifizieren, sogenannte Elementlandkarten zu erstellen und somit die Elementverteilung innerhalb des Betons zu visualisieren. Durch das Scannen eines Bohrkernquerschnittes und der simultanen Erfassung von mehreren Elementen mit einer Messung, ist es zudem möglich, die Gesteinskörnung in den Messdaten zu identifizieren und den Chloridgehalt auf die Zementsteinmatrix zu beziehen. Fehlerquellen aus der Umrechnung der betonbezogenen Chloridgehalte können dadurch minimiert werden. Neben den Grundlagen von LIBS werden vor allem aktuelle Praxisbeispiele vorgestellt, die die aktuellen Möglichkeiten des Verfahrens veranschaulichen. T2 - 9. Kolloquium Parkbauten CY - Esslingen, Germany DA - 04.02.2020 KW - LIBS KW - Chemische Analyse KW - Spektroskopie KW - Beton PY - 2020 UR - https://elibrary.narr.digital/article/99.125005/kpb202010305 SN - 2510-7763 VL - 9 IS - 1 SP - 305 EP - 319 AN - OPUS4-50615 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thummerer, G. A1 - Mayr, G. A1 - Hirsch, Philipp Daniel A1 - Ziegler, Mathias A1 - Burgholzer, P. T1 - Photothermal Image Reconstruction in Opaque Media with Virtual Wave Backpropagation N2 - Thermographic reconstruction of defects that lie in the bulk of a sample is a difficult task because entropy production during heat diffusion leads to information loss. To reconstruct defects one has to solve an inverse heat conduction problem. The quality of the reconstruction is closely related to the information content of the observed data set that is reflected by the decreasing ability to spatially resolve a defect with growing defect depth. In this work we show a 2D reconstruction of rectangular slots with different width-to-depth ratios in a metallic sample. For this purpose, we apply the virtual wave concept and incorporate positivity and sparsity as prior information to overcome the diffusion-based information loss partially. The reconstruction is based on simulated and experimental pulse thermography data. In the first reconstruction step, we compute a virtual wave field from the surface temperature data. This allows us, in the second step, to use ultrasonic backpropagation methods for image reconstruction. KW - Virtual wave concept KW - Thermography KW - Photothermal Technique KW - Image reconstruction PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506166 DO - https://doi.org/10.1016/j.ndteint.2020.102239 VL - 112 SP - 102239 PB - Elsevier Ltd. CY - Netherlands AN - OPUS4-50616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - The internet of things in the lab and in process - The digital transformation challenges for the laboratory 4.0 T1 - Das Internet of Things in Labor und Prozess - Herausforderungen des digitalen Wandels für das Labor 4.0 N2 - It is a fact that much of the time spent on analytical laboratory instrumentation these days goes into system maintenance. Digital transformation could give us more time again for creativity and our actual laboratory work – if we shape it the right way. N2 - Fakt ist: Einen Großteil der Zeit, der an analytischen Laborgeräten verbracht wird, nimmt heute die Systempflege in Anspruch. Der digitale Wandel kann uns endlich wieder mehr Zeit für Kreativität und die eigentliche Laborarbeit geben – wenn wir ihn richtig gestalten. KW - Lab of the Future KW - Digitalisation KW - Automation KW - Data Analysis KW - Instrument Communication KW - Labor der Zukunft KW - Digitale Transformation KW - Automatisierung KW - Gerätekommunikation PY - 2020 IS - 4 SP - 1 EP - 3 PB - Lumitos AG CY - Darmstadt AN - OPUS4-50618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Epple, Niklas T1 - Monitoring of bridges with coda waves - first steps towards an imaging strategy N2 - Monitoring of concrete structures is of utmost importance in maintenance and preservation of infrastructure. As a part of the DFG research group CoDA (Concrete Damage Assessment by Coda Waves), the works within this PhD project aim for identification of damage sensitive parameters extracted from ultrasonic measurements obtained with embedded sensors, the determination of environmental (reversible) influences on the signal and the localisation of damaged areas. The main technique used for the detection of changes in the monitored material is the so-called Coda Wave Interferometry (CWI). It uses the later part of the ultrasonic recording for the detection of small changes in the sensed area and the calculation of a relative velocity change. Using this technique we can show that we are able to detect changes in concrete temperature with ultrasound measurements. This enables temperature correction for ultrasound monitoring with embedded sensors. The crucial point for imaging and localisation with coda waves is the calculation of the so-called sensitivity kernels. We propose the application of numerical wave simulations for the kernel calculations instead of the commonly used diffusivity equation. Using finite-difference wave modelling code from our DFG project partners we are able to calculate those Kernels and first results are shown in this presentation. The major task for the second year will be the development and implementation of the inversion algorithm as well as the preparation of validation experiments. T2 - Doktorandenseminar BAM Abt. 8 CY - Berlin, Germany DA - 30.03.2020 KW - Ultrasound KW - Non-destructive testing KW - Numerical modelling KW - Structural health monitoring PY - 2020 AN - OPUS4-50624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Zhiyang A1 - Li, Y. A1 - Frisch, J. A1 - Bär, M. A1 - Rappich, J. A1 - Kneipp, Janina T1 - In situ surface-enhanced Raman scattering shows ligand-enhanced hot electron harvesting on silver, gold, and copper nanoparticles N2 - Hot carriers (electrons and holes) generated from the decay of localized surface plasmon resonances can take a major role in catalytic reactions on metal nanoparticles. By obtaining surface enhanced Raman scattering (SERS) spectra of p-aminothiophenol as product of the reduction of p-nitrothiophenol by hot electrons, different catalytic activity is revealed here for nanoparticles of silver, gold, and copper. As a main finding, a series of different ligands, comprising halide and non-halide species, are found to enhance product formation in the reduction reaction on nanoparticles of all three metals. A comparison with the standard electrode potentials of the metals with and without the ligands and SERS data obtained at different electrode potential indicate that the higher catalytic activity can be associated with a higher Fermi level, thereby resulting in an improved efficiency of hot carrier generation. The concept of such a ligand-enhanced hot electron reduction provides a way to make light-to-chemical energy conversion more efficient due to improved electron harvesting. KW - Ligands KW - Hot electrons KW - SERS KW - p-Nitrothiophenol KW - p-Aminothiophenol PY - 2020 DO - https://doi.org/10.1016/j.jcat.2020.01.006 VL - 383 SP - 153 EP - 159 PB - Elsevier Inc. CY - Amsterdam, NL AN - OPUS4-50626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Zentrifugentechnologie zur statistischen Untersuchung von Stumpfklebungen: Ergebnisse ZENSUS-Ringversuchs N2 - Der Vortrag widmet sich der „Zentrifugentechnologie zur statistischen Untersuchung von Stumpfklebungen“ und beschreibt drei wesentlich verschiedene Realsysteme (Fügefläche 1/Klebstoff/ Fügefläche 2), um die Statistik ZPM (wiederholte Ein-Proben-Prüfung) vs. CAT (Mehr-Proben-Prüfung) zu vergleichen. Dazu wurden drei unterschiedliche Klebstoff-klassen mit typischen Fügeteilmaterialkombinationen ausgewählt und in einem Vorversuch mit jeweils 3 unterschiedlichen Prüfgeschwindigkeiten sowohl im Weg-geregelten als auch Kraft-geregelten Mode beansprucht. Die Ergebnisse ZPM vs. CAT und Kraft- vs. Weg-Regelung des Vorversuches zeigten keinerlei Unterschiede auf. Im Ergebnis wurde ein Ringversuch im Kraft-geregelten Mode (6xZPM vs. 8xCAT) für ein Referenzsystem durchgeführt, der nachwies, dass die CAT-Technologie statistisch relevante Prüfergebnisse zur Klebfestigkeit bereitstellt. Es zeigte sich, dass für zwei ZPM-Teilnehmer im Vertrauensbereich 99% statistisch signifikant etwas kleinere Werte der Klebfestigkeit bestimmt wurden, was auf geringfügige Abweichungen von der axialen Ausrichtung des eingespannten Prüflings bei der Ein-Proben-ZPM-Zugprüfung zurückgeführt wird. T2 - VCI CY - Frankfurt/Main, Germany DA - 10.03.2020 KW - Zentrifugentechnologie KW - Statistischen Untersuchung KW - Normung KW - Prüfgeschwindigkeiten KW - Stumpfklebungen PY - 2020 AN - OPUS4-50581 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang T1 - International standardization and metrology as tools to address the comparability and reproducibility challenges in XPS measurements N2 - The status of standardization related to x-ray photoelectron spectroscopy (XPS, ESCA) at ASTM International (Subcommittee E42.03) and ISO (TC 201) is presented and commented upon in a structured manner. The survey also identifies other active bodies, here VAMAS Technical Working Area 2 and the Surface Analysis Working Group at the International Meter Convention, contributing to prestandardization Research and metrology of XPS and reports their specific activities. It is concluded that existing standardization is delivering good practices in the use of XPS and has a high potential to avoid the recently observed erroneous use, misapplications, and misinterpretation by new and inexperienced users of the method—which seems to be the main reason for the “reproducibility crisis” in the field of XPS applications. A need for a more proactive publicizing of international documentary standards by experienced XPS users, specifically those who are involved in standardization, is identified. Because the existing portfolio of standards addressing the use of XPS is not complete, future standardization projects planned or already ongoing are mentioned. The way the standardization bodies are identifying future needs is shortly explained. KW - Standardisation KW - Comparability KW - Reproducibility KW - XPS KW - VAMAS KW - Metrology PY - 2020 DO - https://doi.org/10.1116/1.5131074 VL - 38 IS - 2 SP - 021201-1 EP - 021201-8 PB - AVS AN - OPUS4-50560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Genath, A. A1 - Hofmann, Michael A1 - Tiebe, Carlo A1 - Einspanier, R. T1 - Auf dem Weg zum Monitoring der Ameisensäurekonzentration in der Bienenstock-Luft mit einem Multigassensorsystem N2 - Die Varroose gilt weltweit als eine der bedeutendsten Erkrankungen der westlichen Honigbiene, Apis mellifera. Verursacht wird sie durch den Ektoparasiten Varroa destructor, der durch Saugen der Hämolymphe und Virenübertragung sowohl die Bienenbrut als auch die adulten Individuen schädigt. Ohne imkerliche Unterstützung gehen betroffene Bienenvölker in der Regel innerhalb von drei Jahren ein. Als bewährte, häufige Behandlung wird flächendeckend 60%ige Ameisensäure (AS) - im Bienenstock appliziert über verschiedene Verdampfungssysteme - eingesetzt. Sie wirkt als einziger zugelassener Stoff gegen die Varroamilbe auch in die verdeckelte Brut hinein und birgt kein Risiko der Resistenzentwicklung. Allerdings ist das therapeutische Fenster, der Bereich zwischen Milbenabtötung und Bienenschädigung, relativ schmal und die tatsächliche AS-Konzentration im Bienenstock stark abhängig von äußeren Einflussfaktoren, wie Temperatur, Luftfeuchte oder Applikationsart. Eine Bestimmung der exakten AS-Konzentration im Bienenstock ist also notwendig, um einerseits das Wirkungsoptimum zu bestimmen und andererseits bei Übersteigen der Maximalkonzentrationen mit Folge-Schädigung der Bienen, ein rechtzeitiges Eingreifen der Imker zu ermöglichen. T2 - 6. HSN-Fachsymposium „Innovative Sensorik, verteilte Sensorsysteme, neue Technologien und Anwendungsfelder“ CY - Karlsruhe, Germany DA - 06.11.2019 KW - Biene KW - Apis mellifera KW - Varroa destructor KW - Ameisensäure KW - Multigassensorik PY - 2019 SP - 22 EP - 25 AN - OPUS4-49605 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Schukar, Vivien A1 - Bartholmai, Matthias A1 - Beck, Uwe T1 - Abschlussbericht zum DFG-Projekt „FAMOS²“ FAser-basierter Magneto-Optischer SchichtSensor N2 - Der Mangel an Anwendungsrichtlinien und Validierungsverfahren für struktur-eingebettete faseroptische Dehnungssensoren, insbesondere auf Faser-Bragg-Gitter (FBG)-Basis, führte bislang dazu, dass diese Sensoren trotz ihrer hervorragenden Eigenschaften im Bereich der kommerziellen Material- und Strukturüberwachung nur in geringem Umfange eingesetzt wurden. Fragen zur Degradation der Sensoren unter Beanspruchung, Alterung durch klimatische Einflüsse und Enthaftung infolge Belastung der Struktur konnten bisher nur theoretisch simuliert oder anhand exemplarischer Proben für einzelne einflussnehmende Parameter im Labor untersucht werden. Die Erfassung des Sensorverhaltens im Bauteil unter komplexen Umwelteinflüssen während des Bauteilbetriebes, um damit eine Aussage zur Zuverlässigkeit der Sensormessdaten zu gewinnen, war bisher nicht möglich. Im Forschungsprojekt FAMOS² wurde deshalb von 2014 bis 2018 die Realisierung eines Autodiagnoseverfahrens für faseroptische Dehnungssensoren erarbeitet, um die Funktionszuverlässigkeit und Langzeitstabilität der Sensoren während des Bauteilbetriebes innerhalb einer Bauteilstruktur bewerten zu können. Im Rahmen des Forschungsprojektes wurde gezeigt, dass ein FBG-Sensor mit einer speziell angepassten magnetostriktiven Schicht magnetisch so angeregt werden kann, dass mit einer zugeschnittenen Messmethodik zu jedem Zeitpunkt eine Bewertung der Sensorzuverlässigkeit unter Betriebsbedingungen möglich ist. Die auf den Sensor aufgebrachte magnetostriktive Schicht erzeugt bei Anregung mit einem passenden Magnetfeld eine gepulste, synthetische Dehnung. Diese Dehnung steht in einem definierten Verhältnis zum anregenden Magnetfeld und wird optisch über die Verschiebung der Bragg-Wellenlänge ausgelesen. Die Konstanz dieses Verhältnisses stellt dann ein Maß für die korrekte Funktionsfähigkeit des Sensors dar. Das Beschichtungs-verfahren, das magnetische Anregungs- und optische Ausleseverfahren, wie auch die Validierung des Sensors unter Berücksichtigung faseroptischer Effekte wurden während des Projekts konzeptionell entwickelt, aufgebaut und charakterisiert. Qualitativ kann mit diesem Verfahren zunächst eine Gut-/Schlecht-Beurteilung des Sensors vorgenommen werden. Perspektivisch bietet das Verfahren jedoch auch die Möglichkeit, verschiedene Versagensmechanismen bestimmen und klassifizieren zu können. Es zeichnete sich schon während des Projektverlaufs ab, dass sich aus den erzielten Ergebnissen über das Autodiagnoseverfahren hinaus weitere Anwendungsmöglichkeiten für den Einsatz des kombinierten magnetostriktiv-faseroptischen Sensorprinzips, beispielsweise als reiner Magnetfeldsensor, ergeben. Nach Abschluss dieses Forschungsprojekts besteht nun die Möglichkeit, den Funktionszustand faseroptischer Dehnungssensoren jederzeit unabhängig von Alter, Belastung oder Kenntnis eines Referenzzustands zu einem bestimmten Zeitpunkt bestimmen zu können. Aufbauend auf diesen Ergebnissen können weiterführende Forschungen die Messmethodik vertiefend charakterisieren und weitere Anwendungsfälle erschließen. KW - Faser-Bragg-Gitter (FBG) KW - Sensorvalidierung KW - Magnetostriktive Beschichtung KW - Structural Health Monitoring (SHM) PY - 2018 N1 - Das Dokument unterliegt der Vertraulichkeit und kann nicht zugänglich gemacht werden - Projektlaufzeit: 01.04.2014 - 31.07.2018 The document is subject to confidentiality restrictions and cannot be made accessible - project runtime: 01.04.2014 - 31.07.2018 SP - 1 EP - 28 AN - OPUS4-50418 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmadi, Samim A1 - Burgholzer, P. A1 - Mayr, G. A1 - Jung, P. A1 - Caire, G. A1 - Ziegler, Mathias T1 - Photothermal super resolution imaging: A comparison of different thermographic reconstruction techniques N2 - This paper presents different super resolution reconstruction techniques to overcome the spatial resolution limits in thermography. Pseudo-random blind structured illumination from a onedimensional laser array is used as heat source for super resolution thermography. Pulsed thermography measurements using an infrared camera with a high frame rate sampling lead to a huge amount of data. To handle this large data set, thermographic reconstruction techniques are an essential step of the overall reconstruction process. Four different thermographic reconstruction techniques are analyzed based on the Fourier transform amplitude, principal component analysis, virtual wave reconstruction and the maximum thermogram. The application of those methods results in a sparse basis representation of the measured data and serves as input for a compressed sensing based algorithm called iterative joint sparsity (IJOSP). Since the thermographic reconstruction techniques have a high influence on the result of the IJOSP algorithm, this paper Highlights their Advantages and disadvantages. KW - Super resolution KW - Compressed sensing KW - Laser thermography KW - Virtual wave KW - Defect reconstruction PY - 2020 DO - https://doi.org/10.1016/j.ndteint.2020.102228 VL - 111 SP - 2228 PB - Elsevier Ltd. CY - Netherlands AN - OPUS4-50419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Beck, Uwe A1 - Stockmann, Jörg M. T1 - AiF Projekt GmbH, KONTRAST – schnell, sicher, sichtbar N2 - Das Projekt KONTRAST adressiert die Qualitätskontrolle (QC) zur Erfassung nano- und mikroskaliger Belegung/Degradation mittels abbildender Ellipsometrie (IE). Das BAM-Teilvorhaben beinhaltet das Screening von Benchmark-Materialsystemen und die Validierung von Messstrategien. Im Ergebnis erfolgte eine Fokussierung auf das im Vergleich zur off Null Ellipsometrie (ONE) aussichtereichere Verfahren der referenzkompensierten Ellipsometrie(RKE), das marktstrategisch in RSE (referenced spectral ellipsometry) umbenannt wurde. Alle Materialsysteme der BAM-Unterauftragnehmer konnten mit IE visualisiert werden, mit dem RSE-System in wesentlich kürzeren Zeiten, auf größeren Flächen, bei vergleichbarer Empfindlichkeit und Auflösung, Komplementärverfahren waren für den schnellen Nachweis nano- und mikroskaliger Belegung nicht konkurrenzfähig, wobei zusätzliche Materialsysteme mit niedrigem Kontrast (SnO:Ni auf Glas bzw. Cr auf Chromstahl) in der BAM hergestellt wurden. Die öffentliche Präsentation des RSE-Prototyps erfolgte auf der ICSE-7 2016 mit der Publikation 2017 in Applied Surface Science. KW - Abbildende Ellipsometrie (IE) KW - Imaging Null Ellipsometrie (INE) KW - Referenced Spectral Ellipsometry (RSE) KW - Oberflächenverunreinigungen KW - Visualisierung bei geringem Kontrast PY - 2017 N1 - Das Dokument unterliegt der Vertraulichkeit und kann nicht zugänglich gemacht werden Projektlaufzeit: 01.10.2014 bis 28.08.2017 The document is subject to confidentiality restrictions and cannot be made accessible Project runtime: 01.10.2014 to 28.08.2017 SP - 1 EP - 16 AN - OPUS4-50420 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Kricheldorf, H. R. T1 - Matrix-assisted laser desorption/ionization behavior of neat linear and cyclic poly(L-lactide)s and their blends N2 - Numerous new tin catalysts that enable the synthesis of cyclic polylactides with broad variation in their molecular mass were recently developed. The abundance of cyclics in matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectra is, however, frequently reported to greatly exceed that of linears. Thus, the MALDI ionization behavior of various end-capped linear poly(L-lactide)s and one cyclic poly(L-lactide) was investigated and compared. Neat compounds and various blends of cyclic and linear species were prepared and studied under identical conditions with regard to sample preparation and instrumental condition, except for the laser power. For this purpose, two different MALDI-TOF mass spectrometers were applied. Our results reveal that cyclics indeed show a slightly better ionization in MALDI, although their ionization as a neat compound seems to be less effective than that of linear polylactides. The ionization of most linear polylactides investigated does not depend on the end group structure. However, linear polylactides containing 12-bromododecyl end groups reveal an unexpected saturation effect that is not caused by fragmentation of the polymer or the end group, or by electronic saturation of the detector digitizer. Furthermore, polylactides with a 2-bromoethyl end group did not show such a saturation effect. An overestimation of cyclic species in MALDI-TOF mass spectra of poly(L-lactide)s must be considered, but the commonly assumed peak suppression of linear polymers in mixtures of both structures can be excluded. KW - Polylactide KW - MALDI-TOF MS KW - Blends KW - Ionization PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504216 DO - https://doi.org/10.1002/rcm.8673 VL - 34 SP - e8673 PB - Wiley Online Libary AN - OPUS4-50421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Friedrich, C. M. A1 - Weigel, S. A1 - Marvin, H. A1 - Rauscher, H. A1 - Wohlleben, W. A1 - Babick, F. A1 - Löschner, K. A1 - Mech, A. A1 - Brüngel, R. A1 - Hodoroaba, Vasile-Dan A1 - Gilliland, D. A1 - Rasmussen, K. A1 - Ghanem, A. T1 - The NanoDefine Methods Manual N2 - This document is a collection of three JRC Technical Reports that together form the “NanoDefine Methods Manual”, which has been developed within the NanoDefine project ‘Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial’, funded by the European Union’s 7th Framework Programme, under grant agreement 604347. The overall goal of the NanoDefine project was to support the implementation of the European Commission Recommendation on the definition of nanomaterial (2011/696/EU). The project has developed an integrated empirical approach, which allows identifying a material as a nano- or not a nanomaterial according to the EC Recommendation. The NanoDefine Methods Manual consists of three parts: Part 1: The NanoDefiner Framework and Tools, which covers the NanoDefiner framework, general information on measurement methods and performance criteria, and tools developed by NanoDefine such as a materials categorisation system, a decision support flow scheme and an e-tool. Part 2: Evaluation of Methods, which discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size. Part 3: Standard Operating Procedures (SOPs), which presents the 23 Standard Operating Procedures developed within the NanoDefine project. In this combined document, these three parts are included as stand-alone reports, each having its own abstract, table of contents, page, table and figure numbering, and references. KW - Nanomaterial KW - Particle size distribution KW - Nanoparticles KW - NanoDefine KW - Nanomaterial classification PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504250 SN - 978-92-76-12335-4 DO - https://doi.org/10.2760/79490 VL - JRC117501 SP - 1 EP - 451 PB - Publications Office of the European Union CY - Luxembourg AN - OPUS4-50425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, C. T1 - Computation of scattering curves for particles with arbitrary shapes using Debye’s formula N2 - Small-angle scattering data from particle dispersions with narrow size distributions are usually analysed by fitting a model function to the data, which is composed of a monodisperse form factor with a size distribution and, optionally, a structure factor. For common particle shapes like solid spheres, core-shell particles, ellipsoids or rods, the form factor can be computed analytically, and several software packages are readily available which provide a compilation of form factors.1,2 Recently, highly monodisperse nanoparticles with a variety of shapes have been synthesized, e.g. cubes and bipyramids3,4 with lightly capped edges, for which analytic form factors are harder to derive. We compute an approximation to the scattering curve of arbitrary shapes by filling the shape with a quasi-random distribution of point scatterers and using Debye’s formula to get the overall scattering curve. The highly optimized debyer code is used to perform an efficient evaluation of Debye’s formula,5 which can perform the evaluation of 500,000 point scatterers in two minutes on commodity hardware. Moderate polydispersity is handled by interpolating the computed scattering curve over q from a master curve. In this way, the code is fast enough to perform data fitting of particle ensembles with moderate polydispersity for arbitrary shapes to experimental data. This work was partly funded by the 17NRM04 nPSize project of the EMPIR programme co-financed by the EMPIR participating states and by the European Union’s Horizon 2020 research and innovation programme. T2 - 17th Nordic Workshop on Scattering from Soft Matter CY - Linköping, Sweden DA - 14.01.2020 KW - X-ray scattering KW - Nanoparticles KW - Particle shape KW - Modelling KW - Form factor PY - 2020 UR - http://nssm2020.se/ AN - OPUS4-50368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mech, A. A1 - Rauscher, H. A1 - Rasmussen, K. A1 - Babick, F. A1 - Hodoroaba, Vasile-Dan A1 - Ghanem, A. A1 - Wohlleben, W. A1 - Marvin, H. A1 - Brüngel, R. A1 - Friedrich, C. M. A1 - Löschner, K. A1 - Gilliland, D. T1 - The NanoDefine Methods Manual - Part 3: Standard Operating Procedures (SOPs) N2 - The present series of reports, the NanoDefine Methods Manual, has been developed within the NanoDefine project 'Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial'1 funded by the European Union's 7th Framework Programme, under grant agreement 604347. In 2011 the European Commission (EC) published the recommendation (2011/696/EU) for a definition of the term 'nanomaterial'1, the EC NM Definition, as a reference to determine whether an unknown material can be considered as a 'nanomaterial' for regulatory purposes. One challenge is the development of methods that reliably identify, characterize and quantify nanomaterials (NM) both as substances and in various products and matrices. The overall goal of NanoDefine was to support the implementation of the EC NM Definition. It can also support the implementation of any NM definition based on particle size. The project has developed an integrated approach, which allows identifying any material as a nano or non-nano material according to the EC NM Definition. NanoDefine explicitly supported the governance challenges associated with the implementation of legislation concerning nanomaterials by: - addressing the issues on availability of suitable measuring techniques, reference materials, validated methods, acceptable to all - developing an integrated and interdisciplinary approach and a close international co-operation and networking with academia, commercial firms and standardization bodies. Thus, the NanoDefine Methods Manual provides guidance on practical implementation of the EC NM Definition throughout the nanomaterial characterization process, and on the characterization techniques employed as well as their application range and limits. It assists the user in choosing the most appropriate measurement method(s) to identify any substance or mixture for a specific purpose, according to the EC NM Definition of a nanomaterial. The NanoDefine project also explored how to assess a material against the criteria of the definition through proxy solutions, i.e. by applying measurement techniques that indirectly determine the D50. Those findings were developed through empirically based scientific work and are included in Part 1 of this Manual. As they go beyond the text of the EC NM Definition, they may be used as practical approach to indicate whether a material is a nanomaterial or not, but keeping in mind that they should not be taken as recommendation for the implementation of the EC NM Definition in a regulatory context. The NanoDefine Methods Manual consists of the following three parts:  Part 1: The NanoDefiner Framework and Tools  Part 2: Evaluation of Methods  Part 3: Standard Operating Procedures (SOPs) Part 1 covers the NanoDefiner framework, general information on measurement methods and performance criteria and tools developed by NanoDefine such as a materials categorisation system, a decision support flow scheme and an e-tool. Part 2 discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size. Part 3 presents the 23 Standard Operating Procedures developed within the NanoDefine project. The current document is part 3. KW - Nanomaterial KW - Nanoparticles KW - Particle size distribution KW - NanoDefine KW - Standard Operation Procedures KW - Nanomaterial classification KW - SOP PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503710 SN - 978-92-76-11955-5 DO - https://doi.org/10.2760/02910 SN - 1831-9424 VL - JRC117501 SP - 1 EP - 215 PB - Publications Office of the European Union CY - Luxembourg AN - OPUS4-50371 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von der Au, Marcus T1 - SPE HR-CS GF MAS – A New Sum Parameter Method for Extractable Organically Bound Fluorine (EOF) in Surface Water N2 - Introducing fluorine into organic molecules leads to new chemical/physical properties. Up to now, the OECD identified and categorized 4730 per- and polyfluoroalkyl substances-related CAS numbers. Especially in the field of technical applications (e.g. surface coatings, fire extinguishing foams) as well as pharmaceuticals, fluorinated substances gain in importance. Thus, an increasing release of fluorinated compounds into the environment is expected. The high environmental persistence of perfluorinated compounds leads to the risk of bioaccumulation. Partially fluorinated substances (polyfluorinated compounds) undergo degradation; thus, further possible fluorine species occur, which may exhibit different toxic/chemical properties. However, current target methods (e.g., HPLC/MS-MS) are not applicable for a comprehensive screening as well as assessment of pollution. Thus, the poster presents a new sum parameter method for quantitative determination of extractable organically bound fluorine (EOF) in surface water samples. The method is based on solid-phase extraction (SPE) for fluorinated compounds as well as quantitative separation of interfering inorganic fluoride in combination with high-resolution-continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) for quantitative analysis. By means of this technique, the detection of high resolution molecular absorption spectra (MAS) is enabled upon the addition of a modifier and the formation of a diatomic molecule (e.g. GaF) After successful optimization of the SPE procedure (maximum concentration of extractable organic fluorine), enrichment factors of about 1000 were achieved, allowing for highly sensitive fluorine detection. Next to a species-unspecific response, limits of detection in the low nanogram per liter range were achieved and real surface water samples were analyzed. EOF values in the range of about 50-300 ng/L were detected. The developed method allows for a fast and sensitive as well as selective screening of organically bound fluorine (EOF) in surface water samples, helping to elucidate pollution hotspots as well as discharge routes. T2 - 2020 Winter Conference on Plasma Spectrochemistry CY - Tucson, AZ, USA DA - 12.01.2020 KW - SPE HR-CS GF MAS KW - Sum parameter KW - Fluorine Detection PY - 2020 AN - OPUS4-50352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ebel, Kenny A1 - Bald, Ilko T1 - Length and Energy Dependence of Low-Energy Electron-Induced Strand Breaks in Poly(A) DNA N2 - The DNA in living cells can be effectively damaged by high-energy radiation, which can lead to cell death. Through the ionization of water molecules, highly reactive secondary species such as low-energy electrons (LEEs) with the most probable energy around 10 eV are generated, which are able to induce DNA strand breaks via dissociative electron attachment. Absolute DNA strand break cross sections of specific DNA sequences can be efficiently determined using DNA origami nanostructures as platforms exposing the target sequences towards LEEs. In this paper, we systematically study the effect of the oligonucleotide length on the strand break cross section at various irradiation energies. The present work focuses on poly-adenine sequences (d(A4), d(A8), d(A12), d(A16), and d(A20)) irradiated with 5.0, 7.0, 8.4, and 10 eV electrons. Independent of the DNA length, the strand break cross section shows a maximum around 7.0 eV electron energy for all investigated oligonucleotides confirming that strand breakage occurs through the initial formation of negative ion resonances. When going from d(A4) to d(A16), the strand break cross section increases with oligonucleotide length, but only at 7.0 and 8.4 eV, i.e., close to the maximum of the negative ion resonance, the increase in the strand break cross section with the length is similar to the increase of an estimated geometrical cross section. For d(A20), a markedly lower DNA strand break cross section is observed for all electron energies, which is tentatively ascribed to a conformational change of the dA20 sequence. The results indicate that, although there is a general length dependence of strand break cross sections, individual nucleotides do not contribute independently of the absolute strand break cross section of the whole DNA strand. The absolute quantification of sequence specific strand breaks will help develop a more accurate molecular level understanding of radiation induced DNA damage, which can then be used for optimized risk estimates in cancer radiation therapy. KW - DNA origami KW - DNA radiation damage KW - DNA strand breaks KW - Low-energy electrons KW - Sequence dependence PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503563 DO - https://doi.org/10.3390/ijms21010111 VL - 21 IS - 1 SP - 1 EP - 11 PB - MDPI CY - Basel, Switzerland AN - OPUS4-50356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, C. A1 - Schierack, P. A1 - Gerber, U. A1 - Schröder, C. A1 - Choi, Youngeun A1 - Bald, Ilko A1 - Lehmann, W. A1 - Rödiger, S. T1 - Streptavidin Homologues for Applications on Solid Surfaces at High Temperatures N2 - One of the most commonly used bonds between two biomolecules is the bond between biotin and streptavidin (SA) or streptavidin homologues (SAHs). A high dissociation constant and the consequent high-temperature stability even allows for its use in nucleic acid detection under polymerase chain reaction (PCR) conditions. There are a number of SAHs available, and for assay design, it is of great interest to determine as to which SAH will perform the best under assay conditions. Although there are numerous single studies on the characterization of SAHs in solution or selected solid phases, there is no systematic study comparing different SAHs for biomolecule-binding, hybridization, and PCR assays on solid phases. We compared streptavidin, core streptavidin, traptavidin, core traptavidin, neutravidin, and monomeric streptavidin on the surface of microbeads (10–15 μm in diameter) and designed multiplex microbead-based experiments and analyzed simultaneously the binding of biotinylated oligonucleotides and the hybridization of oligonucleotides to complementary capture probes. We also bound comparably large DNA origamis to capture probes on the microbead surface. We used a real-time fluorescence microscopy imaging platform, with which it is possible to subject samples to a programmable time and temperature profile and to record binding processes on the microbead surface depending on the time and temperature. With the exception of core traptavidin and monomeric streptavidin, all other SA/SAHs were suitable for our investigations. We found hybridization efficiencies close to 100% for streptavidin, core streptavidin, traptavidin, and neutravidin. These could all be considered equally suitable for hybridization, PCR applications, and melting point analysis. The SA/SAH–biotin bond was temperature-sensitive when the oligonucleotide was mono-biotinylated, with traptavidin being the most stable followed by streptavidin and neutravidin. Mono-biotinylated oligonucleotides can be used in experiments with temperatures up to 70 °C. When oligonucleotides were bis-biotinylated, all SA/SAH–biotin bonds had similar temperature stability under PCR conditions, even if they comprised a streptavidin variant with slower biotin dissociation and increased mechanostability. KW - Biopolymers Probes KW - Hybridization KW - Fluorescence KW - Genetics PY - 2020 DO - https://doi.org/10.1021/acs.langmuir.9b02339 VL - 36 IS - 2 SP - 628 EP - 636 PB - American Chemical Society Publication CY - Washington AN - OPUS4-50357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Gaft, M. A1 - Nagli, L. A1 - Raichlin, Y. T1 - Laser-induced breakdown spectroscopy (LIBS) of BaF2-Tm3+ N2 - Our recent study was focused on the emission from Laser Induced Plasma (LIP) at the delay times of tenths of microseconds after the laser pulse. At these long delays, the spectrum is dominated by the broadband molecular emission and plasma induced luminescence (PIL) produced by a luminescent matrix; only solitary atomic emission lines can be seen. Barium fluoride BaF2 activated by thulium (Tm) is a famous scintillator that presents the promising object for LIP in terms of both the potential for BaF molecular emission and Tm3+ PIL. The detection of molecular and PIL bands presents a new opportunity for analysis of halogens and rare-earth elements, which are the difficult objects for LIBS. In this paper, we show that the UV, Green, Extreme Red, and Infrared molecular bands from BaF and blue luminescence from Tm3+ are present in the LIP emission spectra while the detection of atomic Emission from F I and Tm I was impossible with the same experimental setup. Thus, the detection of molecular emission and PIL can be more sensitive than the traditional detection of Emission from atoms and ions. KW - BaF KW - Laser-Induced Breakdown Spectroscopy (LIBS) KW - Rare-Earth elements (Tm3+) KW - Plasma-induced luminescence PY - 2020 DO - https://doi.org/10.1016/j.sab.2020.105767 VL - 164 SP - 105767 PB - Elsevier B.V. AN - OPUS4-50360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Plasma Fundamentals and Diagnostics N2 - This course will provide an introduction to plasma diagnostic techniques. The major focus of the course will be on the discussions of the practical procedures as well as the underlying physical principles for the measurements of plasma fundamental characteristics (e.g., temperatures, thermodynamic properties, and electron number density). Particular emphasis will be placed on inductively coupled plasma–atomic emission spectrometry, but other analytical plasmas will also be used as examples when appropriate. Selected examples on how one can manipulate the operating conditions of the plasma source, based on the results of plasma diagnostic measurements, to improve its performance used for spectrochemical analysis will also be covered. Topics to be covered include thermal equilibrium, line profiles, temperatures, electron densities, excitation processes, microreactions, pump and probe diagnostics, tomography, temporal and spatial resolution. Basis of plasma computer modeling will be presented. T2 - Winter Plasma Conference CY - Tucson, AZ, USA DA - 10.01.2020 KW - Plasma modeling KW - Thermal equilibrium KW - Plasma processes KW - Electron number density KW - Temperatures KW - Emission line profiles KW - Spatial information PY - 2020 AN - OPUS4-50324 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Particle Scattering Simulations with Geant4: An Overview N2 - A brief overview over the capabilities of Geant4 is provided together with some example applications T2 - Seminar of the bioanalysis group CY - Universidad Nacional de Colombia, Bogotá, Columbia DA - 03.02.2020 KW - Geant4 KW - Geant4-DNA KW - MCS KW - Simulation KW - Monte-Carlo simulation KW - Particle scattering simulation KW - Dosimetry KW - Xrays KW - Electrons KW - Radiation PY - 2020 AN - OPUS4-50332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Hands on: Particle scattering simulations A practical introduction N2 - A practical introduction is given for the necessary steps to start with particle scattering simulations based on Geant4/Topas. T2 - Seminar of the bioanalysis group CY - Universidad Nacional de Colombia, Bogotá, Columbia DA - 04.02.2020 KW - Geant4 KW - Geant4-DNA KW - MCS KW - Monte-Carlo simulations KW - Simulations KW - Particle scattering simulation KW - Scattering KW - Topas PY - 2020 AN - OPUS4-50333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Martin A1 - Weller, Michael G. T1 - Antibody screening by microarray technology - Direct identification of selective high-affinity clones N2 - The primary screening of hybridoma cells is a time-critical and laborious step during the development of monoclonal antibodies. Often, critical errors occur in this phase, which supports the notion that the generation of monoclonal antibodies with hybridoma technology is difficult to control and hence, a risky venture. We think that it is crucial to improve the screening process to eliminate most of the critical deficits of the conventional approach. With this new microarray-based procedure, several advances could be achieved: Selectivity for excellent binders, high-throughput, reproducible signals, avoidance of misleading avidity (multivalency) effects, and performance of simultaneous competition experiments. The latter can also be used to select clones of desired cross-reactivity properties. In this paper, a model system with two excellent clones against carbamazepine, two weak clones, and blank supernatant containing fetal bovine serum was designed to examine the effectiveness of the new system. The excellent clones could be detected largely independent of the immunoglobulin G (IgG) concentration, which is usually unknown during the clone screening since the determination and subsequent adjustment of the antibody concentration are not feasible in most cases. Furthermore, in this approach, the enrichment, isolation, and purification of IgG for characterization is not necessary. Raw cell culture supernatant can be used directly, even when fetal calf serum (FCS) or other complex media is used. In addition, an improved method for the oriented antibody-immobilization on epoxy-silanized slides is presented. Based on the results of this model system with simulated hybridoma supernatants, we conclude that this approach should be preferable to most other protocols leading to many false positives, causing expensive and lengthy elimination steps to weed out the poor clones. KW - ELISA KW - Immunoassay KW - Microarray KW - Lab-on-a-chip KW - Miniaturization KW - Aautomatisation KW - HTS KW - High-throughput KW - Screening KW - Fluorescence KW - Label KW - Hybridoma KW - Inhibition PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503361 DO - https://doi.org/10.3390/antib9010001 SN - 2073-4468 VL - 9 IS - 1 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-50336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Helmerich, Rosemarie A1 - Moldenhauer, Laura A1 - Voigt, Gerrit A1 - Köppe, E. T1 - Considerations for identification of moisture in building materials using Bluetooth (R) N2 - The vulnerability of low-quality concrete of some bridges to ageing and deterioration while they are exposed to environmental conditions during their service life, influence of growing population and climate changes, is a well-known effect and requires survey. For survey, the development of a low cost, cost-efficient sensor network to be embedded for continuous or attached to the surface for periodic monitoring is essential. Changing ground water conditions, flood or even leakage in fresh or disposal of waste water can lead to in-creased moisture content in building materials and structural elements as walls or floors. Moisture allows the transport of other adverse chemicals that might reduce the durability of structures. The paper presents a feasibility study about the capability of microwave modules as bluetooth® or ZigBee with frequency range at 2,4 GHz to create advanced Wireless Sensor Networks (WSN) for estimation and visualization of moisture distribution in infrastructure assets. It was found that the value of the received signal strength indication (RSSI) depends on the moisture content and can be the basis for the moisture distribution inside a massive structure. The microwave modules may be used to compose networks outside and inside of building materials or structural elements. The higher the number of connections between BLE modules, the more precise and the more distant information can be obtained from the network. Mesh networking was applied to increase the quantitative information. T2 - 9th International Conference on Bridge Maintenance, Safety and Management (IABMAS) CY - Melbourne, Australia DA - 09.07.2018 KW - Structural Health Monitoring KW - Moisture KW - Bluetooth PY - 2018 SN - 978-1-315-18939-0 SN - 978-1-138-73045-8 SP - 2752 EP - 2759 AN - OPUS4-50340 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Beck, Uwe T1 - Abschlussbericht zum BMWi / MNPQ – Verbundprojekt Quo Vadis Qualitätssicherung von Verbundwerkstoffen und Validierung des Zentrifugenversuchs – eines neuartigen Prüfverfahrens zur Bestimmung von Verbundfestigkeiten N2 - Quo Vadis – Kurzdarstellung Im Fokus von Quo Vadis stehen die Qualitätssicherung von Verbundwerkstoffen und die Validierung der Zentrifugentechnologie zur quantitativen Bestimmung von Festigkeitswerten in der Beanspruchung auf Zug als Mehr-Proben-Prüfverfahren unter Verwendung einer analytischen Zentrifuge (nachfolgend als „Adhesion Analyser LUMiFrac®“ bezeichnet). Zu den Festigkeiten, die mit Hilfe des LUMiFrac® unter Verwendung aufgeklebter Prüfstempel bestimmt werden, gehören die Fügefestigkeit (FF) von Klebverbindungen, die Haftfestigkeit (HF) von Beschichtungen sowie die Verbundfestigkeit (VF) von Faserverbundwerkstoffen. Aufbauend auf zwei Funktionsmustern der analytischen Zentrifuge sollen für die genannten Anwendungsszenarien (FF, HF, VF) in Anlehnung an die geltenden Normen DIN EN 15870 „Klebstoffe – Zugprüfung zur Bestimmung der Zugfestigkeit von Stumpfklebungen“ und DIN EN ISO 4624 „Beschichtungsstoffe – Abreißversuch zur Beurteilung der Haftfestigkeit“ geeignete Prüfstrategien und -abläufe sowie zum Klebprozess kompatible Aufnahmen für den Prüfkörperverbund in der Zentrifuge entwickelt werden. Im Ergebnis des Vorhabens soll ein automatisiertes und validiertes Mehr-Proben-Prüfverfahren zur Qualitätssicherung von Verbundfestigkeiten zur Verfügung stehen, welches neben der Hardware auch eine Software für die angepassten Prüfstrategien in Form von SOPs (standard operating procedures) bereitstellt. KW - Zentrifugentechnologie KW - Mehr-Proben-Prüfverfahren KW - Fügefestigkeit KW - Klebverbindungen KW - Haftfestigkeit KW - Beschichtungen KW - Verbundfestigkeit KW - Zugfestigkeit PY - 2015 N1 - Das Dokument unterliegt der Vertraulichkeit und kann nicht zugänglich gemacht werden Projektlaufzeit: 01.05.2012 bis 31.08.2015 The document is subject to confidentiality restrictions and cannot be made accessible Project runtime: 01.05.2012 bis 31.08.2015 SP - 1 EP - 12 AN - OPUS4-50390 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - EURAMET.QM-S14 "Measurement capabilities for the quantification of ethanol in water" - Summary of results N2 - The presentation summarizes the results of the EURAMET key comparison QM-S14 “Measurement capabilities for the quantification of ethanol in water”. Possible options for the key comparison reference value are discussed. T2 - EURAMET TC-MC Meeting 2020 CY - Bern, Switzerland DA - 05.02.2020 KW - EURAMET KW - Key comparison KW - Ethanol in water PY - 2020 AN - OPUS4-50391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kondo, M. A1 - Melzer, Michael A1 - Karnaushenko, D. A1 - Uemura, T. A1 - Yoshimoto, S. A1 - Aklyama, M. A1 - Noda, Y. A1 - Araki, T. A1 - Schmidt, O. G. A1 - Sekitani, T. T1 - Imperceptible magnetic sensor matrix system integrated with organic driver and amplifier circuits N2 - Artificial electronic skins (e-skins) comprise an integrated matrix of flexible devices arranged on a soft, reconfigurable surface. These sensors must perceive physical interaction spaces between external objects and robots or humans. Among various types of sensors, flexible magnetic sensors and the matrix configuration are preferable for such position sensing. However, sensor matrices must efficiently map the magnetic field with real-time encoding of the positions and motions of magnetic objects. This paper reports an ultrathin magnetic sensor matrix system comprising a 2 × 4 array of magnetoresistance sensors, a bootstrap organic shift register driving the sensor matrix, and organic signal amplifiers integrated within a single imperceptible platform. The system demonstrates high magnetic sensitivity owing to the use of organic amplifiers. Moreover, the shift register enabled real-time mapping of 2D magnetic field distribution. KW - Imperceptible electronics KW - Magnetic sensor system KW - Electronic skin KW - Organic electronics KW - Giant magnetoresistance PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503855 DO - https://doi.org/10.1126/sciadv.aay6094 SN - 2375-2548 VL - 6 IS - 4 SP - Paper eaay6094, 1 EP - 10 PB - American Association for the Advancement of Science AN - OPUS4-50385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Beck, Uwe A1 - Krüger, A. T1 - Abschlussbericht für das Kooperationsprojekt zwischen Unternehmen und Forschungseinrichtungen (KF) - Nanoskalige Haftvermittler zur Erhöhung der Haft- bzw. Klebfestigkeit kritischer Verbundsysteme unter Verwendung von ALD-Hybridprozessen N2 - Aufzählung der wichtigsten wissenschaftlich-technischen und anderer wesentlicher Ergebnisse • ALD Abscheidungen auf Polymeren (PE, PP, PTFE) unter Atmosphärendruck und im Vakuum mit Ozon als Oxidationsmittel wurden durchgeführt: - Mit Variation der Schichtdicke - Mit Variation der Zykluszeit - Mit und ohne Ozon Vorbehandlung der Oberfläche • ALD Abscheidungen auf (PE, PP, PTFE) in Vakuum mit O2- und H2-Plasma Vorbehandlung wurden durchgeführt. - Mit Variation der Schichtdicke - Mit Variation der Zykluszeit - Mit und ohne Plasma Vorbehandlung der Oberfläche • Die ALD Prozesse wurden mit in situ Laserellipsometrie untersucht. • Die ALD Schichten wurden für die Haftfestigkeit bei der BAM ausgewerte KW - ALD-Abscheidungen KW - Plasma Vorbehandlung KW - Laserellipsometrie KW - Haftfestigkeit PY - 2017 N1 - Das Dokument unterliegt der Vertraulichkeit und kann nicht zugänglich gemacht werden - The document is subject to confidentiality restrictions and cannot be made accessible - Projektlaufzeit: 01.07.2015-30.06.2017 - Project runtime: 01.07.2015-30.06.2017 SP - 1 EP - 17 AN - OPUS4-50386 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulka, M. W. A1 - Donskyi, Ievgen A1 - Wurzler, Nina A1 - Salz, D. A1 - Özcan Sandikcioglu, Özlem A1 - Unger, Wolfgang A1 - Haag, R. T1 - Mussel-Inspired Multivalent Linear Polyglycerol Coatings Outperform Monovalent Polyethylene Glycol Coatings in Antifouling Surface Properties N2 - Biofouling constitutes a major challenge in the application of biosensors and biomedical implants, as well as for (food) packaging and marine equipment. In this work, an antifouling surface coating based on the combination of mussel-inspired dendritic polyglycerol (MI-dPG) and an amine-functionalized block copolymer of linear polyglycerol (lPG−b−OA11, OA = oligo-amine) was developed. The coating was compared to a MI-dPG surface which was postfunctionalized with commercially available amine-terminated Polyethylene glycol (HO−PEG−NH2) of similar molecular weight. In the current work, These coatings were compared in their chemical stability, protein fouling characteristics, and cell fouling characteristics. The lPG−b−OA11-functionalized coating showed high chemical stability in both phosphate buffered saline (PBS) and sodium dodecyl sulfate (SDS) solutions and reduced the adhesion of fibrinogen from human plasma with 99% and the adhesion of human serum albumin with 96%, in comparison to the bare titanium dioxide substrate. Furthermore, the Proliferation of human umbilical vein endothelial cells (HUVECs) was reduced with 85% when the lPG−b−OA11 system was compared to bare titanium dioxide. Additionally, a reduction of 94% was observed when the lPG−b−OA11 system was compared to tissue culture polystyrene. KW - Antifouling surface coatings KW - Human umbilical cell adhesion KW - Linear polyglycerol KW - Polyethylene glycol KW - Mussel-inspired adhesives PY - 2019 DO - https://doi.org/10.1021/acsabm.9b00786 VL - 2 IS - 12 SP - 5749 EP - 5759 PB - ACS AN - OPUS4-50342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, C. A1 - Hensen, C. A1 - Wallmann, K. A1 - Liebetrau, V. A1 - Tatzel, Michael A1 - Schurr, S. L. A1 - Kutterolf, S. A1 - Haffert, L. A1 - Geilert, Sonja A1 - Hübscher, C. A1 - Lebas, E. A1 - Heuser, A. A1 - Schmidt, M. A1 - Strauss, H. A1 - Vogl, Jochen A1 - Hansteen, T. T1 - Origin of High Mg and SO4 Fluids in Sediments of the Terceira Rift, Azores‐Indications for Caminite Dissolution in a Waning Hydrothermal System N2 - During R/V Meteor cruise 141/1, pore fluids of near surface sediments were investigated to find indications for hydrothermal activity in the Terceira Rift (TR), a hyperslow spreading center in the Central North Atlantic Ocean. To date, submarine hydrothermal fluid venting in the TR has only been reported for the D. João de Castro seamount, which presently seems to be inactive. Pore fluids sampled close to a volcanic cone at 2,800‐m water depth show an anomalous composition with Mg, SO4, and total alkalinity concentrations significantly higher than seawater and a nearby reference core. The most straightforward way of interpreting these deviations is the dissolution of the hydrothermally formed mineral caminite (MgSO4 0.25 Mg (OH)2 0.2H2O). This interpretation is corroborated by a thorough investigation of fluid isotope systems (δ26Mg, δ30Si, δ34S, δ44/42Ca, and 87Sr/86Sr). Caminite is known from mineral assemblages with anhydrite and forms in hydrothermal recharge zones only under specific conditions such as high fluid temperatures and in altered oceanic crust, which are conditions generally met at the TR. We hypothesize that caminite was formed during hydrothermal activity and is now dissolving during the waning state of the hydrothermal system, so that caminite mineralization is shifted out of its stability zone. Ongoing fluid circulation through the basement is transporting the geochemical signal via slow advection toward the seafloor. KW - Isotope ratio KW - Delta value KW - Pore fluids KW - Magnesium KW - Hydrothermal fluid PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503430 DO - https://doi.org/10.1029/2019GC008525 VL - 20 IS - 12 SP - 6078 EP - 6094 PB - Wiley AN - OPUS4-50343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope ratio working group at CCQM N2 - The presentation gives the reasons for initiation of an isotope ratio working group at CCQM level, describes the process and provides the auduince with the initial working plan. T2 - EURAMET TC-MC Workshop on Isotope Ratio Analysis CY - Bern, Switzerland DA - 05.02.2020 KW - Metrology KW - Absolute isotope ratio KW - Isotope ratio KW - Delta value PY - 2020 AN - OPUS4-50344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - CCQM IRWG draft strategy for all elements except for noble gases and H, C, N, O N2 - The presentation describes the draft strategy for metalloids and semi-metals within the IRWG at CCQM. This includes the definition of the measurements space, a suitable set of key comparisons and pilot studies and a proposal for a harmonized CMC application. T2 - EURAMET TC-MC Workshop on Isotope Ratio Analysis CY - Bern, Switzerland DA - 05.02.2020 KW - CMC KW - Measurement space KW - Metrology KW - Isotope ratio PY - 2020 AN - OPUS4-50345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Absolute isotope ratios - a proposed research topic N2 - An introduction into absolute isotope ratios is given, with application fields ranging from fundamental science to geochronology and forensics. This is followed by a proposal for developing new calibration approaches for obtaining absolute isotope ratios at unrivaled uncertainty levels. This new developments will set the basis for improvements in all scientific fields. T2 - EURAMET TC-MC Workshop on Isotope Ratio Analysis CY - Bern, Switzerland DA - 05.02.2020 KW - Absolute isotope ratio KW - Isotope fractionation KW - Metrology KW - Fundamental science PY - 2020 AN - OPUS4-50346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hampel, U. A1 - Schütze, A. A1 - Rädle, M. A1 - Rück, T. A1 - Krawczyk-Becker, M. A1 - Musch, T. A1 - Maiwald, Michael A1 - Fröhlich, H. J. A1 - Zeck, S. T1 - Positionspapier Sensorik für die Digitalisierung chemischer Produktionsanlagen N2 - Die chemische Industrie steht derzeit, wie viele andere Industriebereiche, vor den Herausforderungen einer Digitalisierung der Produktion. Sie ist der Schlüssel für die Flexibilisierung von Prozessen und Anlagen, für die Verkürzung von Produkteinführungszeiten sowie für den Zuschnitt der Produktion auf wechselnde Nachfrage und kürzere Produktlebenszyklen. Die Messtechnik und Sensorik spielt neben der intelligenten Datenverarbeitung eine Schlüsselrolle für die Digitalisierung. Flexiblere Anlagen benötigen Sensorik zur Überwachung des Anlagenzustandes, zur Früherkennung nicht bestimmungsgemäßer Betriebszustände sowie für eine bedarfsgerechte Wartung. Da die Entwicklung neuer und verbesserter Messtechnik und Sensorik grundlegend aus verschiedenen Richtungen gedacht werden muss, haben sich Akteure aus verschiedenen Branchen zusammengetan und dieses Positionspapier erstellt. Es basiert auf einer grundlegenden Analyse des Ist-Stands sowie des Bedarfs der Industrie, die unter anderem auf einem eigens dafür durchgeführten Workshop mit Sensorentwicklern, Anlagenherstellern sowie Anlagenbetreibern am 18. Juni 2019 bei der DECHEMA in Frankfurt a. M. diskutiert wurden. Diese Aktivitäten wurden maßgeblich von der Initiative Wanted Technologies der ProcessNet sowie dem AMA Verband für Sensorik und Messtechnik e.V. initiiert. KW - Prozessindustrie KW - Smarte Sensoren KW - Prozessanalytik KW - DECHEMA KW - Positionspapier PY - 2020 UR - https://dechema.de/Sensorik SP - 1 EP - 20 PB - DECHEMA CY - Frankfurt am Main AN - OPUS4-50403 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Beck, Uwe A1 - Hielscher, Stefan A1 - Lerche, D. T1 - Abschlussbericht zum BMWi - MNPQ – Verbundprojekt QUO VADIS PLUS (Mehr-Proben-Festigkeitsprüfung zur Qualitätssicherung in der Materialtechnik und Validierung der Zentrifugentechnologie bei Druck- bzw. Zugbeanspruchung) N2 - Im Fokus des Vorhabens steht das mit dem Innovationspreis Berlin-Brandenburg 2012 ausgezeichnete Mehr-Proben-Prüfverfahren zur Festigkeitsprüfung unter Verwendung einer analytischen Zentrifuge mit dem Ziel des Einsatzes in der Qualitätssicherung. Nachdem im MNPQ-Projekt QUO VADIS die grundsätzliche Anwendbarkeit der Zentrifugentechnologie auf Beanspruchungen auf Zug (Kleb-, Haft- und Verbundfestigkeit) nachgewiesen worden war, wurden im Vorhaben QUO VADIS PLUS folgende erweiterte Prüfszenarien und technische Weiterentwicklungen etabliert: 1. Beanspruchung auf Druck (Härte von Materialien, Kompressibilität von Schäumen, Kompaktierbarkeit von Pulvern), 2. Erweiterung der Beanspruchung auf Zug (Kombination von Normal- und Lateralkräften), 3. Erweiterung auf die Bewertung plasto-elastischenn Materialverhaltens, 4. Vermeidung von Schockwellen im Hochlastbereich KW - Analytische Zentrifuge KW - Mehr-Proben-Prüfverfahren KW - Härte KW - Kompressibilität KW - Kompaktierbarkeit KW - Haftfestigkeit KW - Klebfestigkeit KW - Verbundfestigkeit PY - 2019 N1 - Das Dokument unterliegt der Vertraulichkeit und kann nicht zugänglich gemacht werden Projektlaufzeit: 01.05.2015 bis 28.02.2019 The document is subject to confidentiality restrictions and cannot be made accessible Project runtime: 01.05.2015 to 28.02.2019 SP - 1 EP - 20 AN - OPUS4-50406 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kowarik, Stefan T1 - Smart materials and structures based on fiber optic sensing N2 - This talk gives an overview of basic techniques. Towards the end some applications of neural networks are discussed. T2 - BAM - IFW workshop CY - Berlin, Germany DA - 25.11.2019 KW - Artificial neural networks KW - Fiber optic sensing PY - 2019 AN - OPUS4-49901 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kowarik, Stefan T1 - Neue Entwicklungen der Faseroptische Sensorik: von Infrastruktur-Monitoring zu neuronalen Netzen N2 - Der Vortrag gibt eine Einführung zu obigen Themen auf Niveau von Master Studierenden. T2 - TUM-Tag CY - BAM, Berlin, Adlershof DA - 19.06.2019 KW - Faseroptische Sensorik PY - 2019 AN - OPUS4-49902 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael A1 - Völker, J. T1 - Wir dürfen uns nicht zu sicher werden N2 - Die Erwartungen der Prozessindustrie an die NAMUR Open Architecture sind groß, schließlich soll das Konzept der Garant für die digitale Transformation der Branche sein. Im atp-Interview warnt Dr. Michael Maiwald, Fachbereichsleiter „Prozessanalytik“ an der Bundesanstalt für Materialforschung und -prüfung (BAM), allerdings davor, NOA als Allheilmittel zu betrachten. KW - Prozessindustrie KW - NAMUR Open Architecture KW - NOA KW - Industrie 4.0 KW - Digitale Transformation PY - 2019 UR - https://www.atpinfo.de/produkte/2019-atp-magazin-10-2019/ SN - 2190-4111 IS - 10 SP - 40 EP - 43 PB - Vulkan-Verlag GmbH CY - Essen AN - OPUS4-49501 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Z., Zhang A1 - Ewert, Uwe A1 - Barrett, T. D. A1 - Bond, L. J. T1 - Paper Watermark Imaging using Electron and Low Energy X-ray Radiography N2 - Historians and librarians are interested in watermarks and mould surface patterns in historic papers, because they represent the “fingerprints” of antique papers. However, these features are usually covered or hidden by printing, writing or other media. Different techniques have been developed to extract the watermarks in the paper while avoiding interference from media on the paper. Beta radiography provides good results, but this method cannot be widely used because of radiation safety regulations and the long exposure times required due to weak isotope sources employed. In this work, two promising methods are compared which can be used to extract digital high-resolution images for paper watermarks and these are electron radiography and low energy X-ray radiography. For electron radiography a “sandwich” of a lead sheet, the paper object, and a film in a dark cassette, is formed and it is exposed at higher X-ray potentials (> 300 kV). The photoelectrons escaping from the lead sheet penetrate the paper and expose the film. After development, the film captures the watermark and mould surface pattern Images for the paper being investigated. These images are then digitized using an X-ray film digitizer. The film employed could potentially be replaced by a special type of imaging plate with a very thin protection layer to directly generate digital Images using computed radiography (CR). For the second method, a low energy X-ray source is used with the specimen paper placed on a digital detector array (DDA). This method directly generates a low energy digital radiography (DR) image. Both methods provide high quality images without interference from the printing media, and provide the potential to generate a “fingerprint” database for historical papers. There were nevertheless found to be differences in the images obtained using the two methods. The second method, using a low energy X-ray source, has the potential to be integrated in a portable device with a small footprint incorporating user safety requirements. Differences obtained using the two methods are shown and discussed. T2 - 45th Annual Conference on Review of Progress in Quantitative Nondestructive Evaluation (QNDE) CY - Burlington, VT, USA DA - 15.07.2018 KW - X-ray Radiography KW - Paper watermark PY - 2019 SN - 978-0-7354-1832-5 DO - https://doi.org/10.1063/1.5099750 SN - 0094-243X VL - 2102 IS - 1 SP - 030004-1 EP - 030004-9 PB - American Institute of Physics AN - OPUS4-49922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Puthiyaveettil, N. A1 - Kidangan, R. A1 - Unnikrishnakurup, Sreedhar A1 - Krishnamurthy, C. V. A1 - Ziegler, Mathias A1 - Myrach, Philipp A1 - Balasubramaniam, K. T1 - Numerical study of laser line thermography for crack detection at high temperature N2 - The detection of cracks before the failure is highly significant when it comes to safety-relevant structures. Crack detection in metallic samples at high surface temperature is one of the challenging situation in manufacturing industries. Laser thermography has already proved its detection capability of surface cracks in metallic samples at room temperature. In this work a continuous wave (CW) laser use to generate a laser, which is using to scan the metal surface with notch. The corresponding heat distribution on the surface monitored using infrared thermal (IR) camera. A simplified 3D model for laser thermography is developed and validated with experimental results. A dedicated image processing algorithm developed to improve the detectability of the cracks. To understand the dependency of surface temperature, laser power, laser scanning speed etc. in defect detection, we carried out parametric studies with our validated model. Here we Report the capability of laser thermography in crack detection at elevated temperature. T2 - 14th Quantitative InfraRed Thermography Conference CY - Berlin, Germany DA - 25.06.2018 KW - Thermal contrast KW - Laser Thermography KW - FEM KW - Surface cracks KW - NDT PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499113 DO - https://doi.org/10.21611/qirt.2018.076 SN - 2371-4085 VL - 2018 SP - 685 EP - 686 AN - OPUS4-49911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Burgholzer, P. T1 - Blind structured illumination as excitation for super-resolution photothermal radiometry N2 - Photothermal radiometry with an infrared camera allows the contactless temperature measurement of multiple surface pixels simultaneously. A short light pulse heats the sample. The heat propagates through the sample by diffusion and the corresponding temperature increase is measured at the samples surface by an infrared camera. The main drawback in radiometric imaging is the loss of the spatial resolution with increasing depth due to heat diffusion, which results in blurred images for deeper lying structures. We circumvent this information loss due to the diffusion process by using blind structured illumination, combined with a non-linear joint sparsity reconstruction algorithm. T2 - Fifth NDTonAIR Training Event: Thermography Workshop CY - Linz, Austria DA - 13.02.2019 KW - Super resolution KW - Thermography KW - Laser Thermography KW - Compressed Sensing KW - NDT PY - 2019 AN - OPUS4-49912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sentker, K. A1 - Yildirim, Arda A1 - Lippmann, M. A1 - Zantop, A. W. A1 - Bertram, F. A1 - Hofmann, T. A1 - Seeck, O. H. A1 - Kityk, A. A1 - Mazza, M. G. A1 - Schönhals, Andreas A1 - Huber, P. T1 - Self-assembly of liquid crystals in nanoporous solids for adaptive photonic metamaterials N2 - Nanoporous media exhibit structures significantly smaller than the wavelengths of visible light and can thus act as photonic metamaterials. Their optical functionality is not determined by the properties of the base materials, but rather by tailored, multiscale structures, in terms of precise pore shape, geometry, and orientation. Embedding liquid crystals in pore space provides additional opportunities to control light–matter interactions at the single-pore, meta-atomic scale. Here, we present temperature-dependent 3D reciprocal space mapping using synchrotron-based X-ray diffraction in combination with high-Resolution birefringence experiments on disk-like mesogens (HAT6) imbibed in self-ordered arrays of parallel cylindrical pores 17 to 160 nm across in monolithic anodic aluminium oxide (AAO). In agreement with Monte Carlo computer simulations we observe a remarkably rich self-assembly behaviour, unknown from the bulk state. It encompasses transitions between the isotropic liquid state and discotic stacking in linear columns as well as circular concentric ring formation perpendicular and parallel to the pore axis. These textural transitions underpin an optical birefringence functionality, tuneable in magnitude and in sign from positive to negative via pore size, pore surface-grafting and temperature. Our study demonstrates that the advent of large-scale, self-organised nanoporosity in monolithic solids along with confinement-controllable phase behaviour of liquid-crystalline matter at the single-pore scale provides a reliable and accessible tool to design materials with adjustable optical anisotropy, and thus offers versatile pathways to finetune polarisation-dependent light propagation speeds in materials. Such a tailorability is at the core of the emerging field of transformative optics, allowing, e.g., adjustable light absorbers and extremely thin metalenses. KW - Discotic Liquid Crystals PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499601 DO - https://doi.org/10.1039/c9nr07143a SP - 1 EP - 14 PB - RSC Royal Society of Chemistry AN - OPUS4-49960 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - X-ray fluorescence imaging with coded apertures N2 - We developed a new method for full field X-ray fluorescence imaging at the BAMline @ BESSY II. We combined an energy dispersive array detector for X-rays with a coded aperture to get high resolution images. In coded aperture imaging, an object is projected through a mask, producing many overlapping images on the detector. To get the information about the investigated object out of the projected image, a decoding step is necessary. The first part of our project was to develop the decoding algorithms. We tested the reported reconstruction with an antimask and compared the results with the performance of self-written reconstruction programs based on an iterative and a genetic algorithm. First tests were performed with raytracing simulations. The next step was the collection of experimental data at the BAMline @ BESSY II (HZB). A test objects could be successfully reconstructed with our newly developed algorithm. T2 - PRORA 2019 CY - Berlin, Germany DA - 28.11.2019 KW - X-ray KW - Imaging KW - Fluorescence KW - Coded apertures PY - 2019 AN - OPUS4-49963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - Full field X-ray fluorescence imaging with coded apertures N2 - Our aim is to develop a new simple and inexpensive method for full field X-ray fluorescence imaging. We combine an energy-dispersive array detector with a coded aperture. To obtain the information from the recorded image, a reconstruction step is necessary. First tests were carried out at the BAMline at BESSY II. This method enables the simultaneous detection of multiple elements, which is important e.g. in the field of catalysis. T2 - BESSY Usermeeting CY - Berlin, Germany DA - 05.12.2019 KW - X-ray KW - Fluorescence KW - Imaging KW - Coded Apertures PY - 2019 AN - OPUS4-49964 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - NSO-Heterozyklen – Zwischen Rattengift und Normung N2 - Warfarin als ein Vertreter der NSO-Hetereozyklen, ist seit den 1950er Jahren einer der bekanntesten Gerinnungshemmer. Beim Menschen wird es bis heute zur Vorbeugung von Thrombose und der Behandlung von Vorhofflimmern und Arrhythmie eingesetzt. Doch schon einige Jahre vor der FDA Zulassung als Medikament wurde es zur Bekämpfung von Nagetieren eingesetzt. Bis heute wurde es nur teilweise durch weitaus wirksamere antikoagulante Rodentizide (ARs) der zweiten Generation, sogenannte Superwarfarine, ersetzt. In der Fachliteratur finden sich zahlreiche Beispiele für sekundäre und tertiäre Vergiftung mit ARs bei Wildtieren und anderen Nichtzieltieren. Bisher ist relativ wenig über die Bioakkumulation, Persistenz und Toxizität von ARs und deren Transformationsprodukten (TPs) in der terrestrischen und aquatischen Umwelt, sowie der Nahrungskette bekannt. Um Einblicke in mögliche Transformations- und Abbauprozesse von Warfarin zu erhalten und um Umwelteinflüsse zu simulieren, wurde es in einer elektrochemischen Reaktorzelle oxidativ umgesetzt und mittels Massenspektrometrie analysiert. Hinsichtlich der Wasseraufbereitung in Kläranlagen wurden technisch relevante Simulationsverfahren wie Chlorung, UV-Bestrahlung und Ozonung angewendet um potentielle Eliminierungswege aufzuklären. Gebildete Transformationsprodukte wurden daher mittels unterschiedlicher chromatografischer Verfahren getrennt, massenspektrometrisch analysiert und verglichen. T2 - MS-Tage CY - Düsseldorf, Germany DA - 03.12.2019 KW - GC-MS KW - Warfarin KW - NSO-Heterozyklen PY - 2019 AN - OPUS4-49974 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina T1 - Structure-properties relationships in cadmium benzylphosphonates N2 - The exploration of metal phosphonates has gained great interest during the last decades, because of their structural diversity. They are promising candidates for a variety of applications ranging from adsorbance to electrocatalysis. The knowledge of the Crystal structure is significant for assigning a coordination polymer for a specific function. We investigated the influence of the fluorination degree of the organic linker on the Crystal packing, the interlayer distance, and the hydrophobicity of the resulting compounds. With fluorinated and nonfluorinated benzylphosphonic acids as starting materials in mechanochemical synthesis, four novel cadmium benzylphosphonates were obtained. Their structures were solved from powder X-ray diffraction. T2 - 2nd European Workshop on Metal Phosphonates CY - Berlin, Germany DA - 24.09.2019 KW - Mechanochemistry KW - Metal phosphonates KW - PXRD KW - DVS PY - 2019 AN - OPUS4-49933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Verbesserung des räumlichen Auflösungsvermögens der Impuls-Thermografie durch strukturierte Laser-Erwärmung und Joint Sparsity Rekonstruktion N2 - Die thermografische ZfP basiert auf der Wechselwirkung von thermischen Wellen mit Inhomogenitäten. Diese Inhomogenitäten hängen mit der Probengeometrie oder der Materialzusammensetzung zusammen. Obwohl die Thermografie für ein breites Spektrum von Inhomogenitäten und Materialien geeignet ist, ist die grundlegende Einschränkung die diffuse Natur der thermischen Wellen und die Notwendigkeit, ihre Wirkung lediglich an der Probenoberfläche radiometrisch messen zu können. Die Ausbreitung der thermischen Wellen von der Wärmequelle über die Inhomogenität zur Detektionsoberfläche führt zu einer Verschlechterung des räumlichen Auflösungsvermögens der thermografischen Technik. Ein neuer konzertierter Ansatz auf Basis einer räumlich strukturierten Erwärmung und einer Joint Sparsity des Signalensembles ermöglicht eine verbesserte Rekonstruktion von Inhomogenitäten. Im Beitrag wird die Implementierung dieses Ansatzes auf Basis einer strukturierten Beleuchtung mit einem 1D-Laser-Array vorgestellt. Die einzelnen Emitterzellen des Laser-Arrays werden durch ein pseudozufälliges Binärmuster gesteuert und zusätzlich leicht verschoben. Die wiederholte Messung dieser verschiedenen Konfigurationen bei gleichzeitig konstanter Inhomogenität ermöglicht eine Rekonstruktion der Inhomogenität unter Ausnutzung der Joint Sparsity. T2 - Thermographie Kolloquium 2019 CY - Halle, Germany DA - 19.09.2019 KW - Thermografie KW - Laser-Thermografie KW - ZfP KW - Compressed Sensing KW - Super Resolution PY - 2019 AN - OPUS4-49938 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Burgholzer, P. T1 - Blind structured illumination as excitation for super-resolution photothermal radiometry N2 - The main drawback in radiometric imaging is the degradation of the spatial resolution with increasing depth, which results in blurred images for deeper lying structures. We circumvent this degradation with blind structured illumination, combined with a non-linear joint sparsity reconstruction algorithm. We demonstrate this by imaging a line pattern and a star-shaped structure through a metal sheet with a resolution four times better than the width of the thermal point-spread-function. The ground-breaking concept of super-resolution can be transferred from optics to diffusive imaging by defining a thermal point-spread-function similar to the Abbe limit for a certain optical wavelength. T2 - 14th Quantitative InfraRed Thermography Conference, QIRT 2018 CY - Berlin, Germany DA - 25.06.2018 KW - Thermography KW - Laser Thermography KW - Compressed Sensing KW - Super Resolution PY - 2018 AN - OPUS4-49940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Puthiyaveettil, N. A1 - Thomas K, R. A1 - Unnikrishnakurup, S. A1 - Myrach, Philipp A1 - Ziegler, Mathias A1 - Balasubramaniam, K. T1 - Laser line scanning thermography for surface breaking crack detection modeling and experimental study N2 - Crack detection in metallic samples at high surface temperature, hostile and hazardous environments, etc. is challenging situation in any manufacturing industries. Most of the present NDE methods are suitable only for lower surface temperatures, especially room temperature. In this situation, we need a fast and non-contact NDT method which can be applied even in high sample surface temperature. Laser thermography is one of the techniques having a high potential in non-contact inspection. As a preliminary investigation, in this article, we have studied the potentiality of laser line thermography in crack detection at room temperature. In laser line thermography, a continuous wave (CW) laser is used to generate a laser line, which in turn is used to scan the metal surface. The heat distribution over the sample surface is recorded by an infrared thermal (IR) camera. Two different approaches are reported in this work. Firstly, a stationary laser line source and its interaction with cracks; secondly, moving laser line source scanning over a surface with crack. When the distance between crack centre to laser line centre increases, crack detectability will decrease; and when laser power increases, crack detectability will increase. A dedicated image processing algorithm was developed to improve the detectability of the cracks. To understand the heat transfer phenomenon, a simplified 3D model for laser thermography was developed for the heat distribution during laser heating and was validated with experimental results. Defects were incorporated as a thermally thin resistive layer (TTRL) in numerical modeling, and the effect of TTRL in heat conduction is compared with experimental results. KW - Thermography KW - Laser Thermography KW - Cracks KW - FEM KW - NDT PY - 2019 DO - https://doi.org/10.1016/j.infrared.2019.103141 VL - 104 SP - 103141 PB - Elsevier B.V. AN - OPUS4-49941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Separation and surface groups quantification of polystyrene nanoparticles using capillary electrophoresis (CE) and asymmetrcal flow-field-flow fractionation (AF4) N2 - Nowadays, different nanoparticles have been developed for commercial applications. However, since data on toxicity are barely available, their increasing application in cosmetic products, food and their release in the environment might cause severe problems. Since a range of physical, chemical, and biological characteristics of NPs are closely related to particle size and surface functionalization, precise separation and surface groups quantification is essential to acquire an in-depth understanding of their properties. In this work, the performance of asymmetrical flow field flow fractionation (AF4) and capillary electrophoresis (CE) for the separation of nanoparticles (NPs) with different sizes, coatings, and coating densities was investigated and optimized. For the first time, a two-dimensional off-line hyphenation of both techniques (AF4-CE) was developed. The results clearly demonstrated, that AF4-CE hyphenation can significantly improve the separation resolution and reduce the peak broadening in CE. Also, for the first time, CE was employed to determine the coating density of NPs and the results were in good agreement with the values acquired with conductometric titration. T2 - 2nd CE Forum CY - Karlsruhe, Germany DA - 11.12.2019 KW - Capillary electrophoresis KW - Nanoparticle PY - 2019 AN - OPUS4-49985 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Borghetti, P. A1 - Ortel, Erik A1 - Wirth, Thomas A1 - Garcia, S. A1 - Gómez, E. A1 - Blanco, M. A1 - Alberto, G. A1 - Martra, G. T1 - Organic surface modification and analysis of titania nanoparticles for self‐assembly in multiple layers N2 - The characteristics of TiO2 coatings can greatly influence their final performance in large‐scale applications. In the present study, self‐assembly of TiO2 nanoparticles (NPs) in multiple layers was selected as a deposition procedure on various substrates. For this, the main prerequisite constitutes the surface modification of both NPs and substrate with, for example, silane coupling agents. A set of functionalized TiO2 NPs has been produced by reaction with either (3‐aminopropyl)triethoxysilane (APTES) or (3‐aminopropyl)phosphonic acid (APPA) to functionalize the NP surface with free amino‐groups. Then, the complementary functionalized NP set can be obtained from an aliquot of the first one, through the conversion of free surface amino groups to aldehydes by reaction with glutaraldehyde (GA). Several types of TiO2 NPs differing in size, shape, and specific surface area have been functionalized. Fourier‐transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), SEM/ energy‐dispersive X‐ray spectroscopy (EDS), XPS, Auger electron spectroscopy (AES), and Time‐of‐Flight (ToF)‐SIMS analyses have been carried out to evaluate the degree of functionalization, all the analytical methods employed demonstrating successful functionalization of TiO2 NP surface with APTES or APPA and GA. KW - TiO2 KW - Nanoparticles KW - Surface functionalization KW - Layer-by-layer deposition KW - Surface chemical analysis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508601 DO - https://doi.org/10.1002/sia.6842 SN - 1096-9918 VL - 52 IS - 12 SP - 829 EP - 834 PB - John Wiley & Sons Ltd AN - OPUS4-50860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Borovinskaya, O. A1 - Flamigni, L. A1 - Kuhlmeier, K. A1 - Büchel, C. A1 - Meermann, Björn T1 - Single cell-inductively coupled plasma-time of flight-mass spectrometry approach for ecotoxicological testing N2 - Diatoms play a key role in assessing the eco-toxicology of metals and are already part of several national and international guidelines and regulations. Data on metal uptake and its correlation with a natural metal composition of the diatoms are mostly lacking on a cellular basis - mainly due to the lack of a suitable method on both the preparation and detection side. Therefore, within this work a fully automated approach based on the on-line coupling of a high performance liquid chromatograph (HPLC) and an inductively coupled plasma-time of flight-mass spectrometer (ICP-ToF-MS) was applied to analyze single cells of the alga Cyclotella meneghiniana multi-elementally in order to provide a deeper insight into the metal composition and its response to environmental stress. Multi-elemental analysis in single diatoms also enables assessment of combined toxicity of a set of metals. A set of four fingerprint elements, characteristically for diatoms (Mg, P, Si, Fe), were identified and hence the investigation of environmental stress onto the cells was enabled by performing incubation experiments with environmentally relevant toxic elements. It could be shown at moderate environmental stress caused by increasing the metal concentration in the medium (zinc) that the fingerprint element concentrations remained stable and thus the suitability of the selected elements for algae tracing was demonstrated. With regard to further ecotoxicological assessments, a multivariate approach was successfully applied allowing for cell classification upon different incubation concentration levels. This multivariate approach also facilitated an effective identification of three different diatom species (Cyclotella meneghiniana, Thalassiosira weissflogii and Thalassiosira pseudonana). KW - ICP-TOF-MS KW - Ecotoxicological Testing KW - Diatoms PY - 2020 DO - https://doi.org/10.1016/j.algal.2020.101964 VL - 49 SP - 101964 PB - Elsevier B.V. AN - OPUS4-50875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej A1 - Lapalus, Antoin A1 - Tiebe, Carlo A1 - Bartholmai, Matthias T1 - Design and Implementation of Smart Multisensor Monitoring System for Safe Workplaces with LoRaWAN N2 - This project addresses the application of safe workplaces in offices and chemical laboratories where indoor air quality plays an important role. The LoRaWAN (Long Range Wide Area Network) is used as a communication interface to make important sensor data globally accessible. The goal of the development is to create a sensor node and an online and offline solution that collects the data from the sensor nodes and stores it on a local server or in a cloud. In cooperation with the companies WISTA GmbH and IONOS, a test sensor network is going to be established in the Berlin-Adlershof area. T2 - SMSI 2020 CY - Meeting was canceled DA - 22.06.2020 KW - Smart sensors KW - Air quality monitoring KW - LoRaWAN KW - VOC KW - Multisensor system PY - 2020 DO - https://doi.org/10.5162/SMSI2020/E5.4 SP - 388 EP - 389 AN - OPUS4-50878 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Pauw, Brian Richard A1 - Qu, Xintong A1 - Schönhals, Andreas T1 - Competition of nanoparticle-induced mobilization and immobilization effects on segmental dynamics of an epoxy-based nanocomposite N2 - The complex effects of nanoparticles on a thermosetting material based on an anhydride cured DGEBA/Boehmite nanocomposite with different particle concentrations is considered. A combination of X-ray scattering, calorimetry, including fast scanning calorimetry as well as temperature modulated calorimetry and dielectric spectroscopy, was employed to study the structure, the vitrification kinetics and the molecular dynamics of the nanocomposites. For the first time in the literature for an epoxy-based composite a detailed analysis of the X-ray data was carried out. Moreover, the unfilled polymer was found to be intrinsically heterogeneous, showing regions with different crosslinking density, indicated by two separate dynamic glass transitions. The glass transition temperature decreases with increasing nanoparticle concentration, resulting from a change in the crosslinking density. Moreover, on the one hand, for nanocomposites the incorporation of nanofiller increased the number of mobile segments for low nanoparticle concentrations, due to the altered crosslinking density. On the other hand, for higher loading degrees the number of mobile segments decreased, resulting from the formation of an immobilized interphase (RAF). The simultaneous mobilization and immobilization of the segmental dynamics cannot be separated unambiguously. Taking the sample with highest number of mobile segments as reference state it was possible to estimate the amount of RAF. KW - Nanocomposite PY - 2020 DO - https://doi.org/10.1039/d0sm00744g SN - 1744-683X VL - 16 IS - 23 SP - 5406 EP - 5421 PB - Royal Chemical Society AN - OPUS4-50883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - EURAMET.QM-S14 Measurement capabilities for the quantification of ethanol in water - Summary of results N2 - The presentation summarizes the results of the EURAMET key comparison QM-S14 “Measurement capabilities for the quantification of ethanol in water”. Possible options for the key comparison reference value are discussed. T2 - CCQM Organic Analysis Working Group videoconference CY - Online meeting DA - 05.06.2020 KW - Certified Reference Material KW - EURAMET KW - Key comparison PY - 2020 AN - OPUS4-50890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - DNA basierte Dosimetrie N2 - We propose the development of a standardized DNA based dosimeter. This dosimeter will improve the comparability between the results of different laboratories in radiation research. Compared to conventional methods in dosimetry, this Approach provides direct access to the relation between radiation interaction and biological damage. Moreover, it enables the systematic investigation of the relation between the microscopic characteristics of radiation and DNA damage over a wide dose range. T2 - Zertkom CY - Online meeting DA - 13.05.2020 KW - DNA KW - Dosimetrie KW - Dosimetry KW - Effective dose KW - Energy dose KW - Energiedosis KW - Equivalent dose KW - Absorbed dose PY - 2020 AN - OPUS4-50779 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marques, T. S. A1 - Schürmann, Robin A1 - Ebel, Kenny A1 - Heck, C. A1 - Smialek, M. A1 - Eden, Sam A1 - Mason, N. A1 - Bald, Ilko T1 - Kinetics of molecular decomposition under irradiation of gold nanoparticles with nanosecond laser pulses-A 5-Bromouracil case study N2 - Laser illuminated gold nanoparticles (AuNPs) efficiently absorb light and heat up the surrounding medium, leading to versatile applications ranging from plasmonic catalysis to cancer photothermal therapy. Therefore, an in-depth understanding of the thermal, optical, and electron induced reaction pathways is required. Here, the electrophilic DNA nucleobase analog 5-Bromouracil (BrU) has been used as a model compound to study its decomposition in the vicinity of AuNPs illuminated with intense ns laser pulses under various conditions. The plasmonic response of the AuNPs and the concentration of BrU and resulting photoproducts have been tracked by ultraviolet and visible (UV–Vis) spectroscopy as a function of the irradiation time. A kinetic model has been developed to determine the reaction rates of two parallel fragmentation pathways of BrU, and their dependency on laser fluence and adsorption on the AuNP have been evaluated. In addition, the size and the electric field enhancement of the decomposed AuNPs have been determined by atomic force microscopy and finite domain time difference calculations, respectively. A minor influence of the direct photoreaction and a strong effect of the heating of the AuNPs have been revealed. However, due to the size reduction of the irradiated AuNPs, a trade-off between laser fluence and plasmonic response of the AuNPs has been observed. Hence, the decomposition of the AuNPs might be limiting the achievable temperatures under irradiation with several laser pulses. These findings need to be considered for an efficient design of catalytic plasmonic systems. KW - Kinetics KW - Gold nanoparticles KW - 5-Bromouracil PY - 2020 DO - https://doi.org/10.1063/1.5137898 VL - 152 IS - 12 SP - 24712 EP - 24712 PB - AIP Publishing AN - OPUS4-50787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - The Ring-Opening Polymerisation-Polycondensation (ROPPOC) Approach to cyclic Polymers N2 - A new concept called “Ring-Opening Polymerization (ROP) combined with simultaneous POlyCondensation” (ROPPOC) is presented and discussed. This synthetic strategy is based on the intermediate formation of chains having two end groups that can react with each other. The ROPPOC syntheses are subdivided into three groups according to the nature of the chain ends: two ionic end groups, one ionic and one covalent chain end and a combination of two reactive covalent end groups may be involved, depending on the catalyst. The usefulness for the preparation of cyclic polymers is discussed with a review of numerous previously published examples. These examples concern to following classes of cyclic polymers: polypeptides, polyamides, polyesters, including polycarbonates, and cyclic polysiloxanes. It is demonstrated, that the results of certain ROPPOC syntheses are in contradiction to the Jacobson-Stockmayer theory. Finally, the usefulness of ROPPOCs for the detection of polydisperse catenanes is discussed. KW - Ring-opening Polymerisation KW - MALDI-TOF MS KW - ROPPOC KW - Cyclic PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508509 DO - https://doi.org/10.1002/marc.202000152 SP - 2000152 PB - Wiley AN - OPUS4-50850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Differences in MALDI Ionization of neat linear and cyclic poly(L-lactide)s N2 - In addition to molar mass distribution (MMD) synthetic polymers often exhibit an additional chemical heterogeneity distribution, expressed by different end groups and other structural variations (e.g. tacticity, copolymer composition etc.). Ionization in MALDI MS is always strongly affected by such chemical properties. For example, the abundance of cyclics in MALDI TOF mass spectra is frequently reported to greatly exceed that of linears. Thus, the MALDI ionization behavior of various neat end-capped linear poly(L-lactide)s and one cyclic poly(L-lactide) was investigated and compared with that of blends of both structures. Moreover, the influence of the cationizing salt was investigated too. Neat compounds and various blends of cyclic and linear species were prepared and studied using two MALDI TOF mass spectrometers under identical conditions with regard to sample preparation and instrumental conditions, except for the laser power and the salt used for cationization. Polymer samples were additionally characterized by NMR and SEC. The steady increase of the laser intensity caused an exponential increase of the peak intensities of both linear and cyclic polylactides.The response of linear polylactides (in the investigated molecular mass range), whether as neat polymer or in blends with other linear polylactides was almost similar. This clearly supports our assumption that ionization in MALDI is probably unaffected by the end group structure.The variation of the laser power shows only little effect on the intensity ratio of linear-to linear and cyclic-to-linear polylactides in blends. Whereas neat linear polylactides at all laser intensities have a significantly higher abundance than neat cyclics, in mixtures of both an overestimation of cyclic species in MALDI TOF mass spectra of polylactides was found. However, this is far less distinct than frequently reported for other polymers.Concluding, peak suppression of linear polymers in mixtures of both architectures can be excluded, which also means, that polylactides showing only peaks of cyclic compounds in their MALDI - TOF mass spectra do not contain a significant fraction of linear analogues. Our study is the first systematic comparison of the MALDI ionization of neat and blended cyclic and linear polylactides. T2 - ASMS 2020 Reboot CY - Online meeting DA - 01.06.2020 KW - MALDI KW - Ionization KW - Linear KW - Cyclic KW - Polylactide PY - 2020 AN - OPUS4-50852 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reifschneider, O. A1 - Vennemann, A. A1 - Buzanich, Günter A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Hogeback, J A1 - Köppen, C. A1 - Großgarten, M. A1 - Sperling, M. A1 - Wiemann, M. A1 - Karst, U. T1 - Revealing Silver Nanoparticle Uptake by Macrophages Using SR-μXRF and LA-ICP-MS N2 - To better study the impact of nanoparticles on both in vitro and in vivo models, tissue distribution and cellular doses need to be described more closely. Here silver nanoparticles were visualized in alveolar macrophages by means of synchrotron radiation micro X-ray fluorescence spectroscopy (SR-μXRF) with high spatial resolution of 3 × 3 μm2. For the spatial allocation of silver signals to cells and tissue structures, additional elemental labeling was carried out by staining with eosin, which binds to protein and can be detected as bromine signal with SR-μXRF. The method was compatible with immunostaining of macrophage antigens. We found that the silver distribution obtained with SR-μXRF was largely congruent with distribution maps from a subsequent laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) of the same tissue sites. The study shows a predominant, though not exclusive uptake of silver into alveolar macrophages in the rat lung, which can be modeled by a similar uptake in cultured alveolar macrophages. Advantages and limitations of the different strategies for measuring nanoparticle uptake at the single cell level are discussed. KW - Synchrotron KW - BAMline KW - XRF KW - Nanoparticle KW - Macrophagen PY - 2020 DO - https://doi.org/10.1021/acs.chemrestox.9b00507 VL - 33 IS - 5 SP - 1250 EP - 1255 PB - American Chemical Society AN - OPUS4-50855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim A1 - Hirsch, Philipp Daniel A1 - Lecompagnon, Julien A1 - Hassenstein, Christian A1 - Jung, P. A1 - Caire, G. A1 - Ziegler, Mathias T1 - New techniques in super resolution photothermal imaging for nondestructive testing N2 - In this work we focus on our most recent studies to super resolution (SR) laser thermography. The goal of SR nondestructive testing methods is to facilitate the separation of closely spaced defects. We explain how to combine laser scanning with SR techniques. It can be shown that stepwise as well as continuous scanning techniques are applicable. Finally, we discuss the effect of experimental parameters and im-age processing techniques to find the optimal SR technique which leads to the highest reconstruction quality within laser thermography. T2 - SMSI 2020 Conference CY - Online meeting DA - 22.06.2020 KW - Super resolution KW - Laser thermography KW - Nondestructive testing KW - Laser scanning KW - Photothermal imaging PY - 2020 DO - https://doi.org/10.5162/SMSI2020/C4.1 SP - 169 EP - 170 AN - OPUS4-50895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias A1 - Ahmadi, Samim A1 - Hirsch, Philipp Daniel A1 - Lecompagnon, Julien A1 - Hassenstein, Christian A1 - Thiel, Erik A1 - Pech May, Nelson Wilbur T1 - Using spatial and temporal shaping of laser-induced diffuse thermal wave fields in thermography N2 - The diffuse nature of thermal waves is a fun-damental limitation in thermographic nonde-structive testing. In our studies we investigated different approaches by shaping the thermal wave fields which result from heating. We have used high-power laser sources to heat metallic samples. Using these spatial and temporal shaping techniques leads to a higher detection sensitivity in our measurements with the infra-red camera. In this contribution we show our implementation of shaping laser-induced diffuse thermal wave fields and the effect on the defect reconstruction quality. T2 - SMSI 2020 Conference CY - Online meeting DA - 22.06.2020 KW - Thermal wave KW - Diffusion KW - High-power laser KW - Thermography KW - Spatiotemporal shaping PY - 2020 DO - https://doi.org/10.5162/SMSI2020/C5.1 SP - 179 EP - 180 AN - OPUS4-50897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kanwal, S. A1 - Ali, Naveed Zafar A1 - Hussain, R. A1 - Shah, F.U. A1 - Akhter, Z. T1 - Poly-thiourea formaldehyde based anticorrosion marine coatings on Type 304 stainless steel N2 - In the present study, hexamethylene diisocyanate (HMDI) encapsulated poly-thiourea formaldehyde (PTF) (10 wt%) coating was developed in an epoxy-polyamine matrix and their anticorrosion studies on Type SS304 stainless steel substrate have been conducted using electrochemistry techniques. The compact and hydrophobic shell wall of PTF proved to be a potent shell wall material for HMDI encapsulation. The effect of temperature and pH values was found to be decisive factor in the synthesis of microcapsules. The PTF microcapsules were synthesized in acidic condition with a pH value of 3. Over 90% of the core fraction is retained in water after 21 days immersion. However, core content decreased with increasing temperature. The capsules were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Electrochemical Impedance spectroscopy (EIS). Scanning electron microscopic analysis depicts the uniform morphology of coating with a particle size in the range of 1.08 µm–22.06 µm. The vibrational band at 2271 cm−1 attributed to NCO signal further endorses the successful encapsulation of HMDI into the PTF capsules. Electrochemical testing on steel specifies the appreciable anticorrosion performance of the synthesized poly thiourea formaldehyde (PTF) coating against artificial sea water. KW - In-situ polymerization KW - Encapsulation KW - Thiourea-formaldehyde KW - Marine corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507932 DO - https://doi.org/10.1016/j.jmrt.2019.12.045 VL - 9 IS - 2 SP - 2146 EP - 2153 PB - Elsevier B.V. AN - OPUS4-50793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona T1 - Presentation at AVIC-Workshop: BAM initiative QI-FoKuS N2 - QI-FoKuS stands for „Quality Infrastructure – Research for Conformity Assessment and Safety“. Supported by the BMWi, a new recurring survey of companies was launched under this name in end-September 2019 in a joint project between the TU Berlin and the Federal Institute for Materials Research and Testing (BAM). The first company survey deals with the use and certification of management systems with a special focus on information security and the criteria for the selection of certification bodies. T2 - Visit & Workshop of NQI Lab SAMR/AVIC and BAM CY - Berlin, Germany DA - 29.10.2019 KW - Conformity Assessment KW - Information Security KW - Accreditation KW - Certification KW - QI-FoKuS PY - 2019 AN - OPUS4-49477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona T1 - Presentation at AVIC-Workshop: Exploring the diffusion of the information security management system standard ISO/IEC 27001 N2 - We explore the adoption and diffusion of the international information security management system standard ISO/IEC 27001 with Web Mining of German firm websites using the Mannheim Enterprise Panel dataset (MUP). T2 - Visit & Workshop of NQI Lab SAMR/AVIC and TU-Berlin CY - Berlin, Germany DA - 31.10.2019 KW - ISO/IEC 27001 KW - Web Mining KW - Information security PY - 2019 AN - OPUS4-49478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Dariz, P. ED - Ziemann, M. T1 - Raman band widths of anhydrite II reveal the burning history of high-fired medieval gypsum mortars N2 - The use of high-fired gypsum as binder for masonry and joint mortars or stuccowork in Central Europe in the Early and High Middle Ages was a regional specific as it depended on local gypsum deposits. The calcination technology possible at the time resulted in an assemblage of calcium sulphate phases dehydrated to different degrees and partly thermally damaged accessory minerals of the raw gypsum. Because of the absence of medieval textbooks, the observation of high-temperature, low-pressure mineral transformations and the correlation of phases coexisting in not hydrated binder relicts in the gypsum matrix to the mineralogy of the raw material and the burning conditions constitute the only source to the historical technological know-how. The CaSO4–H2O system consists of five crystalline phases, which can be discriminated by structural analysis methods, such as Raman spectroscopy, due to obvious differences in their spectroscopic data: gypsum (CaSO4 ⋅ 2 H2O), bassanite (hemihydrate, CaSO4 ⋅ ½ H2O), anhydrite III (CaSO4), anhydrite II (CaSO4), and anhydrite I (CaSO4). Only recently, it was possible to demonstrate that small spectroscopic variations exist also within the relatively large stability range of anhydrite II from approx. 180°C to 1180°C: all Raman bands narrow with increasing burning temperature applied in the synthesis from gypsum powder. The determination of band widths of down to 3 cm-1 and differences between them of a few tenths of a wavenumber is not a trivial task. Thus, this contribution discusses peak fitting and strategies for correction of instrument-dependent band broadening. Raman maps of polished thin sections of gypsum mortars provide access to the burning histories of individual remnant thermal anhydrite grains and enable the discrimination of natural anhydrite originating from the gypsum deposit. This novel analytical method was applied to samples from medieval South Tyrolean stucco decorations and sculptures. Beyond that, Raman microspectroscopy was employed for following pyrometamorphic reactions in natural impurities of the raw material. In the presented examples mineral thermometry indicates process temperatures above 800°C: the breakdown of magnesium-rich chlorite led to the formation of forsterite Mg2SiO4, while the thermal decomposition of dolomite CaMg(CO3)2 yielded – after hydration and carbonation – magnesite MgCO3, CaCO3 polymorphs and magnesian calcite. Lower burning temperatures, which leave the accessory minerals in their pristine form, can be traced by measuring the spectra of anhydrite crystalites in grains of firing products and evaluating Raman band widths. Throughout the applications of this analytical method so far, calcination temperatures ranging from approx. 600°C to 900°C were determined. T2 - 10th International Congress on the Application of Raman Spectroscopy in Art and Archaeology CY - Potsdam, Germany DA - 03.09.2019 KW - Raman microspectroscopy KW - High-fired medieval gypsum mortars KW - Raman band width KW - Gypsum dehydration KW - Thermal anhydrite PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496204 SP - 36 EP - 37 PB - University of Potsdam CY - Potsdam AN - OPUS4-49620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Growth Kinetics and molecular mobility of irreversibly adsorbed layers in thin Polymer films investigated by Nanosized relaxation spectroscopy and complimentary methods N2 - In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is expected to from. These adsorbed layers have shown greate potential for technological applications. However, their growth kinetics and molecular dynamics are still not fully understood. This is partly due to the hard accessibility of these layers in thin films. Here, the irreversibly adsorbed layers of homopolymer thin films are revealed by solvent-leaching experiments. First, the growth kinetics of these layers is investigated as a function of annealing time, annealing temperature, leaching time and the original filme thickness. The film thickness, topography and the quality of the adsorbed layer is controlled by Atomic Force Microscopy (AFM). Secondly, the molecular mobility of the adsorbed layer is investigated by Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor arrangement is employed to measure the layer with a free surface. The results are quantitatively compared and discussed with respect to recently published work. T2 - Polymers on the nanoscale CY - Princeton, New Jersey, USA DA - 31.10.2019 KW - Thin polymer films PY - 2019 AN - OPUS4-49559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chapartegui-Arias, Ander A1 - Villajos Collado, José Antonio A1 - Myxa, Anett A1 - Beyer, Sebastian A1 - Falkenhagen, Jana A1 - Schneider, Rudolf A1 - Emmerling, Franziska T1 - Covalently Fluorophore-Functionalized ZIF‑8 Colloidal Particles as a Sensing Platform for Endocrine-Disrupting Chemicals Such as Phthalates Plasticizers N2 - We present the optical sensing of phthalate Esters (PAEs), a group of endocrine-disrupting chemicals. The sensing takes place as changes in the fluorescence emission intensity of aminopyrene covalently bound to the organic ligands of the metal−organic framework compound ZIF-8. In the presence of PAEs, a quenching of the fluorescence emission is observed. We evaluated strategies to engineer colloidal size distribution of the sensing particles to optimize the sensory response to PAEs. A thorough characterization of the modified ZIF-8 nanoparticles included powder X-ray diffractometry, transmission electron microscopy, high-performance liquid chromatography, and photophysical characterization. The presented capability of the fluorophore-functionalized ZIF-8 to sense PAEs complements established methods such as chromatography-based procedures, which cannot be used on-site and paves the way for future developments such as hand-held quick sensing devices. KW - Sensing KW - MOF PY - 2019 DO - https://doi.org/10.1021/acsomega.9b01051 VL - 4 IS - 17 SP - 17090 EP - 17097 PB - ACS AN - OPUS4-49562 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino A1 - Neumann, Patrick P. A1 - Scheuschner, Nils A1 - Bartholmai, Matthias A1 - Lilienthal, A.J. T1 - Experimental Validation of the Cone-Shaped Remote Gas Sensor Model N2 - Remote gas sensors mounted on mobile robots enable the mapping of gas distributions in large or hardly accessible areas. A challenging task, however, is the generation of threedimensional distribution maps from these gas measurements. Suitable reconstruction algorithms can be adapted, for instance, from the field of computed tomography (CT), but both their performance and strategies for selecting optimal measuring poses must be evaluated. For this purpose simulations are used, since, in contrast to field tests, they allow repeatable conditions. Although several simulation tools exist, they lack realistic models of remote gas sensors. Recently, we introduced a model for a Tunable Diode Laser Absorption Spectroscopy (TDLAS) gas sensor taking into account the conical shape of its laser beam. However, the novel model has not yet been validated with experiments. In this paper, we compare our model with a real sensor device and show that the assumptions made hold. T2 - IEEE Sensors 2019 CY - Montreal, Canada DA - 27.10.2019 KW - Remote gas sensor model KW - TDLAS KW - Gas dispersion simulation PY - 2019 SN - 978-1-7281-1634-1 SP - 104 EP - 107 PB - IEEE AN - OPUS4-49548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias T1 - Experimental Validation of the Cone-Shaped Remote Gas Sensor Model N2 - Remote gas sensors mounted on mobile robots enable the mapping of gas distributions in large or hardly accessible areas. A challenging task, however, is the generation of threedimensional distribution maps from these gas measurements. Suitable reconstruction algorithms can be adapted, for instance, from the field of computed tomography (CT), but both their performance and strategies for selecting optimal measuring poses must be evaluated. For this purpose simulations are used, since, in contrast to field tests, they allow repeatable conditions. Although several simulation tools exist, they lack realistic models of remote gas sensors. Recently, we introduced a model for a Tunable Diode Laser Absorption Spectroscopy (TDLAS) gas sensor taking into account the conical shape of its laser beam. However, the novel model has not yet been validated with experiments. In this paper, we compare our model with a real sensor device and show that the assumptions made hold. T2 - IEEE Sensors 2019 CY - Montreal, Canada DA - 27.10.2019 KW - Remote gas sensor model KW - TDLAS KW - Gas dispersion simulation PY - 2019 AN - OPUS4-49549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Linear and matrix phased array inspection of complex thin wall components N2 - The application of phased arrays in either linear or matrix arrangement in combination with signal processing opens the door for the mechanized inspection of different thin wall materials itself as well as their joining methods. Modern lightweight components are typically manufactured by a composition of different types of e.g. steels, metals, fiber reinforced plastics and glass. Dependent on the material combinations e.g. welding, brazing, bonding, cladding or coating may be applied during the manufacturing process to join different semi-finished products to form the component. The resulting complex material composition and different damage mechanisms pose new challenges to non-destructive testing with ultrasound due to the different material properties and the overall arrangement of the materials employed. The sound field variation capabilities of array probes may be helpful to overcome some of these challenges if adapted to the specific inspection task. Examples for the non-destructive mechanized phased array inspection of different types of materials and joining methods will be presented. T2 - KINT Symposium CY - Amsterdam, The Netherlands DA - 30.10.2019 KW - Matrix array KW - Phased array KW - Joints PY - 2019 AN - OPUS4-49538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prager, Jens A1 - Vogt, T. T1 - Zum Einsatz geführter Wellen für die Ultraschallprüfung – Ergebnisse der Onlineumfrage N2 - Der Unterausschuss „Geführte Wellen“ im Fachausschuss „Zustandsüberwachung“ der Deutschen Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) hat in einer Online-Umfrage den aktuellen Stand des Einsatzes geführter Ultraschallwellen für die zerstörungsfreie Prüfung und die Strukturüberwachung (structural health monitoring) ermittelt. Es wurden deutsche und internationale Firmen und Forschungseinrichtungen befragt und mehr als 400 beantwortete Fragebögen ausgewertet. Die Umfrageergebnisse zeigen deutlich, welche Vorteile geführte Wellen bringen, aber auch welche Probleme zu bewältigen sind, um einen breiteren Einsatz der Verfahren zu ermöglichen. Aus den Ergebnissen werden Schlussfolgerungen für die weitere Ausrichtung der Forschungs- und Entwicklungsarbeiten aber auch von Aktivitäten zur Normung und zur Bewertung der Zuverlässigkeit der Prüfverfahren abgeleitet KW - Structural Health Monitoring KW - Geführte Wellen KW - Zustandsüberwachung PY - 2019 UR - https://www.dgzfp.de/Portals/24/Zeitung/Ausgaben/Zeitung166.pdf SN - 1616-069X VL - 166 IS - Oktober SP - 8 EP - 9 PB - DGZfP e.V. CY - Berlin AN - OPUS4-49508 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Cu project on calibration approaches for absolute isotope ratios N2 - This presentations summarizes the difficulties in the purification of enriched copper isotopes by high vacuum subimation. It shows as well thelimitations for a CCQM key comparison on this topic. T2 - CCQM Isotope Ratio Work Group Meeting CY - Bern, Switzerland DA - 09.10.2019 KW - Absolute isotope ratio KW - Isotope purification KW - Metal sublimation KW - Gravimtric isotope mixtures PY - 2019 AN - OPUS4-49518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. A1 - Lilienthal, A. J. A1 - Neumann, Patrick P. ED - Zemčík, R. ED - Krystek, J. T1 - Boosting a Low-Cost Sensor Network with Mobile High-Quality Sensors N2 - Occupational health is an important topic, especially in industry, where workers are exposed to airborne by-products (e.g., dust particles and gases). Therefore, continuous monitoring of the air quality in industrial environments is crucial to meet safety standards. For practical and economic reasons, high-quality, costly measurements are currently only carried out sparsely, both in time and space, i.e., measurement data are collected in single day campaigns at selected locations only. Recent developments in sensor technology enable cost-efficient gas monitoring in real-time for long-term intervals. This knowledge of contaminant distribution inside the industrial environment would provide means for better and more economic control of air impurities, e.g., the possibility to regulate the workspace’s ventilation exhaust locations, can reduce the concentration of airborne contaminants by 50%. This paper describes a concept proposed in the project “Robot-assisted Environmental Monitoring for Air Quality Assessment in Industrial Scenarios“ (RASEM). RASEM aims to bring together the benefits of both – low- and high-cost – measuring technologies: A stationary network of low-cost sensors shall be augmented by mobile units carrying high-quality sensors. Additionally, RASEM will develop procedures and algorithms to map the distribution of gases and particles in industrial environments. T2 - 36th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Pilsen, Czech Republic DA - 24.09.2019 KW - RASEM KW - Sensor network KW - Low-cost KW - Occupational health KW - Mobile Robot Olfaction PY - 2019 SP - 61 EP - 62 CY - Plzeň AN - OPUS4-49630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. T1 - Boosting a Low-Cost Sensor Network with Mobile High-Quality Sensors N2 - The Motivation of RASEM (Robot-assisted Environmental Monitoring): Monitoring of the air quality in industrial environments is inevitable to meet safety Standards. Because of economic and practical reasons, measurements are carried out sparsely in terms of time and space. Newest developments on the field of low cost sensor technology enable cost efficient long term monitoring of gases and dust T2 - 36th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Pilsen, Czech Republic DA - 24.09.2019 KW - RASEM KW - Sensor network KW - Low-cost KW - Occupational health KW - Mobile Robot Olfaction PY - 2019 AN - OPUS4-49632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - Full field X-ray fluorescence imaging with coded apertures N2 - Our aim is to develop a simple and inexpensive method for full field X-ray fluorescence imaging.We combine an energy-dispersive array detector with a coded aperture to obtain high resolution images. To obtain the information from the recorded image a reconstruction step is necessary. The reconstruction methods we have developed, were tested on simulated data and then applied to experimental data. The first tests were carried out at the BAMline @ BESSY II. This method enables the simultaneous detection of multiple elements, which is important e.g. in the field of catalysis. T2 - CONEXS 2020 CY - Newcastle, UK DA - 18.02.2020 KW - X-ray fluorescence spectroscopy KW - Coded apertures KW - Imaging KW - Iterative reconstruction PY - 2020 AN - OPUS4-50461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kepsutlu, B. A1 - Wycisk, V. A1 - Achazi, K. A1 - Kapishnikov, S. A1 - Perez-Berna, A.J. A1 - Guttmann, P. A1 - Cossmer, Antje A1 - Pereiro, E. A1 - Ewers, H. A1 - Ballauff, M. A1 - Schneider, G. A1 - McNally, J.G. T1 - Cells Undergo Major Changes in the Quantity of Cytoplasmic Organelles after Uptake of Gold Nanoparticles with Biologically Relevant Surface Coatings N2 - Here, we use cryo soft X-ray tomography (cryo-SXT), which delivers 3D ultrastructural volumes of intact cells without chemical fixation or staining, to gain insight about nanoparticle uptake for nanomedicine. We initially used dendritic polyglycerol sulfate (dPGS) with potential diagnostic and therapeutic applications in inflammation. Although dPGS-coated gold nanoparticle (dPGS-AuNP) uptake followed a conventional endocytic/degradative pathway in human lung epithelial cell lines (A549), with cryo-SXT, we detected ∼5% of dPGS-AuNPs in the cytoplasm, a level undetectable by confocal light microscopy. We also observed ∼5% of dPGS-AuNPs in a rarely identified subcellular site, namely, lipid droplets, which are important for cellular energy metabolism. Finally, we also found substantial changes in the quantity of cytoplasmic organelles upon dPGS-AuNP uptake over the 1–6 h incubation period; the number of small vesicles and mitochondria significantly increased, and the number of multivesicular bodies and the number and volume of lipid droplets significantly decreased. Although nearly all organelle numbers at 6 h were still significantly different from controls, most appeared to be returning to normal levels. To test for generality, we also examined cells after uptake of gold nanoparticles coated with a different agent, polyethylenimine (PEI), used for nucleic acid delivery. PEI nanoparticles did not enter lipid droplets, but they induced similar, albeit less pronounced, changes in the quantity of cytoplasmic organelles. We confirmed these changes in organelle quantities for both nanoparticle coatings by confocal fluorescence microscopy. We suggest this cytoplasmic remodeling could reflect a more common cellular response to coated gold nanoparticle uptake. KW - Cellular trafficking KW - Confocal laser scanning microscopy KW - Cytoplasmic remodeling KW - Dendritic polyglycerol sulfate KW - Polyethylenimine KW - 3D ultrastructural analysis KW - Cryo-soft X-ray tomography PY - 2020 DO - https://doi.org/10.1021/acsnano.9b09264 VL - 14 IS - 2 SP - 2248 EP - 2264 AN - OPUS4-50464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yildirim, Arda A1 - Krause, Christina A1 - Zorn, R. A1 - Lohstroh, W. A1 - Schneider, G. J. A1 - Zamponi, M. A1 - Holerer, O. A1 - Frick, B. A1 - Schönhals, Andreas T1 - Complex molecular dynamics of a symmetric model discotic liquid crystal revealed by broadband dielectric, thermal and neutron spectroscopy N2 - The molecular dynamics of the triphenylene-based discotic liquid crystal HAT6 is investigated by broadband dielectric spectroscopy, advanced dynamical calorimetry and neutron scattering. Differential scanning calorimetry in combination with X-ray scattering reveals that HAT6 has a plastic crystalline phase at low temperatures, a hexagonally ordered liquid crystalline phase at higher temperatures and undergoes a clearing transition at even higher temperatures. The dielectric spectra show several relaxation processes: a localized gamma-relaxation a lower temperature and a so called alpha-2-relaxation at higher temperatures. The relaxation rates of the alpha-2-relaxation have a complex temperature dependence and bear similarities to a dynamic glass transition. The relaxation rates estimated by hyper DSC, Fast Scanning calorimetry and AC Chip calorimetry have a different temperature dependence than the dielectric alpha-2-relaxation and follows the VFT-behavior characteristic for glassy dynamics. Therefore, this process is called alpha-1-relaxation. Its relaxation rates show a similarity with that of polyethylene. For this reason, the alpha-1-relaxation is assigned to the dynamic glass transition of the alkyl chains in the intercolumnar space. Moreover, this process is not observed by dielectric spectroscopy which supports its assignment. The alpha-2-relaxation was assigned to small scale translatorial and/or small angle fluctuations of the cores. The neutron scattering data reveal two relaxation processes. The process observed at shorter relaxation times is assigned to the methyl group rotation. The second relaxation process at longer time scales agree in the temperature dependence of its relaxation rates with that of the dielectric gamma-relaxation. KW - Discotic Liquid Crystals PY - 2020 DO - https://doi.org/10.1039/c9sm02487e VL - 16 IS - 8 SP - 2005 EP - 2016 PB - Royal Chemical Society AN - OPUS4-50466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Streli, C. A1 - Radtke, Martin T1 - On the way to full-field X-ray fluorescence spectroscopy imaging with coded apertures N2 - Imaging with X-rays is a challenging field, due to the optical properties of X-rays. The fabrication of appropriate optics is usually expensive and requires an elaborate manufacturing process. One simpler and less expensive possibility of imaging high energy radiation is coded aperture imaging, a technique well established in astrophysics and also used in nuclear medicine or radiation detection, e.g., for nuclear decommissioning. Our aim is to adapt coded aperture imaging for X-ray fluorescence spectroscopy in the nearfield. In this work we show theoretical considerations and preliminary simulations of Image formation through a coded aperture and three different reconstruction methods to prepare the experiments. We used a new mask based on an inverted modified uniformly redundant array (MURA) that could be used for the construction of a decoding mask for all investigated geometrical arrangements. The most commonly used reconstruction method, convoluting the detected image with a Decoding mask, does not always deliver satisfactory results. This is more noticeable for small distances between the object, mask and detector. Hence, we developed two new reconstruction methods, one based on iterative algebraic optimization and another one based on a genetic algorithm. Both show good performance even in those cases where the convolution method fails. This provides a basis for further investigations of the ideal parameters for near field coded aperture imaging and refinements of the algorithms. We performed first measurements with a coded aperture at the BAMline at BESSY II and could successfully reconstruct a test object from the obtained recorded images. KW - X-ray fluorescence spectroscopy KW - Coded aperture KW - Imaging KW - Iterative reconstruction PY - 2020 DO - https://doi.org/10.1039/c9ja00232d VL - 35 IS - 2 SP - 347 EP - 356 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-50459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eckel, S. A1 - Zscherpel, Uwe A1 - Huthwaite, P. A1 - Paul, N. A1 - Schumm, A. T1 - Radiographic film system classification and noise characterisation by a camera-based digitisation procedure N2 - Extracting statistical characteristics from radiographic films is vital for film system classification and contrast sensitivity evaluation and serves as a basis for film noise simulation. A new method for digitising radiographic films in order to extract these characteristics is presented. The method consists of a camera-based setup and image processing procedure to digitise films. Correct optical density values and granularity can be extracted from the digitised images, which are equal to results obtained by standardised measurement procedures. Specific statistical characteristics of film noise are theoretically derived and subsequently verified by the obtained data, including characteristics such as Gaussianity and spatial spectral characteristics of the optical density fluctuations. It is shown that the presented method correctly measures the granularity of film noise and can therefore replace time-consuming microdensitometer measurements traditionally required for film system classifications. Additionally, the inherent unsharpness of film systems was investigated and compared with literature data. This comparison serves as another validation approach of the presented method. KW - Radiography KW - Image processing KW - Film noise KW - Film system classification KW - Digitisation PY - 2020 DO - https://doi.org/10.1016/j.ndteint.2020.102241 SN - 0963-8695 VL - 111 IS - 4 SP - 102241 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-50517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eckel, S. A1 - Huthwaite, P. A1 - Zscherpel, Uwe A1 - Schumm, A. A1 - Paul, N. T1 - Realistic film noise generation based on experimental noise spectra N2 - Generating 2D noise with local, space-varying spectral characteristics is vital where random noise fields with spatially heterogeneous statistical properties are observed and need to be simulated. A realistic, non-stationary noise generator relying on experimental data is presented. That generator is desired in areas such as photography and radiography. For example, before performing actual X-ray imaging in practice, output images are simulated to assess and improve setups. For that purpose, realistic film noise modelling is crucial because noise downgrades the detectability of visual signals. The presented film noise synthesiser improves the realism and value of radiographic simulations significantly, allowing more realistic assessments of radiographic test setups. The method respects space-varying spectral characteristics and probability distributions, locally simulating noise with realistic granularity and contrast. The benefits of this approach are to respect the correlation between noise and image as well as internal correlation, the fast generation of any number of unique noise samples, the exploitation of real experimental data, and its statistical non-stationarity. The combination of these benefits is not available in existing work. Validation of the new technique was undertaken in the field of industrial radiography. While applied to that field here, the technique is general and can also be utilised in any other field where the generation of 2D noise with local, space-varying statistical properties is necessary. KW - Nondestructive testing KW - Image quality KW - Noise simulation KW - Radiography PY - 2020 DO - https://doi.org/10.1109/TIP.2019.2955284 SN - 1057-7149 VL - 29 SP - 2987 EP - 2998 PB - IEEE Xplore CY - Washington, D.C. AN - OPUS4-50518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Zscherpel, Uwe ED - Kasperl, S. T1 - Proceedings of the International Symposium on Digital Industrial Radiology and Computed Tomography (DIR) 2019 N2 - This international symposium is devoted to promote a broad exchange of information on technologies, applications and quality assurance in the area of digital industrial radiology and computed tomography. The meeting provides a unique opportunity for users, scientists, equipment suppliers and all who are interested to discuss the present and future possibilities for industrial applications of the following topics: - Xray detectors and sources - Image processing algorithms - Quantitative imaging - Defect detection & localisation - Feature extraction - Dimensional control - CT, multi-angle - radiography - Laminography & Tomosynthesis - Modelling - Film replacement - Phase contrast - Multi-energies and photon counting - Other radiation techniques (e.g. - neutrons) - Multi-techniques fusion - Standardisation - Qualification & system reliability - Inspection for Additive Manufacturing - Scattering T2 - International Symposium on Digital Industrial Radiology and Computed Tomography (DIR) 2019 CY - Fürth, Germany DA - 02.07.2019 KW - Digital Industrial Radiology KW - Computed Radiography KW - Image Processing PY - 2019 UR - https://www.ndt.net/search/docs.php3?MainSource=264 VL - 264 SP - Paper 24743-1 EP - Paper 24764-17 PB - NDT.net CY - Bad Breisig AN - OPUS4-50519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Röntgentomographie von metallischen Mikropartikeln: Ein leistungsfähiges Werkzeug für die Additive Fertigung N2 - Metallische Mikropartikel in der Größenfraktion von ca. 10 – 100 Mikrometer bilden das Grundmaterial für den additiven Aufbau komplexer Strukturen durch lokales Aufschmelzen mit einem Laserstrahl. Entscheidend für dieses Verfahren ist die Kenntnis der Größen-, Form- und Defektverteilungen von Partikelfraktionen, da sie direkten Einfluss auf die Fließfähigkeit des Pulvers während des lagenweisen Auftragens, als auch auf die finale innere Porosität des Bauteils haben. Im Pulver vorhandene Poren verlassen in der Regel das Schmelzbad vor dem Erstarren nicht wieder, da deren Konvektionszeiten größer sind als die Zeit, während der das lokale Schmelzbad besteht, so dass einmal durch die Ausgangspartikel eingebrachte Poren in der Regel auch im fertigen Bauteil verbleiben. Eine strenge Qualitätskontrolle des Ausgangspulvers ist also Voraussetzung, um hochwertige Bauteile mit geringer Restporosität zu erhalten. Der Vorteil der Röntgentomographie ist dabei, dass mit nur sehr geringem Präparationsaufwand innenliegende Poren bis zu einem Durchmesser von wenigen Mikrometern detektiert werden können. Dies ist mit konkurrierenden Verfahren (Licht- / Elektronenmikroskopie, Laserbeugung) so nicht möglich. Zusammenfassend werden wir zeigen, dass die zerstörungsfreie Bildgebung mit der Röntgen-Mikrotomographie für die Qualitätskontrolle in der additiven Fertigung ein leistungsfähiges Werkzeug ist. Wir erörtern die Grenzen der Methode durch eine numerische Studie mithilfe des Simulationsprogramms aRTist. Dabei werden verschiedene Partikelgrößen dahingehend untersucht, welche Poren mit mikroradiographischen Verfahren detektierbar sind. Dazu wird ein Modell für eine dreilagige dichteste Kugelpackung entwickelt, so dass auch Überlagerungen von Anzeigen untersucht werden können. Im Ergebnis werden verschiedene Partikel- und Porengrößenkombinationen untersucht und die entsprechenden Detektionsgrenzen bestimmt. T2 - DGZfP Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 26.05.2019 KW - Computertomographie KW - Additive Fertigung KW - Mikropartikel PY - 2019 UR - https://jt2019.dgzfp.de/Programm#Di.1.B.1 AN - OPUS4-50520 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Röntgenrückstreutechnik für die additive Fertigung N2 - Neben der klassischen Durchstrahlung wird die bildgebende Röntgen-rückstreuung bisher nur sehr begrenzt eingesetzt. Vor über 20 Jahren hatte Philips mit „COMSCAN“ eine erste industrielle Anwendung in der Luftfahrt gefunden, die sogar eine Tiefenauflösung besaß. Die Firma AS&E in Boston bietet Röntgenrückstreu-Anlagen für den Sicherheitsbereich an. In diesen wird mit einem hochkollimierten Nadelstrahl aus einem rotierenden Blendenrad ein Objekt einseitig abgetastet. Zur Detektion der gestreuten Strahlung aus dem Objekt werden großflächige Detektoren direkt neben dem rotierenden Nadelstrahlkollimator eingesetzt. Ein solcher Prototyp wird an der BAM für den Einsatz in der zerstörungsfreien Prüfung untersucht und optimiert. Als neues industrielles Einsatzgebiet wird dabei die in situ Überwachung in der additiven Fertigung avisiert. Hier ist die Zugänglichkeit zum entstehenden Werkstück in den 3D-Druckanlagen stark eingeschränkt, was den Einsatz einer zweiseitigen Durchstrahlung oder der Computer-Tomographie, bei der das Objekt rotiert wird, verhindert. Auch sind die in der additiven Fertigung eingesetzten Werkstoffe (Polymere, Keramik, Leichtmetalle wie Al oder Ti) für die Rückstreuung besser geeignet als Metalle höherer Dichte, da das Streusignal mit der Ordnungszahl und der Materialdichte abnimmt. Allerdings sind die Anforderungen an räumliche Auflösung und Kontrastempfindlichkeit in der zerstörungsfreien Prüfung additiv gefertigter Bauteil deutlich höher als im Sicherheitsbereich, da hier Bauteilfehler mit typischen Dimensionen kleiner als 1 mm sicher detektiert werden müssen. Die Untersuchung dieser Grenzen des derzeitigen Standes der Röntgenrückstreutechnik mit Nadelstrahl ist ein Teilbereich des mehrjährigen BAM-Themenfeldprojektes „ProMoAM“. Im Vortrag werden die ersten Ergebnisse der Optimierung sowie die gefundenen Anwendungsgrenzen an Beispielen erläutert. T2 - DGZfP Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 26.05.2019 KW - Röntgenrückstreuung KW - Additive Fertigung PY - 2019 UR - https://jt2019.dgzfp.de/Programm#Di.1.B.2 AN - OPUS4-50521 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Gassensitive Flugroboter der BAM T1 - Aerial robot olfaction @ BAM N2 - Der Vortrag gibt Beispiele dafür, wie Drohnen sinnvoll im zivilen Bereich eingesetzt werden können. Insbesondere werden die Lokalisierung von Gasemissionsquellen und die Erstellung von Gasverteilungskarten vorgestellt. T2 - InnoTesting2020 „Innovative Ideen - neue Testmethoden” CY - Wildau, Berlin, Germany DA - 27.02.2020 KW - Mobile Robot Olfaction KW - Erstellung von Gasverteilungskarten KW - Lokalisierung von Gasemissionsquellen KW - UAV / UAS PY - 2020 AN - OPUS4-50476 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Sekine, R. A1 - Huang, J. A1 - Steckenmesser, D. A1 - Steffens, D. A1 - Huthwelker, T. A1 - Borca, C. A1 - Pradas del Real, A. A1 - Castillo-Michel, H. A1 - Adam, Christian T1 - Effects of a nitrification inhibitor on nitrogen species in the soil and the yield and phosphorus uptake of maize N2 - Phosphorus (P) resource availability is declining and the efficiency of applied nutrients in agricultural soils is becoming increasingly important. This is especially true for P fertilizers from recycled materials, which often have low plant availability. Specific co-fertilization with ammoniumcan enhance P plant availability in soils amended with these P fertilizers, and thus the yield of plants. To investigate this effect, we performed a pot experiment with maize in slightly acidic soil (pH 6.9) with one water-soluble (triple superphosphate [TSP]) and two water-insoluble (sewage sludge-based and hyperphosphate [Hyp]) P fertilizers and anammoniumsulfate nitrate with or without a nitrification inhibitor (NI). The dry matter yield of maize was significantly increased by the NI with the Hyp (from 14.7 to 21.5 g/pot) and TSP (from 40.0 to 45.4 g/pot) treatments. Furthermore, P uptake was slightly increased in all three P treatments with the NI, but not significantly. Olsen-P extraction and P K-edge micro-X-ray absorption near-edge structure (XANES) spectroscopy showed that apatite-P of the water insoluble P fertilizers mobilized during the plant growth period. In addition, novel nitrogen (N) K-edge micro-XANES spectroscopy and the Mogilevkina method showed that the application of an NI increased the fixation of ammonium in detectable hot spots in the soil. Thus, the delay in the nitrification process by the NI and the possible slow-release of temporarily fixed ammoniumin the soil resulted in a high amount of plant available Ammonium in the soil solution. This development probably decreases the rhizosphere pH due to release of H+ by plants during ammoniumuptake, whichmobilizes phosphorus in the amended soil and increases the dry matter yield of maize. This is especially important for water-insoluble apatite-based P fertilizers (conventional and recycled), which tend to have poor plant availability. KW - Fertilzer KW - Phosphorus recovery KW - Ammonium KW - Nitrification inhibitor KW - XANES spectroscopy KW - Diffusive gradients in thin films (DGT) PY - 2020 DO - https://doi.org/10.1016/j.scitotenv.2020.136895 SN - 1879-1026 VL - 715 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-50477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Diehn, S. A1 - Zimmermann, B. A1 - Tafintseva, V. A1 - Seifert, S. A1 - Bagcioglu, M. A1 - Ohlson, M. A1 - Weidner, Steffen A1 - Fjellheim, S. A1 - Kohler, A. A1 - Kneipp, Janina T1 - Combining Chemical Information From Grass Pollen in Multimodal Characterization N2 - The analysis of pollen chemical composition is important to many fields, including agriculture, plant physiology, ecology, allergology, and climate studies. Here, the potential of a combination of different spectroscopic and spectrometric methods regarding the characterization of small biochemical differences between pollen samples was evaluated using multivariate statistical approaches. Pollen samples, collected from three populations of the grass Poa alpina, were analyzed using Fourier-transform infrared (FTIR) spectroscopy, Raman spectroscopy, surface enhanced Raman scattering (SERS), and matrix assisted laser desorption/ionization mass spectrometry (MALDI-TOF MS). The variation in the sample set can be described in a hierarchical framework comprising three populations of the same grass species and four different growth conditions of the parent plants for each of the populations. Therefore, the data set can work here as a model system to evaluate the classification and characterization ability of the different spectroscopic and spectrometric methods. ANOVA Simultaneous Component Analysis (ASCA) was applied to achieve a separation of different sources of variance in the complex sample set. Since the chosen methods and sample preparations probe different parts and/or molecular constituents of the pollen grains, complementary information about the chemical composition of the pollen can be obtained. By using consensus principal component analysis (CPCA), data from the different methods are linked together. This enables an investigation of the underlying global information, since complementary chemical data are combined. The molecular information from four spectroscopies was combined with phenotypical information gathered from the parent plants, thereby helping to potentially link pollen chemistry to other biotic and abiotic parameters. KW - Pollen KW - MALDI-TOF MS KW - FTIR KW - Raman KW - Multivariate analyses PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504822 DO - https://doi.org/10.3389/fpls.2019.01788 VL - 10 SP - 1788 AN - OPUS4-50482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - Applied Crystallography as a tool for a better understanding of Fundamental Questions of high temperature corrosion phenomena N2 - Corrosion Science Meets X-Rays, Neutrons and Electrons. The presentation gives an overview on current research activities applying in-situ X-ray diffraction and spectroscopy for a better understanding of fundamental mechanisms of high temperature corrosion. Additionally the knowledge gain by applying neutron powder diffraction and EBSD analysis is presented. T2 - Joint meeting of german and polish crystallographic association 2020 CY - Wroclaw, Poland DA - 24.02.2020 KW - Corrosion KW - Oxidation KW - In situ KW - Diffraction PY - 2020 AN - OPUS4-50483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Beck, Uwe A1 - Lange, Thorid T1 - Validierung der Oberflächenbehandlung für hochfeste Klebverbindungen und Beschichtungen als durchgehendes Mehr-Proben-Konzept in den Schritten Reinigung, Vorbehandlung, Klebung und Prüfung der Verbundfestigkeit "OKTETT - Acht auf einen Streich" N2 - Aus der Möglichkeit mittels Zentrifugentechnologie bis zu 8 Proben gleichzeitig einer Zugprüfung unter wirklich identischen Bedingungen, schnell über einfaches Einstecken der Proben und unter Ausschluss jeglicher Querkräfte, zu unterziehen , ergab sich für Klebverbindungen erstmals die Möglichkeit einer statistisch abgesicherten Prüfung identischer bzw. einer vergleichend bewertenden Prüfung unterschiedlicher Verbundsysteme. Es war deshalb naheliegend, auch das Aufkleben der Prüfstempel unter möglichst identischen Bedingungen und ebenfalls frei von Querkräften im OKTETT durchzuführen. Außerdem sind beim durchgehenden Handling im OKTETT die identische Vorbehandlung vor dem Kleben, identische Transferzeiten und -bedingungen zwischen den verschiedenen Prozessschritten, eine weitgehend gleichartige Klebstoffaufbereitung und -applikation sowie die bessere Einhaltung von gleichen Verarbeitungs- und Aushärtezeiten der Klebstoffe vor der Prüfung der Verbundfestigkeit für jeweils 8 Proben sichergestellt. Im Ergebnis dieser Überlegungen stellte sich schnell heraus, dass das Mehr-Proben-Kleben unter identischen Bedingungen für in Grenzen unterschiedliche Verbundsysteme eine ungelöste Aufgabenstellung ist. KW - Zentrifugentechnologie KW - Mehr-Proben-Handling KW - Ranking und Statistik KW - Verbundfestigkeit KW - Klebfestigkeit PY - 2014 N1 - Das Dokument unterliegt der Vertraulichkeit und kann nicht zugänglich gemacht werden Projektlaufzeit: 01.10.2014 bis 30.09.2014 The document is subject to confidentiality restrictions and cannot be made accessible Project runtime: 01.10.2014 to 30.09.2014 SP - 1 EP - 14 AN - OPUS4-50429 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietz, T. A1 - Gottlieb, Cassian A1 - Kohns, P. A1 - Ankerhold, G. T1 - Comparison of atomic and molecular emission in LIBS for the quantification of harmful species in cement-based materials N2 - Due to the penetration of harmful chlorides into concrete, e.g. from de-icing salt, damage processes such as chloride-related pitting corrosion can occur if critical values are exceeded. In this study, multiphase materials such as chloride-contaminated concrete are examined in detail. A direct comparison is made by analyzing the spectroscopic information of simultaneously measured atomic and molecular emissions with laser-induced breakdown spectroscopy (LIBS). In addition, the influence on the calibration is examined on the basis of the combined spectral information of both reaction paths of the penetrated chlorides. The calibration models of univariate and multivariate methods were validated using reference samples with wet chemical analysis. The results are applied to a concrete sample of a parking deck, which was also analyzed by potentiometric wet chemistry. In order to account for the heterogeneity of concrete, spatially (200 μm) and spectroscopically (0.1 nm) resolved LIBS measurements were performed using a fully automated laboratory system. Simultaneous measurements with three spectrometers allow the analysis of the emission processes of several elements such as Cl, Ca, O, Si and Mg as well as the newly formed molecules CaO and CaCl. The evaluation of the molecular emission in combination with atomic lines extends the analytical performance, since different concrete phases such as aggregates and cement matrix can be better represented. The measurements were carried out in ambient air and with helium purge gas. The limit of detection (LOD) achieved for a combined evaluation of atomic and molecular emission was determined to be 0.028 wt%. KW - Laser-induced breakdown spectroscopy (LIBS) KW - Cement-based materials KW - Atomic and molecular mapping KW - Chemometrics PY - 2019 DO - https://doi.org/10.1016/j.sab.2019.105707 SN - 0584-8547 VL - 161 SP - 105707 PB - Elsevier B.V. AN - OPUS4-50438 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Abschlusspräsentation zum Unterauftrag des BMWi Projekts ARGUS N2 - Im Rahmen eines BMWi Projekts der Fa. Innovent Jena, bei dem ein neuartiger optischer Sensor zur Bewertung der Oberflächenqualität und Reinheit von optischen Gläsern im Fokus stand, wurden die abbildende Ellipsometrie, die IR-Mikroskopie und die Weißlichtinterferenzmikroskopie als Referenzverfahren herangezogen. Mittels Brewster-Winkelmessungen konnten „Wolkenstrukturen“ identifiziert werden, die bei nachfolgenden Beschichtungsprozessen zu Schichtdefekten führen können. Außerdem wurden mittels Ellipsometrie Änderungen im Brechungsindex der Floatgläser (Luft- bzw. Zinnseite) nachgewiesen. Topographie Oberflächenmerkmale wie Welligkeit, Rauheit und Kreuzrillen konnten mittels Weißlichtinterferenzmikroskopie bzw. abbildender Ellipsometrie identifiziert werden. T2 - Projektverteidigung: Abschlusspräsentation zum Unterauftrag ARGUS, 14.12.2017, Jena, Innovent CY - Jena, Germany DA - 14.12.2017 KW - Glasoberflächen KW - Imaging Ellipsometrie KW - Verunreinigungen KW - Fehlstellen KW - Weißlichtinterferenzmikroskopie KW - Topographie PY - 2017 AN - OPUS4-50439 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon T1 - Spectroscopic analysis of colourants and binders of Chinese reverse glass paintings tracing a cultural dialogue N2 - Scientific analysis based on spectroscopic methods provide essential information on the composition of colourants and binders in paintings. These results can be set in a historical context and help to confirm art historical interpretations. Proofs of certain pigments can be used for dating purposes and may reveal if the artist used not only local but also imported materials. A pilot study of two Chinese reverse glass paintings from the late 19th (Yingying and Hongniang) and early 20th centuries (The Archer) was performed using a multi-analytical approach including X-ray fluorescence (XRF), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and Raman spectroscopy. This approach allowed the identification of the pigments and the classification of the binding media. The results reveal a combined use of traditional Chinese and imported European materials. Several pigments like cinnabar, lead white, orpiment, carbon black and copper-arsenic green (probably emerald green) were found in both paintings; red lead, artificial ultramarine blue, Prussian blue and ochre appear in at least one of the paintings. The proof of limewash (calcite and small amounts of portlandite) as a backing layer in “Yingying and Hongniang” indicates that clamshell white was also used for reverse glass paintings. Drying oil was classified as a binding media in most areas of both paintings. However, the orange background of The Archer yielded prominent bands of both proteinaceous and fatty binder. T2 - China and the West Reconsidering Chinese Reverse Glass Painting CY - Romont, Switzerland DA - 14.02.2020 KW - Reverse glass painting KW - DRIFTS KW - Raman spectroscopy PY - 2020 AN - OPUS4-50445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Datenformate für die zerstörungsfreie Prüfung N2 - Der Vortrag gibt eine Übersicht über die Versuche der Vergangenheit, ein standardisiertes Datenformat für die zerstörungsfreie Prüfung zu etablieren. T2 - 4. Sitzung DGZfP FA ZfP 4.0 UA Schnittstellen CY - Stockelsdorf, Germany DA - 19.02.2020 KW - ZfP KW - Datenformat KW - TRAPPIST KW - STEP KW - NDTML KW - DICONDE KW - HDF5 PY - 2020 AN - OPUS4-50448 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Neues aus der BAM 2019 N2 - Neuentwicklungen im Fachbereich 8.3 "Radiologische Verfahren" der BAM T2 - BHGE Field Radiography Days 2019 CY - Ahrensburg, Germany DA - 03.09.2019 KW - Industrielle Radiographie KW - Zerstörungsfreie Prüfung PY - 2019 AN - OPUS4-50522 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - X-ray back scatter techniques for additive manufacturing N2 - X-ray back scatter imaging is rarely applied compared to classical X-ray projection imaging. More than 20 years ago the company Philips developed “COMSCAN”, a first application case for aircraft industry, which allowed even a depth resolution using back scatter imaging. The company AS&E in Boston offers back scatter imaging solutions for the security market. The principle is to scan the object with a highly collimated X-ray needle beam from one side only and to detect the backscattered radiation by a large area detector side by side with the collimation wheel. A new prototype is investigated at BAM for application and optimization in non-destructive testing. As modern industrial application field in-situ inspection in additive manufacturing is targeted. The accessibility of the printed part during the production process is very limited. This prevent the application of a two sided X-ray inspection or Computed Tomography, were an rotation of the object is required to acquire projections from 360 degrees. An important advantage for the X-ray back scatter technique are also the materials used in additive manufacturing (polymers, ceramics, light metals like Aluminum or Titanium). These materials with lower density and lower Z values give better scatter signals than metals with higher densities and Z values. The back scatter intensity decreases with increasing density and Z value of the material. But the requirements on spatial resolution and contrast sensitivity are more stringent for non-destructive testing of additive manufactured parts compared to the security area. In NDT sizes of indications smaller than 1 mm have to be detected clearly. The investigation of these limits on a state-of-the-art prototype for X-ray back scattering using rotating collimated X-ray needle beams is a part of the BAM project “ProMoAM”. The contribution shows first results of the optimization for NDT and the achieved application limits for several example cases. T2 - International Symposium on Nondestructive Characterization of Materials CY - Portoroz, Slovenia DA - 17.09.2019 KW - Non-destructive testing KW - X-ray back scattering KW - Additive Manufacturing PY - 2019 AN - OPUS4-50523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, Uwe T1 - Prediction of the visibility of indications in X-ray computed tomography by the contrast detail diagram N2 - X-Ray Computed Tomography (CT) is applied in industry for flaw detection, flaw evaluation and dimensional measurement. This requires the correct CT system settings for sufficient visibility and detectability of flaws and structure elements. The visibility of indications for human observers on a monitor depends on the square root of the reconstructed flaw area (here pores with diameter < ½ inch) in the cross sectional 2D images, the Contrast to Noise Ratio (CNR) and the Modulation Transfer Function (MTF). This applies also to 2D-projections, meaning also to “normal” digital radiographs. The ASTM guide E 1441 describes three essential functions for prediction of the visibility of small circular indications in slice images of a 3D reconstruction or a 2D reconstruction. This is the Contrast Discrimination Function (CDF), the MTF (see also the revision of ASTM E 1695), and the Contrast Detail Dose (CDD) function. The prediction of the visibility of circular indications in reconstructed slice images can be determined from the Contrast Detail Dose function, which is the combination of CDF and MTF and a physiological factor c. The measurement procedures and formulas for the prediction of the detail visibility by CDD will be corrected, tested and verified by modelling and in a Round Robin Test with modern commercial 3D CT systems of different manufacturers. Conclusions will be reported and recommendations will be given for the correct psychological factor c and the consideration of the influence of artefacts, as e.g. cupping and scatter. T2 - International Symposium on Nondestructive Characterization of Materials CY - Portoroz, Slovenia DA - 17.09.2019 KW - Nondestructive Testing KW - Computed Tomography KW - Visibility of Indications KW - Prediction from system parameters PY - 2019 AN - OPUS4-50524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Digitale industrielle Rdiographie im Anlagenbau N2 - Der Ersatz von Röntgenfilmen durch digitale Detektoren in der Zerstörungsfreien Prüfung im Anlagenbau wird seit 2013 durch neue ISO-Normen unterstützt. Nach der Erfolgsgeschichte der digitalen Photographie und der fast voll-ständigen Ablösung der Filmtechnik in der optischen Bilderfassung wird erwartet, dass sich der Übergang von der Filmradiographie zur digitalen Radiographie schnell vollzieht. Dieser Trend ist derzeit so noch nicht zu beobachten. Zur mobilen Prüfung wird in Europa immer noch vorrangig die Filmradiographie und nur teilweise die Computerra-diographie mit Speicherfolien eingesetzt. Im Bereich der stationären Prüftechnik haben sich die Matrixdetektoren (DDA) weitgehend durchgesetzt, wobei es auch hier noch alternative Detektoren wie Bildverstärker und Fluorosko-pe gibt. Mit Einführung der DIN EN ISO 17636-2 zur Schweißnahtprüfung wird seit 2013 erstmalig geregelt, wie man einen digitalen Detektor für die technische Radiographie auswählen soll, um im Vergleich zur Filmradiographie eine äquivalente Bildqualität zu erhalten. Essentielle Parameter bestimmen, ob die geforderte Bildgüte (Fehlernachweiß-empfindlichkeit) erreicht wird. Ein Überblick zeigt, welche Parameter für den praktischen Einsatz wichtig sind und wie sie ermittelt werden. Praktische Einsatzbeispiele im Anlagenbau werden diskutiert. T2 - 47. Sondertagung - Schweißen im Anlagenbau CY - Munich, Germany DA - 17.02.2019 KW - Industrielle Radiographie KW - Filmersatz KW - Normung KW - Bildqualitätsnachweis PY - 2019 UR - www.sondertagung.de AN - OPUS4-50525 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe A1 - Ewert, Uwe T1 - Digitale industrielle Radiographie im Anlagenbau N2 - Der Ersatz von Röntgenfilmen durch digitale Detektoren in der Zerstörungsfreien Prüfung im Anlagenbau wird seit 2013 durch neue ISO-Normen unterstützt. Nach der Erfolgsgeschichte der digitalen Photographie und der fast vollständigen Ablösung der Filmtechnik in der optischen Bilderfassung wird erwartet, dass sich der Übergang von der Filmradiographie zur digitalen Radiographie schnell vollzieht. Dieser Trend ist derzeit so noch nicht zu beobachten. Zur mobilen Prüfung wird in Europa immer noch vorrangig die Filmradiographie und nur teilweise die Computerradiographie mit Speicherfolien eingesetzt. Im Bereich der stationären Prüftechnik haben sich die Matrixdetektoren (DDA) weitgehend durchgesetzt, wobei es auch hier noch alternative Detektoren wie Bildverstärker und Fluoroskope gibt. Mit Einführung der DIN EN ISO 17636-2 zur Schweißnahtprüfung wird seit 2013 erstmalig geregelt, wie man einen digitalen Detektor für die technische Radiographie auswählen soll, um im Vergleich zur Filmradiographie eine äquivalente Bildqualität zu erhalten. Essentielle Parameter bestimmen, ob die geforderte Bildgüte (Fehlernachweißempfindlichkeit) erreicht wird. Ein Überblick zeigt, welche Parameter für den praktischen Einsatz wichtig sind und wie sie ermittelt werden. Praktische Einsatzbeispiele im Anlagenbau werden diskutiert. T2 - 47. Sondertagung: Schweißen im Anlagen- und Behälterbau CY - Munich, Germany DA - 19.02.2019 KW - Industrielle Radiographie KW - Digitaler Filmersatz KW - Stand der Normung KW - Bildqualitätsnachweis PY - 2019 SN - 978-3-96144-055-9 VL - 350 SP - 19 EP - 22 PB - DVS Media CY - Düsseldorf AN - OPUS4-50526 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Status of Digital RT Education in Germany considering ISO 9712:2012, the IAEA guidline on DIR and ISO/TS 25107.2:2019 N2 - Status Report on education of personnel for radiographic testing in Germany according to ISO 9712:2012, the IAEA Guideline and ISO/TS 25107 T2 - Seminar NDT Niva 3-Personell CY - Oslo, Norway DA - 11.11.2019 KW - Nondestructive Testing KW - Radiographic Testing KW - Personnel Education KW - Status in Germany KW - Requirements of Standards PY - 2019 AN - OPUS4-50527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Neue Trends bei Photonen zählenden und Energie auflösenden Detektoren N2 - Die Technologie der hybriden Teilchen (oder Photonen) zählenden Bilddetektoren wurde seit mehr als 2 Jahrzehnten durch Institutionen wie das CERN (MediPix-/ TimePix-Chips) oder das Paul-Scherrer-Institut (Pilatus-/ Eiger-Chips) entwickelt. Die Ursprünge dieser Technologie kommen aus der Hochenergie-Physik mit ihren Beschleuniger-basierten Experimenten, bei denen ein zuverlässiger und rauschfreier Nachweis jedes ionisierten Teilchens gefordert wird. Eine Energieauflösung wird ebenfalls oft verlangr. Das ist auch in der klassischen Radiographie von Nutzen, so wurden diese Detektoren auch dafür optimiert. Neueste Photonen zählenden Detektoren besitzen folgende exzellenten Bildeigenschaften: rauschfreie Photonen-Detektion in einem hohen Dynamikbereich (SNR >2500 erreichbar), hohe räumliche Auflösung (bis zu 10 µm Pixelgröße), Energieschwellen bis zur vollen spektralen Auflösung und eine sehr hohe Geschwindigkeit (bis zu Tausenden Bildern pro Sekunde). Diese hybriden Detektoren können mit hochabsorbierenden Sensorschichten aus CdTe, CZT oder GaAs bestückt werden, um bildgebende Anwendungen mit Gamma- oder harten Röntgenstrahlen zu realisieren, in denen bisher Szintillator basierende Bilddetektoren dominierten (z.B. für NDT, SPECT, PET). Im Beitrag wird der erste wirklich große Photonen zählende Detektor mit CdTe und einer lückenlosen Detektionsfläche, die aus einer theoretisch unbegrenzten Anzahl von MediPix-/ TimePix-Modulen besteht, gezeigt. Die erste kommerzielle Version eines solchen Detektors hat eine Fläche von 7cm x7cm, 1,6 Megapixel und erfüllt die Anforderungen der Prüfklasse „B“ in der industriellen Radiographie. Die Energie auflösenden Fähigkeiten dieses Detektors erlauben eine „Farb-Radiographie“, in der verschiedene Materialien in verschiedene Farben dargestellt werden. Der 2. Teil dieses Beitrags stellt einen voll spektral auflösenden Gamma- und Röntgen-Bilddetektor mit dickem CdTe und 2,4 Megapixel vor, der auf TimePix3-Chips basiert und eine sehr hohe Ortsauflösung von ~10 µm erreicht. Die hohe Zeitauflösung von TimePix3 wird mit großem Nutzen für eine substantielle Verbesserung der erhaltenen Bilder und Spektren zur Unterdrückung interner Fluoreszenzstrahlung sowie Comptonstreuungsanteilen, die die Bildinformation verschmieren, verwendet. T2 - 18. Seminar der DGZfP zu aktuellen Fragen der Durchstrahlungsprüfung und des Strahlenschutzes CY - Kassel, Germany DA - 28.03.2019 KW - Radiographische Prüfung KW - Direktumwandelnde Detektoren KW - Energieauflösende Detektoren PY - 2019 AN - OPUS4-50528 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Aktuelle Entwicklungen in der Standardisierung N2 - In den letzten zwei Jahren wurden 11 neue Standards/Standardrevisionen zur RT veröffentlicht (ohne Strahlenschutz) und 5 werden dafür gestrichen. Es wird über die neuen Anforderungen ausgewählter Normen bzw. Normrevisionen informiert und insbesondere auch über die veränderten Parameter, die bei Prüfpraxis und bei der Klassifizierung zu berücksichtigen sind. Das wichtigste Projekt ist die Revision der DIN EN ISO 17636-1, -2, RT von Schweißverbindungen, in ISO TC 44 SC 5 WG 1. Die Standards zur Schweißnahtprüfung in der Kerntechnik, DIN 25435, wurden ins Englische übertragen und bei ISO TC 85 SC 6 bearbeitet. Hauptaktivität bei ASTM ist gegenwärtig die Überarbeitung der CT-Standards und die Berücksichtigung der Anforderungen an das dimensionelle Messen. Der Guide ASTM E 1441 zur Bestimmung von MTF, Kontrast-Detail-Funktion (CDF) und Kontrast-Diskrimination-Diagramm (CDD) wird revidiert. E 2445 zur CR Long Term Stability wird ebenfalls revidiert. Die Revision soll auch in die ISO 16371-1 eingehen. Dazu ist ein Round Robin-Test geplant. Auch die Standards zur Durchstrahlungsprüfung auf Korrosion und Ablagerungen in Rohren mit Röntgen- und Gammastrahlen (EN 16407-1, -2, 2014) wurden revidiert. Diese Revision wurde als DIN EN ISO 20769-1, -2 2018 veröffentlicht und EN 16407 wird zurückgezogen. Die Revision der Standards EN 12543 und EN 12679 zur Messung der Brennfleckgröße und der Strahlergröße ist mit Verzögerung in Überarbeitung, um die digitalen Detektoren und Messmöglichkeiten mit Bildverarbeitungsprogrammen zu berücksichtigen. Ein Entwurf zur Messung der Brennfleckgröße von nano-Fokusröhren wird derzeit vom Europäischen Metrologie-Programm EMPIR gefördert. Zur radiographischen Gussteilprüfung wurde der Standard EN 12681 revidiert und 2018 veröffentlicht. Er wurde um Zulässigkeitsgrenzen erweitert und die digitale Radiographie wurde in Teil 2 berücksichtigt. T2 - 18. Seminar der DGZfP zu aktuellen Fragen der Durchstrahlungsprüfung und des Strahlenschutzes CY - Kassel, Germany DA - 28.03.2019 KW - Radiographische Prüfung KW - Standardisierung bei DIN, CEN und ISO KW - DGZfP-Richtlinien PY - 2019 AN - OPUS4-50529 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - X-ray back scatter techniques for additive manufacturing N2 - X-ray back scatter imaging is rarely applied compared to classical X-ray projection imaging. 20 years ago the company Philips developed “COMSCAN”, a first application case in the aircraft industry, which allowed even a depth resolution using back scatter imaging. The company AS&E in Boston offers back scatter imaging solutions for the security market. Their principle is to scan the object with a highly collimated X-ray needle beam from one side only and detect the backscattered radiation by a large area detector side by side with the collimation wheel. A new prototype is investigated at BAM for application and optimization in non-destructive testing. As modern industrial application field in-situ testing in additive manufacturing is targeted. The accessibility of the printed part during the production process is very limited. This prevent the application of a two sided X-ray inspection or Computed Tomography, were an rotation of the object is required to acquire projections from 360 degrees. An important advantage for the X-ray back scatter technique are also the materials used in additive manufacturing (polymers, ceramics, light metals like Aluminum or Titanium). These materials with lower density and lower Z values give better scatter signals than metals with higher densities and Z values. The back scatter intensity decreases with increasing density and Z value of the material. But the requirements on spatial resolution and contrast sensitivity are more stringent for non-destructive testing of additive manufactured parts compared to the security area. In NDT sizes of indications smaller than 1 mm have to be detected clearly. The investigation of these limits on a stateof-the-art prototype for X-ray back scattering using rotating collimated X-ray needle beams is a part of the BAM project “ProMoAM”. The contribution shows first results of the optimization for NDT and the achieved application limits for several example cases. T2 - International symposium on digital industrial radiology and computed tomography DIR2019 CY - Fürth, Germany DA - 02.07.2019 KW - Radiographic testing KW - X-ray back scattering KW - Additive manufacturing PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505317 UR - https://www.ndt.net/search/docs.php3?id=24760 AN - OPUS4-50531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Osterloh, Kurt A1 - Röhrs, S. A1 - Schwabe, A. A1 - Radujcovic, S. A1 - Bücherl, T. A1 - Dangendorf, V. A1 - Zscherpel, Uwe A1 - Reiche, I. A1 - Nüsser, A. ED - Zscherpel, Uwe ED - Kasperl, S. T1 - Elucidating the distribution of organic consolidants in wood by Neutron Tomography N2 - While the absorption of X-rays and gamma radiation is determined by the Z-number of the elements a specimen is composed of, it is the hydrogen making an effective contrast with neutron imaging. As a consequence, interrogating with neutrons presents a suitable tool to study the distribution of organic consolidants in materials such as wood as encountered in impregnated wooden artworks. Four different examples of objects are presented here to demonstrate the potential of neutron CT: 1) small wooden pieces of ship wrecks (< 2 cm thickness) interrogated with cold neutrons (0.5 meV at the ANTARES facility of the FRM II in Garching) to demonstrate the potential and the limitation of using low energy neutrons, 2) a wooden statue soaked with carbolineum (fission neutrons 1.8 MeV at the NECTAR facility of the FRM II), 3) a smaller wooden figure of a skull heavily soaked with carbolineum so it was too tight for the fission neutrons used before with accelerator neutrons (broad range about 5.5 MeV at the PTB in Braunschweig) and 4) pieces of charred wood to study the impregnation with a consolidant (NECTAR, FRM II). With the exception of the last example, all results have been combined with X-ray tomography (BAM 8.3 in Berlin). In the case of the charred wood specimens (example 4) the density histograms of the neutron tomography results were compared with those obtained from untreated references. The observed gain in specific density of the soaked specimens corresponded with an increase of specific weight. All results obtained so far showed distinct distribution patterns attributable to structural peculiarities or organic consolidants providing valuable support for subsequent restoration works. T2 - International symposium on digital industrial radiography and computed tomography DIR2019 CY - Fürth, Germany DA - 02.07.2019 KW - Neutron Imaging KW - Cold to fast neutron testing KW - Tomography of wood samples KW - Art restauration PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505326 UR - https://www.ndt.net/search/docs.php3?id=24740 SN - 1435-4934 VL - 24 IS - 11 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-50532 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulze-Makuch, D. A1 - Haque, S. A1 - Beckles, D. A1 - Schmitt-Kopplin, P. A1 - Harir, M. A1 - Schneider, Beate A1 - Stumpp, C. A1 - Wagner, D. T1 - A chemical and microbial characterization of selected mud volcanoes in Trinidad reveals pathogens introduced by surface water and rain water N2 - Terrestrial mud volcanoes are unique structures driven by tectonic pressure and fluids from the deep subsurface. These structures are mainly found in active tectonic zones, such as the area near the Los Bajos Fault in Trinidad. Here we report a chemical and microbiological characterization of three mud volcanoes, which included analyses of multiple liquid and solid samples from the mud volcanoes. Our study confirms previous suggestions that at least some of the mud volcano fluids are a mixture of deeper salt-rich water and surficial/precipitation water. No apparent water quality differences were found between sampling sites north and south of a major geological fault line. Microbiological analyses revealed diverse communities, both aerobic and anaerobic, including sulfate reducers, methanogens, carbon dioxide fixing and denitrifying bacteria. Several identified species were halophilic and likely derived from the deeper salt-rich subsurface water, while we also cultivated pathogenic species from the Vibrionaceae, Enterobacteriaceae, Shewanellaceae, and Clostridiaceae. These microorganisms were likely introduced into the mud volcano fluids both from surface water or shallow ground-water, and perhaps to a more minor degree by rain water. The identified pathogens are a major health concern that needs to be addressed. KW - Water stable isotope analysis KW - Mud volcanoe fluids KW - Metabolomics PY - 2020 DO - https://doi.org/10.1016/j.scitotenv.2019.136087 VL - 707 SP - 136087 PB - Elsevier B.V. AN - OPUS4-50499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Faßbender, Sebastian T1 - On-line hyphenation of CE with multicollector-ICP-MS for species-specific isotopic analysis of sulfur N2 - In many scientific fields, isotopic analysis can offer valuable information, e.g., for tracing the origin of food products, environmental contaminants, forensic and archaeological samples (provenance determination), for age determination of minerals (geochronological dating) or for elucidating chemical processes. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement. In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared with data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was high enough to distinguish the rivers from one another by the isotopic signature of the river water sulfate. Next to environmental applications, a future field could be species-specific isotopic analysis of biomolecules, as sulfur is the only covalently bound constituent of proteins which can be analyzed by MC-ICP-MS. T2 - DGMS 2020 CY - Münster, Germany DA - 01.03.2020 KW - Capillary electrophoresis KW - Hyphenated techniques KW - Isotopic analysis KW - Multicollector-ICP-MS KW - Speciation analysis PY - 2020 AN - OPUS4-50501 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von der Au, Marcus T1 - HR-CS-GF-MAS as a new screening method for emerging pollutants - per- and polyfluorinated substances in the environment N2 - The introduction of fluorine in organic molecules leads to new chemical/physical properties. Especially in the field of pharmaceuticals, fluorinated organic molecules are becoming more and more popular and at present amount up to 25% of market share, with an upward trend. The main benefits of fluorinated pharmaceuticals are: (i) enhanced fat solubility; (ii) enhanced interaction of catalytic-center of enzymes with fluorine-drugs; (iii) a delayed metabolism within the human body. Highly fluorinated organic substances are also used in technical applications (e.g. coatings, fire-extinguishing agents). Due to the broad variety of fluorinated substances and increasing production volumes numerous and up to date unknown fluorine-species are most likely to be present in the (aquatic) environment. Analytical methods to assess the degree of contamination of surface waters with organically bound fluorine are highly needed and up to now only combustion ion chromatography based method is available, which is relatively laborious. Since a few years’ high resolution-continuum source-graphite furnace atomic absorption spectrometers (HR-CS-GFAAS) are commercially available from Analytik Jena. By means of this technique, the detection of high resolution molecular absorption spectra (MAS) is enabled. Thus, fluoride is detectable upon the addition of a modifier and the formation of a diatomic molecule (e.g. GaF). Just recently, we applied this technique for total fluorine (mainly dissolved fluoride) analysis in river water samples. In the present work a HR-CS-GFMAS method for extractable organically bound fluorine (EOF) analysis in surface water samples was developed by us. The method is based on SPE extraction of organically bound fluorine even in the presence of high fluoride concentrations followed by HR-CS-GFMAS analysis upon elution. Due to high enrichment factors, LODs in the low ng/L range were achieved. We successfully applied our SPE HR-CS-GFMAS method to Rhine water samples and EOF in the range of about 50-300 ng/L was detectable. T2 - DGMS 2020 CY - Münster, Germany DA - 01.03.2020 KW - SPE HR-CS GF MAS PY - 2020 AN - OPUS4-50503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von der Au, Marcus T1 - HR-CS-GF-MAS as a new screening method for emerging pollutants - per- and polyfluorinated substances in the environment N2 - The introduction of fluorine in organic molecules leads to new chemical/physical properties. Especially in the field of pharmaceuticals, fluorinated organic molecules are becoming more and more popular and at present amount up to 25% of market share, with an upward trend. The main benefits of fluorinated pharmaceuticals are: (i) enhanced fat solubility; (ii) enhanced interaction of catalytic-center of enzymes with fluorine-drugs; (iii) a delayed metabolism within the human body. Highly fluorinated organic substances are also used in technical applications (e.g. coatings, fire-extinguishing agents). Due to the broad variety of fluorinated substances and increasing production volumes numerous and up to date unknown fluorine-species are most likely to be present in the (aquatic) environment. Analytical methods to assess the degree of contamination of surface waters with organically bound fluorine are highly needed and up to now only combustion ion chromatography based method is available, which is relatively laborious. Since a few years’ high resolution-continuum source-graphite furnace atomic absorption spectrometers (HR-CS-GFAAS) are commercially available from Analytik Jena. By means of this technique, the detection of high resolution molecular absorption spectra (MAS) is enabled. Thus, fluoride is detectable upon the addition of a modifier and the formation of a diatomic molecule (e.g. GaF). Just recently, we applied this technique for total fluorine (mainly dissolved fluoride) analysis in river water samples. In the present work a HR-CS-GFMAS method for extractable organically bound fluorine (EOF) analysis in surface water samples was developed by us. The method is based on SPE extraction of organically bound fluorine even in the presence of high fluoride concentrations followed by HR-CS-GFMAS analysis upon elution. Due to high enrichment factors, LODs in the low ng/L range were achieved. We successfully applied our SPE HR-CS-GFMAS method to Rhine water samples and EOF in the range of about 50-300 ng/L was detectable. T2 - DGMS 2020 CY - Münster, Germany DA - 01.03.2020 KW - SPE HR-CS GF MAS PY - 2020 AN - OPUS4-50504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane T1 - Corrigendum to "Measurement of the radiative energy output of flash lamps by means of thermal thin probes" [Infrared Phys. Technol. 67 (2014) 363-370] N2 - This is a corrigendum to the original article "Measurement of the radiative energy output of flash lamps by means of thermal thin probes" that was published in the journal "Infrared physics & technology", vol. 67 (2014), pp. 363-370. PY - 2018 DO - https://doi.org/10.1016/j.infrared.2017.11.011 SN - 1350-4495 VL - 91 SP - 278 PB - Elsevier CY - Amsterdam AN - OPUS4-50505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lemke, Nora T1 - Sulfur isotope dilution ICP MS for traceable protein quantification N2 - Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful method for the matrix-independent quantitative analysis of target elements. Developed for the use in inorganic trace analysis, ICP-MS is nowadays a valuable tool for bioanalytical questions. Especially the use of ICP-MS for quantitative proteomics by measuring heteroatoms has gained recognition in the last decade, considering that established quantification methods like organic mass spectrometry depend on labelling of the target protein or the existence of matched protein and peptide standards. The need for reliable quantification of proteins is continuously growing, but only a limited number of well-characterized and quantified protein standards are available so far. Accurately quantified, traceable protein standards are necessary to ensure comparability of measurements between laboratories, not only in basic research but also in a clinical context. One example of this is the Alzheimer’s disease biomarker tau protein. However, existing tau standards lack comparability, emphasizing the need for a well-quantified protein standard. Therefore, we developed a method for the quantification of pure proteins via sulfur isotope dilution ICP-MS (IDMS). As sulfur is present in two amino acids, cysteine and methionine, it exists in nearly all proteins and can be used for the quantification of proteins of known stoichiometry. We employed simple offline strategies for the separation of non-protein bound sulfur species. Quantification of these contaminations by IDMS allows for correction of the protein content and enables reliable protein quantification. We report the protein mass fractions of a standard reference material and commercially available proteins determined by sulfur IDMS, including the expanded uncertainties. The developed method can be applied for the reliable and traceable quantification of pure proteins for use as in-house standards. Here, we successfully used this method for the quantification of the tau protein. T2 - 53rd annual conference of the DGMS including 27th ICP-MS User's Meeting CY - Münster, Germany DA - 01.03.2020 KW - ICP-MS KW - Isotope dilution KW - Protein KW - Quantification KW - Tau protein PY - 2020 AN - OPUS4-50510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schaepe, Kaija A1 - Jungnickel, H. A1 - Heinrich, Thomas A1 - Tentschert, J. A1 - Luch, A. A1 - Unger, Wolfgang ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Secondary ion mass spectrometry N2 - This chapter provides an introduction in secondary ion mass spectrometry as one of the leading surface chemical analysis and imaging techniques with molecular specificity in the field of material sciences. The physical basics of the technique are explained along with a description of the typical instrumental setups and their modes of operation. The application paragraph specifically focuses on nanoparticle analysis by SIMS in terms of surface spectrometry, imaging, analysis in organic and complex media, and depth profiling. A review of the existing literature is provided, and selected studies are showcased. Limitations and pitfalls as well as current technical developments of SIMS application in nanoparticle surface chemical analysis are equally discussed. KW - Time-of-flight secondary ion mass spectrometry KW - Surface chemical analysis KW - Imaging KW - Nanomaterials KW - Nanoparticles KW - Core-shell PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00025-0 SP - 481 EP - 509 PB - Elsevier CY - Amsterdam AN - OPUS4-50187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hein, Sebastian T1 - Ansätze und Herausforderungen für das QM-System einer Ressortforschungseinrichtung N2 - Die BAM betreibt ein QM-System, das stark an der DIN EN ISO/IEC 17025 orientiert ist und welches in den meisten Fachabteilungen durch Akkreditierungen untersetzt wird. Mit der Zunahme der Forschungsaktivitäten in den letzten Jahren ist der DFG-Kodex zur Sicherstellung der Guten wissenschaftlichen Praxis deutlicher in den Fokus des Qualitätsmanagements gerückt. Der Vortrag zeigt auf, welche QM-Anforderungen an die Leistungen der BAM gestellt werden und mit welchen Instrumenten sie diese umsetzt, so dass Gute wissenschaftliche Praxis und Akkreditierungen gut harmonieren können. T2 - QM-Seminar; Robert-Koch-Institut CY - Berlin, Germany DA - 21.01.2020 KW - Qualitätsmanagement KW - Gute wissenschaftliche Praxis PY - 2020 AN - OPUS4-50311 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Changes in passive film chemistry of stainless steels in the presence of iron reducing bacteria N2 - Summary of the results obtained at DELTA-Beamline 8 in 2018. T2 - DELTA User Treffen CY - Dortmund, Germany DA - 28.11.2018 KW - MIC KW - Corrosion KW - XANES PY - 2018 AN - OPUS4-50312 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Combined electrochemical techniques for the investigation of corrosion processes N2 - Short presentation of BAM, a summary of the methods available in FB 6.2 and recent results on MIC and high resolution corrosion studies T2 - Institute Seminar: Jerzy Haber Institute of Catalysis and Surface Chemistry CY - Cracow, Poland DA - 07.11.2018 KW - MIC KW - Corrosion KW - Atomic Force Microscopy (AFM) KW - Combined corrosive and mechanical load PY - 2018 AN - OPUS4-50313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Melzer, Michael A1 - Makarov, D. A1 - Schmidt, O. G. T1 - A review on stretchable magnetic field sensorics N2 - The current establishment of stretchable electronics to form a seamless link between soft or even living materials and the digital world is at the forefront of multidisciplinary research efforts, bridging physics, engineering and materials science. Magnetic functionalities can provide a sense of displacement, orientation or proximity to this novel formulation of electronics. This work reviews the recent development of stretchable magnetic field sensorics relying on the combination of metallic thin films revealing a giant magnetoresistance effect with elastomeric materials. Stretchability of the magnetic nanomembranes is achieved by specific morphologic features (e.g. wrinkles or microcracks), which accommodate the applied tensile deformation while maintaining the electrical and magnetic integrity of the sensor device. The entire development, from the demonstration of the world’s first elastically stretchable magnetic sensor to the realization of a technology platform for robust, ready-to-use elastic magnetosensorics is described. Soft giant magnetoresistive elements exhibiting the same sensing performance as on conventional rigid supports, but with fully strain invariant properties up to 270% stretching have been demonstrated. With their unique mechanical properties, these sensor elements readily conform to ubiquitous objects of arbitrary shapes including the human skin. Stretchable magnetoelectronic sensors can equip soft and epidermal electronic systems with navigation, orientation, motion tracking and touchless control capabilities. A variety of novel technologies, like electronic skins, smart textiles, soft robotics and actuators, active medical implants and soft consumer electronics will benefit from these new magnetic functionalities. KW - Stretchable electronics KW - Giant magnetoresistance KW - Magnetic sensors KW - Magnetic thin films PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502049 DO - https://doi.org/10.1088/1361-6463/ab52cf SN - 0022-3727 (Druck) SN - 1361-6463 (Web) VL - 53 IS - 8 SP - Paper 083002, 34 PB - IOP Publishing AN - OPUS4-50204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duwe, M. A1 - Quast, J.-H. A1 - Schneider, S. A1 - Fischer, Daniel A1 - Beck, Uwe T1 - Thin-film metrology of tilted and curved surfaces by imaging Mueller-matrix ellipsometry N2 - For the vast majority of ellipsometric measurements, the application of planar substrates is mandatory and requires a proper sample alignment prior to the measurement. Here, the authors present a generalized approach of how to extract the isotropic ellipsometric sample parameters from an imaging Mueller-matrix measurement even if the sample is significantly misaligned. They validate the method by layer-thickness calculations based on imaging Mueller-matrix measurements of flat crystalline silicon samples that were misaligned on purpose. Furthermore, they also exploit this method’s capabilities to perform spatially resolved layer-thickness measurements of a single-layer indium-tin-oxide coating on a fused-silica microlens without the need of realignment or repositioning of the sample during the measurement. T2 - 8th International conference on spectroscopic ellipsometry (ICSE-8) CY - Barcelona, Spain DA - 26.05.2019 KW - Metrology KW - Thin films KW - Polarization spectroscopy KW - Spectroskopic Imaging KW - Mueller-Matrix imaging ellipsometry PY - 2019 DO - https://doi.org/10.1116/1.5122757 SN - 2166-2746 SN - 2327-9877 VL - 37 IS - 6 SP - 062908 PB - AIP CY - New York, NY AN - OPUS4-50209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - Electromagnetic testing for additive manufacturing N2 - With rising popularity and availability of additive manufacturing (AM), companies mainly in the aerospace sector, set high requirements on quality control of AM parts, especially produced with selective laser melting (SLM). Since it was shown that those parts are prawn to flaws like pores or cracks, every part needs to be tested. Therefore, NDT Methods, like eddy current testing (ET), could help to characterize SLM parts. Research on ET has shown, that offline ET with high spatial resolution MR (magneto resistive) sensor arrays is possible and that flaws as small as 50 µm could be detected while significantly reducing testing time. A first approach on automated online ET method for testing SLM parts is proposed in this contribution. T2 - IIW 2019 CY - Bratislava, Slovakia DA - 08.07.2019 KW - Additive manufacturing KW - Giant magneto resistance KW - Online monitoring KW - Eddy current testing PY - 2019 AN - OPUS4-50244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - Hochauflösende Wirbelstromprüfung in der additiven Fertigung N2 - In den letzten Jahren wurden enorme Fortschritte bei der additiven Fertigung erzielt. So sind heutzutage industrielle Kleinserienfertigungen mit den 3D-Druckverfahren wirtschaftlich und konkurrenzfähig. Allerdings ist der Einsatz in Bezug auf sicherheitsrelevante Komponenten noch nicht vollumfänglich möglich. Grund hierfür sind die Materialeigenschaften 3D-gedruckter Komponenten, welche sich von den Eigenschaften konventionell gefertigter Materialien unterscheiden (Variationen im Gefüge, der Härte usw.). Ein Ansatz zur Lösung dieses Problems ist der Einsatz geeigneter online-Prüfverfahren zur Qualitätssicherung. Diese befinden sich –abgesehen von kamerabasierten Verfahren– aber noch im Entwicklungsstadium. Bei metallischen Werkstoffen stellt die Wirbelstromprüfung ein geeignetes Verfahren zur lagenweisen Online-Überprüfung des Fertigungsprozesses dar. Der Beitrag gibt einen Überblick über die derzeitige Patentlage sowie den Stand der Forschung zum Einsatz der Wirbelstromprüfung beim 3D-Druck metallischer Komponenten. Am Beispiel des pulverbasierten SLM-Verfahrens (selective laser melting; selektives Laserschmelzen) werden zudem Arbeiten der BAM und erste Ergebnisse einer angepassten Wirbelstromtechnik unter Verwendung von GMR-Sensoren (giant magneto resistance) vorgestellt. Hier wird das Ziel verfolgt, hochauflösend kleinste Fehler und Poren (im Bereich ≈100 µm) in der Oberfläche zu detektieren und durch lagenweises Abrastern einen 3D-Datensatz für die Qualitätskontrolle zu erstellen. Schließlich soll das System in der Lage sein, aktiv in den Fertigungsprozess einzugreifen, wodurch entweder die Produktion fehlerhafter Bauteile gestoppt wird oder durch geeignete Maßnahmen Fehler ausgeheilt werden. T2 - Wirbelstromprüfung – Aktuelle Anwendungen und Entwicklungen CY - Celle, Germany DA - 10.09.2019 KW - Additive Fertigung KW - Wirbelstromprüfung KW - Onlinemonitoring KW - Riesenmagnetwiderstand KW - GMR PY - 2019 AN - OPUS4-50245 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, C. A1 - Lierenfeld, M. B. A1 - Wilsch, Gerd A1 - Bohling, C. T1 - Es geht auch einfacher N2 - Mit laserbasiertem Verfahren Zustand von Betonbauwerken erfassen: Die Laserinduzierte Breakdown Spektroskopie (LIBS) stellt eine Alternative zur nasschemischen Analyse dar, um den Zustand von Betonbauwerken zu erfassen. Bei diesem Verfahren laufen der Analysevorgang und die Auswertung automatisiert ab. Ein Prototyp für die mobile Anwendung auf der Baustelle steht zur Verfügung. So kann auf Knopfdruck ein schriftlicher Bericht erstellt werden, der einen genauen Wert für die Eindringtiefe eines relevanten Elements wie Chlorid ausgibt. KW - Beton KW - LIBS KW - Chlorid KW - Vor-Ort-Untersuchung PY - 2019 VL - 42 IS - 7 SP - 28 EP - 31 PB - Verlagsgesellschaft Rudolf Müller GmbH CY - Köln AN - OPUS4-50283 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Characterization of nanoparticles - Measurement processes for nanoparticles N2 - Characterization of Nanoparticles: Measurement Processes for Nanoparticles surveys this fast growing field, including established methods for the physical and chemical characterization of nanoparticles. The book focuses on sample preparation issues (including potential pitfalls), with measurement procedures described in detail. In addition, the book explores data reduction, including the quantitative evaluation of the final result and its uncertainty of measurement. The results of published inter-laboratory comparisons are referred to, along with the availability of reference materials necessary for instrument calibration and method validation. The application of these methods are illustrated with practical examples on what is routine and what remains a challenge. In addition, this book summarizes promising methods still under development and analyzes the need for complementary methods to enhance the quality of nanoparticle characterization with solutions already in operation. KW - Nanoparticles KW - Characterization method KW - Sample preparation KW - Inter-laboratory comparison KW - Standardisation KW - Measurement uncertainty KW - Case studies PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/C2017-0-00312-9 SP - 1 EP - 566 PB - Elsevier CY - Amsterdam AN - OPUS4-50284 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Voss, L. A1 - Saloga, Patrick E. J. A1 - Stock, V. A1 - Böhmert, L. A1 - Braeuning, A. A1 - Thünemann, Andreas A1 - Lampen, A. A1 - Sieg, H. T1 - Environmental impact of ZnO nanoparticles evaluated by in vitro simulated digestion N2 - ZnO nanoparticles are found in different food and consumer products, and their toxicological effects are still under investigation. It is therefore important to understand their behavior in the gastrointestinal tract. Here, we used an in vitro model to assess the physicochemical fate of ZnO nanoparticles during the digestive process in artificial saliva, stomach juice, and intestinal juice. Atomic absorption spectrometry and small-angle X-ray scattering were employed to investigate two ZnO nanomaterials, one intensively characterized reference material and soluble ZnCl2 in a broad range of concentrations between 25 and 1000 μg/mL in the intestinal fluid. Because food components may influence the behavior of nanomaterials in the gastrointestinal tract, starch, milk powder, and olive oil were used to mimic carbohydrates, protein, and fat, respectively. Additionally, ion release of all Zn species was assessed in cell culture media and compared to artificial intestinal juice to investigate relevance of typical cell culture conditions in ZnO nanotoxicology. ZnCl2 as well as the ZnO species were present as particles in artificial saliva but were solubilized completely in the acidic stomach juice. Interestingly, in the intestinal fluid a concentration-independent de novo formation of particles in the nanoscale range was shown. This was the case for all particles as well as for ZnCl2, regardless of the concentration used. Neither of the food components affected the behavior of any Zn species. On the contrary, all Zn species showed a Zn-concentration-dependent ion release in common cell culture medium. This questions the suitability of cell culture studies to investigate the effect of ZnO nanoparticles on intestinal cells. Our results show that Zn-containing nanoparticles reach the intestine. This underlines the importance of determining the influence of the test environment on nanoparticle fate. KW - SAXS KW - Digestion KW - Zinc oxide KW - Nanoparticles PY - 2020 DO - https://doi.org/10.1021/acsanm.9b02236 VL - 3 IS - 1 SP - 724 EP - 733 AN - OPUS4-50288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rautenberg, Max T1 - Metal phosphonates as proton conductors and ORR catalysts N2 - Metal phosphonates are promising materials for applications in fuel cells, due to their high proton conductivity and higher chemical and thermal stability compared to the industry standard (e.g. Nafion®). Additionally, metal phosphonates are precursors to porous carbon materials with evenly distributed centers for ORR catalysis. As a fast and sustainable synthesis, mechanochemistry is the synthesis method of choice. Thorough characterization is carried out by XRD, MAS-NMR, XAS, BET, and DVS. T2 - 2nd European Workshop on Metal Phosphonates CY - Berlin, Germany DA - 24.09.2019 KW - Phosphonates KW - Proton cunductor KW - Oxygen reduction reaction KW - Catalysis KW - Mechanochemistry PY - 2019 AN - OPUS4-50257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Polymer mass spectrometry at BAM with special emphasis on MALDI and ESI N2 - Since its introduction mass spectrometric techniques like Matrix-assisted Laser Desorption/ionization (MALDI) and Electrospray Ionization (ESI) have become indispensable for synthetic polymer analyses. Ideally, various polymer properties (monomer structure, masses, mass distribution, end groups) can be determined simultaneously. However, in real life these experiments are always affected by important structural parameters and instrumental limitations. A short introduction focussing on latest findings with respect to ionisation principles and mechanisms will be given. Recent results from our group will be presented and efforts to avoid common drawbacks of polymer mass spectrometry will be discussed. In this regard, MALDI - Imaging mass spectrometry and the 2D hyphenation of MS with different chromatographic separation techniques were especially useful, since they can provide additional information and reduce the complexity of polymer analyses. T2 - 21. European Symposium on Polymer Spectroscopy CY - Linz, Austria DA - 13.01.2020 KW - Mass spectrometry KW - MALDI-TOF MS KW - ESI-TOF MS KW - Polymer PY - 2020 AN - OPUS4-50260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gojani, Ardian T1 - Combined Raman and LIBS using Spatial Heterodyne Spectrometer with High Repetition Rate Laser N2 - Spatial heterodyne spectroscopy is used for Raman and laser-induced breakdown spectroscopy of six rocks with various mineral content, using high repetition rate diode-pumped solid state lasers. While LIBS data are obtained for all samples, Raman signal was determined only for half of those. This work shows that it is possible to combine LIBS and Raman spectrometry into a single instrument consisting of a DPSS laser for excitation and SHS for spectral recording. For better results and gain from complementary spectrochemical information that the system provides, it is necessary to optimize light collection. T2 - 2020 Winter Conference on Plasma Spectrochemistry CY - Tucson, Arizona, USA DA - 13.01.2020 KW - Laser-Induced Background Spectroscopy KW - Spatial heterodyne spectroscopy KW - Raman spectroscopy PY - 2020 AN - OPUS4-50265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kneipp, Janina A1 - Zancajo, Victor M.R. A1 - Diehn, S. A1 - Filiba, N. A1 - Elbaum, R. T1 - Spectroscopic Discrimination of Sorghum Silica Phytoliths N2 - Grasses accumulate silicon in the form of silicic acid, which is precipitated as amorphous silica in microscopic particles termed phytoliths. These particles comprise a variety of morphologies according to the cell type in which the silica was deposited. Despite the evident morphological differences, phytolith chemistry has mostly been analysed in bulk samples, neglecting differences between the varied types formed in the same species. In this work, we extracted leaf phytoliths from mature plants of Sorghum bicolor (L.) Moench. Using solid state NMR and thermogravimetric analysis, we show that the extraction methods alter greatly the silica molecular structure, its condensation degree and the trapped organic matter. Measurements of individual phytoliths by Raman and synchrotron FTIR microspectroscopies in combination with multivariate analysis separated bilobate silica cells from prickles and long cells, based on the silica molecular structures and the fraction and composition of occluded organic matter. The variations in structure and composition of sorghum phytoliths suggest that the biological pathways leading to silica deposition vary between these cell types. KW - Phytoliths KW - Biosilicification KW - Raman KW - Sorghum KW - Solid state NMR KW - Synchrotron FTIR PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502672 DO - https://doi.org/10.3389/fpls.2019.01571 VL - 10 SP - 1571 PB - Frontiers Media CY - Lausanne AN - OPUS4-50267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lauschkin, Maik A1 - Bulling, Jannis A1 - Lugovtsova, Yevgeniya A1 - Wasmer, P. A1 - Prager, Jens T1 - Bestimmung von Materialparametern aus dem dispersiven Verhalten geführter Wellen mittels neuronaler Netze N2 - Damit eine Simulationsrechnung, beispielsweise mit einer FEM-Software, eine ausreichend hohe Genauigkeit erreicht, muss vorausgesetzt werden, dass die Modellparameter eine sehr hohe Güte aufweisen. Die genaue Kenntnis der Materialparameter ist dabei von besonderer Bedeutung. Um diese Parameter bestimmen zu können, müssen die verwendeten Werkstoffe messtechnisch charakterisiert werden. Neben anderen Ansätzen sind dafür akustische Verfahren im Ultraschallbereich geeignet. Für dünnwandige und plattenförmige Materialien können aus den sich ausbreitenden geführten Wellen messtechnisch Dispersionskurven bestimmt und aus diesen die Materialparameter abgeleitet werden. Da für die Signalverarbeitung und für Optimierungsaufgaben aktuell zunehmend Machine Learning Tools zum Einsatz kommen, stellt sich die Frage, ob diese Werkzeuge auch für die Ermittlung der Materialparameter aus den gemessenen Dispersionskurven eingesetzt werden können. In der vorgestellten Untersuchung soll ein Convolutional Neural Network aufgestellt werden, welches aus Dispersionsbildern Muster extrahiert und aus diesen eine Schätzung für die Materialparameter ermittelt. Um die Machbarkeit dieses Ansatzes zu prüfen, werden zunächst nur isotrope Materialien betrachtet. Für das Netz werden mit der Scaled-Boundary-Finite-Element-Methode synthetische Daten für das Trainieren und Validieren generiert. Zusätzlich werden die Hyperparameter des neuronalen Netzes variiert, um ein optimales Model für die Schätzung zu finden. Anschließend kann das Netz mit experimentellen Daten getestet und das Ergebnis hinsichtlich der Genauigkeit bewertet werden. T2 - DAGA 2020 - 46. Jahrestagung für Akustik CY - Meeting was canceled DA - 16.03.2020 KW - Machinelles Lernen KW - Geführte Ultraschallwellen KW - Materialcharakterisierung KW - Elastische Konstanten KW - Isotrope Materialien PY - 2020 SN - 978-3-939296-17-1 SP - 571 EP - 574 PB - Deutsche Gesellschaft für Akustik e.V. CY - Berlin AN - OPUS4-50765 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Galbacs, G. A1 - Keri, A. A1 - Kalomista, I. A1 - Kovacs-Szeles, E. A1 - Gornushkin, Igor B. T1 - Deuterium analysis by inductively coupled plasma mass spectrometry using polyatomic species: An experimental study supported by plasma chemistry modeling N2 - based on the use of the signal from hydrogen-containing polyatomic ions formed in the inductively coupled plasma. Prior to analytical experiments, a theoretical study was performed to assess the concentration of polyatomic species present in an equilibrium Ar-O-D-H plasma, as a function of temperature and stoichiometric composition. It was established that the highest sensitivity and linearity measurement of D concentration in a wide range can be achieved by monitoring the ions of D2 and ArD, at masses 4 and 42, respectively. Results of the calculations are in good agreement with the experiments. Signal stability, spectral interferences, as well as the effect of plasma parameters were also assessed. Under optimized conditions, the limit of detection (LOD) was found to be 3 ppm atom fraction for deuterium when measured as ArD (in calcium and potassium free water), or 78 ppm when measured as D2. The achieved LOD values and the 4 to 5 orders of magnitude dynamic range easily allow the measurement of deuterium concentrations at around or above the natural level, up to nearly 100% (or 1 Mio ppm) in a standard quadrupole ICP-MS instrument. An even better performance is expected from the method in high resolution ICP-MS instruments equipped with low dead volume sample introduction systems KW - ICP MS KW - Deuterium KW - Deuterium enriched water PY - 2020 DO - https://doi.org/10.1016/j.aca.2020.01.011 VL - 1104 SP - 28 EP - 37 PB - Elsevier B.V. AN - OPUS4-50777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tscheuschner, Georg A1 - Schwaar, Timm A1 - Weller, Michael G. T1 - Fast Confirmation of Antibody Identity by MALDI-TOF MS Fingerprints N2 - Thousands of antibodies for diagnostic and other analytical purposes are on the market. However, it is often difficult to identify duplicates, reagent changes, and to assign the correct original publications to an antibody. This slows down scientific progress and might even be a cause of irreproducible research and a waste of resources. Recently, activities were started to suggest the sole use of recombinant antibodies in combination with the open communication of their sequence. In this case, such uncertainties should be eliminated. Unfortunately, this approach seems to be rather a long-term vision since the development and manufacturing of recombinant antibodies remain quite expensive in the foreseeable future. Nearly all commercial antibody suppliers also may be reluctant to publish the sequence of their antibodies, since they fear counterfeiting. De novo sequencing of antibodies is also not feasible today for a reagent user without access to the hybridoma clone. Nevertheless, it seems to be crucial for any scientist to have the opportunity to identify an antibody undoubtedly to guarantee the traceability of any research activity using antibodies from a third party as a tool. For this purpose, we developed a method for the identification of antibodies based on a MALDI-TOF MS fingerprint. To circumvent lengthy denaturation, reduction, alkylation, and enzymatic digestion steps, the fragmentation was performed with a simple formic acid hydrolysis step. Eighty-nine unknown monoclonal antibodies were used for this study to examine the feasibility of this approach. Although the molecular assignment of peaks was rarely possible, antibodies could be easily recognized in a blinded test, simply from their mass-spectral fingerprint. A general protocol is given, which could be used without any optimization to generate fingerprints for a database. We want to propose that, in most scientific projects relying critically on antibody reagents, such a fingerprint should be established to prove and document the identity of the used antibodies, as well as to assign a specific reagent to a datasheet of a commercial supplier, public database record, or antibody ID. KW - Reproducibility KW - Quality Control KW - Traceability KW - Diagnostics KW - Hybridoma KW - Monoclonal Antibody KW - Recombinant Antibody PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506611 DO - https://doi.org/10.3390/antib9020008 SN - 2073-4468 VL - 9 IS - 2 SP - 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-50661 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Paul, Martin A1 - Weller, Michael G. T1 - Antibody screening by microarray technology – Direct identification of selective high-affinity clones N2 - The primary screening of hybridoma cells is a time-critical and laborious step during the development of monoclonal antibodies. Often critical errors occur in this phase, which supports the notion that the generation of monoclonal antibodies with hybridoma technology is difficult to control and hence a risky venture. We think that it is crucial to improve the screening process to eliminate most of the immanent deficits of the conventional approach. With this new microarray-based procedure, several advances could be achieved: Selectivity for excellent binders, high throughput, reproducible signals, avoidance of misleading avidity (multivalency) effects, and simultaneous performance of competition experiments. The latter can directly be used to select clones of desired cross-reactivity properties. In this paper, a model system with two excellent clones against carbamazepine, two weak clones and blank supernatant has been designed to examine the effectiveness of the new system. The excellent clones could be detected largely independent of the IgG concentration, which is unknown during the clone screening since the determination and subsequent adjustment of the antibody concentration is not possible in most cases. Furthermore, in this approach, the enrichment, isolation, and purification of IgG for characterization is not necessary. Raw cell culture supernatant can be used directly, even when fetal calf serum (FCS) or other complex media had been used. In addition, an improved method for the oriented antibody-immobilization on epoxy-silanized slides is presented. Based on the results of this model system, we conclude that this approach should be preferable to most other protocols leading to many of false positives, causing expensive and lengthy confirmation steps to weed out the poor clones. KW - Hybridoma KW - Monoclonal Antibodies KW - Clones KW - Competitive Immunoassay KW - Hapten Immunoassay KW - False Positives PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506621 DO - https://doi.org/10.20944/preprints201911.0023.v1 SN - 2310-287X SP - 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-50662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marquardt, Julien T1 - Investigating the morphology of nanostructured mixed metal oxides (Ir/TiOx) and its impact on the electrocatalytic OER-activity N2 - The electrocatalytic conversion of water into molecular hydrogen and oxygen under the utilization of excess renewable energies, such as wind power, photovoltaics and hydroelectric power is one possible pathway to establish a sustainable hydrogen economy. The obtained hydrogen is either stored and used in a fuel cell or consumed on-site in industrial applications. Water electrolysis systems (WES) are based on two half cell reactions, such as oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) which both proceed simultaneously. The OER suffers from slow reaction kinetics and thus limits the overall performance. The most promising compounds in acidic electrolysis are IrO2 and RuO2. Due to their rare abundance and extremely high price a wide use of acidic WES was prevented. Lowering the catalysts noble metal content by mixing iridium with titanium reduces the production costs. Thin films are produced by dip coating a solution of metal oxide precursors alongside with a polymer template dissolved in ethanol. The obtained samples are subsequently calcined to the remove the template and adjust crystallinity. Finally, an additional iridium deposition step was performed on the outer surface plane area. Understanding the influence of structural and morphological aspects on the OER-activity is beneficial to further optimize WES. The current presentation will thus give detailed insights to structural aspects obtained by Raman spectroscopy, small- and wide-angle X-ray scattering which are then combined with electrochemical parameters to deduce structure-activity relationships. T2 - Joint Polish-German Crystallographic Meeting 2020 CY - Wrocław, Poland DA - 24.02.2020 KW - nanostructured KW - electrocatalysis PY - 2020 AN - OPUS4-50664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baláž, M. A1 - Tešinský, M. A1 - Marquardt, Julien A1 - Škrobian, M. A1 - Daneu, N. A1 - Rajňák, M. A1 - Baláž, P. T1 - Synthesis of copper nanoparticles from refractory sulfides using a semi-industrial mechanochemical approach N2 - The large-scale mechanochemical reduction of binary sulfides chalcocite (Cu2S) and covellite (CuS) by elemental iron was investigated in this work. The reduction of Cu2S was almost complete after 360 min of milling, whereas in the case of CuS, a significant amount of non-reacted elemental iron could still be identified after 480 min. Upon application of more effective laboratory-scale planetary ball milling, it was possible to reach almost complete reduction of CuS. Longer milling leads to the formation of ternary sulfides and oxidation product, namely cuprospinel CuFe2O4. The rate constant calculated from the magnetometry measurements using a diffusion model for Cu2S and CuS reduction by iron in a large-scale mill is 0.056 min−0.5 and 0.037 min−0.5, respectively, whereas for the CuS reduction in a laboratory-scale mill, it is 0.1477 min−1. The nanocrystalline character of the samples was confirmed by TEM and XRD, as the produced Cu exhibited sizes up to 16 nm in all cases. The process can be easily scaled up and thus copper can be obtained much easier from refractory minerals than in traditional metallurgical approaches. KW - Mechanochemistry KW - Copper sulfides KW - Copper nanoparticles KW - Magnetometry KW - Oxidation PY - 2020 DO - https://doi.org/10.1016/j.apt.2019.11.032 VL - 31 IS - 2 SP - 782 EP - 791 PB - Elsevier B.V. AN - OPUS4-50665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Hirschberger, Paul A1 - Bartholmai, Matthias ED - Zemčík, R. ED - Krystek, J. T1 - Influence of rotor downwash on vertically displaced nanobots in flight N2 - One challenge associated with navigating a nano aerial robot swarm indoors in unstructured environments is, i.a., the limited air space. To avoid an over-regulation of the available indoor air space (e.g., prohibit copters to fly above each other), a safety region around each copter must be defined. In this paper, we investigate the impact of the downwash of a nano-drone on the stability of another nearby nano-drone. In the experiments, we found out that this downwash has a negative influence of a second nano-drone in a distance of around 1 m vertically and 0.2 m horizontally. Based on the obtained data, we developed a model describing the above-mentioned safety region to enable a safe operation of the swarm in these environments with fewer constraints. T2 - 36th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Pilsen, Czech Republic DA - 24.09.2019 KW - Mobile Robot Olfaction KW - Nano aerial robot KW - Swarm KW - Collision-free navigation KW - Safety region model PY - 2020 DO - https://doi.org/10.1016/j.matpr.2020.03.047 VL - 32 IS - 2 SP - 108 EP - 111 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-50673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brinker, U. A1 - Bērziņš, V. A1 - Ceriņa, A. A1 - Gerhards, G. A1 - Kalniņš, M. A1 - Schmölcke, U. A1 - Meinel, Dietmar A1 - Luebke, H. T1 - Two burials in a unique freshwater shell midden: insights into transformations of Stone Age hunter-fisher daily life in Latvia N2 - The Stone Age site Riņņukalns, Latvia, is the only well-stratified shell midden in the Eastern Baltic. In this paper, we present new interdisciplinary results concerning its dating, stratigraphy, features, and finds to shed light on the daily life of a fisher population prior to the introduction of domesticated animals. The undisturbed part of the midden consists of alternating layers of unburnt mussel shell, burnt mussel shell and fish bone, containing artefacts, some mammal and bird bones, and human burials. Two of them, an adult man and a baby, are discovered recently and date to the calibration plateau between 3350 and 3100 cal BC, and to the later 4th millennium, respectively. Stable isotopes suggest a diet based heavily on freshwater fish, and this is supported not only by ten thousands of identified fish remains, but also by a fish bone concentration nearby the skull of the man, which is interpreted as remain of a grave gift (possible fish soup). Of special interest are the baby’s stable isotope values. It shows that the mother’s diet was atypical (perhaps because she was non-local), and/or that dietary stress during pregnancy increased fractionation between the mother’s diet and her bloodstream KW - Baltic Stone Age KW - Palaeoanthropology PY - 2020 DO - https://doi.org/10.1007/s12520-020-01049-7 VL - 12 IS - 5 SP - Article number: 97 PB - Springer-Verlag GmbH CY - Germany AN - OPUS4-50653 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aratsu, K. A1 - Takeya, R. A1 - Pauw, Brian Richard A1 - Hollamby, M.J. A1 - Kitamoto, Y. A1 - Shimizu, N. A1 - Takagi, H. A1 - Haruki, R. A1 - Adachi, S. A1 - Yagai, S. T1 - Supramolecular copolymerization driven by integrative self-sorting of hydrogen-bonded rosettes N2 - Molecular recognition to preorganize noncovalently polymerizable supramolecular complexes is a characteristic process of natural supramolecular polymers, and such recognition processes allow for dynamic self-alteration, yielding complex polymer systems with extraordinarily high efficiency in their targeted function. We herein show an example of such molecular recognition-controlled kinetic assembly/disassembly processes within artificial supramolecular polymer systems using six-membered hydrogen-bonded supramolecular complexes (rosettes). Electron-rich and poor monomers are prepared that kinetically coassemble through a temperature-controlled protocol into amorphous coaggregates comprising a diverse mixture of rosettes. Over days, the electrostatic interaction between two monomers induces an integrative self-sorting of rosettes. While the electron-rich monomer inherently forms toroidal homopolymers, the additional electrostatic interaction that can also guide rosette association allows helicoidal growth of supramolecular copolymers that are comprised of an alternating array of two monomers. Upon heating, the helicoidal copolymers undergo a catastrophic transition into amorphous coaggregates via entropy-driven randomization of the monomers in the rosette. KW - Self-assembly KW - Coaggregation KW - Scattering KW - Simulation KW - AFM PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506555 DO - https://doi.org/10.1038/s41467-020-15422-6 VL - 11 IS - 1 SP - Article number: 1623 PB - Springer Nature AN - OPUS4-50655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Tscheuschner, Georg A1 - Schwaar, Timm A1 - Weller, Michael G. T1 - Fast Confirmation of Antibody Identity by MALDI-TOF-MS Fingerprints N2 - Thousands of antibodies for diagnostic and other analytical purposes are on the market. However, it is often difficult to identify duplicates, reagent changes, and to assign the correct original publications to an antibody. This slows down scientific progress and might even be a cause of irreproducible research and a waste of resources. Recently, activities were started to suggest the sole use of recombinant antibodies in combination with the open communication of their sequence. In this case, such uncertainties should be eliminated. Unfortunately, this approach seems to be rather a long-term vision since the development and manufacturing of recombinant antibodies remain quite expensive in the foreseeable future. Also, nearly all commercial antibody suppliers may be reluctant to publish the sequence of their antibodies, since they fear counterfeiting. De-novo sequencing of antibodies is also not feasible today for a reagent user without access to the hybridoma clone. Nevertheless, it seems to be crucial for any scientist to have the opportunity to identify an antibody undoubtedly to guarantee the traceability of any research activity using antibodies from a third party as a tool. For this purpose, we developed a method for the identification of antibodies based on a MALDI-TOF-MS fingerprint. To circumvent lengthy denaturation, reduction, alkylation, and enzymatic digestion steps, the fragmentation was performed with a simple formic acid hydrolysis step. Eighty-nine unknown monoclonal antibodies were used for this study to examine the feasibility of this approach. Although the molecular assignment of peaks was rarely possible, antibodies could be easily recognized in a blinded test, simply from their mass-spectral fingerprint. A general protocol is given, which could be used without any optimization to generate fingerprints for a database. We want to propose that in most scientific projects relying critically on antibody reagents, such a fingerprint should be established to prove and document the identity of the used antibodies and to assign a specific reagent to a datasheet of a commercial supplier, a public database record or an antibody ID. KW - Reproducibility KW - Quality Control KW - Traceability KW - Diagnostics KW - ELISA KW - Immunoassay PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506590 DO - https://doi.org/10.20944/preprints202002.0207.v1 SN - 2310-287X SP - 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-50659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Bernsmeier, D. A1 - Schmack, R. A1 - Häusler, I. A1 - Hertwig, Andreas A1 - Kraffert, K. A1 - Nissen, J. A1 - Kraehnert, R. T1 - Colloidal bimetallic platinum–ruthenium nanoparticles in ordered mesoporous carbon films as highly active electrocatalysts for the hydrogen evolution reaction N2 - Hydrogen features a very high specific energy density and is therefore a promising candidate for clean fuel from renewable resources. Water electrolysis can convert electrical energy into storable and transportable hydrogen gas. Under acidic conditions, platinum is the most active and stable monometallic catalyst for the hydrogen evolution reaction (HER). Yet, platinum is rare and needs to be used efficiently. Here, we report a synthesis concept for colloidal bimetallic platinum–ruthenium and rhodium–ruthenium nanoparticles (PtRuNP, RhRuNP) and their incorporation into ordered mesoporous carbon (OMC) films. The films exhibit high surface area, good electrical conductivity and well-dispersed nanoparticles inside the mesopores. The nanoparticles retain their size, crystallinity and composition during carbonization. In the hydrogen evolution reaction (HER), PtRuNP/OMC catalyst films show up to five times higher activity per Pt than Pt/C/Nafion® and PtRu/C/Nafion® reference catalysts. KW - Ordered mesoporous carbon KW - Bimetallic noble metal nanoparticles KW - Platinum-ruthenium colloid KW - Electrolysis KW - Hydrogen evolution reaction PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506868 DO - https://doi.org/10.1039/C9CY02285F SN - 2044-4753 VL - 10 IS - 7 SP - 2057 EP - 2068 PB - Royal Society of Chemistry AN - OPUS4-50686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittmann, Daniel A1 - Eisentraut, Paul A1 - Goedecke, Caroline A1 - Wiesner, Yosri A1 - Jekel, M A1 - Ruhl, A S A1 - Braun, Ulrike T1 - Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine N2 - The adsorption of organic micropollutants onto activated carbon is a favourable solution for the treatment of drinking water and wastewater. However, these adsorption processes are not sufficiently understood to allow for the appropriate prediction of removal processes. In this study, thermogravimetric analysis, alongside evolved gas analysis, is proposed for the characterisation of micropollutants adsorbed on activated carbon. Varying amounts of carbamazepine were adsorbed onto three different activated carbons, which were subsequently dried, and their thermal decomposition mechanisms examined. The discovery of 55 different pyrolysis products allowed differentiations to be made between specific adsorption sites and conditions. However, the same adsorption mechanisms were found for all samples, which were enhanced by inorganic constituents and oxygen containing surface groups. Furthermore, increasing the loadings led to the evolution of more hydrated decomposition products, whilst parts of the carbamazepine molecules were also integrated into the carbon structure. It was also found that the chemical composition, especially the degree of dehydration of the activated carbon, plays an important role in the adsorption of carbamazepine. Hence, it is thought that the adsorption sites may have a higher adsorption energy for specific adsorbates, when the activated carbon can then potentially increase its degree of graphitisation. KW - Aktivkohle KW - TED-GC/MS KW - Adsorption KW - Thermoanalytik PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506946 DO - https://doi.org/10.1038/s41598-020-63481-y VL - 10 IS - 1 SP - 6695 PB - Nature Publishing Group AN - OPUS4-50694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Annual report of sub commission V-A “Radiography-based weld inspection” N2 - Report on the annual activities of IIW commission V, Sub-Commission V-A "Radiography based weld inspection" chaired by Uwe Zscherpel, BAM Berlin T2 - 72. Annual Assembly of the International Institute of Welding 2019 CY - Bratislava, Slovakia DA - 07.07.2019 KW - International Institute of Welding KW - Sub-Commission V-A KW - Radiography based weld inspection PY - 2019 AN - OPUS4-50533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - X-ray back scatter techniques for additive manufacturing N2 - X-ray back scatter imaging is rarely applied compared to classical X-ray projection imaging. 20 years ago the company Philips developed “COMSCAN”, a first application case in the aircraft industry, which allowed even a depth resolution using back scatter imaging. The company AS&E in Boston offers back scatter imaging solutions for the security market. Their principle is to scan the object with a highly collimated X-ray needle beam from one side only and detect the backscattered radiation by a large area detector side by side with the collimation wheel. A new prototype is investigated at BAM for application and optimization in non-destructive testing. As modern industrial application field in-situ testing in additive manufacturing is targeted. The accessibility of the printed part during the production process is very limited. This prevent the application of a two sided X-ray inspection or Computed Tomography, were an rotation of the object is required to acquire projections from 360 degrees. An important advantage for the X-ray back scatter technique are also the materials used in additive manufacturing (polymers, ceramics, light metals like Aluminum or Titanium). These materials with lower density and lower Z values give better scatter signals than metals with higher densities and Z values. The back scatter intensity decreases with increasing density and Z value of the material. But the requirements on spatial resolution and contrast sensitivity are more stringent for non-destructive testing of additive manufactured parts compared to the security area. In NDT sizes of indications smaller than 1 mm have to be detected clearly. The investigation of these limits on a stateof-the-art prototype for X-ray back scattering using rotating collimated X-ray needle beams is a part of the BAM project “ProMoAM”. The contribution shows first results of the optimization for NDT and the achieved application limits for several example cases. T2 - 72. annual assembly of the international institute of welding 2019 CY - Bratislava, Slovakia DA - 07.07.2019 KW - Nondestructive tesing KW - X-ray back scattering KW - Additive manufacturing PY - 2019 AN - OPUS4-50534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Revision of ISO 24497 – NDT – Metal Magnetic Memory (MMM) N2 - The revision of ISO 24497:2007 started in 2017 (by decision of Com-V at the IIW annual assembly in Shanghai). After 3 years of discussions and incorporation of many comments from all over the world the working group C-V-E-b headed by Uwe Zscherpel finalized the work with a final draft to be forwarded for final vote at ISO TC 44. The working group C-V-E-b finalised the work and can be resolved. The chair thanks for all the successfully work done, the vote to forward the latest draft to ISO for final vote was done without any negative. T2 - 72. Annaul assebly of the international institute of welding CY - Bratislava, Slovakia DA - 07.07.2019 KW - International Institute of Welding KW - General Assembly KW - Revision of ISO 24497 KW - Metal Magnetic Memory PY - 2019 AN - OPUS4-50535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zscherpel, Uwe A1 - Ewert, Uwe T1 - Aktuelle Entwicklungen in der Standardisierung N2 - In den letzten zwei Jahren wurden 11 neue Standards/Standardrevisionen zur RT veröffentlicht (ohne Strahlenschutz) und 5 werden dafür gestrichen. Es wird über die neuen Anforderungen ausgewählter Normen bzw. Normrevisionen informiert und insbesondere auch über die veränderten Parameter, die bei Prüfpraxis und bei der Klassifizierung zu berücksichtigen sind. Das wichtigste Projekt ist die Revision der DIN EN ISO 17636-1, -2, RT von Schweißverbindungen, in ISO TC 44 SC 5 WG 1. Die Standards zur Schweißnahtprüfung in der Kerntechnik, DIN 25435, wurden ins Englische übertragen und bei ISO TC 85 SC 6 bearbeitet. Hauptaktivität bei ASTM ist gegenwärtig die Überarbeitung der CT-Standards und die Berücksichtigung der Anforderungen an das dimensionelle Messen. Der Guide ASTM E 1441 zur Bestimmung von MTF, Kontrast-Detail-Funktion (CDF) und Kontrast-Diskrimination-Diagramm (CDD) wird revidiert. E 2445 zur CR Long Term Stability wird ebenfalls revidiert. Die Revision soll auch in die ISO 16371-1 eingehen. Dazu ist ein Round Robin-Test geplant. Auch die Standards zur Durchstrahlungsprüfung auf Korrosion und Ablagerungen in Rohren mit Röntgen- und Gammastrahlen (EN 16407-1, -2, 2014) wurden revidiert. Diese Revision wurde als DIN EN ISO 20769-1, -2 2018 veröffentlicht und EN 16407 wird zurückgezogen. Die Revision der Standards EN 12543 und EN 12679 zur Messung der Brennfleckgröße und der Strahlergröße ist mit Verzögerung in Überarbeitung, um die digitalen Detektoren und Messmöglichkeiten mit Bildverarbeitungsprogrammen zu berücksichtigen. Ein Entwurf zur Messung der Brennfleckgröße von nano-Fokusröhren wird derzeit vom Europäischen Metrologie-Programm EMPIR gefördert. Zur radiographischen Gussteilprüfung wurde der Standard EN 12681 revidiert und 2018 veröffentlicht. Er wurde um Zulässigkeitsgrenzen erweitert und die digitale Radiographie wurde in Teil 2 berücksichtigt. T2 - 17. Seminar der DGZfP "Aktuelle Fragen der Durchstrahlungsprüfung und des Strahlenschutzes" CY - Kassel, Germany DA - 28.03.2019 KW - Digitale Radiographie KW - Standards KW - Bildqualität KW - Klassifizierung PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505371 UR - https://www.ndt.net/search/docs.php3?id=24807 VL - 24 IS - 12 SP - 1 EP - 5 PB - NDT.net CY - Kirchwald AN - OPUS4-50537 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Daniel A1 - Griepentrog, Michael A1 - Beck, Uwe A1 - Duwe, M. A1 - Quast, J.-H. A1 - Schneider, S. T1 - Effect of curvature of spherical microscopic indentations on the ellipsometric readout N2 - The authors describe and interpret curvature-related changes to the ellipsometric readout. As model system for a concave curvature, a set of three spherical microscopic indents in silicon (100) of different sizes was prepared by instrumented indentation testing using a spherical indenter. For reference, these samples were characterized by AFM to reveal the topography of each structure. The concavelike indents were analyzed by Mueller-Matrix imaging ellipsometry to extract lateral intensity images of 12 elements of the Mueller-Matrix. As a result of the detailed analysis of the image elements m22, m23, and m14, it was possible to correlate intensity changes and symmetry properties to depolarization and cross polarization induced by the edge threshold and the curved surface of the indent. KW - Spectroskopic Imaging KW - Mueller-Matrix imaging ellipsometry KW - Structural anomalies KW - Structural inhomogenities PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498105 DO - https://doi.org/10.1116/1.5122252 VL - 37 IS - 6 SP - 062906-1 EP - 062906-5 PB - American Vacuum Society AN - OPUS4-49810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Metz, Christian A1 - Franz, Philipp A1 - Fischer, C. A1 - Wachtendorf, Volker A1 - Maierhofer, Christiane T1 - Active thermography for quality assurance of 3D-printed polymer structures N2 - Additively manufactured test specimens made of polyamide 12 (PA 12) by Laser Sintering as well as of acrylonitrile butadiene styrene (ABS) by Fused Layer Modelling, were characterised with active thermography directly after manufacturing and after artificial weathering. For this, two different excitation methods (flash and pulse heating) were used and compared, regarding their suitability for the detection of constructed and imprinted defects inside the test specimens. To increase the quality of the thermograms, data processing methods like thermal signal reconstruction (TSR) and Fourier Transformation after TSR were applied. To further investigate the long-term stability of the additively manufactured test specimens towards environmental stress, like UV radiation, heat, humidity, water contact and frost with active thermography, an artificial weathering test over 2000 hours (~3 months) was applied to the specimens. The monitoring of the changes in the optical properties of the weathered plastics was supplemented by spectral reflectance and UV/VIS spectroscopy. KW - Additive manufacturing KW - Polymers KW - Artificial weathering KW - Active thermography KW - UV/VIS spectroscopy PY - 2019 DO - https://doi.org/10.1080/17686733.2019.1686896 SN - 1768-6733 (Print) 2116-7176 (Online) VL - 18 IS - 1 SP - 50 EP - 72 PB - Taylor & Francis AN - OPUS4-49817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Rosner, M. A1 - Henehan, M. J. A1 - Tütken, T. T1 - Triple Isotope Fractionation Exponents of Elements Measured by MC-ICP-MS - An Example of Mg N2 - In most chemical reactions, stable isotopes are fractionated in a mass-dependent manner, yielding correlated isotope ratios in elements with three or more stable isotopes. The proportionality between isotope ratios is set by the triple isotope fractionation exponent θ that can be determined precisely for, e.g., sulfur and oxygen by IRMS, but not for metal(loid) elements due to the lower precision of MC-ICP-MS analysis and smaller isotopic variations. Here, using Mg as a test case, we compute a complete metrologically robust uncertainty budget for apparent θ values and, with reference to this, present a new measurement Approach that reduces uncertainty on θ values by 30%. This approach, namely, direct educt-product bracketing (sample−sample bracketing), allows apparent θ values of metal(loid) isotopes to be determined precisely enough to distinguish slopes in three-isotope space. For the example of Mg, we assess appropriate quality Control standards for interference-to-signal ratios and Report apparent θ values of carbonate−seawater pairs. We determined apparent θ values for marine biogenic carbonates, where the foraminifera Globorotalia menardii yields 0.514 ± 0.005 (2 SD), the coral Porites, 0.515 ± 0.006 (2 SD), and two specimens of the giant clam Tridacna gigas, 0.508 ± 0.007 (2 SD) and 0.509 ± 0.006 (2 SD), documenting differences in the uptake pathway of Mg among marine calcifiers. The capability to measure apparent θ values more precisely adds a new dimension to metal(loid) δ values, with the potential to allow us to resolve different modes of fractionation in industrial and natural processes. KW - Isotope fractionation KW - Delta value KW - Biogenic carbonates KW - Calcification KW - Magnesium isotope ratios KW - Measurement uncertainty KW - Sample-sample bracketing PY - 2019 DO - https://doi.org/10.1021/acs.analchem.9b02699 VL - 91 IS - 22 SP - 14314 EP - 14322 PB - ACS Publications AN - OPUS4-49818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frielinghaus, H. A1 - Butler, P. D. A1 - Pauw, Brian Richard A1 - Rennie, A. R. T1 - Eleventh canSAS Meeting: International Cooperation and Collaboration in Small-Angle Scattering N2 - The eleventh canSAS workshop was held in Freising, Germany, July 8–10, 2019. These international meetings, promoting collective action for nomadic small-angle scatterers, have been taking place since 1998 and act as forums to catalyze cooperation amongst the SAS community in order to provide better facilities and equipment, combined with reliable data interpretation and analysis. The meeting attracted over 60 participants from major neutron and X-ray laboratories, as well as manufacturers of SAXS equipment, and users from academia and industry. There was also a wide geographical spread with participants from Australia, Asia, and North America joining European colleagues. T2 - canSAS XI CY - Freising, Germany DA - 08.07-2019 KW - Small angle scattering KW - Conference KW - Standardisation PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498192 DO - https://doi.org/10.1080/08940886.2019.1680215 SN - 0894-0886 SN - 1931-7344 VL - 32 IS - 6 SP - 48 EP - 49 PB - Taylor & Francis CY - Abingdon, UK AN - OPUS4-49819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona T1 - Introducing web mining of firm websites to explore innovation indicators using the example of management system standards N2 - Traditional innovation indicators often lack coverage, granularity as well as timeliness and involve high data collection costs, especially when conducted at a large scale. Based on the assumption that firms publish information about their products and services on their own websites, the Centre for European Economic Research in Mannheim (ZEW) has developed a framework to extract information from German firm websites applying Web Mining using a free-to-use web-scraping tool. Categorized as an intraorganizational procedural innovation, management system standards often lack research especially during the early stages of their diffusion mainly due to low data availability. Therefore, we introduce Web Mining to study the diffusion of the international management system standard ISO/IEC 27001 in Germany. Using the Mannheim Enterprise panel dataset, we first apply Web Mining to identify firms that refer to these and other common management system standards, followed by manual categorization. Second, we estimate a probit model to identify drivers for its implementation. Finally, we derive recommendations for policy makers. T2 - Collaborative research seminar series autumn 2019 CY - Linköping, Schweden DA - 26.11.2019 KW - Management System Standard KW - ISO/IEC 27001 KW - Information security KW - Web Mining PY - 2019 AN - OPUS4-49821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim T1 - Thermal Super Resolution Image Reconstruction Using Structured Laser Heating N2 - The separation of two closely located defects in fields of Thermographic NDE is very challenging. The diffusive nature of thermal waves leads to a fundamental limitation in spatial resolution. Therefore, super resolution image reconstruction can be used. The measured thermal waves can be transformed to virtual (ultrasound) waves that can be processed by applying ultrasound reconstruction algorithms and finally the super resolution algorithm. Otherwise, it is also possible to make use of a Fourier transform with a subsequent super resolution routine. These super resolution thermographic image reconstruction techniques in post-processing are discussed and evaluated regarding performance, accuracy and repeatability. T2 - 7th Autumn School METTI (Thermal Measurements and Inverse Techniques) CY - Porquerolles Island, Hyères, France DA - 29.09.2019 KW - Super resolution KW - Virtual wave KW - Laser thermography KW - VCSEL array KW - Joint sparsity KW - Compressed sensing PY - 2019 AN - OPUS4-49881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Xue, Boyang T1 - Ultrasound-Assisted Underwater Laser-induced Breakdown Spectroscopy with HighRepetition-Rate μJ-DPSS laser N2 - The elemental analysis of seawater is often critical to the understanding of marinechemistry, marine geochemistry, and the deep-sea ecosystems. Laser-induced breakdownspectroscopy (LIBS) with the advantage of rapid multi-elements detection, has a greatpotential for in-situ elemental analysis of seawater. In practice, it is crucial to create acompact, low cost and power saving instrument for the long-term deep-sea observation. Arecently appeared diode-pumped solid-state (DPSS) laser seems to be a promising candidateas it is both compact and robust. Additionally, its high repetition rate up to hundreds of kHzcan provide a considerable throughput for LIBS analysis. However, the DPSS lasers operateat moderate pulse energies, usually less than one mJ, which cannot sustain stablebreakdowns in bulk water. To ensure stable laser-induced plasmas underwater with such aμJ-DPSS laser, we introduced an ultrasound source to assist the breakdown process. Thephase interface and mass flow generated by the near-field ultrasound can greatly reduce thebreakdown threshold and enhance element-specific emissions. Meanwhile, the highrepetition-rate pulses can also improve the breakdown probability and generate uniqueemission lines originated from the water molecule. We further demonstrate that the highrepetition-rate DPSS laser combined with the Echelle spectrometer can provide effectivequantitative analysis for metal elements in bulk water. T2 - 10th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy CY - Brno, Czech Republic DA - 08.09.2019 KW - LIBS KW - Laser induced plasma KW - Plasma modeling KW - Plasma diagnostics KW - Underwater LIBS PY - 2019 AN - OPUS4-49769 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kepes, E. T1 - Tomography of asymmetrical laser-induced plasmas N2 - Asymmetrical laser-induced plasmas were investigated by a tomography approach based onthe inverse Radon transform. Two distinct sources of asymmetricity were investigated:double-pulsed laser-induced plasmas in the orthogonal configuration and single-pulsedlaser-induced plasmas under an inclined incidence angle. Both cases were observed atvarious delay times. The optical thinness of the laser-induced plasmas was achieved byappropriately adjusting the pulse energies. High temporal resolution was achieved by agated intensified charge-coupled-device camera. The asymmetrical laser-induced plasmaswere investigated in terms of their total emissivity, spectrally resolved emissivity, andtemperature. The latter was obtained by the Saha–Boltzmann plot method. The imagesrequired for the inverse Radon transform technique were obtained with a high angularaccuracy and reproducibility provided by mounting the spectrometer on a high-precisionnano-positioning rotary stage. The plasmas were induced in the center of rotation of thestage. This arrangement enabled the reconstruction of emissivity which was integrated overthe full spectral range (200–800 nm) or over a desired spectral range selected by a bandpassfilter (~10 nm). It also allowed for the reconstruction of spectrally-resolved emissivity ineach cross-sectional plasma slice by scanning the plasma across a spectrometer slit. The 3Dmaps of the temperature and electron density were thus obtained for different types ofasymmetric plasmas. The work will provide a more detailed description of the twoasymmetrical laser-induced plasmas. This might help with the development of LIBSinstrumentation using the orthogonal double-pulse geometry, or remote LIBS applicationswhich inherently rely on inclined-angle ablation. T2 - 10th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy CY - Brno, Czech Republic DA - 08.09.2019 KW - LIBS KW - Laser induced plasma KW - Plasma modeling KW - Plasma diagnostics PY - 2019 AN - OPUS4-49771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Palásti, David J. T1 - Optical modelling of spectroscopiccharacteristics of a dual-grating tunablespatial heterodyne LIBS spectrometer N2 - The spatial heterodyne spectrometer (SHS) concept, which is based on an interferometricoptical setup, boasts both the Fellgett and Jacquinot advantages. Theoretically it can provideboosted sensitivity and spectral resolution with respect to dispersion spectrometers in acompact, reasonably cheap arrangement without any moving components – this set ofcharacteristics can be attractive to a number of industrial, space and other field applications. The potential of SHS has already been demonstrated in IR and Raman spectroscopies(e.g.), and more recently also in LIBS. The scientific goal of our present project is toapply the SHS concept to the development of an optimized, but practical dual-grating,tunable SH-LIBS setup, which would possess appealing spectroscopic characteristics.During this development, we extensively rely on the computer-based simulation of theoptical setup, which is an efficient approach that we found to have been missing from earlierSHS efforts published. It can provide application-specific optimization of the SHS systemand predict the performance of the final system. In particular, we use optical simulation tostudy the effect of various important parameters on the relevant spectroscopic figures ofmerits of the system. We used the non-sequential ray-tracing mode of the Zemax/OpticStudio software for optical modelling of the SH-LIBS setup (Optical distortions were studiedin sequential mode). Characteristics of the setup and interferograms were calculated with atleast one million rays. All calculations were carried out for the visible spectral range(400-700 nm), using stepwise extension of monochromatic simulations with 5 nm steps.Wherever applicable, characteristic discrete visible wavelengths from the emissionspectrum of Hg discharge lamps (404.7 nm, 435.8 nm, 546.1 nm, 579.0 nm) were used for thecalculation of spectroscopy figures of merit and for the validation of simulation. T2 - 10th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy CY - Brno, Czech Republic DA - 08.09.2019 KW - Spatial Heterodyne Spectroscopy KW - Laser induced plasma KW - Plasma modeling KW - Plasma diagnostics KW - LIBS KW - Modeling PY - 2019 AN - OPUS4-49772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling equilibrium chemistry in laser induced plasmas and plasma chemical reactors N2 - A goal of this work is to apply the model, which was initially developed for laser induced plasmas, to plasmas used in chemical reactors, in particular, the inductively-coupled-RF discharge plasma. The model predicts equilibrium chemical compositions of reaction mixtures as functions of plasma temperature and stoichiometry of reactants. The mixtures investigated are BCl3/H2/Ar and BF3/H2/Ar where Ar serves as the plasma-forming gas and H2 as a binding agent which binds the active species Cl and F and Cl- and F-containing intermediates to produce gaseous B and its condensate. An additional goal is to obtain information about intermediate reaction products for different ratios of BCl3/H2 and BF3/H2 and at different temperatures and different Ar flow rates. Also, chemical reactions in laser induced plasmas (LIPs) created on calcium hydrate and calcium carbonate targets in argon are modeled. The results are compared with those obtained by means of the equilibrium model based on the minimization of Gibbs free energy. T2 - SciX 2019 CY - Palm Springs, USA DA - 13.10.2019 KW - LIBS KW - Laser induced plasma KW - Plasma modeling PY - 2019 AN - OPUS4-49774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Molecule formation in calcium carbonate and calcium hydroxide libs plasmas: model and experiment N2 - Analysis of calcium hydrate and calcium carbonate samples and their mixtures is important for archeology, anthropology, and geology. Laser-induced plasma spectroscopy (LIBS) is a suitable tool for such the analysis as it allows for in- and on-line real time chemical assays. LIBS is inherently a technique for atomic analysis; however, since recently, it is also used for molecular analysis. The information attained by the latter is mainly related to “secondary” chemistry that deals with re-association of atoms and ions into molecules at long delay times (≥10 μs) after the initial breakdown. Even though the direct information about the initial molecular content in the target may be lost, the molecular analysis by LIBS can still be useful to assess the composition of samples. In this work, chemical reactions in laser induced plasmas (LIPs) created on calcium hydrate and calcium carbonate targets in argon are modeled and compared to experiment. The model is based on the assumption that all ionization processes and chemical reactions are at local thermodynamic equilibrium. A chemical composition of argon-calcium-oxygen and argon-calcium-hydrogen plasmas is studied as a function of plasma temperature and pressure. It is established that more than twenty simple and composite molecules and ions can be formed in the course of chemical reactions. The results are compared with those obtained by means of the equilibrium model based on the minimization of Gibbs free energy. T2 - SciX 2019 CY - Palm Springs, USA DA - 13.10.2019 KW - Plasma diagnostics KW - LIBS KW - Laser induced plasma KW - Plasma modeling PY - 2019 AN - OPUS4-49775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Laser induced plasma as a chemical reactor: how feasible? N2 - A goal of this work is to apply the model, which was initially developed for laser induced plasmas, to plasmas used in chemical reactors, in particular, the inductively-coupled-RF discharge plasma. The model predicts equilibrium chemical compositions of reaction mixtures as functions of plasma temperature and stoichiometry of reactants. The mixtures investigated are BCl3/H2/Ar and BF3/H2/Ar where Ar serves as the plasma-forming gas and H2 as a binding agent which binds the active species Cl and F and Cl- and F-containing intermediates to produce gaseous B and its condensate. An additional goal is to obtain information about intermediate reaction products for different ratios of BCl3/H2 and BF3/H2 and at different temperatures and different Ar flow rates. Also, chemical reactions in laser induced plasmas (LIPs) created on calcium hydrate and calcium carbonate targets in argon are modeled. The results are compared with those obtained by means of the equilibrium model based on the minimization of Gibbs free energy. T2 - 1st workshop on Tandem LIBS/LA-ICP-MS CY - BAM, Berlin, Adlershof DA - 18.11.2019 KW - LIBS KW - Laser induced plasma KW - Plasma modeling KW - Plasma chemical reactor PY - 2019 AN - OPUS4-49776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Forschungsthemen im Bereich der ZfP mit akustischen und elektromagnetischen Methoden N2 - Die zerstörungsfreien Methoden zur Untersuchung und Charakterisierung von Materialien sowie zur Detektion von betriebsbedingten und herstellungsbedingten Fehlern mit akustischen und elektrischen Methoden werden vorgestellt. Schwerpunkt bilden die Ultraschall-, die Wirbelstrom- und die Streuflussprüfung. Die Verfahren werden anhand des Aufgabenspektrums des Fachbereiches 8.4 der BAM dargestellt. T2 - Lehrveranstaltung 0334 L 119 „Instrumentelle Analytik“ innerhalb des Moduls „Untersuchungsverfahren“ im Masterstudium des Studiengangs Werkstoffwissenschaften CY - BAM Berlin, Germany DA - 06.12.2019 KW - Ultraschallprüfung KW - Wirbelstromprüfung KW - Streuflussprüfung PY - 2019 AN - OPUS4-50014 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bäßler, Ralph T1 - Review: Physical Electrochemistry – Fundamentals, Techniques, and Applications N2 - The second edition of this textbook on physical electrochemistry, written by two experienced teachers of physical chemistry, corrosion engineering and materials science and engineering, covers the current knowledge which should be transferred to students of these fields. In 20 chapters the fundamentals of electrochemistry, the most important electrochemical measurement techniques and applications of electrochemistry are covered. It can be concluded that this study fulfills its intension of “serving as a key textbook in undergraduate courses” dealing with electrochemistry and being “a reference source for graduated students, researchers and engineers” interested in this field. Teachers will find sufficient content for preparing lectures on this topic. Even self‐learning is well supported by the clear structure, presented content and provided sources for further reading. KW - Corrosion KW - Electrochemistry PY - 2019 DO - https://doi.org/10.1002/maco.201970124 SN - 1521-4176 SN - 0947-5117 VL - 70 IS - 12 SP - 2345 EP - 2346 PB - WILEY‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope ratios and delta values with minimal measurement uncertainties -measuring magnesium using MC-ICP-MS N2 - Multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS) has evolved significantly since its introduction in 1992. The second and third generation instruments now allow isotope ratio measurements at unprecedented precisions, 0.001 % or better. However, precision alone is not enough for producing accurate and reliable isotope ratio measurements. Metrological considerations such as the selection of suitable calibration strategies, proper assessment of instrumental biases, and the estimation of overall measurement uncertainty remain critical to the measurement process. Properly assessed, measurement uncertainty then provides the interval within which a result can be considered both accurate and precise. All mass spectrometric measurements are affected by instrumental mass discrimination and produce isotope ratios that are biased relative to their “true” ratio. To produce accurate and traceable isotope ratio measurements, it is imperative that certified isotope reference materials (iCRMs) be used for calibration and validation purposes. iCRMs reporting absolute isotope ratios are an analyst’s first choice, particularly when its uncertainty is sufficient for the intended use. However, when smaller uncertainties are required to resolve subtle differences between samples, delta-scale measurements become important. Here, the difference between an isotope ratio measured in a sample and in an internationally accepted isotope reference material (iRM) is determined. This deviation can be positive or negative relative to the iRM, is called a delta value, and is often expressed in per mil units. This presentation will highlight the potential for MC-ICP-MS to produce isotope ratio measurements with minimal uncertainties by examining three applications involving Mg isotopes: 1) the certification of a set of iCRMs for their absolute isotope ratio using a gravimetric isotope mixture approach; 2) the comparison of these iCRMs with currently accepted Mg delta-scale reference materials through intercalibration, and 3) the determination of isotope fractionation exponents for geochemical applications. T2 - 4th International Conference on Frontiers in Mass Spectrometry CY - Kottayam, Kerala, India DA - 04.12.2019 KW - Triple isotope fractionation KW - Absolute isotope ratio KW - Delta value KW - Mangesium PY - 2019 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. AN - OPUS4-50004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Energy-dispersive X-ray spectroscopy (EDS) N2 - As one of the widely used analytical methods for the analysis of elemental composition of solid matter, energy dispersive X-ray spectroscopy (EDS) has recently gained significant importance regarding its application to the chemical analysis of nanoparticles, especially in conjunction with the use of a scanning electron microscope (SEM) and the use of the transmission operation mode of SEM (STEM-in-SEM). This development was mainly driven by the technological progress with highly sensitive EDS detectors, such that individual nanoparticles can be quickly inspected with EDS at a SEM. Qualitative information on elemental composition with about 10 nm spatial resolution can be achieved complementary to the high-resolution information of the sample surface morphology within the same scanned area as provided by the electron microscope. Representative examples with successful EDS analysis on nanoparticles are presented, but also limitations of the method are described. KW - EDS KW - EPMA KW - X-rays KW - SEM/EDS PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00021-3 SP - 397 EP - 417 PB - Elsevier CY - Amsterdam AN - OPUS4-49991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mech, A. A1 - Gaillard, C. A1 - Marvin, H. A1 - Wohlleben, W. A1 - Hodoroaba, Vasile-Dan A1 - Babick, F. A1 - Friedrich, C. M. A1 - Brüngel, R. A1 - Rückert, J. A1 - Ghanem, A. A1 - Weigel, S. T1 - The NanoDefine Decision Framework and NanoDefiner e-Tool: a practical guide to the identification of nanomaterials N2 - The European Commission's recommendation on the definition of nanomaterial [2011/696/EU] is broadly applicable across different regulatory sectors and requires the quantitative size Determination of constituent particles in samples down to 1 nm. A material is a nanomaterial if 50 % or more of the particles are in the size range 1-100 nm. The implementation of the definition in a regulatory context challenges measurement methods to reliably identify nanomaterials and ideally also nonnanomaterials as substance or product ingredient as well as in various matrices. The EU FP7 NanoDefine project [www.nanodefine.eu] addressed these challenges by developing a robust, readily implementable and cost-effective measurement strategy to decide for the widest possible range of materials whether it is a nanomaterial or not. It is based on existing and emerging particle measurement techniques evaluated against harmonized, material-dependent performance criteria and by intra- and inter-lab comparisons. Procedures were established to reliably measure the size of particles within 1-100 nm, and beyond, taking into account different shapes, coatings and chemical compositions in industrial materials and consumer products. Case studies prove their applicability for various sectors, including food, pigments and cosmetics. A main outcome is the establishment of an integrated tiered approach including rapid screening (Tier 1) and confirmatory methods (tier 2), a decision support flow scheme and a user manual to guide end-users, such as manufacturers, in selecting appropriate methods. Another main product is the “NanoDefiner” e-Tool which implements the flow scheme in a user-friendly software and guides the user in a semi-automated way through the entire decision procedure. It allows a cost-effective selection of appropriate methods for material classification according to the EC's nanomaterial definition and provides a comprehensive report with extensive explanation of all decision steps to arrive at a transparent identification of nanomaterials as well as non-nanomaterials for regulatory purposes. T2 - NanoWorkshop 2018: Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - Definition of nanomaterial KW - Regulation PY - 2019 SN - 978-3-95606-440-1 SN - 0179-0609 VL - F-61 SP - 114 EP - 124 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig und Berlin AN - OPUS4-49992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maurino, V. A1 - Pellutiè, L. A1 - Pellegrino, F. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Isopescu, R. T1 - Synthesis of size and shape controlled TiO2 nanoparticles: possible CRM’s candidates for size, shape and functional properties N2 - Titanium dioxide is one of the most studied metal oxides due to its chemical, surface, electronic and (photo)catalytic properties, providing this material of multisectorial applications ranging from healthcare, photocatalysis, smart materials with self cleaning and self sterilizing properties and solar energy harvesting. However it is difficult to correlate the functional properties of TiO2 nanomaterials to the properties at single nanoparticle level due to the high polydispersity in shape, size and surface features of the currently available TiO2 nanoparticles (NPs). Although intensive experimental and theoretical studies have been conducted on the reactivity of different surfaces of metal oxides such as TiO2 much less attention is paid on the dependence of functional properties, like photocatalytic activity, dye adsorption, open circuit potential and fill factor in dye sensitized solar cells, on crystal facets in different orientations. One of the goal of SETNanoMetro project was the development of design rules to tune crystal facets of TiO2 NPs in order to optimize and control functional properties. In the present work we have developed a series of design rules in order to obtain sets of anatase TiO2 NPs with low polydispersity and to tune their shape and size by hydrothermal processing of Ti(IV)- Triethanolamine complex in presence of different shape controllers. Through a careful experimental design, a predictive soft model was developed. The model is able to predict the synthesis outcome allowing to tune the shape factor from 5 (prisms) to 1.5 (bipyramids) to 0.2 (platelets). This allows to control the main crystal facets exposed ranging from (100) to (001). Due to the dependence of functional properties of nanomaterials on shape distribution and not only size, the availability of NPs sets with uniform and well defined and tunable shapes can be of paramount relevance in order to produce reference nanomaterials for shape measurement. T2 - NanoWorkshop 2018: Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - Anatase KW - shape control KW - Hydrothermal synthesis PY - 2019 SN - 978-3-95606-440-1 SN - 0179-0609 VL - F-61 SP - 146 EP - 162 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig und Berlin AN - OPUS4-49993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Faßbender, Sebastian T1 - On-line hyphenation of CE with multicollector-ICP-MS for species-specific isotopic analysis of sulfur N2 - In many scientific fields, isotopic analysis can offer valuable information, e.g., for tracing the origin of food products, environmental contaminants, forensic and archaeological samples (provenance determination), for age determination of minerals (geochronological dating) or for elucidating chemical processes. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement. In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared with data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was high enough to distinguish the rivers from one another by the isotopic signature of the river water sulfate. Next to environmental applications, a future field could be species-specific isotopic analysis of biomolecules, as sulfur is the only covalently bound constituent of proteins which can be analyzed by MC-ICP-MS. T2 - CE-Forum 2019 CY - Waldbronn, Germany DA - 11.12.2019 KW - Isotopic analysis KW - Multicollector-ICP-MS KW - Capillary electrophoresis KW - Hyphenated techniques KW - Speciation analysis PY - 2019 AN - OPUS4-50038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küchler, S. T1 - Zentrifugalkraftbasierte Mehrprobenprüfung in einer analytischen Zentrifuge zur Bestimmung von Kleb- und Haftfestigkeiten; Optimierung der Plasmaaktivierung von Polymeren N2 - Das Fügeverfahren Kleben bietet viele Vorteile, wie z.B. das Verbinden unterschiedlicher Materialklassen, geringe thermische Belastung (und damit ggf. verbundene Strukturveränderung/-schwächung) der Fügeteile und eine Lastverteilung über den gesamten Fügebereich. Die Auswahl an verfügbaren Klebstoffen und Vorbehandlungsoptionen sind dabei - wie die Applikationen auch - vielfältig. Es werden vier Applikationsbeispiele zu Referenzklebverbunden aus Edelstahl, zur Plasmaaktivierung von Niedrigenergie-Polymeren, zur Bestimmung der Haftfestigkeit von Lackierungen auf GFK und zur Wirkung von Primern vorgestellt. Einige Polymere weisen z.B. Eigenschaften auf, die eine Herstellung von festen und dauerhaft beanspruchbaren Kleb-verbindungen erschweren. Im Allgemeinen geht dies mit geringen Oberflächenenergien einher. Mittels Oberflächenvorbehandlung, z.B. durch Plasmafeinreinigung bzw. Plasmaaktivierung, können die Grenzflächen solcher Polymere - bezogen auf die Eignung als Fügeteile (Klebfestigkeit) oder als Substrat (Haftfestigkeit) – optimiert bzw. die Oberflächenenergie erhöht werden. Schnelle, zuverlässige und statistisch abgesicherte Prüfverfahren zur Ermittlung von Verbund-eigenschaften sind dabei unverzichtbar. T2 - 35. ak-adp Workshop: Haftung nach Maß – atmosphärische Plasmen für optimierte Adhäsion CY - Nuremberg, Germany DA - 20.11.2019 KW - Adhäsion KW - Mehrprobenprüfung KW - Analytische Zentrifuge KW - Kleb- und Haftfestigkeit PY - 2019 AN - OPUS4-50042 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ratassepp, M. T1 - Considering anisotropy in guided wave tomography for composite laminates N2 - Recently, various guided wave tomography algorithms have been developed to map structural changes from remote locations. The focus has been on structures made of isotropic materials and little work has been done on structures made of anisotropic materials. Primary complication to implement tomography in composite laminates is associated with the complex forward model to accurately simulate the 3-D guided wave propagation. In this study, we demonstrate that guided wave propagation can be approximated by an equivalent 2-D acoustic model. It is based on finite-difference discretization method in which the wave-field is parameterized by phase velocity and dimensionless anisotropic parameters. The reconstruction of defects is based on a full-waveform inversion algorithm and was implemented on the data obtained from finite element simulations. Results on a localized stiffness defects in composite plates with various layups demonstrate the attractiveness of the proposed methodology. T2 - International Symposium on Nondestructive Characterization of Materials (ISNCM 2019) CY - Portoroz, Slovenia DA - 17.09.2019 KW - Lamb waves KW - Ultrasonic Guided Waves KW - Multilayered structures PY - 2019 AN - OPUS4-50059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Magkos, Sotirios T1 - Advanced algorithms for image reconstruction in Computed Tomography N2 - This PhD project is part of the Marie Skłodowska-Curie International Training Network MUMMERING. The overarching goal of MUMMERING is the creation of a research tool that exploits the wealth of 3D imaging modalities applied in materials engineering. The focus of this work is advanced reconstruction algorithms. The primary objective is the development and implementation of the DIRECTT algorithm. Due to restrictions introduced by the sample or the imaging setup during a measurement, it is not always possible to acquire data that fulfil the Nyquist sampling criterion. The DIRECTT algorithm is intended to produce reconstructions of superior quality for such cases of limited data sets, compared to those of other available algorithms, such as algebraic iterative ones. Although DIRECTT has been developed primarily for the reconstruction of volumes from data acquired by an X-ray Computed Tomography scanner, it can also be applied to the different modalities, such as laminography. The talk describes the reconstruction principle of DIRECTT. Furthermore, reconstructions of measured data are presented and compared to reconstructions produced by other established algorithms. T2 - Doktorandenseminar CY - BAM Berlin, Germany DA - 16.12.2019 KW - Computed Tomography KW - Reconstruction KW - DIRECTT PY - 2019 AN - OPUS4-50066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Linberg, Kevin T1 - A Comparative Study of Ionic Cocrystals N2 - The mechanochemical formation of the ionic cocrystals of glucose (Glc) and sodium salts is presented. Products are formed by co-milling Glc with three sodium salts (NaCl, NaBr, NaI). The reaction pathways of the three ionic cocrystals were investigated using our tandem approach comprising a combination of in situ synchrotron powder X-ray diffraction and Raman spectroscopy. T2 - HZB User Meeting 2019 CY - Berlin, Germany DA - 04.12.2019 KW - In situ KW - Co-crystal KW - Mechanochemistry KW - Glucose PY - 2019 AN - OPUS4-50047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zimmermann, T. A1 - von der Au, Marcus A1 - Reese, A. A1 - Klein, O. A1 - Hildebrandt, L. A1 - Pröfrock, D. T1 - Substituting HF by HBF4 – an optimized digestion method for multi-elemental sediment analysis via ICP-MS/MS N2 - Determination of elemental mass fractions in sediments plays a major role in evaluating the environmental status of aquatic ecosystems. Herewith, the optimization of a new total digestion protocol and the subsequent analysis of 48 elements in different sediment reference materials (NIST SRM 2702, GBW 07313, GBW 07311 and JMC-2) based on ICP-MS/MS detection is presented. The developed method applies microwave acid digestion and utilizes HBF4 as fluoride source for silicate decomposition. Similar to established protocols based on HF, HBF4 ensures the dissolution of the silicate matrix, as well as other refractory oxides. As HBF4 is not acutely toxic; no special precautions have to be made and digests can be directly measured via ICP-MS without specific sample inlet systems, evaporation steps or the addition of e.g. H3BO3, in order to mask excess HF. Different acid mixtures with and without HBF4 were evaluated in terms of digestion efficiency based on the trace metal recovery. The optimized protocol (5 mL HNO3, 2 mL HCL, 1 mL HBF4) allows a complete dissolution of the analyzed reference materials, as well as quantitative recoveries for a wide variety of certified analytes. Low recoveries for e.g. Sr, Ba and rare earth elements due to fluoride precipitation of HF-based digestions protocols, can be avoided by the usage of HBF4 instead. Based on the usage of high purity HBF4 all relevant trace, as well as matrix elements can be analyzed with sufficiently low LOQs (0.002 μg L−1 for U up to 6.7 μg L−1 for Al). In total, 34 elements were within a recovery range of 80%–120% for all three analyzed reference materials GBW 07313, GBW 07311 and JMC-2. 14 elements were outside a recovery range of 80%–120% for at least one of the analyzed reference materials. KW - Reference Materials KW - Sediment KW - HF free Digestion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510480 DO - https://doi.org/10.1039/D0AY01049A SP - 1 EP - 10 PB - Royal Society of Chemistry AN - OPUS4-51048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lumpe, H. A1 - Menke, A. A1 - Haisch, C. A1 - Mayer, P. A1 - Kabelitz, Anke A1 - Yusenko, Kirill A1 - de Oliveira Guilherme Buzanich, Ana A1 - Block, T. A1 - Pöttgen, R. A1 - Emmerling, Franziska A1 - Daumann, L. J. T1 - The Earlier the Better: Structural Analysis and Separation of Lanthanides with Pyrroloquinoline Quinone N2 - Lanthanides (Ln) are critical raw materials, however, their mining and purification have a considerable negative environmental impact and sustainable recycling and separation strategies for these elements are needed. In this study, the precipitation and solubility behavior of Ln complexes with pyrroloquinoline quinone (PQQ), the cofactor of recently discovered lanthanide (Ln) dependent methanol Dehydrogenase (MDH) enzymes, is presented. In this context, the molecular structure of a biorelevant europium PQQ complex was for the first time elucidated outside a protein environment. The complex crystallizes as an inversion symmetric dimer, Eu2PQQ2, with binding of Eu in the biologically relevant pocket of PQQ. LnPQQ and Ln1Ln2PQQ complexes were characterized by using inductively coupled Plasma mass spectrometry (ICP-MS), infrared (IR) spectroscopy, 151Eu-Mössbauer spectroscopy, X-ray total scattering, and Extended X-ray absorption fine structure (EXAFS). It is shown that a natural enzymatic cofactor is capable to achieve Separation by precipitation of the notoriously similar, and thus difficult to separate, lanthanides to some extent. KW - Lanthanides KW - Structural Analysis KW - Separation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510821 DO - https://doi.org/10.1002/chem.202002653 SN - 0947-6539 VL - 26 SP - 1 EP - 8 PB - WILEY-VCH Verlag GmbH & co. KGaA AN - OPUS4-51082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Raschpichler, C. A1 - Goroncy, C. A1 - Langer, B. A1 - Antonsson, E. A1 - Wassermann, B. A1 - Graf, C. A1 - Klack, Patrick A1 - Lischke, T. A1 - Rühl, E. T1 - Surface Properties and Porosity of Silica Particles Studied by Wide-Angle Soft X-ray Scattering N2 - Wide-angle soft X-ray scattering on free silica particles of different porosity prepared in a beam is reported. The explored q region is mostly dominated by features due to surface roughness and bulk porosity. A comprehensive experimental and theoretical analysis of silica particles of different porosity is presented for various incident photon energies. A correlation analysis, based on the theory of Porod, is used to test the validity of exact Mie theory in different pore density limits. The ability of the discrete dipole scattering model (DDSCAT) to resolve local effects, caused by various pore distributions, is discussed. Characteristic differences between the soft X-ray scattering patterns of the particle samples of different surface properties and porosity are detected. For all mentioned cases, it was confirmed that the effective radius concept of the Guinier model can be successfully extended to Mie theory and DDSCAT in describing the additive contributions of the primary particles, including a thin inhomogeneous solvent-rich surface shell and empty bulk pores. Close agreement, within ±15%, between the calculated and observed pore sizes and porosity values is reached. The influence of pores is alternatively described either in terms of secondary Mie scattering, which is modulated by the local internal electrical field within the particles, or by an independent Mie scattering process induced by the incident field on isolated pores. It is found that for the typical pore/particle size ratios the latter approach presents the best choice. KW - Wide-Angle Soft X‑ray Scattering KW - Silica KW - Porosity PY - 2020 DO - https://doi.org/10.1021/acs.jpcc.0c04308 SN - 1932-7447 SN - 1932-7455 VL - 124 SP - 16663 EP - 16674 AN - OPUS4-51089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mech, A. A1 - Wohlleben, W. A1 - Ghanem, A. A1 - Hodoroaba, Vasile-Dan A1 - Weigel, S. A1 - Babick, F. A1 - Brüngel, R. A1 - Friedrich, C. M. A1 - Rasmussen, K. A1 - Rauscher, H. T1 - Nano or Not Nano? A Structured Approach for Identifying Nanomaterials According to the European Commission’s Definition N2 - Identifying nanomaterials (NMs) according to European Union Legislation is challenging, as there is an enormous variety of materials, with different physico-chemical properties. The NanoDefiner Framework and its Decision Support Flow Scheme (DSFS) allow choosing the optimal method to measure the particle size distribution by matching the material properties and the performance of the particular measurement techniques. The DSFS leads to a reliable and economic decision whether a material is an NM or not based on scientific criteria and respecting regulatory requirements. The DSFS starts beyond regulatory requirements by identifying non-NMs by a proxy Approach based on their volume-specific surface area. In a second step, it identifies NMs. The DSFS is tested on real-world materials and is implemented in an e-tool. The DSFS is compared with a decision flowchart of the European Commission’s (EC) Joint Research Centre (JRC), which rigorously follows the explicit criteria of the EC NM definition with the focus on identifying NMs, and non-NMs are identified by exclusion. The two approaches build on the same scientific basis and measurement methods, but start from opposite ends: the JRC Flowchart starts by identifying NMs, whereas the NanoDefiner Framework first identifies non-NMs. KW - Classification KW - Definition KW - Identification KW - Nanomaterials KW - Particle size KW - Regulation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510917 DO - https://doi.org/10.1002/smll.202002228 SN - 1613-6829 SP - 2002228-1 EP - 2002228-16 PB - Wiley-VCH CY - Weinheim AN - OPUS4-51091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gauert, C. A1 - Schannor, M. A1 - Hecht, L. A1 - Radtke, Martin A1 - Reinholz, Uwe T1 - A comparison of in situ analytical methods for trace element measurement in gold samples from various South African gold deposits N2 - Trace element concentrations in gold grains from various geological units in South Africa were measured in situ by field emission-electron probe microanalysis (FE-EPMA), laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and synchrotron micro X-ray fluorescence spectroscopy (SR-µ-XRF). This study assesses the accuracy, precision and detection limits of these mostly non-destructive analytical methods using certified reference materials and discusses their application in natural sample measurement. FE-EPMA point analyses yielded reproducible and discernible concentrations for Au and trace concentrations of S, Cu, Ti, Hg, Fe and Ni, with detection limits well below the actual concentrations in the gold. LA-ICP-MS analyses required larger gold particles (> 60 µm) to avoid contamination during measurement. Elements that measured above detection limits included Ag, Cu, Ti, Fe, Pt, Pd, Mn, Cr, Ni, Sn, Hg, Pb, As and Te, which can be used for geochemical characterisation and gold fingerprinting. Although LA-ICP-MS measurements had lower detection limits, precision was lower than FE-EPMA and SR-µ-XRF. The higher variability in absolute values measured by LA-ICP-MS, possibly due to micro-inclusions, had to be critically assessed. Non-destructive point analyses of gold alloys by SR-µ-XRF revealed Ag, Fe, Cu, Ni, Pb, Ti, Sb, U, Cr, Co, As, Y and Zr in the various gold samples. Detection limits were mostly lower than those for elements measured by FE-EPMA, but higher than those for elements measured by LA-ICP-MS. N2 - Les concentrations en éléments traces de grains d'or provenant de différentes unités géologiques d'Afrique du Sud ont été mesurées in situ par microsonde électronique à émission de champ (FE-EPMA), spectrométrie de masse couplée à une source plasma et un système d'ablation laser (LA-ICP-MS) et micro spectroscopie de fluorescence des rayons X au Synchrotron (SR-µ-XRF). Cette étude évalue l'exactitude, la précision et les limites de détection de ces méthodes d'analyse pour la plupart non-destructives en utilisant des matériaux de référence certifiés, et discute de leur application dans les mesures sur échantillon naturel. Les points d'analyses FE-EPMA ont fournis des concentrations reproductibles et discernables pour l'Au et des concentrations en traces de S, Cu, Ti, Hg, Fe et Ni, avec des limites de détection bien inférieures aux concentrations réelles dans l'or. Les analyses LA-ICP-MS ont nécessitées des particules d'or de plus grande taille (> 60 µm) pour éviter toute contamination pendant la mesure. Les éléments mesurés au-dessus des limites de détection inclus Ag, Cu, Ti, Fe, Pt, Pd, Mn, Cr, Ni, Sn, Hg, Pb, A et Te, qui peuvent être utilisés pour les caractérisations géochimique et le «fingerprinting» de l'or. Bien que les mesures LA-ICP-MS aient des limites de détection plus basses, la précision est inférieure par rapport à celles de la microsonde FE et de la SR-µ-XRF. La plus grande variabilité des valeurs absolues mesurées par LA-ICP-MS, probablement reliée à la présence de micro-inclusions, a du être évaluée de manière critique. Les points d'analyse non-destructifs des alliages d'or par SR-µ-XRF ont révélés la présence de Ag, Fe, Cu, Ni, Pb, Ti, Sb, U, Cr, Co, As, Y et Zr dans les différents échantillons. Les limites de détection ont été pour la plupart inférieures à celles des éléments mesurés par FE-EPMA, mais supérieures à celles des éléments mesurés par LA-ICP-MS. KW - Trace elements KW - Gold KW - FE-EPMA KW - LA-ICP-MS KW - SR-µ-XRF KW - Precision KW - Précision KW - Comparison of techniques KW - Éléments traces PY - 2016 DO - https://doi.org/10.1111/j.1751-908X.2015.00362.x SN - 1639-4488 SN - 1751-908X VL - 40 IS - 2 SP - 267 EP - 289 PB - Blackwell CY - Oxford AN - OPUS4-34882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lehmann, Jens A1 - Burkert, Andreas T1 - KorroPad - Beurteilung der Korrosionsbeständigkeit von Oberflächen nichtrostender Stähle N2 - Mit dem KorroPad Verfahren ist es dem Anwender möglich den Zustand der Passivschicht nichtrostender Stähle auf sehr einfache und schnelle Weise einschätzen zu können. Das Verfahren eignet sich dazu, den Grad der Passivität in Abhängigkeit der Umgebungsbedingungen und der Zeit nachzuvollziehen. Dies ermöglicht dem Anwender und Verarbeiter von nichtrostenden Stählen, die Lagerungsbedingungen und –zeiten einer frisch bearbeiteten Stahloberfläche zu ermitteln, welche für die Ausbildung einer stabilen Passivschicht notwendig sind, bevor diese risikoarm eingesetzt werden kann. Wie die hier dargestellten Beispiele und auch weitere zahlreiche praktische Anwendungen gezeigt haben, eignet sich das KorroPad ebenfalls für die Identifikation kritischer Prozessparameter bei der Verarbeitung nichtrostender Stähle. Mit dem Verfahren lassen sich viele prozessbedingte Einflussfaktoren auf die Oberflächengüte wie auch auf den Werkstoff charakterisieren. Aufgrund der schnellen und einfachen Auswertung der Prüfergebnisse können positive wie auch negative Veränderungen hinsichtlich der Passivschichtstabilität zügig erkannt werden. Dies ermöglicht es dem Anwender schnell zu reagieren, um kritische Einflüsse zu korrigieren und um eine Optimierung von Inhouse-Prozessen durchzuführen. Weitere Einsatzgebiete sind im Bereich der Wareneingangs- und/oder Warenausgangskontrolle denkbar, überall wo es um die Frage der Passivschichtstabilität einer nichtrostenden Stahloberfläche geht. T2 - Fachtagung Bauwerksdiagnose - Praktische Anwendungen Zerstörungsfreier Prüfungen und Zukunftsaufgaben CY - Berlin, Germany DA - 25.02.2016 KW - Korrosionsschnelltest, Nichtrostender Stahl, Passivschicht, KorroPad PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355146 SN - 978-3-940283-77-1 VL - 157 SP - 1 EP - 7 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-35514 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Schienenprüfung mit Wirbelstrom N2 - Ausgehend von einer Machbarkeitsstudie im Jahr 1999 wurde von der BAM in Zusammenarbeit mit der DB AG und verschiedenen anderen Partnern ein Schienenprüfsystem zur Detektion und Bewertung von Schienenfehlern des Typs Head Checks entwickelt. Dieses Prüfsystem arbeitet nach dem Wirbelstromprinzip. Die Firma Prüftechnik Linke & Rühe GmbH aus Magdeburg fertigt und vertreibt seit geraumer Zeit verschiedene manuelle und zuggestützte Prüfsysteme, die auf dieser Entwicklung basieren. Seit Januar 2013 wird in Deutschland der Qualitätsnachweis nach der Schienenbearbeitung mittels Wirbelstromprüfung gefordert. Im Laufe der Entwicklungsarbeiten wurden verschiedentlich benachbarte Themenfelder rund um die Prüfung auf Head Checks gestreift. Der Schwerpunkt dieses Vortrages liegt auf diesen erweiterten Möglichkeiten der magnetinduktiven Prüfung von verlegten Schienen. Hierbei wird sowohl auf die Verbesserung der Möglichkeiten des bestehenden Systems (z. B. durch Kopplung mit anderen Prüfverfahren) als auch auf mögliche Neuentwicklungen (z. B. durch Einsatz neuer Sensorik) eingegangen. Angestrebte Ziele sind z. B. die Verbesserung der Prüfaussage bei der Head Check Prüfung, Erweiterung der Prüfaussage auf andere Schienenfehlertypen oder die Bestimmung von Schieneneigenschaften wie Härte und Rauigkeit. T2 - ZfP im Eisenbahnwesen CY - Wittenberge DA - 15.03.2016 KW - Schienenprüfung KW - Wirbelstromprüfung KW - Zerstörungsfreie Prüfung PY - 2016 AN - OPUS4-35516 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steinkönig, J. A1 - Bloesser, F. R. A1 - Huber, B. A1 - Welle, A. A1 - Trouillet, V. A1 - Weidner, Steffen A1 - Barner, L. A1 - Roesky, P. W. A1 - Yuan, J. A1 - Goldmann, A. S. A1 - Barner-Kowollik, C. T1 - Controlled radical polymerization and in-depth mass-spectrometric characterization of poly(ionic liquid)s and their photopatterning on surfaces N2 - The preparation and characterization of poly(ionic liquid)s (PILs) bearing a polystyrene backbone via reversible addition fragmentation chain transfer (RAFT) polymerization and their photolithographic patterning on silicon wafers is reported. The controlled radical polymerization of the styrenic ionic liquid (IL) monomers ([BVBIM]X, X = Cl− or Tf2N−) by RAFT polymerization is investigated in detail. We provide a general synthetic tool to access this class of PILs with controlled molecular weight and relatively narrow molecular weight distribution (2000 g mol−1 ≤ Mn ≤ 10 000 g mol−1 with dispersities between 1.4 and 1.3 for p([BVBIM]Cl); 2100 g mol−1 ≤ MP ≤ 14 000 g mol−1 for p([BVBIM]Tf2N)). More importantly, we provide an in-depth characterization of the PILs and demonstrate a detailed mass spectrometric analysis via matrix-assisted laser desorption ionization (MALDI) as well as – for the first time for PILs – electrospray ionization mass spectrometry (ESI-MS). Importantly, p([BVBIM]Cl) and p([DMVBIM]Tf2N) were photochemically patterned on silicon wafers. Therefore, a RAFT agent carrying a photoactive group based on ortho-quinodimethane chemistry – more precisely photoenol chemistry – was photochemically linked for subsequent controlled radical polymerization of [BVBIM]Cl and [DMVBIM]Tf2N. The successful spatially-resolved photografting is evidenced by surface-sensitive characterization methods such as X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The presented method allows for the functionalization of diverse surfaces with poly(ionic liquid)s. KW - reversible addition fragmentation chain transfer (RAFT) polymerization KW - polyionic liquids KW - mass spectrometry KW - surface modification PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355202 DO - https://doi.org/10.1039/C5PY01320H VL - 7 SP - 451 EP - 461 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-35520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stroh, Julia T1 - In situ Untersuchungen von Hydratations- und Schädigungsmechanismen an Baustoffen N2 - In diesem Vortrag werden hochauflösende analytische Methoden für die Untersuchungen von zementgebundenen Baustoffen vorgestellt. Zum einen werden frühe Hydratationsprozesse in situ und mit hoher Zeitauflösung untersucht und die Einflüsse von polymeren Fließmittel und Stabilisierer auf die Erstarrungsverzögerung beobachtet. Zum anderen werden Phasenübergänge unter schädigenden Angriffen im Gefügeprofil auf µm-Skala verfolgt. Die Möglichkeit die Auswirkungen der niedrigen realen Konzentrationen von schädigenden Agenten zu identifizieren stellt ein großes Potential für die Schädigungsanalyse unter realen Bedingungen dar. Insgesamt haben die vorgestelletn analytischen Techniken ein großes Potential für die Analyse der Phasenentwicklung in zementgebundenen Baustoffen. T2 - Gemeinsamer Workshop der Sektion Angewandte Mineralogie in Umwelt & Technik und der Sektion Chemie, Physik und Kristallographie der Minerale von der Deutschen Mineralogischen Gesellschaft CY - Bad Windsheim, Germany DA - 24.02.2016 KW - Portlandzement KW - Hydratation KW - Additive KW - Schädigung KW - komplexe Angriffe PY - 2016 AN - OPUS4-35469 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stroh, Julia T1 - High resolution in situ monitoring of the initial cement hydration influenced by organic admixtures N2 - Numerous admixtures are used in the building practice to customize the properties of the cement paste during application. The influences of admixtures on the course of cement hydration and formation of hydrate phases have to be considered. Polycarboxylate ether (PCE) based polymeric superplasticizers (SPs) are known to retard the setting of the cement paste. The extent of the retardation differs depending on the molecular structure of the SP. Additionally, the presence of a stabilizing agent (SA) in the cement paste has a retarding side effect on the setting. The initial cement hydration processes and the detailed mechanisms of the retardation influenced by PCEs, as well as their interactions with particular SAs, are insufficiently understood. Up to now, only the results of phenomenological studies were taken into account to describe this retardation process. A detailed structure analysis monitoring the change of the phase composition during the hydration was never applied. Both SP and SA affect the adsorption of the sulphate ions on the clinker particles, causing changes in the formation of ettringite during the initial hydration, and are therefore a crucial part of the setting process itself. Here, the initial hydration of cement influenced by the interaction of SP and SA was monitored in situ by synchrotron X-ray diffraction. The high time resolution of the measurements allowed a continuous detection of the hydrates formed. The hydration was followed from the starting point of water addition and for couple of hours afterwards. The hydration of the levitated cement pellets containing starch as SA was initialized by adding aqueous solutions of different commercial SPs. Changes in the ettringite formation were detected in comparison to the reference hydration of pure cement. T2 - Early Age Concrete: From the Research Lab to the Construction Site CY - Tomsk, Russia DA - 02.06.2015 KW - Portland cement KW - Initial hydration KW - Superplasticizer KW - Stabilizer KW - Synchrotron XRD PY - 2015 AN - OPUS4-35470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Myrach, Philipp A1 - Maierhofer, Christiane A1 - Rahammer, M. A1 - Kreutzbruck, Marc T1 - Parameters in lock-in thermography of CFRP laminates N2 - Active thermography with lock-in excitation is a non-destructive testing method that is also feasible for testing of carbon fiber reinforced polymers (CFRP). For validating the method extensive investigations were done during a research project in order to advance a standardization process. The most important parameters of optical and ultrasonic excitation thermography were investigated. For example, the appropriate selection of spectral sensitivity of the used infrared camera systems is important for recording undisturbed thermal signals. Regarding excitation, influences of excitation power and ultrasonic frequency were studied. Furthermore, material parameters such as CFRP layup are known for strongly affecting the results of measurement. KW - Standardisierung KW - Lock-in thermography KW - Lock-in Thermografie KW - CFRP KW - CFK KW - optical excitation KW - ultrasonic excitation KW - Ultraschall KW - standardization PY - 2016 DO - https://doi.org/10.3139/120.110814 SN - 0025-5300 VL - 58 IS - 1 SP - 31 EP - 35 PB - Carl Hanser Verlag CY - München AN - OPUS4-35479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jonietz, Florian A1 - Myrach, Philipp A1 - Suwala, H. A1 - Ziegler, Mathias T1 - Examination of Spot Welded Joints with Active Thermography N2 - The method described here allows to determine the size of the thermal contact between two metal sheets joined by spot welding. This size is a measure for the size of the weld nugget, i.e. the zone melted during the welding process, and thus the quality of the welded joint. The method applies active thermography in transmission or reflection setup. Especially the reflection setup offers an attractive possibility for non-destructive testing when components can be accessed from one side only. The spot weld region is optically heated by laser or flash light radiation. The weld nugget provides the mechanical joint, but also constitutes a thermal bridge between the two welded sheets. The latter will be exploited in this method. The better thermal contact at the weld Nugget contrasts with the surrounding material, where the heat transfer between the two sheets is comparatively low. A major advantage of the described method is the applicability on sheets without any surface treatment. This is achieved by a proper normalization of the data, allowing for a correction of the varying surface emissivity. KW - Active thermography KW - Spot weld KW - Automotive industry PY - 2016 UR - http://link.springer.com/article/10.1007/s10921-015-0318-4?wt_mc=internal.event.1.SEM.ArticleAuthorIncrementalIssue DO - https://doi.org/10.1007/s10921-015-0318-4 VL - 35:1 SP - 1 EP - 14 PB - Springer CY - New York AN - OPUS4-35480 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Helmecke, E. A1 - Fleßner, M. A1 - Kaufmann, M. A1 - Staude, Andreas A1 - Hausotte, T. T1 - Numerical measurement uncertainty determination for dimensional measurements of microparts with CT N2 - Up to now, the only standardized method to determine the measurement uncertainty for computed tomography (CT) is to use calibrated workpieces as specified in the Guideline VDI/VDE 2630 Part 2.1. This paper discusses a promising numerical method for uncertainty determination with help of a virtual metrological CT (VMCT). It gives an explanation of the adjustments, the input parameters and the execution of the simulation. Furthermore, it discusses the first results of uncertainty determination compared to the method of using calibrated workpieces with the aid of two example cases. T2 - 6th Conference on Industrial Computed Tomography (iCT) CY - Wels, Austria DA - 09.02.2016 KW - simulation KW - Simulation KW - Computertomographie KW - Dimensionelle Metrologie KW - Normung KW - numerische Messunsicherheitsbestimmung KW - computed tomography KW - dimensional metrology KW - standardization KW - numerical uncertainty determination PY - 2016 UR - http://www.ndt.net/article/ctc2016/papers/ICT2016_paper_id17.pdf SP - Paper ID17, 1 EP - 7 AN - OPUS4-35481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Burkert, Andreas A1 - Mietz, Jürgen T1 - Investigations proofing the passive layer stability of stainless steels N2 - The presented investigations have proved the principal suitability of the KorroPad method to assess the passive layer stability of stainless steels. The electrochemical mode of action could be described in detail and limitations of the applicability have been demonstrated. The influence of different surface finishes has been investigated and verified by known methods for describing corrosion resistances. As a result, the increased corrosion susceptibility of two ground surfaces has been detected, but also the corrosion resistance of further surface finishes could be confirmed. KW - Stainless steel KW - KorroPad KW - Passive layer PY - 2016 DO - https://doi.org/10.1002/maco.201408202 VL - 1 IS - 67 SP - 84 EP - 91 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-35545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmack, R. A1 - Eckhardt, B. A1 - Koch, G. A1 - Ortel, Erik A1 - Kraehnert, R. T1 - ZnO coatings with controlled pore size, crystallinity and electrical conductivity N2 - Zinc oxide is a wide bandgap semiconductor with unique optical, electrical and catalytic properties. Many of its practical applications rely on the materials pore structure, crystallinity and electrical conductivity. We report a synthesis method for ZnO films with ordered mesopore structure and tuneable crystallinity and electrical conductivity. The synthesis relies on dip-coating of solutions containing micelles of an amphiphilic block copolymer and complexes of Zn2+ ions with aliphatic ligands. A subsequent calcination at 400 °C removes the template and induces crystallization of the pore walls. The pore structure is controlled by the template polymer, whereas the aliphatic ligands control the crystallinity of the pore walls. Complexes with a higher thermal stability result in ZnO films with a higher content of residual carbon, smaller ZnO crystals and therefore lower electrical conductivity. The paper discusses the ability of different types of ligands to assist in the synthesis of mesoporous ZnO and relates the structure and thermal stability of the precursor complexes to the crystallinity and electrical conductivity of the zinc oxide. KW - conductivity KW - EISA KW - pore templating KW - pore size control KW - ligands KW - zinc oxide PY - 2016 DO - https://doi.org/10.5755/j01.ms.22.1.8634 SN - 1392–1320 VL - 22 IS - 1 SP - 74 EP - 81 PB - Kaunas University of Technology, Lithuania AN - OPUS4-35550 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 21. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik. KW - Eignungsprüfung KW - Boden KW - PAK KW - MKW KW - Spurenelemente KW - Gesamtcyanid KW - Proficiency testing KW - Soil KW - PAH KW - TPH KW - Trace elements KW - Total cyanide PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355586 SP - 1 EP - 234 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35558 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fasano, A. A1 - Woyessa, G. A1 - Stajanca, Pavol A1 - Markos, C. A1 - Stefani, A. A1 - Nielsen, K. A1 - Rasmussen, H. K. A1 - Krebber, Katerina A1 - Bang, O. T1 - Fabrication and characterization of polycarbonate microstructured polymer optical fibers for high-temperature-resistant fiber Bragg grating strain sensors N2 - Here we present the fabrication of a solid-core microstructured polymer optical fiber (mPOF) made of polycarbonate (PC), and report the first experimental demonstration of a fiber Bragg grating (FBG) written in a PC optical fiber. The PC used in this work has a glass transition temperature of 145°C. We also characterize the mPOF optically and mechanically, and further test the sensitivity of the PC FBG to strain and temperature. We demonstrate that the PC FBG can bear temperatures as high as 125°C without malfunctioning. In contrast, polymethyl methacrylate-based FBG technology is generally limited to temperatures below 90°C. KW - Fiber optics sensors KW - Fiber Bragg gratings KW - Microstructured fibers KW - Fiber characterization KW - Polymers PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355591 DO - https://doi.org/10.1364/OME.6.000649 SN - 2159-3930 VL - 6 IS - 2 SP - 649 EP - 659 PB - OSA Publishig AN - OPUS4-35559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Hübert, Thomas A1 - Boon-Brett, L. A1 - Buttner, W. J. T1 - Sensors for Safety and Process Control in Hydrogen Technologies N2 - This book is on sensors which are regularly deployed in technologies and processes related to hydrogen production, storage, distribution, and use. Not all types of sensors are equally suitable for specific hydrogen applications. The information in this book is intended to help the reader understand the basics of sensors, sensing technologies, sensor applications, and to provide guidelines for choosing the right sensors and the use of them correctly. Correct deployment of appropriate sensors demands knowledge of the sensing principle and of the physical or chemical quantities being measured. Because of the properties of hydrogen, the potential for its vastly increased use in a future low-carbon economy and possible hazards associated with its use, special attention is paid to hydrogen sensors. This book will not focus on the details of the hydrogen technologies nor on the many safety-related aspects of these technologies. Many books are already available on these topics. Instead the detection principle of hydrogen sensors and other sensor types used, in the dynamic and rapidly developing field of hydrogen technologies, are treated in detail in this book. In the first chapter a brief overview is presented on basic hydrogen properties and particularly on those properties which are most relevant for safety and for sensing. To illustrate the extensive field of contemporary applications and the exciting possibilities for near future sensor applications, existing and emerging markets using large quantities of hydrogen are mentioned. The role of sensors as devices for monitoring and control of processes and as safety monitoring devices is outlined. The second chapter gives an introduction to sensing technology and provides the Reader with relevant information pertaining to sensor definitions and classification, sensor metrics, and performance arameters, in addition to background information on sensor preparation technologies and techniques. While there are many books available which provide more exhaustive information on each of these topics, e.g., the level of detail provided in this chapter is sufficient to appreciate the salient features of sensing and sensing Technology which are central to hydrogen safety and monitoring of relevant applications. Chapter 3 provides a comprehensive overview of emerging and commercially available hydrogen sensors, an explanation of their sensing principle, and important aspects of their performance. A comprehensive and up-to-date account of the theory (physical or chemical principles), design, and practical implementations of hydrogen sensors for use in hydrogen related applications is presented. Similar information on chemical sensors for other gases, such as oxygen and trace components, which are also highly important in hydrogen technologies because of potential hazards to human health, process safety or facility performance, is provided in Chapter 4. In Chapter 5 descriptions of physical sensors for temperature, pressure, gas flow, and fire indication, which are also germane for the safe use of hydrogen, are provided. Standards, codes, and regulatory documents, which provide practical advice and legislative requirements regarding sensor deployment and performance, are described in Chapter 6. This chapter also makes reference to the main procedures for sensor testing in gas Standards including precise analytical methods and reference methods. The chapter concludes with a discussion on sensor selection and some installation guidelines are provided. In Chapter 7 traditional and emerging processes and technologies involving hydrogen are described. The application of sensors in processes for the production of hydrogen, hydrogen storage, distribution, and the use of hydrogen in stationary and mobile fuel cells is discussed. Furthermore, the use of hydrogen as a coolant and chemical reagent (medium) in various processes is described. The exploitation of sensors for replacing traditional analytical instrumentation is also discussed. Finally supplementary information is provided on hydrogen properties, measuring quantities, and sensor parameters. KW - Hydrogen Technologies KW - Hydrogen Sensors KW - Gas Sensors, Safety KW - Process Control PY - 2016 SN - 978-1-4665-9654-2 SP - 1 EP - 414 PB - CRC Press Taylor & Francis Group CY - Boca Raton, Florida, USA AN - OPUS4-35507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Andrzejuk, W. A1 - Bau, A. A1 - Charoud-Got, J. A1 - de Vos, P. A1 - Emteborg, H. A1 - Lamberty, A. A1 - Linsinger, T. A1 - Oostra, A. A1 - Quetel, C. A1 - Roebben, G. A1 - Tresl, I. A1 - Hearn, R. A1 - Wood, S. A1 - Pritzkow, W. A1 - Vogl, Jochen T1 - Certification of the sulfur mass fraction in three commercial petrol materials - Certified reference materials ERM-EF211, ERM-EF212 and ERM-EF213 N2 - Three petrol reference materials were certified for their total sulfur content in support of Directive 2003/17/EC of the European Parliament and of the European Council, which stipulates that petrol with a maximum S content of 10 mg/kg must be available in all member states by 2009. Commercially available petrol was obtained and filled into borosilicate ampoules without further treatment. Homogeneity of the materials was tested and no heterogeneity was detected for two of the materials, whereas minor heterogeneity was observed for the third material. Stability of the materials was tested for 8-12 months at 60 °C and no degradation was observed. Characterisation was based on isotope-dilution mass spectrometry (IDMS) applied as primary method of measurement by three European metrology institutes and certified values were assigned using all results. The certified uncertainties include contributions of (potential) heterogeneity, potential degradation as well as characterisation. The final assigned values are: ERM-EF211: 48.8 ± 1.7 mg/kg ERM-EF212: 20.2 ± 1.1 mg/kg ERM-EF213: 9.1 ± 0.8 mg/kg The materials are available from IRMM (ERM-EF211), LGC (ERM-EF212) and BAM (ERMEF213) KW - Sulfur KW - Petrol KW - IDMS PY - 2007 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355804 SN - 978-92-79-05370-2 SN - 1018-5593 SP - 1 EP - 37 PB - European Communities CY - Luxembourg AN - OPUS4-35580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Becker, Dorit A1 - Koenig, Maren A1 - Rosner, M. T1 - Certification report for the reference materials ERM-AE102a, -AE104a, -AE120, -AE121 and -AE122 N2 - Isotope reference materials are essential to enable reliable and comparable isotope data. Besides the correction of mass fractionation or mass discrimination isotope reference materials are indispensible for validation and quality control of analytical procedures. This article describes the production and certification of a set of five isotope reference materials ERM-AE102a, 104a, AE120, 121 and 122, for boron isotope analysis. The isotopic composition of all materials has been adjusted by mixing boron mother solutions enriched in 10B or 11B with a boron mother solution having natural-like isotopic composition under full gravimetric control. All mother solutions have been analysed for their boron mass fraction as well as their boron isotopic composition by TIMS using IDMS as calibration technique. For all five reference materials the isotopic composition obtained on the basis of the gravimetric data agrees very well with the isotopic composition obtained from different TIMS techniques. Performed stability and homogeneity studies show no significant influence on the isotopic composition as well as on the related uncertainties. The certified isotope abundances for 10B are 0.29995 (27) for ERM-AE102a and 0.31488 (28) for ERM-AE104a. The certified δ11B values are -20.2 (6) ‰ for ERM-AE120, 19.9(6) ‰ for ERM-AE121 and 39.7 (6) ‰ for ERM-AE122. Together with the formerly certified ERM-AE101 and -AE103 a unique set of seven certified reference materials (CRM) for boron isotope analysis is now available from BAM. KW - Boron KW - Delta value KW - Isotope ratio KW - ICPMS KW - TIMS PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355813 SP - 1 EP - 24 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Becker, Dorit A1 - Koenig, Maren T1 - Certification report for the reference materials ERM-AE123 and ERM-AE124 - Certified for their boron isotope composition N2 - Isotope reference materials are essential to enable reliable and comparable isotope data. Besides the correction of mass fractionation or mass discrimination, isotope reference materials are indispensible for validation and quality control of analytical procedures. This report describes the production and certification of two isotope reference materials, ERM-AE123 and ERM-AE124, for boron isotope analysis. The isotopic composition of ERM-AE123 is the unaltered natural-like isotopic composition of the base material. The isotopic composition of ERM-AE124 has been adjusted by mixing two boron stock solutions enriched in 10B and 11B respectively under full gravimetric control. All stock solutions have been prepared fully under gravimetrical control. The corresponding boron isotopic composition has been analysed by TIMS. For both reference materials the isotopic composition obtained on the basis of the gravimetric data agrees very well with the isotopic composition obtained by TIMS. The certified isotope abundances for 10B are 0.19832 (21) for ERM-AE123 and 0.96006 (6) for ERM-AE124. Together with the formerly certified ERM-AE101, -AE102a, -AE103, -AE104a, -AE120, -AE121 and AE122, a unique set of nine certified reference materials (CRM) for boron isotope analysis is now available from BAM covering a range for the 10B isotope amount fraction from 0.2 to 0.96 and for the δ11B value from -20 ‰ to +40 ‰. KW - boron KW - isotope ratio KW - enriched isotope KW - ICPMS KW - TIMs PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355826 SP - 1 EP - 17 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Becker, Dorit A1 - Koenig, Maren A1 - Rienitz, O. A1 - Noordmann, J. T1 - Certification report for the reference materials ERM-AE140 and ERM-AE141 - Pd and Pt single spikes certified for their Pd and Pt mass fraction and isotopic composition N2 - Isotope dilution mass spectrometry often is applied for the quantification of platinum group elements in environmental and geological samples. In most cases, however, certified spike solutions offering complete uncertainty statements and SI-traceability are missing. This report describes the production and certification of two isotope reference materials, ERM-AE140 and ERM-AE141, serving as calibrated spike solutions for IDMS based quantification of Pd and Pt, respectively. Both materials were produced by dissolving highly enriched isotopes 106Pd and 194Pt and determining the mass fraction of 106Pd and 194Pt in the final solution by reverse IDMS. Two independent back-spikes were produced for each material from high purity Pd and Pt. Characterization measurements were carried out by MC-ICPMS. For ERM-AE140 the certified mass fractions are w(106Pd) = 20.24(5) mg/kg and w(Pd) = 20.54(5) mg/kg. For ERM-AE141 the certified mass fractions are w(194Pt) = 18.18(11) mg/kg and w(Pt) = 19.90(12) mg/kg. These values are traceable to the International System of Units (SI) in the shortest possible way. KW - Palladium KW - Enriched isotope KW - Platinum KW - Spike KW - IDMS PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355833 SP - 1 EP - 25 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Pritzkow, W. T1 - Bericht zur Herstellung und Zertifizierung eines Cadmium-Isotopenreferenzmaterials - Zertifiziertes Referenzmaterial BAM-I012 N2 - Dieser Bericht beschreibt die Herstellung und Zertifizierung einer Cadmiumlösung mit natürlicher Isotopenzusammensetzung. Für das Isotopen-Referenzmaterial sind sowohl die Isotopenverhältnisse als auch Isotopenhäufigkeiten und die molare Masse von Cadmium zertifiziert. Die Unsicherheiten sind erweiterte Messunsicherheiten U = k.uc mit k = 2. Der Cadmium-Massenanteil in der Lösung wird als indikativer Wert angegeben mit einer erweiterten Messunsicherheit U = k.uc mit k = 4,5. KW - Absolute Isotopenverhältnisse KW - Primäres Isotopenreferenzmaterial KW - Cadmium PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355845 SP - 1 EP - 15 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35584 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik T1 - Spatial and temporal control of thermal waves by using DMDs for interference based crack detection N2 - Active Thermography is a well-established non-destructive testing method and used to detect cracks, voids or material inhomogeneities. It is based on applying thermal energy to a samples’ surface whereas inner defects alter the non-stationary heat flow. Conventional excitation of a sample is hereby done spatially, either planar (e.g. using a lamp) or local (e.g. using a focused laser) and temporally, either pulsed or periodical. In this work we combine a high power laser with a Digital Micromirror Device (DMD) allowing us to merge all degrees of freedom to a spatially and temporally controlled heat source. This enables us to exploit the possibilities of coherent thermal wave shaping. Exciting periodically while controlling at the same time phase and amplitude of the illumination source induces – via absorption at the sample’s surface - a defined thermal wave propagation through a sample. That means thermal waves can be controlled almost like acoustical or optical waves. However, in contrast to optical or acoustical waves, thermal waves are highly damped due to the diffusive character of the thermal heat flow and therefore limited in penetration depth in relation to the achievable resolution. Nevertheless, the coherence length of thermal waves can be chosen in the mm-range for modulation frequencies below 10 Hz which is perfectly met by DMD technology. This approach gives us the opportunity to transfer known technologies from wave shaping techniques to thermography methods. We will present experiments on spatial and temporal wave shaping, demonstrating interference based crack detection. T2 - Photonics West 2016, OPTO, 9761 CY - San Francisco, Cal, USA DA - 15.02.2016 KW - Thermal Waves KW - Laser KW - DMD KW - Active Thermography PY - 2016 AN - OPUS4-35586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik A1 - Kreutzbruck, M. A1 - Ziegler, Mathias T1 - Spatial and temporal control of thermal waves by using DMDs for interference based crack detection N2 - Active Thermography is a well-established non-destructive testing method and used to detect cracks, voids or material inhomogeneities. It is based on applying thermal energy to a samples’ surface whereas inner defects alter the nonstationary heat flow. Conventional excitation of a sample is hereby done spatially, either planar (e.g. using a lamp) or local (e.g. using a focused laser) and temporally, either pulsed or periodical. In this work we combine a high power laser with a Digital Micromirror Device (DMD) allowing us to merge all degrees of freedom to a spatially and temporally controlled heat source. This enables us to exploit the possibilities of coherent thermal wave shaping. Exciting periodically while controlling at the same time phase and amplitude of the illumination source induces – via Absorption at the sample’s surface - a defined thermal wave propagation through a sample. That means thermal waves can be controlled almost like acoustical or optical waves. However, in contrast to optical or acoustical waves, thermal waves are highly damped due to the diffusive character of the thermal heat flow and therefore limited in penetration depth in relation to the achievable resolution. Nevertheless, the coherence length of thermal waves can be chosen in the mmrange for modulation frequencies below 10 Hz which is perfectly met by DMD technology. This approach gives us the opportunity to transfer known technologies from wave shaping techniques to thermography methods. We will present experiments on spatial and temporal wave shaping, demonstrating interference based crack detection. T2 - Photonics West 2016, OPTO, 9761 CY - San Francisco, CA, USA DA - 15.02.2016 KW - Active thermography KW - Thermal wave KW - Spatial light modulation KW - Crack detection KW - DMD KW - DMD coupled laser PY - 2016 DO - https://doi.org/10.1117/12.2210918 SN - 0277-786X VL - 9761 SP - 97610N-1 EP - 97610N-13 AN - OPUS4-35587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Rades, Steffi A1 - Salge, T. A1 - Mielke, Johannes A1 - Ortel, Erik A1 - Schmidt, R. T1 - Characterisation of nanoparticles by means of high-resolution SEM/EDS in transmission mode N2 - Advances in scanning electron microscopy (SEM) enable the high-resolution imaging of single nanoparticles (NPs) with sizes well below 10 nm. The SEM analysis in transmission mode (T-SEM) of NPs on thin film supports has many benefits when compared to the analysis of NPs on bulk substrates. The enhanced material (mass – thickness) contrast of the T-SEM imaging mode is well suited for in-depth and, particularly valuable, to very accurate, traceable, lateral dimensional measurements of NPs. Compared to samples prepared on bulk substrates, T-SEM with energy dispersive X-ray spectroscopy (EDS) achieves a drastically improved spatial resolution of the emitted X-rays. The poor signal-to-noise ratio of the X-ray spectra emitted by a single nanoparticle (NP) can be improved by the use of high-sensitivity (high collection solid angle) silicon drift (SDD), energy-dispersive X-ray spectrometers (EDS). The EDS spectral imaging of a single NP with a spatial resolution below 10 nm has become possible. This is demonstrated by means of various examples of nanostructures. Advanced data processing of T-SEM/EDS results sets the stage for the automated classification of NPs by feature analysis. This method combines the detection of morphological structures of interest by image processing of T-SEM micrographs with the chemical classification by EDS. T2 - European Microbeam Analysis Society’s 14th European Workshop on Modern Developments and Applications in Microbeam Analysis (EMAS 2015) CY - Portorož, Slovenia DA - 03.05.2015 KW - High-resolution KW - SEM KW - T-SEM KW - EDX KW - Nanoparticles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355628 UR - http://iopscience.iop.org/article/10.1088/1757-899X/109/1/012006 DO - https://doi.org/10.1088/1757-899X/109/1/012006 SN - 1757-899X VL - 109 SP - 012006-1 EP - 012006-12 PB - IOP Publishing Ltd CY - Bristol, UK AN - OPUS4-35562 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lehmann, Jens T1 - KorroPad - Beurteilung der Korrosionsbeständigkeit von Oberflächen nichtrostender Stähle N2 - Mit dem KorroPad Verfahren ist es dem Anwender möglich den Zustand der Passivschicht nichtrostender Stähle auf sehr einfache und schnelle Weise einschätzen zu können. Das Verfahren eignet sich dazu, den Grad der Passivität in Abhängigkeit der Umgebungsbedingungen und der Zeit nachzuvollziehen. Dies ermöglicht dem Anwender und Verarbeiter von nichtrostenden Stählen, die Lagerungsbedingungen und –zeiten einer frisch bearbeiteten Stahloberfläche zu ermitteln, welche für die Ausbildung einer stabilen Passivschicht notwendig sind, bevor diese risikoarm eingesetzt werden kann. Wie die hier dargestellten Beispiele und auch weitere zahlreiche praktische Anwendungen gezeigt haben, eignet sich das KorroPad ebenfalls für die Identifikation kritischer Prozessparameter bei der Verarbeitung nichtrostender Stähle. Mit dem Verfahren lassen sich viele prozessbedingte Einflussfaktoren auf die Oberflächengüte wie auch auf den Werkstoff charakterisieren. Aufgrund der schnellen und einfachen Auswertung der Prüfergebnisse können positive wie auch negative Veränderungen hinsichtlich der Passivschichtstabilität zügig erkannt werden. Dies ermöglicht es dem Anwender schnell zu reagieren, um kritische Einflüsse zu korrigieren und um eine Optimierung von Inhouse-Prozessen durchzuführen. Weitere Einsatzgebiete sind im Bereich der Wareneingangs- und/oder Warenausgangskontrolle denkbar, überall wo es um die Frage der Passivschichtstabilität einer nichtrostenden Stahloberfläche geht. T2 - Fachtagung Bauwerksdiagnose - Praktische Anwendungen Zerstörungsfreier Prüfungen und Zukunftsaufgaben CY - Berlin, Germany DA - 25.02.2016 KW - Korrosionsschnelltest KW - nichtrostender Stahl KW - Passivschicht KW - KorroPad PY - 2016 AN - OPUS4-35570 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Platin- und Palladium-Analytik mit ID-ICPMS N2 - Zertifizierung von Pt und Pd-Spikes und deren Anwendung auf die Quantifizierung von Pd und Pt in Kfz-Emissionen T2 - 15. Edelmetallforum CY - Freising, Germany DA - 14.03.2016 KW - PGE KW - Emissionen KW - IDMS KW - ICPMS PY - 2016 AN - OPUS4-35572 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Real-world examples of how to calculate a KCRV N2 - In this presentation the different ways are presented, which are used to calculate in practice the key comparison reference value. T2 - EURAMET TC Metrology in Chemistry Meeting CY - Geel, Belgium DA - 03.02.2016 KW - key comparison KW - CCQM KW - Degree of equivalence PY - 2016 AN - OPUS4-35573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ecker, K. H. A1 - Wätjen, U. A1 - Berger, Achim A1 - Grötzschel, R. A1 - Persson, L. A1 - Pritzkow, W. A1 - Radtke, Martin A1 - Riebe, Gundel A1 - Riesemeier, Heinrich A1 - Vogl, Jochen T1 - Certification of antimony implanted in silicon wafer with a silicon dioxide diffusion barrier - IRMM-302 and BAM-L001 N2 - This Report describes the certification of the reference material antimony implanted in Si/SiO2 intended to be used for calibration of surface and near surface analytical methods. It describes the preparation, homogeneity measurements and the analytical work performed for the certification of both Areal density of antimony Atoms (retained dose) and the isotope amount Ratio as well as giving considerations on the stability of the material. KW - Isotope ratio KW - Areal density KW - Surface analysis PY - 2002 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355752 SP - 1 EP - 40 PB - Institute for Reference Materials and Measurements CY - Geel, Belgium AN - OPUS4-35575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Becker, Dorit A1 - Janisch, N. A1 - Klingbeil, P. A1 - Ludwig, H. P. A1 - Riebe, G. A1 - Pritzkow, W. A1 - Wermann, G. T1 - Zertifizierungsbericht für ERM-AE101 (auch BAM-I001), ERM-AE102 (auch BAM-I002) und ERM-AE103 (auch BAM-I003) N2 - Dieser Bericht beschreibt die Zertifizierung von 3 synthetischen Isotopenmischungen aus natürlicher und angereicherter Borsäure. Diese Isotopen-ZRM liegen als konzentrierte, wäs-serige Borsäure-Lösungen vor und sind bezüglich ihrer Isotopenzusammensetzung zertifi¬ziert. Der Bor-Gesamtgehalt ist als Richtwert angegeben. Die Unsicherheiten sind erweiterte Messunsicherheiten mit k=2. Sie sind in Klammern angegeben und beziehen sich auf die letzten beiden Stellen. Die vorliegenden Isotopen-ZRM sind bezüglich ihrer Isotopenzu¬sam-mensetzung mit erweiterten relativen Messunsicherheiten kleiner 0,12% zertifiziert. Die ab-solute, kombinierte Standardunsicherheit des prozentualen Stoffmengenanteils der Isotope (Isotopenhäufigkeit) liegt zwischen 0.012 und 0.017. KW - Isotope KW - Bor KW - Kernkraftwerke PY - 2009 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355777 SP - 1 EP - 21 CY - Berlin AN - OPUS4-35577 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Ostermann, Markus A1 - Becker, Dorit A1 - Janisch, N. T1 - Zertifiziertes Referenzmaterial ERM-AE104 bzw. BAM-I004 N2 - Dieser Bericht beschreibt die Zertifizierung einer synthetischen Isotopenmischung aus natürlicher und angereicherter Borsäure. Dieses Isotopen-ZRM liegt als konzentrierte, wässerige Borsäure-Lösung vor und ist bezüglich ihrer Isotopenzusammensetzung zertifiziert. Der Bor-Gesamtgehalt ist als Richtwert angegeben. Die Unsicherheiten sind erweiterte Messunsicherheiten mit k=2. Sie sind in Klammern angegeben und beziehen sich auf die letzten beiden Stellen. Das vorliegende Isotopen-ZRM ist bezüglich der Isotopenzusammensetzung mit erweiterten relativen Messunsicherheiten kleiner 0,08% zertifiziert. Die absolute, kombinierte Standardmessunsicherheit des prozentualen Stoffmengenanteils der Isotope (Isotopenhäufigkeit) liegt bei 0,014. In diesem Zertifizierungsbericht wird nur auf die Kapitel eingegangen, die abweichend vom bestehenden Zertifizierungsreport für die Referenzmaterialien BAM I001 bis BAM I003 sind und Einfluss auf die Endergebnisse haben. Dabei handelt es sich um die Kapitel 3.3, 3.4, 4, 6, 7 und 8, Die Kapitel 1, 2, 3, 3.1, 3.2, 5, 9 und 10 des alten Zertifizierungsberichts für die Referenzmaterialien BAM I001 bis BAM I003 behalten unverändert ihre Gültigkeit und sind nicht noch einmal aufgeführt worden. KW - Isotope KW - Kernkraftwerk KW - Bor PY - 2009 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355786 SP - 1 EP - 9 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35578 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Klingbeil, P. A1 - Pritzkow, W. A1 - Riebe, Gundel A1 - Wermann, G. A1 - Turner, P. A1 - Wortel, N. A1 - Woittiez, J. T1 - HIIRM final report N2 - Accurate analytical results have become more and more an absolute essential tool for further progresses in technology and science. Precision however, often used in this context as a quality criterion for analytical methods, is not a replacement for accuracy in any way. Therefore, analytical procedures are necessary, which will generate reliable and accurate results and can be used for evaluation of other analytical procedures and certification of reference materials (RM). Especially the certification of reference materials for the amount content of trace elements requires highly accurate results with a small combined uncertainty. The best example for an analytical procedure having this capability is undoubtedly Isotope Dilution Mass Spectrometry, for inorganic as well as for organic applications. Applied on Thermal Ionization Mass Spectrometry (TIMS) isotope dilution provides results of highest quality and proven high accuracy especially in the field of RM certifications for more than 30 years. The major drawback of this approach often is the necessity for a complex chemical separation step. A major advantage of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is the potential to cope with a simplified or an on-line-carried-out sample preparation. A key requirement of isotope dilution analysis however is the accurate and precise determination of isotope ratios, because of its limiting factor for the accuracy and the total uncertainty of the result. Very precise isotope ratios can be determined in combination with a detection system that is capable of simultaneous detection of different isotopes, a so-called multi-collector system. The objective of the presented project is to evaluate the advantages of such a multi-collector ICP-MS for the application of IDMS in the field of trace elemental analysis in reference materials. The focus is on the development of simple and fast procedures for isotope ratio measurements in general and IDMS analysis in particular. Furthermore, it is an objective to develop and evaluate on-line spiking procedures. One of the first conclusions, which had a severe impact on the HIIRM project, arose during the early days of the project. Currently most certification experiments are accomplished by certification campaign based on a variety of participants’ results. The sample preparation, sending, analyzing and data evaluation however require lot of resources and the process may take a long time. An alternative way is given by using fewer participants with methods of higher metrological quality. For elemental amount contents such a method undoubtedly is isotope dilution analysis and multi-collector ICP-MS offers the necessary precision and matrix robustness and ruggedness as said above. Therefore, a multiple collector ICP-MS was manufactured as part of the project instead of the originally planned high-resolution instrument. Due to the novelty of the multicollector ICP-MS instrument, a lot of additional fundamental research became necessary. Especially interferences needed further attention. Fortunately, the IsoProbe is additionally equipped with a high-resolution option and with a brand new collison cell. The high-resolution option however can only be used to identify interferences but cannot be used to quantify them. On the other hand, the use of the collision cell proved to be a vital tool to overcome interferences. This is especially true because high resolution would have reduced the available sensitivity by a factor of ~100. Applying the collision cell technology the high sensitivity was maintained whilst most interferences were eliminated. However finding the right parameters of operation for the collision cell became a huge part of the method development process. A variety of gases like argon, helium, hydrogen, deuterium, nitrogen, krypton and xenon were tested for their suitability. Especially the tests accomplished for iron determinations revealed that carefully selected parameters have an incredible influence on the quality of the final results. Nonetheless collision cell technology will undoubtedly be widely used for newer ICP-MS instrumentation and contribute to eliminate wrong analytical values caused by interferences. The enhanced sensitivity of the instrument revealed also problems not detectable by other means. The control of contaminations seems to be one of the major analytical challenges in the future. Sector field based ICP-MS will give the user an opportunity to trace sources of contamination back to their origin and eliminate them. Even lower limits of detection will be the result as well as an enhanced reliability for analysts dealing with higher amount contents. The analyst will also benefit in controlling blank levels when the method of isotopically spiked procedure blanks is used as demonstrated in this project. Another main part of the project was the validation of the developed procedures. The first validation step was successfully accomplished by applying these procedures on the standard solutions provided by NRG. The main part of this validation however consisted of the evaluation of the fundamental parameters of the isotope dilution process and related measurements. This approach turned out to be superior compaired to the first step as a highly reliable uncertainty calculation can be easily performed. The best reputation and acceptance of the methods can however only be accomplished by participating in certification campaigns or in interlaboratory comparisons on highest metrological level. The results of the participations in general were brilliant. Not only the results but also the obtained realistic uncertainties were of superior quality. Direct comparisons at BAM with the results obtained by a multicollector TIMS applying the same calculation schemes showed the benefits of using multicollector ICP-MS. The main benefits of ICP-MS were identified, of which the first one is the enhanced precision of the isotope ratio measurement. For a variety of elements the values obtained by multicollector ICP-MS are even more precise than the ones obtainable by multicollector TIMS. The second important advantage identified was the simplified sample preparation. The laborious and time consuming analyte-matrix-separation step as necessary for TIMS measurements can either be omitted or at least be drastically reduced. Therefore, the advantages regarding time and enhanced sample throughput will result in further spread of ICP-MS in general and multicollector ICP-MS in particular. The third major part in terms of the method development process was mainly focused on developing an online isotope dilution system. The volumetric instead of the gravimetric IDMS approach proved difficult, if the high demands necessary for RM definition measurements are to be fulfilled. The major obstacle in this case is the missing stability and precision in terms of mass flow. Consequently, the initial development failed as the system made up of two piezoelectric droplet injectors was unable to reach the required stability as well as precision. The thereupon-created system consisting of two HPLC pumps proved to be far more valuable regarding automation and particularly the quantification of transient signals. Nevertheless, such a system will probably be rarely used in certification campaigns, as the gain of time is too small compared to the loss of reliability. However, this system proved most valuable in terms of species-specific elemental analysis as preliminary investigations showed. In this context this system will be suitable for certification measurements, as the major uncertainty contributions derive from sampling, sample treatment and species distribution and as moreover all availabel methods demonstrate far beyond. During the whole project, one of the main concerns regarding the multicollector ICP-MS instrument were software issues caused by the early development state of the original control programs. A lot of effort was necessary to accomplish the necessary data manipulations externally. The development of a new software suite by Micromass for the HIIRM project has solved this issue almost completely. With the new software suite and the validated parameters of measurement a step forward for institutes dealing with reference material certifications was achieved. Future certifications campaigns for minor elemental contents in different matrices should be performed by a small number of participants from highly qualified institutes. These institutes should apply very reliable methods of measurement like the ones developed in the HIIRM project. Many resources may be saved that way while the outcome of the certifications may easily be improved. ICP-MC-MS has the potential to be an important method in this context. Stable isotope dilution analysis in combination with a multi-detector ICP-MS, equipped with a hexapole collision cell for the suppression of important spectral interferences and for enhanced sensitivity, proved to be an advanced method of elemental analysis with a high potential for matrix independent measurements. Since ICP mass spectrometers of this type have only recently been introduced, no systematic evaluation of the capabilities of this specific application of the ICP-IDMS method has yet been made. KW - interferences KW - collision cell KW - ICPMS KW - IDMS PY - 2002 SP - 1 EP - 166 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35579 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kästner, Claudia T1 - Aggregation and deaggregation of silver nanoparticles - what does your gut say? N2 - Due to the increasing utilization of silver nanoparticles in consumer related products, many studies focus on investigations regarding their toxicological potential. This includes investigations concerning uptake, distribution and excretion of the particles. So far, little attention was paid to changes of physical and chemical properties in the human body. During processes like digestion, the question arises whether they can pass this barrier in a nanoscale form. In this study we analytically monitored the changes in the size distribution of silver nanoparticles during an artificial digestion process with the help of small angle x-ray scattering (SAXS). Therefore, we synthesized polyacrylic acid stabilized ultra-small silver nanoparticles with a radius of 3 nm and a size distribution width of 18%. The artificial digestion process mimics the gastro-intestinal passage and simulates the oral, gastric and small intestinal conditions. Additionally, food components like oil, starch, glucose and skimmed milk powder are used to provide a preferably realistic environment. In absence of any food components the low pH initiates aggregation of the particles in the stomach. However, the particles unexpectedly stabilize in a defined cluster form with a mean radius of 12 nm. By the use of the food components oil and starch we observed that the particles are dispersed again. Now we found a bimodal size distribution of primary particles and aggregates. In contrast to that, with skimmed milk powder only a slight aggregation occurs in the stomach. In the gastric tract the particle distribution is stabilized at a mean volume weighted radius of 5 nm. Hence, skimmed milk powder acts as a colloidal stabilizer. For comparison we also used silver nitrate as a control substance. Surprisingly, we observed a formation of nanoparticles already in the saliva. During the digestion process the distribution narrows and finally in the intestine it shows a stable distribution with a mean volume weighted radius of 3 nm and a small fraction of aggregates. These results indicate that the silver nanoparticles can pass the biological barriers of the digestion process in a nanoscale form but undergo a transformation in the size distribution. However, even from pure silver nitrate nanoparticle formation can be observed. This sketches a complex mechanism in which not only food components but also silver ions cause changes in nanoparticle size and aggregation. T2 - 11th International Conference on Biological Barriers CY - Saarbrücken, Germany DA - 07.03.2016 KW - digestion KW - small-angle X-ray scattering KW - silver nanoparticles PY - 2016 AN - OPUS4-35539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abali, B. E. A1 - Wu, Cheng-Chieh A1 - Müller, W.H. T1 - An energy-based method to determine material constants in nonlinear rheology with applications N2 - Many polymer-type materials show a rate-dependent and nonlinear rheological behavior. Such a response may be modeled by using a series of spring-dashpot systems. However, in order to cover different time scales the number of systems may become unreasonably large. A more appropriate treatment based on continuum mechanics will be presented herein. This approach uses representation theorems for deriving material equations and allows for a systematic increase in modeling complexity. Moreover, we propose an approach based on energy to determine thematerial parameters.This method results in a simple linear regression problemeven for highly nonlinearmaterial equations. Therefore, the inverse problem leads to a unique solution. The significance of the proposed method is that the stored and dissipated energies necessary for the procedure are measurable quantities. We apply the proposed method to a 'semi-solid' material and measure its material parameters by using a simple-shear rheometer. KW - Material equations KW - Constitutive relations KW - Nonlinear rheology KW - Simple-shear rheometer KW - Inverse analysis PY - 2016 DO - https://doi.org/10.1007/s00161-015-0472-z SN - 0935-1175 SN - 1432-0959 VL - 28 IS - 5 SP - 1221 EP - 1246 PB - Springer CY - Berlin AN - OPUS4-34333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Helmerich, Rosemarie A1 - Mielentz, Frank A1 - Milmann, Boris A1 - Adam, Louisa A1 - Villalobos, S. A1 - Guimaraes, M. A1 - Wiggenhauser, Herbert T1 - Detection of cracks perpendicular to the surface using acoustic methods N2 - Cracks perpendicular to the surface may be initial indicators for a deterioration process of concrete structures. Moisture penetrates inside the structure and transports adverse chemicals. The paper presents an investigation about the reliability of available commercial non-destructive evaluation techniques to reliably estimate the depth of surface-breaking cracks in reinforced concrete structures. Aim of the study was the investigation of surface-braking cracks under laboratory conditions. Commercial acoustic devices as impact echo equipment, single ultrasonic transducers and arrays were applied even if they have not been developed for this purpose. The commercial software and descriptions for application was followed strictly to compare the function, precision and repeatability of the measurements. Both, perpendicular notches and cracks have been considered. The study was completed with a discussion about reference specimens. The study was the basis for formulation of gaps in research. The Electric Power Research Institute (EPRI) has initiated and funded a Project. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - Acoustic test KW - Commercial acoustic devices KW - Ultrasonic test KW - Crack depth KW - Concrete specimens PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-345729 UR - https://www.ndt.net/?id=18412 SN - 1435-4934 VL - 20 IS - 11 SP - 1 EP - 9 PB - NDT.net CY - Kirchwald AN - OPUS4-34572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Millar, Steven A1 - Gottlieb, Cassian A1 - Wilsch, Gerd A1 - Eichler, Thorsten A1 - Bohling, C. A1 - Molkenthin, A. T1 - Laser induced breakdown spectroscopy (LIBS) - On-site investigatioons on a bridge with a mobile LIBS-system N2 - LIBS is on the step from a laboratory application to on-site analysis. A validated mobile LIBS-system for on-site application on building materials is under development at BAM in cooperation with industrial partners (system developers and companies), who will use this technique for investigation on building structures like bridges and parking decks. The system is designed to measure the content of harmful species like chlorine, sulfur or alkalis, to give the engineer a tool for the estimation of the condition of concrete structures and for quality assurance during concrete repair work on-site. In these work results of on-site measurements on a chloride contaminated bridge are shown. Further work will focus on providing guidelines to establish LIBS as a standard procedure for chemical investigations of building materials. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - LIBS KW - Chlorides KW - Sulfur KW - Alkalis KW - Corrosion KW - ASR KW - Chemical analysis KW - Chloride KW - Elementanalyse KW - Natrium KW - Baustoffuntersuchungen KW - Baustoffe KW - Dauerhaftigkeit KW - Messsysteme KW - Mobiles LIBS PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-345795 UR - http://www.ndt.net/?id=18296 SN - 1435-4934 VL - 20 IS - 11 SP - 1 EP - 5 PB - NDT.net CY - Kirchwald AN - OPUS4-34579 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fiedler Bremer, C. A1 - Scholz, R. A1 - Myslicki, S. A1 - Starke, P. A1 - Boller, C. A1 - Walther, F. A1 - Krause, Martin T1 - NDT-based characteriazation of timber and vulcanized fiber for civil infrastructure N2 - The paper addresses beech wood as well as vulcanized fiber and discusses the results obtained when using acoustic emission and thermography as non-destructive testing techniques along tensile and load increase fatigue tests to characterize the wooden material’s behavior under increasing fatigue loads to get enhanced information regarding the fatigue behavior of both materials. Reference is mainly made to the materials’ anisotropic and microstructural behavior and what implications this has with respect to the materials’ strength. The influence of moisture is discussed, as well as parameters that may deserve monitoring in the sense of structural health monitoring to be applied in timber structures in general. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - Ermüdung KW - Belastungsversuch KW - Thermographie KW - ZfP KW - Timber PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-346377 UR - https://www.ndt.net/?id=18419 SN - 1435-4934 VL - 20 IS - 11 SP - 1 EP - 11 PB - NDT.net CY - Kirchwald AN - OPUS4-34637 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grothe, Sven T1 - Ultrasonic signal evaluation used to detect weather-related temperature changes in a concrete specimen N2 - Ultrasonic measurement evaluation methods have been proven to be effective for detection of subtle changes, caused by temperature, load or moisture. However, for its application outdoors it is necessary to analyse unavoidable influences, such as weather. Therefore an ultrasonic monitoring system with 40 ultrasonic sensors (20 transmitters, 20 receivers; 25 kHz central frequenzy) has been implemented on a concrete specimen (4×5×0.8m3), that is exposed to weather conditions. Data from 400 sensor combinations was collected over a period of six months with an interval of two hours. The data was evaluated by both qualitative (correlation techniques) and quantitative (ultrasonic velocity changes via Coda Wave Interferometry and time of flight method) evaluation methods and compared to the temperature changes caused by weather. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-346398 UR - https://www.ndt.net/?id=18336 SN - 1435-4934 VL - 20 IS - 11 SP - 1 EP - 4 PB - NDT.net CY - Kirchwald AN - OPUS4-34639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 18. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik. KW - Eignungsprüfung KW - Boden KW - MKW KW - PAK KW - Gesamtcyanid KW - Spurenelemente KW - Proficiency testing KW - Soil KW - TPH KW - PAH KW - Total cyanide KW - Trace elements PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-357399 SP - 1 EP - 226 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35739 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unnikrishnakurup, Sreedhar A1 - Krishnamurthy, C. V. A1 - Balasubramaniam, Krishnan T1 - Monitoring TIG welding using Infrared Thermography - Simulations and Experiments N2 - In the current work a 3D model has been developed to predict the thermal cycles during the Tungsten Inert Gas welding of Aluminum 2219. This paper describes the step by step procedure adopted to get the actual cooling rate during the TIG welding process both experimentally and numerically. The model was developed in the COMSOL Finite Element Package and considered a Gaussian heat distribution. The developed model then validated using the experimental data collected in field experiments on actual large propellant tanks. Temperature measurements were performed using Infrared Camera. Results show a close comparison between model and experiment. KW - Image Analysis KW - Infrared Thermography KW - Online Monitoring KW - Finite Element Method PY - 2016 DO - https://doi.org/10.15199/48.2016.04.02 SN - 0033-2097 IS - 4/2016 SP - 6 EP - 9 AN - OPUS4-35743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bartholmai, Matthias A1 - Kammermeier, Michael A1 - Koeppe, Tabea A1 - Werner, Klaus-Dieter ED - Nicoletto, G. ED - Pastrama, S.D. ED - Emri, I. T1 - High dynamic measurement of strain and acceleration using a multichannel measuring system with single cable serial connection N2 - Strain and acceleration measurement during high dynamic drop tests, e.g., of containments for dangerous goods is performed using high speed multichannel measuring systems. So far established and operated systems need a cable connection of every strain gauge and acceleration sensor with the measuring device, often counting up to a number of more than 100 cables, corresponding to the number of applied sensors. The result is a massive cable harness consisting of all single cables, which is difficult to handle and causes a number of practical problems. An innovative approach is proposed by using a single cable measuring system, consisting of measuring modules with data bus connection and local data acquisition. Promising results were presented in a previous study. This paper follows up with additional results from full-scale testing of a further enhanced single cable system for the application in drop tests. T2 - 32nd DANUBIA ADRIA SYMPOSIUM on Advances in Experimental Mechanics CY - Starý Smokovec, Slovakia DA - 22.09.2015 KW - Multichannel measuring KW - Single cable serial connection KW - Dangerous goods container KW - Drop test KW - High impact testing PY - 2016 DO - https://doi.org/10.1016/j.matpr.2016.03.023 SN - 2214-7853 VL - 3 IS - 4 SP - 931 EP - 935 PB - Elsevier Ltd. AN - OPUS4-35689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 19. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik. KW - Eignungsprüfung KW - Boden KW - MKW KW - PAK KW - Gesamtcyanid KW - Spurenelemente KW - Proficiency testing KW - Soil KW - TPH KW - PAH KW - Total cyanide KW - Trace elements PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-356963 SP - 1 EP - 233 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35696 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Levee inspection - geophysics between science, standards, reliability and budgets N2 - Numerous case histories show evidence that geophysical methods are valuable tools for levee inspection and monitoring. National and international standards and recommendations recommend the use of geophysics for a variety of tasks. However, in some cases reported have been flaws missed or false indications given. Due to the larger variety in type, size and construction of levees and the even larger variety of potential tasks and targets the success of geophysical surveys still pretty much depends on the available budget and the experience and capabilities of the clients and contractors involved. It is strongly recommended that all relevant parties agree on the detailed objectives of the survey, required accuracy and reliability of the results and any follow up measures. For the most common tasks more research and practical work using techniques as POD (probability of detection), which are well established in other fields of non-destructive testing, would be of benefit. T2 - SAGEEP 2016 CY - Denver, CO, USA DA - 20.03.2016 KW - Levee KW - Geophysics KW - Inspection PY - 2016 SP - paper levees 07, 1 EP - 4 AN - OPUS4-35705 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schürmann, Robin A1 - Bald, Ilko T1 - Decomposition of DNA nucleobases by laser irradiation of gold nanoparticles monitored by surface-enhanced Raman scattering N2 - Different approaches have been proposed to treat cancer cells using gold nanoparticles (AuNPs) in combination with radiation ranging from infrared lasers to high-energy ion beams. Here we study the decomposition of the DNA/RNA nucleobases thymine (T) and uracil (U) and the well-known radiosensitizer 5-bromouracil (BrU) in close vicinity to AuNPs, which are irradiated with a nanosecond pulsed laser (532 nm) matching the surface plasmon resonance of the AuNPs. The induced damage of nucleobases is analyzed by UV−vis Absorption spectroscopy and surface-enhanced Raman scattering (SERS). A clear DNA damage is observed upon laser irradiation. SERS spectra indicate the fragmentation of the aromatic ring system of T and U as the dominant form of damage, whereas with BrU mainly the cleavage of the Br−C bond and formation of Br− ions is observed. This is accompanied by a partial transformation of BrU into U. The observed damage is at least partly ascribed to the intermediate formation of lowenergy electrons from the laser-excited AuNPs and subsequent dissociative electron attachment to T, U, and BrU. These reactions represent basic DNA damage pathways occurring on the one hand in plasmon-assisted cancer therapy and on the other hand in conventional cancer radiation therapy using AuNPs as sensitizing agents. KW - Gold nanoparticles KW - SERS KW - Electrons KW - DNA damage KW - Gold-Nanopartikel KW - Elektronen KW - DNA-Schädigung PY - 2016 DO - https://doi.org/10.1021/acs.jpcc.5b10564 VL - 120 IS - 5 SP - 3001 EP - 3009 PB - AMER CHEMICAL SOC AN - OPUS4-35673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Kühn, Julius T1 - Composition and chemistry of Pd-Ni-Co thin film alloys for hydrogen related applications N2 - The discovery and design of high performance Pd-alloys is of great interest for the use of hydrogen as a future energy carrier. Therefore hydrogen has to be detected, separated from other gases and stored. In this respect this thesis presents the combinatorial synthesis and characterization of the ternary Pd-Ni-Co alloy System over a wide composition range based on so-called thin film alloy libraries. Those libraries are model systems to characterize a large number of alloy compositions at the same time. The sputter-deposition process is optimized for the gradient of the Pd concentration on the surface of the alloy library by the use of electron-excited Auger electron spectroscopy. The scientific goal of this work is the experimental Investigation of adsorbate-induced surface segregation phenomena on alloy libraries. The surface and bulk compositions of an alloy library are studied after deposition, H2 exposure and H2S poisoning. The co-segregation of Ni and Co to the surface is observed. The segregation process is influenced by the oxidation of Ni and Co due to the contact with ambient air, by H2 and by H2S poisoning. Also at very high Pd concentrations in the range of 87 at.% to 97 at.%, which is interesting for the detection of very low H2-Concentrations in air, the co-segregation of Ni and Co takes place. The poisoning effects were investigated in detail on a pre-selected Pd-Ni-Co alloy by photoelectron spectroscopy (XPS, HAXPES) in addition to AES and EDX. The composition profile of the alloy on the nm scale is acquired and the surface and bulk chemistry is discussed before and after poisoning. The composition of the alloy only changed within the first 3 nm due to H2S exposure. In the ternary Pd-Ni-Co alloy system Pd is present in its metallic state, while Ni and Co show several oxidation states. The presented concepts of ternary alloy development pave the way for the systematic synthesis and characterization of new ternary transition metal alloy systems. KW - Hydrogen sensor KW - Library of ternary Pd-alloys KW - AES KW - (HAX)PES KW - REM/EDX KW - Wasserstoffsensor KW - Bibliothek ternärer Pd-Legierungen PY - 2016 DO - https://doi.org/10.14279/depositonce-5002 SP - 1 EP - 127 PB - Technische Universität CY - Berlin AN - OPUS4-35680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Petrov, Sergej A1 - Neumann, Patrick P. A1 - Werner, Klaus-Dieter A1 - Wosniok, Aleksander A1 - Lazik, D. A1 - Bartholmai, Matthias ED - Nicoletto, G. ED - Pastrama, S.D. ED - Emri, I. T1 - Concept for investigating mechanical and thermal impacts on distributed subsurface gas monitoring N2 - A multifunctional sensor in line shape was developed and introduced in previous work for measuring of gas concentrations, temperature change, and strain. A current field study focuses on a spatially distributed monitoring of subsurface CO 2 gas storage sites in near real time. Mechanical impacts, e.g., caused by construction work, denudation, and seismic activity, can affect the integrity of underground gas storage sites. Thermal or moisture impacts, e.g., caused by weather conditions, can influence the gas Distribution behavior. In this paper, we briefly describe the setup of a CO 2 injection soil test field. This setup contains actuating elements for the investigation of mechanical and thermal impacts on distributed subsurface gas monitoring. A concept is given for evaluating these impacts and first experimental results are presented. T2 - 32nd DANUBIA ADRIA SYMPOSIUM on Advances in Experimental Mechanics CY - Starý Smokovec, Slovakia DA - 22.09.2015 KW - Linear sensor KW - Distributed sensor KW - Monitoring of CO 2 KW - Subsurface monitoring KW - Gas storage areas KW - Membrane-based gas sensing KW - Fibre optical sensing PY - 2016 DO - https://doi.org/10.1016/j.matpr.2016.03.060 SN - 2214-7853 VL - 3 IS - 4 SP - 1124 EP - 1128 PB - Elsevier Ltd. AN - OPUS4-35688 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hosseini, Seyed M.H. A1 - Ségur, D. A1 - Boehm, Rainer A1 - Gohlke, Dirk A1 - Heckel, Thomas A1 - Riemer, S. A1 - Brackrock, Daniel A1 - Gaal, Mate T1 - Characterization and optimization of ultrasonic tests for inspection of fiber-reinforced plastic composites in energy related applications N2 - Applications of fibre reinforced plastic (FRP) composites in modern industries are increasing due to their considerable advantages such as light weight and excellent mechanical properties. Accordingly, importance of operational safety of modern structures made of advanced composites by ensuring the material quality has led to increasing demands for development of non-destructive evaluation (NDE) systems. In the context of a European project entitled “Validated Inspection Techniques for Composites in Energy Applications” (VITCEA), the aim is to develop and validate traceable procedures for novel NDE techniques with contrasting damage detection capabilities in energy related applications such as wind and marine turbine blades, nacelles, oil and gas flexible risers. Accordingly, VITCEA focuses on optimization of ultrasonic tests (UTs) for quantitative defect detection and quality characterization of FRP structures. In this context, the present study describes the ultrasound field in heterogeneous composite materials. The theoretical predictions are compared with simulation results obtained from CIVA a software package dedicated to NDT simulations based on the asymptotic ray theory. T2 - WCNDT 2016 - - 19th World Conference on Non-Destructive Testing CY - München DA - 13.06.2016 KW - Ultrasonic tests KW - Composite KW - Wave propagation KW - Analytical approach PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-356398 SP - We.4.D.5, 1 EP - 8 AN - OPUS4-35639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 20. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik. KW - Eignungsprüfung KW - Boden KW - MKW KW - PAK KW - Spurenelemente KW - Chrom(VI) KW - Proficiency testing KW - Soil KW - TPH KW - PAH KW - Trace elements KW - Chromium(VI) PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-356424 SP - 1 EP - 228 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35642 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Die neue Technologie-Roadmap "Prozess-Sensoren 4.0" - Chancen für neue Automationskonzepte N2 - Vorstellung der neuen Technologie-Roadmap "Prozess-Sensoren 4.0" T2 - Sitzung des AMA-Wissenschaftsrates CY - Saarbrücken, Germany DA - 16.03.2016 KW - Roadmap KW - Prozess-Sensoren 4.0 KW - Sensoren KW - Industrie 4.0 PY - 2016 AN - OPUS4-35716 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Clever und Smart - Die neuen Prozess-Sensoren 4.0 N2 - Die gravierenden Veränderungen im Umfeld der Informations- und Kommunikationstechnik beeinflussen auch die Prozessautomation und sind zugleich eine Chance. Denn die Automatisierungskonzepte gemäß Industrie 4.0 sichern den Wettbewerbsvorteil einer Volkswirtschaft. Ein zentrales Element bilden dabei smarte Sensoren, die Dienste innerhalb eines Netzwerks bereitstellen und Information daraus nutzen. Die im November 2015 vorgestellte Technologieroadmap Prozess-Sensoren 4.0 [1] zeigt Anforderungen an smarte Prozess-Sensoren auf. Der Beitrag befasst sich mit den Fragen „Was kann der Prozess-Sensor zu Industrie 4.0 beitragen?“ und „Welchen Nutzen bringt Industrie 4.0 für den Prozess-Sensor?“ KW - Technologieroadmap KW - Prozess-Sensoren 4.0 KW - Industrie 4.0 KW - Prozessanalytik PY - 2016 SN - 0178-2320 VL - 58 IS - 3 SP - 28 EP - 35 PB - DIV Deutscher Industrieverlag CY - München AN - OPUS4-35717 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Birgit Angelika A1 - Ziemann, M. A A1 - Pentzien, Simone A1 - Gabsch, T. A1 - Koch, W. A1 - Krüger, Jörg T1 - Technical analysis of a Central Asian wall painting detached from a Buddhist cave temple on the northern Silk Road N2 - A great number of Central Asian wall paintings, archeological materials, architectural fragments, and textiles, as well as painting fragments on silk and paper, make up the so called Turfan Collection at the Asian Art Museum in Berlin. The largest part of the collection comes from the Kucha region, a very important cultural center in the third to ninth centuries. Between 1902 and 1914, four German expeditions traveled along the northern Silk Road. During these expeditions, wall paintings were detached from their original settings in Buddhist cave complexes. This paper reports a technical study of a wall painting, existing in eight fragments, from the Buddhist cave no. 40 (Ritterhöhle). Its original painted surface is soot blackened and largely illegible. Grünwedel, leader of the first and third expeditions, described the almost complete destruction of the rediscovered temple complex and evidence of fire damage. The aim of this case study is to identify the materials used for the wall paintings. Furthermore, soot deposits as well as materials from conservation interventions were of interest. Non-invasive analyses were preferred but a limited number of samples were taken to provide more precise information on the painting technique. By employing optical and scanning electron microscopy, energy dispersive X-ray spectroscopy, micro X-ray fluorescence spectroscopy, X-ray diffraction analysis, and Raman spectroscopy, a layer sequence of earthen render, a ground layer made of gypsum, and a paint layer containing a variety of inorganic pigments were identified. KW - Wall paintings KW - Central Asia KW - Silk Road KW - Pigments KW - Microscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-357297 DO - https://doi.org/10.1179/2047058414Y.0000000152 VL - 61 IS - 2 SP - 113 EP - 122 PB - Routledge Taylor & Francis Group CY - London AN - OPUS4-35729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bierstedt, Andreas T1 - Development of a laser induced plasma ion source coupled to ambient mass spectrometry N2 - Only a few years after the invention of the laser, the concept of laser microprobe mass spectrometry (LMMS), a technique which employed intense laser radiation for ion generation, was introduced. In these early studies at excessive irradiation microplasma formation could be observed to be an effective channel for ion formation. However, this plasma generation in vacuum led to undesired distortions of the mass analyzers and, thus, was discarded as an analytical ion source. Under ambient conditions, the surrounding air effectively cools the plasma cloud, making the plasma more controllable. The resulting laser induced plasma is nowadays commonly used in laser induced breakdown spectroscopy (LIBS) applications as excitation source for optical emission spectroscopy experiments. However, little effort has been made to introduce a LIBS plasma as a promising ion source for ambient mass spectrometry. The main hindrance is the transient character of laser induced plasmas that typically only has a lifetime on the order of several microseconds. This drastically reduces the duty cycle of these plasma sources. After these microseconds, the generated ions recombinate to uncharged atoms and even newly bound molecules, making them inaccessible to mass-to-charge analyzers. The advent of high repetition lasers together with the ever growing knowledge about manipulation of charged species at atmospheric pressures allow overcoming these obstacles. This presentation will introduce an ionization scheme using a laser induced plasma as the primary ion source. We believe that this novel ionization strategy will pave the way for future applications in ambient mass spectrometry. T2 - 5. Berliner Chemie Symposium CY - Berlin, Germany DA - 12.04.2016 KW - Laser induced plasma KW - Time-of-flight mass spectrometry KW - Ambient mass spectrometry KW - Ionization KW - Laser induziertes Plasma KW - Flugzeitmassenspektrometer KW - Atmosphärendruckmassenspektrometrie KW - Ionisierung PY - 2016 AN - OPUS4-35732 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tschaikner, Martin T1 - Laminographic inspection of large fibre composite structures at the production site N2 - Short describtion of the technology and results of laminography. T2 - 7th International Symposium on NDT in Aerospace CY - Bremen, Germany DA - 16.11.2015 KW - Laminography KW - 3D Reconstruction KW - Inspection of CFRP KW - Laminografie KW - 3D Rekonstruktion KW - Untersuchung von CFK PY - 2015 AN - OPUS4-35610 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Innovative seismic and resistivity tools for determining the diameter of jet grouting columns N2 - Jet grouting is used for soil improvement, foundation support and groundwater low control all over the world. It is well accepted and subject of standardization in many countries. However, some issues with the method remain. As the grout columns are produced in the subsurface without visual control in an often inhomogeneous soil, the prediction of the column’s diameter is still a challenge. All methods applied so far have their limitations. The approach presented in this study is twofold. At Colorado School of Mines a resistivity probe has been developed, which is pushed into the fresh grout directly after production. ERT sections are measured and inverted. Given some background information is available, the diameter of the columns can be evaluated. At BAM the focus has been on post-production investigations using seismic borehole methods. After hardening of the concrete seismic waves are sent through the column downhole (sensors placed in a casing in the column’s axis, source on top) and crosshole (source and sensor in boreholes on opposite sides of the column). We have developed a scheme to evaluate the diameter of the column based on travel time measurements without calibration. As this method is eventually more time and cost intensive we assume its application mainly for test columns. These are casted and dug out for visual inspection to determine appropriate grouting parameters. Our method would replace the often very cost intensive visual inspection. Both approaches have been tested at three test columns produced at BAM’s test site at Horstwalde, Germany and on an actual constructions site. Both methods have been in good agreement with the diameters predicted by the jet grouting contractors, which were confirmed in one case by mechanical measurements. T2 - SAGEEP 2016 CY - Denver, CO, USA DA - 20.03.2016 KW - Jet grouting KW - Diameter KW - Quality assurance KW - Seismic PY - 2016 AN - OPUS4-35708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andres, S. A1 - Hansen, Ulf A1 - Niemann, B. A1 - Palavinskas, R. A1 - Lampen, A. T1 - Determination of the isoflavone composition and estrogenic activity of commercial dietary supplements based on soy or red clover N2 - Dietary supplements high in isolated isoflavones are commercially available for human consumption primarily to alleviate menopausal symptoms in women. The isoflavone composition, quantity and importantly their estrogenic potency are poorly standardised and can vary considerably between different products. The aim of this study was to analyse the isoflavone composition of 11 dietary supplements based on soy or red clover using the HPLC/MS/MS technique. Furthermore, we investigated the transactivational potential of the supplements on the estrogen receptors (ER), ERα and ERβ, performing luciferase reporter gene assays. As expected, we found that the isoflavone composition varies between different products. The measured total isoflavone contents in various supplements were mostly comparable to those claimed by the manufacturers in their product information. However expressing the isoflavone content as isoflavone aglycone equivalents, soy-based supplements had a clearly lower quantity compared to the manufacturer information. All supplements transactivated more or less ERα and ERβ with a preference for ERβ. The transactivational efficiency exceeded partly the maximal 17β-estradiol induced ER activation. While the different soy-based supplements revealed similar transactivation potential to both ERs, red clover-based supplements differed considerably. We conclude that different commercial dietary supplements based on soy or red clover vary in their isoflavone composition and quantity. They are estrogenically active, although especially the red clover-based supplements show considerable differences in their estrogenic potential to ERα and ERβ. Thus, different isoflavone-rich products cannot be necessarily compared regarding possible biological effects. KW - estrogenic activity KW - HPLC/MS/MS technique KW - Estrogen receptor (ER) KW - nutritional supplements PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-357093 DO - https://doi.org/10.1039/C5FO00308C IS - 6 SP - 2017 EP - 2025 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-35709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoesl, Simone A1 - Neumann, B. A1 - Techritz, Sandra A1 - Sauter, G. A1 - Simon, R. A1 - Schlüter, H. A1 - Linscheid, M. W. A1 - Theruing, F. A1 - Müller, Larissa A1 - Jakubowski, Norbert T1 - Internal standardization of LA-ICP-MS immunoimaging via printing of universal metal spiked inks onto tissue sections N2 - Formalin-fixed paraffin-embedded (FFPE) specimen from biopsy materials are a widespread sample format for pathologists and medical researchers. Pathologists are archiving vast numbers of FFPE samples which can be stored for decades. Conventional immunohistochemical staining (IHC) of biomarkers on FFPE tissue sections is one of the most important analytical techniques for cancer diagnosis and pathology in general. However standardization for IHC samples and quality management is tedious and differs significantly from clinic to clinic. Combining established IHC staining strategies with modern mass spectrometry mediated methods would increase it`s potential and enable access of large FFPE archives for multiplexed quantitation purposes. In this work element mass spectrometry and a new ink-jet printed internal standardization approach was successfully combined with IHC staining to facilitate quantitative multiplex assays for archived FFPE samples. The printing strategy improves elemental image resolution and reproducibility of paraffin embedded breast cancer tissue sections in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) using conventional IHC staining as a model system to investigate the new capabilities of this technique. For the internal standardization we applied a conventional CD-ink-jet printer to print a metal spiked ink onto the top of thin layer tissue sections with constant density. Printing was carried out in a direct comparison to an iodination of the tissue section as previously described as an alternative standardization method. The use of the printed internal standard allowed correction of the fluctuation during the laser ablation process and compensated instrumental drift effects. Mediated by the ink correction approach we achieved better signal-to-background-ratios (SBR) of 74 and better spatial resolution of 30 µm compared to iodination (SBR=23). This improved performance was demonstrated on tumorous areas in FFPE breast cancer tissue sections and allowing detection of Her-2 in tumorous areas of this tissue with significantly improved contrast. KW - Internal standardization KW - LA-ICP-MS KW - Immuno imaging PY - 2016 DO - https://doi.org/10.1039/c5ja00409h SN - 0267-9477 SN - 1364-5544 VL - 31 IS - 3 SP - 801 EP - 808 AN - OPUS4-35711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Die neue Technologie-Roadmap „Prozess-Sensoren 4.0“ – Chancen für neue Automationskonzepte N2 - Derzeit finden gravierende Veränderungen im Umfeld der Informations- und Kommunikationstechnik statt, die eine große Chance für die optimierte Prozessführung und Wertschöpfung mit darauf abgestimmten vernetzt kommunizierenden Sensoren bieten. Diese Art „smarte“ Sensoren stellen Dienste innerhalb eines Netzwerks bereit und nutzen Informationen daraus. Dieses ist die Voraussetzung für die Realisierung von Cyber Physical Systems (CPS) innerhalb zukünftiger Automatisierungskonzepte für die Prozessindustrie, wie sie auch durch das Zukunftsprojekt „Industrie 4.0“ adressiert werden. Initiiert von NAMUR und VDI/GMA und unter Mitwirkung der Unternehmen ABB, BASF, BTS, Bilfinger Maintenance, Endress+Hauser, Evonik, Festo, Krohne, Lanxess, Siemens, des Fraunhofer ICT, der HS Reutlingen und der BAM (Projektleitung) entstand jetzt die grundlegend aktualisierte und überarbeitete Technologie-Roadmap „Prozess-Sensoren 4.0“, die am 06. November 2015 auf der NAMUR-Hauptsitzung in Bad Neuenahr wurde. T2 - Sitzung des fms/ProcessNet-Gemeinschafts-Ausschusses „Sensoren und Sensorsysteme“ CY - Frankfurt am Main, Germany DA - 28.01.2016 KW - Roadmap KW - Prozess-Sensoren 4.0 KW - Sensoren KW - Industrie 4.0 PY - 2016 AN - OPUS4-35715 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weller, Michael G. T1 - Quality issues of research antibodies N2 - According to several recent studies, an unexpectedly high number of landmark papers seem to be not reproducible by Independent laboratories. Nontherapeutic antibodies used for research, diagnostic, food analytical, environmental, and other purposes play a significant role in this matter. Although some papers have been published offering suggestions to improve the situation, they do not seem to be comprehensive enough to cover the full complexity of this issue. In addition, no obvious improvements could be noticed in the field as yet. This article tries to consolidate the remarkable variety of conclusions and suggested activities into a more coherent conception. It is concluded that funding agencies and journal publishers need to take first and immediate measures to resolve these problems and lead the way to a more sustainable way of bioanalytical research, on which all can rely with confidence. KW - reproducibility crisis KW - irreproducibility KW - replication KW - paper retraction KW - peer reviewimmunochemistry KW - immunoassay KW - ligand binding assay KW - monoclonal antibody KW - quality control KW - cross-reactivity KW - non-specific binding KW - selectivity PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-356254 DO - https://doi.org/10.4137/ACI.S31614 SN - 1177-3901 VL - 11 SP - 21 EP - 27 PB - Libertas Academica CY - Auckland, New Zealand AN - OPUS4-35625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Ebert, S. A1 - Lazik, D. A1 - Bartholmai, Matthias ED - Nicoletto, G. ED - Dan Pastrama, S. ED - Emri, I. T1 - Inverse calibration routine for linear soil gas sensors N2 - Gas sensors in linear form based on the measuring principle of gas selective permeability through a membrane were developed and introduced for the detection and quantification of gas concentrations. A current field study focuses on measuring CO2 concentrations for a spatially distributed monitoring of subsurface CO2 gas storage sites in near real time. A 400 m² test site and a corresponding laboratory system were built up to characterize, validate, and optimize the sensor. A calibration routine was developed, which can be applied subsequently to underground installation. First measurement results indicate the potential of the method. T2 - 32nd Danubia Adria Symposium on Advances in Experimental Mechanics CY - Starý Smokovec, Slovakia DA - 22.09.2015 KW - Linear sensor KW - Distributed sensor KW - Subsurface monitoring KW - Gas storage areas KW - Membrane-based gas sensing KW - Calibration PY - 2016 UR - http://www.sciencedirect.com/science/article/pii/S221478531600256X DO - https://doi.org/doi:10.1016/j.matpr.2016.03.051 SN - 2214-7853 VL - 3 IS - 4 SP - 1074 EP - 1078 PB - Elsevier Ltd. AN - OPUS4-35633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Akcakayiran, D. A1 - Grigoriev, D.O. A1 - Shchukin, D.G. T1 - Characterization of micro- and nanocapsules for self-heating anti-corrosion coatings by high-resolution SEM with coupled transmission mode and EDX N2 - The observation of morphological details down to the nanometer range of the outer surface of micro-, submicro- and nanoparticles in a high-resolution scanning electron microscope (SEM) was extended with in-depth observation by enabling the transmission mode in the SEM, i.e. TSEM. The micro- and nanocapsules characterized in this study were fabricated as depots for protective agents to be embedded in innovative self-healing coatings. By combining the two imaging modes (upper and in-depth observation) complementing each other a better characterisation by a more comprehensive interpretation of the 'consistency' of the challenging specimens, e.g. including details 'hidden' beyond the surface or the real specimen shape at all, has been attained. Furthermore, the preparation of the quasi electron transparent samples onto thin supporting foils enables also elemental imaging by energy dispersive X-ray spectroscopy (EDX) with high spatial resolution. Valuable information on the elemental distribution in individual micro-, submicro- and even nanocapsules completes the '3D' high resolution morphological characterization at the same multimodal SEM/TSEM/EDX system. KW - Scanning electron microscopy (SEM) KW - High-resolution transmission in SEM (TSEM) KW - Energy dispersive X-ray spectroscopy (EDX) KW - Micro- and nanocapsules KW - Anti-corrosion coatings PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-304201 DO - https://doi.org/10.1039/c3an01717f SN - 0003-2654 SN - 1364-5528 VL - 139 IS - 8 SP - 2004 EP - 2010 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-30420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pohl, Rainer A1 - Kreutzbruck, Marc A1 - Commandeur, Colin A1 - Pelkner, Matthias T1 - Development of adapted GMR-probes for automated detection of hidden defects in thin steel sheets N2 - Thin steel sheets with a thickness of 0.3 mm and less are the base materials of many everyday life products (cans, batteries, etc.). Potential inhomogeneities such as non-metallic inclusions inside the steel can lead to a rupture of the sheets when it is formed into a product such as a beverage can. Therefore, there is a need to develop automated NDT techniques to detect hidden defects and inclusions in thin sheets during production. For this purpose Tata Steel Europe and BAM, the Federal Institute for Materials Research and Testing (Germany), collaborate in order to develop an automated NDT-system. Defect detection systems have to be robust against external influences, especially when used in an industrial environment. In addition, such a facility has to achieve a high sensitivity and a high spatial resolution in terms of detecting small inclusions in the μm-regime. In a first step, we carried out a feasibility study to determine which testing method is promising for detecting hidden defects and inclusions inside ferrous thin steel sheets. Therefore, two methods were investigated in more detail – magnetic flux leakage testing (MFL) using giant magneto resistance sensor arrays (GMR) as receivers [1,2] and eddy current testing (ET). The capabilities of both methods were tested with 0.2 mm-thick steel samples containing small defects with depths ranging from 5 μm up to 60 μm. Only in case of GMRMFL-testing, we were able to detect parts of the hidden defects with a depth of 10 μm trustworthily with a SNR better than 10 dB. Here, the lift off between sensor and surface was 250 μm. On this basis, we investigated different testing scenarios including velocity tests and different lift offs. In this contribution we present the results of the feasibility study leading to first prototypes of GMR-probes which are now installed as part of a demonstrator inside a production line. T2 - Review of Progress in Quantitative Nondestructive Evaluation CY - Minneapolis, MN, USA DA - 26.07.2015 KW - GMR KW - NDT PY - 2016 DO - https://doi.org/10.1063/1.4940464 VL - 1706 SP - Article Number: 020018 PB - Amer institute physics CY - Melville, New York, USA AN - OPUS4-36100 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moraleja, I. A1 - Esteban-Fernández, Diego A1 - Lázaro, A. A1 - Humanes, B. A1 - Neumann, B. A1 - Tejedor, A. A1 - Mena, M. A1 - Jakubowski, Norbert A1 - Gómez-Gómez, M. T1 - Printing metal-spiked inks for LA-ICP-MS bioimaging internal standardization: comparison of the different nephrotoxic behavior of cisplatin, carboplatin, and oxaliplatin N2 - The study of the distribution of the cytostatic drugs cisplatin, carboplatin, and oxaliplatin along the kidney may help to understand their different nephrotoxic behavior. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) allows the acquisition of trace element images in biological tissues. However, results obtained are affected by several variations concerning the sample matrix and instrumental drifts. In this work, an internal standardization method based on printing an Ir-spiked ink onto the surface of the sample has been developed to evaluate the different distributions and accumulation levels of the aforementioned drugs along the kidney of a rat model. A conventional ink-jet printer was used to print fresh sagittal kidney tissue slices of 4 μm. A reproducible and homogenous deposition of the ink along the tissue was observed. The ink was partially absorbed on top of the tissue. Thus, this approach provides a pseudo-internal standardization, due to the fact that the ablation sample and internal standard take place subsequently and not simultaneously. A satisfactory normalization of LA-ICP-MS bioimages and therefore a reliable comparison of the kidney treated with different Pt-based drugs were achieved even for tissues analyzed on different days. Due to the complete ablation of the sample, the transport of the ablated internal standard and tissue to the inductively coupled plasma-mass spectrometry (ICP-MS) is practically taking place at the same time. Pt accumulation in the kidney was observed in accordance to the dosages administered for each drug. Although the accumulation rate of cisplatin and oxaliplatin is high in both cases, their Pt distributions differ. The strong nephrotoxicity observed for cisplatin and the absence of such side effect in the case of oxaliplatin could explain these distribution differences. The homogeneous distribution of oxaliplatin in the cortical and medullar areas could be related with its higher affinity for cellular transporters such as MATE2-k. KW - Bioimaging KW - LA-ICP-MS KW - Cisplatin KW - Standardization KW - Printed internal standard KW - Pt-based drugs KW - Nephrotoxicity PY - 2016 DO - https://doi.org/10.1007/s00216-016-9327-0 SN - 1618-2642 SN - 1618-2650 VL - 408 IS - 9 SP - 2309 EP - 2318 AN - OPUS4-36110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ryan, T. M. A1 - Xun, Y. A1 - Cowieson, N. P. A1 - Mata, J. P. A1 - Jackson, A. A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Kirby, N. A1 - McGillivray, D. T1 - Combined pressure and temperature denaturation of ribonuclease A produces alternate dentatured states N2 - Protein folding, unfolding and misfolding have become critically important to a range of health and industry applications. Increasing high temperature and high pressure are used to control and speed up reactions. A number of studies have indicated that these parameters can have a large effecton protein structure and function. Here we describe the additive effects of these parameters on the small angle scattering behaviour of ribonuclease A. We find that alternate unfolded structures can be obtained with combined high pressure and temperature treatment of the protein. KW - Protein unfolding KW - Small angle scattering KW - Ribonuclease A KW - High pressure PY - 2016 DO - https://doi.org/10.1016/j.bbrc.2016.03.135 SN - 0006-291X IS - 473 SP - 834 EP - 839 PB - Academic Press Inc Elsevier Science CY - San Diego, USA AN - OPUS4-36052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hachmöller, O. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Aichler, M. A1 - Radtke, Martin A1 - Dietrich, D. A1 - Schwamborn, K. A1 - Lutz, L. A1 - Werner, M. A1 - Sperling, M. A1 - Walch, A. A1 - Karst, U. T1 - Elemental bioimaging and speciation analysis for the investigation of Wilsons disease using μXRF and XANES N2 - A liver biopsy specimen from a Wilson’s disease (WD) patient was analyzed by means of micro-X-ray fluorescence (mXRF) spectroscopy to determine the elemental distribution. First, bench-top mXRF was utilized for a coarse scan of the sample under laboratory conditions. The resulting distribution maps of copper and iron enabled the determination of a region of interest (ROI) for further analysis. In order to obtain more detailed elemental information, this ROI was analyzed by synchrotron radiation (SR)-based mXRF with a beam size of 4 mm offering a resolution at the cellular level. Distribution maps of additional elements to copper and iron like zinc and manganese were obtained due to a higher sensitivity of SR-mXRF. In addition to this, X-ray absorption near edge structure spectroscopy (XANES) was performed to identify the oxidation states of copper in WD. This speciation analysis indicated a mixture of copper(I) and copper(II) within the WD liver tissue. KW - progressive hepatolenticular degeneration KW - mXRF Micro-X-ray fluorescence spectroscopy KW - XANES X-ray absorption near edge structure spectroscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-360811 DO - https://doi.org/10.1039/C6MT00001K SN - 1756-5901 SN - 1756-591X PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-36081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Process analytical technology for resource analytics – The role of reference materials N2 - Resource Analytics with the help of process analytical technology and the use of online methods is becoming increasingly important for mining and processing technologies and for the recovery of raw materials from secondary raw materials. Current online analytical methods like laser-induced breakdown spectroscopy (LIBS), X-ray fluorescence analysis (RFA), or Raman spectroscopy for the characterization of primary and secondary raw materials are increasingly being used in close association with the technologies for exploration and extraction, mechanical and metallurgical processing, as well as for recycling. Because of the complex matrices such methods are a considerable challenge at the same time. The use of reference materials, which are derived from appropriate matrices, can considerably shorten calibration and method development times. As an example, the development of an online process control method for recovery of phosphorus from sewage sludge ashes is discussed. A combination of LIBS and RFA was developed for the determination of element contents in sewage sludge ashes and their products coming from a thermo-chemical reprocessing step, which removes pollutants. T2 - Analytica Conference CY - München, Germany DA - 10.05.2016 KW - Resource Analytics KW - Ressourcenanalytik KW - Prozessanalytik KW - Process Analytical Technology PY - 2016 AN - OPUS4-36043 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illner, M. T1 - Systematic approach for online spectroscopy in technical systems - Experimental design for Raman Spectroscopy in micro emulsions N2 - Hydroformylation represents an important homogeneous catalyzed process, which is widely used within chemical industry. Usually applied for short-chained alkenes like Propene and Butene aldehydes obtained from alkenes >C6 are relevant intermediates in production of plasticizers, surfactants and polymers. Today the active catalyst species is often based on valuable Rhodium complexes in aqueous solution. This implies the problem of limited water solubility of the reactants, which is acceptable for short chain lengths, but states a problem in case of higher alkenes. Along with that efficient separation and recycling of the catalyst becomes more complicated. There are different approaches tackling this problem, e.g., by using of salt formation in the BASF process or downstream distillation within the Shell process. Another promising approach is the processing within a microemulsion by using a suitable surfactant system. This maintains a large interface between catalyst and reactants, as well as the possibility of catalyst recycling via downstream phase separation in a settler. Optimized processing within the three-phase region in accordance with Kahlweit fish leads to an efficient product separation, while the valuable catalyst and surfactant can be recycled into the process. In this work we present reaction monitoring of Rh-catalyzed hydroformylation of 1 dodecene. Experiments were conducted on a specialized laboratory setup, which allows coupling of different online spectroscopic methods (Raman, HR-NMR, LF-NMR, UV/VIS) under process-similar conditions. The focus of this contribution lies on results of high-resolution Online-NMR obtained during calibration experiments for development of a multivariate model for Raman spectroscopy, which will be part of another contribution. T2 - Analytica Conference CY - München, Germany DA - 10.05.2016 KW - Prozess-Sensoren KW - Process Analytical Technology KW - Hydroformylation KW - Design of Experiments PY - 2016 AN - OPUS4-36044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sieg, H. T1 - Artificial digestion of aluminium-containing nanomaterials and their effects on the gastrointestinal tract in vitro N2 - Although aluminium is one of the most common elements in the biosphere, up to now little is known about its impact on human health. aluminium and its chemical derivatives are highly abundant in food, food contact materials and consumer products. Humans are exposed to aluminium via the gastrointestinal tract (GI tract). Exposition can change substantially due to consumer behavior since aluminium is also a compound of numerous food additives. Recently, aluminium exposition is increasingly considered to cohere with cancer and neurodegenerative disorders. Lately, due to an increasing attentiveness on this topic, limiting values for food additives have been tightened by the EFSA. However, cellular effects of aluminium and especially aluminium-containing nanomaterials, that represent a significant part of chemicals found in food products, are widely unknown and in the focus of our research activities, for example in the bilateral SolNanoTOX project. We established an in vitro simulation system of the GI tract, where nanomaterials undergo the different physiological, chemical and proteinbiochemical conditions of saliva, gastric juice and the intestine. The artificially digested nanomaterials, as well as soluble aluminium chloride as ionic control substance, were subjected to several analytical and biochemical methods to characterize their change of appearance and their cytotoxic effects on intestinal cellular models. We observed the fate of the nanomaterials during typical pH-values of saliva, gastric and intestinal juice with Dynamic light scattering measurements and ICP-MS in the single particle mode. After observable disappearance at pH 2 the particles recovered in the simulated intestinal fluid. The simulation of the GI tract, mainly the change of pH settings, can lead to a certain chemical activation of aluminium that can increase bioavailability in the intestine after oral uptake of aluminium-containing food products. In vitro assays like CTB, MTT and cellular impedance measurements showed that there were no acute cytotoxic effects measurable after a period up to 48h after incubation, comparable to undigested particles. In contrast, high amounts of aluminium ions showed synergistic effects on cell viability compared to non-digested aluminium ions. Although toxicological potential of Al ions to healthy tissue appears to be low, increased hazardous potential cannot be ruled out to pre-damaged tissue and can have a relevance in risk assessment for special consumer groups with for example chronical intestinal inflammation or dietary eating behavior combined with high exposure to Al-containing food products. T2 - 82nd Annual Meeting of the German Society for Experimental and Clinical Pharmacology and Toxicology CY - Berlin, Germany DA - 29.02.2016 KW - Nanoparticles KW - Digestion KW - SAXS KW - Cytotoxicity PY - 2016 AN - OPUS4-36026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Road-map for purity determination N2 - From several CCQM studies (CCQM-P107, CCQM-K72 and CCQM-P149) conclusions can be drawn for the purity assessment of a pure (metallic) element. These conclusions will be put together in this document in order to assist all NMIs/DIs in performing a purity assessment, whenever needed. T2 - CCQM IAWG Meeting CY - Paris, France DA - 18.04.2016 KW - Purity KW - Metrology KW - Traceability PY - 2016 AN - OPUS4-36063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Applicability of CCQM-P149 to support CMCs N2 - CCQM-P149 is an attempt to obtain a snapshot on actual procedures the NMIs and DIs within CCQM-IAWG applied to the purity characterization of their “fit for purpose” elemental Standards. This presentation describes how the results of CCQM-P149 may be used to underpin calibration and measurement capabilities being claimed in the BIPM database. T2 - CCQM IAWG Meeting CY - Paris, France DA - 18.04.2016 KW - metrology KW - purity KW - traceability PY - 2016 AN - OPUS4-36064 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Using information from CC Tables for supporting CMC claims N2 - Core capability tables list the skills and experiences, which at least partially are needed to successfully carry out a specific analytical task within the IAWG. The required skills and experiences, so-called core capabilities (CC), are identified for each analytical procedure. The summarized CC tables are listed in the appendix of each report on the corresponding key comparison or pilot study. These CC tables enable us to demonstrate that we have the analytical procedure we claim under control by means of other Key Comparison, which do not exactly meet the claimed calibration and measurement capability. This is especially important for: a) fields where no Key Comparison is available, b) Revision of CMC claims or c) when a participation in a Key Comparison was not possible. T2 - CCQM IAWG Meeting CY - Paris, France DA - 18.04.2016 KW - metrology KW - traceability PY - 2016 AN - OPUS4-36066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - 10. Interdisziplinäres Doktorandenseminar N2 - Das 10. Interdisziplinäre Doktorandenseminar wendet sich an Arbeitskreise, die auf den Gebieten der Prozessanalytik, Sensoren, Datenauswertung, Automation und angrenzenden Fachthemen tätig sind. Sie wurde wie immer organisiert von den Arbeitskreisen „Prozessanalytik“, „Chemo- und Biosensoren“, „Chemometrik und Qualitätsmanagement“ sowie „Elektrochemie“ der GDCh-Fachgruppe „Analytische Chemie“ in Kooperation mit den kreativen jungen Verfahrensingenieuren (kjVIs). Die Fachvorträge zeichneten sich durch ihre Vielfalt an Themen und Anwendungsmöglichkeiten aus. Für alle Themen zeichnet sich gleichermaßen der Trend ab, dass neben dem Erzeugen analytischer oder sensorischer Daten auch ein intelligentes Datenmanagement gefordert ist, um die Informationen zu Entscheidungsdaten zu verarbeiten und entsprechend zu präsentieren. Auch die Poster zeigten eine große Vielfalt an Forschungsbereichen. Von der Charakterisierung und Identifizierung von Pollen mit Hilfe von SERS, MALDI-TOF-MS und neuronalen Netzen, über Bioprozessüberwachung/-Regelung von CHO-Zellkultivierungen, bis hin zur Prozesskontrolle an hoch trüben Polymerdispersionen mit PDW-Spektroskopie, wurde ein breites Themenspektrum präsentiert.“ T2 - 10. Doktorandentagung CY - Berlin, Germany DA - 28.02.2016 KW - Doktorandentagung KW - Prozessanalytik KW - Sensoren PY - 2016 SP - 1 EP - 34 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin, Germany AN - OPUS4-36149 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Staude, Andreas T1 - Computed tomography and its potential for cultural heritage studies N2 - Since the advent of industrial computed tomography (CT), this new analysis method has been used also for the investigation of objects of cultural heritage and art. CT provides the possibility to determine the inner and outer surfaces and to investigate the material structure without causing damage to the valuable objects. In this talk I will present examples of measurements performed at BAM, which demonstrate what CT can do for objects of diverse materials and for different objectives. T2 - Italian-German Worshop on "Technology and infrastructures for Cultural Heritage" CY - Bode-Museum, Berlin, Germany DA - 12.04.2016 KW - Computed tomography KW - Computertomographie KW - Cultural heritage KW - Art KW - Archaeology KW - Kulturelles Erbe KW - Kunst KW - Archäologie PY - 2016 AN - OPUS4-36162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Forler, D. A1 - Schmidt, J. P. A1 - Staude, Andreas T1 - Ein Becken aus Beckentin! - Fund des Monats Mai 2016 N2 - Bronzezeitlicher Hortfund in Mecklenburg-Vorpommern mit CT-Untersuchung an der BAM KW - Computertomographie KW - Hortfund KW - Bronzezeit KW - Mecklenburg-Vorpommern PY - 2016 UR - http://www.kulturwerte-mv.de/cms2/LAKD1_prod/LAKD1/de/Landesarchaeologie/Fund_des_Monats/index.jsp SP - 1 EP - 3 CY - Schwerin AN - OPUS4-36163 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - The Analytical centrifuge – an additional tool to optimize ceramic slurries for spray drying N2 - Spray drying is a widely used process step in ceramic technology to convert fine grained raw powders to free-flowing granules. Type and amount of the organic additives (dispersants, binders and plasticizers) define viscosity and stability of the slurry, the granulate structure and the compaction behaviour. Alumina and Zirconia powders were characterized with regard to particle size, shape and specific surface area (BET). Zeta-potential measurements by Stabino® were used to investigate the effect of different dispersants on slurry stability. Unfortunately, this method is restricted to suspensions with less than about 30% by weight of solid content. The multi-sample analytical centrifuge LUMiSizer® overcomes this problem. This device enables analysis of the separation behaviour of suspensions over a wide range of solid content. On the basis of position and time resolved photometric detection of transmitted light, it is possible to determine the instability index, the sedimentation velocity, and the sediment height in dependence of type and amount of organic additives at various centrifugal accelerations. Additional information is obtained from the shape of the transmission profiles. Based on LUMiSizer® measurements, suitable additive concentrations were derived. Thereby, the number of investigations by viscometry and spray drying experiments can be significantly reduced. Finally, it was possible to produce alumina, zirconia and ZTA aqueous slurries with up to 80 weight-% of solid. The optimized suspensions were successfully spray dried and the resulted granules show good compaction behaviour. T2 - Jahrestagung der Deutschen Keramischen Gesellschaft und Symposium Hochleistungskeramik CY - Freiberg, Germany DA - 07.03.2016 KW - Analytical centrifuge KW - Ceramic suspension KW - Slurry KW - Spray drying KW - Granules PY - 2016 AN - OPUS4-36130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neukammer, J. A1 - Hussels, M. A1 - Kummrow, A. A1 - Devonshire, A. A1 - Foy, C. A1 - Huggett, J. A1 - Parkes, H. A1 - Zel, J. A1 - Milavec, M. A1 - Schimmel, H. A1 - Unger, Wolfgang A1 - Akgoz, M. A1 - McHugh, V. A1 - Grunert, H.-P. A1 - Zeichhardt, H. T1 - Survey results on nucleic acid tests of infectious diseases: present status and need for rapid and patient near diagnostics N2 - This survey will discuss current and emerging isothermal and rapid polymerase chain reaction (PCR) based nucleic acid amplification methods for patient near diagnostics. To assess the clinical need of rapid diagnostics for infectious diseases based on nucleic acid tests (NATs) we performed and analysed a questionnaire among laboratories participating in corresponding INSTAND ring trials for external quality assurance. The questions concerning new amplification technologies like isothermal nucleic acid amplification, potentially suited to significantly decrease turnaround times, were complemented by questions to evaluate the present status of NATs. Besides end-users, companies were also addressed by sending out a manufacturer specific questionnaire. Analysis of the answers from 48 laboratories in 14 European countries revealed that a much shorter turnaround time is requested for selected pathogens compared to about 2 h or longer when applying temperature cycling amplification, i.e. PCR. In this context, most frequently mentioned were MRSA, norovirus, influenza A and B viruses, cytomegalovirus (CMV) as well as hepatitis B virus (HBV) and hepatitis C virus (HCV). At present, 8% of the laboratories having participated in this survey apply isothermal amplification of nucleic acid to identify infectious pathogens. KW - Nucleic acid tests KW - Infectious diseases KW - Virus detection KW - Bacteria detection KW - Isothermal nucleic acid amplification KW - Status report KW - Questionnaire KW - NAT KW - PCR PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:0183-lab0000160 UR - http://www.egms.de/static/en/journals/lab/2015-6/lab000016.shtml DO - https://doi.org/10.3205/lab000016 SN - 1869-4241 VL - 6 SP - 1 EP - 11 PB - GMS CY - Düsseldorf AN - OPUS4-36133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zientek, Nicolai A1 - Laurain, C. A1 - Meyer, Klas A1 - Paul, Andrea A1 - Engel, D. A1 - Guthausen, G. A1 - Kraume, M. A1 - Maiwald, Michael T1 - Automated data evaluation and modelling of simultaneous F-19-H-1 medium-resolution NMR spectra for online reaction monitoring N2 - Medium-resolution nuclear magnetic resonance spectroscopy (MR-NMR) currently develops to an important analytical tool for both quality control and processmonitoring. In contrast to high-resolution onlineNMR (HR-NMR),MR-NMRcan be operated under rough environmental conditions. A continuous re-circulating stream of reaction mixture fromthe reaction vessel to the NMR spectrometer enables a non-invasive, volume integrating online analysis of reactants and products. Here, we investigate the esterification of 2,2,2-trifluoroethanol with acetic acid to 2,2,2-trifluoroethyl acetate both by 1H HR-NMR (500MHz) and 1H and 19F MRNMR (43MHz) as amodel system. The parallel online measurement is realised by splitting the flow,which allows the adjustment of quantitative and independent flow rates, both in the HR-NMR probe as well as in the MR-NMR probe, in addition to a fast bypass line back to the reactor. One of the fundamental acceptance criteria for online MR-MNR spectroscopy is a robust data treatment and evaluation strategy with the potential for automation. The MR-NMR spectra are treated by an automated baseline and phase correction using the minimum entropy method. The evaluation strategies comprise (i) direct integration, (ii) automated line fitting, (iii) indirect hard modelling (IHM) and (iv) partial least squares regression (PLS-R). To assess the potential of these evaluation strategies for MR-NMR, prediction results are compared with the line fitting data derived from the quantitative HR-NMR spectroscopy. Although, superior results are obtained from both IHM and PLS-R for 1H MR-NMR, especially the latter demands for elaborate data pretreatment, whereas IHM models needed no previous alignment. KW - NMR KW - 1H-NMR KW - 19F-NMR KW - Medium-resolution NMR KW - Online NMR KW - Quantitative NMR KW - Reaction monitoring KW - Data processing KW - Automation KW - Process analytical technology KW - IHM KW - Indirect hard modeling KW - Chemometrics KW - PLS-R KW - Partial least squares regression PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/mrc.4216/abstract DO - https://doi.org/doi:10.1002/mrc.4216 VL - 54 SP - 513 EP - 520 PB - John Wiley & Sons, Ltd CY - Hoboken, New Jersey, USA AN - OPUS4-36135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael A1 - Sperling, M. A1 - Huber, C. A1 - Hayen, H. A1 - Teutenberg, T. A1 - Belder, D. A1 - Karst, U. A1 - Hagenhoff, B. A1 - Vogel, M. T1 - Prozessanalytik: Spektroskopie und Miniaturisierung N2 - Forderungen nach höherer Geschwindigkeit und die Komplexität der Fragen geben der analytischen Chemie neue Impulse. So nutzt die Prozessanalytik gepulste Ramanspektrometer, die Elemente Arsen und Quecksilber dominieren die Forschung in der Speziesanalytik, und die Omics-Techniken entwickeln sich zu Multi-Omics-Ansätzen. Ambiente MS-Techniken benötigen keine aufwendige Probenvorbereitung, multidimensionale Trenntechniken werden verstärkt in der Routine eingesetzt, und Chip-basierte Trennungen fallen durch Schnelligkeit auf. Molekülspektroskopie und Massenspektrometrie dominieren die bildgebenden Verfahren, und die Lateralauflösung der ToF-Sekundärionenmassenspektrometrie hat sich bei Oberflächenuntersuchungen verbessert. KW - Prozessanalytik KW - Quanten-Kaskadenlaser KW - Photonendichtewellen-Spektroskopie KW - Gepulste Ramanspektrometer KW - Partikelmesstechnik KW - Prozesssensoren PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-361371 UR - http://onlinelibrary.wiley.com/doi/10.1002/nadc.20164046080/abstract DO - https://doi.org/10.1002/nadc.20164046080 SN - 1868-0054 VL - 64 IS - 5 SP - 497 EP - 508 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-36137 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - qNMR-Referenzmaterialien und "Indirect Hard Modeling" (IHM) als Integrationsmethode N2 - Resolving overlapping peaks of multiple components. Relative primary analytical method - Fundamental relationship of qNMR. T2 - 4. Sitzung der Next-NMR-Arbeitsgruppe CY - Karlsruhe, Germany DA - 08.12.2015 KW - qNMR KW - Quantitative NMR-Spektroskopie KW - Indirect Hard Modeling (IHM) KW - Referenzmaterialien PY - 2015 AN - OPUS4-36138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Schmid, Thomas T1 - Möglichkeiten zur Sonderprobenanalytik - Gemeinsame Aktivitäten mit dem Salsa-Applikationslabor der Humboldt Universität zu Berlin N2 - Troubleshooting Samples Analytics: Impurities in products: unexpected & unwanted occurrence, unknown identity, analytical method unclear, often various analytical methods, necessary, short response time important (< 1 d), benefits: allocation of its source within hours safes cost • Investigations planned, coordinated and documented by TSA team • Variety of analytical methods available T2 - 3. Analytic-City-Forum Berlin Adlershof CY - Berlin, Germany DA - 08.10.2015 KW - Troubleshooting Samples Analytics KW - TSA KW - Sonderprobenanalytik KW - Salsa KW - Applikationslabor PY - 2015 AN - OPUS4-36139 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - „NMR-METRONOMIE“ Die quantitative NMR-Spektroskopie (qNMR) gibt den Takt an N2 - qNMR is a pelative primary analytical method: Overview on fundamental relationships of qNMR T2 - Festkolloquium NMR-Spektroskopie (zum 25 jährigen Jubiläum der Firma Spectral Service, Köln) CY - Köln, Germany DA - 18.09.2015 KW - qNMR KW - Quantitative NMR-Spektroskopie KW - Metrologie PY - 2015 AN - OPUS4-36140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Low field NMR spectroscopy for online monitoring N2 - Online NMR spectroscopy is an excellent tool to study complex reacting multicomponent mixtures and gain process insight and understanding. For online studies under process conditions, flow NMR probes can be used in a wide range of temperature and pressure. This paper compiles the most important aspects towards quantitative process NMR spectroscopy in complex multicomponent mixtures and provides examples. After NMR spectroscopy is introduced as an online method and for technical samples without sample preparation in deuterated solvents, influences of the residence time distribution, pre-magnetization, and cell design are discussed. NMR acquisition and processing parameters as well as data preparation methods are presented and the most practical data analysis strategies are introduced. T2 - Sonderkolloquium der INVITE-GmbH CY - Leverkusen, Germany DA - 07.09.2016 KW - Industrie 4.0 KW - CONSENS KW - Prozessanalytik KW - Online NMR spectroscopy PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-361417 AN - OPUS4-36141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Forschung und Entwicklung für Prozessanalytik und Automatisierung in der Prozessindustrie N2 - Neue Prozess-Sensoren für neue Produktionskonzepte. Wie entsteht Innovation? Forschungsimpulse aus der Technologie-Roadmap „Prozess-Sensoren 2015+“. Herausforderungen durch das Zukunftsprojekt „Industrie 4.0“. Technologie-Roadmap „Prozess-Sensoren 4.0“ T2 - ACHEMA 2015: Automation im Dialog – Meet the experts CY - Frankfurt a. M., Germany DA - 15.06.2015 KW - Industrie 4.0 KW - Smart Sensors KW - Smarte Sensoren KW - Process Analytical Technology KW - Prozessanalytik PY - 2015 AN - OPUS4-36142 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Quantitative and online NMR Spectroscopy at BAM N2 - Online NMR spectroscopy, Determination of impurities of fluids, NMR process Monitoring, purity assessment T2 - NMR-Kolloquium Buchs CY - Buchs, Switzerland DA - 29.05.2015 KW - qNMR KW - Quantitative NMR-Spektroskopie KW - Online NMR Spectroscopy KW - Reaction monitoring KW - Reference material KW - Metrology PY - 2015 AN - OPUS4-36143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - qNMR forever – reference material metrology at high pressures and high purities N2 - Due to recent advances in technical developments of NMR instruments such as acquisition electronics and probe design, detection limits of components in liquid mixtures were improved into the lower ppm range (approx. 5–10 ppm amount of substance). This showed that modern NMR equipment is also suitable for the observation of hydrocarbon samples in the expanded fluid phase or gas phase. Since Quantitative NMR spectroscopy (qNMR) is a direct ratio method of analysis without the need of calibration it was used to determine impurities in appropriate liquid and liquefied hydrocarbon isomers up to C6, which are used for preparation of primary gas standards, e.g., natural gas or exhaust gas standards. At the same time it is possible to yield structural information with a minimum of sample preparation. Thus, cross contaminations between different isomers of the observed hydrocarbons and their (NMR-active) impurities can be identified and quantified. In general, most quantitative organic chemical measurements rely on the availability of highly purified compounds to act as calibration standards. The traceability and providence of these standards is an essential component of any measurement uncertainty budget and provides the final link of the result to the units of measurement, ideally the SI. The more recent increase in the use of qNMR for the direct assessment of chemical purity however can potentially improve the traceability and reduce the uncertainty of the measured chemical purity at a reduced cost and with less material. For example the method has beneficially been used by National Measurement institutes for recent CCQM comparisons including the CCQM–K55 series of purity studies. Traditional ‘indirect’ methods of purity analysis require that all impurities are identified and quantified, leading to a minimum of 4 individual analytical methods (organic impurities, water, solvents, inorganic residue). These multiple technique approaches measure an array of different chemical impurities normally present in purified organic chemical compounds. As many analytical methodologies have compound-specific response factors, the accuracy and traceability of the purity assessment is dependent on the availability of reference materials of the impurities being available. qNMR provides the most universally applicable form of direct purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. The development of CRMs addressing qNMR specific measurement issues will give analysts compounds ideally suited for the analytical method and also provide full characterisation of qNMR related parameters to enable more realistic uncertainty budgets. These materials will give users the tools to exploit qNMR more easily and enable them to speed up analytical method development and reduce the time and financial burden of multiple analytical testing. T2 - 3rd Practical Application of NMR in Industry Conference (PANIC) 2015 CY - La Jolla, CA, USA DA - 09.02.2015 KW - qNMR KW - Quantitative NMR-Spektroskopie KW - Reference Material KW - Metrology PY - 2015 AN - OPUS4-36144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Meyer, Klas A1 - Zientek, Nicolai T1 - Towards online reaction monitoring with fully automated NMR data evaluation and modelling - Current results from simultaneous 19F-1H medium resolution NMR experiments N2 - NMR Process Monitoring Towards an automated field integration T2 - 3rd Practical Applications of NMR in Industry Conference (PANIC) - Mestrelab users' meeting CY - La Jolla, CA, USA DA - 08.02.2015 KW - Online NMR spectroscopy KW - Reaction monitoring KW - Prozessanalytik KW - Process analytical technology PY - 2015 AN - OPUS4-36145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Innovationen in der Prozessanalytik – Welches sind die neuen Herausforderungen? N2 - Der Vortrag stellt die aktuellen Forschungsschwerpunkte zum Thema Prozessanalytik an der Bundesanstalt für Materialforschung und -prüfung (BAM) vor und nennt aktuelle Entwicklungsfelder mit dem Ziel gemeinsamer F&E-Projekte. Zunächst wird die Prozessindustrie und ihre Wertschöpfungskette vorgestellt. Daraus ergibt sich eine Motivation für Prozessanalytik. Zwischen der Prozessanalytik in der Pharmazeutische Industrie und der Chemischen Industrie bzw. Verfahrenstechnik gibt es Unterschiede, die herausgearbeitet werden. Der Vortrag schließt mit Technologiewünschen und Technologievisionen und nennt Konkrete Beispiele für Visionen für PAT, insbesondere im Kontext des Zukunftsprojekts „Industrie 4.0“ T2 - Innovationen entwickeln – Von der Idee bis zum Projektstart CY - Göttingen, Germany DA - 11.12.2014 KW - Prozessanalytik KW - Prozessindustrie KW - Innovationen KW - Pharmazeutische Industrie KW - Technologiewünsche KW - Technologievisionen KW - Industrie 4.0 PY - 2014 AN - OPUS4-36146 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guthausen, G. T1 - Online measurements in a bypass: challenges and possibilities N2 - The design of sample flow cells, commonly used in online analytics and especially for medium resolution NMR spectroscopy (MR-NMR) in low magnetic fields, was experimentally and theoretically investigated by 1H-NMR and numerical simulations. The flow pattern was characterised to gain information about the residence time distribution and mixing effects. Both 1H-NMR imaging and spectroscopy were used to determine the characteristics of flow cells and their significance for on-line measurements such as reaction monitoring or hyphenated separation spectroscopy. The volume flow rates investigated were in the range from 0.1 to 10 ml/min, typically applied in the above mentioned applications. When compared to those commonly used in high-field NMR, the special characteristics of flow cells for MR-NMR were revealed by various NMR experiments and compared with CFD simulations. The influence of the design of the inlet and outlet on the flow pattern was investigated as well as the effect of the length of the cell. For practical use, a numerical estimation of the inflow length was given. In addition, it was shown how experiments on the polarisation build-up revealed insight into the flow characteristics in MR-NMR. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) Symposium CY - Kaiserslautern, Germany DA - 15.01.2015 KW - Online NMR spectroscopy KW - Process analytical technology KW - Flow profiles KW - Online monitoring KW - Reaction monitoring PY - 2015 AN - OPUS4-36147 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zientek, Nicolai T1 - Automated data evaluation and modeling of simultaneous 19F-1H medium resolution NMR spectra for online reaction monitoring N2 - The development of innovative medium resolution NMR spectrometers (MR-NMR) is remarkable due to their possible applications in quality control, education, or process monitoring. The use of compact permanent magnets allows to employ NMR devices in an industrial environment without high maintenance requirements and without the need for cryogenic liquids. A benchtop 43 MHz MR-NMR spectrometer was used for reaction monitoring. Quasi-simultaneous proton and fluorine NMR spectra were acquired. Automatic data pretreatment and evaluation methods were applied and compared to quantitative 500 MHz HR-NMR spectroscopy T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) Symposium CY - Kaiserslautern, Germany DA - 15.01.2015 KW - Online NMR Spectroscopy KW - 1H-NMR KW - 19F-NMR KW - Reaction Monitoring KW - Benchtop NMR Spectroscopy KW - Process Analytical Technology PY - 2015 AN - OPUS4-36148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jakubowski, Norbert T1 - Book review: Freddy Adams and Carlo Barbante - Chemical imaging analysis N2 - In this book many practical hints are given and analytical problems are discussed by the authors from their own experiences. A critical assessment of the methods is given, which is most important for decision makers to select a good combination of complementary methods to solve practical analytical problems. KW - Chemical imaging analysis KW - Surface analysis KW - Interface analysis PY - 2016 DO - https://doi.org/10.1007/s00216-016-9517-9 SN - 1618-2642 SN - 1618-2650 VL - 408 IS - 16 SP - 4199 EP - 4201 PB - Springer AN - OPUS4-36216 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Nietzold, Carolin A1 - Weise, Matthias A1 - Unger, Wolfgang A1 - Alnabulsi, Saad A1 - Moulder, John T1 - XPS depth profiling of an ultrathin bioorganic film with an argon gas cluster ion beam N2 - The growing interest in artificial bioorganic Interfaces as a platform for applications in emerging Areas as personalized medicine, clinical diagnostics, biosensing, biofilms, prevention of biofouling, and other fields of bioengineering is the origin of a need for in Detail multitechnique characterizations of such layers and interfaces. The in-depth analysis of biointerfaces is of special interest as the properties of functional bioorganic coatings can be dramatically affected by in-depth variations of composition. In worst cases, the functionality of a device produced using such coatings can be substantially reduced or even fully lost. KW - XPS KW - Ar gas cluster gun KW - Depth profiling KW - Bioorganic film PY - 2016 UR - http://scitation.aip.org/content/avs/journal/bip/11/2/10.1116/1.4948341 DO - https://doi.org/10.1116/1.4948341 SN - 1934-8630 VL - 11 IS - 2 SP - 029603-1 EP - 029603-5 PB - American Vacuum Society CY - New York AN - OPUS4-36218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gemeinert, Marion T1 - Stability assessment of ceramic high dielectric N2 - Resolution of capacitive sensors can be improved enormously by replacement of the dielectric material between the capacitor plates (e.g. air-dielectric) by a dielectric fluid with high permittivity. High dielectric liquid dispersions of ceramic micro and nano powders should be qualified as dielectric fluid with longtime shelf life. For this purpose it was necessary to produce stabilized ceramic suspensions with high particle concentration and to investigate sedimentation processes of the particles. Characterization of particles was done by use of zeta potential measurement, gas adsorption measurements (BET), density measurement with gas pycnometer as well as particle sizing by ultrasound spectroscopy and by use of an optical centrifuge. Shelf life of optimized electrostatic and steric stabilized ceramic suspension was investigated by use of an optical centrifuge, a LUMISizer 651 MW (LUM Ltd.) with STEP technology and front tracking analysis. Two different wave lengths – NIR (865 nm) and blue light (470 nm) were available for examination. Centrifugation measurements with different rotation speed were used to study the rheological behavior and the sedimentation process. By this way it was possible to achieve accelerated stability determination. Measured values could be used to simulate the sedimentation process under gravity acceleration and to predict shelf life for suspensions with different dispersants. T2 - PARTEC 2016 CY - Nürnberg, Germany DA - 19.04.2016 KW - Ceramic dispersion KW - Stability assessment KW - Analytical centrifuge KW - Shelf life prediction PY - 2016 AN - OPUS4-36184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scharlach, C. A1 - Müller, Larissa A1 - Wagner, S. A1 - Kobayashi, Y. A1 - Kratz, H. A1 - Ebert, M. A1 - Jakubowski, Norbert A1 - Schellenberger, E. T1 - LA-ICP-MS allows quantitative microscopy of europium-doped iron oxide nanoparticles and is a possible alternative to ambiguous Prussian blue iron staining N2 - The development of iron oxide nanoparticles for biomedical applications requires accurate histological evaluation. Prussian blue iron staining is widely used but may be unspecific when tissues contain substantial endogenous iron. Here we tested whether microscopy by laser ablation coupled to inductively coupled plasma mass spectrometry (LA-ICP-MS) is sensitive enough to analyze accumulation of very small iron oxide particles (VSOP) doped with europium in tissue sections. KW - Atherosclerotic plaques KW - LA-ICP-MS microscopy KW - Quantification KW - Element microscopy KW - Histology PY - 2016 DO - https://doi.org/10.1166/jbn.2016.2230 SN - 1550-7033 SN - 1550-7041 VL - 12 IS - 5 SP - 1001 EP - 1010 AN - OPUS4-36189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heck, Christian T1 - Plasmonic gold nanolenses self-assembled by DNA origami N2 - Surface-enhanced Raman scattering (SERS) exploits the enhancement of electromagnetic fields in close vicinity of plasmonic nanostructures. The nanometer-scale spatial arrangement of plasmonic metal nanoparticles and analyte molecules has a significant effect on the observed signal enhancements and represents a great challenge in this technique. Especially interesting effects are expected for complex gold nanolenses (AuNLs), consisting of three or more differently-sized AuNPs. We use DNA origami to assemble AuNLs with 10, 20 and 60 nm AuNPs, arranged in three different geometries. Using correlated AFM and Raman spectroscopy, and probing single AuNLs, we systematically examined the SERS properties of the three different assemblies. T2 - DNA Nanotechnology 2016 CY - Jena, Germany DA - 19.05.2016 KW - gold nanoparticles KW - DNA origami KW - plasmonics PY - 2016 AN - OPUS4-36205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prinz, J. A1 - Heck, Christian A1 - Ellerik, L. A1 - Merk, V. A1 - Bald, Ilko T1 - DNA origami based Au–Ag-core–shell nanoparticle dimers with single-molecule SERS sensitivity N2 - DNA origami nanostructures are a versatile tool to arrange metal nanostructures and other chemical entities with nanometer precision. In this way gold nanoparticle dimers with defined distance can be constructed, which can be exploited as novel substrates for surface enhanced Raman scattering (SERS). We have optimized the size, composition and arrangement of Au/Ag nanoparticles to create intense SERS hot spots, with Raman enhancement up to 10^10, which is sufficient to detect single molecules by Raman scattering. This is demonstrated using single dye molecules (TAMRA and Cy3) placed into the center of the nanoparticle dimers. In conjunction with the DNA origami nanostructures novel SERS substrates are created, which can in the future be applied to the SERS analysis of more complex biomolecular targets, whose position and conformation within the SERS hot spot can be precisely controlled. KW - single molecule spectroscopy KW - DNA origami KW - SERS KW - gold nanoparticles KW - silver nanoparticles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-358761 UR - http://pubs.rsc.org/en/content/articlelanding/2016/nr/c5nr08674d#!divAbstract DO - https://doi.org/10.1039/C5NR08674D SP - 5612 EP - 5620 PB - Royal Society of Chemistry CY - Cambridge, England AN - OPUS4-35876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Muhammad, R. T1 - Influence of the of dealumination and porosity on the acid sites of natural zeolite clinoptilolite N2 - Heavy feedstock from crude and bio oil is a widely available and renewable resource for production of fuel and starting materials for other organic valuables by cracking or hydrocracking. Catalytic processing of heavy feedstock can meet the increased demand of energy up to a great extent. It requires the application of acidic catalysts like zeolites. However, the used synthetic catalysts are difficult to recover and reuse and are mostly spent. The use of natural zeolite as spent catalysts may open new perspectives in the chemical use of heavy feed feedstock by chemical conversion. Natural zeolites are not expensive, widely available and environment friendly. Clinoptilolite is the most abundant natural zeolite. Clinoptilolite has a crystalline structure with a defined micropore system of medium size showing unique ion exchange and sorption properties. However, it is catalytically active only in the H-form. Also certain porosity is required for improvement of the accessibility of active sites. This paper deals with the tuning of acid properties and of the mesoporosity of the clinoptilolite by variation of the Si/Al framework ratio, extra-framework aluminum and modification of the porosity by specific acid and water vapor treatment. The preparation of hierarchical pore structures containing interconnected micro-meso-macropores is an important factor influencing the catalytic performance. The obtained materials have been characterized by XRD, TEM, FTIR, Raman, TG/DSC. The chemical composition has been determined by ICP-AES. The porosity have been investigated by nitrogen adsorption desorption measurements. The acidity has been measured by Ammonia-TPD. The extent of dealumination, stability of the clinoptilolite against acid treatment and the change in the nature of acid sites and their local structure has been studied by solid state 29Si and 27Al MAS NMR spectroscopy in detail. The catalytic activity has been investigated in the acetalization of benzaldehyde with 1,3-butanediol. The impact of the porosity, change of the Si/Al ratio as well as present Al species on catalytic properties will be discussed. T2 - 28. Deutsche Zeolith-Tagung CY - Giessen, Germany DA - 02.03.2016 KW - NMR KW - Zeolite KW - Clinoptilolite KW - Catalyst PY - 2016 AN - OPUS4-35886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Method evaluation and selection N2 - In this contribution the particle sizing techniques evaluated in NanoDefine are presented together with recommendations for their application/implementation on real-world materials. The experimental evaluation is discussed based on examples on NanoDefine materials. A systematic study on volume specific surface area as derived from BET measurements versus electron microscopy on powdered materials is also presented. T2 - NanoDefine NSC Synergy workshop CY - Brussels, Belgium DA - 02.02.2016 KW - nanomaterial PY - 2016 AN - OPUS4-35923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Can today’s methods afford to easily and reliably classify nanomaterials? N2 - In the contribution the NanoDefine sizing techniques are discussed after their systematic evaluation on NanoDefine materials. The results of the comparative study BET versus electron microscopy are also discussed. Furthermore, recommendations for application of the gained knowledge are given. T2 - NanoDefine Workshop Analytical Challenges and Industry Needs CY - Frankfurt, Germany DA - 08.02.2016 KW - Nanomaterial PY - 2016 AN - OPUS4-35924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Doriti, A. A1 - Brosnan, S. A1 - Weidner, Steffen A1 - Schlaad, H. T1 - Synthesis of polysarcosine from air and moisture stable N-phenoxycarbonyl-N-methylglycine assisted by tertiary amine base N2 - Polysarcosine (M-n = 3650-20 000 g mol(-1), D similar to 1.1) was synthesized from the air and moisture stable N-phenoxycarbonyl-N-methylglycine. Polymerization was achieved by in situ transformation of the urethane precursor into the corresponding N-methylglycine-N-carboxyanhydride, when in the presence of a non-nucleophilic tertiary amine base and a primary amine initiator. KW - Polysarcosine KW - MALDI-TOF MS KW - Synthesis PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-359309 DO - https://doi.org/10.1039/c6py00221h SN - 1759-9954 SN - 1759-9962 VL - 7 IS - 18 SP - 3067 EP - 3070 AN - OPUS4-35930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pellegrino, F. T1 - Experimental approaches and paradigms for shape controlled synthsis of TiO2 nanoparticles N2 - Titanium dioxide is one of the most studied metal oxides due to its interesting chemical, surface, electronic and (photo)catalytic properties. These properties provide this material of multisectorial applications, ranging from healthcare, photocatalysis, smart materials with self cleaning and self sterilizing properties and solar energy harvesting (photovoltaics and water photosplitting). However it is difficult to correlate the functional properties of TiO₂ nanomaterials to the properties at single nanoparticle level due to the high polydispersity in shape, size and surface properties of the currently available TiO₂ nanoparticles (NPs) Although intensive experimental and theoretical studies have been conducted on the reactivity of different surfaces of metal oxides such as TiO₂ [1,2] much less attention is paid on the dependence of functional properties, like photocatalytic activity, dye adsorption, open circuit potential and fill factor in dye sensitized solar cells, on crystal facets in different orientations [3]. One of the goal of SETNanoMetro is the development of design rules to tune crystal facets of TiO₂ NPs in order to optimize and control functional properties. By tuning the ratio of different facets, the functional properties would be correspondingly changed. In the present work we have developed a series of design rules in order to obtain sets of anatase TiO₂ NPs with low polydispersity and to tune their shape and their size though hydrothermal processing of Ti(IV)-Triethanolamine complex in presence of different shape controllers (OH-, triethanolamine, fluoride). Through a careful experimental design the influence of many process parameters (pH, temperature, shape controller type and concentration) on the synthesis outcome (size, shape and polydispersity), a predictive soft model was developed. The model is able to predict reasonably well the synthesis outcome allowing to tune the shape factor from 5 (prisms) to 1.5 (bipyramids) to 0.2 (platelets). This allows to control the main crystal facets exposed ranging from (100) to (001). T2 - EMEC16, 16th European Meeting on Environmental Chemistry CY - Turin, Italy DA - 30.11.2015 KW - TiO2 KW - nanoparticles PY - 2015 AN - OPUS4-35933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ye, S. A1 - Loll, B. A1 - Berger, A. A1 - Mülow, Ulrike A1 - Alings, C. A1 - Wahl, M. A1 - Koksch, B. T1 - Fluorine teams up with water to restore inhibitor activity to mutant BPTI N2 - Introducing fluorine into molecules has a wide range of effects on their physicochemical properties, often desirable but in most cases unpredictable. The fluorine atom imparts the C–F bond with low polarizability and high polarity, and significantly affects the behavior of neighboring functional groups, in a covalent or noncovalent manner. Here, we report that fluorine, present in the form of a single fluoroalkyl amino acid side chain in the P1 position of the well-characterized serine-protease inhibitor BPTI, can fully restore inhibitor activity to a mutant that contains the corresponding hydrocarbon side chain at the same site. High resolution crystal structures were obtained for four BPTI variants in complex with bovine b-trypsin, revealing changes in the stoichiometry and dynamics of water molecules in the S1 subsite. These results demonstrate that the introduction of fluorine into a protein environment can result in “chemical complementation” that has a significantly favorable impact on protein–protein interactions. KW - serine-protease inhibitor KW - crystal structures KW - Peptide synthesis PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-358987 DO - https://doi.org/10.1039/C4SC03227F IS - 9 SP - 5246 EP - 5254 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-35898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gründer, Klaus-Peter A1 - Geburtig, Anja T1 - Optical Methods in Single Crystal Deformation Analysis at High Temperature N2 - This poster deals with grating methods, white light intereference microscopy, a setup for HT investigation and applications. T2 - International Symposium on „Photonics in Measurement“ CY - Aachen, Germany DA - 11.06.2002 KW - Grating method KW - White light intereference microscopy KW - HT investigation PY - 2002 AN - OPUS4-35899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Menzel, M. A1 - Scharf, O. A1 - Novak, S. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Hischenhuber, P. A1 - Buzanich, Günter A1 - Meyer, A. A1 - Lopez, V. A1 - McIntosh, K. A1 - Streli, C. A1 - Havrilla, G. A1 - Fittschen, U. T1 - Shading in TXRF: calculations and experimental validation using a color X-ray camera N2 - Absorption effects in total reflection X-ray fluorescence (TXRF) analysis are important to consider, especially if external calibration is to be applied. With a color X-ray camera (CXC), that enables spatially and energy resolved XRF analysis, the absorption of the primary beam was directly visualized for mL-droplets and an array of pL-droplets printed on a Si-wafer with drop-on-demand technology. As expected, deposits that are hit by the primary beam first shade subsequent droplets, leading to a diminished XRF signal. This shading effect was quantified with enhanced precision making use of sub-pixel analysis that improves the spatial resolution of the camera. The measured absorption was compared to simulated results using three different model calculations. It was found they match very well (average deviation < 10%). Thus errors in quantification due to absorption effects can be accounted for in a more accurate manner. KW - absorption KW - X-ray Fluorescence analysis PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-359000 DO - https://doi.org/10.1039/C5JA00127G IS - 10 SP - 2184 EP - 2193 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-35900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska ED - de Oliveira Guilherme Buzanich, Ana ED - Strange, R. W. T1 - Time- and spatial-resolved XAFS spectroscopy in a single shot: new analytical possibilities for in situ material characterization N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ–2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 mm is achieved. KW - Single-shot XAFS KW - Time resolution PY - 2016 UR - http://scripts.iucr.org/cgi-bin/paper?S1600577516003969 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 VL - 23 SP - 769 EP - 776 PB - International Union of Crystallography CY - Liverpool, UK AN - OPUS4-35903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heck, Christian T1 - Gold nanolenses on DNA origami substrates for surface-enhanced Raman scattering N2 - Surface-enhanced Raman scattering (SERS) exploits the enhancement of electromagnetic fields in close vicinity of plasmonic nanostructures, enabling characterization of analytes at the single-molecule level. The nanometer-scale spatial arrangement of plasmonic metal nanoparticles and analyte molecules has a significant effect on the observed signal enhancements and represents a great challenge in this technique. In our work, DNA origami is used as platform for precise positioning of gold nanoparticles (AuNPs). Especially high sensitivities are expected for gold nanolenses (AuNLs), consisting of rows of three or more differently-sized AuNPs. We assembled different AuNL designs and determined respective SERS enhancement factors by collecting Raman spectra from single AuNLs. Finite difference time domain calculations estimate attainable electromagnetic field enhancements. Ultimately, we aim to develop a versatile platform for various SERS applications. T2 - DNA meets Plasmonics Konferenz CY - Bad Honnef, Germany DA - 07.12.2015 KW - DNA origami KW - SERS KW - Plasmonics PY - 2015 AN - OPUS4-35906 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, G. A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - Mechanochemical synthesis, characterization, and structure determination of new alkaline earth metal-tetrafluoroterephthalate frameworks: Ca(pBDC‑F4 )·4H2O, Sr(pBDC‑F4 )·4H2O, and Ba(pBDC‑F4 ) N2 - New fluorinated alkaline earth metal−organic frameworks were successfully synthesized by milling of metal hydroxides M(OH)2 with tetrafluoroterephthalic acid H2 pBDC-F4. Both calcium- and strontium-tetrafluoroterephthalates are tetrahydrated, while the barium tetrafluoroterephthalate is free of coordinating water molecules. The two isomorphic structures Ca(pBDC-F4)·4H2O and Sr(pBDC-F4)·4H2O were solved from the powder diffraction data by ab initio structure determination and subsequent Rietveld refinement. The products were thoroughly characterized by elemental analysis, thermal analysis, magicangle spinning NMR, Fourier transform infrared spectroscopy, scanning electron microscopy imaging, and Brunauer−Emmett−Teller measurements. Our findings suggest that the mechanochemical synthesis route is a promising approach for the preparation of new fluorinated alkaline earth metal−organic frameworks. KW - Mechanochemistry KW - MOFs KW - XRD PY - 2016 UR - http://pubs.acs.org/doi/abs/10.1021/acs.cgd.5b01457 DO - https://doi.org/10.1021/acs.cgd.5b01457 SN - 1528-7483 VL - 16/4 SP - 1923 EP - 1933 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-35940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brown, A. S. T1 - Traceable standards and methods for the analysis of non-conventional energy gases N2 - Declining European natural gas resources and increasing legislation mean that diversification towards ‘non-conventional gases’ is essential. Accurate and traceable measurements of the composition of non- conventional gases are required to ensure gases can be transported in existing pipeline networks, and used with existing appliances. The EMRP ‘Characterisation of energy gases’ project is successfully developing a metrology infrastructure to underpin these measurements. New standards and methods have been developed for biogas composition, biogas impurities, coal mine gases, refinery gases and environmentally-friendly odorants. The project is set to conclude in 2013 with the challenging analysis of a series of real non-conventional gas samples. T2 - 28th Meeting of the CCQM Gas Analysis Working Group (GAWG) CY - Saint Petersburg, Russian Federation DA - 24.10.2012 KW - metrology KW - traceable standards KW - energy gases PY - 2012 AN - OPUS4-35946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Sloniec-Myszk, Jagoda ED - Hennig, Andreas T1 - Chiral, J-aggregate-forming dyes for alternative signal modulation mechanisms in self-immolative enzyme-activatable optical probes N2 - Enzyme-activatable optical probes are important for future advances in cancer imaging, but may easily suffer from low signal-to-background ratios unless not optimized. To address this shortcoming, numerous mechanisms to modulate the fluorescence signal have been explored. We report herein newly synthesized probes based on selfimmolative linkers containing chiral J-aggregate-forming dyes. Signal modulation by formation of chiral J-aggregates is yet unexplored in optical enzyme probe design. The comprehensive characterization of the probes by absorption, CD, fluorescence, and time-resolved fluorescence spectroscopy revealed dye−dye interactions not observed for the free dyes in solution as well as dye−protein interactions with the enzyme. This suggested that J-aggregate formation is challenging to achieve with current probe design and that interactions of the dyes with the Enzyme may interfere with achieving high signal-to-background ratios. The detailed understanding of the interactions provided herein provides valuable guidelines for the future design of similar probes. KW - Signal amplification KW - Fluorescence KW - Quantum yield KW - Optical spectroscopy KW - Dye KW - Cyanine KW - Characterization KW - Assay KW - Chiral KW - Aggregation KW - Activatable probe PY - 2016 DO - https://doi.org/10.1021/acs.jpcb.5b10526 SN - 1520-5207 SN - 1520-6106 VL - 120 IS - 5 SP - 877 EP - 885 PB - ACS Publications AN - OPUS4-35949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Simple method for the quantification of PEG ligands and guidelines to the spectroscopic characterization of upconversion nanoparticles N2 - The surface modification of nanometer- and micrometer-sized particles with polyethylene glycol (PEG) ligands of varying length is a very common strategy to tune their hydrophilicity and biocompatibility, minimize unspecific interactions, improve biofunctionalization efficiencies, and enhance blood circulation times. Nevertheless, simple methods for the quantification of PEG ligands are rare. This is similarly true for the spectroscopic characterization of lanthanide-doped upconverting nanoparticles (UCNPs), novel near infrared (NIR)-excitable nonlinear fluorescence reporters for bioanalysis and theranostics, providing background-free multiple narrow emission bands in the visible and NIR, excellent photostability, and long luminescence lifetimes. We present here a simple method for the determination of the number of PEG ligands on nanomaterials and screening methods for the fast identification of nonradiative deaction pathways in UCNPs. T2 - SPIE Photonics West CY - San Francisco, CA, USA DA - 15.02.2016 KW - Optical assay KW - Fluorescence KW - Integrating sphere spectroscopy KW - Quantum yield KW - NIR KW - IR KW - Optical spectroscopy KW - Nanomaterials KW - Semiconducor nanocrystals KW - Upconversion nanocrystals KW - Surface analysis; KW - Ligand analysis PY - 2016 AN - OPUS4-35951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Methods for the determination of the optical properties and the surface chemistry of fluorescent particles N2 - Fluorescent particles like nm- and m-sized polymeric beads doped or labeled with different types of fluorophores and nanocrystalline systems like quantum dots and upconversion phosphors emitting in the visible (vis), near-infrared (NIR), and IR (infrared) region are of increasing importance as fluorescent reporters for bioanalysis and medical diagnostics. The assessment and comparison of material performance and the development of rational design strategies for improved systems requires suitable spectroscopic tools for the determination of signal-relevant optical properties and analytical tools for the determination of the number of surface groups, ligands, biomolecules and /or fluorophores per bead. In this respect, suitable spectroscopic tools for the characterization of the optical properties of such materials like photoluminescence quantum yields and brightness values and the determination of their surface chemistry are introduced. This includes integrating sphere setups for absolute measurements of fluorescence quantum yields of liquid and solid, transparent and scattering materials in the wavelength region of 350 nm to 1600 nm at varying excitation power densities for the study of multi-photon processes and simple optical assays, validated by comparison with established analytical techniques relying on different detection principles. Here, different examples for the optical and analytical characterization of different types of nanoscale reporters are presented. T2 - MoLife Research Seminar CY - Bremen, Germany DA - 26.04.2016 KW - Optical assay KW - Fluorescence KW - Integrating sphere spectroscopy KW - Quantum yield KW - NIR KW - IR KW - Optical spectroscopy KW - Nanomaterials KW - Semiconducor nanocrystals KW - Upconversion nanocrystals KW - Surface analysis KW - Ligand analysis PY - 2016 AN - OPUS4-35954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Bartusch, Jürgen A1 - Schadow, Florian A1 - Köppe, Enrico A1 - Dohse, Elmar ED - Chimenti, D. E. ED - Bond, L. J. T1 - Focusing of ferroelectret air-coupled ultrasound transducers N2 - Air-coupled ultrasound has been applied increasingly as a non-destructive testing method for lightweight construction in recent years. It is particularly appropriate for composite materials being used in automotive and aviation industry. Air-coupled ultrasound transducers mostly consist of piezoelectric materials and matching layers. However, their fabrication is challenging and their signal-to-noise ratio often not sufficient for many testing requirements. To enhance the efficiency, air-coupled ultrasound transducers made of cellular polypropylene have been developed. Because of its small density and sound velocity, this piezoelectric ferroelectret matches the small acoustic impedance of air much better than matching layers applied in conventional transducers. In our contribution, we present two different methods of spherical focusing of ferroelectret transducers for the further enhancement of their performance in NDT applications. Measurements on carbon-fiber-reinforced polymer (CFRP) samples and on metal adhesive joints performed with commercially available focused air-coupled ultrasound transducers are compared to measurements executed with self-developed focused ferroelectret transducers. T2 - 42nd Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Minneapolis, Minnesota, USA DA - 26.07.2015 KW - Ferroelectret KW - Transducer KW - Air-coupled KW - Ultrasonic KW - Focusing PY - 2016 SP - 080001 PB - AIP Publishing CY - Melville, NY, USA AN - OPUS4-35955 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gaal, Mate A1 - Bovtun, Viktor A1 - Stark, Wolfgang A1 - Erhard, Anton A1 - Yakymenko, Y. A1 - Kreutzbruck, Marc T1 - Viscoelastic properties of cellular polypropylene ferroelectrets N2 - Viscoelastic properties of cellular polypropylene ferroelectrets (PP FEs) were studied at low frequencies (0.3–33 Hz) by dynamic mechanical analysis and at high frequencies (250 kHz) by laser Doppler vibrometry. Relaxation behavior of the in-plane Young’s modulus (Y´ 11~1500 MPa at room temperature) was observed and attributed to the viscoelastic response of polypropylene matrix. The out-of-plane Young’s modulus is very small (Y´33≈0.1 MPa) at low frequencies, frequency- and stress-dependent, evidencing nonlinear viscoelastic response of PP FEs. The highfrequency mechanical response of PP FEs is shown to be linear viscoelastic with Y´33≈0.8 MPa. It is described by thickness vibration mode and modeled as a damped harmonic oscillator with one degree of freedom. Frequency dependence of Y*33 in the large dynamic strain regime is described by the broad Cole-Cole relaxation with a mean frequency in kHz range attributed to the Dynamics of the air flow between partially closed air-filled voids in PP FEs. Switching-off the relaxation contribution causes dynamic crossover from the nonlinear viscoelastic regime at low frequencies to the linear viscoelastic regime at high frequencies. In the small strain regime, contribution of the air flow seems to be insignificant and the power-law response, attributed to the mechanics of polypropylene cell walls and closed air voids, dominates in a broad frequency range. Mechanical Relaxation caused by the air flow mechanism takes place in the sound and ultrasound frequency range (10 Hz–1MHz) and, therefore, should be taken into account in ultrasonic applications of the PP FEs deal with strong exciting or receiving signals. KW - Viscoelastic KW - Cellular polypropylene KW - Ferroelectret PY - 2016 DO - https://doi.org/10.1063/1.4944798 SN - 0021-8979 SN - 1089-7550 SN - 1520-8850 VL - 119 SP - Article Number: 125101 PB - AIP Publishing AN - OPUS4-35956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Focusing of ferroelectret air-coupled ultrasound transducers N2 - Air-coupled ultrasound has been applied increasingly as a non-destructive testing method for lightweight construction in recent years. It is particularly appropriate for composite materials being used in automotive and aviation industry. Air-coupled ultrasound transducers mostly consist of piezoelectric materials and matching layers. However, their fabrication is challenging and their signal-to-noise ratio often not sufficient for many testing requirements. To enhance the efficiency, air-coupled ultrasound transducers made of cellular polypropylene have been developed. Because of its small density and sound velocity, this piezoelectric ferroelectret matches the small acoustic impedance of air much better than matching layers applied in conventional transducers. In our contribution, we present two different methods of spherical focusing of ferroelectret transducers for the further enhancement of their performance in NDT applications. Measurements on carbon-fiber-reinforced polymer (CFRP) samples and on metal adhesive joints performed with commercially available focused air-coupled ultrasound transducers are compared to measurements executed with self-developed focused ferroelectret transducers. T2 - 42nd Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Minneapolis, Minnesota, USA DA - 26.07.2015 KW - Focusing KW - Ferroelectret KW - Air-coupled KW - Transducer KW - Ultrasonic PY - 2015 AN - OPUS4-35957 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane A1 - Myrach, Philipp A1 - Röllig, Mathias A1 - Jonietz, Florian A1 - Illerhaus, Bernhard A1 - Meinel, Dietmar A1 - Richter, U. A1 - Miksche, R. ED - Chimenti, Dale E. ED - Bond, Leonard J. T1 - Characterization of pores in high pressure die cast aluminum using active thermography and computed tomography N2 - Larger high pressure die castings (HPDC) and decreasing wall thicknesses are raising the issue of casting defects like pores in aluminum structures. Properties of components are often strongly influenced by inner porosity. As these products are being established more and more in lightweight construction (e.g. automotive and other transport areas), non-destructive testing methods, which can be applied fast and on-site, are required for quality assurance. In this contribution, the application of active thermography for the direct detection of larger pores is demonstrated. The analysis of limits and accuracy of the method are completed by numerical simulation and the method is validated using computed tomography. T2 - 42nd Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Minneapolis, Minnesota, USA DA - 26.07.2015 KW - flash thermography KW - aluminum KW - pores KW - computed tomography PY - 2016 SN - 978-0-7354-1353-5 DO - https://doi.org/10.1063/1.4940580 VL - 1706 SP - 110009-1 EP - 110009-8 PB - AIP Publishing LLC CY - Melville, New York, USA AN - OPUS4-35848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Christina A1 - Völker, J. A1 - Scharmach, Martina T1 - Zuverlässigkeit von ZfP-Verfahren - Internationaler Stand der Diskussion im Jahre 2001 N2 - Dieses Poster beschäftigt sich mit den Interessen der Industrie, der ISO 17025 und ISO 9001, den wissenschaftlichen Konzepten, dem European-American-Workshop, der Zuverlässigkeitsformel, der ASNT Reliability ad hoc Group und der EPERC TTF3 T2 - DGZfP Jahrestagung 2001 CY - Berlin, Germany DA - 21.05.2001 KW - ISO 17025 KW - ISO 9001 KW - Zuverlässigkeitsformel PY - 2001 AN - OPUS4-35850 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Metrology for spatially resolved chemical analysis at the micro and nanometre scales N2 - CCQM has established a framework of comparisons to demonstrate the international comparability of chemical measurements. The key point is the establishment of comparable measurements, with traceability to internationally or nationally stated references. The Surface Analysis Working Group (SAWG) has been formally founded in 2003. CCQM ratified the group as a full working group of CCQM in April 2003 with these terms of reference: - to develop pilot studies and carry out key comparisons of national measurement standards for surface and micro/nano-analysis; - to assist in identifying and establishing inter-laboratory work to improve the traceability of surface and micro/nano-analysis; - to establish and update a work plan to be adopted by CCQM; - to discuss and review the scope of the working group and to liase with other working groups related to nanotechnology. Following the 2015 meeting of the CCQM, the pilot study CCQM-P130 “WD and ED Electron Probe Micro Analysis on Au-Cu alloys” lead by BAM&NIST has been finalized. The Key Comparison K-129 “Measurement of atomic fractions in Cu(In,Ga)Se2 Films” lead by KRISS has made substantial progress and is about to be finalized. The new Key Comparison K-136 on “BET specific surface of ” lead by UNIIM&BAM has made strong progress in 2015 and will be finished in 2016. T2 - 22nd Meeting of CCQM CY - Sevres, France DA - 21.4.16 KW - Surface chemical analysis KW - Metrology PY - 2016 AN - OPUS4-35865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - 2-D materials standardization N2 - The implementation of new 2-D materials based technologies in production processes requires the development of quality management tools. These have to be underpinned by appropriate measurements. Consequently there is a need for the development of the metrology for measurement methods, the development of certified reference materials (CRM) and finally standardization. This chain represents the ideal way to practically useful standards. The presentation will give an overview on the main players in the field and summarize the recent status of activities. At the highest level the metrology of chemical characterization of 2D materials is in the scope of the International Meter Convention, specifically the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM). Pre-standardization is an activity field of the Versailles Project on Advanced Materials and Standards (VAMAS). Standardization is mainly addressed by addressed ISO Technical Committees. A summary on available CRMs relevant to the characterization of nano materials has been prepared by BAM. Examples from the work of BAM’s Division 6.1 “Surface Analysis and Interfacial Chemistry” showcasing the characterization of chemically modified graphene surfaces are given and specific needs for the development of metrology are addressed. In the discussion the audience is invited to define specific needs which will be streamlined to the respective bodies! T2 - Science-Industry-Workshop 2D Materials CY - EMPA Akademie, Dübendorf, Switzerland DA - 21.3.16 KW - Standardization KW - Graphene PY - 2016 AN - OPUS4-35866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roth, Christina T1 - Incorporating mechanically interlocked molecules into crystalline coordination networks on surfaces: Electro-active SURMOFs to translate molecular switching into macroscopic function and devices N2 - We aim at preparing, characterising, and applying SURMOFs incorporating electro-active and -switchable mechanically interlocked molecules such as rotaxanes as the basis of functional devices. Preparation and Positioning Synthesis, purification and analytical characterization of electro-switchable rotaxanes suitable for SURMOF-formation as well as Layer-by-Layer assembly on surfaces. Controlled deposition of electro-active SURMOFs and Layer-by-Layer self-assembled multilayers based on these switchable rotaxanes. Construction of SURMOFs on micro-patterned surfaces. Structural Characterisation and Physico-Chemical Properties Electrochemical characterization of these rotaxanes in solution with cyclic voltammetry, chronoamperometry and impedance spectroscopy. Surface characterization of SURMOFs and multilayers with XPS, NEXAFS, AFM, contact-angle measurements, transmission UV/Vis, ToF-SIMS and – in cooperation with partners from SPP – XRD. Development of ToF-SIMS (also assisted by Principle Component Analysis of the fragment-ion data) as a method for imaging and depth-profiling. Development of an appropriate electrochemical cell to perform cyclic voltammetry, chronoamperometry and impedance spectroscopy with SURMOFS and multilayers as working electrodes in a three-electrode cell. Comparison of the structural and electrochemical properties of the redox-active unit in solution, multilayers and SURMOF focusing on the advantages of SURMOFs. System Integration and Function Demonstration Examination of the usability of the electroactive SURMOFS as optoelectronic switch or data storage device with a focus on the robustness of the system. Usage of the SURMOFs as functional electrodes for electrochemical application. Selective switching of ordered nanostructures to translate molecular motion to macroscopic property changes. T2 - Colloquium of the priority programme "Coordination networks: building blocks for functional systems” SPP 1928 CY - Garching, Germany DA - 30.3.16 KW - SurfMOF KW - XPS KW - NEXAFS KW - Characterization PY - 2016 AN - OPUS4-35867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roth, C. T1 - Incorporating mechanically interlocked molecules into crystalline coordination networks on surfaces: Electro-active SURMOFs to translate molecular switching into macroscopic function and devices N2 - We aim at preparing, characterising, and applying SURMOFs incorporating electro-active and -switchable mechanically interlocked molecules such as rotaxanes as the basis of functional devices. Preparation and Positioning Synthesis, purification and analytical characterization of electro-switchable rotaxanes suitable for SURMOF-formation as well as Layer-by-Layer assembly on surfaces. Controlled deposition of electro-active SURMOFs and Layer-by-Layer self-assembled multilayers based on these switchable rotaxanes. Construction of SURMOFs on micro-patterned surfaces. Structural Characterisation and Physico-Chemical Properties Electrochemical characterization of these rotaxanes in solution with cyclic voltammetry, chronoamperometry and impedance spectroscopy. Surface characterization of SURMOFs and multilayers with XPS, NEXAFS, AFM, contact-angle measurements, transmission UV/Vis, ToF-SIMS and – in cooperation with partners from SPP – XRD. Development of ToF-SIMS (also assisted by Principle Component Analysis of the fragment-ion data) as a method for imaging and depth-profiling. Development of an appropriate electrochemical cell to perform cyclic voltammetry, chronoamperometry and impedance spectroscopy with SURMOFS and multilayers as working electrodes in a three-electrode cell. Comparison of the structural and electrochemical properties of the redox-active unit in solution, multilayers and SURMOF focusing on the advantages of SURMOFs. System Integration and Function Demonstration Examination of the usability of the electroactive SURMOFS as optoelectronic switch or data storage device with a focus on the robustness of the system. Usage of the SURMOFs as functional electrodes for electrochemical application. Selective switching of ordered nanostructures to translate molecular motion to macroscopic property changes. T2 - Colloquium of the Priority Programme "Coordination Networks: Building Blocks for Functional Systems” SPP 1928 CY - Garching, Germany DA - 30.3.16 KW - SURMOF KW - XPS KW - NEXAFS KW - Characterization PY - 2016 AN - OPUS4-35868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shokouhi, P. A1 - Heideklang, Rene T1 - Fusion of multi-sensory NDT data for reliable detection of surface cracks: Signal-level vs. decision-level N2 - We present and compare two different approaches for NDT multi-sensor data fusion at signal (low) and decision (high) levels. Signal-level fusion is achieved by applying simple algebraic rules to strategically post-processed images. This is done in the original domain or in the domain of a suitable signal transform. The importance of signal normalization for low-level fusion applications is emphasized in regard to heterogeneous NDT data sets. For fusion at decision level, we develop a procedure based on assembling joint kernel density estimation (KDE). The procedure involves calculating KDEs for individual sensor detections and aggregating them by applying certain combination rules. The underlying idea is that if the detections from more than one sensor fall spatially close to one another, they are likely to result from the presence of a defect. On the other hand, single-senor detections are more likely to be structural noise or false alarm indications. To this end, we design the KDE combination rules such that it prevents single-sensor domination and allows data-driven scaling to account for the influence of individual sensors. We apply both fusion rules to a three-sensor dataset consisting in ET, MFL/GMR and TT data collected on a specimen with built-in surface discontinuities. The performance of the fusion rules in defect detection is quantitatively evaluated and compared against those of the individual sensors. Both classes of data fusion rules result in a fused image of fewer false alarms and thus improved defect detection. Finally, we discuss the advantages and disadvantages of low-level and high-level NDT data fusion with reference to our experimental results. T2 - 42nd Annual Review of Progress in Quantitative Nondestructive Evaluation (QNDE) CY - Minneapolis, USA DA - 26.07.2015 KW - multi-sensory KW - NDT KW - signal-level KW - decision-level PY - 2016 SN - 978-0-7354-1353-5 DO - https://doi.org/10.1063/1.4940634 SN - 0094-243X VL - 1706 SP - Article Number: 180004 PB - AMER INST PHYSICS CY - Melville, USA AN - OPUS4-35870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nguyen, Thi Yen T1 - Desolvation of indometacin solvates characterized structurally and kinetically N2 - The structure of indometacin solvates and the desolvation process of these compounds are investigated by synchrotron X-ray radiation, Raman spectroscopy and thermal analysis. T2 - Annual CM1402 crystallize COST meeting CY - Coimbra, Portugal DA - 06.04.2016 KW - Crystallization KW - In situ analysis KW - Indometacin KW - Active pharmaceutical ingredient (API) PY - 2016 AN - OPUS4-35872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nguyen, Thi Yen T1 - Direct evidence of polyamorphism in paracetamol N2 - While polymorphism is a common phenomenon in the crystallization processes of organic compounds, polyamorphism has gained importance only recently. Using sophisticated sample environments and applying in situ scattering methods and vibrational spectroscopy, the complete crystallization process of organic compounds from solution can be traced and characterized. Diffuse scattering from amorphous intermediates can be investigated by analyzing the atomic pair Distribution function (PDF) to gain further insights into molecular pre-orientation. The crystallization behavior of Paracetamol was studied exemplarily under defined, surface-free conditions. Based on the choice of the solvent, the formation of different polymorphs is promoted. The thermodynamically stable form I and the metastable orthorhombic form II could be isolated in pure form directly from solution. For both polymorphs, the crystallization from solution proceeds via a distinct amorphous precursor phase. PDF analyses of these different amorphous states indicate a specific pre-orientation of the analyte molecules introduced by the solvent. The resulting crystalline polymorph is already imprinted in these proto-crystalline precursors. Direct experimental evidence for the polyamorphism of paracetamol is provided. T2 - Annual CM1402 crystallize COST meeting CY - Coimbra, Portugal DA - 06.04.2016 KW - Paracetamol KW - Crystallization KW - In situ analysis KW - Active pharmaceutical ingredient (API) PY - 2016 AN - OPUS4-35873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matkovic, A. A1 - Vasic, B. A1 - Pesic, J. A1 - Prinz, J. A1 - Bald, Ilko A1 - Milosavljevic, A. R. A1 - Gajic, R. T1 - Enhanced structural stability of DNA origami nanostructures by graphene encapsulation N2 - Wedemonstrate that a single-layer graphene replicates the shape ofDNAorigami nanostructures very well. It can be employed as a protective layer for the enhancement of structural stability of DNA origami nanostructures. Using the AFM based manipulation, we show that the normal force required to damage graphene encapsulated DNA origami nanostructures is over an order of magnitude greater than for the unprotected ones. In addition, we show that graphene encapsulation offers protection to the DNA origami nanostructures against prolonged exposure to deionized water, and multiple immersions. Through these results we demonstrate that graphene encapsulated DNA origami nanostructures are strong enough to sustain various solution phase processing, lithography and transfer steps, thus extending the limits of DNA-mediated bottom-up fabrication. KW - atomic force microscopy KW - graphene KW - DNA origami nanostructures PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-358741 UR - http://iopscience.iop.org/article/10.1088/1367-2630/18/2/025016 DO - https://doi.org/10.1088/1367-2630/18/2/025016 SN - 1367-2630 VL - 18 SP - 025016 PB - IOP PUBLISHING LTD CY - Bristol, UK AN - OPUS4-35874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ermilov, Eugeny A. A1 - Liu, J.-Y. A1 - Menting, R. A1 - Huang, Y.-S. A1 - Röder, B. A1 - Ng, D. K. P. T1 - An artificial photosynthetic model based on a molecular triad of boron dipyrromethene and phthalocyanine N2 - A boron dipyrromethene (BDP) unit and its monostyryl derivative (MSBDP) were introduced at the axial positions of a silicon(IV) phthalocyanine (SiPc) core. The absorption spectrum of this compound virtually covered the entire visible region (300-700 nm) and could be interpreted as a superposition of the spectra of individual components. The intramolecular photoinduced energy and charge transfer processes of this triad were studied using steady-state and time-resolved spectroscopic methods in polar and nonpolar solvents. Upon BDP-part excitation, a fast and highly efficient excitation energy transfer (EET) occurred resulting in strong quenching of its fluorescence and the formation of the first excited singlet state of SiPc or MSBDP. It was found that both EET and charge transfer (CT) processes competed with each other in the depopulation of the first excited singlet state of the MSBDP moiety. The former strongly superseded CT in nonpolar toluene, whereas the latter was dominant in a polar environment. Direct or indirect (via EET) excitation of the SiPc-part of the triad was followed by CT yielding the charge-separated (CS) species BDP-SiPc center dot--MSBDP center dot+. The energy gap between the CS state and the S-1-state of the SiPc moiety was found to be only 0.06 eV in toluene, which facilitated the back CT process and resulted in the appearance of thermally activated delayed fluorescence. With increasing solvent polarity, the energy of the CS state reduced resulting in the disappearance of the delayed fluorescence in CHCl3, tetrahydrofuran or N,N-dimethylformamide. The charge recombination rate, k(CR), was very fast in polar DMF (3.3 x 10(10) s(-1)), whereas this process was two-orders of magnitude slower in nonpolar toluene (k(CR) = 4.0 x 10(8) s(-1)). KW - Photoinduced electron-transfers KW - Zinc phthalocyanine KW - Solar-energy KW - Charge separation KW - Solvent polarity KW - Porphyrin KW - Excitation KW - Fullerene KW - Recombination KW - Carotenoids PY - 2016 DO - https://doi.org/10.1039/c6cp00920d VL - 18 IS - 16 SP - 10964 EP - 10975 PB - Royal Soc Chemistry CY - Cambridge, UK AN - OPUS4-36271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nagli, L. A1 - Gaft, M. A1 - Gornushkin, Igor B. A1 - Glaus, Reto T1 - Stimulated emission and lasing in laser-induced plasma plume N2 - The lasing effect is demonstrated in laser plasmas induced on various metal targets and pumped by a laser tuned in resonance with a strong optical transition of a metal. The intense, polarized and lowdivergent radiation is emitted from a longitudinally pumped plasma plume in forward and backward directions with respect to the pump beam. Lasing occurs only within duration of the pumping pulse. The effect is found for elements of 13th and 14th groups and for Ca, Ti, Zr, Fe and Ni. The Einstein coefficients for spontaneous emission of all lasing transitions are higher than 10⁷ s⁻¹. For some elements like Al and In, a three-level lasing scheme is realized. For others, like Tl, both three- and four-level lasing schemes are realized. It is found that the longitudinal pump geometry is more efficient than the transversal one. KW - Optically pumped plasma lasers KW - Laser Induced Breakdown Spectroscopy (LIBS) KW - Laser Induced Fluorescence (LIF) PY - 2016 DO - https://doi.org/10.1016/j.optcom.2016.05.071 SN - 0030-4018 VL - 378 SP - 41 EP - 48 PB - Elsevier CY - Amsterdam, Netherlands AN - OPUS4-36320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Olejko, Lydia A1 - Cywinski, P. A1 - Bald, Ilko T1 - An ion-controlled four-color fluorescent telomeric switch on DNA origami structures N2 - The folding of single-stranded telomeric DNA into guanine (G) quadruplexes is a conformational change that plays a major role in sensing and drug targeting. The telomeric DNA can be placed on DNA origami nanostructures to make the folding process extremely selective for K+ ions even in the presence of high Na+ concentrations. Here, we demonstrate that the K+-selective G-quadruplex formation is reversible when using a cryptand to remove K+ from the G-quadruplex. We present a full characterization of the reversible switching between single-stranded telomeric DNA and G-quadruplex structures using Förster resonance energy transfer (FRET) between the dyes fluorescein (FAM) and cyanine3 (Cy3). When attached to the DNA origami platform, the G-quadruplex switch can be incorporated into more complex photonic networks, which is demonstrated for a three-color and a four-color FRET cascade from FAM over Cy3 and Cy5 to IRDye700 with G-quadruplex-Cy3 acting as a switchable transmitter. KW - DNA origami KW - FRET KW - Photonic wire KW - G quadruplex PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-362560 DO - https://doi.org/10.1039/C6NR00119J SN - 2040-3364 SN - 2040-3372 VL - 8 IS - 19 SP - 10339 EP - 10347 PB - Royal Soc Chemistry CY - Cambridge, UK AN - OPUS4-36256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Anwendungsbeispiele für den Einsatz von Drohnen - Lokalisierung von Gasemissionsquellen, Erstellung von Gasverteilungskarten und Bekämpfung des Eichenprozessionsspinners N2 - Der Vortrag gibt Beispiele dafür, wie Drohnen sinnvoll im zivilen Bereich eingesetzt werden können. Insbesondere werden die Lokalisierung von Gasemissionsquellen, die Erstellung von Gasverteilungskarten und die Bekämpfung des Eichenprozessionsspinners näher vorgestellt. T2 - DRONEMASTERS.Berlin MeetUp #01.16 CY - Berlin, Germany DA - 27.01.2016 KW - Lokalisierung von Gasemissionsquellen KW - Erstellung von Gasverteilungskarten KW - Eichenprozessionsspinner PY - 2016 AN - OPUS4-36225 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Lazik, D. A1 - Bartholmai, Matthias T1 - Tomographic reconstruction of soil gas distribution from multiple gas sources based on sparse sampling N2 - A monitoring method is introduced that creates twodimensional (2D) maps of the soil gas distribution. The method combines linear gas sensing technology for in-situ monitoring of gases in soil with the mapping capabilities of Computed Tomography (CT) to reconstruct spatial and temporal resolved gas distribution maps. A weighted iterative algebraic reconstruction method based on Maximum Likelihood with Expectation Maximization (MLEM) in combination with a source-by-source reconstruction approach is introduced that works with a sparse setup of orthogonally-aligned linear gas sensors. The reconstruction method successfully reduces artifact production, especially when multiple gas sources are present, allowing the discrimination between true and non-existing so-called ghost source locations. Experimental validation by controlled field experiments indicates the high potential of the proposed method for rapid gas leak localization and quantification with respect to Pipeline or underground gas storage issues. KW - Computed tomography KW - Gas distribution mapping and gas source localization KW - Discrimination of multiple gas sources KW - Distributed linear sensor KW - Membrane-based gas sensing KW - Subsurface monitoring KW - Gas storage areas PY - 2016 DO - https://doi.org/10.1109/JSEN.2016.2545103 SN - 1530-437X VL - 16 IS - 11 SP - 4501 EP - 4508 PB - IEEE - Inst. Electrical Electronics Engineers Inc CY - Hoes Lane, NJ, USA AN - OPUS4-36228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Glamsch, Stephan A1 - Ehlert, Christopher A1 - Lippitz, Andreas A1 - Kulak, N. A1 - Unger, Wolfgang T1 - Synchrotron-radiation XPS analysis of ultra-thin silane films: Specifying the organic silicon N2 - The analysis of chemical and elemental in-depth variations in ultra-thin organic layers with thicknesses below 5 nm is very challenging. Energy- and angle-resolved XPS (ER/AR-XPS) opens up the possibility for non-destructive chemical ultra-shallow depth profiling of the outermost surface layer of ultra-thin organic films due to its exceptional surface sensitivity. For common organic materials a reliable chemical in-depth analysis with a lower limit of the XPS information depth z95 of about 1 nm can be performed. As a proof-of-principle example with relevance for industrial applications the ER/AR-XPS analysis of different organic monolayers made of amino- or benzamidosilane molecules on silicon oxide surfaces is presented. It is demonstrated how to use the Si 2p core-level region to non-destructively depth-profile the organic (silane monolayer) – inorganic (SiO2/Si) interface and how to quantify Si species, ranging from elemental silicon over native silicon oxide to the silane itself. The main advantage of the applied ER/AR-XPS method is the improved specification of organic from inorganic silicon components in Si 2p core-level spectra with exceptional low uncertainties compared to conventional laboratory XPS. KW - Synchrotron radiation XPS KW - Depth profiling KW - Silanes KW - Monolayer KW - Amines KW - Amides PY - 2016 DO - https://doi.org/10.1016/j.apsusc.2015.12.052 SN - 0169-4332 SN - 1873-5584 VL - 363 SP - 406 EP - 411 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-35262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schott, M. A1 - Szczerba, Wojciech A1 - Posset, U. A1 - Vuk, A.S. A1 - Beck, M. A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas A1 - Kurth, D. G. T1 - In operando XAFS experiments on flexible electrochromic devices based on Fe(II)-metallo-supramolecular polyelectrolytes and vanadium oxides N2 - Flexible electrochromic devices (ECDs) based on Fe(II)-metallo-supramolecular polyelectrolytes (Fe-MEPE) and vanadium oxide are studied in operando by means of x-ray absorption fine structure (XAFS) spectroscopy. The ECDs are blue-purple in the colored state at 0.0 V and become light yellow when a voltage of 1.6 V is applied. The XAFS studies at the K-edge of Fe(II) reveals that the absorption edge is shifted toward higher energies by 1.8 eV in the transparent state. Comparison of two different ECDs and different charge cycles demonstrates the reversibility and repeatability of the process. We attribute the shift to a charge transfer and a change of oxidation state of the ions from Fe2+ to Fe3+. The transition is not accompanied by a noticeable structural change of the octahedral coordination geometry as confirmed by analysis of the extended x-ray absorption fine structure (EXAFS) data. (C) 2015 Elsevier B.V. All rights reserved. KW - Metallo-supramolecular polyelectrolytes KW - Vanadium oxide KW - Electrochromism KW - Electrochromic device KW - Cyclic voltammetry KW - XAFS PY - 2016 DO - https://doi.org/10.1016/j.solmat.2015.10.015 SN - 0927-0248 VL - 147 SP - 61 EP - 67 PB - Elsevier B.V. CY - Amsterdam [u.a.] AN - OPUS4-35251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mieller, Björn A1 - Vogl, Jochen A1 - Noordmann, J. A1 - Kaltenbach, A. A1 - Rienitz, O. T1 - Preparation and characterization of primary magnesium mixtures for the ab initio calibration of absolute magnesium isotope ratio measurements N2 - We report an appropriate preparation of binary isotope calibration mixtures of the three stable isotopes of magnesium to be used in the ab initio calibration of multicollector mass spectrometers (ICPMS and TIMS). For each of the three possible combinations of binary mixtures ("24Mg" + "25Mg", "24Mg" + "26Mg", and "25Mg" + "26Mg"), three individual setups have been prepared under gravimetric control, each of them with an isotope ratio close to unity, and a total magnesium mass fraction close to 20 mg kg-1. The preparation was designed to occur via an intermediate dilution of a parent solution of a highly purified specimen of the isotopically enriched magnesium materials. For the application as calibration mixtures, a complete uncertainty budget was set up, and is presented and discussed in detail, including the aspects that went into the design of the dilution and mixing approach to minimize uncertainty. The principle parameters for the purpose of the later calibration of the mass spectrometers are the absolute masses of isotopically enriched magnesium materials in the primary calibration mixtures. For the first time relative expanded uncertainties U (k = 2) for these masses of ≤0.005% could be achieved for all mixtures. KW - Atomic weight KW - Magnesium KW - Isotope mixture KW - Purity PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-352564 DO - https://doi.org/10.1039/c5ja00284b SN - 0267-9477 SN - 1364-5544 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. N1 - Corrigendum: Journal of analytical atomic spectrometry 34 (2019) 2340 VL - 31 IS - 1 SP - 179 EP - 196 PB - Royal Society of Chemistry CY - London AN - OPUS4-35256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Field integration of benchtop NMR instruments for online monitoring and process control of a modular industrial reaction step N2 - Online monitoring and process control requires fast and noninvasive analytical methods, which are able to monitor the concentration of reactants in multicomponent mixtures with parts-per-million resolution. Online NMR spectroscopy can meet these demands when flow probes are directly coupled to reactors, since this method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical comparison method being independent on the matrix. Due to improved magnet design and field shimming strategies portable and robust instruments have been introduced to the market by several manufacturers during the last few years. First studies with this technology showed promising results to monitor chemical reaction in the laboratory. Within the project CONSENS, the continuous production of high-value products in small production scale is advanced by introducing benchtop NMR spectroscopy. CONSENS is a research and innovation project on integrated control and sensing for sustainable operation of flexible intensified processes. This poster will present the first steps of the process integration of a benchtop NMR instrument for a lithiation process and outlines further fields of activity and potential challenges. Hereby, the following issues are going to be addressed: explosion-proof housing for the spectrometer, automation of signal processing (data pretreatment, evaluation and communication to the control system), flow cells and measuring conditions. Furthermore, first online spectra of the lithiation reaction in batch mode were acquired in lab scale. The reaction was performed in a 25 mL glass reactor with thermal jackets for temperature control of the reaction mixture. The Li-HMDS was dosed stepwise by using a glass syringe. First spectra in the proton and fluorine domain were recorded online using a flowrate of 3.5 mL min–1 and a simple 5 mm polytetrafluoroethylene tube (PTFE) as a flow cell. T2 - 4th Practical Applications of NMR in Industry Conference (PANIC) CY - Houston, Texas, USA DA - 15.02.2016 KW - Reaction monitoring KW - Online NMR spectroscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-354427 AN - OPUS4-35442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Hübert, Thomas A1 - Tiebe, Carlo A1 - Banach, Ulrich ED - Rodriguez Mendez, M. T1 - Electronic Noses for the Quality Control of Spices N2 - The chapter describes the application of electronic noses (multigas sensors) for the quality control of spices and spice mixtures. Electronic noses were successfully applied for headspace analysis of spices. It was demonstrated in many investigations that electronic noses can contribute to the characterization of spices and spice mixtures in order to distinguish spices and spice mixtures, differentiate by origin, growth seasons,and processing,indicate adulteration from original, detect mold infestation. Electronic noses can be used as a fast screening method to provide information about the product quality. However, it needs samples and methods for reference, careful training, and complex calibration to consider influencing and disturbing effects as well as the possible limitations of the instrumentation. The correlation to classical chemical analysis methods is always advisable. Machined olfaction methods are capable to support the sensory analysis; however, they cannot yet substitute them. KW - Spice KW - Electronic Nose KW - Multigas sensor KW - Quality control PY - 2016 SN - 978-0-12-800243-8 DO - https://doi.org/10.1016/B978-0-12-800243-8.00012-3 SP - Chapter 12, 115 EP - 124 PB - Academic Press CY - Oxford AN - OPUS4-35443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Online low-field NMR spectroscopy of an industrial lithiation reaction step for process control N2 - Online monitoring and process control requires fast and noninvasive analytical methods, which are able to monitor the concentration of reactants in multicomponent mixtures with parts-per-million resolution. Online NMR spectroscopy can meet these demands when flow probes are directly coupled to reactors, since this method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical comparison method being independent on the matrix. Due to improved magnet design and field shimming strategies portable and robust instruments have been introduced to the market by several manufacturers during the last few years. First studies with this technology showed promising results to monitor chemical reaction in the laboratory. Within the project CONSENS, the continuous production of high-value products in small production scale is advanced by introducing benchtop NMR spectroscopy. CONSENS is a research and innovation project on integrated control and sensing for sustainable operation of flexible intensified processes. This poster will present the first steps of the process integration of a benchtop NMR instrument for a lithiation process and outlines further fields of activity and potential challenges. Hereby, the following issues are going to be addressed: explosion-proof housing for the spectrometer, automation of signal processing (data pretreatment, evaluation and communication to the control system), flow cells and measuring conditions. Furthermore, first online spectra of the lithiation reaction in batch mode were acquired in lab scale. The reaction was performed in a 25 mL glass reactor with thermal jackets for temperature control of the reaction mixture. The Li-HMDS was dosed stepwise by using a glass syringe. First spectra in the proton and fluorine domain were recorded online using a flowrate of 3.5 mL min–1 and a simple 5 mm polytetrafluoroethylene tube (PTFE) as a flow cell. T2 - 10. Interdisziplinaeres Doktorandenseminar Fachgruppe "Analytische Chemie" der GDCh CY - Berlin, Germany DA - 28.02.2016 KW - Online NMR Spectroscopy KW - Reaction monitoring PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-354443 AN - OPUS4-35444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mull, Birte A1 - Jann, Oliver T1 - Biozidemissionen aus Materialien in die Luft N2 - Die meisten organischen Biozide gehören zu der Gruppe der schwerflüchtigen organischen Verbindungen (SVOC – semi volatile organic compounds). Zu den klassischen Bioziden zählen u.a. Lindan, Pentachlorphenol PCP) und Dichlordiphenyltrichlorethan (DDT) und zu den neueren u.a. Dichlofluanid, Tebuconazol und Permethrin. Biozide kamen in Museen vor allem in den 50er und 60er Jahren zum Schutz der Exponate zum Einsatz,1 wo sie hauptsächlich in Depoträumen zu finden sind, in welchen sie zum akuten und zum präventiven Schutz vor Schadorganismen eingesetzt wurden.2 Im Laufe der Zeit wurde jedoch festgestellt, dass sich der Einsatz von Bioziden negativ auf die menschliche Gesundheit auswirkt und auch zu Schäden an den behandelten Exponaten führen kann. 3 Verschiedene Möglichkeiten der Biozidanalytik und der Einfluss von Senkeneffekten auf die Analytik werden in diesem Beitrag vorgestellt. KW - Biozidanalytik KW - Schwerflüchtige organische Verbindungen KW - Emissionsmesskammer PY - 2015 SP - 12 EP - 14 CY - Berlin AN - OPUS4-35394 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröter, Maria-Astrid A1 - Sturm, Heinz A1 - Holschneider, M. T1 - Phase and amplitude patterns in DySEM mappings of vibrating microstructures N2 - We use a dynamic scanning electron microscope (DySEM) to analyze the movement of oscillating micromechanical structures. A dynamic secondary electron (SE) signal is recorded and correlated to the oscillatory excitation of scanning force microscope (SFM) cantilever by means of lock-in amplifiers. We show, how the relative phase of the oscillations modulate the resulting real part and phase pictures of the DySEM mapping. This can be used to obtain information about the underlying oscillatory dynamics. We apply the theory to the case of a cantilever in oscillation, driven at different flexural and torsional resonance modes. This is an extension of a recent work (Schr¨oter et al 2012 Nanotechnology 23 435501), where we reported on a general methodology to distinguish nonlinear features caused by the Imaging process from those caused by cantilever motion. KW - DySEM KW - mechanical nonlinearity KW - vibration KW - DySEM KW - mechanische Nichtlinearitäten KW - Vibration PY - 2013 DO - https://doi.org/doi:10.1088/0957-4484/24/21/215701 VL - 24 IS - 21 SP - 215701-1 EP - 215701-10 PB - IOP PUBLISHING LTD CY - Bristol, UK AN - OPUS4-35396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Siebler, Daniel T1 - A new generation of elastomeric polymer optical fibers and its potential for sensor applications N2 - This talk reflects recent progress in the detection of partial discharges in cables accessories with polymer optical fibers. T2 - Mahanakorn University of Technology, Bangkok, Thailand CY - Bangkok, Thailand DA - 17.01.2016 KW - fluorescence KW - partial discharge KW - silicone rubber KW - high voltage cable accessories KW - elastomeric polymer optical fiber POF KW - coincidence PY - 2016 AN - OPUS4-35397 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online NMR spectroscopy as a reference tool for model developments - Successful approaches in process analytical technology N2 - Quantitative Online NMR spectroscopy as a direct ratio method of analysis represents a perfect reference for calibration of further process analytical techniques, e.g., optical spectroscopic techniques. In this work we present a combined approach including Online NMR and Raman spectroscopy on a laboratory setup for development of suitable models for process monitoring. Therefore we investigated the absorption process of carbon dioxide in solutions of monoethanolamine, as well as the homogeneous catalyzed hydroformylation reaction of 1-dodecene taking place in an emulsion stabilized by a technical surfactant. The models for Raman spectroscopy were tested and approved during several days of operational studies of miniplant-scale setups for both mentioned applications. T2 - 4th Annual Practical Applications of NMR in Industry Conference (PANIC) CY - Houston, Texas, USA DA - 15.02.2016 KW - Online-NMR spectroscopy KW - Online-Raman spectroscopy KW - Process Analytical Technology PY - 2016 AN - OPUS4-35423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - di Matteo, G. A1 - Staude, Andreas A1 - Kuhn, R. A1 - Hertel, I. A1 - Seyfried, F. A1 - Reiche, I. ED - Reiche, I. T1 - Investigation of Ancient Egyptian Metallic Artefacts by Means of Micro-Computed Tomography N2 - In this paper we present the results of imaging studies of ancient Egyptian metallic artifacts using micro-Computed Tomography (micro-CT). Micro-CT is a non-destructive imaging method with high spatial resolution, which enables the examination of the internal structure of objects. It is thus especially suitable for the investigation of cultural heritage and archaeological findings, when it is not possible to sample or difficult to manipulate the object. Using specialized software for 3D visualization and segmentation, data sets of two objects were analyzed. We gained a clear view of the inner structure of a metallic archaeological artifact from the necropolis of Abusir el-Meleq, which is believed to be very ancient in the Egyptian archaeological context (from the Predynastic Era), and were able to distinguish its different omponents under the thick layers of external concretions. These components give hints about the production technology of the object. We also investigated the contents of a closed metal box found near Abusir dated to the Late/Greco-Roman Period. The identified Content corresponds either to sediments or to mineral remains of the original content of the box. Both artifacts are from excavations conducted in Egypt and are part of the archeological collection of the Ägyptisches Museum und Papyrussammlung in Berlin. KW - Computertomographie KW - computed tomography KW - Archäologie KW - archaeology KW - Metall KW - metal PY - 2015 SN - 0344-5089 VL - 23 SP - 79 EP - 84 CY - Berlin AN - OPUS4-35432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - qNMR under pressure - applications on compressed and liquefied gases N2 - During the last years quantitative NMR spectroscopy has become a general method for solving complex problems in science and industry. The opportunity of a calibration-free quantification, related to a simple counting of the nuclear spins in the active volume of the spectrometer represents a key advantage comparing to other analytical techniques. With modern NMR systems detection limits in the lower ppm range on a molar basis are accessible in a reasonable time period, which makes it a promising method for purity assessment, as well as applications in metrological research. First experiments showed that qNMR is suitable for gas analysis with respect to components used for production of primary reference gas mixtures. For this a laboratory setup for high-pressure NMR experiments up to 20 MPa (2900 psi) in fluid and gas phase was built and tested. In this work we show the determination of the composition of high precision mixtures, consisting of liquid and liquefied hydrocarbons commonly supplied in floating piston cylinders. Therefore an experimental setup was developed allowing sampling, as well as circulation of the mixture within a high-pressure NMR tube by using a concentric tubing assembly. Additionally, a piston-cylinder pressure cell was designed and manufactured allowing wide-range volume displacement. Mainly intended for density variation within supercritical fluid experiments, it can also function as a compression element for further increasing of gas-pressure in the system. Equipped with liquid thermostat and a motor-powered screw drive unit it is designed to operate at pressure levels up to 60 MPa (8700 psi) and temperatures up to 130 °C. T2 - 4th Annual practical applications of NMR in industry conference (PANIC) CY - Houston, TX, USA DA - 15.02.2016 KW - Gas-phase NMR KW - High-pressure NMR KW - Liquefied gases PY - 2016 AN - OPUS4-35435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bierstedt, Andreas T1 - Laser induced plasma ion source for ambient mass spectrometry N2 - Laser microprobe mass analysis (LMMS) employs local ionization by a focused laser and subsequent mass analysis. At excessive irradiation microplasmas led to undesired distortions. Thus, LMMS was discarded as promising ion source. Effective cooling under ambient conditions resulted in more controllable plasmas and development of laser induced breakdown spectroscopy (LIBS). However, little effort has been made to combine LIBS and ambient MS, since these plasmas only provide microsecond lifetimes. After these, recombination yields uncharged and newly bound species, making them inaccessible for MS. The combination of high repetition rate lasers together with growing knowledge about manipulation of charged species at atmospheric pressure allow overcoming these obstacles. T2 - 49. Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie (DGMS) CY - Hamburg, Germany DA - 28.02.2016 KW - laser induced plasma KW - ion source KW - ambient mass spectrometry KW - emission spectroscopy KW - laser induziertes Plasma KW - Ionenquelle KW - Atmosphärendruck-Massenspektrometrie KW - Emissionsspektroskopie PY - 2016 AN - OPUS4-35454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Warschat, Carsten T1 - Field-induced droplet ionization assisted by ultra sound N2 - Charge separation in liquid droplets within a strong electric field leads to opposite directed progeny droplet jets. That phenomenon is called field induced droplet ionization (FIDI). The jets contain charged molecules, which enables a mass spectrometric analysis. Acoustic levitation of droplets has matured to a powerful tool for containerless sample handling in micro fluidic systems in order to suppress agglomeration and classic contamination pathways. Herein we present the combination of both: FIDI assisted By Ultra-Sound (FIDIBUS). Compared to FIDI, it felicitates a steady observation of a single droplet during its jet formation. Furthermore, it allows for using different shaped electrodes and a multiple droplet interrogation. T2 - 49. Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie CY - Hamburg, Germany DA - 28.02.2016 KW - Massenspektrometrie KW - Mass Spectrometry KW - Akustische Levitation KW - Acoustic Levitation KW - Feld-induzierte Tropfenionisation KW - Field-Induced Droplet Ionization PY - 2016 AN - OPUS4-35462 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nachtigall, O. A1 - Kusserow, M. A1 - Clerac, R. A1 - Wernsdorfer, W. A1 - Menzel, Michael A1 - Renz, F. A1 - Mrozinski, J. A1 - Spandl, J. T1 - [Fe19] “Super-Lindqvist” Aggregate and Large 3D Interpenetrating Coordination Polymer from Solvothermal Reactions of [Fe2(OtBu)6] with Ethanol N2 - The syntheses, crystal structures, and physical properties of [HFe19O14(OEt)30] and {Fe11(OEt)24}1 are reported. [HFe19O14(OEt)30] has an octahedral shape. Its core with a central Fe metal ion surrounded by six m6-oxo ligands is arranged in the rock salt structure. {Fe11(OEt)24}1 is a mixedvalence coordination polymer in which FeIII metal ions form three 3D interpenetrating (10,3)-b nets. The arrangement of the FeIII ions can also be compared to that of Si ions in a-ThSi2. Thus, the described structures are at the interface between molecular and solid-state chemistry. KW - Solvothermal syntheses KW - Coordination polymers KW - Koordinationspolymere KW - Iron KW - Eisen KW - Polyoxometalates KW - Single-molecule magnets KW - Einzelmolekülmagnete PY - 2015 DO - https://doi.org/10.1002/anie.201503647 VL - 54 SP - 10361 EP - 10364 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-35368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heideklang, René A1 - Shokouhi, P. T1 - Decision-level fusion of spatially scattered multi-modal data for nondestructive inspection of surface defects N2 - This article focuses on the fusion of flaw indications from multi-sensor nondestructive materials testing. Because each testing method makes use of a different physical principle, a multi-method approach has the potential of effectively differentiating actual defect indications from the many false alarms, thus enhancing detection reliability. In this study, we propose a new technique for aggregating scattered two- or three-dimensional sensory data. Using a density-based approach, the proposed method explicitly addresses localization uncertainties such as registration errors. This feature marks one of the major of advantages of this approach over pixel-based image fusion techniques. We provide guidelines on how to set all the key parameters and demonstrate the technique's robustness. Finally, we apply our fusion approach to experimental data and demonstrate its capability to locate small defects by substantially reducing false alarms under conditions where no single-sensor method is adequate. KW - Multi-sensor data fusion KW - Density estimation KW - Scattered data KW - Defect detection KW - Nondestructive testing KW - Registration errors PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-352977 DO - https://doi.org/10.3390/s16010105 SN - 1424-8220 VL - 16 SP - Article Number: 105 PB - MDPI CY - Basel, Switzerland AN - OPUS4-35297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zerbst, Uwe A1 - Heckel, Thomas A1 - Carboni, M. T1 - Non-destructive testing and fracture mechanics - A short discussion N2 - A discussion is provided on the relation between non-destructive testing (NDT) and fracture mechanics. The basic tasks behind this are to guarantee the safety of a component at a potential hazard loading event, to specify inspection intervals or, alternatively, of demands on NDT for a fixed inspection regime, to plan accompanying measures for cases of temporary continued operation of structures in which cracks have been detected, and, finally, fatigue strength considerations which take into account initial defects. T2 - 42nd Annual review of progress in quantitative nondestructive evaluation conference CY - Minneapolis, Minnesota, USA DA - 2015-07-26 KW - Zerstörungsfreie Prüfung KW - Schwingfestigkeit KW - Schadenstoleranz KW - Bruchmechanik KW - probability KW - damage tolerance KW - railway axles KW - inspection PY - 2016 SN - 978-0-7354-1353-5 DO - https://doi.org/10.1063/1.4940614 SN - 0094-243X VL - 1706 SP - 150002-1 EP - 150002-5 PB - AIP Publishing CY - Melville, New York, USA AN - OPUS4-33866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wäsche, Rolf A1 - Hartelt, Manfred A1 - Hodoroaba, Vasile-Dan T1 - Analysis of nanoscale wear particles from lubricated steel-steel contacts N2 - A new method for sampling wear particles directly from the lubricant reservoir has been developed and applied successfully for analyzing wear particles by high-resolution scanning electron microscopy in transmission mode having coupled energy-dispersive X-ray spectroscopy. The lubricated tribological testing was carried out with fully formulated as well as with non-formulated synthetic base oil. It was possible to analyze individual particles with dimensions as small as about 5–30 nm which are likely the 'primary' wear particles. A majority of the particles, however, are agglomerated and, thus, lead to the formation of larger agglomerates of up to a few micrometers. Chemical analysis led to the conclusion that most of the observed particles generated in formulated oil, especially the larger ones, are composed of the additives of the lubricant oil. In non-formulated base oil, the primary particles are of similar dimensions but contain only iron, chromium and oxygen, but most likely stem from the mating materials. This finding points to the fact that the main wear mechanism under lubricated conditions with fully formulated oil is more like a continuous shearing process rather than a catastrophic failure with the generation of larger primary particles. When the oil is non-formulated, however, several wear mechanisms act simultaneously and the wear rate is increased significantly. Generated larger primary particles are milled down to the nanoscale. When the oil is fully formulated, wear mainly takes places at the additive layer or tribofilm; thus, the steel surface is protected. KW - Particle KW - Wear particle analysis KW - Lubricated contact KW - Bearing steel KW - Nanoscale T-SEM KW - Nanoscale EDX analysis PY - 2015 DO - https://doi.org/10.1007/s11249-015-0534-1 SN - 1023-8883 SN - 1573-2711 VL - 58 IS - 3 SP - 49-1 - 49-10 PB - Springer Science Business Media B.V. CY - Dordrecht AN - OPUS4-33525 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kabelitz, Anke A1 - de Oliveira Guilherme Buzanich, Ana A1 - Joester, Maike A1 - Reinholz, Uwe A1 - Radtke, Martin A1 - Bienert, Ralf A1 - Schulz, K. A1 - Schmack, R. A1 - Kraehnert, R. A1 - Emmerling, Franziska T1 - Time-resolved in situ studies on the formation mechanism of iron oxide nanoparticles using combined fast-XANES and SAXS N2 - The reaction of iron chlorides with an alkaline reagent is one of the most prominent methods for the synthesis of iron oxide nanoparticles. We studied the particle formation mechanism using triethanolamine as reactant and stabilizing agent. In situ fast-X-ray absorption near edge spectroscopy and small-angle X-ray scattering provide information on the oxidation state and the structural information at the same time. In situ data were complemented by ex situ transmission electron microscopy, wide-angle X-ray scattering and Raman analysis of the formed nanoparticles. The formation of maghemite nanoparticles (γ-Fe2O3) from ferric and ferrous chloride was investigated. Prior to the formation of these nanoparticles, the formation and conversion of intermediate phases (akaganeite, iron(II, III) hydroxides) was observed which undergoes a morphological and structural collapse. The thus formed small magnetite nanoparticles (Fe3O4) grow further and convert to maghemite with increasing reaction time. KW - oxidation state KW - structural information KW - maghemite PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351376 DO - https://doi.org/10.1039/C5CE01585E SN - 1466-8033 VL - 17 IS - 44 SP - 8463 EP - 8470 CY - London, UK AN - OPUS4-35137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hornemann, A. A1 - Eichert, D. A1 - Flemig, Sabine A1 - Ulm, G. A1 - Beckhoff, B. T1 - Qualifying label components for effective biosensing using advanced high-throughput SEIRA methodology N2 - The need for technological progress in bio-diagnostic assays of high complexity requires both fundamental research and constructing efforts on nano-scaled assay recognition elements that can provide unique selectivity and design-enhanced sensitivity features. Nanoparticle induced sensitivity enhancement and its application related to multiplexed capability Surface-Enhanced InfraRed Absorption (SEIRA) assay formats are well suitable for these purposes. The potential of diverse fluorophore–antibody conjugates, being chemisorbed onto low-cost gold nanoparticulate SEIRA substrates, has been explored with respect to their spectral discriminability. These novel biolabels deliver molecular SEIRA fingerprints that have been successfully analyzed by both uni- and multivariate analyzing tools, to discriminate their multiplexing capabilities. We show that this robust spectral encoding via SEIRA fingerprints opens up new opportunities for a fast, reliable and multiplexed high-end screening in biodiagnostics. KW - SEIRA methodology KW - bio-diagnostic KW - nanotechnology PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351389 DO - https://doi.org/10.1039/C4CP05944A SN - 1463-9076 SN - 1463-9084 VL - 17 IS - 14 SP - 9471 EP - 9479 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-35138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraehnert, R. A1 - Ortel, Erik A1 - Paul, B. A1 - Eckhardt, B. A1 - Kanis, M. A1 - Liu, R. A1 - Antoniou, A. T1 - Electrochemically dealloyed platinum with hierarchical pore structure as highly active catalytic coating N2 - Micro structured reactors are attractive candidates for further process intensification in heterogeneous catalysis. However, they require catalytic coatings with significantly improved space-time yields compared to traditional supported catalysts. We report the facile synthesis of homogeneous nanocrystalline Pt coatings with hierarchical pore structure by electrochemical dealloying of amorphous sputter-deposited platinum silicide layers. Thickness, porosity and surface composition of the catalysts can be controlled by the dealloying procedure. XPS analysis indicates that the catalyst surface is primarily composed of metallic Pt. Catalytic tests in gas-phase hydrogenation of butadiene reveal the typical activity, selectivity and activation energy of nanocrystalline platinum. However, space time yields are about 13 to 200 times higher than values reported for Pt-based catalysts in literature. The highly open metallic pore structure prevents heat and mass transport limitations allowing for very fast reactions and reasonable stability at elevated temperatures. KW - Pt catalysts KW - Pt–Si layers KW - Scanning Electron Microscopy (SEM) KW - Transmission Electron Microscopy (TEM) KW - pore structure KW - electrochemical dealloying PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351393 DO - https://doi.org/10.1039/C4CY00851K SN - 2044-4753 SN - 2044-4761 VL - 5 IS - 1 SP - 206 EP - 216 PB - RSC Publ. CY - Cambridge AN - OPUS4-35139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abbott, A. P. A1 - Abolibda, T. Z. A1 - Davis, S.J. A1 - Emmerling, Franziska A1 - Lourdin, D. A1 - Leroy, E. A1 - Wise, W. R. T1 - Glycol based plasticisers for salt modified starch N2 - Starch is one of the most common and easily obtained natural polymers, making it attractive as a potential bio-based alternative to synthetic polymers. This study shows that a simple quaternary ammonium salt combined with urea or glycols forms effective modifiers that produce flexible plastics with good mechanical properties that are comparable to some polyolefin plastics. The processing conditions are shown to significantly affect the structure of the polymer which has a concomitant effect upon the mechanical and physical properties of the resulting plastic. Using a glycerol based modifier results in a totally sustainable and biodegradable material which can be injection moulded. KW - biodegradable material KW - flexible plastics KW - injection moulded PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351426 DO - https://doi.org/10.1039/C4RA06220E SN - 2046-2069 VL - 4 IS - 76 SP - 40421 EP - 40427 PB - RSC Publishing CY - London AN - OPUS4-35142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hemmann, Felix A1 - Agirrezabal-Telleria, Iker A1 - Jäger, Christian A1 - Kemnitz, E. T1 - Quantification of acidic sites of nanoscopic hydroxylated magnesium fluorides by FTIR and 15N MAS NMR spectroscopy N2 - Lewis and Brønsted sites were quantified in a series of weak acidic hydroxylated magnesium fluorides by Fourier transform infrared spectroscopy (FTIR) and solid state nuclear magnetic resonance spectroscopy (NMR) with pyridine as probe molecule. Molar extinction coefficients, which are necessary for quantitative FTIR measurements, were calculated by an easy approach. It utilizes the fact that both signals, used for the quantification by FTIR, are caused by the same deformation vibration mode of pyridine. Comparison of quantitative FTIR experiments and quantification by NMR shows that concentrations of acidic sites determined by FTIR spectroscopy have to be interpreted with caution. Furthermore, it is shown that the transfer of molar extinction coefficients from one catalyst to another may lead to wrong results. Molar extinction coefficients and concentrations of acidic sites determined by FTIR spectroscopy are affected by grinding and probably the particle size of the sample. High temperature during FTIR experiments has further impact on the quantification results. KW - Acidity KW - Fluoride catalyst KW - Infrared spectroscopy KW - Adsorption of pyridine KW - Molar extinction coefficient determination PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351448 DO - https://doi.org/10.1039/C5RA15116C SN - 2046-2069 VL - 5 IS - 109 SP - 89659 EP - 89668 PB - RSC Publishing CY - London AN - OPUS4-35144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Christoph A1 - Shokouhi, P. T1 - Data aggregation for improved honeycomb detection in concrete using machine learning-based algorithms N2 - We present the results of several machine learning (ML)- inspired data fusion algorithms applied to multi-sensory nondestructive testing (NDT) data. Our dataset consists of Impact-Echo (IE), Ultrasonic Pulse Echo (US) and Ground Penetrating Radar (GPR) data collected on large-scale concrete specimens with built–in simulated honeycombing defects. The main objective is to improve the detectability of honeycombs by fusing the information from the three different sensors. We describe normalization, feature detection and optimal feature selection. We have used unsupervised and supervised ML, i.e., classification and clustering, for data fusion. We demonstrate the advantage of data fusion in reducing the false positives up to 10% compared to the best single sensor, thus, improving the detectability of the defects. The methods were evaluated on a concrete specimen. The effectiveness of the proposed approach was demonstrated on a separate full-scale concrete specimen. The results indicate the transportability of the conclusions from one specimen to the other. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - Data fusion KW - Concrete evaluation KW - Honeycombing KW - Machine learning KW - Clustering PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-350968 UR - https://www.ndt.net/?id=18364 SN - 1435-4934 VL - 20 IS - 11 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-35096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feldmann, Rüdiger A1 - Zoёga, Andreas A1 - Milmann, Boris A1 - Krause, Martin T1 - Ortung tiefliegender Bewehrung durch Ultraschall mit bildgebender Phasenauswertung N2 - Die Ortung von schlaffer Bewehrung in Beton erfolgt routinemäßig mit bildgebenden Radar- oder Wirbelstromverfahren. Die Anwendung dieser Verfahren ist aber begrenzt, wenn es sich um die Ortung tiefliegender Bewehrung (ab ca. 30 cm) oder um jungen Beton handelt. Grund ist die Schwächung der Radarpulse durch oberflächennahe Bewehrung oder durch die Betonfeuchte. Das bildgebende Ultraschallechoverfahren bietet den Vorteil, dass die Ultraschallpulse in diesen Fällen eine wesentlich höhere Eindringtiefe erreichen. Im vorliegenden Beitrag wird eine Fallstudie vorgestellt, bei der mehrlagig eingebrachte Bewehrungseisen in einer nur einseitig zugänglichen 60 cm dicken Betonplatte geortet werden sollten, um eine Kernbohrung ohne Verkanten der Bohrkrone durchzuführen. Zur Ortung der Bewehrung wurde das Ultraschallechoverfahren mitScherwellen der Mittenfrequenz 50 kHz mit einem automatisch arbeitenden Bauwerksscanner eingesetzt. Aus den flächig aufgenommenen Messdaten wurde mit der Rekonstruktionsrechnung nach dem Prinzip der synthetischen Apertur (SAFT, Synthetic Aperture Focusing Technique) die Position der Bewehrungseisen bildhaft ortsgenau dargestellt. Dies gelingt mit einer Auswertungsoption, bei der die Phase der reflektierten Ultraschallpulse ermittelt und farbcodiert dargestellt wird (Phasenauswertung). Damit lassen sich Reflexionen der Bewehrung eindeutig von eventuellen Fehlstellen oder Rückwandechos unterscheiden. T2 - Fachtagung Bauwerksdiagnose 2014 CY - Berlin, Germany DA - 13.02.2014 KW - Ultraschallecho-Verfahren KW - SAFT KW - Bewehrung KW - Beton KW - Abbildungsverfahren PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351056 UR - https://www.ndt.net/?id=15885 SN - 1435-4934 VL - 19 IS - 8 SP - 1 EP - 11 PB - NDT.net CY - Kirchwald AN - OPUS4-35105 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rothbart, Nick A1 - Maierhofer, Christiane A1 - Goldammer, M. A1 - Hohlstein, F. A1 - Koch, J. A1 - Kryukov, I. A1 - Mahler, G. A1 - Stotter, B. A1 - Oswald-Tranta, B. A1 - Sengebusch, M. T1 - A round robin test of flash thermography of CFRP and metal structures N2 - Within the scope of a DIN INS project, a flash thermography round robin test that evaluates reliability, comparability and efficiency of different testing situations is organized. The results give information about the detectability of defects e.g. by their size and depth, the evaluation method and by the materials used. Besides, the influence of equipment and parameters used by the participants on the results were analysed. All of the quantitative results as well as the feedback given by the participants will be presented in a DIN committee in order to contribute to a flash thermography standard. T2 - 7th International Symposium on NDT in Aerospace CY - Bremen, Germany DA - 16.11.2015 KW - Flash thermography KW - Round robin test KW - Metal KW - Flat bottom holes KW - SNR PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-351070 UR - https://www.ndt.net/?id=18921 SN - 1435-4934 VL - 21 IS - 4 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-35107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Wilke, Manuel A1 - Szczerba, Wojciech A1 - Reinholz, Uwe A1 - Emmerling, Franziska T1 - Mechanochemical synthesis and characterisation of two new bismuth metal organic frameworks N2 - Two metal organic structures composed of the ligands benzene-1,4-dicarboxylate and pyridine-2,5-dicarboxylate and bismuth cations are presented: (H2Im)[Bi(1,4-bdc)2] (1) and [Bi(pydc)(NO3)2(H2O)2]*H2O (2) (bdc = benzenedicarboxylate, H2Im = imidazole cation, pydc = pyridinedicarboxylate). Both compounds were synthesised via grinding and the crystal structure of compound (2) was solved based on its powder diffraction pattern. Compound 1 crystallises isostructurally to the dimethyl ammonium containing compound (dma)[(Bi(1,4-bdc)2]. Raman spectroscopy and Extended X-ray absorption fine structure (EXAFS) measurements provided additional information about the two mechanochemically synthesised metal organic compounds. KW - Crystal structure KW - Mechanochemically synthesis KW - Powder diffraction measurements PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-306296 DO - https://doi.org/10.1039/C3CE42633E SN - 1466-8033 N1 - Geburtsname von Batzdorf, Lisa: Tröbs, L. - Birth name of Batzdorf, Lisa: Tröbs, L. VL - 16 IS - 25 SP - 5560 EP - 5565 CY - London, UK AN - OPUS4-30629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Emmerling, Franziska T1 - Mechanochemical synthesis and characterisation of cocrystals and metal-organic compounds N2 - The mechanochemical synthesis of two model compounds, a metal organic framework ([Bi(1,4-bdc)2]*(Im) (bdc = benzene dicarboxylate, Im = imidazole cation)) and a cocrystal (Carbamazepine:Indometacin 1:1) were followed ex situ by combined analytical methods. Powder X-ray diffraction (XRD) and Raman spectroscopy data were evaluated for the synthesis of the metal organic framework. XRD measurements and REM images were analysed for the synthesis of the cocrystal. The measurements revealed that both model compounds were synthesised within minutes. The metal organic framework [Bi(1,4-bdc)2]*(Im) is synthesised via an intermediate structure. The cocrystal Carbamazepine:Indometacin 1:1 is formed within few seconds and afterwards the crystallite size decreases extremely. KW - Powder X-ray diffraction (XRD) KW - Raman spectroscopy KW - mechanochemical synthesis PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-306305 UR - http://pubs.rsc.org/en/content/articlepdf/2014/fd/c3fd00163f DO - https://doi.org/10.1039/C3FD00163F SN - 1359-6640 SN - 1364-5498 N1 - Geburtsname von Batzdorf, Lisa: Tröbs, L. - Birth name of Batzdorf, Lisa: Tröbs, L. SP - 109 EP - 119 PB - RSC CY - Cambridge [u.a.] AN - OPUS4-30630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Hodoroaba, Vasile-Dan A1 - Salge, T. A1 - Wirth, Thomas A1 - Lobera, M.P. A1 - Labrador, R.H. A1 - Natte, Kishore A1 - Behnke, Thomas A1 - Gross, Thomas A1 - Unger, Wolfgang T1 - High-resolution imaging with SEM/T-SEM, EDX and SAM as a combined methodical approach for morphological and elemental analyses of single engineered nanoparticles N2 - The combination of complementary characterization techniques such as SEM (Scanning Electron Microscopy), T-SEM (Scanning Electron Microscopy in Transmission Mode), EDX (Energy Dispersive X-ray Spectroscopy) and SAM (Scanning Auger Microscopy) has been proven to be a powerful and relatively quick characterization strategy for comprehensive morphological and chemical characterization of individual silica and titania nanoparticles. The selected “real life” test materials, silica and titania, are listed in the OECD guidance manual as representative examples because they are often used as commercial nanomaterials. Imaging by high resolution SEM and in the transmission mode by T-SEM allows almost simultaneous surface and in-depth inspection of the same particle using the same instrument. EDX and SAM enable the chemical characterization of bulk and surface of individual nanoparticles. The core–shell properties of silica based materials are addressed as well. Titania nominally coated by silane purchased from an industrial source has been found to be inhomogeneous in terms of chemical composition. KW - surface and in-depth inspection KW - silica nanoparticles KW - titania nanoparticles PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-316296 DO - https://doi.org/10.1039/c4ra05092d SN - 2046-2069 VL - 4 IS - 91 SP - 49577 EP - 49587 PB - RSC Publishing CY - London AN - OPUS4-31629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beckmann, Jörg A1 - Marchetti, B. A1 - von Chrzanowski, Lars S. A1 - Ritter, E. A1 - Puskar, L. A1 - Aziz, E. F. A1 - Schade, U. T1 - Optical constants of harmful and highly energetic liquids for application to THz screening systems N2 - The far-infrared (IR) optical constants of a set of hazardous and flammable liquids have been obtained by means of spectroscopic ellipsometry in attenuated total reflection configuration over a broad spectral range. Such liquids recently became of considerable concern for transportation security measures worldwide. Their optical identification at check-in gates can only become possible if the characteristic spectra are already known. The refractive indices and the extinction coefficients reported here contribute to a spectroscopic data base in the far-IR and terahertz (THz) spectral regions and may support modeling the performance of THz screening systems on liquids for airports and other security sensitive areas. Examples of several container material/liquid systems are discussed. From the measured optical constants typical THz waveforms are calculated and discussed. KW - liquids material characterization KW - Ellipsometry KW - FT-IR spectroscopy KW - THz time-domain spectroscopy (THz-TDS) PY - 2016 DO - https://doi.org/10.1109/TTHZ.2016.2547319 SN - 2156-342X VL - 2016 / Vol. PP IS - 99 SP - 1 EP - 12 PB - IEEE - Inst. Electrical Electronics Engineers Inc CY - New York, NY, USA AN - OPUS4-36366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schäferling, Michael T1 - Nanoparticle-based luminescent probes for intracellular sensing and imaging of pH N2 - Fluorescence imaging microscopy is an essential tool in biomedical research. Meanwhile, various fluorescent probes are available for the staining of cells, cell membranes, and organelles. Though, to monitor intracellular processes and dysfunctions, probes that respond to ubiquitous chemical parameters determining the cellular function such as pH, pO2, and Ca2+ are required. This review is focused on the progress in the design, fabrication, and application of photoluminescent nanoprobes for sensing and imaging of pH in living cells. The advantages of using nanoprobes carrying fluorescent pHindicators compared to single molecule probes are discussed as well as their limitations due to the mostly lysosomal uptake by cells. Particular attention is paid to ratiometric dual wavelength nanosensors that enable intrinsic referenced measurements. Referencing and proper calibration procedures are basic prerequisites to carry out reliable quantitative pH determinations in complex samples such as living cells. A variety of examples will be presented that highlight the diverseness of nanocarrier materials (polymers, micelles, silica, quantum dots, carbon dots, gold, photon upconversion nanocrystals, or bacteriophages), fluorescent pH indicators for the weak acidic range, and referenced sensing mechanisms, that have been applied intracellularly up to now. KW - pH sensing KW - Luminescent probes KW - Imaging PY - 2016 DO - https://doi.org/10.1002/wnan.1366 SN - 1939-0041 SN - 1939-5116 VL - 8 IS - 3 SP - 378 EP - 413 PB - Wiley-Blackwell CY - Hoboken, New Jersey, USA AN - OPUS4-36367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Quantitative NMR spectroscopy of technical mixtures and gases from elevated to high-pressure N2 - Recent technical developments of NMR instruments such as in acquisition electronics and probe design allow detection limits of components in liquid mixtures in the lower ppm range (approx.. 5–10 ppm amount of substance). The major advantage of quantitative NMR spectroscopy (qNMR) is that it is a direct ratio method of analysis without the need of calibration. This means that the signal for a specific NMR-active nucleus (e.g., a proton) in an analyte can be compared and quantified by reference to a different nucleus of a separate compound, comparable to a counting of spins in the active volume of the spectrometer. Technical mixtures can be investigated online directly next to a process setup by using flow probes. This makes it a promising method for process analytical applications, especially during process development in laboratory and pilot plant scale. With the growing market of Benchtop devices based on permanent magnets nowadays an integration of NMR spectroscopy in an industrial environment becomes reasonable. A special application of qNMR in technical mixtures is the observation in the gas phase, which is rarely applied compared to liquid and solid NMR studies. Because of the low density it results in a reduced sensitivity, which can be improved by applying pressure. Therefore a high-pressure NMR setup was developed based on a commercially available NMR tube made of zirconia. This is currently tested up to 20 MPa, but can be extended up to 100 MPa with regard to pressure rating of its components. This work shows results of gas-phase application on natural-gas like reference gas mixtures produced at BAM, as well as investigations on liquefied gas mixtures with high accuracy provided in piston cylinders. Besides that amine gas treatment and hydroformylation in a microemulsion represent two other examples of applications in process analytical technology. These show the potential of combination of online NMR spectroscopy with other spectroscopic methods, especially during model development for data evaluation. T2 - Presentation at Statoil Research Center CY - Trondheim, Norway DA - 27.05.2016 KW - Quantitative NMR spectroscopy KW - Process analytical technology KW - Gas-phase NMR PY - 2016 AN - OPUS4-36330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Batzdorf, Lisa A1 - Fischer, Franziska A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - Cadmium phenylphosphonates: preparation, characterisation and in situ investigation N2 - The successful mechanochemical syntheses of three cadmium phenylphosphonates indicates that mechanochemistry is ideally suited for synthesizing metal phosphonates. With this powerful synthesis tool it is possible to synthesize rapidly and efficiently both known and novel phosphonates. The Crystal structures of the two new compounds, and, were solved from PXRD data. They contain monodeprotonated phenylphosphonate and neutral phenylphosphonic acid ligands. The synthesis pathways of all three compounds were investigated in situ. A diffusion mechanism is corroborated by our findings. Intermediates could be detected and identified. The kinetically favored product (3) could always be detected during the syntheses. The thermodynamic stability of the compounds and the stoichiometric ratio of the starting materials are the two directing factors for the synthesis of the final products. KW - Mechanochemistry KW - Metal phosphonate KW - In situ KW - MOF KW - XRD PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-363322 DO - https://doi.org/10.1039/c6ra01080f SN - 2046-2069 VL - 6 IS - 42 SP - 36011 EP - 36019 PB - Royal Soc Chemistry CY - Cambridge, UK AN - OPUS4-36332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zientek, Nicolai A1 - Meyer, Klas A1 - Kern, Simon A1 - Maiwald, Michael T1 - Quantitative online NMR spectroscopy in a nutshell N2 - Online NMR spectroscopy is an excellent tool to study complex reacting multicomponent mixtures and gain process insight and understanding. For online studies under process conditions, flow NMR probes can be used in a wide range of temperature and pressure. This paper compiles the most important aspects towards quantitative process NMR spectroscopy in complex multicomponent mixtures and provides examples. After NMR spectroscopy is introduced as an online method and for technical samples without sample preparation in deuterated solvents, influences of the residence time distribution, pre-magnetization, and cell design are discussed. NMR acquisition and processing parameters as well as data preparation methods are presented and the most practical data analysis strategies are introduced. KW - Prozessanalytik KW - Process analytical technology KW - Online NMR spectroscopy KW - Online monitoring PY - 2016 DO - https://doi.org/10.1002/cite.201500120 SN - 0009-286X VL - 88 IS - 6 SP - 698 EP - 709 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim, Germany AN - OPUS4-36333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tulke, A. T1 - Technologie-Roadmap „Prozesssensoren 4.0“ - Einführung und Beispiele N2 - Inhalt des Vortrags sind die Einführung und Erläuterung der Ziele und Inhalte der Technologie-Roadmap „Prozesssensoren 4.0“, welche von der NAMUR im November 2015 veröffentlicht wurde. Dazu werden Beispiele von aktuellen und zukünftigen Anwendungen erläutert. Derzeit finden gravierende Veränderungen im Umfeld der Informations- und Kommunikationstechnik statt, die eine große Chance für die optimierte Prozessführung und Wertschöpfung mit darauf abgestimmten vernetzt kommunizierenden Sensoren bieten. Diese Art „smarter“ Sensoren stellen Dienste innerhalb eines Netzwerks bereit und nutzen Informationen daraus. Dadurch ergibt sich aktuell die Notwendigkeit, die Anforderungen an Prozesssensoren sowie an deren Kommunikationsfähigkeiten detaillierter zu beschreiben. Vernetzte Sensoren sind die Voraussetzung für die Realisierung von Cyberphysischen Produktionssystemen (CPPS) und zukünftiger Automatisierungskonzepte für die Prozess-industrie. Wesentliche Ziele der Roadmap sind das Zusammenbringen von Technologie- und Marktsicht, Analyse und Priorisierung des (zukünftigen) Informationsbedarfs in verfahrenstechnischen Prozessen, das Erarbeiten von Entwicklungszielen für neue Sensorik sowie das Aufzeigen möglicher Lösungsansätze und ihres Realisierungszeitraums. Darüber hinaus liefert sie Perspektiven für Forschungs- und Entwicklungsförderung und gibt Ansätze für die Normungsarbeit. T2 - Automation 2016 - 17. Branchentreff der Mess- und Automatisierungstechnik CY - Baden Baden DA - 07.06.2016 KW - Prozessanalytik KW - Smart Sensors KW - Industrie 4.0 KW - Automation PY - 2016 AN - OPUS4-36392 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - The structure and in situ synthesis investigation of isomorphic mononuclear molecular metal phenylphosphonates N2 - We describe a fast and effective synthesis for molecular metal phosphonates. Isomorphic compounds [M(II)(HO₃PPh)₂(H₂O₃PPh)₂(H₂O)₂] (M = Mn (1), Co (2), Ni (3); Ph = C₆H₅) were obtained by grinding. The complexes are mononuclear compounds containing neutral and monodeprotonated phenylphosphonic acid and water as ligands. The crystal structures were determined using powder X-ray diffraction (PXRD) data and validated by extended X-ray absorption fine structure (EXAFS) data. Combined synchrotron XRD measurements and Raman spectroscopy were conducted for investigating the reactions in situ. Based on these data, the intermediates were characterized and the formation mechanism was derived. KW - Mechanochemistry KW - Metal phosphonate KW - In situ KW - XRD PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-363944 DO - https://doi.org/10.1039/c6dt00787b SN - 1477-9226 SN - 1477-9234 SN - 1364-5447 VL - 45 IS - 23 SP - 9460 EP - 9467 AN - OPUS4-36394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Katsikini, M. A1 - Pinakidou, F. A1 - Paloura, E.C. A1 - Arvanitidis, J. A1 - Ves, S. A1 - Reinholz, Uwe A1 - Ppadomanolaki, E. A1 - Iliopoulos, E. T1 - Simulation of the EXAFS and Raman spectra of InxGa1-xN utilizing the equation of motion routine of FEFF8 N2 - A combined analysis of EXAFS and Raman spectra is applied for the study of InxGa1-xN alloys with 0.3 100 μm). Data for a sedimentation basin indicate that the fine fraction ( < 50 μm) is preferentially transported by road runoffinto receiving waters. The size distribution and density data of TRWP gathered by three different quantitation approaches also suggest that aging of TRWPs leads to changes in their particle density. An improved understanding of the dynamics of TRWP properties is essential to assess the distribution and dissipation of this contaminant of emerging concern in the environment. KW - Tire Wear KW - Density separation KW - Microplastic KW - Urban PY - 2020 DO - https://doi.org/10.1016/j.watres.2020.116262 VL - 185 SP - 116262 PB - Elsevier Ltd. AN - OPUS4-51256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Smol, M. A1 - Adam, Christian A1 - Kugler, Stefan T1 - Analiza możliwości wykorzystania w Polsce popiołów ze spalania komunalnych osadów ściekowych na cele nawozowe T1 - Use of municipal sewage sludge ash for fertilizing purposes. An analysis of possibilities in Poland N2 - Popioły pochodzące z instalacji do spalania komunalnych osadów ściekowych, znajdującej się na terytorium Polski, poddano procesom termochemicznego przekształcania, dzięki czemu otrzymano produkty nawozowe spełniające kryteria dopuszczające je do obrotu jako nawozy mineralne. Ponadto dokonano analizy możliwości wykorzystania popiołów na cele nawozowe zgodnie z obecnie przyjętymi dokumentami strategicznymi i planistycznymi dotyczącymi gospodarki odpadami na poziomie krajowym i europejskim. N2 - Ashes from thermal transformation of municipal sewage sludge were thermochem. modified at 1000°C in the presence of NaHCO3 and sewage sludge to obtain CaNaPO4 and reduce the content of heavy metals in the produced fertilizer. Its bioavailability was more than 99% higher than that of raw ashes (50%). The nutrient content was 13.56 % Ca, 6.33% P, 4.36% K and 5.0% Fe. The content of heavy metals in fertilizer products met the std. requirements and was exceeded only in the case of Pb (278.3 mg/kg d.m.). KW - Ashes KW - Waste KW - Phosphorus KW - Recovery KW - Fertilizer PY - 2020 DO - https://doi.org/10.15199/62.2020.8.14 VL - 99 IS - 8 SP - 1186 EP - 1191 AN - OPUS4-51267 LA - pol AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lumpe, H. A1 - Menke, Annika A1 - Haisch, C. A1 - Mayer, P. A1 - Kabelitz, Anke A1 - Yusenko, Kirill A1 - de Oliveira Guilherme Buzanich, Ana A1 - Block, T. A1 - Pöttgen, R. A1 - Emmerling, Franziska A1 - Daumann, L. T1 - The Earlier the Better: Structural Analysis and Separation of Lanthanides with Pyrroloquinoline Quinone N2 - Lanthanides (Ln) are critical raw materials, however, their mining and purification have a considerable negative environmental impact and sustainable recycling and separation strategies for these elements are needed. In this study, the precipitation and solubility behavior of Ln complexes with pyrroloquinoline quinone (PQQ), the cofactor of recently discovered lanthanide (Ln) dependent methanol dehydrogenase (MDH) enzymes, is presented. In this context, the molecular structure of a biorelevant europium PQQ complex was for the first time elucidated outside a protein environment. The complex crystallizes as an inversion symmetric dimer, Eu2PQQ2, with binding of Eu in the biologically relevant pocket of PQQ. LnPQQ and Ln1Ln2PQQ complexes were characterized by using inductively coupled plasma mass spectrometry (ICP‐MS), infrared (IR) spectroscopy, 151Eu‐Mössbauer spectroscopy, X‐ray total scattering, and extended X‐ray absorption fine structure (EXAFS). It is shown that a natural enzymatic cofactor is capable to achieve separation by precipitation of the notoriously similar, and thus difficult to separate, lanthanides to some extent. KW - PQQ KW - Lanthanoide KW - Coordination chemistry KW - Rare earth elements separations PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512707 DO - https://doi.org/10.1002/chem.202002653 VL - 26 IS - 44 SP - 10133 EP - 10139 AN - OPUS4-51270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland T1 - Non-invasive cancer detection using volatile biomarkers: Is urine superior to breath? N2 - In recent years numerous reports have highlighted the options of chemical breath analysis with regard to noninvasive cancer detection. Certain volatile organic compounds (VOC) supposedly present in higher amounts or in characteristic patterns have been suggested as potential biomarkers. However, so far no clinical application based on a specific set of compounds appears to exist. Numerous reports on the capability of sniffer dogs and sensor arrays or electronic noses to distinguish breath of cancer patients and healthy controls supports the concept of genuine cancer-related volatile profiles. However, the actual compounds responsible for the scent are completely unknown and there is no correlation with the potential biomarkers suggested on basis of chemical trace analysis. It is outlined that specific features connected with the VOC analysis in breath – namely small concentrations of volatiles, interfering background concentrations, considerable sampling effort and sample instability, impracticability regarding routine application - stand in the way of substantial progress. The underlying chemicalanalytical challenge can only be met considering the severe susceptibility of VOC determination to these adverse conditions. Therefore, the attention is drawn to the needs for appropriate quality assurance/quality control as the most important feature for the reliable quantification of volatiles present in trace concentration. Consequently, the advantages of urine as an alternative matrix for volatile biomarker search in the context of diagnosing lung and other cancers are outlined with specific focus on quality assurance and practicability in clinical chemistry. The headspace over urine samples as the VOC source allows adapting gas chromatographical procedures well-established in water analysis. Foremost, the selection of urine over breath as non-invasive matrix should provide considerably more resilience to adverse effects during sampling and analysis. The most important advantage of urine over breath is seen in the option to partition, dispense, mix, spike, store, and thus to dispatch taylor-made urine samples on demand for quality control measures. Although it is still open at this point if cancer diagnosis supported by non-invasively sampled VOC profiles will ultimately reach clinical application the advantages of urine over breath should significantly facilitate urgently required steps beyond the current proof-of-concept stage and towards standardisation. KW - VOC KW - Breath KW - Urine KW - Lung cancer KW - Volatile organic compounds PY - 2020 DO - https://doi.org/10.1016/j.mehy.2020.110060 VL - 143 SP - 110060 PB - Elsevier Ltd. AN - OPUS4-51066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sennikov, P. A1 - Gornushkin, Igor B. A1 - Kornev, R. A1 - Nazarov, V. A1 - Polyakov, V. A1 - Shkrunin, V. T1 - Hydrogen Reduction of MoF6 and Molybdenum Carbide Formation in RF Inductively Coupled Low‑Pressure Discharge: Experiment and Equilibrium Thermodynamics Consideration N2 - The physical plasma parameters, temperature and electron number density, are studied in the RF-IC (RF inductively coupled) discharge at a reduced pressure of 3 Torr in mixtures of MoF6 with Ar, H2 and CH4. The emission spectra of mixtures are investigated. It is shown that in the presence of argon, the concentration of free electrons in plasma and dissociation rate of MoF6 increase. A main role of molecular hydrogen is the generation of atomic hydrogen that binds atomic fuorine and leads to the formation of gaseous and solid products. Exhaust gas mixtures exiting the reactor are analyzed by mass spectrometry. It is shown that for all cases, the conversion of MoF6 into reaction products is close to 100%. A thermodynamic analysis of the equilibrium composition of MoF6 systems with Ar, H2 and CH4 was carried out and the obtained results are in good agreement with experimentally observed composition of the solid and gas phases. Analysis of solid deposits from mixture MoF6/H2/Ar revealed the presence of molybdenum powder and large amount of amorphous MoFx. The deposit obtained from mixtures with methane, MoF6/H2/Ar/CH4, contained crystalline molybdenum carbide, Mo3C2. KW - Molybdenum carbide KW - RF ICP discharge KW - Reduction of MoF6 KW - Thermodynamic KW - Molybdenum PY - 2020 DO - https://doi.org/10.1007/s11090-020-10138-3 SN - 0272-4324 VL - 41 IS - 2 SP - 673 EP - 690 PB - Springer AN - OPUS4-51569 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Puthiyaveettil, N. A1 - Thomas, K. R. A1 - Myrach, Philipp A1 - Ziegler, Mathias A1 - Rajagopal, P. A1 - Balasubramaniamam, K. T1 - Defect detection in steel bars up to 600 °C using laser line thermography N2 - Crack detection in steel bars at high surface temperatures is a critical problem in any manufacturing industry. Surface breaking cracks are the major problems during the billet casting. Many NDT techniques are proven its capability in crack detection at room temperature. Here, we are demonstrating the possibility of exposure of cracks using laser line thermography at higher surface temperatures (up to 600 °C). A continuous-wave (CW) laser is used to excite the sample kept at higher surface temperatures. The temperature distribution over the sample due to the laser line scanning is captured using a temperature calibrated infrared (IR) thermal camera. The response of the sample temperature in crack detection is investigated using a validated FE model. The impact of the oxide layer in crack detection is investigated by using two types of samples; one without any oxide layer and the second is with the oxide layer. The influence of laser power in the detection of defects at high temperatures is studied. 3D numerical models were developed for the cases; when the sample is with oxide layer and without any oxide layer for a better understanding of physics. The surface temperature rise due to laser heating is higher for the scaled sample compared to the no-scale sample. The presence of the oxide layer above the parent metal will reduce the reflectivity of the surface. Lower reflectivity will lead to increased absorption of incident energy so that the surface temperature rise will be higher than the surface with no scale. Thermal contrast linearly depends on laser power, which means higher laser power will increase the defect detectability even at a higher surface temperature. KW - Laser thermography KW - High temperature KW - Modeling KW - Surface cracks KW - Non-destructive testing PY - 2020 DO - https://doi.org/10.1016/j.infrared.2020.103565 SN - 1350-4495 VL - 111 SP - 103565 PB - Elsevier B.V. AN - OPUS4-51573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Beck, Uwe A1 - Fischer, Daniel T1 - MISTRAL-Müller-Matrix-basierte Identifizierung von Inhomogenitäten und strukturellen Anomalien N2 - Mit abbildender Ellipsometrie (imaging ellipsometry: IE) können Nanometer-Beschichtungen/ Degradationen visualisiert und bezüglich Brechungsindex n, Extinktionskoeffizient k und Schichtdicke d charakterisiert werden. Materialseitig werden lokal Homogenität und Isotropie innerhalb eines/mehrerer Bildpunkte (field of analysis: FOA) und messtechnisch global die Ebenheit der Proben bezüglich aller Bildpunkte des Messfeldes vorausgesetzt. Für die Müller-Matrix-basierte abbildende Ellipsometrie (MM-IE), die den optischen Response anisotroper Materialien in jedem Bildpunkt über die bis zu 16 Müller-Matrix-Elemente erfasst, ist dies von besonderer Relevanz. Reale Substrate sind aber oft nicht eben, können lokal Noppen/Mulden (im FOA) aufweisen oder sind global konvex/ konkav im möglichen Messfeld (field of view: FOV) gekrümmt. Diese lokalen/globalen strukturellen Anomalien des Substrats werden schon für die IE messtechnisch/modellseitig oft nicht beherrscht und sind für die MM-IE in der Wirkung auf die MM-Elemente unbekannt. Diese Defizite sollen messtechnisch bzw. modellmäßig behoben und somit die Messung lokal/global gekrümmter Oberflächen ermöglicht werden (MM-CSIE, CS curved surface). KW - Abbildende Ellipsometrie (IE) KW - Müller-Matrix Ellipsometrie (MM-IE) KW - Gekrümmte Oberflächen KW - Schichtdicke KW - Optische Konstanten PY - 2020 SP - 1 EP - 7 AN - OPUS4-51574 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim A1 - Strangfeld, Christoph A1 - Ritzer, Tobias A1 - Kruschwitz, Sabine T1 - Nondestructive determination of moisture damage in layered building floors N2 - In this ongoing research project, we study the influence of moisture damage on Ground Penetrating Radar (GPR) in different floor constructions. For this purpose, a measurement setup with interchangeable layers is developed to vary the screed material (cement or anhydrite) and insulation material (glass wool, perlite, expanded and extruded polystyrene), as well as the respective layer thickness. The evaluation of the 2 GHz common-offset radar measurements is focused on the extraction of distinctive signal features that can be used to classify the underlying case of damage without any further information about the hidden materials or layer thicknesses. In the collected dataset, we analyze the horizontal distribution of A-scan features in corresponding B-scans to detect water in the insulation layer. Furthermore, possible combinations of these features are investigated with the use of multivariate data analysis and machine learning (logistic regression) in order to evaluate the mutual dependencies. In this study, the combination of an amplitude- and frequency-based feature achieved an accuracy of 93.2 % and performed best to detect a damage in floor insulations. T2 - 18th International Conference on Ground Penetrating Radar CY - Meeting was canceled DA - 14.07.2020 KW - Radar KW - Feuchte KW - Moisture KW - Building floors PY - 2020 DO - https://doi.org/10.1190/gpr2020-045.1 SN - 2159-6832 SP - 164 EP - 167 AN - OPUS4-51575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Luftultraschall N2 - Dieser Vortrag bietet eine Einführung zur luftgekoppelten Ultraschallprüfung. Es werden die theoretischen Grundlagen erläutert und Beispiele für Anwendungen in der Praxis gegeben. T2 - Schulung Ultraschallprüfung Stufe 3 CY - Berlin, Germany DA - 28.09.2020 KW - Luftgekoppelte Ultraschallprüfung KW - Luftankopplung KW - Ultraschallwandler PY - 2020 AN - OPUS4-51578 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weber, K. T1 - Diagenetic stability of Ca, Mg, Zn and Sr isotopes in teeth N2 - Stable isotope ratios and trace element concentrations of fossil bones and teeth are important geochemical proxies for the reconstruction of diet and past environment in archaeology and palaeontology. However, since diagenesis can significantly alter in vivo incorporated isotope signatures and elemental compositions, it is important to understand alteration processes. Here, we present the results of in vitro alteration experiments of dental tissues from a modern African elephant molar in aqueous solutions at 30 °C and 90 °C for 4 to 63 days each. Dental cubes with ≈3 mm edge length, comprising both enamel and dentin, were placed into 2 ml of an acidic (HNO3) aqueous solution (pH ≈1) enriched with different isotopes (25Mg, 44Ca, 67Zn, 86Sr). Element and isotope distribution profiles across the different dental cubes were measured with LA-(MC-)ICP-MS and EMPA, while potential changes of the bioapatite crystal structure were characterised by Raman spectroscopy. Isotope ratios measured by LA-(MC-)ICP-MS revealed an alteration of the outer ≈200-300 μm of the enamel in all experiments. Dentin was fully altered after one week (at 90 °C) and the tracer solution started to penetrate through the dentin even into the innermost enamel. However, the central part of the enamel remained unaltered. The Raman spectra suggest a strong recrystallization in the dentin and in the outer ≈40 μm of the enamel and a partial demineralisation of the outer rim of the cubes. Our results indicate that independent of time, temperature or low initial pH, enamel apatite shows a high resistance against the experimental alteration in structure and isotopic composition, in contrast to dentin apatite. T2 - Goldschmidt Conference CY - Online meeting DA - 21.06.2020 KW - Isotope ratio KW - Diagenesis KW - Alteration KW - Bio-apatite PY - 2020 AN - OPUS4-51499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rienitz, O. A1 - Pramann, A. A1 - Vogl, Jochen A1 - Lee, K.-S. A1 - Yim, Y.-H. A1 - Malinovskiy, D. A1 - Hill, S. A1 - Dunn, P. A1 - Goenaga-Infante, H. A1 - Ren, T. A1 - Wang, J. A1 - Vocke jr., R. D. A1 - Rabb, S: A. A1 - Narukawa, T. A1 - Yang, L. A1 - Mester, Z. A1 - Meija, J. A1 - Aref'ev, D. G. A1 - Marchin, V. A1 - Sharin, A. G. A1 - Bulanov, A. D. A1 - Potapov, A. M. A1 - Otopkova, P. A. A1 - Kessel, R. T1 - The comparability of the determination of the molar mass of silicon highly enriched in 28Si: results of the CCQM-P160 interlaboratory comparison and additional external measurements N2 - An international comparison study on the accurate determination of the molar mass M(Si) of silicon artificially enriched in 28Si (x(28Si) > 0.9999 mol mol−1) has been completed. The measurements were part of the high level CCQM-P160 pilot study assessing the ability of National Metrology Institutes (NMIs) and Designated Institutes (DIs) to make such measurements at the lowest possible levels of measurement uncertainty and to identify possible difficulties when measuring this kind of sample. This study supports the molar mass measurements critical to disseminating the silicon route to realizing the new definitions for the kilogram and the mole. Measurements were also made by one external research institute and an external company. The different institutes were free to choose their experimental (mass spectrometric) set-ups and equipment, thereby enabling also the comparison of different techniques. The investigated material was a chemically pure, polycrystalline silicon material. The subsequent modified single crystalline secondary product of this material was intended for the production of silicon which was used for two additional spheres in the context of the redetermination of the Avogadro constant NA, required for the revision of the International System of Units (SI) via fundamental constants which came into force from May 2019. The CCQM pilot study was organized by Physikalisch-Technische Bundesanstalt (PTB). Aqueous silicon solutions were shipped to all participating institutions. The data analysis as well as the uncertainty modelling and calculation of the results was predefined. The participants were provided with an uncertainty budget as a GUM Workbench® file as well as a free software license for the duration of the comparison. The agreement of the values of the molar mass (M(Si) = 27.976 942 577 g mol−1) was excellent with ten out of 11 results reported within the range of relative uncertainty of 1 × 10−8 required for the revision of the SI. KW - Absolute isotope ratio KW - Molar mass KW - Avogadro constant KW - Revision of the SI PY - 2020 DO - https://doi.org/10.1088/1681-7575/abbdbf VL - 57 IS - 6 SP - 065028 PB - IOP Science CY - Cambridge AN - OPUS4-51500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pellegrino, F. A1 - Isopescu, R. A1 - Pellutiè, L. A1 - Sordello, F. A1 - Rossi, A. M. A1 - Ortel, Erik A1 - Martra, G. A1 - Hodoroaba, Vasile-Dan A1 - Maurino, V. T1 - Machine learning approach for elucidating and predicting the role of synthesis parameters on the shape and size of TiO2 nanoparticles N2 - In the present work a series of design rules are developed in order to tune the morphology of TiO2 nanoparticles through hydrothermal process. Through a careful experimental design, the influence of relevant process parameters on the synthesis outcome are studied, reaching to the develop predictive models by using Machine Learning methods. The models, after the validation and training, are able to predict with high accuracy the synthesis outcome in terms of nanoparticle size, polydispersity and aspect ratio. Furthermore, they are implemented by reverse engineering approach to do the inverse process, i.e. obtain the optimal synthesis parameters given a specific product characteristic. For the first time, it is presented a synthesis method that allows continuous and precise control of NPs morphology with the possibility to tune the aspect ratio over a large range from 1.4 (perfect truncated bipyramids) to 6 (elongated nanoparticles) and the length from 20 to 140 nm. KW - Machine learning KW - Nanoparticles KW - Titanium dioxide KW - Size KW - Shape KW - Synthesis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515084 DO - https://doi.org/10.1038/s41598-020-75967-w VL - 10 IS - 1 SP - 18910 PB - Springer Nature AN - OPUS4-51508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xue, Boyang A1 - You, Yi A1 - Gornushkin, Igor B. A1 - Zheng, R. A1 - Riedel, Jens T1 - High-throughput underwater elemental analysis by μJ-laser-induced breakdown spectroscopy at kHz repetition rates: part I, ultrasound-enhanced optical emission spectroscopy towards application perspectives N2 - In recent years, laser-induced breakdown spectroscopy (LIBS) has gained significant attention as a means for simple elemental analyses. The suitability of LIBS for contactless analysis allows it to be a perfect candidate for underwater applications. While the majority of LIBS systems still rely upon sub-kHz pulsed lasers, this contribution introduces 10s-kHz low pulse-energy lasers into underwater LIBS to improve the throughput and statistical validity. Interestingly, the spectral component significantly changed above a critical laser repetition-rate threshold. Spectral lines of atomic hydrogen and oxygen stemming from water become visible beyond a ∼10 kHz repetition rate. This observation suggests a different plasma dynamic compared to low repetition rates. When the pulse-to-pulse interval becomes sufficiently short, a cumulative effect begins to be significant. Apparently, the new phenomena occur on a timescale corresponding to a threshold rate of ∼10 kHz, i.e. ∼100 μs. Analytically, the high repetition rates result in improved statistical validity and throughput. More plasma events per unit time allowed the use of low efficiency Echelle spectrometers without compromising on the analytical performance. Meanwhile, the presence of H I and O I out of the water (as the matrix) also offers internal standardization in underwater elemental analysis. Since the laser fluence was on the lower edge of the plasma threshold, an additional ultrasound source was introduced to induce external perturbation, which significantly improved the plasma formation stability. A huge advantage of LIBS is the possibility of detecting almost all elements within a sample simultaneously. Throughout the periodic table, chlorine is one of the most challenging elements. Consequently, Ca2+ and Na+ were used as samples to demonstrate the capability of this high repetition-rate LIBS platform. As an ambitious benchmark for our system, chlorine detection in water was also discussed. KW - High repetition rate KW - Laser-induced breakdown spectroscopy PY - 2020 DO - https://doi.org/10.1039/D0JA00290A VL - 35 IS - 12 SP - 2901 EP - 2911 PB - The Royal Society of Chemistry AN - OPUS4-51564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xue, Boyang A1 - You, Yi A1 - Riedel, Jens T1 - High-throughput underwater elemental analysis by μJ-laser-induced breakdown spectroscopy at a kHz repetition rate: part II, understanding the high repetition-rate from a fundamental perspective N2 - The technological advances in lasers enabled the wide application of laser-induced breakdown spectroscopy (LIBS) as a powerful analytical means for elemental analyses. Rather than commonly used lasers that operate at several to several-tens of Hz, the high repetition rate ones that operate at tens of kHz showed superior analytical advantages while implying unique excitation pathways. Specifically, the production of excited atomic hydrogen and oxygen, which can serve as internal standards, is quite different from that in commonly reported double-pulse LIBS. In this part of the work, it was found that the atomic emitters stemming from water are not related to cavitation bubbles. Moreover, the emitter productions of dissolved species, e.g., Na+, and water-related species, e.g., H-α, are two distinctive mechanisms. Towards analytical applications of the high repetition-rate system, the fundamental investigation can provide important guidelines to address real-life challenges. In this part of the work, the high repetition-rate regime of operation is explored from a more kinetic perspective. KW - High repetition rate KW - Laser-induced breakdown spectroscopy PY - 2020 DO - https://doi.org/10.1039/D0JA00291G VL - 35 IS - 12 SP - 2912 EP - 2919 PB - Royal Society of Chemistry AN - OPUS4-51565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Roesch, Philipp A1 - Fischer, E. A1 - von der Au, Marcus A1 - Pfeifer, Jens A1 - Cossmer, Antje A1 - Wittwer, Philipp A1 - Vogel, Christian A1 - Simon, Franz-Georg A1 - Meermann, Björn T1 - Determination of organically bound fluorine sum parameters in river water samples - Comparison of combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) N2 - In this study, we compare combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) with respect to their applicability for determining organically Bound fluorine sum parameters. Extractable (EOF) and adsorbable (AOF) organically bound fluorine as well as total fluorine (TF) were measured in samples fromriver Spree in Berlin, Germany, to reveal the advantages and disadvantages of the two techniques used as well as the two established fluorine sum Parameters AOF and EOF. TF concentrations determined via HR-CS-GFMAS and CIC were comparable between 148 and 270 μg/L. On average, AOF concentrations were higher than EOF concentrations, with AOF making up 0.14–0.81% of TF (determined using CIC) and EOF 0.04–0.28% of TF (determined using HR-CSGFMAS). The results obtained by the two independent methods were in good agreement. It turned out that HR-CS-GFMAS is a more sensitive and precise method for fluorine analysis compared to CIC. EOF and AOF are comparable tools in Risk evaluation for the emerging pollutants per- and polyfluorinated alkyl substances; however, EOF is much faster to conduct. KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Combustion ion chromatography (CIC) KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Adsorbable organically bound fluorine (AOF) KW - Extractable organically bound fluorine (EOF) KW - Surface waters PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515351 DO - https://doi.org/10.1007/s00216-020-03010-y SN - 1618-2650 VL - 413 IS - 28 SP - 103 EP - 115 PB - Springer CY - Berlin AN - OPUS4-51535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Microstructure characterization of oligomers by analysis of UPLC / ESI-TOF-MS reconstructed ion chromatograms N2 - It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. Small, often isobaric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector. Nowadays a wide range of different analytical separation techniques and multi-detection possibilities are available. The challenge consists in a clever combination of these techniques with a specific approach of data analysis. In this presentation different liquid chromatographic separation modes were combined with Electrospray Time-of-Flight mass spectrometry. The online coupling allows the analysis of reconstructed ion chromatograms (RIC) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities in microstructure or topology, that are otherwise inaccessible This method is suitable to detect small differences in e. g. branching, topology, monomer sequence or tacticity and could potentially be used in production control of oligomeric products or other routinely done analyses to quickly indicate deviations from set parameters. Based on a variety of examples e.g. the topology elucidation of branched EO-PO copolymers, the possibilities and limitations of this approach were demonstrated. T2 - Analyticon 2020 CY - Online meeting DA - 05.11.2020 KW - Microstructure KW - Copolymer KW - LC-MS PY - 2020 AN - OPUS4-51540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Hampel, S. A1 - Fittschen, U.E.A. A1 - Streli, C. A1 - Radtke, Martin T1 - Comparison of three reconstruction methods based on deconvolution, iterative algorithm and neural network for X-ray fluorescence imaging with coded apertures N2 - X-ray imaging methods are used in many fields of research, as they allow a non-destructive Investigation of the elemental content of various samples. As for every imaging method, for X-ray imaging the optics are of crucial importance. However, these optics can be very expensive and laborious to build, as the requirements on surface roughness and precision are extremely high. Angles of reflection and refraction are often in the range of a few mrad, making a compact design hard to achieve. In this work we present a possibility to simplify X-ray imaging. We have adapted the coded aperture method, a high energy radiation imaging method that has its origins in astrophysics, to full field X-ray fluorescence imaging. In coded aperture imaging, an object is projected through a known mask, the coded aperture, onto an area sensitive detector. The resulting image consists of overlapping projections of the object and a reconstruction step is necessary to obtain the information from the recorded image. We recorded fluorescence images of different samples with an energy-dispersive 2D detector (pnCCD) and investigated different reconstruction methods. With a small coded aperture with 12 holes we could significantly increase the count rate compared to measurements with a straight polycapillary optic. We show that the reconstruction of two different samples is possible with a deconvolution approach, an iterative algorithm and a neural network. These results demonstrate that X-ray fluorescence imaging with coded apertures has the potential to deliver good results without scanning and with an improved count rate, so that measurement times can be shortened compared to established methods. KW - X-ray fluorescence imaging KW - Coded apertures KW - Imaging KW - Elemental mapping KW - Image reconstruction PY - 2020 DO - https://doi.org/10.1039/d0ja00146e VL - 35 IS - 7 SP - 1423 EP - 1434 PB - Royal Society of Chemistry CY - United Kingdom AN - OPUS4-51518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mirtsch, Mona A1 - Kinne, J. A1 - Blind, K. T1 - Exploring the Adoption of the International Information Security Management System Standard ISO/IEC 27001: A Web Mining-Based Analysis N2 - In the light of digitalization and recent EU policy initiatives, information is an important asset that organizations of all sizes and from all sectors should secure. However, in order to provide common requirements for the implementation of an information security management system, the internationally well-accepted ISO/IEC 27001 standard has not shown the expected growth rate since its publication more than a decade ago.In this article, we apply web mining to explore the adoption of ISO/IEC 27001 through a series of 2664 out of more than 900 000 German firms from the Mannheim Enterprise Panel dataset that refers to this standard on their websites. As a result, we present a “landscape” of ISO/IEC 27001 in Germany, which shows that firms not only seek certifications themselves but often refer on their websites to partners who are certified instead. Consequently, we estimate a probit model and find that larger and more innovative firms are more likely to be certified to ISO/IEC 27001 and that almost half of all certified firms belong to the information and communications technology (ICT) service sector. Based on our findings, we derive implications for policymakers and management and critically assess the suitability of web mining to explore the adoption of management system standards. KW - Adoption KW - Information security KW - Management system standards KW - Standards KW - Web mining PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513284 DO - https://doi.org/10.1109/TEM.2020.2977815 VL - 68 IS - 1 SP - 87 EP - 100 AN - OPUS4-51328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Van den Bossche, T. A1 - Verschaffelt, P. A1 - Schallert, K. A1 - Barsnes, H. A1 - Dawyndt, P. A1 - Benndorf, D. A1 - Renard, B. Y. A1 - Mesuere, B. A1 - Martens, L. A1 - Muth, Thilo T1 - Connecting MetaProteomeAnalyzer and PeptideShaker to Unipept for Seamless End-to-End Metaproteomics Data Analysis N2 - Although metaproteomics, the study of the collective proteome of microbial communities, has become increasingly powerful and popular over the past few years, the field has lagged behind on the availability of user-friendly, end-to-end pipelines for data analysis. We therefore describe the Connection from two commonly used metaproteomics data processing tools in the field, MetaProteomeAnalyzer and PeptideShaker, to Unipept for downstream analysis. Through these connections, direct end-to-end pipelines are built from database searching to taxonomic and functional annotation. KW - Metaproteomics KW - Bioinformatics KW - Software KW - Pipelines PY - 2020 DO - https://doi.org/10.1021/acs.jproteome.0c00136 VL - 19 IS - 8 SP - 3562 EP - 3566 PB - ACS Publications AN - OPUS4-51331 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schiebenhoefer, H. A1 - Schallert, K. A1 - Renard, B. Y. A1 - Trappe, K. A1 - Schmid, E. A1 - Benndorf, D. A1 - Riedel, K. A1 - Muth, Thilo A1 - Fuchs, S. T1 - A complete and flexible workflow for metaproteomics data analysis based on MetaProteomeAnalyzer and Prophane N2 - Metaproteomics, the study of the collective protein composition of multi-organism systems, provides deep insights into the biodiversity of microbial communities and the complex functional interplay between microbes and their hosts or environment. Thus, metaproteomics has become an indispensable tool in various fields such as microbiology and related medical applications. The computational challenges in the analysis of corresponding datasets differ from those of pure-culture proteomics, e.g., due to the higher complexity of the samples and the larger reference databases demanding specific computing pipelines. Corresponding data analyses usually consist of numerous manual steps that must be closely synchronized. With MetaProteomeAnalyzer and Prophane, we have established two open-source software solutions specifically developed and optimized for metaproteomics. Among other features, peptide-spectrum matching is improved by combining different search engines and, compared to similar tools, metaproteome annotation benefits from the most comprehensive set of available databases (such as NCBI, UniProt, EggNOG, PFAM, and CAZy). The workflow described in this protocol combines both tools and leads the user through the entire data analysis process, including protein database creation, database search, protein grouping and annotation, and results visualization. To the best of our knowledge, this protocol presents the most comprehensive, detailed and flexible guide to metaproteomics data analysis to date. While beginners are provided with robust, easy-to-use, state-of-the-art data analysis in a reasonable time (a few hours, depending on, among other factors, the protein database size and the number of identified peptides and inferred proteins), advanced users benefit from the flexibility and adaptability of the workflow. KW - Bioinformatics KW - Protocol KW - Microbial proteomics KW - Software KW - Mass spectrometry KW - Metaproteomics PY - 2020 DO - https://doi.org/10.1038/s41596-020-0368-7 SN - 1750-2799 VL - 15 IS - 10 SP - 3212 EP - 3239 PB - Nature Publishing Group AN - OPUS4-51335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bäßler, Ralph T1 - Rezension: Analytik - Daten, Formeln, Übungsaufgaben N2 - Seit seiner erstmaligen Veröffentlichung im Jahre 1894 als „Logarithmische Rechentafeln für Chemiker“ und ab 1982 als „Rechentafeln für die chemische Analyse“ begleitet der „Küster‐Thiel“ Generationen nicht nur von Laborantinnen und Laboranten sowie Studierende hilfreich bei der analytischen Arbeit. Mit der 108. Auflage änderte sich 2016 der Titel dieses in der „Studium“‐Reihe des De Gruyter Verlages herausgegebenen Standardwerkes ein weiteres Mal. Die 109. Auflage des Klassikers der chemischen Analytik‐Literatur setzt die Tradition fort, mit zahlreichen anschaulichen Erklärungen, Beispiele und Rechnungen Chemikern, Physikern und Ingenieurswissenschaftlern an Universitäten und Fachhochschulen; Auszubildenden und Laboranten ein übersichtliches und aktuelles Arbeitsmittel für den analytischen Alltag zur Verfügung zu stellen. Nutzern früherer Ausgaben wird der Umstieg auf die neue Ausgabe empfohlen, damit auch sie auf dem neuesten Stand arbeiten können. KW - Analyse KW - Labor KW - Formeln KW - Laborarbeit PY - 2020 DO - https://doi.org/10.1002/maco.202070106 SN - 1521-4176 SN - 0947-5117 VL - 71 IS - 10 SP - 2 EP - 3 PB - WILEY‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-51415 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya A1 - Tavernaro, Isabella T1 - Synthesis and Optical Quantification of Surface Groups on Organic and Inorganic Particle-Carriers N2 - Differently sized organic and inorganic particles are of great interest in the life and material sciences, as they can be used e.g. as drug carriers, fluorescent sensors, and multimodal labels in bioanalytical assays and imaging applications.1 Particle performance in such applications depends mainly on the sum of their intrinsic physicochemical properties. Here, the surface chemistry, i.e., the total number of surface functional groups (FG) and the number of FG accessible for subsequent modification with ligands and/or biomolecules, is one of the key parameters. Moreover, the surface chemistry of these materials controls the behavior and fate of the particles when released to the environment or taken up by cells. Nevertheless, it is still relatively rare that FG are quantified in particle safety studies. Methods for FG quantification should be simple, robust, reliable, fast, and inexpensive, and allow for the characterization of a broad variety of materials differing in size, chemical composition, and optical properties. Aiming at the development of simple, versatile, and multimodal tools for the quantification of bioanalytically relevant FG such as amine2,3, carboxy2,3, thiol, and aldehyde4 functionalities, we designed a catch-and-release assay utilizing cleavable probes that enable the quantification of the cleaved-off reporters in the supernatant after particle separation, and thus, circumvent interferences resulting from particle light scattering and sample-inherent absorption or emission.2 The potential of our cleavable probes for the quantification of carboxy and amino groups was demonstrated for commercial and custom-made polymer and silica particles of varying FG densities, underlining the benefit of the catch-and-release assays as a versatile method for the FG quantification on all types of transparent, scattering, absorbing and/or fluorescent particles.2,3 In the future, our cleavable probe strategy can be easily adapted to other analytical techniques requiring different reporters, or to different types of linkers that can be cleaved thermally, photochemically, or by pH, utilizing well-established chemistry, e.g. from drug delivery systems. It can contribute to establish multi-method characterization strategies for particles to provide a more detailed picture of the structure-properties relationship and thus can support the design of sustainable and safe(r) materials. T2 - Nanosafety 2020 CY - Online meeting DA - 05.10.2020 KW - Optical quantification KW - Surface functional groups KW - Polymer particles KW - Silica particles KW - Cleavable probe PY - 2020 AN - OPUS4-51418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gaft, M. A1 - Nagli, L. A1 - Gornushkin, Igor B. A1 - Raichlin, Y. T1 - Review on recent advances in analytical applications of molecular emission and modelling N2 - The review mainly deals with two topics that became important in applications of laser-induced breakdown spectroscopy (LIBS) in recent years: the emission of halogen- and rare-earth-containing molecules and selective excitation of molecules by molecular laser-induced fluorescence (MLIF). The first topic is related to the emission of alkaline-earth diatomic halides MX, M = Ca, Mg, Ba, Sr and X = F, Cl, Br, and I and rare-earth element (REE) oxides LaO, YO, and ScO. These molecules form in laser-induced plasma (LIP) soon after its ignition and persist for a long time, emitting broad bands in a visible part of the spectrum. They are best detected after relatively long delay times when emission from interfering plasma species (atoms and ions) has already been quenched. Such behavior of molecular spectra allows of using, for their detection, inexpensive CCD detectors equipped with simple electronic or mechanical shutters and low-resolution spectrometers. A main target for analysis by molecular spectroscopy is halogens; these elements are difficult to detect by atomic spectroscopy because their most intense atomic lines lie in the vacuum UV. Therefore, in many situations, emission from CaF and CaCl may provide a substantially more sensitive detection of F and Cl than emission from elemental F and Cl and their ions. This proved to be important in mining and concrete industries and even Mars exploration. A similar situation is observed for REEs; their detection by atomic spectroscopy sometimes fails even despite the abundance of atomic and ionic REEs' lines in the UV-VIS. For example, in minerals and rocks with low concentrations of REEs, emission from major and minor mineral elements hinders the weak emission from REEs. Many REEs do not form molecules that show strong emission bands in LIP but can still be detected with the aid of LIP. All REEs except La, Y, and Sc exhibit long-lived luminescence in solid matrices that is easily excited by LIP. The luminescence can be detected simultaneously with molecular emission of species in LIP within the same time and spectral window. The second topic is related to the combination of MLIF and LIBS, which is a technique that was proved to be efficient for analysis of isotopic molecules in LIP. For example, the characteristic spectral signals from isotopic molecules containing 10B and 11B are easier to detect with MLIF-LIBS than with laser ablation molecular isotopic spectrometry (LAMIS) because MLIF provides strong resonance excitation of only targeted isotopes. The technique is also very efficient in detection of halogen molecules although it requires an additional tunable laser that makes the experimental setup bulky and more expensive. KW - Plasma induced luminescence KW - Molecular emission KW - Laser induced plasma KW - Plasma modeling KW - Molecular analysis KW - LIBS PY - 2020 DO - https://doi.org/10.1016/j.sab.2020.105989 VL - 173 SP - 105989 PB - Elsevier B. V. AN - OPUS4-51420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan T1 - Gold nanocubes with monodispersed size distribution (SEM SE) N2 - Gold nanocubes with a monodispersed size distribution (edge = 55 nm) deposited on a silicon wafer. These tiny uniform cubes were produced as reference nanoparticles in the frame of the European project nPSize - Improved traceability chain of nanoparticle size measurements. SEM Image acquired at 10 kV with an in-lens secondary electron detector. Image colored in ImageJ using LUT “Orange hot.” Published in Microscopy and Microanalysis 25(S2) (2019) 2328. KW - Nanoparticles KW - Nanocubes KW - Electron microscopy KW - Reference materials PY - 2020 DO - https://doi.org/10.1017/S1551929520001157 VL - 28 IS - 4 SP - 12 EP - 12 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weber, A. A1 - von Randow, M. A1 - Voigt, A.-L. A1 - von der Au, Marcus A1 - Fischer, E. A1 - Meermann, Björn A1 - Wagner, M. T1 - Ingestion and toxicity of microplastics in the freshwater gastropodLymnaea stagnalis: No microplastic-induced effects alone or incombination with copper N2 - The interaction of microplastics with freshwater biota and their interaction with other stressors is still not very well understood. Therefore, we investigated the ingestion, excretion and toxicity of microplastics in the freshwater gastropod Lymnaea stagnalis. MP ingestion was analyzed as tissues levels in L. stagnalis after 6–96 h of exposure to 5–90 μm spherical polystyrene (PS) microplastics. To understand the excretion, tissue levels were determined after 24 h of exposure followed by a 12 h–7 d depuration period. To assess the toxicity, snails were exposed for 28 d to irregular PS microplastics (<63 μm, 6.4–100,000 particles mL−1), both alone and in combination with copper as additional stressor. To compare the toxicity of natural and synthetic particles, we also included diatomite particles. Microplastics ingestion and excretion significantly depended on the particle size and the exposure/depuration duration. An exposure to irregular PS had no effect on survival, reproduction, energy reserves and oxidative stress. However, we observed slight effects on immune cell phagocytosis. Exposure to microplastics did not exacerbate the reproductive toxicity of copper. In addition, there was no pronounced difference between the effects of microplastics and diatomite. The tolerance towards microplastics may originate from an adaptation of L. stagnalis to particle-rich environments or a general stress resilience. In conclusion, despite high uptake rates, PS fragments do not appear to be a relevant stressor for stress tolerant freshwater gastropods considering current environmental levels of microplastics. KW - Lymnaea stagnalis KW - Microplastic-induced effects KW - Mixture toxicity PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513551 DO - https://doi.org/10.1016/j.chemosphere.2020.128040 VL - 263 SP - 128040 PB - Elsevier Ltd. AN - OPUS4-51355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan T1 - 2020 Microscopy Today Micrograph Awards N2 - Gold nanocubes with a monodispersed size distribution (edge = 55 nm) deposited on a silicon wafer. These tiny uniform cubes were produced as reference nanoparticles within the EMPIR project nPSize - Improved traceability chain of nanoparticle size measurements. SEM image acquired at 10 kV with an in-lens secondary electron detector. Image colored in ImageJ using LUT “Orange hot.” Published in Microscopy and Microanalysis 25(S2) (2019) 2328. KW - Nanoparticles KW - Au-nanocubes KW - Reference materials KW - Electron microscopy PY - 2020 DO - https://doi.org/10.1017/S1551929520001339 VL - 28 IS - 5 SP - 14 EP - 15 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Faßbender, Sebastian T1 - On-line Species-specific Isotopic Analysis of Sulfur by Hyphenation of Capillary Electrophoresis with Multicollector-ICP-MS N2 - In many scientific fields, isotopic analysis can offer valuable information. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement. Whereas some works hyphenating GC and IC with MC-ICP-MS have already been reported, LC and CE hyphenations are still inadequately represented based on the capabilities of these separation techniques. In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species using a multiple-injection approach for instrumental mass bias correction by standard-sample bracketing. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared to data from off-line analysis of the same samples for validation. The repeatability of the results of the on-line measurements was promising regarding the differentiation of the river systems by the isotopic signature of river water sulfate. The great potential of this method is based on the versatility of the applied separation technique, not only in the environmental field but also for, e.g., biomolecules because sulfur is the only covalently bound constituent of proteins that can be analyzed by MC-ICP-MS. T2 - SciX 2020 CY - Online meeting DA - 12.10.2020 KW - Capillary electrophoresis KW - Hyphenated techniques KW - Isotopic analysis KW - Speciation analysis PY - 2020 AN - OPUS4-51402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine T1 - Determination of readiness for laying based on material moisture, corresponding relative humidity, and water release N2 - The moisture content of the subfloor has to be determined before installation to avoid damages of the floor covering. Only if the readiness for layering is reached, an installation without damages can be expected in all cases. In general, three different approaches exist to measure the residual water content: determination of the moisture content, determination of the water release, or determination of the corresponding relative humidity. All three approaches are tested in laboratory at eight different screed types including two different samples thicknesses in each case. The moisture content and the water release are measured by sample weighing, the corresponding relative humidity is measured by embedded sensors. All three approaches are compared and correlated to each other. The evaluations show only weak correlation and, in several cases, contradicting results. Samples are considered as being ready for layering and not-being ready for layering at the same time, depending on the chosen approach. Due to these contradicting results, a general threshold for the risk of damage cannot be derived based on these measurements. Furthermore, the experiment demonstrates that the measurement of corresponding relative humidity is independent of the considered screed type or screed composition. This makes the humidity measurement to very promising approach for the installation of material moisture monitoring systems in the future. KW - Material moisture KW - Readiness for laying KW - Screed KW - Corresponding relative humidity KW - Partially saturated pores PY - 2020 DO - https://doi.org/10.3139/120.111581 VL - 62 IS - 10 SP - 1033 EP - 1040 PB - Carl Hanser Verlag GmbH & Co. KG CY - München AN - OPUS4-51405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schade, U. A1 - Dawei, C. A1 - Puskar, L. A1 - Ritter, E. A1 - Beckmann, Jörg T1 - Removal of Etalon Features in the Far-Infrared–Terahertz Transmittance Spectra of Thin Polymer Films N2 - Etalon features in infrared spectra of stratified samples, their influence on the interpretation and methods to circumvent their presence in infrared spectra have been in discussion for decades. This paper focuses on the application of a method originally developed to remove interference fringes in the mid-infrared spectra for far-infrared Fourier transform spectroscopy on thin polymer films. We show that the total transmittance-reflectance technique, commonly used for mid-infrared, also works successfully in the far infrared spectral range where other approaches fail. Experimental spectra obtained by such technique are supported by model calculations and reveal the possibility and limits to obtain almost undisturbed far-infrared spectra which are suitable to determine low energy vibrations of ionomer salts under certain sample conditions. KW - Far-infrared spectroscopy KW - Absorption KW - Etalon feature KW - Total transmittance reflectance PY - 2020 DO - https://doi.org/10.1177/0003702820922295 VL - 74 IS - 12 SP - 1530 EP - 1539 PB - Sage journals AN - OPUS4-51367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baumann, Maria A1 - Falkenhagen, Jana A1 - Weidner, Steffen A1 - Wold, C. A1 - Uliyanchenko, E. T1 - Characterization of copolymers of polycarbonate and polydimethylsiloxane by 2D chromatographic separation, MALDI-TOF mass spectrometry, and FTIR spectroscopy N2 - The structure and composition of polycarbonate polydimethylsiloxane copolymer (PC-co-PDMS) was investigated by applying various analytical approaches including chromatographic separation methods, spectrometric, and spectroscopic detection techniques. In particular, size exclusion chromatography (SEC) and liquid adsorption chromatography operating at different conditions (e.g. using gradient solvent systems) were used to achieve separations according to molar mass and functionality distribution. The coupling of both techniques resulted in fingerprint two-dimensional plots, which could be used to easily compare different copolymer batches. Matrix-assisted laser desorption/ionization-time-of-flight (MALDI-TOF) mass spectrometry was applied for structural investigations. The different ionization behavior of both comonomers, however, strongly limited the applicability of this technique. In contrast to that, Fourier-transform Infrared (FTIR) spectroscopy could be used to quantify the amount of PDMS in the copolymer at different points in the chromatogram. The resulting methodology was capable of distinguishing PC-co-PDMS copolymer from PC homopolymer chains present in the material. KW - FTIR KW - Liquid chromatography KW - Mass spectrometry KW - Gradient elution KW - Polycarbonate-co-dimethylsiloxane copolymer PY - 2020 DO - https://doi.org/10.1080/1023666X.2020.1820170 VL - 25 IS - 7 SP - 1 EP - 12 PB - Taylor & Francis AN - OPUS4-51369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jenning, M. A1 - Marklein, B. A1 - Ytterberg, J. A1 - Zubarev, R. A. A1 - Joshua, V. A1 - van Schaardenburg, D. A1 - van de Stadt, L. A1 - Catrina, A. I. A1 - Nonhoff, U. A1 - Häupl, T. A1 - Konthur, Zoltán A1 - Burmester, G. R. A1 - Skriner, K. T1 - Bacterial citrullinated epitopes generated by Porphyromonas gingivalis infection—a missing link for ACPA production N2 - Objectives: Porphyromonas gingivalis (P.g.) is discussed to be involved in triggering self-reactive immune responses. The aim of this study was to investigate the autocitrullinated prokaryotic peptidylarginine deiminase (PPAD) from P.g. CH2007 (RACH2007-PPAD) from a rheumatoid arthritis (RA) patient and a synthetic citrullinated PPAD peptide (CPP) containing the main autocitrullination site as potential targets for antibody reactivity in RA and to analyse the possibility of citrullinating native human proteins by PPAD in the context of RA. Methods: Recombinant RACH2007-PPAD was cloned and expressed in Escherichia coli. Purified RACH2007-PPAD and its enzymatic activity was analysed using two-dimensional electrophoresis, mass spectrometry, immunoblot and ELISA. Autoantibody response to different modified proteins and peptides was recorded and bioinformatically evaluated. Results: RACH2007-PPAD was capable to citrullinate major RA autoantigens, such as fibrinogen, vimentin, hnRNP-A2/B1, histone H1 and multiple peptides, which identify a common RG/RGG consensus motif. 33% of RA patients (n=30) revealed increased reactivity for α-cit-RACH2007-PPAD before RA onset. 77% of RA patients (n=99) presented α-cit-specific signals to CPP amino acids 57-71 which were positively correlated to α-CCP2 antibody levels. Interestingly, 48% of the α-CPP-positives were rheumatoidfactor IgM/anti-citrullinated peptide/protein antibodies (ACPA)-negative. Anti-CPP and α-RACH2007-PPAD antibody levels increase with age. Protein macroarrays that were citrullinated by RACH2007-PPAD and screened with RA patient sera (n=6) and controls (n=4) uncovered 16 RACH2007-PPAD citrullinated RA autoantigens and 9 autoantigens associated with lung diseases. We showed that the α-CPP response could be an important determinant in parenchymal changes in the lung at the time of RA diagnosis (n=106; p=0.018). Conclusions: RACH2007-PPAD induced internal citrullination of major RA autoantigens. Anti-RACH2007-PPAD correlates with ACPA levels and interstitial lung disease autoantigen reactivity, supporting an infection-based concept for induction of ACPAs via enzymatic mimicry. KW - Zitrullin KW - Rheumatoide Arthritis KW - Proteinmodifikation KW - Autoantikörper PY - 2020 DO - https://doi.org/10.1136/annrheumdis-2019-216919 VL - 79 IS - 9 SP - 1194 EP - 1202 PB - BMJ Publishing Group Ltd AN - OPUS4-51372 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yildirim, Arda A1 - Kolmangadi, Mohamed Aejaz A1 - Bühlmeyer, A. A1 - Huber, P. A1 - Laschat, S. A1 - Schönhals, Andreas T1 - Electrical conductivity and multiple glassy dynamics of crow-ether based columnar liquid crystals N2 - The phase behavior of two unsymmetrical triphenylene crown ether-based columnar liquid crystals (CLCs) bearing different lengths of alkyl chains, KAL465 and KAL468, was investigated using differential scanning calorimetry (DSC). A plastic crystalline (Cry), columnar liquid crystalline (Colh) and an isotropic phase were observed along with two glass transitions in the Cry phase. The molecular mobility of the KAL compounds was further studied by a combination of broadband dielectric spectroscopy (BDS) and advanced calorimetric techniques. By the BDS investigations, three dielectric active relaxation processes were observed for both samples. At low temperatures, a γ-process in the Cry state was detected and is assigned to the localized fluctuations taking place in the alkyl chains. An α2-process takes place at higher temperatures in the Cry phase. An α3 process was found in the Colh mesophase. The advanced calorimetric techniques consist of fast scanning calorimetry (FSC) and specific heat spectroscopy (SHS) employing temperature modulated DSC and FSC (TMDSC and TMFSC). The advanced calorimetric investigations revealed that besides the α2 process in agreement with BDS, a second dynamic glass transition (α1-process) is present which is not observed by dielectric spectroscopy. The results are in good agreement with the glass transitions detected by DSC for this process. The temperature dependences of the relaxation rates of the α1 , α2 and α3 processes are all different. Therefore, different molecular assignments for the relaxation processes are proposed. In addition to the relaxation processes, a conductivity contribution was explored by BDS for both KAL compounds. The conductivity contribution appears in both Cry and Colh phases, where the conductivity increases by ca. one order of magnitude at phase transition from the crystalline to the hexagonal phase. KW - Columnar Liquid Crystal PY - 2020 DO - https://doi.org/10.1021/acs.jpcb.0c06854 VL - 124 IS - 39 SP - 8728 EP - 8739 PB - ACS AN - OPUS4-51374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - An ELISA-inspired electrochemical detection system for the quantification of ochratoxin A N2 - Toxic secondary metabolites produced by fungi (aka mycotoxins) are often identified as contaminants in cereals or other food and pose a severe health risk, since they can be carcinogenic, neurotoxic, mutagenic or harmful in other respect. The highly nephrotoxic ochratoxin A (OTA) is one of the most important and widespread mycotoxins found in grains such as rye, wheat or oats. Thus, the fast and cost-effective detection of OTA is of great importance, to ensure that the toxin concentration is below the legal limits. Currently, the mycotoxin detection in mill operations is typically performed by means of the antibody-based ELISA method, which requires extensive laboratory equipment and specialized personnel. It was the aim of this study to develop an ELISA-inspired sensor method enabling the on-site quantification of OTA. Based on a classical competitive ELISA, an electrochemical detection system was developed. Anti-OTA-antibodies were captured on magnetic beads on which the competitive affinity reaction between OTA and an OTA- horseradish peroxidase (HRP) tracer was performed. Here the OTA concentration is inversely proportional to the amount of the bound OTA-HRP tracer, which was electrochemically quantified. For this purpose, oxidized tetramethylbenzidine (TMB), which is enzymatically produced by the reduction of H2O2 by the OTA-HRP tracer, is quantified by amperometry with screen-printed electrodes in a flow system. With this method a detection limit of 250 ng L-1 could be achieved which meets the current requirements for the detection of OTA in food and feed. T2 - Interdisziplinäres Doktorandenseminar des AK Prozessanalytik CY - Online meeting DA - 21.09.2020 KW - Ochratoxin A KW - Cyclic voltammetry KW - Amperometry KW - ELISA KW - Magnetic beads PY - 2020 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-51375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona A1 - Koch, Claudia T1 - Nutzung und Wirkung von (zertifizierten) Managementsystemen – aktuelle Erkenntnisse N2 - Ergebnisvorstellung im mitgliederexklusiven Webinar der Deutschen Gesellschaft für Qualität - DGQ zur Nutzung und Wirkung von genormten Managementsystemen als die erste Erhebung im Rahmen von QI-FoKuS. Neben der Motivation hinsichtlich der Anwendung verschiedener Normen, die Anforderungen an Managementsysteme darlegen, sowie den Wirkungen werden insbesondere die Zertifizierung für diese Normen sowie daran anknüpfend die Rolle und Funktion der Akkreditierung – und somit verschiedene Bausteine der QI – adressiert. T2 - Mitgliederexklusives Webinar CY - Online meeting DA - 15.10.2020 KW - Management Systeme KW - QI-FoKuS KW - ISO 9001 KW - ISO/IEC 27001 KW - Zertifizierung KW - Kundenaudit KW - Konformitätsbewertung KW - Akkreditierung PY - 2020 AN - OPUS4-51431 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Usmani, Shirin M. A1 - Plarre, Rüdiger A1 - Hübert, Thomas A1 - Kemnitz, E. ED - Richter, K. ED - Van de Kulien, J.-W. T1 - Termite resistance of pine wood treated with nano metal fluorides N2 - Fluorides are well-known as wood preservatives. One of the limitations of fluoride-based wood preservatives is their high leachability. Alternative to current fluoride salts such as NaF used in wood protection are low water-soluble fluorides. However, impregnation of low water-soluble fluorides into wood poses a challenge. To address this challenge, low water-soluble fluorides like calcium fluoride (CaF2) and magnesium fluoride (MgF2) were synthesized as nanoparticles via the fluorolytic sol−gel synthesis and then impregnated into wood specimens. In this study, the toxicity of nano metal fluorides was assessed by termite mortality, mass loss and visual analysis of treated specimens after eight weeks of exposure to termites, Coptotermes formosanus. Nano metal fluorides with sol concentrations of 0.5 M and higher were found to be effective against termites resulting in 100% termite mortality and significantly inhibited termite feeding. Among the formulations tested, the least damage was found for specimens treated with combinations of CaF2 and MgF2 with an average mass loss less than 1% and visual rating of “1”. These results demonstrate the efficacy of low water-soluble nano metal fluorides to protect wood from termite attack. KW - Holzschutzmittel KW - Nanoparticles KW - Fluorides KW - Termites PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514325 DO - https://doi.org/10.1007/s00107-020-01522-z VL - 78 SP - 493 EP - 499 PB - Springer CY - Berlin AN - OPUS4-51432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dittmann, Daniel T1 - Aktivkohlecharakterisierung von GAK-Filtern bei unterschiedlichen Laufzeiten N2 - Eine umfangreich ausgestaltete Trinkwasseraufbereitung als Multibarrieren-System ist notwendig, wenn das Rohwasser direkt aus Fließgewässern entnommen wird (z. B. für das Mülheimer Verfahren). Eine der Barrieren wird, als gezielte Behandlungs- oder Sicherheitsstufe, oft als Filter mit granulierter Aktivkohle (GAK-Filter) realisiert. Ihre Standzeit kann bei geringer Wasserbelastung (DOC < 2 mg/L), z. B. bei der Landeswasserversorgung Langenau, bis zu 5 Jahre betragen. Bei Rohwasser mit höherem Organikgehalt (DOC > 7 mg/L), wie bei der Nordwasser in Rostock, wird hingegen mindestens alle drei Jahre die GAK in den Filterkolonnen ausgetauscht. Die Rest-Adsorptionskapazität der GAK kann durch verschiedene Verfahren abgeschätzt werden, ist aber nach wie vor Gegenstand aktueller Forschung. Die weitergehende Charakterisierung der beladenen GAK kann hierbei helfen. Auf dem Poster sollen erste Ergebnisse zu den in Langenau und Rostock eingesetzten Aktivkohlen präsentiert werden. Hierzu wurden die frischen und nach unterschiedlichen Laufzeiten beladenen GAK untersucht. Die Zusammensetzung der Anorganik und der adsorbierten Organik, welche mittels Zersetzungs¬gasanalyse charakterisiert wurde, zeigt deutliche Unterschiede. Bspw. nimmt der Calcium-Gehalt der GAK in Langenau kontinuierlich zu, wohingegen dieser in den Proben aus Rostock mit zunehmender Laufzeit zurückgeht. Umgekehrt verhält es sich mit der Organik: Die GAK aus Rostock zeigen Hinweise auf biologische Besiedelung, während diese in Langenau trotz längerer Filterlaufzeit auszubleiben scheint. T2 - 4. Mülheimer Wasseranalytisches Seminar (MWAS2020) CY - Mülheim an der Ruhr, Germany DA - 16.09.2020 KW - Thermogravimetrie KW - Trinkwasser KW - Wasseraufbereitung KW - Aktivkohle PY - 2020 AN - OPUS4-51433 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittmann, Daniel A1 - Lucke, T. A1 - Ruhl, A. S. A1 - Winzenbacher, R. A1 - Jekel, M. A1 - Braun, Ulrike T1 - Untersuchungen zu biologischen, organischen und anorganischen Veränderungen granulierter Aktivkohlen während der Trinkwasseraufbereitung N2 - Untersuchungen zu biologischen, organischen und anorganischen Veränderungen granulierter Aktivkohlen während der Trinkwasseraufbereitung des Landeswasserversorgers Langenau. KW - Thermogravimetrie KW - Trinkwasser KW - Wasseraufbereitung KW - Aktivkohle PY - 2020 SN - 0083-6915 VL - 118 IS - 2 SP - 47 EP - 50 PB - Wiley-VCH Verlag GmbH & Co. KGaA AN - OPUS4-51434 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scherb, T. A1 - Fantin, Andrea A1 - Checcia, S. A1 - Stephan-Scherb, Christiane A1 - Escolástico, S. A1 - Franz, A. A1 - Seeger, J. A1 - Meulenberg, W. A. A1 - d'Acapito, F. A1 - Serra, J. M. T1 - Unravelling the crystal structure of Nd5.8WO12-d and Nd5.7W0.75Mo0.25O12-d mixed ionic electronic conductors N2 - Mixed ionic electronic conducting ceramics Nd6-yWO12-d (d is the Oxygen deficiency) provide excellent stability in harsh environments containing strongly reactive gases such as CO2, CO, H2, H2O or H2S. Due to this chemical stability, they are promising and cost-efficient candidate materials for gas separation, catalytic membrane reactors and protonic ceramic fuel cell technologies. As in La6-yWO12-d, the ionic/electronic transport mechanism in Nd6-yWO12-d is expected to be largely controlled by the crystal structure, the conclusive determination of which is still lacking. This work presents a crystallographic study of Nd5.8WO12-d and molybdenum-substituted Nd5.7W0.75Mo0.25O12-d prepared by the citrate complexation route. High-resolution synchrotron and neutron powder diffraction data were used in combined Rietveld refinements to unravel the crystal structure of Nd5.8WO12-d and Nd5.7W0.75Mo0.25O12-d. Both investigated samples crystallize in a defect fluorite crystal structure with space group Fm3m and doubled unit-cell parameter due to cation ordering. Mo replacesWat bothWyckoff sites 4a and 48h and is evenly distributed, in contrast with La6-yWO12-d. X-ray absorption spectroscopy as a function of partial pressure pO2 in the near-edge regions excludes oxidation state changes of Nd (Nd3+) and W(W6+) in reducing conditions: the enhanced hydrogen permeation, i.e. ambipolar conduction, observed in Mo-substituted Nd6-yWO12-d is therefore explained by the higher Mo reducibility and the creation of additional – disordered – oxygen vacancies. KW - Powder diffraction KW - Mixed conductors KW - X-ray absorption spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514607 DO - https://doi.org/10.1107/S1600576720012698 VL - 53 SP - 1471 EP - 1483 AN - OPUS4-51460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Stockmann, Jörg M. A1 - Senoner, Mathias A1 - Weimann, T. A1 - Bütefisch, S. A1 - Passiu, C. A1 - Spencer, N. D. A1 - Rossi, A. T1 - Introduction to lateral resolution and analysis area measurements in XPS N2 - Imaging and small-spot (small area) XPS have become increasingly important components of surface chemical analysis during the last three decades, and its use is growing. Some ambiguity in the use of terminology, understanding of concepts, and lack of appropriate reference materials leads to confusing and not always reproducible data. In this paper, it is shown that by using existing knowledge, appropriate test specimens, and standardized approaches, problems of comparability and such reproducibility issues recently observed for XPS data reported in the scientific literature can be overcome. The standardized methods of ISO 18516:2019, (i) the straight-edge, (ii) the narrow-line, and (iii) the grating method, can be used to characterize and compare the lateral resolution achieved by imaging XPS instruments and are described by reporting examples. The respective measurements are made using new test specimens. When running an XPS instrument in the small-spot (small area) mode for a quantitative analysis of a feature of interest, the question arises as to what contribution to the intensity originates from outside the analysis area. A valid measurement approach to control the intensity from outside the nominal analysis area is also described. As always, the relevant resolution depends on the specific question that needs to be addressed. The strengths and limitations of methods defining resolution are indicated. KW - Imaging XPS KW - Lateral resolution KW - Analysis area measurements KW - Small-spot XPS PY - 2020 DO - https://doi.org/10.1116/6.0000398 VL - 38 IS - 5 SP - 053206 AN - OPUS4-51394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gojani, Ardian A1 - Gornushkin, Igor B. T1 - Räumlich aufgelöste Heterodyne-Spektroskopie N2 - Die räumlich aufgelöste Heterodyn-Spektroskopie (SHS) kombiniert dispersive und interferometrische Techniken zur Gewinnung spektroskopischer Informationen und kann in einem anpassbaren Instrument realisiert werden. SHS wird für die chemische Analyse von verschiedenen Materialien mit Hilfe der Laser-induzierten Plasmaspektroskopie (LIBS) und der Raman-Spektroskopie eingesetzt. KW - Raman spectroscopy KW - Spatial heterodyne spectroscopy KW - Laser-induced breakdown spectroscopy PY - 2020 UR - https://analyticalscience.wiley.com/do/10.1002/was.00080118/full VL - 5 SP - 2 EP - 4 PB - Wiley CY - Weinheim AN - OPUS4-51397 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - Reply to the comment on “synthesis of cyclic polymers and flaws of the Jacobson-Stockmayer theory” by R. Szymanski N2 - In a recent publication the authors have presented theoretical and experimental results indicating that the Jacobson–Stockmayer (JS) theory does not provide a correct description of reversible polycondensations for all polymers and for high conversions (e.g. polycondensation in bulk). In this context reversibility means that all condensation step whether resulting in chain growth or in cyclization are reversible and thus, part of an equilibrium. The first two sections of that paper were focused on the demonstration that small, and above all, large cycles can be formed by end-to-end (ete) cyclization in reversible like in irreversible polycondensations. A significant contribution of ete-cyclization to the course of reversible polycondensations was denied by J + S apparently as a contribution to Florýs dogma, that the end groups of long polymer chains will never meet. KW - Polylactide KW - MALDI-TOF MS KW - Jacobsen-Stockmayer theory PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513985 DO - https://doi.org/10.1039/D0PY01118E VL - 11 IS - 38 SP - 6226 EP - 6228 PB - Royal Society of Chemistry AN - OPUS4-51398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. T1 - Mapping the Distribution of Air Pollutants with Mobile Robots and Stationary Sensors N2 - Precise knowledge about the distribution of air pollutants is necessary to develop plausible occupational health measures. Combinatory systems, consisting of mobile robots and stationary sensors, can be effective solutions for the coverage of large measurement areas. However, further research is needed to fully understand their performance in comparison to traditional sensing strategies. Therefore, multiple sensor networks layouts will be set up in a simulation environment as well as in real industrial environments. Models for distribution mapping will be developed and evaluated to investigate the performance and opportunities of hybrid-mobility sensor networks for the task of distribution mapping. T2 - AASS Seminar CY - Online meeting DA - 24.09.2020 KW - Mobile Robot Olfaction KW - Aerial Robot Olfaction KW - Wireless Sensor Network KW - Occupational Health PY - 2020 AN - OPUS4-51399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bröcker, S. A1 - Klaer, R.-H. A1 - Kockmann, N. A1 - Maiwald, Michael T1 - Process Industry United in the Digital World - The current landscape of research for the digitalization of the process industry N2 - The Tutzing Symposium "100 % digital: survival strategies for the process industry" (see 4.1) in April 2018 was characterized by a great momentum which has been taken up and continued until today. The aim was to implement the ideas from the Tutzing Symposium in a coordinated and targeted manner. For this purpose, development needs as well as the numerous currently planned or already started research and development activities in the context of digitalisation were first compiled and analysed. This resulted in the current research landscape for digitalization in the process industry. It now enables to identify open topics and to translate them into research funding programs as well as to define new projects in the dialogue between users, suppliers and research, which are to be meaningfully interlinked and consolidated with existing projects. Due to the strong interest in digitalisation, activities are constantly being added, so that this paper can only provide a snapshot of the situation in the period 2019-2020. KW - Process Industry KW - Digitalisation KW - Tutzing Symposion KW - research landscape KW - Process Control PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512265 UR - https://processnet.org/en/TAKdigital.html SP - 1 EP - 15 AN - OPUS4-51226 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhuckory, S. A1 - Wegner, Karl David A1 - Qiu, X. A1 - Wu, Y.T. A1 - Jennings, T. L. A1 - Incamps, A. A1 - Hildebrandt, N. T1 - Triplexed CEA-NSE-PSA Immunoassay Using Time-Gated Terbium-to-Quantum Dot FRET N2 - Time-gated Förster resonance energy transfer (TG-FRET) between Tb complexes and luminescent semiconductor quantum dots (QDs) provides highly advantageous photophysical properties for multiplexed biosensing. Multiplexed Tb-to-QD FRET immunoassays possess a large potential for in vitro diagnostics, but their performance is often insufficient for their application under clinical conditions. Here, we developed a homogeneous TG-FRET immunoassay for the quantification of carcinoembryonic antigen (CEA), neuron-specific enolase (NSE), and prostatespecific antigen (PSA) from a single serum sample by multiplexed Tb-to-QD FRET. Tb–IgG antibody donor conjugates were combined with compact QD-F(ab’)2 antibody acceptor conjugates with three different QDs emitting at 605, 650, and 705 nm. Upon antibody–antigen–antibody Sandwich complex formation, the QD acceptors were sensitized via FRET from Tb, and the FRET ratios of QD and Tb TG luminescence intensities increased specifically with increasing antigen concentrations. Although limits of detection (LoDs: 3.6 ng/mL CEA, 3.5 ng/mL NSE, and 0.3 ng/mL PSA) for the triplexed assay were slightly higher compared to the single-antigen assays, they were still in a clinically relevant concentration range and could be quantified in 50 μL serum samples on a B·R·A·H·M·S KRYPTOR Compact PLUS clinical immunoassay plate reader. The simultaneous quantification of CEA, NSE, and PSA at different concentrations from the same serum sample demonstrated actual multiplexing Tb-to-QD FRET immunoassays and the potential of this technology for translation into clinical diagnostics. KW - Lanthanides KW - Nanoparticles KW - Biosensing KW - Multiplexing KW - FRET KW - Fluorescence KW - PSA KW - NSE KW - CEA PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512290 DO - https://doi.org/10.3390/molecules25163679 VL - 25 IS - 16 SP - 3679 PB - MDPI AN - OPUS4-51229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Adhesion of Coatings vs. Strength of Composite Materials – A Review of Applications Evaluated by Centrifugal Adhesion Testing (CAT) N2 - Sufficient adhesion/tensile strength are basic requirements for any coating/composite material. For coatings, adhesive strength in N/mm2 is of Major interest for various applications such as decorative and water-repellent coatings on wood (paints and varnishes), optical coatings on glass and polymers (reflectors and filters), electrical coatings on semiconductors, glass and polymers (conducting and bondable layers), mechanical coatings on metals and polymers (wear-reduction, scratch-resistance) and adhesion-promoting layers. For composite materials, tensile strength in N/mm2 is also a key quantity for carbon fiber reinforced composites (CFC), laminates and adhesive-bonded joints. Centrifugal adhesion testing (CAT) transfers the single-sample tensile test from a tensile or universal testing machine into an analytical centrifuge as multiple-sample test of up to eight test pieces. The one-sided sample support instead of a two-sided sample clamping and the absence of mounting- and testing-correlated shear forces provides fast and reliable results both for adhesive strength and bonding strength by means of bonded test stamps. For bonding strength, the evaluation of failure pattern from microscopic inspection is required in order to determine the failure pattern according to ISO 10365 such as adhesive failure (AF), delamination failure (DF) and cohesive failure (CF). Hence, one test run by CAT-technology provides either statistics or ranking of up to eight samples at once. For adhesive strength of coatings, a variety of examples is discussed such as ALD-Al203 layers as adhesion promoters, evaporated Ag-layers on N-BK7 glass, sputtered Cr- and Al-layers on Borofloat 33 glass, evaporated Au-films on N-BK7 glass and sputtered SiO2 -layers on CR39 Polymer. Provided adhesive or bonding strength are high enough, the substrate or the joining part may also fail. T2 - Special PSE 2020 CY - Online meeting DA - 07.09.2020 KW - Centrifugal adhesion testing (CAT) KW - Adhesive strength KW - Pull-off test KW - Failure pattern KW - Compound strength PY - 2020 AN - OPUS4-51231 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Rosner, M. A1 - Kasemann, S. A. A1 - Kraft, R. A1 - Meixner, A. A1 - Noordmann, J. A1 - Rabb, S. A1 - Rienitz, O. A1 - Schuessler, J. A. A1 - Tatzel, Michael A1 - Vocke, R. D. T1 - Intercalibration of Mg isotope delta scales and realisation of SI traceability for Mg isotope amount ratios and isotope delta values N2 - The continuous improvement of analytical procedures using multi-collector technologies in ICP-mass spectrometry has led to an increased demand for isotope standards with improved homogeneity and reduced measurement uncertainty. For magnesium, this has led to a variety of available standards with different quality levels ranging from artefact standards to isotope reference materials certified for absolute isotope ratios. This required an intercalibration of all standards and reference materials, which we present in this interlaboratory comparison study. The materials Cambridge1, DSM3, ERMAE143, ERM-AE144, ERM-AE145, IRMM-009 and NIST SRM 980 were cross-calibrated with expanded measurement uncertainties (95% confidence level) of less than 0.030‰ for the δ25/24Mg values and less than 0.037‰ for the δ26/24Mg values. Thus, comparability of all magnesium isotope delta (δ) measurements based on these standards and reference materials is established. Further, ERM-AE143 anchors all magnesium δ-scales to absolute isotope ratios and therefore establishes SI traceability, here traceability to the SI base unit mole. This applies especially to the DSM3 scale, which is proposed to be maintained. With ERM-AE144 and ERM-AE145, which are product and educt of a sublimation-condensation process, for the first time a set of isotope reference materials is available with a published value for the apparent triple isotope fractionation exponent θapp, the fractionation relationship ln α(25/24Mg)/ln α(26/24Mg). KW - Delta scale KW - Traceability KW - Scale anchor KW - Absolute isotope ratio KW - Comparability KW - Triple isotope fractionation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511557 DO - https://doi.org/10.1111/ggr.12327 SN - 1751-908X VL - 44 IS - 3 SP - 439 EP - 457 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-51155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rienitz, O. A1 - Jährling, R. A1 - Noordmann, J. A1 - Pape, C. A1 - Röhker, K. A1 - Vogl, Jochen A1 - Manzano, J. V. L. A1 - Kozlowski, W. A1 - Caciano de Siena, R. A1 - Marques Rodrigues, J. A1 - Galli, A. H. A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Lee, J. H. A1 - Min, H.-S. A1 - Chingbo, C. A1 - Naijie, S. A1 - Qian, W. A1 - Ren, T. A1 - Jun, W. A1 - Tangpaisarnkul, N. A1 - Suzuki, T. A1 - Nonose, N. A1 - Mester, Z. A1 - Yang, L. A1 - Pagliano, E. A1 - Greenberg, P. A1 - Mariassy, M. A1 - Näykki, T. A1 - Cankur, O. A1 - Coskun, F. G. A1 - Ari, B. A1 - Can, S. Z. T1 - CCQM-K122 "Anionic impurities and lead in salt solutions" N2 - The determination of the mass fractions of bromide, sulfate, and lead as well as the isotopic composition of the lead (expressed as the molar mass and the amount fractions of all four stable lead isotopes) in an aqueous solution of sodium chloride with a mass fraction of 0.15 g/g was the subject of this comparison. Even though the mass fractions ranged from 3 μg/g (bromide) to 50 ng/g (lead), almost all results reported agreed with the according KCRVs. KW - Absolute isotope ratio KW - Lead isotope ratios KW - Metrology KW - Traceability PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1A/08012 VL - 57 IS - 1A SP - 8012 PB - IOP Science AN - OPUS4-51156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkler, Nicolas P. A1 - Neumann, Patrick P. A1 - Säämänen, A. A1 - Schaffernicht, E. A1 - Lilienthal, A. J. ED - Zemčík, R. ED - Krystek, J. T1 - High-quality meets low-cost: Approaches for hybrid-mobility sensor networks N2 - Air pollution within industrial scenarios is a major risk for workers, which is why detailed knowledge about the dispersion of dusts and gases is necessary. This paper introduces a system combining stationary low-cost and high-quality sensors, carried by ground robots and unmanned aerial vehicles. Based on these dense sampling capabilities, detailed distribution maps of dusts and gases will be created. This system enables various research opportunities, especially on the fields of distribution mapping and sensor planning. Standard approaches for distribution mapping can be enhanced with knowledge about the environment’s characteristics, while the effectiveness of new approaches, utilizing neural networks, can be further investigated. The influence of different sensor network setups on the predictive quality of distribution algorithms will be researched and metrics for the quantification of a sensor network’s quality will be investigated. T2 - 36th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Pilsen, Czech Republic DA - 24.09.2019 KW - Mobile robot olfaction KW - Air quality monitoring KW - Wireless sensor network KW - Gas distribution mapping KW - Occupational health PY - 2020 DO - https://doi.org/10.1016/j.matpr.2020.05.799 VL - 32 SP - 250 EP - 253 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-51108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liaskos, C. A1 - Rhoderick, G. A1 - Hodges, J. A1 - Possolo, A. A1 - Wilke, Olaf T1 - Pilot comparison CCQM-P177 - monoterpenes in nitrogen at 2.5 nmol/mol - final report N2 - Growing awareness of the impact of monoterpenes on climate, atmospheric chemistry, and indoor air quality has necessitated the development of measurement standards to globally monitor and control their emissions. For National Metrology Institutes to develop such standards, it is essential that they demonstrate measurement equivalence for assigned values at the highest levels of accuracy. This report describes the results of a pilot comparison for 4 key monoterpene species: α-pinene, 3-carene, R-limonene and 1,8-cineole, at a nominal amount-of-substance fraction of 2.5 nmol mol-1. The objective of this comparison is to evaluate participant capabilities to measure trace-level monoterpenes using their own calibration techniques. KW - Pilot comparison KW - CCQM KW - Monoterpene KW - Accuracy PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1A/08018 SN - 0026-1394 SN - 1681-7575 VL - 57 IS - 1A SP - 08018-1 EP - 08018-21 PB - IOP Science AN - OPUS4-51111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Analysis of Particle Size Distribution for Bimodal Model Nanoparticles by Scanning Electron Microscopy N2 - The present study addresses the capability of measurement of relative particle number concentration by scanning electron microscopy for model bimodal silica and gold samples prepared in the frame of the European research project “nPSize - Improved traceability chain of nanoparticle size measurements” as candidate reference nanoparticles. T2 - Microscopy and Microanalysis 2020 CY - Online meeting DA - 03.08.2020 KW - Nanoparticles KW - Silica KW - Gold KW - Electron microscopy KW - Particle size distribution PY - 2020 AN - OPUS4-51112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Towards 3D understanding of non spherical nanoparticles by Transmission Kikuchi Diffraction (TKD) for improved particle size distribution by electron microscopy N2 - In this paper one refined approach is applied to determine the exact orientation of bipyramidal TiO2 nanoparticles prepared with good dispersion as almost isolated particles on a carbon TEM grid. The advantages of the recently developed high-throughput Transmission Kikuchi Diffraction (TKD) are used to identify quickly and reliably the geometrical orientation of the crystalline TiO2 nanoparticle bipyramids (anatase) on a statistically relevant number of particles. T2 - Microscopy and Microanalysis 2020 CY - Online meeting DA - 03.08.2020 KW - Nanoparticles KW - Transmission Kikuchi Diffraction (TKD) KW - TiO2 KW - 3D KW - Electron microscopy PY - 2020 AN - OPUS4-51113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Towards automated electron microscopy image segmentation for nanoparticles of complex shape by convolutional neural networks N2 - In this contribution different ways are explored with the aim to generate suitable training data for ‘non-ideal’ samples using various approaches, e.g., computer-generated images or unsupervised learning algorithms such as generative adversarial networks (GANs). We used these data to train simple CNNs to produce segmentation masks of SEM images and tested the trained networks on real SEM images of complex nanoparticle samples. The novel use of CNN for the automated analysis of the size of nanoparticles of complex shape and with a high degree of agglomeration has proved to be a promising tool for the evaluation of particle size distribution on a large number of constituent particles. Further development and validation of the preliminary model, respectively larger training and validation data sets are necessary. T2 - Microscopy and Microanalysis 2020 CY - Online meeting DA - 03.08.2020 KW - Nanoparticles KW - Automatisation KW - Image segmentation KW - Convolutional neural networks KW - Electron microscopy PY - 2020 AN - OPUS4-51114 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moskovchenko, A. I. A1 - Vavilov, V. P. A1 - Bernegger, Raphael A1 - Maierhofer, Christiane A1 - Chulkov, A. O. T1 - Detecting Delaminations in Semitransparent Glass Fiber Composite by Using Pulsed Infrared Thermography N2 - Thanks to its good strength/mass ratio, a glass fibre reinforced plastic (GFRP) composite is a common material widely used in aviation, power production, automotive and other industries. In its turn, active infrared (IR) nondestructive testing (NDT) is a common inspection technique for detecting and characterizing structural defects in GFRP. Materials to be tested are typically subjected to optical heating which is supposed to occur on the material surface. However, GFRP composite is semitransparent for optical radiation of both visual and IR spectral bands. Correspondingly, the inspection process represents a certain combination of both optical and thermal phenomena. Therefore, the known characterization algorithms based on pure heat diffusion cannot be applied to semi-transparent materials. In this study, the phenomenon of GFRP semi-transparency has been investigated numerically and experimentally in application to thermal NDT. Both Xenon flash tubes and a laser have been used for thermal stimulation of opaque and semi-transparent test objects. It has been shown that the Penetration of optical heating radiation into composite reduces detectability of shallower defects, and the signal-to-noise ratio can be enhanced by applying the technique of thermographic signal reconstruction (TSR). In the inspection of the semi-transparent GFRP composite, the most efficient has been the laser heating followed by the TSR data processing. The perspectives of defect characterization of semi-transparent materials by using laser heating are discussed. A neural network has been used as a candidate tool for evaluating defect depth in composite materials, but its training should be performed in identical with testing conditions. KW - Infrared thermography KW - Thermal testing KW - GFRP KW - Semi-transparent composite KW - Laser heating PY - 2020 DO - https://doi.org/10.1007/s10921-020-00717-x VL - 39 SP - 69 PB - Springer Science+Business Media, LLC, part of Springer Nature 2020 AN - OPUS4-51179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Aktivitätsfeld Security an der BAM N2 - Vortrag über das Aktivitätsfeld Security an der BAM und der beiden, im Foresight-Prozess identifizierten Schwerpunktthemen "Auswirkungsbetrachtung" und "Analytik, Detektion, Messung, Identifikation". T2 - Workshop / Informationsveranstaltung Sicherheitsforschung TGZ PM CY - Online meeting DA - 09.09.2020 KW - Aktivitätsfeld Security KW - Auswirkungsbetrachtung KW - Identifikation KW - Analytik KW - Detektion KW - Messung PY - 2020 AN - OPUS4-51188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - Characterization of a Flexible Piezopolymer-based Interdigital Transducer for Selective Excitation of Ultrasonic Guided Waves N2 - Structural health monitoring (SHM) is a term that groups together techniques adopted to evaluate in a continued fashion the structural integrity and degradation of technical appliances. SHM is particularly attractive for components that are difficult to access or expensive to take off-line. Among many other techniques, SHM can be performed using ultrasonic guided waves (UGW) which have an advantage of traveling over Long distances. Various guided wave modes exist along with many methods for their generation and sensing, e.g by means of interdigital transducers (IDT). This contribution is dedicated to the design and characterization of a flexible piezopolymerbased IDT which allows for the selective excitation of UGW, resulting in more straightforward data analysis. The designed IDT was characterized using a 3D Laser Doppler Vibrometer (3D LDV) in the air to identify and analyze the IDT’s Vibration modes. Then the transducer was mounted on an aluminum plate, and the generated wavefield was measured with the 3D LDV. According to this investigation, we demonstrate that it is possible to selectively excite desired guided wave mode, namely the A0 mode, suppressing the excitation of the S0 mode. Moreover, the measured wavefield allows for analysis of the directivity of the designed IDT. All in all the results show good correlation between theoretical predictions and measured values, thus allowing to use the current design in terms of selective excitation as it is. T2 - IEEE International Ultrasonics Symposium CY - Online meeting DA - 06.09.2020 KW - Lamb waves KW - Non-Destructive Testing KW - Structural Health Monitoring KW - Polyvinylidene Fluoride (PVDF) PY - 2020 AN - OPUS4-51202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Faghani, A. A1 - Gholami, M. F. A1 - Trunk, M. A1 - Müller, J. A1 - Pachfule, P. A1 - Vogl, S. A1 - Donskyi, Ievgen A1 - Li, M. A1 - Nickl, Philip A1 - Shao, J. A1 - Huang, M. R. S. A1 - Unger, Wolfgang A1 - Arenal, R. A1 - Koch, C. T. A1 - Paulus, B. A1 - Rabe, J. P. A1 - Thomas, A. A1 - Haag, R. A1 - Adeli, M. T1 - Metal-Assisted and Solvent-Mediated Synthesis of Two-Dimensional Triazine Structures on Gram Scale N2 - Covalent triazine frameworks are an emerging material class that have shown promising performance for a range of applications. In this work, we report on a metal-assisted and solvent-mediated reaction between calcium carbide and cyanuric chloride, as cheap and commercially available precursors, to synthesize two-dimensional triazine structures (2DTSs). The reaction between the solvent, dimethylformamide, and cyanuric chloride was promoted by calcium carbide and resulted in dimethylamino-s-triazine intermediates, which in turn undergo nucleophilic substitutions. This reaction was directed into two dimensions by calcium ions derived from calcium carbide and induced the formation of 2DTSs. The role of calcium ions to direct the two-dimensionality of the final structure was simulated using DFT and further proven by synthesizing molecular intermediates. The water content of the reaction medium was found to be a crucial factor that affected the structure of the products dramatically. While 2DTSs were obtained under anhydrous conditions, a mixture of graphitic material/2DTSs or only graphitic material (GM) was obtained in aqueous solutions. Due to the straightforward and gram-scale synthesis of 2DTSs, as well as their photothermal and photodynamic properties, they are promising materials for a wide range of future applications, including bacteria and virus incapacitation. KW - XPS KW - Triazine KW - 2D PY - 2020 DO - https://doi.org/10.1021/jacs.0c02399 VL - 142 IS - 30 SP - 12976 EP - 12986 PB - ACS American Chemical Society AN - OPUS4-51203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hildebrandt, L. A1 - von der Au, Marcus A1 - Zimmermann, T. A1 - Reese, A. A1 - Ludwig, J. A1 - Pröfrock, D. T1 - A metrologically traceable protocol for the quantification of trace metals in different types of microplastic N2 - The presence of microplastic (MP) particles in aquatic environments raised concern About possible enrichment of organic and inorganic pollutants due to their specific surface and chemical properties. In particular the role of metals within this context is still poorly understood. Therefore, the aim of this work was to develop a fully validated acid digestion protocol for metal analysis in different polymers, which is a prerequisite to study such interactions. The proposed digestion protocol was validated using six different certified reference materials in the microplastic size range consisting of polyethylene, polypropylene, acrylonitrile butadiene styrene and polyvinyl chloride. As ICP-MS/MS enabled time-efficient, sensitive and robust analysis of 56 metals in one measurement, the method was suitable to provide mass fractions for a multitude of other elements beside the certified ones (As, Cd, Cr, Hg, Pb, Sb, Sn and Zn). Three different microwaves, different acid mixtures as well as different temperatures in combination with different hold times were tested for optimization purposes. With the exception of Cr in acrylonitrile butadiene styrene, recovery rates obtained using the optimized protocol for all six certified reference materials fell within a range from 95.9% ± 2.7% to 112% ± 7%. Subsequent optimization further enhanced both precision and recoveries ranging from 103% ± 5% to 107 ± 4% (U; k = 2 (n = 3)) for all certified metals (incl. Cr) in acrylonitrile butadiene styrene. The results clearly show the analytical challenges that come along with metal analysis in chemically resistant plastics. Addressing specific analysis Tools for different sorption scenarios and processes as well as the underlying kinetics was beyond this study’s scope. However, the future application of the two recommended thoroughly validated total acid digestion protocols as a first step in the direction of harmonization of metal analysis in/on MP will enhance the significance and comparability of the generated data. It will contribute to a better understanding of the role of MP as vector for trace metals in the environment. KW - Microplatic KW - Digestion KW - Analytical Chemistry PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510727 DO - https://doi.org/10.1371/journal.pone.0236120 VL - 15 IS - 7 SP - e0236120 AN - OPUS4-51072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hielscher-Bofinger, Stefan A1 - Beck, Uwe T1 - Multiple-sample Testing: Adhesive Strength of Coatings and Bonding Strength of Adhesives evaluated by Centrifugal Adhesion Testing (CAT) N2 - The quantitative determination of adhesion and cohesion properties is a key requirement for adhesive-bonded joints and coated components in both R&D and Quality assurance. Because of the huge variety of layer/substrate Systems in terms of materials and large thickness range, adhesion tests display the same diversity as layer/substrate systems. There are only two tensile testing procedures available, that determine adhesive strength in terms of force per area (N/mm²), the single-sample pull-off test in a tensile testing machine and the multiple-sample-test using the Centrifugal Adhesion Testing (CAT) Technology. The CAT Technology is a testing method which uses centrifugal force as tensile testing force in a multiple-sample arrangement within a drum rotor of a Desktop centrifuge. Hence, the adhesive/bonding strength A/B can be determined on a statistical basis under identical testing conditions for up to eight samples. A variety of examples for bonding strength of adhesives, adhesive strength of coatings and compound strength of composite materials is discussed such as metalto-metal and glass-to-metal bonding, sputtered SiO2-layers on CR39 Polymer and carbon fiber reinforced polymer. T2 - Colloquium Department 6. CY - Berlin, BAM, Germany DA - 03.09.2020 KW - Centrifugal Adhesion Testing (CAT) KW - Adhesive strength KW - Bonding strength KW - Composite strength KW - Interlaboratory comparision PY - 2020 AN - OPUS4-51178 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - The dark side of science N2 - This talk explores the various ways in which bad science can proliferate in the current academic environment, and what can be done to recognize and (maybe) correct it. T2 - Better with Scattering workshop 2020 CY - BAM, Berlin, Germany DA - 16.03.2020 KW - Scientific rigor KW - Academic fraud KW - Academic metrics PY - 2020 AN - OPUS4-51017 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - McSAS for SAS analysis: Usage, Benefits and Potential Pitfalls N2 - This talk introduces McSAS, code for analysis of scattering patterns to extract particle size distributions. It highlights how it works, how it should be used, and when it may (not) be applied T2 - Better with Scattering workshop 2020 CY - BAM, Berlin, Germany DA - 16.03.2020 KW - Small angle scattering KW - Software KW - Analysis PY - 2020 AN - OPUS4-51019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rautenberg, Max A1 - Bhattacharya, Biswajit A1 - Akhmetova, Irinia A1 - Emmerling, Franziska T1 - Mechanochemical and solution syntheses of two novel cocrystals of orcinol with two N,N0-Dipyridines: Structural diversity with varying ligand flexibility N2 - We studied the influence of coformers flexibility on the supramolecular assembly of 5-substituted resorcinol. Two cocrystals of orcinol (ORL) with two dipyridine molecules, i.e. 1,2-di(4-pyridyl)ethane (ORLeBPE) and 1,2-di(4-pyridyl)ethylene (ORLeBPY), were prepared by mechanochemical synthesis and slow evaporation of solvent. The new crystalline solids were thoroughly characterized by single crystal Xray diffraction (SCXRD), powder X-ray diffraction analysis (PXRD), Fourier-transform infrared spectroscopy (FT-IR), differential thermal analysis (DTA), and thermogravimetric analysis (TGA). Structural determination reveals that in both cocrystals, the phenolepyridine, i.e. OeH/N(py) heterosynthon takes the main role in the formation of cocrystals. In ORLeBPE, the components form infinite 1D zig-zag chains, which are extended to 2D layer structure by inter-chain CeH/O interactions between BPE hydrogen atoms and hydroxyl oxygen atoms of ORL. In ORLeBPY, the components form a 0D fourcomponent complex. Formation of the discrete assemblies is attributed to the comparative rigid nature of BPY, which restricts the formation of an extended network. KW - Cocrystal KW - Single crystal KW - X-ray diffraction KW - Mechanochemistry PY - 2020 DO - https://doi.org/10.1016/j.molstruc.2020.128303 SN - 0022-2860 VL - 1217 SP - 128303 PB - Elsevier B.V. AN - OPUS4-51023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sattari, S. A1 - Beyranvand, S. A1 - Soleimani, K. A1 - Rassoli, K. A1 - Salahi, P. A1 - Donskyi, Ievgen A1 - Shams, A. A1 - Unger, Wolfgang A1 - Yari, A. A1 - Farjanikish, G. A1 - Nayebzadeh, H. A1 - Adeli, M. T1 - Boronic Acid-Functionalized Two-Dimensional MoS2 at Biointerfaces N2 - While noncovalent interactions at two-dimensional nanobiointerfaces are extensively investigated, less knowledge about covalent interactions at this interface is available. In this work, boronic acid-functionalized 2D MoS2 was synthesized and its covalent multivalent interactions with bacteria and nematodes were investigated. Polymerization of glycidol by freshly exfoliated MoS2 and condensation of 2,5-thiophenediylbisboronic acid on the produced platform resulted in boronic acid-functionalized 2D MoS2. The destructive interactions between 2D MoS2 and bacteria as well as nematodes were significantly amplified by boronic acid functional groups. Because of the high antibacterial and antinematodal activities of boronic acid-functionalized 2D MoS2, its therapeutic efficacy for diabetic wound healing was investigated. The infected diabetic wounds were completely healed 10 days after treatment with boronic acid-functionalized 2D MoS2, and a normal structure for recovered tissues including different layers of skin, collagen, and blood vessels was detected. KW - XPS KW - Boronic acid-functionalized 2D MoS2 KW - Covalent interactions KW - Bacteria KW - Nanobiointerfaces PY - 2020 DO - https://doi.org/10.1021/acs.langmuir.0c00776 VL - 36 IS - 24 SP - 6706 EP - 6715 PB - ACS American Chemical Society AN - OPUS4-51024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Luco Colilles, Arnau T1 - Evaluation of two compact near-infrared spectrometers for the detection of microplastics in soil samples N2 - In the last years, the Process Analytical Technology (PAT) research field has become of great importance due to its connection with the industrial world. This industry related research, along with the evolutionary progress that technology has seen lately, has allowed that key analytical techniques in an industrial environment have undergone a radical development. One of these techniques has been the near-infrared spectroscopy (NIRS). This technique, currently common in "online" industrial analysis, has seen a remarkable revolution, especially since the introduction of the microelectromechanical systems technology (MEMS) in the spectroscopy field. Nowadays it is possible to find compact spectrometers no bigger than a wristwatch in the market. Although there is an unavoidable question: can these compact spectrometers actually compete against the traditional spectrometers? In this project different calibration parameters of two compact NIR spectrometers ("Spectral Engines Oy NIR-One Sensor NM2.0", with 1550 to 1950 nm range; and "NeoSpectra Si-ware", with 1300 to 2550 nm range) were evaluated, and the obtained results were compared with a reference spectrometer ("Bruker Optik GmbH Matrix-F", with 15000 to 4000 cm–1 range). In order to obtain the different calibration parameters, a sequence of quality performance tests were conducted. The results obtained after the different experiments carried out with both compact spectrometers prove that their performance is more than acceptable for routine analysis. Afterward, model samples of different microplastics in soil at different known concentration were analyzed with all three spectrometers. Chemometric models capable to identify and classify microplastics in soil were established. For this analysis five of the most used plastics worldwide were used: polyethylene (PE), polyethylene terephthalate (PET), polypropylene (PP), polystyrene (PS), and polyvinyl chloride (PVC). After the Principal component analysis (PCA), it can be seen that only the NIR-One NM2.0 is capable to differentiate all types of microplastics in soil at concentrations of 1–2 %, while the NeoSpectra Si-ware is unable to identify the PET sample. KW - Near-infrared KW - Microplastics KW - Compact spectrometers PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511626 UR - http://hdl.handle.net/2445/138198 SP - 1 EP - 29 PB - Universitat de Barcelona CY - Barcelona AN - OPUS4-51162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Schwaar, Timm T1 - Entwicklung von multidimensionalen Hochdurchsatzmethoden zur Analyse von Partikel-basierten Peptidbibliotheken N2 - Gegenwärtig ist das Interesse und der Bedarf von Proteinbindern insbesondere in der Biotechnik und Pharmaforschung sehr groß. Kombinatorische, Partikel-basierte (One-Bead-One-Compound) Peptidbibliotheken sind eine Technik, um selektiv bindende Proteine zu identifizieren. Allerdings beinhaltet das Screening dieser Peptidbibliotheken aufwendige Schritte, wie die Separation, Sequenzierung und Charakterisierung von identifizierten Bindern. In dieser Arbeit wurde ein Chip-System entwickelt, auf dem alle Schritte eines Screenings durchgeführt werden können. Dafür wurde ein Glasobjektträger mit einem magnetisch leitenden, doppelseitigen Klebeband versehen. Die Partikel der Bibliothek wurden durch ein Sieb aufgetragen. Dies führte zu einer geordneten Immobilisierung der Partikel auf dem Chip. Über 30.000 Partikel konnten so auf einem Chip immobilisiert werden. Für die Identifizierung von selektiven Protein-bindenden Peptiden wird die immobilisierte Peptidbibliothek mit einem Fluorophor-markierten Protein inkubiert, bindende Partikel mittels Fluoreszenzscan identifiziert und die Peptidsequenz direkt auf dem Chip mittels Matrix-Assisted-Laser-Desorption/Ionization-(MALDI)-Flugzeit-(TOF)-Massenspektroskopie (MS) bestimmt. Die Durchführung einer Abbruchsequenz-Methode erlaubt die eindeutige Bestimmung der Peptidsequenzen mit einer nahezu 100 % Genauigkeit. Die entwickelte Technologie wurde in einem FLAG-Peptid-Modell validiert. Bei dem Screening wurden neue anti-FLAG-Antikörper-bindende Peptide identifiziert. Anschließend wurden in einem Screening von ca. 30.000 Partikeln IgG-bindende Peptide mit mittleren mikromolaren Dissoziationskonstanten identifiziert. Für die Identifizierung stärkerer Binder wurde eine magnetische Anreicherung entwickelt, die dem Chip-Screening vorgeschaltet werden kann. Hiermit wurden aus ca. 1 Million gescreenter Partikel, Peptide mit Dissoziationskonstanten im niedrigen mikromolaren Bereich identifiziert. N2 - The screening of one-bead-one-compound (OBOC) libraries is a well-established technique for the identification of protein-binding ligands. The demand for binders with high affinity and specificity towards various targets has surged in the biomedical and pharmaceutical field in recent years. The combinatoric peptide screening traditionally involves tedious steps such as affinity selection, bead picking, sequencing and characterization. In this thesis, a high-throughput “all-on-one chip” system is presented to avoid slow and technically complex bead picking steps. Beads of a combinatorial peptide library are immobilized on a conventional glass slide equipped with an electrically conductive tape. The beads are applied by using a precision sieve, which allows the spatially ordered immobilization of more than 30,000 beads on one slide. For the target screening, the immobilized library is subsequently incubated with a fluorophore-labeled target protein. In a fluorescence scan followed by matrix-assisted laser desorption/ionization (MALDI)-time of flight (TOF) mass spectrometry (MS), high-affinity binders are directly and unambiguously sequenced directly from the bead. The use of an optimized ladder sequencing approach improved the accuracy of the de-novo sequencing step to 100 %. This new technique was validated by employing a FLAG-based model system. In a first step, new peptide binders for the M2 anti-FLAG monoclonal antibody were identified. Finally, this system was utilized to screen for IgG-binding peptides. The screening of about 30.000 peptides on one chip led to the identification of peptide binders in the mid micromolar range. A magnetic enrichment technique was developed to increase the number of screened beads. By combining the magnetic enrichment strategy with the chip system, 1 million beads were screened and IgG-binders in the low micromolar range were identified. KW - Peptidbibliotheken KW - Hochdurchsatzscreening KW - Peptidsequenzierung KW - Chip-Screening PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511649 DO - https://doi.org/10.18452/21793 SP - 1 EP - 153 PB - Humboldt-Universität CY - Berlin AN - OPUS4-51164 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya A1 - Bulletti, A. A1 - Giannelli, P. A1 - Capineri, L. A1 - Prager, Jens T1 - Characterization of a Flexible Piezopolymer-based Interdigital Transducer for Selective Excitation of Ultrasonic Guided Waves N2 - Structural health monitoring (SHM) is a term that groups together techniques adopted to evaluate in a continued fashion the structural integrity and degradation of technical appliances. SHM is particularly attractive for components that are difficult to access or expensive to take off-line. Among many other techniques, SHM can be performed using ultrasonic guided waves (UGW) which have an advantage of traveling over Long distances. Various guided wave modes exist along with many methods for their generation and sensing, e.g by means of interdigital transducers (IDT). This contribution is dedicated to the design and characterization of a flexible piezopolymerbased IDT which allows for the selective excitation of UGW, resulting in more straightforward data analysis. The designed IDT was characterized using a 3D Laser Doppler Vibrometer (3D LDV) in the air to identify and analyze the IDT’s Vibration modes. Then the transducer was mounted on an aluminum plate, and the generated wavefield was measured with the 3D LDV. According to this investigation, we demonstrate that it is possible to selectively excite desired guided wave mode, namely the A0 mode, suppressing the excitation of the S0 mode. Moreover, the measured wavefield allows for analysis of the directivity of the designed IDT. All in all the results show good correlation between theoretical predictions and measured values, thus allowing to use the current design in terms of selective excitation as it is. T2 - I2020 IEEE International Ultrasonics Symposium (IUS) CY - Online meeting DA - 07.09.2020 KW - Lamb waves KW - Non-Destructive Testing KW - Structural Health Monitoring KW - Polyvinylidene Fluoride (PVDF) PY - 2020 SN - 978-1-7281-5448-0 SP - 1261, 45 AN - OPUS4-51441 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Immunomagnetic ochratoxin A assay with smartphone-based amperometric detection N2 - Toxic secondary metabolites produced by fungi (aka mycotoxins) are often identified as contaminants in food and pose a severe health risk. Ochratoxin A (OTA) is one of the most abundant mycotoxins found in grains such as wheat, rye or oats. Thus, the fast and cost-effective detection of OTA is of great importance, to ensure that the toxin concentration is below the legal limits. Currently, mycotoxin detection in mill operations is typically performed by means of the antibody-based ELISA (Enzyme-linked Immunosorbent Assay) method, which requires extensive laboratory equipment and specialized personnel. The aim of this project is to establish a more user-friendly detection method. Thus, we developed a magnetic bead-based assay enabling the quantification of OTA with a miniaturized potentiostat connected to a smartphone. T2 - SALSA Make and Measure 2020 CY - Online meeting DA - 15.10.2020 KW - ochratoxin A KW - smartphone KW - amperometry KW - cyclic voltammetry KW - magnetic beads KW - screen-printed electrodes PY - 2020 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-51445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kunkel, B. A1 - Kabelitz, Anke A1 - de Oliveira Guilherme Buzanich, Ana A1 - Wohlrab, S. T1 - Increasing the Efficiency of Optimized V-SBA-15 Catalysts in the Selective Oxidation of Methane to Formaldehyde by Artificial Neural Network Modelling N2 - The present study investigates the possibility of improving the selective oxidation of methane to formaldehyde over V-SBA-15 catalysts in two different ways. In a classical approach of catalyst optimization, the in situ synthesis of V-SBA-15 catalysts was optimized with regard to the applied pH value. Among the set of catalysts synthesized, a higher amount of incorporated vanadium, a higher content of polymeric VOx species as well as a less ordered structure of the support material were observed by increasing the pH values from 2.0 to 3.0. An optimum in performance during the selective oxidation of methane to formaldehyde with respect to activity and selectivity was found over V-SBA-15 prepared at a pH value of 2.5. With this knowledge, we have now evaluated the possibilities of reaction control using this catalyst. Specifically, artificial neural network modelling was applied after the collection of 232 training samples for obtaining insight into the influence of different reaction parameters (temperature; gas hourly space velocity (GHSV); and concentration of O2, N2 and H2O) onto methane conversion and selectivity towards formaldehyde. This optimization of reaction conditions resulted in an outstanding high space-time yield of 13.6 kgCH2O∙kgcat∙h−1 KW - Artificial neural network modelling KW - Selective oxidation KW - Molecular VOx catalysts KW - Formaldehyde PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517420 DO - https://doi.org/10.3390/catal10121411 VL - 10 IS - 12 SP - 1411 PB - MDPI AN - OPUS4-51742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaenisch, Gerd-Rüdiger A1 - Ewert, Uwe A1 - Waske, Anja A1 - Funk, Alexander T1 - Radiographic Visibility Limit of Pores in Metal Powder for Additive Manufacturing N2 - The quality of additively manufactured (AM) parts is determined by the applied process parameters used and the properties of the feedstock powder. The influence of inner gas pores in feedstock particles on the final AM product is a phenomenon which is difficult to investigate since very few non-destructive measurement techniques are accurate enough to resolve the micropores. 3D X-ray computed tomography (XCT) is increasingly applied during the process chain of AM parts as a non-destructive monitoring and quality control tool and it is able to detect most of the pores. However, XCT is time-consuming and limited to small amounts of feedstock powder, typically a few milligrams. The aim of the presented approach is to investigate digital radiography of AM feedstock particles as a simple and fast quality check with high throughput. 2D digital radiographs were simulated in order to predict the visibility of pores inside metallic particles for different pore and particle diameters. An experimental validation was performed. It was demonstrated numerically and experimentally that typical gas pores above a certain size (here: 3 to 4.4 µm for the selected X-ray setup), which could be found in metallic microparticles, were reliably detected by digital radiography. KW - Additive manufacturing KW - Feedstock powder KW - Porosity KW - Digital radiography KW - Numerical simulation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517880 DO - https://doi.org/10.3390/met10121634 VL - 10 IS - 12 SP - 1634 PB - MDPI AN - OPUS4-51788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Laser-Induced Breakdown Spectroscopy (LIBS) Automated 2D chemical analysis of chloride content in concrete structures N2 - The application of a LIBS system is presented. A diode-pumped low energy laser (3 mJ, 1.5 ns, 100 Hz) and a compact NIR spectrometer are used. A scanner allows the two-dimensional element mapping. For the quantitative analysis calibration of the system is carried out with reference samples in a concentration range of chlorine of 0.05 wt.% to 2.5 wt.%. To determine the 2D distribution of harmful elements (Cl, C), concrete cores were drilled, split and analyzed directly. By comparing the chloride ingress and the carbonation, the interaction of both processes can be visualized in one measurement that takes less than 10 minutes with a drill core of 50 mm x 100 mm. Results obtained were compared and verified with standard measurements. T2 - Concrete Solutions 2019 CY - Cluj Napoca, Romania DA - 30.09.2019 KW - Chloride KW - Beton KW - LIBS KW - Schädigung PY - 2019 AN - OPUS4-51703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Fast quantitave chemical analysis of concrete using LIBS N2 - Overview of application of LIBS for the fast and automated quantitative chemical analysis of concrete. T2 - NDT-E Workshop CY - Berlin, Germany DA - 12.06.2019 KW - Sulphate KW - LIBS KW - Concrete KW - Damage KW - Chloride KW - Mapping PY - 2019 AN - OPUS4-51704 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - LIBS for the analysis of concrete N2 - Special features and examples of using LIBS on concrete. T2 - Workshop on tandem LIBS/LA-ICP-MS CY - Berlin, Germany DA - 18.11.2019 KW - Mobile system KW - LIBS KW - Concrete KW - Damage KW - Chloride KW - Sulphate KW - Mapping PY - 2019 AN - OPUS4-51710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Mobile LIBS system for evaluation of concrete structures on site N2 - Features and application of a mobile LIBS system for evaluation of concrete structures on-site. T2 - EMSLIBS 2019 CY - Brno, Czech Republic DA - 08.09.2019 KW - On-site KW - LIBS KW - Concrete KW - Mapping KW - Evaluation PY - 2019 AN - OPUS4-51711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziegler, K. A1 - Kunert, A. T. A1 - Reinmuth-Selzle, K. A1 - Leifke, A. L. A1 - Widera, D. A1 - Weller, Michael G. A1 - Schuppan, D. A1 - Fröhlich-Nowoisky, J. A1 - Lucas, K. A1 - Pöschl, U. T1 - Chemical modification of pro-inflammatory proteins by peroxynitrite increases activation of TLR4 and NF-κB: Implications for the health effects of air pollution and oxidative stress N2 - Environmental pollutants like fine particulate matter can cause adverse health effects through oxidative stress and inflammation. Reactive oxygen and nitrogen species (ROS/RNS) such as peroxynitrite can chemically modify proteins, but the effects of such modifications on the immune system and human health are not well understood. In the course of inflammatory processes, the Toll-like receptor 4 (TLR4) can sense damage-associated molecular patterns (DAMPs). Here, we investigate how the TLR4 response and pro-inflammatory potential of the proteinous DAMPs α-Synuclein (α-Syn), heat shock protein 60 (HSP60), and high-mobility-group box 1 protein (HMGB1), which are relevant in neurodegenerative and cardiovascular diseases, changes upon chemical modification with peroxynitrite. For the peroxynitrite-modified proteins, we found a strongly enhanced activation of TLR4 and the pro-inflammatory transcription factor NF-κB in stable reporter cell lines as well as increased mRNA expression and secretion of the pro-inflammatory cytokines TNF-α, IL-1β, and IL-8 in human monocytes (THP-1). This enhanced activation of innate immunity via TLR4 is mediated by covalent chemical modifications of the studied DAMPs. Our results show that proteinous DAMPs modified by peroxynitrite more potently amplify inflammation via TLR4 activation than the native DAMPs, and provide first evidence that such modifications can directly enhance innate immune responses via a defined receptor. These findings suggest that environmental pollutants and related ROS/RNS may play a role in promoting acute and chronic inflammatory disorders by structurally modifying the body's own DAMPs. This may have important consequences for chronic neurodegenerative, cardiovascular or gastrointestinal diseases that are prevalent in modern societies, and calls for action, to improve air quality and climate in the Anthropocene. KW - Protein nitration KW - Protein oligomerization KW - Damage-associated molecular patterns (DAMPs) KW - Pattern recognition receptor KW - Anthropocene KW - Environmental pollutants PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517128 DO - https://doi.org/10.1016/j.redox.2020.101581 VL - 37 SP - 101581 PB - Elsevier B.V. AN - OPUS4-51712 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steglich, P. A1 - Bondarenko, S. A1 - Mai, C. A1 - Paul, Martin A1 - Weller, Michael G. A1 - Mai, A. T1 - CMOS-Compatible Silicon Photonic Sensor for Refractive Index Sensing Using Local Back-Side Release N2 - Silicon photonic sensors are promising candidates for lab-on-a-chip solutions with versatile applications and scalable production prospects using complementary metal-oxide semiconductor (CMOS) fabrication methods. However, the widespread use has been hindered because the sensing area adjoins optical and electrical components making packaging and sensor handling challenging. In this work, a local back-side release of the photonic sensor is employed, enabling a separation of the sensing area from the rest of the chip. This approach allows preserving the compatibility of photonic integrated circuits in the front-end of line and metal interconnects in the back-end of line. The sensor is based on a micro-ring resonator and is fabricated on wafer-level using a CMOS technology. We revealed a ring resonator sensitivity for homogeneous sensing of 106 nm/RIU. KW - Photonic biosensor KW - Lab-on-a-chip KW - Ring resonator KW - Resonance wavelength shift KW - PIC technology KW - Back-side integration PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517139 DO - https://doi.org/10.1109/LPT.2020.3019114 VL - 32 IS - 19 SP - 1241 EP - 1244 PB - IEEE AN - OPUS4-51713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brangsch, J. A1 - Reimann, C. A1 - Kaufmann, Jan Ole A1 - Adams, L. C. A1 - Onthank, D. A1 - Thöne-Reineke, C. A1 - Robinson, S. A1 - Ponader, Marco A1 - Weller, Michael G. A1 - Buchholz, R. A1 - Karst, U. A1 - Botnar, R. A1 - Hamm, B. A1 - Makowski, M. R. T1 - Molecular MR-Imaging for Noninvasive Quantification of the Anti-Inflammatory Effect of Targeting Interleukin-1β in a Mouse Model of Aortic Aneurysm N2 - Background: Molecular-MRI is a promising imaging modality for the assessment of abdominal aortic aneurysms (AAAs). Interleukin-1β (IL-1β) represents a new therapeutic tool for AAA-treatment, since pro-inflammatory cytokines are key-mediators of inflammation. This study investigates the potential of molecular-MRI to evaluate therapeutic effects of an anti-IL-1β-therapy on AAA-formation in a mouse-model. Methods: Osmotic-minipumps were implanted in apolipoprotein-deficient-mice (N = 27). One group (Ang-II+01BSUR group, n = 9) was infused with angiotensin-II (Ang-II) for 4 weeks and received an anti-murine IL-1β-antibody (01BSUR) 3 times. One group (Ang-II-group, n = 9) was infused with Ang-II for 4 weeks but received no treatment. Control-group (n = 9) was infused with saline and received no treatment. MR-imaging was performed using an elastin-specific gadolinium-based-probe (0.2 mmol/kg). Results: Mice of the Ang-II+01BSUR-group showed a lower aortic-diameter compared to mice of the Ang-II-group and control mice (p < 0.05). Using the elastin-specific-probe, a significant decrease in elastin-destruction was observed in mice of the Ang-II+01BSUR-group. In vivo MR-measurements correlated well with histopathology (y = 0.34x-13.81, R2 = 0.84, p < 0.05), ICP-MS (y = 0.02x+2.39; R2 = 0.81, p < 0.05) and LA-ICP-MS. Immunofluorescence and western-blotting confirmed a reduced IL-1β-expression. Conclusions: Molecular-MRI enables the early visualization and quantification of the anti-inflammatory-effects of an IL-1β-inhibitor in a mouse-model of AAAs. Responders and non-responders could be identified early after the initiation of the therapy using molecular-MRI. KW - Cardiovascular KW - Molecular-MRI KW - Magnetic resonance imaging KW - Gadolinium-based contrast agent KW - Elastin-specific contrast agent ESMA KW - Gadovist KW - Gadofosveset KW - MR Angiography KW - Inductively Coupled Mass Spectroscopy KW - Element Specific Bioimaging Using Laser Ablation KW - Visualization PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517150 DO - https://doi.org/10.1177/1536012120961875 N1 - Geburtsname von Ponader, Marco: Wilke, M. - Birth name of Ponader, Marco: Wilke, M. VL - 19 SP - 61875 PB - SAGE AN - OPUS4-51715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg T1 - One-Line Monitoring of the Curing Process of FRP N2 - The knowledge of the cure situation during the production process of thermosetting material is of enormous importance. • Mid- and near- infrared (IR) spectroscopy in attenuated total reflectance (ATR) geometry are promising techniques for curing studies. • An IR/THz sensor system was developed to investigate its suitability for future online monitoring of curing processes in the production line. T2 - BESSY@HZB User Meeting 2020 CY - Online meeting DA - 10.12.2020 KW - Fiber Reinforced Polymers KW - Curing Monitoring KW - Attenuated Total Reflectance PY - 2020 AN - OPUS4-51804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Understanding distributed data – a semantic web approach for data based analysis of NDT data in civil engineering N2 - In the field of non-destructive testing (NDT) in civil engineering, a large number of measurement data are collected. Although they serve as a basis for scientific analyses, there is still no uniform representation of the data. An analysis of various distributed data sets across different test objects is therefore only possible with high manual effort. We present a system architecture for an integrated data management of distributed data sets based on Semantic Web technologies. The approach is essentially based on a mathematical model - the so-called ontology - which represents the knowledge of our domain NDT. The ontology developed by us is linked to data sources and thus describes the semantic meaning of the data. Furthermore, the ontology acts as a central concept for database access. Non-domain data sources can be easily integrated by linking them to the NDT construction ontology and are directly available for generic use in the sense of digitization. Based on an extensive literature research, we outline the possibilities that this offers for NDT in civil engineering, such as computer-aided sorting, analysis, recognition and explanation of relationships (explainable AI) for several million measurement data. The expected benefits of this approach of knowledge representation and data access for the NDT community are an expansion of knowledge through data exchange in research (interoperability), the scientific exploitation of large existing data sources with data-based methods (such as image recognition, measurement uncertainty calculations, factor analysis, material characterization) and finally a simplified exchange of NDT data with engineering models and thus with the construction industry. Ontologies are already the core of numerous intelligent systems such as building information modeling or research databases. This contribution gives an overview of the range of tools we are currently creating to communicate with them. T2 - EGU General Assembly 2020 CY - Online meeting DA - 04.05.2020 KW - Ontology KW - NDT KW - Concrete KW - Onotology KW - Semantic Data Management KW - Reproducible Science PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518076 DO - https://doi.org/10.5194/egusphere-egu2020-19332 AN - OPUS4-51807 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Daten verständlich machen mit einem Semantic Web basierten Ansatz für die ZfP im Bauwesen N2 - Im Bereich der Zerstörungsfreien Prüfung (ZfP) im Bauwesen werden eine Vielzahl von Messdaten erfasst. Obwohl Sie als Grundlage für wissenschaftliche Analysen dienen, gibt es noch keine einheitliche Repräsentation der Daten. Eine Analyse verschiedener verteilter Datensätze über unterschiedliche Prüfobjekte hinweg ist daher kaum möglich. Wir stellen einen Ansatz für ein integriertes Datenmanagement verteilter Datensätze auf Basis von Semantic-Web Technologien vor. Der Ansatz basiert im Kern auf einem mathematischen Modell – der sogenannten Ontologie – welches das Wissen unserer Domäne ZfPBau repräsentiert. Die von uns entwickelte ZfPBau Ontologie wird mit Datenquellen verknüpft und beschreibt so die semantische Bedeutung der Daten. Darüber hinaus fungiert die Ontologie als zentrales Konzept für den Datenbankzugriff. Domänen-fremde Datenquellen können durch die Verknüpfung mit der ZfPBau Ontologie einfach integriert werden und stehen zur generischen Nutzung im Sinne der Digitalisierung direkt zur Verfügung. Basierend auf einer umfangreichen Literaturrecherche, skizzieren wir die Möglichkeiten die sich daraus für die ZfP im Bauwesen ergeben, wie zum Beispiel Messdaten computergestützt zu sortieren, zu analysieren, Zusammenhänge zu erkennen und zu erklären. Der erwartete Nutzen dieses Ansatzes der Wissensrepräsentation und des Datenzugriffs für die ZfP-Community ist eine Erweiterung des Wissens durch Datenaustausch in der Forschung (Interoperabilität), die wissenschaftliche Verwertung großer existierender Datenquellen mit datenbasierten Verfahren (wie Bilderkennung, Messunsicherheitsberechnungen, Faktoranaylsen, Materialcharackterisierung) und letztlich ein vereinfachter Transfer von ZFP-Daten in Ingenieurmodelle und somit in die Baupraxis. Ontologien sind bereits Kern vielzähliger intelligenter Systeme wie Building-Information-Modeling oder Forschungsdatenbanken. Der Beitrag gibt einen Überblick über die Werkzeuge die wir derzeit für die Kommunikation mit ihnen schaffen. T2 - Seminar ZfP 4.0 Die ZfP im Zeichen der Digitalisierung CY - Frankfurt am Main, Germany DA - 08.10.2020 KW - Ontologien KW - Semantisches Datenmanagement KW - Reproduzierbare Wissenschaft PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518092 AN - OPUS4-51809 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Laser induced gas breakdown in reactive mixtures containing halides of boron and silicon: diagnostics and modeling N2 - We run two pilot LIP experiments in reactive gas mixtures. First, LIP is excited in BCl3 or BF3 plus H2 or CH4 to evaluate the efficiency of deposition of solid boron and boron carbide, materials that are largely used for refractory coatings. Second, we investigate a possibility of synthesis of fluorochlorosilanes SiFxCl4-x (x = 1, 2, 3) by LIP induced in SiF4+SiCl4 gas mixtures. Using fluorochlorosilanes with different combinations of F and Cl in the SiFxCly molecule may add flexibility in processes of silicon deposition and etching. The gases used and solid deposits are analyzed by optical emission spectroscopy (OES) and IR and mass spectrometry (MS). We also model the laser induced plasma by performing static equilibrium chemistry calculations to see whether desired reaction products are thermodynamically favorable and dynamic calculations of the expanding plasma plume to see how and where the products form. T2 - International Workshop on Laser Induced breakdown Spectroscopy CY - Online meeting DA - 01.12.2020 KW - Silicon halides KW - Chemical vapor deposition KW - Laser induced dielectric breakdown KW - Hydrogen reduction PY - 2020 AN - OPUS4-51725 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Bohling, Christian A1 - Wilsch, Gerd T1 - New possibilities for concrete analysis 4.0 with the Laser-Induced Breakdown Spectroscopy (LIBS) N2 - In civil engineering the damage assessment of concrete infrastructures is an important task to monitor and ensure the estimated life-time. The aging of concrete is caused by different damage processes like the chloride induced pitting corrosion of the reinforcement. The penetration depth and the concentration of harmful species are crucial factors in the damage assessment. As a highly cost and time-consuming standard procedure, the analysis of concrete drill cores or drilling by wet-chemistry is widely used. This method provides element concentration to the total mass as aggregates and binder are homogenized. In order to provide a method that is capable to detect the element concentration regarding the cement content only, the laser-induced breakdown spectroscopy (LIBS) will be presented. The LIBS method uses a focused pulsed laser on the sample surface to ablate material. The high-power density and the laser-material interaction causes a laser-induced plasma that emits elemental and molecular line emission due to energy transition of the excited species in the plasma during the cooling phase. As each element provides element-specific line emission, it is in principle possible to detect any element on the periodic table (spectroscopic fingerprint) with one laser shot. In combination with a translation stage the sample under investigation can be spatially resolved using a scan raster with a resolution up to 100 µm (element mapping). Due to the high spatial resolution, the element distribution and the heterogeneity of the concrete can be evaluated. By using chemometrics the non-relevant aggregates can be excluded from the data set and the element concentration can be quantified and referred to a specific solid phase like the binding matrix (cement) only. In order to analyze transport processes like diffusion and migration the twodimensional element distributions can provide deep insight into the transport through the pore space and local enrichments of elements. As LIBS is a multi-elemental method it is also possible to compare the ingress and transport process of different elements like Cl, Na, K, S, C, and Li simultaneously and evaluate cross-correlations between the different ions. Furthermore, the element mapping allows to visualize the transport along cracks. This work will show the state of the art in terms of hardware and software for an automated LIBS system as well as different application for a concrete analysis 4.0. Focus will be the application of LIBS for a fast concrete analysis. T2 - SMAR 2019 CY - Potsdam, Germany DA - 27.08.2019 KW - Damage KW - LIBS KW - Concrete KW - Mapping KW - Chlorine PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517282 UR - https://www.ndt.net/?id=24963 SN - 1435-4934 VL - 25 IS - 1 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-51728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Olivera, Paulo A1 - Michalchuk, Adam A1 - de Oliveira Guilherme Buzanich, Ana A1 - Bienert, Ralf A1 - Torresi, R. A1 - Camargo, P. A1 - Emmerling, Franziska T1 - Tandem X-ray absorption spectroscopy and scattering for in situ time-resolved monitoring of gold nanoparticle mechanosynthesis N2 - Current time-resolved in situ approaches limit the scope of mechanochemical investigations possible. Here we develop a new, general approach to simultaneously follow the evolution of bulk atomic and electronic structure during a mechanochemical synthesis. This is achieved by coupling two complementary synchrotron-based X-ray methods: X-ray absorption spectroscopy (XAS) and X-ray diffraction. We apply this method to investigate the bottom-up mechanosynthesis of technologically important Au micro and nanoparticles in the presence of three different reducing agents, hydroquinone, sodium citrate, and NaBH4. Moreover, we show how XAS offers new insight into the early stage generation of growth species (e.g. monomers and clusters), which lead to the subsequent formation of nanoparticles. These processes are beyond the detection capabilities of diffraction methods. This combined X-ray approach paves the way to new directions in mechanochemical research of advanced electronic materials. KW - Mechanochemistry KW - XANES KW - X-ray diffraction KW - Nano particles PY - 2020 DO - https://doi.org/10.1039/d0cc03862h SN - 1364-548X VL - 56 SP - 10329 EP - 10332 PB - Royal Society of Chemistry AN - OPUS4-51760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Cios, G. A1 - Tokarski, T. A1 - Mansfeld, Ulrich A1 - Ortel, Erik A1 - Mielke, Johannes A1 - Pellegrino, F. A1 - Maurino, V. T1 - Towards 3D Understanding of Non-spherical Nanoparticles by Transmission Kikuchi Diffraction (TKD) for Improved Particle Size Distribution by Electron Microscopy N2 - In this paper one refined approach is applied to determine the exact orientation of bipyramidal TiO2 nanoparticles prepared with good dispersion as almost isolated particles on a carbon TEM grid. The advantages of the recently developed high-throughput Transmission Kikuchi Diffraction (TKD) are used to identify quickly and reliably the geometrical orientation of the crystalline TiO2 nanoparticle bipyramids (anatase) on a statistically relevant number of particles. KW - Nanoparticles KW - Transmission Kikuchi Diffraction (TKD) KW - Electron microscopy KW - TiO2 KW - 3D PY - 2020 DO - https://doi.org/10.1017/S1431927620013999 VL - 26 IS - S2 SP - 260 EP - 261 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kepes, E. A1 - Gornushkin, Igor B. A1 - Pořízka, P. A1 - Kaiser, J T1 - Spatiotemporal spectroscopic characterization of plasmas induced by non-orthogonal laser ablation N2 - Ablation geometry significantly affects the plasma parameters and the consequent spectroscopic observations in laser-induced breakdown spectroscopy. Nevertheless, plasmas induced by laser ablation under inclined incidence angles are studied to a significantly lesser extent compared to plasmas induced by standard orthogonal ablation. However, inclined ablation is prominent in stand-off applications, such as the Curiosity Mars rover, where the orthogonality of the ablation laser pulse cannot be always secured. Thus, in this work, we characterize non-orthogonal ablation plasmas by applying plasma imaging, tomography, and spectral measurements. We confirm earlier observations according to which non-orthogonal ablation leads to a laser-induced plasma that consists of two distinct parts: one expanding primarily along the incident laser pulse and one expanding along the normal of the sample surface. Moreover, we confirm that the former emits mainly continuum radiation, while the latter emits mainly sample-specific characteristic radiation. We further investigate and compare the homogeneity of the plasmas and report that inclined ablation affects principally the ionic emissivity of laser-induced plasmas. Overall, our results imply that the decreased fluence resulting from inclined angle ablation and the resulting inhomogeneities of the plasmas must be considered for quantitative LIBS employing non-orthogonal ablation. KW - Radon transformation KW - Laser induced plasma KW - Plasma tomography PY - 2020 DO - https://doi.org/10.1039/d0an01996h VL - 146 IS - 3 SP - 920 EP - 929 PB - The Royal Society of Chemistry AN - OPUS4-51774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bäßler, Ralph T1 - Rezension: Einführung in die Physikalische Chemie N2 - Unabhängig vom im Chemieunterricht erworbenen Wissensstand der Studienanfänger liefert dieses, in der Reihe „De Gruyter Studium“ erschienene Lehrbuch einen Einstieg in die Physikalische Chemie. Basierend auf den Erfahrungen seiner Lehrtätigkeit für Erstsemester der Fachrichtung Chemie an der Universität des Saarlandes geht der Autor auf beinahe alle Themengebiete der Physikalischen Chemie ein, wobei die Schwerpunkte auf klassischer Thermodynamik und Grundlagen der chemischen Bindung liegen. Dieses Lehrbuch ist nicht nur für Studierende im Bachelorstudium der Chemie sowohl im Haupt‐ als auch im Nebenfach geeignet. Es liefert zudem Interessierten anderer Fachrichtungen einen übersichtlichen und verständlichen Einstieg in die komplexe Welt der Physikalischen Chemie und sorgt für ein Grundverständnis. KW - Elektrochemie PY - 2020 DO - https://doi.org/10.1002/maco.202070126_2 SN - 1521-4176 SN - 0947-5117 VL - 71 IS - 12 SP - 3 EP - 4 PB - WILEY‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-51779 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan T1 - You Ask – ACEnano Replies N2 - The workshop starts with introductory information about the workshop and the H2020 project ACEnano, followed by two expert round tables, focussing on how the project could address regulator and industry needs, respectively. This is be followed by parallel sessions on tools (based on preferences expressed by those registered to attend, see “Questions”) and finally a question-and-answer session with the attendees. The experts invited in Round Table 1 have been prepared to answer to questions related to obstacles and advantages for stakeholders such as SMEs to use the ACEnano approaches/tools. Standardisation needs are discussed. T2 - nanoSafety Cluster Training (NSC) Day @ NanoSAFE 2020: ACEnano users’ workshop “You Ask – ACEnano Replies” CY - Online meeting DA - 23.11.2020 KW - ACEnano KW - Standardisation KW - Nanomaterials KW - Nano-characterisation PY - 2020 UR - https://www.nanosafetycluster.eu/ SP - 1 EP - 2 AN - OPUS4-51693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bennet, Francesca T1 - Towards a method for quantitative evaluation of nanoparticles in suspension via Microprinting and SEM analysis N2 - A series of different nanoparticle suspensions (Gold, Latex, and SiO2 in varying concentrations) were microprinted onto TEM grids in a 4 x 4 array in the concentration range 7x10^8 to 1x10^11 NP/mL and imaged with SEM and TSEM. Concentrations and printing conditions (temperature, relative humidity) were varied in order to minimize the coffee ring effect. T2 - nanoSAFE 2020 CY - Online meeting DA - 16.11.2020 KW - Nanoparticles KW - Microprinting KW - Image analysis PY - 2020 AN - OPUS4-51699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steglich, P. A1 - Mai, C. A1 - Bondarenko, S. A1 - Paul, Martin A1 - Weller, Michael G. A1 - Schrader, S. A1 - Mai, A. T1 - BioPIC - Integration of Biosensors based on Photonic Integrated Circuits by Local-Backside Etching N2 - Silicon photonic sensors are promising candidates for lab-on-a-chip solutions with versatile applications and scalable production prospects using complementary metal-oxide semiconductor (CMOS) fabrication methods. However, the widespread use has been hindered because the sensing area adjoins optical and electrical components making packaging and sensor handling challenging. In this work, a local back-side release of the photonic sensor is employed, enabling a separation of the sensing area from the rest of the chip. This approach allows preserving the compatibility of photonic integrated circuits in the front-end of line and metal interconnects in the back-end of line. T2 - ATTRACT online Conference CY - Online meeting DA - 22.09.2020 KW - Silicon Photonics KW - Photonic Sensor KW - Photonic Integrated Circuits KW - Point-Of-Care-Diagnostics KW - CMOS KW - Microfluidics KW - Lab-on-a-chip KW - Ring resonator PY - 2020 UR - https://attract-eu.com/showroom/project/integration-of-biosensors-based-on-photonic-integrated-circuits-by-local-backside-etching-biopic/ SP - 1 EP - 5 AN - OPUS4-51735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keller, S. A1 - Borde, T. A1 - Brangsch, J. A1 - Reimann, C. A1 - Kader, A. A1 - Schulze, D. A1 - Buchholz, R. A1 - Kaufmann, Jan Ole A1 - Karst, U. A1 - Schellenberger, E. A1 - Hamm, B. A1 - Makowski, M. R. T1 - Assessment of the hepatic tumor extracellular matrix using elastin‑specific molecular magnetic resonance imaging in an experimental rabbit cancer model N2 - To investigate the imaging performance of an elastin-specific molecular magnetic resonance imaging (MRI) probe with respect to the extracellular matrix (ECM) in an experimental hepatic cancer model. Twelve rabbits with hepatic VX2 tumors were examined using 3 T MRI 14, 21, and 28 days after tumor implantation for two subsequent days (gadobutrol, day 1; elastin-specific probe, day 2). The relative enhancement (RE) of segmented tumor regions (central and margin) and the peritumoral matrix was calculated using pre-contrast and delayed-phase T1w sequences. MRI measurements were correlated to histopathology and element-specific and spatially resolved mass spectrometry (MS). Mixed-model analysis was performed to assess the performance of the elastin-specific probe. In comparison to gadobutrol, the elastin probe showed significantly stronger RE, which was pronounced in the tumor margin (day 14–28: P ≤ 0.007). In addition, the elastin probe was superior in discriminating between tumor regions (χ2(4) = 65.87; P < 0.001). MRI-based measurements of the elastin probe significantly correlated with the ex vivo elastinstain (R = .84; P <0 .001) and absolute gadolinium concentrations (ICP-MS: R = .73, P <0 .01). LA-ICP-MS imaging confirmed the colocalization of the elastin-specific probe with elastic fibers. Elastin-specific molecular MRI is superior to non-specific gadolinium-based contrast agents in imaging the ECM of hepatic tumors and the peritumoral tissue. KW - Elastin-specific molecular agent KW - Extracellular matrix KW - Hepatocellular carcinoma KW - Inductively coupled plasma mass spectroscopy KW - Laser ablation-inductively coupled plasma-mass spectrometry KW - Magnetic resonance imaging KW - MR imaging KW - ESMA KW - Gadolinium PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517360 DO - https://doi.org/10.1038/s41598-020-77624-8 VL - 10 IS - 1 SP - 20785 PB - Nature AN - OPUS4-51736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von Boehn, B. A1 - Scholtz, Lena A1 - Imbihl, R. T1 - Reactivity and Stability of Ultrathin VOx Films on Pt(111) in Catalytic Methanol Oxidation N2 - The growth of ultrathin layers of VOx (<12 monolayers) on Pt(111) and the activity of these layers in catalytic methanol oxidation at 10−4 mbar have been studied with low-energy electron difraction, Auger electron spectroscopy, rate measurements, and with photoemission electron microscopy. Reactive deposition of V in O2 at 670 K obeys a Stranski–Krastanov growth mode with a (√3 × √3)R30° structure representing the limiting case for epitaxial growth of 3D-VOx. The activity of VOx/Pt(111) in catalytic methanol oxidation is very low and no redistribution dynamics is observed lifting the initial spatial homogeneity of the VOx layer. Under reaction conditions, part of the surface vanadium difuses into the Pt subsurface region. Exposure to O2 causes part of the V to difuse back to the surface, but only up to one monolayer of VOx can be stabilized in this way at 10−4 mbar. KW - Vanadium oxide catalysts KW - Pt(111) KW - Supported catalyst KW - Methanol oxidation KW - Stranski–Krastanow growth PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517376 DO - https://doi.org/10.1007/s11244-020-01321-z SN - 1022-5528 VL - 63 IS - 15-18 SP - 1545 EP - 1556 PB - Springer AN - OPUS4-51737 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fittschen, U. A1 - Lutz, C. T1 - Element Species Determination in Polymer Electrolyte Membranes N2 - Polymer electrolyte membranes (PEM) are polymers which act as separator in an electrochemical cell and allow ionic charge flow to close the circuit. Widely used membranes are perfluorinated sulfonic-acid (PFSA) ionomers (e.g. Nafion™), a class of ion-conducting polymers with remarkable ion conductivity and chemical-mechanical stability. A nanoscopic water system around the sulfonic acid capped side-chains of the otherwise hydrophobic polymer allows the ion transport. Only approx. 14 molecules of water per sulfonic group are present in the fully hydrated state. In vanadium redox flow batteries (VRFB) ideally only protons are transported. The weak ion selectivity of Nafion™ is the main cause for the transportation of vanadium, briefly vanadium crossover, in VRFBs a system we have investigated more closely, lately. The consequences of crossover are a concentration imbalance and a self-discharge of the battery, which leads to a decrease of the capacity. The development of efficient energy storage systems is crucial for the transformation towards a renewable energy based economy. The VRFB has a great potential as a commercial electrochemical energy storage system due to properties including, but not limited to, no cross-contamination, a long cycle-life and a theoretically unlimited capacity. VRFB consists of two half-cells, which are linked to electrolyte tanks and separated by a membrane. The membrane plays a major role in overall cell performance. So far, vanadium transportation models, which include diffusion, migration, electroosmotic convection and pressure gradients, are inconsistent. There is no agreement in the literature on the diffusion coefficients of vanadium species (e.g. published diffusion coefficients of V2+ are located between 3.13·10-12 m²s-1 and 9.44·10-12 m²s-1) indicate that thevanadium crossover is not well understood and there is a lack on a more fundamental level. Since the membrane transport is the rate-determining step of the crossover as well as of the proton exchange it is extremely important to understand these phenomena on a fundamental level. This will eventually allow us to design better membranes. Alternative materials need to show equivalent performance compared with Nafion™ and ideally be more selective regarding ion cross-membrane transport.There are several options to approach the chemistry i.e. the interaction of dissolved and bound ions inside the confined water body of ionomeric membranes. Vanadium ions are a versatile model as UV/VIS data can be used to distinguish between the 5 species V2+, V3+, VO2+, VO2+ and V2O33+ of the electrolyte. Infrared spectroscopy has been applied to study the interaction of sulfonic groups and the ions. Molecular dynamic modeling is another approach to study the distribution and distances of ions. We now introduce X-ray absorption near edge structure spectroscopy (XANES) to study species and species changes inside Nafion™ and a novel membrane based on poly(1,1-difluoroethylene) (PVDF). We evaluated the methods and investigated the influence of irradiation, temperature and hydration on the measurements. T2 - Denver X-Ray Conference CY - Online meeting DA - 03.08.2020 KW - Batteries KW - BAMline KW - XANES PY - 2020 AN - OPUS4-51910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fittschen, U. T1 - Improving surface sensitive XRF using ink jet printing and information from the angle dependent signal N2 - Total Reflection X-ray Fluorescence (TXRF) is a small footprint, ressource efficient micro-analytical tool for trace elemental determination. However, depending on the matrix TXRF is also challenging in several ways: the preparation of a representative aliquot maybe difficult for slurries, shading effects and matrix effects may occur and the applicability of an IS maybe hampered by interferences (fitting may be impaired as well) or inhomogeneities. It is therefore crucial to understand and if applicable mitigate the influence of the before mentioned phenomena. We have used the small volume approach using pL droplets to study shading in TXRF previously.Using this approach thin specimens in a favorable geometry are prepared with a well defined morphology; this way minimizing matrix effects and shading. To be used as standard it is also necessary to determine the delivered elemental amounts. Here we will present on the performance of a commercial ink-jet printer cartridge to deliver defined volumes and elemental amounts. The microscopic specimens obtained have been successfully applied to determine relative sensitivities in TXRF and prepare references to study coded apertures in grazing incidence full field micro-XRF.The homogeneous lateral distribution of analyte and IS may be probed by micro-XRF, to obtain information on alikeness of analyte and IS. To study the alikeness of the in depth distribution (film-like or particle-like) angle scans can deliver valuable data. Here we present first results on angle scans using a prototype GIXRF set up and a commercial TXRF instrument. T2 - Denver X-Ray Conference CY - Online meeting DA - 03.08.2020 KW - TXRF KW - Coded Aperture PY - 2020 AN - OPUS4-51913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - ZfP 4.0: Neue Herausforderungen für die Mensch-Maschine-Interaktion N2 - Im Zeitalter von Industrie 4.0 muss die zerstörungsfreie Prüfung (ZfP) mit den Anforderungen Schritt halten. Die erfolgreiche Umsetzung von Digitalisierung, Automatisierung, komplexer Vernetzung, künstlicher Intelligenz, Assistenzsystemen, intelligenten Sensortechnologien usw. hängt stark mit einer erfolgreichen und optimalen Mensch-Maschine-Interaktion (MMI) zusammen. In der ZfP 4.0 wird sich die Rolle des Prüfers zum flexiblen Problemlöser und Entscheider verändern. Dieser Wandel wird andere Anforderungen an die Prüfer stellen und eine andere Organisation der Prüfung, Ausbildung etc. erfordern. Der Mensch wird also weiterhin im Mittelpunkt der ZfP stehen. Zu den Herausforderungen, die dieser Wandel mit sich bringen wird, gehören das Vertrauen in automatisierte Systeme und die Akzeptanz neuer Technologien, für die Wege gefunden werden müssen, um sie zu bewältigen. T2 - DGZfP AK Zwickau-Chemnitz CY - Zwickau, Germany DA - 28.01.2020 KW - Mensch-Maschine-Interaktion KW - Zerstörungsfreie Prüfung (ZfP) KW - Industrie 4.0 KW - ZfP 4.0 PY - 2020 AN - OPUS4-51918 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - Reliability in NDT and the influence of human factors N2 - This presentation offers a holistic view on the assessment of reliability of NDT including the intrinsic reliability (typically expressed in terms of probability of detection (POD) curves), application, human and organisational factors. In addition to POD, advanced methods such as multiparameter POD, volume POD and POD for combined data are presented. Human and organisational factors in NDT require a systematic approach, i.e. it is not just the individual that determines how the inspections are carried out but also the interactions of individuals with the technology, team, organisation and the extra-organisational environment. Lessons learned from the literature as well as from own studies are presented. T2 - DFG SHM Netzwerk CY - Berlin, Germany DA - 27.01.2020 KW - Human Factors KW - Non-destructive testing (NDT) KW - Reliability PY - 2020 AN - OPUS4-51919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Chemometrics for the analysis of cement-based materials N2 - The analysis of the chemical composition of cement-based materials like concrete is a crucial task in civil engineering. Concrete is a multi-phase material made of cement, water, aggregates, additives and admixtures. During the damage assessment of concrete structures, the external ingress of harmful species like chlorine, alkalis or sulfates needs to be determined. In order to provide a fast and precise analysis of concrete the application of LIBS offers unique possibilities as the technique can detect all elements at air atmosphere. To determine the condition of concrete, the information about the chemical composition, the ingress of harmful species as well as the evaluation of characteristic values like the used cement type or the type of aggregates are needed. This work presents the two-dimensional evaluation of concrete samples using LIBS and multivariate data analysis of atomic and molecular emission. For the evaluation of the main components different classification methods will be applied to identify the heterogeneity of the samples. With respect to their specific phase, different species will be quantified using multivariate regression (PLS) and important figures of merit will be presented. All results will be verified using Standard procedure of wet chemistry (XRF, potentiometric titration and ICP-OES). T2 - 10th Euro-Mediterranean Symposium CY - Brno, Czech Republic DA - 08.09.2019 KW - Heterogeneous material KW - Chemometics KW - Cement KW - Concrete PY - 2019 AN - OPUS4-51838 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Raysyan, Anna A1 - Moerer, R. A1 - Coesfeld, Bianca A1 - Eremin, S. A1 - Schneider, Rudolf T1 - Fluorescence polarization immunoassay for the determination of diclofenac in wastewater N2 - Pharmacologically active compounds are often detected in wastewater and surface waters. The nonsteroidal anti-inflammatory drug diclofenac (DCF) was included in the European watch list of substances that requires its environmental monitoring in the member states. DCF may harmfully influence the ecosystem already at concentrations ≤ 1 μg L−1. The fast and easy quantification of DCF is becoming a subject of global importance. Fluorescence polarization immunoassay (FPIA) is a homogeneous mix-and-read method which does not require the immobilization of reagents. FPIA can be performed in one phase within 20–30 min, making it possible to analyse wastewater without any complicated pre-treatment. In this study, new tracermolecules with different structures, linking fluorophores to derivatives of the analyte, were synthesized, three homologous tracers based on DCF, two including a C6 spacer, and one heterologous tracer derived from 5-hydroxy-DCF. The tracer molecules were thoroughly assessed for performance. Regarding sensitivity of the FPIA, the lowest limit of detection reached was 2.0 μg L−1 with a working range up to 870 μg L−1. The method was validated for real wastewater samples against LC-MS/MS as reference method with good agreement of both methods. KW - Abwasser KW - Umweltschadstoffe KW - Antikörper KW - Antibody PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518398 DO - https://doi.org/10.1007/s00216-020-03058-w SN - 1618-2642 VL - 413 IS - 4 SP - 999 EP - 107 PB - Springer CY - Heidelberg AN - OPUS4-51839 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Immunoanalytical platforms for on-site environmental health and food safety testing N2 - An overview of methods developed in the division. T2 - FoodSmartphone.eu - Online Symposium CY - Online meeting DA - 25.11.2020 KW - Umweltanalytik KW - Lebensmittelanalytik KW - Immunoassay KW - Biosensor PY - 2020 AN - OPUS4-51841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pignatelli, Giuseppe T1 - Optical Sensor for Monitoring Quality of 3D Metal Printing N2 - Additive Manufacturing (AM) becomes widespread in many technological fields including the precise machining of steel. To assure quality of final products, thorough monitoring of online process is required. We test several monitoring techniques during the AM printing to quickly detect and possibly correct flaws while building a workpiece. Here we show how optical emission spectroscopy can be used to recognize defects that are artificially introduced on a steel printing substrate. T2 - Scix 2020 CY - Online meeting DA - 12.10.2020 KW - Additive manufacturing KW - Spectroscopy KW - Analytical chemistry PY - 2020 AN - OPUS4-51858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Explore and Exploit - Strategische Erweiterung der fraktographischen Datenbank mit Machine Learning N2 - In diesem Vortrag stellen wir den aktuellen Stand zu einer Masterarbeit zusammen die sich mit dem Thema beschäftigt wie die Generalisierbarkeit von Datenmodellen auf Basis kleiner Datensätze erhöht werden kann. Wir stellen vor, wie die Datenbasis eines fraktogafischen Bildklassifizierers mit einem statistischen Model strategische erweitert, bzw. an eine Anwendung angepasst werden kann. T2 - AG Fraktographie im DVM/DGM Gemeinschaftsausschuss „Rasterelektronenmikroskopie in der Materialprüfung“ CY - Online meeting DA - 20.11.2020 KW - Bild Klassifizierung KW - Small Data KW - Unsicherheitsberechnung KW - Erklärbare KI PY - 2020 AN - OPUS4-51810 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Prospects and challenges of data-driven NDT - current work in junior research group 8.K N2 - We have arrived in the data age. But why is it so difficult for the NDT community to achieve real breakthroughs with data-driven science? In this seminar, we will take a brief look at the evolution of mainstream data science to understand why the most exciting times are perhaps just ahead. We will give an overview of our activities in the junior research group 8.K which are aimed at enabling the next generation of data science methods in NDT. The seminar addresses the two main work fields of our group: semantic data management and the handling of limited data resources. The first field addresses the problem that a uniform representation of our data is not yet available. However, knowledge creation in data science - whose main contribution lies in the analysis of distributed resources - requires common data access based on a collective understanding. To achieve this, we present an ontology-based approach. Ontologies are already the core of many intelligent systems such as building information models or research databases. We summarize some of the basic principles of this technology and describe our approach to create an NDT ontology. The second field ties in with the first and addresses the application of data-based methods in engineering practice. Especially in the field of non-destructive testing many successful applications have been published. In most cases, however, the creation of referenced data is extremely expensive and therefore much sparser than in other research areas. As a result, the available data may cover only one scenario, so that common benchmarks often do not reflect the actual performance of the model in practical applications. Estimates that quantify the transferability from one scenario to another are not only necessary to overcome this challenge - they also prove to be a powerful tool for the strategic expansion of what we consider knowledge. T2 - Abteilungsseminar der Abteilung 8 CY - Online meeting DA - 18.11.2020 KW - Machine Learning KW - Small Data KW - Semantic Web KW - Materials Discovery KW - Explainable AI PY - 2020 AN - OPUS4-51811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Artificial intelligence in NDT (AI NDT) a networking workshop N2 - Data-driven research is considered the new paradigm in science. In this field, data is the new resource from which knowledge is extracted that is too complex for traditional methods. Several factors such as national funding and advances in information technology, are driving the development. In particular, the creation of databases and the analysis of data with artifical intelligence are playing an important role in establishing the new paradigm. However, there are numerous challenges that must be overcome to realize the full potential of data-driven methods. This talk sets the stage for the upcoming workshop by reviewing some of the historical developments and the current state of data-driven science in NDT and materials science. T2 - Workshop on Artificial Intelligence in NDT (AI-NDT) CY - Online meeting DA - 30.10.2020 KW - Data Science KW - Materials Informatics KW - NDT PY - 2020 AN - OPUS4-51812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sanabria, S. J. A1 - Baensch, Franziska A1 - Zauner, M. A1 - Niemz, P. T1 - In‑situ quantification of microscopic contributions of individual cells to macroscopic wood deformation with synchrotron computed tomography N2 - Wood-based composites hold the promise of sustainable construction. Understanding the influence on wood cellular microstructure in the macroscopic mechanical behavior is key for engineering highperformance composites. In this work, we report a novel Individual Cell Tracking (ICT) approach for in-situ quantification of nanometer-scale deformations of individual wood cells during mechanical loading of macroscopic millimeter-scale wood samples. Softwood samples containing > 104 cells were subjected to controlled radial tensile and longitudinal compressive load in a synchrotron radiation micro-computed tomography (SRμCT) setup. Tracheid and wood ray cells were automatically segmented, and their geometric variations were tracked during load. Finally, interactions between microstructure deformations (lumen geometry, cell wall thickness), cellular arrangement (annual growth rings, anisotropy, wood ray presence) with the macroscopic deformation response were investigated. The results provide cellular insight into macroscopic relations, such as anisotropic Poisson effects, and allow direct observation of previously suspected wood ray reinforcing effects. The method is also appropriate for investigation of non-linear deformation effects, such as buckling and deformation recovery after failure, and gives insight into less studied aspects, such as changes in lumen diameter and cell wall thickness during uniaxial load. ICT provides an experimental tool for direct validation of hierarchical mechanical models on real biological composites. KW - Wood materials KW - Micro-comuted tomography (µCT) KW - Individual cell tracking KW - Stress-strain behaviour PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518157 DO - https://doi.org/10.1038/S41598-020-78028-4 SN - 2045-2322 VL - 10 SP - 1 EP - 16 PB - Springer nature AN - OPUS4-51815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Surov, A. A1 - Vasilev, N. A1 - Voronin, A. A1 - Churakov, A. A1 - Emmerling, Franziska A1 - Perlovich, G. T1 - Ciprofloxacin salts with benzoic acid derivatives: structural aspects, solid-state properties and solubility performance N2 - n this work, three new pharmaceutical hydrated salts of ciprofloxacin with selected derivatives of benzoic acid, namely 4-hydroxybenzoic acid, 4-aminobenzoic acid and gallic acid, were obtained and systematically investigated by several solid-state analytical techniques. In situ Raman spectroscopy was applied to elucidate the alternative pathways of the solid forms' formation under mechanochemical conditions. Crystal structure analysis and a CSD survey allowed us to establish a distinct supramolecular motif formed by infinite columnar stacks of ciprofloxacin dimers arranged in the “head-to-tail” manner. An alternative “head-to-head” packing arrangement was only observed in the crystal of the hydrated ciprofloxacin salt with 4-aminobenzoic acid. In addition, the pH-solubility behavior of the solid forms was thoroughly investigated. Furthermore, a distinct structure–property relationship between the specific features of the supramolecular organization of the hydrated salts and their solubility was observed and discussed. KW - Mechanochemistry KW - XRD PY - 2020 DO - https://doi.org/10.1039/D0CE00514B VL - 22 IS - 25 SP - 4238 EP - 4249 AN - OPUS4-51818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Opitz, P. A1 - Asta, M. A1 - Fernandez-Martinez, A. A1 - Panthöfer, M. A1 - Kabelitz, Anke A1 - Emmerling, Franziska A1 - Mondeshki, M. A1 - Tremel, W. T1 - Monitoring a Mechanochemical Syntheses of Isostructural Luminescent Cocrystals of 9-Anthracenecarboxylic Acid with two Dipyridines Coformers N2 - Amorphous calcium carbonate (ACC) is an important precursor in the biomineralization of crystalline CaCO3. In nature, it serves as a storage material or as a permanent structural element, whose lifetime is regulated by an organic matrix. The relevance of ACC in materials science is primarily related to our understanding of CaCO3 crystallization pathways and CaCO3/(bio)polymer nanocomposites. ACC can be synthesized by liquid–liquid phase separation, and it is typically stabilized with macromolecules. We have prepared ACC by milling calcite in a planetary ball mill. Phosphate “impurities” were added in the form of monetite (CaHPO4) to substitute the carbonate anions, thereby stabilizing ACC by substitutional disorder. The phosphate anions do not simply replace the carbonate anions. They undergo shear-driven acid/base and condensation reactions, where stoichiometric (10%) phosphate contents are required for the amorphization to be complete. The phosphate anions generate a strained network that hinders ACC recrystallization kinetically. The amorphization reaction and the structure of BM-ACC were studied by quantitative Fourier transform infrared spectroscopy and solid state 31P, 13C, and 1H magic angle spinning nuclear magnetic resonance spectroscopy, which are highly sensitive to symmetry changes of the local environment. In the first—and fast—reaction step, the CO32– anions are protonated by the HPO42– groups. The formation of unprecedented hydrogen carbonate (HCO3–) and orthophosphate anions appears to be the driving force of the reaction, because the phosphate group has a higher Coulomb energy and the tetrahedral PO43– unit can fill space more efficiently. In a competing second—and slow—reaction step, pyrophosphate anions are formed in a condensation reaction. No pyrophosphates are formed at higher carbonate contents. High strain leads to such a large energy barrier that any reaction is suppressed. Our findings aid in the understanding of the mechanochemical amorphization of calcium carbonate and emphasize the effect of impurities for the stabilization of the amorphous phases in general. Our approach allowed the synthesis of new amorphous alkaline earth defect variants containing the unique HCO3– anion. Our approach outlines a general strategy to obtain new amorphous solids for a variety of carbonate/phosphate systems that offer promise as biomaterials for bone regeneration. KW - Crystallization KW - Mechanochemistry KW - PDF PY - 2020 DO - https://doi.org/10.1021/acs.cgd.0c00912 VL - 20 IS - 10 SP - 6831 EP - 6846 PB - American Chemical Society AN - OPUS4-51819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Szymoniak, Paulina T1 - Dataset and Jupyter worksheet interpreting the (results from) small- and wide-angle scattering data from a series of boehmite/epoxy nanocomposites. Accompanies the publication "Competition of nanoparticle-induced mobilization and immobilization effects on segmental dynamics of an epoxy-based nanocomposite" N2 - Dataset and Jupyter worksheet interpreting the (results from) small- and wide-angle scattering data from a series of boehmite/epoxy nanocomposites. Accompanies the publication "Competition of nanoparticle-induced mobilization and immobilization effects on segmental dynamics of an epoxy-based nanocomposite", by Paulina Szymoniak, Brian R. Pauw, Xintong Qu, and Andreas Schönhals. Datasets are in three-column ascii (processed and azimuthally averaged data) from a Xenocs NanoInXider SW instrument. Monte-Carlo analyses were performed using McSAS 1.3.1, other analyses are in the Python 3.7 worksheet. Graphics and result tables are output by the worksheet. KW - Small angle scattering KW - X-ray scattering KW - Nanocomposite KW - Polymer nanocomposite KW - Boehmite KW - Analysis KW - SAXS/WAXS PY - 2020 DO - https://doi.org/10.5281/zenodo.4321087 PB - Zenodo CY - Geneva AN - OPUS4-51829 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - The Dark Side of Science N2 - An overview of the dark side of science: what it is, how it occurs, and what you can do to understand it and fight for the light side. T2 - First training event of the ITN-Project GW4SHM CY - Online meeting DA - 23.11.2020 KW - Scientific rigor KW - Scientific misconduct KW - Data manipulation KW - Image manipulation PY - 2020 AN - OPUS4-51830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Rakotondrajoa, A. T1 - Machine learning based quantification of synchrotron radiation-induced X-ray fluorescence measurements - a case study N2 - In this work, we describe the use of artificial neural networks for the quantification of X-ray fluorescence measurements. The training data were generated using Monte Carlo simulation, which avoided the use of adapted reference materials. The extension of the available data set by means of an ANN to generate additional data was demonstrated. Particular emphasis was put on the comparability of simulated and experimental data and how the influence of deviations can be reduced. The search for the optimal hyperparameter, manual and automatic, is also described. For the presented case, we were able to train a network with a mean absolute error of 0.1 weight percent for the synthetic data and 0.7 weight percent for a set of experimental data obtained with certified reference materials. KW - Machine learning KW - BAMline KW - XRF KW - Synchrotron KW - Neural network PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519008 DO - https://doi.org/10.1088/2632-2153/abc9fb SP - 1 EP - 16 PB - IOP Publishing AN - OPUS4-51900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmadi, Samim A1 - Lecompagnon, Julien A1 - Hirsch, Philipp Daniel A1 - Burgholzer, P. A1 - Jung, P. A1 - Caire, G. A1 - Ziegler, Mathias T1 - Laser excited super resolution thermal imaging for nondestructive inspection of internal defects N2 - A photothermal super resolution technique is proposed for an improved inspection of internal defects. To evaluate the potential of the laser-based thermographic technique, an additively manufactured stainless steel specimen with closely spaced internal cavities is used. Four different experimental configurations in transmission, reflection, stepwise and continuous scanning are investigated. The applied image post-processing method is based on compressed sensing and makes use of the block sparsity from multiple measurement events. This concerted approach of experimental measurement strategy and numerical optimization enables the resolution of internal defects and outperforms conventional thermographic inspection techniques. KW - Super Resolution KW - Laser Thermography KW - Non Destructive Testing KW - Comressed Sensing KW - Inverse Problem KW - Thermography PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519016 DO - https://doi.org/10.1038/s41598-020-77979-y VL - 10 IS - 1 SP - 22357 PB - Springer Nature AN - OPUS4-51901 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Dittmann, Daniel T1 - Experimental raw data for "Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine" N2 - This is the repository of all experimental raw data used in the Scientific Reports publication "Specific adsorption sites and conditions derived by thermal decomposition of activated carbons and adsorbed carbamazepine" by Daniel Dittmann, Paul Eisentraut, Caroline Goedecke, Yosri Wiesner, Martin Jekel, Aki Sebastian Ruhl, and Ulrike Braun. It includes - overview_measurements.xlsx and overview_measurements.ods containing a list of all TGA experiments (TGA, TGA-FTIR, TED-GC-MS, and ramp-kinetics) - TED-GC-MS.zip containing gas chromatography-mass spectrometry experimtent files for the Chemstation and OpenChrom - TGA.zip containing thermogravimetric analyses raw data on evolved gas analyses experiments (TGA-FTIR and TED-GC-MS) - TGA_kinetics.zip containing thermogravimetric analyses raw data on decomposition kinetic experiments (ramp-kinetics) - TGA-FTIR.zip containing Fourier-transform infrared spectroscopy series files for OMNIC - XRF.zip containing x-ray flourescence data on elemental composition KW - Adsorption KW - Aktivkohle KW - TED-GC/MS KW - Thermoanalytik PY - 2020 DO - https://doi.org/10.5281/zenodo.3716316 PB - Zenodo CY - Geneva AN - OPUS4-51902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waske, Anja T1 - X-ray Non-destructive testing of materials and composites N2 - Functional materials for energy conversion are important technology drivers needed for the implementation of low carbon energy. Therefore, researchers commonly focus on improving the intrinsic properties of a functional material. However, for applications, the extrinsic properties are at least as important as the intrinsic ones. Consequently, it is important to investigate and understand the external and internal structure of semi-finished products and especially defect dependent properties. The extrinsic properties may change during application and the life cycle of the material as well as through processing and molding steps. Our studies show how X-ray tomographic (XCT) investigations can contribute to structure investigations in composites and massive samples using the example of magnetic materials for energy conversion. T2 - Ruhr Universität Bochum - Seminar materials science and technology CY - Online meeting DA - 12.11.2020 KW - X-ray imaging KW - Non-destructuve testing KW - Functional materials PY - 2020 AN - OPUS4-51905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waske, Anja T1 - Mikro-Computertomographie für die Werkstoffforschung N2 - Preisträgervortrag Georg-Sachs-Preis der DGM Röntgencomputertomographie (CT) ist heute ein Standardwerkzeug in der Materialcharakterisierung. Im Vortrag zeigen wir ihre Anwendung für die Untersuchung magnetischer Funktionsmaterialien, additiv gefertigter Bauteile und deren Feedstockpulver und stellen erste CT-Ergebnisse biogener Feedstockpulver vor. T2 - DGM-Tag 2020 CY - Online meeting DA - 21.09.2020 KW - X-ray imaging KW - Non-destructuve testing PY - 2020 AN - OPUS4-51906 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lutz, C. T1 - Investigation on Vanadium Crossover in Nafion ™ and Novel PVDF Based Membranes for Vanadium Redox Flow Batteries N2 - Vanadium redoxflow batteries (VRFB)are currently one of the most promising candidates for stationary energys torage.For large scale applications the ion conducting membranes currently in use need to be improved. Ideally,they need to become more cost efficient and selective regarding the vanadium crossover.For a better understanding of the vanadium crossover, the development of reliable analytical methods and procedures, that elucidate uptake and transport of vanadium ions in the membrane, is necessary. First, we present the uptake of V2+,V3+,VO2+, VO2+ and V2O33+ in Nafion™ and in a novel membrane based onpoly(1,1-difluoroethylene)(PVDF). In preliminary discharge/charge experiments the ETFE-based membrane, the precursor of PVDF-based membrane, performed comparable to Nafion™. The methods of choice for speciation are UV/Vis and X-ray absorption near edge structure spectroscopy (XANES). According to the results, V2O33+, formed from VO2+ and VO2+, diffuses also into the membrane. In present models, the diffusion of V2O33+ is neglected. In addition,we study whether reactions could take place inside the membranes’ nanoscopic water body using XANES. Exposing Nafion™ from one site with V3+a nd from the other site with VO2+ realized the experiment. The results verified that VO2+ was formed inside the membrane. However,in present models reactions inside the membrane are neglected, too. T2 - Denver X-Ray Conference CY - Online meeting DA - 03.08.2020 KW - Batteries KW - BAMline KW - XANES KW - VRF PY - 2020 AN - OPUS4-51909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumacher, David T1 - From W. C. Röntgen to modern Tomography N2 - A not complete review of X-Ray related milestones from 1895 to the 21st century. T2 - ITN GW4SHM, First Training Event CY - Online Meeting DA - 23.11.2020 KW - X-Ray KW - Computed Tomography KW - Laminography KW - Digital Detector Arrays KW - Wilhelm Conrad Röntgen PY - 2020 AN - OPUS4-51881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Ahmadi, Samim A1 - Lecompagnon, Julien A1 - Hirsch, Philipp Daniel A1 - Burgholzer, P. A1 - Jung, P. A1 - Caire, G. T1 - Laser excited super resolution thermal imaging for nondestructive inspection of internal defects N2 - A photothermal super resolution technique is proposed for an improved inspection of internal defects. To evaluate the potential of the laser-based thermographic technique, an additively manufactured stainless steel specimen with closely spaced internal cavities is used. Four different experimental configurations in transmission, reflection, stepwise and continuous scanning are investigated. The applied image post-processing method is based on compressed sensing and makes use of the block sparsity from multiple measurement events. This concerted approach of experimental measurement strategy and numerical optimization enables the resolution of internal defects and outperforms conventional thermographic inspection techniques. KW - Super resolution KW - Photothermal KW - Imaging KW - Compressed sensing KW - Internal defects KW - Nondestructive testing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518866 DO - https://doi.org/10.48550/arXiv.2007.03341 SN - 2331-8422 SP - 1 EP - 9 PB - Cornell University CY - Ithaca, NY AN - OPUS4-51886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kowarik, Stefan A1 - Pithan, L. T1 - kowarik-labs/AI-reflectivity: v0.1 N2 - AI-reflectivity is a code based on artificial neural networks trained with simulated reflectivity data that quickly predicts film parameters from experimental X-ray reflectivity curves. This project has a common root with (ML-reflectivity)[https://github.com/schreiber-lab/ML-reflectivity] and evolved in parallel. Both are linked to the following publication: Fast Fitting of Reflectivity Data of Growing Thin Films Using Neural Networks A. Greco, V. Starostin, C. Karapanagiotis, A. Hinderhofer, A. Gerlach, L. Pithan, S. Liehr, F. Schreiber, S. Kowarik (2019). J. Appl. Cryst. For an online live demonstration using a pre-trained network have a look at github. KW - Artificial neural networks KW - X-ray reflectivity PY - 2019 DO - https://doi.org/10.5281/zenodo.3477583 PB - Zenodo CY - Geneva AN - OPUS4-51888 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - Non-Destructive Testing - Electromagnetic Methods N2 - This presentation contains a short summary about the basics of eddy current testing and magnetic flux leakage testing. In addition, the main focus of the talk lies on the application of point-like sensors like GMR for NDT. T2 - 1st Training Event - ITN project GW4SHM CY - Online meeting DA - 23.11.2020 KW - GMR KW - Magnetic flux leakage testing KW - Eddy current testing PY - 2020 AN - OPUS4-51889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Trace element analysis with synchrotron radiation N2 - Trace elements are chemical elements whose concentration in a material is very low. The exact definition depends on the application and varies for example between 100 micrograms per gram in analytical chemistry and 1000 micrograms per gram in geology. The ability to detect trace elements fast and quantitatively is of great importance in many areas of science and technology. With its high brilliance and flexibility in the excitation conditions, synchrotron radiation is an ideal tool for detecting traces even in small sample quantities. In this contribution I will report about the use of X-ray fluorescence(XRF)for qualitative and quantitative element sensitiveanalysis. In addition to the fundamentals of XRF and its quantification methods, the advantages and problems of different geometries like e.g. microXRF, Total Reflection X-ray Fluorescence (TXRF)or Double Dispersive XRF (D²XRF) will be discussed. Practical examples from BAMline from the research fields of medicine, geology and archaeometry will complete the lecture. T2 - Denver X-Ray Conference CY - Online meeting DA - 03.08.2020 KW - Synchrotron KW - BAMline KW - XRF PY - 2020 AN - OPUS4-51890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Artificial intelligence for spectroscopy examples from BAMline N2 - Various applications for artificial intelligence in the context of spectroscopy will be presented. in particular, examples from bamline will be featured. After a short introduction to synchrotron radiation, artificial intelligence algorithms for the quantification of X-ray fluorescence measurement are discussed. In the second example, information retrieval by natural language processing is reviewed. As a last example the reconstruction of measurements with the X-ray color camera and coded apertures is presented. T2 - Seminar Strahlenphysikalische Anwendungen in Technik und Medizin CY - ATi Wien, Austria DA - 22.01.2020 KW - Machine learning KW - Natural language processing KW - Neural networks KW - Synchrotron KW - BAMline PY - 2020 AN - OPUS4-51891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - Wirbelstromprüfung von Komposit-Druckbehältern N2 - Komposit-Druckgefäße für den Gefahrguttransport sowie für Wasserstoff-und Erdgasfahrzeuge bestehen aus einem lasttragenden Komposit und einer gasdichten, metallischen oder polymeren Barriereschicht (Liner). Zur Untersuchung der Integrität der Druckflaschen wurde die Wirbelstromprüfung eingesetzt. Hierbei wurden verschiedene Frequenzbereiche angewendet, um so die unterschiedlichen Materialien untersuchen zu können. Ziel der Untersuchungen war es, alterungsbedingte Schädigungen rechtzeitig zu detektieren. Der Vortrag stellt diese Ergebnisse vor. T2 - Carbon United - Gemeinsame Sitzung 3er-AG Zerstörungsfreie Werkstoff- u. Bauteilprüfung, Verbindungstechnik, Engineering CY - Online meeting DA - 07.12.2020 KW - Wirbelstromprüfung KW - CFK KW - Druckbehälter PY - 2020 AN - OPUS4-51892 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Von Ägypten bis Hiddensee Analyse von Gold mit Synchrotronstrahlung III N2 - Gold ist eines der sieben schon im Altertum bekannten Metalle und wurde wg. seines Glanzes und seiner Seltenheit von alters her als Tauschmittel und zur Herstellung von Schmuck benutzt. Außerdem ist es einfach bearbeitbar und weitestgehend gegen chemische Einflüsse resistent. Die Untersuchungen von Gold mit synchrotronstrahlungsangeregter Röntgenfluoreszenzanalyse sind zerstörungsfrei und geben Auskunft über die in der untersuchten Probe vorhandenen chemischen Elemente. Bei den hier vorgestellten Untersuchungen an der BAMline stehen Fragestellungen wie Herkunft, Herstellungsverfahren und Zusammengehörigkeit von Goldfunden im Vordergrund. Die verschiedenen Fragestellungen werden an einer Reihe von Beispielen erläutert die vom Wikingerschatz aus Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten langen. Der Fund von Bernstorf wird ausführlich diskutiert. T2 - Vorlesung FU Berlin Einführung in die Archäometrie CY - Berlin, Germany DA - 06.11.2020 KW - Synchrotron KW - BAMline KW - XRF KW - Gold KW - Archäometrie PY - 2020 AN - OPUS4-51893 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - X-Ray fluorescence with synchrotron radiation basics and applications N2 - In this talk, the features of X-ray fluorescence analysis with synchrotron radiation will be presented. First, the basics of the origin of synchrotron radiation and X-ray fluorescence analysis and the experimental setup will be discussed. Then, examples of trace element detection, micrometer resolution, and application of the X-ray color camera will be shown. T2 - HZB Photon school 2020 CY - Berlin, Germany DA - 09.03.2020 KW - Synchrotron KW - BAMline KW - XRF KW - Machine learning PY - 2020 AN - OPUS4-51894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - SRXRF examples from the BAMline N2 - Synchrotron radiation sources with their unique properties in terms of intensity, polarization and adjustability offer a wide range of possibilities in materials research. A basic introduction about the creation and special properties of synchrotron radiation will be given. Examples of current work at BAMline, the high-energy measuring facility of the Federal Institute for Materials Research and Testing at the synchrotron BESSY, are used to illustrate the possibilities and limitations of existing measuring methods. T2 - Better with Scattering CY - Online meeting DA - 16.03.2020 KW - Synchrotron KW - BAMline KW - XRF PY - 2020 AN - OPUS4-51895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Léonard, Fabien T1 - Overview of XCT data processing workflow for ammonium nitrate prills quantitative analysis N2 - This video presents the data processing workflow that was developed to perform the quantitative structural and morphological analysis of ammonium nitrate prills by x-ray computed tomography. KW - ANFO KW - Data processing KW - Explosives KW - Porosity KW - Surface area KW - XCT PY - 2020 DO - https://doi.org/10.5281/zenodo.3611339 PB - Zenodo CY - Geneva AN - OPUS4-51897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Machine learning: examples from BAMline N2 - Various applications for artificial intelligence in the context of spectroscopy will be presented. in particular, examples from BAMline will be presented. After a short introduction to synchrotron radiation, artificial intelligence algorithms for the quantification of X-ray fluorescence measurement are discussed. In the second example, information retrieval by natural language processing is discussed. T2 - Analytical Academy CY - Online meeting DA - 02.06.2020 KW - Machine learning KW - BAMline KW - XRF KW - Synchrotron PY - 2020 AN - OPUS4-51898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bühling, Benjamin T1 - Entwicklung eines luftgekoppelten Ultraschall-Echo-Prüfverfahrens mittels fluidischer Anregung N2 - In vielen technischen Bereichen werden Ultraschallverfahren zur zerstörungsfreien Werkstoffprüfung (ZfP) eingesetzt um auf Basis der Signalstärke und der Laufzeit Einbauteile und Beschädigungen zu orten. Luftgekoppelter Ultraschall spielt bisher in kommerziellen Anwendungen vor Allem im Bauwesen eine untergeordnete Rolle, da die Differenz der akustischen Impedanzen von Luft und Festkörpern immense Verluste beim Übergang des Schallsignals hervorruft. Im Rahmen des Promotionsvorhabens soll die Eignung eines neuartigen Anregungsprinzip untersucht werden, mit dem ein Großteil dieser Verluste vermieden werden soll. Anstelle eines Festkörpers soll mit Hilfe einer fluidischen Düse Druckluft zur Signalerzeugung eingesetzt werden. Die Impedanzverluste zwischen Aktuatormembran und Umgebungsluft entfallen daher. Die gezielte Schallerzeugung durch einen pulsierenden Freistrahl ist weitgehend unerforscht. Es ist daher notwendig, den so erzeugten Schallpuls in der Interaktion mit dem transienten Strömungsfeld zu untersuchen. Das kompressible Medium Luft und die geringen räumlichen Dimensionen einer hochfrequenten Pulsdüse werfen darüber hinaus einige Herausforderungen hinsichtlich der eingesetzten Messtechnik auf. Hier sollen geeignete Verfahren weiterentwickelt und validiert werden, um die Eignung des fluidisch erzeugten Pulses zu überprüfen. In diesem Vortrag werden erste Messungen an einem fluidischen Schalter mit denen an einem kommerziellen Luftultraschallprüfkopf verglichen. T2 - Doktorandenseminar BAM Abt. 8 CY - Berlin, Germany DA - 17.02.2020 KW - ZfP KW - Ultraschall KW - NDT KW - Ultrasound KW - Air-coupled KW - Non-Contact KW - Luftgekoppelt KW - Kontaktlos PY - 2020 AN - OPUS4-51120 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Juds, Carmen A1 - Schmidt, J. A1 - Weller, Michael G. A1 - Lange, Thorid A1 - Beck, Uwe A1 - Conrad, T. A1 - Boerner, H. G. T1 - Combining phage display and next-generation sequencing for materials sciences: A case study on probing polypropylene surfaces N2 - Phage display biopanning with Illumina next-generation sequencing (NGS) is applied to reveal insights into peptide-based adhesion domains for polypropylene (PP). One biopanning round followed by NGS selects robust PP-binding peptides that are not evident by Sanger sequencing. NGS provides a significant statistical base that enables motif analysis, statistics on positional residue depletion/enrichment, and data analysis to suppress false-positive sequences from amplification bias. The selected sequences are employed as water-based primers for PP-metal adhesion to condition PP surfaces and increase adhesive strength by 100% relative to nonprimed PP. KW - Polymers KW - Polypropylene KW - Glue KW - Plastics KW - Surface Activation KW - Primer KW - Peptide Library KW - Epoxy KW - Solid-binding Peptides KW - Functionalization KW - Polymer-binding Peptides KW - Adhesion KW - Material-binding Peptides KW - Adhesives PY - 2020 DO - https://doi.org/10.1021/jacs.0c03482 SN - 0002-7863 SN - 1520-5126 VL - 142 IS - 24 SP - 10624 EP - 10628 PB - ACS CY - Washington, DC, USA AN - OPUS4-51123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Martin A1 - Tscheuschner, Georg A1 - Herrmann, Stefan A1 - Weller, Michael G. T1 - Fast Detection of 2,4,6-Trinitrotoluene (TNT) at ppt Level by a Laser-Induced Immunofluorometric Biosensor N2 - The illegal use of explosives by terrorists and other criminals is an increasing issue in public spaces, such as airports, railway stations, highways, sports venues, theaters, and other large buildings. Security in these environments can be achieved by different means, including the installation of scanners and other analytical devices to detect ultra-small traces of explosives in a very short time-frame to be able to take action as early as possible to prevent the detonation of such devices. Unfortunately, an ideal explosive detection system still does not exist, which means that a compromise is needed in practice. Most detection devices lack the extreme analytical sensitivity, which is nevertheless necessary due to the low vapor pressure of nearly all explosives. In addition, the rate of false positives needs to be virtually zero, which is also very difficult to achieve. Here we present an immunosensor system based on kinetic competition, which is known to be very fast and may even overcome affinity limitation, which impairs the performance of many traditional competitive assays. This immunosensor consists of a monolithic glass column with a vast excess of immobilized hapten, which traps the fluorescently labeled antibody as long as no explosive is present. In the case of the explosive 2,4,6-trinitrotoluene (TNT), some binding sites of the antibody will be blocked, which leads to an immediate breakthrough of the labeled protein, detectable by highly sensitive laser-induced fluorescence with the help of a Peltier-cooled complementary metal-oxide-semiconductor (CMOS) camera. Liquid handling is performed with high-precision syringe pumps and chip-based mixing-devices and flow-cells. The system achieved limits of detection of 1 pM (1 ppt) of the fluorescent label and around 100 pM (20 ppt) of TNT. The total assay time is less than 8 min. A cross-reactivity test with 5000 pM solutions showed no signal by pentaerythritol tetranitrate (PETN), 1,3,5-trinitroperhydro-1,3,5-triazine (RDX), and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX). This immunosensor belongs to the most sensitive and fastest detectors for TNT with no significant cross-reactivity by non-related compounds. The consumption of the labeled antibody is surprisingly low: 1 mg of the reagent would be sufficient for more than one year of continuous biosensor operation. KW - Airport KW - Aviation KW - Bombs KW - Terrorism KW - Biosensing KW - Continuous Sensor KW - High-Speed KW - Ultrasensitive PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511245 DO - https://doi.org/10.3390/bios10080089 VL - 10 IS - 8 SP - 89 PB - MDPI CY - Basel AN - OPUS4-51124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - High molar mass cyclic poly(L-lactide)s by means of neat tin (II) 2-ethylhexanoate N2 - L-lactide was polymerized in bulk at 120, 140, 160 and 180°C with neat tin(II) 2-ethylhexanoate (SnOct2) as catalyst. At 180°C the Lac/Cat ratio was varied from 25/1 up to 8 000/1 and at 160°C from 25/1 up to 6 000/1. The vast majority of the resulting polylactides consist of cycles in combination with a small fraction of linear chains having one octanoate and one COOH end group. The linear chains almost vanished at high Lac/Cat ratios, as evidenced by MALDI-TOF mass spectrometry and measurements of intrinsic viscosities and dn/dc values. At Lac/Cat ratios <1000/1 the number average molar masses (Mn) are far higher than expected for stoichiometic initiation, and above 400/1 the molar masses vary relatively little with the Lac/Cat ratio. At 180° slight discoloration even at short times and degradation of the molar masses were observed, but at 160°C or below colorless products with weight average molar masses (Mw) up to 310 000 g mol-1 were obtained. The formation of high molar mass cyclic polylactides is explained by a ROPPOC (Ring-Opening Polymerizatiom with simultaneous Polycondensation) mechanism with intermediate formation of linear chains having one Sn-O-CH end group and one mixed anhydride end group. Additional experiments with tin(II)acetate as catalyst confirm this interpretation. These findings together with the detection of several transesterification mechanisms confirm previous critique of the Jacobson-Stockmayer theory. KW - Polylactide KW - MALDI-TOF MS KW - Cyclization PY - 2020 DO - https://doi.org/10.1039/d0py00811g VL - 11 IS - 32 SP - 5249 EP - 5260 PB - Royal Society for Chemistry AN - OPUS4-51130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Sparnacci, K. A1 - Unger, Wolfgang A1 - Tougaard, S. T1 - Determining nonuniformities of core-shell nanoparticle coatings by analysis of the inelastic background of X-ray photoelectron spectroscopy survey spectra N2 - Most real core-shell nanoparticle (CSNP) samples deviate from an ideal core-shell structure potentially having significant impact on the particle properties. An ideal structure displays a spherical core fully encapsulated by a shell of homogeneous thickness, and all particles in the sample exhibit the same shell thickness. Therefore, analytical techniques are required that can identify and characterize such deviations. This study demonstrates that by analysis of the inelastic background in X-ray photoelectron spectroscopy (XPS) survey spectra, the following types of deviations can be identified and quantified: the nonuniformity of the shell thickness within a nanoparticle sample and the incomplete encapsulation of the cores by the shell material. Furthermore, CSNP shell thicknesses and relative coverages can be obtained. These results allow for a quick and straightforward comparison between several batches of a specific CSNP, different coating approaches, and so forth. The presented XPS methodology requires a submonolayer distribution of CSNPs on a substrate. Poly(tetrafluoroethylene)-poly(methyl methacrylate) and poly(tetrafluoroethylene)-polystyrene polymer CSNPs serve as model systems to demonstrate the applicability of the approach. KW - Core-shell KW - Nanoparticles KW - Inelastic background KW - Polymers KW - QUASES KW - XPS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511315 DO - https://doi.org/10.1002/sia.6865 SN - 0142-2421 SN - 1096-9918 VL - 52 SP - 1 EP - 8 PB - Wiley CY - Chichester AN - OPUS4-51131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grossegesse, M. A1 - Hartkopf, F. A1 - Nitsche, A. A1 - Schaade, L. A1 - Doellinger, J. A1 - Muth, Thilo T1 - Perspective on Proteomics for Virus Detection in Clinical Samples N2 - One of the most widely used methods to detect an acute viral infection in clinical specimens is diagnostic real-time polymerase chain reaction. However, because of the COVID-19 pandemic, mass-spectrometry-based proteomics is currently being discussed as a potential diagnostic method for viral infections. Because proteomics is not yet applied in routine virus diagnostics, here we discuss its potential to detect viral infections. Apart from theoretical considerations, the current status and technical limitations are considered. Finally, the challenges that have to be overcome to establish proteomics in routine virus diagnostics are highlighted. KW - COVID-19 KW - Mass spectrometry KW - Virus diagnostics KW - Virus detection KW - Targeted mass spectrometry KW - Proteomics PY - 2020 DO - https://doi.org/10.1021/acs.jproteome.0c00674 SN - 1535-3907 VL - 19 IS - 11 SP - 4380 EP - 4388 PB - ACS AN - OPUS4-51633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sajulga, R. A1 - Easterly, C. A1 - Riffle, M. A1 - Mesuere, B. A1 - Muth, Thilo A1 - Mehta, S. A1 - Kumar, P. A1 - Johnson, J. A1 - Gruening, B. A1 - Schiebenhoefer, H. A1 - Kolmeder, C. A1 - Fuchs, S. A1 - Nunn, B. A1 - Rudney, J. A1 - Griffin, T. A1 - Jagtap, P. T1 - Survey of metaproteomics software tools for functional microbiome analysis N2 - To gain a thorough appreciation of microbiome dynamics, researchers characterize the functional relevance of expressed microbial genes or proteins. This can be accomplished through metaproteomics, which characterizes the protein expression of microbiomes. Several software tools exist for analyzing microbiomes at the functional level by measuring their combined proteome-level response to environmental perturbations. In this survey, we explore the performance of six available tools, to enable researchers to make informed decisions regarding software choice based on their research goals. Tandem mass spectrometry-based proteomic data obtained from dental caries plaque samples grown with and without sucrose in paired biofilm reactors were used as representative data for this evaluation. Microbial peptides from one sample pair were identified by the X! tandem search algorithm via SearchGUI and subjected to functional analysis using software tools including eggNOG-mapper, MEGAN5, MetaGOmics, MetaProteomeAnalyzer (MPA), ProPHAnE, and Unipept to generate functional annotation through Gene Ontology (GO) terms. Among these software tools, notable differences in functional annotation were detected after comparing differentially expressed protein functional groups. Based on the generated GO terms of these tools we performed a peptide-level comparison to evaluate the quality of their functional annotations. A BLAST analysis against the NCBI non-redundant database revealed that the sensitivity and specificity of functional annotation varied between tools. For example, eggNOG-mapper mapped to the most number of GO terms, while Unipept generated more accurate GO terms. Based on our evaluation, metaproteomics researchers can choose the software according to their analytical needs and developers can use the resulting feedback to further optimize their algorithms. To make more of these tools accessible via scalable metaproteomics workflows, eggNOG-mapper and Unipept 4.0 were incorporated into the Galaxy platform. KW - Bioinformatics KW - Metaproteomics KW - Mass spectrometry PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-516358 DO - https://doi.org/10.1371/journal.pone.0241503 SP - e0241503 AN - OPUS4-51635 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen T1 - The triple-isotope calibration approach: a universal and standard-free calibration approach for obtaining absolute isotope ratios of multi-isotopic elements N2 - The theory of a new calibration approach for obtaining absolute isotope ratios of multi-isotopic elements without the use of any standard has been developed. The calibration approach basically uses the difference in the instrumental isotope fractionation of two different types of mass spectrometers, leading to two different fractionation lines in a three-isotope diagram. When measuring the same sample with both mass spectrometers, the different fractionation lines have one point in common: this is the ‘true’ logarithmized isotope ratio pair of the sample. Thus, the intersection of both fractionation lines provides us with the absolute isotope ratios of the sample. This theory has been tested in practice by measuring Cd and of Pb isotope ratios in the certified reference materials BAM-I012 and NIST SRM981 by thermal ionization mass spectrometry and by inductively coupled plasma mass spectrometry while varying the ionization conditions for both mass spectrometers. With this experiment, the theory could be verified, and absolute isotope ratios were obtained, which were metrologically compatible with the certified isotope ratios. The so-obtained absolute isotope ratios are biased by − 0.5% in average, which should be improved with further developments of the method. This calibration approach is universal, as it can be applied to all elements with three or more isotopes and it is not limited to the type of mass spectrometers applied; it can be applied as well to secondary ion mass spectrometry or others. Additionally, this approach provides information on the fractionation process itself via the triple-isotope fractionation exponent θ. KW - Triple isotope fractionation KW - Absolute isotope ratio KW - Mass spectrometry KW - Calibration KW - Uncertainty PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-516364 DO - https://doi.org/10.1007/s00216-020-03050-4 VL - 413 IS - 3 SP - 821 EP - 826 PB - Springer Verlag AN - OPUS4-51636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pramann, A. A1 - Vogl, Jochen A1 - Rienitz, O. T1 - The Uncertainty Paradox: Molar Mass of Enriched Versus Natural Silicon Used in the XRCD Method N2 - The X-ray crystal density method uses silicon spheres highly enriched in 28Si as a primary method for the dissemination of the SI base unit kilogram yielding smallest possible uncertainties associated with the mass m within a few parts in 10-8. This study compares different available and newly developed analytical methods and their results for the determination of the molar mass M of silicon highly enriched in 28Si (Me) and of silicon (Mx) with an almost natural isotopic distribution. While for Me relative uncertainties urel(Me) in the lower 10-9 range are obtained routinely, it was not possible to fall below a value of urel(Mx) < 4 x 10-6 in the case of natural silicon, which is approximately three orders of magnitude larger. The application of the state-of the-art isotope ratio mass spectrometry accompanied with sophisticated thoroughly investigated methods suggests an intrinsic cause for the large uncertainty associated with the molar mass of natural silicon compared to the enriched material. KW - silicon KW - Molar mass KW - Isotope ratios KW - SI KW - Kilogram KW - Mole KW - XRCD method PY - 2020 DO - https://doi.org/10.1007/s12647-020-00408-y VL - 35 SP - 499 EP - 510 PB - Springer Verlag AN - OPUS4-51637 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reichel, V. E. A1 - Matuszak, J. A1 - Bente, Klaas A1 - Heil, T. A1 - Kraupner, A. A1 - Dutz, S. A1 - Cicha, I. A1 - Faivre, D. T1 - Magnetite-Arginine Nanoparticles as a Multifunctional Biomedical Tool N2 - Iron oxide nanoparticles are a promising platform for biomedical applications, both in terms of diagnostics and therapeutics. In addition, arginine-rich polypeptides are known to penetrate across cell membranes. Here, we thus introduce a system based on magnetite nanoparticles and the polypeptide poly-l-arginine (polyR-Fe3O4). We show that the hybrid nanoparticles exhibit a low cytotoxicity that is comparable to Resovist®, a commercially available drug. PolyR-Fe3O4 particles perform very well in diagnostic applications, such as magnetic particle imaging (1.7 and 1.35 higher signal respectively for the 3rd and 11th harmonic when compared to Resovist®), or as contrast agents for magnetic resonance imaging (R2/R1 ratio of 17 as compared to 11 at 0.94 T for Resovist®). Moreover, these novel particles can also be used for therapeutic purposes such as hyperthermia, achieving a specific heating power ratio of 208 W/g as compared to 83 W/g for Feridex®, another commercially available product. Therefore, we envision such materials to play a role in the future theranostic applications, where the arginine ability to deliver cargo into the cell can be coupled to the magnetite imaging properties and cancer fighting activity. KW - Iron oxide KW - Nanoparticle KW - Theranostics KW - MRI KW - Hyperthermia PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515993 DO - https://doi.org/10.3390/nano10102014 VL - 10 IS - 10 SP - 2014 PB - MDPI AN - OPUS4-51599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Goedecke, Caroline A1 - Dittmann, Daniel A1 - Eisentraut, Paul A1 - Wiesner, Yosri A1 - Schartel, Bernhard A1 - Klack, Patrick A1 - Braun, Ulrike T1 - Evaluation of thermoanalytical methods equipped with evolved gas analysis for the detection of microplastic in environmental samples N2 - Microplastic particles are currently detected in almost all environmental compartments. The results of detection vary widely, as a multitude of very different methods are used with very different requirements for analytical validity. In this work four thermoanalytical methods are compared and their advantages and limitations are discussed. One of them is thermal extraction-desorption gas chromatography mass spectrometry (TED-GC/MS), an analysis method for microplastic detection that has become established in recent years. In addition, thermogravimetric analysis coupled with Fourier-transform infrared spectroscopy (TGA-FTIR) and mass spectrometry (TGA-MS) were applied, two methods that are less common in this field but are still used in other research areas. Finally, microscale combustion calorimeter (MCC) was applied, a method not yet used for microplastic detection. The presented results are taken from a recently published interlaboratory comparison test by Becker et al. (2020). Here a reference material consisting of suspended matter and specified added polymer masses was examined, and only the results of the recoveries were presented. In the present paper, however, the results for the individual polymers are discussed in detail and individual perspectives for all instruments are shown. It was found that TED-GC/MS is the most suitable method for samples with unknown matrix and unknown, variable kinds and contents of microplastic. TGA-FTIR is a robust method for samples with known matrix and with defined kinds of microplastic. TGA-MS may offer a solution for the detection of PVC particles in the future. MCC can be used as a very fast and simple screening method for the identification of a potential microplastic load of standard polymers in unknown samples. KW - Microplastic KW - TED-GC/MS KW - TGA-MS KW - TGA-FTIR KW - MCC KW - Thermal analysis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-516687 DO - https://doi.org/10.1016/j.jaap.2020.104961 VL - 152 SP - 104961 PB - Elsevier B.V. AN - OPUS4-51668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - LIBS – Betonanalytik mir dem Laser N2 - Es wird ein alternatives Verfahren zur schnellen zweidimensionalen Analyse der chemischen Zusammensetzung von Baustoffen vorgestellt. Dieses beruht auf der Kombination des Abtrags einer geringen Materialmenge durch einen gepulsten Laser, der Plasmaerzeugung und der Analyse der Lichtemission des Plasmas mittels optischer Spektroskopie. Es können prinzipiell alle Elemente gleichzeitig nachgewiesen werden. Damit ist es möglich einerseits Informationen über den Baustoff an sich als auch über den Eintrag potentiell schädigender Elemente (z. B. Cl, C, Na, K, S) zu gewinnen. Das Verfahren kann automatisiert im Labor oder als mobile Version direkt vor Ort eingesetzt werden. Es liefert zweidimensionale Bilder der Elementverteilung in Echtzeit. Es kann ohne große Probenvorbereitung z. B. direkt an der Querschnittsfläche eines Bohrkernes gemessen werden. Die Messung dauert nur wenige Minuten. Das Prinzip der Messung, die Vor- und die Nachteile, sowie die verfügbare Gerätetechnik für den Einsatz im Labor oder direkt am Bauwerk werden vorgestellt. Abschließend werden praktische Beispiele für die Anwendung des LIBS-Verfahrens zur Erfassung des Chlorid-Eintrages, der Karbonatisierung und der Verteilung von Schwefel präsentiert. T2 - 9. Betonfachtagung CY - Berlin, Germany DA - 12.11.2019 KW - Chloride KW - Beton KW - LIBS KW - Schädigung PY - 2019 AN - OPUS4-51673 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Günther, Tobias A1 - Völker, Tobias T1 - LIBS – Betonanalytik mit dem Laser N2 - Es wird ein alternatives Verfahren zur schnellen zweidimensionalen Analyse der chemischen Zusammensetzung von Baustoffen vorgestellt. Dieses beruht auf der Kombination des Abtrags einer geringen Materialmenge durch einen gepulsten Laser, der Plasmaerzeugung und der Analyse der Lichtemission des Plasmas mittels optischer Spektroskopie. Es können prinzipiell alle Elemente gleichzeitig nachgewiesen werden. Damit ist es möglich einerseits Informationen über den Baustoff an sich als auch über den Eintrag potentiell schädigender Elemente (z. B. Cl, C, Na, K, S) zu gewinnen. Das Verfahren kann automatisiert im Labor oder als mobile Version direkt vor Ort eingesetzt werden. Es liefert zweidimensionale Bilder der Elementverteilung in Echtzeit. Es kann ohne große Probenvorbereitung z. B. direkt an der Querschnittsfläche eines Bohrkernes gemessen werden. Die Messung dauert nur wenige Minuten. Das Prinzip der Messung, die Vor- und die Nachteile, sowie die verfügbare Gerätetechnik für den Einsatz im Labor oder direkt am Bauwerk werden vorgestellt. Abschließend werden praktische Beispiele für die Anwendung des LIBS-Verfahrens zur Erfassung des Chlorid-Eintrages, der Karbonatisierung und der Verteilung von Schwefel präsentiert. T2 - 9. Betonfachtagung CY - Berlin, Germany DA - 12.11.2019 KW - Chloride KW - Beton KW - LIBS KW - Schädigung PY - 2019 SP - 1 PB - InformationsZentrum Beton GmbH CY - Berlin AN - OPUS4-51675 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, C. A1 - Bohling, C. A1 - Millar, S. A1 - Günther, Tobias A1 - Wilsch, Gerd ED - Krieger, J. ED - Isecke, B. T1 - Schnelle ortsaufgelöste Chloridbestimmung mit der laserinduzierten Plasmaspektroskopie (LIBS) N2 - Im Zuge der Ist-Zustandserfassung von Stahl- und Spannbetonbauwerken spielt die chemische Analyse von Beton eine zentrale Rolle. Durch den externen Eintrag von schädigenden Substanzen wie Chlorid oder Alkalien aus Tausalzen oder Meerwasser, kann u.U. der Beton und/oder die Stahlbewehrung angegriffen werden. Bei Überschreitung kritischer korrosionsauslösender Chloridgehalte, z.B. bei Stahlbeton 0,4 M.-% (bzw. 0,5 M.-%) und Spannbeton 0,2 M.-% bezogen auf den Zement, erhöht sich das Risiko für eine Chlorid-induzierte Korrosion. Für die Beurteilung eines Instandsetzungsbedarfs und, sofern notwendig, der Erarbeitung eines Instandsetzungskonzeptes muss nach der Rili-SIB1 ein sachkundiger Planer herangezogen werden. Standardmäßig werden für die chemische Analyse Bohrkerne bzw. Bohrmehlproben aus dem zu untersuchenden Bauwerk entnommen und nach aufwendiger Probenvorbereitung nasschemisch analysiert (nach DAfStb Heft 401 oder DIN 14629). Dabei wird der Gesamtchloridgehalt bezogen auf die Einwaage angegeben. Eine Umrechnung auf den Zementgehalt erfolgt i.d.R. durch Schätzwerte. Der Einsatz der laserinduzierten Plasmaspektroskopie (LIBS) wird seit Mitte der 90er Jahren an der Bundesanstalt für Materialforschung und -prüfung erforscht, um den Chloridgehalt durch eine ortsaufgelöste Elementanalyse an einer Betonprobe möglichst genau zu ermitteln. Die zweidimensionale LIBS-Messung mit einer lateralen Auflösung von 100 µm x 100 µm erlaubt die Berücksichtigung der Heterogenität von Beton. Dabei lassen sich die Bindemittelmatrix und die Gesteinskörnung separat betrachten, wodurch sich die Aussagekraft der Ergebnisse und somit die Sicherheit der chemischen Zustandserfassung erhöht. Durch die stetige Weiterentwicklung von Komponenten wie Laser, Spektrometer und analytischer Auswerteroutinen sind mittlerweile automatisierte Systeme für die schnelle LIBS-Analyse auf dem Markt verfügbar. In diesem Vortrag wird der aktuelle Stand der Technik anhand von Praxisbeispielen präsentiert und entscheidende Vorteile gegenüber dem Standardverfahren herausgestellt. Aufgrund der Möglichkeit für eine simultane Multielementanalyse mit LIBS werden weitere Anwendungen, wie z.B. die Ermittlung der Karbonatisierungstiefe, Untersuchungen von Transportprozessen, Chlorideintrag entlang von Rissen oder Untersuchungen von Elementverteilungen im Kontext einer AKR vorgestellt. T2 - 4. Brückenkolloquium CY - Online meeting DA - 08.09.2020 KW - Chloride KW - Beton KW - LIBS KW - Schädigung PY - 2020 SN - 978-3-8169-3518-6 SP - 465 EP - 471 PB - Narr Francke Attempto Verlag GmbH + Co. KG CY - Tübingen AN - OPUS4-51681 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, C. T1 - Schnelle ortsaufgelöste Chloridbestimmung mit der laserinduzierten Plasmaspektroskopie N2 - Im Zuge der Ist-Zustandserfassung von Stahl- und Spannbetonbauwerken spielt die chemische Analyse von Beton eine zentrale Rolle. Durch den externen Eintrag von schädigenden Substanzen wie Chlorid oder Alkalien aus Tausalzen oder Meerwasser, kann u.U. der Beton und/oder die Stahlbewehrung angegriffen werden. Bei Überschreitung kritischer korrosionsauslösender Chloridgehalte, z.B. bei Stahlbeton 0,4 M.-% (bzw. 0,5 M.-%) und Spannbeton 0,2 M.-% bezogen auf den Zement, erhöht sich das Risiko für eine Chlorid-induzierte Korrosion. Für die Beurteilung eines Instandsetzungsbedarfs und, sofern notwendig, der Erarbeitung eines Instandsetzungskonzeptes muss nach der Rili-SIB1 ein sachkundiger Planer herangezogen werden. Standardmäßig werden für die chemische Analyse Bohrkerne bzw. Bohrmehlproben aus dem zu untersuchenden Bauwerk entnommen und nach aufwendiger Probenvorbereitung nasschemisch analysiert (nach DAfStb Heft 401 oder DIN 14629). Dabei wird der Gesamtchloridgehalt bezogen auf die Einwaage angegeben. Eine Umrechnung auf den Zementgehalt erfolgt i.d.R. durch Schätzwerte. Der Einsatz der laserinduzierten Plasmaspektroskopie (LIBS) wird seit Mitte der 90er Jahren an der Bundesanstalt für Materialforschung und -prüfung erforscht, um den Chloridgehalt durch eine ortsaufgelöste Elementanalyse an einer Betonprobe möglichst genau zu ermitteln. Die zweidimensionale LIBS-Messung mit einer lateralen Auflösung von 100 µm x 100 µm erlaubt die Berücksichtigung der Heterogenität von Beton. Dabei lassen sich die Bindemittelmatrix und die Gesteinskörnung separat betrachten, wodurch sich die Aussagekraft der Ergebnisse und somit die Sicherheit der chemischen Zustandserfassung erhöht. Durch die stetige Weiterentwicklung von Komponenten wie Laser, Spektrometer und analytischer Auswerteroutinen sind mittlerweile automatisierte Systeme für die schnelle LIBS-Analyse auf dem Markt verfügbar. In diesem Vortrag wird der aktuelle Stand der Technik anhand von Praxisbeispielen präsentiert und entscheidende Vorteile gegenüber dem Standardverfahren herausgestellt. Aufgrund der Möglichkeit für eine simultane Multielementanalyse mit LIBS werden weitere Anwendungen, wie z.B. die Ermittlung der Karbonatisierungstiefe, Untersuchungen von Transportprozessen, Chlorideintrag entlang von Rissen oder Untersuchungen von Elementverteilungen im Kontext einer AKR vorgestellt. T2 - 4. Brückenkolloquium CY - Online meeting DA - 08.09.2020 KW - Beton KW - LIBS KW - Schädigung KW - Chloride PY - 2020 AN - OPUS4-51683 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karapanagiotis, Christos T1 - Machine learning for strain and temperature discrimination in Brillouin distributed sensing N2 - Short presentation of the PhD project in machine learning based Brillouin distributed sensing. Machine learning can be used to enhance the performance of BOFDA and reduce considerably the measurement time. Apart from this, ML can also be used to extract more information from the Brillouin gain spectrum in order to render the temperature and strain discrimination possible T2 - PhD Day 2020 CY - Online meeting DA - 15.09.2020 KW - Fiber optics sensors KW - Machine learning PY - 2020 AN - OPUS4-51689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Sennikov, P. A1 - Kornev, R. A1 - Ermakov, A. A1 - Shkrunin, V. A1 - Polyakov, V. T1 - Laser induced dielectric breakdown for synthesis of chlorofluorosilanes N2 - Tetrafluorosilane (SF4) and tetrachlorosilane (SiCl4) plasmas have been widely used as a source of either F or Cl for etching silicon or as a source of silicon for deposition of Si-based materials. Using different combinations of F and Cl in molecules of chlorofluorosilane SiFxCly adds additional flexibility in realization of these processes. Direct synthesis of SiFxCl4-x (x=1, 2, 3) from SiF4 and SiCl4 is thermodynamically forbidden under standard conditions. This restriction is removed in low-temperature plasmas studied in this work: a laser induced dielectric breakdown (LIDB) plasma and steady-state inductively-coupled plasma (ICP). The plasmas differ in many respects including energy content, temperature, and electron density that lead to different ionization/excitation states of plasma species, which are observed from plasma optical emission spectra. IR spectroscopy and mass-spectrometry confirm the formation of three chlorofluorosilanes, SiF3Cl, SiF2Cl2, and SiFCl3 that constitute ~60% in products of LIDB plasma and split 50/50 between SiF3Cl, SiFCl3 and SiF2Cl2. Experimental observations are verified by equilibrium static calculations via the minimization of Gibbs free energy and by dynamic calculations via the chemical-hydrodynamic plasma model of a spherically expanding plasma plume. The both types of calculations qualitatively agree with the results of spectroscopic analysis and reproduce dominant presence of SiF2Cl2 as the temperature of the gas approaches the room temperature. KW - Chemical-hydrodynamic modeling KW - Chlorofluorosilanes KW - Laser induced dielectric breakdown KW - Inductively coupled plasma KW - Equilibrium chemical modeling PY - 2020 DO - https://doi.org/10.1016/j.jfluchem.2020.109692 VL - 241 SP - 109692 PB - Elsevier B.V. AN - OPUS4-51646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg T1 - Novel Technique for On-Line Monitoring of the Curing Process of Fiber Reinforced Polymer Composites N2 - A specially designed experimental set up has been integrated into a commercially available FT IR Spectrometer for ATR experiments on Epoxy Systems. Representative data of far infrared spectra measured during the curing process at different temperatures of an epoxy system will be presented in dependency of the curing situation. The experiments and the selected set up are discussed to demonstrate its potential for future monitoring and ageing control applications during a manufacturing process of polymer composites. T2 - 45. International Confercene on infrared, milimeter and terahertz waves CY - Online meeting DA - 08.11.2020 KW - Far-infrared spectroscopy KW - Curing Monitoring PY - 2020 UR - https://live-irmmwthz.pantheonsite.io/technical-program AN - OPUS4-51649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Evaluation of Advanced NDT-Methods for Measurement of Fibre Orientation in Concrete N2 - Integration of fibre reinforcement in high-performance cementitious materials has become widely applied in many fields of construction. One of the most investigated advantages of steel fibre reinforced concrete (FRC) is the deceleration of crack growth and hence it’s improved sustainability due to e.g. decrease of permeability of concrete by aggressive substances. Additional benefits are associated with the structural properties of FRC, where fibres can significantly increase the ductility and the tensile strength of concrete. In some applications, such as tunnel linings or industrial slabs, it is even possible to entirely replace the conventional reinforcement, leading to significant logistical and environmental benefits. Fibre reinforcement can, however, have critical disadvantages and even hinder the performance of concrete, since it can induce an anisotropic material behaviour of the mixture if the fibres are not appropriately oriented. For a safe use of FRC in the future, reliable non-destructive methods need to be identified to assess the fibres’ orientation in hardened concrete. In this study, ultrasonic material testing, electrical impedance testing, and X-ray computer tomography have been investigated for this purpose using specially produced samples with biased or random fibre orientations. This paper demonstrates the capabilities of each of these NDT techniques for fibre orientation measurements and draws conclusions based on these results about the most promising areas for future research and development using these techniques. T2 - fib2020 Shanghai CY - Online meeting DA - 22.11.2020 KW - Ultrasonic testing KW - Steel fibre reinforced concrete (FRC) KW - Fibre orientation KW - X-ray computed tomography (CT) KW - Electrical impedance PY - 2020 AN - OPUS4-51651 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schade, U. T1 - Etalon Effects in THz Film Measurements N2 - Etalon effects in THz transmittance spectra, either taken in time-domain or frequency-domain, often hamper or even hinder the interpretation of film properties. In this paper we discuss the transferability and applicability of spectroscopic methods usually employed in the near and mid infrared spectral range and exemplarily present the application field. T2 - 45. International Confercene on infrared, milimeter and terahertz waves CY - Online meeting DA - 08.11.2020 KW - Far-infrared spectroscopy KW - Etalon Effects PY - 2020 UR - https://live-irmmwthz.pantheonsite.io/technical-program AN - OPUS4-51652 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Focused ion beam techniques beyond the ordinary - Methodological developments within ADVENT N2 - This poster presents the focused ion beam preparation methodologies developed within the framework of the EU funded EURAMET project ADVENT (Advanced Energy-Saving Technology). It summarises the key breakthroughs achieved for various in situ investigation techniques, e.g. in situ experiments at the Synchrotron facility BESSY II (IR-SNOM and XRS), TEM and SMM instrumentation. The created experimental devices from diverse thin-film semiconductor materials paved the way to dynamic structural studies bearing the potential to determine nanoscale correlations between strain and electric fields and, moreover, for the fundamental development of new in situ capabilities. N2 - Dieses Poster zeigt die FIB Präparationstechniquen, die im Rahmen des EU-finanzierten EURAMET-Projekts ADVENT (Advanced Energy Saving Technology) entwickelt wurden. Es fasst die wichtigsten Errungenschaften zusammen, die für verschiedene in situ Untersuchungstechniken erzielt wurden, z.B. situ-Experimente in dem Synchrotronring BESSY II (IR-SNOM und XRS), in situ TEM Experimente und für die SMM Technik. Die experimentellen Probenstrukturen, die aus verschiedenen Dünnschicht-Halbleitermaterialien erzeugt wurden, ebneten den Weg für dynamische Strukturstudien, die das Potenzial haben, nanoskalige Korrelationen zwischen Dehnung und elektrischen Feldern zu bestimmen und darüber hinaus neue in situ Messmethoden zu entwickeln. T2 - Final Meeting CY - Online Meeting DA - 30.06.2020 KW - FIB KW - Sample preparation KW - In situ KW - TEM KW - AFM PY - 2020 AN - OPUS4-51606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Kulow, Anicó T1 - Spatial Resolved Dispersive X-Ray Absorption Spectroscopy and Coded Aperture X-Ray Fluorescence Imaging N2 - One aim of this work was the development of a new setup for time- and laterally resolved XAFS measurements, based on the pronciple of dispersive XAFS. This setup is scanning free, stable, inexpensive, and straightforward to adjust for probing different elements. The second part of this work describes the impelemntation of a method for full-field X-ray fluorescence imaging with coded apertures. Expensive and complicated X-ray otpics, that are usually used for full-field imaging, are replaced with a coded aperture that consists of many pinholes drilled in an X-ray opaque material. Coded apertures are inexpensive to fabricate, energy independent and easy to use. The working principle is the same as with a pinhole camera, but the multiple holes allow a higher photon flux compared to a single pinhole or even a polycalippary optic, thus alowwing the reduction of measurement time. KW - X-ray fluorescence imaging KW - Coded Apertures KW - X-ray absorption spectroscopy KW - Synchrotron PY - 2021 SP - 1 EP - 175 CY - Berlin AN - OPUS4-52054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Reference Materials at BAM N2 - A introduction into reference materials, the certification process and brief over current reference projects at BAM is given. T2 - AK-Postdoc seminar CY - BAM Berlin, Germany DA - 02.02.2021 KW - Referenzmaterialien KW - Reference material KW - Homogeneity KW - Stability KW - Quality testing KW - Analytic KW - DNA KW - Dosimetry KW - Certification PY - 2021 AN - OPUS4-52060 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Garwek, Marcel A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Do Interfacial Layers in Thin Films Act as an Independent Layer Within Thin Films? N2 - The thermodynamic behavior of thin PVME films including the irreversible adsorbed layer on the substrate is investigated. In a first step, the growth kinetics of the adsorbed layer was studied combining a leaching technique and atomic force microscopy. Further, it was shown that there is a critical initial film thickness for the formation of a surface-filling adsorbed layer. Additionally, spectroscopic ellipsometry measurements were carried out to investigate the influence of the adsorbed layer on the glass transition temperature of the thin films. For 30 nm films and below, the influence of the adsorbed layer percolates strongly to the bulk-like layer of the film. Finally, the molecular dynamics of the adsorbed layer was studied by broadband dielectric spectroscopy, employing nanostructured-electrode systems. One process was revealed, which was assigned either to molecular fluctuations taking place in a loosely-bounded the part of the adsorbed layer, or to the desorption/adsorption of segments at the substrate. KW - Thin polymer films PY - 2021 DO - https://doi.org/10.1021/acs.macromol.0c02149 VL - 54 IS - 1 SP - 509 EP - 519 PB - ACS Publications AN - OPUS4-52037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Kalbe, Ute A1 - Schatten, René A1 - Szuppa, Tony T1 - Monitoringprogramm zur Verwertung von Bodenmaterial gemäß §§ 6-8 Novelle BBodSchV N2 - Mit der Novellierung der Bundes-Bodenschutz- und Altlastenverordnung (BBodSchV) (am 6.11.2020 im Bundesratsverfahren beschlossen) werden Regelungen zum Auf- und Einbringen von Bodenmaterial außerhalb der durchwurzelbaren Bodenschicht aufgenommen (sogenannte Verfüllungen). Ziel des Vorhabens war es, durch die Auswertung vorhandener und durchzuführender Untersuchungen eine Einstufung von Bodenmaterialien (jährlich fallen weit über 100 Mio. Tonnen davon an) für bestimmte Verwertungswege vornehmen zu können. Es sollte herausgefunden werden, ob Veränderungen hinsichtlich des Verwertungspotentials nachgewiesen werden können. Basis für die Durchführung und Bewertung waren die neuen Regelungen (hier insbesondere die Untersuchung mit einem Wasser/Feststoffverhältnis von 2:1, neue nationale und europäische Elutions- und Untersuchungsverfahren) der novellierten BBodSchV. Der Fokus lag dabei auf den polyzyklischen aromatischen Kohlenwasserstoffen (PAK) sowie ausgewählte anorganische Stoffe (Schwermetalle und Anionen) unter der Berücksichtigung unterschiedlicher Bodenmaterialien zur Verwertung. Dabei handelte es sich um: - Böden aus urban geprägten Gebieten, - Oberböden aus dem Straßenrandbereich in Form von Bankettschälgut, - Baggergut aus Gewässern mit Verdacht auf eine Kontamination, - Bergematerial (Mischung von Abraum- und Bodenmaterial), - Auenböden mit vermuteten Verunreinigungen aus Industrie und Gewerbe. Anhand der vorgelegten Ergebnisse kann nun eine Versachlichung der Diskussion um Ressorcenschutz vs. Schadlosigkeit der Verwertung erfolgen. Sie zeigen für die untersuchten Stoffe, dass bei einer Einführung der §§ 6-8 Novelle BBodSchV mit einer Erhöhung der Verwertungsquote für Bodenmaterial gerechnet werden kann. Eine Erhöhung des Deponievolumens ist somit nicht zu befürchten. Neben den ermittelten Daten konnten Grundlagen für die Überarbeitung verschiedener DIN-Normen für Bodenuntersuchungen erarbeitet werden. KW - Verwertung Bodenmaterial KW - Schadstofftransfer KW - Elutionsverfahren KW - BBodSchV KW - PAK PY - 2020 UR - https://www.umweltbundesamt.de/publikationen/monitoringprogramm-zur-verwertung-von-bodenmaterial SN - 1862-4804 VL - 127/2020 SP - 1 EP - 248 PB - Umweltbundesamt CY - Dessau AN - OPUS4-52039 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Karbach, H. A1 - Bell, A. M. A1 - Bauer, O. B. A1 - Karst, U. A1 - Meermann, Björn T1 - Determination of metal uptake in single organisms, Corophiumvolutator, via complementary electrothermal vaporization/inductively coupled plasma mass spectrometry and laserablation/inductively coupled plasma mass spectrometry N2 - Rationale: (Eco-)toxicological effects are mostly derived empirically and are notcorrelated with metal uptake. Furthermore, if the metal content is determined,mostly bulk analysis of the whole organism population is conducted; thus, biologicalvariability is completely disregarded, and this may lead to misleading results. Toovercome this issue, we compared two different solid sampling techniques for theanalysis of single organisms.Methods: In this study, complementary electrothermal vaporization/inductivelycoupled plasma mass spectrometry (ETV/ICP-MS) , laser ablation/inductivelycoupled plasma mass spectrometry (LA/ICP-MS)-based methods for the analysisof individual organisms were developed and the results obtained were comparedwith the concentrations obtained after digestion and measured using ICP-MS.For this purpose, a common (eco-)toxicological test organism, the mud shrimpCorophium volutator, was selected. As proof-of-concept application, these organismswere incubated with environmentally relevant metals from galvanic anodes, whichare often used for protection against metal corrosion in, for example, offshorewind farms.Results: The bulk analysis revealed that large quantities of the incubated elementswere detectable. Using the ETV/ICP-MS method, we could identify a highbiovariability within the population of organisms tested. Using the LA/ICP-MSmethod, it could be determined that the large quantities of the elements detectedwere due to adsorption of the metals and not due to uptake, which correlates wellwith the absence of (eco-)toxicological effects.Conclusions: The results obtained imply the efficiency of complementary methods toexplain the absence or presence of (eco-)toxicological effects. In particular, methodsthat allow for single-organism analysis or provide even a spatial resolution supportthe interpretation of ecotoxicological findings. KW - ICP-MS KW - Metal toxicity KW - Metal uptake KW - Corophium volutator KW - Seawater PY - 2021 DO - https://doi.org/10.1002/rcm.8953 VL - 35 IS - 2 SP - e8953 AN - OPUS4-52077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dinter, Adelina-Elisa T1 - Deciphering corrosion processes of MIC organisms - single cell-ICP-ToF-MS analysis of archaea on solid steels N2 - ICP-ToF (time of flight) MS enables the analysis of the multi-element fingerprint of single cells. The single cell ICP-ToF-MS is used in the presented poster for the analysis of archaea involved in microbiologically influenced corrosion (MIC) of steel. By means of sc-ICP-ToF-MS, the possible uptake of individual elements from the respective steel is investigated - the information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts. The work combines modern methods of analytical sciences with materials. T2 - SALSA - Make & Measure 2021 CY - Online meeting DA - 16.09.2021 KW - Sc-ICP-ToF-MS KW - Single cell analysis KW - Microbiologically influenced corrosion KW - Archaea KW - Poster presentation PY - 2021 AN - OPUS4-53337 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Zhiyang A1 - Kneipp, Janina T1 - Surface Molecular Patterning by Plasmon-Catalyzed Reactions N2 - Self-assembled monolayers (SAMs) on plasmonic substrates play a significant role applications of surface-enhanced Raman scattering (SERS). At the same time, localized surface plasmon resonances (LSPRs) can be employed for a broad range of plasmon-supported chemical modifications. Here, micropatterning using the derivatization of SAMs on gold nanosubstrates for rewritable SERS-based security labels or as the basis for sensing arrays functionalized with biomolecules is demonstrated using different plasmon-catalyzed reactions. The formation of 4,4′-dimercaptoazobenzene (DMAB) from p-aminothiophenol (PATP) as well as from p-nitrothiophenol (PNTP) and the reduction of PNTP to PATP are used to change the functionality of the substrate in specified positions. Employing LSPR, the reactions are started by illumination using visible laser light at a high intensity in a focal spot of a microscope objective and yield microscopic patterns of the reaction product. The obtained molecular patterns can be erased by other reactions, enabling different strategies for rewriting, encryption, or stepwise functionalization. KW - 4,4′-dimercaptoazobenzene KW - Surface molecular patterning KW - Plasmon-catalyzed reactions KW - p-aminothiophenol KW - p-nitrothiophenol PY - 2021 DO - https://doi.org/10.1021/acsami.1c12410 SN - 1944-8252 VL - 13 IS - 36 SP - 43708 EP - 43714 PB - ACS Publications AN - OPUS4-53341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Reverse deposition of TI-oxides under nanosecond laser ablation of TI N2 - Processes of laser induced oxidation of metals are typically studied in the framework of heterogeneous chemical reactions occurring on the irradiated surface, which lead to the formation of dense oxide films deposited on it. Such technology has many applications like color-laser marking technology and laser recording on thin metal films for creation of diffractive optical elements . Under the conditions of strong laser ablation, another oxidation mechanism becomes possible: evaporated atoms react with oxygen in a surrounding atmosphere and the products of such reaction are redeposited back onto the substrate. The chemical and phase composition of such deposited layer, its density, morphology and structure depend on the conditions of laser ablation. By varying these conditions, the main properties of such coating can be controlled that is important for some potential application (for example in biomedicine). In our report we present the study of the processes of redeposition of oxides structure under the conditions of multipulse nanosecond laser ablation of titanium (Grade 2) in air atmosphere at normal conditions. Our experiments show that titanium-implants with such deposited oxide layer have increased biocompatibility. Modelling of chemical reaction in laser-induced plasma coupled with experimental methods of plasma optical emission spectroscopy allows us to determine the types of main chemical reactions in laser plasma as well as it influences on the plume dynamics and vapor condensation kinetics. As a result, we propose the general physical picture of reverse deposition of oxides structure under the condition of strong nanosecond laser ablation. The formation of the titanium oxide precipitate is explained not only by collisions in the plasma, but also by the chemical interaction of titanium and oxygen, which leads to the formation of а low pressure area near the substrate and additionally stimulates the reverse deposition of oxides. We expect, similar processes are valid not only for titanium but also for other metals and, possibly, semiconductors. T2 - 28th International Conference on Advanced Laser Technologies CY - Online meeting DA - 06.09.2021 KW - Laser ablation KW - Laser induced plasma deposition KW - Surface coating KW - Emission spectroscopy KW - Titanium dioxide KW - Hydrodynamic model KW - Plasma chemistry PY - 2021 AN - OPUS4-53245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Optical Detection of Defects during Laser Metal Deposition - Simulations and Experiment N2 - Laser metal deposition is a rapidly evolving method for additive manufacturing that combines high performance and simplified production routine. Quality of production depends on instrumental design and operational parameters that require constant control during the process. In this work, feasibility of using optical spectroscopy as a control method is studied via modeling and experimentally. A simplified thermal model is developed based on the time-dependent diffusion-conduction heat equation and geometrical light collection into detection optics. Intense light emitted by a laser-heated spot moving across a sample surface is collected and processed to yield the temperature and other temperature-related parameters. In a presence of surface defects the temperature field is distorted in a specific manner that depends on a shape and size of the defect. Optical signals produced by such the distorted temperature fields are simulated and verified experimentally using a 3D metal printer and a sample with artificially carved defects. Three quantities are tested as possible metrics for process monitoring: temperature, integral intensity, and correlation coefficient. The shapes of the simulated signals qualitatively agree with the experimental signals; this allows a cautious inference that optical spectroscopy is capable of detecting a defect and, possibly, predicting its character, e.g. inner or protruding. T2 - 28th International Conference on Advanced Laser Technologies CY - Online meeting DA - 06.09.2021 KW - Additive manufacturing KW - Laser metal deposition KW - Optical sensor KW - Optical emission spectroscopy KW - Process control PY - 2021 AN - OPUS4-53246 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pech May, Nelson Wilbur A1 - Paul, A. A1 - Ziegler, Mathias T1 - Pulse-compression laser thermography using a modified Barker code: Enhanced detection of subsurface defects N2 - Pulse-compression thermography is an emerging technique that has shown versatility by combination of pulsed and lock-in thermography. Accordingly, several aspects of this technique are still unexplored, and some others not fully developed yet. Barker codes were widely used in radar applications due to their simplicity and their optimum autocorrelation function. Nevertheless, applications were limited by the amplitude of the sidelobes present in the autocorrelation function and therefore, several filters have been developed which aim to reduce the sidelobes. However, the filters usually depend on empirical parameters which must be determined for each application. A better alternative would improve the applicability of the Barker codes. In this work, we further develop the pulse-compression thermography technique by introducing a 13-bit modified Barker code (mBC): This allows to drastically reduce the sidelobes characteristic of the 13-bit Barker code (BC). Consequently, the thermographic impulse response, obtained by cross-correlation, is almost free of such sidelobes. Deeper defects become easier to detect in comparison with using a 13-bit Barker code. Numerical simulations using the finite element method are used for comparison and experimental measurements are performed in a sample of steel grade St 37 with machined notches of three different depths: 2 mm, 4 mm and 6 mm. T2 - SPIE Defense + Commercial Sensing 2021 CY - Online meeting DA - 13.04.2021 KW - Pulse-compression laser thermography KW - Barker codes KW - Non-destructive testing PY - 2021 DO - https://doi.org/10.1117/12.2586078 SN - 0277-786X VL - 11743 SP - 1 EP - 11 PB - SPIE CY - Bellingham, Wash. AN - OPUS4-53247 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pech May, Nelson Wilbur A1 - Paul, A. A1 - Ziegler, Mathias T1 - Pulse-compression laser thermography using a modified Barker code: Enhanced detection of subsurface defects N2 - Pulse-compression thermography is an emerging technique that has shown versatility by combination of pulsed and lock-in thermography. Accordingly, several aspects of this technique are still unexplored, and some others not fully developed yet. Barker codes were widely used in radar applications due to their simplicity and their optimum autocorrelation function. Nevertheless, applications were limited by the amplitude of the sidelobes present in the autocorrelation function and therefore, several filters have been developed which aim to reduce the sidelobes. However, the filters usually depend on empirical parameters which must be determined for each application. A better alternative would improve the applicability of the Barker codes. In this work, we further develop the pulse-compression thermography technique by introducing a 13-bit modified Barker code (mBC): This allows to drastically reduce the sidelobes characteristic of the 13-bit Barker code (BC). Consequently, the thermographic impulse response, obtained by cross-correlation, is almost free of such sidelobes. Deeper defects become easier to detect in comparison with using a 13-bit Barker code. Numerical simulations using the finite element method are used for comparison and experimental measurements are performed in a sample of steel grade St 37 with machined notches of three different depths: 2 mm, 4 mm and 6 mm. T2 - SPIE Defense + Commercial Sensing 2021 CY - Online meeting DA - 13.04.2021 KW - Pulse-compression laser thermography KW - Barker codes KW - Non-destructive testing PY - 2021 AN - OPUS4-53249 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena T1 - Development of a standard series for ellipsometry N2 - Ellipsometry is a powerful tool, which allows the investigation of material properties over a broad spectral range. Over the course of several years, the ellipsometry lab at BAM has become an accredited testing lab according to ISO/IEC 17025 laying bare the need of better methods for accuracy and traceability. Despite its wide range of application in both research and development as well as industry, there have been no generally accepted standards dealing with model validation and measurement uncertainties. Based on the first German standard DIN 50989 – 1: 2018 Ellipsometry - Part 1: Principles (currently international standard ISO 23131: 2021) and under consideration of GUM [1] a series of standards for ellipsometry was developed. The entire 6-part series covers several model-based application cases. This standards series avoids having narrow and material specific application cases but instead classifies applications of ellipsometry according to the sample complexity. The concept of ellipsometric transfer quantities (Ψ and Δ or alternatively the elements of transfer matrices) is implemented in the series. For each application case a model-based validation strategy was developed. Thus, the standards are applicable to all materials, instruments and measuring principles. The uniform structure concept of the series facilitates its practical applicability for users. The standards include the model-based GUM-compliant determination/estimation of the measurement uncertainties. In addition, the appendices of the documents contain numerous measurement and simulation examples as well as recommendations for measuring practice. In this contribution we present the application cases and basic structure of the standards developed in collaboration with Accurion GmbH and SENTECH Instruments GmbH in the project SNELLIUS. T2 - 11th Workshop Ellipsometry (WSE 11) CY - Steyr, Austria DA - 06.09.2021 KW - Standardization of ellipsometry KW - DIN 50989 Parts 1 – 6 KW - ISO 23131: 2021 KW - Validation concepts of ellipsometric measurements KW - Uncertainty budgets KW - GUM-compliance PY - 2021 AN - OPUS4-53250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Martin T1 - Development of a high-sensitivity biosensor for the quasi-continuous detection of the explosive TNT and the illegal drug cocaine N2 - An immunofluorometric biosensor with laser-induced fluorescence detection was presented. For TNT an LOD of 60 ppb and for cocaine an LOD of 9 ppb was achieved. A swipe test was performed in less than 3 minutes. No significant cross-reactivity was observed. T2 - 15. Interdisziplinäres Doktorandenseminar des Arbeitskreises Prozessanalytik der GDCh CY - Online meeting DA - 06.09.2021 KW - PETN KW - HMX KW - RDX KW - Microfluidic mixing KW - Lab-on-a-chip KW - Affinity column KW - Monolithic material KW - Sintered glass KW - Dy-654 KW - Flowcell KW - Epifluorescence KW - CMOS camera KW - Diode laser KW - Antibody screening PY - 2021 AN - OPUS4-53329 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gehrenkemper, Lennart T1 - Detection of PFAS pollution in environmental samples - A Fast & sensitive PFAS sum parameter method using HR CS GFMAS N2 - The substance class of per- and polyfluorinated alkyl substances (PFAS) comprises more than 5300 organic compounds. PFAS are completely fluorinated on at least one carbon atom. They are associated with negative impacts on human and animal health, are extremely persistent in the environment, and bioaccumulate along food chains. Therefore, PFAS are classified as emerging pollutants. At the same time, their physicochemical properties make them attractive for use in diverse technical applications. They are both hydrophobic and lipophobic and show high thermal as well as chemical resistance due to the strong C-F bond. First regulations of some PFAS in combination with the technically excellent properties generated an innovation pressure and led to an enormous increase in the number of fluorinated substitution compounds. Due to the increasing complexity of this substance class, target analysis is not able to cover such a variety and multitude of analytes. Therefore, a suitable PFAS sum parameter method is necessary for an accurate detection of PFAS pollution in the environment, the identification of PFAS hotspots and an evaluation of appropriate remediation measures. Here we provide insights into the current state of PFAS sum parameter development and present our latest results on method development for the quantitative analysis of PFAS as extractable organically bound fluorine (EOF) in environmental samples using high-resolution molecular absorption spectrometry (HR-CS-GFMAS). For this purpose, we optimized the extraction of PFAS from different solid matrices with simultaneous separation of inorganic fluoride. For quantification resulting extracts were measured using a fluorine specific HR-CS-GFMAS method. By adding gallium salt solutions as modifiers in HR-CS-GFMAS, fluorine can be indirectly quantified very selectively by the in situ formation of GaF with low limits of quantification (instrumental LOQ c(F) < 3 µg/L). Here we will show results from real soil samples from sites with and without known contamination. T2 - 6. Doktorandenseminar des Deutschen Arbeitskreises für Analytische Spektroskopie (DAAS) CY - Online meeting DA - 20.09.2021 KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Soil KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction PY - 2021 AN - OPUS4-53333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tscheuschner, Georg T1 - MALDI-TOF MS Fingerprinting of Antibodies in Less Than One Hour N2 - Antibodies are the most used biomolecules in analytical research. Nevertheless, the sequence and structure information of antibodies is often limited, since manufacturers keep them secret or suppliers sell them under different names. This can make it difficult to reproduce even basic experiments performed in publications as the antibodies used might not be identifiable. To overcome these problems, we developed a simple and cheap method for antibody identification by MALDI-TOF-MS fingerprinting. This technique was used to generate a library of antibody fingerprints, which enables the identification and comparison of antibodies in short time. T2 - SALSA Make and Measure 2021 CY - Online meeting DA - 16.09.2021 KW - Hydrolysis KW - Acid KW - Trypsin KW - Digestion KW - Fragment KW - Peptides KW - Mass spectrometry KW - Database KW - Clones KW - Monoclonal antibodies PY - 2021 AN - OPUS4-53294 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas T1 - Accuracy, traceability, and standardization in spectroscopic ellipsometry N2 - Ellipsometry has been an extremely successful and fast expanding method in the past decades along with other related techniques using polarisation sensitive measurements. Opening new fields of application for a successful measurement technique brings some requirements and issues that have to be solved. From a metrological point of view, ellipsometry has the problem that uncertainties are difficult to determine for model-based analysis techniques in general. In this presentation, we will explore how the usefulness of polarimetric methods like ellipsometry can be increased. Ellipsometry as a method could profit from several current developments which will be discussed in this presentation: • Standardisation initiatives on national and international level developing standards for best practice when using ellipsometry. A series of at least six standards is currently developed on national German and international level covering different levels of sample complexity. • Projects on traceability of ellipsometry and structured surface spectrometry as well as new dielectric function database initiatives. • Metadata handling and data ontology providing a better framework for exchange and collaborative use of research data. We will also explore the quantification of measurement uncertainty using examples from projects in which BAM is involved. Examples will be presented of multilayer and non-ideal materials as well as the determination of layer properties for technical applications such as thin layer catalysts and complex polymers. The definition of reference materials will be discussed. T2 - 11th Workshop Ellipsometry (WSE 11) CY - Steyr, Austria DA - 06.09.2021 KW - Ellipsometry KW - Uncertainty KW - Surface analytics KW - Data science PY - 2021 AN - OPUS4-53295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - A fast and simple PFAS extraction method for soil samples utilizing HR-CS-GFMAS N2 - Here, we describe a fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) utilizing extractable organic fluorine (EOF) sum parameter analysis and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) in soil samples. After extraction and separation of inorganic and organic fluorinated compounds, organically bound fluorinated compounds were indirectly determined via the molecular absorption of gallium mono-fluoride at 211.248 nm. The implementation of the decisions of the “Stockholm Convention on persistent organic pollutants” as well as the “Protocol on Persistent Organic Pollutants of the Convention on Long-Range Transboundary Air Pollution” of the UNECE include the reduction respectively the elimination of PFASs in the environment. Currently, regulations aim to target single compounds (mostly C8-PFAS). But the PFAS group includes over 4700 substances, which are potentially persistent and toxic, thus target analytical approaches are not suitable for a holistic approach investigating the PFAS pollutant situation. Furthermore, forbidden PFASs are substituted by short-chain PFASs, thus the number of unknow substances is steadily increasing. For this reason, sum parameter approaches are more suitable to investigate and assess the pollution situation as well as derive exposure limits. Our developed analytical method was successfully applied to determine PFASs in soil samples from a polluted site. In view of steadily increasing numbers of PFAS substances, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFAS in the future. T2 - SALSA Make and Measure ... and Machines CY - Online meeting DA - 16.09.2021 KW - PFAS KW - HR-CS-GFMAS KW - IC KW - EOF KW - Soil PY - 2021 AN - OPUS4-53302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - The Dark side of Science N2 - We all may have started out as bright-eyed students trying to do science to the best of our abilities, but over time, some of us have gradually drifted to the dark side. The dark side of science has an impressive publication rate in high-ranking journals, good success with funding agencies, and rocks the world with stellar findings. Unfortunately, these findings aren't real, either by accident or on purpose. As the presenter and his colleagues found, trying to correct or even dispute any of these findings in literature is a supremely complex and time-consuming effort. With no recent reduction in the frequency of such false findings, it is up to us to try to stem the flow. Besides looking at examples, we need to understand the underlying driving forces behind this dark scientific movement. By combining this understanding with a refresher of the core scientific principles, we can then develop the necessary argumentative tools and mechanisms that may prevent our own slide down the slippery slope. This talk will therefore start out with several entertaining examples of probably accidental, as well as definitely deliberate, false scientific findings in literature (and in particular in the field of materials research). We will then take a brief look at the possible causes for these developments, after which some tools will be presented that can help both the fresh as well as the well-seasoned scientist to rise up against the dark side. T2 - DGM special event (invited lecture) CY - Online meeting DA - 23.06.2021 KW - Scientific fraud KW - Reproducibility crisis KW - Bad science KW - Scientific method KW - Publication pressure PY - 2021 AN - OPUS4-53274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Völker, Tobias T1 - Laser-based building material sorting for the processing of construction and demolition waste for the circular economy N2 - A joint project of partners from industry and research institutions for the research and construction of an analysis system for an automated, sensor-supported sorting of construction and demolition waste will be presented. This is intended to supplement or replace the previously practiced manual sorting, which harbors many risks and dangers for the staff and only enables obvious, visually detectable differences for separation. The method of laser-induced breakdown spectroscopy is to be used in combination with hyperspectral sensors. Due to the jointly processed information (data fusion), this should lead to a significant improvement in the separation of types. In addition to the sorting of different materials (concrete, main masonry building materials, organic components, glass, etc.), impurities such as SO3-containing building materials (gypsum, aerated concrete, etc.) could also be detected and separated. The subsequent recycling and sales opportunities are examined, such as the use of recycled aggregates in concrete, the recycling of building materials containing sulphate as a gypsum substitute for the cement industry or the agglomeration of synthetic lightweight aggregates for lightweight concrete or as a substrate for green roofs. At the same time, it is investigated whether soluble components (sulfates, heavy metals, etc.) can be detected by LIBS without a wet chemical analysis and what impact the recycling materials have on the environment. The entire value chain is examined using the example of the Berlin location in order to minimize economic / technological barriers and obstacles on a cluster level and to sustainably increase the recovery and recycling rates. T2 - Materials Week 2021 CY - Online meeting DA - 07.09.2021 KW - Laser induced breakdown spectroscopy KW - Building waste KW - Circular economy KW - Material sorting PY - 2021 AN - OPUS4-53286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gantois, F. T1 - ALCOREF "Certified forensic alcohol reference materials" N2 - The poster presents the main achievements of the capacity building project ALCOREF “Forensic alcohol reference materials”. The project was part of the European Metrology Programme for Innovation and Research (EMPIR). Altogether 43 certified ethanol in water reference materials (CRMs) in the mass fraction range of 0.1 to 7 mg/g were developed by project partners. These CRMS are suitable for the calibration and verification of evidential breath alcohol analysers according to the requirements of the International Organisation of Legal Metrology (OIML). Furthermore, 10 new or improved Calibration and Measurement Capability (CMC) claims for purity assessment of ethanol and ethanol quantification were prepared. Newly established measurement capabilities and the new CRMs were successfully tested in three intercomparisons conducted as official intercomparisons of EURAMET Technical Committee for Metrology in Chemistry. T2 - 20th International Metrology Congress CIM CY - Lyon, France DA - 07.09.2021 KW - Certified reference material KW - EMPIR project KW - Evidential breath alcohol measurement PY - 2021 AN - OPUS4-53288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Pignatelli, Giuseppe A1 - Straße, Anne T1 - Optical detection of defects during laser metal deposition: Simulations and experiment N2 - Laser metal deposition is a rapidly evolving method for additive manufacturing that combines high performance and simplified production routine. Quality of production depends on instrumental design and operational parameters that require constant control during the process. In this work, feasibility of using optical spectroscopy as a control method is studied via modeling and experimentally. A simplified thermal model is developed based on the time-dependent diffusion-conduction heat equation and geometrical light collection into detection optics. Intense light emitted by a laser-heated spot moving across a sample surface is collected and processed to yield the temperature and other temperature-related parameters. In a presence of surface defects the temperature field is distorted in a specific manner that depends on a shape and size of the defect. Optical signals produced by such the distorted temperature fields are simulated and verified experimentally using a 3D metal printer and a sample with artificially carved defects. Three quantities are tested as possible metrics for process monitoring: temperature, integral intensity, and correlation coefficient. The shapes of the simulated signals qualitatively agree with the experimental signals; this allows a cautious inference that optical spectroscopy is capable of detecting a defect and, possibly, predicting its character, e.g. inner or protruding. KW - Additive manufacturing KW - Laser metal deposition (LMD) KW - Thermal model KW - Optical sensor KW - Process control PY - 2021 DO - https://doi.org/10.1016/j.apsusc.2021.151214 SN - 0169-4332 VL - 570 SP - 1 EP - 13 PB - Elsevier CY - Amsterdam AN - OPUS4-53292 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wittwer, Philipp T1 - Herausforderungen bei der Anwendung von Summenparametern (EOF) in der PFAS Analytik N2 - Problemstellen die bei der Arbeit mit der CIC in unserem Fachbereich aufgetreten sind und wie wir diese Probleme angegangen sind und die verwendeten Methoden weiterentwickelt haben. T2 - 25.Jahrestagung SETAC & GDCh "Umwelt 2021" CY - Online meeting DA - 07.09.2021 KW - PFAS KW - EOF KW - CIC PY - 2021 AN - OPUS4-53267 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lee, Hee-Jin A1 - Rühl, Isabel T1 - Phosphorus sum parameter analysis using HR-CS-GFMAS N2 - Organophosphate (OP) esters (OPEs) are widely used as flame retardants (FRs) and can for that purpose be found in textiles, furnitures, electronics and more. They can also be used as plasticizers or lubricants. OPEs have been found in air, water and sediment as environmental pollutants and are associated with potential health risks like cancer. In this study, a method for the phosphorus sum parameter analysis using HR-CS-GFMAS was optimized for environmental (water) samples. For this purpose, three FR substances (TPP, VPA, TDCPP) were used. T2 - SALSA Make and Measure ... and Machines CY - Online meeting DA - 16.09.2021 KW - HR-CS-GFMAS KW - Phosphorus KW - Organophosphate esters KW - Flame retardants PY - 2021 AN - OPUS4-53303 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis T1 - Ein inverses Verfahren zur Schadensrekonstruktion mittels geführter Wellen N2 - Eine zentrale Aufgabe der zerstörungsfreien Prüfung und der Strukturüberwachung (engl. Structural Health Monitoring - SHM) mit Ultraschallwellen ist die Bewertung von Schäden in Bauteilen. In vielen Bauteilen, wie zum Beispiel platten- und schalenförmigen Strukturen, Rohrleitungen oder Laminaten, breitet sich der Ultraschall in Form geführter Wellen aus. Zwar haben geführte Wellen eine relativ große Reichweite innerhalb des Bauteils und ermöglichen so eine großflächige Prüfung, ihre multimodalen und dispersiven Eigenschaften erschweren jedoch die Analyse der vom Schaden kommenden Reflexionen. Eine Möglichkeit, die Messsignale zu interpretieren und die Schäden zu charakterisieren, ist deren Vergleich mit der Wellenausbreitung in einem digitalen Modell. Hierbei stellt sich die Aufgabe, den Schaden im digitalen Modell anhand der Messdaten zu rekonstruieren. Diese Rekonstruktion beschreibt ein inverses Problem, das mehrere Vorwärtsrechnungen braucht, um das Schadensmodell an die Messdaten anzupassen.Durch die kleine Wellenlänge von Ultraschallwellen sind klassische Vorwärtsmethoden wie die Finte Elemente Methode rechenintensiv, weshalb die Autoren die semi-analytische Scaled Boundary Finite Element Method (SBFEM) benutzen, um den Rechenaufwand zu verringern. Im Beitrag wird ein inverses Verfahren basierend auf dem Automatischen Differenzieren in Kombination mit der SBFEM vorgestellt und an verschiedenen Schadenstypen in 2D-Querschnittmodellen von Wellenleitern getestet. In der präsentierten Vorstudie werden dafür „Messdaten“ aus unabhängigen Simulationen verwendet. T2 - DAGA 2021 - 47. Jahrestagung für Akustik CY - Vienna, Austria DA - 15.08.2021 KW - SBFEM KW - Inverse Verfahren KW - AD KW - SHM KW - NDT PY - 2021 AN - OPUS4-53304 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis A1 - Jurgelucks, B. A1 - Prager, Jens A1 - Walther, A. T1 - Ein inverses Verfahren zur Schadensrekonstruktion mittels geführter Wellen N2 - Eine zentrale Aufgabe der zerstörungsfreien Prüfung und der Strukturüberwachung (engl. Structural Health Monitoring - SHM) mit Ultraschallwellen ist die Bewertung von Schäden in Bauteilen. In vielen Bauteilen, wie zum Beispiel platten- und schalenförmigen Strukturen, Rohrleitungen oder Laminaten, breitet sich der Ultraschall in Form geführter Wellen aus. Zwar haben geführte Wellen eine relativ große Reichweite innerhalb des Bauteils und ermöglichen so eine großflächige Prüfung, ihre multimodalen und dispersiven Eigenschaften erschweren jedoch die Analyse der vom Schaden kommenden Reflexionen. Eine Möglichkeit, die Messsignale zu interpretieren und die Schäden zu charakterisieren, ist deren Vergleich mit der Wellenausbreitung in einem digitalen Modell. Hierbei stellt sich die Aufgabe, den Schaden im digitalen Modell anhand der Messdaten zu rekonstruieren. Diese Rekonstruktion beschreibt ein inverses Problem, das mehrere Vorwärtsrechnungen braucht, um das Schadensmodell an die Messdaten anzupassen. Durch die kleine Wellenlänge von Ultraschallwellen sind klassische Vorwärtsmethoden wie die Finte Elemente Methode rechenintensiv, weshalb die Autoren die semi-analytische Scaled Boundary Finite Element Method (SBFEM) benutzen, um den Rechenaufwand zu verringern. Im Beitrag wird ein inverses Verfahren basierend auf dem Automatischen Differenzieren in Kombination mit der SBFEM vorgestellt und an verschiedenen Schadenstypen in 2D-Querschnittmodellen von Wellenleitern getestet. In der präsentierten Vorstudie werden dafür „Messdaten“ aus unabhängigen Simulationen verwendet. T2 - DAGA 2021 - 47. Jahrestagung für Akustik CY - Vienna, Austria DA - 15.08.2021 KW - SBFEM KW - Inverse Probleme KW - SHM KW - NDT KW - AD PY - 2021 SP - 1 EP - 4 PB - Deutsche Gesellschaft für Akustik (DEGA) CY - Berlin AN - OPUS4-53305 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tannenberg, Robert T1 - Detection of Cardiac Troponin I with Chemiluminescence Biosensor N2 - Cardiovascular diseases are the number one cause of death worldwide and responsible for 3.9 million deaths in Europe and over 1.8 million deaths in the European Union (2017) [1]. Cardiac Troponin I (cTnI) is part of a triple protein complex and the most important biomarker for acute events such as heart attacks. Once a heart attack occurs, the blood stream within the heart is interrupted and further oxygen supply cannot be maintained. As a result, heart cells undergo apoptosis and their proteins will be released into the blood stream. Within the project CardioMet of the European Metrology Program of Research and Innovation (EMPIR) a biosensor for online-monitoring of acute myocardial infarction by detecting cTnI is being developed. T2 - SALSA Make and Measure 2021 CY - Online meeting DA - 16.09.2021 KW - Sensor KW - Luminol KW - ECL KW - Peroxidase KW - Monolith KW - Lab on a Chip KW - EMPIR KW - 18HTL10 KW - CardioMet KW - Horizon 2020 PY - 2021 AN - OPUS4-53306 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ecke, Alexander T1 - An Electrochemical Immunosensor for Pharmaceutical Contaminants in Water N2 - Contamination of drinking water with pharmaceuticals is an emerging problem and a potential health threat. Immunochemical methods based on the binding of the analyte to specific antibodies enable fast & cost-effective on-site analyses. Magnetic bead-based immunoassays allow for implementation into an immunosensor for online testing. Particles are prepared by either coupling the analyte molecule (diclofenac) or the respective antibody (amoxicillin) to the surface. For miniaturization, detection is performed electrochemically (chronoamperometry) on a microfluidic chip. The developed immunosensor will enable detection of pharmaceuticals directly in water supply pipes. T2 - SALSA Make & Measure CY - Online meeting DA - 16.09.2021 KW - Immunosensor KW - Magnetic Beads KW - Amoxicillin KW - Diclofenac KW - Microfluidics KW - Chronoamperometry PY - 2021 AN - OPUS4-53307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heilmann, Maria A1 - Simões, R. G. A1 - Bernardes, C. E. S. A1 - Ramisch, Yen A1 - Bienert, Ralf A1 - Röllig, Matthias A1 - Emmerling, Franziska A1 - Minas da Piedade, M. E. T1 - Real-Time In situ XRD Study of Simvastatin Crystallization in Levitated Droplets N2 - Simvastatin (SV) is an important active pharmaceutical ingredient (API) for treatment of hyperlipidemias, which is known to exist in different crystalline and amorphous phases. It is, therefore, an interesting model to investigate how the outcome of evaporative crystallization in the contactless environment of an acoustically levitated droplet may be influenced by key experimental conditions, such as temperature, solvent properties (e.g., polarity and hygroscopicity), and dynamics of the evaporation process. Here, we describe a real-time and in situ study of simvastatin evaporative crystallization from droplets of three solvents that differ in volatility, polarity, and protic character (acetone, ethanol, and ethyl acetate). The droplet monitorization relied on synchrotron X-ray diffraction (XRD), Raman spectroscopy, imaging, and thermographic analysis. A pronounced solvent-dependent behavior was observed. In ethanol, a simvastatin amorphous gel-like material was produced, which showed no tendency for crystallization over time; in ethyl acetate, a glassy material was formed, which crystallized on storage over a two-week period to yield simvastatin form I; and in acetone, form I crystallized upon solvent evaporation without any evident presence of a stable amorphous intermediate. The XRD and Raman results further suggested that the persistent amorphous phase obtained from ethanol and the amorphous precrystallization intermediate formed in ethyl acetate were similar. Thermographic analysis indicated that the evaporation process was accompanied by a considerable temperature decrease of the droplet surface, whose magnitude and rate correlated with the solvent volatility (acetone > ethyl acetate > ethanol). The combined thermographic and XRD results also suggested that, as the cooling effect increased, so did the amount of residual water (most likely captured from the atmosphere) remaining in the droplet after the organic solvent was lost. Finally, the interpretation of the water fingerprint in the XRD time profiles was aided by molecular dynamics simulations, which also provided insights into the possible role of H2O as an antisolvent that facilitates simvastatin crystallization. KW - Simvastatin KW - In-situ KW - API KW - Crystallization PY - 2021 DO - https://doi.org/10.1021/acs.cgd.1c00509 SN - 1528-7483 VL - 21 IS - 8 SP - 4665 EP - 4673 PB - ACS Publications AN - OPUS4-53663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Möckel, J. A1 - Brangsch, J. A1 - Reimann, C. A1 - Kaufmann, Jan Ole A1 - Sack, I. A1 - Mangarova, D. B. A1 - Kader, A. A1 - Taupitz, M. A1 - Adams, L. C. A1 - Keller, S. A1 - Ludwig, A. A1 - Hamm, B. A1 - Botnar, R. M. A1 - Makowski, M. R. T1 - Assessment of Albumin ECM Accumulation and Inflammation as Novel In Vivo Diagnostic Targets for Multi-Target MR Imaging N2 - Atherosclerosis is a progressive inflammatory vascular disease characterized by endothelial dysfunction and plaque burden. Extracellular matrix (ECM)-associated plasma proteins play an important role in disease development. Our magnetic resonance imaging (MRI) study investigates the feasibility of using two different molecular MRI probes for the simultaneous assessment of ECM-associated intraplaque albumin deposits caused by endothelial damage and progressive inflammation in atherosclerosis. Male apolipoprotein E-deficient (ApoE-/-)-mice were fed a high-fat diet (HFD) for 2 or 4 months. Another ApoE-/--group was treated with pravastatin and received a HFD for 4 months. T1- and T2*-weighted MRI was performed before and after albumin-specific MRI probe (gadofosveset) administration and a macrophage-specific contrast agent (ferumoxytol). Thereafter, laser ablation inductively coupled plasma mass spectrometry and histology were performed. With advancing atherosclerosis, albumin-based MRI signal enhancement and ferumoxytol-induced signal loss areas in T2*-weighted MRI increased. Significant correlations between contrast-to-noise-ratio (CNR) post-gadofosveset and albumin stain (R2 = 0.78, p < 0.05), and signal loss areas in T2*-weighted MRI with Perls’ Prussian blue stain (R2 = 0.83, p < 0.05) were observed. No interference of ferumoxytol with gadofosveset enhancement was detectable. Pravastatin led to decreased inflammation and intraplaque albumin. Multi-target MRI combining ferumoxytol and gadofosveset is a promising method to improve diagnosis and treatment monitoring in atherosclerosis. KW - Magnetic resonance imaging KW - MRI KW - Imaging KW - Human serum albumin KW - Extracellular matrix KW - Macrophages KW - Contrast agent KW - Atherosclerotic plaques KW - Gadofosveset KW - Aneurysm PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536725 DO - https://doi.org/10.3390/biology10100964 VL - 10 IS - 10 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-53672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sennikov, P. A1 - Ermakov, A. A1 - Kornev, R. A1 - Gornushkin, Igor B. T1 - Laser induced dielectric breakdown in reactive mixture SiF4 + H2 N2 - Important chemical process of reduction of SiF4 by hydrogen is realized in laser induced dielectric breakdown (LIDB) plasma in a gas mixture of SiF4 and H2. The process may be an alternative to a method of Plasma enhanced chemical vapor deposition (PECVD) which is commonly used for production of pure and isotopically pure silicon films. The composition of laser induced plasma in gases SiF4, SiF4 + H2, SiF4 + H2 + Ar at atmospheric pressure is studied and compared to the composition of inductively coupled plasma (ICP) in the same gases but at reduced pressure of 3 Torr. The gaseous products of chemical reactions are inferred from optical emission spectroscopy (OES) and IR spectroscopy. The reaction products of silicon fluoride SiF and fluorosilanes SiHxFy (x, y = 1, 2, 3) in LIDB plasma are observed and confirmed by equilibrium chemistry calculations and simulations of plasma expansion dynamics using a fluid dynamic-chemical plasma model. It is further suggested that chemisorption of fluorinated species like SiFx (x = 1, 2) followed by the surface reaction with H-atoms lead to a formation of silicon-to‑silicon bonds on a substrate surface. A conclusion is drawn that energetic laser induced plasma can prove efficient for one-step PECVD by hydrogen reduction of SiF4. KW - Silicon halides KW - Chemical vapor deposition KW - Laser induced dielectric breakdown KW - Hydrogen reduction PY - 2021 DO - https://doi.org/10.1016/j.sab.2021.106099 VL - 179 SP - 106099 PB - Elsevier B.V. AN - OPUS4-53583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Application of Diffusive Gradients in Thin-films (DGT) and spectroscopic techniques to analyze phosphorus in soils N2 - A wide range of analytical methods are used to estimate the plant-availability of soil phosphorus (P). Previous investigations showed that analytical methods based on the Diffusive Gradients in Thin films (DGT) technique provide a very good correlations to the amount of bioavailable nutrients and pollutants in environmental samples (Davison 2016, Vogel et al. 2017). However, the DGT results do not identify which P compound of the soil has the high bioavailability. But there are various spectroscopic techniques (infrared, Raman, P K-edge and L-edge XANES and P NMR spectroscopy) available to characterize P species in soils. Therefore, spectroscopic investigation of DGT binding layers after deployment allow us to determine the specific compounds. Nutrients such as phosphorus and nitrogen are often, together with other elements, present as molecules in the environment. These ions are detectable and distinguishable by infrared, P K- and L-edge X-ray absorption near-edge structure (XANES) and NMR spectroscopy, respectively. Additionally, microspectroscopic techniques make it also possible to analyze P compounds on the DGT binding layer with a lateral resolution down to 1 μm2. Therefore, species of elements and compounds of e.g. a spatial soil segment (e.g. rhizosphere) can be mapped and analyzed, providing valuable insight to understand the dynamics of nutrients in the environment. T2 - SPP1685 Closing Conference: New Approaches to Ecosystem Nutrition - Phosphorus and Beyond CY - Freiburg, Germany DA - 25.10.2021 KW - Phosphorus KW - Diffusive gradients in thin-films (DGT) KW - Passive sampling PY - 2021 AN - OPUS4-53641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling Equilibrium Chemistry in Laser Induced Plasmas and Plasma Chemical Reactors N2 - A brief introduction will be given on modeling chemical reactions in laser induced plasmas using stoichiometric and non-stoichiometric approaches. Several applications will be considered, which can benefit from such modeling. Those include plasma enhanced chemical vapor deposition (PECVD), surface modification and surface coating, and molecular analysis by LIBS. Each application will be illustrated by simulations of relevant chemical systems. For PECVD, chemical systems are BCl3/H2/Ar, BF3/H2/Ar, BCl3/BF3, Mo/BF3/H2; for surface modification/coating it is Ti/air; for molecular LIBS they are CaCO3/Ar, Ca(OH)2/Ar, and CaCl2/Ar. Advantages and shortcomings of equilibrium chemical hydrodynamic models of laser induced plasmas will be discussed. T2 - Moscow University, Department of Chemistry CY - Moscow, Russia DA - 26.10.2021 KW - Laser ablation KW - Laser induced plasma deposition KW - Emission spectroscopy KW - Surface coating KW - Hydrodynamic model KW - Plasma chemistry PY - 2021 AN - OPUS4-53629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Senoner, M. A1 - Stockmann, Jörg Manfred A1 - Fernandez, V. A1 - Fairley, N. A1 - Passiu, C. A1 - Spencer, N. D. A1 - Rossi, A. T1 - Summary of ISO/TC 201 International Standard ISO 18516:2019 Surface chemical analysis - Determination of lateral resolution and sharpness in beam-based methods with a range from nanometres to micrometres and its implementation for imaging laboratory X-ray photoelectron spectrometers (XPS) N2 - ISO 18516:2019 Surface chemical analysis—Determination of lateral resolution and sharpness in beam-based methods with a range from nanometres to micrometres revises ISO 18516:2006 Surface chemical analysis—Auger electron spectroscopy and X-ray photoelectron spectroscopy—Determination of lateral resolution. It implements three different methods delivering parameters useful to express the lateral resolution: (1) the straight edge method, (2) the narrow line method and (3) the grating method. The theoretical background of these methods is introduced in ISO/TR 19319:2013 Surface chemical analysis—Fundamental approaches to determination of lateral resolution and sharpness in beam-based methods. The revised International Standard ISO 18516 delivers standardized procedures for the determination of the (1) effective lateral resolution by imaging of square-wave gratings, the (2) lateral resolution expressed as the parameter D12–88 characterizing the steepness of the sigmoidal edge spread function (ESF) determined by imaging a straight edge and (3) the lateral resolution expressed as the full width of half maximum of the line spread function (LSF), wLSF, determined by imaging a narrow line. The last method also delivers information on the shape of the LSF, which characterizes an individual imaging instrument. Finally, the implementation of all three standardized methods in the field of imaging laboratory X-ray photoelectron spectroscopy (XPS) is shortly presented. This part of the letter is based on the use of a new test sample developed at ETH Zurich, Switzerland. This test sample displays a micrometre scaled pattern motivated by the resolving power of recent imaging XPS instruments. KW - Grating method KW - Imaging AES KW - Imaging SIMS KW - Imaging XPS KW - Lateral resolution KW - Narrow line method KW - Noise in image KW - Resolution criterion KW - Straight edge method PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536330 DO - https://doi.org/10.1002/sia.7025 SN - 1096-9918 VL - 54 IS - 4 SP - 320 EP - 327 PB - Wiley CY - Chichester AN - OPUS4-53633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Microplastic analysis using TED-GC/MS: H/D-Exchange of decomposition products of D-marked polystyrene as an internal standard N2 - Deuterated polystyrene (D-PS) improves microplastic detection with TED-GC / MS, among other things through higher reproducibility. It is inexpensive (0.1 ct / analysis) and can be dosed quickly and reproducibly thanks to its good solubility (e.g. in toluene). However, certain matrices lead to an exchange of the deuterium with hydrogen. The poster shows the measuring principle, in which matrices H/D-exchange takes place, the results of kinetic studies and ways of preventing or circumventing the H/D-exchange. T2 - SALSA MAKE AND MEASURE 2021 CY - Online meeting DA - 16.09.2021 KW - Microplastic KW - H/D-Exchange KW - Internal Standard KW - TED-GC/MS KW - Thermoanalytic PY - 2021 AN - OPUS4-53681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Towards hydrogen economy: correlative ex-situ ellipsometric analysis and operando investigation during oxygen evolution reaction of mesoporous iridium oxides films N2 - In the face of rising energy demand and the impending climate change the development of a sustainable, fossil-free fuel and chemical production is of global importance. One possible goal is the development of electrochemical conversion processes using catalysts. Porous materials play an important role in such energy applications. The key to the development of improved catalysts is a better understanding of the relations between their performance, stability and physico-chemical properties. However, the complex morphology of such catalysts constitutes a challenge even for modern analytical techniques. Spectroscopic ellipsometry (SE) is a versatile method for studying material properties by using appropriate models (e.g. film thickness, optical and electronic properties). The fact that the material properties cannot be taken directly from the measured spectra, the developed models have to be validated. In a first step, the model for the ellipsometric fit studies of a calcination series of mesoporous iridium oxide films (300 – 600 °C) was investigated and validated with respect to their material properties. Moreover, the electronic structures of the catalysts reveal a direct correlation with electrochemical activities. The development of an environmental cell offers the possibility of investigations under real conditions. This will allow changes in the optical and electronic properties during the electrocatalytic oxygen evolution reaction. T2 - Colloquium Department Seminar 6. CY - BAM, Berlin, Germany DA - 03.03.2020 KW - Hydrogen economy KW - Correlative ex-situ ellipsometric analysis KW - Ellipsometric operando investigation KW - Oxygen evolution reaction KW - Mesoporous iridium oxides films PY - 2020 AN - OPUS4-51215 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Melzer, Michael A1 - Fischer, Michael A1 - Thomas, Marcus A1 - Subaric-Leitis, Andreas A1 - Bartholmai, Matthias T1 - Calibration Service as a Gateway to Sustainable Research and Development N2 - Over decades, the German Federal Institute for Materials Research and Testing (BAM) has established a sophisticated calibration laboratory for force, temperature and electrical quantities. Since more than 15 years it is accredited, currently by the national accreditation body (DAkkS), and offers its service also to external entities on a global scale. As a public provider, we are furthermore committed to research and development activities that demand measurements with highest quality and low level of uncertainties. Two R&D examples are highlighted within this contribution. T2 - SMSI 2020 CY - Meeting was canceled DA - 22.06.2020 KW - Calibration of force KW - Calibration of temperature KW - Calibration of electrical quantities KW - Measurement uncertainty KW - New sensor principles PY - 2020 SN - 978-3-9819376-2-6 DO - https://doi.org/10.5162/SMSI2020/E3.3 SP - 374 EP - 375 AN - OPUS4-51222 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Song, L. A1 - You, Yi A1 - Perdomo, R. A1 - Evans-Nguyen, T. T1 - Inexpensive Ultrasonic Nebulization Coupled with Direct Current Corona Discharge Ionization Mass Spectrometry for Liquid Samples and Its Fundamental Investigations N2 - The concept of direct mass-spectrometric analysis, especially exploited by ambient desorption/ionization (ADI) methods, provides numerous means for convenient sample analysis. While many simple and versatile ionization sources have been developed, challenges lay in achieving efficient sample introduction. In previous work, a sample introduction method employing direct current corona discharge (CD) coupled to a surface acoustic wave nebulization (SAWN) device enhanced sampling performance for both polar and nonpolar analytes by up to 4 orders of magnitude. In fact, the SAWN-CD method generated a multiply charged peptide ion signal comparable to that of conventional ESI. Unfortunately, the high cost of the SAWN devices themselves limits their accessibility. Herein, we report on an analogous implementation of CD with an inexpensive ultrasonic nebulizer (USN) on the basis of a commercial room humidifier demonstrating equivalent exemplary performance. We subsequently compare the two methods of SAWN-CD and USN-CD in a screening application of milk for the detection of two antibiotic drugs, ciprofloxacin and ampicillin. Finally, we further investigate the relative softness of these CD-coupled acoustic nebulization methods in comparison to that of ESI using a survival yield study of the thermometer ion nitrobenzylpyridinium. KW - Rapid Analysis KW - Ultrasonic Nebulization KW - Corona Discharge PY - 2020 DO - https://doi.org/10.1021/acs.analchem.0c00524 VL - 92 IS - 16 SP - 11072 PB - ACS Publication AN - OPUS4-51225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nitsche, Michael T1 - Federal Research & development supports market surveillance N2 - Example: Testing and rating of heat pumps and air conditioners Example: Surveillance of Toys Example: Safety of compressed gas storage vessels for Hydrogen T2 - EU Market Surveillance Conference 2020 CY - Online meeting DA - 05.11.2020 KW - Market surveillance PY - 2020 AN - OPUS4-51930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Solovyev, N. A1 - El-Khatib, Ahmed A1 - Costas-Rodrigues, M. A1 - Schwab, K. A1 - Griffin, E. A1 - Raab, A. A1 - Platt, B. A1 - Theuring, F. A1 - Vogl, Jochen A1 - Vanhaecke, F. T1 - Cu, Fe and Zn isotope ratios in murine Alzheimer's disease models suggest specific signatures of amyloidogenesis and tauopathy N2 - Alzheimer’s disease (AD) is characterized by accumulation of tau and amyloid-beta in the brain, and recent evidence suggests a correlation between associated protein aggregates and trace elements, such as copper, iron and zinc. In AD, distorted brain redox homeostasis and complexation by amyloid-beta and hyperphosphorylated tau May alter the isotopic composition of essential mineral elements. Therefore, high-precision isotopic analysis may reveal changes in the homeostasis of these elements. We used inductively coupled plasma-mass spectrometry (ICP-MS)-based techniques to determine the total Cu, Fe and Zn contents in the brain, as well as their isotopic compositions in both mouse brain and serum. Results for male transgenic tau (Line 66, L66) and amyloid/presenilin (5xFAD) mice were compared to those for the corresponding age- and gendermatched wild-type control mice (WT). Our data show that L66 brains showed significantly higher Fe levels than the corresponding WT. Significantly less Cu, but more Zn was found in 5xFAD brains. We observed significantly lighter isotopic compositions of Fe (enrichment in the lighter isotopes) in the brain, and in serum of L66 mice compared to WT. For 5xFAD mice, Zn exhibited a trend towards a lighter isotopic composition in brain and a heavier isotopic composition in serum compared to WT. Neither mouse model yielded differences in the isotopic composition of Cu. Our findings indicate significant pathology-specific alterations of Fe and Zn brain homeostasis in mouse models of AD. The associated changes in isotopic composition May serve as a marker for proteinopathies Underlying AD and other types of dementia. KW - Alzheimer’s disease KW - Tau KW - Amyloid-beta KW - Copper KW - Iron KW - Zinc KW - Multi-collector inductively coupled plasma-mass spectrometry (ICP-MS) KW - Brain KW - Serum KW - Isotopic analysis KW - Total element determination PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520214 DO - https://doi.org/10.1016/j.jbc.2021.100292 VL - 296 SP - 100292 PB - Elsevier Inc. CY - Amsterdam AN - OPUS4-52021 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Kricheldorf, H. R. A1 - Scheliga, F. T1 - Ring-expansion copolymerization of L-lactide and glycolide N2 - 1:1 Copolymerizations of glycolide (GL) and L-lactide (LA) is performed in bulk at 100°C and at 160°C with four cyclic tin catalysts. The resulting copolyesters are characterized by SEC measurements, 1H and 13C NMR spectroscopy and by MALDI TOF mass spectrometry. At 160°C and longer reaction time (22 h) nearly complete conversion of both monomers is achieved, and cyclic copolymers with nearly random sequences are formed. At shorter times (0.5-3.0 h, depending on catalyst) the conversion of LA is incomplete, and only cyclics having even numbers of lactyl units are obtained. At 100°C at 22 h again cycles mainly consisting of even numbered lactyl units are formed, but with even and odd numbers of glycolyl units. Copolymerization of lactide at 160°C with small amounts of GL show that formation of high Tm crystallites (Tm > 190°C) is hindered even when only > 2% of GL is added. For polyglycolide containing a smaller amount of lactide complete solubility in hexafluoroisopropanol is only observed around and above 20 mol% of lactide. KW - Ring-expansion polymerization KW - Copolymerization KW - MALDI-TOF MS KW - L-lactide KW - Glycolide KW - Crystallization PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520270 DO - https://doi.org/10.1002/macp.202000307 SN - 1022-1352 VL - 22 IS - 3 SP - 307 PB - WileyVCH AN - OPUS4-52027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Becker, S. A1 - Beckmann, Jörg A1 - Cojocari, O. A1 - Feige, V. A1 - Fischer, B. A1 - Friederich, F. A1 - Globisch, B. A1 - Hechtfischer, G. A1 - Hens, K. A1 - Hübers, H.-W. A1 - Jelonnek, J. A1 - Jonuscheit, J. A1 - Keil, A. A1 - Kleine-Ostmann, T. A1 - Mayr, M. A1 - Nüßler, D. A1 - Peichl, M. A1 - Peters, O. A1 - Schür, J. A1 - Sprenger, T. A1 - Steiger, A. A1 - van Frank, S. A1 - Vieweg, N. A1 - Wilk, R. T1 - Terahertzsysteme - Zeitbereichsspektrometer (TDS-Systeme) N2 - Diese Richtlinie definiert Kenngrößen und Messverfahren, um Terahertzsysteme für die Zeitbereichsspektroskopie (TDS)zu spezifizieren. So können Hersteller ihre Systeme übereinstimmend beschreiben und Anwender einfach Systeme vergleichen. Systeme für die Terahertz-Zeitbereichsspektroskopie sind aktive Systeme und nutzen verschiedene Techniken sowohl zur Erzeugung als auch zur zeitaufgelösten Messung von breitbandigen Terahertzimpulsen. Die dazugehörigen Terahertzspektren und -Phasen werden nach einer zeitlichen Abtastung über eine Fourier-Transformation berechnet. In dieser Richtlinie wird ein Überblick über die Funktionsweisen von Zeitbereichsspektrometern gegeben, die eingesetzten Messverfahren näher erläutert sowie die benötigten Begriffe und Kenngrößen definiert. Die Richtlinie konzentriert sich dabei auf Systeme, die auf sogenannten Abtastmessverfahren (Sampling-Messverfahren) basieren. KW - TDS-Systeme PY - 2020 UR - https://www.vdi.de/5590 VL - VDI/VDE 5590 Blatt 2 SP - 1 EP - 22 PB - VDI-Verlag CY - Düsseldorf ET - Entwurf - Oktober 2020 AN - OPUS4-51947 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kader, A. A1 - Brangsch, J. A1 - Kaufmann, Jan Ole A1 - Zhao, J. A1 - Mangarova, D. B. A1 - Moeckel, J. A1 - Adams, L. C. A1 - Sack, I. A1 - Taupitz, M. A1 - Hamm, B. A1 - Makowski, M. R. T1 - Molecular MR Imaging of Prostate Cancer N2 - This review summarizes recent developments regarding molecular imaging markers for magnetic resonance imaging (MRI) of prostate cancer (PCa). Currently, the clinical standard includes MR imaging using unspecific gadolinium-based contrast agents. Specific molecular probes for the diagnosis of PCa could improve the molecular characterization of the tumor in a non-invasive examination. Furthermore, molecular probes could enable targeted therapies to suppress tumor growth or reduce the tumor size. KW - Prostate cancer KW - Magnetic resonance imaging KW - Molecular imaging KW - Imaging KW - Molecular marker KW - Screening KW - MRI KW - Diagnosis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519503 DO - https://doi.org/10.3390/biomedicines9010001 VL - 9 IS - 1 SP - 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-51950 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - High molecular weight poly(l-lactide) via ring-opening polymerization with bismuth subsalicylate-The role of cocatalysts N2 - The catalytic potential of bismuth subsalicylate (BiSub), a commercial drug, for ring-opening polymerization (ROP) of L-lactide was explored by variation of co-catalyst and polymerization time. Various monofunctional phenols or carboxylic acids, aromatic ortho-hydroxy acids and diphenols were examined as potential co-catalysts. 2,2´-Dihydroxybiphenyl proved to be the most successful co-catalyst yielding weight average molecular weights (uncorrected Mw values up to 185 000) after optimization of reaction time and temperature. Prolonged heating (>1-2h) depending on catalyst concentration) caused thermal degradation. In polymerization experiments with various commercial Bi(III) salts a better alternative to BiSub was not found. By means of matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry a couple of unusual and unexpected transesterification reactions were discovered. Finally, the effectiveness of several antioxidants and potential catalyst poisons was explored, and triphenylphosphine was found to be an effective catalyst poison. KW - Polylactide KW - MALDI-TOF MS KW - Ring-opening polymerization KW - Bismuth PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519513 DO - https://doi.org/10.1002/app.50394 SN - 0021-8995 VL - 138 IS - 19 SP - 50394 PB - Wiley AN - OPUS4-51951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Nisi, A. A1 - Koch, Claudia A1 - Mirtsch, Mona A1 - Blind, K. T1 - Effetti della pandemia COVID-19 sulle attività di valutazione della conformità svolte da organismi e laboratori accreditati in Italia N2 - Die Studie fasst Ergebnisse einer Befragung von Konformitätsbewertungsstellen in Italien zu deren Lage und den Aussichten während der Corona-Pandemie zusammen. Besondere Schwerpunkte wurden auf die wirtschaftlichen Auswirkungen und die Arbeitsfähigkeit, aber auch auf die Resilienz und die Wirkungen auf die Digitalisierung gelegt. N2 - Lo scoppio della pandemia da Covid-19 ha travolto Italia a inizio anno e i suoi effetti sull’economia sono stati particolarmente pesanti. Proprio per analizzare gli effetti della pandemia sul mercato della valutazione della conformità, lo scorso settembre Accredia, in collaborazione con l’Istituto Federale tedesco della Ricerca e del Collaudo dei Materiali (BAM), la Technische Universität di Berlino e l’Istituto Fraunhofer ISI, ha condotto un’indagine presso gli organismi e i laboratori accreditati in Italia. KW - Corona KW - Konformitätsbewertungsstellen KW - Resilienz KW - COVID-19 KW - Qualitätsinfrastruktur KW - Zertifizierung KW - Kalibrierung KW - Digitalisierung KW - Konformitätsbewertung KW - Laboratorium KW - Prüfung PY - 2020 UR - https://www.accredia.it/pubblicazione/corona-monitor-effetti-della-pandemia-da-covid-19-sulle-attivita-accreditate/ SP - 1 EP - 22 CY - Rom, Italien AN - OPUS4-51975 LA - ita AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - Psychology at BAM: Is it science and how can we benefit from it? N2 - The aim of this presentation is twofold: first, to present the field of psychology including its research methods and, second, to show on an example how psychology can be used in material research. The example is of the study of human factors in non-destructive testing (NDT), in which the author has more than 10 years of experience. The conclusion is that psychological methods can be used to identify human-related problems during different tasks and to generate mitigation strategies that can be used to decrease human error and enhance safety. T2 - Abteilungsseminar der Abteilung 8 CY - Berlin, Germany DA - 20.04.2020 KW - Psychology KW - Human factors KW - Non-destructive testing (NDT) KW - Safety PY - 2020 AN - OPUS4-51920 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - Human machine interaction in the era of industry 4.0 N2 - The fourth industrial revolution (also known as “Industry 4.0”) promises to relieve people from manual and physical work by developing cyber-physical systems and smart automation and thereby achieving a more efficient, reliable and safe performance. This will change people’s work from being operators of the system into becoming strategical decision makers and flexible problem solvers. This shift will require a new division of work between people and technical systems, a new division of responsibilities and new ways of interacting with technology, which in turn will pose new demands on people. People will require different physical and cognitive capabilities, different competencies and new strategies to cope with the upcoming challenges. The focus of Industry 4.0 is therefore on designing systems with human in the centre: systems that will extend people’s capabilities, that will allow collaborative work and take advantage of performances in which either people or technology excel. This presentation will focus on the benefits of consideration of human-machine interaction in the context of industry 4.0. T2 - Les assises de L’Industrie 4.0 CY - INSA Centre Val de Loire, Campus de Blois, France DA - 29.09.2020 KW - Human machine interaction KW - Industry 4.0 KW - NDT 4.0 KW - Safety KW - non-destructive testing (NDT) PY - 2020 AN - OPUS4-51921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schoonjans, Tom A1 - Brunetti, A. A1 - Golosio, B. A1 - Sanchez del Rio, M. A1 - Solé, V. A. A1 - Ferrero, C. A1 - Vincze, L. T1 - xraylib 3.1.0 N2 - Quantitative estimate of elemental composition by spectroscopic and imaging techniques using X-ray fluorescence requires the availability of accurate data of X-ray interaction with matter. Although a wide number of computer codes and data sets are reported in literature, none of them is presented in the form of freely available library functions which can be easily included in software applications for X-ray fluorescence. This work presents a compilation of data sets from different published works and an xraylib interface in the form of callable functions. Although the target applications are on X-ray fluorescence, cross sections of interactions like photoionization, coherent scattering and Compton scattering, as well as form factors and anomalous scattering functions, are also available. xraylib provides access to some of the most respected databases of physical data in the field of x-rays. The core of xraylib is a library, written in ANSI C, containing over 40 functions to be used to retrieve data from these databases. This C library can be directly linked with any program written in C, C++ or Objective-C. Furthermore, the xraylib package contains bindings to several popular programming languages: Fortran 2003, Perl, Python, Java, IDL, Lua, Ruby, PHP and .NET, as well as a command-line utility which can be used as a pocket-calculator. Although not officially supported, xraylib has been reported to be useable from within Matlab and LabView. The source code is known to compile and run on the following platforms: Linux, Mac OS X, Solaris, FreeBSD and Windows. Development occurs on Github: http://github.com/tschoonj/xraylib Downloads are hosted by the X-ray Micro-spectroscopy and Imaging research group of Ghent University: http://lvserver.ugent.be/xraylib Version 3.1.0 release notes: - Database of commonly used radionuclides for X-ray sources added (new API: GetRadioNuclideDataByName, GetRadioNuclideDataByIndex, GetRadioNuclideDataList and FreeRadioNuclideData) - numpy Python bindings added, generated with Cython. Performance basically the same as the core C library. (suggested by Matt Newville) - docstring support added to Python bindings (suggested by Matt Newville) - Windows SDKs now have support for Python 3.4. - Windows 64-bit SDK now comes with IDL bindings - Confirmed support for LabView (thanks to Dariush Hampai!) - Universal Intel 32/64 bit Framework built for Mac OS X - Perl support for Debian/Ubuntu - Several bugfixes: thanks to those that reported them! KW - Quantitative estimation KW - Elemental composition KW - Spectroscopic techniques KW - Imaging techniques PY - 2014 DO - https://doi.org/10.5281/zenodo.12378 PB - Zenodo CY - Geneva AN - OPUS4-51924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schoonjans, Tom A1 - Vincze, L. A1 - Solé, V. A. A1 - Sanchez del Rio, M. A1 - Brondeel, P. A1 - Silversmit, G. A1 - Appel, K. A1 - Ferrero, C. T1 - XMI-MSIM 5.0 N2 - XMI-MSIM is an open source tool designed for predicting the spectral response of energy-dispersive X-ray fluorescence spectrometers using Monte-Carlo simulations. It comes with a fully functional graphical user interface in order to make it as user friendly as possible. Considerable effort has been taken to ensure easy installation on all major platforms. Development of this package was part of my PhD thesis. The algorithms were inspired by the work of my promotor Prof. Laszlo Vincze of Ghent University. Links to his and my own publications can be found in our manual. A manuscript has been published in Spectrochimica Acta Part B that covers the algorithms that power XMI-MSIM. Please include a reference to this publication in your own work if you decide to use XMI-MSIM for academic purposes. A second manuscript was published that covers our XMI-MSIM based quantification plug-in for PyMca. Soon information on using this plug-in will be added to the manual. XMI-MSIM is released under the terms of the GPLv3. Development occurs at Github: http://github.com/tschoonj/xmimsim Downloads are hosted by the X-ray Micro-spectroscopy and Imaging research group of Ghent University: http://lvserver.ugent.be/xmi-msim Version 5.0 release notes: Changes: 1. Custom detector response function: build a own plug-in containing your own detector response function and load it at run-time to override the builtin routines. Instructions can be found in the manual. 2. Escape peak improvements: new algorithm is used to calculate the escape peak ratios based on a combined brute-force and variance-reduction approach. Ensures high accuracy even at high incoming photon energies and thin detector crystals. Downside: it's slower… 3. Removed maximum convolution energy option. Was a bit confusing anyway. 4. Number of channels: moved from simulation controls into input-file 5. Radionuclide support added: Now you can select one or more commonly used radionuclide sources from the X-ray sources widget. 6. Advanced Compton scattering simulation: a new alternative implementation of the Compton scattering has been implemented based on the work of Fernandez and Scot (http://dx.doi.org/10.1016/j.nimb.2007.04.203), which takes into account unpopulated atomic orbitals. Provides an improved simulation of the Compton profile, as well as fluorescence contributions due to Compton effect (extremely low!), but slows the code down considerably. Advanced users only. Default: OFF 7. Plot spectra before convolution in results 8. Windows: new Inno Setup installers. Contains the headers and import libraries 9. Windows: compilers changed to GCC 4.8.1 (TDM-GCC) 10. Windows: rand_s used to generate seeds on 64-bit version (requires Vista or later) 11. Windows: new gtk runtime for the 64-bit version (see also https://github.com/tschoonj/GTK-for-Windows-Runtime-Environment-Installer) 12. Mac OS X: compilers changed to clang 5.1 (Xcode) and gfortran 4.9.1 (MacPorts) 13. Original input-files from our 2012 publication (http://dx.doi.org/10.1016/j.sab.2012.03.011) added to examples 14. Updater performs checksum verification after download 15. X-ray sources last used values stored in preferences.ini 16. xmimsimdata.h5 modified: even bigger now... Bugfixes: 1. Windows: support for usernames with unicode characters. Fixed using customized builds of HDF5. Thanks to Takashi Omori of Techno-X for the report! 2. Spectrum import from file fixes. Was never properly tested apparently Note: For those that compiled XMI-MSIM from source: you will need to regenerate the xmimsimdata.h5 file with xmimsim-db. Old versions of this file will not work with XMI-MSIM 5.0. KW - Spectral response KW - Energy-dispersive X-ray fluorescence spectrometers KW - Monte-Carlo simulations PY - 2014 DO - https://doi.org/10.5281/zenodo.12381 PB - Zenodo CY - Geneva AN - OPUS4-51925 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Molloy, J. L. A1 - Winchester, M. R. A1 - Butler, T. A. A1 - Possolo, A. M. A1 - Rienitz, O. A1 - Roethke, A. A1 - Goerlitz, V. A1 - Caciano de Sena, R. A1 - Dominguez Almeida, M. A1 - Yang, L. A1 - Methven, B. A1 - Nadeau, K. A1 - Romero Arancibia, P. A1 - Bing, W. A1 - Tao, Z. A1 - Snell, J. A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Kotnala, R. K. A1 - Swarupa Tripathy, S. A1 - Elishian, C. A1 - Ketrin, R. A1 - Suzuki, T. A1 - Oduor Okumu, T. A1 - Yim, Y.-H. A1 - Heo, S. W. A1 - Min, H. S. A1 - Sub Han, M. A1 - Lim, Y. A1 - Velina Lara Manzano, J. A1 - Segoviano Regalado, F. A1 - Arvizu Torres, M. A1 - Valle Moya, E. A1 - Buzoianu, M. A1 - Sobina, A. A1 - Zyskin, V. A1 - Sobina, E. A1 - Migal, P. A1 - Linsky, M. A1 - Can, S. Z. A1 - Ari, B. A1 - Goenaga Infante, H. T1 - CCQM-K143 Comparison of Copper Calibration Solutions Prepared by NMIs/DIs N2 - CCQM-K143 is a key comparison that assesses participants’ ability to prepare single element calibration solutions. Preparing calibration solutions properly is the cornerstone of establishing a traceability link to the International System of Units (SI), and therefore should be tested in order to confirm the validity of CCQM comparisons of more complex materials. CCQM-K143 consisted of participants each preparing a single copper calibration solution at 10 g/kg copper mass fraction and shipping 10 bottled aliquots of that solution to the coordinating laboratory, the National Institute of Standards and Technology (NIST). The masses and mass fraction for the prepared solutions were documented with the submitted samples. The solutions prepared by all participants were measured at NIST by high performance inductively coupled plasma optical emission spectroscopy (HP-ICP-OES). The intensity measurements for copper were not mapped onto values of mass fraction via calibration. Instead, ratios were computed between the measurements for copper and simultaneous measurements for manganese, the internal standard, and all subsequent data reductions, including the computation of the KCRV and the degrees of equivalence, were based on these ratios. Other than for two participants whose measurement results appeared to suffer from calculation or preparation errors, all unilateral degrees of equivalence showed that the measured values did not differ significantly from the KCRV. These results were confirmed by a second set of ICP-OES measurements performed by the Physikalisch-Technische Bundesanstalt (PTB). CCQM-K143 showed that participants are capable of preparing calibration solutions starting from high purity, assayed copper metal. Similar steps are involved when preparing solutions for other elements, so it seems safe to infer that similar capabilities should prevail when preparing many different, single-element solutions. KW - Metrology KW - Primary calibration solution KW - Traceability PY - 2020 DO - https://doi.org/10.1088/0026-1394/58/1A/08006 SN - 0026-1394 VL - 58 IS - 1A SP - 08006 PB - IOP Science CY - Cambridge AN - OPUS4-51983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Molecule formation in reactive LIBS plasmas: model and experiment N2 - Formation and detection of molecules in laser induced plasmas (LIP) is a hot topic. In analytical plasmas like LIBS, the detection of molecules is important for identification of geological and other materials, analysis of isotopes and difficult elements (Cl, F, etc.) via molecular emission. In chemical plasmas, like PECVD (plasma enhanced chemical vapor deposition) or PLD (pulsed laser deposition), molecules formed in the plasma determine a composition and a thickness of deposits. Similarly, molecules play an important role in microstructuring and oxidizing metal surfaces by laser ablation. It is unfortunate that different communities, which utilize plasma methods and seek for solutions of similar problems, do not strongly overlap, and do not fully use knowledge accumulated by each other. In this presentation, mechanisms of formation of molecules will be analyzed on the example of LIPs used for chemical vapor deposition and metal microstructuring. Theoretical analysis includes equilibrium chemistry calculations combined with plasma hydrodynamics. First, LIP excited in a gas mixture of BCl3 or BF3 with H2 or CH4 will be analyzed; this chemical system is used for obtaining deposits of refractory solid boron and boron carbide. Second, a breakdown in the SiF4 + SiCl4 gas mixtures will be described; this method allows synthesis of fluorochlorosilanes SiFxCl4-x (x = 1, 2, 3), the good etching agents (Figure). Third, solid ablation of Mo in BF3+H2 and Ti in air will be considered aimed at obtaining deposits of high hardness MoxBy and films of TixOy on textured Ti surfaces, correspondingly. In experiment, reaction gases before and after laser illumination, and solid deposits are analyzed by optical emission spectroscopy (OES), IR and mass spectrometry (MS), SEM, X-ray, and AFM. It will be shown that the hydrodynamic-chemical model adequately predicts the composition of LIPs, zones of molecular formation, dependence on reactant stoichiometry, plasma temperature and pressure. T2 - Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy CY - Gijon, Spain DA - 29.11.2021 KW - Laser induced plasma KW - Plasma chemistry KW - Molecules formation KW - Plasma enhanced chemical deposition PY - 2021 AN - OPUS4-53850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Küttenbaum, Stefan T1 - Zur Validierung von zerstörungsfreien Messverfahren für die probabilistische Beurteilung von Bestandsbauwerken mit gemessenen Daten T1 - Validation of non-destructive measurement procedures for reliability assessments of existing structures using measured data N2 - The aging of existing bridge structures coincides with the progressing degradation and increasing requirements on the bridge stock caused by increasing traffic densities as well as heavy traffic. The resulting demand for structural assessments of existing bridges is of substantial importance, both nationally and internationally. The information available about the considered system provides the basis for reassessments. Both the structural reliability and the validity of the computation results depend primarily on the condition, i.e. the quality and the relevance of this information. The purposeful measurement of quality-evaluated and relevant information can significantly increase the engineer’s power of judgement regarding the structural reliability. It is advisable to keep the destructive structural interventions necessary to obtain such information to a minimum. The purpose of the present thesis is the development and evaluation of a methodology for the probabilistic reassessment of existing structures using non-destructively measured data and for the validation of the suitability of non-destructive measurement procedures for the application in the context of reassessments. For this purpose, the applicability of the rules established within the Guide to the Expression of Uncertainty (GUM)-framework for evaluating the quality of the measured information to be used later in the reassessment is emphasized. The requirements on measured data-based basic variables are derived from the First Order Reliability Method (FORM), a probabilistic approximation procedure. Based on this, the metrology and the reassessment are brought together. The measurement-based basic variables are explicitly appreciated as random variables in reliability analyses. The developed methodology is evaluated by means of two prestressed concrete bridges and four basic variables. Geometrical measurement results gathered by radar and ultrasound measurements are incorporated into reassessments regarding the limit states ULS bending, ULS shear and SLS decompression. The modelling of the measurements is an essential part in order to calculate the measurement results, each consisting of a measured value and the attributed measurement uncertainty. It is shown that the incorporation of the non-destructively collected measurement results reduces the uncertainty to be covered and increases the level of approximation of the considered models. The measurement results are reliable and comparable. Extensive sensitivity analyses provide information about crucial structure parameters to be measured, since they significantly influence the structural reliability. This way, the relevance of the information is derived. Such analyses are suitable for the design and commissioning of investigations meeting the demands as well as for the purposeful refinement of initially insufficient computation models. Furthermore, the appreciation of measured data-based basic variables can increase the robustness of structural analyses. Measurement-based reliability reassessments are particularly useful if required information is missing or doubts have arisen about the available information. In the best case, the incorporation of non-destructively measured data results in the extension of estimated remaining service lives, in the enhancement of infrastructural availabilities and in the optimization of the consumption of resources. N2 - Die Alterung bestehender Brückenbauwerke fällt mit dem sich verschlechternden Zustand und zunehmenden Anforderungen an die Bausubstanz zusammen, die eine Folge von steigenden Verkehrszahlen und der Zulassung des Schwerlastverkehrs sind. Der daraus erwachsende Bedarf an Beurteilungen von bestehenden Brücken ist national und international fortwährend groß. Die Grundlage für Nachrechnungen sind die über das System verfügbaren Informationen. Sowohl die rechnerische Zuverlässigkeit eines Tragwerks als auch die Validität der Ergebnisse hängen im Wesentlichen vom Zustand, also von der Qualität und der Relevanz dieser Informationen ab. Die gezielte Messung von gütebewerteten, relevanten Informationen kann die Urteilsfähigkeit des Beurteilenden über die Zuverlässigkeit eines Tragwerks signifikant steigern. Wünschenswert ist die Erhebung derartiger Informationen ohne signifikante Eingriffe in die Bausubstanz. Das Ziel der vorliegenden Arbeit ist die Entwicklung und Erprobung einer Vorgehensweise für die probabilistische Beurteilung von bestehenden Bauwerken mit zerstörungsfrei gemessenen Daten und einer Methodik zum objektiven Nachweis der Eignung von zerstörungsfreien Messverfahren zur Anwendung im Zuge einer Nachrechnung. Herausgestellt wird die Eignung der im Guide to the Expression of Uncertainty in Measurement (GUM) publizierten Regeln zur Bewertung der Qualität der gemessenen Informationen, die später im statischen Nachweis verwendet werden sollen. Die Anforderungen an die Basisvariablen, d. h. an die Eingangsgrößen im probabilistischen Nachweis, werden aus den Vorschriften zur Zuverlässigkeitsanalyse mit dem probabilistischen Näherungsverfahren FORM, der First Order Reliability Method, abgeleitet. Darauf basiert die Entwicklung der Schnittstelle zwischen der Messtechnik und der Nachrechnung. Im Kern werden die messdatenbasierten Basisvariablen explizit als Zufallsgrößen bei der Zuverlässigkeitsanalyse berücksichtigt. Die entwickelte Vorgehensweise wird am Beispiel von zwei Spannbetonbrücken und vier Basisvariablen erprobt. In die Nachweise der Biege- und der Querkrafttragfähigkeit sowie in einen Nachweis der Dekompression fließen geometrische Messergebnisse ein, die mithilfe von Radar- und Ultraschallmessungen generiert werden. Ein wichtiger Bestandteil ist die Bildung von Modellen zur Auswertung der Messungen und zur Berechnung der Messergebnisse. Es wird gezeigt, dass die Einbeziehung der zerstörungsfrei generierten Messergebnisse die Unsicherheit in den Berechnungsmodellen reduzieren und den Grad der Annäherung der Modelle an die Realität steigern kann. Die Messergebnisse sind zuverlässig und vergleichbar. Umfassende Sensitivitätsanalysen geben Aufschluss über sinnvollerweise zu messende Bauwerksparameter, die einen maßgeblichen Einfluss auf die Tragwerkszuverlässigkeit ausüben. Auf diese Weise wird die Relevanz der Informationen ermittelt. Das Potential derartiger Analysen für die gezielte Planung und Beauftragung von Messungen sowie für die bedarfsgerechte Zuschärfung von initial unzureichenden Berechnungsmodellen erscheint groß. Die messdatenbasierten Modelle können darüber hinaus die Robustheit einer Tragwerksanalyse steigern. Die Berücksichtigung von Messergebnissen ist dann besonders nützlich, wenn zur Beurteilung erforderliche Informationen fehlen oder Zweifel an den verfügbaren Informationen aufgekommen sind. Im besten Fall resultiert daraus die Verlängerung von rechnerischen Restnutzungsdauern, die Steigerung der Verfügbarkeit der Infrastruktur, die Optimierung des Ressourcenverbrauchs und insgesamt eine realitätsnahe Bauwerksbewertung. KW - Zerstörungsfreie Prüfung im Bauwesen KW - Nachrechnung KW - Spannbetonbrücken KW - Zuverlässigkeitsanalyse KW - Messunsicherheit PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:bvb:706-7686 SN - 1431-5122 VL - 21/2 SP - I EP - 314 PB - Universität der Bundeswehr München CY - Neubiberg AN - OPUS4-53851 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - von der Au, Marcus A1 - Meermann, Björn T1 - Dem Leben auf der Spur – Einzelzellanalytik N2 - Zellen, als Grundeinheit für Organismen, bilden einen wesentlichen Eckpfeiler für das Leben. Die Untersuchung von einzelnen Zellen liefert wertvolle Einblicke in fundamentale Prozesse des Lebens. So können Anomalien auf der Zelleebene Indikatoren für Krankheiten sein und durch eine Analyse früh erkannt werden. Weiterhin kann durch ein tiefgreifendes Verständnis von Vorgängen in Zellen auch gezielt Forschung zu z.B. neuen Medikamenten betrieben werden. Damit können die Wirksamkeit erhöht und die Nebenwirkungen reduziert werden. KW - SC-ICP-MS KW - Algen KW - Cispaltin PY - 2021 UR - https://faszinationchemie.de/wissen-und-fakten/news/dem-leben-auf-der-spur-einzelzellanalytik/ SP - 1 EP - 4 AN - OPUS4-53859 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Uncertainty budgets in surface technology: stepheigt, layerthickness, indentation hardness, adehesive strength N2 - The object (sample) and the measurement/testing procedure may always have unknown degrees of freedom, i.e. instead of 𝐯 ≥ n – 1 in many cases 𝐯 ≫ n - 1 may apply, in particular in the micro- and nano-world! T2 - 10. VDI-Fachtagung, Messunsicherheit und Prüfprozesse CY - Erfurt, Germany DA - 10.11.2021 KW - Methodology in metrology KW - Methodology in testing KW - Spectroscopic Ellipsometry KW - Instrumented Indentation Testing (IIT) KW - Centrifugal Adhesion Testing (CAT) PY - 2021 AN - OPUS4-53986 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Moor, Maëlle A1 - Kraehnert, Ralph A1 - Hodoroaba, Vasile-Dan A1 - Hertwig, Andreas T1 - Ellipsometry-based approach for the characterization of mesoporous thin films for H2 technologies N2 - Porous thin layer materials are gaining importance in different fields of technology and pose a challenge to the accurate determination of materials properties important for their function. In this work, we demonstrate a hybrid measurement technique using ellipsometry together with other independent methods for validation. Ellipsometry provides information about the porosity of different mesoporous films (PtRuNP/OMC = 45%; IrOx = 46%) as well as about the pore size (pore radius of ca. 5 nm for PtRuNP/OMC). In addition, the electronic structure of a material, such as intraband transitions of a mesoporous IrOx film, can be identified, which can be used to better understand the mechanisms of chemical processes. In addition, we show that ellipsometry can be used as a scalable imaging and visualization method for quality assurance in production. These require accurate and traceable measurements, with reference materials playing an important role that include porosity and other related properties. We show that our novel analytical methods are useful for improving analytical work in this entire field. KW - Porous materials KW - Electrolysis KW - Spectroscopic ellipsometry KW - Hybrid metrology measurement KW - Electron microscopy PY - 2021 DO - https://doi.org/10.1002/adem.202101320 SP - 1 EP - 17 PB - Wiley-VCH AN - OPUS4-53960 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von Törne, Jannik Wipert A1 - Piechotta, Christian A1 - Karnstedt, L. T1 - Einblicke in das Transformationsverhalten von Warfarin N2 - Warfarin ist seit den 1950er Jahren einer der bekanntesten Gerinnungshemmer. Beim Menschen wird es bis heute zur Vorbeugung von Thrombose und der Behandlung von Vorhofflimmern und Arrhythmie eingesetzt. Doch schon einige Jahre vor der FDA Zulassung (U. S. Food and Drug Administration) als Medikament wurde es zur Bekämpfung von Nagetieren eingesetzt. Bis heute wurde es nur teilweise durch weitaus wirksamere antikoagulante Rodentizide (ARs) der zweiten Generation, sogenannte Superwarfarine, ersetzt. In der Fachliteratur finden sich zahlreiche Beispiele für sekundäre und tertiäre Vergiftung mit ARs bei Wildtieren und anderen Nichtzieltieren. Bisher ist relativ wenig über die Bioakkumulation, Persistenz und Toxizität von ARs und deren Transformationsprodukten (TPs) in der terrestrischen und aquatischen Umwelt, sowie der Nahrungskette bekannt. Um Einblicke in mögliche Transformations- und Abbauprozesse von Warfarin unter umweltrelevanten Bedingungen zu erhalten und um diese Einflüsse zu simulieren, wurde hierzu eine elektrochemische Reaktorzelle in Kopplung mit einem Massenspektrometer verwendet. So können mögliche Phase-I-Metabolite und sogenannte „oxidation products“ vorausgesagt werden. Hinsichtlich des Verhaltens während der Wasseraufbereitung in Kläranlagen wurden technisch relevante Prozesse wie Chlorung, UV-Bestrahlung und Ozonung in Modellen simuliert, um hier potenzielle Abbauwege und -prozesse aufzuklären. Gebildete Transformationsprodukte wurden daher mittels unterschiedlicher chromatografischer Verfahren getrennt und massenspektrometrisch identifiziert, charakterisiert und verglichen. T2 - 49. Jahrestagung der GUS 2020 CY - Stutensee, Blankenloch DA - 24.03.2021 KW - Warfarin KW - Transformationsprodukte KW - Umweltverhalten PY - 2021 SN - 978-3-9818507-6-5 VL - 49 SP - 265 EP - 272 AN - OPUS4-53963 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hirschberger, Paul A1 - Bartholmai, Matthias T1 - Flying Ant Robot – Aerial Chemical Trail Detection and Localization N2 - This paper presents first advances in the area of aerial chemical trail following. For that purpose, we equipped a palm-size aerial robot, based on the Crazyflie 2.0 quadrocopter, with a small lightweight metal oxide gas sensor for measuring evaporated ethanol from chemical trails. To detect and localize the chemical trail, a novel detection criterion was developed that uses only relative changes in the transient phase of the sensor response, making it more robust in its application. We tested our setup in first crossing-trail experiments showing that our flying ant robot is able to correlate an odor hit with the chemical trail within 0.14 m. Principally, this could enable aerial chemical trail following in the future. T2 - IEEE Sensors 2021 CY - Online meeting DA - 31.10.2021 KW - Nano aerial robot KW - Trail following KW - Trail detection KW - Localization PY - 2021 DO - https://doi.org/10.1109/sensors47087.2021.9639857 SP - 1 EP - 4 PB - IEEE AN - OPUS4-53933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Flying Ant Robot – Aerial Chemical Trail Detection and Localization N2 - This poster presents first advances in the area of aerial chemical trail following. For that purpose, we equipped a palm-size aerial robot, based on the Crazyflie 2.0 quadrocopter, with a small lightweight metal oxide gas sensor for measuring evaporated ethanol from chemical trails. To detect and localize the chemical trail, a novel detection criterion was developed that uses only relative changes in the transient phase of the sensor response, making it more robust in its application. We tested our setup in first crossing-trail experiments showing that our flying ant robot is able to correlate an odor hit with the chemical trail within 0.14 m. Principally, this could enable aerial chemical trail following in the future. T2 - IEEE Sensors 2021 CY - Online meeting DA - 31.10.2021 KW - Nano aerial robot KW - Trail following KW - Trail detection KW - Localization PY - 2021 AN - OPUS4-53934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Thermal behavior of high preformance polymers - Fast Scanning Calorimetry and more N2 - The glass tranistion behavior of polymers of intrinsic microporosity and polynornornes is discussed. T2 - Flash DSC Conference 2021 CY - Online meeting DA - 06.12.2021 KW - Polymer of Intrisic Maicroporosity KW - Highly permeable polynorbornenes PY - 2021 AN - OPUS4-53938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. A1 - Neumann, Patrick P. A1 - Schaffernicht, E. A1 - Lilienthal, A. J. T1 - Using Redundancy in a Sensor Network to Compensate Sensor Failures N2 - Wireless sensor networks provide occupational health experts with valuable information about the distribution of air pollutants in an environment. However, especially low-cost sensors may produce faulty measurements or fail completely. Consequently, not only spatial coverage but also redundancy should be a design criterion for the deployment of a sensor network. For a sensor network deployed in a steel factory, we analyze the correlations between sensors and build machine learning forecasting models, to investigate how well the sensor network can compensate for the outage of sensors. While our results show promising prediction quality of the models, they also indicate the presence of spatially very limited events. We, therefore, conclude that initial measurements with, e.g., mobile units, could help to identify important locations to design redundant sensor networks. T2 - IEEE SENSORS 2021 CY - Online meeting DA - 31.10.2021 KW - Environmental monitoring KW - Wireless sensor network KW - Sensor placement KW - Machine learning PY - 2021 SN - 978-1-7281-9501-8 DO - https://doi.org/10.1109/sensors47087.2021.9639479 SP - 1 EP - 4 PB - IEEE AN - OPUS4-53939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. T1 - Using Redundancy in a Sensor Network to Compensate Sensor Failures N2 - Sensors can fail. Redundancy should therefore be a design driver of wireless sensor networks. For a sensor network deployed in a steel factory, we analyze the correlations between sensors and build machine learning forecasting models, to investigate how well the network can compensate for the outage of sensors. T2 - IEEE SENSORS 2021 CY - Online meeting DA - 31.10.2021 KW - Environmental monitoring KW - Wireless sensor network KW - Sensor placement KW - Machine learning PY - 2021 AN - OPUS4-53940 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Shaken not stirred: enhancing the flavor of mechanochemistry N2 - Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals.1 The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms.2-4 We recently introduced different setups enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy and thermography. The presented setup allows the detection of crystalline, amorphous, eutectic, and liquid intermediates. Furthermore, the chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. In this contribution, we will discuss our recent results investigating the formation of (polymorphic) cocrystals and coordination polymers.2,3,5 Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemical syntheses. T2 - BCA/BACG joint spring meeting CY - Online meeting DA - 29.03.2021 KW - Mechanochemistry KW - Cocrystals KW - Crystal Engineering PY - 2021 AN - OPUS4-53995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Shaken not stirred: in situ investigations of mechanochemical processes N2 - Mechanochemistry has emerged as one of the most interesting synthetic protocols to produce new materials. The development of mechanochemistry as a synthetic method is supported by excellent research by many groups worldwide in a wide range of applications. The potential of mechanochemistry is also reflected in the inclusion in IUPAC’s 10 chemical innovations that will change our world’.[1] Solvent-free methodologies lead to unique chemical processes during synthesis with the consequent formation of martials with new properties.2 In this contribution, we will discuss our recent results investigating the formation of (polymorphic) cocrystals, coordination polymers, metal oxides and metal nanoparticles.[3-8] We introduced different setups enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy and thermography. T2 - Deutsche Kristallzüchtertagung CY - Berlin, Germany DA - 06.10.2021 KW - Mechanochemistry KW - In situ real-time monitoring KW - Crystal PY - 2021 AN - OPUS4-53996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana T1 - Recent developments of X-ray absorption spectroscopy as analytical tool for biological and biomedical applications N2 - X-ray absorption spectroscopy (XAS), in its various modalities, has gained exponential attention and applicability in the field of biological and biomedical systems. Particularly in this field, challenges like low concentration of analyte or proneness to radiation damage have certainly settle the basis for further analytical developments, when using X-ray based methods. Low concentration calls for higher sensitivity—by increasing the detection limits (DL); while susceptibility for radiation damage requires shorter measurement times and/or cryogenic sample environment possibilities. This manuscript reviews the latest analytical possibilities that make XAS more and more adequate to investigate biological or biomedical systems in the last 5 years. KW - Biological & biomedical applications KW - TXRF-XAS KW - HERFD-XAS KW - RXES KW - Quick-XAS KW - Dispersive-XAS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531206 DO - https://doi.org/10.1002/xrs.3254 SN - 0049-8246 VL - 51 IS - 3 SP - 1 EP - 10 PB - John Wiley & Sons Ltd AN - OPUS4-53120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Küttenbaum, Stefan T1 - Zur Validierung von ZfP-Verfahren für die Nachrechnung von Brücken N2 - "Die effiziente Verwendung von Messergebnissen bei der Nachrechnung und von Ergebnissen aus zerstörungsfreien Prüfungen im Speziellen setzt voraus, dass die Relevanz der messbaren Informationen beziffert, die Qualität der gemessenen Information berechnet und die Anforderungen an die Genauigkeit der Inspektionen aus der statischen Berechnung abgeleitet werden können. Der Vergleich der Anforderungen an eine zu messende Information mit der Qualität der gemessenen Information wird in diesem Aufsatz als Validierung eines Messverfahrens aufgefasst. Es wird gezeigt, wie zerstörungsfreie Prüfverfahren für die Nachrechnung validiert werden können. Die Methodik wird anhand einer mit der Ultraschallecho- und Impulsradarmethode untersuchten Spannbetonbrücke demonstriert." KW - Bestandsbauwerke KW - Zuverlässigkeitsbewertung KW - Messunsicherheit PY - 2021 UR - https://www.dgzfp.de/Portals/24/Zeitung/Ausgaben/Zeitung176.pdf SN - 1616-069X IS - 176 SP - 41 EP - 48 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung e.V. (DGZfP), Österreichische Gesellschaft für Zerstörungsfreie Prüfung (ÖGfZP), Schweizerische Gesellschaft für Zerstörungsfreie Prüfung (SGZP) AN - OPUS4-53470 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Held, Mathias A1 - Rashwan, Abdalla A1 - Bulling, Jannis A1 - Lugovtsova, Yevgeniya A1 - Lauschkin, Maik A1 - Prager, Jens T1 - Inverse Bestimmung elastischer Materialparameter aus dem Ausbreitungsverhalten geführter Ultraschallwellen mittels eines Convolutional Neuronal Networks N2 - Detailliertes Wissen über die mechanischen Eigenschaften verwendeter Materialien ist Grundvoraussetzung für viele ingenieurtechnische Aufgaben und Dienstleistungen. Zur Bestimmung der elastischen Materialparameter gibt es verschiedene klassische, zerstörende Prüfverfahren. Eine Möglichkeit der zerstörungsfreien Bestimmung liegt in der Auswertung von Messergebnissen, die auf Basis des Ausbreitungsverhaltens geführter Ultraschallwellen gewonnen wurden. Das Ausbreitungsverhalten geführter Ultraschallwellen kann mittels Dispersionsabbildungen dargestellt werden. Um aus messtechnisch ermittelten Dispersionsabbildungen Rückschlüsse auf die Materialparameter zu ziehen, werden in der aktuellen Forschung verschiedene inverse Methoden diskutiert. Maschinelles Lernen und insbesondere Convolutional Neural Networks (CNNs) stellen eine Möglichkeit der automatisierten inversen Modellierung und Evaluierung von Bilddaten dar. In diesem Beitrag wird gezeigt, wie das Ausbreitungsverhalten von geführten Ultraschallwellen unter Verwendung von CNNs genutzt werden kann, um die isotropen elastischen Konstanten einer plattenförmigen Struktur zu bestimmen. Hierfür werden die verwendeten Daten analysiert, das Preprocessing erläutert und eine grundlegende CNN-Architektur gewählt. Zur Auswertung des generierten Modells werden verschiedene Verfahren wie Gradienten-Mapping und die Visualisierung der verschiedenen Schichten vorgestellt. Die Anwendbarkeit der Methode wird anhand synthetischer Daten demonstriert. T2 - DAGA 2021 CY - Vienna, Austria DA - 15.08.2021 KW - Geführte Ultraschallwellen KW - Inverse Probleme KW - Materialcharakterisierung KW - Maschinelles Lernen KW - Dispersion KW - Lamb Wellen PY - 2021 SN - 978-3-939296-18-8 VL - 47 SP - 659 EP - 662 AN - OPUS4-53492 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gernhard, M. A1 - Rautenberg, Max A1 - Hörner, G. A1 - Weber, B. A1 - Emmerling, Franziska A1 - Roth, C. T1 - Mechanochemical Synthesis as a Greener Way to ProduceIron-based Oxygen Reduction Catalysts N2 - Iron-based catalysts have been reported manifold and studied as platinum group metal (PGM) free alternatives for the catalysis of the oxygen reduction reaction (ORR). However, their sustainable preparation by greener synthesis approaches is usually not discussed. In this work, we propose a new method for the sustainable preparation of such catalysts by using a mechanochemical approach, with no solvents and non-toxic chemicals. The materials obtained from low temperature carbonization (700 °C) exhibit considerable and stable catalytic performance for ORR in alkaline medium. A catalyst obtained from iron hydroxide, tryptophan, dicyandiamide, and ammonium nitrate shows the best electrocatalytic Performance with an overpotential of 921 mV vs. RHE at 0.1 mA/cm2 and an electron transfer number of 3.4. KW - PGM-free catalyst KW - Oxygen Reduction Reaction KW - AEMFC KW - Mössbauer Spectroscopy KW - Sustainable Synthesis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535326 DO - https://doi.org/10.1002/zaac.202100194 VL - 647 IS - 22 SP - 2080 EP - 2087 PB - Weinheim-VCH GmbH AN - OPUS4-53532 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rautenberg, Max T1 - The Effect of Fluorine on Catalysts for the Oxygen Reduction Reaction obtained from Metal Organic Frameworks N2 - The oxygen reduction reaction (ORR) – an important reaction in electrochemical devices, such as fuel cells - is characterized by its sluggish kinetics and therefore requires catalysis. The industry currently relies on platinum as a catalyst, although it is scarce and expensive, hindering the commercial breakthrough of fuel cells in automotive applications. Platinum-free catalysts on basis of nitrogen- and metal doped carbons (NMCs) and fluorinated carbons are promising materials to replace platinum-based catalysts for the ORR. In this work we prepared six metal-organic frameworks (MOFs) by mechanical ball mill grinding and studied their formation by in-situ powder X-ray diffraction. Furthermore, the samples were carbonized under controlled conditions (900°C, 1h, N2-atmosphere) to yield carbon materials, that were employed in ORR-electrocatalysis. The effect of Co-doping and fluorination was systematically studied and outstanding ORR activity was found for the catalyst prepared from the Co-doped fluorinated ZIF-8. T2 - International Symposium on Fluorine-specific interactions CY - Berlin, Germany DA - 27.09.2021 KW - PGM-free catalyst KW - Oxygen Reduction Reaction KW - Mechanochemistry KW - MOFs PY - 2021 AN - OPUS4-53533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zeipert, H. A1 - Johannesmann, S. A1 - Nicolai, Marcel A1 - Lugovtsova, Yevgeniya A1 - Prager, Jens A1 - Henning, B. T1 - Quantifying the coupling strength of adhesively bonded materials by investigating mode repulsion regions N2 - In the field of non-destructive testing, Lamb waves are often used for material characterisation. The increasing computational capabilities further enable complex and detailed simulations to predict the material behaviour in reality. Since adhesive bonding of different materials is a widely used method in modern applications, a reliable measurement system to determine the quality of these adhesive bonds is needed. Investigations of the dispersive behaviour of acoustic waves in adhesively bonded multi-layered waveguides show mode repulsions in the dispersion diagrams in regions where the modes of the single materials would otherwise intersect. In previous works, changes of the distance between those modes with respect to the bonding quality are observed. The experimental data for this investigation is generated using pulsed laser radiation to excite broadband acoustic waves in plate like specimens which are detected by a piezoelectric ultrasonic transducer. Numerical data is generated using simulations via a semi-analytical finite element method. Using a combination of experimental and numerical data, the present work introduces an approach to determine a parameter which indicates the bonding quality in relation to an ideal material coupling. T2 - DAGA 2021 CY - Vienna, Austria DA - 15.08.2021 KW - Ultrasonic guided waves KW - Multi-layered structures KW - Laser excited ultrasonic waves PY - 2021 SP - 1532 EP - 1535 AN - OPUS4-53581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rautenberg, Max T1 - Fluorination and co-doping of ZIF-8 by ball mill grinding for efficient oxygen reduction electrocatalysis N2 - The oxygen reduction reaction (ORR) is a common process in a variety of electrochemical devices, like fuel cells and metal air batteries. The sluggish kinetics of the ORR require an electrocatalyst to pass this bottleneck.[1] Currently, the most used catalytical systems are platinum-based, with several drawbacks, such as the high cost, low availability, and deactivation by CO poisoning.[2] Efforts are made to develop efficient, durable and low cost catalysts to promote the commercialization of fuel cells. Non-precious metal catalysts are promising candidates for efficient ORR catalysis. It has been shown that pyrolyzing metal organic frameworks (MOFs) under inert conditions yields carbon-rich materials, with evenly distributed metal sites, which possess promising electrocatalytic activity.[3] One widely used type of MOF as ORR catalyst precursors is the zeolitic imidazole framework (ZIF) where metal cations are linked through imidazole-based ligands. Their porous nature is partially retained after carbonization, making MOFs very suitable precursor materials. Herein we report the mechanochemical synthesis and structural analysis of Co-doped ZIF-8 (Zn), as well as two polymorphs (dense and prorous) of fluorinated Co-doped CF3-ZIF-8 (Zn). The samples showed electrochemical performance comparable to platinum after carbonization for 1 h at temperatures ranging between 850 – 1000°C. T2 - XXV General Assembly and Congress of the International Union of Crystallography - IUCr 2021 CY - Prague, Czech Republic DA - 14.08.2021 KW - PGM-free catalyst KW - Oxygen Reduction Reaction KW - Mechanochemistry KW - MOFs PY - 2021 AN - OPUS4-53535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rautenberg, Max T1 - Fluorine Modified ZIF 8 for Electrochemical Catalysis: Where does the Fluorine go? N2 - Carbonization of fluorinated metal-organic frameworks (MOFs) should yield fluorinated nitrogen- and metal-doped carbons (F-NMCs), which are a combination of NMCs and fluorinated carbons, each promising electrocatalysts on their own. We synthesized two polymorphs of a fluorinated MOF by mechanical ball mill grinding, and carbonized them to yield potential electrocatalyt materials. The catalytical activity towards the oxygen reduction reaction (ORR) was examined, finding good activites. Simulations from a theoretic model helped assesing the stability of proposed catalytic sites and understanding the measured activites towards the ORR catalysis. T2 - Online symposium of the CRC 1349 "fluorine-specific interactions" CY - Online meeting DA - 29.06.2021 KW - PGM-free catalyst KW - Oxygen Reduction Reaction KW - Mechanochemistry KW - MOFs KW - Computational chemistry PY - 2021 AN - OPUS4-53538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rautenberg, Max T1 - Synthesis and characterization of fluorinated Co-Zn-Zeolitic imidazole frameworks for catalysis of the oxygen reduction reaction N2 - The oxygen reduction reaction (ORR) is a common process in a variety of electrochemical devices, like fuel cells and metal air batteries. The sluggish kinetics of the ORR require an electrocatalyst to pass this bottleneck.[1] Currently, the most used catalytical systems are platinum-based, with several drawbacks, such as the high cost, low availability, and deactivation by CO poisoning.[2] Efforts are made to develop efficient, durable and low cost catalysts to promote the commercialization of fuel cells. Non-precious metal catalysts are promising candidates for efficient ORR catalysis. It has been shown that pyrolyzing metal organic frameworks (MOFs) under inert conditions yields carbon-rich materials, with evenly distributed metal sites, which possess promising electrocatalytic activity.[3] One widely used type of MOF as ORR catalyst precursors is the zeolitic imidazole framework (ZIF) where metal cations are linked through imidazolebased ligands. Herein we report the mechanochemical synthesis, structural analysis and of Co-doped ZIF-8 (Zn), as well as its fluorinated counterpart Co-doped CF3 -ZIF-8 (Zn). The samples showed electrochemical performance comparable to platinum after carbonization for 1h at temperatures ranging between 850 – 1000°C. T2 - 15th International conference on materials chemistry (MC15) CY - Online meeting DA - 12.07.2021 KW - PGM-free catalyst KW - Oxygen Reduction Reaction KW - Mechanochemistry KW - MOFs PY - 2021 AN - OPUS4-53539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martins, I. A1 - Carta, M. A1 - Haferkamp, Sebastian A1 - Feiler, Torvid A1 - Delogu, F. A1 - Colacino, E. A1 - Emmerling, Franziska T1 - Mechanochemical N‑Chlorination Reaction of Hydantoin: In Situ Real-Time Kinetic Study by Powder X‑ray Diffraction and Raman Spectroscopy N2 - Mechanochemistry has become a valuable tool for the synthesis of new molecules, especially in the field of organic chemistry. In the present work, we investigate the kinetic profile of the chlorination reaction of N-3-ethyl-5,5-dimethylhydantoin (EDMH) activated and driven by ball milling. The reaction has been carried out using 2 mm, 4 mm, 5 mm, 6 mm, and 8 mm ball sizes in a new small custom-made Perspex milling jar. The Crystal structure of the starting material EDMH and the 1-chloro-3-ethyl5,5′-dimethyl hydantoin (CEDMH) chlorination product was solved by single-crystal X-ray diffraction. The reaction was monitored, in situ and in real time, by both powder X-ray diffraction (PXRD) and Raman spectroscopy. Our kinetic data show that the reaction progress to equilibrium is similar at all milling ball sizes. The induction period is very short (between 10 and 40 s) when using 4 mm, 5 mm, 6 mm, and 8 mm balls. For the reaction performed with a 2 mm ball, a significantly longer induction period of 9 min was observed. This could indicate that an initial energy accumulation and higher mixing efficiency are necessary before the reaction starts. Using different kinetic models, we found that the amount of powder affected by critical loading conditions during individual impacts is significantly dependent on the ball size used. An almost linear correlation between the rate of the chemical transformations and the ball volume is observed. KW - Mechanochemistry KW - In situ real-time monitoring KW - N-Chlorination KW - Kinetics KW - Hydantoin KW - Powder X-ray diffraction KW - Raman spectroscopy PY - 2021 DO - https://doi.org/10.1021/acssuschemeng.1c03812 VL - 9 IS - 37 SP - 12591 EP - 12601 AN - OPUS4-53541 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - The Past and the Future of Human Factors: The “Uncontrollable” Aspect of NDT Reliability? N2 - That human factors (HF) affect the reliability of NDT is not novelty. Still, when it comes to reliability assessments, the role of people is often neglected. Reliability is typically expressed in terms of POD curves, and the effects of human and organisational factors on the inspection are typically tackled by the regulations, procedures and by the qualification and training of the inspection personnel. However, studies have shown that even the most experienced personnel can make mistakes and that the reliability in the field is never as high as the reliability measured in the POD experiments. Generally, HF are considered too unpredictable and too uncontrollable to model. If that is the fact, then what can we do? The engineering perspective to this problem has often been to find ways to automate inspections and, recently, to make use of artificial intelligence tools to decrease the direct effect of people on the inspection results and improve the overall efficiency and reliability. However, despite automation and AI, people remain the key players, though their tasks change. The contemporary approach to HF is not to engineer them out of the system but to design human-machine systems that make the best use of both. In this talk, ways of tackling HF in the design of systems and processes will be presented. T2 - Reliability of NDT webinar, The Scottish Branch of the British Institute of NDT CY - Online meeting DA - 29.01.2021 KW - Non-Destructive Testing KW - NDT KW - Human Factors KW - Reliability PY - 2021 UR - www.bindt.org/admin/Downloads/2021-01%20BINDT_Bertovic_Human%20factors_new.pdf AN - OPUS4-53544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kanzler, D. A1 - Rentala, V. A1 - Bertovic, Marija A1 - Heckel, Thomas A1 - Rosenthal, Martina A1 - Keßler, S. A1 - Dethof, F. A1 - Stolz, R. A1 - Jüngert, A. A1 - Vrana, J. T1 - Die deutschen Bestrebungen zur Normierung der Fähigkeits- und Zuverlässigkeitsbewertung der zerstörungsfreien Prüfung N2 - Seit 1999 existiert das MIL-HDBK 1823, die us-amerikanische Leitfaden zur Erstellung einer Probability of Detection (POD; Fehlerdetektionswahrscheinlichkeit). Obwohl das Dokument als internationaler Stand der Technik angesehen wird, ist die allgemeine Anwendung in der ZfP-Praxis von einigen Nachteilen begleitet: 1. Die beschriebenen POD‘s bilden ausschließlich die Grundlagen-POD ab, jeweils mit nur einem Fehlerparameter und einem Signalparameter. Modernere Ansätze werden hier nicht adressiert. 2. Die aktuelle Version verzichtet fast vollständig auf konkrete mathematische Formulierungen. 3. Die Richtlinie richtet sich hauptsächlich an die militärische Luftfahrt. 4. Das Dokument ist nur in englischer Sprache verfügbar. Mit Hilfe eines BMWi-Förderprojekts wird ein weiterführendes Regelwerk auf Basis der MIL-HDBK 1823 unter deutscher Federführung erarbeitet, welches die Anwendung der POD-Berechnung auf eine breitere Basis stellt und die oben genannten Nachteile der MIL-HDBK 1823 behebt. Das vorgestellte Projekt „normPOD“ wird eine normative, branchenübergreifend einsetzbare Beschreibung des Vorgehens bei der Berechnung einer POD zur Zuverlässigkeitsbewertung zerstörungsfreier Prüfungen entwickeln. Hierbei wird Klarheit über unterschiedliche POD-Ansätze geschaffen und anhand praktischer Beispiele aus Maschinenbau und Bauwesen ein Leitfaden für den Praxiseinsatz erarbeitet. Das Poster gibt einen Überblick über die geplanten Arbeiten innerhalb des Projekts und lädt die Beteiligten der DGZfP-Jahrestagung zur Diskussion ein, um eine breite Basis und Akzeptanz für die entwickelten Berechnungsverfahren zu schaffen, insbesondere in Hinblick auf ZfP 4.0 und Digitalisierung. T2 - Jahrestagung der DGZfP CY - Online meeting DA - 10.05.2021 KW - Zerstörungsfreie Prüfung KW - ZfP KW - Zuverlässigkeit KW - Standardisierung KW - Human Factors PY - 2021 AN - OPUS4-53547 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Laser induced gas breakdown in reactive mixtures N2 - Plasma-chemical approach is used for synthesis of various gaseous, liquid, and solid substances since 1960th. Nowadays, the method of plasma enhanced chemical vapor deposition (PECVD) is used for production of thin films, protective coatings, carbon-based nanostructures, high purity isotopic materials, biomaterials, and other products. Plasma for PECVD is typically created in various electrical discharges, e.g. DC and AC glow discharges or discharges operated at audio (10-20 kHz), radio (13.56 MHz), and microwave (2.45 GHz) frequencies. Plasma induced by a laser, a laser induced plasma (LIP), is rarely used to deposit materials from the gas phase as in PECVD. This work is aimed at reviving interest to this latter technology and showing its efficiency and potential. We run several pilot experiments. First, LIP is excited in BCl3 or BF3 plus H2 or CH4 to evaluate the efficiency of deposition of solid boron and boron carbide, the materials, which are largely used for refractory coatings. Second, we investigate a possibility of synthesis of fluorochlorosilanes SiFxCl4-x (x = 1, 2, 3) by LIP induced in SiF4 + SiCl4 gas mixtures. Using fluorochlorosilanes with different combinations of F and Cl in the SiFxCly molecule may add flexibility in processes of silicon deposition and etching. Third, LIP is excited in reactive mixture MoF6+H2+BF3 or on a Mo target ablated into H2/BF3 atmosphere. The goal is obtaining superhard molybdenum borides MoB, Mo2B, or MoB2. The gases used and solid deposits are analyzed by optical emission spectroscopy (OES), IR and mass spectrometry (MS). We also model the plasma and perform static equilibrium chemistry calculations to see if the desired reaction products are thermodynamically favorable. Dynamic calculations of the expanding plasma plume are performed using a hydrodynamic code combined with the open source chemical software. T2 - SciX 2021, The Federation of Analytical Chemistry and Spectroscopy Societies (FACSS) CY - Providence, RI, USA DA - September 26, 2021 KW - Laser ablation KW - Laser induced plasma deposition KW - Emission spectroscopy KW - Surface coating KW - Plasma chemistry KW - Hydrodynamic model PY - 2021 AN - OPUS4-53560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kanzler, D. A1 - Bertovic, Marija A1 - Dethof, F. A1 - Heckel, Thomas A1 - Jüngert, A. A1 - Keßler, S. A1 - Rentala, V. A1 - Rosenthal, Martina A1 - Stolz, R. A1 - Vrana, J. T1 - Die deutschen Bestrebungen zur Normierung der Fähigkeits- und Zuverlässigkeitsbewertung der zerstörungsfreien Prüfung N2 - Seit 1999 existiert das MIL-HDBK 1823, die us-amerikanische Leitfaden zur Erstellung einer Probability of Detection (POD; Fehlerdetektionswahrscheinlichkeit). Obwohl das Dokument als internationaler Stand der Technik angesehen wird, ist die allgemeine Anwendung in der ZfP-Praxis von einigen Nachteilen begleitet: 1. Die beschriebenen POD‘s bilden ausschließlich die Grundlagen-POD ab, jeweils mit nur einem Fehlerparameter und einem Signalparameter. Modernere Ansätze werden hier nicht adressiert. 2. Die aktuelle Version verzichtet fast vollständig auf konkrete mathematische Formulierungen. 3. Die Richtlinie richtet sich hauptsächlich an die militärische Luftfahrt. 4. Das Dokument ist nur in englischer Sprache verfügbar. Mit Hilfe eines BMWi-Förderprojekts wird ein weiterführendes Regelwerk auf Basis der MIL-HDBK 1823 unter deutscher Federführung erarbeitet, welches die Anwendung der POD-Berechnung auf eine breitere Basis stellt und die oben genannten Nachteile der MIL-HDBK 1823 behebt. Das vorgestellte Projekt „normPOD“ wird eine normative, branchenübergreifend einsetzbare Beschreibung des Vorgehens bei der Berechnung einer POD zur Zuverlässigkeitsbewertung zerstörungsfreier Prüfungen entwickeln. Hierbei wird Klarheit über unterschiedliche POD-Ansätze geschaffen und anhand praktischer Beispiele aus Maschinenbau und Bauwesen ein Leitfaden für den Praxiseinsatz erarbeitet. Das Poster gibt einen Überblick über die geplanten Arbeiten innerhalb des Projekts und lädt die Beteiligten der DGZfP-Jahrestagung zur Diskussion ein, um eine breite Basis und Akzeptanz für die entwickelten Berechnungsverfahren zu schaffen, insbesondere in Hinblick auf ZfP 4.0 und Digitalisierung. T2 - Jahrestagung der DGZfP CY - Online meeting DA - 10.05.2021 KW - Zerstörungsfreie Prüfung KW - ZfP KW - Zuverlässigkeit KW - Standardisierung KW - Human Factors PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535628 UR - www.ndt.net/article/dgzfp2021/papers/P40.pdf SP - 1 EP - 8 AN - OPUS4-53562 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - OPC-UA für Prozessindustrie und Laborwelt - Offener Standard für die störungsfreie Kommuniktaion N2 - Im privaten Umfeld machen wir uns keine Gedanken mehr über die Einbindung von elektronischen Geräten in Netzwerke, sei es bei der Verbindung des Mobiltelephons mit dem W-Lan-Netzwerk des Hotels oder von Freunden oder des drahtlosen Kopfhörers mit dem Notebook: Wir erwarten, dass es auf Anhieb funktioniert. Dahinter stecken offene Standards für die Konnektivität. Dafür braucht man immer zwei Dinge: Einen physischen Kommunikationskanal, auf dem die Datenpakete zwischen den Komponenten und Geräten hin- und herwandern und eine einheitliche Kommunikationssprache, so dass sich die Komponenten und Geräte auch untereinander verstehen, weil sie dieselbe Sprache sprechen und automatisch wissen, was sie miteinander zu besprechen haben. Wenn man eine sichere Konnektivität bevorzugt, werden weitere Informationen benötigt, wie etwa ein Passwort. Auch für die störungsfreie Kommunikation aller Automatisierungskomponenten der Prozessindustrie untereinander oder etwa für die Kommunikation von Geräten in einem analytischen Labor wird ein einheitliches Protokoll (Kommunikationssprache) und ein einheitlicher Feldbus (Kommunikationskanal) benötigt. Mittlerweile gilt der Standard OPC Unified Architecture (OPC-UA) für das Erstere als gesetzt und kann als ein kleiner Triumph von Industrie 4.0 betrachtet werden. OPC-UA kann auf verschiedenen Kommunikationskanälen laufen – am liebsten solchen, die eine angemessene Bandbreite oder Datenrate haben. Was den dazu notwendigen physischen Kommunikationskanal betrifft, findet man aus verschiedenen Gründen einen sehr spezialisierten und historisch über Jahrzehnte gewachsenen Lebensraum vor, der Operational Technology (OT) genannt wird. Zumeist findet man Zwei- und Vierdraht-Techniken mit Strom- und Spannungs-Signalübertragung, zum Beispiel mit 4–20 mA. Kommunikationsstandards wie eingangs erwähnt, wie Ethernet oder W-Lan sind absolut die Seltenheit. Dieses wird für die sogenannte Informationstechnik (Information Technology, IT) eingesetzt und ist aus Sicherheitsgründen heute komplett von der OT getrennt. Auch wenn es der OT nicht gefällt, wachsen die beiden Welten IT und OT aber stetig weiter zusammen, da die IT bereits viele funktionierende und preislich attraktive Lösungen bereithält. Die vermeintliche Sicherheit, Verfügbarkeit und Echtzeitfähigkeit der klassischen OT, aber auch ihre Komplexität müssen im Zuge der Digitalen Transformation nun sorgfältig abgewogen werden. KW - Prozessindustrie KW - Laborkommunikation KW - Konnektivität KW - OPC-UA KW - Digital Transformation KW - Labor-IT PY - 2021 UR - https://analyticalscience.wiley.com/do/10.1002/was.00170277/full/blaetterkatalog_git1021.pdf SN - 0016-3538 VL - 65 IS - 10 SP - 1 EP - 4 PB - Wiley CY - Weinheim AN - OPUS4-53566 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - NDE 4.0: Redefining Traditional Inspector Roles N2 - The successful shift to NDE 4.0 will not only require developing and embracing new technologies associated with the fourth industrial revolution or becoming an integral part of the overall Industry 4.0, but also developing and adopting new ways of working. It is undoubtful that people will remain in charge of the inspections. However, it is arguable if the current “procedure-following” “level I-III” paradigm can withstand the changes that come along NDE 4.0. With the increased autonomy and interconnectedness expected with NDT 4.0, the majority of traditional NDE tasks will no longer be needed. Instead, different skills, such as that of programming and adapting systems, as well as problem solving, will become vital for the inspections. Therefore, we suggest that a new paradigm is needed—one in which inspector roles and, thus, also the requirements will have to be reinvented. We expect the inspectors to be relieved from the tedious and error prone aspects of the current system and to take responsibility for increasingly complex automated systems and work in closer collaboration with other experts. Thus, we propose that the traditional inspector roles will be transformed into that of the system developer, caretaker and problem solver, each requiring a specific set of skills and assuming different responsibilities. In this talk, we will present the new roles and discuss the challenges that may arise with them. T2 - NDE for industry – annual workshop CY - Online meeting DA - 29.06.2021 KW - Non-Destructive Evaluation KW - NDE 4.0 KW - Human-Machine Interaction KW - Industry 4.0 KW - Inspection Personnel KW - Human-Centered Approach KW - Human Factors KW - Acceptance PY - 2021 AN - OPUS4-53548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - NDE 4.0: Redefining Traditional Inspector Roles N2 - The successful shift to NDE 4.0 will not only require developing and embracing new technologies associated with the fourth industrial revolution or becoming an integral part of the overall Industry 4.0, but also developing and adopting new ways of working. It is undoubtful that people will remain in charge of the inspections. However, it is arguable if the current “procedure-following” “level I-III” paradigm can withstand the changes that come along NDE 4.0. With the increased autonomy and interconnectedness expected with NDT 4.0, the majority of traditional NDE tasks will no longer be needed. Instead, different skills, such as that of programming and adapting systems, as well as problem solving, will become vital for the inspections. Therefore, we suggest that a new paradigm is needed—one in which inspector roles and, thus, also the requirements will have to be reinvented. We expect the inspectors to be relieved from the tedious and error prone aspects of the current system and to take responsibility for increasingly complex automated systems and work in closer collaboration with other experts. Thus, we propose that the traditional inspector roles will be transformed into that of the system developer, caretaker and problem solver, each requiring a specific set of skills and assuming different responsibilities. In this talk, we will present the new roles and discuss the challenges that may arise with them. T2 - HOIS Digitalisation Forum (HDF) virtual seminar CY - Online meeting DA - 10.08.2021 KW - Non-Destructive Evaluation KW - NDE 4.0 KW - Human-Machine Interaction KW - Industry 4.0 KW - Inspection Personnel KW - Human-Centered Approach KW - Human Factors KW - Acceptance PY - 2021 AN - OPUS4-53549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bertovic, Marija A1 - Feistkorn, S. A1 - Kanzler, D. A1 - Valeske, B. A1 - Vrana, J. T1 - ZfP aus der Sicht der ZfP-Community: Umfrageergebnisse, Herausforderungen und Perspektiven N2 - Im vorliegenden Artikel werden die Ergebnisse des Fragebogens der DGZfP zur Thematik „ZfP 4.0“ vorgestellt und diskutiert. Die Befragung zielte darauf ab, das allgemeine Verständnis der ZfP-Community zur Begrifflichkeit „ZfP 4.0“ herauszuarbeiten und daraus Bedarfe und Handlungsempfehlungen für die identifizierten Herausforderungen abzuleiten. Außerdem zeigt sich aus Sicht der Autor*innen, dass relevante Terminologien zu dem Themenkomplex Digitalisierung einer weiteren Klärung bedürfen, was im Bericht aufgegriffen wird. Im Ausblick zu den angelaufenen Arbeiten im nationalen Fachausschuss ZfP 4.0 und in den sich etablierenden internationalen Fachkreisen werden daraus abgeleitete Perspektiven für die Zukunftsgestaltung vorgestellt. KW - Zerstörungsfreie Prüfung KW - ZfP 4.0 KW - Zuverlässigkeit KW - Human Factors KW - Mensch-Maschine-Interaktion KW - Automatisierung KW - Schnittstellen KW - Fachausschuss KW - Digitalisierung PY - 2021 UR - www.dgzfp.de/DesktopModules/Bring2mind/DMX/API/Entries/Download?Command=Core_Download&EntryId=30879&language=de-DE&PortalId=24&TabId=1515 SN - 1616-069X IS - 174 SP - 43 EP - 49 PB - DGZfP e.V., ÖGfZP und SGZP AN - OPUS4-53550 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Bertovic, Marija A1 - Virkkunen, I. ED - Meyendorf, N. ED - Ida, N. ED - Singh, R. ED - Vrana, J. T1 - NDE 4.0: New Paradigm for the NDE Inspection Personnel N2 - Nondestructive evaluation (NDE) is entering an era of the fourth industrial revolution and will undergo a major transformation. NDE is a vital part of industry and a successful move to NDE 4.0, it will require not just developing and embracing new technologies, but also developing and adopting new ways of working and becoming an integral part of the overall Industry 4.0. This will pose new challenges for the inspection personnel. To ensure the expected benefits from NDE 4.0, inspectors need stay in charge of the changing inspections. The promised autonomy and interconnectedness of NDE 4.0 will supersede the majority of traditional inspector tasks and will in turn require a different set of skills and raise different demands and challenges for the inspection personnel, thus conflicting the current “procedure-following”-“level I-III” paradigm. The new industry 4.0 technologies can be integrated into the current framework, but exploiting their full potential requires changes in the role of the inspectors. The inspectors will be relieved from the tedious and error-prone aspects of the current system. At the same time, they will need to take responsibility for increasingly complex automated systems and work in closer collaboration with other experts. We propose that the traditional inspector roles will be transformed into that of the system developer, caretaker, and problem solver, each requiring a specific set of skills and assuming different responsibilities. For full NDE 4.0, NDE must abandon its traditional role as a self-contained entity with well-defined boundaries and take its role in the wider system that is the industry 4.0. KW - Non-Destructive Evaluation KW - NDE 4.0 KW - Industry 4.0 KW - Inspection Personnel KW - Human-Centered Approach KW - Human-Machine Interaction KW - Human Factors KW - Acceptance PY - 2021 SN - 978-3-030-48200-8 DO - https://doi.org/10.1007/978-3-030-48200-8_9-1 SP - 1 EP - 31 PB - Springer, Cham AN - OPUS4-53551 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - NDE 4.0: Redefining Traditional Inspector Roles N2 - The successful shift to NDE 4.0 will not only require developing and embracing new technologies associated with the fourth industrial revolution or becoming an integral part of the overall Industry 4.0, but also developing and adopting new ways of working. It is undoubtful that people will remain in charge of the inspections. However, it is arguable if the current “procedure-following” “level I-III” paradigm can withstand the changes that come along NDE 4.0. With the increased autonomy and interconnectedness expected with NDT 4.0, the majority of traditional NDE tasks will no longer be needed. Instead, different skills, such as that of programming and adapting systems, as well as problem solving, will become vital for the inspections. Therefore, we suggest that a new paradigm is needed—one in which inspector roles and, thus, also the requirements will have to be reinvented. We expect the inspectors to be relieved from the tedious and error prone aspects of the current system and to take responsibility for increasingly complex automated systems and work in closer collaboration with other experts. Thus, we propose that the traditional inspector roles will be transformed into that of the system developer, caretaker and problem solver, each requiring a specific set of skills and assuming different responsibilities. In this talk, we will present the new roles and discuss the challenges that may arise with them. T2 - International Virtual Conference on NDE 4.0, DGZfP CY - Online meeting DA - 14.04.2021 KW - Non-Destructive Evaluation KW - NDE 4.0 KW - Human-Machine Interaction KW - Industry 4.0 KW - Inspection Personnel KW - Human-Centered Approach KW - Human Factors KW - Acceptance PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535524 UR - www.ndt.net/search/docs.php3?id=26328 AN - OPUS4-53552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steglich, Patrick A1 - Paul, Martin A1 - Mai, C. A1 - Böhme, A. A1 - Bondarenko, S. A1 - Weller, Michael G. A1 - Mai, A. T1 - A monolithically integrated microfluidic channel in a silicon-based photonic-integrated-circuit technology for biochemical sensing N2 - In this work, a cost-effective optofluidic system is proposed and preliminary experimental results are presented. A microfluidic channel monolithically integrated into a photonic integrated circuit technology is used in conjunction with a cyclic olefin copolymer (COC) substrate to provide fluidic in- and output ports. We report on initial experimental results as well as on the simple and cost-effective fabrication of this optofluidic system by means of micro-milling. KW - Biosensors KW - Biophotonics KW - Optical sensors KW - Photonic sensors KW - Ring resonators KW - Silicon photonics KW - Lab-on-a-chip KW - Microfluidics KW - Chip KW - Biochip PY - 2021 DO - https://doi.org/10.1117/12.2588791 VL - 11772 SP - 1 EP - 5 PB - SPIE AN - OPUS4-53559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - van de Kreeke, Johannes T1 - Current developments in PT N2 - This presentation was held at a laboratory conference in Colombia, and aimed at sharing some current, bigger developments with the audience that are influencing the role and impact of PT (and, to a lesser extent, RM) on labs and society. T2 - Simposio Latinoamericano de Calibracíon y Ensayos CY - Bogotá, Colombia DA - 10.11.2021 KW - Proficiency Testing KW - Reference Materials KW - COMAR KW - EPTIS PY - 2021 AN - OPUS4-53813 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kunc, F. A1 - Nirmalananthan-Budau, Nithiya A1 - Rühle, Bastian A1 - Sung, Y. A1 - Johnston, L.J. A1 - Resch-Genger, Ute T1 - Interlaboratory Comparison on the Quantification of Total and Accessible Amine Groups on Silica Nanoparticles with qNMR and Optical Assays N2 - Risk assessment of nanomaterials requires not only standardized toxicity studies but also validated methods for nanomaterial surface characterization with known uncertainties. In this context, a first bilateral interlaboratory comparison on Surface group quantification of nanomaterials is presented that assesses different reporter-free and labeling methods for the quantification of the total and accessible number of amine functionalities on commercially available silica nanoparticles that are widely used in the life sciences. The overall goal of this comparison is the identification of optimum methods as well as achievable measurement uncertainties and the comparability of the results across laboratories. We also examined the robustness and ease of implementation of the applied analytical methods and discussed method-inherent limitations. In summary, this comparison presents a first step toward the eventually required standardization of methods for surface group quantification. KW - Nano KW - Nanomaterial KW - Surface KW - Method KW - QNMR KW - Quantification KW - Comparison KW - Quality assurance KW - Optical probe KW - Sensor KW - Interlabority comparison KW - Standardization KW - Optical assay KW - Functional group analysis KW - Silica KW - Particle KW - Safety KW - Environment PY - 2021 DO - https://doi.org/10.1021/acs.analchem.1c02162 SN - 1520-6882 VL - 93 IS - 46 SP - 15271 EP - 15278 PB - ASC Publications AN - OPUS4-53818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silva, W. A1 - Zscherpel, Uwe A1 - Ewert, U. A1 - Lopes, R. T1 - Analysis of angular dependent spatial frequency response of Digital Coplanar Translational Laminography N2 - Digital Coplanar Translational Laminography (CTL) is a radiographic imaging technique that permits the visualization of structural details and discontinuities in the object of interest after 3D reconstruction from multiple projections. This technique becomes quite competitive regarding to computed tomography in situations of arrangements in which no complete rotation of the X-ray source - detector system around the object of interest is accessible or in cases where the part to be inspected has a high geometric asymmetry. The literature does not show many studies about image quality for different laminographic reconstructions and scan geometries. Different methodologies for measuring the Modulation Transfer Function (MTF) as a key image quality parameter for the aforementioned technique are applied. The MTF was measured using different approaches, presampled MTF or sampled MTF, both based on the Fourier Transform-Magnitude Spectrum or the square wave MTF using line pattern gauges. A sample known as Siemens Star with a converging line pattern was used to measure the circular square wave MTF. This circular MTF provides information on the direction dependent contrast transfer related to the measurement conditions, the reconstruction algorithms and the translational scan direction. For this purpose, several MTF measurements were performed in multiple angular directions. Beyond it, reconstructions were performed using different algorithms (Filtered Shifted Average) and an iterative one (MART – Multiplicative Algebraic Reconstruction Technique). Image quality analysis were done for both reconstruction methods. MART showed an image quality improvement for challenging conditions for laminographic arrangements, such as for a low number of projections (down to 25 for this study, considered as limited view, limited angle reconstruction). Additionally, a Gadolinium gauge with parallel line patterns within a range from 10 μm to 1000 μm was used to compare the square wave MTF with the sine MTFs, measured by the different techniques mentioned above. The results show that the MTF techniques presented are equivalent in this study. The results obtained for this Gadolinium plate showed a good agreement between MTF10% and SRb image measurements. The methodology presented here is used for the characterization of the frequency dependent spatial resolution of measurements obtained from different laminographic reconstruction techniques and scan geometries. Finally, from the acquisitions and reconstructions obtained with the Siemens Star, cross laminographic images were calculated in order to improve the direction dependent sensitivity. The results showed a better detectability for cross laminographic images in comparison to unidirectional coplanar translational laminographic images covering dead zones. KW - Laminography KW - Image quality KW - Modulation transfer function KW - Cross laminography KW - Reconstruction algorithms PY - 2021 DO - https://doi.org/10.1016/j.ndteint.2021.102546 SN - 0963-8695 VL - 124 SP - 1 EP - 13 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-53845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Importance of Radiation Damage to DNA-Protein Complexes N2 - The formation of DNA-protein complexes ocurrs during replication and repair within cells. They are assumed to modify the damage caused by ionization radiation during radaition therapy. Hereby the assumption is, that the underlying damaging channels in DNA and proteins are modified, especially when compared to single molecules. T2 - Scientific online presentations workshop CY - Online meeting DA - 03.12.2021 KW - DNA KW - Proteins KW - Radiation damage KW - Ionizing radiation KW - Hydroxyl radicals PY - 2021 AN - OPUS4-53894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roesch, Philipp A1 - Vogel, Christian A1 - Huthwelker, T. A1 - Wittwer, Philipp A1 - Simon, Franz-Georg T1 - Investigation of per‑ and polyfluoroalkyl substances (PFAS) in soils and sewage sludges by fluorine K‑edge XANES spectroscopy and combustion ion chromatography N2 - For the first time, fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy was applied to detect per- and polyfluoroalkyl substances (PFAS) in various soil and sewage sludge samples. The method can be used to determine the speciation of inorganic and organic fluorides, without pre-treatment of solid samples. Therefore, XANES spectra of several inorganic fluorides as well as selected fluorinated organic compounds were recorded. While inorganic fluorides partially exhibit a variety of sharp spectral features in the XANES spectrum, almost all inspected organofluorine compounds show two distinct broad features at 688.5 and 692.0 eV. Moreover, the peak intensity ratio 688.5 eV/692.0 eV in the PFAS XANES spectrum can be inversely correlated to the chain length of the perfluoro sulfonic acid group. The detection of targeted PFAS by bulk-XANES spectroscopy in combination with linear combination fitting in soils and sewage sludges was not applicable due to the low organic fluorine to total fluorine ratio of the samples (0.01–1.84%). Nonetheless, direct analysis of pure PFAS revealed that analysis of organofluorine species might be achieved in higher concentrated samples. Furthermore, quantitative measurements by combustion ion chromatography (CIC) evaluated as sum parameters extractable organically bound fluorine (EOF) and total fluorine (TF) emphasize that besides soils, sewage sludges are a significant source of organic fluorine in agriculture (154–7209 μg/kg). KW - Sewage sludge KW - Combustion ion chromatography KW - Oil KW - X-ray absorption near-edge structure (XANES) spectroscopy KW - Per- and polyfluoroalkyl substances (PFAS) PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538953 DO - https://doi.org/10.1007/s11356-021-17838-z VL - 29 IS - 18 SP - 26889 EP - 26899 PB - Springer AN - OPUS4-53895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, C. T1 - Optimization of LIBS experiments using Design of experiment (DoE) N2 - To conduct a reliable, repeatable and accurate LIBS analysis, the optimization of the experimental setup is an important task. Hardware parameters of lasers and spectrometers used in the setup as well as additionally required components such as optics or process gas pipes must be carefully aligned and adjusted because factors like (i) focal conditions of the optics, (ii) alignment of the sample, (iii) process purge gas (types, flow rate) or (iv) measurement settings (integration time, accumulation of pulses) have a big impact on the signal quality. Therefore, in most cases the effect of different factors is evaluated empirically due to changing one factor at a time while keeping the overall configuration the same. In the end, the optimal configuration is selected based on the best parameters for each influencing factor. During optimization, a configuration of the experimental setup is aimed at, which allows e.g. the highest signal intensity or the lowest variation. In most cases, cross-correlation, interference and interaction among the various factors are not considered. For this reason, the possibilities of using Design of Experiment (DoE) to optimize a LIBS experiment will be shown and advantages of (i) reduction of testing plans using a feature space, (ii) identifying and considering cross-correlations and interactions, (iii) evaluating individual impacts on the measurement (e.g. contour and surface plots) as well as (iv) multivariate models for prediction of impacts will be presented. T2 - 11th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy (EMSLIBS) CY - Online meeting DA - 29.11.2021 KW - LIBS KW - Chlorine KW - DoE PY - 2021 AN - OPUS4-53899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Laser dielectric breakdown as a novel method for producing molybdenum borides N2 - Superhard materials with a Vickers hardness in the range of 30-40 GPa are of great interest, both from a fundamental and a practical viewpoints, since they have outstanding mechanical, thermal and chemical properties. Molybdenum borides belong to this group of materials. A review of publications on synthesis of molybdenum boride indicates a) great interest in this superhard material and b) the need for new effective methods of its synthesis, especially in a nanocrystalline form. Very promising are the plasma-chemical methods based on laser induced breakdown. The breakdown can be created either in reactive gases containing volatile compounds of boron and molybdenum or on solid samples. For gas breakdown, molybdenum hexafluoride MoF6 and boron trifluoride BF3 were used in the mixture with hydrogen and argon; for solid breakdown, the pure molybdenum sample was ablated into the mixture of H2 and BF3. The plasma-chemical synthesis of MoxBy structures was carried out in the reactor shown in Figure. Laser breakdown was created by a pulsed Nd: YAG laser operating at 1064 nm with a 15 ns pulse duration, 5 Hz repetition rate, and 800 mJ pulse energy. The laser was focused by a 5 cm focal length lens to produce 26 J/cm3 energy density in the focal point. The ratios H2:BF3: MoF6 = 5:2:1 and H2:BF3 = 3:1 were used in a pressure range 30 - 760 Torr. After ablation in the mixture H2 + BF3 + MoF6, the deposit contained an amorphous phase with a small impurity of crystalline molybdenum and no boride phase. After ablation of metallic Mo into H2 + BF3, the main phase was MoB2 in the form of nano dispersed powder with an average grain size of 100 nm. The degree of conversion of boron trifluoride and the yield of molybdenum boride were studied as a function of pressure. It was established that 30 Torr is optimal for the formation of MoB2. This work was supported by the Russian Science Foundation grant No. 20-13-00035. T2 - Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy CY - Online meeting DA - 29.11.2021 KW - Plasma enhanced chemical deposition KW - Laser induced plasma KW - Plasma chemistry KW - Molybdenum boride PY - 2021 AN - OPUS4-53901 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Aßmann, Norman A1 - Bühling, Benjamin T1 - Impact-echo dataset "Radarplatte" N2 - This dataset contains raw data resulting from Impact-Echo measurements at the reference conrete block "Radarplatte", located at BAM (German Federal Institute for Materials Research and Testing). This specimen has been described in detail by Niederleithinger et al. (2021), who applied muon tomography, ultrasonic echo measurements, radar and X-ray laminography to visualize its internal structure. The Impact-Echo method is based on the excitation of the zero-group-velocity frequency of the first symmetric Lamb mode of a plate-like structure, in order to assess its thickness. Numerous publication elaborate on Impact-Echo theory, examples are (Gibson and Popovics 2005, Schubert and Köhler 2008 , Abraham and Popovics 2010). The measurements have been conducted using a setup that contains only commercially available components. The setup consists of an Olson CTG-2 concrete thickness gauge (Olsen Instruments, USA) for actuation and sensing and an 8-bit NI USB-5132 digital storage oscilloscope (National Instruments, USA) combined with the Echolyst software (Schweizerischer Verein für technische Inspektionen (SVTI), Switzerland) for data acquisition. Measurements were conducted using a grid of 23x23 points with a spacing of 50 mm. At each point 8192 samples were recorded at a sampling rate of 1 MS/s. The dataset contains the (X,Y) location in mm of the individual measurement points as well as the raw measurement data at those points. The data is provided in the formats *.mir/*.mhdr (Echolyst), *.npy (Python) and *.mat (Matlab) and *.csv to ease the import in various post-processing tools. KW - Nondestructive testing KW - Impact-echo KW - S1-ZGV mode KW - Concrete PY - 2021 DO - https://doi.org/10.7910/DVN/UNOH2U PB - Harvard College CY - Cambridge, MA, USA AN - OPUS4-53886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - Elemental Analysis Methods in Material- & Environmental Analysis N2 - Materials in contact with the environment release e.g., metal-ions, elemental species and/or (nano-)particles. Once these species and/or particles are released, they are ingested by organisms and cells and thus, might have a negative impact on the environment. Thus, identification as well as quantification of potentially harmful substances is of utmost importance and highly needed to assess ecotoxicological impact of (emerging) pollutants. The oral presentation provides an overview on the power of elemental analytical techniques, in particular ICP-MS as well as HR-CS-GFMAS in environmental research. Current research topics from Division 1.1 @ BAM - Inorganic trace analysis will be highlighted: i) Elemental Speciation & Isotope analysis - new tools: Among elemental species separation and quantification, one of the main challenges in environmental elemental speciation analysis is the distinction between anthropogenic and natural elemental species. The on-line combination of elemental speciation and isotope analysis combines “the best from both worlds” - species specific isotopic information becomes available. As an application example the analysis of current anti-fouling agents via CE/MCICP-MS will be highlighted. ii) HR-CS-GFMAS for PFC analysis: Per- and polyfluorinated compounds (PFC) are emerging contaminants in particular in soil and surface water samples. Due to the large number of compounds (>4700), target analytical methods are not sufficient and sum parameter methods for organically bound fluorine are highly needed. High resolution-continuum source-graphite furnace molecular absorption spectroscopy (HR-CS-GFMAS) based methods for organically bound fluorine analysis will be presented. Application examples (soil and surface water) will be highlighted. iii) Single cell-ICP-ToF-MS - ecotox. assessment: Single cell and single organism analysis for e.g. ecotoxicological/medicinal assessment are hot topics in the research field of ICP-MS. In particular ICP-ToF-MS is a powerful, emerging techniques in terms of single cell/particle analysis. Automated single cell/diatom-ICP-ToF-MS as a potential tool in ecotoxicological testing will be presented. T2 - Eingeladener Fachvortrag Kolloquium AG Bleiner - EMPA CY - Online meeting DA - 03.11.2021 KW - HR-CS-GFMAS KW - SC-ICP-ToF-MS KW - Speciation analysis PY - 2021 AN - OPUS4-53707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scala-Benuzzi, M. L. A1 - Soler-Illia, G. J. A. A. A1 - Rabia, J. A1 - Battaglini, F. A1 - Schneider, Rudolf A1 - Pereira, S. V. A1 - Messina, G. A. T1 - Immunosensor based on porous gold and reduced graphene platform for the determination of EE2 by electrochemical impedance spectroscopy N2 - In this work, we report an electrochemical immunosensor to detect ethinylestradiol in water samples, using electrochemical impedance spectroscopy (EIS) as a detection technique. For the development of this immunosensor, the direct modification of the working electrode of a screen-printed carbon electrode was carried out. First, to reduce the resistance of the electrode, electroreduced graphene was incorporated on the surface. Second, a porous gold structure was electrodeposited on reduced graphene by electrodeposition and the dynamic hydrogen bubble template assisted method. Thus, a marked increase in surface area was obtained for anti-EE2 antibodies immobilization. Subsequently, the specific anti-EE2 antibodies were covalently immobilized using α-lipoic acid for attaching them to the gold surface. The electrode modified with the antibodies was incubated for 30 min in the samples containing EE2, producing the specific Antigen antibody binding. As the charge transfer resistance of a redox probe in the electrode surface is governed by the surface blocking effects, the charge transfer resistance was related to the amount of EE2 captured to realize a quantitative determination. For this, the EIS measurements were performed in a 4 mM [Fe(CN)6]4−/3− solution in 0.1 M KCl. The obtained Nyquist diagrams were adjusted using the Randles circuit as an equivalent circuit to obtain the corresponding resistances. The developed methodology showed good selectivity, precision, and sensitivity; although the LOD obtained was higher than those presented in other published articles, it turned out to be an alternative that allows the determination of ethinylestradiol using a simple disposable electrode. KW - Ethinylestradiol KW - Biosensor KW - Elektrochemisch KW - Impedanz PY - 2021 DO - https://doi.org/10.1016/j.jelechem.2021.115604 SN - 1572-6657 VL - 897 SP - 115604 EP - 115611 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-54048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Raysyan, Anna A1 - Schneider, Rudolf T1 - Development of a Lateral Flow Immunoassay (LFIA) to Screen for the Release of the Endocrine Disruptor Bisphenol A from Polymer Materials and Products N2 - One of the most important chemicals used in the production of polymer plastics and coatings is bisphenol A. However, despite the large number of studies on the toxicity and hormonal activity of BPA, there are still open questions and thus considerable media attention regarding BPA toxicity. Hence, it is necessary to develop a sensitive, simple, cost-efficient, specific, portable, and rapid method for monitoring bisphenol A and for high sample throughput and on-site screening analysis. Lateral flow immunoassays have potential as rapid tests for on-site screening. To meet sensitivity criteria, they must be carefully optimized. A latex microparticle-based LFIA for detection of BPA was developed. The sensitivity of the assay was improved by non-contact printing of spot grids as the control and test lines with careful parameter optimization. Results of the test could be visually evaluated within 10 min with a visual cut-off of 10 µg/L (vLOD). Alternatively, photographs were taken, and image analysis performed to set up a calibration, which allowed for a calculated limit of detection (cLOD) of 0.14 µg/L. The method was validated for thermal paper samples against ELISA and LC–MS/MS as reference methods, showing good agreement with both methods KW - Endokrine Disruptoren KW - Polymere KW - Schnelltest KW - Endocrine disruptor KW - Bisphenol A KW - LFIA KW - Immunoassay PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-540492 DO - https://doi.org/10.3390/bios11070231 VL - 11 IS - 7 SP - 1 EP - 11 PB - MDPI CY - Basel AN - OPUS4-54049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, Rudolf T1 - Portable, antikörperbasierte Analysenverfahren für die Schadstofferfassung im Wasserkreislauf N2 - Die Wasseranalytik wird bestimmt von zwei Hauptbedarfen, einerseits der Erfassung der Gewässergüte und Grundwassergüte als Basis für die Bereitstellung einwandfreien Trinkwassers und zum anderen des Monitorings der Wasserqualität in den Prozessen der Wasseraufbereitung und der Abwasserreinigung. Für beide Anwendungsbereiche ist eine laborbasierte Analytik eher hinderlich, werden die Analysenergebnisse doch eigentlich vor Ort benötigt, um etwa Beprobungskampagnen rasch anpassen zu können. Des Weiteren werden die Daten auch schnell benötigt, um zeitnah in die technischen Prozesse einzugreifen. Organische Kontaminanten werden meist über chromatographische Verfahren, häufig gekoppelt mit einer massenspektrometrischen Detektion, in instrumentellen Labormethoden erfasst, und die hochauflösende Massenspektrometrie und die Non-target-Analytik haben viel zum Wissen über das Vorkommen, insbesondere von sogenannten „Emerging Contaminants“, beigetragen, sowie zum Verständnis der beteiligten Eintragspfade und Abbauwege. Moderne, portable Analysenmethoden und insbesondere Sensoren werden zukünftig aber ihren Platz in der Schadstofferfassung im Wasserkreislauf einnehmen. Dies gilt insbesondere für antikörperbasierte Analysenverfahren, da erst diese oft die nötige Selektivität und Sensitivität in die Detektionsmethoden einbringen. KW - Biosensoren KW - Schnelltests KW - Immunoassay KW - Abwasser PY - 2021 DO - https://doi.org/10.1002/vomw.202100005 VL - 119 IS - 2 SP - 35 EP - 53 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-54050 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Portable, antikörperbasierte Analysenverfahren für die Schadstofferfassung im Wasserkreislauf N2 - Die Wasseranalytik wird bestimmt von zwei Hauptbedarfen, einerseits der Erfassung der Gewässergüte und Grundwassergüte als Basis für die Bereitstellung einwandfrei-en Trinkwassers und zum anderen des Monitorings der Wasserqualität in den Prozes-sen der Wasseraufbereitung und der Abwasserreinigung. Für beide Anwendungsbe-reiche ist eine laborbasierte Analytik eher hinderlich, werden die Analysenergebnisse doch eigentlich vor Ort benötigt, um etwa Beprobungskampagnen rasch anpassen zu können. Desweiteren werden die Daten auch schnell benötigt, um zeitnah in die technischen Prozesse einzugreifen. Organische Kontaminanten werden meist über chromatographische Verfahren, häufig gekoppelt mit einer massenspektrometrischen Detektion, in instrumentelle Labormethoden erfasst und die hochauflösende Massen-spektrometrie und die Non-target-Analytik haben viel zum Wissen über das Vorkom-men, insbesondere von sog. „emerging contaminants“, beigetragen, sowie zum Ver-ständnis der beteiligten Eintragspfade und Abbauwege. Moderne, portable Analy-senmethoden und insbesondere Sensoren werden zukünftig aber ihren Platz in der Schadstofferfassung im Wasserkreislauf einnehmen. Dies gilt insbesondere für anti-körperbasierte Analysenverfahren, da erst diese oft die nötige Selektivität und Sensitivität in die Detektionsmethoden einbringen. T2 - Wasser 2021 - Jahrestagung der Wasserchemischen Gesellschaft in der GDCh CY - Online meeting DA - 10.05.2021 KW - Immunoassay KW - Biosensoren KW - Schnelltest KW - Elektrochemisch PY - 2021 AN - OPUS4-54051 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Environmental monitoring by high-throughput immunoanalytical methods and portable devices N2 - A vast number of emerging pollutants has been detected in the environment over the last decades. Analytical methods suitable for trace analysis are needed that are desirably also fast, inexpensive and, if possible, robust and portable. Immunoanalytical, i.e. antibody-based, methods which are available in a broad range of formats, can be profitably used here to analyse for the distribution and the trends of concentration levels of contaminants in the environment. Some of these formats are single-analyte but high-throughput methods. In order to use them wisely, indicator substances, sometimes called anthropogenic markers, should be selected and used in screening approaches. Other methods are suitable to be performed on portable instrumentation in the field (on-site) or in facilities such as wastewater treatment plants for on-line monitoring. Furthermore, there are array technologies that allow for parallel (multiplex) analysis of several analytes of interest. The microtiter-plate based ELISA (Enzyme-linked Immunosorbent Assay) is the method of choice for the analysis of a large number of samples [1]. ELISAs are available to monitor for anthropogenic markers such as the antiepileptic carbamazepine, the analgesic diclofenac, the antihistaminic cetirizine, the steroid hormone estrone, the antimicrobial sulfamethoxazole, the stimulants caffeine and cocaine, the priority pollutant bisphenol A, and the bile acid isolithocholic acid. For on-site screening and monitoring, simpler formats, like mix-and-read assays, e.g. the Fluorescence Polarization Immunoassay (FPIA) [2] or Lateral-flow Immunoassays (LFIA) [3] are more suitable tools, the latter based on dipsticks or cassettes, that is why they are also called pregnancy test-like assays. The suitability of multi-analyte formats such as immunomicroarrays depends on the choice of a signal-producing system that provides small uncertainties and good reproducibility of the measurements. Bead-based (“suspension”) arrays read out in flow cytometers are a powerful platform for multiplex assays [4]. Electrochemical formats run on portable devices provide additional advantages as no light source is required. They are most promising for stand-alone analysers and biosensors T2 - European Biosensor Symposium 2021 CY - Online meeting DA - 09.03.2021 KW - Biosensoren KW - Schnelltest KW - Elektrochemisch KW - Immunoassay PY - 2021 AN - OPUS4-54052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lee, P.-W. A1 - Kaynak, T. A1 - Al-Sabbagh, Dominik A1 - Emmerling, Franziska A1 - Schalley, C. T1 - Effect of Perfluorinated Side-Chain Length on the Morphology, Hydrophobicity, and Stability of Xerogel Coatings N2 - Superhydrophobic surfaces can be quickly formed with supramolecular materials. Incorporating low-molecular-weight gelators (LMWGs) with perfluorinated chains generates xerogel coatings with low surface energies and high roughness. Here, we examine and compare the properties of the xerogel coatings formed with eight different LMWGs. These LMWGs all have a trans-1,2-diamidocyclohexane core and two perfluorinated ponytails, whose lengths vary from three to ten carbon atoms (CF3 to CF10). Investigation of the xerogels aims to provide in-depth information on the chain length effect. LMWGs with a higher degree of fluorination (CF7 to CF10) form superhydrophobic xerogel coatings with very low surface energies. Scanning electron microscopy images of the coatings show that the aggregates of CF5 and CF7 are fibrous, while the others are crystal-like. Aggregates of CF10 are particularly small and further assemble into a porous structure on the micrometer scale. To test their stabilities, the xerogel coatings were flushed multiple times with a standardized water flush test. The removal of material from the surface in these flushes was monitored by a combination of the water contact angle, contact angle hysteresis, and coating thickness measurements. A new method based on image processing techniques was developed to reliably determine the change of the coating thickness. The CF7, CF9, and CF10 surfaces show consistent hydrophobicity and coating durability after repetitive flushing tests. The length of the perfluorinated side chains thus has a significant effect on the morphology of the deposited xerogel coatings, their roughness, and, in consequence, their hydrophobicity and mechanical durability. KW - Coating materials KW - Amorphous materials KW - Hydrophobicity KW - Materials Stability PY - 2021 DO - https://doi.org/10.1021/acs.langmuir.1c02341 SN - 1520-5827 VL - 37 IS - 49 SP - 14390 EP - 14397 PB - ACS Publications AN - OPUS4-54071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Van Den Bossche, T. A1 - Kunath, B. A1 - Schallert, K. A1 - Schäpe, S. A1 - Abraham, P. E. A1 - Armengaud, J. A1 - Arntzen, M. Ø. A1 - Bassignani, A. A1 - Benndorf, D. A1 - Fuchs, S. A1 - Giannone, R. J. A1 - Griffin, T. J. A1 - Hagen, L. H. A1 - Halder, R. A1 - Henry, C. A1 - Hettich, R. L. A1 - Heyer, R. A1 - Jagtap, P. A1 - Jehmlich, N. A1 - Jensen, M. A1 - Juste, C. A1 - Kleiner, M. A1 - Langella, O. A1 - Lehmann, T. A1 - Leith, E. A1 - May, P. A1 - Mesuere, B. A1 - Miotello, G. A1 - Peters, S. L. A1 - Pible, O. A1 - Queiros, P. T. A1 - Reichl, U. A1 - Renard, B. Y. A1 - Schiebenhoefer, H. A1 - Sczyrba, A. A1 - Tanca, A. A1 - Trappe, K. A1 - Trezzi, J.-P. A1 - Uzzau, S. A1 - Verschaffelt, P. A1 - von Bergen, M. A1 - Wilmes, P. A1 - Wolf, M. A1 - Martens, L. A1 - Muth, Thilo T1 - Critical Assessment of MetaProteome Investigation (CAMPI): A multi-laboratory comparison of established workflows N2 - Metaproteomics has matured into a powerful tool to assess functional interactions in microbial communities. While many metaproteomic workflows are available, the impact of method choice on results remains unclear. Here, we carry out a community-driven, multi-laboratory comparison in metaproteomics: the critical assessment of metaproteome investigation study (CAMPI). Based on well-established workflows, we evaluate the effect of sample preparation, mass spectrometry, and bioinformatic analysis using two samples: a simplified, laboratory-assembled human intestinal model and a human fecal sample. We observe that variability at the peptide level is predominantly due to sample processing workflows, with a smaller contribution of bioinformatic pipelines. These peptide-level differences largely disappear at the protein group level. While differences are observed for predicted community composition, similar functional profiles are obtained across workflows. CAMPI demonstrates the robustness of present-day metaproteomics research, serves as a template for multi-laboratory studies in metaproteomics, and provides publicly available data sets for benchmarking future developments. KW - Metaproteomics KW - Mass spectrometry KW - Data science KW - Benchmarking KW - Bioinformatics PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-541220 DO - https://doi.org/10.1038/s41467-021-27542-8 SN - 2041-1723 VL - 12 SP - 1 EP - 15 PB - Nature Publishing Group CY - London AN - OPUS4-54122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Quantifizierung der Unsicherheit für einen dünnbesetzten maschinellen Lerndatensatz (ML) in der zerstörungsfreien Prüfung im Bauwesen (ZfPBau) N2 - Das maschinelle Lernen (ML) wurde erfolgreich zur Lösung vieler Aufgaben in der zerstörungsfreien Prüfung im Bauwesen (ZfPBau) eingesetzt. Allerdings ist die Erstellung von Referenzdaten in den meisten Fällen extrem teuer und daher viel knapper als in anderen Forschungsbereichen. Auch decken die verfügbaren Daten mitunter nur ein einziges Szenario ab, so dass die Leistungsindikatoren oft nicht die tatsächliche Leistung des ML-Modells in der praktischen Anwendung widerspiegeln. Schätzungen, die die Übertragbarkeit von einem Szenario auf ein anderes quantifizieren, sind erforderlich, um dieser Herausforderung gerecht zu werden und den Weg für Anwendungen in der Praxis zu ebnen. In diesem Beitrag stellen wir Werkzeuge zur Beschreibung der Unsicherheit von ML in neuen ZfPBau-Szenarien vor. Zu diesem Zweck haben wir einen bestehenden Trainingsdatensatz zur Klassifizierung von Korrosionsschäden der Bewehrung in Beton um eine neue Fallstudie erweitert. Die Messungen wurden an großflächigen Betonproben mit eingebauter chloridinduzierter Korrosion des Bewehrungsstahls durchgeführt. Das Experiment simulierte den gesamten Lebenszyklus von chloridinduzierten Sichtbetonbauteilen im Labor. Unser Datensatz umfasst Potenzialfeld- und Radarmessungen. Die einzigartige Fähigkeit, die Schädigung zu überwachen und eine gezielte Korrosion einzuleiten, ermöglichte es, die Daten zu labeln - was für die Konstruktion von ML-Modellen entscheidend ist. Um die Übertragbarkeit zu untersuchen, erweitern wir unser Modell um Metadaten - wie etwa Konstruktionsmerkmale des Prüfkörpers und Umweltbedingungen. Dies erlaubt es, die Veränderung dieser Merkmale in neuen Szenarien mit statistischen Methoden als Unsicherheiten auszudrücken. Wir vergleichen verschiedene auf Stichproben und statistischer Verteilung basierende Ansätze und zeigen, wie diese Methoden eingesetzt werden können, um Wissenslücken von ML-Modellen in der ZfP zu schließen T2 - DGZfP Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Machine Learning KW - Zerstörungsfreie Prüfung KW - Datenfusion KW - Multi Sensor KW - Unsicherheitsquantifizierung PY - 2021 AN - OPUS4-54124 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Uncertainty quantification for a sparse machine learning (ML) data set in non-destructive testing in civil engineering (NDT-CE) N2 - ML has been successfully applied to solve many NDT-CE tasks. This is usually demonstrated with performance metrics that evaluate the model as a whole based on a given set of data. However, since in most cases the creation of reference data is extremely expensive, the data used is generally much sparser than in other areas, such as e-commerce. As a result, performance indicators often do not reflect the practical applicability of the ML model. Estimates that quantify transferability from one case to another are necessary to meet this challenge and pave the way for real world applications. In this contribution we invetigate the uncertainty of ML in new NDT-CE scenarios. For this purpose, we have extended an existing training data set for the classification of corrosion damage by a new case study. Our data set includes half-cell potential mapping and ground-penetrating radar measurements. The measurements were performed on large-area concrete samples with built-in chloride-induced corrosion of reinforcement. The experiment simulated the entire life cycle of chloride induced exposed concrete components in the laboratory. The unique ability to monitor deterioration and initiate targeted corrosion initiation allowed the data to be labelled - which is crucial to ML. To investigate transferability, we extend our data by including new design features of the test specimen and environmental conditions. This allows to express the change of these features in new scenarios as uncertainties using statistical methods. We compare different sampling and statistical distribution-based approaches and show how these methods can be used to close knowledge gaps of ML models in NDT. T2 - EGU General Assembly 2021 CY - Online meeting DA - 19.04.2021 KW - Data fusion KW - Non-destructive testing PY - 2021 DO - https://doi.org/10.5194/egusphere-egu21-8798 AN - OPUS4-54125 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Winkelmann, A. T1 - About the reliability of EBSD measurements: Data enhancement N2 - An extensive set of information about the diffracting volume is carried by EBSD patterns: the crystal lattice, the reciprocal lattice, the crystal structure, the crystal symmetry, the mean periodic number of the diffracting phase, the source point from where it has been projected (projection centre), the crystal orientation, the sample topography (local tilt), the (preparation) quality of defect density of the crystal, and possible pattern overlaps. Some of this information is used regularly in conventional EBSD analyses software while others are still waiting for a more widespread application. Despite the wealth of information available, the accuracy and precision of the data that are presently extracted from conventional EBSD patterns are often well below the actual physical limits. Using a selection of example applications, we will demonstrate the gain in angular resolution possible using relatively low-resolution patterns of approximately 20k pixels in combination with pattern matching (PM) approaches. In this way, fine details in a microstructure can be revealed which would otherwise be hidden in the orientation noise. KW - EBSD KW - Orientation precision KW - Disorientation KW - Grain boundary KW - Phase transformation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521618 DO - https://doi.org/10.1088/1757-899X/891/1/012018 VL - 891 SP - 012018 PB - IOP Science AN - OPUS4-52161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Albarrán Martínez, M. J. A1 - Ghigo, Tea T1 - The practice of writing inside an Egyptian monastic settlement N2 - Over the last few years, the Federal Institute for material research (BAM, Berlin) together with the Centre for the Study of Manuscript Cultures (CSMC, University of Hamburg) have initiated a systematic material investigation of black inks produced from Late Antiquity to the Middle Ages (ca. fourth century CE–fourteenth/fifteenth centuries CE), aimed primarily at extending and complementing findings from previous sporadic studies. Part of this systematic investigation has focused on Egyptian Coptic manuscripts, and the present preliminary study is one of its outputs. It centres on a corpus of 45 Coptic manuscripts—43 papyri and 2 ostraca—preserved at the Palau-Ribes and Roca-Puig collections in Barcelona. The manuscripts come from the Monastery of Apa Apollo at Bawit, one of the largest monastic settlements in Egypt between the Late Antiquity and the Early Islamic Period (sixth–eighth centuries CE). The composition of their black inks was investigated in situ using near-infrared reflectography (NIRR) and X-ray fluorescence (XRF). The analyses determined that the manuscripts were written using different types of ink: pure carbon ink; carbon ink containing iron; mixed inks containing carbon, polyphenols and metallic elements; and iron-gall ink. The variety of inks used for the documentary texts seems to reflect the articulate administrative system of the monastery of Bawit. This study reveals that, in contrast to the documents, written mostly with carbon-based inks, literary biblical texts were written with iron-gall ink. The frequent reuse of papyrus paper for certain categories of documents may suggest that carbon-based inks were used for ephemeral manuscripts, since they were easy to erase by abrasion. KW - Papyrus KW - Ink analysis KW - Coptic manuscripts KW - Bawit KW - Mixed ink KW - Near-infrared refectography KW - X-ray fuorescence PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528833 DO - https://doi.org/10.1186/s40494-021-00541-0 SN - 2050-7445 VL - 9 IS - 1 SP - 1 EP - 15 PB - Springer Open CY - Rome, Italy AN - OPUS4-52883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wurzler, Nina A1 - Schütter, Jan David A1 - Wagner, R. A1 - Dimper, Matthias A1 - Hodoroaba, Vasile-Dan A1 - Lützenkirchen-Hecht, D. A1 - Özcan Sandikcioglu, Özlem T1 - Preconditioning of AISI 304 stainless steel surfaces in the presence of flavins—Part II: Effect on biofilm formation and microbially influenced corrosion processes N2 - Biofilm formation and microbially influenced corrosion of the iron-reducing microorganism Shewanella putrefaciens were investigated on stainless steel surfaces preconditioned in the absence and presence of flavin molecules by means of XANES (X-ray absorption near-edge structure) analysis and electrochemical methods. The results indicate that biofilm formation was promoted on samples preconditioned in electrolytes containing minute amounts of flavins. On the basis of the XANES results, the corrosion processes are controlled by the iron-rich outer layer of the passive film. Biofilm formation resulted in a cathodic shift of the open circuit potential and a protective effect in terms of pitting corrosion. The samples preconditioned in the absence of flavins have shown delayed pitting and the samples preconditioned in the presence of flavins did not show any pitting in a window of −0.3- to +0.0-V overpotential in the bacterial medium. The results indicate that changes in the passive film chemistry induced by the presence of minute amounts of flavins during a mild anodic polarization can change the susceptibility of stainless steel surfaces to microbially influenced corrosion. KW - Biofilms KW - XANES KW - Microbially influenced corrosion (MIC) PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528130 DO - https://doi.org/10.1002/maco.202012192 VL - 72 IS - 6 SP - 983 EP - 994 PB - Wiley AN - OPUS4-52813 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim A1 - Lecompagnon, Julien A1 - Hirsch, Philipp Daniel A1 - Burgholzer, Peter A1 - Jung, Peter A1 - Caire, Giuseppe A1 - Ziegler, Mathias T1 - Laser excited super resolution thermal imaging for nondestructive testing N2 - The work to be presented focuses on our most recent studies to laser excited super resolution (SR) thermography. The goal of nondestructive testing with SR is to facilitate the separation of closely spaced defects. Photothermal SR can be realized by performing structured illumination measurements in com-bination with the use of deconvolution algorithms in post-processing. We explain that stepwise as well as continuous scanning techniques are applicable to generate structured illumination measurements. Finally, we discuss the effect of experimental parameters and image processing techniques to find the optimal SR technique which leads to the highest reconstruction quality within laser thermography. T2 - Sensor and Measurement Science International Conference SMSI 2021 CY - Online meeting DA - 03.05.2021 KW - Super resolution KW - Laser thermography KW - Nondestructive testing KW - Laser scanning KW - Photothermal imaging PY - 2021 SP - 181 EP - 182 AN - OPUS4-52780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim T1 - Laser excited super resolution thermal imaging for nondestructive testing N2 - The work to be presented focuses on our most recent studies to laser excited super resolution (SR) thermography. The goal of nondestructive testing with SR is to facilitate the separation of closely spaced defects. Photothermal SR can be realized by performing structured illumination measurements in com-bination with the use of deconvolution algorithms in post-processing. We explain that stepwise as well as continuous scanning techniques are applicable to generate structured illumination measurements. Finally, we discuss the effect of experimental parameters and image processing techniques to find the optimal SR technique which leads to the highest reconstruction quality within laser thermography. T2 - Sensor and Measurement Science International Conference SMSI 2021 CY - Online meeting DA - 03.05.2021 KW - Super resolution KW - Laser thermography KW - Nondestructive testing KW - Laser scanning KW - Photothermal imaging PY - 2021 AN - OPUS4-52781 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim T1 - Neue Verfahren der thermografischen Super Resolution mit strukturierter 1D-Lasererwärmung N2 - Die thermografische ZfP basiert auf der Wechselwirkung von thermischen Wellen mit Inhomogenitäten. Die Ausbreitung von thermischen Wellen von der Wärmequelle zur Inhomogenität und zur Detektionsoberfläche entsprechend der thermischen Diffusionsgleichung führt dazu, dass zwei eng beieinander liegende Defekte fälschlicherweise als ein Defekt im gemessenen Thermogramm erkannt werden können. Um diese räumliche Auflösungsgrenze zu durchbrechen, also eine Super Resolution zu realisieren, kann die Kombination von räumlich strukturierter Erwärmung und numerischen Verfahren des Compressed Sensings verwendet werden. Für unsere Arbeiten benutzen wir Hochleistungs-Laser im Kilowatt-Bereich um die Probe entweder hochaufgelöst entlang einer Linie (1D) abzurastern oder strukturiert zu erwärmen. Die Verbesserung des räumlichen Auflösungsvermögens zur Defekterkennung hängt dann im klassischen Sinne direkt von der Anzahl der Messungen ab. Mithilfe des Compressed Sensings und Vorkenntnissen über das System ist es jedoch möglich die Anzahl der Messungen zu reduzieren und trotzdem Super Resolution zu erzielen. Wie viele Messungen notwendig sind und wie groß der Auflösungsgewinn gegenüber der konventionellen thermografischen Prüfung mit flächiger Erwärmung ist, hängt von einer Reihe von Messparametern, der Messstrategie, Probeneigenschaften und den verwendeten Rekonstruktionsalgorithmen ab. Unsere Studien befassen sich mit dem Einfluss der experimentellen Parameter, wie z.B. der Pulslänge der Laserbeleuchtung und der Größe des Laserspots. Weiterhin haben wir uns mit der Wahl der Parameter in der Rekonstruktion auseinandergesetzt, die einen Einfluss auf das im Compressed Sensing zugrundeliegende Minimierungsproblem haben. Für jeden getesteten Parametersatz wurde eine Rekonstruktionsqualität berechnet. Schließlich wurden die Defektrekonstruktionen basierend auf den Parameternsätzen verglichen, sodass eine Parameterwahl für hohe Rekonstruktionsqualitäten mit thermografischer Super Resolution empfohlen werden kann. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Super resolution KW - Thermografie KW - Strukturiert KW - Photothermisch PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527820 AN - OPUS4-52782 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim T1 - Neue Verfahren der thermografischen Super Resolution mit strukturierter 1D-Lasererwärmung N2 - Die thermografische ZfP basiert auf der Wechselwirkung von thermischen Wellen mit Inhomogenitäten. Die Ausbreitung von thermischen Wellen von der Wärmequelle zur Inhomogenität und zur Detektionsoberfläche entsprechend der thermischen Diffusionsgleichung führt dazu, dass zwei eng beieinander liegende Defekte fälschlicherweise als ein Defekt im gemessenen Thermogramm erkannt werden können. Um diese räumliche Auflösungsgrenze zu durchbrechen, also eine Super Resolution zu realisieren, kann die Kombination von räumlich strukturierter Erwärmung und numerischen Verfahren des Compressed Sensings verwendet werden. Für unsere Arbeiten benutzen wir Hochleistungs-Laser im Kilowatt-Bereich um die Probe entweder hochaufgelöst entlang einer Linie (1D) abzurastern oder strukturiert zu erwärmen. Die Verbesserung des räumlichen Auflösungsvermögens zur Defekterkennung hängt dann im klassischen Sinne direkt von der Anzahl der Messungen ab. Mithilfe des Compressed Sensings und Vorkenntnissen über das System ist es jedoch möglich die Anzahl der Messungen zu reduzieren und trotzdem Super Resolution zu erzielen. Wie viele Messungen notwendig sind und wie groß der Auflösungsgewinn gegenüber der konventionellen thermografischen Prüfung mit flächiger Erwärmung ist, hängt von einer Reihe von Messparametern, der Messstrategie, Probeneigenschaften und den verwendeten Rekonstruktionsalgorithmen ab. Unsere Studien befassen sich mit dem Einfluss der experimentellen Parameter, wie z.B. der Pulslänge der Laserbeleuchtung und der Größe des Laserspots. Weiterhin haben wir uns mit der Wahl der Parameter in der Rekonstruktion auseinandergesetzt, die einen Einfluss auf das im Compressed Sensing zugrundeliegende Minimierungsproblem haben. Für jeden getesteten Parametersatz wurde eine Rekonstruktionsqualität berechnet. Schließlich wurden die Defektrekonstruktionen basierend auf den Parameternsätzen verglichen, sodass eine Parameterwahl für hohe Rekonstruktionsqualitäten mit thermografischer Super Resolution empfohlen werden kann. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Super resolution KW - Laserthermografie KW - Strukturiertes Heizen KW - Photothermisch PY - 2021 AN - OPUS4-52783 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lugovtsova, Yevgeniya A1 - Bulling, Jannis A1 - Mesnil, O. A1 - Prager, Jens A1 - Gohlke, Dirk A1 - Boller, C. T1 - Damage quantification in an aluminium-CFRP composite structure using guided wave wavenumber mapping: Comparison of instantaneous and local wavenumber analyses N2 - Composite-overwrapped pressure vessels (COPV) are increasingly used in the transportation industry due to their high strength to mass ratio. Throughout the years, various designs were developed and found their applications. Currently, there are five designs, which can be subdivided into two main categories - with a load-sharing metal liner and with a non-load-sharing plastic liner. The main damage mechanism defining the lifetime of the first type is fatigue of the metal liner, whereas for the second type it is fatigue of the composite overwrap. Nevertheless, one damage type which may drastically reduce the lifetime of COPV is impact-induced damage. Therefore, this barely visible damage needs to be assessed in a non-destructive way to decide whether the pressure vessel can be further used or has to be put out of service. One of the possible methods is based on ultrasonic waves. In this contribution, both conventional ultrasonic testing (UT) by high-frequency bulk waves and wavenumber mapping by low frequency guided waves are used to evaluate impact damage. Wavenumber mapping techniques are first benchmarked on a simulated aluminium panel then applied to experimental measurements acquired on a delaminated aluminium-CFRP composite plate which corresponds to a structure of COPV with a load-sharing metal liner. The analysis of experimental data obtained from measurements of guided waves propagating in an aluminium-CFRP composite plate with impact-induced damage is performed. All approaches show similar performance in terms of quantification of damage size and depths while being applied to numerical data. The approaches used on the experimental data deliver an accurate estimate of the in-plane size of the large delamination at the aluminium-CFRP interface but only a rough estimate of its depth. Moreover, none of the wavenumber mapping techniques used in the study can quantify every delamination between CFRP plies caused by the impact, which is the case for conventional UT. This may be solved by using higher frequencies (shorter wavelengths) or more advanced signal processing techniques. All in all, it can be concluded that imaging of complex impact damage in fibre-reinforced composites based on wavenumber mapping is not straightforward and stays a challenging task. KW - Ultrasonic guided waves KW - Instantaneous wavenumber analysis KW - Local wavenumber analysis KW - Signal processing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528203 DO - https://doi.org/10.1016/j.ndteint.2021.102472 SN - 0963-8695 VL - 122 SP - 2472 PB - Elsevier Ltd. CY - Amsterdam, Netherlands AN - OPUS4-52820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tschöke, K. A1 - Müller, I. A1 - Memmolo, V. A1 - Moix-Bonet, M. A1 - Moll, J. A1 - Lugovtsova, Yevgeniya A1 - Golub, M. A1 - Sridaran Venkat, R. A1 - Schubert, L. T1 - Feasibility of Model-Assisted Probability of Detection Principles for Structural Health Monitoring Systems based on Guided Waves for Fibre-Reinforced Composites N2 - In many industrial sectors, Structural Health Monitoring (SHM) is considered as an addition to Non-Destructive Testing (NDT) that can reduce maintenance effort during lifetime of a technical facility, structural component or vehicle. A large number of SHM methods is based on ultrasonic waves, whose properties change depending on structural health. However, the wide application of SHM systems is limited due to the lack of suitable methods to assess their reliability. The evaluation of the system performance usually refers to the determination of the Probability of Detection (POD) of a test procedure. Up to now, only few limited methods exist to evaluate the POD of SHM systems, which prevent them from being standardised and widely accepted in industry. The biggest hurdle concerning the POD calculation is the large amount of samples needed. A POD analysis requires data from numerous identical structures with integrated SHM systems. Each structure is then damaged at different locations and with various degrees of severity. All of this is connected to high costs. Therefore, one possible way to tackle this problem is to perform computer-aided investigations. In this work, the POD assessment procedure established in NDT according to the Berens model is adapted to guided wave-based SHM systems. The approach implemented here is based on solely computer-aided investigations. After efficient modelling of wave propagation phenomena across an automotive component made of a carbon fibre-reinforced composite, the POD curves are extracted. Finally, the novel concept of a POD map is introduced to look into the effect of damage position on system reliability. KW - Reliability KW - Acoustics KW - Monitoring KW - Automotive engineering KW - Elastodynamic Finite Inegration Technique PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528218 DO - https://doi.org/10.1109/TUFFC.2021.3084898 VL - 68 IS - 10 SP - 3156 EP - 3173 AN - OPUS4-52821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gantois, F. T1 - ALCOREF "Certified forensic alcohol reference materials" N2 - The presentation provides an overview of the EMPIR project ALCOREF “Certified forensic alcohol reference materials”. Results of an EURAMET intercomparison of ethanol in water reference materials developed in the project are presented, and two different statistical models for the key comparison reference function are discussed, the Frequentist approach and a Bayesian approach. T2 - CCQM Organic Analysis Working Group Meeting CY - Online meeting DA - 04.05.2021 KW - Certified reference material KW - EMPIR project KW - Interlaboratory comparison PY - 2021 AN - OPUS4-52852 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Non-Destructive Testing of Composite Pressure Vessels using Conventional and High-Frequency Eddy Current Technique N2 - Pressure vessels for the transport of hazardous gases are subjected to a hydraulic internal pressure test. Basis for the design of metallic pressure vessels is the fatigue strength according to Wöhler, whereby the number of load changes can be equated with the number of filling / emptying cycles of the pressure vessel. Metallic pressure vessels are increasingly replaced by composite pressure vessels due to the weight savings. However, at composite preasure vessels it is not possible to conclude from the number of load cycles on the fatigue strength, because composite pressure vessels are ageing even at constant internal pressure. Non-destructive conventional and high frequency eddy current testing of the metallic liner and load bearing CFRP layer are presented as an alternative to hydraulic internal pressure test. T2 - TAHYA Workshop CY - Online meeting DA - 02.06.2021 KW - Non-destructive testing KW - Composite preasure vessel KW - Eddy currnet testing PY - 2021 AN - OPUS4-52856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Beck, Uwe A1 - Ermilova, Elena A1 - Schneider, S. A1 - Peters, S. T1 - Gemeinsamer Abschlussbericht WIPANO-Vorhaben „Standardisierung und Normung der Ellipsometrie als universeller Spektroskopie“ N2 - Im Vorhaben SNELLIUS wurden in enger Zusammenarbeit der BAM mit den Firmen Accurion und SENTECH Instruments aufbauend auf der Norm DIN 50989-1 „Ellipsometrie - Teil 1: Grundlagen; Ellipsometry – Part 1: Principles“ insgesamt fünf Normenentwürfe erarbeitet, die fünf Modell-basierten Anwendungsfällen der Ellipsometrie entsprechen. Unter Berücksichtigung des neuartigen Modell-basierten Normungskonzepts wurde in den Normenentwürfen erstmals eine GUM- und DIN EN ISO/IEC 17025:2018 konforme Bestimmung bzw. Abschätzung der Messunsicherheit umgesetzt. Dies erforderte neben der textlichen Erstellung auch umfangreiche experimentelle Arbeiten bei den Firmen, Vergleichsversuche und komplementäre Modell- und Datenevaluierungen, da sowohl die verwendete ellipsometrische Hardware (unterschiedliche ellipsometrische Funktionsprinzipien) als auch die ellipsometrische Software (Modell-Randbedingungen, Fitalgorithmus) firmenspezifisch zum Teil sehr unterschiedlich sind. Hierbei mussten in einem Konsensprozess Lösungen gefunden werden, die die beiden deutschen Ellipsometer-Anbieter Accurion (Imaging-Ellipsometrie) und SENTECH Instruments (Mapping Ellipsometrie) gleichermaßen akzeptieren konnten und die zudem einen Transfer auf die Internationale Ebene (ISO Norm) ermöglichen, also vom Grundsatz her auch auf weitere Ellipsometerhersteller wie (J. A. Woollam Co., USA; SEMILAB, Ungarn; HORIBA, Japan) mit wieder anderen ellipsometrischen Funktionsprinzipien, Hard- und Softwarelösungen anwendbar sind. Die weitgehende Unabhängigkeit von ellipsometrischen Funktionsprinzipien, Hard- und Softwarelösungen wurde dadurch erreicht, dass normativ festgelegt wurde, dass die ellipsometrischen Größen PSI und DELTA im Sinne von DIN ENISO/IEC 17025 als Rohdaten fungieren. KW - Ellipsometrie-Norm KW - Messunsicherheit ellipsometrischer Messungen KW - Validierungskonzepte ellipsometrischer Messungen KW - DIN 50989, Teile 1 bis 6 KW - DIN EN ISO/IEC 17025:2018 und GUM Kompatibilität PY - 2021 SP - 1 EP - 16 AN - OPUS4-52857 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Mapping und Imaging modifizierter Oberflächen: Generische Kenngrößen, Fehlstellen, Reinigungszustand und Haftfestigkeit N2 - Der Vortrag widmet sich dem Mapping und Imaging modifizierter Oberflächen: Generische Kenngrößen, Fehlstellen, Reinigungszustand und Haftfestigkeit. Es werden Untersuchungsmethoden zu ihrer Prüfung dargestellt. T2 - 37. ak-adp 2021, Jena CY - Online meeting DA - 16.06.2021 KW - Qualitätssicherung KW - Mapping modifizierter Oberflächen KW - Generische Kenngrößen KW - Haftfestigkeit KW - Klebfestigkeit PY - 2021 AN - OPUS4-52870 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - HR-CS-GFMAS as a promising new tool for the analysis of organo-fluorine in environmental samples N2 - New HR-CS-GFMAS based methods for organically bound fluorine detection in environmental samples. T2 - CRC Colloquium - CRC 1349 Fluorine-Specific Interactions CY - Online meeting DA - 21.06.2021 KW - HR-CS-GFMAS KW - Organically bound fluorine KW - Fluorine sum parameter KW - Environmental analysis PY - 2021 AN - OPUS4-52844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bennet, Francesca A1 - Burr, L. A1 - Schmid, D. A1 - Hodoroaba, Vasile-Dan T1 - Towards a method for quantitative evaluation of nanoparticle from suspensions via microarray printing and SEM analysis N2 - As part of the development of a library of accurate and efficient methods for measurement of nanoparticle properties, we develop and optimize a method for the efficient analysis of nanoparticle size distribution from suspensions via microprinting and digital analysis of electron microscopy (SEM and TEM) images, with the ultimate aim of automated quantitative concentration analysis (calculated from drop volume). A series of different nanoparticle suspensions (gold, latex, and SiO2 in varying sizes and concentrations) were printed onto TEM grids in a 4 x 4 array in the concentration range 7x10^8 to 1x10^11 nanoparticles/mL and imaged with SEM. Concentrations and printing conditions (temperature, relative humidity) were varied in order to minimize the coffee-ring effect. KW - Nanoparticles KW - Particle size distribution KW - Electron microscopy KW - Microarray printing KW - Sample preparation KW - Nanoparticle concentration PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528455 DO - https://doi.org/10.1088/1742-6596/1953/1/012002 VL - 1953 SP - 012002 PB - IOP Publishing AN - OPUS4-52845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simões, R. G. A1 - Melo, P. L. T. A1 - Bernardes, C. E. S. A1 - Heilmann, Maria A1 - Emmerling, Franziska A1 - Minas da Piedade, M. E. T1 - Linking Aggregation in Solution, Solvation, and Solubility of Simvastatin: An Experimental and MD Simulation Study N2 - The solubility is generally thought to be higher if the solvent effectively solvates solute molecules that are well-separated from each other. The present work suggests, however, that the formation of large solute aggregates does not necessarily imply less effective solvation and lower solubility. Measurements of the solubility of simvastatin (one of the most commonly prescribed antihyperlipidemic drugs) in three solvents with different polarities and protic characters, led to the solubility order acetone > ethyl acetate > ethanol, in the full temperature range covered by the experiments (283–308 K). An analysis of the structures of the different solutions on the basis of molecular dynamics simulation results indicated that this trend seems to be determined by a balance between the solute tendency toward aggregation and the ability of the solvent to efficiently solvate it, by integrating the cluster structures, regardless of their size, and effectively establishing solvent–solute interactions. KW - Simvastatin KW - Solubility KW - API KW - Aggregation PY - 2021 DO - https://doi.org/10.1021/acs.cgd.0c01325 VL - 21 IS - 1 SP - 544 EP - 551 AN - OPUS4-52185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thinnes, A. A1 - Westenberger, M. A1 - Piechotta, Christian A1 - Letho, L. A1 - Wirth, F. A1 - Lau, H. A1 - Klein, J. T1 - Cholinergic and metabolic effects of metformin in mouse brain N2 - Metformin is widely used as a first-line treatment for type 2 diabetes, but central effects of metformin have received little attention. When metformin (200 mg/kg i.p.) was administered to C57Bl6 mice, metformin concentration in cerebrospinal fluid peaked at 29 μM after 30 min but dropped quickly and was low at 90 min. In mouse hypothalamus sampled by microdialysis, systemically administered metformin caused minor and transient increases of acetylcholine, glucose and lactate while choline levels decreased. When metformin (0.2−10 mM) was locally infused via retrodialysis, there was a short-lasting increase of acetylcholine in the hypothalamus. Extracellular lactate levels in hypothalamus showed a massive increase upon metformin infusion while glucose levels decreased. In isolated mitochondria of mouse brain, metformin inhibited oxygen consumption and the activity of complex I. Inhibition of mitochondrial respiration likely explains lactate formation in the brain during metformin infusion which may cause lactic acidosis during metformin intoxication. The changes of cholinergic activity in the hypothalamus may be associated with appetite suppression observed during metformin treatment. KW - Metformin KW - Blood-brain barrier KW - Lactate KW - Glucose KW - Microdialysis KW - Hypothalamus PY - 2021 DO - https://doi.org/10.1016/j.brainresbull.2021.02.018 SN - 0361-9230 VL - 170 SP - 211 EP - 217 PB - Elsevier CY - Amsterdam, Niederlande AN - OPUS4-52189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - ROP of L-lactide and ε-caprolactone catalyzed by tin(ii) andtin(iv) acetates–switching from COOH terminated linear chains to cycles N2 - The catalytic potential of tin(II)acetate, tin(IV)acetate, dibutyltin-bis-acetate and dioctyl tin-bis-acetate was compared based on polymerizations of L-lactide conducted in bulk at 160 or 130°C. With SnAc2 low-Lac/Cat ratios (15/1–50/1) were studied and linear chains having one acetate and one carboxyl end group almost free of cyclics were obtained. Higher monomer/catalyst ratios and lower temperatures favored formation of cycles that reached weight average molecular weights (Mw's) between 100,000 and 2,500,000. SnAc4 yielded mixtures of cycles and linear species under all reaction conditions. Dibutyltin- and dioctyl tin bis-acetate yielded cyclic polylactides under most reaction conditions with Mw's in the range of 20,000–80,000. Ring-opening polymerizations performed with ε-caprolactone showed similar trends, but the formation of COOH-terminated linear chains was significantly more favored compared to analogous experiments with lactide. The reactivity of the acetate catalysts decreased in the following order: SnAc2> SnAc4>Bu2SnAc2~Oct2SnAc2 KW - Polylactide KW - MALDI-TOF MS KW - Catalyst KW - Ring-opening polymerization KW - Tin acetates PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521923 DO - https://doi.org/10.1002/pol.20200866 VL - 59 IS - 5 SP - 439 EP - 450 PB - Wiley Online Library AN - OPUS4-52192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, U. T1 - Schnelle Messung und tomographische Rekonstruktion von Brennflecken < 5 μm durch Aufnahmen strukturierter Prüfkörper N2 - Im Europäischen EMPIR-Projekt „NanoXSpot“ (Measurement of the focal spot size of Xray tubes with spot sizes down to 100 nm) werden neue Messmethoden für Brennflecke von Röntgenröhren entwickelt. Teil des Projektes ist die Entwicklung eines zur Lochkameramethode äquivalenten Messverfahrens für kleine Brennflecke. ASTM E 1165-20, Annex A, beschreibt die Bestimmung von Brennfleckgrößen aus Kantenprofilen von Lochaufnahmen für Röntgenröhren mit Brennflecken > 50 μm. Es wurde bereits vorgeschlagen über die Analyse der richtungsabhängigen Kantenunschärfe einer Lochblende und anschließender CT-Rekonstruktion die Intensitätsverteilung des Brennflecks äquivalent zur Lochkameraaufnahme zu berechnen. Die Lochkameramethode, wie in EN 12543-2 und ASTM E 1165-20 beschrieben, ist im unteren Größenbereich für Mikrofokusröhren nicht geeignet, da Pinholes < 10 μm schwer zu fertigen sind und lange Belichtungszeiten erwartet werden. Mit Hilfe exakt gefertigter Lochblenden sowie strukturierter Targets mit konvergierenden Strukturen wird der Bereich mit der Single-Shot-CT-Methode auf die Messung von Mikrofokusröhren, alternativ zur Vermessung von Kanten oder Strichgruppenkörpern, erweitert. Die rekonstruierten Brennfleckformen werden mit Kanten und Lochkameraaufnahmen quantitativ verglichen, um die Messgenauigkeit zu bewerten. Außerdem werden CNR und Messzeit bestimmt, um die Wirtschaftlichkeit der Verfahren zu bewerten. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Radiographie KW - Tomographie KW - Röntgenröhren KW - Charakterisierung von Brennflecken PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526692 UR - https://jahrestagung.dgzfp.de/Programm#P15 AN - OPUS4-52669 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - How to trace a cereal killer? N2 - How to trace the "cereal" killer? Fungal secondary metabolites, aka mycotoxins, pose a severe health risk for humans and animals. Since their occurrence in food, such as cereal products, is inevitable, the detection is of considerable importance. I want to demonstrate how the trace analysis of mycotoxins in foodstuff can be performed outside the laboratory. For this purpose, sensitive, antibody-based methods are combined with electrochemical smartphone-based detection. T2 - Bionnale 2021 CY - Online meeting DA - 12.05.2021 KW - Mycotoxins KW - Electrochemistry KW - Ochratoxin A KW - Food safety PY - 2021 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-52658 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reuter, T. A1 - Plotzki, David A1 - Borges de Oliveira, F. A1 - Hausotte, T. T1 - Simulative Untersuchung des Einflusses von Bildrauschen auf dimensionelle Messungen mit industriellen Computertomografen N2 - Die industrielle Röntgen-Computertomografie (CT) etabliert sich für die Anwendung in der dimensionellen Messtechnik. Sie bietet als zerstörungsfreies Messverfahren das Potential, sowohl innen- als auch außenliegende Merkmale holistisch zu erfassen. Für die Bestimmung der Güte eines Messwerts muss die dem Messwert zugeordnete Messunsicherheit ermittelt werden. Dabei kann, nach derzeitigem Stand der Technik und Normung, die aufgabenspezifische Messunsicherheit nach VDI/VDE 2630 Blatt 2.1 nur unter hohem Aufwand mit einer Vielzahl an experimentellen Wiederholmessungen ermittelt werden. Ziel diverser Forschungs-projekte zu diesem Thema ist es daher, eine numerische Messunsicherheitsbestimmung zu erreichen. Dafür ist es notwendig, alle signifikanten Einflussgrößen zu erfassen, deren Unsicherheitsbeiträge zu bestimmen und zu bewerten. In diesem Beitrag wird der Einfluss des Bildrauschens auf verschiedene dimensionelle Messgrößen simulativ untersucht. Mithilfe eines prismatischen Prüfkörpers, der eine Vielzahl an Geometrieelementen aufweist, werden verschiedene Messgrößen unterschiedlicher Komplexität betrachtet. Ziel ist es, für diese Messgrößen zu testen, wie diese auf das Bildrauschen reagieren. Dieses wird dabei durch das Signal-Rausch-Verhältnis (SNR) der Projektionsgrauwerte beschrieben und variiert. Es werden Wiederholsimulationen durchgeführt, damit eine statistische Aussage über die Verteilung der Messwerte möglich ist und der Einfluss des Rauschens auf verschiedene Messgrößen individuell beurteilt werden kann. Das Simulationsszenario wird so gestaltet, dass lediglich das Bildrauschen Einfluss auf die Messung hat. Die berechneten Verteilungsbreiten lassen mit sinkendem SNR eine deutliche Zunahme erkennen, insbesondere bei der Bestimmung von Formabweichungen. Simuliert wird mit der Software aRTist 2.10 (BAM). T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Rauschen KW - Computertomografie KW - Dimensionelle Messung KW - Simulation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527144 SP - 1 EP - 11 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung e.V. (DGZfP) CY - Berlin AN - OPUS4-52714 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adams, L. C. A1 - Brangsch, J. A1 - Kaufmann, Jan Ole A1 - Mangarova, D. B. A1 - Moeckel, J. A1 - Kader, A. A1 - Buchholz, R. A1 - Karst, U. A1 - Botnar, R. M. A1 - Hamm, B. A1 - Makowski, M. R. A1 - Keller, S. T1 - Effect of Doxycycline on Survival in Abdominal Aortic Aneurysms in a Mouse Model N2 - Background. Currently, there is no reliable nonsurgical treatment for abdominal aortic aneurysm (AAA). This study, therefore, investigates if doxycycline reduces AAA growth and the number of rupture-related deaths in a murine ApoE−/− model of AAA and whether gadofosveset trisodium-based MRI differs between animals with and without doxycycline treatment. Methods. Nine ApoE−/− mice were implanted with osmotic minipumps continuously releasing angiotensin II and treated with doxycycline (30 mg/kg/d) in parallel. After four weeks, MRI was performed at 3T with a clinical dose of the albumin-binding probe gadofosveset (0.03 mmol/kg). Results were compared with previously published wild-type control animals and with previously studied ApoE−/− animals without doxycycline treatment. Differences in mortality were also investigated between these groups. Results. In a previous study, we found that approximately 25% of angiotensin II-infused ApoE−/− mice died, whereas in the present study, only one out of 9 angiotensin II-infused and doxycycline-treated ApoE−/− mice (11.1%) died within 4 weeks. Furthermore, doxycycline-treated ApoE−/− mice showed significantly lower contrast-to-noise (CNR) values in MRI compared to ApoE−/− mice without doxycycline treatment. In vivo measurements of relative signal enhancement (CNR) correlated significantly with ex vivo measurements of albumin staining (R2 = 0.58). In addition, a strong visual colocalization of albumin-positive areas in the fluorescence albumin staining with gadolinium distribution in LA-ICP-MS was shown. However, no significant difference in aneurysm size was observed after doxycycline treatment. Conclusion. The present experimental in vivo study suggests that doxycycline treatment may reduce rupture-related deaths in AAA by slowing endothelial damage without reversing aneurysm growth. KW - Ggadolinium KW - MRI KW - Magnetic resonance imaging KW - Osmotic minipumps KW - Tetracyclin KW - Antibiotics KW - Angiotensin II KW - LA-ICP-MS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527015 DO - https://doi.org/10.1155/2021/9999847 SP - 9999847 PB - Hindawi CY - London AN - OPUS4-52701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Tokarski, T. A1 - Rychlowski, L. A1 - Cios, G. A1 - Winkelmann, A. T1 - Crystallographic analysis of the lattice metric (CALM) from single electron backscatter diffraction or transmission Kikuchi diffraction patterns N2 - A new software is presented for the determination of crystal lattice parameters from the positions and widths of Kikuchi bands in a diffraction pattern. Starting with a single wide-angle Kikuchi pattern of arbitrary resolution and unknown phase, the traces of all visibly diffracting lattice planes are manually derived from four initial Kikuchi band traces via an intuitive graphical user interface. A single Kikuchi bandwidth is then used as reference to scale all reciprocal lattice point distances. Kikuchi band detection, via a filtered Funk transformation, and simultaneous display of the band intensity profile helps users to select band positions and widths. Bandwidths are calculated using the first derivative of the band profiles as excess-deficiency effects have minimal influence. From the reciprocal lattice, the metrics of possible Bravais lattice types are derived for all crystal systems. The measured lattice parameters achieve a precision of <1%, even for good quality Kikuchi diffraction patterns of 400 x 300 pixels. This band-edge detection approach has been validated on several hundred experimental diffraction patterns from phases of different symmetries and random orientations. It produces a systematic lattice parameter offset of up to ±4%, which appears to scale with the mean atomic number or the backscatter coefficient. KW - Electron backscatter diffraction KW - Kikuchi patterns KW - Lattice parameters KW - Radon transform PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527076 DO - https://doi.org/10.1107/S1600576721004210 SN - 1600-5767 VL - 54 IS - Pt 3 SP - 1012 EP - 1022 AN - OPUS4-52707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ecke, Alexander A1 - Bohm, Konrad A1 - Schneider, Rudolf T1 - Magnetpartikelbasierte Immunoassays als vielseitiges Werkzeug für die Umweltanalytik N2 - Der Bedarf nach schnellen und kostengünstigen Analysemethoden in der (Trink-)Wasseranalytik steigt mit dem zunehmenden Eintrag pharmazeutisch aktiver Substanzen in die Umwelt. Insbesondere die Kontamination mit Antibiotika erscheint neben ökotoxikologischen Effekten vor allem in Hinblick auf die Evolution resistenter Keime im Wasser besorgniserregend. Wir berichten hier über die Entwicklung eines magnetpartikelbasierten Immunoassays (MBBA) zur Detektion des Breitbandantibiotikums Amoxicillin (AMX) in Wasserproben, der im Vergleich zum entsprechenden Enzyme-linked Immunosorbent Assay (ELISA) eine wesentlich kürzere Analysendauer sowie einen breiteren Messbereich mit niedrigerer Nachweisgrenze aufweist. Das angewendete Assayprinzip ist dabei leicht auf weitere Analyten übertragbar und ermöglicht die Implementierung in einen Immunosensor. KW - Magnetpartikel KW - Amoxicillin KW - Immunoassay KW - Wasser KW - Antikörper PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527366 UR - https://www.gdch.de/netzwerk-strukturen/fachstrukturen/umweltchemie-und-oekotoxikologie/publikationen/mitteilungen/archiv/2021.html SN - 1618-3258 VL - 27 IS - 2 SP - 48 EP - 51 PB - Gesellschaft Deutscher Chemiker (GDCh) CY - Frankfurt/Main AN - OPUS4-52736 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ponader, Marco A1 - Röder, Bettina A1 - Paul, Martin A1 - Weller, Michael G. T1 - Sintered glass monoliths as supports for affinity columns N2 - A novel stationary phase for affinity separations is presented. This material is based on sintered borosilicate glass readily available as semi-finished filter plates with defined porosity and surface area. The material shows fast binding kinetics and excellent long-term stability under real application conditions due to lacking macropores and high mechanical rigidity. The glass surface can be easily modified with standard organosilane chemistry to immobilize selective binders or other molecules used for biointeraction. In this paper, the manufacturing of the columns and their respective column holders by 3D printing is shown in detail. The model system protein A/IgG was chosen as an example to examine the properties of such monolithic columns under realistic application conditions. Several specifications, such as (dynamic) IgG capacity, pressure stability, long-term performance, productivity, non-specific binding, and peak shape, are presented. It could be shown that due to the very high separation speed, 250 mg antibody per hour and column can be collected, which surpasses the productivity of most standard columns of the same size. The total IgG capacity of the shown columns is around 4 mg (5.5 mg/mL), which is sufficient for most tasks in research laboratories. The cycle time of an IgG separation can be less than 1 min. Due to the glass material’s excellent pressure resistance, these columns are compatible with standard HPLC systems. This is usually not the case with standard affinity columns, limited to manual use or application in low-pressure systems. The use of a standard HPLC system also improves the ability for automation, which enables the purification of hundreds of cell supernatants in one day. The sharp peak shape of the elution leads to an enrichment effect, which might increase the concentration of IgG by a factor of 3. The final concentration of IgG can be around 7.5 mg/mL without the need for an additional nano-filtration step. The purity of the IgG was > 95% in one step and nearly 99% with a second polishing run. KW - Affinity Chromatography KW - Affinity Extraction KW - Affinity Separation KW - Protein Purification KW - Down Stream Processing KW - Antibody Purification KW - Diagnostic Antibodies KW - Therapeutic Antibodies KW - Automated Purification KW - HPLC KW - FPLC KW - IgG determination KW - Concentration step KW - Monoclonal Antibodies KW - Polyclonal Antibodies KW - Human Plasma KW - Glass Support KW - Borosilicate Glass KW - Monolith KW - Sintered Material KW - Additive Manufacturing KW - Column holder KW - Construction KW - Open Science KW - Citizen Science KW - Protein A KW - Regeneration KW - High-Speed Separations KW - Robustness PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527581 DO - https://doi.org/10.3390/separations8050056 SN - 2297-8739 N1 - Geburtsname von Ponader, Marco: Wilke, M. - Birth name of Ponader, Marco: Wilke, M. VL - 8 IS - 5 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-52758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Mikroplastikanalytik mittels TED-GC/MS: H/D-Austausch an Zersetzungsprodukten von D-markiertem Polystyrol als interner Standard N2 - Deuteriertes Polystyrol (D-PS) verbessert die Mikroplastikdetektion mit der TED-GC/MS, u.a. durch höhere Reproduzierbarkeit. Es ist kostengünstig (0,1 ct/Analyse) und durch die gute Löslichkeit (z.B. in Toluol) schnell und reproduzierbar zu dosieren. Bestimmte Matrices führen jedoch zu einem Austausch des Deuteriums durchWasserstoff. Das Poster zeigt das Messprinzip, bei welchen Matrices H/D-Austausch erfolgt, Ergebnisse von Kinetikuntersuchungen sowie Möglichkeiten, den Austausch zu verhindern oder zu umgehen. T2 - Tagung der Wasserchemischen Gesellschaft CY - Online Meeting DA - 10.05.2021 KW - Mikroplastik KW - Analyse KW - Interner Standard KW - H/D-Austausch PY - 2021 AN - OPUS4-52727 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Yildirim, Arda A1 - Sentker, K. A1 - Butschies, M. A1 - Bühlmeyer, A. A1 - Huber, P. A1 - Lachat, S. A1 - Schönhals, Andreas T1 - Molecular dynamics and electrical conductivity of Guanidinium based Ionic liquid crystals: Influence of cation headgroup configuration N2 - Molecular mobility and conductivity of four bent shaped tetramethylated guanidinium based ionic liquid crystals (ILCs) with varying head group configuration (cyclic or acyclic) and alkyl chain length is investigated by a combination of broadband dielectric spectroscopy (BDS) and specific heat spectroscopy (SHS). Two dielectrically active processes observed in the plastic crystalline phase at low and high temperatures are denoted as γ and α1 relaxation. The former is assigned to localized fluctuations of methyl groups including nitrogen atoms in the guanidinium head groups. SHS investigations reveal one calorimetrically active process termed as α2 relaxation process. The temperature dependencies of the relaxation rates of α1 and α2 are similar for the cyclic ILC while for the acyclic counterpart they are different. Possible molecular assignments for the α1 and α2 relaxation are discussed in detail. Alongside relaxation processes, a significant conductivity contribution was observed for all ILCs, where the absolute value of DC conductivity increases by 4 orders of magnitude at the transition from the crystalline to the hexagonal columnar phase. The increase is traced to the change in the underlying conduction mechanism from the delocalized electrical conduction in the Cry phase to ionic conduction in the quasi 1D ion columns formed in the hexagonal columnar mesophase. KW - Ionic liquid crystal PY - 2021 DO - https://doi.org/10.1016/j.molliq.2021.115666 VL - 330 SP - 115666 PB - Elsevier B.V. AN - OPUS4-52284 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Denkler, Tilman T1 - Accreditation in Europe: Benchmarking the operations of European accreditation bodies using an innovative management tool N2 - Accreditation is one of the pillars of a national Quality Infrastructure, as the competence of conformity assessment bodies is assured through accreditation performed by accreditation bodies. To compare the operation of accreditation bodies in Europe and to identify best practices, a management tool, the Process Maturity Benchmarking Tool, was developed and validated by applying it to European accreditation bodies. The benchmarking project comprised two major phases: In the first phase, the processes of accreditation bodies were systematically analyzed. A process map was developed, and processes of special relevance were identified and underpinned by indicators. In the second phase, the practical applicability of the theoretical model was demonstrated by analyzing the processes of eight European accreditation bodies. The results of this comparative assessment were subsequently discussed in a workshop with experts from those accreditation bodies, giving the opportunity to identify best practices. This article has a twofold objective. First, to present a method to benchmark European accreditation bodies, based on the European Foundation for Quality Management excellence model. The successful application of the Process Maturity Benchmarking Tool gives evidence that it is a suitable and capable management tool to assess the processes of the European accreditation bodies and to benchmark them. Second, the article presents the results of the first adaption of the Process Maturity Benchmarking Tool. A general trend of process maturity was identified: While processes based on stakeholder involvement tend to have an overall lower maturity on average, internal processes are more mature. KW - Accreditation KW - Benchmarking KW - Quality Infrastructure KW - EFQM Excellence Modell KW - Total Quality Management KW - Akkreditierung PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521706 DO - https://doi.org/10.1007/s00769-021-01459-7 VL - 26 IS - 1 SP - 47 EP - 57 PB - Springer Nature CY - Jersey City, NJ 07302, USA AN - OPUS4-52170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Denkler, Tilman T1 - Comparison of the Operation of Accreditation Bodies in Europe - Final Report Pilot Phase N2 - This study was designed to examine and compare the operation of accreditation bodies in Europe. A management tool, the Process Maturity Benchmarking Tool (PMBT), was elaborated and validated by applying it to various accreditation bodies. By applying the tool, the values of indicators were determined, thus enabling a comparison of the accreditation bodies despite different operational processes and organizational forms. The management tool PMBT is based on the analysis of selected processes with high relevance for the operation of accreditation bodies. The processes are derived from a process map designed for accreditation bodies in a universally applicable way. The indicators used to characterize the processes come from two sources: The first source relates to data already available from internal databases, reports, financial audits etc. The second source is derived from a self-evaluation of process maturity performed by the accreditation bodies. The criteria for evaluating process maturity were designed by applying the criteria of the EFQM excellence model 2013 of the European Foundation for Quality Management (EFQM) to the processes identified in the process map. The project Comparison of the Operation of Accreditation Bodies in Europe comprised three stages. In the first stage, the processes of accreditation bodies were systematically analyzed. A process map was developed and processes of special relevance for the performance of accreditation bodies were identified and underpinned by indicators as described above. In the second stage, the processes of the German accreditation body DAkkS were assigned to the tool. This stage was used to check and modify the indicators when necessary. In the third stage, the transferability of the model was analyzed by extension to seven other accreditation bodies operating in Europe. The third stage of the project ended with a workshop attended by the eight accreditation bodies, which was used to present and discuss the results of the comparison and to identify best practices. KW - Accreditation KW - Benchmarking KW - Quality Infrastructure KW - EFQM Excellence Modell KW - Total Quality Management KW - Akkreditierung PY - 2019 SP - 1 EP - 82 AN - OPUS4-52172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Detjens, Marc T1 - Untersuchung des Elektrolyseprinzips zur Bestimmung von geringen Feuchtegehalten und der Einsatz von ionischen Flüssigkeiten als neuartige Sensorbeschichtung N2 - Feuchte, sei es Material- oder Gasfeuchte, ist eine wichtige Messgröße bei der Qualitätsbeurteilung von Kunststoffen, landwirtschaftlichen Erzeugnissen, Energieträgern, Arzneimitteln, industriell und medizinisch verwendeten Gasen. Deswegen gibt es ein Interesse Feuchtemesserfahren hinsichtlich Präzision, Wiederholbarkeit, Rückführbarkeit und Stabilität kontinuierlich zu verbessern. Ein bewährtes Messprinzip für diese Aufgabe wurde bereits 1959 von Keidel entwickelt und basiert auf der Absorption und Elektrolyse von Wasserdampf. Der einfache Aufbau dieses Prinzips besteht aus einem Sensorelement, einer Gleichspannungsquelle, einem Digitalmultimeter und einen geregelten Gasstrom über den Sensor. Nach dem Faraday’schen Gesetz der Elektrolyse korreliert bei dem Messprinzip die Ladungsmenge mit der elektrolysierten Wassermasse. Jedoch bedarf es in der heutigen Zeit einer Validierung der Sensoren, weil durch gezielte Miniaturisierung weniger aktive Fläche vorhanden ist und somit das Faraday’sche Gesetz nicht vollständig anwendbar ist. In dieser Arbeit wurden coulometrische Sensoren mit einer planaren Elektrodenstruktur hinsichtlich der Einflüsse von unterschiedlichen Gasen, der Gastemperatur und dem -druck untersucht. Zusätzlich wurde eine neuartige Sensorbeschichtung basierend auf einer ionischen Flüssigkeit getestet. Des Weiteren wurde ein Messgerät für die abgestufte Bestimmung der Materialfeuchte und Wasseraktivität entwickelt und dessen messtechnischer Einsatz untersucht. KW - Coulometrie KW - Feuchtigkeitsmessung KW - Ionische Flüssigkeit KW - Mikrosensor PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:gbv:ilm1-2019000209 SP - 1 EP - 118 CY - Technische Universität Ilmenau AN - OPUS4-52177 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Qu, Xintong A1 - Abbasi, M. A1 - Pauw, Brian Richard A1 - Henning, S. A1 - Li, Z. A1 - Wang, D.-Y. A1 - Schick, C. A1 - Saalwächter, K. A1 - Schönhals, Andreas T1 - Spatial inhomogeneity, Interfaces and Complex Vitrification Kinetics in a Network Forming Nanocomposite N2 - A detailed calorimetric study on an epoxy-based nanocomposite system was performed employing bisphenol A diglycidyl ether (DGEBA) cured with diethylenetriamine (DETA) as the polymer matrix and taurine-modified MgAL layered double hydroxide (T-LDH) as nanofiller. The -NH2 group of taurine can react with DGEBA improving the interaction of the polymer with the filler. The combined X-ray scattering, and electron microscopy data showed that the nanocomposite has a partially exfoliated morphology. Calorimetric studies were performed with conventional DSC, temperature modulated DSC (TMDSC) and fast scanning calorimetry (FSC) in the temperature modulated approach (TMFSC) to investigate the vitrification and molecular mobility in dependence of the filler concentration. First, TMDSC and NMR were used to estimate the amount of the rigid amorphous fraction which consists of immobilized polymer segments at the nanoparticle surface. It was found to be 40 wt% for the highest filler concentration, indicating that the interface dominates the overall macroscopic properties and behavior of the material to a great extent. Second, the relaxation rates of the α-relaxation obtained by TMDSC and TMFSC were compared with the thermal and dielectric relaxation rates measured by static FSC. The investigation revealed that the system shows two distinct α-relaxation processes. Furthermore, also two separate vitrification mechanisms were found for a bulk network-former without geometrical confinement as also confirmed by NMR. This was discussed in terms of the intrinsic spatial heterogeneity on a molecular scale, which becomes more pronounced with increasing nanofiller content. KW - Polymer based Nanocomposites PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523199 DO - https://doi.org/10.1039/d0sm01992e SN - 1744-6848 VL - 17 IS - 10 SP - 2775 EP - 2790 PB - Royal Society of Chemistry AN - OPUS4-52319 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Marc Benjamin A1 - Zutta Villate, J. M. ED - Zutta Villate, J. M. T1 - Combined cell and nanoparticle models for TOPAS to study radiation dose enhancement in cell organelles N2 - Dose enhancement by gold nanoparticles (AuNP) increases the biological effectiveness of Radiation damage in biomolecules and tissue. To apply them effectively during cancer therapy their influence on the locally delivered dose has to be determined. Hereby, the AuNP locations strongly influence the energy deposit in the nucleus, mitochondria, membrane and the cytosol of the targeted cells. To estimate these effects, particle scattering simulations are applied. In general, different approaches for modeling the AuNP and their distribution within the cell are possible. In this work, two newly developed continuous and discrete-geometric models for simulations of AuNP in cells are presented. These models are applicable to simulations of internal emitters and external radiation sources. Most of the current studies on AuNP focus on external beam therapy. In contrast, we apply the presented models in Monte-Carlo particle scattering simulations to characterize the energy deposit in cell organelles by radioactive 198AuNP. They emit beta and gamma rays and are therefore considered for applications with solid tumors. Differences in local dose enhancement between randomly distributed and nucleus targeted nanoparticles are compared. Hereby nucleus targeted nanoparticels showed a strong local dose enhancement in the radio sensitive nucleus. These results are the foundation for future experimental work which aims to obtain a mechanistic understanding of cell death induced by radioactive 198Au. KW - AuNP KW - Beta decay KW - Brachytherapy KW - Cancer treatment KW - DNA KW - DNA damage KW - Dosimetry KW - Energy deposit KW - Geant4 KW - Geant4-DNA KW - Gold Nanoparticles KW - LEE KW - MCS KW - Microdosimetry KW - Monte-Carlo simulation KW - NP KW - Ectoine KW - OH radicals KW - Radiation damage KW - Radiationtherapy KW - Radioactive decay KW - Simulation KW - Beta particle KW - Clustered nanoparticles KW - Gamma ray KW - Low energy electrons KW - Particle scattering KW - Radiolysis KW - Livermore model KW - Penelope model KW - TOPAS KW - TOPAS-nbio PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523276 DO - https://doi.org/10.1038/s41598-021-85964-2 SN - 2045-2322 VL - 11 IS - 1 SP - 6721 PB - Springer Nature AN - OPUS4-52327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Even, Morgane T1 - Formaldehyde Emissions from Wooden Toys: Method Comparison and Exposure Assessment N2 - Formaldehyde is considered as carcinogenic and is emitted from particleboards and plywood used in toy manufacturing. Currently, the flask method is frequently used in Europe for market surveillance purposes to assess formaldehyde release from toys, but its concordance to levels measured in emission test chambers is poor. Surveillance laboratories are unable to afford laborious and expensive emission chamber testing to comply with a new amendment of the European Toy Directive; they need an alternative method that can provide reliable results. Therefore, the application of miniaturised emission test chambers was tested. Comparisons between a 1 m3 emission test chamber and 44 mL microchambers with two particleboards over 28 days and between a 24 L desiccator chamber and the microchambers with three puzzle samples over 10 days resulted in a correlation coefficient r2 of 0.834 for formaldehyde at steady state. The correlation between the results obtained in microchambers vs. flask showed a high variability over 10 samples (r2: 0.145), thereby demonstrating the error-proneness of the flask method in comparison to methods carried out under ambient parameters. An exposure assessment was also performed for three toy puzzles: indoor formaldehyde concentrations caused by puzzles were not negligible (up to 8 μg/m3), especially when more conservative exposure scenarios were considered. T2 - OE conference CY - Online meeting DA - 23.03.2021 KW - Formaldehyde KW - Wooden toys PY - 2021 AN - OPUS4-52330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Hahn, Marc Benjamin A1 - Sturm, Heinz A1 - Bier, F A1 - Solomun, Tihomir T1 - Biologische Konsequenzen einer nanoskaligen Energiedeposition: Fokussierung auf die Rolle niederenergetischer Elektronen T1 - Biological Consequence of Nanoscale Energy Deposition: Focusing on the Role of Low-Energy Electrons N2 - Bei der Behandlung von Krebs mittels Strahlentherapie sollen Tumorzellen abgetötet werden ohne das umliegende gesunde Gewebe zu zerstören. Um Strahlentherapien für Patienten verträglicher zu machen, ist ein besseres Verständnis der zugrundeliegenden Prozesse auf der molekularen Ebene nötig. Dabei sind der Energieeintrag und die Streuprozesse der Strahlung in der Umgebung der DNA von besonderem Interesse. Durch Streuung von hochenergetischer Strahlung in Wasser werden besonders viele Sekundärelektronen mit niedriger Energie erzeugt. Zur Untersuchung der Schädigungseffizienz dieser Elektronen wurde ein Verfahren zur direkten Bestrahlung von Lösungen mittels Elektronen variabler Energien enwtickelt. Dies wurde durch einen neu entwickelten Probenhalter mit einer für Elektronen durchlässigen Nanomembran ermöglicht. Mit diesem können Bestrahlungen an DNA, Proteinen, und Zellen bei verschiedenen pH-Werten oder Salzkonzentrationen durchgeführt werden. Parallel dazu wurde der ortsabhängige Energieeintrag innerhalb des Wassers durch Elektronenstreusimulationen bestimmt. Diese neuartige Kombination von Experiment und Simulation ermöglicht die Bestimmung der Schaden-Dosis-Relation für Elektronenbestrahlung von biologischen Systemen unter realistischen physiologischen Bedingungen. So konnten für die genutzten Primärelektronen wie die mittlere letale Dosis, bei der 50 Prozent der DNA geschädigt sind, mit 1,7 Gy bestimmt. Ebenfalls wurde das für mikrodosimetrische Modellierungen und Betrachtungen der sogenannten Linear energy transfer (LET) Effekte, wichtige Verhältnis von DNA Einzelstrangbrüchen (SSB) zu Doppelstrangbrüchen (DSB) als SSB/DSB = 12/1 bestimmt. Mit Hilfe eines Modells für das Targetvolumen der DNA wurde der mittlere mikroskopische letale Energieeintrag berechnet als E1/2 = 6 ± 4 eV . Es wurde gefolgert, dass weniger als zwei Ionisationsprozesse im sensitiven Targetvolumen der DNA im Mittel zu einem Einzelstrangbruch führen. Diese Methode ist unabhängig von den Primärpartikel und geometrischen Bedingungen. Deshalb ermöglicht sie die Vergleichbarkeit experimenteller Systeme mit inhomogenen Energieverteilungen, welches sonst nicht gegeben ist. Des weiteren wurden die Strahlenschutzfunktionen des Zellschutzmoleküls Ectoines und sein Einfluss auf Wasser und Biomoleküle untersucht. Seine Schutzfunktion gegen ionisierende Strahlung wurde auf die Erhöhung des Streuquerschnitts niederenergetischer Elektronen und seine Eigenschaft als OH-Radikalfänger zurückgeführt. Aufbauend auf unseren Erkenntnissen finden in klinischen Arbeitsgruppen Untersuchungen zu Einsatzmöglichkeiten im Umfeld der Strahlentherapie statt. Projektkennung Deutsche Forschungsgemeinschaft (DFG) - Projektnummer 245767821 N2 - To cure cancer radiation therapy is used to kill tumor cells. It is based on radiation induced damage to biomolecules. Here DNA damage is of key interest due to its central role in apoptosis and mutation. Because of the high amount of water in biological tissue, most of the damage is caused by the secondary particles produced by the inelastic scattering of ionizing radiation and water. A detailed understanding of the underlying molecular processes under physiological conditions is the prerequisite to develop more efficient the-rapies. Therefore irradiations have to be performed in liquid, under consideration of the chemical environment. To make it possible to irradiate liquids with electrons within scanning electron microscopes a new sample holder was constructed incorporating an electron transparent nanomembrane. It makes it possible to irradiate DNA, proteins or cells at different pH and salinity. The median lethal dose for a model system of plasmid DNA and water was determined by the combination of experimental data, particle scattering simulations (Geant4-DNA) and diffusion calculations as D1/2 = 1.7 ± 0.3 Gy. From the convolution of plasmid positions and the spatially resolved energy deposit, as determined by electron scattering simulations, the histogram of the energy deposit within the target volume of the plasmids and the microscopic median lethal energy deposit was calculated as E1/2 = 6 ± 4 eV . It could be deduced, that on average less than two ionization Events are sufficient to cause a single-strand-break. The relation of single-strand-breaks (SSB) to double-strand-breaks (DSB), which is of importance for microdosimetric modeling, was determined as SSB : DSB = 12 : 1. The presented method for the Determination of microscopic dose-damage relations was further extended to be applicable for General irradiation experiments. It is independent of the type of primary radiation used, the experimental geometry, and the diffusional properties of the molecules under investigation. This way different experimental systems with varying, inhomogeneous energy deposit characteristics become comparable with each other, which is not possible when only macroscopic averaged values are taken into account. In addition, the radiation protection properties of the compatible solute Ectoine was investigated. The protective properties of ectoine result from the increase of the inelastic scattering probabilities of low Energy electrons at the acoustic vibrational modes of water and its properties as OH-radical scavenger. Based on our results, further investigations are conducted to evaluate the application of Ectoine in the context of radiation therapy. Projektkennung Deutsche Forschungsgemeinschaft (DFG) - Projektnummer 245767821 KW - Ectoin KW - Ectoine KW - DNS KW - DNA KW - Cancer therapy KW - DNA damage KW - DNA radiation damage KW - Dosimetry KW - DFG KW - Electron irradiation KW - Ectoine DNA interaction KW - Ectoine radiation protection KW - Hydroxyl radicals KW - OH radicals KW - LEE KW - Low energy electrons KW - Microdosimetry KW - Radiation KW - Geant4 KW - Geant4-DNA KW - Radiation therapy KW - LET PY - 2021 UR - https://gepris.dfg.de/gepris/projekt/245767821/ergebnisse?context=projekt&task=showDetail&id=245767821&selectedSubTab=2& SP - 1 EP - 14 AN - OPUS4-52389 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Immunomagnetic ochratoxin a assay with electrochemical 3,3′,5,5′ tetramethylbenzidine detection N2 - The demand for miniaturized analytical devices monitoring important parameters in the food and medical industry has increased strongly in the past decades. With fast progress, smart technologies are finding their way into our everyday life. For the future, it is, therefore, a major goal to also link analytical methods with smart technologies to create user-friendly on-site devices. In food industry the monitoring of harmful substances such as dioxins, heavy metals or mycotoxins plays a key role, since the European Commission prescribes legal limits for various food products and beverages[1]. Therefore, companies often have their own laboratories and trained personnel. For one of the most abundant and toxic mycotoxins, Ochratoxin A (OTA) we want to present an electrochemical detection system in which the read-out can be performed with a smartphone connected via Bluetooth to a miniaturized potentiostat. The recognition of OTA is performed with specific antibodies in a competitive assay format. Anti-OTA-antibodies were captured on magnetic beads on which the competitive binding between OTA and an OTA horseradish peroxidase (HRP) tracer was performed. To quantify OTA, the enzymatic reaction of the tracer with 3,3′,5,5′-tetramethylbenzidine (TMB) and H2O2 is employed. Oxidized TMB, which is enzymatically produced by the reduction of H2O2, is quantified by amperometry with screen-printed electrodes in a custom-made flow system. The results of the electrochemical detection method are in good correlation with the photometric detection of TMB. To demonstrate the applicability, we tested our system with OTA-spiked beer and performed the measurement via smartphone. T2 - 23rd JCF-Frühjahrssymposium 2021 CY - Online meeting DA - 29.03.2021 KW - Ochratoxin A KW - Cyclic voltammetry KW - Amperometry KW - Electrochemistry PY - 2021 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-52390 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Even, Morgane A1 - Juritsch, Elevtheria A1 - Richter, Matthias T1 - Measurement of very volatile organic compounds (VVOCs) in indoor air by sorbent-based active sampling: Identifying the gaps towards standardisation N2 - The ISO 16000-6 standard describes a method for the determination of volatile organic compounds (VOCs) in indoor and test chamber air by sorbent-based active sampling, thermal desorption and gas chromatography coupled with mass spectrometry (GC/MS). It also gives directions to adapt this methodology to very volatile organic compounds (VVOCs). Indeed, toxicologically based guideline values are being implemented for these compounds and it becomes necessary to measure them. But a comprehensive and robust measurement method is lacking. This work highlights the points that still need to be explored towards the standardisation of a suitable procedure: investigations on sorbent combinations, the suitability of chromatography columns and the use of gaseous standards are required. The biggest challenge remains in the fact that strong sorbents adsorb water together with VVOCs. Water may impair the analysis and the optimal approach to eliminate it is still to be found and integrated into the sampling strategy. KW - Solvents KW - Air analysis KW - VOC KW - Thermal desorption KW - Gas chromatography KW - ISO 16000-6 PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523919 DO - https://doi.org/10.1016/j.trac.2021.116265 VL - 140 SP - 116265 PB - Elsevier B.V. AN - OPUS4-52391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Smartphone-based amperometric detection of 3,3′,5,5′-tetramethylbenzidine (TMB) – An immunomagnetic Ochratoxin A assay N2 - The demand for miniaturized analytical devices monitoring important parameters in the food and medical industry has increased strongly in the past decades. With fast progress, smart technologies are finding their way into our everyday life. For the future, it is, therefore, a major goal to also link analytical methods with smart technologies to create user-friendly on-site devices. In food industry the monitoring of harmful substances such as dioxins, heavy metals or mycotoxins plays a key role, since the European Commission prescribes legal limits for various food products and beverages[1]. Therefore, companies often have their own laboratories and trained personnel. For one of the most abundant and toxic mycotoxins, Ochratoxin A (OTA) we want to present an electrochemical detection system in which the read-out can be performed with a smartphone connected via Bluetooth to a miniaturized potentiostat. The recognition of OTA is performed with specific antibodies in a competitive assay format. Anti-OTA-antibodies were captured on magnetic beads on which the competitive binding between OTA and an OTA horseradish peroxidase (HRP) tracer was performed. To quantify OTA, the enzymatic reaction of the tracer with 3,3′,5,5′-tetramethylbenzidine (TMB) and H2O2 is employed. Oxidized TMB, which is enzymatically produced by the reduction of H2O2, is quantified by amperometry with screen-printed electrodes in a custom-made flow system. Since it is well-known that oxidized TMB can precipitate on electrode surfaces[2], we have studied pitfalls of the electrochemical detection of TMB. By cyclic voltammetry we have compared the stability of the electrochemistry of TMB at different electrode materials (gold and carbon) and pH values (pH 1 and pH 4). It was found that a stable response of the electrode could be achieved at pH 1 on gold electrodes. Thus, we applied these reaction conditions for amperometric detection of TMB in the OTA assay. The results of the electrochemical detection method are in good correlation with the photometric detection of TMB. To demonstrate the applicability, we tested our system with OTA-spiked beer and performed the measurement via smartphone. T2 - European Biosensor Symposium 2021 CY - Online meeting DA - 09.03.2021 KW - Ochratoxin A KW - Cyclic voltammetry KW - Amperometry KW - Smartphone KW - Immunoassay PY - 2021 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-52269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Enzyme activity determination of human monoamine oxidase B (Mao B) by amperometric hydrogen peroxide detection N2 - Parkinson’s disease (PD) is one of the most common neurodegenerative disorders worldwide. About 0.3 % of the global population and approximately 2 % of people older than 80 years are affected by PD. Monoamine oxidase B (Mao B) is an enzyme, which is a drug target in Parkinson’s disease (PD), since it is involved in dopamine metabolism. Several Mao B inhibitors are well established as medication for PD patients. However, the medical treatment is only little personalized since the monitoring of the patients Mao B activity is complex and requires sophisticated laboratory equipment. Here a sensorial Mao B activity determination system has been developed which has potential in the personalization of the medical PD treatment. The enzyme activity is quantified by amperometric detection of enzymatically produced H2O2. Therefore, the enzyme is enriched from the solution via cellulose particles which are functionalized with antibodies against human Mao B. The successful capturing of the enzyme can be verified by SDS-PAGE. For activity determination the enzyme is brought in contact with a suitable substrate - here benzylamine. Selectivity of the amperometric hydrogen peroxide detection in the presence of co-reactants has been verified. Within the time span of 30 min, a linear dependency of enzymatically produced H2O2 with the substrate incubation time can be observed. This allows the evaluation of the Mao B activity. The results have been correlated to an optical detection method. Furthermore, the method has been tested for different amounts of enzyme used in the experiments and found to be sensitive enough for Mao B analysis in blood samples. T2 - European Biosensor Symposium 2021 CY - Online meeting DA - 09.03.2021 KW - Monoamine oxidase B KW - Amperometry KW - Prussian blue KW - Parkinsons's disease KW - Screen-printed electrodes PY - 2021 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-52270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis T1 - Numerical methods (part II) Finite element method (FEM), Spectral element method (SEM) and Scaled Boundary FEM (SBFEM) N2 - A general presentation on numerical methods. In particular, the Finite Element Method, the Spectral Element Method, and the Scaled Boundary Finite Element Method. T2 - ITN-Trainingsevent CY - Online meeting DA - 22.11.2020 KW - FEM KW - SBFEM KW - SEM PY - 2020 AN - OPUS4-52271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis T1 - A Combination of the Scaled Boundary Finite Element Method with the Mortar Method N2 - The simulation of ultrasonic waves in a linearly elastic body can be computationally intensive. The reason is the relatively short wavelength compared to the body size for high frequencies. One possible approach to counteract the high computational costs is to decompose the domain into small parts and strive for parallelization. The Mortar Method is a well-established approach for domain decomposition. A rather new approach to discretize the emerging subdomains is the Scaled Boundary Finite Element Method. This semi-analytical method has many attractive properties. Some of these properties are listed subsequently. The grid consists of polygonal elements, which leaves much freedom in the meshing process. A variety of material distributions, including anisotropic materials, can be considered. High-order shape functions can be used for optimal convergence properties. The approach treats singularities at crack tips and corners analytically. Especially in the frequency domain, the Scaled Boundary Finite Element Method reduces the dimension of the approximation because only degrees of freedom which are associated with the boundary of a polygonal element are necessary. Those desirable properties make the method particularly suitable for calculating the dynamic responses in bodies with cracks, as it is essential for many non-destructive testing and structural health monitoring applications. In this contribution, we present a combination of the Scaled Boundary Finite Element Method with the Mortar Method in two dimensions. The presentation starts with a theoretical overview of both approaches. Subsequently, numerical examples demonstrate the stability of the combination for the polygonal boundary of the elements. The numerical examples increase in complexity and are compared to results computed on non-divided domains with the Finite Element Method. T2 - WCCM-ECCOMAS CONGRESS CY - Online meeting DA - 11.01.2021 KW - Ultrasound KW - Numerical Simulation KW - Scaled Boundary Finite Element Method, Mortar Method PY - 2021 AN - OPUS4-52275 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - MALDI-TOF MS in der Synthese hochmolekularer Polylaktid Homo- und Copolymere N2 - Die MALDI-TOF Massenspektrometrie stellt eine wichtige Methode zur simultanen Bestimmung von Molmassen, Molmassenverteilungen und Endgruppen von synthetischen Polymeren dar. In dem Vortrag wird gezeigt, welche zusätzlichen Informationen über die Art der Polymerisation, der Nebenreaktionen und der Topologie der gebildeten hochmolekularen Polylaktid-Homo- und Copolymere im Verlauf ihrer Synthese erhalten werden können. T2 - Bruker Anwendertreffen CY - Online meeting DA - 05.03.2021 KW - MALDI KW - Polylaktide PY - 2021 AN - OPUS4-52278 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Scheliga, F. A1 - Weidner, Steffen T1 - What does conversion mean in polymer science? N2 - The definition of the term “conversion” is discussed for a variety of polymer syntheses. It is demonstrated that in contrast to organic and inorganic chemistry several different definitions are needed in polymer science. The influence of increasing conversion on structure and topology of homo- and Copolymers is illustrated. Chain-growth polymerizations, such as radical polymerization or living anionic polymerizations of vinyl monomers, condensative chain polymerization, two and three-dimensional step-growth polymerizations, ring–ring or chain–chain equilibration and chemical modification of polymers are considered. KW - Polymers KW - Polymerization KW - Conversion KW - Polycondensation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523597 DO - https://doi.org/10.1002/macp.202100010 VL - 222 IS - 8 SP - 10 PB - Wiley VCH AN - OPUS4-52359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - DNA based Reference Materials: In Biodosimetry and Pharmaceutical Quality Control N2 - Applications of plasmid DNA base reference materials in dosimetry and pharmaceutical research. T2 - Physical and Chemical Analysis of Polymers seminar CY - Online meeting DA - 29.03.2021 KW - Analytic KW - Certification KW - DNA KW - Dosimetry KW - Homogeneity KW - Quality testing KW - Reference material KW - Referenzmaterialien KW - Stability KW - Dose KW - Radiation KW - Pharmacy KW - Electrohpresis PY - 2021 AN - OPUS4-52361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ullner, Christian A1 - Subaric-Leitis, Andreas A1 - Bartholmai, Matthias T1 - Uncertainty of Elastoplastic Material Parameters Calculated from the Spherical Indentation in the Macro Range N2 - The applicability of three methods developed by finite element analysis (FEM) and proposed in the literature are studied on steel S355. Instrumented indentation tests using spherical indenters of radius 200 and 500 μ m are performed in the macro range at depths of more than 6 μ m. The results of the selected methods are compared with the tensile test. To evaluate the partially strongly varying results, the uncertainties of the calculated strain hardening exponent, n, and yield stress, Y, are estimated. Recommendations for an appropriated procedure of the indentation test are given. The machine compliance and the determination of the zero point of Depth play an essential role. If the certain conditions are considered, the instrumented indentation Tests can be used, in particular for investigations of specimens with inhomogeneous elastoplasticity. KW - Indentation KW - Elastoplastic material parameters KW - Uncertainty PY - 2021 DO - https://doi.org/10.1520/JTE20200683 SN - 0090-3973 VL - 49 IS - 6 SP - 4576 EP - 4592 PB - ASTM International AN - OPUS4-52416 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Holstein, Tanja A1 - Kurths, J. A1 - Wiedermann, M. T1 - Optimization of coupling and global collapse in diffusively coupled socio-ecological resource exploitation networks N2 - Single- and multi-layer complex networks have been proven as a powerful tool to study the dynamics within social, technological, or natural systems. An often observed common goal is to optimize these systems for specific purposes by minimizing certain costs while maximizing a desired output. Acknowledging that especially real-world systems from the coupled socio-ecological realm are highly intertwined this work exemplifies that in such systems the optimization of a certain subsystem, e.g. to increase the resilience against external pressure in an ecological network, may unexpectedly diminish the stability of the whole coupled system. For this purpose we utilize an adaptation of a previously proposed conceptual bi-layer network model composed of an ecological network of diffusively coupled resources co-evolving with a social network of interacting agents that harvest these resources and learn each other’s strategies depending on individual success. We derive an optimal coupling strength that prevents collapse in as many resources as possible if one assumes that the agents’ strategies remain constant over time. We then show that if agents socially learn and adapt strategies according to their neighbors’ success, this optimal coupling strength is revealed to be a critical parameter above which the probability for a global collapse in terms of irreversibly depleted resources is high—an effect that we denote the tragedy of the optimizer. We thus find that measures which stabilize the Dynamics within a certain part of a larger co-evolutionary system may unexpectedly cause the emergence of novel undesired globally stable states. Our results therefore underline the importance of holistic approaches for managing socio-ecological systems because stabilizing effects which focus on single subsystems may be counter-beneficial for the system as a whole. KW - Network science KW - Complex systems KW - Socio-ecological models KW - Non linear dynamics KW - Physics KW - Physics and society PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524176 DO - https://doi.org/10.1088/1367-2630/abe0db VL - 23 IS - 3 SP - 033027 PB - IOP Publishing CY - Bristol, England AN - OPUS4-52417 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kästner, L. A1 - Ahmadi, Samim A1 - Jonietz, Florian A1 - Jung, P. A1 - Caire, G. A1 - Ziegler, Mathias A1 - Lambrecht, J. T1 - Classification of Spot-Welded Joints in Laser Thermography Data Using Convolutional Neural Networks N2 - Spot welding is a crucial process step in various industries. However, classification of spot welding quality is still a tedious process due to the complexity and sensitivity of the test material, which drain conventional approaches to its limits. In this article, we propose an approach for quality inspection of spot weldings using images from laser thermography data. We propose data preparation approaches based on the underlying physics of spot-welded joints, heated with pulsed laser thermography by analyzing the intensity over time and derive dedicated data filters to generate training datasets. Subsequently, we utilize convolutional neural networks to classify weld quality and compare the performance of different models against each other. We achieve competitive results in terms of classifying the different welding quality classes compared to traditional approaches, reaching an accuracy of more than 95 percent. Finally, we explore the effect of different augmentation methods. KW - Active thermal imaging KW - Laser thermography KW - Spot-welded joints KW - Convolutional neural network KW - Classification KW - Data processing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524216 DO - https://doi.org/10.1109/ACCESS.2021.3063672 VL - 9 SP - 48303 EP - 48312 AN - OPUS4-52421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ecke, Alexander T1 - Magnetic Bead-Based Immunoassays for Online Drinking Water Analysis N2 - We present the development of magnetic bead-based immunoassays for two potential contaminants of drinking water: the nonsteroidal anti-inflammatory drug diclofenac and the broad-spectrum antibiotic amoxicillin. For these analytes, different assay formats were developed which can generally be transferred to other analytes. The use of magnetic beads not only enables implementation of the assays into an online system since the beads can be reversibly immobilized by applying a magnetic field. Furthermore, our MBBAs hold several advantages over the conventional ELISAs (enzyme-linked immunosorbent assays) for both analytes, such as lower limits of quantification, shorter assay duration and less washing steps required. Strategies for the setup and miniaturization of an online immunosensor including electrochemical readout on a microfluidic chip will be discussed. T2 - JCF-Frühjahrssymposium CY - Online Meeting DA - 29.03.2021 KW - Magnetic Beads KW - Immunoassay KW - Immunosensor KW - Diclofenac KW - Amoxicillin PY - 2021 AN - OPUS4-52426 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, M. A. A1 - Khan, I. A1 - Opitz, P. A1 - Hartmann, J: A1 - Ashraf, M. A1 - Qurashi, A. A1 - Prädel, L. A1 - Panthöfer, M. A1 - Cossmer, Antje A1 - Pfeifer, Jens A1 - Simon, Fabian A1 - von der Au, Marcus A1 - Meermann, Björn A1 - Mondeshki, M. A1 - Tahir, M. N. A1 - Tremel, W. T1 - A Generalized Method for High-Speed Fluorination of Metal Oxides by Spark Plasma Sintering Yields Ta3O7F and TaO2F with High Photocatalytic Activity for Oxygen Evolution from Water N2 - A general method to carry out the fluorination of metal oxides with poly(tetrafluoroethylene) (PTFE, Teflon) waste by spark plasma sintering (SPS) on a minute scale with Teflon is reported. The potential of this new approach is highlighted by the following results. i) The tantalum oxyfluorides Ta3O7F and TaO2F are obtained from plastic scrap without using toxic or caustic chemicals for fluorination. ii) Short reaction times (minutes rather than days) reduce the process time the energy costs by almost three orders of magnitude. iii) The oxyfluorides Ta3O7F and TaO2F are produced in gram amounts of nanoparticles. Their synthesis can be upscaled to the kg range with industrial sintering equipment. iv) SPS processing changes the catalytic properties: while conventionally prepared Ta3O7F and TaO2F show little catalytic activity, SPS-prepared Ta3O7F and TaO2F exhibit high activity for photocatalytic oxygen evolution, reaching photoconversion efficiencies up to 24.7% and applied bias to photoconversion values of 0.86%. This study shows that the materials properties are dictated by the processing which poses new challenges to understand and predict the underlying factors. KW - Fluorination KW - Oxygen evolution reaction KW - Photocatalysis KW - Spark plasma sintering KW - Tantalum oxyfluorides PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524329 DO - https://doi.org/10.1002/adma.202007434 VL - 23 IS - 20 SP - 7434 PB - Wiley‐VCH GmbH AN - OPUS4-52432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - New applications and reference materials in isotope analysis N2 - The presentations gives a short introduction into isotope analysis illustrated by examples from archaeology, food provenancing and metrology. In the main part current projects on the provenance determination of cement, the intercalibration of Mg isotope reference materials and the development of a new calibration approach for isotope measurements are presented. T2 - Seminar der Abteilung 1 CY - Online meeting DA - 19.01.2021 KW - Isotope reference material KW - Absolute isotope ratio KW - Metrology KW - Traceability KW - Triple isotope fractionation KW - Archaeometry KW - Cement PY - 2021 AN - OPUS4-52460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hernandez-Castillo, A. O. A1 - Bischoff, J. A1 - Lee, J. H. A1 - Langenhan, Jennifer A1 - Karra, M. A1 - Meijer, G. A1 - Eibenberger-Arias, S. T1 - High-resolution UV spectroscopy of 1-indanol N2 - We report on rotationally resolved laser induced fluorescence (LIF) and vibrationally resolved resonanceenhanced multiphoton ionization (REMPI) spectroscopy of the chiral molecule 1-indanol. Spectra of the S1 ’ S0 electronic transition are recorded in a jet-cooled, pulsed molecular beam. Using two timedelayed pulsed lasers, the lifetimes of the S1 state of the two most stable conformers, referred to as eq1 and ax2, have been determined. The S1 ’ S0 origin bands of these conformers as well as the Transition to a vibrationally excited level in the S1 state of eq1 are recorded with full rotational resolution (25 MHz observed linewidth) by measuring the LIF intensity following excitation with a tuneable, narrowband cw laser. On selected rotationally resolved electronic transitions, Lamb-dips are measured to confirm the Lorentzian lifetime-contribution to the observed lineshapes. The rotationally resolved S1 ’ S0 origin band of a neon-complex of eq1 is measured via LIF as well. The fit of the rotationally resolved LIF spectra of the origin bands to those of an asymmetric rotor yields a standard deviation of about 6 MHz. The resulting spectroscopic parameters are tabulated and compared to the outcome of ab initio calculations. For both conformers as well as for the Ne-eq1 complex, the geometric structures in the S0 and S1 states are discussed. For all systems, the transition dipole moment is mainly along the a-axis, the contributions along the b- and c-axes being about one order of magnitude smaller. KW - REMPI KW - LIF KW - 1-indanol PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525056 DO - https://doi.org/10.1039/d0cp06170k VL - 23 IS - 12 SP - 7048 EP - 7056 PB - Royal Society of Chemistry AN - OPUS4-52505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Usmani, Shirin T1 - Wood treated with nano metal fluorides - relations between composition, size, and durability N2 - In this study, nanoscopic particles of magnesium Fluoride (MgF2) and calcium fluoride (CaF2) also known as nano metal fluorides (NMFs), were evaluated for their potential to improve wood durability. Even though these fluorides are sparingly soluble, their synthesis in the form of nano-sized particles turns them into promising candidates for wood preservation. Their distinct property of low-water solubility is proposed to maintain long-lasting protection of treated wood by reducing the leaching of fluoride. Analytical methods were used to characterize the synthesized NMFs and their distribution in treated wood specimens. Transmission electron microscopy images showed that these fluoride particles are smaller than 10 nm. In nano metal fluoride (NMF) treated specimens, aggregates of these particles are uniformly distributed in the wood matrix as confirmed with scanning electron microscopy images and their corresponding energy-dispersive X-ray spectroscopy maps. The fluoride aggregates form a protective layer around the tracheid walls and block the bordered pits, thus reducing the possible flow path for water absorption into wood. This is reflected in the reduced swelling and increased hydrophobicity of wood treated with NMFs. The biocidal efficacy of NMFs was tested against brown-rot fungi (Coniophora puteanaand Rhodonia placenta), white-rot fungus (Trametes versicolor), and termites (Coptotermes formosanus). The fungal and termite tests were performed in accordance with the EN 113 (1996) and EN 117 (2012) standards, respectively. Prior to fungal tests, the NMF treated wood specimens were leached according to the EN 84 (1997)standard. Compared to untreated specimens, the NMF treated wood specimens have a higher resistance to decay caused by brown-rot fungi, white-rot fungus, and termites. Although all NMF treatments in wood reduce the mass loss caused by fungal decay, only the combined treatment of MgF2 and CaF2 has efficacy against both brown-rot fungi and white-rot fungus. Similarly, wood treated with the combined NMF formulation is the least susceptible to attack by C. formosanus.It is proposed that combining MgF2 and CaF2changes their overall solubility to promote the release of fluoride ions at the optimal concentration needed for biocidal efficacy against fungi and termites. In this thesis, it was proven that even after leaching, sufficient fluoride was present to protect NMF treated wood from fungal decay. This shows that NMFs are robust enough for above ground contact outdoor applications of wood, where permanent wetness cannot be avoided according to Use Class 3.2, as per the EN 335 (2013) standard. Also, they pose a low risk to human health and the environment because they are sparingly soluble. Since NMFs significantly reduce the decay of wood, the CO2 fixed in it will be retained for longer than in unpreserved wood. Overall, the novel results of this study show the potential of NMFs to increase the service life of building materials made from non-durable wood. KW - Termites KW - Nano metal fluorides KW - Solubility KW - Wood protection KW - Fungi PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525108 DO - https://doi.org/10.18452/22553 SP - i EP - 118 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-52510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schweitzer, T. A1 - Hörmann, M. A1 - Bühling, Benjamin A1 - Bobusch, B. T1 - Switching Action of a Bistable Fluidic Amplifier for Ultrasonic Testing N2 - Air-coupled ultrasonic testing is widely used in the industry for the non-destructive testing of compound materials. It provides a fast and efficient way to inspect large concrete civil infrastructures for damage that might lead to catastrophic failure. Due to the large penetration depths required for concrete structures, the use of traditional piezoelectric transducer requires high power electric systems. In this study, a novel fluidic transducer based on a bistable fluidic amplifier is investigated. Previous experiments have shown that the switching action of the device produces a high-power broadband ultrasonic signal. This study will provide further insight into the switching behaviour of the fluidic switch. Therefore, parametric CFD simulations based on compressible supersonic RANS simulations were performed, varying the inlet pressure and velocity profiles for the control flow. Switching times are analyzed with different methods, and it was found that These are mostly independent of the slope of the velocity profile at the control port. Furthermore, it was found that an inversely proportional relationship exists between flow velocity in the throat and the switching time. The results agree with the theoretical background established by experimental studies that can be found in the literature. KW - Ultrasound KW - Non-destructive testing KW - Fluidic devices KW - Computational fluid dynamics KW - Concrete KW - Bistable fluidic amplifier PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525115 DO - https://doi.org/10.3390/fluids6050171 SN - 2311-5521 VL - 6 IS - 5 SP - 171 PB - MDPI CY - Basel, Switzerland AN - OPUS4-52511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dinter, Adelina-Elisa T1 - Examination of biological samples by means of single-cell ICP-ToF-MS N2 - Up to now, different analytical methods for single cell analysis exist focusing on key features such as size, shape, morphology and elemental composition. The combination of the latest ICP-MS techniques - ICP-ToF-MS - together with the latest developments in the field of sample delivery - micro droplet generator (MDG) – will allow a Deep insight into the composition and size of cells. Microbiologically influenced corrosion (MIC) is an oxidation of metals affected by the presence or activity (or both) of microorganisms e.g. Shewanella Putrefaciens in biofilms on the surface of the corroding material. As this can happen for example in the soil on iron pipes of water pipes, in oil tanks or on steel sheet piling, there is great interest in MIC research, not only from various industrial sectors, but also from the environmental aspect. T2 - SALSA - Make & Measure CY - Online Meeting DA - 15.10.2020 KW - SC-ICP-ToF-MS KW - Single cell analysis KW - MDG ICP-ToF-MS KW - Microdroplet generator PY - 2020 AN - OPUS4-52441 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tiebe, Carlo A1 - Johann, Sergej A1 - Dessel, S. T1 - Prüfanweisung für Gassensoren N2 - Viele Sensoren sind auf dem Markt, die flüchtige organische Substanzen im Innenraum nicht nur messen, sondern gleichzeitig auch die Luftgüte bewerten. Damit diese Sensoren gute und vergleichbare Daten liefern, erarbeitet ein Fachausschuss der VDI/VDE-Gesellschaft Mess- und Automatisierungstechnik (GMA) eine neue VDI-Richtlinie. KW - VOC KW - Gassensor KW - Innenraumluft KW - IAQ KW - Richtlinie KW - Gasmesssystem PY - 2021 VL - 51 IS - 03-04 SP - 41 EP - 42 AN - OPUS4-52445 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weber, K. A1 - Weber, M. A1 - Menneken, M. A1 - Kral, A. G. A1 - Mertz-Kraus, R. A1 - Geisler, T. A1 - Vogl, Jochen A1 - Tütken, T. T1 - Diagenetic stability of non-traditional stable isotope systems (Ca, Sr, Mg, Zn) in teeth – An in-vitro alteration experiment of biogenic apatite in isotopically enriched tracer solution N2 - Stable isotope ratios and trace element concentrations of fossil bones and teeth are important geochemical proxies for the reconstruction of diet and past environment in archaeology and palaeontology. However, since diagenesis can significantly alter primary diet-related isotope signatures and elemental compositions, it is important to understand and quantify alteration processes. Here, we present the results of in-vitro Alteration experiments of dental tissues from a modern African elephant molar reacted in aqueous solutions at 30 °C and 90 °C for 4 to 63 days. Dental cubes with ≈ 3 mm edge length, comprising both enamel and dentin, were placed into 2 mL of acidic aqueous solution enriched in different isotopes (25Mg, 44Ca, 67Zn, 86Sr, initial pH 1). Element and isotope distribution profiles across the reacted cubes were measured with LA-(MC-)ICP-MS and EMPA, while potential effects on the bioapatite crystal structure were characterised by Raman spectroscopy. In all experiments isotope ratios measured by LA-(MC-)ICP-MS revealed an alteration of the enamel in the outer ≈ 200–300 μm. In contrast, dentin was fully altered (≈ 1.4 mm) after one week at 90 °C while the alteration did not exceed a depth of 150–200 μm during the 30 °C experiments. Then, the tracer solution started also to penetrate through the enamel-dentin junction into the innermost enamel, however, leaving the central part of the enamel unaltered, even after three months. The Raman spectra suggest an initial demineralisation in the acidic environment while organic matter (i.e. collagen) is still preserved. In the 90 °C experiment, Raman spectra of the v1 PO4) band of the dentin shift over time towards synthetic hydroxylapatite patterns and the Ca (and Sr) concentrations in the respective solutions decrease. This indicates precipitation of newly formed apatite. Isotope and element concentration profiles across the dental tissues reveal different exchange mechanisms for different isotope systems. Magnesium is leached from enamel and dentin, while Zn is incorporated into the apatite crystal structure. However, the distribution of both elements is not affected in the innermost enamel where their concentrations do not change over the whole duration of the experiments. We found no correlation of reaction depth in the cubes and experimental duration, which might be caused by natural variability of the dental material already at the beginning of the experiment. Our alteration experiments in a closed system at high temperatures ≤90 °C and low initial pH demonstrate that at least the central part of mm-thick mammalian enamel apatite seems to be resistant against alteration preserving its pristine bioapatite mineral structure as well as its in-vivo elemental and isotopic composition. The experiments assess diagenetic alteration in a novel multi-proxy approach using in-situ analyses in high spatial resolution. It is demonstrated that the isotopes of Ca, Sr, Zn and Mg in the dentin are prone for diagenetic alteration, while enamel is more resistant against alteration and could be used for dietary and physiological reconstructions in fossil teeth. KW - Bioapatite KW - Isotopes KW - Raman spectroscopy KW - Diagenesis KW - LA-(MC-)ICP-MS KW - EPMA PY - 2021 DO - https://doi.org/10.1016/j.chemgeo.2021.120196 VL - 572 SP - 120196 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-52447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gehrenkemper, Lennart T1 - Organically bound fluorine in river water - A methode comparison of CIC and HR-CS-GFMAS N2 - Abstract: Since it is unknown for many applications, which PFASs are used and how they enter the environment, target analysis-based methods reach their limits. The two most frequently used sum parameters are the adsorbable organically bound fluorine (AOF) and the extractable organically bound fluorine (EOF). Both can be quantified using either combustion ion chromatography (CIC) or high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). Here we provide an insight on the advantageous and disadvantageous of both sum parameters and both detection methods. Our study is based on the analysis of surface water samples. Next to total fluorine (TF) analysis, AOF and EOF were determined as well as CIC and HR-CS-GFMAS are compared and results are comparatively discussed. Fluorine mass balancing revealed that, the AOF/TF proportion was higher than the EOF/TF proportion. The AOF made up 0.14–0.81% of TF and the EOF 0.04–0.28% of TF. Although, organically bound fluorine represents only a small portion of TF, PFASs are of worldwide concern, because of their extreme persistence and their bioaccumulation potential. The EOF-HR-CS-GFMAS method turned out to be more precise and sensitive than the AOF-CIC method and is a promising tool for future monitoring studies/routine analysis of PFASs in the environment. T2 - SALSA Make and Measure 2020: Advanced Characterization of Materials CY - Online meeting DA - 15.10.2020 KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Combustion ion chromatography (CIC) KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Adsorbable organically bound fluorine (AOF) KW - Extractable organically bound fluorine (EOF) KW - Surfacewaters PY - 2020 AN - OPUS4-52451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ecke, Alexander T1 - Magnetpartikelbasierte Immunoassays für die Bestimmung von Amoxicillin und Diclofenac im Trinkwasser N2 - Wir berichten hier über die Entwicklung von magnetpartikelbasierten Immunoassays für die Bestimmung zweier relevanter Kontaminanten des Trinkwassers: Diclofenac (DCF) und Amoxicillin (AMX). Für die beiden Analyten wurden die Assays nach unterschiedlichen Prinzipien entwickelt, die sich auch auf weitere Analyten übertragen lassen. Im Vergleich zum herkömmlichen ELISA weisen die hier entwickelten magnetpartikelbasierten Assays einen größeren Messbereich mit niedrigeren Bestimmungsgrenzen bei gleichzeitig deutlich reduzierter Analysendauer auf. Darüber hinaus können die Immunoassays in ein automatisierbares Onlinesystem zur Analyse in der Trinkwasserversorgung implementiert werden. Strategien hierfür werden erläutert. T2 - Spurenstoffe und Krankheitserreger im Wasserkreislauf CY - Online Meeting DA - 19.04.2021 KW - Immunoassay KW - Amoxicillin KW - Diclofenac KW - Immunosensor KW - Magnetpartikel PY - 2021 AN - OPUS4-52466 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Yi A1 - Song, L. A1 - Young, M.D. A1 - van der Wielen, M. A1 - Evans-Nguyen, T. A1 - Riedel, Jens A1 - Shelley, J.T. T1 - Unsupervised Reconstruction of Analyte-Specific Mass Spectra Based on Time-Domain Morphology with a Modified Cross-Correlation Approach N2 - Concomitant species that appear at the same or very similar times in a mass-spectral analysis can clutter a spectrum because of the coexistence of many analyte-related ions (e.g., molecular ions, adducts, fragments). One method to extract ions stemming from the same origin is to exploit the chemical information encoded in the time domain, where the individual temporal appearances inside the complex structures of chronograms or chromatograms differ with respect to analytes. By grouping ions with very similar or identical time-domain structures, single-component mass spectra can be reconstructed, which are much easier to interpret and are library-searchable. While many other approaches address similar objectives through the Pearson’s correlation coefficient, we explore an alternative method based on a modified cross-correlation algorithm to compute a metric that describes the degree of similarity between features inside any two ion chronograms. Furthermore, an automatic workflow was devised to be capable of categorizing thousands of mass-spectral peaks into different groups within a few seconds. This approach was tested with direct mass-spectrometric analyses as well as with a simple, fast, and poorly resolved LC–MS analysis. Single-component mass spectra were extracted in both cases and were identified based on accurate mass and a mass-spectral library search. KW - Mass-Spectral Reconstruction KW - Mass Spectrometry KW - Correlation PY - 2021 DO - https://doi.org/10.1021/acs.analchem.0c04396 VL - 93 IS - 12 SP - 5009 EP - 5014 PB - ACS AN - OPUS4-52467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - van Wasen, S. A1 - You, Yi A1 - Beck, S. A1 - Riedel, Jens A1 - Volmer, D. T1 - Quantitative Analysis of Pharmaceutical Drugs Using a Combination of Acoustic Levitation and High Resolution Mass Spectrometry N2 - A combination of acoustic levitation, laser vaporization, and atmospheric pressure chemical ionization mass spectrometry (APCI-MS) is presented in this study that enabled sensitive analysis of pharmaceutical drugs from an aqueous sample matrix. An unfocused pulsed infrared laser provided contactless sample desorption from the droplets trapped inside an acoustic levitator by activation of the OH stretching band of aqueous and alcoholic solvents. Subsequent atmospheric pressure chemical ionization was used between the levitated droplet and the mass spectrometer for postionization. In this setup, the unfocused laser gently desorbed the analytes by applying very mild repulsive forces. Detailed plume formation studies by temporally resolved schlieren experiments were used to characterize the liquid gas transition in this process. In addition, the role of different additives and solvent composition was examined during the ionization process. The analytical application of the technique and the proof-of-concept for quantitative analysis were demonstrated by the determination of selected pharmaceutical drugs in aqueous matrix with limits of quantification at the lower nanomolar level and a linear dynamic range of 3–4 orders of magnitude. KW - Atmospheric Pressure Chemical Ionization KW - Ultrasonic Levitation KW - Mass Spectrometry KW - Laser Desorption PY - 2021 DO - https://doi.org/10.1021/acs.analchem.1c00762 VL - 93 IS - 15 SP - 6019 EP - 6024 PB - ACS AN - OPUS4-52470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ciornii, Dmitri T1 - Knowledge Readiness Level (KaRL) approach for nanorisk governance and beyond N2 - Regulatory decisions require reliable data and knowledge derived from this. Among stakeholders in nanotechnology, however, there is often uncertainty about the quality of data for regulatory purposes. In addition, the general public often finds itself excluded from nanoregulation and policy decisions. This creates uncertainty in the nanotechnology field and also in other branches of technology and leads to concerns among the society. To address these issues, NANORIGO elaborates a framework to support decision making as well as data, information and knowledge sharing and use. We refer to “reliability” of data and knowledge as a degree of readiness or maturity. According to these criteria we worked out a 9-level scale in analogy to TRL (technology readiness level), the KaRL system (Knowledge, Data and Information Readiness Level). KaRL allows assessment of knowledge readiness for decision making by applying defined quality criteria for each level. It also provides guidance on how to enhance the readiness level by the help of available tools and procedures. KaRL addresses SEIN[1] principles, circular economy and thus involves the public concerns in regulation. A specialized nanorisk governance council (being under development in NANORIGO) is suggested to perform quality check of an actionable document, thus, aiding in consensus on the reliability (maturity) of knowledge for decision making. Moreover, KaRL facilitates traceability of knowledge before its use in decision making. This enables the transparency demanded by all stakeholders. T2 - EuroNanoForum 2021 CY - Online meeting DA - 05.05.2021 KW - Knowledge Readiness Level KW - Nanorisk KW - Nanomaterials KW - Data PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524725 AN - OPUS4-52472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Bayat, Mehmet E. A1 - Bartholmai, Matthias T1 - Identifizierung und Bewertung von Einflussgrößen bei der Sprengstoffspuren-detektion durch Ionenmobilitätsspektrometrie N2 - IMS trägt zur Luftfrachtsicherheit bei Luftsicherheitsgesetze verpflichten Luftsicherheitsbehörden, Flughafenbetreiber und Fluggesellschaften umfassende Sicherheitsmaßnahmen auf den Flughäfen zu ergreifen, um Gefahren z. B. durch potenziell gefährliche Frachtgüter zu erkennen. Von der Europäische Zivilluftfahrt-Konferenz (ECAC) zertifizierte IMS-Geräte werden vor Ort an den Kontrollpunkten orthogonal zur Radiologie eingesetzt, um chemische Informationen von verdächtiger Fracht über Gefahrstoffe wie Sprengstoffe oder Drogen vor dem Verladen zu erhalten. Vor der Detektion von Sprengstoffen beginnt die Untersuchung eines verdächtigen Objekts mit der Probenahme mittels Wischprobensammlern. Eine Luftsicherheitskontrollkraft wischt dabei Oberflächen des Objekts mit einem Probensammler ab, um Partikel von Gefahrstoffen zu sammeln. Der beladene Probensammler wird anschließend in einen Probeneinlass eingeführt. Nach thermischer Desorption der gesammelten Stoffe erhält der Bediener (z. B. Luftsicherheitskontrollkraft) ein boolesches Ergebnis - "Alarm" oder "Kein Alarm". Verfahren und Ergebnisse In dieser Studie wurden drei Verfahren mit vier ECAC-zertifizierten ETD-Geräten zur Identifizierung und Beurteilung der Probenahme (PN) entwickelt: I) direkte PN durch lösemittelbasierten Auftrag einer bekannten Sprengstoffmenge auf einem Probensammler, II) Auftrag einer bekannten Menge eines gelösten Sprengstoffs auf einem 10 cm × 10 cm Substrat (Aluminium, Papier, Eisen und Polyvinylchlorid) und manuelle PN nach Lösemittelverdampfung, III) lösemittelbasierter Sprengstoffauftrag auf eine PTFE- oder PTFE-beschichtete Glasfaseroberfläche, nach Lösemittelverdunstung trockene Übertragung auf das zu beprobende Substrat zur PN. Der Zusammenhang zwischen vorgelegter Sprengstoffmenge und der Detektionswahrscheinlichkeit (POD) erfolgt durch Anwendung des binären Regressionsverfahrens mit einer Logit-Funktion: POD=1/(1+exp⁡(-A(m-B)) )·100% Dabei entspricht m der vorgelegten Sprengstoffmasse bis 1000 ng, Parameter A / ng-1 der logistischen Wachstumsrate der Kurve und Parameter B / ng dem m-Wert des Mittelpunktes des Sigmoids. Die Bestimmung der Parameter wurde nach der Methode der kleinsten Quadrate berechnet. Das entwickelte Messunsicherheitsmodell kombiniert quantitative Ergebnisse aus Stammlösung und deren Verdünnungen sowie Stoffauftrag und qualitative Ergebnisse nach Anzeige "Alarm" oder "Kein Alarm". Dieses Auswerteverfahren wurde auf die Probenahme angewandt. Identifizierte Unsicherheitsursachen sind die Durchführung der Wischprobenahme, Staub, Lösemitteleffekte und die Unsicherheit bei der Herstellung von Testlösungen. T2 - 8. Ionenmobilitätsspektrometrie (IMS)-Anwendertreffen CY - Online meeting DA - 17.03.2021 KW - IMS KW - Ionenmobilitätsspektrometrie KW - Ion mobility spectrometry KW - Sprengstoffspurendetektion KW - Luftfrachtsicherheit PY - 2021 UR - https://www.uni-potsdam.de/de/ims2021/tagungsprogramm AN - OPUS4-52474 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knelles, J. A1 - Wanner, C. A1 - Schulz, F. A1 - Freund, M. A1 - Kolmangadi, Mohamed Aejaz A1 - Baro, A. A1 - Huber, P. A1 - Schönhals, Andreas A1 - Lachat, S. T1 - Liquid crystalline hydrazones revisited: dipolar interactions vs hydrogen bonding affecting mesomorphic properties N2 - In order to understand the role of dipolar interactions vs. H-bonding, a series of hydrazones were synthesised from 4-alkoxy-, 3,4-dialkoxy- or 3,4,5-trialkoxybenzaldehydes and phenyl, bromo- or nitrophenylhydrazine, respectively. Their mesomorphic properties were investigated by differential scanning calorimetry (DSC), polarising optical microscopy (POM), X-ray diffraction (WAXS, SAXS) and compared with known members. Only those hydrazones derived from 3,4,5-trisalkoxybenzaldehyde and either meta, meta-dinitro- or ortho, para-dinitrophenylhydrazine displayed hexagonal columnar mesophases. All other derivatives were non-mesomorphic, even when H-bonds were present. Dipole moments of the various nitro-substituted hydrazones were experimentally determined by dielectric measurements and supported by theoretical DFT calculations, which indicated that the mesophase formation is mostly governed by strong dipole moment and further enforced by intramolecular H-bonding. KW - Discotic liquid crystals PY - 2021 DO - https://doi.org/10.1080/02678292.2021.1873438 VL - 48 IS - 10 SP - 1382 EP - 1391 PB - Taylor & Francis AN - OPUS4-52409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, Uwe A1 - Zscherpel, Uwe T1 - Aktuelle Entwicklungen in der Normung N2 - Es wird über die neuen Anforderungen ausgewählter Normen bzw. Normrevisionen informiert und insbesondere auch über die veränderten Parameter, die bei der Prüfpraxis, der Qualitätssicherung in der digitalen Radiographie und bei der Klassifizierung zu berücksichtigen sind. Das wichtigste Projekt ist die Revision der DIN EN ISO 17636-1, -2, RT von Schweißverbindungen, in ISO TC 44 SC 5 WG 1. Hauptaktivität bei ASTM ist gegenwärtig die Überarbeitung der CT-Standards und die Berücksichtigung der Anforderungen an das dimensionelle Messen. Der „Standard Guide for Computed Tomography“, ASTM E 1441, zur Bestimmung von MTF, Kontrast-Detail-Funktion (CDF) und Kontrast-Diskrimination-Diagramm (CDD) wurde revidiert und veröffentlicht. Die Mehrzahl der Hersteller von CT-Anlagen bietet entsprechende Software-Tools an. Weiterhin werden neue Festkörperentwürfe zur Charakterisierung von CT-Anlagen vorgestellt. Die folgenden Revisionen sind bei ASTM derzeit in Bearbeitung: ASTM E 2445, „CR Long Term Stability“ nach einem Round Robin-Test und für DDAs der Standard zur System-Charakterisierung, ASTM E2597/E2597M−14, und zur „DDA Long Term Stability“. Das Spider-Net-Diagramm zur Klassifizierung von DDAs wird um die Position „ISO Material Thickness limit“ erweitert. Der Standard EN 12679 zur Messung der Größe von Gammastrahlern wurde nach Revision unter Berücksichtigung von digitalen Messverfahren veröffentlicht. Die Revision der Standardserie EN 12543 zur Messung der Brennfleckgröße ist mit Verzögerung in Überarbeitung, um die digitalen Detektoren und Messmöglichkeiten mit Bildverarbeitungsprogrammen zu berücksichtigen. Die Messprozedur für Lochkameras wurde grundlegend revidiert und ist harmonisiert mit ASTM E 1165-12(2017). Die gemessenen Brennflecke unterscheiden sich und passen besser zu den Unschärfe-Messungen mit Doppeldraht BPKs (ISO 19232-5:2018) bei Vergrößerung. Ein Entwurf zur Messung der Brennfleckgröße von nano-Fokusröhren und Mikro-Fokusröhren (< 5 µm) wird derzeit vom Europäischen Metrologie-Programm EMPIR gefördert. Es wird über erste Ergebnisse informiert. T2 - 19. Seminar Aktuelle Fragen der Durchstrahlungsprüfung und Strahlenschutz CY - Online meeting DA - 23.03.2021 KW - Industrielle Durchstrahlungsprüfung KW - ZfP KW - Normentwicklung RT KW - DIN ISO ASTM International PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524149 SP - Paper 8, 1 EP - Paper 8, 15 PB - DGZfP AN - OPUS4-52414 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silva, W. A1 - Lopes, R. A1 - Zscherpel, Uwe A1 - Meinel, Dietmar A1 - Ewert, Uwe T1 - X-ray imaging techniques for inspection of composite pipelines N2 - The literature has shown that the application of laminography provides advantages as 3D radiographic imaging with depth information for in house and mobile testing. This permits to distinguish between overlapping indications, measure the extension along radiation direction and classify indications as surface open or subsurface ones as required in critical engineering assessment. This work provides a comparative study and measurements of the three techniques Digital Radiography (DR) with Digital Detector Arrays (DDA), Coplanar Translational Laminography (CTL) and Computed Tomography (CT), applied for composite pipeline inspection. It is demonstrated that CTL and CT provide advantages for the evaluation of pipe-to-pipe connections and the evaluation of adhesive applications. They show indications of discontinuities with higher contrast sensitivity than radiography. Beyond it, two specimen, namely Phantom 1 and Phantom 2, were developed and manufactured by additive manufacturing to analyze the preferential detection sensitivity and the direction of features and depth information for laminographic measurements. Another goal was to show the laminographic capabilities to distinguish between overlapping discontinuities. CTL is especially suitable for mobile inspection. Special glass fiber reinforced polymer samples (GRP) were manufactured for further analysis and comparisons between the abovementioned techniques. Finally, Phantoms 1 and 2 show the capability of laminography to detect overlapping indications and also show that discontinuities oriented perpendicular to the scan direction have the highest contrast sensitivity for laminographic measurements. KW - Digital Radiography KW - Laminography KW - Computed Tomography KW - Composite Pipes KW - Image Quality PY - 2021 DO - https://doi.org/10.1016/j.micron.2021.103033 SN - 0968-4328 VL - 145 SP - 103033 PB - Elsevier Ltd. AN - OPUS4-52415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Meermann, Björn T1 - PFAS-Summenparameteranalytik - Neue analytische Methoden zum Nachweis von per- und polyfluorierten Verbindungen in der Umwelt N2 - Per- und polyfluorierte Alkylverbindungen (PFAS) sind sehr persistent und reichern sich in der Umwelt und im menschlichen Organismus in immer höheren Konzentrationen an. PFAS stellen deshalb eine große Gefährdung für Mensch und Umwelt dar. Eingesetzt werden sie u. a. als wasser- und fettabweisende Beschichtung in z. B. der Papier- und Textilindustrie und gelangen so während Produktion, Gebrauch und Entsorgung u. a. in den Wasserkreislauf. PFAS konnten sogar in der arktischen Umwelt in relevanten Konzentrationen detektiert werden und zählen somit zu den „emerging pollutants“. Ein prominenter Vertreter der PFAS stellt Perfluoroctansulfonsäure (PFOS) dar - die jedoch bereits im Anhang des Stockholmer Abkommen gelistet wurde und deren Einsatz somit stark eingeschränkt bzw. verboten ist. Im Hinblick auf die Vielzahl von Verbindungen werden neue analytische Methoden benötigt, die eine PFAS-Belastungssituation möglichst umfassend und nachweisstark widerspiegeln, um zukünftig mögliche Grenzwerte ableiten zu können. KW - PFAS KW - HR-CS-GFMAS KW - CIC KW - Fluor KW - Oberflächenwasser PY - 2021 UR - https://analyticalscience.wiley.com/do/10.1002/was.00080223 SN - 0016-3538 VL - 2021 IS - März SP - was.00080223, 2 EP - 4 PB - Wiley-VCH CY - Weinheim AN - OPUS4-52261 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Olaf T1 - Contaminants of Emerging Concern from Materials and Products: Measurement and Evaluation N2 - Test chamber measurements are an important tool to improve indoor air quality and occupational safety. Test chamber measurements are possible for a wide range of materials, products and technologies. Determination of concerning contaminants is important to ensure good indoor air quality. The detection of concerning contaminants depends on the approriate sampling and analysis. T2 - Webinar BAM-University of Birmingham CY - Online meeting DA - 24.02.2021 KW - Emerging Contaminants KW - Emission Test Chamber KW - Thermal Extraction KW - Thermal Desorption PY - 2021 AN - OPUS4-52262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - MALDI Mass spectrometry of synthetic polymers – making molecular elephants to fly N2 - The importance of MALDI TOF mass spectrometry for the analysis of synthetic polymers is shown and some specific issues influencing the analysis e.g. polymer mass dispersity, matrix and matrix homogeneity, nature of cations and end groups, sequence distribution are discussed by means of examples. T2 - Merck Polymer Seminar CY - Online meeting DA - 29.04.2021 KW - MALDI-ToF MS KW - Ionization KW - Desorption KW - Polymers PY - 2021 AN - OPUS4-52545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard T1 - Set of technical drawings, associated with manuscript entitled: "Extending Synchrotron SAXS instrument ranges through addition of a portable, inexpensive USAXS module with vertical rotation axes" N2 - This is a set of drawings accompanying the submitted paper entitled "Extending Synchrotron SAXS instrument ranges through addition of a portable, inexpensive USAXS module with vertical rotation axes". The parts described herein will combine with commercial off-the-shelf components to build a high precision pair of rotation stages for accurate measurement of scattering angles with a sub-microradian precision. KW - X-ray scattering KW - USAXS KW - ultra-small-angle X-ray scattering KW - technical drawings KW - module KW - extension PY - 2021 DO - https://doi.org/10.5281/zenodo.4604703 PB - Zenodo CY - Geneva AN - OPUS4-52547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adams, L. C. A1 - Brangsch, J. A1 - Reimann, C. A1 - Kaufmann, Jan Ole A1 - Nowak, K. A1 - Buchholz, R. A1 - Karst, U. A1 - Botnar, R. M. A1 - Hamm, B. A1 - Makowski, M. R. T1 - Noninvasive imaging of vascular permeability to predict the risk of rupture in abdominal aortic aneurysms using an albumin binding probe N2 - Abdominal aortic aneurysm (AAA) remains a fatal disease. Its development encompasses a complex interplay between hemodynamic stimuli on and changes in the arterial wall. Currently available biomarkers fail to predict the risk of AAA rupture independent of aneurysm size. Therefore, novel biomarkers for AAA characterization are needed. In this study, we used a mouse model of AAA to investigate the potential of magnetic resonance imaging (MRI) with an albumin-binding probe to assess changes in vascular permeability at different stages of aneurysm growth. Two imaging studies were performed: a longitudinal study with follow-up and death as endpoint to predict rupture risk and a week-by-week study to characterize AAA development. AAAs, which eventually ruptured, demonstrated a significantly higher in vivo MR signal enhancement from the albumin-binding probe (p = 0.047) and a smaller non-enhancing thrombus area compared to intact AAAs (p = 0.001). The ratio of albumin-binding-probe enhancement of the aneurysm wall to size of non-enhancing-thrombus-area predicted AAA rupture with high sensitivity/specificity (100%/86%). More advanced aneurysms with higher vascular permeability demonstrated an increased uptake of the albumin-binding-probe. These results indicate that MRI with an albumin-binding probe may enable noninvasive assessment of vascular permeability in murine AAAs and prediction of rupture risk. KW - Magnetic resonance imaging KW - Imaging KW - Tomography KW - Gadolinium KW - Contrast agent KW - Atherosclerosis KW - ICP-MS KW - Gadofosveset KW - Angiography KW - LA-ICP-MS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525541 DO - https://doi.org/10.1038/s41598-020-59842-2 VL - 10 SP - Article number: 3231 PB - Springer Nature Limited CY - London, New York, Berlin, Shanghai and Tokyo AN - OPUS4-52554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmadi, Samim A1 - Thummerer, G. A1 - Breitwieser, S. A1 - Mayr, G. A1 - Lecompagnon, Julien A1 - Burgholzer, P. A1 - Jung, P. A1 - Caire, G. A1 - Ziegler, Mathias T1 - Multi-dimensional reconstruction of internal defects in additively manufactured steel using photothermal super resolution combined with virtual wave based image processing N2 - We combine three different approaches to greatly enhance the defect reconstruction ability of active thermographic testing. As experimental approach, laser-based structured illumination is performed in a step-wise manner. As an intermediate signal processing step, the virtual wave concept is used in order to effectively convert the notoriously difficult to solve diffusion-based inverse problem into a somewhat milder wavebased inverse problem. As a final step, a compressed-sensing based optimization procedure is applied which efficiently solves the inverse problem by making advantage of the joint sparsity of multiple blind measurements. To evaluate our proposed processing technique, we investigate an additively manufactured stainless steel sample with eight internal defects. The concerted super resolution approach is compared to conventional thermographic reconstruction techniques and shows an at least four times better spatial resolution. KW - Active thermography KW - Additive manufacturing KW - Stainless steel KW - ADMM KW - Block regularization KW - Internal defects KW - Joint sparsity KW - Laser excitation KW - Multi-dimensional reconstruction KW - Photothermal super resolution KW - Virtual waves PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525330 DO - https://doi.org/10.1109/tii.2021.3054411 SN - 1551-3203 SN - 1941-0050 VL - 17 IS - 11 SP - 7368 EP - 7378 PB - IEEE CY - New York, NY AN - OPUS4-52533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Ahmadi, Samim A1 - Hauffen, Jan Christian A1 - Kästner, L. A1 - Jung, P. A1 - Caire, G. A1 - Ziegler, Mathias T1 - Learned block iterative shrinkage thresholding algorithm for photothermal super resolution imaging N2 - Block-sparse regularization is already well-known in active thermal imaging and is used for multiple measurement based inverse problems. The main bottleneck of this method is the choice of regularization parameters which differs for each experiment. To avoid time-consuming manually selected regularization parameters, we propose a learned block-sparse optimization approach using an iterative algorithm unfolded into a deep neural network. More precisely, we show the benefits of using a learned block iterative shrinkage thresholding algorithm that is able to learn the choice of regularization parameters. In addition, this algorithm enables the determination of a suitable weight matrix to solve the underlying inverse problem. Therefore, in this paper we present the algorithm and compare it with state of the art block iterative shrinkage thresholding using synthetically generated test data and experimental test data from active thermography for defect reconstruction. Our results show that the use of the learned block-sparse optimization approach provides smaller normalized mean square errors for a small fixed number of iterations than without learning. Thus, this new approach allows to improve the convergence speed and only needs a few iterations to generate accurate defect reconstruction in photothermal super resolution imaging. KW - Iterative shrinkage thresholding algorithm KW - Neural network KW - Deep learning KW - Active thermography KW - Photothermal super resolution PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525364 DO - https://doi.org/10.48550/arXiv.2012.03547 SN - 2331-8422 SP - 1 EP - 11 PB - Cornell University CY - Ithaca, NY AN - OPUS4-52536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Ahmadi, Samim A1 - Kästner, L. A1 - Hauffen, Jan Christian A1 - Jung, P. A1 - Ziegler, Mathias T1 - Photothermal-SR-Net: A customized deep unfolding neural network for photothermal super resolution imaging N2 - This paper presents deep unfolding neural networks to handle inverse problems in photothermal radiometry enabling super resolution (SR) imaging. Photothermal imaging is a well-known technique in active thermography for nondestructive inspection of defects in materials such as metals or composites. A grand challenge of active thermography is to overcome the spatial resolution limitation imposed by heat diffusion in order to accurately resolve each defect. The photothermal SR approach enables to extract high-frequency spatial components based on the deconvolution with the thermal point spread function. However, stable deconvolution can only be achieved by using the sparse structure of defect patterns, which often requires tedious, hand-crafted tuning of hyperparameters and results in computationally intensive algorithms. On this account, Photothermal-SR-Net is proposed in this paper, which performs deconvolution by deep unfolding considering the underlying physics. This enables to super resolve 2D thermal images for nondestructive testing with a substantially improved convergence rate. Since defects appear sparsely in materials, Photothermal-SR-Net applies trained blocksparsity thresholding to the acquired thermal images in each convolutional layer. The performance of the proposed approach is evaluated and discussed using various deep unfolding and thresholding approaches applied to 2D thermal images. Subsequently, studies are conducted on how to increase the reconstruction quality and the computational performance of Photothermal-SR-Net is evaluated. Thereby, it was found that the computing time for creating high-resolution images could be significantly reduced without decreasing the reconstruction quality by using pixel binning as a preprocessing step. KW - Photothermal super resolution KW - Nondestructive testing KW - Deep unfolding KW - Deep learning KW - Deep imaging KW - Physics-based deep learning KW - Laser thermography KW - Elastic net KW - Iterative shrinkage thresholding algorithm PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525371 DO - https://doi.org/10.48550/arXiv.2104.10563 SN - 2331-8422 SP - 1 EP - 10 PB - Cornell University CY - Ithaca, NY AN - OPUS4-52537 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grabicki, N. A1 - Nguyen, K. T. G. A1 - Weidner, Steffen A1 - Dumele, O. T1 - Confined Spaces in [n]Cyclo-2,7-pyrenylenes N2 - A set of strained aromatic macrocycles based on [n]cyclo2,7-(4,5,9,10-tetrahydro)pyrenylenes is presented with size dependent photophysical properties. The K-region of pyrene was functionalized with ethylene glycol groups to decorate the outer rim and thereby confine the space inside the macrocycle. This confined space is especially pronounced for n = 5, which leads to an internal binding of up to 8.0×104 M–1 between the ether-decorated [5]cyclo-2,7-pyrenylene and shape complementary crown ether–cation complexes. Both, the ether-decorated [n]cyclo-pyrenylenes as well as one of their host–guest complexes have been structurally characterized by single crystal X-ray analysis. In combination with computational methods the structural and thermodynamic reasons for the exceptionally strong binding have been elucidated. The presented rim confinement strategy makes cycloparaphenylenes an attractive supramolecular host family with a favorable, size-independent read-out signature and binding capabilities extending beyond fullerene guests. KW - Cycloparaphenylenes KW - Host–guest systems KW - Macrocycles KW - Molecular recognition KW - Supramolecular chemistry PY - 2021 DO - https://doi.org/10.1002/anie.202102809 SN - 1433-7851 VL - 60 IS - 27 SP - 1 EP - 7 PB - Wiley VCH AN - OPUS4-52517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien A1 - Ahmadi, Samim A1 - Hirsch, Philipp Daniel A1 - Ziegler, Mathias ED - Zalameda, J. N. ED - Mendioroz, A. T1 - Full-frame thermographic super-resolution with 2D-structured laser heating N2 - Thermographic super-resolution techniques allow the resolution of defects/inhomogeneities beyond the classical limit, which is governed by the diffusion properties of thermal wave propagation. Photothermal super-resolution is based on a combination of an experimental scanning strategy and a numerical optimization which has been proven to be superior to standard thermographic methods in the case of 1D linear defects. In this contribution, we report on the extension of this approach towards a full frame 2D photothermal super-resolution technique. The experimental approach is based on a repeated spatially structured heating using high power lasers. In a second post-processing step, several measurements are coherently combined using mathematical optimization and taking advantage of the (joint) sparsity of the defects in the sample. In our work we extend the possibilities of the method to efficiently detect and resolve defect cross sections with a fully 2D-structured blind illumination. T2 - Thermosense: Thermal Infrared Applications XLIII CY - Online meeting DA - 12.04.2021 KW - Thermography KW - super-resolution KW - NDT KW - Inspection KW - Image resolution PY - 2021 DO - https://doi.org/10.1117/12.2586093 VL - 11743 SP - 11743-26, 10 PB - SPIE AN - OPUS4-52524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien T1 - Full-frame thermographic super-resolution with 2D-structured laser heating N2 - Thermographic super-resolution techniques allow the resolution of defects/inhomogeneities beyond the classical limit, which is governed by the diffusion properties of thermal wave propagation. Photothermal super-resolution is based on a combination of an experimental scanning strategy and a numerical optimization which has been proven to be superior to standard thermographic methods in the case of 1D linear defects. In this contribution, we report on the extension of this approach towards a full frame 2D photothermal super-resolution technique. The experimental approach is based on a repeated spatially structured heating using high power lasers. In a second post-processing step, several measurements are coherently combined using mathematical optimization and taking advantage of the (joint) sparsity of the defects in the sample. In our work we extend the possibilities of the method to efficiently detect and resolve defect cross sections with a fully 2D-structured blind illumination. T2 - Thermosense: Thermal Infrared Applications XLIII CY - Online meeting DA - 12.04.2021 KW - Thermography KW - Super-resolution KW - NDT KW - Inspection KW - Image resolution PY - 2021 UR - https://www.spiedigitallibrary.org/conference-proceedings-of-spie/11743/117430T/Full-frame-thermographic-super-resolution-with-2D-structured-laser-heating/10.1117/12.2586093.full AN - OPUS4-52526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien T1 - 2D-Photothermal super-resolution with sparse matrix stacking N2 - Thermographic super resolution techniques allow the spatial resolution of defects/inhomogeneities below the classical limit, which is governed by the diffusion properties of thermal wave propagation. In this work, we re-port on the extension of this approach towards a full frame 2D super resolution technique. The approach is based on a repeated spatially structured heating using high power lasers. In a second post-processing step, several measurements are coherently combined using mathematical optimization and taking advantage of the (joint) sparsity of the defects in the sample. T2 - Sensor and Measurement Science International Conference SMSI 2021 CY - Online meeting DA - 03.05.2021 KW - Thermography KW - Super-resolution KW - NDT KW - Inspection KW - Image resolution PY - 2021 AN - OPUS4-52579 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adams, L. C. A1 - Brangsch, J. A1 - Reimann, C. A1 - Kaufmann, Jan Ole A1 - Buchholz, R. A1 - Karst, U. A1 - Botnar, R. M. A1 - Hamm, B. A1 - Makowski, M. R. T1 - Simultaneous molecular MRI of extracellular matrix collagen and inflammatory activity to predict abdominal aortic aneurysm rupture N2 - Abdominal aortic aneurysm (AAA) is a life-threatening vascular disease with an up to 80% mortality in case of rupture. Current biomarkers fail to account for size-independent risk of rupture. By combining the information of different molecular probes, multi-target molecular MRI holds the potential to enable individual characterization of AAA. In this experimental study, we aimed to examine the feasibility of simultaneous imaging of extracellular collagen and inflammation for size-independent prediction of risk of rupture in murine AAA. The study design consisted of: (1) A outcome-based longitudinal study with imaging performed once after one week with follow-up and death as the end-point for assessment of rupture risk. (2) A week-by-week study for the characterization of AAA development with imaging after 1, 2, 3 and 4 weeks. For both studies, the animals were administered a type 1 collagen-targeted gadolinium-based probe (surrogate marker for extracellular matrix (ECM) remodeling) and an iron oxide-based probe (surrogate marker for inflammatory activity), in one imaging session. In vivo measurements of collagen and iron oxide probes showed a significant correlation with ex vivo histology (p < 0.001) and also corresponded well to inductively-coupled plasma-mass spectrometry and laser-ablation inductively-coupled plasma mass spectrometry. Combined evaluation of collagen-related ECM remodeling and inflammatory activity was the most accurate predictor for AAA rupture (sensitivity 80%, specificity 100%, area under the curve 0.85), being superior to information from the individual probes alone. Our study supports the feasibility of a simultaneous assessment of collagen-related extracellular matrix remodeling and inflammatory activity in a murine model of AAA. KW - Atherosclerosis KW - Specific probe KW - Magnetic resonance imaging KW - Gadolinium KW - Iron oxide KW - Ferumoxytol KW - Inductively‑coupled mass spectrometry KW - ICP-MS KW - LA-ICP-MS KW - Laser ablation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525864 UR - https://www.nature.com/articles/s41598-020-71817-x DO - https://doi.org/10.1038/s41598-020-71817-x VL - 10 IS - 1 SP - 15206 PB - Springer Nature Limited CY - London, New York, Berlin, Shanghai and Tokyo AN - OPUS4-52586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien A1 - Ahmadi, Samim A1 - Hirsch, Philipp Daniel A1 - Ziegler, Mathias T1 - 2D-Photothermal Super Resolution with Sparse Matrix Stacking N2 - Thermographic super resolution techniques allow the spatial resolution of defects/inhomogeneities below the classical limit, which is governed by the diffusion properties of thermal wave propagation. In this work, we report on the extension of this approach towards a full frame 2D super resolution technique. The approach is based on a repeated spatially structured heating using high power lasers. In a second post-processing step, several measurements are coherently combined using mathematical optimization and taking advantage of the (joint) sparsity of the defects in the sample T2 - Sensor and Measurement Science International Conference SMSI 2021 CY - Online meeting DA - 03.05.2021 KW - Thermography KW - Super-resolution KW - NDT KW - Inspection KW - Image resolution PY - 2021 SN - 978-3-9819376-4-0 DO - https://doi.org/10.5162/SMSI2021/C2.2 VL - SMSI 2021 - Sensors and Instrumentation SP - 183 EP - 184 AN - OPUS4-52589 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lay, Vera T1 - 3D seismic imaging of the Alpine Fault and the glacial valley at Whataroa, New Zealand N2 - The Alpine Fault at the West Coast of the South Island (New Zealand) is a major plate boundary that is expected to rupture in the next 50 years, likely as a magnitude 8 earthquake. The Deep Fault Drilling Project (DFDP) aimed to deliver insight into the geological structure of this fault zone and its evolution by drilling and sampling the Alpine Fault at depth. Here we present results from a seismic survey around the DFDP-2 drill site in the Whataroa Valley where the drillhole almost reached the fault plane. This unique 3D seismic survey includes several 2D lines and a 3D array at the surface as well as borehole recordings. Within the borehole, the unique option to compare two measurement systems is used: conventional three-component borehole geophones and a fibre optic cable (heterodyne Distributed Vibration Sensing system (hDVS)). Both systems show coherent signals but only the hDVS system allowed a recording along the complete length of the borehole. Despite the challenging conditions for seismic imaging within a glacial valley filled with sediments and steeply dipping valley flanks, several structures related to the valley itself as well as the tectonic fault system are imaged. The pre-processing of the seismic data also includes wavefield separation for the zero-offset borehole data. Seismic images are obtained by prestack depth migration approaches. Within the glacial valley, particularly steep valley flanks are imaged directly and correlate well with results from the P-wave velocity model obtained by first arrival travel-time tomography. Additionally, a glacially over-deepened trough with nearly horizontally layered sediments is identified about 0.5 km south of the DFDP-2B borehole. With regard to the expected Alpine fault zone, a set of several reflectors dipping 40-56° to the southeast are identified in a ~600 m wide zone between depths of 0.2 and 1.2 km that is interpreted to be the minimum extent of the damage zone. Different approaches image one distinct reflector dipping at 40°, which is interpreted to be the main Alpine Fault reflector. This reflector is only ~100 m ahead from the lower end of the borehole. At shallower depths (z<0.5 km), additional reflectors are identified as fault segments and generally have steeper dips up to 56°. About 1 km south of the drill site, a major fault is identified at a depth of 0.1-0.5 km that might be caused by the regional tectonics interacting with local valley structures. A good correlation is observed among the separate seismic data sets and with geological results such as the borehole stratigraphy and the expected surface trace of the fault. In conclusion, several structural details of the fault zone and its environment are seismically imaged and show the complexity of the Alpine Fault at the Whataroa Valley. Thus, a detailed seismic characterization clarifies the subsurface structures, which is crucial to understand the transpressive fault’s tectonic processes. T2 - EGU 2021 General Assembly CY - Online meeting DA - 19.04.2021 KW - Imaging KW - Signal processing KW - Seismic KW - Borehole KW - DAS PY - 2021 AN - OPUS4-52614 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - EURAMET.QM-S14 Measurement capabilities for the quantification of ethanol in water N2 - The presentation summarizes the results of the EURAMET key comparison QM-S14 “Measurement capabilities for the quantification of ethanol in water”. Possible options for the key comparison reference value (KCRV) are discussed. A Bayesian approach is finally used to estimate the KCRV and the degrees of equivalence of participants. T2 - EURAMET TC-MC Sector Committee Bio- and Organic Analysis Meeting CY - Online meeting DA - 02.02.2021 KW - Certified reference material KW - EMPIR project KW - Interlaboratory comparison PY - 2021 AN - OPUS4-52615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gantois, F. T1 - EURAMET.QM-S13 Comparison of value assigned forensic alcohol in water reference materials N2 - The presentation summarizes the results of the EURAMET key comparison QM-S13 “Comparison of value assigned forensic alcohol in water reference materials”. Possible options for the key comparison reference function (KCRF) are discussed: the frequentist approach and a Bayesian approach. Both methods are used to determine the degrees of equivalence of materials and participants. T2 - EURAMET TC-MC Sector Committee Bio- and Organic Analysis Meeting CY - Online meeting DA - 02.02.2021 KW - Certified reference material KW - EMPIR project KW - Iinterlaboratory comparison PY - 2021 AN - OPUS4-52617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Held, Mathias A1 - Rashwan, Abdalla A1 - Lauschkin, Maik A1 - Bulling, Jannis A1 - Lugovtsova, Yevgeniya A1 - Prager, Jens T1 - Inverse determination of elastic material parameters from ultrasonic guided waves dispersion measurements using Convolutional Neuronal Networks N2 - In the context of Industry 4.0 and especially in the field of Structural Health Monitoring, Condition Monitoring and Digital Twins, simulations are becoming more and more important. The exact determination of material parameters is required for realistic results of numerical simulations of the static and dynamic behavior of technical structures. There are many possibilities to determine elastic material parameters. One possibility of non-destructive testing are ultrasonic guided waves. For the evaluation of the measurement results, mostly inverse methods are applied in order to be able to draw conclusions about the elastic material parameters from analysing the ultrasonic guided wave propagation. For the inverse determination of the elastic material Parameters with ultrasonic guided waves, several investigations were carried out, e.g. the determination of the isotropic material parameters through the point of zero-groupvelocity or anisotropic material parameters with a simplex algorithm. These investigations are based on the evaluation of dispersion images. Machine learning and in particular Convolutional Neural Networks (CNN) are one possibility of the automated evaluation from Image data, e.g. classification or object recognition problems. This article shows how the dispersive behavior of ultrasonic guided waves and CNNs can be used to determine the isotropic elastic constants of plate-like structures. T2 - SMSI 2021 2021-05-03 - 2021-05-06 digital CY - Online meeting DA - 03.05.2021 KW - Convolutional Neuronal Networks KW - Inverse Probleme KW - Materialcharakterisierung KW - guided waves KW - Dispersion PY - 2021 SN - 978-3-9819376-4-0 DO - https://doi.org/10.5162/SMSI2021/A10.2 VL - 2021 SP - 239 EP - 240 AN - OPUS4-52618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. A1 - Neumann, Patrick P. A1 - Kohlhoff, Harald A1 - Erdmann, Jessica A1 - Schaffernicht, Erik A1 - Lilienthal, Achim J. T1 - Development of a Low-Cost Sensing Node with Active Ventilation Fan for Air Pollution Monitoring N2 - A fully designed low-cost sensing node for air pollution monitoring and calibration results for several low-cost gas sensors are presented. As the state of the art is lacking information on the importance of an active ventilation system, the effect of an active fan is compared to the passive ventilation of a lamellar structured casing. Measurements obtained in an urban outdoor environment show that readings of the low-cost dust sensor (Sharp GP2Y1010AU0F) are distorted by the active ventilation system. While this behavior requires further research, a correlation with temperature and humidity inside the node shown. T2 - SMSI 2021 Conference: Sensor and Measurement Science International CY - Online meeting DA - 03.05.2021 KW - Wireless sensing node KW - Air pollution KW - Sensor network KW - Environmental monitoring PY - 2021 DO - https://doi.org/10.5162/SMSI2021/D3.5 VL - 2021 SP - 260 EP - 261 AN - OPUS4-52607 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - A fast and simple extraction method for the determination of PFASs in soil samples - HR-CS-GFMAS a new screening tool N2 - Here, we describe a fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) utilizing extractable organic fluorine (EOF) sum parameter analysis and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) in soil samples. After extraction and separation of inorganic and organic fluorinated compounds, organically bound fluorinated compounds were indirectly determined via the molecular absorption of gallium mono-fluoride at 211.248 nm. The implementation of the decisions of the “Stockholm Convention on persistent organic pollutants” as well as the “Protocol on Persistent Organic Pollutants of the Convention on Long-Range Transboundary Air Pollution” of the UNECE include the reduction respectively the elimination of PFASs in the environment. Currently, regulations aim to target single compounds (mostly C8-PFAS). But the PFAS group includes over 4700 substances, which are potentially persistent and toxic, thus target analytical approaches are not suitable for a holistic approach investigating the PFAS pollutant situation. Furthermore, forbidden PFASs are substituted by short-chain PFASs, thus the number of unknow substances is steadily increasing. For this reason, sum parameter approaches are more suitable to investigate and assess the pollution situation as well as derive exposure limits. Our developed analytical method was successfully applied to determine PFASs in soil samples from a polluted site. In view of steadily increasing numbers of PFAS substances, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFAS in the future. T2 - ENSOr - International Workshop on Emerging policy challenges on new soil contaminants CY - Online Meeting DA - 06.05.2021 KW - PFAS KW - HR-CS-GFMAS KW - Soil KW - Sediment PY - 2021 AN - OPUS4-52608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. T1 - Development of a Low-Cost Sensing Node with Active Ventilation Fan for Air Pollution Monitoring N2 - A fully designed low-cost sensing node for air pollution monitoring and calibration results for several low-cost gas sensors are presented. As the state of the art is lacking information on the importance of an active ventilation system, the effect of an active fan is compared to the passive ventilation of a lamellar structured casing. Measurements obtained in an urban outdoor environment show that readings of the low-cost dust sensor (Sharp GP2Y1010AU0F) are distorted by the active ventilation system. While this behavior requires further research, a correlation with temperature and humidity inside the node shown. T2 - SMSI 2021 Conference: Sensor and Measurement Science International CY - Online meeting DA - 03.05.2021 KW - Wireless sensing node KW - Air pollution KW - Environmental monitoring PY - 2021 AN - OPUS4-52609 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brauckmann, C. A1 - Pramann, A. A1 - Rienitz, O. A1 - Schulze, A. A1 - Phukphatthanachai, Pranee A1 - Vogl, Jochen T1 - Combining Isotope Dilution and Standard Addition—Elemental Analysis in Complex Samples N2 - A new method combining isotope dilution mass spectrometry (IDMS) and standard addition has been developed to determine the mass fractions w of different elements in complex matrices: (a) silicon in aqueous tetramethylammonium hydroxide (TMAH), (b) sulfur in biodiesel fuel, and (c) iron bound to transferrin in human serum. All measurements were carried out using inductively coupled plasma mass spectrometry (ICP–MS). The method requires the gravimetric preparation of several blends (bi)—each consisting of roughly the same masses (mx,i) of the sample solution (x) and my,i of a spike solution (y) plus different masses (mz,i) of a reference solution (z). Only these masses and the isotope ratios (Rb,i) in the blends and reference and spike solutions have to be measured. The derivation of the underlying equations based on linear regression is presented and compared to a related concept reported by Pagliano and Meija. The uncertainties achievable, e.g., in the case of the Si blank in extremely pure TMAH of urel (w(Si)) = 90% (linear regression method, this work) and urel (w(Si)) = 150% (the method reported by Pagliano and Meija) seem to suggest better applicability of the new method in practical use due to the higher robustness of regression analysis. KW - Isotope dilution mass spectrometry KW - tandard addition KW - ICP-MS KW - lank characterization KW - Silicon KW - Sulfur KW - Transferrin KW - Tetramethylammonium hydroxide KW - Biodiesel fuel KW - Human serum PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526376 DO - https://doi.org/10.3390/molecules26092649 VL - 26 IS - 9 SP - 2649 PB - MDPI CY - Basel AN - OPUS4-52637 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien T1 - Thermografische Super Resolution mit 2D-strukturierter Erwärmung N2 - Thermografische Super Resolution ermöglicht die Auflösung von Defekten/Inhomogenitäten unterhalb des klassischen Limits, welches durch die Diffusionseigenschaften der thermischen Wellenausbreitung bestimmt wird. Basierend auf einer Kombination aus der Anwendung spezieller Abtaststrategien und einer anschließenden numerischen Optimierungsschritt bei der Datenauswertung hat sich die thermografische Super Resolution bereits bei der Detektion von 1D-Defekten gegenüber den Standard-Thermografieverfahren als überlegen erwiesen. In unserer Arbeit erweitern wir die Möglichkeiten der Methode zur effizienten Detektion und Auflösung von Defektquerschnitten mit einer vollständig 2D-strukturierten Erwärmung. Der experimentelle Ansatz basiert auf einer wiederholten räumlich strukturierten Erwärmung durch einen Hochleistungslaser. In einem zweiten Nachbearbeitungsschritt werden mehrere kohärente Messungen mittels mathematischer Optimierung und unter Ausnutzung der (Joint-) Sparsity der Defekte innerhalb des Prüfkörpers kombiniert. Als Ergebnis kann eine 2D-sparse Defekt-/ Inhomogenitätskarte erhalten werden. Da die Kombination von räumlich strukturierter Erwärmung und anschließender numerischer Kombination mehrerer kohärenter Messungen nicht nur die Auflösung verbessert, sondern auch die Messkomplexität drastisch erhöht, werden verschiedene Scanstrategien untersucht. Abschließend werden die erhaltenen Ergebnisse mit denen konventioneller thermografischer Prüfverfahren verglichen. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Thermography KW - Super-resolution KW - NDT KW - Inspection KW - Image resolution PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526396 UR - https://jahrestagung.dgzfp.de/Programm#P45 AN - OPUS4-52639 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ecke, Alexander T1 - Magnetpartikelbasierte Immunoassays für die Online-Trinkwasseranalytik N2 - Die zunehmende Kontamination von (Trink)-Wasser mit pharmazeutischen Rückständen stellt ein potenzielles Gesundheitsrisiko dar und verlangt nach schnellen und zuverlässigen Analysemethoden. Hierbei können antikörper-basierte Methoden helfen, da sie schnelle und kostengünstige Vor-Ort-Messungen sowie Onlineanalysen ermöglichen. Der Übergang von konventionellen plattenbasierten Formaten, wie ELISA (Enzyme-linked Immunosorbent Assay), zu einem Immunosensor für Online-Messungen wird durch den Einsatz magnetischer Mikropartikel als mobile Messplattform ermöglicht. Die Partikel werden dazu entweder mit dem Antikörper oder dem Analyten gekoppelt. Diese beiden Strategien werden am Beispiel zweier relevanter Kontaminanten des Wassers gezeigt: Diclofenac (DCF) & Amoxicillin (AMX), und sind leicht auf andere Analyten übertragbar. Die magnetpartikelbasierten Assays (MBBAs) weisen niedrigere Nachweisgrenzen, breitere Messbereiche sowie kürzere Analysezeiten als die entsprechenden ELISAs auf und können in einen Immunosensor mit elektrochemischer Detektion auf einem mikrofluidischen Chip integriert werden. T2 - Wasser 2021 CY - Online meeting DA - 10.05.2021 KW - Immunoassay KW - Immunosensor KW - Magnetpartikel KW - Amoxicillin KW - Diclofenac PY - 2021 AN - OPUS4-52640 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Charakterisierung von luftgekoppelten Ultraschallwandlern N2 - Mit dem steigenden Einsatz der luftgekoppelten Ultraschallprüfung steigt auch der Bedarf an verlässlichen Methoden der Charakterisierung der eingesetzten Technik. Mehrere unterschiedliche Verfahren zur Charakterisierung von luftgekoppelten Wandlern und der entsprechenden Gerätetechnik werden verwendet. Prüfkopf-Datenblätter verschiedener Hersteller beinhalten unterschiedliche Prüfkopfparameter, wobei oft eigene Verfahren für die Charakterisierung dieser Prüfköpfe verwendet werden. Diese Vielfalt der Parameter und Verfahren erschwert den potenziellen Kunden den Vergleich zwischen den Prüfköpfen unterschiedlicher Hersteller. Daraus ergibt sich der Bedarf, die Verfahren zur Charakterisierung von luftgekoppelten Ultraschallwandlern zu standardisieren. Vorrangig diese Überlegungen bewegten Hersteller von luftgekoppelten Ultraschallwandlern, Forschungseinrichtungen und Anwender sich zu vernetzen und im Rahmen des Fachausschusses „Ultraschall“ den Unterausschuss „Luftgekoppelte Ultraschallprüfung“ zu gründen. Als erstes Ziel hat sich der Unterausschuss die Erarbeitung einer Richtlinie zur Charakterisierung von luftgekoppelten Ultraschallwandlern gesetzt. Dieser Beitrag ist ein Überblick über viele Methoden zur Charakterisierung von luftgekoppelten Ultraschallwandlern, mit dem Schwerpunkt auf der akustischen Charakterisierung. Zu den wichtigsten Wandlerparametern gehören Empfindlichkeit, Mittenfrequenz, Bandbreite, Fokusgröße und Fokusabstand. Verschiedene Methoden der Schallfeldvermessung werden untereinander verglichen. Diese Überlegungen bieten den Ausgangspunkt für spätere Arbeit an einer Richtlinie zur Charakterisierung von luftgekoppelten Ultraschallwandlern. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Luftgekoppelte Ultraschallprüfung KW - Richtlinie KW - Ultraschallwandler KW - Charakterisierung PY - 2021 AN - OPUS4-52642 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gautzsch, T. T1 - Luftgekoppelte Ultraschallprüfung, eine Alternative in der zerstörungsfreien Prüfung N2 - Die luftgekoppelte Ultraschallprüfung (ACUT) ist ein vielfach bewährtes zerstörungsfreies Prüfverfahren, welches von vielen Anwendern jedoch nur am Rande oder gar nicht wahrgenommen wird. Insbesondere, die nach wie vor in der Ultraschallausbildung gelehrten Theorien zur wellenlängenabhängigen minimalen detektierbaren Fehlergröße und die vermeintliche Notwendigkeit der Verwendung von Koppelmittel schrecken viele potentielle Anwender davon ab für ihr Prüfproblem ACUT in Betracht zu ziehen. Des Weiteren wird ACUT häufig nicht als eigenständiges Prüfverfahren erkannt, sodass versucht wird, flüssigkeitsgekoppelte Ultraschallprüfungen ohne Beachtung der Besonderheiten zu ersetzen. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Luftgekoppelte Ultraschallprüfung PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526431 UR - https://jahrestagung.dgzfp.de/Programm#P53 AN - OPUS4-52643 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Testing of Gas and Humidity Sensors N2 - The testing of gas and humidity sensors is essential for the application of sensing devices. The testing determines properties of an investigated humidity sensor or gas sensor. In testing, the sensor property is the observed response of a sensing system to an input stimulus in comparison to a reference within a test procedure. This tutorial is structured into six chapters. The first chapter is about basics of hygrometry and gas sensing. It includes definitions, sensor classification, overview of application categories, as well as construction and functional principles. The chapter on requirements of deployed sensors focus on stability, response time, cross-sensitivity, electrical and mechanical requirements, and other. The sensing performance is characterised by determinations of parameters like accuracy, repeatability, detection limits (low and high), and response/recovery time. The description of testing signals on specified qualitative and quantitative characteristics, and the adequately estimated measurement uncertainty is the content of the analysis chapter. All chapters contain examples of testing procedures from testing/calibration labs for hygrometers and gas sensors which are essential for implementation into quality management systems. T2 - SMSI 2021 - Sensor and Measurement Science International CY - Online m DA - 03.05.2021 KW - Testing KW - Gas sensor KW - Humidity sensor KW - Tutorial KW - Multi-gas sensor PY - 2021 UR - https://www.smsi-conference.com/tutorials-2/ AN - OPUS4-52645 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Held, Mathias T1 - Inverse determination of elastic material parameters from ultrasonic guided waves dispersion measurements using Convolutional Neuronal Networks N2 - This presentation shows how the dispersive behavior of ultrasonic guided waves in isotropic materials can be used by means of Convolutional Neural Networks to determine the elastic parameters. For this purpose, the preprocessing, the training, the chosen architecture and the results are evaluated on the basis synthetic image data. This presentation was given at the SMSI 2021. T2 - SMSI 2021 2021-05-03 - 2021-05-06 digital CY - Online Meeting DA - 03.05.2021 KW - Guided waves KW - Inverse Probleme KW - Materialcharakterisierung KW - Convolutional Neuronal Networks KW - Dispersion PY - 2021 AN - OPUS4-52625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moufid, M. A1 - Bouchikhi, B. A1 - Tiebe, Carlo A1 - Bartholmai, Matthias A1 - El Bari, N. T1 - Assessment of outdoor odor emissions from polluted sites using simultaneous thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS), electronic nose in conjunction with advanced multivariate statistical approaches N2 - Poor air quality, particularly in urban areas, causes various diseases and degrades living standards. Air Quality could be affected by emissions of odor, Volatile Organic Compounds (VOCs), and other gases. Therefore, assessment and monitoring of odorous air quality using sensitive, simple, rapid, accurate and portable tools is very important for public health. This study aimed to characterize odor emissions to detect malfunctions in facilities and to prevent air pollution and olfactory nuisance in the environment. A gas chromatographic method, in conjunction with sensorial analysis were performed for odorous air samples analysis collected from neighborhood of Meknes city (Morocco). Advanced multivariate statistical approaches, such as Principal Components Analysis (PCA), Discriminant Function Analysis (DFA), Support Vector Machines (SVMs), and Hierarchical Cluster Analysis (HCA), were used to describe samples similarities. The electronic nose (e-nose) data processing exhibits a satisfactory discrimination between the odorous air samples. Twenty-four VOCs with known molecular formulas were identified with Thermal Desorption-Gas Chromatography-Mass Spectrometry (TD-GC-MS). A validated Partial Least Square (PLS) model foresees good calibration between e-nose measurement and TD-GCMS analysis. The finding indicates that TD-GC–MS approach in conjunction with e-nose unit could be suitable tool for environmental measurement-based odor emissions. KW - Electronic nose KW - TD-GC-MS KW - PLS regression KW - Multivariate analysis KW - Outdoor odor emissions PY - 2021 DO - https://doi.org/10.1016/j.atmosenv.2021.118449 SN - 1352-2310 VL - 256 SP - 118449 PB - Elsevier Ltd. AN - OPUS4-52626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Even, Morgane T1 - Formaldehydemissionen aus Holzspielzeug: Methodenvergleich und Expositionsabschätzung N2 - Formaldehyd gilt als krebserregend und wird von Spanplatten und Sperrholz emittiert, die bei der Spielzeugherstellung verwendet werden. Die Untersuchungsänter benötigen eine wirtschaftliche und zuverlässige Methode. Die Anwendung miniaturisierter Emissionsprüfkammern wurde getestet und mit größeren Emissionsprüfkammern und die Flaschenmethode verglichen. Eine Expositionsabschätzung wird auch vorgestellt. T2 - 28. WaBoLu-Innenraumtage CY - Online Meeting DA - 10.05.2021 KW - Formaldehyd KW - Emission KW - Spielzeug KW - Methoden PY - 2021 AN - OPUS4-52628 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter T1 - Partikelbasierte Multianalyt- Fluoreszenzimmunoassays für die Unweltanalytik und Biotechnologie N2 - Zur Beurteilung der Wasserqualität können Markersubstanzen, wie Carbamazepin, Diclofenac, Koffein und Gallensäuren, verwendet werden. Erhöhte Konzentrationen dieser anthropogenen Marker weisen auf Einleitstellen von Abwasser hin und zeigen somit an, wo Gewässer verschmutzt werden. Diese Arbeit beschreibt deshalb die Etablierung, Optimierung und Validierung eines partikelbasierten Suspensionsarray Fluoreszenzimmunoassays (SAFIA), mit dem diese Substanzen gleichzeitig und parallel in vielen Proben quantitativ bestimmt werden können. Für SAFIA wurde das Format des kompetitiven indirekten Immunoassays gewählt. Als Plattform wurden fluoreszenzintensitätscodierte Polystyrol-Kern/Siliziumdioxid-Schale-Partikel, auf deren Oberfläche Haptene als kompetitive Bindungsstellen für Antikörper immobilisiert wurden, verwendet. Hier zeigte sich, dass eine selektive Erkennung der Haptenstruktur auf der Oberfläche der Partikel durch die Antikörper nur gegeben war, wenn die Partikel zusätzlich mit Polyethylenglykolgruppen funktionalisiert wurden. Zum Auslesen des Fluoreszenzsignals wurde ein Durchflusszytometer verwendet. Kompatibilität mit der Durchführung in Mikrotiterplatten wurde erreicht, indem eine Stopp-lösung für den SAFIA, basierend auf Formaldehyd, entwickelt wurde. Nach der Optimierung der Assayparameter können die oben genannten vier Analyten gleichzeitig in einer Probe mindestens bis zu einer Konzentration von 0.3 μg L-1 nachgewiesen werden. Der Assay kann ohne Wasch-schritte ausgeführt werden und ist somit einfacher als konventionelle Immunoassays, wie z. B. ELISA. Der SAFIA wurde hinsichtlich Interferenzen und Selektivität untersucht. Dabei zeigte sich, dass Matrixbestandteile, die in wässrigen Umweltproben vorkommen, keinen bzw. nur einen ge-ringen Einfluss auf den SAFIA hatten. Im simulierten Umweltscreening eines Flusses und mithilfe der Analyse von Abwasserproben wurde SAFIA validiert; hier zeigte SAFIA eine mit ELISA vergleich-bare Genauigkeit, bei gleichzeitiger Senkung der Analysenzeit und -kosten. Die gleichzeitige Detektion mehrerer anthropogener Marker erlaubte zudem Rückschlüsse auf die Art von Verschmutzungsquellen, im Gegensatz zu ELISA, mit dem nur ein Analyt bestimmt werden kann. Da hochaffine Antikörper für Immunoassays essenziell sind, wurde ein SAFIA zum Screening antikörperproduzierenden Zellen (Hybridomzellen) entwickelt und eingesetzt. Durch die Implementierung eines Sandwichimmunoassays zur IgG Bestimmung und durch Verwendung von homo- und heterologen Haptenstrukturen konnten aus einem Pool von Hybridomzellen diejenigen ausgewählt werden, deren sekretierter Antikörper die geringsten Nachweisgrenzen im Immunoassay erlauben. Damit konnte das Anwendungsspektrum des SAFIA maßgeblich vergrößert werden. Er vereinfacht als biotechnologisches Werkzeug stark sowohl die Produktion von monoklonalen Antikörpern als auch die Analyse von Umweltproben. T2 - Wasser 2021 Jahrestagung der Wasserchemischen Gesellschaft CY - Online Meeting DA - 10.05.2021 KW - SAFIA KW - Anthropogene Marker KW - Immunoassay KW - Partikel KW - Isolithocholsäure KW - Screening KW - Carbamazepin KW - Diclofenac KW - Coffein PY - 2021 AN - OPUS4-52629 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Validierung von ZfP-Verfahren für die Nachrechnung von Brücken N2 - Vortrag über die Bewertung der Zuverlässigkeit von bestehenden Brücken mit gezielt am Bauwerk erhobenen ZfP-Ergebnissen im Rahmen der Verleihung des DGZfP-Nachwuchspreises 2021 auf der Jahrestagung der DGZfP. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Zuverlässigkeit KW - Messunsicherheit KW - Reliability assessment KW - Existing structures PY - 2021 AN - OPUS4-52630 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Meyer, A. A1 - Falkenhagen, Jana A1 - Kricheldorf, H. R. T1 - SnOct2-catalyzed and alcohol-initiated ROPs of L-lactide – About the influence of initiators on chemical reactions in the melt and the solid state N2 - SnOct2 (Sn(II) 2-ethylhexanoate) catalyzed ROPs of L-lactide were performed in bulk with eight different alcohols as initiators. The time was varied between 1 h and 24 h for all initiators. For two initiators the temperature was also lowered to 115 ◦C. Even-numbered chains were predominantly formed in all polymerizations at short times, but the rate of transesterification (e.g. even/odd equilibration) and the molecular weight distribution were found to depend significantly on the nature of the initiator. Observed transesterification reactions also continued in solid poly (L-lactide), and with the most active initiator, almost total equilibration was achieved even at 130 ◦C. This means that all chains including those of the crystallites were involved in transesterification reactions proceeding across the flat surfaces of the crystallites. The more or less equilibrated crystalline polylactides were characterized by DSC and SAXS measurements with regard to their melting temperature (Tm), crystallinity and crystal thickness. KW - Polylactide KW - MALDI-TOF MS KW - Crystallization KW - Catalysts KW - SAXS PY - 2021 DO - https://doi.org/10.1016/j.eurpolymj.2021.110508 VL - 153 SP - 110508 PB - Elsevier Ltd. AN - OPUS4-52633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zeipert, H. A1 - Claes, L. A1 - Johannesmann, S. A1 - Webersen, M. A1 - Lugovtsova, Yevgeniya A1 - Prager, Jens A1 - Henning, B. T1 - Measurement and simulation of Lamb waves in adhesive-bonded multilayer systems N2 - Lamb waves are a common tool in the field of non-destructive testing and are widely used for materialcharacterisation. Further, the increasing computational capability of modern systems enables the Simulation of complex and detailed material models. This work demonstrates the possibility of simulating an adhesive-bonded multilayer system by characterising each layer individually, and introduces an Approach for determining the dispersive behaviour of acoustic waves in a multilayer system via real measurements. T2 - SMSI 2021 Conference – Sensor and Measurement Science International CY - Online meeting DA - 03.05.2021 KW - Adhesive bonds KW - Lamb waves KW - Elastic constants KW - Non-Destructive Testing KW - Ultrasound PY - 2021 DO - https://doi.org/10.5162/SMSI2021/A8.2 SP - 91 EP - 92 AN - OPUS4-52634 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zeipert, H. T1 - Measurement and simulation of Lamb waves in adhesive-bonded multilayer systems N2 - Lamb waves are a common tool in the field of non-destructive testing and are widely used for material characterisation. Further, the increasing computational capability of modern systems enables the Simulation of complex and detailed material models. This work demonstrates the possibility of simulating an adhesive-bonded multilayer system by characterising each layer individually, and introduces an Approach for determining the dispersive behaviour of acoustic waves in a multilayer system via real measurements. T2 - SMSI 2021 Conference – Sensor and Measurement Science International CY - Online meeting DA - 03.05.2021 KW - Adhesive bonds KW - Lamb waves KW - Elastic constants KW - Non-Destructive Testing KW - Ultrasound PY - 2021 AN - OPUS4-52635 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - Elemental analytical methods in material- & environmental analysis N2 - Materials in contact with the environment release e.g., metal-ions, elemental species and/or (nano-)particles. Once these species and/or particles are released, they are ingested by organisms and cells and thus, might have a negative impact on the environment. Thus, identification as well as quantification of potentially harmful substances is of utmost importance and highly needed to assess ecotoxicological impact of (emerging) pollutants. The oral presentation provides an overview on the power of elemental analytical techniques, in particular: ICP-MS as well as HR-CS-GFMAS in environmental research. Current research topics will be highlighted: i) Elemental Speciation analysis of anti-fouling agents via CE/MC-ICP-MS; ii) Per- and polyfluorinated compounds in surface waters via high resolution-continuum source-graphite furnace molecular absorption spectroscopy (HR-CS-GFMAS); iii) Single cell and single organism analysis via sc-ICP-ToF-MS and ETV/ICP-MS for ecotoxicological assessment. T2 - Analytical Colloquium at MERCK CY - Online meeting DA - 19.04.2021 KW - HR-CS-GFMAS KW - ICP-ToF-MS KW - ETV/ICP-MS PY - 2021 AN - OPUS4-52566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiesner, Yosri A1 - Altmann, Korinna A1 - Braun, U. T1 - Determination of Microplastic Mass Content by Thermal Extraction Desorption Gas Chromatography– Mass Spectrometry N2 - The scientific and practical challenge of detecting microplastics (MPs) in the environment in a targeted and rapid manner is solved by innovative coupling of thermogravimetric analysis with mass spectrometric methods. Fast identification and quantitative determination of most thermoplastic polymers and elastomers is possible by using thermal extraction Desorption gas chromatography–mass spectrometry (TED-GC–MS). KW - Microplastics KW - Mikroplastik KW - TED-GC/MS KW - Microplastics analytic KW - Mikroplastik Massegehalt PY - 2021 VL - 17 IS - 3 SP - 2 EP - 7 PB - MultiMedia (UK) LLC CY - Cranbury AN - OPUS4-52570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shipov, A. A1 - Zaslansky, P. A1 - Riesemeier, Heinrich A1 - Segev, G. A1 - Atkins, A. A1 - Kalish-Achrai, N. A1 - Weiner, S. A1 - Shahar, R. T1 - The influence of estrogen deficiency on the structural and mechanical properties of rat cortical bone N2 - Background. Post-menopausal osteoporosis is a common health problem worldwide, most commonly caused by estrogen deficiency. Most of the information regarding the skeletal effects of this disease relates to trabecular bone, while cortical bone is less studied. The purpose of this study was to evaluate the influence of estrogen deficiency on the structure and mechanical properties of cortical bone. Methods. Eight ovariectomized (OVH) and eight intact (control) Sprague Dawley rats were used. Structural features of femoral cortical bone were studied by light microscopy, scanning electron microscopy and synchrotron-based microcomputer-tomography and their mechanical properties determined by nano-indentation. Results. Cortical bone of both study groups contains two distinct regions: organized circumferential lamellae and disordered bone with highly mineralized cartilaginous islands. Lacunar volume was lower in the OVH group both in the lamellar and disorganized regions (182 ± 75 µm3 vs 232 ± 106 µm3 , P < 0.001 and 195 ± 86 µm3 vs. 247 ± 106 µm3 , P < 0.001, respectively). Lacunar density was also lower in both bone regions of the OVH group (40 ± 18 ×103 lacunae/mm3 vs. 47 ± 9×103 lacunae/mm3 in the lamellar region, P = 0.003 and 63 ± 18×103 lacunae/mm3 vs. 75 ± 13×103 lacunae/mm3 in the disorganized region, P < 0.001). Vascular canal volume was lower in the disorganized region of the bone in the OVH group compared to the same Region in the control group (P < 0.001). Indentation moduli were not different between the study groups in both bone regions. Discussion. Changes to cortical bone associated with estrogen deficiency in rats require high-resolution methods for detection. Caution is required in the application of These results to humans due to major structural differences between human and rat bone. KW - Estrogen KW - Disorganized bone KW - Rat KW - Lacunae KW - Ovariectomy PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520798 DO - https://doi.org/10.7717/peerj.10213 VL - 9 SP - e10213 AN - OPUS4-52079 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - ROP of L-lactide and ε-caprolactone catalyzed by tin(ii) and tin(iv) acetates–switching from COOH terminated linear chains to cycles N2 - The catalytic potential of tin(II)acetate, tin(IV)acetate, dibutyltin-bis-acetate and dioctyl tin-bis-acetate was compared based on polymerizations of L-lactide conducted in bulk at 160 or 130C. With SnAc2 low-Lac/Cat ratios (15/1–50/1) were studied and linear chains having one acetate and one carboxyl end group almost free of cyclics were obtained. Higher monomer/catalyst ratios and lower temperatures favored formation of cycles that reached weight average molecular weights (Mw's) between 100,000 and 2,500,000. SnAc4 yielded mixtures of cycles and linear species under all reaction conditions. Dibutyltin- and dioctyl tin bis-acetate yielded cyclic polylactides under most reaction conditions with Mw's in the range of 20,000–80,000. Ring-opening polymerizations performed with ε-caprolactone showed similar trends, but the formation of COOH-terminated linear chains was significantly more favored compared to analogous experiments with lactide. The reactivity of the acetate catalysts decreased in the following order: SnAc2> SnAc4>Bu2SnAc2 Oct2SnAc2. KW - Catalyst KW - MALDI-TOF MS KW - Ring-opening polymerization KW - Tin acetates KW - Polylactide PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520831 DO - https://doi.org/10.1002/pol.20200866 SP - 1 EP - 12 PB - Wiley Online Library AN - OPUS4-52083 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lai, W. W.L. A1 - Chang, R.K.W. A1 - Völker, Christoph A1 - Cheung, B. W.Y. T1 - GPR wave dispersion for material characterization N2 - This paper studies the dispersion of GPR wave’s phase velocity at different wideband frequencies in plywood and concrete with varying moisture content. This study makes use of two GPR antennas with 2 GHz centre frequency operating in wide angle reflection and refraction (WARR) mode and with computation of spectral analysis of the surface wave (SASW). Computation of phase velocities is based on the Acquisition of the cross-power spectrum and phase unwrap of two distorted ground waves at positions Closer to and farther away from the transmitting antenna. The velocities of the ground waves are found to experience greater dispersion in low frequency regimes within the effective frequency bandwidths determined and thresholded by time–frequency analysis (TFA) and coherence plotting of the ground waves. This study validates not only the methodology, but also identifies the optimal distance between the first (Rx1) and second (Rx2) receivers as k/2, which is based on a fixed transmitter (Tx) minus the first Receiver (Rx1) distance. It serves as an indication of changeable separation distance when other lower frequency GPR is used because the distances of Tx-Rx1 and Rx1-Rx2 are wavelength dependent and thus also frequency dependent. Effects of moisture contents and chloride contamination in concrete were also characterized according to the dispersion plots . that wave traelling in lower frequencies in GPR wave is much decelerated than that in higher frequencies. This research also contributes to the building of the ‘‘GPRWARR machine” suggested in Annan and Jackson (2017) [1], within which the effects of wave Dispersion on phase velocity can be inversely modelled to characterize variations in the material properties of infrastructure as a means of detecting surface damage. KW - Ground penetrating radar KW - Wide angle reflection and refraction PY - 2021 DO - https://doi.org/10.1016/j.conbuildmat.2021.122597 SN - 0950-0618 VL - 282 SP - 122597 PB - Elsevier Ltd. AN - OPUS4-52197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Anzt, H. A1 - Bach, F. A1 - Druskat, S. A1 - Löffler, F. A1 - Loewe, A. A1 - Renard, B. Y. A1 - Seemann, G. A1 - Struck, A. A1 - Achhammer, E. A1 - Aggarwal, P. A1 - Appel, F. A1 - Bader, M. A1 - Brusch, L. A1 - Busse, C. A1 - Chourdakis, G. A1 - Dabrowski, P. W. A1 - Ebert, P. A1 - Flemisch, B. A1 - Friedl, S. A1 - Fritzsch, B. A1 - Funk, M. D. A1 - Gast, V. A1 - Goth, F. A1 - Grad, J. A1 - Hegewald, J. A1 - Hermann, S. A1 - Hohmann, F. A1 - Janosch, S. A1 - Kutra, D. A1 - Linxweiler, J. A1 - Muth, Thilo A1 - Peters-Kottig, W. A1 - Rack, F. A1 - Raters, F. H. C. A1 - Rave, S. A1 - Reina, G. A1 - Reißig, M. A1 - Ropinski, T. A1 - Schaarschmidt, J. A1 - Seibold, H. A1 - Thiele, J. P. A1 - Uekermann, B. A1 - Unger, S. A1 - Weeber, R. T1 - An environment for sustainable research software in Germany and beyond: current state, open challenges, and call for action N2 - Research software has become a central asset in academic research. It optimizes existing and enables new research methods, implements and embeds research knowledge, and constitutes an essential research product in itself. Research software must be sustainable in order to understand, replicate, reproduce, and build upon existing research or conduct new research effectively. In other words, software must be available, discoverable, usable, and adaptable to new needs, both now and in the future. Research software therefore requires an environment that supports sustainability. Hence, a change is needed in the way research software development and maintenance are currently motivated, incentivized, funded, structurally and infrastructurally supported, and legally treated. Failing to do so will threaten the quality and validity of research. In this paper, we identify challenges for research software sustainability in Germany and beyond, in terms of motivation, selection, research software engineering personnel, funding, infrastructure, and legal aspects. Besides researchers, we specifically address political and academic decision-makers to increase awareness of the importance and needs of sustainable research software practices. In particular, we recommend strategies and measures to create an environment for sustainable research software, with the ultimate goal to ensure that software-driven research is valid, reproducible and sustainable, and that software is recognized as a first class citizen in research. This paper is the outcome of two workshops run in Germany in 2019, at deRSE19 - the first International Conference of Research Software Engineers in Germany - and a dedicated DFG-supported follow-up workshop in Berlin. KW - Research Software KW - Sustainable Software Development KW - Academic Software KW - Software Infrastructure KW - Software Training KW - Software Licensing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522029 DO - https://doi.org/10.12688/f1000research.23224.2 VL - 9 SP - 1 EP - 35 AN - OPUS4-52202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pech, S. A1 - Rehberg, M. A1 - Janke, R. A1 - Benndorf, D. A1 - Genzel, Y. A1 - Muth, Thilo A1 - Sickmann, A. A1 - Rapp, E. A1 - Reichl, U. T1 - Tracking changes in adaptation to suspension growth for MDCK cells: cell growth correlates with levels of metabolites, enzymes and proteins N2 - Adaptations of animal cells to growth in suspension culture concern in particular viral vaccine production, where very specific aspects of virus-host cell interaction need to be taken into account to achieve high cell specific yields and overall process productivity. So far, the complexity of alterations on the metabolism, enzyme, and proteome level required for adaptation is only poorly understood. In this study, for the first time, we combined several complex analytical approaches with the aim to track cellular changes on different levels and to unravel interconnections and correlations. Therefore, a Madin-Darby canine kidney (MDCK) suspension cell line, adapted earlier to growth in suspension, was cultivated in a 1-L bioreactor. Cell concentrations and cell volumes, extracellular metabolite concentrations, and intracellular enzyme activities were determined. The experimental data set was used as the input for a segregated growth model that was already applied to describe the growth dynamics of the parental adherent cell line. In addition, the cellular proteome was analyzed by liquid chromatography coupled to tandem mass spectrometry using a label-free protein quantification method to unravel altered cellular processes for the suspension and the adherent cell line. Four regulatory mechanisms were identified as a response of the adaptation of adherent MDCK cells to growth in suspension. These regulatory mechanisms were linked to the proteins caveolin, cadherin-1, and pirin. Combining cell, metabolite, enzyme, and protein measurements with mathematical modeling generated a more holistic view on cellular processes involved in the adaptation of an adherent cell line to suspension growth. KW - MDCK cell KW - Proteome KW - Metabolism KW - Enzyme activity KW - Suspension growth PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522070 DO - https://doi.org/10.1007/s00253-021-11150-z VL - 105 IS - 5 SP - 1861 EP - 1874 PB - Springer AN - OPUS4-52207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kling e Silva, L. A1 - Almeida, G. A1 - Kadoke, Daniel A1 - Daum, Werner A1 - Ribeiro Pereira, G. T1 - Automation of pipe defect detection and characterization by structured light N2 - High quality tubular products are essential to the oil and gas industry. Quality control during their production focuses on the non-destructive detection of surface defects. The structured light technique is a candidate for the challenge to detect, monitor and evaluate such defects in real-time. In the present study the automatic processing of structured light measurements is performed and validated. The algorithm for the automatic Analysis of inspection data has an advantage over current data evaluation methods based on individual assessments of operators. KW - Non-destructive testing KW - Data processing KW - Defect evaluation KW - Materials evaluation KW - Structured light scanning (SLS) PY - 2021 DO - https://doi.org/10.1515/mt-2020-0008 SN - 0033-8230 VL - 63 IS - 1 SP - 55 EP - 61 PB - Walter de Gruyter GmbH CY - Berlin/ Boston AN - OPUS4-52124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frisch, M. A1 - Laun, J. A1 - Marquardt, Julien A1 - Arinchtein, A. A1 - Bauerfeind, K. A1 - Bernsmeier, D. A1 - Bernicke, M. A1 - Bredow, T. A1 - Kraehnert, R. T1 - Bridging experiment and theory: enhancing the electrical conductivities of soft-templated niobium-doped mesoporous titania films† N2 - Theoretical calculations suggest a strong dependence of electrical conductivity and doping concentration in transition-metal doped titania. Herein, we present a combined theoretical and experimental approach for the prediction of relative phase stability and electrical conductivity in niobium-doped titania as model system. Our method paves the way towards the development of materials with improved electrical properties. KW - Electrical conductivity KW - Prediction relative KW - Transition-metal doped KW - System method PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521371 DO - https://doi.org/10.1039/d0cp06544g SN - 1463-9084 VL - 23 IS - 5 SP - 3219 EP - 3224 PB - Royal Society of Chemistry AN - OPUS4-52137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Z. A1 - Kneipp, Janina T1 - Ligand-Supported Hot Electron Harvesting: Revisiting the pHResponsive Surface-Enhanced Raman Scattering Spectrum of p‑Aminothiophenol N2 - The discussion of the surface-enhanced Raman scattering (SERS) spectra of p-aminothiophenol (PATP) and of ist photocatalytic reaction product 4,4′-dimercaptoazobenzene (DMAB) is important for understanding plasmon-supported spectroscopy and catalysis. Here, SERS spectra indicate that DMAB forms also in a nonphotocatalytic reaction on silver nanoparticles. Spectra measured at low pH, in the presence of the acids HCl, H2SO4, HNO3, and H3PO4, show that DMAB is reduced to PATP when both protons and chloride ions are present. Moreover, the successful reduction of DMAB in the presence of other, halide and nonhalide, ligands suggests a central role of these species in the reduction. As discussed, the ligands increase the efficiency of hot-electron harvesting. The pH-associated reversibility of the SERS spectrum of PATP is established as an Observation of the DMAB dimer at high pH and of PATP as a product of its hot-electron reduction at low pH, in the presence of the appropriate ligand. KW - Redox reactions KW - Metal nanoparticles KW - Ligands KW - Raman spectroscopy KW - Nanoparticle formation PY - 2021 DO - https://doi.org/10.1021/acs.jpclett.0c03732 SN - 1948-7185 VL - 12 IS - 5 SP - 1542 EP - 1547 PB - ACS Publications AN - OPUS4-52140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Ochratoxin A detection by an immunomagnetic assay and smartphone-based amperometry N2 - The demand for miniaturized analytical devices monitoring important parameters in the food and medical industry has increased strongly in the past decades. With fast progress, smart technologies are finding their way into our everyday life. For the future, it is, therefore, a major goal to also link analytical methods with smart technologies to create user-friendly on-site devices. In food industry the monitoring of harmful substances such as dioxins, heavy metals or mycotoxins plays a key role, since the European Commission prescribes legal limits for various food products and beverages. Therefore, companies often have their own laboratories and trained personnel. For one of the most abundant and toxic mycotoxins, Ochratoxin A (OTA) we want to present an electrochemical detection system in which the read-out can be performed with a smartphone connected via Bluetooth to a miniaturized potentiostat. The recognition of OTA is performed with specific antibodies in a competitive assay format. Anti-OTA-antibodies were captured on magnetic beads on which the competitive binding between OTA and an OTA horseradish peroxidase (HRP) tracer was performed. To quantify OTA, the enzymatic reaction of the tracer with 3,3′,5,5′-tetramethylbenzidine (TMB) and H2O2 is employed. Oxidized TMB, which is enzymatically produced by the reduction of H2O2, is quantified by amperometry with screen-printed electrodes in a custom-made flow system. Since it is well-known that oxidized TMB can precipitate on electrode surfaces, we have studied pitfalls of the electrochemical detection of TMB. By cyclic voltammetry we have compared the stability of the electrochemistry of TMB at different electrode materials (gold and carbon) and pH values (pH 1 and pH 4). It was found that a stable response of the electrode could be achieved at pH 1 on gold electrodes. Thus, we applied these reaction conditions for amperometric detection of TMB in the OTA assay. The results of the electrochemical detection method are in good correlation with the photometric detection of TMB. To demonstrate the applicability, we tested our system with OTA-spiked beer and performed the measurement via smartphone. T2 - Rapid Methods Europe CY - Online meeting DA - 01.02.2021 KW - Ochratoxin A KW - Cyclic voltammetry KW - Amperometry KW - Smartphone KW - Electrochemistry PY - 2021 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-52095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Melzer, Michael T1 - Seminar about the expression of uncertainty in measurement N2 - The evaluation of measurement uncertainty is essential for testing and calibration laboratories. This paper provides a general process description for the determination of the measurement uncertainty of quantitative data and its application to the conformity assessment with examples, and how to deal with the uncertainty of qualitative (Boolean) results, e. g. when "Alarm" or "No alarm" occours in an instrument display. T2 - GW4SHM - 1st Training Event CY - Online meeting DA - 23.11.2020 KW - Uncertainty KW - Conformity assessment KW - Boolean results PY - 2020 AN - OPUS4-52040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rühle, Bastian A1 - Krumrey, Julian Frederic A1 - Hodoroaba, Vasile-Dan T1 - Dataset accompanying the publication "Workflow towards automated segmentation of agglomerated, non-spherical particles from electron microscopy images using artificial neural networks" N2 - This dataset accompanies the following publication, first published in Scientific Reports (www.nature.com/articles/s41598-021-84287-6): B. Ruehle, J. Krumrey, V.-D. Hodoroaba, Scientific Reports, Workflow towards Automated Segmentation of Agglomerated, Non-Spherical Particles from Electron Microscopy Images using Artificial Neural Networks, DOI: 10.1038/s41598-021-84287-6 It contains electron microscopy micrographs of TiO2 particles, the corresponding segmentation masks, and their classifications into different categories depending on their visibility/occlusion. Please refer to the publication and its supporting information for more details on the acquisition and contents of the dataset, as well as the GitHub repository at https://github.com/BAMresearch/automatic-sem-image-segmentation KW - Electron microscopy KW - Neural networks KW - Image segmentation KW - Automated image analysis PY - 2021 DO - https://doi.org/10.5281/zenodo.4563942 PB - Zenodo CY - Geneva AN - OPUS4-52246 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Essig, W. A1 - Bernhardt, Y. A1 - Döring, D. A1 - Solodov, I. A1 - Gautzsch, T. A1 - Gaal, Mate A1 - Hufschläger, Daniel A1 - Sommerhuber, R. A1 - Marhenke, T. A1 - Hasener, J. A1 - Szewieczek, A. A1 - Hillger, W. T1 - Air-coupled ultrasound - emerging NDT method N2 - This paper deals with the state of the art of air-coupled ultrasonic testing. KW - Air-coupled KW - Ultrasonic testing KW - Transducers PY - 2021 SN - 1616-069X VL - 173 SP - 32 EP - 43 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-52231 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weller, Michael G. T1 - The Protocol Gap N2 - Although peer review is considered one of the main pillars of modern science, experimental methods and protocols seem to be not a rigorous subject of this process in many papers. Commercial equipment, test kits, labeling kits, previously published concepts, and standard protocols are often considered to be not worth a detailed description or validation. Even more disturbing is the extremely biased citation behavior in this context, which sometimes leads to surrogate citations to avoid low-impact journals, preprints, or to indicate traditional practices. This article describes some of these surprising habits and suggests some measures to avoid the most unpleasant effects, which in the long term may undermine the credibility of science as a whole. KW - Validation KW - Peer review KW - Experiment KW - Documentation KW - Scientific publication KW - Reproducibility crisis KW - Replication crisis KW - Trust KW - Citation KW - References KW - Surrogate citations KW - Impact PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521440 DO - https://doi.org/10.3390/mps4010012 SN - 2409-9279 VL - 4 IS - 1 SP - 1 EP - 5 PB - MDPI CY - Basel AN - OPUS4-52144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Paul, Martin A1 - Tannenberg, Robert A1 - Tscheuschner, Georg A1 - Ponader, Marco A1 - Weller, Michael G. T1 - Cocaine detection by a laser-induced immunofluorometric biosensor N2 - The trafficking of illegal drugs by criminal networks at borders, harbors, or airports is an increasing issue in public health as these routes ensure the main supply of illegal drugs. The prevention of drug smuggling, including the installation of scanners and other analytical devices to detect ultra-small traces of drugs within a reasonable time frame, remains a challenge. The presented immunosensor is based on a monolithic affinity column with a large excess of immobilized hapten, which traps fluorescently labeled antibodies as long as the analyte cocaine is absent. In the presence of the drug, some binding sites of the antibody will be blocked, which leads to an immediate breakthrough of the labeled protein, detectable by highly sensitive laser-induced fluorescence with the help of a Peltier-cooled complementary metal-oxide-semiconductor (CMOS) camera. Liquid handling is performed with high-precision syringe pumps and microfluidic chip-based mixing devices and flow cells. The biosensor achieved limits of detection of 23 pM (7 ppt) of cocaine with a response time of 90 seconds and a total assay time below 3 minutes. With surface wipe sampling, the biosensor was able to detect 300 pg of cocaine. This immunosensor belongs to the most sensitive and fastest detectors for cocaine and offers near-continuous analyte measurement. KW - Drug search KW - Customs KW - Confiscation KW - Border surveillance KW - Narcotics KW - International drug trade KW - Drug trafficking KW - Illicit drug KW - Immunosensor KW - Antibodies KW - Detection PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529951 DO - https://doi.org/10.20944/preprints202107.0521.v1 SN - 2310-287X N1 - Geburtsname von Ponader, Marco: Wilke, M. - Birth name of Ponader, Marco: Wilke, M. SP - 1 PB - MDPI CY - Basel AN - OPUS4-52995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Faßbender, Sebastian A1 - von der Au, Marcus A1 - Koenig, Maren A1 - Pelzer, J. A1 - Piechotta, Christian A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Species-specific isotope dilution analysis of monomethylmercury in sediment using GC/ICP-ToF-MS and comparison with ICP-Q-MS and ICP-SF-MS N2 - A recently introduced inductively coupled plasma-time-of-flight-mass spectrometer (ICP-ToF-MS) shows enhanced sensitivity compared to previous developments and superior isotope ratio precision compared to other ToF and commonly used single-collector ICP-MS instruments. Following this fact, an improvement for isotope dilution ICP-MS using the new instrumentation has been reported. This study aimed at investigating whether this improvement also meets the requirements of species-specific isotope dilution using GC/ICP-MS, where short transient signals are recorded. The results of the analysis of monomethylmercury (MMHg) of a sediment reference material show that isotope ratio precision of ICP-MS instruments equipped with quadrupole, sector-field, and time-of-flight mass analyzers is similar within a broad range of peak signal-to-noise ratio when analyzing one isotopic system. The procedural limit of quantification (LOQ) for MMHg, expressed as mass fraction of Hg being present as MMHg, w(Hg)MMHg, was similar as well for all investigated instruments and ranged between 0.003 and 0.016 μg/kg. Due to the simultaneous detection capability, the ICP-ToF-MS might, however, be more favorable when several isotopic systems are analyzed within one measurement. In a case study, the GC/ICP-ToF-MS coupling was applied for analysis of MMHg in sediments of Finow Canal, a historic German canal heavily polluted with mercury. Mass fractions between 0.180 and 41 μg/kg (w(Hg)MMHg) for MMHg, and 0.056 and 126 mg/kg (w(Hg)total) for total mercury were found in sediment samples taken from the canal upstream and downstream of a former chemical plant. KW - Methylmercury KW - Legacy pollution KW - Finow Canal KW - Isotope dilution KW - Mercury speciation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529967 DO - https://doi.org/10.1007/s00216-021-03497-z SN - 1618-2642 VL - 413 IS - 21 SP - 5279 EP - 5289 PB - Springer CY - Berlin AN - OPUS4-52996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - The triple isotope calibration approach BT - A new calibration approach for obtaining absolute isotope ratios of multi-isotopic elements N2 - The calibration of isotope ratio measurements is an ongoing challenge since instrumental isotope fractionation (IIF) has been detected in mass spectrometry (MS). There is a variety of approaches which either bypass IIF such as delta measurements or refer to reference materials (RMs) and thus shifting the problem of calibration to somebody else: the RM producer. For certifying isotope RMs with absolute isotope ratios only a few approaches are available, namely the isotope mixture approach, the double spike approach, the mass bias regression model and total evaporation in TIMS. All of them require either enriched isotopes, isotope RMs of another element or an RM for correcting residual error. As the enriched isotopes required for the isotope mixture and the double spike approach need to be fully characterized beforehand, all mentioned calibration approaches require a standard. Here, a new and standard-free calibration approach for obtaining absolute isotope ratios of multi-isotopic elements has been developed. The underlying principle is that each MS suffers from IIF and thus yields a specific isotope fractionation line in a three-isotope diagram. When applying a second MS featuring a different ionization mechanism, we obtain a second isotope fractionation line with a different slope in the same three-isotope diagram. In both cases the absolute isotope ratios range somewhere on the isotope fractionation line. Consequentially, the intersect of both lines yield the absolute isotope ratios of the measured sample. This theory has been tested by measuring Cd and Pb isotope ratios of suitable isotope RMs with a TIMS and an ICP-MS, both equipped with multi-collector array. During the measurements the ionization conditions were changed such that different extent of the isotope fractionation has been achieved. With the resulting data set the theory described above could be verified. The obtained absolute isotope ratios were metrologically compatible with the certified isotope ratios. The remaining average bias of -5 ‰ can be reduced with further improvements. The calibration approach is universal and can be applied to any multi-isotopic element and it is not limited by the type of the mass spectrometer. T2 - Virtual Goldschmidt 2021 CY - Online meeting DA - 04.07.2021 KW - Absolute isotope ratio KW - Traceability KW - Metrology KW - Calibration KW - Uncertainty KW - Triple isotope fractionation PY - 2021 AN - OPUS4-53023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Backes, A. T. A1 - Reinmuth-Selzle, K. A1 - Leifke, A. L. A1 - Ziegler, K. A1 - Krevert, C. S. A1 - Tscheuschner, Georg A1 - Lucas, K. A1 - Weller, Michael G. A1 - Berkemeier, T. A1 - Pöschl, U. A1 - Fröhlich-Nowoisky, J. T1 - Oligomerization and Nitration of the Grass Pollen Allergen Phl p 5 by Ozone, Nitrogen Dioxide, and Peroxynitrite: Reaction Products, Kinetics, and Health Effects N2 - The allergenic and inflammatory potential of proteins can be enhanced by chemical modification upon exposure to atmospheric or physiological oxidants. The molecular mechanisms and kinetics of such modifications, however, have not yet been fully resolved. We investigated the oligomerization and nitration of the grass pollen allergen Phl p 5 by ozone (O3), nitrogen dioxide (NO2), and peroxynitrite (ONOO–). Within several hours of exposure to atmospherically relevant concentration levels of O3 and NO2, up to 50% of Phl p 5 were converted into protein oligomers, likely by formation of dityrosine cross-links. Assuming that tyrosine residues are the preferential site of nitration, up to 10% of the 12 tyrosine residues per protein monomer were nitrated. For the reaction with peroxynitrite, the largest oligomer mass fractions (up to 50%) were found for equimolar concentrations of peroxynitrite over tyrosine residues. With excess peroxynitrite, the nitration degrees increased up to 40% whereas the oligomer mass fractions decreased to 20%. Our results suggest that protein oligomerization and nitration are competing processes, which is consistent with a two-step mechanism involving a reactive oxygen intermediate (ROI), as observed for other proteins. The modified proteins can promote pro-inflammatory cellular signaling that may contribute to chronic inflammation and allergies in response to air pollution. KW - Protein KW - Nitrotyrosine KW - Dityrosine KW - Allergy KW - Hay fever KW - Diesel exhaust KW - Combustion KW - Exhaust PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529729 DO - https://doi.org/10.3390/ijms22147616 VL - 22 IS - 14 PB - MDPI CY - Basel AN - OPUS4-52972 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cant, D. J. H. A1 - Müller, Anja A1 - Clifford, C. A. A1 - Unger, Wolfgang A1 - Shard, A. G. T1 - Summary of ISO/TC 201 Technical Report 23173—Surface chemical analysis—Electron spectroscopies—Measurement of the thickness and composition of nanoparticle coatings N2 - ISO Technical Report 23173 describes methods by which electron spectroscopies, including X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and synchrotron techniques, can be employed to calculate the Coating thicknesses and compositions of nanoparticles. The document has been developed to review and outline the current state-of-the-art for such measurements. Such analyses of core–shell nanoparticles are common within the literature, however the methods employed are varied; the relative advantages and disadvantages of These methods, and the optimal usage of each may not be clear to the general analyst. ISO Technical Report 23173 aims to clarify the methods that are available, describe them in clear terms, exhibit examples of their use, and highlight potential issues users may face. The information provided should allow analysts of electron spectroscopy data to make clear choices regarding the appropriate analysis of electron spectroscopy data from coated nanoparticle systems and provide a basis for understanding and comparing results from different methods and systems. KW - Electron spectroscopy KW - Core-shell KW - Nanoparticles KW - ISO 23173 KW - XPS KW - Thickness KW - Composition PY - 2021 DO - https://doi.org/10.1002/sia.6987 SN - 0142-2421 VL - 53 IS - 10 SP - 893 EP - 899 PB - John Wiley & Sons Ltd AN - OPUS4-52976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Stephan-Scherb, Christiane ED - Schorr, S. ED - Weidenthaler, C. T1 - Crystallographic challenges in corrosion research N2 - High-temperature corrosion is a widespread problem in various industries. As soon as a hot and reactive gas (CO2, O2, H2O, SO2, NOx, etc.) is in contact with a solid, physico-chemical processes at the surface and interfaces lead to material degradation. The processes are dynamic and controlled by thermodynamic and kinetic boundary conditions. Whether a reaction product is protective or not depends on various factors, such as chemical composition of the solid and the reactive media, surface treatment as well as diffusion and transport paths of cations and anions. Resulting chemical and structural inhomogeneities with the corrosion layers are characterized by off stoichiometry within cationic and anionic sub lattices. The competitive processes can be studied by various techniques of applied crystallography. This chapter gives an overview on the challenges of chemical-structural Analysis of reaction products by crystallographic methods such as X-ray diffraction and X-ray near-edge structure spectroscopy and scanning electron microscopy electron backscatter diffraction (SEM-EBSD) for corrosion science. KW - High-temperature corrosion KW - Oxidation KW - Diffraction KW - Spectroscopy KW - Oxides PY - 2021 DO - https://doi.org/10.1515/9783110674910-009 SP - 291 PB - De Gruyter ET - 1 AN - OPUS4-52903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dinter, Adelina-Elisa ED - Dinter, Adelina-Elisa T1 - Development of a MIC single archaea-ICP-ToF-MS-method for analysis of various elements in solid steel samples N2 - With the latest ICP-MS technology - ICP-ToF (time of flight)-MS - it is possible to analyze the multi-element fingerprint of individual cells. The interface between material and environmental analysis thus receives special attention, e.g. when considering corrosion processes. Microbiologically influenced corrosion (MIC) is highly unpredictable due to the diversity of microbial communities involved. The development of the MIC-specific ICP-ToF-MS analytical method presented here at the single cell level, in combination with the investigation of steel-MIC interactions, contributes significantly to progress in instrumental MIC analysis and will enable clarification of the processes taking place. The supplied document shows the basis of a four minutes lightning talk. T2 - EuroMIC 2021 CY - Online meeting DA - 22.06.2021 KW - SC-ICP-ToF-MS KW - Single cell analysis KW - Microbiologically influenced corrosion KW - Lightning talk PY - 2021 AN - OPUS4-52905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Ponader, Marco A1 - Röder, Bettina A1 - Paul, Martin A1 - Weller, Michael G. T1 - Sintered glass monoliths as new supports for affinity columns N2 - A novel stationary phase for affinity separations is presented. This material is based on sintered borosilicate glass readily available as semi-finished filter plates with defined porosity and surface area. The material shows fast binding kinetics and excellent long-term stability under real application conditions due to lacking macropores and high mechanical rigidity. The glass surface can be easily modified with standard organosilane chemistry to immobilize selective binders or other molecules used for biointeraction. In this paper, the manufacturing of the columns and their respective column holders by 3D printing is shown in detail. The model system protein A/IgG was chosen as an example to examine the properties of such monolithic columns under realistic application conditions. Several specifications, such as (dynamic) IgG capacity, pressure stability, long-term performance, productivity, non-specific binding, and peak shape, are presented. It could be shown that due to the very high separation speed, 250 mg antibody per hour and column can be collected, which surpasses the productivity of most standard columns of the same size. The total IgG capacity of the shown columns is around 4 mg (5.5 mg/mL), which is sufficient for most tasks in research laboratories. The cycle time of an IgG separation can be less than 1 minute. Due to the glass material's excellent pressure resistance, these columns are compatible with standard HPLC systems. This is usually not the case with standard affinity columns, limited to manual use or application in low-pressure systems. The use of a standard HPLC system also improves the ability for automation, which enables the purification of hundreds of cell supernatants in one day. The sharp peak shape of the elution leads to an enrichment effect, which might increase the concentration of IgG by a factor of 3. The final concentration of IgG can be around 7.5 mg/mL without the need for an additional nanofiltration step. The purity of the IgG was > 95% in one step and nearly 99% with a second polishing run. KW - Affinity Chromatography KW - Glass KW - Purification KW - Antibodies KW - Solid support KW - HPLC KW - FPLC KW - Separation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529117 DO - https://doi.org/10.20944/preprints202103.0298.v1 SN - 2310-287X N1 - Geburtsname von Ponader, Marco: Wilke, M. - Birth name of Ponader, Marco: Wilke, M. SP - 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-52911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dinter, Adelina-Elisa T1 - Development of a MIC single archaea-ICP-ToF-MS-method for analysis of various elements in solid steel samples N2 - ICP-ToF (Flugzeitanalysator, engl. time of flight)-MS ermöglicht den Multielement Fingerabdruck einzelner Zellen (single cell) zu analysieren. Die single cell-ICP-ToF-MS kommt bei dem vorgestellten Poster bei der Analyse von Archaeen, die an mikrobiell beeinflusster Korrosion (engl. microbiologically influenced corrosion, MIC) von Stahl eine Rolle spielen, zum Einsatz. Mittels sc-ICP-ToF-MS wird die mögliche Aufnahme von einzelnen Elementen aus dem jeweiligen Stahl untersucht – die erhaltenen Informationen fließen zukünftig in die Aufklärung zugrunde liegender Mechanismen sowie Entwicklung möglicher Materialschutzkonzepte ein. Die Arbeiten Verknüpfen moderne Methoden der Analytical Sciences mit Materialien. T2 - Tag der Chemie 2021 CY - Online meeting DA - 06.07.2021 KW - SC-ICP-ToF-MS KW - Single cell analysis KW - Microbiologically influenced corrosion KW - Archaea PY - 2021 AN - OPUS4-52941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marcoulaki, E. A1 - M. López de Ipina, J. A1 - Vercauteren, S. A1 - Bouillard, J. A1 - Himly, M. A1 - Lynch, I. A1 - Witters, H. A1 - Shandilya, N. A1 - van Duuren-Stuurman, B. A1 - Kunz, Valentin A1 - Unger, Wolfgang A1 - Hodoroaba, Vasile-Dan A1 - Bard, D. A1 - Evans, G. A1 - Jensen, K. A. A1 - Pilou, M. A1 - Viitanen, A.-K. A1 - Bochon, A. A1 - Duschl, A. A1 - Geppert, M. A1 - Persson, K. A1 - Votgreave, I. A1 - Niga, P. A1 - Gini, M. A1 - Eleftheriadis, K. A1 - Scalbi, S. A1 - Caillard, B. A1 - Arevalillo, A. A1 - Frejafon, E. A1 - Aguerre-Chariol, O. A1 - Dulio, V. T1 - Blueprint for a self-sustained European Centre for service provision in safe and sustainable innovation for nanotechnology N2 - The coming years are expected to bring rapid changes in the nanotechnology regulatory landscape, with the establishment of a new framework for nano-risk governance, in silico approaches for characterisation and Risk assessment of nanomaterials, and novel procedures for the early identification and management of nanomaterial risks. In this context, Safe(r)-by-Design (SbD) emerges as a powerful preventive approach to support the development of safe and sustainable (SSbD) nanotechnology-based products and processes throughout the life cycle. This paper summarises the work undertaken to develop a blueprint for the deployment and operation of a permanent European Centre of collaborating laboratories and research organisations supporting safe Innovation in nanotechnologies. The proposed entity, referred to as “the Centre”, will establish a ‘one-stop shop’ for nanosafety-related services and a central contact point for addressing stakeholder questions about nanosafety. Its operation will rely on significant business, legal and market knowledge, as well as other tools developed and acquired through the EU-funded EC4SafeNano project and subsequent ongoing activities. The proposed blueprint adopts a demand-driven service update scheme to allow the necessary vigilance and flexibility to identify opportunities and adjust its activities and services in the rapidly evolving regulatory and nano risk governance landscape. The proposed Centre will play a major role as a conduit to transfer scientific knowledge between the Research and commercial laboratories or consultants able to provide high quality nanosafety services, and the end-users of such services (e.g., industry, SMEs, consultancy firms, and regulatory authorities). The Centre will harmonise service provision, and bring novel risk assessment and management approaches, e.g. in silico methodologies, closer to practice, notably through SbD/SSbD, and decisively support safe and sustainable innovation of industrial production in the nanotechnology industry according to the European Chemicals Strategy for Sustainability. KW - Nanotechnology KW - European Centre KW - Nano-safety KW - Nanomaterials KW - analytical service PY - 2021 DO - https://doi.org/10.1016/j.impact.2021.100337 VL - 23 SP - 100337 PB - Elsevier B.V. AN - OPUS4-52942 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Faßbender, Sebastian T1 - Mercury speciation in sediments of a historic industrially used canal in Northern Germany using SSID GC-ICP-ToF-MS N2 - Sediments and soils can act as sinks of species of inorganic mercury (Hg2+), while they are simultaneously sources of volatile (Hg0) and organic species, such as monomethylmercury (MMHg). Although the fraction of MMHg in total Hg of sediments is suggested to be as low as 0.1 1%, MMHg is a serious threat for humans and wildlife due to its high potential for bioaccumulation and biomagnification and the ability to pass the blood-brain barrier. This is highlighted by exceptionally high MMHg concentrations found in fish and fish predators, as well as aquatic insects and birds living in close vicinity to Hg contaminated waterbodies. Humans are exposed to MMHg mainly by ingestion of (predatory) fish and rice. One example of a highly Hg contaminated waterbody is Finow Canal, the oldest artificial waterway still in operation in Germany, with Hg mass fractions of up to or even more than 100 µg/g found in the sediment, which are suggested to be attributable to a chemical plant producing (among other things) mercury-based seed dressings. Despite this high mass fraction of Hg, anaerobic conditions, high amounts of organic matter and iron, which are all favorable for Hg methylation, no investigations of Hg speciation have been conducted there up to now. We investigated Hg speciation in sediments of Finow Canal on length from before the known polluted sited into the confluence with another waterway using species-specific isotope dilution (SSID) GC-ICP-ToF-MS. Mass fraction of up to 41 ng/g MMHg were determined in samples taken from Finow Canal and elevated concentrations could also be found around 14 km downstream of the confluence of Finow Canal with another waterway. In addition to this, highly toxic monoethylmercury (EtHg) could be detected in most of the sediment samples. These results are the first evidence of the occurrence of MMHg in this region and show the need for further investigation of the whole regional ecosystem, as well as the consideration of possible measures of remediation. T2 - Virtual Goldschmidt 2021 CY - Online meeting DA - 04.07.2021 KW - Methylmercury KW - Finow Canal KW - Legacy pollution KW - Isotope dilution PY - 2021 AN - OPUS4-52945 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Bestimmung der Messunsicherheit bei der instrumentierten Eindringprüfung N2 - In der DIN EN ISO 14577 Metallische Werkstoffe – Instrumentierte Eindringprüfung zur Bestimmung der Härte und anderer Werkstoffparameter sind die Durchführung und Auswertung des Verfahrens, sowie die Kalibrierung der zu verwendenden Prüfmaschine genormt. In dieser Norm werden auch grundsätzliche Aussagen zur Bestimmung der Messunsicherheit gemacht. An Beispielen aus der täglichen Prüfpraxis werden verschiedene Möglichkeiten, aber auch die Grenzen der Bestimmung der Messunsicherheitbei der Instrumentierten Eindringprüfung beschrieben und kritisch diskutiert. T2 - 3. Zwick Roell Symposium –Nanoindentation CY - Ulm, Germany DA - 04.07.2019 KW - ISO 14577 KW - Instrumentierte Eindringprüfung KW - Bestimmung der Messunsicherheit PY - 2019 AN - OPUS4-48431 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumacher, David A1 - Ou, D. A1 - Ghafafian, Carineh A1 - Zscherpel, Uwe A1 - Trappe, Volker T1 - Wind turbine rotor blade testing by dual-energy laminography N2 - Modern wind turbine rotor blades consist of sandwich shell segments made from glass fiber reinforced polymers. During manufacturing, defects can arise which could lead to failure of the whole component under dynamic mechanical and thermal loads. Hence during operation defects can arise which, if detected, can be repaired locally and in-situ by applying repair patches instead of taking the whole rotor blade down and repair it remotely. This method is much more time and cost effective, since the shut-down time of the energy converter is limited to a minimum. These repair patches can, however, also lead to new defects if not applied optimally. Therefore, it is necessary to control the quality of the repair patches to ensure the best possible restoration of structural integrity of the component. As a rotor blade is an object with a large aspect ratio, X-ray laminography is predestined to provide 3D information of the objective volume. To enhance the amount of information gained from laminographic reconstruction, we use in this study a photon counting and energy discriminating X-ray detector and apply a material decomposition algorithm to the data. By inherently separating the incident spectra within the detection process into two distinct energy bins, the basis material decomposition can provide material resolved images. Choosing glass and epoxy resin as basis materials and numerically solving the inverse dual-energy equation system, the reconstructed laminographic datasets contain highly valuable information about the distribution of the basis materials within the structure. Furthermore, cross- artifacts arising from the limited angle of the projection data can be reduced by this method which allows to investigate structures that were hidden underneath the artefacts. T2 - International Symposium on Digital Industrial Radiology and Computed Tomography – DIR2019 CY - Fürth, Germany DA - 02.07.2019 KW - Laminography KW - Wind energy KW - Fiber reinforced polymer KW - Photon counting detector KW - Repair patch PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-484380 UR - https://www.dir2019.com/portals/dir2019/bb/Tu.3.A.1.pdf SN - 978-947971-06-0 SP - 1 EP - 13 AN - OPUS4-48438 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, U. A1 - Jaenisch, Gerd-Rüdiger A1 - Deresch, A. A1 - Bircher, B. A. A1 - Meli, F. T1 - New concepts for the measurement of focal spot parameters of nano- and microfocus X-ray tubes N2 - Accurate measurement of focal spot sizes of X-ray tubes, betatrons and linear accelerators is still an open problem. Several standards are currently active, which provide different results depending on the focal spot shape. CEN published the standard series EN 12543 (five parts) in 1999, which describes the measurement of focal spot sizes of X-ray tubes for NDT applications. The measurement procedure and its tolerances deviate from the measurement standards for medical X-ray tubes, e.g. EN 60336:2006 / IEC 60336:2005. EN 12543 describes different measurement methods for X-ray tubes with focal spots in several size ranges, defined as macrofocus, minifocus and microfocus. CEN TC 138 WG 1 und ASTM E 07.01 are revising (CEN) or have just revised (ASTM) the standards for focal spot size measurements, basing them on pin hole or edge measurements only. Slit cameras are applied for medical tube evaluation only. Tomographic methods for focal spot size shape reconstruction were proposed and will be discussed, but have not yet been used for standardization. The currently available standards cover the range of spot sizes from 5 µm up to several millimetres. During the last years, more and more nanofocus tubes have been developed for high-resolution applications and microscopy. Manufacturers and users apply different methods for measurement of nanofocus spot sizes and image resolution, which differ by a factor of up to two. These well-known methods and new alternative methods for the measurement of nanofocus spots (size and shape) will be evaluated and improved in the EMPIR project “NanoXSpot” in order to develop a related measurement standard. T2 - International Symposium on Digital Industrial Radiology and Computed Tomography CY - Fürth, Germany DA - 02.07.2019 KW - X-Ray tube KW - Focal spot measurement KW - Standadization PY - 2019 AN - OPUS4-48442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Investigations of HKUST-1 exposed to water vapor, methanol and pyridine atmospheres by near-ambient pressure XPS N2 - Metal-organic frameworks (MOFs) are suitable materials for gas storage of small molecules due to their nanoporous, crystalline structure. The extensively studied MOF HKUST-1 consist of Cu(II)-dimers in a paddlewheel structure, with 1,3,5-benzenetricarboxylic acid (BTC) as organic linker. Instability to humidity remains an issue for many types of MOFs, and for HKUST-1, it has been found that exposure to water vapor creates a surface barrier which reduces the gas uptake rate. Near-ambient pressure XPS (NAP-XPS) is a promising method for investigations of the stability and interaction of HKUST-1 with various gas molecules. The oxidation state of copper can be monitored before, during and after exposure to various gases. This does not only provide information on the stability of the MOFs, but also on the interaction with the gas molecules. NAP-XPS measurements of HKUST-1 exposed to methanol, pyridine and water vapor were performed with EnviroESCA, a laboratory NAP-XPS instrument developed by SPECS. Cu 2p, O 1s and C 1s core level spectra and Cu LMM Auger spectra were acquired at pressures ranging from high vacuum to 4 mbar to assess the oxidation state of copper and the stability of the organic linker. Reference measurements in argon atmosphere were conducted in order to have reference spectra with similar full width of half maxima (FHWM) as the spectra measured in reactive atmospheres. Peak fit analysis of the Cu 2p3/2 core level spectra shows that, as expected, the photoelectron signal mainly originates from Cu(II) species. The contribution from Cu(I) is negligible for samples exposed to argon and methanol, but approximately 4% for samples exposed to water vapor and 8% for samples exposed to pyridine. Within the error of the peak fit analysis, there are no changes in relative Cu(II) percentage with increasing water, methanol or pyridine exposure time pointing to saturation reached already at the lowest time of exposure. T2 - Seminar X-Ray and Electron Spectroscopy at Interfaces group: Chemistry of oxydic and organic interfaces CY - Karlsruhe, Germany DA - 11.10.2019 KW - XPS KW - MOF KW - HKUST-1 KW - NAP-XPS PY - 2019 AN - OPUS4-49289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Mechanische, topometrische und optische Charakterisierung von Schichten mit Stand der Normung N2 - Der Vortrag „MECHANISCHE, TOPOMETRISCHE UND OPTISCHE CHARAKTERISIERUNG VON SCHICHTEN MIT STAND DER NORMUNG“ widmet sich unterschiedlichen Beschichtungssystemen und deren mechanischer, topometrischer und optischer Charakterisierung. Über die entsprechenden aktuellen Normen wird informiert. Es betrifft Verfahren wie die Instrumentierte Eindringprüfung (IIT), Centrifugal Adhesion Testing, Weißlichtinterferenzmikroskopie, Tastschnittverfahren und Ellipsometrie (SE). T2 - EFDS, V2019, Vakuum und Plasma CY - Dresden, Germany DA - 08.10.2019 KW - Normung KW - Spektrale Ellipsometrie (SE) KW - Instrumentierte Eindringprüfung (IIT) KW - Centrifugal Adhesion Testing (CAT) KW - Weißlichtinterferenzmikroskopie (WLIM, 3D) PY - 2019 AN - OPUS4-49320 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weise, Matthias T1 - Scanning White Light Interference Microscopy - Measurement of Topometry and Layer Thickness N2 - 3D coherence scanning interferometry (CSI) is anoptical, non-contact and rapide measurement technique using a defined bandwidth of white light at normal incidence. White light interference microscopy (WLIM) providest here-dimensional surface topometry data up to a resolution of 0.4 µm lateral and 0.1 nm vertical. Three operating modi, surface, films and advanced films, enable measurements of step heights, roughness, wear volume, cone angle, surface pattern and layer thickness. Traceability to SI system is ensured by certified standards (PTB/NIST) within a DAkkS DIN EN ISO/IEC 17025:2018 accredited lab. T2 - EFDS, V2019, Vakuum und Plasma, WS 4, Beschichtungen für Werkzeuge & Bauteile CY - Dresden, Germany DA - 08.10.2019 KW - DIN EN ISO/IEC 17025:2018 KW - Certified standards KW - White light interference microscopy(WLIM) KW - 3D coherence scanning interferometry (CSI) KW - Topometry PY - 2019 AN - OPUS4-49323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, I. T1 - SHM using Guided Waves – Recent Activities and Advances in Germany N2 - Issues that prevent Structural Health Monitoring (SHM) based on Guided Waves (GW) from being a part of today’s monitoring solutions in industry are not all obvious to the scientific community. To uncover and overcome these issues, scientists working on SHM and GW problems joined in an expert committee under the patronage of the German Society for Non-Destructive Testing. An initiated online survey among more than 700 experts and users reveals the hurdles hindering the practical application of GWbased SHM. Firstly, methods for proof of reliability of SHM approaches are missing. Secondly, detailed understanding of phenomenological described wave-damage interactions is needed. Additionally, there are significant unsolved implementation issues and unsolved problems of signal processing including handling of environmental influences. To enable substantial proof of reliability without unaffordable experimental effort also efficient simulation tools including realistic damage interaction are needed, enabling the joint use of experimental and simulated data to predict the capabilities of the Monitoring system. Considering these issues, the committee focusses on simulation, signal processing, as well as probability of detection and standardization. In the presented work, recent activities of the expert committee starting with survey results are summarized. An open access data basis of life-like measurements is presented to allow testing and comparison of signal processing and simulation algorithms. Finally, a strategy for efficient proof of reliability increasing the acceptance of SHM in industry and for successful Integration of SHM into real-world engineering structures is proposed. T2 - The 12th International Workshop on Structural Health Monitoring (IWSHM) CY - Stanford, California, USA DA - 10.09.2019 KW - Structural Health Monitoring KW - Ultrasonic Guided Waves KW - Non-Destructive Testing KW - Survey KW - Probability of Detection KW - Reliability PY - 2019 AN - OPUS4-49231 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, I. A1 - Moll, J. A1 - Kexel, C. A1 - Schubert, L. A1 - Tschöke, K. A1 - Prager, Jens A1 - Lugovtsova, Yevgeniya A1 - Bach, M. A1 - Vogt, T. T1 - SHM using Guided Waves – Recent Activities and Advances in Germany N2 - Issues that prevent Structural Health Monitoring (SHM) based on Guided Waves (GW) from being a part of today’s monitoring solutions in industry are not all obvious to the scientific community. To uncover and overcome these issues, scientists working on SHM and GW problems joined in an expert committee under the patronage of the German Society for Non-Destructive Testing. An initiated online survey among more than 700 experts and users reveals the hurdles hindering the practical application of GWbased SHM. Firstly, methods for proof of reliability of SHM approaches are missing. Secondly, detailed understanding of phenomenological described wave-damage interactions is needed. Additionally, there are significant unsolved implementation issues and unsolved problems of signal processing including handling of environmental influences. To enable substantial proof of reliability without unaffordable experimental effort also efficient simulation tools including realistic damage interaction are needed, enabling the joint use of experimental and simulated data to predict the capabilities of the Monitoring system. Considering these issues, the committee focusses on simulation, signal processing, as well as probability of detection and standardization. In the presented work, recent activities of the expert committee starting with survey results are summarized. An open access data basis of life-like measurements is presented to allow testing and comparison of signal processing and simulation algorithms. Finally, a strategy for efficient proof of reliability increasing the acceptance of SHM in industry and for successful Integration of SHM into real-world engineering structures is proposed. T2 - The 12th International Workshop on Structural Health Monitoring (IWSHM) CY - Stanford, California, USA DA - 10.09.2019 KW - Structural Health Monitoring KW - Ultrasonic Guided Waves KW - Non-Destructive Testing KW - Survey KW - Probability of Detection KW - Reliability PY - 2019 SP - 1 EP - 10 AN - OPUS4-49232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Performance of SEM/EDS systems with the Test Material EDS-TM001/002 and Evaluation Software EDS Spectrometer Test – Application and Updates N2 - The test material EDS-TM001 together with an accompanying software package, “EDS spectrometer check”, have been made available in 2009 by BAM to be employed by EDS (energy-dispersive X-ray spectrometer) users to check the performance of an EDS with a SEM. With EDS-TM001/002 test material, this periodical check is simplified to the acquisition of only one 10 kV spectrum. The software “EDS spectrometer check” is destined to evaluate automatically this spectrum and determine the EDS performance in terms of energy resolution and calibration, as well as possible alteration of low-energy efficiency due to detector contamination. Energy resolution can be compared with the specified values according to the international ISO standard ISO 15632:2012. EDS-TM is a synthetic material consisting of a 6 μm thick layer of C, Al, Mn, Cu and Zr deposited on a steel (EDS-TM001) or silicon (EDS-TM002) substrate. The chemical composition of EDS-TM was chosen such as to give nearly equal intensities of the low energy lines in a 10 kV spectrum, thus, making it very sensitive against spectrometer efficiency changes. New results and gained experiences will be presented. When the FWHM of the X-ray lines in the EDS-TM spectrum are determined, the spectrum Background must be subtracted accurately. The applied physical background subtraction procedure is robust and considers the transmission of the detector window. While the previous version considers only Moxtek AP windows, the new software version includes selection of silicon nitride window and the case of windowless detector. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Test material KW - EDS X-ray spectrometer KW - EPMA KW - Performance check PY - 2019 AN - OPUS4-49233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Correlative analysis of mesoporous thin IrOx-TiOx mixed oxide films for understanding the impact of synthesis conditions N2 - Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of thin porous films is affected by properties like porosity, film thickness, chemical composition of the material as well as the homogenous dispersion of the active species within the porous matrix. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution we characterize thin mesoporous iridium-titanium mixed oxide film properties by complementary analysis of SEM/EDS, ToF-SIMS, NanoSIMS, AES and spectroscopic ellipsometry. Mesoporous iridium oxide - titanium oxide (IrOx-TiOx) films can be prepared by a well-established Synthesis route via soft-templating. IrOx-TiOx films are very sensitive to the conditions of synthesis. Analysis by SEM and NanoSIMS imaging suggests IrOx-TiOx films with and without a homogenous dispersion of IrOx within the TiOx film matrix under different synthesis conditions. Auger electron spectroscopy (AES) analysis in the depth-profile mode as well as cross-section line-scan AES measurements of an inhomogeneous IrOx-TiOx film indicate the presence of an IrOx-rich Phase dispersion both at the surface of IrOx-TiOx film as well as within the film. The contribution will assess in detail the sensitivity of the synthesis conditions and the characterization of the thin metal oxide films. Moreover, the correlation between and comparison to other measurement techniques will be discussed. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Mesoporous films KW - Iridium oxide KW - SIMS KW - SEM/EDS KW - Titanium dioxide KW - Ellipsometry KW - Auger Electron Spectroscopy PY - 2019 AN - OPUS4-49234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brüngel, R. A1 - Rückert, J. A1 - Wohlleben, W. A1 - Babick, F. A1 - Ghanem, A. A1 - Gaillard, C. A1 - Mech, A. A1 - Rauscher, H. A1 - Hodoroaba, Vasile-Dan A1 - Weigel, S. A1 - Friedrich, C. M. T1 - NanoDefiner e-Tool: An Implemented Decision Support Framework for Nanomaterial Identification N2 - The European Commission’s recommendation on the definition of nanomaterial (2011/696/EU) established an applicable standard for material categorization. However, manufacturers face regulatory challenges during registration of their products. Reliable categorization is difficult and requires considerable expertise in existing measurement techniques (MTs). Additionally, organizational complexity is increased as different authorities’ registration processes require distinct reporting. The NanoDefine project tackled these obstacles by providing the NanoDefiner e-tool: A decision support expert system for nanomaterial identification in a regulatory context. It providesMT recommendations for categorization of specific materials using a tiered approach (screening/confirmatory), and was constructed with experts from academia and industry to be extensible, interoperable, and adaptable for forthcoming revisions of the nanomaterial definition. An implemented MT-driven material categorization scheme allows detailed description. Its guided workflow is suitable for a variety of user groups. Direct feedback and explanation enable transparent decisions. Expert knowledge is Held in a knowledge base for representation of MT performance criteria and physicochemical particle type properties. Continuous revision ensured data quality and validity. Recommendations were validated by independent case studies on industry-relevant particulate materials. Besides supporting material identification and registration, the free and open-source e-tool may serve as template for other expert systems within the nanoscience domain. KW - EC nanomaterial definition KW - Decision support KW - Expert system KW - Nanomaterial KW - Nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492449 DO - https://doi.org/10.3390/ma12193247 VL - 12 IS - 19 SP - 3247 PB - MDPI CY - Basel, CH AN - OPUS4-49244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. A1 - Kim, K. J. T1 - Analysis of Elemental Composition of Fe1-xNix and Si1-xGex Alloy Thin Films by EPMA and μ-XRF N2 - The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values.zeige mehr KW - Thin film analysis KW - EPMA KW - XRF KW - Fe-Ni KW - Si-Ge PY - 2019 DO - https://doi.org/10.1017/S1431927619009668 VL - 25 SP - 1786 EP - 1787 PB - Cambridge University Press AN - OPUS4-49245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan T1 - High-Quality Experimental Data in Electron Microscopy and Microanalysis – What Can, and Should We Jointly Do? N2 - There are different ways how to prove the quality of the analytical results obtained in a laboratory, e.g. use of validated standard operation procedures, participation in proficiency testing exercises, use of certified reference materials, etc. International standards provide requirements, specifications, Guidelines or characteristics of methods, instruments or samples with the final goal that these can be used consistently in accredited laboratories. In the field of electron microscopy and microbeam analysis standardization and metrology are terms which are encountered rather seldom at major conferences and scientific publications. Nevertheless, spectra formats like EMSA/MSA for spectral-data exchange or tagged image file format (TIFF) for SEM, guidelines for performing quality assurance procedures or for the specification of X-ray spectrometers as well as of certified reference materials (CRMs) in EPMA, or measurement of average grain size by electron backscatter diffraction (EBSD), or guidelines for calibrating image magnification in SEM or TEM are ISO standards already published and used successfully by a large part of the electron microscopy and microbeam analysis community. A main and continuous task of ISO/TC 202 and its subcommittees is to identify and evaluate feasible projects/proposals to be developed into new international standards, particularly with respect to recent but established technology, such the silicon drift detector (SDD) EDS. An international platform in the frame of which pre-standardization work can be organized is VAMAS (Versailles Project on Advanced Materials and Standards). International collaborative projects involving aim at providing the technical basis for harmonized measurements, testing, specifications, and standards to be further developed at ISO level. One key point of VAMAS activities is constituted by inter-laboratory comparisons for high-quality data. In the field of microbeam analysis, the technical working area (TWA) 37 Quantitative Microstructural Analysis deals with corresponding projects. Good ideas, e.g. on analysis of low-Z materials/elements and at low energies are particularly encouraged by directly contacting the author. Support and already available guidance will be supplied. KW - Data KW - Electron probe microanalysis KW - Electron microscopy KW - VAMAS KW - Iinter-laboratory comparison PY - 2019 DO - https://doi.org/10.1017/S1431927619009541 VL - 25 SP - 1762 EP - 1763 PB - Cambridge University Press AN - OPUS4-49246 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reimann, C. A1 - Kaufmann, Jan Ole A1 - Adams, L. C. A1 - Onthank, D. C. A1 - Thöne-Reineke, C. A1 - Robinson, S. P. A1 - Hamm, B. A1 - Botnar, R. M. A1 - Makowski, M. R. T1 - Dual-probe molecular MRI for the in vivo characterization of atherosclerosis in a mouse model: Simultaneous assessment of plaque inflammation and extracellular-matrix remodeling N2 - Molecular MRI is a promising in-vivo modality to detect and quantify morphological and molecular vessel-wall changes in atherosclerosis. The combination of different molecular biomarkers may improve the risk stratification of patients. This study aimed to investigate the feasibility of simultaneous visualization and quantification of plaque-burden and inflammatory activity by dual-probe molecular MRI in a mouse-model of progressive atherosclerosis and in response-to-therapy. Homozygous apolipoprotein E knockout mice (ApoE−/−) were fed a high-fat-diet (HFD) for up to four-months prior to MRI of the brachiocephalic-artery. To assess response-to-therapy, a statin was administered for the same duration. MR imaging was performed before and after administration of an elastin-specific gadolinium-based and a macrophage-specific iron-oxide-based probe. Following in-vivo MRI, samples were analyzed using histology, immunohistochemistry, inductively-coupled-mass-spectrometry and laser-inductively-coupled-mass-spectrometry. In atherosclerotic-plaques, intraplaque expression of elastic-fibers and inflammatory activity were not directly linked. While the elastin-specific probe demonstrated the highest accumulation in advanced atherosclerotic-plaques after four-months of HFD, the iron-oxide-based probe showed highest accumulation in early atherosclerotic-plaques after two-months of HFD. In-vivo measurements for the elastin and iron-oxide-probe were in good agreement with ex-vivo histopathology (Elastica-van-Giesson stain: y = 298.2 + 5.8, R2 = 0.83, p < 0.05; Perls‘ Prussian-blue-stain: y = 834.1 + 0.67, R2 = 0.88, p < 0.05). Contrast-to-noise-ratio (CNR) measurements of the elastin probe were in good agreement with ICP-MS (y = 0.11x-11.3, R² = 0.73, p < 0.05). Late stage atherosclerotic-plaques displayed the strongest increase in both CNR and gadolinium concentration (p < 0.05). The gadolinium probe did not affect the visualization of the iron-oxide-probe and vice versa. This study demonstrates the feasibility of simultaneous assessment of plaque-burden and inflammatory activity by dual-probe molecular MRI of progressive atherosclerosis. The in-vivo detection and quantification of different MR biomarkers in a single scan could be useful to improve characterization of atherosclerotic-lesions. KW - In-vivo KW - Molecular MRI PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492514 DO - https://doi.org/10.1038/s41598-019-50100-8 VL - 9 IS - 1 SP - Article number: 13827 PB - Nature AN - OPUS4-49251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Furche, A. T1 - Surface analyses and cleaning of blackened Italian marble sculptures burnt during the Second World War from the collection of the Bode-Museum in Berlin N2 - The cleaning of black carbon covered Italian marble and limestone sculptures is a challenging task for restorers and scientists, especially when black soot is penetrated into the porous surface of a stone. Numerous sculptures of the Bode-Museum underwent two domestic fires at the repository in Berlin in May 1945, where soot damaged the surface of these artworks. Promising results in removing black layers were achieved by the application of modified gels to artificially weathered and sooted Carrara marble mockups. However, transferring the cleaning method to original samples requires a cautious proceeding with respect to short-term and long-term implications. To understand physico-chemical reactions, the analytics of gel-treated marble surfaces is of essential importance. Time-of-Flight Secondary Ion Mass Spectroscopy (ToF-SIMS) and Auger electron spectroscopy (AES) were used to gain insights into surface chemistry and the distribution of chemical groups or fragments and enable a deeper understanding of the functionality of the applied gels and of the efficiency of tested cleaning processes. Depth profiling by ToF-SIMS is introduced as a tool to study the penetration behavior of applied cleaning chemicals. The contribution presents the analytical methods, their possibilities and challenges, and summarizes initial results of this study. T2 - IPERION CH CY - Amsterdam, The Netherlands DA - 06.02.2019 KW - Cleaning KW - Surface analyses KW - Marble sculptures PY - 2019 AN - OPUS4-49334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement of Elemental Composition of and SiGe Alloy Thin Films by EPMA and µ-XRF N2 - The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Thin films KW - EPMA KW - XRF KW - FeNi KW - SiGe PY - 2019 AN - OPUS4-49278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Organic Surface Modification and Analysis of Titania Nanoparticles for Self-Assembly in Multiple Layers N2 - The characteristics of TiO2 coatings can greatly influence their final performance in large-scale applications. In the present study self-assembly of TiO2 nanoparticles (NPs) in multiple layers was selected as a deposition procedure on various substrates. For this, the main prerequisite constitutes the surface modification of both NPs and substrate with e.g. silane coupling agents. A set of functionalized TiO2 NPs has been produced by reaction with either (3- aminopropyl)triethoxysilane (APTES) or (3-aminopropyl)phosphonic acid (APPA) to functionalize the NP surface with free amino-groups. Then, the complementary functionalized NP set can be obtained from an aliquot of the first one, through the conversion of free surface amino-groups to aldehydes by reaction with glutaraldehyde (GA). Several types of TiO2 NPs differing in size, shape and specific surface area have been functionalized. FTIR, TGA, SEM/EDS, XPS, Auger electron spectroscopy (AES) and ToF-SIMS analyses have been carried out to evaluate the degree of functionalization, all the analytical methods employed demonstrating successful functionalization of TiO2 NP surface with APTES or APPA and GA. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - TiO2 KW - Layer-by-layer deposition KW - Surface functionalization KW - P25 KW - Surface characterization PY - 2019 AN - OPUS4-49279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Presentation at AVIC-Workshop - Analysis of the operation of accreditation bodies in Europe N2 - Accreditation is one of the relevant tasks in a modern Quality Infrastructure, as the competence of conformity assessment bodies is assured through accreditation performed by accreditation bodies. To compare the operation of accreditation bodies in Europe and identify best practices a management tool was elaborated and validated by applying it to eight accreditation bodies. The tool made a comparison of the operations of the accreditation bodies possible, despite different sizes, operational processes and organizational forms. The benchmarking project comprised three stages. In the first stage, the processes of accreditation bodies were systematically analyzed. A process map was developed and processes of special relevance for the performance of accreditation bodies were identified and underpinned by indicators. In the second stage, the processes of the German accreditation body Deutsche Akkreditierungsstelle GmbH (DAkkS) were assigned to the tool. This validation stage was used to check and modify the indicators when necessary. In the third stage, the transferability of the model was analyzed by extension to seven other accreditation bodies operating in Europe. The third stage of the project resulted in a workshop attended by experts from the participating ABs, which was used to discuss the results of the comparison and to identify best practices. T2 - Visit & Workshop of NQI Lab SAMR/AVIC and BAM CY - Berlin, Germany DA - 29.10.2019 KW - Accreditation KW - Benchmarking PY - 2019 AN - OPUS4-49449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lugovtsova, Yevgeniya A1 - Bulling, Jannis A1 - Boller, Christian A1 - Prager, Jens T1 - Analysis of Guided Wave Propagation in a Multi-Layered Structure in View of Structural Health Monitoring N2 - Guided waves (GW) are of great interest for non-destructive testing (NDT) and structural health monitoring (SHM) of engineering structures such as for oil and gas pipelines, rails, aircraft components, adhesive bonds and possibly much more. Development of a technique based on GWs requires careful understanding obtained through modelling and analysis of wave propagation and mode-damage interaction due to the dispersion and multimodal character of GWs. The Scaled Boundary Finite Element Method (SBFEM) is a suitable numerical approach for this purpose allowing calculation of dispersion curves, mode shapes and GW propagation analysis. In this article, the SBFEM is used to analyse wave propagation in a plate consisting of an isotropic aluminium layer bonded as a hybrid to an anisotropic carbon fibre reinforced plastics layer. This hybrid Composite corresponds to one of those considered in a Type III composite pressure vessel used for storing gases, e.g., hydrogen in automotive and aerospace applications. The results show that most of the wave energy can be concentrated in a certain layer depending on the mode used, and by that damage present in this layer can be detected. The results obtained help to understand the wave propagation in multi-layered structures and are important for further development of NDT and SHM for Engineering structures consisting of multiple layers. KW - Lamb waves KW - Composite KW - Ultrasonic Testing KW - Numerical Modelling KW - Pressure Vessels PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494385 DO - https://doi.org/10.3390/app9214600 VL - 9 IS - 21 SP - 4600 PB - MDPI CY - 4052 Basel, Switzerland AN - OPUS4-49438 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Future projects in Microbeam Analysis better Prepared within VAMAS N2 - The presentation points out and discusses potential future projects on microbeam analysis which shall benefit from the pre-standardisation platform VAMAS (Versailles Project on Advanced Materials and Standards) which is basically related to Organisation and participation in international inter-laboratory comparisons. Ideas and strategies of better synergies between VAMAS and ISO projects (including promotion and a dedicated liaison) are discusssed. T2 - 26th Plenary Meeting of ISO/TC 202 Microbeam Analysis CY - Hangzhou, China DA - 23.10.2019 KW - Standardisation KW - Microbeam analysis KW - VAMAS KW - Pre-standardisation PY - 2019 AN - OPUS4-49443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Discussion on the Systematic Review of ISO/DIS 15632 Instrumental Parameters for the Specification and Checking of EDS for Use in EPMA N2 - The Systematic Review of ISO/DIS 15632 Selected Instrumental Parameters for the Specification and Checking of Energy-Dispersive X-Ray Spectrometers for Use in Electron Probe Microanalysers is discusssed. Zero strobe peak, better description of dead-time and of the pulse-processing electronics are the major issues under discussion. T2 - 26th Plenary Meeting of ISO/TC 202 Microbeam Analysis CY - Hangzhou, China DA - 23.10.2019 KW - Standardisation KW - Electron probe microanalysis KW - EDS performance check KW - ISO KW - X-ray detectors PY - 2019 AN - OPUS4-49447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - Erstellung von Wellenzahlkarten zur Schadensquantifizierung auf Basis von geführten Ultraschallwellen N2 - Die Verwendung von Verbundwerkstoffen ist nicht nur mit den Vorteilen einer Gewichtsreduzierung und einer verbesserten strukturellen Leistung verbunden, sondern auch mit der Gefahr von kaum sichtbaren Impakt- oder Herstellungsschäden. Eine der vielversprechenden Methoden zur Erkennung und Charakterisierung solcher Schäden basiert auf der Ausbreitung und Analyse geführter Ultraschallwellen. Der multimodale und dispersive Charakter dieser Wellen erschweren jedoch die Analyse. Verschiedene Signalverarbeitungsmethoden wurden vorgeschlagen, um die Interpretation von Signalen und die Extraktion der notwendigen Informationen über den Schaden zu erleichtern. Eine davon ist die Erstellung einer Wellenzahlkarte. Die Wellenzahlkarte erlaubt es jeden Punkt in einer hochaufgelöste Wellenfeldaufnahme eine Wellenzahl zuzuordnen. Diese Methode ermöglicht sowohl die Quantifizierung der Größe als auch der Tiefe des Schadens. In diesem Beitrag wird diese Bildgebungsmethode auf delaminierte Aluminium-CFK-Verbundstrukturen angewendet. Solche Strukturen entsprechen den umwickelten Druckbehältern, die zur Speicherung von Gasen in der Luft- und Raumfahrt sowie in der Automobilindustrie verwendet werden. Zunächst werden die numerischen Untersuchungen zur einfachen Delamination in unterschiedlicher Tiefe vorgestellt. Als nächstes wird die Analyse von experimentellen Ergebnissen von einer geschädigten Aluminium-CFK-Platte präsentiert. Das Ergebnis der Bildgebung ist eine dreidimensionale Darstellung, die sowohl die Größe als auch die Tiefe des Impakt-Schadens liefert. T2 - Doktorandenseminar "Geführte Wellen" CY - Delbrück, Germany DA - 21.10.2019 KW - Schaden Quantifizierung KW - Faserverbundwerkstoffe KW - Geführte Wellen KW - Ultraschall KW - Impakt-Schaden PY - 2019 AN - OPUS4-49392 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lüdecke, Nils A1 - Weidner, Steffen A1 - Schlaad, Helmut T1 - Poly(2‐oxazoline) s Based on Phenolic Acids N2 - A series of phenolic-acid-based 2-oxazoline monomers with methoxysubstituted phenyl and cinnamyl side chains is synthesized and polymerized in a microwave reactor at 140 °C using methyl tosylate as the initiator. The obtained poly(2-oxazoline)s are characterized by NMR spectroscopy, MALDITOF mass spectrometry, and size-exclusion chromatography (SEC). Kinetic studies reveal that the microwave-assisted polymerization is fast and completed within less than ≈10 min for low monomer-to-initiator ratios of ≤25. Polymers with number-average molar masses of up to 6500 g mol−1 and low dispersity (1.2–1.3) are produced. The aryl methyl ethers are successfully cleaved with aluminum triiodide/N,N′ diisopropylcarbodiimide to give a poly(2-oxazoline) with pendent catechol groups. KW - 2-oxazoline KW - Catechol KW - Cationic ring opening polymerization KW - Microwave KW - Phenolic acid PY - 2019 DO - https://doi.org/10.1002/marc.201900404 SP - 1900404 PB - Wiley VCH-Verlag AN - OPUS4-49396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - De Samber, B. A1 - Scharf, Oliver A1 - Buzanich, Günter A1 - Garrevoet, J. A1 - Tack, P. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Reinholz, Uwe A1 - Evens, R. A1 - De Schamphelaere, K. A1 - Falkenberg, G. A1 - Janssen, C. A1 - Vincze, L. T1 - Three-dimensional X-ray fluorescence imaging modes for biological specimens using a full-field energy dispersive CCD camera N2 - Besides conventional scanning X-ray fluorescence imaging at synchrotron sources, full-field X-ray fluorescence (FF-XRF) imaging techniques that do not implicitly require spatial scanning of the sample have become available. FF-XRF has become achievable thanks to the development of a new type of energy dispersive CCD-based 2D detector, also referred to as a 'color X-ray camera (CXC)' or 'SLcam'. We report on different imaging schemes for biological samples using FF-XRF imaging: (a) 2D 'zoom' imaging with pinhole optics using the 'camera obscura' principle; (b) 2D 'fixed magnification' imaging using magnifying polycapillary optics; and (c) 3D-FF-XRF imaging using an X-ray sheet beam or computed tomography (CT). The different FF-XRF imaging modes are illustrated using the crustacean Daphnia magna, a model organism for investigating the effects of metals on organism/ecosystem health, and foraminifera, a class of amoeboid protist. Detailed analytical characterization of the set-up is performed through analyzing various reference materials in order to determine limits of detection (LODs) and sensitivities. Experiments were performed using the BAMline at the BESSY synchrotron (Berlin, Germany) and using the P06 Hard X-ray Microprobe at the PETRAIII synchrotron (Hamburg, Germany). KW - CXC KW - BAMline KW - Maia detector KW - Synchrotron PY - 2019 DO - https://doi.org/10.1039/c9ja00198k VL - 34 IS - 10 SP - 2083 EP - 2093 PB - Royal Society of Chemistry CY - Cambridge, United Kingdom AN - OPUS4-49359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul T1 - Ultrasonic measurement system based on phononic crystals N2 - An essential task in many industries, e.g. food, petrol or chemical industry, is the precise and accurate characterization of liquids. Therefore, the development of innovative in-line sensors is of great interest. New concepts based on periodic structures, so-called phononic crystals (PnCs), are an interesting idea for the design of innovative sensors. A PnC-based sensor can be designed by introducing a resonance inside a bandgap, a frequency region where no wave propagation is allowed. High-Q measurement systems using PnCs are already reported in the literature. However, existing designs cannot be implemented into a piping system directly, but need special fittings, openings or by-passes to be in contact with the liquid. To circumvent this issue, we develop a new sensor based on PnCs, which can be directly implemented as part of the piping system. For this purpose, we use a PnC consisting of hollow cylinders with a periodic change of the outer diameter. A bandgap could be found for the described geometry without fluid in simulation and measurement. However, simulations show, that a bandgap for fluid-filled cylinders can only be obtained for quasi-longitudinal modes. Hence, we propose a mode selective excitation for the sensor. T2 - ICA 2019 CY - Aachen, Germany DA - 09.09.2019 KW - Phononic crystal KW - Ultrasound PY - 2019 AN - OPUS4-49430 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - X-ray fluorescence imaging with coded apertures N2 - Our aim is to develop a new method for full field X ray fluorescence imaging at the BAM line @ BESSY II. We will combine an energydispersive array detector for X rays with a coded aperture to get high resolution images . In coded aperture imaging , an object is projected through a mask , producing many overlapping images on the detector . The first part of the project is to perform raytracing simulations to get realistic data and to develop a reconstruction method that allows to get the Information about the investigated object out of the projected image . T2 - Symposium "IRIS 2019" CY - Berlin, Germany DA - 24.10.2019 KW - X-ray spectroscopy KW - X-ray fluorescence KW - Imaging KW - Coded Apertures PY - 2019 AN - OPUS4-49434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Olaf T1 - Emission Testing for Indoor Products N2 - The chemical emissions from products are tested by means of emission test chambers under defined conditions (climate, loading, air change rate). The standard method for the determination of volatile organic compounds (VOC) is the sampling onto Tenax-tubes followed by thermal desorption (TDS) and gas chromatography-mass spectrometry (GC-MS) analysis. The EU-LCI list includes some very volatile organic compounds (VVOC) and some VOC for which there are limitations when using the standard method. For VVOC additional sampling is required using stronger absorbers like Carbotrap or multi-bed adsorption tubes. The analysis of VVOC also requires a different GC oven program and a different column for the separation. For the determination of formaldehyde and other low boiling aldehydes (e.g. acetaldehyde, acetone, propanal, propenal) DNPH-cartridges are used which are extracted with acetonitrile followed by liquid chromatography (HPLC-UV) analysis. The derivatisation of propenal and other unsaturated aldehydes (e.g. 2-butenal) with DNPH might lead to lower findings due to incomplete derivatization and forming of by-products. For a better quantification of acetic acid the use of ion chromatography (IC) is recommended because the analysis of acetic acid with the standard method (TDS) leads to lower findings due to break through during sampling. The use of ion chromatography for the analysis of organic acids requires a third sampling technique. The acids are adsorbed onto silica-gel and extracted with water. T2 - ISESISIAQ 2019 CY - Kaunas, Lituania DA - 18.08.2019 KW - Indoor Air Quality KW - Emission Testing KW - Indoor Products KW - VOC Emission KW - Construction Products PY - 2019 AN - OPUS4-49406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - HR-CS-GFMAS als leistungsstarkes Werkzeug zur Analyse von organisch gebundenem Fluor (EOF) in Oberflächengewässern N2 - Methodenentwicklung Fluoranalytik (anorganisch - organisch) als Summenparameter mittels HR-CS-GFMAS in Umweltproben T2 - Analytik Jena Days 2019 CY - Idstein, Germany DA - 26.06.2019 KW - Hochauflösende continuum source-Graphitrohr Molekülabosprtionsspektrometrie (HR-CS-GFMAS) KW - Methodenentwicklung KW - Summenparameter Fluor KW - Umweltanalytik PY - 2019 AN - OPUS4-48633 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul M. A1 - Lange, Nele A1 - Lippitz, Andreas A1 - Holzweber, Markus A1 - Kulak, N. A1 - Unger, Wolfgang T1 - Click chemistry on silicon nitride for biosensor fabrication N2 - Biosensors are of essential importance in medical and biological diagnostics. Often, they are produced using silane chemistry on glass or silicon oxide surfaces. However, controlling that silane chemistry is challenging. Here, we present an alternative strategy to form functional organic layers and biosensors on silicon Nitride (Si3N4). H-terminated Si3N4 films are used to generate reactive azide groups by various azidation methods. Biomolecular probes can then be immobilized using click chemistry reactions with the azide groups and due to its high sensitivity in XPS a fluorine-substituted test alkyne was utilized to optimize click chemistry conditions. After that a biotinylated alkyne was clicked to Si3N4 surfaces followed by immobilization of streptavidin as analyte in a model assay. The functionalized surfaces were thoroughly characterized by surface chemical analysis using X-ray photoelectron spectroscopy (XPS) and near edge X-ray absorption fine structure (NEXAFS)spectroscopy. KW - Biosensors KW - H-terminated Si3N4 films KW - Click chemistry KW - X-ray photoelectron spectroscopy KW - Near edge X-ray absorption fine structure KW - Streptavidin binding PY - 2019 DO - https://doi.org/10.1016/j.apsusc.2019.03.002 SN - 0169-4332 VL - 481 SP - 10 EP - 15 PB - Elsevier B.V. AN - OPUS4-48634 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Daneshnia, S. A1 - Adeli, M. A1 - Yari, A. A1 - Shams, A. A1 - Donskyi, Ievgen A1 - Unger, Wolfgang T1 - Low temperature functionalization of two-dimensional boron nitride for electrochemical sensing N2 - Two-dimensional hexagonal boron nitride(h-BN)as an emerging nanomaterial exhibits uniquephysicochemical properties, making it suitable candidate for a wide spectrum of applications.However, due to its poor functionality, the processability of this nanomaterial is low. In this work, wereport on a straightforward and scalable approach for the functionalization of h-BN by nitrene[2+1]cycloaddition at room temperature. The triazine-functionalized h-BN(Trz-BNs)showed ahigh reactivity toward nucleophiles, through which post-modifications are performable. The post-modification of Trz-BNs by L-cysteine was studied using cyclic voltammetry and differential pulsevoltammetry. Taking advantage of the scalable and straightforward functionalization as well as abilityof triazine functional groups for the controlled post-modifications, Trz-BNs is a promisingnanoplatform for a wide range of future applications. KW - Two-dimensional hexagonal boron nitride(h-BN) KW - Nitrene[2+1]cycloaddition KW - Post-modification by L-cysteine KW - Electrochemical sensing KW - XPS PY - 2019 DO - https://doi.org/10.1088/2053-1591/ab317b SN - 2053-1591 VL - 6 IS - 9 SP - 095076, 1 EP - 11 PB - IOP Publishing Ltd AN - OPUS4-48635 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schürmann, Robin A1 - Ebel, Kenny A1 - Nicolas, C. A1 - Milosavljevic, A. R. A1 - Bald, Ilko T1 - Role of valence band states and plasmonic enhancement in electron-transfer-induced transformation of nitrothiophenol N2 - Hot-electron-induced reactions are more and more recognized as a critical and ubiquitous reaction in heterogeneous catalysis. However, the kinetics of these reactions is still poorly understood, which is also due to the complexity of plasmonic nanostructures. We determined the reaction rates of the hot-electron-mediated reaction of 4-nitrothiophenol (NTP) on gold nanoparticles (AuNPs) using fractal kinetics as a function of the laser wavelength and compared them with the plasmonic enhancement of the system. The reaction rates can be only partially explained by the plasmonic response of the NPs. Hence, synchrotron X-ray photoelectron spectroscopy (XPS) measurements of isolated NTP-capped AuNP clusters have been performed for the first time. In this way, it was possible to determine the work function and the accessible valence band states of the NP systems. The results show that besides the plasmonic enhancement, the reaction rates are strongly influenced by the local density of the available electronic states of the system. KW - Photocatalytic reduction KW - Raman-spectroscopy KW - Hot-electrons KW - Work function KW - Surface KW - Nanaoparticles KW - Scattering KW - Molecule KW - Carriers KW - Layers PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486464 DO - https://doi.org/10.1021/acs.jpclett.9b00848 SN - 1948-7185 VL - 10 IS - 11 SP - 3153 EP - 3158 PB - American Chemical Society CY - Washington, DC AN - OPUS4-48646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heck, Christian A1 - Kanehira, Y. A1 - Kneipp, Janina A1 - Bald, Ilko T1 - Amorphous Carbon Generation as a Photocatalytic Reaction on DNA-Assembled Gold and Silver Nanostructures N2 - Background signals from in situ-formed amorphous carbon, despite not being fully understood, are known to be a common issue in few-molecule surface-enhanced Raman scattering (SERS). Here, discrete gold and silver nanoparticle aggregates assembled by DNA origami were used to study the conditions for the formation of amorphous carbon during SERS measurements. Gold and silver dimers were exposed to laser light of varied power densities and wavelengths. Amorphous carbon prevalently formed on silver aggregates and at high power densities. Time-resolved measurements enabled us to follow the formation of amorphous carbon. Silver nanolenses consisting of three differently-sized silver nanoparticles were used to follow the generation of amorphous carbon at the single-nanostructure level. This allowed observation of the many sharp peaks that constitute the broad amorphous carbon signal found in ensemble measurements. In conclusion, we highlight strategies to prevent amorphous carbon formation, especially for DNA-assembled SERS substrates. KW - Amorphous carbon KW - DNA origami KW - SERS KW - Nanoparticle dimers KW - Nanolenses PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486484 DO - https://doi.org/10.3390/molecules24122324 SN - 1420-3049 VL - 24 IS - 12 SP - Article Number: 2324-1 EP - 10 PB - MDPI AN - OPUS4-48648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Gawek, Marcel A1 - Madkour, S. A1 - Schönhals, Andreas T1 - Confinement and localization effects revealed for thin films of the miscible blend Poly(vinyl methyl ether) / Polystyrene with a composition of 25/75 wt% N2 - Thin films (200-7nm) of the asymmetric polymer blend poly(vinyl methyl ether) (PVME)/polystyrene (PS) (25/75wt%) were investigated by broadband dielectric spectroscopy (BDS). Thicker samples ([Formula: see text]37 nm) were measured by crossed electrode capacitors (CEC), where the film is capped between Al-electrodes. For thinner films ([Formula: see text]37 nm) nanostructured capacitors (NSC) were employed, allowing one free surface in the film. The dielectric spectra of the thick films showed three relaxation processes ( [Formula: see text] -, [Formula: see text] - and [Formula: see text] -relaxation), like the bulk, related to PVME fluctuations in local spatial regions with different PS concentrations. The thickness dependence of the [Formula: see text] -process for films measured by CECs proved a spatially heterogeneous structure across the film with a PS-adsorption at the Al-electrodes. On the contrary, for the films measured by NSCs a PVME segregation at the free surface was found, resulting in faster dynamics, compared to the CECs. Moreover, for the thinnest films ([Formula: see text]26 nm) an additional relaxation process was detected. It was assigned to restricted fluctuations of PVME segments within the loosely bounded part of the adsorbed layer, proving that for NSCs a PVME enrichment takes place also at the polymer/substrate interface. KW - Thin polymer films KW - Broadband dielectric spectroscopy PY - 2019 DO - https://doi.org/10.1140/epje/i2019-11870-3 SN - 1292-895X VL - 42 IS - 8 SP - 101, 1 EP - 11 PB - Springer AN - OPUS4-48651 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jain, V. A1 - Kjaervik, Marit A1 - Bahr, S. A1 - Dietrich, P. A1 - Meyer, M. A1 - Thissen, A. A1 - Linford, M. R. T1 - Bovine serum albumin, aqueous solution, by near-ambient pressure XPS N2 - Near-ambient pressure x-ray photoelectron spectroscopy (NAP-XPS) is a less traditional form of XPS that allows samples to be analyzed at relatively high pressures, i.e., at greater than 2500 Pa. With NAP-XPS, XPS can probe moderately volatile liquids, biological samples, porous materials, and/or polymeric materials that outgas significantly. In this submission, we show survey, C 1s, O 1s, and N 1s narrow scans from an aqueous solution of a common protein, bovine serum albumin. The C 1s peak envelope is well fit to four symmetric peaks of equal width that correspond to carbon bonded to carbon and hydrogen (C-1), carbon singly bonded to oxygen (C-2), carbonyl and/or amide carbon (C-3), and carboxyl carbon (C-4). Two possible peak fits are considered for the N 1s and O 1s peak envelopes. The N 1s signal is fit to four peaks that correspond to amine (—NH2), Amide (OvCZNH2), ammonium (—NH3 +), and N2(g) nitrogen, and alternatively to three peaks that correspond to amine, amide, and N2(g) nitrogen. The O 1s peak envelope is similarly fit to three and four components. KW - NAP-XPS KW - BSA KW - Bovine serum albumin KW - XPS KW - Near-ambient pressure PY - 2019 DO - https://doi.org/10.1116/1.5055229 VL - 26 IS - 1 SP - 014027 PB - American Vacuum Society CY - New York, USA AN - OPUS4-48655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Yi A1 - Bierstedt, Andreas A1 - Riedel, Jens T1 - Spatial, temporal, and spectral characterization and kinetic investigations of a high repetition-rate laser-induced micro-plasma in air N2 - Advances in laser-induced plasmas have enabled various rapid and simple analytical applications. Especially, their uses in the analyses of condensed-phase samples have drawn significant attention in the past few decades. Depending on the laser energy per pulse, various analytical goals can be achieved. Laser-induced airborne plasmas allow direct analysis of species in ambient air. Importantly, all of these applications are based on a fundamental understanding of the laser–medium interaction. Recent developments of diode-pumped solid-state lasers offer an alternative to conventional powerful, yet bulky lasers, which can specifically operate at high Repetition rates. Although these lasers deliver much lower power per pulse (mJ compared to mJ), the outstanding repetition rates offer significant improvement to meet statistical needs in some cases. In the present work, a mJ-laserinduced airborne plasma was characterized through optical emission analysis. By using a ns-timegated image detector coupled with specific bandpass filters, spatially, temporally, and spectrally resolved plasma images were recorded. Compared to conventional mJ-laser-induced plasmas, the one induced by mJ-lasers demonstrated unique features during its evolution. Specifically, measurements of the distribution of ionic and atomic species revealed distinctive energy/matter transfer processes during early ignition of the plasma. Meanwhile, dynamic investigations suggested subsequent matter transport in the later stage. KW - Laser-induced plasma KW - Plasma KW - DPSS-laser PY - 2019 UR - https://pubs.rsc.org/en/content/articlehtml/2019/ja/c9ja00163h DO - https://doi.org/10.1039/C9JA00163H SN - 0267-9477 VL - 34 IS - 8 SP - 1618 EP - 1629 PB - Royal Society of Chemistry CY - London AN - OPUS4-48622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - Fluoranalytik mittels hochauflösender-continuum source Graphitrohr Molekülabsorptionsspektrometrie (HR-CS-GFMAS) - Screening von Organofluor im Oberflächenwasser N2 - Vortrag zur Entwicklung von Organo-Fluor Summenparametermethoden auf Basis der HR-CS-GFMAS für die Umweltanalytik T2 - PerFluSan Treffen; 1. Workshop zur PFC-Sanierung_Schwerpunkt Analytik CY - Karlsruhe, Germany DA - 25.06.2019 KW - Hochauflösende-continuum source Graphitrohr Molekülabsorptionsspektrometrie (HR-CS-GFMAS) KW - Fluorierte Organische Verbindungen KW - Umweltanalytik KW - (Organisch gebundenes) Fluor-Summenparameter PY - 2019 AN - OPUS4-48632 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Duwe, M. T1 - Curved-surface metrology by imaging Mueller-matrix ellipsometry N2 - Outline - maging ellipsometry: oncept and setup - Basic theory: ellipsometry on tilted/curved surfaces - Geometric considerations - Tilt-induced cross-polarization - Application: coating analysis on microlensarray - Mueller-Matrix Imaging - Conversion to Delta-Psi Image - Layer-thickness of ITO coating T2 - 8th International conference on spectroscopic CY - Barcelona, Spain DA - 26.05.2019 KW - Spectroscopic Imaging KW - Mueller-Matrix Ellipsometry KW - Curved surfaces PY - 2019 AN - OPUS4-48366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - Fantastic guided modes and how to find them N2 - Ultrasonic guided waves (UGW) have been shown to be suitable for non-destructive testing (NDT) and structural health monitoring (SHM) of many engineering structures. Development of a technique based on UGWs requires careful understanding obtained through modelling and analysis of wave propagation and mode-damage interaction due to their dispersion and multimodal character. This presentation will provide insights into the Scaled Boundary Finite Element Method and its applicability for tackling wave propagation problems. Features and limitations of the SBFEM will be presented on an example of a multi-layered plate structure consisting of isotropic and anisotropic materials bonded together. You will be guided through the process of picking up the wave modes for your application. Starting from the calculation of dispersion curves and mode shapes to the analysis of wave propagation and mode-damage interaction. The main highlight of the presentation lies in the ability to detect damage in a certain layer depending on the mode used. The resulting deeper understanding of the wave propagation in multi-layered structures is the key to further developments of NDT and SHM for engineering structures consisting of multiple layers. T2 - Von CEA Eingeladener Vortrag CY - Saclay, France DA - 07.06.2019 KW - Structural Health Monitoring KW - Pressure tanks KW - Hydrogen storage KW - Natural gas KW - Composites KW - Scaled Boundary Finite Element Method PY - 2019 AN - OPUS4-48375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Multiple glass transitions in dipole functionalized discotic liquid crystals N2 - A selected series of dipole functionalized triphenylene-based discotic liquid crystals (DLCs) was synthesized and investigated in a systematic way to reveal the phase behavior and molecular dynamics. The later point is of particular importance to understand the charge transport in such systems which is the key property for their applications such as organic field effect transistors, solar cells or as nanowires in molecular electronics, and also to tune the properties of DLCs. The mesomorphic properties were studied by polarizing optical microscopy, X-ray diffraction, and differential scanning calorimetry, which were compared to the corresponding unfunctionalized DLC. The molecular dynamics were investigated by a combination of state-of-the-art broadband dielectric spectroscopy (BDS) and advanced calorimetry such as fast scanning calorimetry (FSC) and specific heat spectroscopy (SHS). Besides localized fluctuations, surprisingly multiple glassy dynamics were detected for all materials for the first time. Glassy dynamics were proven for both processes unambiguously due to the extraordinary broad frequency range covered. The α1-process is attributed to fluctuations of the alky chains in the intercolumnar space because a polyethylene-like glassy dynamics is observed. This corresponds to a glass transition in a confined three-dimensional space. The α2-process found at temperatures lower than α1-process, is assigned to the fluctuation of translational in plane movements of the triphenylene core inside distorted columns. This can be considered as a glass transition of a one-dimensional fluid. Therefore, obtained results are of general importance to understand the glass transition, which is an unsolved problem of condensed matter science. T2 - Workshop on dynamics in dissordered materials CY - Dortmund, Germany DA - 25.08.2019 KW - Discotic Liquid Crystals PY - 2019 AN - OPUS4-48778 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ali, Naveed Zafar A1 - Campbell, B. J. A1 - Jansen, M. T1 - Topotactic, pressure-driven, diffusion-less phasetransition of layered CsCoO2to a stuffedcristobalite-type configuration N2 - CsCoO2, featuring a two-dimensional layered architecture of edge- and vertex-linked CoO4tetrahedra, is subjected to a temperature-driven reversible second-order phase transformation at 100 K, which corresponds to a structuralrelaxation with concurrent tilting and breathing modes of edge-sharing CoO4tetrahedra. In the present investigation, it was found that pressure induces a phase transition, which encompasses a dramatic change in the connectivity ofthe tetrahedra. At 923 K and 2 GPa, beta-CsCoO2 undergoes a first-order phasetransition to a new quenchable high-pressure polymorph,alpha-CsCoO2. It is built up of a three-dimensional cristobalite-type network of vertex-sharing CoO4 tetrahedra. According to a Rietveld refinement of high-resolution powderdiffraction data, the new high-pressure polymorph gamma-CsCoO2 crystallizes in the tetragonal space groupI41/amd:2 (Z= 4) with the lattice constants a= 5.8711 (1) and c= 8.3214 (2) A, corresponding to a shrinkage in volume by 5.7% compared with the ambient-temperature and atmospheric pressure-CsCoO2polymorph.The pressure-induced transition (beta>gamma) is reversible;-CsCoO2 stays metastable under ambient conditions, but transforms back to the-CsCoO2structure upon heating to 573 K. The transformation pathway revealed isremarkable in that it is topotactic, as is demonstrated through a clean displacive transformation track between the two phases that employs the symmetry oftheir common subgroupPb21a(alternative setting of space group No. 29 that matches the conventional-phase cell). KW - Structures under extreme conditions KW - Topotactic phase transitions KW - Transformation pathways KW - Oxocobaltates KW - Cristobalite frameworks PY - 2019 DO - https://doi.org/10.1107/S2052520619008436 SN - 2052-5206 VL - 75 IS - 4 SP - 704 EP - 710 PB - International Union of Crystallography AN - OPUS4-48782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yildirim, Arda A1 - Bühlmeyer, A. A1 - Hayash, S A1 - Haenle, J. C. A1 - Sentker, K. A1 - Krause, Christina A1 - Huber, Patrick A1 - Laschat, Sabine A1 - Schönhals, Andreas T1 - Multiple glassy dynamics in dipole functionalized triphenylene-based discotic liquid crystals revealed by broadband dielectric spectroscopy and advanced calorimetry – assessment of the molecular origin N2 - A selected series of dipole functionalized triphenylene-based discotic liquid crystals (DLCs) was synthesized and investigated in a systematic way to reveal the phase behavior and molecular dynamics. The later point is of particular importance to understand the charge transport in such systems which is the key property for their applications such as organic field-effect transistors, solar cells or as nanowires in molecular electronics, and also to tune the properties of DLCs. The mesomorphic properties were studied by polarizing optical microscopy, X-ray diffraction, and differential scanning calorimetry, which were compared to the corresponding unfunctionalized DLC. The molecular dynamics were investigated by a combination of state-of-the-art broadband dielectric spectroscopy (BDS) and advanced calorimetry such as fast scanning calorimetry (FSC) and specific heat spectroscopy (SHS). Besides localized fluctuations, surprisingly multiple glassy dynamics were detected for all materials for the first time. Glassy dynamics were proven for both processes unambiguously due to the extraordinary broad frequency range covered. The a1-process is attributed to fluctuations of the alky chains in the intercolumnar space because a polyethylene-like glassy dynamics is observed. This corresponds to a glass transition in a confined three-dimensional space. The a2-process found at temperatures lower than a1-process, is assigned to small scale rotational and/or translational in plane fluctuations of the triphenylene core inside distorted columns. This can be considered as a glass transition in a one-dimensional fluid. Therefore, obtained results are of general importance to understand the glass transition, which is an unsolved problem of condensed matter science. KW - Discotic Liquid Crystals KW - Broadband dielectric spectroscopy KW - Flash DSC KW - Specific heat spectroscopy PY - 2019 DO - https://doi.org/10.1039/c9cp03499d SN - 1463-9076 VL - 21 IS - 33 SP - 18265 EP - 18277 PB - RSC AN - OPUS4-48739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munasir, A1 - Triwikantoro, A1 - Zainuri, M. A1 - Bäßler, Ralph A1 - Darminto, T1 - Corrosion Polarization Behavior of Al-SiO2 Composites in 1M NaCl and Related Microstructural Analysis N2 - The composites combining aluminum and silica nanoparticles with the addition of tetramethylammonium hydroxide (Al-SiO2(T)) and butanol (Al-SiO2(B)) as mixing media have been successfully fabricated. Corrosion behavior of Al-SiO2 composites before and after exposure in 1M NaCl solution was examined using potentiodynamic polarization (Tafel curve analysis). The study was also equipped with scanning electron microscopy (SEM), energy dispersive X-ray (EDX), and X-ray diffraction (XRD) investigations. Before exposure, Al-SiO2(T) exhibited the best corrosion resistance. Performance improvement was indicated by Al-SiO2(B) up to 10 times better than Al-SiO2(T) after exposure. The increased SiO2 content did not significantly enhance the corrosion resistance of the composites. The Al-SiO2 composites with 5% SiO2 content showed very high corrosion resistance (as the optimum composition). Furthermore, pitting corrosion was observed in the Al-SiO2 composites, indicated by the formation of corrosion products at grain boundaries. The product was affected by the presence of SiO2 in the Al matrix and the NaCl environment at 90 °C (approach to synthetic geothermal media: Na+, Cl, H+, OH-). Our study revealed the presence of γ-Al2O3, γ-Al(OH)3, and Al(OH)2Cl as the dominant corrosion products. KW - Al-Composite KW - Corrosion KW - Corrosion rate KW - SiO2 Nanoparticle KW - Tafel Plot PY - 2019 DO - https://doi.org/10.5829/ije.2019.32.07a.11 SN - 1025-2495 SN - 1735-9244 VL - 7 IS - 32 SP - 982 EP - 990 PB - Materials and Energy Research Center AN - OPUS4-48742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Huan, Y. A1 - Gojani, Ardian A1 - Gornushkin, Igor B. A1 - Wang, X. A1 - Liu, D. A1 - Rong, M. T1 - Dynamics of laser-induced plasma splitting N2 - The dynamics of laser-induced plasma plume splitting is investigated using spatiotemporal plasma imaging and spectrometry in this paper. Plasma plume splitting into fast and slow components is clearly observed using plasma optical emission as time evolves. The spatial resolved plasma spectra are used to investigate the plasma species distribution, which reveals that the charged copper ions, which radiate at wavelength range 485 nm - 504 nm, are merely present in the fast component. In order to further interpret the mechanism, the pressure-dependent and laser energy-dependent plume splitting are analyzed. Based on the results, the charge separation field is proposed to explain this phenomenon. This work can be of importance for such areas as laser induced breakdown spectroscopy, laser-induced ion source formation, pulse laser deposition, film growth, and nanoscale synthesis. KW - Spectroscopy KW - Laser induced plasma KW - Splitting KW - Imaging PY - 2020 DO - https://doi.org/10.1016/j.optlaseng.2019.105832 SN - 0143-8166 VL - 124 SP - 1 EP - 5 PB - Elsevier CY - Amsterdam AN - OPUS4-48746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst A1 - Abraham, Odile A1 - Larose, Eric T1 - A review on ultrasonic monitoring of concrete: coda wave interferometry and beyond N2 - The propagation of ultrasonic waves in concrete is affected by its micro- and macro-structure, geometry and properties as well as external influences as stress, temperature or moisture. In addition, age and degradation have a strong influence. Therefore, Ultrasound has been used to monitor concrete samples and structures since decades. However, early applications using conventional techniques as time-of flight or changes in amplitudes have been limited to detect changes in a late stage close to serviceability or ultimate load states. Around 2000, several new, more sensitive techniques adopted from geophysics or other field of material sciences have been introduced to research in ultrasonic monitoring of concrete. The most discussed methodologies are coda wave interferometry, a technique which allows to detect very subtle changes from repeated ultrasonic measurements. Nonlinear acoustic techniques help to identify e. g. cracks even in an inhomogeneous background. Both techniques can be combined. This paper reviews methods and results achieved so far on the laboratory scale and with full scale models the directions for future research and application is given as well. T2 - QNDE 2019 CY - Portland, OR, USA DA - 14.07.2019 KW - Ultrasound KW - Coda wave interferometry KW - Concrete KW - Nonlinear KW - Monitoring PY - 2019 SP - Paper 1234 AN - OPUS4-48686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Johann, Sergej A1 - Wu, Cheng-Chieh T1 - 3D-Gestalts- und -Verformungsmessung - Anwendungsbeispiele N2 - Der Fokus des Arbeitsfelds ist die messtechnisch fundierte Anwendung der 3D-Verfahrenskombination zur Lösung vielfältiger Messaufgaben mit optimaler Datenqualität für interne und externe Kunden. Das setzt insbesondere eine jeweils problembezogene Messmethodik voraus. Dazu setzen wir kameragestützte 3D-Koordinatenmessverfahren ein, die auf dem fotogrammetrischen Prinzip der Bildtriangulation beruhen. Darunter fallen folgende miteinander flexibel kombinierbare Verfahrensmodifikationen: Mehrbildfotogrammetrie, Messadapter für Geometriemerkmale, Streifenprojektionsverfahren, statische bis hochdynamische Stereofotogrammetrie auf Punktebasis oder aufgabenangepasster Oberflächenmuster und mechanisch-optische Taster. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures (SMAR 2019) CY - Potsdam, Germany DA - 27.08.2019 KW - 3D-Verformungsmessung KW - Koordinatenmessung KW - Verschiebungsfeld PY - 2019 AN - OPUS4-48791 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Uncertainties in Secondary Fluorescence Correction in EPMA N2 - Secondary fluorescence is an inevitable effect that has to be taken into account in any algorithm for quantitative electron probe microanalysis (EPMA) as an additional correction. Moreover, secondary fluorescence worsens spatial resolution of EPMA, as discussed once more in two recent papers. Secondary fluorescence is excited both by characteristic radiation and by the X-ray continuum. In most cases the correction is small. There are, however, cases, e.g. the determination of low heavy metal concentration in a light matrix, where the contribution of secondary fluorescence exceeds 10% of the measured X-ray line intensity. For secondary fluorescence correction the measured X-ray line intensity has to be divided by the correction factor (1+I_flchar/I_p +I_flcont/I_p )≈(1+I_flchar/I_p )(1+I_flcont/I_p ) in order to get those intensity I_p, which is excited only by the primary electrons and enables the determination of specimen composition. I_flchar and I_flcont mean the calculated characteristic and continuums fluorescence intensities. In order to get the intensity of fluorescence radiation, the absorption of the exciting radiation in the specimen, the photoionization probability and the self-absorption of the emitted line must be calculated. This can be performed in a straightforward way. The critical quantity is the X-ray yield of the exciting atoms in case of fluorescence by characteristic radiation and the bremsstrahlung yield of the specimen in case of continuum fluorescence. In the former case it is reasonable to apply the same physical model to calculate I_flchar and I_p. T2 - Microscopy & Microanalysis 2019 CY - Portland, OR, USA DA - 03.08.2019 KW - EPMA KW - Secondary fluorescence KW - Uncertainties KW - X-ray spectrometry KW - Fluorescence correction PY - 2019 AN - OPUS4-48673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Introduction meeting PCA - Analysis of the operation of accreditation bodies in Europe N2 - The long-term goal of the benchmarking project for European accreditation bodies is twofold: First of all, the project is supposed to help the European accreditation attending bodies to improve their processes by identifying best practices and by learning from others. Possibly Secondly, the results of the analysis can be used by the European Cooperation for Accreditation (EA) to identify differences in the operation of the European accreditation bodies and based on this knowledge to promote harmonization of accreditation activities in Europe. T2 - Kick-off at PCA, Warsawa CY - Warsawa, Poland DA - 11.06.2019 KW - Accreditation KW - Benchmarking PY - 2019 AN - OPUS4-48678 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Introduction meeting NAH - Analysis of the operation of accreditation bodies in Europe N2 - The long-term goal of the benchmarking project for European accreditation bodies is twofold: First of all, the project is supposed to help the European accreditation attending bodies to improve their processes by identifying best practices and by learning from others. Possibly Secondly, the results of the analysis can be used by the European Cooperation for Accreditation (EA) to identify differences in the operation of the European accreditation bodies and based on this knowledge to promote harmonization of accreditation activities in Europe. T2 - Kick-off at NAH, Budapest CY - Budapest, Hungary DA - 19.06.2019 KW - Accreditation KW - Benchmarking PY - 2019 AN - OPUS4-48679 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Introduction meeting DANAK - Analysis of the operation of accreditation bodies in Europe N2 - The long-term goal of the benchmarking project for European accreditation bodies is twofold: First of all, the project is supposed to help the European accreditation attending bodies to improve their processes by identifying best practices and by learning from others. Possibly Secondly, the results of the analysis can be used by the European Cooperation for Accreditation (EA) to identify differences in the operation of the European accreditation bodies and based on this knowledge to promote harmonization of accreditation activities in Europe. T2 - Kick-off at DANAK, Copenhagen CY - Copenhagen, Denmark DA - 27.06.2019 KW - Accreditation KW - Benchmarking PY - 2019 AN - OPUS4-48680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Introduction meeting CAI - Analysis of the operation of accreditation bodies in Europe N2 - The long-term goal of the benchmarking project for European accreditation bodies is twofold: First of all, the project is supposed to help the European accreditation attending bodies to improve their processes by identifying best practices and by learning from others. Possibly Secondly, the results of the analysis can be used by the European Cooperation for Accreditation (EA) to identify differences in the operation of the European accreditation bodies and based on this knowledge to promote harmonization of accreditation activities in Europe. T2 - Kick-off at CAI, Prag CY - Prag, Czech Republic DA - 07.07.2019 KW - Accreditation KW - Benchmarking PY - 2019 AN - OPUS4-48681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Preparation meeting at the EA General AssemblyI - Analysis of the operation of accreditation bodies in Europe N2 - The 2nd benchmarking round of the project “Analysis of the operation of accreditation bodies in Europe” is envisaged for 2019. In contrast to the 1st round, the BAM will conduct this benchmarking solely without the DAkkS as partner. The 2nd round will make use of the Process Maturity Benchmarking Tool PMBT, the management tool which was developed for and applied in the 1st round. The PMBT will be optimized in advance based on the suggestions and experiences gathered in the benchmarking conducted in 2016. To discuss this adjustment a preparation meeting was conducted in the course of the EA GA in Rome. T2 - General Assembly of the Europeam Co-operation for Accreditation (EA) CY - Rome, Italy DA - 21.05.2019 KW - Accreditation KW - Benchmarking PY - 2019 AN - OPUS4-48682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Faes, W. A1 - Lecompte, S. A1 - van Bael, J. A1 - Salenbien, R. A1 - Bäßler, Ralph A1 - Bellemans, I. A1 - Cools, P. A1 - de Geyter, N. A1 - Morent, R. A1 - Verbeken, K. A1 - de Paepe, M. T1 - Corrosion behaviour of different steel types in artificial geothermal fluids N2 - Geothermal energy is an interesting alternative to polluting fossil energy sources. Therefore, in Belgium, two wells have been drilled for a deep geothermal power plant. However, the environment to which the installations are exposed is challenging. The geothermal brine has 165 g/l total dissolved solids (of which 90% are sodium and chlorine) and the production temperature can be up to 130 °C. To assess their suitability to be used in a geothermal power plant, the corrosivity of the artificial brine to three common construction materials was investigated with exposure and electrochemical tests. The metals under consideration are a low-alloyed carbon steel (S235JR), an austenitic stainless steel (UNS S31603) and a duplex stainless steel (UNS S31803). The carbon steel, that was found to corrode uniformly, could be considered as a constructional material if a sufficient wall thickness is chosen. The austenitic stainless steel and the duplex stainless steel demonstrate very low uniform corrosion rates. They are however susceptible to pitting and crevice corrosion. To guarantee safe operation of the geothermal power plant, the susceptibility of the alloys to stress corrosion cracking should be tested and in situ experiments should be performed. KW - Geothermal energy KW - Corrosion KW - Carbon dioxide KW - Carbon steel KW - Stainless steel PY - 2019 DO - https://doi.org/10.1016/j.geothermics.2019.05.018 SN - 0375-6505 VL - 82 IS - 11 SP - 182 EP - 189 PB - Elsevier Ltd. AN - OPUS4-48759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - The Dark Side of Science N2 - The Joint Summer School of the two Marie Skłodowska-Curie Innovative Training Networks (ITN) “BioCapture” and “GlycoImaging”, funded by the EU within the Horizon 2020 framework programme, which are both devoted to the development of new methods for cancer biomarker and cancer cell detection, will take place at the Adlershof Campus of BAM. 19 Early stage researchers of both projects will convene, discuss their own science and plan future collaborative research. Training in scientific writing (instructor: Luita Spangler, Free University of Berlin), an employability workshop (Antti Kapanen, University of Applied Sciences Berlin) and first contacts with the “dark side of science” (Brian R. Pauw, BAM) will complement the programme of the summer school. T2 - EU-ITN-Summer School CY - Adlershof, Berlin, Germany DA - 26.08.2019 KW - Scientific communication KW - Scientific rigour KW - Scientific method PY - 2019 AN - OPUS4-48760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Analysis of elemental composition and porosity of mesoporous iridium titanium mixed oxide thin films for energy application by SEM/EDS N2 - Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution we characterize thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with energy dispersive X-ray spectroscopy (EDS) at an SEM. T2 - Microscopy & Microanalysis 2019 Meeting CY - Portland, OR, USA DA - 04.08.2019 KW - Mesoporous mixed metal oxide films KW - SEM/EDS/STRATAGem KW - EPMA KW - Ellipsometry KW - NanoSIMS PY - 2019 AN - OPUS4-48767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Hodoroaba, Vasile-Dan A1 - Hertwig, Andreas A1 - Kotil, L. A1 - Kraehnert, R. T1 - Analysis of elemental composition and porosity of mesoporous iridium titanium mixed oxide thin films for energy application by SEM/EDS N2 - Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution we characterize thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with energy dispersive X-ray spectroscopy (EDS) at an SEM. KW - Electron probe microanalysis (EPMA) KW - Iridium-titanium mixed oxides KW - Spectroscopic ellipsometry KW - Mesoporous thin films KW - NanoSIMS PY - 2019 DO - https://doi.org/10.1017/S1431927619009589 SN - 1431-9276 (Print) SN - 1435-8115 (Online) VL - 25 IS - S2 (August) SP - 1770 EP - 1771 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-48768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Analysis of elemental composition and porosity of mesoporous IrOx-TiOx thin films by SEM/EDS N2 - Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution we characterize thin mesoporous iridium-titanium mixed oxide film properties by Electron Probe Microanalysis (EPMA) with energy dispersive X-ray spectroscopy (EDS) at an SEM. T2 - EMAS 2019 - 16th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS CY - Trondheim, Norway DA - 19.05.2019 KW - Electron probe microanalysis (EPMA) KW - Iridium-titanium mixed oxides KW - Spectroscopic ellipsometry KW - Mesoporous thin films PY - 2019 AN - OPUS4-48769 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Dell’Aglio, M. A1 - Motto-Ros, V. A1 - Pelascini, F. A1 - De Giacomo, A. T1 - Investigation on the material in the plasma phase by high temporally and spectrally resolved emission imaging during Pulsed Laser Ablation (PLAL) in Liquid for NPs production and consequent considerations on NPs formation N2 - In this paper experimental temperature and density maps of the laser induced plasma in water during Pulsed Laser ablation in Liquid (PLAL) for the production of metallic nanoparticles (NPs) has been determined. A detection system based on the simultaneous acquisition of two emission images at 515 and 410 nm has been constructed and the obtained images have been processed simultaneously by imaging software. The results of the data analysis show a variation of the temperature between 4000 and 7000 K over the plasma volume. Moreover, by the study of the temperature distribution and of the number densities along the plasma expansion axis it is possible to observe the condensation zone of the plasma where NPs can be formed. Finally, the time associated to the electron processes is estimated and the plasma charging effect on NPs is demonstrated. The set of observations retrieved from these experiments suggests the importance of the plasma phase for the growth of NPs and the necessity of considering the spatial distribution of plasma parameters for the understanding of one of the most important issues of the PLAL process, that is the source of solid material in the plasma phase. KW - LIBS KW - Laser induced plasma KW - Plasma modeling KW - Plasma diagnostics KW - Nanoparticle formation PY - 2019 DO - https://doi.org/10.1088/1361-6595/ab369b VL - 28 IS - 8 SP - Article Number: 085017 PB - IOP Publishing AN - OPUS4-48753 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ickert, Stefanie A1 - Beck, S. A1 - Linscheid, M. A1 - Riedel, Jens T1 - VUV Photodissociation Induced by a Deuterium Lamp in an Ion Trap N2 - Tandem mass spectrometry represents an important analytical tool to unravel molecular structures and to study the gas-phase behavior of organic molecules. Besides commonly used methods like collision-induced dissociation and electron capture or transfer dissociation, new ultraviolet light–based techniques have the potential to synergistically add to the activation methods. Here, we present a new simple, yet robust, experimental design for polychromatic activation of trapped ions using the 115–160 nm output of a commercially available deuterium lamp. The resulting continuous dissociative excitation with photons of a wide energy range from 7.7 to 10.8 eV is studied for a comprehensive set of analyte classes in both positive and negative ion modes. While being simple, affordable, compact, and of low maintenance, the new setup initiates fragmentation of most precursor ions via their known dissociation pathways. Additionally, some new fragmentation patterns were discovered. Especially, electron loss and electron capture reactions with subsequent fragmentations were observed. For oligonucleotides, peptides, carbohydrates, and organic dyes, in comparison to collision-induced dissociation, a significantly wider fragment distribution was obtained, resulting in an information increase. Since the individual photons carry enough energy to post-ionize the nascent fragments, a permanent vacuum ultraviolet light exposure inside the ion trap potentially goes along with a general increase in detection capability. KW - Fragmentation activation KW - Vacuum ultraviolet (VUV) light KW - Mass spectrometry KW - Tandem MS PY - 2019 DO - https://doi.org/10.1007/s13361-019-02282-8 SN - 1044-0305 VL - 30 IS - 10 SP - 2114 EP - 2122 PB - Springer Nature CY - Heidelberg AN - OPUS4-48756 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beck, Joana T1 - Review: Fitz's Atlas™of coating surveys N2 - Fitz's Atlas of coating surveys is designed as loose‐leave binder with a resistant cover that not only provides the possibility of updating the Atlas easily but also makes it practicable for on‐site use. This binder is well structured by sheet dividers with tabs for each of the 16 chapters. All in all, this atlas supports the surveyor by giving practicable hints and advice, lists and pictures to prepare and conduct investigations and write surveys. KW - Coating KW - Survey KW - Protection PY - 2019 DO - https://doi.org/10.1002/maco.201970084 SN - 1521-4176 SN - 0947-5117 VL - 70 IS - 8 SP - 1508 PB - Wiley VCH-Verlag CY - Weinheim AN - OPUS4-48720 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska T1 - Towards predictor development for assessing structural integrity of components made from wood materials using Acoustic Emission monitoring and signal analysis N2 - Against the background of sustainable resource management and efficiency, wood-based materials are currently experiencing a revival and, among others, plywood, Laminated Veneer Lumber and glued laminated timber are becoming increasingly more important in the building sector. Even though these materials are so-called engineered products, the element wood is naturally grown with intrinsic variability in mechanical properties and requires professional handling on-site. Otherwise, load-bearing structures made of wood materials may entail certain risks. Critical situations can, in principle, be avoided by implementing a structural health monitoring system into components or structures made from wood material. The aim is to indicate accumulation of mechanical damage and to eliminate or at least significantly reduce the risk of unexpected failure. Toward this purpose, the failure behavior of several layered wood materials under quasi-static tension was investigated in laboratory-scale experiments by means of acoustic emission (AE) measurement. Based on spectral analysis and pattern recognition, two classes of AE signals are identified for each investigated lay-up that are characterized by either low or high frequency contents in the respective power spectra. AE activity and intensity of both signal classes are analyzed, striving for predictors appropriate for AE monitoring concepts. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures CY - Potsdam, Germany DA - 27.08.2019 KW - Wood materials KW - Acoustic Emission KW - Structural integrity PY - 2019 AN - OPUS4-48802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Maiwald, Michael A1 - Klaer, R.-H. A1 - Wagner, A. ED - Kockmann, N. T1 - 100 % Digital in der Prozessindustrie Tutzing-Symposion Teil 3: Intelligente Nutzung von Daten und Bausteinen der Digitalisierung N2 - Digitalisierung und Industrie 4.0 verändern komplette Geschäftsmodelle, heben neue Effizienzpotenziale und stärken die Wettbewerbsfähigkeit. Auf dem 57. Tutzing-Symposion vom 15.–18.04.2018 wurde mit Vorträgen und Kreativworkshops erkundet, welche speziellen Anforderungen die Prozessindustrie hat, welche digitalen Innovationen bereits umgesetzt wurden und wo noch Handlungsbedarf besteht. Ein Workshop befasste sich mit den Themenfeldern Datenkonzepte, Datenanalyse, Big Data und künstliche Intelligenz. KW - Prozessindustrie KW - Digitalisierung KW - Industrie 4.0 KW - Datenanalyse KW - Künstliche Intelligenz PY - 2019 SN - 1436-2597 VL - 22 SP - 14 EP - 19 PB - Wiley-VCH CY - Weinheim AN - OPUS4-48838 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - DICONDE für ET N2 - Evaluierung der Eignung von DICONDE zur Speicherung von Wirbelstromprüfdaten im Kontext der Industrie/ZfP 4.0. T2 - 3. Sitzung des DGZfP FA ZfP 4.0 UA Schnittstellen CY - Bochum, Germany DA - 28.08.2019 KW - Wirbelstromprüfung KW - DICONDE KW - ZfP 4.0 KW - Industrie 4.0 PY - 2019 AN - OPUS4-48839 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul T1 - Acoustic-structure interaction in the scaled boundary finite element method for primsatic geometries N2 - Due to the short wavelength compared to the dimensions of the structure, the simulation of ultrasonic waves is still a challenging task. A numerical method well suited for this purpose is the semi-analytical Scaled Boundary Finite Element Method (SBFEM). When applying this method, only the boundary of a computational domain is discretized using finite elements, while the interior is described by an analytical ansatz. Hence, the number of degrees of freedom is reduced significantly compared to the classical Finite Element Method (FEM). In recent years, a particular formulation of the SBFEM for the simulation of ultrasonic guided waves was developed. The method constitutes an efficient algorithm for prismatic structures of arbitrary length, such as plates, pipes, or beams. Wave propagation phenomena in such structures can be modeled for isotropic and anisotropic inhomogeneous waveguides. Even though the method is an efficient tool for the simulation of guided waves in solid media, a reliable model for the simulation of acoustic wave propagation in fluids as well as acoustic-structure interaction in terms of SBFEM is still missing. In principle, the fluid can be described by a displacement-based formulation and thus be implemented in existing SBFEM algorithms for solid bodies. However, due to the discretization with classical finite elements, spurious modes occur, which cannot be separated from the physical modes straightforwardly. The spurious modes can be suppressed using a penalty parameter. Although very accurate results were achieved for some problems, this procedure has been proven unreliable for certain cases. For this reason, we propose a different approach in this contribution. We employ a pressure model to simulate the acoustic behavior of fluids. The implementation of the pressure model results in a higher effort due to the necessity of incorporating coupling terms, but it presents a stable alternative without spurious modes. The accuracy of the method is demonstrated in comparison with analytical solutions and results obtained using the FEM. T2 - GACM 2019 CY - Kassel, Germany DA - 28.08.2019 KW - Scaled Boundary Finite Element Method KW - Guided Waves KW - Acoustic-structure interaction PY - 2019 AN - OPUS4-48846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Plasma Germany, Fachausschuss Normung, Berichtszeitraum Herbst 2018 – Frühjahr 2019 N2 - Der Vortrag gibt den aktuellen Stand der Normung im Bereich der Oberflächentechnik insbesondere der Oberflächenanalytik und der Oberflächenmess- und -prüftechnik wider. Vorgestellt wird der Status technischer Berichte, Normenentwürfe und Normen u.a. zur Bewertung von Auflösung und Schärfe mit strahlbasierten Methoden im Nanometer- und Mikrometerbereich, zur Messung von Schichtdicken und Nanopartikeln in kritischen Dimensionen einschließlich Größen- und Formverteilungen mittels REM, zur Messung der Schichtdicke von Nanomaterialien und zur Klassifizierung von Kohlenstoffschichten mittels Ellipsometrie, zur Standardisierung der Ellipsometrie, zur Kalibrierung von Konfokalmikros-kopen für die Formmessung, zur linear elastisch dynamischen instrumentierten Eindringprüfung, zur Messung der flächenbezogenen Masse mittels AAS und ICP, zur Schichtpotentialmessung von Mehrfach-Nickelschichten, zur Schichtdicken und Flächen-widerstandsbestimmung sowie zur Bestimmung der Schichthaftung mittels Zentrifugentechnologie. T2 - Plasma Germany, Fachausschuss Normung, CY - Karlsruhe, Germany DA - 09.04.2019 KW - Stand der Normung KW - Oberflächenanalytik KW - Oberflächenmesstechnik KW - Qualitätssicherung PY - 2019 AN - OPUS4-48874 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Optical properties of different types of luminescent nanocrystals at the ensemble and single emitter level N2 - Applications of luminescent nanomaterials like semiconductor nanocrystals (QDs) and lanthanide-based upconversion nanocrystals (UCNPs) in the life sciences such as bioimaging studies or their use as reporter in assays call for a correlation of the photoluminescence (PL) properties of these nanomaterials on ensemble and single particle levels. This is particularly relevant within the context of continuously decreasing detection limits. Aiming at optimum nanomaterials for spectroscopic and microscopic applications, we examine the optical properties of QDs like II/VI QDs and cadmium-free AgInS2/ZnS QDs (AIS/ZnS) and UCNPs of different chemical composition, size, and particle architecture for ensembles and single particles. This includes PL spectra, PL quantum yields (ΦF), brightness values, blinking behavior, and PL decay kinetics. For UCNPs with their nonlinear spectrally converted PL excited by sequential multiphoton absorption, these measurements were also done as a function of excitation power density (P). Special emphasis is dedicated to the performance parameters ΦF and brightness, that determine signal size and provide a measure for nanocrystal quality.[1-5] Systematic studies of the excitation energy dependence (EED) [6] of the PL properties of II/VI and ternary AgInS2/ZnS QDs reveal the potential of this relatively simple method for providing insights into the electronic energy structure of QDs. The intrinsic nature of the inhomogeneous broadening of the PL bands of AIS/ZnS QDs was confirmed by single particle spectroscopy.[5] By combining P-dependent integration spectroscopy and single particle measurements of UCNPs, using a new custom-made setup, consisting of different lasers, an inverted microscope, different detectors, and an AFM, we could study the P-dependent optical properties of these nonlinear emitters from ~10 W/cm2 up to ~105 W/cm2. These results provide optimum dopant ion concentrations for bioanalytical, spectroscopic, and microscopic applications of UCNP. Acknowledgement. Financial support by grants RE1203/12-3 and RE1203/20-1 (support of F. Weigert, L. Dhamo, and F. Frenzel) from German Research Council (DFG) is acknowledged. T2 - 17th Internatinal Congress on Photobiology CY - Barcelona, Spain DA - 25.08.2019 KW - Nanoparticle KW - Quantum dot KW - Fluorescence KW - Single particle spectroscopy KW - Mechanism KW - Lifetime KW - Exciton KW - Ternary quantum dot KW - AIS QD KW - Synthesis KW - Shell KW - Surface chemistry PY - 2019 AN - OPUS4-48877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - Human Factors bei der Ultraschall-Handprüfung von Radsatzwellen mit Längsbohrung in der Ausbildung N2 - Ziel dieser Arbeit war es, menschliche und organisatorische Einflussfaktoren auf die Ultraschall-Handprüfung von Radsatzwellen zu identifizieren, um Empfehlungen zur Optimierung der Ausbildung auszuarbeiten. Dazu, wurden prüfungsbezogene Risiken in der Praxis mittels Fehlzustandsart- und –auswirkungsanalyse (FMEA) analysiert sowie von den Prüfern empfundene Probleme während der Ausbildung und in der Praxis mittels Fragebogen identifiziert. Die Ergebnisse der FMEA haben gezeigt, dass während der gesamten ZfP-Prozesses Fehler auftreten können, für die Gegenmaßnahmen getroffen und implementiert werden sollten. Zu den vorgeschlagenen Gegenmaßnahmen zählen: Optimierung der Organisation, Prüftechnik, Dokumentation, Ausbildung, Arbeitsbedingungen und des Prüfprozesses. Die Auswertung der Fragebögen zeigte eine relativ große Zufriedenheit mit den zur Ausbildung bereitgestellten Prüfunterlagen. Hinsichtlich der Praxis tendierten die Antworten der Prüfer in Richtung Verbesserung der Prüfunterlagen, Arbeitsbedingungen vor Ort, Arbeitsvorbereitung im Werk und Anweisung/fachlichen Einweisung durch die Prüfaufsichten. Aus den Hinweisen und Erkenntnissen wurden einige Empfehlungen zur Optimierung der Prüfunterlagen, Kompetenzen und des Prüfprozesses erarbeitet. Es wurde empfohlen, die Qualität der Prüfunterlagen systematisch zu untersuchen und zusammen mit den Prüfern zu verbessern, um Missverständnisse bei der Nutzung der Prüfunterlagen zu minimieren und somit Fehler bei der Prüfung zu vermeiden. Eine weitere Empfehlung betraf die Entwicklung und das Angebot neuer Ausbildungsmodule zur Weiterbildung von Prüfaufsichten und Führungskräften, um ein Grundverständnis über Einflüsse auf die Qualität der Zerstörungsfreien Prüfungen zu schaffen. Zur Optimierung des gesamten ZfP-Prüfprozesses wird empfohlen, die mittels FMEA erarbeitete Liste möglicher Gegenmaßnahmen in der Praxis umzusetzen. Diese Liste sollte den Verantwortlichen zur Verfügung gestellt werden, um potenziell auftretende Fehler zu erkennen und zu vermeiden. T2 - DACH Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Human Factors KW - ZfP KW - UT-Ausbildung KW - Radsatzwellen PY - 2019 AN - OPUS4-48857 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul A1 - Bulling, Jannis A1 - Prager, Jens T1 - Ultrasonic sensor based on phononic crystals N2 - An essential task in many industries, e.g. food, petrol or chemical industry, is the precise and accurate characterization of liquids. Therefore, the development of innovative in-line sensors is of great interest. New concepts based on periodic structures, so-called phononic crystals (PnCs), are an interesting idea for the design of innovative sensors. A PnC-based sensor can be designed by introducing a resonance inside a bandgap, a frequency region where no wave propagation is allowed. High-Q measurement systems using PnCs are already reported in the literature. However, existing designs cannot be implemented into a piping system directly, but need special fittings, openings or by-passes to be in contact with the liquid. To circumvent this issue, we develop a new sensor based on PnCs, which can be directly implemented as part of the piping system. For this purpose, we use a PnC consisting of hollow cylinders with a periodic change of the outer diameter. A bandgap could be found for the described geometry without fluid in simulation and measurement. However, simulations show, that a bandgap for fluid-filled cylinders can only be obtained for quasi-longitudinal modes. Hence, we propose a mode selective excitation for the sensor. T2 - ICA 2019 CY - Aachen, Germany DA - 09.09.2019 KW - Phononic crystal KW - Ultrasound PY - 2019 SN - 978-3-939296-15-7 SN - 2226-7808 SN - 2415-1599 SP - 969 EP - 976 AN - OPUS4-48860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Procop, Mathias A1 - Hodoroaba, Vasile-Dan T1 - Uncertainties in secondary fluorescence correction in EPMA N2 - Secondary fluorescence is an inevitable effect that has to be taken into account in any algorithm for quantitative electron probe microanalysis (EPMA) as an additional correction. Moreover, secondary fluorescence worsens spatial resolution of EPMA. Secondary fluorescence is excited both by characteristic radiation and by the X-ray continuum. In most cases the correction is small. There are, however, cases, e.g. the determination of low heavy metal concentration in a light matrix, where the contribution of secondary fluorescence exceeds 10% of the measured X-ray line intensity. For secondary fluorescence correction the measured X-ray line intensity has to be divided by the correction factor (1+I_flchar/I_p +I_flcont/I_p )≈(1+I_flchar/I_p )(1+I_flcont/I_p ) in order to get those intensity I_p, which is excited only by the primary electrons. I_flchar and I_flcont mean the calculated characteristic and continuums fluorescence intensities. In order to get the intensity of fluorescence radiation, the absorption of the exciting radiation in the specimen, the photoionization probability and the self-absorption of the emitted line must be calculated. The critical quantity is the X-ray yield of the exciting atoms in case of fluorescence by characteristic radiation and the bremsstrahlung yield of the specimen in case of continuum fluorescence. In the former case it is reasonable to apply the same physical model to calculate I_flchar and I_p. KW - EPMA KW - Secondary fluorescence correction KW - Uncertainties KW - Microanalysis PY - 2019 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/uncertainties-in-secondary-fluorescence-correction-in-epma/AA92E973D350A74C574067AAFB2D9044 DO - https://doi.org/10.1017/S1431927619012534 SN - 1431-9276 SN - 1435-8115 VL - 25 IS - Suppl. 2 SP - 2360 EP - 2361 PB - Cambridge University Press AN - OPUS4-48863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Plasma Germany, Fachausschuss Normung, Berichtszeitraum Frühjahr 2018 - Herbst 2018 N2 - Der Vortrag gibt den aktuellen Stand der Normung im Bereich der Oberflächen-technik insbesondere der Oberflächenanalytik und der Oberflächenmess- und -prüftechnik wider. Vorgestellt wird der Status technischer Berichte, Normenentwürfe und Normen u.a. zur Charakterisierung von funktionellen Glasoberflächen für bioanalytische Anwendungen, zur Messung der Schichtdicke von Nanomaterialien mittels Ellipsometrie, zur Kalibrierung von Interferometern und Interferenzmikroskopen für die Formmessung, zur Rockwelleindringprüfung zur Bewertung der Schicht-haftung, zu den Grundlagen der Ellipsometrie, zur Messung der Schichtdicke mittels Wirbelstromverfahren, zur Schichtpotentialmessung von Mehrfach-Nickelschichten, zu Filtern und Augenschutzgeräten gegen Laserstrahlung sowie zur Bestimmung der Schichthaftung mittels Zugversuch. T2 - Fachausschuss Normung, Herbstsitzung CY - Jena, Germany DA - 06.11.2018 KW - Stand der Normung KW - Oberflächentechnik KW - Oberflächenanalytik KW - Oberflächenmesstechnik KW - Oberflächenprüftechnik PY - 2018 AN - OPUS4-48894 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Materials research with synchrotron radiation N2 - Synchrotron radiation sources with their unique properties in terms of intensity, polarization and adjustability offer a wide range of possibilities in materials research. A basic introduction about the creation and special properties of synchrotron radiation will be given. Examples of current work at BAMline, the high-energy measuring facility of the Federal Institute for Materials Research and Testing at the synchrotron BESSY, are used to illustrate the possibilities and limitations of existing measuring methods. It will be shown how the formation of corrosion layers can be tracked, how the abrasion of implants leads to the introduction of heavy metals into the surrounding bone matrix and how the detection of smallest impurities in gold is possible by optimizing the measuring conditions. Finally, an outlook at the hardware and software developments to be expected in the coming years is given. T2 - INCT-FNA Symposium 2019 CY - Niteroi, Brazil DA - 27.05.2019 KW - Synchrotron KW - XRF KW - XANES KW - EXAFS KW - TXRF KW - Color X-ray Camera PY - 2019 AN - OPUS4-48897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fittschen, U.E.A. A1 - Möckel, R. A1 - Schreiner, M. A1 - klinger, M. A1 - Radtke, Martin A1 - Meyer, B. A1 - Guhl, S. A1 - Renno, A. A1 - Godinho, J. A1 - Gloaguen, R. A1 - Gutzmer, J. T1 - Bundling analytical capacities to understand phase formation in recycling of functional materials N2 - Transitioning from combustion engine-driven transportation to e-mobility demands a paradigm shift – from a system geared to maximize energy efficiency (i.e. fuel consumption) to a system that may be constrained by the availability of high technology (critical) metals required for electrical energy storage systems and drives. In the wake of these developments efforts in securing new resources of these metals from recycling of end-of-life products are increasing steadily. Recycling of Li-Ion batteries has recently been evaluated. The results pinpoint to a critical need for understanding slag Formation and its dependence on metal components like Mn under extreme conditions. This will allow researchers to predict optimal Operation setting and to react quickly to changing market demands (which may be Li or Co at one point but may also shift to Ni or rare earth elements (REE)). The long-term goal is to control the formation of specific phases in slags allowing for a Maximum yield of elements of interest and optimal recovery in the separation processes that follows. The combination of data on the physical micro structure and local chemistry of the multi-Phase products during and after processing will help to understand and derive thermodynamic and kinetic data on its formation. In this paper we are giving an overview on the analytical challenges and approaches to provide robust data on local element concentration and species (especially Mn which is a common component of next generation Li-ion batteries cathodes), spanning the dimensions from the nanometer scale to the bulk material. The complementary interactions of X-rays and electrons make them ideal probes to collect Interface and “in-depth” information. Before- and -after studies as well as in situ structural changes and Phase (trans)formation, changes in elemental and elemental species (e.g. oxidation state) distribution may be tracked by X-ray diffraction (XRD), X-ray fluorescence microscopy and X-ray Absorption spectroscopy. The application of such advanced analytical tools will not only provide essential clues during early lab-based experiments towards the development of new recycling technologies, but may also be deployed for on-line and in-line monitoring of industrial processes. KW - Synchrotron KW - XANES KW - Slags KW - Battery PY - 2019 DO - https://doi.org/10.4028/www.scientific.net/MSF.959.183 SN - 1662-9752 VL - 959 SP - 183 EP - 190 PB - Trans Tech Publ. AN - OPUS4-48900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - Human-machine interaction in the era of NDT 4.0 N2 - This presentation discusses industry 4.0 from the perspective of human machine interaction (HMI). Based on available literature the changes, new demands and possible problems related to people’s jobs as a result of increased digitisation and use of artificial intelligence are addressed. Combining literature with own experience in non-destructive testing (NDT), the author addresses the possible challenges and chances for the NDT personnel in the era of NDT 4.0. T2 - The BINDT Aerospace Event 2019 CY - National Composites Centre NCC, Bristol, UK DA - 09.04.2019 KW - ZfP 4.0 KW - Human Factors KW - NDT 4.0 PY - 2019 AN - OPUS4-48850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - Usability of the written procedures: an eye tracking study N2 - Usability of the written procedures: an eye tracking study Non-destructive evaluation (NDE) is regarded as one of the key elements in ensuring quality of engineering systems and their safe use. A failure of NDE to detect critical defects in safety-relevant components, such as those in the nuclear industry, may lead to catastrophic consequences for the environment and the people. NDE inspection procedure is one of the most important tools in the everyday life of an NDE inspector. Experience and research studies have shown that NDE procedures are not always used as foreseen and may need to be optimized. Both the content and format play an important role in producing reliable procedures. Whereas the content aids in the understanding of the task and in its subsequent correct execution, the format determines the efficiency and frequency of the procedure’s use. For the purposes of this study, an inspection procedure - designed to be used in the inspection of components used in the final disposal of spent nuclear fuel - was further developed by adopting a user-centered design. This was achieved by following the eye movements during a data evaluation task whilst using the procedure, by interviews and group discussions, accompanied by a review from a human factors’ perspective, the suggestions from relevant literature and by reiterating the entire process once again. This process resulted in identifying shortcomings and in suggesting alterations to the existing procedure. The newly created procedure was empirically tested for its usability using eye tracking. By comparing the old instruction format to the newly developed one, the results showed that appropriately highlighting warnings, exceptions, or reminders, and placing them at a logical position assures that they will be read and identified with ease rather than overlooked. The presentation of the information in a stepwise manner, with one action per step, allows the user to follow more easily the steps that must be carried out to save time and effort. This study - the first of its kind in the field of non-destructive evaluation - showed that the procedure can be improved by applying human factors principles to the design and by involving the users into the process of procedure development and quality assurance. Introduction of the speaker – Marija Bertovic Marija Bertovic has a degree in psychology and a PhD in human factors. Since 2006 she has been working on topics related to human factors in non-destructive testing at the BAM Federal Institute for Materials Research and Testing, German Society for Non-Destructive Testing and as an independent consultant. The focus of her research has been on identifying and studying human factors’ related risks during NDT inspections and suggesting ways of optimizing the inspections and inspection procedures. She is currently a research staff member at BAM responsible for probabilistic safety and reliability analyses AND human factors analyses. She is the chairwoman of the German Society for Non-Destructive Testing’s (DGZfP) subcommittee on human machine interaction and the winner of the DGZfP Science Award in 2018. T2 - AHFE International, 10th International Conference on Applied Human Factors and Ergonomics CY - Washington Hilton, Washington D.C., USA DA - 24.07.2019 KW - Human Factors KW - ZfP KW - NDE PY - 2019 AN - OPUS4-48851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - Human-Factors in model-assisted POD approaches N2 - It is known that human factors (HF) affect the reliability of non-destructive testing (NDT). However, reliability is often expressed in probability of detection (POD) curves, obtained in practical trials, where human and organisational factors are considered only indirectly, through the few people taking part in the trials. Recently, we have observed an increase in the use of numerical modelling to obtain POD curves outside of practical trials. The so-called model-assisted POD(MAPOD) approaches have so far only very rarely included some kind of variation to account for HF. This talk presents different possibilities to include HF in MAPOD and discusses the advantages and disadvantages of each approach. T2 - The BINDT Aerospace Event 2019 CY - National Composites Centre NCC, Bristol, UK DA - 09.04.2019 KW - Human Factors KW - NDT KW - ZfP KW - MAPOD PY - 2019 AN - OPUS4-48852 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - Ironien der Automatisierung: Ein Blick von der menschlichen Seite N2 - In traditional NDT, human is seen as the main source of error. The advances in NDT 4.0 lead to believe that by increased automation, people, and therefore human error, can be diminished. The research on human-automation interaction shows that increased automation does not necessarily lead to a decrease of human error, a phenomenon dubbed as “automation ironies”, introduced by Bainbridge in 1987. The research shows that whereas with automation the known human error can be prevented, there is still room for new risks and error sources, which are unknown. As we advance from automation to industry 4.0 concepts, the possibility for human error shifts slightly to the developers of systems but remains in the interaction with systems as well, as the tasks and task demands change and give rise for possible failure at different stages of the NDT process, as once known. In der traditionellen zerstörungsfreien Prüfung wird der Mensch als Hauptfehlerquelle angesehen. Die Fortschritte bei der zerstörungsfreien Prüfung 4.0 lassen vermuten, dass durch eine verstärkte Automatisierung Menschen und damit menschliche Fehler verringert werden können. Die Untersuchung der Mensch-Automatisierungs-Interaktion zeigt, dass eine zunehmende Automatisierung nicht unbedingt zu einer Verringerung des menschlichen Fehlers führt, ein Phänomen, das 1987 von Bainbridge als „Automatisierungs-Ironien“ bezeichnet wurde. Die Untersuchungen zeigten, dass obwohl bei der Automatisierung bekannte menschliche Fehler verhindert werden können, gibt es noch Raum für neue Risiken und Fehlerquellen, die unbekannt sind. Während wir von der Automatisierung zu Industrie-4.0-Konzepten übergehen, verlagert sich die Möglichkeit menschlicher Fehler geringfügig auf die Entwickler von Systemen, bleibt jedoch auch in der Interaktion mit Systemen erhalten, da sich die Aufgaben und Aufgabenanforderungen ändern und es zu möglichen Fehlern in verschiedenen Phasen von ZfP-Prozessen kommen kann. T2 - Forum Produktionsmonitoring: Ausschussfrei produzieren CY - Frauenhofer EZRT, Fürth, Germany DA - 22.05.2019 KW - Human Factors KW - ZfP 4.0 PY - 2019 AN - OPUS4-48853 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - ZfP 4.0: Neue Herausforderungen für die Mensch-Maschine-Interaktion (MMI) N2 - Im Zeitalter von Industrie 4.0 muss die zerstörungsfreie Prüfung (ZfP) mit den Anforderungen Schritt halten. Eine erfolgreiche Umsetzung von Digitalisierung, Automatisierung, komplexen Vernetzungen, künstlicher Intelligenz, Assistenzsystemen, intelligenten Sensortechnologien etc. hängt in hohem Maße mit einer erfolgreichen und optimalen Mensch-Maschine-Interaktion (MMI) zusammen. Auf dem Gebiet der ZfP wurde erkannt, dass mit zunehmender Automatisierung neue Herausforderungen in Bezug auf die Mensch-Maschine-Interaktion entstehen können: Herausforderungen, die angegangen werden müssen. Der neu gegründete DGZfP FA "ZfP 4.0" hat sich diesem Thema angenommen und einen Unterausschuss (UA) zur Mensch-Maschine-Interaktion gegründet. Die Ziele dieses Unterausschusses bestehen darin, das Bewusstsein für die Mensch-Maschine-Interaktion in der ZfP zu sensibilisieren, sowie die Akzeptanz neuer Technologien in Hinblick auf Mensch-Maschine-Systeme und deren Umsetzung zu schaffen, um die Zuverlässigkeit und die Effektivität (Kostenreduktion + Sicherheit) der Mensch-Maschine-Systeme durch optimierte Mensch-Maschine-Interaktion zu gewährleisten. Einige der Themen, mit denen sich dieser UA auseinandersetzten möchte, sind: Entwurf und Entwicklung neuer Schnittstellen, Implementierung neuer Schnittstellen, Optimierung bestehender Technologien und Schnittstellen, Ausarbeitung von Technologien für das optimale MMI, Berücksichtigung der Zuverlässigkeit des gesamten Mensch-Maschine-Systems, Ausarbeitung der Inhalte für die Ausbildung, Wissenstransfer zwischen Disziplinen (z. B Psychologie, Ingenieurwesen, ZfP), usw. Ziel dieses Vortrags ist es, Herausforderungen zu beschreiben, die Mensch-Maschine-Systeme im Zeitalter von ZfP 4.0 begegnen könnten. Dazu gehören beispielsweise Vertrauen in automatisierte Systeme, Out-of-the-Loop-Phänomene, Verlust von Fähigkeiten, Akzeptanz der Automatisierung, Usability, usw. T2 - DACH Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Human Factors KW - ZfP 4.0 KW - MMI PY - 2019 AN - OPUS4-48854 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mansfeld, Ulrich A1 - Pellegrino, F. A1 - Maurino, V. A1 - Marguet, S. A1 - Testard, F. A1 - Tache, O. A1 - Hodoroaba, Vasile-Dan T1 - Towards accurate analysis of particle size distribution for non-spherically shaped nanoparticles as quality control materials N2 - Most industrial nanoparticles have non-spherical shapes and also possess polydisperse size distributions, and due to their agglomeration/ aggregation state are difficult (or even impossible) to be addressed individually. Further, driven by regulatory purposes related to the identification of a material as a nanomaterial, the accurate measurement of the smallest dimension of a (nano)particulate material makes the analysis even more complex. In the first phase of the EU Project nPSize - Improved traceability chain of nanoparticle size measurements (https://www.bam.de/Content/DE/Projekte/laufend/nPSize/npsize.html), the efforts are focused on synthesis of nanoparticles of well-defined, non-spherical shape. Following candidates of reference materials (CRM) with certifiable particle size (distribution) are under characterization with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-60 nm lateral), (ii) titania bipyramides (~60 nm length x 40 nm width), (iii) titania acicular particles (100 nm length x 15-20 nm width; aspect ratio 5.5/6), (iv) gold nanorods (~10 nm width x 30 nm length), and (v) gold nanocubes (~55 nm x 55 nm x 55 nm). KW - Nanoparticles KW - Imaging KW - Non-spherical KW - Reference material KW - Particle size distribution PY - 2019 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/towards-accurate-analysis-of-particle-size-distribution-for-nonspherically-shaped-nanoparticles-as-quality-control-materials/CD48E9298865410124E22837D8CF73A0 DO - https://doi.org/10.1017/S1431927619012376 SN - 1431-9276 SN - 1435-8115 VL - 25 IS - Suppl. 2 SP - 2328 EP - 2329 PB - Cambridge University Press AN - OPUS4-48856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jarvis, B. A1 - Wilrich, Cordula A1 - Wilrich, Peter-Th. T1 - Estimation of the POD function and the LOD of a binary microbiological measurement method from an interlaboratory experiment N2 - Background: We deal with interlaboratory experiments (collaborative studies) in which k participating laboratories, selected randomly from a population of laboratories, use samples from one and the same material or matrix. They perform binary microbiological measurements for which the measurement results are either “0” (target microorganisms not detected) or “1” (target microorganisms detected). The performance of such a measurement method is described by its probability of detection (POD) function, i.e., the POD as a function of the contamination of the sample (CFU per gram or CFU per milliliter), or by the level of detection (LODp), i.e., the contamination level of the sample that is detected (measurement result “1”) with a specified probability p. Objective: We derive an approximate statistical analysis that is simple enough to be implemented in a spreadsheet application. Methods: Under the assumption of a Poisson distribution of the number of CFU in the samples, we estimate the mean POD function of the laboratories and the SD of the laboratory effect based on a complementary log-log model, a special case of the Generalized Linear Model in the special situation in which the contamination level is known by means other than the POD. The estimates are obtained by maximization of the Laplace approximation of the likelihood function. By simulation, a bias correction factor for the estimate of the SD is obtained. With the estimated POD function, LODs can be estimated. The model can also be used to evaluate the relative LOD of an alternative method with repect to a reference method. Results: The EXCEL program PODLOD-interlab_ver1.xls for this method of statistical analysis can be downloaded from http://www.wiwiss.fu-berlin.de/fachbereich/vwl/iso/ehemalige/wilrich. Highlights: A simple approximate statistical method for the estimation of the POD and LOD is derived. The method also allows the estimation of the RLOD of an alternative Microbiological Methods Received December 11, 2018. Accepted by AH April 5, 2019. Estimation of the POD Function and the LOD of a Binary Microbiological Measurement Method from an Interlaboratory Experiment Basil Jarvis, Ross Biosciences Ltd, Upton Bishop, Ross-on-Wye HR9 7UR, United Kingdom; Cordula Wilrich, Bundesanstalt für Materialforschung und –prüfung, Unter den Eichen 87, D-12205 Berlin, Germany; Peter-Theodor Wilrich, Freie Universität Berlin, Institut für Statistik und Ökonometrie, Garystrasse 21, D-14195 Berlin, Germany. DOI: https://doi.org/10.5740/jaoacint.18-0412 method with respect to reference method. The method is implemented in an EXCEL program that can be downloaded from http://www.wiwiss.fu-berlin.de/fachbereich/vwl/iso/ehemalige/wilrich. KW - Probability of detection KW - POD KW - Level of detection KW - Limit of detection KW - LOD KW - Interlaboratory experiment KW - Collaborative studies KW - Qualitative measurements KW - Binary measurement KW - Microbiological measurement PY - 2019 UR - https://aoac.publisher.ingentaconnect.com/contentone/aoac/jaoac/2019/00000102/00000005/art00042 DO - https://doi.org/10.5740/jaoacint.18-0412 SN - 1060-3271 SN - 1944-7922 VL - 102 IS - 5 SP - 1617 EP - 1623 PB - AOAC International CY - Gaithersburg, USA, MD, 20877-2504 AN - OPUS4-48883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Machine learning for direct quantification of XRF measurements N2 - In X-ray fluorescence (XRF), a sample is excited with X-rays, and the resulting characteristic radiation is detected to detect elements quantitatively and qualitatively. Quantification is traditionally done in several steps: 1. Normalization of the data 2. Determination of the existing elements 3. Fit of the measured spectrum 4. Calculation of concentrations with fundamental parameters / MC simulations / standard based The problem with standard based procedures is the availability of corresponding standards. The problem with the calculations is that the measured intensities for XRF measurements are matrix-dependent. Calculations must, therefore, be performed iteratively (= time consuming) in order to determine the chemical composition. First experiments with gold samples have shown the feasibility of machine learning based quantification in principle. A large number of compositions were simulated (> 10000) and analyzed with a deep learning network. For first experiments, an ANN (Artificial Neural Network) with 3 hidden layers and 33x33x33 neurons was used. This network learned the mapping of spectra to concentrations using supervised learning by multidimensional regression. The input layer was formed by the normalized spectrum, and the output layer directly yielded the searched values. The applicability for real samples was shown by measurements on certified reference materials. T2 - Denver X-ray Conference CY - Lombard, IL, USA DA - 05.08.2019 KW - Machine learning KW - Artificial intelligence KW - Neural network KW - XRF KW - Synchrotron PY - 2019 AN - OPUS4-48903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya A1 - Johannesmann, S. A1 - Henning, B. A1 - Prager, Jens T1 - Analysis of Lamb wave mode repulsion and its implications to the characterisation of adhesive bonding strength N2 - Lamb waves are widely used for non-destructive evaluation of material parameters as well as for detection of defects. Another application of Lamb waves is quality control of adhesive joints. Researchers are currently investigating shear horizontal and zero-group velocity modes for characterisation of the adhesive bonding strength. In a new approach, Lamb wave mode repulsion is used to obtain the coupling strength between different layers to characterise the adhesive bonding strength. The modes of the individual layers become coupled in the multilayered systems forming particular regions, the so-called mode repulsion regions. This study investigates these modes and their interaction in two-layered plate-like structures with varying coupling strength both numerically, with the Scaled Boundary FEM, and experimentally T2 - International Congress on Ultrasonics CY - Bruges, Belgium DA - 03.09.2019 KW - Lamb waves KW - Multi-layered system KW - Adhesive joint KW - Mechanical strength KW - Scaled Boundary FEM PY - 2019 SP - 1 EP - 4 AN - OPUS4-48911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, M. A1 - Schlaich, C. A1 - Kulka, M. W. A1 - Donskyi, Ievgen A1 - Schwerdtle, T. A1 - Unger, Wolfgang A1 - Haag, R. T1 - Mussel-inspired coatings with tunable wettability, for enhanced antibacterial efficiency and reduced bacterial adhesion N2 - Over the last few decades, there has been a tremendous increase in research on antibacterial surface coatings as an alternative strategy against bacterial infections. Although there are several examples of effective strategies to prevent bacterial adhesion, the effect of the wetting properties on the coating was rarely considered as a crucial factor. Here we report an in-depth study on the effect of extreme wettability on the antibacterial efficiency of a silver nanoparticles (AgNPs)-based coating. By Controlling surface polymerization of mussel-inspired dendritic polyglycerol (MI-dPG) and post-functionalization, surfaces with wetting properties ranging from superhydrophilic to superhydrophobic were fabricated. Subsequently, AgNPs were embedded into the coatings by applying in situ reduction using the free catechols-moieties present in the MI-dPG coating. The resulting polymer coatings exhibited excellent antibacterial ability against planktonic Escherichia coli (E. coli) DH5a and Staphylococcus aureus (S. aureus) SH1000. The antibacterial efficiency of the coatings was analyzed by using inductively coupled plasma mass spectrometry (ICP-MS) and bacterial viability tests. Furthermore, the Antifouling properties of the coatings in relation to the antibacterial properties were evaluated. KW - Antibacterial surface coatings KW - Silver nanoparticles KW - XPS KW - Mussel-inspired dendritic polyglycerol (MI-dPG) PY - 2019 DO - https://doi.org/10.1039/c9tb00534j SN - 2050-750X SN - 2050-7518 VL - 7 IS - 21 SP - 3438 EP - 3445 PB - The Royal Society of Chemistry AN - OPUS4-48520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stroh, Julia A1 - Feiler, Torvid A1 - Ali, N. Z. A1 - Minas da Piedade, M. E. A1 - Emmerling, Franziska T1 - Mechanistic Insights into a Sustainable Mechanochemical Synthesis of Ettringite N2 - Mechanochemistry offers an environmentally benign and facile synthesis method for a variety of cement paste constituents. In addition, these methods can be used to selectively tune the properties of cement components. The mineral ettringite is an important component of cementitious materials and has additional technological potential due to its ion exchange properties. Synthesis of ettringite via mechanochemistry is an environmentally friendly alternative to conventional wet-chemical synthesis established in industry. This contribution explores the mechanism of a two-step mechanochemical synthesis of ettringite, which was previously found to greatly improve the reaction conversion as compared with one-pot synthesis. The crystallinity of Al(OH)3 was found to decrease during the first stage of this mechanochemical synthesis. This was correlated to a significant decrease in the particle size of Al(OH)3 in this stage. No other significant changes were found for the other components, suggesting that mechanochemical activation of Al(OH)3 is responsible for the enhanced formation of ettringite by the two-step approach. The environmentally friendly approach developed for ettringite synthesis offers a versatile synthetic strategy, which can be applied to synthesise further cementitious materials. KW - Ettringite KW - Mechanochemistry KW - Sustainability KW - X-ray diffraction PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-489172 DO - https://doi.org/10.1002/open.201900215 VL - 8 IS - 7 SP - 1012 EP - 1019 PB - ChemPubSoc AN - OPUS4-48917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino A1 - Neumann, Patrick P. A1 - Monroy, J. A1 - Lilienthal, A. J. T1 - A realistic remote gas sensor model for three-dimensional olfaction simulations N2 - Remote gas sensors like those based on the Tunable Diode Laser Absorption Spectroscopy (TDLAS) enable mobile robots to scan huge areas for gas concentrations in reasonable time and are therefore well suited for tasks such as gas emission surveillance and environmental monitoring. A further advantage of remote sensors is that the gas distribution is not disturbed by the sensing platform itself if the measurements are carried out from a sufficient distance, which is particularly interesting when a rotary-wing platform is used. Since there is no possibility to obtain ground truth measurements of gas distributions, simulations are used to develop and evaluate suitable olfaction algorithms. For this purpose several models of in-situ gas sensors have been developed, but models of remote gas sensors are missing. In this paper we present two novel 3D ray-tracer-based TDLAS sensor models. While the first model simplifies the laser beam as a line, the second model takes the conical shape of the beam into account. Using a simulated gas plume, we compare the line model with the cone model in terms of accuracy and computational cost and show that the results generated by the cone model can differ significantly from those of the line model. T2 - 2019 IEEE International Symposium on Olfaction and Electronic Nose (ISOEN) CY - Fukuoka, Japan DA - 26.05.2019 KW - Remote gas sensor KW - Gas detector KW - TDLAS KW - Sensor modelling PY - 2019 SN - 978-1-5386-8327-9 SN - 978-1-5386-8328-6 DO - https://doi.org/10.1109/ISOEN.2019.8823330 SP - 1 EP - 3 PB - IEEE AN - OPUS4-48919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hirschberger, Paul A1 - Baurzhan, Zhandos A1 - Tiebe, Carlo A1 - Hofmann, Michael A1 - Hüllmann, Dino A1 - Bartholmai, Matthias T1 - Indoor air quality monitoring using flying nanobots: Design and experimental study N2 - In this paper, we introduce a nano aerial robot swarm for Indoor Air Quality (IAQ) monitoring applications such as occupational health and safety of (industrial) workplaces. The robotic swarm is composed of nano Unmanned Aerial Vehicles (UAVs), based on the Crazyflie 2.0 quadrocopter, and small lightweight Metal Oxide (MOX) gas sensors for measuring the Total Volatile Organic Compound (TVOC), which is a measure for IAQ. An indoor localization and positioning system is used to estimate the absolute 3D position of the swarm similar to GPS. A test scenario was built up to validate and optimize the swarm for the intended applications. Besides calibration of the IAQ sensors, we performed experiments to investigate the influence of the rotor downwash on the gas measurements at different altitudes and compared them with stationary measurements. Moreover, we did a first evaluation of the gas distribution mapping performance. Based on this novel IAQ monitoring concept, new algorithms in the field of Mobile Robot Olfaction (MRO) are planned to be developed exploiting the abilities of an aerial robotic swarm. T2 - 2019 IEEE International Symposium on Olfaction and Electronic Nose (ISOEN) CY - Fukuoka, Japan DA - 26.05.2019 KW - Indoor air quality KW - Nano aerial robot KW - Aerial robot olfaction KW - Swarm KW - Gas detector PY - 2019 SN - 978-1-5386-8327-9 SN - 978-1-5386-8328-6 DO - https://doi.org/10.1109/ISOEN.2019.8823496 SP - 1 EP - 3 PB - IEEE AN - OPUS4-48920 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Faßbender, Sebastian A1 - Döring, A.-K. A1 - Meermann, Björn T1 - Development of complementary CE-MS methods for speciation analysis of pyrithione-based antifouling agents N2 - In the recent decade, metal pyrithione complexes have become important biocides for antifouling purposes in shipping. The analysis of metal pyrithione complexes and their degradation products/species in environmental samples is challenging because they exhibit fast UV degradation, transmetalation, and ligand substitution and are known to be prone to spontaneous species transformation within a chromatographic system. The environmental properties of the pyrithione species, e.g., toxicity to target and non-target organisms, are differing strongly, and it is therefore inevitable to identify as well as quantify all species separately. To cope with the separation of metal pyrithione species with minimum species transformation during analysis, a capillary electrophoresis (CE)–based method was developed. The hyphenation of CE with selective electrospray ionization- and inductively coupled plasma–mass spectrometry (ESI-, ICP-MS) provided complementary molecular and elemental information for the identification and quantification of pyrithione species. To study speciation of pyrithiones, a leaching experiment of several commercial antifouling paints containing zinc pyrithione in ultrapure and river water was conducted. Only the two species pyrithione (HPT) and dipyrithione ((PT)2) were found in the leaching media, in concentrations between 0.086 and 2.4 μM (HPT) and between 0.062 and 0.59 μM ((PT)2), depending on the paint and leaching medium. The limits of detection were 20 nM (HPT) and 10 nM ((PT)2). The results show that complementary CE-MS is a suitable tool for mechanistical studies concerning species transformation (e.g., degradation) and the identification of target species of metal pyrithione complexes in real surface water matrices, laying the ground for future environmental studies. KW - Complementary MS KW - Environmental speciation KW - Capillary electrophoresis-mass spectrometry KW - Antifouling biocides PY - 2019 DO - https://doi.org/10.1007/s00216-019-02094-5 SN - 1618-2642 VL - 411 IS - 27 SP - 7261 EP - 7272 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-48962 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Advances in air-coupled ultrasonic transducers for non-destructive testing N2 - Conventional ultrasonic testing involves the application of a fluid couplant for impedance matching. Increasing use of lightweight structures, composite materials and adhesive joints mostly in aerospace and automotive industry created an increasing interest in air-coupled ultrasonic testing methods, to protect sensitive surfaces and simplify maintenance. Commercially available air-coupled transducers consist of a piezocomposite material and matching layers to reduce the impedance mismatch between the transducer and air. This contribution is an overview of innovative approaches using new piezoelectric materials and other physical principles to transmit and receive an ultrasonic pulse in air. Capacitive and piezoelectric micromachined ultrasonic transducers (CMUTs and PMUTs) produce high pressure levels, but they exhibit a very narrow bandwidth. Optical laser-based methods for transmitting and receiving ultrasound promise a higher bandwidth, but do not achieve the same sensitivity as conventional air-coupled transducers. Ferroelectrets are charged cellular polymers exhibiting piezoelectric properties, having a very small acoustic impedance well matched to air. Ferroelectret transducers achieve about the same bandwidth as the most broadband conventional air-coupled transducers, having a higher sensitivity. Thermoacoustic transducers use heat to initiate an acoustic wave, acting as transmitters in ultrasonic range. Thermoacoustic transducers enable excitation of extremely broadband pulses while producing high pressure levels, which opens new possibilities for advanced signal processing. The newest member of the family of air-coupled ultrasonic transmitters is the plasma-based transducer, using both the thermoacoustic effect and the movements of the ions (so called ionic wind) to create acoustic waves. T2 - International Congress on Ultrasonics CY - Bruges, Belgium DA - 03.09.2019 KW - Air-coupled transducers KW - Non-destructive testing KW - Ferroelectret KW - Thermoacoustics KW - Plasma acoustics PY - 2019 AN - OPUS4-48963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Özelci, Ersan A1 - Rühle, Bastian A1 - Weigert, Florian A1 - Lubotzky, B. A1 - Kewes, G. A1 - Resch-Genger, Ute A1 - Benson, O. T1 - Quantitative measurements of the pH-sensitive quantum yield of fluorophores in mesoporous silica thin films using a drexhage-type experiment N2 - The photoluminescence quantum yield characterizes the performance of emitters for applications in optical devices, as reporters or probes in material and analytical sciences, and for sensing applications. Quantum yield measurements are challenging for luminescent molecules and nanocrystals immobilized in thin films for many sensor applications, particularly if spatially resolved quantitative luminescence information is desired. We show here that a Drexhage-type experiment, where a silver-coated millimeter-sized sphere is used to modify the local density of states, can provide an elegant approach to counter this challenge. As a representative example of the potential of this method, we measure the pH-dependent photoluminescence quantum yield of fluorescein isothiocyanate bound to a thin mesoporous silica film. The results were compared with those of the studies on the pH dependence of the same dye in solution. We found that our approach can link single fluorophore studies to ensemble measurements and pave the way for the spatially resolved fluorescence measurements of ultralow concentrations of emitters utilized as optically active elements and reporters in thin sensor films or incorporated into membranes. KW - Fluorescence KW - Quantum yield KW - Method KW - pH KW - Dye KW - Sensor KW - Fluorescein KW - Film KW - Silica KW - Single molecule KW - Lifetime KW - Absolute quantum yield PY - 2019 DO - https://doi.org/10.1021/acs.jpcc.9b03917 SN - 1932-7447 SN - 1932-7455 VL - 123 IS - 33 SP - 20468 EP - 20475 PB - ACS Publications AN - OPUS4-48984 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Everything and the kitchen sink: Correcting X-ray data for everything N2 - No matter whether you are doing X-ray diffraction or scattering, at wide or small angles, in a lab or at a synchrotron, you will need a bespoke sequence of up to twenty different corrections before it gets about right (at our latest count). Our library now does this automatically and reliably to get you the data you deserve – in absolute units and with uncertainty estimates – without the pain. This talk will highlight the development of the modular library, the sequence and its foundation, show its applicability to real-world datasets, and highlight a possible way forward T2 - Invited talk at Dectris AG CY - Baden-Daettwil, Switzerland DA - 09.09.2019 KW - Small-angle scattering KW - Software KW - Data corrections PY - 2019 N1 - Video of the talk is available at: https://www.youtube.com/watch?v=AU3XvV4W87M AN - OPUS4-48978 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bulling, Jannis A1 - Gravenkamp, H. A1 - Birk, C. T1 - A high-order finite element technique with automatic treatment of stress singularities by semi-analytical enrichment N2 - This paper presents an approach to the automatic enrichment of finite elements in the vicinity of a stress singularity. The enrichment consists of semi-analytical singular modes constructed using the Scaled Boundary Finite Element Method (SBFEM). In contrast to analytical methods, the SBFEM provides modes for inhomogeneous and anisotropic materials without additional effort. The finite element basis can be of arbitrary order and remains unaltered by the enrichment. The approach requires enrichment in only one layer of elements around a node. Due to the compatibility of SBFEM with FEM, there is no Need for transitional elements, and there are no parasitic terms. The approach is tested for several benchmark problems. The stress intensity factors are computed based on techniques inspired by the SBFEM. The proposed procedure is compared to a Standard finite element implementation and shows a significant improvement in the error of the displacement field for problems involving singular stresses. KW - Enriched finite element method KW - Scaled boundary finite element method KW - Stress intensity factors KW - Singular stress PY - 2019 DO - https://doi.org/10.1016/j.cma.2019.06.025 VL - 355 SP - 135 EP - 156 PB - Elsevier B.V. AN - OPUS4-48979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Boehm, Rainer A1 - Heckel, Thomas A1 - Brackrock, Daniel A1 - Spruch, W. A1 - Beggerow, T. ED - Bond, L. J. ED - Holland, S. ED - Laflamme, S. T1 - High Speed Hollow Axle Inspection with a New Designed Cone Type Phased Array N2 - Hollow axle inspection can be performed without demounting the axles and without dismantling the wheels and the brake discs by using the drilling for the scan. To increase inspection reliability and inspection speed, the application of phased array systems instead of conventional probes is a good choice. For solid shaft inspection phased array setups became standard in the recent years. Nevertheless, for hollow axle inspection typically a number of conventional probes rotating through the axles drilling are applied. The new approach uses an electronically steered rotating sound field from a phased array for the circumferential scan. This is realized by a cone shaped phased array which operates in immersion technique. That allows a significant increase in inspection speed and a reduction of the mechanical effort of the inspection system. The inspection can be carried out by a linear movement of the probe setup along the axles drilling. Applying additional focal laws allows exact inclination and focusing of the sound beam in the plane vertical to the specimen axis to concentrate the sound in the zones close to the external surface. An additional focus in the plane of incidence increases overall resolution and sensitivity. The cone type phased array probe has been optimized to detect transversal flaws in and close to the outer surface of the hollow axle with orientation in the radial-radial plane. The prototype probe system, sound field simulations and measurement results are presented. T2 - 45th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Portland, Oregon, USA DA - 13.07.2019 KW - Cone Shaped Phased Array KW - Hollow Axle Inspection KW - High Speed Testing PY - 2019 SN - 978-0-7354-1832-5 DO - https://doi.org/10.1063/1.5099834 SN - 0094-243X VL - 2102 IS - 1 SP - UNSP 100006-1 EP - UNSP 100006-11 PB - American Institute of Physics CY - Maryland, Vereinigte Staaten AN - OPUS4-48936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mutruc, D. A1 - Goulet-Hanssens, A. A1 - Fairmann, S. A1 - Wahl, S. A1 - Zimathies, Annett A1 - Knie, C. A1 - Hecht, S. T1 - Modulating Guest Uptake in Core-Shell MOFs with Visible Light N2 - A two-component core-shell UiO-68 type metal-organic framework (MOF) with a nonfunctionalized interior for efficient guest uptake and storage and a thin light-responsive outer shell was prepared by initial solvothermal MOF synthesis followed by solvent-assisted linker exchange. The bulky shell linker features two tetra-ortho-fluorinated azobenzene moieties to exploit their advantageous photoisomerization properties. The obtained perfect octahedral MOF single crystals can be switched repeatedly and with an unprecedented efficiency between E- and Z-rich states using visible light only. Due to the high photoswitch density per pore of the shell layer, its steric demand and thus molecular uptake (and release) can be conveniently modulated upon green and blue light irradiation. Therefore, the "smart" shell acts as a light-controlled kinetic barrier or "gate" for the diffusion of cargo molecules in and out of the MOF crystals. KW - Visible light KW - Azobenzene KW - Guest uptake/release KW - Metal– organic frameworks KW - Photochromism PY - 2019 DO - https://doi.org/10.1002/anie.201906606 VL - 58 SP - 12862 EP - 12867 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-48941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pohl, Rainer T1 - Eindraht und GMR versus Spulen - Gegenüberstellung verschiedener Wirbelstromsensoren N2 - An der BAM gibt es seit vielen Jahren Erfahrungen in der Entwicklung und im Bau speziell angepasster Wirbelstromsonden. Mit der Zielstellung, eine möglichst hohe Ortsauflösung zu erreichen, wurde vor einigen Jahren die sogenannte Eindrahtsonde (Patentanmeldung Nr. WO2015177341A1) entwickelt. Diese besteht aus der Kombination eines einzelnen dünnen Drahtes als Sender und GMR-Sensoren (giant magneto-resistance, Riesenmagnetwiderstand) als Empfänger. Beim Aufbau solcher Wirbelstromsonden hat sich der Einsatz sogenannter Starr-Flex-Leiterplatten bewährt. Der Aufbau und die Funktionsweise der Sensoren werden erläutert. Anhand spezieller Muster kleiner Vergleichsfehler werden Ortsauflösung, Richtungsabhängigkeit, Tiefenwirkung und Randeffekt hochauflösender Wirbelstromsonden aus Spulensystemen mit der Eindrahtsonde gegenübergestellt. T2 - Wirbelstromprüfung, Aktuelle Anwendungen und Entwicklungen, 1. Fachseminar der DGZfP CY - Celle, Germany DA - 10.09.2019 KW - GMR-Sensoren KW - Wirbelstromprüfung KW - Wirbelstromsenoren PY - 2019 AN - OPUS4-48949 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - Interaction of digestive biopolymers with zinc chloride as a model for zinc-enriched foods and cosmetics N2 - Zinc is an essential trace element and is ingested daily by humans, partly in dissolved form. The first contact is with saliva, in which many ions are dissolved whose solubility product with zinc can be low. This could result in compounds forming, possibly in nanoparticular form, which could have different effects on the organism than pure zinc ions. Available biopolymers, e.g. α-amylase, can in turn stabilise as-formed nanostructures. In this study, we report on the saliva stage of the artificial digestion of zinc chloride as a model substance for zinc ions. To facilitate in situ measurements, the sample is continuously passed through a small-angle x-ray scattering (SAXS) system. This custom-made machine is capable of measuring over a wide q-range and thereby able to resolve structures from around 250 nm down to the crystal structure. It is thus an excellent tool for investigating both the particle size distribution and the atomic structure of the sample. By curve fitting (see Figure 1), we found that shortly after addition of zinc chloride to saliva, small particles with a mean radius of 1.9 ± 0.1 nm and a distribution width of 0.6 ± 0.1 nm formed. These particles are aggregated to compact mass fractals with a fractal aggregate size of 14.7 ± 0.1 nm and a fractal dimension of 2.96 ± 0.02. Approximately 7200 single particles stick together by protein and form mass fractals, whose radii of gyration were found to be 36 ± 1 nm. To determine the compound that was formed, infrared spectroscopy was used in addition to the SAXS measurements, and zinc phosphate was identified as the product. T2 - POLYDAYS 2019 CY - Berlin, Germany DA - 11.09.2019 KW - SAXS KW - Digestion KW - Zinc PY - 2019 AN - OPUS4-48956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rahrig, M. A1 - Torge, Manfred T1 - 3D inspection of the restoration and conservation of stained glass windows using high resolution structured light scanning N2 - The initial focus of this research was on the development of a general workflow for the documentation and monitoring of historical stained glass windows using structured light scanning. Therefore windows from different churches, time periods and with different corrosion and damage phenomena were scanned before and after conservation measures. To evaluate the execution of the restoration measures the data was compared using 3D inspection software to examine the differences in geometry between the two scans. Various problems had to be solved, for example, how to deal with heavily reflective surfaces and the extreme contrast between light and dark surfaces, as seen in the borders between ‘Schwarzlot’ painting and plain glass. The application of materials for matting the surfaces, such as Cyclododecane spray, was impossible due to the high accuracy of the surface measurement required for 3D inspection. Regarding the contrast differences of the surfaces, the creation of exposure fusions and the use of polarization filters to reduce reflections were tested. In addition to the general problems encountered when recording translucent surfaces, the historical glasses caused additional problems in calculating surface comparisons. For example, the windows have to be moved and turned around several times, both during the conservation process and while scanning, causing deformations of the geometry due to the flexible lead rods allowing a certain degree of movement. T2 - 27th CIPA International Symposium “Documenting the past for a better future” CY - Ávila, Spain DA - 01.09.2019 KW - Stained glass KW - Restoration and conservation KW - Structured light scanning KW - 3D inspection KW - Glass scanning PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491286 DO - https://doi.org/10.5194/isprs-archives-XLII-2-W15-965-2019 VL - XLII-2/W15 SP - 965 EP - 972 PB - International Society of Photogrammetry and Remote Sensing (ISPRS) CY - Hannover AN - OPUS4-49128 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Modena, Mario M. A1 - Rühle, Bastian A1 - Burg, Thomas P. A1 - Wuttke, Steffan T1 - Nanoparticle characterization: What to measure? N2 - What to measure? is a key question in nanoscience, and it is not straightforward to address as different physicochemical properties define a nanoparticle sample. Most prominent among these properties are size, shape, surface charge, and porosity. Today researchers have an unprecedented variety of measurement techniques at their disposal to assign precise numerical values to those parameters. However, methods based on different physical principles probe different aspects, not only of the particles themselves, but also of their preparation history and their environment at the time of measurement. Understanding these connections can be of great value for interpreting characterization results and ultimately controlling the nanoparticle structure–function relationship. Here, the current techniques that enable the precise measurement of these fundamental nanoparticle properties are presented and their practical advantages and disadvantages are discussed. Some recommendations of how the physicochemical parameters of nanoparticles should be investigated and how to fully characterize these properties in different environments according to the intended nanoparticle use are proposed. The intention is to improve comparability of nanoparticle properties and performance to ensure the successful transfer of scientific knowledge to industrial real‐world applications. KW - Nanoparticle characterization KW - Nanoparticles KW - Porosity KW - Shape KW - Size PY - 2019 DO - https://doi.org/10.1002/adma.201901556 SN - 0935-9648 SN - 1521-4095 VL - 31 IS - 32 SP - 1901556, 1 EP - 26 PB - Wiley AN - OPUS4-49129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gaal, Mate A1 - Caldeira, Rui A1 - Bartusch, Jürgen A1 - Schadow, Florian A1 - Vössing, Konrad A1 - Kupnik, M. T1 - Air-coupled ultrasonic ferroelectret receiver with additional bias voltage N2 - High sensitivity is an important requirement for air-coupled ultrasonic sensors applied to materials testing. With a lower acoustic impedance than any piezoelectric material, charged cellular polypropylene (PP) offers better matching to air with a similar piezoelectric coefficient. The piezoelectric properties of charged cellular PP originate from their polarization, creating permanent internal voltage. The sensitivity of the sensor can be increased by applying additional dc bias voltage, as it has been done already for transmitters. This work presents the first ultrasonic sensor based on charged cellular PP including a high-voltage module providing dc bias voltage up to 2 kV. This bias voltage led to an increase in the signal-to-noise ratio of up to 15 ± 1 dB. The measurement of the received signal depending on the applied bias voltage is proposed as a new method of determining the internal voltage of ferroelectrets. The sensor combined with a cellular PP transmitter was applied to nondestructive testing of a rotor blade segment and glued-laminated timber, enabling imaging of the internal structure of these specimens with a thickness around 4 cm. KW - Acoustic sensors KW - Ferroelectret KW - Nondestructive testing KW - Ultrasonic imaging KW - Ultrasonic transducers PY - 2019 DO - https://doi.org/10.1109/TUFFC.2019.2925666 SN - 0885-3010 SN - 1525-8955 VL - 66 IS - 10 SP - 1600 EP - 1605 PB - IEEE AN - OPUS4-49131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - In-situ SAXS/WAXS investigation of zinc oxide nanotube formation N2 - Zinc oxide nanostructures possess optical properties that are dependent on particle shape and size. Here, we report on the synthesis of elongated zinc oxide tubes via the in-situ aggregation of spherical particles. Using a custom-built, lab-based instrument, x-ray scattering can be investigated over more than three decades in scattering vector q, allowing for a complete investigation from atomic distances up to larger-than-nano structures. For this study, the hydrolytic synthesis of stearate stabilized zinc oxide nanostructures in tetrahydrofuran was performed and the reaction mixture was continuously fed through the SAXS/WAXS apparatus by means of a peristaltic pump. For comparison to nanospheres, oleate-functionalized zinc oxide particles were synthesized in a microwave-assisted fashion, and depending on reaction temperature, sphere radii could be adjusted between 2.6 and 3.8 nm, changing the optical and crystal lattice properties. The evaluation of the in-situ measurements showed that at the beginning of the synthesis of the stearate-stabilized zinc oxide, similar, spherical particles are formed as in the oleate-based synthesis. In contrast, as the reaction progresses, the stearate-capped particles aggregate into elongated rods with radii of a few nanometres, which eventually form the nanotubes. These have radii of 30-50 nm and lengths of several hundred nanometres. Nevertheless, these structures still possess optical properties like the ultra-small zinc oxide spheres, i.e. a bright, yellow fluorescence. Therefore, we assume that the originally formed, ultra-small spheres, are still present within the tube structure, but separated by stearate, and thus determine their fluorescence properties. T2 - SAXS excites CY - Graz, Austria DA - 24.09.2019 KW - SAXS KW - Zinc oxide KW - Nanoparticles PY - 2019 AN - OPUS4-49135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saloga, Patrick E. J. A1 - Thünemann, Andreas T1 - Microwave-Assisted Synthesis of Ultrasmall Zinc Oxide Nanoparticles N2 - We report on ultrasmall zinc oxide single-crystalline nanoparticles of narrow size distribution and long-term colloidal stability. These oleate-stabilized nanoparticles were synthesized using microwave-assisted synthesis for 5 min, corresponding to a 99% decrease in synthesis time, when compared to the conventional synthesis method. It was observed that the average particle radius increases from 2.6 ± 0.1 to 3.8 ± 0.1 nm upon increasing synthesis temperature from 125 to 200 °C. This change also corresponded to observed changes in the optical band gap and the fluorescence energy of the particles, from 3.44 ± 0.01 to 3.36 ± 0.01 eV and from 2.20 ± 0.01 to 2.04 ± 0.01 eV, respectively. Small-angle X-ray scattering, dynamic light scattering, and UV–vis and fluorescence spectroscopy were employed for particle characterization. Debye–Scherrer analysis of the X-ray diffraction (XRD) pattern reveals a linear increase of the crystallite size with synthesis temperature. The consideration of the convolution of a Lorentz function with a Gaussian function for data correction of the instrumental peak broadening has a considerable influence on the values for the crystallite size. Williamson–Hall XRD analyses in the form of the uniform deformation model, uniform stress deformation model, and uniform deformation energy density model revealed a substantial increase of strain, stress, and deformation energy density of the crystallites with decreasing size. Exponential and power law models were utilized for quantification of strain, stress, and deformation energy density. KW - SAXS KW - Zinc oxide KW - Microwave synthesis KW - Nanoparticles PY - 2019 DO - https://doi.org/10.1021/acs.langmuir.9b01921 SN - 0743-7463 VL - 35 IS - 38 SP - 12469 EP - 12482 PB - American Chemical Society CY - Washington, D.C., USA AN - OPUS4-49136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hirschberger, Paul A1 - Bartholmai, Matthias ED - Zemčík, Robert ED - Krystek, Jan T1 - Influence of rotor downwash on vertically displaced nanobots in flight N2 - Using a swarm of copter-based gas-sensitive aerial nano robots for monitoring indoor air quality is challenging due to, e.g., limited air space in buildings. To avoid an over-regulation of the available indoor air space (e.g., prohibit copters to fly above each other), a safety region around each copter must be defined to guarantee a safe operation of the swarm. The key contributions of this paper are the realization of experiments that investigate the influence of the rotor downwash on flying vertically displaced nano robots and the development of a model describing the above-mentioned safety region. T2 - 36th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Pilsen, Czech Republic DA - 24.09.2019 KW - Gas sensing KW - Mobile Robot Olfaction KW - Nano aerial robot KW - Swarm PY - 2019 SP - 23 EP - 24 CY - Plzeň AN - OPUS4-49173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Influence of rotor downwash on vertically displaced nanobots in flight N2 - Using a swarm of copter-based gas-sensitive aerial nano robots for monitoring indoor air quality is challenging due to, e.g., limited air space in buildings. To avoid an over-regulation of the available indoor air space (e.g., prohibit copters to fly above each other), a safety region around each copter must be defined to guarantee a safe operation of the swarm. The key contributions of this poster are the realization of experiments that investigate the influence of the rotor downwash on flying vertically displaced nano robots and the development of a model describing the above-mentioned safety region. T2 - 36th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Pilsen, Czech Republic DA - 24.09.2019 KW - Gas sensing KW - Mobile Robot Olfaction KW - Nano aerial robot KW - Swarm PY - 2019 AN - OPUS4-49175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Xue, Boyang T1 - High-throughput underwater elemental analysis through optical emission spectroscopy with ultrasound-assisted μJ-laser-induced breakdown at kHz repetition rate N2 - The elemental analysis of seawater is often critical to the understanding of marine chemistry, marine geochemistry, and the deep-sea ecosystems. Laser-induced breakdown spectroscopy (LIBS) with the advantage of rapid multi-elements detection, has a great potential for in-situ elemental analysis of seawater. In practice, it is crucial to create a compact, low cost and power saving instrument for the long-term deep-sea observation. A recently appeared diode-pumped solid-state (DPSS) laser seems to be a promising candidate as it is both compact and robust. Additionally, its high repetition rate up to hundreds of kHz can provide a considerable throughput for LIBS analysis. However, the DPSS lasers operate at moderate pulse energies, usually less than one mJ, which cannot sustain stable breakdowns in bulk water. To ensure stable laser-induced plasmas underwater with such a μJ-DPSS laser, we introduced an ultrasound source to assist the breakdown process. The phase interface and mass flow generated by the near-field ultrasound can greatly reduce the breakdown threshold and enhance element-specific emissions. Meanwhile, the high repetition-rate pulses can also improve the breakdown probability and generate unique emission lines originated from the water molecule. We further demonstrate that the high repetition-rate DPSS laser combined with the Echelle spectrometer can provide effective quantitative analysis for metal elements in bulk water. T2 - 10th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy, EMSLIBS 2019 CY - Czech, Brno DA - 08.09.2019 KW - Ultrasound KW - Underwater LIBS KW - µJ-DPSS laser KW - High repetition-rate PY - 2019 AN - OPUS4-49223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino A1 - Neumann, Patrick P. A1 - Lilienthal, A. J. T1 - Gas Dispersion Fluid Mechanics Simulation for Large Outdoor Environments N2 - The development of algorithms for mapping gas distributions and localising gas sources is a challenging task, because gas dispersion is a highly dynamic process and it is impossible to capture ground truth data. Fluid-mechanical simulations are a suitable way to support the development of these algorithms. Several tools for gas dispersion simulation have been developed, but they are not suitable for simulations of large outdoor environments. In this paper, we present a concept of how an existing simulator can be extended to handle both indoor and large outdoor scenarios. T2 - 36th Danubia Adria Symposium on Advances in Experimental Mechanics CY - Pilsen, Czech Republic DA - 24.09.2019 KW - Gas dispersion simulation KW - CFD KW - Gas tomography PY - 2019 SN - 978-80-261-0876-4 SP - 49 EP - 50 CY - Pilsen, Czech Republic AN - OPUS4-49224 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino T1 - Gas Dispersion Fluid Mechanics Simulation for Large Outdoor Environments N2 - The development of algorithms for mapping gas distributions and localising gas sources is a challenging task, because gas dispersion is a highly dynamic process and it is impossible to capture ground truth data. Fluid-mechanical simulations are a suitable way to support the development of these algorithms. Several tools for gas dispersion simulation have been developed, but they are not suitable for simulations of large outdoor environments. Here we present a concept of how an existing simulator can be extended to handle both indoor and large outdoor scenarios. T2 - 36th Danubia Adria Symposium on Advances in Experimental Mechanics CY - Pilsen, Czech Republic DA - 24.09.2019 KW - Gas dispersion simulation KW - CFD KW - Gas tomography PY - 2019 AN - OPUS4-49225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lee, C. A1 - Inutan, E. D. A1 - Chen, J. L. A1 - Mukeku, M. M. A1 - Weidner, Steffen A1 - Trimpin, S. A1 - Ni, C.-K. T1 - Toward understanding the ionization mechanism of matrix‐assisted ionization using mass spectrometry experiment and theory N2 - Matrix‐assisted ionization (MAI) mass spectrometry does not require voltages, a laser beam, or added heat to initiate ionization, but it is strongly dependent on the choice of matrix and the vacuum conditions. High charge state distributions of nonvolatile analyte ions produced by MAI suggest that the ionization mechanism may be similar to that of electrospray ionization (ESI), but different from matrix‐assisted laser desorption/ionization (MALDI). While significant information is available for MAI using mass spectrometers operating at atmospheric and intermediate pressure, little is known about the mechanism at high vacuum. Eleven MAI matrices were studied on a high‐vacuum time‐of‐flight (TOF) mass spectrometer using a 266 nm pulsed laser beam under otherwise typical MALDI conditions. Detailed comparisons with the commonly used MALDI matrices and theoretical prediction were made for 3‐nitrobenzonitrile (3‐NBN), which is the only MAI matrix that works well in high vacuum when irradiated with a laser. Screening of MAI matrices with good absorption at 266 nm but with various degrees of volatility and laser energies suggests that volatility and absorption at the laser wavelength may be necessary, but not sufficient, criteria to explain the formation of multiply charged analyte ions. 3‐NBN produces intact, highly charged ions of nonvolatile analytes in high‐vacuum TOF with the use of a laser, demonstrating that ESI‐like ions can be produced in high vacuum. Theoretical calculations and mass spectra suggest that thermally induced proton transfer, which is the major ionization mechanism in MALDI, is not important with the 3‐NBN matrix at 266 nm laser wavelength. 3‐NBN:analyte crystal morphology is, however, important in ion generation in high vacuum. The 3‐NBN MAI matrix produces intact, highly charged ions of nonvolatile compounds in high‐vacuum TOF mass spectrometers with the aid of ablation and/or heating by laser irradiation, and shows a different ionization mechanism from that of typical MALDI matrices. KW - Ionization KW - MALDI-TOF MS KW - Mechanism PY - 2021 DO - https://doi.org/10.1002/rcm.8382 VL - 35 IS - 51 SP - e8382 PB - John Wiley & Sons AN - OPUS4-49209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer T1 - Entwicklung einer reproduzierbaren und quantifizierbaren Heißluftquelle für thermografische Untersuchungen N2 - Der Beitrag beschreibt den Aufbau und die Entwicklung einer Heißluftquelle als Wärmequelle für die aktive Thermografie. Als Ausgangspunkt wird zunächst die Quellenlage betrachtet. In der Literatur über Thermografie spielt Heißluft als Wärmequelle nur in weniger als 0,1% eine Rolle, die Ursache dafür ist nicht bekannt. Es wird vermutet, dass dieser Erwärmungsmethode unterstellt wird, sie hätte Nachteile bezüglich Homogenität der Erwärmung sowie Leistungseintrag. In einer der raren Publikationen über einen Verfahrensvergleich schnitt die Heißluft-Thermografie jedoch nicht schlechter als die Vergleichsverfahren mit optischer Anregung ab, bei gleichzeitig deutlichem Zeitgewinn und geringerem technischen Aufwand. Danach wird der fertige Versuchsaufbau mit seinen wesentlichen Komponenten dargestellt. Der Einfluss der Geometrie der Luftaustrittsdüse auf die erreichbare Wärmeverteilung an einem flachen Blech wurde an mehreren Düsen untersucht. Hierbei erwies sich eine langgestreckte Umlenkdüse mit einer Strahlumlenkung von etwa 20° als optimal zur Erzeugung einer möglichst homogenen Erwärmung. Ein weiterer zu optimierender Parameter war die erreichbare Schaltdynamik des Heißgasstromes. Beim schnellen Schalten großer Volumenströme treten Druckstöße mit entsprechenden Temperaturänderungen auf. Hinzu kommt, dass der verwendete MFC (mass flow controller) bei großen Volumenströmen zum Einschwingen bei Schaltprozessen neigt. Daher enthält der Aufbau einen offenen Bypass zur Stabilisierung des Volumenstroms. Mit dem so realisierten Messplatz wurde die Reproduzierbarkeit der erzielten Erwärmung durch mehrfache Wiederholungsmessungen über einen längeren Zeitraum untersucht. Hierzu wurde ein auch zu Validierungszwecken genutzter PVC-Block mit 13 mm Dicke jeweils für 60 s erwärmt und die Oberflächentemperatur des PVC-Blocks mit einer IR-Kamera aufgezeichnet. Bei jeweiligem Neuaufbau ohne Justierhilfe ergab sich eine Reproduzierbarkeit von etwa 22% bei 5 Versuchen. Unter Nutzung einer Justierhilfe (Schablone für Abstand in der Kamerasoftware) ließ sich die Reproduzierbarkeit auf 5% bei 7 Versuchen reduzieren. Ein weiterer zu klärender Punkt war der erzielbare Wärmeeintrag im Vergleich zu einer Anregung mit Blitzlampen. Hierzu wurde eine Messung mit 60 s Heißluftheizung direkt mit einer Evaluierungsmessung mit Blitzlampen am gleichen PVC-Probekörper mit 4 FBB an der Rückseite verglichen. Die Inhomogenität der Erwärmung wurde durch eine Phasenauswertung unterdrückt. Die Phasenauswertung gestattete den Nachweis aller 4 FBB, wobei das Signal zu Rausch-Verhältnis bei der Heißlufterwärmung deutlich besser war. Der direkte Vergleich der Temperaturkurven zeigt, dass bei 60 s Heizlufterwärmung ca. 4,5 mal mehr Energie als bei der Blitzanregung vom Probekörper absorbiert wurde. Hieraus lässt sich die eingekoppelte Heizleistung mit 100 mW/cm² abschätzen. Das entspricht in etwa dem Niveau, wie es auch mit bewegten Halogenstrahlern, bewegten IR-Strahlern oder der Sonne erreicht wird. Diese Ergebnisse belegen, dass eventuell vorhandene Vorbehalte gegenüber einer Heißluft als Wärmequelle für die aktive Thermografie zumindest für thermisch langsame Materialien wie Kunststoffe oder mineralische Baustoffe unbegründet sind. Die Einsatzgrenzen bei der Untersuchung thermisch schnellerer Materialien wie Metalle steht noch aus, hier ist mit Abstrichen zu rechnen. Auf der anderen Seite lässt eine mögliche Düsenoptimierung noch deutliche Verbesserungen erwarten. T2 - Thermografiekolloquium der DGZfP 2019 CY - Halle, Germany DA - 19.09.2019 KW - Thermografie KW - Zerstörungsfreie Prüfung KW - Heißluftquelle PY - 2019 AN - OPUS4-49217 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Effect of Nitrification Inhibitor on Nitrogen Forms in Soil and Phosphorus Uptake of Plants N2 - Phosphorus (P) resource availability is declining and the efficiency of applied nutrients in agricultural soils is becoming increasingly important. This is especially true for P-fertilizers from recycled materials which often have a lower plant-availability compared to commercial P-fertilizers but are expected to play an increasingly important role into the future (Kratz et al. 2019). One promising way to increase the plant-availability of the fertilizer P is a co-fertilization with specific nitrogen (N) forms which can enhance the P uptake and make P-fertilizers from recycled material more competitive to commercial phosphate rock-based P-fertilizers (Rahmatullah et al. 2006; Vogel et al. 2018). To investigate this effect, we performed a pot experiment with three different P-fertilizers (sewage sludge-based, phosphate rock and triple superphosphate) and ammonium nitrate sulfate as a co-fertilizer, without and with a nitrification inhibitor (NI), and analyzed the form of N and P in soil via a suite of chemical and novel X-ray spectroscopic methods. The application of NI with the P and N fertilizers led to a higher dry matter yield and a higher P uptake of maize. Novel N K-edge micro-X-ray absorption near-edge structure (micro-XANES) spectroscopy identified that the application of a NI promotes the temporary formation of a non-exchangeable N in detectable hot-spots in the soil. The subsequent slow release and prolonged availability of N during plant growth leads to higher yield and nutrient uptake. It can be concluded that NIs lead to a temporary fixation of ammonium-N in a pool that can be accessed by plant roots. Those types of available nutrient pools meet the idea of so-called “next generation fertilizers” as plants have access to nutrients according to their current demand. T2 - Annual Meeting of the German Society of Plant Nutrition (DGP) CY - Berlin, Germany DA - 25.09.2019 KW - Fertilzer KW - X-ray adsorption near-edge structure (XANES) spectroscopy KW - Nitrification inhibitor KW - Agronomic performance PY - 2019 AN - OPUS4-49144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian A1 - Franz, Philipp A1 - Fischer, C. A1 - Wachtendorf, Volker A1 - Maierhofer, Christiane T1 - Zerstörungsfreie Charakterisierung der Alterung additiv gefertigter Kunststoffbauteile N2 - Das vorgestellte Projekt beschäftigt sich mit den optischen, thermophysikalischen und mechanischen Materialeigenschaften von additiv gefertigten Kunststoffteilen und deren Alterung. Dazu wurden mittels Fused Layer Modeling (FLM) Probekörper aus ABS hergestellt, die anschließend für drei Monate einer künstlichen Bewitterung unterzogen wurden. Die dabei erzeugte definierte Alterung wurde nach drei Zeitabschnitten jeweils mit zerstörungsfreien Methoden charakterisiert. Dabei wurde neben den spektroskopischen Standardmethoden auch die aktive Thermografie eingesetzt. Die Ergebnisse zeigen, dass sich mittels der Thermografie sowohl chemische Veränderungen als auch mechanische Schädigungen (Fehlstellen) darstellen lassen. Die Bewitterung beeinflusst die Teiltransparenz der Proben zumindest im sichtbaren Spektralbereich, was bei der Charakterisierung der Fehlstellen, die mittels optisch angeregter aktiver Thermografie detektiert wurden, berücksichtigt werden muss. T2 - DGZfP-Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - 3D Druck KW - Additive Fertigung KW - Thermografie KW - Polymere KW - Künstliche Bewitterung PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491561 UR - https://jt2019.dgzfp.de/Portals/jt2019/bb/Di.3.B.1.pdf SN - 978-3-947971-02-2 VL - 171 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-49156 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Centrifugal force meets materials testing – analytical centrifuge as multipurpose tool for tensile and compressive stress testing N2 - Up until several years ago, tensile and compressive tests have been exclusively carried out as single-sample tests within a tensile, hardness or universal testing machine. The availability of centrifuge technology changed this situation in 2013 in several ways because centrifugal force is used as testing force within a rotational reference frame. Firstly, multiple-sample strength testing became feasible for both tensile load condi-tions, e.g. determination of composite, bonding or adhesive strength, and compressive load conditions, e.g. hardness, compressibility and compactibility. Secondly, there is no need for a two-sided sample clamping and double-cardanic suspensions as samples are simply inserted using a one-sided sample support. Thirdly, shear forces can be avoided by means of guiding sleeves which steer test stamps acting as mass bodies for either tensile or compressive testing. Fourthly, up to eight samples can be tested under identical conditions within a very short period of time, typically within 15 minutes including sample loading and unloading. Hence, either a reliable statistics (of identical samples) or a ranking (of different samples) can be derived from one test run. The bench-top test system is described in detail and demonstrated that centrifugal force acts as testing force in an appropriate way because Euler and Coriolis force do not affect the testing results. Examples for both tensile strength testing, i.e. bonding strength of adhesives-bonded joints and adhesive strength of coatings, and compres-sive strength testing, i.e. Vickers-, Brinell- and ball indentation hardness and deter-mination of spring constants, are presented, discussed and compared with conven-tional tests within tensile, hardness or universal testing machines. At present, a maximum testing force of 6.5 kN can be realized which results at test stamp diameters of 5 mm, 7 mm, and 10 mm in tensile or compressive stress values of 80 MPa, 160 MPa, and 320 MPa. For tensile strength, this is already beyond bonding strength of cold- and warm-curing adhesives. Moreover, centrifuge technology is compliant to standards such as EN 15870, EN ISO 4624, EN ISO 6506/6507 and VDI/VDE 2616. Programmable test cycles allow both short-term stress and log-term fatigue tests. Based on a variety of examples of surface and bonding technology, applications in both fields R&D and QC are presented. Meanwhile, centrifuge technology is also accredited according to DIN EN ISO/IEC 17025. T2 - Intermationa Conference Dispersion Analysis & Materials Testing CY - Berlin, Germany DA - 22.05.2019 KW - Centrifugal Force KW - Compressive Stress KW - Tensile Stress PY - 2019 AN - OPUS4-48310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dudek, Gabriele T1 - Die neue ISO/IEC 17025 – Was ändert sich für Prüf- und Kalibrierungslaboratorien? N2 - Der Vortrag gibt einen Überblick über die Revision der ISO/IEC 17025, einschließlich der Einflüsse auf die Revision und die Veränderungen bezüglich der Anforderungen an Laboratorien. T2 - Shimadzu Expertenzirkel Umweltanalytik CY - Dusseldorf, Germany DA - 04.07.2019 KW - ISO/IEC 17025 KW - Konformitätsbewertung KW - Messunsicherheit KW - Laboratorien PY - 2019 AN - OPUS4-48313 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dudek, Gabriele T1 - Aktuelle Entwicklungen im Bereich der CASCO Normen N2 - Der Vortrag gibt einen Überblick über die Weiterentwicklungen der Normung im Bereich Konformitätsbewertung. Die sogenannten Common Elements werden vorgestellt. Deren Änderungen haben großen Einfluß auf die kommenden Revisionen der CASCO Normnen T2 - Erfahrungsaustausch, Verband akkreditierter Zertifizierungsstellen CY - Berlin, Germany DA - 07.05.2019 KW - Konformitätsbewertung KW - ISO CASCO PY - 2019 AN - OPUS4-48314 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Raysyan, Anna T1 - Ideen nah am Leben N2 - Ein Schnelltest zum Nachweis von Schadstoffen in der Muttermilch und eine Schnittmustersoftware - Wissenschaftstalente mit anwendungsnahen Ideen und auf dem Weg ins Unternehmertum. KW - Diclofenac KW - Schnelltest KW - Lateral Flow Immunoassay KW - Schwangerschaftstest PY - 2019 IS - 01-02 SP - 12 EP - 13 PB - WISTA Management GmbH CY - Berlin AN - OPUS4-48315 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ramos, I. I. A1 - Carl, Peter A1 - Schneider, Rudolf A1 - Segundo, M. A. T1 - Automated lab-on-valve sequential injection ELISA for determination of carbamazepine N2 - The development of an automated miniaturized analytical system that allows for the rapid monitoring of carbamazepine (CBZ) levels in serum and wastewater is proposed. Molecular recognition of CBZ was achieved through its selective interaction with microbeads carrying anti-CBZ antibodies. The proposed method combines the advantages of the micro-bead injection spectroscopy and of the flow-based platform lab-on-valve for implementation of automatic immunosorbent renewal, rendering a new recognition surface for each sample. The sequential (or simultaneous) perfusion of CBZ and the horseradish peroxidase-labelled CBZ through the microbeads is followed by real-time on-column Monitoring of substrate (3,30,5,50-tetramethylbenzidine) oxidation by colorimetry. The evaluation of the initial oxidation rate and also the absorbance value at a fixed time point provided a linear response versus the logarithm of the CBZ concentration. Under the selected assay conditions, a single analysis was completed after only 11 min, with a quantification range between 1.0 and 50 µg L⁻¹. Detection of CBZ levels in undiluted wastewater samples was feasible after a simple filtration step while good recoveries were attained for spiked certified human serum, analyzed without sample clean-up. KW - Automation KW - Bead injection spectroscopy KW - Human serum KW - Microparticles KW - Therapeutic Drug Monitoring KW - Wastewater PY - 2019 DO - https://doi.org/10.1016/j.aca.2019.05.017 SN - 0003-2670 VL - 1076 SP - 91 EP - 99 PB - Elsevier CY - Amsterdam AN - OPUS4-48317 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Schwinn, M. A1 - Kuhlmeier, K. A1 - Büchel, C. A1 - Meermann, Björn T1 - Development of an automated on-line purification HPLC single cell-ICP-MS approach for fast diatom analysis N2 - The most challenging part in performing a single cell ICP-MS (sc-ICP-MS) approach is the sample preparation, in particular the reduction of the ionic background. This step is, in many cases, time-consuming and required for each sample separately. Furthermore, sc-ICP-MS measurements are mostly carried out "manually", given the fact that present systems are not allowing for an automated change of samples. Thus, within this work, we developed an approach based on a HPLC system coupled on-line with sc-ICP-MS via a set of switching valves as well as an in-line filter for automated cell washing. This set-up enables the ionic background removal as well as analysis of single cells completely automated without any manual sample pretreatment. Our approach was applied for the analysis of the single celled diatom species Cyclotella meneghiniana, a marine diatom species, on the basis of Mg24 and facilitates testing in 11 min per sample, requiring only around 10,000 cells in a volume of 10 µL and approx. 10 mL of a 5% MeOH/95% deionized water (v/v) mixture. Even at extremely saline culturing media concentrations (up to 1000 mg L-1 magnesium) our on-line approach worked sufficiently allowing for distinction of ionic and particulate fractions. Furthermore, a set of diatom samples was analyzed completely automated without the need for changing samples manually. So, utilizing this approach enables analyzing a high quantity of samples in a short time and therefore in future the investigation of ecotoxicological effects is simplified for example in terms of metal accumulation by taking biovariability into account. KW - Single cell-ICP-MS KW - Diatoms KW - Ecotoxicology testing KW - Automated system PY - 2019 DO - https://doi.org/10.1016/j.aca.2019.05.045 SN - 1873-4324 VL - 1077 SP - 87 EP - 94 PB - Elsevier AN - OPUS4-48567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Sauer, Andreas A1 - Bremser, Wolfram T1 - Fifteen years of proficiency testing of total petrol hydrocarbon determination in soil: a story of success N2 - The total petrol hydrocarbon (TPH) content in soil is determined by gas chromatographic separation and flame ionisation detection according to ISO 16703 in routine laboratories for about 20 years. The development of the interlaboratory variability observed with this analytical procedure over 15 years in a proficiency testing scheme conducted annually with more than 170 participants is evaluated in detail. A significant improvement of the reproducibility standard deviation among participants is observed over the years and attributed to an increasing familiarity with the procedure. Nevertheless, the determination of TPH in the environmentally relevant mass fraction range between 500 mg/kg and 10 000 mg/kg in soils or sediments is far from reaching the reproducibility standard deviations predicted by the Horwitz curve. It is seen that laboratories with sporadic participation tend to report higher bias, while a core group of laboratories participating on a regular basis arrived at reproducibility standard deviations below 20 %. Results from a given laboratory obtained on two different samples tend to be highly correlated in the same PT round indicating a sound repeatability. Expectedly, the within-laboratory correlation between results from consecutive rounds was considerably lower. However, results from consecutive rounds with a temporal distance of 1, 2 or 3 years revealed largely similar correlations which suggests that the within-laboratory reproducibility adjusts to a constant level at least after a period of 1 year. KW - Mineralölkohlenwasserstoffe KW - Boden KW - Ringversuch KW - Gaschromatographie KW - GC-FID KW - Eingnugsprüfung KW - Proficiency Testing PY - 2019 DO - https://doi.org/10.1007/s00769-019-01383-x SN - 0949-1775 SN - 1432-0517 VL - 24 IS - 4 SP - 289 EP - 296 PB - Springer AN - OPUS4-48419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Genath, A. A1 - Hofmann, Michael A1 - Tiebe, Carlo A1 - Einspanier, R. T1 - Proof-of-concept trial of the portable electronic nose PEN3 for detection of formic acid concentration in the beehive N2 - Formic acid (FA) treatment as measure against the ectoparasitic mite, Varroa destructor, which infests the western honey bee, Apis mellifera, is usually performed twice a year. Although the therapeutic index is very narrow and the success of FA-treatment is highly dependent on various external factors, little is known about the local FA concentrations occuring in the hive. In this study we examined whether a commercially available odour measuring device (“electronic nose”) is suitable for measurements of high FA concentrations, as present during treatment. As measuring systems, two different setups were prepared for detection of FA concentrations in gas mixtures: A polymethyl methacrylate (PMMA) box was used to investigate whether the electronic nose is able to distinguish between different FA concentrations and a two-storied Segeberger hive to test under realistic conditions during bee-keeping. In both experimental systems, the signals from the same sensor components (sensor type no. 1, 6, 7, 8 and 9) showed an increased sensitivity towards the presence of FA in the gas mixture. Principle component analysis (PCA) and linear discriminant analysis (LDA) allowed for identification of specific patterns in the measurement signals and showed clear correlations between the signals and the present FA concentration. These results indicate that the introduced commercial multi gas sensor system is suitable for detection of high FA concentrations, and therefore could be a starting point developing a detection method of FA. The future aim is to successfully monitor the efficiency and effectiveness of this anti-varroa-treatment. T2 - 20. GMA/ITG-Fachtagung Sensoren und Messsysteme 2019 CY - Nuremberg, Germany DA - 25.06.2019 KW - Apis mellifera KW - Varroa destructor KW - Formic Acid KW - Metal-Oxide Gas Sensor Array PY - 2019 AN - OPUS4-48380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Genath, A. A1 - Hofmann, Michael A1 - Tiebe, Carlo A1 - Einspanier, R. T1 - Proof-of-concept trial of the portable electronic nose PEN3 for detection of formic acid concentration in the beehive N2 - Formic acid (FA) treatment as measure against the ectoparasitic mite, Varroa destructor, which infests the western honey bee, Apis mellifera, is usually performed twice a year. Although the therapeutic index is very narrow and the success of FA-treatment is highly dependent on various external factors, little is known about the local FA concentrations occuring in the hive. In this study we examined whether a commercially available odour measuring device (“electronic nose”) is suitable for measurements of high FA concentrations, as present during treatment. As measuring systems, two different setups were prepared for detection of FA concentrations in gas mixtures: A polymethyl methacrylate (PMMA) box was used to investigate whether the electronic nose is able to distinguish between different FA concentrations and a two-storied Segeberger hive to test under realistic conditions during bee-keeping. In both experimental systems, the signals from the same sensor components (sensor type no. 1, 6, 7, 8 and 9) showed an increased sensitivity towards the presence of FA in the gas mixture. Principle component analysis (PCA) and linear discriminant analysis (LDA) allowed for identification of specific patterns in the measurement signals and showed clear correlations between the signals and the present FA concentration. These results indicate that the introduced commercial multi gas sensor system is suitable for detection of high FA concentrations, and therefore could be a starting point developing a detection method of FA. The future aim is to successfully monitor the efficiency and effectiveness of this anti-varroa-treatment. T2 - 20. GMA/ITG-Fachtagung Sensoren und Messsysteme 2019 CY - Nuremberg, Germany DA - 25.06.2019 KW - Apis mellifera KW - Varroa destructor KW - Formic Acid KW - Metal-Oxide Gas Sensor Array PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483812 UR - https://www.ama-science.org/proceedings/details/3430 DO - https://doi.org/10.5162/sensoren2019/P3.10 VL - 2019 SP - 794 EP - 799 AN - OPUS4-48381 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulletti, A. T1 - Charachterization of piezopolymer interdigital transducer's vibrational modes N2 - Lamb waves are widely used for monitoring the health of structures made of laminated materials (metals, composites). Piezoelectric ultrasonic transducers transmit and receive acoustic guided waves that interact with the elastic properties and the defects of the material under test. In recent years, DINFO developed piezopolymer Interdigital Transducers (IDTs) proven to be suitable to build SHM systems for aerospace applications. Their base material is a Cr/Au-coated PVDF-TrFE copolymer sheet, having a thickness of 100μm and a metallization of 0.1μm on both sides. IDTs are attractive for SHM systems for their capability to select specific Lamb wave modes when designed with appropriate electrode pattern. For a reliable application, it is crucial to characterize the in-plane and out-of-plane displacement of the transducer and to correlate the ultrasonic propagating signal with the Lamb waves dispersion curves in laminates. For example, for a 2 mm aluminum plate A0 mode has dominant out-of-plane displacement, whereas S0 mode has dominant in-plane displacement at the plate's surface. In collaboration with BAM the characterization of free vibrational modes using a 3D laser doppler vibrometer was performed. The analysis in the frequency domain was performed using the following parameters: a chirp excitation with frequencies 50-500 kHz and 0.5-1 MHz with 195 Hz and 390 Hz frequency resolution respectively at 100 Vpp for a total of 90 averaged measurements per point. Also propagating modes were characterized by bonding the IDT on a 2 mm aluminum plate and analyzing the in-plane and the out-of-plane components. A0-mode was successfully excited having the main lobe aligned with the main axis of the IDT, confirming the dominant presence of this propagating mode. The results could be used as a basis for design and optimization of the IDTs in terms of directivity and mode selection, and to facilitate interpretation of the ultrasonic guided waves propagating in laminated structures. T2 - 51th Annual Meeting of the Associazione Societa Italiana Di Elettronica CY - Rome, Italy DA - 26.06.2019 KW - Structural Health Monitoring KW - Interdigital Transducer KW - PVDF KW - Ultrasonic guided waves KW - Lamb waves PY - 2019 AN - OPUS4-48382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - Fehlerwechselwirkung in Verbundwerkstoffen mit Geführten Wellen N2 - Der praktische Einsatz von SHM-Verfahren mit geführten Ultraschallwellen basiert auf einem fundierten Verständnis der speziellen physikalischen Zusammenhänge der Wellenausbreitung. Das umfasst nicht nur das multimodale Verhalten, welches von den Dispersionsdiagrammen repräsentiert wird, sondern auch die Vorhersage der Interaktion zwischen verschiedenen Wellenmoden und den zu erwartenden Fehlstellen. Ziel des Workshops ist es, das Verständnis der Ausbreitung geführter Wellen zu verbessern und die vielfältigen Anwendungsmöglichkeiten, die sich aus der multimodalen Wellenausbreitung ergeben, an praktischen Beispielen zu demonstrieren. Die vorgestellten Szenarien beschränken sich dabei nicht nur auf eine Anregung grundlegender Dehnungs- und Biegewellen, sondern beziehen auch geführte Wellenmoden höherer Ordnung zur Verbesserung der Aussagekraft des Prüfergebnisses mit ein. Nach einer theoretischen Einführung werden ausgewählte Demonstratoren, vorrangig mit Bezug zum Automobilbau, vorgestellt. Diese schließen Fragestellungen der Integration der Sensorik in gekrümmte Faserverbundbauteile ebenso mit ein, wie die Überwachung von Metall-Faserverbund-Komposit-Materialien, die in Drucktanks zum Einsatz kommen. T2 - 3. Anwenderseminar Zustandsüberwachung mit geführten Wellen CY - Karlsruhe, Germany DA - 27.03.2019 KW - Wasserstoffspeicher KW - Geführte Ultraschallwellen KW - Kohlenstofffaserverstärkter Kunststoff KW - Faserverbundwerkstoff PY - 2019 AN - OPUS4-48383 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Carl, Peter A1 - Ramos, Inês I. A1 - Segundo, Marcela A. A1 - Schneider, Rudolf T1 - Antibody conjugation to carboxyl-modified microspheres through N-hydroxysuccinimide chemistry for automated immunoassay applications: A general procedure N2 - Immunochemical techniques are the workhorse for sample enrichment and detection of a large variety of analytes. In contrast to classical microtiter plate-based assays, microparticles are a next generation solid support, as they promote automation of immunoassays using flow-based techniques. Antibody immobilization is a crucial step, as these reagentsmare expensive, and inefficient coupling can result in low sensitivities. This paper proposes a general procedure for efficient immobilization of antibodies onto TentaGel particles, via Nhydroxysuccinimide chemistry. The goal was the preparation of solid supports with optimum immunorecognition, while increasing the sustainability of the process. The influence of buffer composition, activation and coupling time, as well as the amount of antibody on the immobilization efficiency was investigated, resorting to fluorophore-labeled proteins and fluorescence imaging. Buffer pH and activation time are the most important parameters for efficient coupling. It is demonstrated, that the hydrolysis of N-hydroxysuccinimide esters occurs at similar rates as in solution, limiting the utilizable time for coupling. Finally, applicability of the generated material for automated affinity extraction is demonstrated on the mesofluidic platform lab-on-valve. KW - Mesofluidics KW - Bead injections KW - ELISA KW - Carbamazepine KW - Biomarkers PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483919 DO - https://doi.org/10.1371/journal.pone.0218686 SN - 1932-6203 VL - 14 IS - 6 SP - e0218686, 1 EP - 18 PB - Public Library of Science CY - San Francisco, California, USA AN - OPUS4-48391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lörchner, Dominique A1 - Dittmann, Daniel A1 - Braun, Ulrike A1 - Kroh, L. W. A1 - Köppen, Robert T1 - Investigation of two triazine-based heterocyclic brominated flame retardants by coupled thermogravimetry-Fourier transform infrared spectroscopy N2 - In this study, the thermal decomposition of 1,3,5-tris-(2,3-dibromopropyl)-1,3,5-triazine-2,4,6-trione (TDBPTAZTO) and 2,4,6-tris-(2,4,6-tribromo-phenoxy)-1,3,5-triazine (TTBP-TAZ) were investigated for the first time by thermogravimetric analysis. Both compounds were thermal degraded between 225 and 350 °C (TDBP-TAZTO) as well as 300 and 400 °C (TTBP-TAZ). As a result, mass loss (%) of 98.5% for TTBP-TAZ and 95.4% for TDBP-TAZTO at 600 °C under N2 were observed. The major pyrolytic degradation products of TTBP-TAZ were formed in a single step and identified by FTIR analysis as 2,4,6-tribromophenol and further bromine-substituted aromatic compounds. In comparison, TDBP-TAZTO was pyrolytic degraded in two steps, whereby on the first step the release of hydrogen Bromide and 1,3,5-triallyl-1,3,5-triazine-2,4,6-trione could be detected. In the second minor step, isocyanic acid could be additionally identified. Subsequently, the obtained products of the TGA-FTIR measurements were used for a targeted search for mass fragments in mass spectrometry measurements. For TTBP-TAZ, only the degradation product 1,3,5-tribromobenzene could be detected by MS/MS analyzes. No comparable thermal degradation products, except hydrogen bromide, were observed in the MS/MS spectra of TDBP-TAZTO. Therefore, the search of further mass fragments was not possible compared to the findings of the TGA-FTIR measurements. KW - Pyrolysis KW - Thermal decomposition KW - TGA-FTIR KW - Mass spectrometry PY - 2019 DO - https://doi.org/10.1016/j.jaap.2019.104635 VL - 141 SP - 104635-1 EP - 104635-5 PB - Elsevier B.V. AN - OPUS4-48506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Everything SAXS N2 - A lecture to introduce small-angle scattering to Master's students at the Humbold University T2 - materials science course at HU Berlin CY - Adlershof, Berlin, Germany DA - 21.06.2019 KW - Small-angle scattering PY - 2019 AN - OPUS4-48518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim T1 - Photothermal super resolution image reconstruction using structured 1d laser illumination N2 - The separation of two closely spaced defects in fields of Thermographic NDE is very challenging. The diffusive nature of thermal waves leads to a fundamental limitation in spatial resolution. Therefore, super resolution image reconstruction can be used. A new concerted ansatz based on spatially structured heating and joint sparsity of the signal ensemble allows for an improved reconstruction of closely spaced defects. This new technique has been studied using a 1D laser array with randomly chosen illumination pattern. This paper presents the results after applying super resolution algorithms, such as the iterative joint sparsity (IJOSP) algorithm, to our processed measurement data. Different data processing techniques before applying the IJOSP algorithm as well as the influence of regularization parameters in the data processing techniques are discussed. Moreover, the degradation of super resolution reconstruction goodness by the choice of experimental parameters such as laser line width or number of measurements is shown. The application of the super resolution results in a spatial resolution enhancement of approximately a factor of four which leads to a better separation of two closely spaced defects. T2 - 46th Annual Review of Profress in Quantitative Nondestructive Evaluation CY - Portland, OR, USA DA - 14.07.2019 KW - Super resolution KW - Virtual wave KW - Laser thermography KW - 1d laser KW - Joint sparsity KW - Laser array KW - VCSEL array KW - High-power laser PY - 2019 AN - OPUS4-48591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim T1 - A comparison of different techniques for photothermal super resolution image reconstruction N2 - The separation of two closely located defects in fields of Thermographic NDE is very challenging. The diffusive nature of thermal waves leads to a fundamental limitation in spatial resolution. Therefore, super resolution image reconstruction can be used. A new concerted ansatz based on spatially structured heating and joint sparsity of the signal ensemble allows an improved reconstruction of closely located defects. This new technique has also been studied using 1D laser arrays in active thermography. The post-processing can be roughly described by two steps: 1. Finding a sparse basis representation using a reconstruction algorithm such as the Fourier transform, 2. Application of an iterative joint sparsity (IJOSP) method to the firstly reconstructed data. For this reason, different methods in post-processing can be compared using the same measured data set. The focus in this work was the variation of reconstruction algorithms in step 1 and its influence on the results from step 2. More precise, the measured thermal waves can be transformed to virtual (ultrasound) waves that can be processed by applying ultrasound reconstruction algorithms and finally the super resolution algorithm. Otherwise, it is also possible to make use of a Fourier transform with a subsequent super resolution routine. These super resolution thermographic image reconstruction techniques in post-processing are discussed and evaluated regarding performance, accuracy and repeatability. T2 - 20-th International Conference on Photoacoustic and Photothermal Phenomena CY - Moscow, Russia DA - 07.07.2019 KW - Super resolution KW - Virtual wave KW - Laser thermography KW - 1d laser KW - Joint sparsity KW - Laser array KW - VCSEL array KW - High-power laser KW - Fourier transform KW - Dimension reduction PY - 2019 AN - OPUS4-48592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Model of stimulated emission in aluminum laser-induced plasma produced by resonance pumping N2 - Stimulated emission observed experimentally in aluminum laser induced plasma is modeled via a kinetic approach. The simulated emission at several cascade transitions is created by a pump laser guided through the plasma at several microseconds after its creation and tuned in resonance with the strong transition at 266 nm. A two-dimensional space-time collisional radiative plasma model explains the creation of the population inversion and lasing at wavelengths 2.1 μm and 396.1 nm. The population inversion for lasing at 2.1 μm is created by depopulation of the ground state and population of the upper state via absorption of resonant radiation at 266 nm. The population inversion for lasing at 396.1 nm occurs during the laser pulse via the decay of the population of the pumped upper state to the lasing state via cascade transitions driven optically and by collisions. The model predicts that the population inversion and corresponding gain may reach high values even at moderate pump energies of several μJ per pulse. The efficiency of lasing at 2.1 μm and 396.1 nm is estimated to be on the order of a percent of laser pump energy. The polarization effect that the pump radiation at 266 nm imposes on the stimulated emission at 396.1 nm is discussed. The calculated results are favorably compared to experiment. T2 - FLAMN, June 30- July 4 2019 CY - St. Petersburg, Russia DA - 30.06.2019 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2019 AN - OPUS4-48598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gojani, Ardian A1 - Palásti, David J. A1 - Paul, Andrea A1 - Galbács, G. A1 - Gornushkin, Igor B. T1 - Analysis and classification of liquid samples by spatial heterodyne spectroscopy N2 - Spatial heterodyne spectroscopy (SHS) is used for quantitative analysis and classification of liquid samples. SHS is a version of a Michelson interferometer with no moving parts and with diffraction gratings in place of mirrors. The instrument converts frequency-resolved information into spatially resolved one and records it in the form of interferograms. The back-extraction of spectral information is done by the Fast Fourier transform. A SHS instrument is constructed with the resolving power 5000 and spectral range 522 - 593 nm. Two original technical solutions are used as compared to previous SHS instruments: the use of a high frequency diode pumped solid state (DPSS) laser for excitation of Raman spectra and a microscope-based collection system. Raman spectra are excited at 532 nm at the repetition rate 80 kHz. Raman shifts between 330 cm-1 and 1600 cm-1 are measured. A new application of SHS is demonstrated: for the first time it is used for quantitative Raman analysis to determine concentrations of cyclohexane in isopropanol and glycerol in water. Two calibration strategies are employed: univariate based on the construction of a calibration plot and multivariate based on partial least square regression (PLSR). The detection limits for both cyclohexane in isopropanol and glycerol in water are at a 0.5 mass% level. In addition to the Raman-SHS chemical analysis, classification of industrial oils (biodiesel, poly(1-decene), gasoline, heavy oil IFO380, polybutenes, and lubricant) is performed using their Raman-fluorescence spectra and principal component analysis (PCA). The oils are easily discriminated as they show distinct non-overlapping patterns in the space of principal components. KW - Spectroscopy KW - Atomic KW - Laser induced breakdown KW - Lasers PY - 2019 DO - https://doi.org/10.1177/0003702819863847 SN - 1943-3530 VL - 73 IS - 12 SP - 1409 EP - 1419 PB - Sage AN - OPUS4-48599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Calibration-free LIBS of steel samples N2 - An improved algorithm for calibration-free laser induced breakdown spectroscopy (CF LIBS) is presented which includes several novel features in comparison with previously proposed similar algorithms. In particular, it allows using spectral lines with arbitrary optical thickness for the construction of Saha-Boltzmann plots, retrieves the absorption path length (plasma diameter) directly from a spectrum, replaces the Lorentzian line profile function by the Voigt function, and allows for self-absorption correction using pre-calculated and tabulated data rather than approximating functions. The tabulated data embody the solutions of the radiative transfer equation for numerous combinations of optical thicknesses and line widths. The algorithm is used to analyze 100 low alloy steel spectra. T2 - 20.06.2019 LTB workshop on LIBS analysis of steel CY - Berlin, LTB, Germany DA - 20.06.2019 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics KW - Chemical reactors PY - 2019 AN - OPUS4-48600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tiebe, Carlo A1 - Hofmann, Michael T1 - Immer mehr Multigassensoren N2 - VDI-Richtlinien geben einen Überblick darüber, wie sich mehrere Gase gleichzeitig messen lassen. Dies ist etwa wichtig, um explosive Zusammensetzungen zu erkennen. Multigassensoren werden auch für Prozessüberwachung und Diagnose benötigt wie auch in den Bereichen Komfort und Umweltschutz. KW - Gassensor KW - Multigassensor KW - Sensorik PY - 2019 UR - https://www.umweltmagazin.de/2019/Ausgabe-06/Special-Mess-Steuer-und-Regeltechnik/Immer-mehr-Multigassensoren IS - 6 SP - 21 EP - 22 PB - VDI Fachmedien GmbH & Co. KG AN - OPUS4-48669 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Towards accurate analysis of particle size distribution for non-spherically shaped nanoparticles as quality control materials N2 - Measurement of nanoparticle size (distribution) becomes a challenging analytical problem when non-spherical nanoparticles must be accurately measured. Most industrial nanoparticles have not only non-spherical shapes but also possess polydisperse size distributions, and due to their agglomeration/aggregation state are difficult (or even impossible) to be addressed individually. Moreover, driven by regulatory purposes related to the identification of a material as a nanomaterial, the accurate measurement of the smallest dimension of a (nano)particulate material makes the analysis even more complex. In the first phase of the EU Project nPSize - Improved traceability chain of nanoparticle size measurements (https://www.bam.de/Content/DE/Projekte/laufend/nPSize/npsize.html), the efforts are focused on synthesis of nanoparticles of well-defined, non-spherical shape. Following candidates of reference materials (CRM) with certifiable particle size (distribution) are under characterization with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-60 nm lateral), (ii) titania bipyramides (~60 nm length x 40 nm width), (iii) titania acicular particles (100 nm length x 15-20 nm width; aspect ratio 5.5/6), (iv) gold nanorods (~10 nm width x 30 nm length), and (v) gold nanocubes (~55 nm x 55 nm x 55 nm). T2 - Microscopy & Microanalysis 2019 CY - Portland, OR, USA DA - 03.08.2019 KW - Nanoparticles KW - Reference materials KW - Traceability KW - Non-spherical shape KW - Titanium dioxide PY - 2019 AN - OPUS4-48671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim T1 - Thermographic super resolution imaging using structured 1D laser illumination N2 - Thermographic nondestructive evaluation (NDE) is based on the interaction of thermal waves with inhomogeneities. These inhomogeneities are related to sample geometry or material composition. Although thermography is suitable for a wide range of inhomogeneities and materials, the fundamental limitation is the diffusive nature of thermal waves and the need to measure their effect radiometrically at the sample surface only. The propagation of the thermal waves from the heat source to the inhomogeneity and to the detection surface results in a degradation in the spatial resolution of the technique. A new concerted ansatz based on a spatially structured heating and a joint sparsity of the signal ensemble allows an improved reconstruction of inhomogeneities. As a first step to establish an improved thermographic NDE method, an experimental setup was built based on structured 1D illumination using a flash lamp behind a mechanical aperture. As a follow-up to this approach, we now use direct structured illumination using a 1D laser array. The individual emitter cells are driven by a pseudo-random binary pattern and are additionally shifted by fractions of the cell period. The repeated measurement of these different configurations enables to illuminate each spot of the sample surface in lateral direction. This allows for a reconstruction that makes use of joint sparsity. The measured data set is processed using super resolution image reconstruction algorithms such as the iterative joint sparsity (IJOSP) algorithm. Using this reconstruction technique and 150 different illumination patterns results in a spatial resolution enhancement of approximately a factor of four compared to the resolution of 5.9 mm for homogenously illuminated thermographic reconstruction. Further, new data processing techniques have been studied before applying the IJOSP algorithm that are more performant or less prone to errors regarding image reconstruction. The choice of regularization parameters in data processing as well as experimental parameters such as the illumination pattern as a variable heat flux density (i.e., the Neumann boundary condition for convolution with the constant Green's function) have a big influence on the reconstruction goodness. With analytical-numerical modelling and numerical FEM simulations, we studied the influence of the experimental parameters on the result of the non-linear IJOSP reconstruction. This has also been investigated experimentally e.g. using different laser line widths or more measurements per position. These studies are used to derive optimal conditions for a certain measurement image reconstruction technique. T2 - 20-th International Conference on Photoacoustic and Photothermal Phenomena CY - Moscow, Russia DA - 07.07.2019 KW - Super resolution KW - Virtual wave KW - Laser thermography KW - 1d laser KW - Joint sparsity KW - Laser array KW - VCSEL array KW - High-power laser PY - 2019 AN - OPUS4-48578 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim T1 - Photothermal super resolution imaging: a comparison of different reconstruction techniques N2 - The diffusive nature of heat propagation complicates the separation of two closely spaced defects. This results in a fundamental limitation in spatial resolution. Therefore, super resolution (SR) image reconstruction can be used. SR processing techniques based on spatially structured heating and joint sparsity of the signal ensemble allows for an improved reconstruction of closely spaced defects. This new technique has been studied using a 1D laser array with randomly chosen illumination pattern. This paper presents the results after applying SR algorithms such as the iterative joint sparsity (IJOSP) algorithm, to our processed measurement data. Two different data processing strategies are evaluated and discussed regarding their influence on the reconstruction goodness as well as their complexity. Moreover, the degradation of the SR reconstruction by the choice of regularization parameters in data processing is discussed. The application of both SR techniques that are evaluated in this paper results in a spatial resolution enhancement of approximately a factor of four which leads to a better separation of two closely spaced defects. The fundamental difference between both SR techniques is their complexity. T2 - 46th Annual Review of Profress in Quantitative Nondestructive Evaluation CY - Portland, OR, USA DA - 14.07.2019 KW - Super resolution KW - Virtual wave KW - Laser thermography KW - 1d laser KW - Joint sparsity KW - Laser array KW - VCSEL array KW - High-power laser KW - Fourier transform KW - Dimension reduction PY - 2019 AN - OPUS4-48579 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. A1 - Neumann, Patrick P. A1 - Hüllmann, Dino A1 - Kohlhoff, Harald A1 - Bartholmai, Matthias A1 - Bennetts, V. H. A1 - Lilienthal, A. J. T1 - Remote Gas Sensing with Multicopter-Platforms N2 - This presentation gives an introduction to the gas-sensitive aerial robots developed at BAM, including various application examples in the field of mobile robot olfaction: gas source localization and gas distribution mapping. T2 - Zweites Innovationsforum "Autonome, mobile Dienste; Services für Mobilität" CY - Berlin, Germany DA - 04.06.2019 KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS); UAV-REGAS KW - Localization of gas sources KW - Mobile Robot Olfaction KW - Nano UAV Swarm KW - Tomographic reconstruction of gas plumes PY - 2019 UR - http://modisem.de/files/Ereignisse/2019-06/Innovationsforum_Downloads/IF2_2019_Tagungsband_WEB.pdf SN - 978-3-942709-22-4 N1 - Tagungsband auf Deutsch, Beitrag auf Englisch. VL - 2019 SP - 24 EP - 34 AN - OPUS4-48699 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Boehm, S. T1 - Analysis of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by EPMA and µ-XRF N2 - The present study reports on measurements on thin Fe-Ni films on silicon and first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide Substrate by electron probe microanalysis (EPMA). Standard-based and standardless EPMA (with EDS) results were used in combination with the thin film analysis software Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. An excellent agreement has been obtained between the atomic fractions determined by EPMA and µ-XRF with the KRISS certified values. T2 - Microscopy & Microanalysis 2019 CY - Portland, OR, USA DA - 03.08.2019 KW - Thin films KW - EPMA KW - µ-XRF KW - Elemental composition KW - Atomic fraction KW - Fe-Ni KW - Si-Ge PY - 2019 AN - OPUS4-48709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Detektion von Mikroplastik mittels Thermoextraktion Desorption Gas Chromatographie Massen Spektrometrie (TED-GC-MS) N2 - Das Poster gibt eine kurze Einleitung in die Thematik Mikroplastik in der Umwelt. Das Funktionsprinzip des Verfahrens und einige Kenndaten werden dargestellt. Optimierte Verfahrensparameter werden aufgezählt und Teilergebnisse aus zwei Messkampagnen gezeigt. T2 - Abschlusskonferenz BMBF-Projekt MiWa CY - Karlsruhe, Germany DA - 09.09.2019 KW - Mikroplastik KW - TED-GC-MS KW - Optimierung PY - 2019 AN - OPUS4-49117 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nöller, Renate A1 - Feldmann, Ines A1 - Kasztovszky, Z. A1 - Szőkefalvi-Nagy, Z. A1 - Kovács, I. T1 - Characteristic Features of Lapis Lazuli from Different Provenances, Revised by µXRF, ESEM, PGAA and PIXE N2 - The objective of this study is to find out, to what extent the geochemical characteristics of lapis lazuli can be utilized in respect to its provenance. A wide range of variables is taken into consideration depending on the quantity of samples analysed from a specific geological region and the methods applied. In order to provide evidence, a multi-technique analytical approach using µXRF, ESEM, PGAA and PIXE is applied to samples from the most famous deposits of lapis lazuli. Special elements determined as fingerprints are compared in relation to the forming conditions obvious in textural features. The results and statistical output allow a differentiation that enables an optimized local classification of the blue stone. An absolute requirement for all geo-tracing performed on blue colored cultural objects of unknown provenance is awareness of the limits of analysis. The possible sources of lapis lazuli are tested by analysing the blue pigment used as paint on murals and ink on manuscripts from the Silk Road. KW - Lapis lazuli KW - Micro-XRF KW - ESEM KW - PGAA KW - PIXE KW - Pigment analyses KW - Provenance studies PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491181 DO - https://doi.org/10.17265/2328-2193/2019.02.003 SN - 2328-2193 VL - 7 IS - 2 SP - 57 EP - 69 PB - David CY - New York, NY AN - OPUS4-49118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska A1 - Brunner, A. J. ED - Rosemarie, Helmerich ED - Ilki, A. ED - Motavalli, M. T1 - Towards predictor development for assessing structural integrity of components made from wood materials using Acoustic Emission monitoring and signal analysis N2 - Against the background of sustainable resource management and efficiency, wood-based materials are currently experiencing a revival and, among others, plywood, Laminated Veneer Lumber and glued laminated timber are becoming increasingly more important in the building sector. Even though these materials are so-called engineered products, the element wood is naturally grown with intrinsic variability in mechanical properties and requires professional handling on-site. Otherwise, load-bearing structures made of wood materials may entail certain risks. Critical situations can, in principle, be avoided by implementing a structural health monitoring system into components or structures made from wood material. The aim is to indicate accumulation of mechanical damage and to eliminate or at least significantly reduce the risk of unexpected failure. Toward this purpose, the failure behavior of several layered wood materials under quasi-static tension was investigated in laboratory-scale experiments by means of acoustic emission (AE) measurement. Based on spectral analysis and pattern recognition, two classes of AE signals are identified for each investigated lay-up that are characterized by either low or high frequency contents in the respective power spectra. AE activity and intensity of both signal classes are analyzed, striving for predictors appropriate for AE monitoring concepts. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures (SMAR 2019) CY - Potsdam, Germany DA - 27.08.2019 KW - Acoustic Emission Monitoring KW - Signal Analysis KW - Structural Integrity KW - Wood Materials PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491198 SN - 978-3-947971-07-7 SP - Paper Tu.2.D.4, 1 EP - 8 PB - German Society for Non-Destructive Testing (DGZfP e.V.) AN - OPUS4-49119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Burgholzer, P. A1 - Berer, T. A1 - Ziegler, Mathias A1 - Thiel, Erik A1 - Ahmadi, Samim A1 - Gruber, J. A1 - Mayr, G. A1 - Hendorfer, G. T1 - Blind structured illumination as excitation for super-resolution photothermal radiometry N2 - Photothermal radiometry with an infrared camera allows the contactless temperature measurement of multiple surface pixels simultaneously. A short light pulse heats the sample. The heat propagates through the sample by diffusion and the corresponding temperature evolution is measured at the sample’s surface by an infrared camera. The main drawback in radiometric imaging is the loss of the spatial resolution with increasing depth due to heat diffusion, which results in blurred images for deeper lying structures. We circumvent this information loss due to the diffusion process by using blind structured illumination, combined with a non-linear joint sparsity reconstruction algorithm. The structured illumination is realized by parallel laser lines from a vertical-cavity surface-emitting laser (VCSEL) array controlled by a random binary pattern generator. By using 150 different patterns of structured illumination and our iterative joint sparsity algorithm, it was possible to resolve 1 mm thick lines at a distance down to 0.5 mm, which results in a resolution enhancement of approximately a factor of four compared to the resolution of 5.9 mm for homogenous illuminated thermographic reconstruction. KW - Super-resolution imaging KW - Thermography KW - Blind structured illumination KW - VCSEL array PY - 2019 DO - https://doi.org/10.1080/17686733.2019.1655247 SN - 1768-6733 VL - 17 IS - 4 SP - 268 EP - 278 PB - Taylor & Francis Group CY - Milton, UK AN - OPUS4-49122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona T1 - Web Mining zur Erforschung von Nutzung von Standards und Zertifikaten N2 - Anhand eines Anwendungsbeispiels im Bereich Informationssicherheit wird das Web Mining von Unternehmenswebseiten vorgestellt und diskutiert. T2 - Abteilungsseminar CY - BAM, Berlin DA - 28.01.2019 KW - Management Systeme KW - Web Mining KW - Informationssicherheit PY - 2019 AN - OPUS4-49028 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona T1 - Exploring the Diffusion of the ISMS Standard ISO/IEC 27001 N2 - We presented and discussed the applicability of Web Mining to explore the Diffusion of Management System Standards, in particular in regards to Information Security T2 - EURAS Conference CY - Rome, Italy DA - 14.06.2019 KW - Diffusion KW - Management system standard KW - Information security KW - Web Mining PY - 2019 AN - OPUS4-49029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona A1 - Blind, K. ED - Jacobs, K. ED - Morone, P. T1 - Exploring the Diffusion of an ISMS Standard N2 - This paper introduces and discusses the applicability of Web Mining of Firm Websites to explore the Diffusion of Management System Standards using the example of an ISMS Standard. T2 - EURAS Conference CY - Rome, Italy DA - 13.06.2019 KW - Management System Standard KW - Information Security KW - Web Mining PY - 2019 SN - 978-3-95886-282-1 VL - 24 SP - 329 EP - 348 PB - Verlagshaus Mainz GmbH CY - Aachen, Germany AN - OPUS4-49031 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Mikroplastik-Bestimmung mit TED-GC-MS N2 - Der Vortrag beschreibt den Entwicklungsprozess des Analysenverfahrens TED-GC-MS zur Bestimmung von Mikroplastikgehalten in Umweltproben im Rahmen des BMBF-Projektes MiWa. Die Funktionsweise, die Automatisierung und die Optimierung einzelner Geräteparameter und Leistungsdaten werden gezeigt. Untersuchungen des Einflusses von Probenmatrices werden dargestellt und die Ergebnisse einiger Messkampagnen und Ringversuche vorgestellt, die die Routinefähigkeit des Verfahrens dokumentieren. T2 - MiWa-Abschlusskonferenz CY - Karlsruhe, Germany DA - 10.09.2019 KW - Mikroplastik KW - Thermoanalyse KW - TED-GC-MS PY - 2019 AN - OPUS4-49115 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg ED - Spranger, Holger T1 - Synthetische Aperturfokussierung für die Terahertzspektroskopie N2 - Die zeitaufgelöste THz-Spektroskopie (THz-TDS) operiert mit elektromagnetischen Impulsen, die ein Amplitudenspektrum im unteren THz-Bereich aufweisen. Die THz-TDS ist in der Lage, dielektrische Volumina zerstörungs- und kontaktfreie zu durchstrahlen. Um eine 3D-THz Bildung zu ermöglichen, wurde für die THz-TDS ein rechnergestütztes Mess- und Rekonstruktionsverfahren (THz-TDSAFT) entwickelt, mit dem es gelingt, unter Verwendung der im Zeitbereich registrierten THz-TDS-Daten das Volumeninnere in Form eines dreidimensionalen Tomogramms zu rekonstruieren. Die THz-TD-SAFT basiert auf die für die Ultraschalltechnik entwickelte Synthetische Apertur Fokussierung (SAFT) bzw. des heuristisch begründeten Algorithmus des Synthetischen Apertur Radars (SAR). Anhand von Beispielen wird die Möglichkeiten der THz-TD-SAFT demonstriert und nachgewiesen, dass mit dem Rekonstruktionsansatz die künstlich eingebauten Fehlstellen bezüglich der Position und Größe geometrisch richtig im Tomogramm abgebildet werden können. T2 - 4. Fachseminar des FA MTHz, Mikrowellen- und Terahertz-Prüftechnik in der Praxis CY - Fürth, Germany DA - 02.04.2019 KW - THz-TDS KW - Tomographie, KW - Zerstörungsfreie Prüfung PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-490481 UR - https://www.ndt.net/search/docs.php3?MainSource=262 SP - 1 EP - 8 PB - DGZfP CY - Berlin AN - OPUS4-49048 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Determination of chromium(VI) in phosphorus fertilizers made from recycled materials by DGT N2 - Phosphorus (P) fertilizers from secondary resources became increasingly important in the last years. However, these novel P-fertilizer can also contain toxic pollutants e.g. chromium (Cr) in the hexavalent state (Cr(VI)), which is regulated with low limit values in agricultural products (German fertilizer ordinance limit: 2 mg/kg Cr(VI)). The determination of Cr(VI) in these novel fertilizer matrices can be hampered by redox processes that lead to false results with the standard wet chemical extraction method (German norm DIN EN 15192). Therefore, we analyzed Cr(VI) in various P-fertilizers with the DGT technique. DGT devices equipped with a APA (polyacrylamide) diffusion layer and Cr(VI) selective N-methyl-D-glucamine (NMDG) binding layer were used for the study. After a 24 h conditioning period of the fertilizer at 60% of the water holding capacity (WHC), the fertilizers were brought to 100% WHC, transferred onto the DGT devices and deployed for 24 h at 25°C. The extraction of Cr from the DGT binding layer was carried out with 1 M HNO3 for 24 h. The Cr-concentrations of the extract were determined by means of ICP-MS. We found a good correlation between the standard wet chemical extraction and the DGT method for the whole range of P-fertilizers. However, partly soluble Cr(VI) compounds cannot be detected in full extent by the DGT method that is best suited for mobile Cr(VI). Furthermore, Cr K-edge XANES spectroscopy showed that the Cr(VI)-selective DGT binding layer also adsorbs mobile Cr(III) compounds from acid treatment of phosphates which can therefore cause an overestimation of Cr(VI). The DGT method was very sensitive and in most cases selective for the analysis of Cr(VI) in P-fertilizers made from recycled materials. However, the results of certain types of P-fertilizers containing mobile Cr(III) or partly immobile Cr(VI) show that still some optimization of the method is required to avoid over- or underestimation of Cr(VI). T2 - 6th Conference on Diffusive Gradients in Thin Films CY - Vienna, Austria DA - 17.09.2019 KW - Fertilzer KW - Pollutant KW - Chromium KW - Diffusive gradients in thin films (DGT) KW - XANES spectroscopy PY - 2019 AN - OPUS4-49058 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - Time- and lateral-resolved X-ray absorption fine structure spectroscopy N2 - We developed a setup for time- and lateral-resolved X-ray absorption fine structure (XAFS) spectroscopy. A dispersive element is placed behind the sample to investigate. The broadband incoming beam transmits the sample, is then dispersed and finally collected by a position sensitive detector. This allows the recording of a whole X-ray absorption near edge structure (XANES) or extended X-ray absorption fine structure (EXAFS) spectrum in a single shot. The dispersive element is a Si(111) crystal, bent by means of a so called wafer bender, developed in house. Our setup is very flexible, easy to adjust and allows a time resolution down to one second which can be used to follow chemical reactions with dynamics on this time scale. T2 - SXR2019 CY - Berlin, Germany DA - 16.09.2019 KW - Spectroscopy KW - X-ray KW - Absorption KW - Synchrotron PY - 2019 AN - OPUS4-49045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Introduction meeting FINAS - Analysis of the operation of accreditation bodies in Europe N2 - The long-term goal of the benchmarking project for European accreditation bodies is twofold: First of all, the project is supposed to help the European accreditation attending bodies to improve their processes by identifying best practices and by learning from others. Possibly Secondly, the results of the analysis can be used by the European Cooperation for Accreditation (EA) to identify differences in the operation of the European accreditation bodies and based on this knowledge to promote harmonization of accreditation activities in Europe. T2 - Kick-off at FINAS, Helsinki CY - Helsinki, Finland DA - 19.08.2019 KW - Accreditation KW - Benchmarking PY - 2019 AN - OPUS4-49046 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Introduction meeting accredia - Analysis of the operation of accreditation bodies in Europe N2 - The long-term goal of the benchmarking project for European accreditation bodies is twofold: First of all, the project is supposed to help the European accreditation attending bodies to improve their processes by identifying best practices and by learning from others. Possibly Secondly, the results of the analysis can be used by the European Cooperation for Accreditation (EA) to identify differences in the operation of the European accreditation bodies and based on this knowledge to promote harmonization of accreditation activities in Europe. T2 - Kick-off at Accredia, Milano CY - Mailand, Italy DA - 28.08.2019 KW - Accreditation KW - Benchmarking PY - 2019 AN - OPUS4-49047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Harmonization in microplastics Analysis N2 - The lecture summarizes the current status of hamonization edr microplastics analytics in Germany. T2 - Symposium on Occurrence and Fate of Microplastics CY - Beijing, China DA - 09.07.2019 KW - Microplastics KW - TED-GC-MS KW - Harmonisation PY - 2019 AN - OPUS4-49063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Messen ist nicht alles, aber ohne Messmethoden ist alles nichts!  N2 - Der Vortrag fasst den aktuellen Methodenstand bei der Analytik für Mikroplastik zusammen. T2 - FACHFORM „Mikroplastik“ anlässlich VUP-Jahrestagung 2019 CY - Gießen, Germany DA - 05.09.2019 KW - Mikroplastik KW - TED-GC-MS KW - Hamonisierung PY - 2019 AN - OPUS4-49066 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Analytik von Mikroplastik - Verfahren-Ergebnisse-Harmonisierung N2 - Die zunehmenden Nachweise von Kunststoffen in verschiedenen Umweltmedien erfahren in den letzten Jahren weltweit ein zunehmendes wissenschaftliches, gesellschaftliches und politisches Interesse. Besondere Aufmerksamkeit erfahren Kunststoffpartikel von 1-1.000 µm, sogenanntes Mikroplastik. Es wurde mittlerweile in Wasser, Böden, Luft und Biota nachgewiesen. Obwohl die Wirkungen auf die natürlichen Umweltfunktionen noch unklar sind und kontrovers diskutiert werden, ist allein durch die ubiquitäre Präsenz eine systematische Erfassung von Eintragsquellen und Verbleib der Partikel über alle Umweltmedien notwendig, um Maßnahmen zur Reduktion der Einträge zu veranlassen. Für eine zuverlässige Erfassung sind medienübergreifende Verfahren zu entwickeln, welche die drei analytischen Schritte, Probennahme, Probenaufbereitung und Detektion beinhalten. Die Verfahren adressieren unterschiedliche Zielgruppen, welche verschiedene analytische Informationen fordern. Für die akademische Bewertung werden Verfahren mit hohem analytischen Aufwand favorisiert, welche möglichst detaillierte Information über Partikelsorte, -größe, -zahl und -oberflächenbeschaffenheit geben. Im Gegensatz dazu, fordern Anwender aus der Praxis schnelle und einfache Monitoring Verfahren, welche die Bestimmung eines Massengehaltes, bzw. eines Grenzwertes zulassen. Allen ist gemeinsam, dass ein hoher interdisziplinärer Anspruch besteht, der sowohl technische Voraussetzungen zur repräsentativen Probennahme und die Limitationen von Detektionsverfahren berücksichtigt, als auch die Fachkompetenz von Biologen, Umweltwissenschaften, Analytiker und Polymerwissenschaftler einschließt. Verfahren zum Mikroplastiknachweis müssen auch verschieden Proben mit sehr unterschiedlichen Gehalten an natürlicher Matrix gerecht werden. So müssen allein für Wasser Verfahren entwickelt werden, die Mikroplastik verschiedener Form (sphärische Partikel, komplexe Bruchstücke, Fasern) aus Medien mit sehr variablen Partikelanteil (u.a. Trinkwasser, Oberflächenwasser, Abwasser) repräsentativ erfassen, sowie schnell und kostengünstig sind – einschließlich der notwendigen Probenaufbereitung. Die jeweiligen Detektionsverfahren müssen z.B. einzelne Partikel oder integrale Gehalte über drei Dekadenklassen für thermoplastische und insbesondere auch elastomere Partikelsorten erfassen können. T2 - GDCh Wissenschaftsforum CY - Aachen, Germany DA - 15.09.2019 KW - Mikroplastik KW - Analytik KW - TED-GC-MS PY - 2019 AN - OPUS4-49068 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaenisch, Gerd-Rüdiger T1 - EMPIR Project NanoXSpot N2 - The overall objective of project NanoXSpot (Nanometre X-ray Focal Spot Measurement) is to develop traceable measurement methods for determining the focal spot size, shape, and position of nanometre resolution X-ray tubes. The impact of the technical results will be ensured by preparing prenormative documents for submission to CEN TC 138 (Non-destructive testing) WG 1 (Radiographic testing), which directly addresses the research needs of CEN, currently revising standards in the series 12543 for focal spot measurements below 5 µm spot size to harmonise standards and measurement method between ASTM and CEN. T2 - DACH-Tagung CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Standardization KW - X-Ray tube KW - Focal spot measurement PY - 2019 AN - OPUS4-48298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, U. T1 - Neue Konzepte zur Messung von Parametern der Brennflecke von Nano- und Mikrofokus-Röntgenröhren N2 - Die exakte Messung der Brennfleckgrößen von Röntgenröhren, Betatrons und Linear-Beschleunigern ist immer noch ein offenes Problem. Es existieren diverse Standards, die alle zu unterschiedlichen Resultaten führen in Abhängigkeit von der Brennfleckform. CEN hat 1999 die Serie EN 12543 (5 Teile) veröffentlicht, die die Messung der Brennfleckgrößen von Röntgenröhren für ZfP-Anwendungen beschreibt. Die Messprozeduren und Toleranzen unterscheiden sich von den Messstandards für medizinische Röntgenröhren, wie z. B. DIN EN 60336:2006 / IEC 60336:2005. EN 12543 beschreibt verschiedene Messmethoden für Standard-, Minifokus- und Mikrofokus-Röntgenröhren. CEN TC 138 WG 1 und ASTM E 07 revidieren bzw. revidierten daher die Standards zur Brennfleckmessung, wobei alle Messungen auf Pin-Hole- oder Kantenabbildungen zurückgeführt werden sollen. Die Schlitzblenden-Messung wird dann nur noch in der Medizin Anwendung finden. Es wurden auch tomographische Verfahren zur Rekonstruktion von Brennflecken vorgeschlagen. Die derzeit verfügbaren Standards decken den Bereich von 5 μm bis zu mehreren Millimetern ab. Mit der Entwicklung von Nanofokus-Röhren haben Hersteller unterschiedliche Verfahren zur Auflösungs- oder Brennfleckmessung eingeführt, deren Werte teilweise um den Faktor 2 unterschiedlich sind. Vorrangig wird hierbei auf ein JIMA-Target zurückgegriffen, dessen Auswertung die Detailerkennbarkeit widerspiegelt. Verschiedene Europäische Partner diskutieren derzeit Konzepte zur Messung von Brennflecken im Bereich von 100 nm bis 5 μm. Dabei werden hauptsächlich Messprozeduren zur Auswertung der Aufnahmen von Strichgruppenkörpern und kleinen Lochplatten untersucht. Als Ergebnis sollen Daten zur Brennflecklänge, -breite und -form bestimmt und standardisiert werden, um Produkte vergleichbar zu klassifizieren. Erste Konzepte hierzu und Ergebnisse früherer Untersuchungen werden vorgestellt. T2 - DACH-Tagung CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Brennfleckmessung KW - Radiographie KW - Röntgenröhren PY - 2019 AN - OPUS4-48299 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Konchina, V. N. T1 - ПОДГОТОВКА И СЕРТИФИКАЦИЯ ПЕРСОНАЛА ПО НЕРАЗРУШАЮЩЕМУ КОНТРОЛЮ ОБЪЕКТОВ ЖЕЛЕЗНОДОРОЖНОГО ТРАНСПОРТА В ПГУПС N2 - Безопасность движения на железнодорожном транспорте обеспечивается широким применением современных компьютеризированных средств неразрушающего контроля (НК), которые требуют квалифицированного персонала для их обслуживания и расшифровки результатов контроля. Персонал, занятый НК элементов инфраструктуры и подвижного состава при их эксплуатации и техническом обслуживании (ремонте), а также в предприятиях, изготавливающих продукцию железнодорожного назначения, включает: инженерные кадры - работников, в функциональные обязанности которых входит организация или организация и выполнение НК (в том числе и разработка технологий и технологической документации по НК), а также расшифровка результатов НК, и рабочих – дефектоскопистов или операторов дефектоскопных тележек. Система подготовки персонала по НК, действующая на железнодорожном транспорте и реализуемая в ПГУПС кафедрой «Методы и приборы неразрушающего контроля», созданной А.К.Гурвичем в 1977 году, включает профессиональнее обучение, высшее профессиональное образование по направлению «Приборостроение», дополнительное профессиональное образование - повышение квалификации и переподготовку (в том числе, для персонала железнодорожных специальностей). В соответствии с требованиями действующих нормативных документов подтверждение квалификации производится путем сертификации. Уполномоченный орган по сертификации персонала по НК, создан и функционирует в ПГУПС в рамках системы добровольной сертификации персонала по НК (Руководящий орган – Регистр систем сертификации персонала), деятельность которой в области железнодорожного транспорта управляется и контролируется Технической комиссией по железнодорожному транспорту, включающей представителей Росжелдора, ОАО «РЖД», промышленных предприятий - работодателей, Уполномоченных органов и Экзаменационных центров системы сертификации. В докладе представлены и проанализированы результаты деятельности кафедры МПНК и Квалификационного центра по НК в ПГУПС. T2 - XXIII Petersburg Scientific and Technical Conference "Ultrasonic flaw detection of metals and advanced materials" UZDM-2019 CY - St. Petersburg, Repino, Russia DA - 28.05.2019 KW - Transportwesen KW - Personalzertifizierung KW - ZfP-Ausbildung KW - Lehrplan Universität PY - 2019 AN - OPUS4-48300 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dümichen, Erik A1 - Eisentraut, Paul A1 - Celina, M. A1 - Braun, Ulrike T1 - Automated thermal extraction-desorption gas chromatography mass spectrometry: A multifunctional tool for comprehensive characterization of polymers and their degradation products N2 - The TED-GC-MS analysis is a two-step method. A sample is first decomposed in a thermogravimetric analyzer (TGA) and the gaseous decomposition products are then trapped on a solid-phase adsorber. Subsequently, the solid-phase adsorber is analyzed with thermal desorption gas chromatography mass spectrometry (TDU-GC-MS). This method is ideally suited for the analysis of polymers and their degradation processes. Here, a new entirely automated System is introduced which enables high sample throughput and reproducible automated fractioned collection of decomposition products. Strengths and limitations of the system configuration are elaborated via three examples focused on practical challenges in materials analysis and identification: i) separate analysis of the components of a wood-plastic-composite material, ii) quantitative determination of weight concentration of the constituents of a polymer blend and iii) quantitative analysis of model samples of microplastics in suspended particulate matter. KW - Thermal extraction-desorption gas chromatography mass spectrometry KW - Analysis KW - Polymers KW - Microplastics KW - Automation PY - 2019 DO - https://doi.org/10.1016/j.chroma.2019.01.033 VL - 1592 SP - 133 EP - 142 PB - Elsevier CY - Amsterdam AN - OPUS4-48287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radunz, Sebastian A1 - Andresen, Elina A1 - Würth, Christian A1 - Koerdt, Andrea A1 - Rune Tschiche, Harald A1 - Resch-Genger, Ute T1 - Simple self-referenced luminescent pH sensors based on upconversion nanocrystals and pH-sensitive fluorescent BODIPY dyes N2 - We present the design and fabrication of pH responsive ratiometric dual component sensor systems based on multicolor emissive upconversion nanoparticles (UCNP) and pH sensitive BODIPY dyes with tunable pKa values embedded into a polymeric hydrogel matrix. The use of NIR excitable NaYF4:Yb3+,Tm3+ UCNPs enables background free read-out. Furthermore, the spectrally matching optical properties of the UCNPs and the dyes allow the UCNPs to serve as excitation light source for the analyteresponsive BODIPY as well as intrinsic reference. The blue upconversion luminescence (UCL) of NaYF4:Yb3+,Tm3+ UCNPs excited at 980 nm, that overlaps with the absorption of the pH-sensitive fluorophore, provides reabsorption based excitation of the dye, the spectrally distinguishable green fluorescence of which is switched ON upon protonation, preventing photoinduced electron transfer (PET) within the dye moiety, and the pH-inert red UCL act as reference. The intensities ratios of the dye’s fluorescence and the analyte-inert red Tm3+ UCL correlate directly with pH, which was successfully utilized for Monitoring timedependent pH changes of a suspension of quiescent E. coli metabolizing D-glucose. KW - pH sensor KW - UpConversion PY - 2019 DO - https://doi.org/10.1021/acs.analchem.9b01174 SN - 0003-2700 SN - 1520-6882 VL - 91 SP - 7756 EP - 7764 PB - acs publications AN - OPUS4-48490 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Daniel T1 - Mueller-matrix imaging ellipsometry of structural anomalies and inhomogenities N2 - In the last years, the implementation of imaging ellipsometry in the variety of optical characterization techniques has shown tremendous potential to analyze the topology of surfaces in the lateral dimension. In the later studies, this contrast-rich surface images were affiliated with changes of the refraction indices, Absorption bands or layer thicknesses. However, it was realized that additional factors like curvature or scattering can have a great Impact on the ellipsometric readout of the analyzed system. In this study, we focus on the systematic evaluation of structural anomalies and inhomogenities of several Basic systems. This includes spherical particles as a model for microscopic curved surfaces in a range of 0.25 to 25 μm in diameter. In the macroscopic regime several conventional convex lenses were analyzed. Additional affords were made to generate microscopic concave model systems by applying nanoindentation with a spherical indentation unit. With this method calottes with a depth of 0.04 to 2 μm and radius of 2.5 μm were made. The macroscopic counterpart is delivered by conventional concave lens systems. For all systems, a variety of different bulk materials was investigated. This includes metal oxides, metals and polymers as well as combinations of each by applying coatings on the bulk materials with different layer thicknesses. To analyze these structural anomalies and inhomogenities properly, Mueller-Matrix imaging ellipsometry is the method of choice to address cross- and depolarization effects that occur due to the curved surfaces. Supplementary methods were used for an independent characterization of the topological properties of all structural anomalies and inhomogenities. This includes AFM and SEM for the microscopic samples (microparticles and nanoindented holes) and white light interferometry for the macroscopic lenses. This study results in a systematic screening of different coated and uncoated material systems with a topology that does not fit into conventional ellipsometry and thus is analyzed by Muller-Matrix imaging ellipsometry. This will help in quality control and is a contribution to the understanding of the polarizing effects of non-ideal Systems analyzed by ellipsometry. T2 - 8th International conference on spectroscopic ellipsometry (ICSE-8) CY - Barcelona, Spain DA - 26.05.2019 KW - Spectroskopic Imaging KW - Mueller-Matrix imaging ellipsometry KW - Structural anomalies KW - Structural inhomogenities PY - 2019 AN - OPUS4-48347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena T1 - Standardization of spectroscopic ellipsometry as GUM-compliant accredited measurement method N2 - Ellipsometry has become a powerful measurement tool in semiconductor industry since the sixties of the last century. Early standardization activities focused exclusively on SiO2/Si (ASTM F 576-01, SEMI 3624). The first generic standard dealing with ellipsometry is DIN 50989-1:2018 Ellipsometry – Part 1: Principles. Standardization is a prerequisite for accreditation according to DIN EN ISO/IEC 17025 and the evaluation of uncertainty budgets. T2 - 8th International conference on spectroscopic CY - Barcelona, Spain DA - 26.05.2019 KW - Standardization of Ellipsometry KW - GUM-compliance KW - Uncertainty budgets KW - Bulk material PY - 2019 AN - OPUS4-48348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pellegrino, F. A1 - Sordello, F. A1 - Mino, L. A1 - Minero, C. A1 - Hodoroaba, Vasile-Dan A1 - Martra, G. A1 - Maurino, V. T1 - Formic acid photoreforming for hydrogen production on shape-controlled anatase TiO2 nanoparticles: Assessment of the role of fluorides, {101}/{001} surfaces ratio, and platinization N2 - Hydrogen production via formate photoreforming on TiO2 is characterized by marked dependence on the ratio between {101} and {001} surfaces for anatase nanoparticles. We observed higher rates of hydrogen Evolution with the increase of the {101} facets presence, owing to their reductive nature. This helps the Pt photodeposition in the early stages of Irradiation and, then, the hydrogen ion reduction reaction. The selective photodeposition of 2 nm Pt nanoparticles on {101} facets was confirmed by transmission electron microscopy (TEM) micrographs. The results are confirmed also by experiments carried out without the use of Pt as cocatalyst and by photoelectrochemical measurements. The work also explains the marginal effect of the fluorination on the H2 evolution. KW - Titanium dioxide KW - Fluoride KW - Platinum KW - Nanoparticles KW - Controlled-shape KW - Hydrogen photoproduction KW - Surface PY - 2019 UR - https://pubs.acs.org/doi/10.1021/acscatal.9b01861 DO - https://doi.org/10.1021/acscatal.9b01861 SN - 2155-5435 VL - 9 IS - 8 SP - 6692 EP - 6697 PB - ACS Publications AN - OPUS4-48355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Beck, Uwe A1 - Baier, Jennifa A1 - Dähne, L. A1 - Lerche, K.-H. T1 - Schlussbericht zum BMWi/MNPQ-Verbundprojekt: PLASMA-FIT (PLASMA-kompatible Partikel zur gepulsten in-situ Injektion von ex-situ hergestellten Partikeln für add-on Funktionen und zur Identifizierung in BeschichTungen) N2 - Im Fokus steht die Qualitätssicherung mit Blick auf Herstellung, Modifizierung, Handling und Erprobung von PLASMA-kompatiblen Partikeln zur gepulsten in-situ Injektion von ex-situ hergestellten Partikeln für add-on Funktionen in und zur Identifikationsprüfung von BeschichTungen (PLASMA-FIT). Im Kern war zunächst zu prüfen, welche Klassen ex-situ hergestellter Partikel unterschiedlichster Materialien überhaupt bzw. unter welchen Bedingungen PLASMA-fit sind oder unter welchen Randbedingungen PLASMA-fit gemacht werden können. In den dazugehörenden Projektphasen Screening und Adaption stand dabei das komplexe Beanspruchungsszenario bestehend aus Vakuum-, Temperatur- und wenigstens kurzzeitiger Plasmabeständigkeit der ex-situ bereitgestellten Partikel im Fokus. In der Projektphase Applikation sollte dann unter Verwendung einer modifizierten Plasmaquelle (BAM-Patentanmeldung, beabsichtigte Lizenznahme durch Fa. CemeCon, Optionsvertrag) hinsichtlich der Realisierbarkeit, Prüfung und Qualitätssicherung von Plasmadispersionsschichten ein erster Praxistest zur in-situ Injektion von Partikeln in einen laufenden Beschichtungsprozess, zur Realisierung funktioneller Eigenschaften z.B. zur Identifikation oder Authentifizierung von Originalteilen, vorgenommen werden KW - Plasma-kompatible Partikel KW - Plasma-Injektion KW - add-on Funktionen PY - 2015 N1 - Das Dokument unterliegt der Vertraulichkeit und kann nicht zugänglich gemacht werden - The document is subject to confidentiality restrictions and cannot be made accessible - Projektlaufzeit: 17.11.2010-16.02.2015 - Project runtime: 17.11.2010-16.02.2015 SP - 1 EP - 10 AN - OPUS4-48360 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Foschung an der BAM - Von Termiten bis zum 3D Druck in der Schwerelosigkeit N2 - Eine Übersicht über die Forschung an der BAM mit Schwerpunkt auf dem Fachbereich Strukturanalytik T2 - Naturwissenschaftstag in Senftenberg CY - Senftenberg, Germany DA - 14.06.19 KW - Mechanochemie KW - XRD PY - 2019 AN - OPUS4-48393 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Majewski, J. T1 - Ansprechzeiten von Wasserstoff-Sensoren N2 - Die Effizienz von Gassensoren zur sicheren Verwendung von Wasserstoff hängt wesentlich von der Reaktion des Sensors auf eine Änderung der Wasserstoffkonzentration ab. Daher wurde die Ansprechzeit von fünf im Handel erhältlichen Wasserstoffsensoren unterschiedlichen Messprinzips bestimmt. Experimente haben gezeigt, dass alle Sensoren die Anforderungen der Norm ISO 26142 übertreffen; es wurden Ansprechzeiten im Bereich (t90-Zeiten) von 2 s bis 16 s ermittelt. Die Ergebnisse können mit Exponential- oder Sigmoidalfunktionen approximiert werden. Es kann gezeigt werden, dass die Ergebnisse zum transienten Verhalten sowohl von den Betriebsparametern der Sensoren und Prüfverfahren als auch von den experimentellen Bedingungen wie Gaswechselrate sowie Konzentrationssprung abhängen. T2 - 7. HYPOS-Dialog - Innovative Wasserstoffsensorik CY - Halle (Saale), Germany DA - 19.06.2019 KW - Wasserstoffsensor KW - Ansprechzeit KW - t90-Zeit KW - Prüfverfahren PY - 2019 AN - OPUS4-48397 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lemke, Nora T1 - Development of a method for protein quantification via isotope dilution ICP-MS for application on an Alzheimer’s biomarker N2 - Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful method for the matrix-independent quantitative analysis of target elements. Developed for the use in inorganic trace analysis, ICP-MS is nowadays emerging as a valuable tool for bioanalytical questions. Especially the use of ICP-MS for quantitative proteomics by measuring heteroatoms has gained popularity in the last decade, considering that established quantification methods like organic mass spectrometry depend on the existence of matched protein and peptide standards or labelling of the target protein. The need for reliable quantification of proteins is constantly growing, but only a limited number of well characterized and quantified protein standards are available so far. Not only in basic research, but also in a clinical context, accurately quantified, traceable protein standards are needed to ensure comparability of measurements between laboratories. One disease with a major impact on our ageing society is Alzheimer’s disease (AD), which is still challenging to diagnose. As this is also due to a lack in comparability and accuracy of existing biomarker assays, the community would greatly benefit from well quantified protein biomarker standards. In this work, we applied isotope dilution analysis (IDA) using ICP-MS to quantify proteins of known stoichiometry via their sulfur content. Sulfur is present in two amino acids, cysteine and methionine, and hence exists in nearly all proteins. Simple strategies were employed for the detection of low molecular sulfur species to correct for sulfur contaminants and allow for reliable quantification of various proteins. We report the protein mass fractions with expanded uncertainties of a standard reference material and commercially available proteins determined by sulfur IDA. The herein developed method can be applied for the reliable and traceable quantification of pure proteins and will be used for the quantification of an AD biomarker. Our target is the tau protein, as brain load and distribution of tau is highly correlated with the clinical progression of AD. T2 - ReMiND 2019 Biomolecules in Neurodegenerative Diseases CY - Braunschweig, Germany DA - 26.06.2019 KW - ICP-MS KW - Isotope dilution KW - Proteins KW - Quantification PY - 2019 AN - OPUS4-48464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - Size-selective microwave-assisted synthesis of pure zinc oxide nanoparticles for precise band gap engineering N2 - Zinc oxide (ZnO) nanoparticles find manifold applications, most prominently in photovoltaics, where their unique optical properties are exploited. Particularly important are their band gap energy of 3.37 eV, which can be widely tuned through doping, and a large exciton binding energy of 60 mV. As a wide-bandgap II-VI semiconductor, the optical band gap energy and fluorescence energy become size-dependent when moving to particle radii of a few nanometers. To gain a deeper insight into this issue, we report on a microwave-assisted, size-selective synthesis of pure ZnO nanoparticles. By hydrolysis of the metal precursor in presence of a strong base at temperatures exceeding the solvent’s boiling point, the reaction is dramatically accelerated, and narrowly dispersed, spherical particles are yielded within seconds – instead of hours at lower temperatures. The determination of their size distributions in high resolution using small-angle x-ray scattering (SAXS) allows for a precise mapping of the optical properties (UV/Vis absorption and fluorescence) to particle size. We observed that the mean particle radii increase from 2.6 ± 0.1 nm with increasing synthesis temperature from 125 °C to 200 °C. This is accompanied by a red shift of the optical band gap and the fluorescence energies, the latter of which can be seen in Figure 1. Thus, undoped ZnO nanoparticles with narrow size distributions and pre-defined size as well as optical properties can be obtained through a microwave-assisted synthesis. T2 - 6th Nano Today Conference CY - Lisbon, Portugal DA - 16.06.2019 KW - SAXS KW - Zinc oxide nanoparticles KW - Microwave synthesis PY - 2019 AN - OPUS4-48340 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - What’s for eats? – Zinc phosphate nanoparticle mass fractals form during the artificial digestion of zinc chloride N2 - Zinc is an essential trace element and is ingested daily by humans, partly in dissolved form. The first contact is with saliva, in which many ions are dissolved whose solubility product with zinc can be low. This could result in compounds forming, possibly in nanoparticular form, which could have different effects on the organism than pure zinc ions. In this study, we report on the saliva stage of the artificial digestion of zinc chloride as a model substance for zinc ions. To facilitate in situ measurements, the sample is continuously passed through a small-angle x-ray scattering (SAXS) system. This custom-made machine is capable of measuring over a wide q-range and thereby able to resolve structures from around 250 nm down to the crystal structure. It is thus an excellent tool for investigating both the particle size distribution and the atomic structure of the sample. By curve fitting, we found that shortly after addition of zinc chloride to saliva, small particles with a mean radius of 1.9 ± 0.1 nm and a distribution width of 0.6 ± 0.1 nm formed. These particles are aggregated to compact mass fractals with a fractal aggregate size of 14.7 ± 0.1 nm and a fractal dimension of 2.96 ± 0.02. Approximately 7200 single particles form each mass fractal, whose radius of gyration was found to be 36 ± 1 nm. The growth of these structures continues over the course of several weeks. To determine the compound that was formed, infrared spectroscopy was used in addition to the SAXS measurements, and zinc phosphate was identified as the product. T2 - 6th Nano Today Conference CY - Lisbon, Portugal DA - 16.06.2019 KW - SAXS KW - digestion KW - nanoparticles PY - 2019 AN - OPUS4-48342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Screening the environment for emerging pollutants by antibody-based methods N2 - Immunoanalytical methods are excellent tools for analysis of the environment with respect to pollutants T2 - ENEQUI Encontro Nacional dos Estudantes de Química CY - Lisbon, Portugal DA - 22.03.2019 KW - Immunoassay KW - Schadstoffe KW - Antikörper PY - 2019 AN - OPUS4-48321 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg A1 - Puskar, L. A1 - Ritter, E. A1 - Schade, U. T1 - Novel Technique for On-Line Monitoring of the Curing Process of Fiber Reinforced Polymer Composites N2 - A specially developed experimental set up has been integrated into a commercially available FT IR Spectrometer to study the curing of Epoxy Systems. MIR and FIR spectra measured during the curing process at different temperatures of an epoxy system will be presented in dependency of the curing time. The experiments and the selected set up are discussed to demonstrate its potential for future monitoring and ageing control applications during a manufacturing process of polymer composites. T2 - 45. International conference on infrared, millimeter, and terahertz waves CY - Online meeting DA - 08.11.2020 KW - Far-infrared spectroscopy KW - Online Curing Monitoring PY - 2021 SN - 978-1-7281-6620-9 DO - https://doi.org/10.1109/irmmw-thz46771.2020.9370646 SP - 1 PB - IEEE AN - OPUS4-53059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karafiludis, Stephanos T1 - Crystallisation of transition metal phosphate as precursors for mesoporous materials N2 - The influence of several precipitation parameters on the crystal morphology and size of transition metal struvite is poorly investigated. We reveal the effect of different reaction conditions on the crystal shape and crystallite size of M-struvites (NH4MPO4∙6H2O, M = Mg2+, Ni2+, Co2+). Furthermore, we characterize the coordination environment of the crystalline end products and their related phases [Co-dittmarite (COD) NH4CoPO4∙H2O and Co(II)phosphate octahydrate (CPO) Co3(PO4)2∙8H2O]. Mg- and Ni-struvite are stable in multiple concentrations of the educts and metal/phosphorus (M/P) ratios in contrast to Co-struvite which forms below M/P ratios of 0.4. A high M/P ratio with high concentrations of the educts decrease the crystallite size and idiomorphism of the crystals while low M/P ratios with low concentrations of the educts increase the crystallite size and the euhedral formation of the crystal planes. In the (Ni, Co)-solid solutions Ni and Co are homogenously distributed in the crystals with similar Ni# as in the aqueous solutions indicating no elemental fractionation in crystallization. Ni and Co-struvite exhibit a more centrosymmetric coordination environment compared to their related phases of COD and CPO determined by EXAFS. The CoO6 octahedron expands slightly the ideal size of the struvite structure and decomposes to Co-dittmarite. It is suggested that the crystallization of Ni- and Co-struvites follow a non-classical crystallization theory which consists of multiple nanophases on the way to the final crystal. T2 - SALSA Make and Measure... and Machines CY - Online meeting DA - 16.09.2021 KW - Crystal Engineering KW - Nucleation KW - Mesoporosity PY - 2021 AN - OPUS4-53444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karafiludis, Stephanos T1 - Crystallisation and nucleation study of transition metal struvite and related compounds N2 - The recycling of critical elements has crucial importance to maintain sustainable use of raw materials. Phosphorus(P) is a sought-after limited natural resource due to its wide use in modern agriculture mainly as P-fertilizers. But it causes major problems for the environment such as eutrophication of ecosystems. In the future it could be depleted due to the high demand and declining natural phosphorite ore deposits. Therefore, the phosphorus recovery from agricultural waste waters will be an important factor in preservation of the global consumption. The precipitation of M-struvite (NH4MPO4·6H2O, M2+= Mg2+, Ni2+, Co2+, Zn2+, Cu2+ etc.) from agricultural and mine waste waters is a promising P-recovery route. Besides avoidance of eutrophication due to extraction of excess phosphates and the restoration of the phosphorus resources the recovered M-struvites may be potentially be up-cycled for industrial applications e.g. Co and Ni-phosphate show excellent electrochemical properties for batteries or supercapacitors. The precipitation processes of M-struvites are strongly dependent on the degree of supersaturation, pH and on the exchange ions M2+.The impact of transition metals on the crystallization of M-struvite has been investigated only to a limited extent. An optimization of the reaction conditions could lead to more efficient M-struvite precipitation and significantly improved P-recovery method. In addition, these materials form transitional amorphous colloidal nanophases on the way to the crystalline product indicating a non-classical crystallization pathway. By interfering the crystallization process a potential highly reactive amorphous precursor material can be preserved for electrocatalysis. Here, we present hints on the crystallization mechanism and the kinetics of precipitation through analysis of the transitional phases. Furthermore, we reveal the effect of different reaction conditions on the crystal shape and crystallite size of M-struvites (NH4MPO4∙6H2O, M = Mg2+, Ni2+, Co2+). In addition, we could evaluate the stability of crystalline M-struvites and their related phases through characterization of the coordination environment [Co-dittmarite (COD) NH4CoPO4∙H2O and Cobalt(II)phosphate octahydrate (CPO) Co3(PO4)2∙8H2O].Due to the low solubility product and their controlled precipitation through adjusting the reaction conditions (c(educts), pH, multi metal solutions) M-struvite is a promising recovery material as it could extract NH4+, PO43- and heavy metals at the same time out of agricultural and mine waste waters. T2 - IUCr 25th International Union of Crystallography Congress CY - Online meeting DA - 14.08.2021 KW - Crystal Engineering KW - Nucleation KW - Amorphous Phases KW - Crystal mechanism PY - 2021 AN - OPUS4-53445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karafiludis, Stephanos T1 - Crystallisation and nucleation study of transition metal phosphates: M-struvite and related compounds N2 - The recycling of critical elements has crucial importance to maintain sustainable use of raw materials. Phosphorus(P) is a sought-after limited natural resource due to its wide use in modern agriculture mainly as P-fertilizers. But it causes major problems for the environment such as eutrophication of ecosystems. In the future it could be depleted due to the high demand and declining natural phosphorite ore deposits. Therefore, the phosphorus recovery from mine and agricultural waste waters will be an important factor in preservation of the global consumption. The precipitation of M-struvite (NH4MPO4·6H2O, M2+= Mg2+, Ni2+, Co2+) from waste waters is a promising P-recovery route. Besides avoidance of eutrophication due to extraction of excess phosphates and the restoration of the phosphorus resources the recovered M-struvites may be potentially be up-cycled for industrial applications e.g. Co and Ni-phosphate show excellent electrochemical properties for batteries or supercapacitors. The precipitation process of M-struvites is strongly dependent on the degree of supersaturation, pH and on the exchange ions M2+.The influence of these precipitation parameters on the crystal morphology and size of transition metal struvite has been investigated only to a limited extent. An optimization of the reaction conditions could lead to more efficient M-struvite precipitation and significantly improved P-recovery method. We reveal the effect of different reaction conditions on the crystal shape and crystallite size of M-struvites (NH4MPO4∙6H2O, M = Mg2+, Ni2+, Co2+). Furthermore, we characterize the coordination environment of the crystalline end products and their related phases [Co-dittmarite (COD) NH4CoPO4∙H2O and Co(II)phosphate octahydrate (CPO) Co3(PO4)2∙8H2O]. Due to the presence of various amorphous phases pH is changing significantly in the different systems. Mg- and Ni-struvite are stable in multiple concentrations of the educts and metal/phosphorus (M/P) ratios in contrast to Co-struvite which forms below M/P ratios of 0.4. A high M/P ratio with high concentrations of the educts decrease the crystallite size and idiomorphism of the crystals while low M/P ratios with low concentrations of the educts increase the crystallite size and the euhedral formation of the crystal planes. In the (Ni, Co)-solid solutions Ni and Co are homogenously distributed in the crystals with similar Ni# as in the aqueous solutions indicating no elemental fractionation in crystallization. Ni and Co-struvite exhibit a more centrosymmetric coordination environment compared to their related phases of COD and CPO determined by EXAFS. The CoO6 octahedron expands slightly the ideal size of the struvite structure and decomposes to Co-dittmarite. From TEM analysis and pH measurements it is suggested that the crystallization of Ni- and Co-struvite follows a non-classical crystallization theory which consists of multiple nanophases, crystalline or amorphous, on the way to the final crystalline product. T2 - Goldschmidt Conference 2021 CY - Online meeting DA - 04.07.2021 KW - Crystal Engineering KW - Nucleation KW - Amorphous Phases KW - Crystal mechanism PY - 2021 UR - https://2021.goldschmidt.info/goldschmidt/2021/meetingapp.cgi/Paper/5288 AN - OPUS4-53446 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Martin A1 - Tannenberg, Robert A1 - Tscheuschner, Georg A1 - Ponader, Marco A1 - Weller, Michael G. T1 - Cocaine detection by a laser-induced immunofluorometric biosensor N2 - The trafficking of illegal drugs by criminal networks at borders, harbors, or airports is an increasing issue for public health as these routes ensure the main supply of illegal drugs. The prevention of drug smuggling, including the installation of scanners and other analytical devices to detect small traces of drugs within a reasonable time frame, remains a challenge. The presented immunosensor is based on a monolithic affinity column with a large excess of immobilized hapten, which traps fluorescently labeled antibodies as long as the analyte cocaine is absent. In the presence of the drug, some binding sites of the antibody will be blocked, which leads to an immediate breakthrough of the labeled protein, detectable by highly sensitive laser-induced fluorescence with the help of a Peltier-cooled complementary metal-oxide-semiconductor (CMOS) camera. Liquid handling is performed with high-precision syringe pumps and microfluidic chip-based mixing devices and flow cells. The biosensor achieved limits of detection of 7 ppt (23 pM) of cocaine with a response time of 90 s and a total assay time below 3 min. With surface wipe sampling, the biosensor was able to detect 300 pg of cocaine. This immunosensor belongs to the most sensitive and fastest detectors for cocaine and offers near-continuous analyte measurement. KW - Online detection KW - Security KW - Monoclonal antibody KW - Microfluidic mixing KW - Microfluidics KW - Lab-on-a-chip KW - Monolithic column KW - Affinity chromatography KW - Laser-induced fluorescence KW - LIF KW - ELISA KW - Wipe test KW - Low-cost PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534487 DO - https://doi.org/10.3390/bios11090313 VL - 11 IS - 9 SP - 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-53448 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Roesch, Philipp A1 - Fischer, E. A1 - von der Au, Marcus A1 - Pfeifer, Jens A1 - Cossmer, Antje A1 - Wittwer, Philipp A1 - Vogel, Christian A1 - Simon, Franz-Georg A1 - Meermann, Björn T1 - Correction to: Determination of organically bound fluorine sum parameters in river water samples - Comparison of combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) N2 - The article “Determination of organically bound fluorine sum parameters in river water samples - Comparison of combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS)” was originally published Online First without Open Access. After publication in volume 413, issue 1, page 103–115 of the journal “Analytical and bioanalytical chemistry”, the authors decided to opt for Open Choice and to make the article an Open Access publication. Therefore, the copyright of the article has been changed to © The Author(s) 2021 and the article is forthwith distributed under the terms of the Creative Commons Attribution 4.0 International License. PY - 2020 DO - https://doi.org/10.1007/s00216-021-03675-z SN - 1618-2650 SP - 1 PB - Springer CY - Berlin AN - OPUS4-53453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marklein, B. A1 - Jenning, M. A1 - Konthur, Zoltán A1 - Häupl, T. A1 - Welzel, F. A1 - Nonhoff, U. A1 - Krobitsch, S. A1 - Mulder, D. M. A1 - Koenders, M. I. A1 - Joshua, V. A1 - Cope, A. P. A1 - Shlomchik, M. J. A1 - Anders, H.-J. A1 - Burmester, G. R. A1 - Hensvold, A. A1 - Catrina, A. I. A1 - Rönnelid, J. A1 - Steiner, G. A1 - Skriner, K. T1 - The citrullinated/native index of autoantibodies against hnRNP-DL predicts an individual "window of treatment success" in RA patients N2 - Background: There is a need for biomarker to identify patients “at risk” for rheumatoid arthritis (risk-RA) and to better predict the therapeutic response and in this study we tested the hypothesis that novel native and citrullinated heterogeneous nuclear ribonucleoprotein (hnRNP)-DL autoantibodies could be possible biomarkers. Methods: Using protein macroarray and ELISA, epitope recognition against hnRNP-DL was analysed in sera from different developed RA disease and diagnosed SLE patients. Toll-like receptor (TLR) 7/9 and myeloid Differentiation primary response gene 88 (MyD88)-dependency were studied in sera from murine disease models. HnRNP-DL expression in cultivated cells and synovial tissue was analysed by indirect immunofluorescence, immunoblot and immunohistochemistry. KW - Citrullinated KW - Rheumatoid arthritis KW - Protein-modification KW - Autoantibodies KW - Antigens PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533682 DO - https://doi.org/10.1186/s13075-021-02603-x SN - 1478-6362 VL - 23 SP - 1 EP - 16 PB - BioMed Central CY - London AN - OPUS4-53368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Herausforderungen bei der Analytik von Technologie-kritischen Elementen (TCE) in Abfällen N2 - Technologie-kritische Elemente (TCE) sind unentbehrliche Materialien für High-Tech Produkte wie Smartphones, Notebooks und Monitors. Ihr Bedarf wird voraussichtlich aufgrund des gesellschaftlichen Wandels hin zu einer grünen Ökonomie exponentiell ansteigen. Dieser Wandel wird vor allem auch durch erneuerbare Energien und Elektromobilität geprägt (European Green Deal). Diese Entwicklung in Verbindung mit einer nahezu fehlenden TCE Produktion in Europa setzt den Markt unter Druck und führt zu steigenden Preisen. Die Sicherung des TCE Nachschubs wurde in der gegenwärtigen Gesundheitskrise noch dringender und wurde daher auch zu einem der Hauptthemen des COVID-19 Recovery Plan, der eine Stärkung der europäischen Resilienz und Autonomie zum Ziel hat. Ein nachhaltige Lösung ist das Recycling der Abfall- bzw. Wertstoffe und letztendlich eine Circular Economy. Allerdings ist die Analyse von Abfallströmen schwierig und erfordert geeignete analytische Lösungen, die SI-rückführbare und somit vergleichbare Messergebnisse im gesamten Recyclingprozess ermöglichen. Die dafür erforderlichen, für TCE zertifizierte, Referenzmaterialien und nötige standardisierte Verfahren fehlen bisher nahezu vollständig. In diesem Beitrag werden die analytischen Herausforderungen, wie z.B. die extreme Heterogenität der Materialien, Schwierigkeiten beim Probenaufschluss und das Fehlen von Referenzmaterialien diskutiert. Und es wird das EMPIR-Projekt MetroCycleEU vorgestellt, dessen Ziel es ist Referenz- und Routineverfahren für ausgewählte TCE (Co, Ga, Ge, In, Ta, Nd, Pr, Dy, Gd, La, Au, Pt, Pd, Rh) zu entwickeln und Referenzmaterialien für Platinen, LEDs und Li-Batterien bereitzustellen. T2 - Workshop Nachhaltige Prozesse für eine Circular Economy CY - Berlin, Germany DA - 23.09.2021 KW - TCE KW - Circular economy KW - Metrology KW - Traceability KW - Uncertainty PY - 2021 AN - OPUS4-53371 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schnur, C. T1 - Explainable machine learning for damage detection - In carbon fiber composite plates under varying temperature conditions N2 - Understanding on how a machine learning model interprets data is a crucial step to verify its reliability and avoid overfitting. While the focus of the scientific community is nowadays orientated towards deep learning approaches, which are considered as black box approaches, this work presents a toolbox that is based on complementary methods of feature extraction and selection, where the classification decisions of the model are transparent and can be physically interpreted. On the example of guided wave benchmark data from the open guided waves platform, where delamination defects were simulated at multiple positions on a carbon fiber reinforced plastic plate under varying temperature conditions, the authors could identify suitable frequencies for further investigations and experiments. Furthermore, the authors presented a realistic validation scenario which ensures that the machine learning model learns global damage characteristics rather than position specific characteristics. T2 - 48th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Online meeting DA - 28.07.2021 KW - Machine Learning KW - Guided waves KW - Damage Detection KW - Structural Health Monitoring KW - Composite Structures PY - 2021 AN - OPUS4-53377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - VIDEO A1 - Pauw, Brian Richard T1 - The SAXS platform at BAM N2 - Presentation of the Small-Angle X-Ray Scattering intrument at BAM (Berlin - Germany). More information about SAXS is available on Brian Pauw's long-running SAXS blog: https://lookingatnothing.com/ KW - X-ray scattering KW - MOUSE KW - Instrumentation KW - SAXS KW - Laboratory PY - 2021 UR - https://www.youtube.com/watch?v=OjYToZQTsqo PB - YouTube, LLC CY - San Bruno, CA, USA AN - OPUS4-53358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shapovalov, Oleg A1 - Shapovalova, M. A1 - Ossenbrink, R. A1 - Heckel, Thomas A1 - Michailov, V. A1 - Weiss, S. A1 - Gaal, Mate T1 - Verbessern der Korrosionsbeständigkeit eines hochtemperaturbeständigen Ultraschalldämpfungskörpers mittels Laserstrahl-Auftragschweißen N2 - Während in einem konventionellen Ultraschallprüfkopf ein Kunststoffdämpfungskörper mit Kleber oder Öl an einen Piezoschwinger angekoppelt ist, werden als Hochtemperaturlösung feinporöse sintermetallische Dämpfungsmaterialien mit einer Flüssigglasankopplung eingesetzt. Um dabei das Sintermetall vor dem korrosiven Angriff der Glasschmelze zu schützten, wird am Dämpfungskörper gegenwärtig Gold- oder Platinfolie zeit- und kostenaufwendig appliziert. In der aktuellen Arbeit wurde eine Methode zum Korrosionsschutz der sintermetallischen Oberfläche aus rostfreiem Stahl mittels Laser-Pulverauftragschweißen entwickelt. Im Laufe einer Schweißparameterstudie auf dem Substratmaterial aus massivem rostfreiem Stahl wurde die Eignung unterschiedlicher Auftragsmaterialien auf Nickel- und Kobaltbasis untersucht. Dabei wurde zunächst der Einfluss verschiedener Schweißparameter wie Laserleistung, Vorschubgeschwindigkeit und Pulvermenge auf die Auftragsqualität (Nahtform, Vermischungsgrad, Porosität) metallografisch bewertet. Anschließend wurden die aufgetragenen Schichten hinsichtlich ihrer Korrosionsbeständigkeit getestet. Der Kontakt mit einer flüssigen Glasmischung bei 500 °C hat bei keiner der beschichteten Proben sichtbare Korrosionswirkung gezeigt. Als Resultat der Schweißparameterstudie haben sich besonders die nickelbasierten Pulver als gut geeignete Materialien für den Prozess gezeigt. Die identifizierten Schweißparameter wurden im nächsten Schritt erfolgreich an das sintermetallische Substrat angepasst. T2 - DVS Congress CY - Online meeting DA - 14.09.2021 KW - Korrosion KW - Hochtemperaturbeständigkeit KW - Ultraschallwandler PY - 2021 SN - 978-3-96144-146-4 SN - 978-3-96144-147-1 VL - 2021 SP - 370 EP - 377 AN - OPUS4-53362 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Duwe, M. T1 - Thickness Profiling of the Superficial Amorphization and Re-Crystallization of Silicon Induced by Femtosecond Laser Pulses N2 - Crystalline Silicon undergoes a complex phase-change dynamic of melting, amorphization, ablation and re-crystallization upon irradiation with high intensity ultra-short laser pulses [1]. The final state of such a modified surface spot depends on many factors, most notably the local fluence and the surface’s crystal orientation. In this study, we induced superficial structure and phase changes in Silicon <111> and <100> wafers using single femtosecond laser pulses (790 nm, 30 fs) for a range of different peak fluences. The resulting surface modifications were studied in great detail using a number of different techniques, including spectroscopic imaging ellipsometry (SIE), atomic force microscopy, high-resolution transmission electron microscopy (HRTEM), and energy dispersive X-ray spectroscopy within scanning transmission electron microscopy (STEM-EDX). Playing a pivotal role in this work, SIE provided non-destructive measurements for the calculation of the radial amorphous layer-thickness profiles of the irradiated spots using a two-layer thin-film model (Silicon dioxide and amorphous Silicon on a crystalline Silicon substrate). The measurements further allowed for the analysis of the oxide-layer modifications induced by the laser treatment. The results of the SIE-calculations were cross-checked by an in-depth material lamella via HRTEM and STEM-EDX. T2 - 11th Workshop Ellipsometry (WSE 11) CY - Steyr, Austria DA - 06.09.2021 KW - Femtosecond Laser KW - Spectroscopic imaging ellipsometry KW - Amorphization KW - Ablation KW - Re-crystallization PY - 2021 AN - OPUS4-53363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Cheng-Chieh A1 - Völker, Daniel A1 - Weisbrich, S. A1 - Neitzel, F. ED - Holl, H. T1 - The Finite Volume Method in point of view of Finite Element Method N2 - The best-known discretization methods for solving engineering problems formulated as partial differential equations are finite difference method (FDM), finite element method (FEM) and finite volume method (FVM). While the finite volume method is used in fluid mechanics, the finite element method is predominant in solid state mechanics. At first glance, FVM and FEM are two highly specialized methods. However, both methods can solve problems of both solid mechanics and fluid mechanics well. Since experimental mechanics deals not only with solid state physics but also with fluid mechanics problems, we want to understand FVM in the sense of FEM in this work. In the long term, we want to use the variational calculus to unify many important numerical methods in engineering science into a common framework. In this way, we expect that experiences can be better exchanged between different engineering sciences and thus innovations in the field of experimental mechanics can be advanced. But in this work, we limit ourselves to the understanding of the FVM with the help of the variational calculus already known in FEM. We use a simple 1D Poisson equation to clarify the point. First, we briefly summarize the FVM and FEM. Then we will deal with the actual topic of this paper, as we establish the FEM and the FVM on a common basis by variation formulation. It is shown here that the FVM can be understood in terms of the finite element method with the so-called Galerkin-Petrov approach. T2 - 37th Danubia Adria Symposium on Advances in Experimental Mechanics CY - Linz, Österreich DA - 21.09.2021 KW - Finite element method KW - Finite volume method KW - Variational calculation KW - Simulation KW - Computational physics PY - 2021 SN - 978-3-9504997-0-4 SP - 12 EP - 13 AN - OPUS4-53422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Cheng-Chieh T1 - The Finite Volume Method in point of view of Finite Element Method N2 - The best-known discretization methods for solving engineering problems formulated as partial differential equations are finite difference method (FDM), finite element method (FEM) and finite volume method (FVM). While the finite volume method is used in fluid mechanics, the finite element method is predominant in solid state mechanics. At first glance, FVM and FEM are two highly specialized methods. However, both methods can solve problems of both solid mechanics and fluid mechanics well. Since experimental mechanics deals not only with solid state physics but also with fluid mechanics problems, we want to understand FVM in the sense of FEM in this work. In the long term, we want to use the variational calculus to unify many important numerical methods in engineering science into a common framework. In this way, we expect that experiences can be better exchanged between different engineering sciences and thus innovations in the field of experimental mechanics can be advanced. But in this work, we limit ourselves to the understanding of the FVM with the help of the variational calculus already known in FEM. We use a simple 1D Poisson equation to clarify the point. First, we briefly summarize the FVM and FEM. Then we will deal with the actual topic of this paper, as we establish the FEM and the FVM on a common basis by variation formulation. It is shown here that the FVM can be understood in terms of the finite element method with the so-called Galerkin-Petrov approach. T2 - 37th Danubia Adria Symposium on Advances in Experimental Mechanics CY - Linz, Austria DA - 21.09.2021 KW - Finite volume method KW - Finite element method KW - Variational calculation KW - Simulation KW - Computational physics PY - 2021 AN - OPUS4-53424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska T1 - Acoustic emission of fibre reinforced AlSi12CuMgNi alloy under compression N2 - Typically, the near-eutectic Al-Si alloys consist of highly interconnected three-dimensional network of the eutectic Silicon (Si) and intermetallics embedded into Aluminium (Al) matrix. For further improvement of the mechanical properties of such alloys, often, one single ceramic reinforcement phase, e.g. silicon carbide (SiC) or aluminium oxide (Al2O3) in the form of fibres or particles is added. However, hybrid reinforcements (fibres and particles) can further improve wear resistance and fracture toughness, and additionally, reduce anisotropy of the material. The engineering of metal matrix composites (MMC) for specific application requirements benefits from a comprehensive knowledge of the failure behaviour. Therefore, damage evolution under compression was investigated on: - pure near-eutectic AlSi12CuMgNi matrix alloy - type I: matrix reinforced with random-planar oriented Al2O3 short fibres (15 vol.%) - type II: matrix reinforced with random-planar oriented Al2O3 short fibres (7 vol.%) and additional SiC particles (15 vol.%) The analysis of damage mechanism was carried out in two rather independent but complementary studies. First, selected sister samples of every material were exposed to quasi-static compression (traverse control). The compression tests were interrupted at different strain levels. Miniature cylinders with a diameter of 1mm were extracted from the pre-strained samples and investigated by synchrotron computed tomography (SX-µCT) with a spatial resolution of about 0.7 µm. For the pure matrix alloy, microcracks are confined to the intermetallic particles and to the eutectic Si, hence no damage was observed in the Aluminium. The composite type II revealed a more effective strain accumulation (less damage) than type I at low plastic strain (up to 5 %), but a more catastrophic damage development due to cracking of the SiC clusters at higher strain levels. The second approach to study the damage initiation and accumulation in the materials subjected to compressive load was Acoustic Emission (AE) analysis. In this case the in-situ monitoring of the acoustic emission signal was performed during compression tests on specimens with dimension of several mm. For all three material types, AE activity set at 2% strain. Differences in AE behaviour of the three materials was proven based on AE hitrate, signal peak amplitudes as well as weighted peak frequencies (WPF). Future work focuses on combination of AE and SX-µCT aiming for more detailed knowledge on damage mechanism of metal matrix composites. T2 - Schall21 CY - Online meeting DA - 24.02.2021 KW - AlSi12CuMgNi KW - Al-Si alloys KW - Acoustic emission KW - Tension PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534268 UR - https://www.dgzfp.de/seminar/schall21 AN - OPUS4-53426 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - Von Elementspezies, Isotope und Zellen oder: wie kommt man eigentlich von Westfalen nach Berlin N2 - Im Rahmen des Vortrages werden die Möglichkeiten der Elementanalytik an Applikationsbeispielen aus Umwelt und life-sciences aufgezeigt. Hierbei kommen ICP-MS Kopplungstechniken, stabile Isotope und Einzellen- und Partikelanalytik (sc-/sp-ICP-ToF-MS) zum Einsatz. T2 - DAAS PhD Seminar CY - Online meeting DA - 20.09.2021 KW - Elementspezies & Isotope KW - ICP-MS & HR-CS-GFMAS KW - Kopplungstechniken PY - 2021 AN - OPUS4-53378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - On-line hyphenation of CE with multicollector-icp-ms for species-specific isotopic analysis of sulfur N2 - In many scientific fields, isotopic analysis can offer valuable information, e.g., for tracing the origin of food products, environmental contaminants, forensic and archaeological samples (provenance determination), for age determination of minerals (geochronological dating) or for elucidating chemical processes. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement. In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species using a multiple-injection approach for instrumental mass bias correction by standard-sample bracketing. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared to data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was promising regarding the differentiation of the river systems by the isotopic signature of river water sulfate. The great potential of this method is based on the versatility of the applied separation technique, not only in the environmental field but also for, e.g., biomolecules, as sulfur is the only covalently bound constituent of proteins that can be analyzed by MC-ICP-MS. T2 - 12th International Conference on Instrumental Methods of Analysis-Modern Trends and Applications (IMA) CY - Online meeting DA - 20.09.2021 KW - CE/MC-ICP-MS KW - Species-specific Isotope Analysis KW - Environmental & life science application KW - Speciation Analysis PY - 2021 AN - OPUS4-53379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haeckel, A. A1 - Ascher, Lena A1 - Beindorff, N. A1 - Prasad, S. A1 - Garczynska, K. A1 - Guo, J. A1 - Schellenberger, E. T1 - Long‑circulating XTEN864‑annexin A5 fusion protein for phosphatidylserine‑related therapeutic applications N2 - Annexin A5 (anxA5) is a marker for apoptosis, but has also therapeutic potential in cardiovascular diseases, cancer, and, due to apoptotic mimicry, against dangerous viruses, which is limited by the short blood circulation. An 864-amino-acid XTEN polypeptide was fused to anxA5. XTEN864-anxA5 was expressed in Escherichia coli and purified using XTEN as tag. XTEN864-anxA5 was coupled with DTPA and indium-111. After intravenous or subcutaneous injection of 111In-XTEN864-anxA5, mouse blood samples were collected for blood half-life determination and organ samples for biodistribution using a gamma counter. XTEN864-anxA5 was labeled with 6S-IDCC to confirm binding to apoptotic cells using flow cytometry. To demonstrate targeting of atherosclerotic plaques, XTEN864-anxA5 was labeled with MeCAT(Ho) and administered intravenously to atherosclerotic ApoE−/−mice. MeCAT(Ho)-XTEN864-anxA5 was detected together with MeCAT(Tm)-MAC-2 macrophage antibodies by imaging mass cytometry (CyTOF) of aortic root sections. The ability of anxA5 to bind apoptotic cells was not affected by XTEN864. The blood half-life of XTEN864-anxA5 was 13 h in mice after IV injection, markedly longer than the 7-min half-life of anxA5. 96 h after injection, highest amounts of XTEN864-anxA5 were found in liver, spleen, and kidney. XTEN864-anxA5 was found to target the adventitia adjacent to atherosclerotic plaques. XTEN864-anxA5 is a long-circulating fusion protein that can be efficiently produced in E. coli and potentially circulates in humans for several days, making it a promising therapeutic drug. KW - Programmed cell death KW - LA/ICP-MS Imaging KW - Medicinal application PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533811 DO - https://doi.org/10.1007/s10495-021-01686-w VL - 26 IS - 9-10 SP - 534 EP - 547 PB - Springer AN - OPUS4-53381 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fink, Friedrich A1 - Emmerling, Franziska A1 - Falkenhagen, Jana T1 - Identification and Classification of Technical Lignins by means of Principle Component Analysis and k-Nearest Neighbor Algorithm N2 - The characterization of technical lignins is a key step for the efficient use and processing of this material into valuable chemicals and for quality control. In this study 31 lignin samples were prepared from different biomass sources (hardwood, softwood, straw, grass) and different pulping processes (sulfite, Kraft, organosolv). Each lignin was analysed by attenuated total reflectance Fourier transform infrared (ATR-FT-IR) spectroscopy. Statistical analysis of the ATR-FT-IR spectra by means of principal component analysis (PCA) showed significant differences between the lignins. Hence, the samples can be separated by PCA according to the original biomass. The differences observed in the ATR-FT-IR spectra result primarily from the relative ratios of the p-hydroxyphenyl, guaiacyl and syringyl units. Only limited influence of the pulping process is reflected by the spectral data. The spectra do not differ between samples processed by Kraft or organosolv processes. Lignosulfonates are clearly distinguishable by ATR-FT-IR from the other samples. For the classification a model was created using the k-nearest neighbor (k NN) algorithm. Different data pretreatment steps were compared for k=1…20. For validation purposes, a 5-fold cross-validation was chosen and the different quality criteria Accuracy (Acc), Error Rate (Err), Sensitivity (TPR) and specificity (TNR) were introduced. The optimized model for k=4 gives values for Acc = 98.9 %, Err = 1.1 %, TPR = 99.2 % and TNR = 99.6 %. KW - Classification KW - PCA KW - K-nearest neighbor KW - FT-IR KW - Technical lignin PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533855 DO - https://doi.org/10.1002/cmtd.202100028 VL - 1 IS - 8 SP - 350 EP - 396 PB - Wiley-VCH GmbH AN - OPUS4-53385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska T1 - Der Verformungswiderstand im Holz und die Rolle der Holzstrahlen N2 - Von den Zellulosefibrillen über die Zellwand und die Anordnung der Früh- und Spätholzzellen in einem Jahrring bis hin zum Balken von Natur aus ist Holz ein optimierter Hochleistungswerkstoff, der Handwerker, Architekten, Ingenieure und Wissenschaftler fasziniert und begeistert. Im digitalen Zeitalter werden neben Standard-Laborexperimenten zunehmend Modelle und Simulationen eingesetzt, um das Verhalten des Materials unter verschiedenen Belastungen besser zu verstehen und vorherzusagen. Dazu werden Zahlenwerte von Verformungen im subzellulären Maßstab benötigt, die nun in Experimenten an der TOMCAT-Beamline (TOmographic Microscopy and Coherent rAdiology ExperimenTs) der SLS (Swiss Light Source) gewonnen werden konnten: Holzproben aus Fichte ( Picea abies Karst.) mit einem Prüfquerschnitt von mindestens 1 mm² auf Zug oder Druck beansprucht. Die strukturellen Veränderungen auf Zellebene wurden mittels Computertomographie erfasst. Für die nachträgliche Analyse der 3D-Mikrostruktur von Holz wurde ein Ansatz entwickelt, der es ermöglicht, einzelne Zellen, die in mehreren Tomogrammen unterschiedlicher Belastungszustände erfasst wurden, zu verfolgen. Dabei wurden die Zellgeometrien und das subzelluläre Deformationsverhalten quantifiziert. Unter Zugbelastung beispielsweise verengt sich die Zellwanddicke um ca. 0,8%, das sind bei der gemessenen mittleren Zellwanddicke von 3,5 µm ca. 28 nm. Diese und andere Erkenntnisse liefern nun einen direkten numerischen Zusammenhang zwischen Verformungen der Holzmikrostruktur und dem daraus resultierenden makroskopischen Verhalten. T2 - 5. Holzanatomisches Kolloquium CY - Dresden, Germany DA - 09.09.2021 KW - Holz KW - Wood materials KW - Individual cell tracking KW - Mikro CT PY - 2021 AN - OPUS4-53403 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - HR-CS-GFMAS for PFAS sum parameter analysis in surface water and soil samples N2 - Vorstellung neuer HR-CS-GFMAS basierter Analysemethoden zur Analytik von PFAS in Oberflächenwasser und Boden. T2 - 2. Online-Workshop "Emissionsmessverfahren für per- und polyfluorierte Chemikalien (PFC)" CY - Online meeting DA - 30.09.2021 KW - HR-CS-GFMAS KW - PFAS KW - Oberflächenwasser und Boden PY - 2021 AN - OPUS4-53465 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska A1 - Sanabria, S. T1 - Der Verformungswiderstand im Holz und die Rolle der Holzstrahlen N2 - Von den Zellulosefibrillen über die Zellwand und die Anordnung der Früh- und Spätholzzellen in einem Jahrring bis hin zum Balken von Natur aus ist Holz ein optimierter Hochleistungswerkstoff, der Handwerker, Architekten, Ingenieure und Wissenschaftler fasziniert und begeistert. Im digitalen Zeitalter werden neben Standard-Laborexperimenten zunehmend Modelle und Simulationen eingesetzt, um das Verhalten des Materials unter verschiedenen Belastungen besser zu verstehen und vorherzusagen. Dazu werden Zahlenwerte von Verformungen im subzellulären Maßstab benötigt, die nun in Experimenten an der TOMCAT-Beamline (TOmographic Microscopy and Coherent rAdiology ExperimenTs) der SLS (Swiss Light Source) gewonnen werden konnten: Holzproben aus Fichte ( Picea abies Karst.) mit einem Prüfquerschnitt von mindestens 1 mm² auf Zug oder Druck beansprucht. Die strukturellen Veränderungen auf Zellebene wurden mittels Computertomographie erfasst. Für die nachträgliche Analyse der 3D-Mikrostruktur von Holz wurde ein Ansatz entwickelt, der es ermöglicht, einzelne Zellen, die in mehreren Tomogrammen unterschiedlicher Belastungszustände erfasst wurden, zu verfolgen. Dabei wurden die Zellgeometrien und das subzelluläre Deformationsverhalten quantifiziert. Unter Zugbelastung beispielsweise verengt sich die Zellwanddicke um ca. 0,8%, das sind bei der gemessenen mittleren Zellwanddicke von 3,5 µm ca. 28 nm. Diese und andere Erkenntnisse liefern nun einen direkten numerischen Zusammenhang zwischen Verformungen der Holzmikrostruktur und dem daraus resultierenden makroskopischen Verhalten. T2 - 5. Holzanatomisches Kolloquium CY - Dresden, Germany DA - 09.09.2021 KW - Wood materials KW - Holz KW - Individual cell tracking KW - Mikro CT PY - 2021 SP - 92 EP - 101 CY - Dresden AN - OPUS4-53405 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hirschberger, Paul A1 - Bartholmai, Matthias ED - Holl, H. T1 - Aerial Chemical-Trail Detection and Localization N2 - This paper presents first advances in the area of aerial chemical trail following. For that purpose, we equipped a palm-size aerial robot, based on the Crazyflie 2.0 quadrocopter, with a small lightweight metal oxide gas sensor for measuring evaporated ethanol from chemical trails. To detect and localize the chemical trail, a novel detection criterion was developed that uses only relative changes in the transient phase of the sensor response, making it more robust in its application. We tested our setup in first crossing-trail experiments showing that our flying ant robot is able to correlate an odor hit with the chemical trail within 0.14 m. Principally, this could enable aerial chemical trail following in the future. T2 - 37th Danubia - Adria Symposium on Advances in Experimental Mechanics CY - Linz, Austria DA - 21.09.2021 KW - Nano aerial robot KW - Trail following KW - Trail detection KW - Localization PY - 2021 SN - 978-3-9504997-0-4 VL - 2021 SP - 39 EP - 40 AN - OPUS4-53409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Aerial Robot Olfaction @BAM N2 - This presentation gives an introduction to the gas-sensitive aerial robots developed at BAM. T2 - Workshop - behördlicher Erfahrungsaustausch im Bereich Drohne (BAM/THW) CY - Berlin, Germany DA - 13.09.2021 KW - Mobile Robot Olfaction KW - Tomographic reconstruction of gas plumes KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - UAV PY - 2021 AN - OPUS4-53413 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hilger, A. A1 - Kardjilov, N. A1 - Lange, A. A1 - Kupsch, Andreas A1 - Hentschel, M. P. A1 - Manke, I. T1 - Neutron darkfield imaging of fiber composites N2 - While X-ray based darkfield imaging with grating interferometers is already widely used, darkfield imaging with neutrons has still a relatively small user community focused mostly on magnetic materials. Here, we demonstrate the application of neutron darkfield imaging byTalbot-Lau type grating interferometry to fiber reinforced plastics. Common carbon and glass fiber composites have been investigated including characteristic damage structures. The darkfield images show a strong signal response caused by fiber delamination, suitable fiber direction, particles, pores and cracks. The basic principles of neutron darkfield imaging applied to fiber composites are highlighted. KW - Neutron radiography KW - Darkfield imaging KW - Talbot-Lau interferometer KW - Fiber composites KW - Non-destructive testing PY - 2021 DO - https://doi.org/10.1515/mt-2020-0103 SN - 2195-8572 SN - 0025-5300 VL - 63 IS - 7 SP - 623 EP - 629 PB - De Gruyter CY - Berlin AN - OPUS4-53077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meermann, Björn T1 - The future of elemental analytical chemistry – the sixth special issue dedicated to young analytical scientists N2 - Editorial for a special issue KW - Editorial KW - Special issue, young analytical scientists KW - Elemental analysis PY - 2021 DO - https://doi.org/10.1039/d1ja90038b VL - 36 IS - 9 SP - 1794 EP - 1796 PB - RSC AN - OPUS4-53086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mirabella, Francesca A1 - Müllner, M. A1 - Touzalin, T. A1 - Riva, M. A1 - Jakub, Z. A1 - Kraushofer, F. A1 - Schmid, M. A1 - Koper, M. T. M. A1 - Parkinson, G. S. A1 - Diebold, U. T1 - Ni-modified Fe3O4(001) surface as a simple model system for understanding the oxygen evolution reaction N2 - Electrochemical water splitting is an environmentally friendly technology to store renewable energy in the form of chemical fuels. Among the earth-abundant first-row transition metal-based catalysts, mixed Ni-Fe oxides have shown promising performance for effective and low-cost catalysis of the oxygen evolution reaction (OER) in alkaline media, but the synergistic roles of Fe and Ni cations in the OER mechanism remain unclear. In this work, we report how addition of Ni changes the reactivity of a model iron oxide catalyst, based on Ni deposited on and incorporated in a magnetite Fe3O4(001) single crystal, using a combination of surface science techniques in ultra-high vacuum such as low energy electron diffraction (LEED), x-ray photoelectron spectroscopy (XPS), low-energy ion scattering (LEIS), and scanning tunneling microscopy (STM), as well as atomic force microscopy (AFM) in air, and electrochemical Methods such as cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) in alkaline media. A significant improvement in the OER activity is observed when the top surface presents an iron fraction among the cations in the range of 20-40%, which is in good agreement with what has been observed for powder catalysts. Furthermore, a decrease in the OER overpotential is observed following surface aging in electrolyte for three days. At higher Ni load, AFM shows the growth of a new phase attributed to an (oxy)-hydroxide phase which, according to CV measurements, does not seem to correlate with the surface activity towards OER. EIS suggests that the OER precursor species observed on the clean and Ni-modified surfaces are similar and Fe-centered, but form at lower overpotentials when the surface Fe:Ni ratio is optimized. We propose that the well-defined Fe3O4(001) surface can serve as a model System for understanding the OER mechanism and establishing the structure-reactivity relation on mixed Fe-Ni oxides. KW - OER KW - Fe-Ni oxides KW - Surface science KW - Electrochemistry KW - Water splitting PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529231 UR - https://www.sciencedirect.com/science/article/pii/S0013468621009282?via%3Dihub DO - https://doi.org/10.1016/j.electacta.2021.138638 VL - 389 SP - 138638 PB - Elsevier Ltd. AN - OPUS4-52923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dymkin, G. Y. A1 - Konshina, V. N. A1 - Jaenisch, Gerd-Rüdiger T1 - Оперативная характеристика обнаружения как метод оценки достоверности неразрушающего контроля T1 - Requirements for Accreditation Appraisal of NDT Laboratories in Nuclear Power Industry N2 - The operational characteristics of detection have been successfully applied for many years in assessing the reliability of non-destructive testing. The main problems for their use, as in the application of any of the methods for assessing the reliability, are the lack of information about the actual defect situation and the limited number of defects in the samples of the objects of control. An additional problem of constructing an operational characteristic of detection is the lack of information about the size of defects and the lack of a universal size for various types of defects. The article summarizes the experience of constructing operational characteristics based on the results of ultrasonic testing. N2 - Оперативные характеристики обнаружения в течение многих лет успешно применяют-ся при оценке достоверности неразрушающего контроля. Основными проблемами для их использования, как и при применении любого из методов оценки достоверности, яв-ляются отсутствие информации о действительной дефектной ситуации и ограниченное количество дефектов в образцах объектов контроля. Дополнительной проблемой постро-ения оперативной характеристики обнаружения является отсутствие информации о раз-мерах дефектов и отсутствие универсального размера для различных типов дефектов. В статье обобщён опыт построения оперативных характеристик по результатам ультра-звукового контроля. KW - Non-destructive testing KW - Reliability KW - Probability of detection KW - Operational characteristics KW - Comparative operational characteristics PY - 2021 DO - https://doi.org/https://doi.org/10.12737/1609-3178-2021-23-26 VL - 24 IS - 2 SP - 23 EP - 26 AN - OPUS4-53121 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Steglich, P. A1 - Rabus, D. G. A1 - Sada, C. A1 - Paul, Martin A1 - Weller, Michael G. A1 - Mai, C. A1 - Mai, A. T1 - Silicon Photonic Micro-Ring Resonators for Chemical and Biological Sensing: A Tutorial N2 - Silicon photonic micro-ring resonators (MRR) developed on the silicon-on-insulator (SOI) platform, owing to their high sensitivity and small footprint, show great potential for many chemical and biological sensing applications such as label-free detection in environmental monitoring, biomedical engineering, and food analysis. In this tutorial, we provide the theoretical background and give design guidelines for SOI-based MRR as well as examples of surface functionalization procedures for label-free detection of molecules. After introducing the advantages and perspectives of MRR, fundamentals of MRR are described in detail, followed by an introduction to the fabrication methods, which are based on a complementary metal-oxide semiconductor (CMOS) technology. Optimization of MRR for chemical and biological sensing is provided, with special emphasis on the optimization of waveguide geometry. At this point, the difference between chemical bulk sensing and label-free surface sensing is explained, and definitions like waveguide sensitivity, ring sensitivity, overall sensitivity as well as the limit of detection (LoD) of MRR are introduced. Further, we show and explain chemical bulk sensing of sodium chloride (NaCl) in water and provide a recipe for label-free surface sensing. KW - Lab on a chip KW - Biosensor KW - Cmos KW - Silanization KW - Surface derivatization KW - Evanescent wave PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529360 DO - https://doi.org/10.36227/techrxiv.14909901.v1 SP - 1 EP - 18 PB - IEEE CY - Piscataway Township AN - OPUS4-52936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Baier, Jennifa A1 - Fischer, Daniel A1 - Griepentrog, Michael A1 - Hertwig, Andreas A1 - Hielscher-Hofinger, Stefan A1 - Stockmann, Jörg Manfred A1 - Weise, Matthias T1 - Mapping und Imaging modifizierter Oberflächen: Generische Kenngrößen, Fehlstellen, Reinigungszustand und Haftfestigkeit N2 - Der Vortrag widmet sich dem Mapping und Imaging modifizierter Oberflächen: generische Kenngrößen, Fehlstellen, Reinigungszustand und Haftfestigkeit. Es werden Untersuchungsmethoden zu ihrer Prüfung dargestellt. T2 - 37. ak-adp 2021 CY - Jena, Germany DA - 16.06.2021 KW - Qualitätssicherung KW - Mapping modifizierter Oberflächen KW - Imaging modifizierter Oberflächen KW - Generische Kenngrößen KW - Haftfestigkeit KW - Klebfestigkeit PY - 2021 SP - 1 EP - 10 AN - OPUS4-52893 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tang, Chi-Long T1 - Chemical characterization of ultrafine particles released from 3D printers N2 - Previous studies have shown that desktop 3D printers (Fused Filament Fabrication) emit high numbers of particulate matter, mainly as ultrafine particles (UFP, particle diameter less than 100 nm). However, the chemical composition of emitted particles has been less extensively investigated. In this study, we therefore focused on the chemical composition of particles emitted from 3D printing. The measurements were conducted in a 1 m³ emission test chamber. Emitted particles were sampled by a 13-stage low-pressure cascade impactor onto aluminum foils and then analyzed by TD-GC/MS to identify their organic compounds. Nine commercial filaments made from basic polymers such as Acrylonitrile Butadiene Styrene (ABS), Acrylonitrile Styrene Acrylate (ASA), Polycarbonate (PC), Poly(methyl methacrylate) (PMMA), Nylon, High Performance Polystyrene (HIPS) and a copper-filled Polylactide (PLA) were investigated. The results show that the organic components of the particles are primarily plastic additives such as plasticizer, antioxidant agents, lubricants, UV-absorbers and UV-stabilizers from the filaments. T2 - Healthy Buildings Europe 2021 CY - Online meeting DA - 21.06.2021 KW - UFP KW - FFF-3D-Printer KW - Chemical characterization PY - 2021 AN - OPUS4-52895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jurgelucks, B. T1 - Defect Characterization in Carbon Fiber Reinforced Polymer via Derivative-based Optimization N2 - In recent years carbon über polymers have become a popular light-weight substitute for high-weight materials such as steel. One advantage of carbon fiber polymers is the high strength-to-weight ratio, thus some popular application areas are weight sensitive such as aeronautics or automobiles. As these application areas are especially sensitive to material failure it is of significant interest to characterize material defects which may arise. In this talk we will propose a method to characterize material defects in carbon fiber reinforced polymers using gradient-based optimization methods. The procedure is based on the solution of an inverse problem where simulation data and experimental data is fitted. Here, gradients of the simulation will be supplied by an Algorithmic Differentiation (AD) tool which greatly enhances the quality of the solution. Numerical examples will be provided. T2 - GAMM 2020@21 CY - Online meeting DA - 15.03.2021 KW - Inverse Method KW - Scaled Boundary Finite Element Method KW - Algorithmic Differentiation PY - 2021 AN - OPUS4-52896 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - From on line sensor validation to in-situ monitoring of layer growth: coatings around fibre bragg gratings N2 - The lack of on-line validation procedures for structure-embedded fiber-optical strain sensors, in particular fiber-Bragg-gratings (FBG), resulted in limited applications in structural health monitoring (SHM). Degradation under service conditions and ageing as a result of climatic influences or delamination under load were unsolved Validation issues. This could be overcome by means of an auto-diagnosis procedure based on FBG-sensors coated by electrochemical deposition (ECD) with a magnetostrictive NiFe-coating on top of an adhesive Cu/Cr adhesive layer deposited by physical vapour deposition (PVD) around the FBG strain sensor. This allows at any time under Service a validation of sensor functionality, stability, and reliability. For this purpose, a magnetic strain-proportional reference field is introduced. The optical read-out is realized by the measurement of the Bragg-wavelength shift. The ratio of resulting strain and exciting magnetic reference field should be constant given that the sensor is in proper function. In principle, the magnetostrictive coating around the FBG should also work as on-line magnetic field sensor and other applications in material science. One of these applications is the in-situ monitoring of ECD processes as the deposition of the ECD NiFe-layer on the FBG revealed. Challenges are the monitoring of temperature, deposition stages/thickness, and resulting mechanical stress under given plating conditions. Monitoring problems can be solved by applying a pre-coated FBG to the electrolytic process as the shift of the Bragg wavelength is affected by both the temperature of the electrolyte near the substrate and the stress formation in the growing layer. The experimental FBG set-up and the quantitative determination of temperature- and stress-related strain are described for a nickeliron electrolyte. The in-situ measurement of Bragg wavelength shifts of a pre-coated FBG during electrochemical deposition allows a detailed analysis of stress states due to changes in the growth morphology of the layer. The separation of mechanical and thermal contributions to this shift provides information on the individual Deposition processes in terms of a process fingerprint. T2 - ICMCTF 2021 San Diego/on-line CY - Online meeting DA - 28.04.2021 KW - Fiber- Bragg-gratings (FBG) KW - Physical vapour deposition (PVD) KW - Electrochemical deposition (ECD) KW - Magnetostrictive coating KW - ECD NiFe-layer PY - 2021 AN - OPUS4-52898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Nanoparticle size, shape, and concentration measurement at once – two VAMAS pre-standardization projects ready to start N2 - A case study on the TEM analysis of the size and shape distribution of TiO2 bipyramidal nanoparticles prepared on TEM grids was included in the recently published ISO standard ISO 21363. It was agreed to organize at a later stage a second inter-lab comparison with the nanoparticles distributed to the participants as a liquid suspension. Protocols for uniform nanoparticle deposition on suited supports developed and optimized within the EMPIR nPSize project are also prepared to be distributed. For this, we have chosen the VAMAS platform (www.vamas.org) which offers an excellent international infrastructure of laboratories with high competence in nanoparticle measurement. The VAMAS technical working area dedicated to nanoparticle measurement is TWA 34 ‘Nanoparticle populations’. For this type of nanoparticles, the size and shape distributions are the primary parameters to be reported. Due to the good deposition protocols developed, an automated image analysis is enabled (in contrast to the manual analysis of irregular TiO2 nanoparticles. In parallel with the TiO2 nanoparticle exercise, two spherical SiO2 nanoparticle samples with bi-modal size distributions (nominal relative number concentrations of 1:1 and 10:1) are prepared for a second VAMAS inter-lab comparison. Here, the nanoparticle concentration is the primary parameter to be measured. For the imaging methods it is targeted to measure the relative nanoparticle concentrations of the two modes. For the absolute nanoparticle concentration to be measured by imaging methods it is necessary to control the volume of the liquid suspension deposited on the substrate and to obtain such a homogeneous nanoparticle deposition on the substrate which allows to count (or extrapolate) all the deposited particles. T2 - Microscopy and Microanalysis 2021 CY - Online meeting DA - 01.08.2021 KW - Nanoparticles KW - Electron microscopy KW - VAMAS KW - Inter-laboratory comparison KW - TiO2 KW - SiO2 PY - 2021 AN - OPUS4-53065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lutz, C. A1 - Breuckmann, M. A1 - Hampel, S. A1 - Kreyenschmidt, M. A1 - Ke, X. A1 - Beuermann, S. A1 - Schafner, K. A1 - Turek, T. A1 - Kunz, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Fittschen, U. E. A. T1 - Characterization of Dimeric Vanadium Uptake and Species in Nafion™ and Novel Membranes from Vanadium Redox Flow Batteries Electrolytes N2 - A core component of energy storage systems like vanadium redox flow batteries (VRFB) is the polymer electrolyte membrane (PEM). In this work, the frequently used perfluorosulfonic-acid (PFSA) membrane Nafion™ 117 and a novel poly (vinylidene difluoride) (PVDF)-based Membrane are investigated. A well-known problem in VRFBs is the vanadium permeation through the membrane. The consequence of this so-called vanadium crossover is a severe loss of capacity. For a better understanding of vanadium transport in membranes, the uptake of vanadium ions from electrolytes containing Vdimer(IV–V) and for comparison also V(II), V(III), V(IV), and V(V) by both membranes was studied. UV/VIS spectroscopy, X-ray absorption near edge structure spectroscopy (XANES), total reflection X-ray fluorescence spectroscopy (TXRF), inductively coupled plasma optical emission spectrometry (ICP-OES), and micro X-ray fluorescence spectroscopy (microXRF) were used to determine the vanadium concentrations and the species inside the membrane. The results strongly support that Vdimer(IV–V), a dimer formed from V(IV) and V(V), enters the nanoscopic water-body of Nafion™ 117 as such. This is interesting, because as of now, only the individual ions V(IV) and V(V) were considered to be transported through the membrane. Additionally, it was found that the Vdimer(IV–V) dimer partly dissociates to the individual ions in the novel PVDF-based membrane. The Vdimer(IV–V) dimer concentration in Nafion™ was determined and compared to those of the other species. After three days of equilibration time, the concentration of the dimer is the lowest compared to the monomeric vanadium species. The concentration of vanadium in terms of the relative uptake λ = n(V)/n(SO3 ) are as follows: V(II) [λ = 0.155] > V(III) [λ = 0.137] > V(IV) [λ = 0.124] > V(V) [λ = 0.053] > Vdimer(IV–V) [λ = 0.039]. The results show that the Vdimer(IV–V) dimer Needs to be considered in addition to the other monomeric species to properly describe the transport of vanadium through Nafion™ in VRFBs. KW - MicroXRF KW - VRFB KW - PVDF-based membrane KW - UV/VIS KW - XANES KW - TXRF KW - ICP-OES PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530676 DO - https://doi.org/10.3390/membranes11080576 VL - 11 IS - 8 SP - 576 PB - MDPI AN - OPUS4-53067 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hicke, Konstantin T1 - Distributed fiber optic sensing for monitoring of pipelines and submarine cables N2 - Division 8.6's competencies and work focus areas are shortly outlined and investigations related to pipeline and submarine power cable monitoring using different distributed fiber optic sensing techniques are presented with some results. Furthermore, BAM 8.6 expertise in the field of sensor application, embedding and integration is shown. T2 - Joint BAM-Vallourec Workshop "Knowledge Exchange NDT" CY - Online meeting DA - 02.09.2021 KW - Distributed fiber optic sensing KW - Infrastructure monitoring KW - DAS KW - DTS KW - Pipeline monitoring PY - 2021 AN - OPUS4-53189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ecke, Alexander T1 - An Immunosensor for Pharmaceutical Contaminants in Water Supply N2 - Contamination of drinking water with pharmaceuticals is an emerging problem and a potential health threat. Immunochemical methods based on the binding of the analyte to specific antibodies enable fast and cost-effective on-site analyses. Magnetic bead-based immunoassays allow for implementation into an immunosensor for online testing. These particles are prepared by either coupling the analyte molecule (diclofenac) or the respective antibody (amoxicillin) to the surface. For miniaturization, detection is performed electrochemically on a microfluidic chip. The developed immunosensor will enable detection of pharmaceuticals directly in water supply pipes. T2 - GDCh Wissenschaftsforum Chemie CY - Online meeting DA - 29.08.2021 KW - Immunosensor KW - Magnetic Beads KW - Diclofenac KW - Amoxicillin KW - Water Analysis PY - 2021 AN - OPUS4-53192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - Untersuchung von PFAS-Summenparameter-Methoden Vergleich zwischen AOF vs. EOF und CIC vs. HR-CS-GFMAS N2 - Per- und polyfluorierte Alkylverbindungen (PFAS) sind eine Substanzklasse mit über 5200 Verbindungen. Aufgrund der Persistenz, Bioakkumulation in Nahrungsketten, Toxizität und der ubiquitären Verbreitung von PFAS zählen sie zu den „emerging pollutants“. Die PFAS-Analytik ist wegen den vielfältigen physikalisch-chemischen Eigenschaften und der sehr hohen Anzahl an PFAS eine große Herausforderung. Da es für viele Anwendungen noch ungewiss ist, welche PFAS verwendet werden, wie sie in die Umwelt gelangen und welche Transformations- bzw. Abbauprodukte entstehen, stoßen analytische Ansätze, die nur auf Einzelsubstanzen abzielen, hier an ihre Grenzen. Weiterhin wird die Analytik aufgrund der Substitution von bereits regulierten PFAS mit ständig steigenden Anzahlen an PFAS-Verbindungen in der Umwelt konfrontiert. PFAS-Summenparameter-Methoden, die ein nahezu vollständiges Abbild der PFAS-Belastungssituation wiedergeben, werden daher immer wichtiger. In unserer Studie haben wir die zwei meistverwendeten PFAS-Summenparameter, das adsorbierbare organisch gebundene Fluor (AOF) und das extrahierbare organisch gebundene Fluor (EOF), miteinander verglichen. Beide Summenparameter können zur Analyse mit entweder combustion-Ionenchromatographie (CIC) oder hochauflösender Molekülabsorptionsspektrometrie (HR-CS-GFMAS) gekoppelt werden. Hierbei diskutieren wir die Vor- und Nachteile sowohl von beiden Summenparameter- als auch beider Detektions-Methoden. Die Untersuchungen wurden mit Oberflächenwasserproben aus der Spree in Berlin durchgeführt. Neben AOF und EOF wurde auch der Gesamt-Fluorgehalt (TF) mit CIC sowie HR-CS-GFMAS bestimmt. Die Fluor-Massenbilanzierung zeigte, dass das Verhältnis AOF/TF höher als das Verhältnis EOF/TF war. Dabei machte der AOF 0.14–0.81% vom TF und der EOF 0.04–0.28% vom TF aus. Insgesamt war die neue EOF/HR-CS-GFMAS-Methode schneller, präziser und sensitiver als die bereits etablierte AOF/CIC-Methode. Beide Methoden sind vielversprechend für die zukünftige Überwachung von Umweltproben und bilden die Grundlage für mögliche Grenzwerte, die auf die Summe PFAS abzielen. T2 - Umwelt 2021 CY - Online meeting DA - 07.09.2021 KW - PFAS KW - HR-CS-GFMAS KW - CIC KW - AOF KW - EOF KW - Fluor PY - 2021 AN - OPUS4-53226 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gehrenkemper, Lennart T1 - Erfassung der PFAS-Belastungssituation in Umweltproben - Schnelle & sensitive PFAS-Summenparameteranalytik mittels HR-CS-GFMAS N2 - In der Verbindungsklasse der per- und polyfluorierte alkylischen Substanzen (PFAS) werden über 5200 organische Verbindungen zusammengefasst. PFAS sind an mindestens einem Kohlenstoffatom vollständig fluoriert. Sie werden mit negativen Einflüssen auf die menschliche und tierische Gesundheit assoziiert, sind extrem persistent in der Umwelt und bioakkumulieren entlang von Nahrungsnetzen. Daher zählen PFAS zu den „emerging pollutants“. Gleichzeitig machen ihre physikalisch-chemischen Eigenschaften sie für die Verwendung in diversen technischen Anwendungen attraktiv. Sie sind sowohl hydro- als auch lipophob und zeigen durch die starke C-F-Bindung hohe thermische wie chemische Beständigkeit. Erste Regulierungen einiger PFAS in Kombination mit den technisch hervorragenden Eigenschaften erzeugt einen Innovationsdruck und führten zu einem enormen Anstieg in der Zahl der Substitutionsverbindungen. Auf Grund der steigenden Komplexität der Substanzklasse ist die Target-Analytik nicht in der Lage eine solche Vielfalt und Vielzahl an Analyten zu erfassen. Für eine akkurate Erfassung der Belastungssituation durch PFAS, die Identifikation von PFAS-Hotspots und eine Bewertung von geeigneten Sanierungsmaßnahmen ist daher eine geeignete PFAS-Summenparameteranalytik notwendig. Daher geben wir hier Einblicke in den aktuellen Stand der PFAS-Summenparameterentwicklung und präsentieren unsere neusten Ergebnisse zur Methodenentwicklung für die quantitative Analyse von PFAS als extrahierbares organisch gebundenes Fluor (EOF) in Umweltproben mittels hochauflösender Molekülabsorptionsspektrometrie (HR-CS-GFMAS). Hierfür optimierten wir die Extraktion von PFAS aus verschieden Feststoff-Matrizes bei zeitgleicher Abtrennung anorganischen Fluorids. Durch den Zusatz von Galliumsalz-Lösungen als modifier in der HR-CS-GFMAS kann Fluor indirekt sehr selektiv durch die in situ Bildung von GaF sehr nachweisstark (instrumentelle LOQ ~3 µg/L) quantifiziert werden. T2 - Umwelt 2021 CY - Online meeting DA - 07.09.2021 KW - Per- and polyfluorinated alkyl substances (PFASs) KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Solid phase extraction (SPE) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction KW - Böden PY - 2021 AN - OPUS4-53227 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gehrenkemper, Lennart T1 - Finding the most suitable PFASs sum parameter method - A Comparison of AOF vs. EOF and CIC vs. HR-CS-GFMAS N2 - Since it is unknown for many applications, which PFASs are used and how they enter the environment, target analysis-based methods reach their limits. The two most frequently used sum parameters are the adsorbable organically bound fluorine (AOF) and the extractable organically bound fluorine (EOF). Both can be quantified using either combustion ion chromatography (CIC) or high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). Here we provide an insight on the advantageous and disadvantageous of both sum parameters and both detection methods. Our study is based on the analysis of surface water samples. Next to total fluorine (TF) analysis, AOF and EOF were determined as well as CIC and HR-CS-GFMAS are compared and results are comparatively discussed. Fluorine mass balancing revealed that, the AOF/TF proportion was higher than the EOF/TF proportion. The AOF made up 0.14–0.81% of TF and the EOF 0.04–0.28% of TF. Although, organically bound fluorine represents only a small portion of TF, PFASs are of worldwide concern, because of their extreme persistence and their bioaccumulation potential. The EOF-HR-CS-GFMAS method turned out to be more precise and sensitive than the AOF-CIC method and is a promising tool for future monitoring studies/routine analysis of PFASs in the environment. T2 - Emerging Contaminants in the Environment Conference CY - Online meeting DA - 27.04.2021 KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Combustion ion chromatography (CIC) KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Adsorbable organically bound fluorine (AOF) KW - Extractable organically bound fluorine (EOF) PY - 2021 AN - OPUS4-53228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Spurenbestandteile in frühmittelalterlichem Ägyptisch Blau als Informationsträger N2 - Naturwissenschaftliche Belege für die Verwendung von Ägyptisch Blau, dem klassischen Blaupigment der römischen Antike, an frühmittelalterlichen Wandmalereien in Mittel- und Südeuropa sind bisher nur vereinzelt greifbar. Das hier diskutierte monochrom blaue Fragment einer Freskomalerei auf Tünche gehört zum zweiten Kirchenbau von St. Peter ob Gratsch (Südtirol, Norditalien); zumindest der Putzmörtel ist gemäß Radiocarbondatierung im 5. oder 6. Jahrhundert n. Chr. zu verorten. Das flächendeckende Abrastern der Probenoberfläche mittels Ramanmikrospektroskopie vermochte neben dem farbgebenden Cuprorivait (und Pflanzenschwarz aus der Untermalung) 26 begleitende Mineralien bis in den Spurenbereich nachzuweisen. Diese erstaunliche Vielfalt ist nur durch mikrospektroskopische Bildgebung in hoher Ortsauflösung zugänglich, ein solch vertiefter Einblick in die Mineralogie der zugrundeliegenden Rohstoffe als auch Umwandlungsreaktionen während Herstellung, Applikation und Alterung des künstlichen Blaupigmentes also an die Weiterentwicklung der analytischen Verfahren gebunden. Insbesondere die natürlichen Verunreinigungen des Quarzsandes liefern Indizien auf die Produktionsstätte: die beiden Klinopyroxene Augit und Aegirin deuten beispielsweise auf magmatischen Aktivitäten ausgesetzte Ablagerungen (oder auf vulkanische Aktivität bereits im Liefergebiet). Zusammen mit Diopsid und Feldspaten, einschließlich des seltenen Celsian, sind sie der Literatur zufolge charakteristischer Bestandteil von vom Fluss Volturno in den Golf von Gaeta transportierten carbonathaltigen Sedimenten. Im Verein mit der archäologischen Evidenz für die Erzeugung von Ägyptisch Blau in Cumae und Liternum und den übereinstimmenden Ausführungen der beiden römischen Fachschriftsteller Vitruv und Plinius der Ältere spricht dies für ein Fabrikat aus dem Golf von Pozzuoli. Als Kupferquelle wurde angesichts des Nachweises von Chalkosin (und Chalkopyrit) vermutlich ein sulfidisches Kupfererz nach Rosten zu Kupferoxid eingesetzt, als schmelzpunktsenkendes Flussmittel wohl ein gemischt-alkalisches, das heißt eine Mischung von Natrium- und Kaliumsalzen in Form von Pflanzenasche. Zum Teil mit Cuprorivait verwachsene, nicht gänzlich umgesetzte Quarzkristalle bei nur geringsten Spuren von Silikatglas lassen auf eine überwiegende Festkörperreaktion (Festphasensintern) schließen; das Aufschmelzen der Rohstoffe zu Glas dürfte bei der Pigmentsynthese eher eine untergeordnete Rolle gespielt haben. KW - Ägyptisch Blau KW - Ramanmikrospektroskopie KW - Spektroskopische Bildgebung KW - Cuprorivait KW - Amorpher Kohlenstoff PY - 2021 VL - 34 SP - 109 EP - 122 PB - Wernersche Verlagsgeselltschaft CY - Worms AN - OPUS4-53758 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Trace compounds in Early Medieval Egyptian blue carry information on provenance, manufacture, application, and ageing N2 - Only a few scientific evidences for the use of Egyptian blue in Early Medieval wall paintings in Central and Southern Europe have been reported so far. The monochrome blue fragment discussed here belongs to the second church building of St. Peter above Gratsch (South Tyrol, Northern Italy, fifth/ sixth century A.D.). Beyond cuprorivaite and carbon black (underpainting), 26 accessory minerals down to trace levels were detected by means of Raman microspectroscopy, providing unprecedented insights into the raw materials blend and conversion reactions during preparation, application, and ageing of the pigment. In conjunction with archaeological evidences for the manufacture of Egyptian blue in Cumae and Liternum and the concordant statements of the antique Roman writers Vitruvius and Pliny the Elder, natural impurities of the quartz sand speak for a pigment produced at the northern Phlegrean Fields (Campania, Southern Italy). Chalcocite (and chalcopyrite) suggest the use of a sulphidic copper ore, and water-insoluble salts a mixed-alkaline flux in the form of plant ash. Not fully reacted quartz crystals partly intergrown with cuprorivaite and only minimal traces of silicate glass portend solid-state reactions predominating the chemical reactions during synthesis, while the melting of the raw materials into glass most likely played a negligible role. KW - Egyptian blue KW - Raman microspectroscopy KW - Spectoscopic imaging KW - Cuprorivaite KW - Amorphous carbon PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537591 DO - https://doi.org/10.1038/s41598-021-90759-6 VL - 11 SP - 1 EP - 12 PB - Nature Portfolio AN - OPUS4-53759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Kraft, Ronja A1 - Dariz, P. T1 - Shedding light onto the spectra of lime - Part 2: Raman spectra of Ca and Mg carbonates and the role of d-block element luminescence N2 - We previously described the observation of a characteristic narrowband red luminescence emission of burnt lime (CaO), whose reason was unknown so far. This study presents Raman spectra of Mg5 CO3)4(OH)2∙4H2O, Mg5(CO3)4(OH)2, MgCO3, CaMgCO3 and CaCO3 (in limestone powder) as well as luminescence spectra of their calcination products. Comparison of the latter revealed MgO:Cr3+ as the source of the red lime luminescence in all studied samples, containing magnesium oxide as major component, minor component or trace. Spectral characteristics and theoretical background of the luminescence emission of d-block elements integrated in crystal lattices are discussed with the aim of sharpening the awareness for this effect in the Raman community and promoting its application in materials analysis. The latter is demonstrated by the Raman microspectroscopic imaging of the distributions of both Raman-active and Raman-inactive phases in clinker remnants in a 19th-century meso Portland cement mortar sample, which contain relatively high amounts of free lime detected in the form of both luminescing CaO and Raman-scattering Ca(OH)2, owing to exposure of the surface of the thin section to humid air. A combination of light and Raman spectroscopy revealed a calcium–magnesium–iron sulphide phase, indicating sulphurous raw materials and/or solid fuels employed in the calcination process, which in contrast to previously described morphologies of sulphides in cement clinker form extensive greenish black layers on free lime crystals. KW - Calcium carbonates KW - Raman spectroscopy KW - Luminescence KW - Magnesium carbonates KW - Meso Portland cement PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537611 DO - https://doi.org/10.1002/jrs.6174 SN - 0377-0486 VL - 52 IS - 8 SP - 1462 EP - 1472 PB - Wiley Analytical Science AN - OPUS4-53761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zeipert, H. A1 - Claes, L. A1 - Johannesmann, S. A1 - Lugovtsova, Yevgeniya A1 - Nicolai, Marcel A1 - Prager, Jens A1 - Henning, Bernd ED - Jumar, U. T1 - An approach to adhesive bond characterisation using guided acoustic waves in multi-layered plates N2 - An approach for the non-destructive characterisation of adhesive bonds using guided ultrasonic waves is presented. Pulsed laser radiation is used to thermoacoustically excite broadband ultrasonic waves in a multi-layered sample, consisting of a metal plate adhesively joined to a polymeric layer using synthetic resin. The resulting signals are received by a purpose-built piezoelectric transducer. Varying the distance between excitation and detection yields spatio-temporal measurement data, from which the dispersive properties of the propagating waves can be inferred using a two-dimensional Fourier transform, assuming the plates to act as coupled waveguides. Coupled multi-layered waveguides show an effect referred to as mode repulsion, where the distance between certain modes in the frequency-wavenumber domain is assumed to be a measure of coupling strength. Measurements at different stages of curing of the adhesive layer are performed and evaluated. A comparison of the results shows changes in the dispersive properties, namely an increased modal bandwidth for the fully cured sample as well as an increased modal distance. KW - Adhesive bonding KW - Guided waves KW - Non-destructive testing KW - Ultrasound PY - 2021 DO - https://doi.org/10.1515/auto-2021-0089 VL - 69 IS - 11 SP - 962 EP - 969 PB - De Gruyter CY - Berlin/Boston AN - OPUS4-53762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Hidde, Julia A1 - Grünier, Sophie A1 - Jungnickel, Robert A1 - Dariz, P. A1 - Riedel, Jens A1 - Neuhaus, B. T1 - Ageing effects in mountig media of microscope slide samples from natural history collections: A case study with Canada balsam and Permount™ N2 - Microscope slide collections represent extremely valuable depositories of research material in a natural history, forensic, veterinary, and medical context. Unfortunately, most mounting media of these slides deteriorate over time, with the reason for this not yet understood at all. In this study, Raman spectroscopy, ultraviolet–visible (UV–Vis) spectroscopy, and different types of light microscopy were used to investigate the ageing behaviour of naturally aged slides from museum collections and the experimentally aged media of Canada balsam and Permount™, representing a natural and a synthetic resin, respectively, with both being based on mixtures of various terpenes. Whereas Canada balsam clearly revealed chemical ageing processes, visible as increasing colouration, Permount™ showed physical deterioration recognisable by the increasing number of cracks, which even often impacted a mounted specimen. Noticeable changes to the chemical and physical properties of these mounting media take decades in the case of Canada balsam but just a few years in the case of Permount™. Our results question whether or not Canada balsam should really be regarded as a mounting medium that lasts for centuries, if its increasing degree of polymerisation can lead to a mount which is no longer restorable. KW - Deterioration KW - Microscope slides KW - Mounting media KW - Raman spectroscopy KW - UV–Vis spectroscopy PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537632 DO - https://doi.org/10.3390/polym13132112 VL - 13 IS - 13 SP - 1 EP - 27 PB - MDPI CY - Basel AN - OPUS4-53763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - model of laser induced plasma relevant to structuring and coating of titanium implants N2 - The presentation will give a brief overview of the processes occurring in laser-induced plasma and methods of modeling these processes. In particular, a chemical-hydrodynamic model will be considered, which is related to the modification of the surface of metallic titanium by laser pulses. The details and simplifications of this model, its shortcomings and the possibilities of their elimination will be discussed. This model is related to the structuring of the surface of dental implants with a laser and the deposition of an oxide film on it. T2 - THE 2-nd THEMATIC INTERNATIONAL SCIENTIFIC AUTUMN SCHOOL ON LASER MICRO- & NANOTHECHNOLOGIES: 2021 – BIOMEDICAL TECHNOLOGIES CY - St. Petersburg, Russia DA - 09.11.2021 KW - Laser ablation KW - Laser induced plasma deposition KW - Surface coating KW - Emission spectroscopy KW - Hydrodynamic model KW - Plasma chemistry PY - 2021 AN - OPUS4-53718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Yi A1 - Riedel, Jens T1 - Approaching phase-imaging through defocusing shadowgraphy for acoustic resonator diagnosis and the capability of direct index-of-refraction measurements N2 - The visualization of index-of-refraction (IoR) distribution is one of the common methods to investigate fluid flow or pressure fields. While schlieren and shadowgraphy imaging techniques are widely accepted, their inherent limitations often lead to difficulties in elucidating the IoR distribution and extracting the true IoR information from the resulting images. While sophisticated solutions exist, the IoR-gradient-to-image was achieved by purposely introducing a commonly avoided “defect” into the optical path of a conventional coincident schlieren/shadowgraphy setup; the defect is a combination of slight defocusing and the use of non-conjugate optical components. As such, the method presented in this work is referred to as defocusing shadowgraphy, or DF-shadowgraphy. While retaining the ease of a conventional schlieren/shadowgraphy geometry, this DF approach allows direct visualization of complicated resonant acoustic fields even without any data processing. For instance, the transient acoustic fields of a common linear acoustic resonator and a two-dimensional one were directly visualized without inversion. Moreover, the optical process involved in DF-shadowgraphy was investigated from a theoretical perspective. A numerical solution of the sophisticated impulse response function was obtained, which converts the phase distortion into intensity distributions. Based on this solution, the IoRs of various gas streams (e.g., CO2 and isopropanol vapor) were determined from single images. KW - Imaging Technique KW - Phase Imaging KW - Shadowgraphy KW - Schlieren Imaging PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537116 DO - https://doi.org/10.1063/5.0058334 SN - 1089-7623 VL - 92 IS - 10 SP - 103703 PB - AIP Publishing Group AN - OPUS4-53711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Uncertainty budgets in surface techno-logy: step height, layer thickness, indentation hardness, adehesive strength N2 - The object (sample) and the measurement/testing procedure may always have unknown degrees of freedom, i.e. instead of 𝐯 ≥ n – 1 in many cases 𝐯 ≫ n - 1 may apply, in particular in the micro- and nano-world! T2 - 10. VDI-Fachtagung, Messunsicherheit und Prüfprozesse CY - Erfurt, Germany DA - 10.11.2021 KW - Methodology in metrology KW - Methodology in testing KW - Spectroscopic Ellipsometry KW - Instrumented Indentation (IIT) KW - Centrifugal Adhesion Testing (CAT) PY - 2021 AN - OPUS4-53739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Heyn, L. A1 - Jung, Christian T1 - Indoor exposure to airborne polycyclic aromatic hydrocarbons: A comparison of stir bar sorptive extraction and pump sampling N2 - Stir bar sorptive extraction (SBSE) was compared with standardized pump sampling regarding the prospects to assess airborne levels of polycyclic aromatic hydrocarbons (PAHs) in indoor environments. A historic railway water tower, which will be preserved as a technical monument for museum purposes, was sampled with both approaches because the built-in insulationmaterial was suspected to release PAHs to the indoor air. The 16 PAHs on the US EPA list were quantified using gas chromatography with mass spectrometric detection in filters from pump sampling after solvent extraction and on SBSE devices after thermal desorption. SBSEwas seen to sample detectable PAHmasseswith excellent repeatability and a congener pattern largely similar to that observed with pump sampling. Congener patterns were however significantly different from that in the PAH source because release from the insulation material is largely triggered by the respective congener vapor pressures. Absolute masses in the ng range sampled by SBSE corresponded to airborne concentrations in the ng L−1 range determined by pump sampling. Principle differences between SBSE and pump sampling as well as prospects of SBSE as cost-effective and versatile complement of pump sampling are discussed. KW - Polycyclic aromatic hydrocarbons KW - Adsorption KW - Extraction KW - Indoor air PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537427 DO - https://doi.org/10.1002/eng2.12419 VL - 3 IS - 12 SP - 1 EP - 10 PB - John Wiley & Sons Ltd. AN - OPUS4-53742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien A1 - Ahmadi, Samim A1 - Hirsch, Philipp Daniel A1 - Rupprecht, C. A1 - Ziegler, Mathias ED - Kimata, M. ED - Shaw, J. A. ED - Valenta, C. R. T1 - Investigations on photothermal super resolution reconstruction using 2D-structured illumination patterns N2 - Active thermography as a nondestructive testing modality suffers greatly from the limitations imposed by the diffusive nature of heat conduction in solids. As a rule of thumb, the detection and resolution of internal defects/inhomogeneities is limited to a defect depth to defect size ratio greater than or equal to one. Earlier, we demonstrated that this classical limit can be overcome for 1D and 2D defect geometries by using photothermal laser-scanning super resolution. In this work we report a new experimental approach using 2D spatially structured illumination patterns in conjunction with compressed sensing and computational imaging methods to significantly decrease the experimental complexity and make the method viable for investigating larger regions of interest. T2 - Future Sensing Technologies Conference 2021 CY - Online meeting DA - 15.11.2021 KW - Thermography KW - Super resolution KW - NDT KW - Inspection KW - Image resolution PY - 2021 DO - https://doi.org/10.1117/12.2603838 VL - 11914 SP - 124 EP - 131 PB - International Society for Optics and Photonics. SPIE AN - OPUS4-53745 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien T1 - Investigations on photothermal super resolution reconstruction using 2D-structured illumination patterns N2 - Active thermography as a nondestructive testing modality suffers greatly from the limitations imposed by the diffusive nature of heat conduction in solids. As a rule of thumb, the detection and resolution of internal defects/inhomogeneities is limited to a defect depth to defect size ratio greater than or equal to one. Earlier, we demonstrated that this classical limit can be overcome for 1D and 2D defect geometries by using photothermal laser-scanning super resolution. In this work we report a new experimental approach using 2D spatially structured illumination patterns in conjunction with compressed sensing and computational imaging methods to significantly decrease the experimental complexity and make the method viable for investigating larger regions of interest. T2 - Future Sensing Technologies Conference 2021 CY - Online meeting DA - 15.11.2021 KW - Thermography KW - Super resolution KW - NDT KW - Inspection KW - Image resolution PY - 2021 UR - https://www.spiedigitallibrary.org/conference-proceedings-of-spie/11914/2603838/Investigations-on-photothermal-super-resolution-reconstruction-using-2D-structured-illumination/10.1117/12.2603838.full AN - OPUS4-53747 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Schallfeldvermessungen von luftgekoppelten Ultraschallwandlern N2 - Zur Charakterisierung von Ultraschallwandlern finden unterschiedliche Methoden und Verfahren Anwendung. Während sich die ISO 22232:2021 verstärkt auf die Charakterisierung von Kontakt- und Tauchtechnikprüfköpfen konzentriert, wird über eine einheitliche Charakterisierung von luftgekoppelten Wandlern noch diskutiert. Durch die unterschiedlichen Herangehensweisen beinhalten Prüfkopf-Datenblätter oft unterschiedliche Prüfkopfparameter und Schallfeldgrößen, was einen direkten Vergleich und eine Applikation im Feld erschwert. So werden bspw. Wandler nach ISO 22232:2021 standardmäßig im Impuls-Echo-Betrieb charakterisiert. Allerdings ist dies nicht auf die in den letzten Jahren entwickelten luftgekoppelten Wandlertechnologien übertragbar, die nur als Sender oder als Empfänger einsetzbar sind. Daher arbeiten aktuell Hersteller, Forschungseinrichtungen und Anwender gemeinsam im Rahmen des Unterausschusses „Luftgekoppelte Ultraschallprüfung“ der DGZfP an der Erstellung einer Richtlinie. Diese Richtlinie stellt dabei den Anspruch dar, die bestehende Normung um die luftgekoppelte Prüfung zu erweitern und somit die Vereinheitlichung der Charakterisierung dieser Wandler zu erleichtern. In diesem Beitrag werden daher verschiedene Methoden der Schallfeldvermessung vorgestellt, untereinander verglichen und ihre Grenzen beschrieben. Abschließend wird auf die besonders herausfordernde Charakterisierung von und mit breitbandigen luftgekoppelten Sendern und Empfängern eingegangen. T2 - Seminar des Fachausschusses Ultraschallprüfung Konventionelle und innovative Anwendungen der Ultraschallprüfverfahren CY - Berlin, Germany DA - 10.11.2021 KW - Luftgekoppelte Ultraschallprüfung KW - Schallfeld KW - Charakterisierung PY - 2021 AN - OPUS4-53750 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - К определению прочности клеевого соединения в многослойных материалах путем исследования областей расталкивания бегущих упругих волн T1 - Towards the determination of adhesive bonding strength of multi-layered materials by investigating guided wave mode repulsion N2 - Бегущие упругие волны часто используются в области неразрушающего контроля для определения механических характеристик материалов. Поскольку склеивание различных материалов является широко используемым методом в автомобильной и авиационной промышленности, необходима надежная система измерения для определения качества таких клеевых соединений. Дисперсионные кривые для многослойных волноводов при наличии клеевых прослоек характеризуются появлением эффекта расталкивания нормальных мод в тех областях, где соответствующие моды для отдельных материалов пересекались бы. Таким образом, в зависимости от качества клеевого соединения расстояние между этими модами изменяется. Используя комбинацию экспериментальных и численных данных, в настоящей работе представлен подход к определению параметра, указывающего на качество клеевого соединения. T2 - XXX Всероссийская школа-конференция МАТЕМАТИЧЕСКОЕ МОДЕЛИРОВАНИЕ В ЕСТЕСТВЕННЫХ НАУКАХ CY - Perm, Russia DA - 06.10.2021 KW - многослойный волновод KW - волны лэмбовского типа KW - контроль качества клеевого соединения PY - 2021 AN - OPUS4-53768 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya A1 - Zeipert, H. A1 - Johannesmann, S. A1 - Nicolai, Marcel A1 - Prager, Jens A1 - Henning, B. T1 - К определению прочности клеевого соединения в многослойных материалах путем исследования областей расталкивания бегущих упругих волн T1 - Towards the determination of adhesive bonding strength of multi-layered materials by investigating guided wave mode repulsion N2 - Бегущие упругие волны часто используются в области неразрушающего контроля для определения механических характеристик материалов. Поскольку склеивание различных материалов является широко используемым методом в автомобильной и авиационной промышленности, необходима надежная система измерения для определения качества таких клеевых соединений. Дисперсионные кривые для многослойных волноводов при наличии клеевых прослоек характеризуются появлением эффекта расталкивания нормальных мод в тех областях, где соответствующие моды для отдельных материалов пересекались бы. Таким образом, в зависимости от качества клеевого соединения расстояние между этими модами изменяется. Используя комбинацию экспериментальных и численных данных, в настоящей работе представлен подход к определению параметра, указывающего на качество клеевого соединения. T2 - XXX Всероссийская школа-конференция МАТЕМАТИЧЕСКОЕ МОДЕЛИРОВАНИЕ В ЕСТЕСТВЕННЫХ НАУКАХ CY - Online meeting DA - 06.10.2021 KW - многослойный волновод KW - волны лэмбовского типа KW - контроль качества клеевого соединения PY - 2021 SP - 1 EP - 3 AN - OPUS4-53769 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Van Den Bossche, T. A1 - Arntzen, M. O. A1 - Becher, D. A1 - Benndorf, D. A1 - Eijsink, V. G. H. A1 - Henry, C. A1 - Jagtap, P. D. A1 - Jehmlich, N. A1 - Juste, C. A1 - Kunath, B. J. A1 - Mesuere, B. A1 - Muth, Thilo A1 - Pope, P. B. A1 - Seifert, J. A1 - Tanca, A. A1 - Uzzau, S. A1 - Wilmes, P. A1 - Hettich, R. L. A1 - Armengaud, J. T1 - The Metaproteomics Initiative: a coordinated approach for propelling the functional characterization of microbiomes N2 - Through connecting genomic and metabolic information, metaproteomics is an essential approach for understanding how microbiomes function in space and time. The international metaproteomics community is delighted to announce the launch of the Metaproteomics Initiative (www.metaproteomics.org), the goal of which is to promote dissemination of metaproteomics fundamentals, advancements, and applications through collaborative networking in microbiome research. The Initiative aims to be the central information hub and open meeting place where newcomers and experts interact to communicate, standardize, and accelerate experimental and bioinformatic methodologies in this feld. We invite the entire microbiome community to join and discuss potential synergies at the interfaces with other disciplines, and to collectively promote innovative approaches to gain deeper insights into microbiome functions and dynamics. KW - Microbiome KW - Metaproteomics KW - Networking KW - Meta-Omics KW - Interactions KW - Education PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542290 DO - https://doi.org/10.1186/s40168-021-01176-w VL - 9 IS - 1 SP - 243 PB - BMC AN - OPUS4-54229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ecke, Alexander A1 - Westphalen, Tanja A1 - Hornung, J. A1 - Voetz, M. A1 - Schneider, Rudolf T1 - A rapid magnetic bead-based immunoassay for sensitive determination of diclofenac N2 - Increasing contamination of environmental waters with pharmaceuticals represents an emerging threat for the drinking water quality and safety. In this regard, fast and reliable analytical methods are required to allow quick countermeasures in case of contamination. Here, we report the development of a magnetic bead-based immunoassay (MBBA) for the fast and cost-effective determination of the analgesic diclofenac (DCF) in water samples, based on diclofenac-coupled magnetic beads and a robust monoclonal anti-DCF antibody. A novel synthetic strategy for preparation of the beads resulted in an assay that enabled for the determination of diclofenac with a significantly lower limit of detection (400 ng/L) than the respective enzyme-linked immunosorbent assay (ELISA). With shorter incubation times and only one manual washing step required, the assay demands for remarkably shorter time to result (< 45 min) and less equipment than ELISA. Evaluation of assay precision and accuracy with a series of spiked water samples yielded results with low to moderate intra- and inter-assay variations and in good agreement with LC–MS/MS reference analysis. The assay principle can be transferred to other, e.g., microfluidic, formats, as well as applied to other analytes and may replace ELISA as the standard immunochemical method. KW - Immunoassay KW - Magnetic beads KW - Diclofenac KW - Water analysis KW - LC-MS/MS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542346 DO - https://doi.org/10.1007/s00216-021-03778-7 SN - 1618-2650 VL - 414 SP - 1563 EP - 1573 PB - Springer CY - Heidelberg AN - OPUS4-54234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Sound field measurements on thermoacoustic air-coupled transducers N2 - There are many different methods to characterize air-coupled ultrasonic transducers for non-destructive testing. Data sheets of various manufacturers contain information about some parameters important for the performance of transducers, but this information is not standardized, so that a comparison between probes of different manufacturers is difficult. Therefore, the German Society for Non-Destructive Testing (DGZfP) is working on a guideline to characterization of air-coupled probes. One of the topics in this guideline is the application of thermoacoustic transducers for the characterization of receivers and another topic is the application of microphones for the characterization of transmitters. In this presentation we compare various characterization methods with the particular focus on the characterization of thermoacoustic transducers using an optical microphone. Both thermoacoustic transmitters and optical microphones have a very large bandwidth compared to conventional air-coupled transducers, but their spectrum is not entirely linear, which needs to be taken into account if they are applied as reference transducers. T2 - JSNDI online workshop “Emerging Technologies of Advanced Ultrasonic Measurement” CY - Online meeting DA - 14.12.2021 KW - Air-coupled ultrasound KW - Transducer KW - Sound field PY - 2021 AN - OPUS4-54195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - ML@BAMLINE N2 - An overview of the machine learning methods used at BAMline. Examples of automatic alignment and optimisation based on Gaussian processes are discussed. Quantification of XRF measurements and reconstruction for coded aperture imaging based on neural networks are also presented. T2 - Machine Learning Workshop BAM CY - Online meeting DA - 18.03.2021 KW - Artificial Intelligence KW - Machine learning KW - Bayesian Optimization KW - Gaussian process KW - Neural Network PY - 2021 AN - OPUS4-54142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Iro, M. T1 - Investigation of the transmission properties of a polycapillary half-lens and their effect on quantification for confocal μXRF N2 - Confocal Micro X-ray fluorescence analysis (μXRF) is a powerful method for the destruction-free investigation of the elemental composition of various samples in three dimensions. Quantitative results rely heavily on the transmission properties of polycapillary optics, used in confocal setups. Different models for the functional correlation between energy and transmission of a polycapillary half-lens are compared with experimental data, established with a monochromatic confocal laboratory setup [1], as well as Monte-Carlo-Simulations [2]. The effect of the different approaches on quantitative results are compared using well known SRMs, ranging from thick samples to thin layers and structured materials. Along with this the basic principles for quantitative evaluations of XRF spectra taken with confocal setups are presented, and compared with experimental results. T2 - Denver X-Ray Conference CY - Online meeting DA - 02.08.2021 KW - Synchrotron KW - BAMline KW - Polycapillaries PY - 2021 AN - OPUS4-54143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lutz, C. A1 - Hampel, S. A1 - Beuermann, S. A1 - Turek, T. A1 - Kunz, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Fittschen, U. E. A. T1 - Investigation on Vanadium Species Distribution in Nafion™ 117 after Cyclization in a Vanadium Redox Flow Battery N2 - The vanadium redox flow battery (VRFB) is currently a potential candidate for stationary energy storage. A major challenge is the unintended vanadium transport through the separator, which results in a fade of capacity. To overcome this issue, it is necessary to understand the transport processes in the membrane on a more fundamental level. In this work, the vanadium species distribution in Nafion™ 117 after cyclization was investigated. Two membranes, one from a charged VRFB and another from a discharged VRFB, were analyzed using ultraviolet–visible spectroscopy (UV/VIS) and X-ray absorption near edge structure spectroscopy (XANES). Little difference between the two membranes was recognizable according to the UV/VIS results. In comparison, the XANES results showed that the membrane from the charged VRFB contains more V3+ than VO2+, whereas for the discharged case, more VO2+ is present in the membrane. KW - Synchrotron KW - BAMline KW - XANES KW - Vanadium redox flow battery PY - 2021 VL - 64 SP - 1 EP - 8 AN - OPUS4-54144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfennig, Anja T1 - Vom Blended Learning zum Full Online – so einfach geht es nicht – Praxiserfahrungen zum Einsatz von Lehrfilmen N2 - Mit Beginn der Covid-19 Pandemie und dem damit verbundenen ausschließlichen Lehren im online-Format war die Hoffnung verbunden ein Blended Learning Lehrformat für die Studieeingangsphase ohne viel konzeptionelle Änderungen übertragen zu können. Der Kurs Werkstofftechnik als Grundlagenfach für den Maschinenbau baut sich auf inverted classroom Lehrszenarien auf, deren Lerngrundlage hierfür eigens produzierte und auf das Lernziel abgestimmte Lehrfilme und Lightboard-Vorlesungen darstellen. Im Kontext der Studieneingangsphase bieten audiovisuell stimulierende Lehrfilme umfassende Lernmedien, wenn sie analog der Lerninhalte einem technischen und didaktischen Qualitätsanspruch genügen. In der Praxis des SS2020 und WS2020/21 hat sich gezeigt, dass die Moderation und Durchführung eines online-Kurses sich deutlich von dem eins blended learning-Kurses unterscheidet. Um denselben Lernerfolg bei Studierenden zu erzielen, müs-sen Anforderungen viel genauer und detaillierter verfasst werden, Studierende enger und persönlicher begleitet werden und Lehrfilme und Lernmedien in einen Gesamtzusammenhang gestellt werden. Im Folgenden werden aus persönlicher Erfahrung heraus niederschwellige, zum Teil ungewöhnliche praktische Erfahrungen zur erfolgreichen Umsetzung von Lehrfilm-basierten inverted classroom Lehrszenarien zusammengefasst und im Hinblick auf die online-Lehre bewertet. T2 - 19. Fachtagung Bildungstechnologien (DELFI) CY - Bonn, Germany DA - 13.09.2021 KW - Inverted classroom KW - Lehrfilm KW - Lehrfilmformate KW - Online KW - Covid-19 PY - 2021 SP - 289 EP - 295 AN - OPUS4-54154 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfennig, Anja T1 - Improving Learning Outcome for GSL (German as a Second Language) Students in a Blended Learning Cumulative Assessment Material Science Course N2 - First year students especially with migration background and language deficiencies rate material science in mechanical engineering as one of the fundamental courses with high work load and necessity of language skills due to the descriptive nature of the course. Therefore a blended learning course structure using based on inverted classroom teaching scenarios was established. Heart of the self-study period are visualizing peer-to-peer lecture films supported by micro-lectures along with various online teaching materials. Although students with migration background generally scored lower in tests due to the lack of language skills improved learning outcomes are demonstrated in high quality class discussions and in overall understanding. This paper introduces the learning structure and graded activities, evaluates the course and compares results of native German-speaking students to those of students with migration background. KW - Portfolio KW - Diversity KW - Blended learning KW - Inverted classroom KW - Lecture films PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-541557 DO - https://doi.org/10.17706/ijeeee.2021.11.3.93-100 SN - 2010-3654 VL - 11 IS - 3 SP - 93 EP - 100 AN - OPUS4-54155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kanzler, D. T1 - Prüf‘ ich noch – oder mess‘ ich schon? Ein Konzept für die Prüfunsicherheitsbestimmung von zerstörungsfreien Prüfsystemen N2 - Häufig stellt sich die Frage, ob eine Materialinhomogenität kritisch für die strukturelle Integrität eines Bauteils ist. Dies ist häufig abhängig von der Größe und der Geometrie dieser Materialinhomogenität. Während die korrekte Bestimmung einer Defektgröße zweifelsfrei eine Messaufgabe darstellt, ist die Detektion eines Materialdefekts die Hauptaufgabe eines Prüfsystems. Allerdings sind manche Defekte zu klein, um detektiert zu werden. Es ist jedoch schwierig, etwas zu bemessen, was nur schwer gefunden werden kann, stellen sowohl die Detektion als auch die Fähigkeit den Defekt zu bemaßen, Teile der der Bewertung eines Prüfsystems dar. Die vorliegende Publikation beschäftigt sich zum einen mit der Notwendigkeit, die Auffindwahrscheinlichkeit von Prüfverfahren zu bewerten, und zum anderen mit den Schritten, mit denen das Konzept der Prüfunsicherheitsbewertung national und international vorangetrieben wird. Final werden die Methoden evaluiert, die den Schulterschluss zwischen Prüf- und Messunsicherheitsbestimmung ermöglichen. Ergänzt wird der Artikel mit Beispielen aus der Industrie, welche die aktuelle Relevanz des Themas untermauern. T2 - 10. VDI-Fachtagung Messunsicherheit praxisgerecht bestimmen – Prüfprozesse in der industriellen Praxis 2021 - Der Weg zum sicheren Messen und Prüfen CY - Erfurt, Germany DA - 10.11.2021 KW - Zerstörungsfreie Prüfung KW - Zuverlässigkeit KW - Human Factors KW - Probability of detection PY - 2021 AN - OPUS4-54248 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kanzler, D. A1 - Rentala, V. A1 - Bertovic, Marija A1 - Heckel, Thomas A1 - Rosenthal, Martina A1 - Keßler, S. A1 - Stolz, R. A1 - Dethof, F. A1 - Jüngert, A. A1 - Vrana, J. T1 - Prüf‘ ich noch – oder mess‘ ich schon? Ein Konzept für die Prüfunsicherheitsbestimmung von zerstörungsfreien Prüfsystemen N2 - Häufig stellt sich die Frage, ob eine Materialinhomogenität kritisch für die strukturelle Integrität eines Bauteils ist. Dies ist häufig abhängig von der Größe und der Geometrie dieser Materialinhomogenität. Während die korrekte Bestimmung einer Defektgröße zweifelsfrei eine Messaufgabe darstellt, ist die Detektion eines Materialdefekts die Hauptaufgabe eines Prüfsystems. Allerdings sind manche Defekte zu klein, um detektiert zu werden. Es ist jedoch schwierig, etwas zu bemessen, was nur schwer gefunden werden kann, stellen sowohl die Detektion als auch die Fähigkeit den Defekt zu bemaßen, Teile der der Bewertung eines Prüfsystems dar. Die vorliegende Publikation beschäftigt sich zum einen mit der Notwendigkeit, die Auffindwahrscheinlichkeit von Prüfverfahren zu bewerten, und zum anderen mit den Schritten, mit denen das Konzept der Prüfunsicherheitsbewertung national und international vorangetrieben wird. Final werden die Methoden evaluiert, die den Schulterschluss zwischen Prüf- und Messunsicherheitsbestimmung ermöglichen. Ergänzt wird der Artikel mit Beispielen aus der Industrie, welche die aktuelle Relevanz des Themas untermauern. T2 - 10. VDI-Fachtagung Messunsicherheit praxisgerecht bestimmen – Prüfprozesse in der industriellen Praxis 2021 CY - Erfurt, Germany DA - 10.11.2021 KW - Zerstörungsfreie Prüfung KW - Zuverlässigkeit KW - Probability of detection KW - Messunsicherheit KW - Human factors PY - 2021 SN - 978-3-18-102390-7 DO - https://doi.org/10.51202/9783181023907-367 SN - 0083-5560 VL - VDI-Bericht 2390 SP - 367 EP - 372 PB - VDI Verlag CY - Düsseldorf AN - OPUS4-54250 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. T1 - Robot-Assisted Air Quality Monitoring N2 - This presentation gives an introduction to robot-assisted air quality monitoring based and shows results of the research project RASEM. T2 - The 6th Meeting of the Investigation Committee on Measurement of Odors and Applications of Their Psychological/Physiological Effects CY - Online meeting DA - 21.01.2022 KW - Environmental Monitoring KW - Air Pollution KW - Air Quality KW - Wireless Sensor Network KW - Mobile Robot Olfaction PY - 2022 AN - OPUS4-54251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Sensors for safety and process control in hydrogen technologies N2 - Sensor systems are widely used in hydrogen technologies. The lecture presents requirements and properties of sensor systems and shows application examples of these technologies for safety and process control for hydrogen technologies. The focus is on gas sensors as well as sensors for pressure, temperature and gas flow. These systems are applied, among other things, for monitoring and control of operating conditions, indication of hazardous conditions and triggering of alarms. T2 - Joint European Summer School 2021 on Fuel Cell, Electrolyser, and Battery Technologies CY - Online meeting DA - 12.09.2021 KW - Sensor KW - Safety KW - Process control KW - Hydrogen technologies PY - 2021 AN - OPUS4-54131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Melzer, Michael T1 - Sensors for safety and process control in hydrogen technologies - Part II - Seminar about the expression of uncertainty in measurement N2 - The determination of the measurement uncertainty of quantitative and qualitative results is an important quality management tool, for example to describe measuring equipment, procedures, measurement results and the quality of products. The lecture presents the process description for the determination of the measurement uncertainty according to GUM, the determination of uncertainties in qualitative measurement results and the application of the measurement uncertainty for conformity assessment. T2 - Joint European Summer School 2021 on Fuel Cell, Electrolyser, and Battery Technologies CY - Online meeting DA - 12.09.2021 KW - Quality management tool KW - Measurement uncertainty KW - Quantiative results KW - Qualitative results KW - Conformity assessment PY - 2021 AN - OPUS4-54132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Introduction of H2Safety@BAM N2 - This contribution for the Open Forum of the 8th HSN Symposium introduces the SensRef activities of the Competence Centre H2Safety@BAM. T2 - 8. HSN-Symposium - HybridSensorNet e. V. CY - Online meeting DA - 11.11.2021 KW - H2Safety@BAM KW - SensRef KW - Hydrogen PY - 2021 AN - OPUS4-54137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Das goldene Zeitalter war damals Analyse von Gold mit Synchrotronstrahlung N2 - Gold ist eines der sieben bereits in der Antike bekannten Metalle und wurde wegen seines Glanzes und seiner Seltenheit seit jeher als Tauschmittel und zur Herstellung von Schmuck verwendet. Außerdem ist es leicht zu bearbeiten und weitgehend resistent gegen chemische Einflüsse. Die Analyse von Gold mit der durch Synchrotronstrahlung angeregten Röntgenfluoreszenzanalyse ist zerstörungsfrei und liefert Informationen über die in der untersuchten Probe vorhandenen chemischen Elemente. Im Mittelpunkt der hier vorgestellten Untersuchungen an der BAMline stehen Fragen nach der Herkunft, dem Herstellungsprozess und der Zugehörigkeit von Goldfunden. Die verschiedenen Fragestellungen werden anhand einer Reihe von Beispielen erläutert, die vom Wikingerschatz von Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten reichen. Darüber hinaus werden die heute am Synchrotron verfügbaren modernen Messmethoden vorgestellt. T2 - WISSENSCHAFT MIT WIRKUNG: Workshop Kulturguterhaltung – vom Dampfkessel zu Nanomaterialien CY - Berlin, Germany DA - 17.11.2021 KW - Gold KW - Synchrotron KW - Bernstorf KW - Nebra KW - XRF PY - 2021 AN - OPUS4-54139 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Machine learning for direct quantification of XRF measurements N2 - In this talk I’ll describe the use of artificial neural networks (ANN) for quantifying X-ray fluorescence (XRF) measurements. The main idea of this talk is to give an overview of the process needed to generate a model that can then be applied to a specific problem. In XRF, a sample is excited with X-rays and the resulting characteristic radiation is detected to determine elements quantitatively and qualitatively. This is traditionally done in several time-consuming steps. I’ll show the possibilities and problems of using a neural network to realise a "one-click" quantification. This includes generating training data using Monte Carlo simulation and augmenting the existing data set with an ANN to generate more data. The search for the optimal hyperparameters, manually and automatically, is also described. For the case presented, we were able to train a network with a mean absolute error of 0.1% by weight for the synthetic data and 0.7% by weight for a set of experimental data obtained with certified reference materials. T2 - Seminar series: Artificial Intelligence applied to X-ray / synchrotron techniques CY - Online meeting DA - 24.06.2021 KW - Artificial intelligence KW - Machine learning KW - Synchrotron KW - XRF PY - 2021 AN - OPUS4-54140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan T1 - Unravelling the depths of complex alloys with grazing exit XANES N2 - High entropy alloys (HEAs) are considered as a new class of alloys containing at least 5 elements with concentrations between 5 and 35 atomic percent. There has been a growing interest in HEAs in the material research field in recent years. Due to their adjustable composition, which enables the modifications of mechanical properties (such as hardness, strength and ductility etc) and their stability at high temperatures, HEAs have been the focus of various studies. Especially the corrosion behavior of HEAs has been a wide research interest. Since the grazing exit X-ray fluorescence (GEXRF) offers a non-destructive way to collect notable information regarding the high temperature oxidation, we consider it as a useful method to investigate how HEAs behave in corrosive environments. The main idea of grazing geometry is to enhance the fluorescence signal of the surface. This enables highly sensitive surface analyses of thin protective film on surface in sub-micrometer scale. Position-sensitive area detectors provide information regarding the signal emitted from the sample as a function of emission angle and thus allow depth-sensitive analysis. Furthermore, the data collected from samples of an incidence energy which lays within a specific energy range provides XANES data to determine oxidation states. Moreover, since GEXRF profiles can also be simulated through physical models (Urbach 1999), they enable us to determine the layer thickness of a given sample in a non-destructive way. In this contribution, we present the preliminary results of a conceptual study regarding layer properties of CrCoNi medium entropy alloy. The successful implementation of such methodological concept will pave the way for the investigation of more complex alloys with multiple layers, which is planned for the later phases of the project. T2 - Denver X-Ray Conference DXC 2021 CY - Online meeting DA - 02.08.2021 KW - GEXRF KW - High entropy alloys KW - XANES KW - Grazing exit KW - XAS PY - 2021 AN - OPUS4-54027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan T1 - Unrevealing the depths of compositionally complex alloys with grazing exit XANES N2 - High entropy alloys (HEAs) are considered as a new class of alloys containing at least 5 elements with concentrations between 5 and 35 atomic percent. There has been a growing interest in HEAs in the material research field in recent years. Due to their adjustable composition, which enables the modifications of mechanical properties (such as hardness, strength and ductility etc) and their stability at high temperatures, HEAs have been the focus of various studies. Especially the corrosion behavior of HEAs has been a wide research interest. Since the grazing exit X-ray fluorescence (GEXRF) offers a non-destructive way to collect notable information regarding the high temperature oxidation, we consider it as a useful method to investigate how HEAs behave in corrosive environments. The main idea of grazing geometry is to enhance the fluorescence signal of the surface. This enables highly sensitive surface analyses of thin protective film on surface in sub-micrometer scale. Position-sensitive area detectors provide information regarding the signal emitted from the sample as a function of emission angle and thus allow depth-sensitive analysis. Furthermore, the data collected from samples of an incidence energy which lays within a specific energy range provides XANES data to determine oxidation states. Moreover, since GEXRF profiles can also be simulated through physical models (Urbach 1999), they enable us to determine the layer thickness of a given sample in a non-destructive way. In this contribution, we present the preliminary results of a conceptual study regarding layer properties of CrCoNi medium entropy alloy. The successful implementation of such methodological concept will pave the way for the investigation of more complex alloys with multiple layers, which is planned for the later phases of the project. T2 - XAFS 2021, The 18th International XAFS Conference CY - Online meeting DA - 02.08.2021 KW - GEXRF KW - High entropy alloys KW - XANES KW - Grazing exit KW - XAS PY - 2021 AN - OPUS4-54028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Analytical Insights at the Point-Of-Need By Immunoanalytical Technologies N2 - A vast number of emerging pollutants is being detected in the environment. Another lingering problem are health-threatening contaminants, such as mycotoxins, that deteriorate food and feed. Analytical methods, suitable for trace analysis, are needed that are desirably also fast, inexpensive and, if possible, robust, and portable. Immunoanalytical, i.e., anti-body-based technologies, which are available in a broad range of formats, can be profitably used here to analyze for the distribution and the concentration trends of contaminants. Some of these formats are single-analyte but high-throughput methods. To use them wisely, indicator substances or sum parameters must be established to be used in screening approaches. Other methods are suitable to be performed on portable in-strumentation in the field (on-site), more precisely at the point-of-need. Furthermore, there are array technologies that allow for parallel analysis of several analytes of interest (multiplexing). The talk reports on methods and data for compounds con-sidered as anthropogenic contamination markers (the antiepileptic carbamazepine, the analgesic diclofenac, the anti-histaminic cetirizine, the steroid hormone estrone, the antimicrobial amoxicillin, the stimulants caffeine and cocaine, the endocrine disruptor bisphenol A, and a bile acid). Some work on mycotoxins (ochratoxin A and ergot alkaloids) is also presented. It is demonstrated that antibody-based technolo-gies have a huge potential to gain analytical insights at the point-of-need. T2 - Virtual International Symposium on Immunoanalytical Technologies for Environmental Monitoring and Human Health CY - Online meeting DA - 10.12.2021 KW - Biosensoren KW - Schnelltest KW - ELISA KW - Lateral Flow Assay PY - 2021 AN - OPUS4-54037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Advanced Materials in antibody-based analytical techniques for environmental analysis N2 - Antibody-based analytical techniques have gained increasing importance in environmental analysis. Rapid assays, portable devices and formats that require a limited number of steps have a high potential for on-site analysis in outdoor environments or in environmentally relevant facilities such as wastewater treatment plants. Many of these methods have become more sensitive and more versatile due to new, advanced materials, such as novel particles, specifically prepared surfaces, new labels, specifically coated electrodes etc. The talk shows some of our works in this context. T2 - V Analytical Chemistry Symposium: Advanced Materials for Environmental Applications CY - Online meeting DA - 24.11.2021 KW - Biosensoren KW - Immunoassay KW - Schnelltest KW - Vor-Ort-Analytik KW - Portable Analytik PY - 2021 AN - OPUS4-54038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Analytical insights at the point-of-need with antibody-based methods N2 - A vast number of emerging pollutants is being detected in the environment. Another lingering problem are health-threatening contaminants, such as mycotoxins, that deteriorate food and feed. Analytical methods, suitable for trace analysis, are needed that are desirably also fast, inexpensive and, if possible, robust, and portable. Immunoanalytical, i.e., antibody-based methods, which are available in a broad range of formats, can be profitably used here to analyze for the distribution and the concen-tration trends of contaminants. Some of these formats are single-analyte but high-throughput methods. To use them wisely, indicator substances or sum parameters are being established and used in screening approaches. Other methods are suitable to be performed on portable instrumentation in the field (on-site), more precisely at the point-of-need. Furthermore, there are array technologies that allow for parallel analysis of several analytes of interest (multiplexing). The talk reports on methods and data for compounds considered as anthropogenic contamination markers (the antiepileptic carbamazepine, the analgesic diclofenac, the anti-histaminic cetirizine, the steroid hormone estrone, the antimicrobial amoxicillin, the stimulants caffeine and cocaine, the endo-crine disruptor bisphenol A, and a bile acid). Some work on mycotoxins (ochratoxin A and ergot alka-loids) is also presented. It is demonstrated that antibody-based approaches have a huge potential to gain analytical insights at the point-of-need. T2 - empa - Seminar of the Laboratory of Advanced Analytical Technologies CY - Online meeting DA - 24.11.2021 KW - Biosensoren KW - Point-of-Care KW - Schnelltests KW - Vor-Ort-Analytik PY - 2021 AN - OPUS4-54040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schnur, C. A1 - Moll, J. A1 - Lugovtsova, Yevgeniya A1 - Schütze, A. A1 - Schneider, T. T1 - Explainable machine learning for damage detection - In carbon fiber composite plates under varying temperature conditions N2 - Understanding on how a machine learning model interprets data is a crucial step to verify its reliability and avoid overfitting. While the focus of the scientific community is nowadays orientated towards deep learning approaches, which are considered as black box approaches, this work presents a toolbox that is based on complementary methods of feature extraction and selection, where the classification decisions of the model are transparent and can be physically interpreted. On the example of guided wave benchmark data from the open guided waves platform, where delamination defects were simulated at multiple positions on a carbon fiber reinforced plastic plate under varying temperature conditions, the authors could identify suitable frequencies for further investigations and experiments. Furthermore, the authors presented a realistic validation scenario which ensures that the machine learning model learns global damage characteristics rather than position specific characteristics. T2 - 48th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Online meeting DA - 28.07.2021 KW - Explainable machine learning KW - Guided waves KW - Damage detection KW - Structural health monitoring KW - Composite structures PY - 2021 SN - 978-0-7918-8552-9 DO - https://doi.org/10.1115/QNDE2021-75215 SP - 1 EP - 6 PB - American Society of Mechanical Engineers (ASME) CY - New York, NY AN - OPUS4-54219 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Tchipilov, Teodor A1 - Raysyan, Anna A1 - Weller, Michael G. T1 - Methods for the quantification of particle-bound protein – Application to reagents for lateral-flow immunoassays (LFIA) N2 - Protein immobilization for the functionalization of particles is used in various applications, including biosensors, lateral-flow immunoassays (LFIA), bead-based assays, and others. Common methods for the quantification of bound protein are measuring protein in the supernatant before and after coating and calculating the difference. This popular approach has the potential for a significant overestimation of the amount of immobilized protein since layers not directly bound to the surface (soft protein corona) are usually lost during washing and handling. Only the layer directly bound to the surface (hard corona) can be used in subsequent assays. A simplified amino acid analysis method based on acidic hydrolysis and RP-HPLC-FLD of tyrosine and phenylalanine (aromatic amino acid analysis, AAAA) is proposed to directly quantify protein bound to the surface of gold nano- and latex microparticles. The results are compared with indirect methods such as colorimetric protein assays, such as Bradford, bicinchoninic acid (BCA), as well as AAAA of the supernatant. For both particle types, these indirect quantification techniques show a protein overestimation of up to 1700% compared to the direct AAAA measurements. In addition, protein coating on latex particles was performed both passively through adsorption and covalently through EDC/sulfo-NHS chemistry. Our results showed no difference between the immobilization methodologies. This finding suggests that usual protein determination methods are no unambiguous proof of a covalent conjugation on particles or beads. KW - Soft protein corona KW - Hard protein corona KW - Gold particles KW - Nanoparticles KW - Mikroparticles KW - Antibody KW - Bioconjugation KW - Protein quantification KW - Supernatant KW - Sodium chloride method KW - Covalent conjugation KW - Latex particles KW - Lateral flow immunoassays PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545365 DO - https://doi.org/10.20944/preprints202203.0332.v1 SP - 1 EP - 8 PB - MDPI CY - Basel AN - OPUS4-54536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mundry, Eberhard T1 - Vortragstagung "Zerstörungsfreie Materialprüfung" vom 28. bis 30. Mai 1962 in Garmisch-Partenkirchen N2 - Die „Gesellschaft zur Förderung Zerstörungsfreier Prüfverfahren e. V.“ und der „Unterausschuß für Zerstörungsfreie Prüfung des Werkstoffausschusses beim Verein Deutscher Eisenhüttenleute“ hatten mit Garmisch-Partenkirchen als Ort für ihre Jahrestagung eine gute Wahl getroffen. Die Aula des Gymnasiums gab den Vorträgen einen Rahmen passender Größe, und Gelegenheiten zum geselligen Beisammensein waren reichlich vorhanden; vor allem die Erinnerung an den gemeinsamen Abend im „Bauerntheater“ wird den meisten Tagungsteilnehmern noch manches Schmunzeln entlocken. Das Vortragsprogramm enthielt in gut ausgewogener Zusammenstellung Beiträge über Grundlagen und Anwendungen verschiedener Prüfmethoden sowie Erfahrungsberichte. Daß es in mehreren Vorträgen um die Gewinnung objektiver Maßstäbe bei der Deutung von Prüfergebnissen ging, ist besonders hervorzuheben. Leider waren erst die Exkursionen am 30. 5. nach München zur Fa. Kraus-Maffei (die Reaktorbesichtigung war kurzfristig von Garching aus abgesagt worden) und zum Walchensee-Kraftwerk mit einem Umweg über den Sylvensteinspeicher vom Wetter nicht begünstigt. Vor allem den Damen hätte man für ihr an sich sehr reizvolles Programm wenigstens etwas mehr Wärme und Sonne gewünscht. Den Organisatoren dieser Tagung gebührt volle Anerkennung für das gelungene Programm. Den vielen Regen und die nötig gewordene Änderung der Exkursionen kann man ihnen nicht zum Vorwurf machen. T2 - Vortragstagung "Zerstörungsfreie Materialprüfung" CY - Garmisch-Partenkirchen, Germany DA - 28.05.1962 PY - 1962 SN - 0025-5300 VL - 4 IS - 7 SP - 339 EP - 343 PB - Hanser CY - München AN - OPUS4-54550 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Herrmann, Stefan T1 - Charakterisierung zweier monoklonaler Antikörper zur Detektion von Sprengstoffen N2 - In 2019 over 30 000 people were killed or injured by explosions caused by explosives like TNT, PETN, HMX and RDX. Therefore, highly sensitive assays for the detection of TNT are needed. In this study we compared two commercially available TNT antibodies: A1.1.1 and EW75C with a highly optimized indirect competitive ELISA based on a BSA-TNA conjugate. As a result, a precision profile for both antibodies was determined with a LOD of 170 pmol L-1 for the clone A1.1.1 and a LOD of 3,2 nmol L-1 for the clone EW75C. The measurements showed that the clone A1.1.1 is a highly sensitive antibody for the detection of TNT while the clone EW75C does show medium performance at most. In the cross-reactivity characterization of both antibodies many substances, closely related to the structure of TNT were tested. Both antibodies showed strong cross reactivity with trinitroaniline and trinitrobenzene. For the clone A1.1.1, which is known to originate from immunization of mice with an TNP-glycine-KLH conjugate, this has to be expected. Interestingly the clone EW75C, which was not characterized yet, showed similar behavior. This suggests a TNA-conjugate as immunogen for the EW75C antibody as well. None of both antibodies showed cross-reactions to the high explosives PETN, HMX and RDX. Also, the cross-reactions of nitro musks with the antibodies were investigated. Despite their prohibition, nitro musks are still used in Asia especially and are particularly popular in India. The overall superior clone A1.1.1 showed a significant cross-reactivity to musk ambrette. For practical reasons the influence of musk ambrette on this assay when used in natural environment should be investigated. In further experiments, the highly sensitive TNT antibody A1.1.1 was digested with papain to obtain monovalent Fab-fragments. Due to its high stability against the digestion, a custom protocol for the IgG1 subclass of mice, to which the clone A1.1.1 belongs, was developed, resulting in a quantitative digestion of the intact antibody to Fab fragments. The success of the digestion was determined with MALDI-TOF-MS and SDS-PAGE. It was shown that this protocol worked for many different antibodies of IgG1 subclass as well. KW - TNT KW - Trinitrotoluol KW - Nitroaromaten KW - Nitromoschus KW - Duftstoffe KW - ELISA KW - Immunoassay KW - Antibody KW - Explosives KW - Klon A1.1.1 KW - Klon EW75C KW - Fab Fragment KW - Kreuzreaktion KW - Crossreactivity KW - Precision Profile KW - Präzisionsprofil KW - Affinity KW - Affinitätskonstante KW - IC50 PY - 2020 SP - 1 EP - 113 PB - Hochschule für Technik und Wirtschaft Berlin - htw CY - Berlin AN - OPUS4-54556 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Wortmann, U. G. A1 - Vogl, Jochen A1 - Schmid, Thomas T1 - Beautiful Pietàs in South Tyrol (Northern Italy): local or imported works of art? N2 - The study, dedicated to Beautiful Pietàs conserved in South Tyrol (Northern Italy), aims to establish, for the first time, a connection between Austroalpine raw materials and the high-fired gypsum mortars constituting the Gothic figure groups in question. The origin and chronology of this stylistically and qualitatively differing ensemble have been subject of art historical debate for nearly a century. The discourse is dominated by three main hypotheses: itinerary of an Austrian artist versus itinerary of the work of art created in an artist’s workshop in Austria versus itinerary of the stylistic vocabulary via graphical or three-dimensional models. The comparison of the δ34S values and the 87Sr/86Sr ratios of the gypsum mortars and Austroalpine sulphate deposits (in a compilation of own reference samples and literature data) points to the exploitation of sediments in the Salzkammergut and possibly also in the evaporite district of the Eastern Calcareous Alps, thus evidencing the import of the sculptures and not the activities of local South Tyrolean or itinerant artists. Two geochronological units are distinguishable: The Pietà in the Church St. Martin in Göflan can be assigned to Upper Permian raw material, whereas the metrologically consistent sculptures in the Church of Our Lady of the Benedictine Abbey Marienberg and in the Chapel St. Ann in Mölten correlate with deposits of the Early Triassic (or the Lower-Middle Triassic transition). The medieval gypsum mortars also differ in their mineralogical characteristics, i.e. in their geologically related minor components, as in the first case, characterised by a significant proportion of primary anhydrite, natural carbonate impurities mainly consist of calcite (partly converted to lime-lump-like aggregates), whereas in the second group dolomite (or rather its hydration products after pyrometamorphic decomposition) predominates, accompanied by celestine, quartz and potassium feldspar. The Pietà in the Cathedral Maria Himmelfahrt in Bozen turned out to be made of Breitenbrunn calcareous sandstone (Leitha Mountains, Burgenland, Austria), which is why the sample is not considered in the geochemical analysis. KW - High-fired gypsum mortar KW - Sulphur isotope KW - Strontium isotope KW - Polarised light microscopy KW - Raman microspectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545610 DO - https://doi.org/10.1186/s40494-022-00678-6 SN - 2050-7445 VL - 10 IS - 1 SP - 1 EP - 17 PB - Springer Nature AN - OPUS4-54561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Coupling of chromatographic and spectrometric techniques for polymer characterization N2 - Coupling of chromatographic and spectrometric techniques for polymer characterization; focus topics: LCxMALDI-TOF-MS and UPLC x ESI-TOF-MS T2 - 16. Tagung des Arbeitskreises Polymeranalytik CY - Online meeting DA - 22.03.2022 KW - Liquid chromatography KW - Mass spectrometry KW - Polymers KW - Two-dimensional chromatography (2D-LC) PY - 2022 AN - OPUS4-54567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hartfiel, Reni T1 - Zweistufiges Screening von One-Bead-One-Peptide-Bibliotheken linearer & cyclischer Peptide gegen Pflanzenviren N2 - In der Masterarbeit wurde ein Screening gegen den CCMV mit einer linearen Peptidbibliothek entwickelt, wobei zwei lineare Binder identifiziert wurden. Das resynthetisierte Peptid wurde auf seine Bindungseigenschaften mittels ELISA und MST untersucht. Aufgrund eines Aminosäurefehlers in der selbst durchgeführten Resynthese des Peptids sind die Ergebnisse nicht vollständig übertragbar. Um eine umsetzbare Cyclusgröße für die Peptidbibliothek zu finden, wurden Ringgrößen mit sechs bis acht Aminosäuren untersucht. Da keiner der gewählten Ringgrößen bevorzugt war, wurde die Ringgröße aus acht Aminosäuren für die Peptidbibliothek gewählt. Der Ringschluss wurde durch die Bildung einer Disulfidbrücke erreicht. Dadurch war die Alkylierung der vorhandenen Thiolgruppe in den Abbruchsequenzen notwendig. Neben den etablierten Alkylierungsreagenzien Iodessigsäure, Iodacetamid und Acrylamid wurden zwei Epoxide mituntersucht. Hierbei konnte nur bei Acrylamid und Propylenoxid eine vollständige Alkylierung beobachtet werden. Eine synthetische Peptidbibliothek aus zehn Aminosäuren pro Kopplungsschritt und einer Peptidlänge von acht Aminosäuren wurde erfolgreich nach der Split-and-Mix-Synthese hergestellt. Neben den kanonischen Aminosäuren wurde die synthetische Aminosäure 3-(3-Pyridyl)-alanin in die Peptidbibliothek mit eingebaut. Peptidsequenzen aus der cyclische Peptidbibliothek konnte mittels MALDI-TOF-MS identifiziert werden. Es konnte außerdem gezeigt werden, dass synthetische Aminosäuren mit proteinogenen Aminosäuren erfolgreich übersetzt werden. Anschließend wurde das entwickelte Screening auf eine cyclische Peptidbibliothek übertragen. Dabei konnte kein Binder identifiziert werden, da zu viele Nebenreaktionen auftraten. Ein alternativer Ringschluss über die Seitenketten von Lysin und Cystein wurden mit ortho-Phthaldialdehyd und 2,4,6-Trichloro-1,3,5-triazin (Cyanurchlorid) untersucht. Beide Bedingungen wiesen keinen erfolgreichen Ringschluss auf. Obwohl der Ringschluss über die Seitenketten von Lysin und Cystein nicht erfolgreich war, sollte ein Austausch von Cystein angestrebt werden, so dass kein freies Cystein in den Abbruchsequenzen vorhanden ist und die Alkylierung überflüssig wäre. Der Ringschluss durch Verwendung anderer Seitenketten bietet einen vielseitigen Ansatz. KW - CCMV KW - Pflanzenvirus KW - Peptidbibliothek KW - Peptid-Aptamer KW - Alkylierung KW - Cyclisierung KW - MALDI-TOF-MS KW - Fluoreszenz KW - Chip KW - Sequenzierung KW - Peptid-Synthese PY - 2022 SP - 1 EP - 81 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54501 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kudela, P. A1 - Radzienski, M. A1 - Moix-Bonet, M. A1 - Willberg, C. A1 - Lugovtsova, Yevgeniya A1 - Bulling, Jannis A1 - Tschöke, K. A1 - Moll, J. T1 - Dataset on full ultrasonic guided wavefield measurements of a CFRP plate with fully bonded and partially debonded omega stringer N2 - The fourth dataset dedicated to the Open Guided Waves platform presented in this work aims at a carbon fiber composite plate with an additional omega stringer at constant temperature conditions. The dataset provides full ultrasonic guided wavefields. A chirp signal in the frequency range 20-500 kHz and Hann windowed tone-burst signal with 5 cycles and carrier frequencies of 16.5 kHz, 50 kHz, 100 kHz, 200 kHz and 300kHz are used to excite the wave. The piezoceramic actuator used for this purpose is attached to the center of the stringer side surface of the core plate. Three scenarios are provided with this setup: (1) wavefield measurements without damage, (2) wavefield measurements with a local stringer debond and (3) wavefield measurements with a large stringer debond. The defects were caused by impacts performed from the backside of the plate. As result, the stringer feet debonds locally which was verified with conventional ultrasound measurements. The dataset can be used for benchmarking purposes of various signal processing methods for damage imaging. The detailed description of the dataset is published in Data in Brief Journal. KW - Open data KW - Ultrasonic guided waves KW - Experimental data PY - 2021 DO - https://doi.org/10.5281/zenodo.5105861 PB - Zenodo CY - Geneva AN - OPUS4-54504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Hirschberger, Paul A1 - Bartholmai, Matthias ED - Holl, H. T1 - Flying ant robot for chemical trail detection and localization N2 - This paper presents first advances in the area of aerial chemical trail following. For that purpose, we equipped a palm-size aerial robot, based on the Crazyflie 2.0 quadrocopter, with a small lightweight metal oxide gas sensor for measuring evaporated ethanol from chemical trails. To detect and localize a 5 cm wide chemical trail, a detection criterion was developed that uses only relative changes in the transient phase of the sensor response. The reduction in signal strength dependence improves the robustness of its application. We tested our setup in first crossing-trail experiments showing that our flying ant robot can correlate an odor hit with the chemical trail within 0.14 m. Principally, this could enable aerial chemical trail following in the future. T2 - 37th Danubia - Adria Symposium on Advances in Experimental Mechanics CY - Linz, Austria DA - 21.09.2021 KW - Aerial robot KW - Trail following KW - Trail detection KW - Localization PY - 2022 DO - https://doi.org/10.1016/j.matpr.2022.02.594 SN - 2214-7853 VL - 62 SP - 2462 EP - 2465 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-54507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kudela, P. A1 - Radzienski, M. A1 - Moix-Bonet, M. A1 - Willberg, C. A1 - Lugovtsova, Yevgeniya A1 - Bulling, Jannis A1 - Tschöke, K. A1 - Moll, J. T1 - Dataset on full ultrasonic guided wavefield measurements of a CFRP plate with fully bonded and partially debonded omega stringer N2 - The fourth dataset dedicated to the Open Guided Waves platform presented in this work aims at a carbon fiber composite plate with an additional omega stringer at constant temperature conditions. The dataset provides full ultrasonic guided wavefields. Two types of signals were used for guided wave excitation, namely chirp signal and tone-burst signal. The chirp signal had a frequency range of 20-500kHz. The tone-burst signals had a form of sine modulated by Hann window with 5 cycles and carrier frequencies 16.5kHz, 50kHz, 100kHz, 200kHz, 300kHz. The piezoceramic actuator used for this purpose was attached to the center of the stringer side surface of the core plate. Three scenarios are provided with this setup: (1) wavefield measurements without damage, (2) wavefield measurements with a local stringer debond and (3) wavefield measurements with a large stringer debond. The defects were caused by impacts performed from the backside of the plate. As result, the stringer feet debonds locally which was verified with conventional ultrasound measurements. KW - Lamb waves KW - Composite panel KW - Impact damage KW - Damage detection KW - Scanning laser Doppler vibrometry KW - Structural health monitoring KW - Non-destructive evaluation KW - Open data PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545242 DO - https://doi.org/10.1016/j.dib.2022.108078 SN - 2352-3409 VL - 42 SP - 1 EP - 13 PB - Elsevier CY - Amsterdam AN - OPUS4-54524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fiedler, Saskia T1 - Cathodoluminescence Spectroscopy of Silicon Nanoparticles N2 - The fabrication of nanostructures with ever-decreasing sizes has increased the demand of suitable characterization methods which allow to determine their shape and size at the true nanoscale, and similarly important, enable the investigation of their optical properties beyond the diffraction limit. Due to its high spectral and spatial resolution down to the (sub-) nanometer range, electron beam-based techniques, namely cathodoluminescence (CL) has become a powerful characterization tool, particularly to study plasmonic and dielectric nanostructures. However, the interpretation of the resulting spectral CL maps is not always unambiguously straightforward. In this work, Mie resonances in single Si nanospheres of different sizes have been systematically studied, using experimental CL spectroscopy and an analytical CL model. For smaller spheres (r ~ 75 nm), the eigenmodes can be unequivocally identified, with relative changes in intensity of the electric and magnetic dipole depending on the electron beam position within the sphere. However, in larger spheres (r ~ 105 nm), the modal assignment becomes increasingly difficult due to a larger number of Mie modes in the visible spectral range. Additionally, penetrating electron beams generate two radiating dipoles at the two Si interfaces – due to the electron and its image charge collapsing at those interfaces – which can, depending on the electron beam’s velocity and its path length inside the particle, produce distinct resonances or dips (constructive or destructive interference of those two radiative dipoles). It is demonstrated that superimposed on the eigenmodes of the studied nanospheres, these resonances can distort the recorded spectrum and lead to potentially erroneous assignment of modal characters to the spectral features. An intuitive analogy is developed to unambiguously distinguish those resonance induced by transition radiation from the nanoparticle-specific Mie resonances. T2 - Optoelectronic Processes at Nanostructured Interfaces 2022 CY - Bad Honnef, Germany DA - 21.03.2022 KW - Cathodoluminescence KW - Silicon nanoparticles KW - Mie resonances PY - 2022 AN - OPUS4-54526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Doolette, A. A1 - Huang, J. T1 - Combining diffusive gradients in thin-films (DGT) and 31P NMR spectroscopy to determine phosphorus species in soil N2 - The diffusive gradients in thin-films (DGT) technique shows in many publications a superior correlation to the amount of plant-available phosphorus (P) in soil. However, this technique cannot give information on the plant-available P species in soil. Therefore, we combined DGT with solution 31P nuclear magnetic resonance (NMR) spectroscopy. This was achieved by using a modified DGT device in which the diffusive layer had a larger pore size, the binding layer incorporated an adsorption material with a higher capacity, and the device had a larger exposure area. The spectroscopic investigation was undertaken after elution of the deployed DGT binding layer in a NaOH solution. Adsorption tests using solutions of known organic P compounds showed that a sufficient amount of these compounds could be adsorbed on the binding layer in order for them to be analyzed by solution 31P NMR spectroscopy. Furthermore, various intermediates of the hydrolysis of trimetaphosphate in soil could be also analyzed over time. KW - Phosphorus KW - Diffusive gradients in thin-films (DGT) KW - Passive sampling KW - fertilizer PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545759 DO - https://doi.org/10.1002/ael2.20068 VL - 7 IS - 1 SP - e20068 PB - Wiley online library AN - OPUS4-54575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling Equilibrium Chemistry in Laser Induced Plasmas and Plasma Chemical Reactors N2 - A brief introduction will be given on modeling chemical reactions in laser induced plasmas using stoichiometric and non-stoichiometric approaches. Several applications will be considered, which can benefit from such modeling. Those include plasma enhanced chemical vapor deposition (PECVD), surface modification and surface coating, and molecular analysis by LIBS. Each application will be illustrated by simulations of relevant chemical systems. For PECVD, chemical systems are BCl3/H2/Ar, BF3/H2/Ar, BCl3/BF3, Mo/BF3/H2; for surface modification/coating it is Ti/air; for molecular LIBS they are CaCO3/Ar, Ca(OH)2/Ar, and CaCl2/Ar. Advantages and shortcomings of equilibrium chemical hydrodynamic models of laser induced plasmas will be discussed. T2 - 1st NIP Conference National Institute of Physics (IKF), the Albanian Academy of Sciences CY - Online meeting DA - 10.02.2022 KW - Laser ablation KW - Laser induced plasma deposition KW - Surface coating KW - Titanium dioxide KW - Emission spectroscopy KW - Hydrodynamic model KW - Plasma chemistry PY - 2022 AN - OPUS4-54328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Plasma Fundamentals and Diagnostics N2 - This course will provide an introduction to plasma diagnostic techniques. The major focus of the course will be on the discussions of the practical procedures as well as the underlying physical principles for the measurements of plasma fundamental characteristics (e.g., temperatures and electron number density). Particular emphasis will be placed on laser induced plasma–atomic emission spectrometry, but other analytical plasmas will also be used as examples when appropriate. Selected examples on how one can manipulate the operating conditions of the plasma source, based on the results of plasma diagnostic measurements, to improve its performance used for spectrochemical analysis will also be covered. Topics to be covered include thermal equilibrium, line profiles, temperatures, electron densities, excitation processes, temporal and spatial resolution. T2 - 2022 Winter Conference on Plasma Spectrochemistry CY - Tucson, Arizona, USA DA - 17.01.2022 KW - Thermal equilibrium KW - Excitation processes KW - Electron number density KW - Temperatures KW - Spatial information KW - Emission line profiles PY - 2022 AN - OPUS4-54288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tang, Chi-Long A1 - Wilke, Olaf A1 - Seeger, Stefan A1 - Kalus, Sabine A1 - Erdmann, Kerstin T1 - Chemical characterization of ultrafine particles released from 3D printers N2 - Previous studies have shown that desktop 3D printers (Fused Filament Fabrication) emit high numbers of particulate matter, mainly as ultrafine particles (UFP, particle diameter less than 100 nm). However, the chemical composition of emitted particles has been less extensively investigated. In this study, we therefore focused on the chemical composition of particles emitted from 3D printing. The measurements were conducted in a 1 m³ emission test chamber. Emitted particles were sampled by a 13-stage low-pressure cascade impactor onto aluminum foils and then analyzed by TD-GC/MS to identify their organic compounds. Nine commercial filaments made from basic polymers such as Acrylonitrile Butadiene Styrene (ABS), Acrylonitrile Styrene Acrylate (ASA), Polycarbonate (PC), Poly(methyl methacrylate) (PMMA), Nylon, High Performance Polystyrene (HIPS) and a copper-filled Polylactide (PLA) were investigated. The results show that the organic components of the particles are primarily plastic additives such as plasticizer, antioxidant agents, lubricants, UV-absorbers and UV-stabilizers from the filaments. T2 - 17th International Conference Healthy Buildings Europe 2021 CY - Online Meeting DA - 21.06.2021 KW - Chemical characterization KW - FFF-3D-Printer KW - UFP KW - Chamber measurement PY - 2021 SP - 251 EP - 252 AN - OPUS4-54255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Held, Mathias T1 - Inverse determination of elastic material parameters from the propagation behavior of ultrasonic waves using convolutional neuronal networks N2 - Um aus messtechnisch ermittelten Dispersionsabbildungen geführter Ultraschallwellen Rückschlüsse auf die Materialparameter zu ziehen, werden in der aktuellen Forschung verschiedene inverse Methoden diskutiert. Maschinelles Lernen und insbesondere Convolutional-Neural-Networks (CNNs) stellen eine Möglichkeit der automatisierten inversen Modellierung und Evaluierung von Bilddaten dar. In diesem Vortrag wird anhand synthetischer Daten gezeigt, wie das Ausbreitungsverhalten von geführten Ultraschallwellen unter Verwendung von CNNs genutzt werden kann, um die isotropen elastischen Konstanten einer plattenförmigen Struktur zu bestimmen. T2 - Doktorandentreffen 2021 CY - Petershagen/Eggersdorf, Germany DA - 25.10.2021 KW - Convolutional Neuronal Networks KW - Inverse Probleme KW - Materialcharakterisierung KW - Maschine learning KW - Guided waves KW - Lamb Wellen PY - 2021 AN - OPUS4-54264 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Casali, C. A1 - Feiler, Torvid A1 - Heilmann, Maria A1 - Braga, D. A1 - Emmerling, Franziska A1 - Grepioni, F. T1 - Too much water? Not enough? In situ monitoring of the mechanochemical reaction of copper salts with dicyandiamide N2 - n situ monitoring of mechanochemical reactions between dicyandiamide (DCD) and CuX2 salts (X = Cl−, NO3−), for the preparation of compounds of agrochemical interest, showed the appearance of a number of phases. It is demonstrated that milling conditions, such as the amount of water added in wet grinding and/or the milling frequency, may affect the course of the mechanochemical reactions, and drive the reaction towards the formation of different products. It has been possible to discover by in situ monitored experiments two novel crystalline forms, namely the neutral complexes [Cu(DCD)2(OH2)2(NO3)2] (2) and [Cu(DCD)2(OH2)Cl2]·H2O (4), in addition to the previously known molecular salt [Cu(DCD)2(OH2)2][NO3]2·2H2O (1, DIVWAG) and neutral complex [Cu(DCD)2(OH2)Cl2] (3, AQCYCU), for which no synthesis conditions were available. Compounds 2 and 4 were fully characterized via a combination of solid-state techniques, including X-ray diffraction, Raman spectroscopy and TGA. KW - Mechanochemistry KW - In situ PY - 2022 DO - https://doi.org/10.1039/d1ce01670a VL - 24 IS - 6 SP - 1292 EP - 1298 PB - RSC AN - OPUS4-54344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - von der Au, Marcus A1 - Wittwer, Phillip A1 - Roesch, Philipp A1 - Pfeifer, Jens A1 - Cossmer, Antje A1 - Meermann, Björn T1 - A fast and simple PFAS extraction method utilizing HR–CS–GFMAS for soil samples N2 - Here, we describe an optimized fast and simple extraction method for the determination of per- and polyfluorinated alkyl substances (PFASs) in soils utilizing high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR–CS–GFMAS). To omit the bias of the solid phase extraction (SPE) step commonly used during the analysis of extractable organically bound fluorine (EOF) we optimized a fast and simple SPE-free extraction method. The developed extraction method consists of a liquid-solid extraction using acidified methanol without any additional SPE. Four extraction steps were representative to determine a high proportion of the EOF (>80% of eight extractions). Comparison of the optimized method with and without an additional SPE clean-up step revealed a drastic underestimation of EOF concentrations using SPE. Differences of up to 94% were observed which were not explainable by coextracted inorganic fluoride. Therefore, not only a more accurate but also a more economic as well as ecologic method (bypassing of unnecessary SPE) was developed. The procedural limit of quantification (LOQ) of the developed method was 10.30 μg/kg which was sufficient for quantifying EOF concentrations in all tested samples. For future PFAS monitoring and potential regulative decisions the herein presented optimized extraction method can offer a valuable contribution. KW - Per- and polyfluorinated alkly substances (PFASs) KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Soils KW - Solid phase extraction (SPE) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction PY - 2022 DO - https://doi.org/10.1016/j.chemosphere.2022.133922 VL - 295 SP - 1 EP - 9 PB - Elsevier Ltd. AN - OPUS4-54359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gojani, Ardian T1 - Motion of an ensemble of magnetic microbeads in a microfluidic system N2 - This study describes the motion of magnetizable particles of spherical shape with radius at most of 1 μm, also referred to as microbeads, immersed in a liquid under laminar flow conditions in a microfluidic channel. An external magnetic field is applied in part of the system such that it permeates the channel and is characterized by a spatially varying magnetic field, i.e., the gradient of the magnetic field is nonzero. The beads are superparamagnetic; hence they can reach high level of magnetization in the presence of a magnetic field, and this magnetization disappears when the field is zero. Therein lies the attractiveness of these microbeads and the potential for applications because their motion can be controlled using an external magnetic field. The motion is governed by several factors, including the magnetic force acting on microbeads (particles), the drag force due to viscosity, the interaction between particles and the fluid, as well as the interaction between particles themselves. For a single particle case, the trajectory of the motion is determined by balancing the drag and magnetic forces acting on the particle, a calculation that in general requires numerical integration. For a system consisting of an ensemble of interacting particles, several regimes of motion dominated by one of the factors are identified. Of particular interest are the systems dominated by the large number of particles in the ensemble, i.e., high particle concentration, in which cases the wake influences the flow downstream. This effect is qualitatively investigated by considering the Navier-Stokes equation with and without the magnetic force contribution. T2 - 1st NIP Conference National Institute of Physics (IKF), the Albanian Academy of Sciences CY - Tirana, Albania DA - 10.02.2022 KW - MamaLoCA KW - Microfluidics KW - Magnetophoresis PY - 2022 AN - OPUS4-54366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frisch, M. A1 - Raza, M. H. A1 - Ye, M.-Y. A1 - Sachse, René A1 - Paul, B. A1 - Gunder, R. A1 - Pinna, N. A1 - Kraehnert, R. T1 - ALD-coated mesoporous iridium-titanium mixed oxides: Maximizing iridium utilization for an outstanding OER performance N2 - With the increasing production of renewable energy and concomitant depletion of fossil resources, the demand for efficient water splitting electrocatalysts continues to grow. Iridium (Ir) and iridium oxides (IrOₓ) are currently the most promising candidates for an efficient oxygen evolution reaction (OER) in acidic medium, which remains the bottleneck in water electrolysis. Yet, the extremely high costs for Ir hamper a widespread production of hydrogen (H₂) on an industrial scale. Herein, the authors report a concept for the synthesis of electrode coatings with template-controlled mesoporosity surface-modified with highly active Ir species. The improved utilization of noble metal species relies on the synthesis of soft-templated metal oxide supports and a subsequent shape-conformal deposition of Ir species via atomic layer deposition (ALD) at two different reaction temperatures. The study reveals that a minimum Ir content in the mesoporous titania-based support is mandatory to provide a sufficient electrical bulk conductivity. After ALD, a significantly enhanced OER activity results in dependency of the ALD cycle number and temperature. The most active developed electrocatalyst film achieves an outstanding mass-specific activity of 2622 mA mg(Ir)⁻¹ at 1.60 V(RHE) in a rotating-disc electrode (RDE) setup at 25 °C using 0.5 m H₂SO₄ as a supporting electrolyte. KW - Acidic oxygen evolution reaction KW - Atomic layer deposition KW - Electrocatalysis KW - Iridium oxide KW - Soft-templated mesoporous films PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542651 DO - https://doi.org/10.1002/admi.202102035 SN - 2196-7350 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eisentraut, Paul A1 - Altmann, Korinna T1 - Repräsentative Mikroplastik-Detektion in Umweltproben - Weiterentwicklung der TED-GC/MS N2 - Die große Herausforderung in der Detektion von Mikroplastik (MP)‑Partikeln (1-1000 µm) besteht darin, sie neben Millionen von natürlichen Partikeln in Umweltproben nachzuweisen. Zum Aufspüren von Senken, Eintragspfaden und für Monitoring-Kampagnen ist ein schnelles, automatisiertes Verfahren unerlässlich. Ein solches Verfahren wurde an der Bundesanstalt für Materialforschung und -prüfung (BAM) mit der ThermoExtraktion/Desorption-Gaschromatographie-Massenspektrometrie (TED-GC/MS) in den letzten Jahren entwickelt. KW - Mikroplastik KW - TED-GC/MS PY - 2021 UR - https://analyticalscience.wiley.com/do/10.1002/was.0004000195 SN - 0016-3538 SP - 2 EP - 5 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54266 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Marklein, B. A1 - Jenning, M. A1 - Konthur, Zoltán A1 - Häupl, T. A1 - Welzel, F. A1 - Nonhoff, U. A1 - Krobitsch, S. A1 - Mulder, D. M. A1 - Koenders, M. I. A1 - Joshua, V. A1 - Cope, A. P. A1 - Shlomchik, M. J. A1 - Anders, H.‑J. A1 - Burmester, G. R. A1 - Hensvold, A. A1 - Catrina, A. I. A1 - Rönnelid, J. A1 - Steiner, G. A1 - Skriner, K. T1 - Correction to: The citrullinated/native index of autoantibodies against hnRNP-DL predicts an individual "window of treatment success" in RA patients N2 - This is a corrigendum to the original article 'The citrullinated/native index of autoantibodies against hnRNP-DL predicts an individual "window of treatment success" in RA patients' that was published in the journal "Arthritis research & therapy", vol. 23 (2021), article no. 239. PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542698 DO - https://doi.org/10.1186/s13075-021-02639-z SN - 1478-6362 VL - 23 SP - 1 EP - 2 PB - BioMed Central CY - London AN - OPUS4-54269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Charakterisierung und Verifizierung der Ultraschall-Prüfausrüstung - Die Normenreihe DIN EN ISO 22232 ersetzt die DIN EN 12668 seit September 2021 N2 - Durch die Internationalisierung in der Standardisierung wurden die Regelwerke zur „Charakterisierung und Verifizierung der Ultraschall-Prüfausrüstung“, die bisher als europäische Regelwerke der DIN EN 12668 Reihe eingeordnet waren, überarbeitet und in internationale Regelwerke überführt. Die Regelwerke sind seit September 2021 als deutsche Übersetzung eingeführt als DIN EN ISO 22232 und ersetzen somit in Deutschland die bisher geltenden Regelwerke der DIN EN 12668 Reihe. Die drei Teile der Reihe beschäftigen sich in Teil 1 mit den Prüfgeräten, in Teil 2 mit den Prüfköpfen und in Teil 3 mit der Prüfausrüstung, die aus Prüfgerät, Prüfkopf und Kabel besteht. In dem Vortrag möchten wir neben dem historischen Werdegang darlegen, welche Gemeinsamkeiten und Unterschiede die Regelwerke aufweisen und worauf bei der Umstellung zu achten ist. T2 - Arbeitskreis Berlin der DGZfP – 431. Sitzung CY - Online meeting DA - 9.11.2021 KW - Ultraschall KW - Zerstörungsfreie Prüfung KW - Standardisierung KW - Gerätetechnik PY - 2021 AN - OPUS4-54308 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hassenstein, Christian T1 - Adaptive TFM approach for turbine blade testing in an NDE 4.0 environment N2 - Turbine blades for gas turbines are exposed to extreme working conditions in a demanding environment. In-service inspection, maintenance and refurbishment of the heavily stressed parts is necessary to ensure both safety and efficiency, e.g. based on immersion ultrasound testing (UT). In the course of NDE 4.0, the European project MRO 2.0 aims to innovate the maintenance, repair and overhaul of turbine blades by linking these with modern digital methods. For this, the goal of this project is to go beyond conventional automated and manual UT testing techniques. The aim is to measure the actual geometry and wall thickness of the complex shaped parts by applying an adaptive TFM that takes into account the refraction of the ultrasonic waves at the transition from the coupling material (water) to the inspected part (steel). In this setup the phased array probe is held by a robotic arm that allows the part to be scanned while remaining mainly perpendicular to the inspected surface. In this way, even complex geometries can be inspected and a 3D model of the actual condition of the part can be created. The laboratory setup is equipped with a Vantage 64 phased array instrument from Verasonics Inc. and an industrial robot from ABB. A 64 element linear array probe operating at 10 MHz is attached to the robot. The focus is on optimizing resolution, reliability and inspection speed, as the reconstructed model will be fed to the digital twin at a later stage of the project and used for targeted repairs. In addition to enhancing the reconstruction algorithms, required probe geometry and the parameters needed to inspect turbine blades with partially thin walls and anisotropic materials will also be investigated. This talk will describe the 3-year project and present the results of the first year. The main focus will be on the development of the reconstruction algorithms used and the experimental setup. T2 - 48th Annual Review of Progress in Quantitative Nondestructive Evaluation (QNDE 2021) CY - Online meeting DA - 28.07.2021 KW - Utrasound testing KW - Turbine blade KW - Maintenance KW - Phased array KW - Automation PY - 2021 AN - OPUS4-54313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Deposition of Titanium Oxides by Nanosecond Laser Ablation: Simulation and Experiment N2 - Surface modification of titanium by laser ablation is investigated theoretically and experimentally. The modification consists in texturing the surface and redeposition of chemically transformed material from the ablation plasma. The redeposition is driven by the hydrodynamic flow in the plasma. Such surface modification improves the biocompatibility of titanium implants. T2 - 2022 Winter Conference on Plasma Spectrochemistry CY - Tucson, Arizona, USA DA - 17.01.2022 KW - Laser ablation KW - Laser induced plasma deposition KW - Surface coating KW - Titanium dioxide KW - Emission spectroscopy KW - Hydrodynamic model KW - Plasma chemistry PY - 2022 AN - OPUS4-54289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kornev, R. A. A1 - Sennikov, P. G. A1 - Gornushkin, Igor B. A1 - Ermakov, A. A. A1 - Shkrunin, V. E. A1 - Polykov, V. S. A1 - Kornev, A. R. A1 - Kornev, K. D. T1 - Laser induced dielectric breakdown as a novel method for the synthesis of molybdenum boride N2 - Laser induced dielectric breakdown (LIDB) on a surface of solid Mo in H2/BF3 atmosphere at 30-760 Torr and in a gaseous mixture MoF6/H2/BF3 + at 760 Torr pressure is tested for synthesis and deposition of superhard molybdenum borides that are needed in many areas of industry and technology. The emission spectra of the plasma and the dynamics of the gas discharge near the substrate are investigated. A comparative analysis of the gas mixture before and after exposure to LIDB plasma is carried out using IR spectroscopy. The conditions for the formation of molybdenum borides are determined. A thermodynamic analysis of the MoF6/H2/BF3 and Mo/H2/BF3 systems is carried out to determine the temperature range for the formation of molybdenum borides and establish the main chemical reactions responsible for their formation. Deposits containing MoB and MoB2 phases are obtained. For the mixture MoF6/H2/BF3, the deposit exhibits an amorphous layered structure, which contains 19.15 wt% F, 30.45% O, and 0.8% Si. For the Mo/H2/BF3 system at the pressures 30 and 160 Torr, nanopowder of molybdenum boride is produced with a characteristic grain size of 100 nm. At pressures above 160 Torr, Mo nanopowder with a grain size <30 nm is obtained. KW - LIDB plasma KW - MoF6 KW - BF3 KW - Hydrogen reduction KW - Molybdenum boride PY - 2022 DO - https://doi.org/10.1007/s11090-021-10224-0 SN - 1572-8986 SP - 1 EP - 18 PB - Springer CY - Dordrecht AN - OPUS4-54290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical processes N2 - Overview of the present BAM activities in the field of in situ analytics of mechanochemical processes. Recent results for the synthesis of metal organic frameworks and cocrystals are presented. T2 - HZB Seminar CY - Online meeting DA - 21.01.2022 KW - Mechanochemistry KW - In situ real-time monitoring PY - 2022 AN - OPUS4-54296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hicke, Konstantin T1 - Monitoring von Strukturverhalten mittels integrierter verteilter faseroptischer Sensorik - Verteilte akustische Sensorik (DAS) N2 - Die verteilte faseroptische akustische Sensorik (DAS) wird vorgestellt, hinsichtlich ihrer Leistungsfähigkeit beschrieben und verschiedenste Anwendungsfelder, z.B. für das Zustandsmonitoring oder für seismische Messungen, beispielhaft gezeigt. Zudem werden mögliche Anwendungsfelder von DAS für den Kontext Kerntechnische Entsorgung (KTE) und Rückbau aufgezeigt. T2 - Online-Workshop „Dauerhafte Verschlussbauwerke für Endlager“ CY - Online meeting DA - 14.02.2022 KW - Verteilte faseroptische Sensorik KW - Verteilte akustische Sensorik KW - DAS KW - KTE KW - Monitoring Endlager PY - 2022 AN - OPUS4-54348 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kruschwitz, Sabine A1 - Oesch, T. A1 - Mielentz, Frank A1 - Meinel, Dietmar A1 - Spyridis, P. T1 - Non-Destructive Multi-Method Assessment of Steel Fiber Orientation in Concrete N2 - Integration of fiber reinforcement in high-performance cementitious materials has become widely applied in many fields of construction. One of the most investigated advantages of steel Fiber reinforced concrete (SFRC) is the deceleration of crack growth and hence its improved sustainability. Additional benefits are associated with its structural properties, as fibers can significantly increase the ductility and the tensile strength of concrete. In some applications it is even possible to entirely replace the conventional reinforcement, leading to significant logistical and environmental benefits. Fiber reinforcement can, however, have critical disadvantages and even hinder the Performance of concrete, since it can induce an anisotropic material behavior of the mixture if the fibers are not appropriately oriented. For a safe use of SFRC in the future, reliable non-destructive testing (NDT) methods need to be identified to assess the fibers’ orientation in hardened concrete. In this study, ultrasonic material testing, electrical impedance testing, and X-ray computed tomography have been investigated for this purpose using specially produced samples with biased or random Fiber orientations. We demonstrate the capabilities of each of these NDT techniques for fiber orientation measurements and draw conclusions based on these results about the most promising areas for future research and development. KW - Spectral induced polarization KW - Steel fiber reiniforced concrete KW - Fiber orientation KW - Non-destructive testing KW - Micro-computed tomography KW - Ultrasound PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543520 DO - https://doi.org/10.3390/app12020697 VL - 12 IS - 2 SP - 1 EP - 14 PB - MDPI CY - Basel Switzerland AN - OPUS4-54352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lakshmipathi, M. A1 - Tothadi, S. A1 - Emmerling, Franziska A1 - Bhattacharya, Biswajit A1 - Ghosh, S. T1 - Different mechanical responses of dimorphic forms of Anthracene Schiffbase crystal N2 - We obtained concomitant dimorphic forms of Anthracene Schiffbase (N-(anthracen-9-yl methylene)-2,5- dichloroaniline) from hexane solvent. Two polymorphs can be differentiated by their morphology and mechanical properties. One form is long acicular type and elastically bendable while another form is block shaped and brittle in nature. Mechanical property is attributed to underlying crystal packing. Hirsh- feld analysis and energy framework calculations were done to corroborate structure-property correlation of two forms. KW - Elasticity KW - Mechanical properties KW - Anthracene schiff base KW - Dimorphs PY - 2021 DO - https://doi.org/10.1016/j.molstruc.2021.132182 VL - 1252 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-54356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, P. M. A1 - Kjærvik, Marit A1 - Willneff, E. A. A1 - Unger, Wolfgang T1 - In-depth analysis of iodine in artificial biofilm model layers by variable excitation energy XPS and argon gas cluster ion sputtering XPS N2 - Here, we present a study on agarose thin-film samples that represent a model system for the exopolysaccharide matrix of biofilms. Povidone-iodide (PVP-I) was selected as an antibacterial agent to evaluate our x-ray photoelectron spectroscopy (XPS)-based methodology to trace specific marker elements, here iodine, commonly found in organic matrices of antibiotics. The in-depth distribution of iodine was determined by XPS analyses with variable excitation energies and in combination with argon gas cluster ion beam sputter cycles. On mixed agarose/PVP-I nanometer-thin films, both methods were found to solve the analytical task and deliver independently comparable results. In the mixed agarose/PVP-I thin film, we found the outermost surface layer depleted in iodine, whereas the iodine is homogeneously distributed in the depth region between this outermost surface layer and the interface between the thin film and the substrate. Depletion of iodine from the uppermost surface in the thin-film samples is assumed to be caused by ultrahigh vacuum exposure resulting in a loss of molecular iodine (I2) as reported earlier for other iodine-doped polymers. KW - Biofilm KW - XPS KW - Argon gas cluster ion sputtering KW - Variable excitation KW - Iodine PY - 2022 DO - https://doi.org/10.1116/6.0001812 SN - 1934-8630 VL - 17 IS - 3 SP - 1 EP - 8 PB - AVS AN - OPUS4-54973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumacher, David T1 - NanoXSpot: Brennfleckvermessung im µm- und nm-Bereich N2 - Im Rahmen des EMPIR-Projektes NanoXSpot (Nanometre X-Ray Focal Spot Measurement) werden rückführbare Messverfahren zur Bestimmung der Brennfleckgröße und -form von Röntgenröhren mit Submikrometerauflösung (100 nm – 20 µm) entwickelt, die die Grundlage für die Erarbeitung eines Standardentwurfes bilden. Der Standardentwurf wird bei CEN TC 138 (Non-destructive testing) WG 1 (Radiographic testing) eingereicht und mit ISO und ASTM harmonisiert. Zur Untersuchung der entwickelten Methoden (Brennfleck-CT, Fit-Prozedur für Strichgruppenkörper) und des im Projekt NanoXSpot neu entworfenen Testkörpers, NxS, wurde ein Ringversuch durchgeführt. Dabei wurde sowohl der angestrebte Überlappungsbereich mit EN 12543 Teil 5 (Messung der effektiven Brennfleckgröße von Mini- und Mikrofokus-Röntgenröhren) und ASTM E 2903 (Standard Test Method for Measurement of the Effective Focal Spot Size of Mini and Micro Focus X-ray Tubes) für Brennflecke >5 µm als auch Brennflecke <5 µm untersucht. Im Mittelpunkt standen dabei Stabilität und Wiederholbarkeit der entwickelten Methoden zur Bestimmung der Brennfleckgröße. In diesem Beitrag werden die Ergebnisse des durchgeführten Ringversuches vorgestellt und diskutiert, um Schlussfolgerungen und Empfehlungen für die Vorbereitung eines erweiterten Ringversuchs mit Partnern und Stakeholdern abzuleiten. T2 - DGZfP Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Brennfleckvermessung KW - Focal spot measurement KW - Gauge design KW - EMPIR KW - Computer Tomographie KW - Standardization PY - 2022 UR - https://jahrestagung.dgzfp.de/Portals/jt2022/bb/P10.pdf AN - OPUS4-54986 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Müller, Anja T1 - Determination of the actual morphology of core-shell nanoparticles by advanced X-ray analytical techniques: A necessity for targeted and safe nanotechnology N2 - Even though we often do not knowingly recognize them, nanoparticles are present these days in most areas of our daily life, including food and its packaging, medicine, pharmaceuticals, cosmetics, pigments as well as electronic products, such as computer screens. The majority of these particles exhibits a core-shell morphology either intendedly or unintendedly. For the purpose of practicability, this core-shell nanoparticle (CSNP) morphology is often assumed to be ideal, namely a spherical core fully encapsulated by a shell of homogeneous thickness with a sharp interface between core and shell material. It is furthermore widely presumed that all nanoparticles in the sample possess the same shell thickness. As a matter of fact, most real CSNPs deviate in several ways from this ideal model with quite often severe impact on how efficiently they perform in a specific application. The topic of this cumulative PhD thesis is the accurate characterization of the actual morphology of CSNPs by advanced X-ray analytical techniques, namely X-ray photoelectron spectroscopy (XPS) and scanning transmission X-ray microscopy (STXM). A special focus is on CSNPs which deviate from an ideal core-shell morphology. In the paper from 2019 nanoparticle shell thicknesses are extracted from the elastic-peak intensities in an XPS spectrum based on an ideal particle morphology. This happens for a series of CSNP samples comprising a poly(tetrafluoroethylene) (PTFE) core and either a poly(methyl methacrylate) (PMMA) or polystyrene (PS) shell. The same paper as well as the paper from 2020 demonstrate for the first time, that the analysis of the inelastic background in an XPS spectrum of CSNPs can identify and quantify the heterogeneity of the shell and the incomplete encapsulation of the core. The result from an XPS experiment is always an average across a large nanoparticle ensemble. Deviations from an ideal morphology within a single particle of the sample cannot be assessed separately. As opposed to that, a spatial resolution of 35 nm enables STXM to visualize the interior of single CSNPs which exhibit a sufficient X-ray absorption contrast between core and shell material. In the paper from 2018 a STXM analysis is demonstrated based on the example of the PTFE-PS CSNP samples already mentioned in the previous paragraph. In the publication from 2021 (Ca/Sr)F₂ core-shell like nanoparticle ensembles for the practical use in, among others, antireflective coatings are investigated. These nanoparticles do not possess a sharp interface between core and shell material, which is why a shell thickness determination as described in the second paragraph is inappropriate. Instead, in-depth profiles of the chemical composition are obtained by XPS experiments based on synchrotron radiation with variable X-ray photon energy to elucidate the internal morphology of the particles. Additionally, theoretical in-depth profiles of Ca and Sr XPS peak intensities are simulated, in order to facilitate the interpretation of the experiments. Thus, an enrichment of CaF₂ at the particle surface was determined, which could hardly have been assessed by any other analytical technique. Because this kind of non-destructive depth profiling by XPS is very demanding, more than usual effort is spent on gapless documentation of the experiments to ensure full reproducibility. Due to the vast diversity of nanoparticles differing in material, composition and shape, a measurement procedure cannot unalteredly be transferred from one sample to another. Nevertheless, because the papers in this thesis present a greater depth of reporting on the experiments than comparable publications, they constitute an important guidance for other scientists on how to obtain meaningful information about CSNPs from surface analysis. N2 - Obwohl wir sie oft nicht bewusst wahrnehmen, sind Nanopartikel heutzutage in den meisten Bereichen unseres Alltags präsent, unter anderem in Lebensmitteln und ihren Verpackungen, Medizin, Medikamenten, Kosmetik, Pigmenten und in elektronischen Geräten wie Computermonitoren. Ein Großteil dieser Partikel weist, beabsichtigt oder unbeabsichtigt, eine Kern-Schale Morphologie auf. Einfachheitshalber wird diese Morphologie eines Kern-Schale-Nanopartikels (CSNP) oft als ideal angenommen, d.h. als ein sphärischer Kern, der komplett von einer Schale homogener Dicke bedeckt ist, mit einer scharfen Grenzfläche zwischen Kern- und Schalenmaterial. Außerdem wird vielfach auch davon ausgegangen, alle Partikel der Probe hätten gleiche Schalendicken. Tatsächlich weichen die meisten realen CSNPs in verschiedenster Weise von diesem Idealmodell ab, mit oft drastischen Auswirkungen darauf, wie gut sie ihre Aufgabe in einer bestimmten Anwendung erfüllen. Das Thema dieser kumulativen Doktorarbeit ist die exakte Charakterisierung der wirklichen Morphologie von CSNPs mit modernen Röntgen-basierten Methoden, konkret Röntgen-Photoelektronen-Spektroskopie (XPS) und Raster-Transmissions-Röntgen-Mikroskopie (STXM). Der Fokus liegt insbesondere auf CSNPs, die von einer idealen Kern-Schale-Morphologie abweichen. Im Artikel von 2019 werden Schalendicken von Nanopartikeln aus den elastischen Peakintensitäten im XPS-Spektrum unter Annahme einer idealen Partikelmorphologie abgeleitet. Dies geschieht für eine Reihe von CSNP-Proben, welche aus einem Polytetrafluoroethylen- (PTFE) Kern und entweder einer Polymethylmethacrylat- (PMMA) oder Polystyrol- (PS) Schale bestehen. Sowohl dieser Artikel als auch der von 2020 zeigen erstmals, dass die Auswertung des inelastischen Untergrunds eines CSNP-XPS-Spektrums in der Lage ist, die Heterogenität der Schale und die unvollständige Ummantelung des Kerns zu identifizieren und zu quantifizieren. Das Ergebnis eines XPS-Experiments ist immer ein Mittelwert über ein großes Nanopartikelensemble. Inwiefern ein einzelner Partikel innerhalb der Probe von einer idealen Morphologie abweicht, kann nicht gesondert erfasst werden. Im Gegensatz dazu kann STXM mit einer räumlichen Auflösung von 35 nm das Innere einzelner CSNPs visualisieren, sofern sie genügend Röntgenabsorptionskontrast zwischen Kern- und Schalenmaterial aufweisen. Im Artikel von 2018 wird am Beispiel der bereits im vorherigen Abschnitt genannt PTFE-PS-CSNPProben eine solche STXM-Untersuchung demonstriert. In der Veröffentlichung von 2021 werden Kern-Schale-artige (Ca/Sr)F₂-Nanopartikel für den praktischen Einsatz in unter anderem entspiegelnden Beschichtungen untersucht. Da hier keine scharfe Grenzfläche zwischen Kern- und Schalenmaterial vorliegt, ist eine Schalendickenbestimmung, wie sie im zweiten Abschnitt diskutiert wird, nicht sinnvoll. Stattdessen werden mit Hilfe von XPS, angeregt mit Synchrotronstrahlung bei variabler Röntgenphotonenenergie, Tiefenprofile der chemischen Zusammensetzung generiert, um die innere Morphologie der Partikel aufzuklären. Zusätzlich werden theoretische Tiefenprofile der Ca- und Sr-XPS-Peakintensitäten simuliert, um die Interpretation der Experimente zu erleichtern. So wurde eine CaF₂-Anreicherung an der Oberfläche der Partikel festgestellt, die kaum mit einer anderen analytischen Methode hätte entdeckt werden können. Da diese zerstörungsfreie Bestimmung von XPS-Tiefenprofilen sehr anspruchsvoll ist, wird noch mehr als üblich auf die lückenlose Dokumentation des Experiments geachtet, um vollständige Reproduzierbarkeit zu gewährleisten. Aufgrund der enormen Vielfalt an CSNPs, die sich in Material, Zusammensetzung und Form unterscheiden, kann eine Messmethode nicht völlig unverändert von einer Probe auf eine andere übertragen werden. Nichtsdestotrotz, da die als Teil dieser Doktorarbeit präsentierten Artikel eine deutlich ausführlichere Beschreibung der Experimente enthalten als vergleichbare Publikationen, stellen sie eine wichtige Anleitung für andere Wissenschaftler dafür dar, wie aussagekräftige Informationen über CSNPs durch Oberflächenanalytik erhalten werden können. KW - Core-shell nanoparticle (CSNP) KW - X-ray photoelectron spectroscopy (XPS) KW - Scanning transmission X-ray microscopy (STXM) PY - 2022 DO - https://doi.org/10.18452/24312 SP - i EP - 243 PB - Humboldt-Universität CY - Berlin AN - OPUS4-54991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufschläger, Daniel A1 - Gaal, Mate A1 - Gohlke, Dirk A1 - Weise, Matthias A1 - Szewieczek, A. A1 - Hillger, W. A1 - Ilse, D. T1 - Array-Prüfköpfe für luftgekoppelte Ultraschallprüfung N2 - Seit Jahren stellt die luftgekoppelte Ultraschallprüfung eine etablierte Alternative zur konventionellen Prüfung von Leichtbaukomponenten aus den Bereichen Luft- und Raumfahrt sowie Automotive dar. Im Gegenteil zur flüssigkeitsgekoppelten Prüfung in Kontakt oder im Tauchbecken ist sie weniger invasiv und bietet daher zeitliche und finanzielle Anreize. Normalerweise wird die luftgekoppelte Prüfung mit Einzelelementschwingern in Durchschallung realisiert, wohingegen die Gruppenstrahlertechnik bereits Industriestandard im Bereich der Kontakttechnik darstellt. Die damit verbundenen Vorteile wie die aktive Fokussierung oder, die gezielte Manipulation des Einschallwinkels zur Anregung von geführten Wellen, finden im Bereich der luftgekoppelten Prüfung dabei noch wenig Anwendung. Im Rahmen dieses Beitrags stellen wir die ersten Zwischenergebnisse des geförderten Projektes „PALUP – Phased- Array-Technik für Luftultraschall-Prüfungen“ vor. Ziel des Projektes ist die Entwicklung von Mehrelementschwingern auf Basis von zellulären Kunststoffen, die Entwicklung einer dedizierten Pulserstufe im Kilovoltbereich, sowie die nötige rauscharme messtechnische Auswertung jedes Einzelelements. T2 - DGZfP Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Phased array KW - Air-coupled ultrasound PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549954 SP - 1 EP - 7 AN - OPUS4-54995 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufschläger, Daniel A1 - Gaal, Mate A1 - Gohlke, Dirk A1 - Weise, Matthias A1 - Szewieczek, A. A1 - Hillger, W. A1 - Ilse, D. T1 - Array-Prüfköpfe für luftgekoppelte Ultraschallprüfung N2 - Seit Jahren stellt die luftgekoppelte Ultraschallprüfung eine etablierte Alternative zur konventionellen Prüfung von Leichtbaukomponenten aus den Bereichen Luft- und Raumfahrt sowie Automotive dar. Im Gegenteil zur flüssigkeitsgekoppelten Prüfung in Kontakt oder im Tauchbecken ist sie weniger invasiv und bietet daher zeitliche und finanzielle Anreize. Normalerweise wird die luftgekoppelte Prüfung mit Einzelelementschwingern in Durchschallung realisiert, wohingegen die Gruppenstrahlertechnik bereits Industriestandard im Bereich der Kontakttechnik darstellt. Die damit verbundenen Vorteile wie die aktive Fokussierung oder, die gezielte Manipulation des Einschallwinkels zur Anregung von geführten Wellen, finden im Bereich der luftgekoppelten Prüfung dabei noch wenig Anwendung. Im Rahmen dieses Beitrags stellen wir die ersten Zwischenergebnisse des geförderten Projektes „PALUP – Phased- Array-Technik für Luftultraschall-Prüfungen“ vor. Ziel des Projektes ist die Entwicklung von Mehrelementschwingern auf Basis von zellulären Kunststoffen, die Entwicklung einer dedizierten Pulserstufe im Kilovoltbereich, sowie die nötige rauscharme messtechnische Auswertung jedes Einzelelements. T2 - DGZfP Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Phased array KW - Air-coupled ultrasound PY - 2022 AN - OPUS4-54996 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufschläger, Daniel A1 - Gaal, Mate A1 - Ahmadzadeh, M. T1 - Simulation und Vermessung von thermoakustischen Schallquellen N2 - Zur Simulation des Schallfeldes von beliebig geformten konventionellen Schallquellen existieren viele Ansätze (EFIT, GPSS). Sie alle basieren auf der Annahme eines monochromatischen akustischen Signals, was meist eine gültige Annäherung darstellt. Allerdings sind bei thermoakustischen Quellen aufgrund ihrer Funktionsweise und der hohen Bandbreite viele der existierenden Ansätze nicht direkt anwendbar und können Beobachtungen bei der Vermessung von thermoakustischen Wandlern nicht vollständig abbilden und erklären. In diesem Beitrag wurde die bekannte Methode der generalisierten Punktquellensynthese (GPSS) für die Berechnung von Schallfeldern von thermoakustischen Schallquellen angewendet. Dabei gehen zahlreiche Parameter wie die Dicke und Geometrie der leitfähigen Schicht, Krümmung des Substrats, sowie die Signalform der Anregung in die Simulation ein. Neu an dem präsentierten Ansatz ist die Abweichung von der üblichen monochromatischen Annäherung und die Berücksichtigung der großen Bandbreite von thermoakustischen Wandlern. Für die Validierung der Simulationen wurden Schallfelder von Quellen mit bekannter Anregung und Geometrie breitbandig durch ein optisches Mikrofon vermessen. T2 - DGZfP Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Thermoacoustics KW - Sensor characterization PY - 2022 AN - OPUS4-54997 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Optical Detection of Defects during Laser Metal Deposition N2 - Laser metal deposition is a rapidly evolving method for additive manufacturing that combines high performance and simplified production routine. Quality of production depends on an instrumental design and operational parameters, which require constant control during the process. In this work, feasibility of using optical spectroscopy as a control method is studied via modeling and experimentally. A simplified thermal model is developed based on the time-dependent diffusion-conduction heat equation and geometrical light collection into detection optics. Intense light emitted by a laser-heated spot moving across a sample surface is collected and processed to yield the temperature and other temperature-related parameters. In the presence of surface defects, the temperature field is distorted in a specific manner that depends on shape and size of the defect. Optical signals produced by such the distorted temperature fields are simulated and verified experimentally using a 3D metal printer and a sample with artificially carved defects. Three quantities are tested as possible metrics for monitoring the process: temperature, integral intensity, and correlation coefficient. The shapes of the simulated signals qualitatively agree with the experimental signals; this allows for a cautious inference that optical spectroscopy can detect surface defects and, possibly, predict their characters, e.g., inner or protruding. T2 - Colloquium Spectroscopicum Internationale XLII (CSI XLII) CY - Gijon, Spain DA - 30 May 2022 KW - Additive manufacturing KW - Laser metal deposition KW - Optical sensor KW - Optical emission spectroscopy KW - Process control PY - 2022 AN - OPUS4-55063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Accorsi, M. A1 - Tiemann, M. A1 - Wehrhan, L. A1 - Finn, Lauren M. A1 - Cruz, R. A1 - Rautenberg, Max A1 - Emmerling, Franziska A1 - Heberle, J. A1 - Keller, B. G. A1 - Rademann, J. T1 - Pentafluorophosphato-Phenylalanines: Amphiphilic Phosphotyrosine Mimetics Displaying Fluorine-Specific Protein Interactions N2 - Phosphotyrosine residues are essential functional switches in health and disease. Thus, phosphotyrosine biomimetics are crucial for the development of chemical tools and drug molecules. We report here the discovery and investigation of pentafluorophosphato amino acids as novel phosphotyrosine biomimetics. A mild acidic pentafluorination protocol was developed and two PF5-amino acids were prepared and employed in peptide synthesis. Their structures, reactivities, and fluorine-specific interactions were studied by NMR and IR spectroscopy, X-ray diffraction, and in bioactivity assays. The mono-anionic PF5 motif displayed an amphiphilic character binding to hydrophobic surfaces, to water molecules, and to protein-binding sites, exploiting charge and H−F-bonding interactions. The novel motifs bind 25- to 30-fold stronger to the phosphotyrosine binding site of the protein tyrosine phosphatase PTP1B than the best current biomimetics, as rationalized by computational methods, including molecular dynamics simulations. KW - Chemical Biology KW - Drug Development KW - Pentafluorophosphates KW - Phosphotyrosine Biomimetics KW - Protein Tyrosine Phosphatases PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549984 DO - https://doi.org/10.1002/anie.202203579 SN - 1433-7851 VL - 134 IS - 25 SP - 1 EP - 6 PB - Wiley-VCH GmbH AN - OPUS4-54998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. T1 - RASEM - Robot-Assisted Environmental Monitoring for Air Quality Assessment N2 - This presentation was held at the SAF€RA symposium and gives an overview to the research project RASEM and its results. T2 - 2022 SAF€RA Symposium CY - Rome, Italy DA - 19.05.2022 KW - Air Pollution KW - Air Quality KW - Environmental Monitoring KW - Mobile Robot Olfaction KW - Wireless Sensor Network PY - 2022 AN - OPUS4-54953 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. T1 - Super-Resolution for Gas Distribution Mapping: Convolutional Encoder Decoder Network N2 - Gas distribution mapping is important to have an accurate understanding of gas concentration levels in hazardous environments. A major problem is that in-situ gas sensors are only able to measure concentrations at their specific location. The gas distribution in-between the sampling locations must therefore be modeled. In this research, we interpret the task of spatial interpolation between sparsely distributed sensors as a task of enhancing an image's resolution, namely super-resolution. Because autoencoders are proven to perform well for this super-resolution task, we trained a convolutional encoder-decoder neural network to map the gas distribution over a spatially sparse sensor network. Due to the difficulty to collect real-world gas distribution data and missing ground truth, we used synthetic data generated with a gas distribution simulator for training and evaluation of the model. Our results show that the neural network was able to learn the behavior of gas plumes and outperforms simpler interpolation techniques. T2 - 19th International Symposium on Olfaction and Electronic Nose CY - Aveiro, Portugal DA - 29.05.2022 KW - Gas Distribution Mapping KW - Spatial Interpolation KW - Deep Learning KW - Super-Resolution KW - Sensor Network PY - 2022 AN - OPUS4-54954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. A1 - Matsukura, H. A1 - Neumann, Patrick P. A1 - Schaffernicht, E. A1 - Ishida, H. A1 - Lilienthal, A. J. ED - Rudnitskaya, A. T1 - Super-Resolution for Gas Distribution Mapping: Convolutional Encoder-Decoder Network N2 - Gas distribution mapping is important to have an accurate understanding of gas concentration levels in hazardous environments. A major problem is that in-situ gas sensors are only able to measure concentrations at their specific location. The gas distribution in-between the sampling locations must therefore be modeled. In this research, we interpret the task of spatial interpolation between sparsely distributed sensors as a task of enhancing an image's resolution, namely super-resolution. Because autoencoders are proven to perform well for this super-resolution task, we trained a convolutional encoder-decoder neural network to map the gas distribution over a spatially sparse sensor network. Due to the difficulty to collect real-world gas distribution data and missing ground truth, we used synthetic data generated with a gas distribution simulator for training and evaluation of the model. Our results show that the neural network was able to learn the behavior of gas plumes and outperforms simpler interpolation techniques. T2 - 19th International Symposium on Olfaction and Electronic Nose CY - Aveiro, Portugal DA - 29.05.2022 KW - Gas Distribution Mapping KW - Spatial Interpolation KW - Deep Learning KW - Super-Resolution KW - Sensor Network PY - 2022 SN - 978-1-6654-5860-3 DO - https://doi.org/10.1109/isoen54820.2022.9789555 SP - 1 EP - 3 PB - IEEE CY - USA AN - OPUS4-54955 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Burgmayer, R. A1 - Bake, Friedrich A1 - Enghardt, L. T1 - Design and Evaluation of a Zero Mass Flow Liner N2 - In this study, the concept of a Zero Mass Flow Liner is evaluated. The concept enables impedance control by the induction of periodic bias flow through the perforated facing sheet of the liner. The periodic bias flow is generated by a secondary high amplitude acoustic actuation. By means of the periodic bias flow, the liner can be tuned to different operating points in a given range of grazing flow velocities. The equivalent fluid impedance model for perforated plates is modified to account for the effects of periodic bias flow and grazing flow. An optimization routine, based on a genetic algorithm, is implemented. The method is applicable to any liner concept and uses the impedance of the lined surface as boundary condition in a numerical simulation. Thereby, a set of liner parameters is derived in order to obtain the desired damping characteristics. Based on the results of the optimization, a Zero Mass Flow Liner is manufactured and consequently evaluated experimentally. The damping characteristics are evaluated in form of the dissipated energy along the lined surface. Prediction and measurements show agreement. The Zero Mass Flow Liner delivers broad band dissipation of high peak value over a range of grazing flow Mach numbers. Under grazing ow conditions, the effect of periodic bias flow is reduced. This poses high energy requirements in high Mach number flow regimes which might restrict the applicability of the Zero Mass Flow concept to grazing flows of low Mach numbers. T2 - 28th AIAA/CEAS Aeroacoustics 2022 Conference CY - Southampton, Great Britain DA - 14.06.2022 KW - Acoustic damping KW - Liner KW - Zero Massflow Liner (ZML) PY - 2022 DO - https://doi.org/10.2514/6.2022-2820 SP - 1 EP - 16 PB - AIAA / CEAS AN - OPUS4-55042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hirschberg, L. A1 - Bake, Friedrich A1 - Hulshoff, S. T1 - Sound production due to main-flow oriented vorticity-nozzle interaction in absence of a net swirl N2 - The downstream acoustic response due to the interaction of main-flow oriented vorticity with a choked nozzle in a swirl-free flow was experimentally demonstrated. The response was obtained by means of impulsive radial air injection in the pipe upstream from the nozzle. The resulting downstream acoustic data are shown to obey a scaling rule that differs, from the one for swirl-nozzle interaction, which according to the literature is proportional to the square of the swirl number. In contrast, here evidence is presented that points to the scaling of main-flow oriented vorticity noise with the cross-sectional average of the square of the transversal velocity at the throat divided by the square of the critical sound speed. T2 - 28th AIAA/CEAS Aeroacoustics 2022 Conference CY - Southampton, Great Britain DA - 14.06.2022 KW - Main-flow oriented vorticity-nozzle interaction KW - Indirect noise PY - 2022 DO - https://doi.org/10.2514/6.2022-3055 SP - 1 EP - 8 PB - AIAA / CEAS AN - OPUS4-55043 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wu, Cheng-Chieh A1 - Völker, Daniel A1 - Weisbrich, S. A1 - Neitzel, F. ED - Holl, H. T1 - The finite volume method in the context of the finite element method N2 - The finite volume method (FVM), like the finite element method (FEM), is a numerical method for determining an approximate solution for partial differential equations. The derivation of the two methods is based on very different considerations, as they have historically evolved from two distinct engineering disciplines, namely solid mechanics and fluid mechanics. This makes FVM difficult to learn for someone familiar with FEM. In this paper we want to show that a slight modification of the FEM procedure leads to an alternative derivation of the FVM. Both numerical methods are starting from the same strong formulation of the problem represented by differential equations, which are only satisfied by their exact solution. For an approximation of the exact solution, the strong formulation must be converted to a so-called weak form. From here on, the two numerical methods differ. By appropriate choice of the trial function and the test function, we can obtain different numerical methods for solving the weak formulation of the problem. While typically in FEM the basis functions of the trial function and test function are identical, in FVM they are chosen differently. In this paper, we show which trial and test function must be chosen to derive the FVM alternatively: The trial function of the FVM is a “shifted” trial function of the FEM, where the nodal points are now located in the middle of an integration interval rather than at the ends. Moreover, the basis functions of the test function are no longer the same as those of the trial function as in the FEM, but are shown to be a constant equal to 1. This is demonstrated by the example of a 1D Poisson equation. KW - Finite Volume Method KW - Finite Element Method KW - Variational Calculation KW - Numerical Methods PY - 2022 DO - https://doi.org/10.1016/j.matpr.2022.05.460 SN - 2214-7853 VL - 62 SP - 2679 EP - 2683 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-55046 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xiao, J. A1 - Vogl, Jochen A1 - Rosner, M. A1 - Jin, Z. T1 - Boron isotope fractionation in soil-plant systems and its influence on biogeochemical cycling N2 - Boron (B) is an essential mineral nutrient for higher plants. Although B plant nutrition is well studied, the B isotope fractionation at the soil-plant interface, within plant metabolism, and its influence on biogeochemical cycling is not fully understood. Boron concentrations and isotope variations (δ11B) of the dicotyledonous plants of Chenopodium album and Brassica napus and their growing soils along a climatic gradient were analyzed to decipher these unresolved issues of the B behavior. The boron concentrations and δ11B values show an increasing trend from roots to leaves for both plants, while a decreasing trend from flower to shell and to seed for Brassica napus. A large boron isotope fractionation occurs within the plants with median Δ11Bleaf-root ≈ +20‰, which is related to different boron transporters and transportation ways. Formation of borate dimerized rhamnogalacturonan II in cell and B(OH)3 transportation in xylem lead to heavier δ11B values from root to stem and leaf while B(OH)4􀀀 transportation in phloem lead to lighter δ11B values from flower to shell and seed. Although samples cover a distinct transect with systematically different climatic conditions, Δδ11B within the individual plant compartments and between the bulk plants and the soil available B do not show any systematic variation. This suggests that B uptake from the soil into Chenopodium album and Brassica napus occurs without a distinct isotope fractionation at the soil-plant interface (median Δ11Bbulkplant-soil = 􀀀 0.2‰) and plants are able to regulate boron uptake. Both the observed large B fractionation within plant and low or absent B isotope fractionation at the soil-plant interface may have profound implications for the biological and geological B cycle. If this observed boron behavior also exists in other plants, their litters would be an important source for exporting 11B-rich biological material from continental ecosystems via rivers to the global oceans. This may be helpful for the explanation of ocean B cycle and the increasing δ11B values over the Cenozoic. KW - Boron isotopic composition KW - Boron isotope fractionation KW - Soil available boron KW - Biological boron recycling KW - Chenopodium album KW - Brassica napus PY - 2022 DO - https://doi.org/10.1016/j.chemgeo.2022.120972 SN - 0009-2541 VL - 606 SP - 1 EP - 8 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-55031 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brauckmann, C. A1 - Pramann, A. A1 - Rienitz, O. A1 - Schulze, A. A1 - Phukphatthanachai, P. A1 - Vogl, Jochen T1 - Combining Isotope Dilution and Standard Addition - Elemental Analysis in Complex Samples N2 - A new method combining isotope dilution mass spectrometry (IDMS) and standard addition has been developed to determine the mass fractions w of different elements in complex matrices: (a) silicon in aqueous tetramethylammonium hydroxide (TMAH), (b) sulfur in biodiesel fuel, and (c) iron bound to transferrin in human serum. All measurements were carried out using inductively coupled plasma mass spectrometry (ICP–MS). The method requires the gravimetric preparation of several blends (bi)—each consisting of roughly the same masses (mx,i) of the sample solution (x) and my,i of a spike solution (y) plus different masses (mz,i) of a reference solution (z). Only these masses and the isotope ratios (Rb,i) in the blends and reference and spike solutions have to be measured. The derivation of the underlying equations based on linear regression is presented and compared to a related concept reported by Pagliano and Meija. The uncertainties achievable, e.g., in the case of the Si blank in extremely pure TMAH of urel (w(Si)) = 90% (linear regression method, this work) and urel (w(Si)) = 150% (the method reported by Pagliano and Meija) seem to suggest better applicability of the new method in practical use due to the higher robustness of regression analysis. T2 - CITAC Best Paper Award Ceremony CY - Online meeting DA - 21.06.2022 KW - Isotope dilution mass spectrometry KW - Standard addition KW - ICP-MS KW - Blank characterization KW - Silicon KW - Sulfur KW - Transferrin KW - Tetramethylammonium hydroxide KW - Biodiesel fuel KW - Human serum PY - 2022 AN - OPUS4-55032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prohaska, T. A1 - Irrgeher, J. A1 - Benefield, J. A1 - Böhlke, J. K. A1 - Chesson, L. A. A1 - Coplen, T. B. A1 - Ding, T. A1 - Dunn, P. J. H. A1 - Gröning, M. A1 - Holden, N. E. A1 - Meijer, H. A. J. A1 - Moossen, H. A1 - Possolo, A. A1 - Takahashi, Y. A1 - Vogl, Jochen A1 - Walczyk, T. A1 - Wang, J. A1 - Wieser, M. E. A1 - Yoneda, S. A1 - Zhu, X.-K. A1 - Meija, J. T1 - Standard atomic weights of the elements 2021 (IUPAC Technical Report) N2 - Following the reviews of atomic-weight determinations and other cognate data in 2015, 2017, 2019 and 2021, the IUPAC (International Union of Pure and Applied Chemistry) Commission on Isotopic Abundances and Atomic Weights (CIAAW) reports changes of standard atomic weights. The symbol Ar(E) was selected for standard atomic weight of an element to distinguish it from the atomic weight of an element E in a specific substance P, designated Ar(E, P). The CIAAW has changed the values of the standard atomic weights of five elements based on recent determinations of terrestrial isotopic abundances: Ar (argon): from 39.948 ± 0.001 to [39.792, 39.963] Hf (hafnium): from 178.49 ± 0.02 to 178.486 ± 0.006 Ir (iridium): from 192.217 ± 0.003 to 192.217 ± 0.002 Pb (lead): from 207.2 ± 0.1 to [206.14, 207.94] Yb (ytterbium): from 173.054 ± 0.005 to 173.045 ± 0.010 The standard atomic weight of argon and lead have changed to an interval to reflect that the natural variation in isotopic composition exceeds the measurement uncertainty of Ar(Ar) and Ar(Pb) in a specific substance. The standard atomic weights and/or the uncertainties of fourteen elements have been changed based on the Atomic Mass Evaluations 2016 and 2020 accomplished under the auspices of the International Union of Pure and Applied Physics (IUPAP). Ar of Ho, Tb, Tm and Y were changed in 2017 and again updated in 2021: Al (aluminium), 2017: from 26.981 5385 ± 0.000 0007 to 26.981 5384 ± 0.000 0003 Au (gold), 2017: from 196.966 569 ± 0.000 005 to 196.966 570 ± 0.000 004 Co (cobalt), 2017: from 58.933 194 ± 0.000 004 to 58.933 194 ± 0.000 003 F (fluorine), 2021: from 18.998 403 163 ± 0.000 000 006 to 18.998 403 162 ± 0.000 000 005 (Ho (holmium), 2017: from 164.930 33 ± 0.000 02 to 164.930 328 ± 0.000 007) Ho (holmium), 2021: from 164.930 328 ± 0.000 007 to 164.930 329 ± 0.000 005 Mn (manganese), 2017: from 54.938 044 ± 0.000 003 to 54.938 043 ± 0.000 002 Nb (niobium), 2017: from 92.906 37 ± 0.000 02 to 92.906 37 ± 0.000 01 Pa (protactinium), 2017: from 231.035 88 ± 0.000 02 to 231.035 88 ± 0.000 01 Pr (praseodymium), 2017: from 140.907 66 ± 0.000 02 to 140.907 66 ± 0.000 01 Rh (rhodium), 2017: from 102.905 50 ± 0.000 02 to 102.905 49 ± 0.000 02 Sc (scandium), 2021: from 44.955 908 ± 0.000 005 to 44.955 907 ± 0.000 004 (Tb (terbium), 2017: from 158.925 35 ± 0.000 02 to 158.925 354 ± 0.000 008) Tb (terbium), 2021: from 158.925 354 ± 0.000 008 to 158.925 354 ± 0.000 007 (Tm (thulium), 2017: from 168.934 22 ± 0.000 02 to 168.934 218 ± 0.000 006) Tm (thulium), 2021: from 168.934 218 ± 0.000 006 to 168.934 219 ± 0.000 005 (Y (yttrium), 2017: from 88.905 84 ± 0.000 02 to 88.905 84 ± 0.000 01) Y (yttrium), 2021: from 88.905 84 ± 0.000 01 to 88.905 838 ± 0.000 002 KW - Argon KW - Ciaaw.org KW - Hafnium KW - Iridium KW - Lead KW - LSVEC KW - Ytterbium PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548443 DO - https://doi.org/10.1515/pac-2019-0603 SN - 0033-4545 VL - 94 IS - 5 SP - 573 EP - 600 PB - De Gruyter Verlag CY - Berlin AN - OPUS4-54844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kornev, R. A1 - Gornushkin, Igor B. A1 - Nazarov, V. A1 - Shkrunin, V. A1 - Ermakov, A. T1 - Features of hydrogen reduction of SiF4 in ICP plasma N2 - Probe diagnostics is used to determine the electron temperature and electron number density in a low pressure inductively coupled plasma (ICP) ignited in the mixture of SiF4, Ar and H2. Emission spectra of mixtures with different stoichiometry of components are investigated and the electron density distribution function (EDDF) is estimated. The optimal conditions for high conversion of SiF4 into Si are found by studying the dependence of the yield of silicon upon the ratio of reagents. The maximum achieved yield of silicon is 85% under the optimal conditions. Based on the analysis of IR and MS spectra of exhaust gases, 5% of initial SiF4 converts into volatile fluorosilanes. A rate of production of Si is 0.9 g/h at the energy consumption 0.56 kWh /g. KW - Plasma enhanced chemical vapor deposition KW - PECVD KW - Silicon tetrafluoride KW - Emission spectroscopy KW - Probe diagnostics PY - 2022 DO - https://doi.org/10.1016/j.sab.2022.106502 SN - 0584-8547 VL - 195 SP - 106502 PB - Elsevier B.V. AN - OPUS4-55316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pech May, Nelson Wilbur T1 - Photothermal characterization of polyester composites loaded with parallelly arranged graphite rods N2 - One of the biggest challenges in the measurement of thermal properties is to measure inhomogeneous materials This work focuses on measuring the thermal properties of cylindrical polyester resin composite materials loaded with graphite rods oriented in the direction of the resin thickness, varying the graphite concentrations starting from zero to 8 75 of volumetric fraction and changing the distribution of graphite rods inside the polyester matrix. T2 - International Conference in Photoacoustics and Photothermal Phenomena (ICPPP21) CY - Bled, Slovenia DA - 19.06.2022 KW - Heat diffusion KW - Heterogeneous materials PY - 2022 AN - OPUS4-55384 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pech May, Nelson Wilbur T1 - Automatic inspection of surface breaking cracks using laser scanning thermography N2 - In this work, we report on a method for automatic inspection of components using laser scanning thermography, in which the relative motion is performed by a robot to fully inspect complex test objects such as turbine blades. We demonstrate our evaluation algorithms with the aim of automatically detecting surface defects on calibrated specimens. We show the influence of the excitation laser, which can be varied in terms of spot geometry, wavelength, and scan scheme. Additionally, we show some advantages, versatility, and current challenges of using a programmed robot for non-destructive evaluation in thermography. T2 - International Conference in Photoacoustics and Photothermal Phenomena (ICPPP21) CY - Bled, Slovenia DA - 19.06.2022 KW - Flying line thermography KW - Surface breaking defects KW - Canny approach PY - 2022 AN - OPUS4-55386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shapovalov, O. A1 - Heckel, Thomas A1 - Gaal, Mate A1 - Weiß, S. T1 - External Acoustical Damping on a Metallic Angle Wedge in a High Temperature Resistant Ultrasonic Probe N2 - Ultrasonic probes for high-temperature applications are provided with metallic wedges, which can withstand the contact with the high temperature of the inspected structure. The ultrasonic signal travels within the wedge and gets reflected from its boundaries, causing interference signals called “ghost echoes”. The current work presents an investigation of the additional damping effect provided by porous sintered metal plates applied onto the surface of the wedge. In particular, the study evaluates the effect of damping plate thickness on the interference signal level at different transmission frequencies. Damping plates made of sintered metal SIKA-R 15 AX were attached to a wedge prototype made of steel 1.4301. The study revealed, that the most effective thickness of damping plates in the selected frequency interval of 1 to 4 MHz is equal to 4 mm. The evaluation of the interference signal has shown that the application of such damping plates to the wedge surface contributes to an additional attenuation of an interference signal of 10 to 30 dB after 500 μs of signal propagation. KW - Ultrasonic testing KW - High temperature KW - Acoustical damping KW - Angle wedge KW - Ultrasonic probe PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553920 DO - https://doi.org/10.1007/s40857-022-00270-9 SN - 0814-6039 SP - 1 EP - 11 PB - Springer AN - OPUS4-55392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nattuveettil, Keerthana A1 - Brunner, Nanine A1 - Tiebe, Carlo A1 - Melzer, Michael A1 - Johann, Sergej A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias T1 - Einsatz von Sensortechnologien an einer Wasserstofftankstelle als Beitrag zur digitalen Qualitätsinfrastruktur T1 - Use of sensor technologies at hydrogen test platform as a part of QI Digital N2 - Die Optimierung und Validierung des digitalen Wasserstofftankstellenmanagements mit Sensortechnologien ist das übergeordnete Ziel des Teilprojekts Digitale Qualitätsinfrastruktur mit Sensortechnologien (QIST) am Use Case H2, im Rahmen der digitalen Qualitätsinfrastruktur (QI digital[1]). Hierfür sollen u.a. Sensornetzwerke mit digital-gestützten Auswertungsstrategien intelligent gestaltet werden (Stichwort KI bzw. digitaler Zwilling). Verschiedene, sich ergänzende Sensoren, Systemkomponenten und KI-Methoden stehen als Bausteine intelligenter Sensorsysteme zur Verfügung, mit dem Zweck, die physikalischen und chemischen Parameter an und in Anlagen umfassend und effizient zu überwachen sowie Fehlfunktionen zuverlässig zu detektieren und zu interpretieren, Abbildung 1. Konkrete Arbeitsschritte sind, nach dem Aufbau der Versuchsplattform „Wasserstofftankstelle“, die Instrumentierung von Sensorik und deren digitale Integration in das Tankstellenmanagementsystem sowie die Validierung im Realbetrieb. Die somit erzielten Messergebisse sowie die Messunsicherheiten, Historien und Verfahren werden in digitaler Form aufbereitet, gespeichert und fortlaufend in die KI-basierte Datenauswertung einbezogen, inkl. der Anbindung an die metrologische Rückführungskette. Ziele sind: • Einführung eines neuen messtechnischen Ansatzes und eines digitalen Zwillings für den Anwendungsfall "Wasserstofftankstelle" auf Basis der H2-Sensorik sowie der Zustandsgrößen Druck und Temperatur • Qualitätssicherung durch Applikationen zuverlässiger Gassensorik, Manometer und Thermometer sowie KI-Methoden zur Prozesskontrolle und Detektion von Fehlfunktionen • Nutzung von digitalen Kalibrierscheinen (DCCs) insbesondere für die Messgröße Temperatur zur Realisierung der metrologischen Rückführung in einer digitalen Qualitätsinfrastruktur T2 - Sensorik für die Digitalisierung chemischer Produktionsanlagen CY - Frankfurt a. M., Germany DA - 13.06.2022 KW - QI Digital KW - H2Safety@BAM KW - Wasserstoff KW - Hydrogen KW - Sensorik KW - Digitalisierung KW - Digitalisation PY - 2022 AN - OPUS4-55399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Richtlinie zur Charakterisierung von luftgekoppelten Ultraschallwandlern N2 - Zur Charakterisierung von luftgekoppelten Ultraschallwandlern werden mehrere verschiedene Methoden und Verfahren angewendet. Durch die unterschiedlichen Herangehensweisen werden oft unterschiedliche Prüfkopfpara-meter und Schallfeldgrößen ermittelt, was einen direkten Vergleich von Datenblättern erschwert. Für die Charakterisierung von Kontakt- und Tauchtechnikprüfköpfen hat sich ISO 22232-2:2021 bereits etabliert, allerdings ist diese Norm nicht auf die luftgekoppelten Wandlertechnologien direkt übertragbar. Daher erkannten Hersteller, Forschungseinrichtungen und Anwender den Bedarf an einer Richtlinie zur einheitlichen Charakterisierung von luftgekoppelten Wandlern. Gemeinsam arbeiten sie aktuell im Rahmen des Unterausschusses „Luftgekoppelte Ultraschallprüfung“ der DGZfP an der Erstellung einer solcher Richtlinie mit dem Anspruch, die bestehende Normung um die luftgekoppelte Prüfung zu erweitern und somit die Vereinheitlichung der Charakterisierung dieser Wandler zu erleichtern. In diesem Beitrag wird ein Überblick über den geplanten Inhalt der Richtlinie und über die Methoden zur akustischen Charakterisierung von luftgekoppelten Ultraschallwandlern gegeben. Insbesondere werden verschiedene Methoden der Ermittlung von wichtigen Wandlerparametern wie z.B. Empfindlichkeit, Mittenfrequenz, Bandbreite, Fokusgröße und Fokusabstand dargestellt und verglichen. T2 - DGZfP-Jahrestagung CY - Kassel, Germany DA - 23.5.2022 KW - Luftgekoppelte Ultraschallprüfung KW - Richtlinie KW - Ultraschallwandler KW - Prüfkopf KW - Charakterisierung PY - 2022 AN - OPUS4-55292 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mazzeo, P. P. A1 - Prencipe, M. A1 - Feiler, Torvid A1 - Emmerling, Franziska A1 - Bacchi, A. T1 - On the mechanism of cocrystal mechanochemical reaction via low melting eutectic: A time-resolved in situ monitoring investigation N2 - Mechanochemistry has become a sustainable and attractive cost-effective synthetic technique, largely used within the frame of crystal engineering. Cocrystals, namely, crystalline compounds made of different chemical entities within the same crystal structure, are typically synthesized in bulk via mechanochemistry; however, whereas the macroscopic aspects of grinding are becoming clear, the fundamental principles that underlie mechanochemical cocrystallization at the microscopic level remain poorly understood. Time-resolved in situ (TRIS) monitoring approaches have opened the door to exceptional detail regarding mechanochemical reactions. We here report a clear example of cocrystallization between two solid coformers that proceeds through the formation of a metastable low melting binary eutectic phase. The overall cocrystallization process has been monitored by time-resolved in situ (TRIS) synchrotron X-ray powder diffraction with a customized ball milling setup, currently available at μ Spot beamline at BESSY-II, Helmholtz-Zentrum Berlin. The binary system and the low melting eutectic phase were further characterized via DSC, HSM, and VT-XRPD. KW - Mechanochemistry KW - In situ KW - Cocrystal PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552977 DO - https://doi.org/10.1021/acs.cgd.2c00262 SN - 1528-7505 VL - 22 IS - 7 SP - 4260 EP - 4267 PB - ACS Publ. CY - Washington, DC AN - OPUS4-55297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kröll, Mirco T1 - Effects of harmonised procedures in tribology testing N2 - i-TRIBOMAT will provide the world's first Open Innovation Test Bed dedicated to analysing and simulating materials in tribological systems. In order to make necessary results of tribological tests comparable, harmonised ways to produce data are mandatory. Many sources influence the outcome of a Tribological test. Different approaches of institutes were evaluated in best practices via quality management tools minimising the impact on results. T2 - 7th World Tribology Congress - WTC 2022 CY - Lyon, France DA - 11.07.2022 KW - Tribology KW - i-TRIBOMAT KW - Characterisation KW - Digitalisation KW - Harmonisation KW - Round robin tests KW - Interlaboratory tests PY - 2022 AN - OPUS4-55317 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zabala, A. T1 - Ball-on-flat linear reciprocating tests: Critical assessment of wear volume determination methods N2 - This work presents a critical assessment of wear volume determination methods for ball-on-flat linear reciprocating sliding tribological tests. T2 - 7th World Tribology Congress - WTC 2022 CY - Lyon, France DA - 11.07.2022 KW - Wear KW - Sliding KW - Surface KW - Analysis PY - 2022 AN - OPUS4-55319 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien A1 - Hirsch, Philipp Daniel A1 - Rupprecht, C. A1 - Ziegler, Mathias ED - Mendioroz, A. ED - Avdelidis, N. P. T1 - Thermographic testing using 2D pseudo-random illumination and photothermal super resolution reconstruction N2 - Due to the diffusive nature of heat propagation in solids, the detection and resolution of internal defects with active thermography based non-destructive testing is commonly limited to a defect-depth-to-defect-size ratio greater than or equal to one. In the more recent past, we have already demonstrated that this limitation can be overcome by using a spatially modulated illumination source and photothermal super resolution-based reconstruction. Furthermore, by relying on compressed sensing and computational imaging methods we were able to significantly reduce the experimental complexity to make the method viable for investigating larger regions of interest. In this work we share our progress on improving the defect/inhomogeneity characterization using fully 2D spatially structured illumination patterns instead of scanning with a single laser spot. The experimental approach is based on the repeated blind pseudo-random illumination using modern projector technology and a high-power laser. In the subsequent post-processing, several measurements are then combined by taking advantage of the joint sparsity of the defects within the sample applying 2D-photothermal super resolution reconstruction. Here, enhanced nonlinear convex optimization techniques are utilized for solving the underlying ill-determined inverse problem for typical simple defect geometries. As a result, a higher resolution defect/inhomogeneity map can be obtained at a fraction of the measurement time previously needed. T2 - Thermosense: Thermal Infrared Applications XLIV CY - Orlando, Florida, USA DA - 05.04.2022 KW - Thermography KW - Super resolution KW - NDT KW - Material testing KW - Internal defects KW - DMD KW - DLP PY - 2022 DO - https://doi.org/10.1117/12.2618562 SN - 0277-786X VL - 12109 SP - 1 EP - 10 PB - SPIE AN - OPUS4-54909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gupta, P. A1 - Karnaushenko, D. D. A1 - Becker, C. A1 - Okur, I. E. A1 - Melzer, Michael A1 - Özer, B. A1 - Schmidt, O. G. A1 - Karnaushenko, D. T1 - Large Scale Exchange Coupled Metallic Multilayers by Roll-to-Roll (R2R) Process for Advanced Printed Magnetoelectronics N2 - Till now application of printed magnetoelectronics is hindered by lack of large area exchange coupled metallic multilayers required to produce printable magneto-sensory inks. Large-scale roll-to-roll (R2R) fabrication process is an attractive approach owing to its capabilities for high volume, high throughput, and large area manufacturing. Precise and high performance R2R sputtering technology is developed to fabricate large area giant magnetoresistive (GMR) thin-films stacks that contain 30 metallic bilayers prepared by continuous R2R sputtering of Co and Cu sequential on a hundred meters long polyethylene terephthalate (PET) web. The R2R sputtered Co/Cu multilayer on a 0.2 × 100 m2 PET web exhibits a GMR ratio of ≈40% achieving the largest area exchange coupled room temperature magneto-sensitive system demonstrated to date. The prepared GMR thin-film is converted to magnetosensitive ink that enables printing of magnetic sensors with high performance in a cost-efficient way, which promotes integration with printed electronics. An average GMR ratio of ≈18% is obtained for 370 printed magnetic sensors. The realized precise R2R sputtering approach can also be extended to a wide range of hybrid thin-film material systems opening up a path for new functional inks applied with printing technologies. KW - Printed Electronics KW - Flexible Magnetic Sensors KW - Roll-to-Roll Processing KW - Functional Materials KW - Upscaling PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552344 DO - https://doi.org/10.1002/admt.202200190 SN - 2365-709X SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim, Deutschland AN - OPUS4-55234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - Reconstruction of Elastic Constants of Isotropic and Anisotropic Materials using Ultrasonic Guided Waves N2 - Acoustic methods are ideally suited for determining the mechanical properties of different materials non-destructively. The availability of such methods is particularly important for fiber-reinforced polymers (FRPs) because their properties strongly depend on the manufacturing process and in-service conditions. Since FRPs are mostly used in thin-walled components, properties can be derived from the dispersion curves of ultrasonic guided waves (UGWs). Our approach is based on an inverse procedure in which the numerically calcu-lated dispersion curves are fitted to the measured curves. The acquisition is done by applying a broadband piezoelectric transducer (PZT) to excite and a 3D laser Doppler vibrometer (3D LDV) to record the waves. Compared to the ap-proaches based on laser excitation, the PZT provides a better signal-to-noise ra-tio because more energy is brought into the structure. Whereas the 3D LDV compared to a 1D LDV or a PZT allows capturing in-plane and out-of-plane components and thus providing more dispersion information. Since the inverse procedure requires many iterations before elastic properties are retrieved, an ef-ficient tool for the calculation of the dispersion curves is necessary. For this, the Scaled Boundary Finite Element Method is used. All in all, a good agreement between theoretical and experimental curves is demonstrated. T2 - 10th European Workshop on Structural Health Monitoring (EWSHM 2022) CY - Palermo, Italy DA - 04.07.2022 KW - Lamb waves KW - Elastic waves KW - Fibre-reinforced polymers KW - Inverse procedure KW - Scaled Boundary Finite Element Method PY - 2022 AN - OPUS4-55236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Even, Morgane T1 - Development of a procedure for the analysis of the emissions of VVOCs N2 - Several aspects were explored towards the standardization of a suitable procedure. The use of gaseous standards is necessary and a standard gas mixture containing 60 substances was successfully generated and employed for further investigations. The suitability of different chromatography columns was addressed: The use of PLOT (Porous Layer Open Tubular) columns is well suitable for VVOC analysis. The recoveries of the 60 analytes on several adsorbents and their combinations were determined: A combination of a graphitized carbon black and a carbon molecular sieve showed great results for all analytes. Carbon molecular sieves adsorb water which can impair the analysis. Different options such as purging, the use of a drying system or splitting were investigated for water removal. This contribution will present experimental results supporting the standardization of a method for VVOC analysis. T2 - Indoor Air conference CY - Kuopio, Finland DA - 12.06.2022 KW - Analytical method KW - EN 16516 KW - ISO 16000-6 KW - VVOCs PY - 2022 AN - OPUS4-55282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lilensten, L. A1 - Provost, K. A1 - Perrière, L. A1 - Fonda, E. A1 - Couzinié, J. A1 - Amman, F. A1 - Radtke, Martin A1 - Dirras, G. A1 - Guillot, I. T1 - Experimental investigation of the local environment and lattice distortion in refractory medium entropy alloys N2 - EXAFS analysis of pure elements, binary and ternary equiatomic refractory alloys within the Nb-Zr-Ti-Hf- Ta system is performed at the Nb and Zr K-edges to analyze the evolution of the chemical local environ- ment and the lattice distortion. A good mixing of the elements is found at the atomic scale. For some compounds, a distribution of distances between the central atom and its neighbors suggests a distortion of the structure. Finally, analysis of the Debye-Waller parameters shows some correlation with the lat- tice distortion parameter δ², and allows to quantify experimentally the static disorder in medium entropy alloys. KW - BAMline KW - Refractory alloys KW - EXAFS KW - Debye-Waller parameter PY - 2022 DO - https://doi.org/10.1016/j.scriptamat.2022.114532 SN - 1359-6462 VL - 211 SP - 1 EP - 6 PB - Elsevier Ltd. AN - OPUS4-55287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Margreiter, R. A1 - Baumann, J. A1 - Mantouvalou, I. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Strub, E. T1 - Investigations on fire-gilding N2 - Fire-gilding is a historic technique for the application of golden layers on a number of different base materials utilizing a gold amalgam. This technique leaves a significant amount of Hg in the golden layer, giving archeometrists a reliable indicator to identify firegildings. Recent findings on presumably fire-gilded objects have shown in several cases significantly lower Hg content than previously studied objects. This prompted a synchrotron-based X-ray fluorescence investigation into the Hg distribution along the material–gilding interface, as well as a series of measurements regarding the Hg content development in fire-gilded samples during artificial aging. This work presents findings on laboratory-prepared fire-gildings, indicating an Hg enrichment at the interface of firegilded silver samples. Notably, such an enrichment is missing in fire-gilded copper samples. Further, it is confirmed that fire-gilded layers typically do not undercut an Hg bulk content of 5%. In this light, it seems improbable that ancient samples that contain <5% Hg are fire-gilded. The results presented in this study might lead to a non-destructive method to identify the Hg enrichment at the interface. This might be obtained by a combination of different non-destructive measurements and might also work unambiguously in samples in which the gold top layer is altered. KW - BAMline KW - X-Ray Fluorescence KW - Gilding KW - Depth profile KW - Archaeometry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552885 DO - https://doi.org/10.1111/arcm.12797 SN - 0003-813X SP - 1 EP - 14 PB - Wiley online library AN - OPUS4-55288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Bernhardt, Y. A1 - Csaszar, L. A1 - Dengiz, N. A1 - Fuchs, M. A1 - Gautzsch, T. A1 - Gohlke, Dirk A1 - Hahn-Jose, T. A1 - Heckel, Thomas A1 - Hillger, W. A1 - Hufschläger, Daniel A1 - Ilse, D. A1 - Kiel, M. A1 - Labud, P. A1 - Schubert, F. A1 - Sommerhuber, R. A1 - Szewieczek, A. A1 - Waschkies, T. T1 - Richtlinie zur Charakterisierung von luftgekoppelten Ultraschallwandlern N2 - Zur Charakterisierung von luftgekoppelten Ultraschallwandlern werden mehrere verschiedene Methoden und Verfahren angewendet. Durch die unterschiedlichen Herangehensweisen werden oft unterschiedliche Prüfkopfpara-meter und Schallfeldgrößen ermittelt, was einen direkten Vergleich von Datenblättern erschwert. Für die Charakterisierung von Kontakt- und Tauchtechnikprüfköpfen hat sich ISO 22232-2:2021 bereits etabliert, allerdings ist diese Norm nicht auf die luftgekoppelten Wandlertechnologien direkt übertragbar. Daher erkannten Hersteller, Forschungseinrichtungen und Anwender den Bedarf an einer Richtlinie zur einheitlichen Charakterisierung von luftgekoppelten Wandlern. Gemeinsam arbeiten sie aktuell im Rahmen des Unterausschusses „Luftgekoppelte Ultraschallprüfung“ der DGZfP an der Erstellung einer solcher Richtlinie mit dem Anspruch, die bestehende Normung um die luftgekoppelte Prüfung zu erweitern und somit die Vereinheitlichung der Charakterisierung dieser Wandler zu erleichtern. In diesem Beitrag wird ein Überblick über den geplanten Inhalt der Richtlinie und über die Methoden zur akustischen Charakterisierung von luftgekoppelten Ultraschallwandlern gegeben. Insbesondere werden verschiedene Methoden der Ermittlung von wichtigen Wandlerparametern wie z.B. Empfindlichkeit, Mittenfrequenz, Bandbreite, Fokusgröße und Fokusabstand dargestellt und verglichen. T2 - DGZfP-Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Lutgekoppelte Ultraschallprüfung KW - Prüfkopf KW - Charakterisierung KW - Richtlinie PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552918 SP - 1 EP - 7 AN - OPUS4-55291 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hillger, W. T1 - Luftultraschall mit Phased Array Technik N2 - Der Vortag berichtet über zwei Forschungsprojekte KALLUP (Vorrichtung zur Charakterisierung und Kalibrierung von luftgekoppelten Prüfköpfen) und PALUP (Phased-Array-Technik für Luftultraschall-Prüfungen). Projektpartner sind die BAM in Berlin und Hillger NDT. Die Phased-Array-Technik ermöglicht bekanntermaßen eine wesentlich flexiblere Anpassung der Ultraschallprüftechnik an unterschiedliche Prüfaufgaben als die klassische einkanalige Prüftechnik. Um diese Flexibilität auch bei berührungslosen Verfahren wie der Ankopplung über Luft zu erreichen, arbeiten die Partner BAM und Hillger NDT intensiv auf dem Gebiet. Entwickelt wurde ein achtkanaliger thermoakustischer Wandler, der als breitbandiger Phased-Array-Sender eingesetzt wird. Das Ziel im PALUP-Projekt ist die Entwicklung eines Phased-Array-Demonstrators mit Luftankopplung, wobei als Sender und Empfänger Sensoren aus zellulären Kunststoffmaterialien eingesetzt werden. Die Arrays erlauben durch das Umschalten der Elemente ein elektronisches Scannen, elektronisches Schwenken des Einschallwinkels und elektronisches Fokussieren, was bisher nur mit der Phased-Array-Technik mit Koppelmitteln möglich ist. Die Teilziele der BAM sind: die Entwicklung des Layouts für Array-Sender und -Empfänger, Auswahl des zellulären Kunststoffs für den Wandlerbau, Konzept und Bau des Sende- und Empfangssensors sowie die Charakterisierung der Sensoren. Die Teilziele von Hillger NDT sind: die Konzipierung der Prüfstrategie, Konzept und Bau der mehrkanaligen Sendetechnik, Konzept und Bau der mehrkanaligen Empfangstechnik, Entwicklung der Software für Datenerfassung. T2 - DGZfP-Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Luftgekoppelte Ultraschallprüfung KW - Phased-Array-Prüfköpfe KW - Thermoakustik KW - Ferroelektret PY - 2022 AN - OPUS4-55203 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raab, A. A1 - Vogl, Jochen A1 - Solovyev, N. T1 - Isotope signature of iron, copper and zinc in mouse models (L66 and 5XFAD) and their controls used for dementia research N2 - Introduction: The influence of copper, iron and zinc concentrations on the formation of ß-amyloid plaques and neurofibrillary tangles in Alzheimer’s disease (AD) is widely discussed in the community. The results from human and animal studies so far are mixed with some studies showing a correlation and others not. From a number of studies, it is known that disease state and isotopic composition of essential elements can be coupled. Aim: The aim of the study was to identify changes in element content and isotopic composition in two transgenic mouse models used in AD research compared to their genetic WT relatives and to establish whether element content and isotopic signature between different laboratories is comparable. Methods: ß-amyloid (5xFAD) and tau overexpressing (L66) mice together with their matching wild-types were bred at dedicated facilities in accordance with the European Communities Council Directive (63/2010/EU). Serum and brain were sampled after sacrifice and the samples distributed among the participants of the study. The tissues were acid digested for total element determination and high-precision isotope ratio determination. Element content was determined by either sector-field or quadrupole-based inductively coupled plasma mass spectrometry (ICPMS). For the determination of isotope ratios multi-collector ICPMS was used. Results: Total copper content was significantly higher for L66 and their matched WT compared to 5xFAD and WT. Brains of L66 mice contained more Fe in brain than their WT, Zn and Cu were not significantly different between L66 and WT. Whereas 5xFAD mice had a slightly lower Cu and slightly higher Zn concentration in brain compared to WT. The isotopic signature in brain of L66 mice for Fe was different from their controls, whereas Zn isotope ratios were influenced in 5xFAD mice compared to their WT. The Cu isotopic ratio did not seem to be influenced in either strain. In serum, the shifts were less pronounced. Conclusion: Even though neither Tau-protein nor amyloid precursor protein are known to be metal-dependent / -containing proteins, the overexpression of both influences the Fe, Cu and Zn metabolism in brain and to some extent also in serum as can be seen not only using total element determination but probably more clearly studying the isotopic signature of Fe, Cu and Zn. T2 - The International Conference of Trace Elements and Minerals (ICTEM) 2022 CY - Aachen, Germany DA - 05.06.2022 KW - Isotope ratio KW - Isotope delta value KW - Metrology KW - Alzheimer disease KW - Measurement uncertainty PY - 2022 AN - OPUS4-55204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schühle, Florian T1 - Bereitstellung qualitätsgesicherter VOC-Aufnahmeraten für axiale Passivsammler N2 - Quality assured uptake rates for passive sampling of indoor air VOCs Passive sampling of VOCs with Tenax® TA and thermal desorption GC-MS analysis is a simple, cost efficient and representative method to determine VOCs concentrations in indoor air. In theory, the uptake into the passive sampler is only dependent on the diffusion coefficient of the analyte in air and the geometry of the sampler (ideal adsorption). For characterization, the uptake rate (UR) is used, defined as the ratio of the uptaken mass and the product of ambient concentration and exposure time. Various reported effective uptake rates (UR,eff) differ considerably from ideal values (UR,id). Literature values in national and international standards, are essentially sorted by the applicable exposure time, while detailed information about the corresponding concentration range is lacking. Moreover the number of itemized substances is limited. The aim of this study was to review and expand this set of uptake rates by determination of own quality assured laboratory values.The determined uptake rates are considered accurate in terms of RSD and comparability to literature values and can be recommended for exposure times of seven days at 50 100 µg/m³ (approximately 100 300 ppm min). Seven day uptake rates in ISO16017 2 and ASTM D6196 are not generally suited for this purpose, as has been exemplarily shown for benzene. N2 - Die passive Probenahme von VOC (Volatile Organic Compounds) mit Tenax® TA und Thermodesorption GC/MS Analytik ist eine einfache, kosteneffiziente und repräsentative Methode zur Bestimmung der VOC-Konzentrationen in der Innenraumluft. In der Theorie ist die Stoffaufnahme in den Passivsammler nur abhängig vom Diffusionskoeffizienten der Substanz in Luft und der Geometrie des Sammlers (ideale Adsorption). Um sie zu charakterisieren, wird die Aufnahmerate (UR), definiert als Quotient der Massenaufnahme und dem Produkt aus Konzentration und Expositionszeit, verwendet. Viele effektive Aufnahmeraten (UR,eff) unterscheiden sich beträchtlich von idealen (theoretischen) Werten (UR,id). Literaturwerte sind in nationalen und internationalen Normen lediglich für bestimmte Expositionszeiten vorgegeben, während detaillierte Informationen über den zugehörigen Konzentrationsbereich fehlen. Außerdem ist die Anzahl der insgesamt in der Literatur beschriebenen Substanzen begrenzt. Das Ziel der vorgestellten Studie ist es diesen Fundus an Aufnahmeraten zu begutachten und zu prüfen und ihn durch die Bestimmung eigener qualitätsgesicherter Laborwerte zu ergänzen. Die bestimmten Aufnahmeraten werden als akkurat bezüglich ihrer relativen Standardabweichung und Vergleichbarkeit zu Literaturwerten betrachtet und können für Expositionszeiten von 7 Tagen bei Konzentrationen von 50 100 µg/m³ (ca. 100 300 ppm min) empfohlen werden. Die Sieben Tage Aufnahmeraten aus ISO16017 2 und ASTM D6196 sind nicht generell für diesen Zweck geeignet, wie exemplarisch für Benzol gezeigt wurde. T2 - Kongress 29. WaBoLu-Innenraumtage CY - Berlin, Germany DA - 24.05.2022 KW - IAQ KW - VOC KW - Passive sampling KW - Uptake rate PY - 2022 SN - 978-3-949241-04-8 AN - OPUS4-55209 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olino, M. A1 - Lugovtsova, Yevgeniya A1 - Memmolo, V. A1 - Prager, Jens T1 - Temperature Compensation Strategies for Lamb Wave Inspection using Distributed Sensor Networks N2 - The application of temperature compensation strategies is crucial in structural health monitoring approaches based on guided waves. Actually, the varying temperature influences the performance of the inspection system inducing false alarms or missed detection, with a consequent reduction of reliability. This paper quantitatively describes a method to compensate the temperature effect, namely the optimal baseline selection (OBS), extending its application to the case of distributed sensor networks (DSN). The effect of temperature separation between baseline time-traces in OBS are investigated considering multiple couples of sensors employed in the DSN. A combined strategy that uses both OBS and frequent value warning is considered. Theoretical results are compared, using data from two several experiments, which use different frequency analysis with either predominantly A0 mode or S0 mode data or both. The focus is given on the fact that different paths are available in a sensor network and several possible combination of results are available. Nonetheless, introducing a frequent value warning it is possible to increase the efficiency of the OBS approach making use of fewer signal processing algorithms. These confirm that the performance of OBS quantitatively agrees with predictions and also demonstrate that the use of compensation strategies improve detectability of damage. T2 - IEEE International Workshop on Metrology for AeroSpace CY - Pisa, Italy DA - 27.06.2022 KW - Ultrasound KW - Ultrasonic Guided Waves KW - Structural Health Monitoring PY - 2022 SN - 978-1-6654-1076-2 DO - https://doi.org/10.1109/MetroAeroSpace54187.2022.9856029 SP - 598 EP - 601 AN - OPUS4-55268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mueller, I. A1 - Freitag, S. A1 - Memmolo, V. A1 - Moix-Bonet, M. A1 - Möllenhoff, K. A1 - Golub, M. A1 - Sridaran Venkat, R. A1 - Lugovtsova, Yevgeniya A1 - Eremin, A. A1 - Moll, J. A1 - Tschöke, K. ED - Rizzo, P. ED - Milazzo, A. T1 - Performance Assessment for Artificial Intelligence-Based Data Analysis in Ultrasonic Guided Wave-Based Inspection: A Comparison to Classic Path-Based Probability of Detection N2 - Performance assessment for GuidedWave (GW)-based Structural Health Monitoring (SHM) systems is of major importance for industrial deployment. With conventional feature extraction methods like damage indices, pathbased probability of detection (POD) analysis can be realized. To achieve reliability quantification enough data needs to be available, which is rarely the case. Alternatives like methods for performance assessment on system level are still in development and in a discussion phase. In this contribution, POD results using an Artificial Intelligence (AI)-based data analysis are compared with those delivered by conventional data analysis. Using an open-access dataset from Open Guided Wave platform, the possibility of performance assessment for GW-based SHM systems using AI-based data analysis is shown in detail. An artificial neural network (ANN) classifier is trained to detect artificial damage in a stiffened CFRP plate. As input for the ANN, classical damage indicators are used. The ANN is tested to detect damage at another position, whose inspection data were not previously used in training. The findings show very high detection capabilities without sorting any specific path but only having a global view of current damage metrics. The systematic evaluation of the ANN predictions with respect to specific damage sizes allows to compute a probability of correct identification versus flaw dimension, somehow equivalent to and compared with the results achieved through classic path-based POD analysis. Also, sensitive paths are detected by ANN predictions allowing for evaluation of maximal distances between path and damage position. Finally, it is shown that the prediction performance of the ANN can be improved significantly by combining different damage indicators as inputs. T2 - 10th European Workshop on Structural Health Monitoring (EWSHM 2022) CY - Palermo, Italy DA - 04.07.2022 KW - Probability of Detection KW - Composites KW - Open Guided Waves Platform KW - Artificial Neural Network PY - 2022 SN - 978-3-031-07257-4 DO - https://doi.org/10.1007/978-3-031-07258-1 SN - 2366-2557 VL - 2 SP - 953 EP - 961 PB - Springer CY - Cham, Switzerland AN - OPUS4-55269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tschöke, K. A1 - Mueller, I. A1 - Memmolo, V. A1 - Sridaran Venkat, R. A1 - Golub, M. A1 - Eremin, A. A1 - Moix-Bonet, M. A1 - Möllenhoff, K. A1 - Lugovtsova, Yevgeniya A1 - Moll, J. A1 - Freitag, S. ED - Rizzo, P. ED - Milazzo, A. T1 - A Model-Assisted Case Study Using Data from Open Guided Waves to Evaluate the Performance of Guided Wave-Based Structural Health Monitoring Systems N2 - Reliability assessment of Structural Health Monitoring (SHM) systems poses new challenges pushing the research community to address many questions which are still open. For guided wave-based SHM it is not possible to evaluate the system performance without taking into account the target structure and applied system parameters. This range of variables would result in countless measurements. Factors like environmental conditions, structural dependencies and wave characteristics demand novel solutions for performance analysis of SHM systems compared to those relying on classical non-destructive evaluation. Such novel approaches typically require model-assisted investigations which may not only help to explain and understand performance assessment results but also enable complete studies without costly experiments. Within this contribution, a multi input multi output approach using a sparse transducer array permanently installed on a composite structure to excite and sense guided waves is considered. Firstly, the method and the analysis of path-based performance assessment are presented considering an open-access dataset from the Open Guided Wave platform. Then, a performance analysis of a guided wave-based SHM system using Probability of Detection is presented. To explain some unexpected results, the model-assisted investigations are used to understand the physical phenomena of wave propagation in the test specimen including the interaction with damage. Finally, issues and future steps in SHM systems’ performance assessment and their development are discussed. T2 - 10th European Workshop on Structural Health Monitoring (EWSHM 2022) CY - Palermo, Italy DA - 04.07.2022 KW - Performance assessment KW - Ultrasonic Guided Waves KW - Open Guided Waves Platform PY - 2022 SN - 978-3-031-07257-4 DO - https://doi.org/10.1007/978-3-031-07258-1 SN - 2366-2557 VL - 2 SP - 938 EP - 944 PB - Springer CY - Cham, Switzerland AN - OPUS4-55270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - von der Au, Marcus A1 - Faßbender, Sebastian A1 - Chronakis, Michail A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Size determination of nanoparticles by ICP-ToF-MS using isotope dilution in microdroplets N2 - Within this work, the combination of a microdroplet generator and an ICP-ToF-MS for nanoparticle analysis is presented. For the size determination of platinum nanoparticles an on-line isotope dilution analysis approach was developed. The 194Pt/195Pt isotopic ratio was used for the characterization of the particles, while the 182W/183W isotopic ratio was monitored simultaneously for mass bias correction. The on-line ID-MDG-sp-ICP-ToF-MS approach was deployed for the size determination of three platinum nanoparticle samples (50 nm, 63 nm, 70 nm); for validation, complementary size characterization techniques (sp-ICP-ToF-MS and TEM) were used. The robustness of this technique was evidenced, by using sodium chloride concentrations up to 100 mg L−1 as a matrix component. Our new on-line ID MDG-sp-ICP-ToF-MS approach is a promising tool for the fast and reliable determination of nanoparticles' size in severe matrix concentrations, e.g., environmental samples. KW - ICP-ToF-MS KW - Nanoparticles KW - Isotope Dilution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552727 DO - https://doi.org/10.1039/D2JA00072E SN - 0267-9477 VL - 37 IS - 6 SP - 1203 EP - 1207 PB - Royal Society of Chemistry AN - OPUS4-55272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Grotelüschen, Bjarne A1 - Bühling, Benjamin T1 - Impact-Echo Dataset "IE Platte" N2 - This dataset contains raw data resulting from Impact-Echo measurements at the reference concrete block "IE Platte", located at BAM (German Federal Institute for Materials Research and Testing). The specimen contains three polystyrene slabs and one polyethylene foil to act as reflectors. The specimen was produced in a three-step process. First, the base plate was cast. Second, the reflectors were taped to the base plate. Finally, the upper layer was cast on top of base plate and reflectors. A drawing is contained in the dataset. The Impact-Echo method is based on the excitation of the zero-group-velocity frequency of the first symmetric Lamb mode of a plate-like structure, in order to assess its thickness. Numerous publications elaborate on Impact-Echo theory, examples are (Gibson and Popovics 2005, Schubert and Köhler 2008 , Abraham and Popovics 2010). The measurements have been conducted using a setup that contains only commercially available components. The setup consists of an Olson CTG-2 concrete thickness gauge (Olsen Instruments, USA) for actuation and sensing and an 8-bit NI USB-5132 digital storage oscilloscope (National Instruments, USA) combined with the Echolyst software (Schweizerischer Verein für technische Inspektionen (SVTI), Switzerland) for data acquisition. Measurements were conducted using a grid of 29x29 points with a spacing of 50 mm. At each point 8192 samples were recorded at a sampling rate of 1 MS/s. The dataset contains the (X,Y) location in mm of the individual measurement points as well as the raw measurement data at those points. The data is provided in the formats *.mir/*.mhdr (Echolyst), *.npy (Python) and *.mat (Matlab) and *.csv to ease the import in various post-processing tools. KW - Concrete KW - Impact-Echo KW - Nondestructive testing PY - 2022 DO - https://doi.org/10.7910/DVN/EH4E9G PB - Harvard College CY - Cambridge, MA, USA AN - OPUS4-55279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Even, Morgane T1 - Weiterentwicklung und Validierung eines leistungsfähigen Verfahrens zur Bestimmung von VVOCs aus Bauprodukten und in der Innenraumluft N2 - Mehrere Aspekte wurden im Hinblick auf die Standardisierung eines geeigneten Verfahrens für die Analyse sehr flüchtiger organischer Verbindungen (VVOCs) untersucht. Die Verwendung gasförmiger Standards ist notwendig und es wurde ein stabiles Standardgasgemisch aus 60 Substanzen erfolgreich erzeugt und auf Stabilität und Reaktivität überprüft. Die Eignungsuntersuchung verschiedener Chromatographiesäulen ergab, dass PLOT-Säulen (Porous Layer Open Tubular) für die VVOC-Analytik gut geeignet sind. Für die 60 Analyten wurden Wiederfindungsraten auf mehreren Adsorbenzien und deren Kombinationen bestimmt. Dabei zeigte eine Kombination aus einem graphitierten Ruß und einem Kohlenstoff-Molekularsieb hervorragende Ergebnisse für alle Zielkomponenten. Nachteilig an Kohlenstoff-Molekularsieben ist, dass sie Wasser adsorbieren, was die Analyse beeinträchtigen kann. Zur Wasserentfernung wurden verschiedene Optionen wie das Trockenspülen oder der Einsatz eines Trocknungssystems untersucht. T2 - WaBoLu Innenraumtage CY - Berlin, Germany DA - 24.05.2022 KW - Analytische Methode KW - EN 16516 KW - ISO 16000-6 KW - VVOCs PY - 2022 AN - OPUS4-55281 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hassenstein, Christian A1 - Heckel, Thomas A1 - Prager, Jens A1 - Berendt, T. A1 - Voehringer, D. T1 - Robotergeführte Ultraschallprüfung von Gasturbinenschaufeln mit adaptiver TFM im ZfP 4.0-Umfeld N2 - Leit- und Laufschaufeln stationärer Gasturbinen sind im Betrieb anspruchsvollen Bedingungen ausgesetzt. Die Prüfung, Wartung und Reparatur der hochbelasteten Teile sind notwendig, um Sicherheit und Effizienz über längere Zeiträume zu gewährleisten. Eine der in diesem Prozess angewandten Methoden ist die Ultraschallprüfung. Im Zuge der fortschreitenden Digitalisierung ist es das Ziel des Projektes MRO 2.0, den Aufbereitungsvorgang um digitale Prozesse zu erweitern und somit zu modernisieren. Eine der Aufgaben ist es, dabei anstelle der konventionellen Ultraschallprüfung eine Array-Technik mit rekonstruierenden Verfahren einzusetzen und eine automatisierte, digital eingebundene Methode im Rahmen von ZfP 4.0 zu entwickeln. Um die Ist-Geometrie der Oberfläche und die verbleibende Wanddicke flächendeckend an den Turbinenschaufeln zu bestimmen, wird ein adaptives TFM Verfahren (Total Focusing Method) in Tauchtechnik eingesetzt, welches die Brechung der Schallwellen an der Grenzfläche zum Prüfkörper in der Rekonstruktion berücksichtigt. In der hierfür entwickelten Prüfanlage führt ein Roboterarm einen Array-Prüfkopf und scannt das Bauteil normal zur inspizierten Oberfläche. Somit kann ein 3D-Modell des Ist Zustandes des zu prüfenden Bauteils erstellt werden. Spezielle Herausforderungen an die Aufgabe stellen die komplexe Geometrie des Prüfobjektes sowie dessen geringe und ortsabhängige Wanddicke dar. Ein weiterer Fokus liegt auf der Optimierung der Prüfparameter, Verbesserung der Prüfgeschwindigkeit sowie der Zuverlässigkeit der Methode. In diesem Beitrag werden die während des Projektes entwickelte Methode und die im zweiten Projektjahr erarbeiteten Ergebnisse vorgestellt, mit dem Schwerpunkt auf die entwickelten Rekonstruktionsalgorithmen und den Versuchsaufbau. T2 - DGZfP Jahrestagung 2022 CY - Kassel, Germany DA - 23.05.2022 KW - Ultraschallprüfung KW - Turbinenschaufel KW - Phased Array KW - Total Focusing Method KW - Automatisierung KW - Tauchtechnik PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551881 UR - https://www.ndt.net/search/docs.php3?id=27055 SP - 1 EP - 11 PB - NDT.net AN - OPUS4-55188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schnur, C. A1 - Goodarzi, P. A1 - Lugovtsova, Yevgeniya A1 - Bulling, Jannis A1 - Prager, Jens A1 - Tschöke, K. A1 - Moll, J. A1 - Schütze, A. A1 - Schneider, T. T1 - Towards interpretable machine learning for automated damage detection based on ultrasonic guided waves N2 - Data-driven analysis for damage assessment has a large potential in structural health monitoring (SHM) systems, where sensors are permanently attached to the structure, enabling continuous and frequent measurements. In this contribution, we propose a machine learning (ML) approach for automated damage detection, based on an ML toolbox for industrial condition monitoring. The toolbox combines multiple complementary algorithms for feature extraction and selection and automatically chooses the best combination of methods for the dataset at hand. Here, this toolbox is applied to a guided wave-based SHM dataset for varying temperatures and damage locations, which is freely available on the Open Guided Waves platform. A classification rate of 96.2% is achieved, demonstrating reliable and automated damage detection. Moreover, the ability of the ML model to identify a damaged structure at untrained damage locations and temperatures is demonstrated. KW - Composite structures KW - Structural health monitoring KW - Carbon fibre-reinforced plastic KW - Interpretable machine learning KW - Automotive industry PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542060 DO - https://doi.org/10.3390/s22010406 SN - 1424-8220 VL - 22 IS - 1 SP - 1 EP - 19 PB - MDPI CY - Basel AN - OPUS4-54206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mellios, N. A1 - Oesch, Tyler A1 - Spyridis, P. T1 - Finite element modelling of UHPC under pulsating load using X-ray computed tomography based fiber distributions N2 - The benefits of including fibers in ultra-high performance concrete (UHPC) are attributed to their good bond with the matrix and, hence, an optimal utilization of their properties. At the same time, though, fiber reinforcement may contribute to anisotropy in the composite material and induce weak areas. The influence of the fibers’ orientation on the material properties is a matter of current scientific discourse and it is known to play a vital role in structural design. In the case studies presented herein, mechanical laboratory tests using pulsating load regimes on UHPC with a strength of more than 200 MPa were simulated by use of finite element models. The orientations of the fibers were measured for each test sample prior to failure using an X-ray computed tomography (CT) scanner, and these orientations are explicitly implemented into the model. The paper discusses the methodology of merging data retrieved by CT image processing and state-of-the-art FE simulation techniques Moreover, the CT scanning was carried out throughout the testing procedure, which further enables the comparison of the mechanical tests and the FE models in terms of damage propagation and failure patterns. The results indicate that the overall fiber configuration and behavior of the samples can be realistically modelled and validated by the proposed CT-FE coupling, which can enhance the structural analysis and design process of elements produced with steel fiber reinforced and UHPC materials. KW - Ultra-high performance concrete KW - Steel fiber reinforced concrete KW - Fiber orientation KW - X-ray computed tomography KW - Non-linear finite element modelling PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542105 DO - https://doi.org/10.1617/s11527-021-01833-4 SN - 1871-6873 VL - 55 IS - 1 SP - 1 EP - 20 PB - Springer CY - Dordrecht AN - OPUS4-54210 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moufid, M. A1 - Tiebe, Carlo A1 - El Bari, N. A1 - Bartholmai, Matthias A1 - Bouchikhi, B. T1 - Characterization of Unpleasant Odors in Poultry Houses Using Metal Oxide Semiconductor-Based Gas Sensor Arrays and Pattern Recognition Methods N2 - In this study, the ability of an electronic nose developed to analyze and monitor odor emissions from three poultry farms located in Meknes (Morocco) and Berlin (Germany) was evaluated. Indeed, the potentiality of the electronic nose (e-nose) to differentiate the concentration fractions of hydrogen sulfide, ammonia, and ethanol was investigated. Furthermore, the impact change of relative humidity values (from 15% to 67%) on the responses of the gas sensors was reported and revealed that the effect remained less than 0.6%. Furthermore, the relevant results confirmed that the developed e-nose system was able to perfectly classify and monitor the odorous air of poultry farms. T2 - 1st International Electronic Conference on Chemical Sensors and Analytical Chemistry CY - Online meeting DA - 01.07.2021 KW - Pattern recognition methods KW - Gas sensors KW - Electronic nose KW - poultry odorous air monitoring PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544005 UR - https://csac2021.sciforum.net/ DO - https://doi.org/10.3390/CSAC2021-10481 VL - 5 IS - 52 SP - 1 EP - 7 PB - MDPI AN - OPUS4-54400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ecke, Alexander T1 - An Immunosensor for Pharmaceutical Contaminants in Water Supply N2 - Contamination of drinking water with pharmaceuticals is an emerging problem and a potential health threat. Immunochemical methods based on the binding of the analyte to specific antibodies enable fast & cost-effective on-site analyses. Magnetic bead-based immunoassays (MBBAs) allow for implementation into an immunosensor for online testing. Particles are prepared by either coupling the analyte molecule (diclofenac) or the respective antibody (amoxicillin) to the surface. For miniaturization, detection is performed electrochemically (chronoamperometry) on a microfluidic chip. The developed immunosensor will enable detection of pharmaceuticals directly in water supply pipes. T2 - 11th SETAC Young Environmental Scientists Meeting CY - Online meeting DA - 07.03.2022 KW - Immunosensor KW - Magnetic Beads KW - Water Analysis KW - Electrochemistry KW - Microfluidics PY - 2022 AN - OPUS4-54432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zancajo, V. M. R. A1 - Lindtner, T. A1 - Eisele, M. A1 - Huber, A. J. A1 - Elbaum, R. A1 - Kneipp, Janina T1 - FTIR Nanospectroscopy Shows Molecular Structures of Plant Biominerals and Cell Walls N2 - Plant tissues are complex composite structures of organic and inorganic components whose function relies on molecular heterogeneity at the nanometer scale. Scattering-type near-field optical microscopy (s-SNOM) in the mid-infrared (IR) region is used here to collect IR nanospectra from both fixed and native plant samples. We compared structures of chemically extracted silica bodies (phytoliths) to silicified and nonsilicified cell walls prepared as a flat block of epoxy-embedded awns of wheat (Triticum turgidum), thin sections of native epidermis cells from sorghum (Sorghum bicolor) comprising silica phytoliths, and isolated cells from awns of oats (Avena sterilis). The correlation of the scanning-probe IR images and the mechanical phase image enables a combined probing of mechanical material properties together with the chemical composition and structure of both the cell walls and the phytolith structures. The data reveal a structural heterogeneity of the different silica bodies in situ, as well as different compositions and crystallinities of cell wall components. In conclusion, IR nanospectroscopy is suggested as an ideal tool for studies of native plant materials of varied origins and preparations and could be applied to other inorganic–organic hybrid materials. KW - Cells KW - Plants KW - Organic polymers KW - Silica KW - Infrared light PY - 2020 DO - https://doi.org/10.1021/acs.analchem.0c00271 SN - 0003-2700 VL - 92 IS - 20 SP - 13694 EP - 13701 PB - ACS Publications AN - OPUS4-54445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Giuseppe, Pignatelli A1 - Anne, Strasse A1 - Gumenyuk, Andrey A1 - Gornushkin, Igor B. T1 - Online monitoring of 3D printing of steel via optical emission spectroscopy N2 - Additive manufacturing by laser metal deposition (LMD) requires continuous online monitoring to ensure quality of printed parts. Optical emission spectroscopy (OES) is proposed for the online detection of printing defects by monitoring minute variations in the temperature of a printed spot during laser scan. A two-lens optical system is attached to a moving laser head and focused on a molten pool created on a substrate during LMD. The light emitted by the pool is collected by an ultraviolet–visible (UV–vis) spectrometer and processed. Two metrics are used to monitor variations in the surface temperature: the spectrally integrated emission intensity and correlation coefficient. The variations in the temperature are introduced by artificial defects, shallow grooves, and holes of various widths and diameters carved on a substrate surface. The metrics show sufficient sensitivity for revealing the surface defects, except for the smallest holes with an under-millimeter diameter. Additionally, numeric simulations are carried out for the detection of emission in the UV–vis and near-infrared (NIR) spectral ranges at various surface temperatures. It is concluded that both the metrics perform better in the NIR range. In general, this work demonstrates that spectrally resolved OES suits well for monitoring surface defects during 3D metal printing. KW - Process control KW - Additive manufacturing KW - Laser metal deposition KW - Optical emission spectroscopy KW - Optical sensor PY - 2022 DO - https://doi.org/10.1515/mt-2021-2082 VL - 64 IS - 1 SP - 24 EP - 32 PB - De Gruyter AN - OPUS4-54413 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Meermann, Björn T1 - Schnelle und einfache Extraktion von PFAS aus Bodenproben: Optimierte EOF-Bestimmung mittels HR-CS-GFMAS N2 - Per- und polyfluorierte Alkylsubstanzen (PFAS) bilden eine sehr komplexe Schadstoffgruppe mit über 6300 Einzelsubstanzen, die in vielfältiger Form in die Umwelt eingetragen werden. Für ein effektives Monitoring dieser Schadstoffklasse benötigt es ein Zusammenspiel aus Summenparameter-Analytik zur hot-spot-Identifizierung und Klassifizierung von Belastungssituationen sowie einer nachgeschalteten target-Analytik zur Identifizierung von Eintragswegen, die zugleich ein tieferes Verständnis von Transformationsprozessen ermöglicht. In diesem Beitrag präsentieren wir eine optimierte Extraktions-Methode für die PFAS-Summenparameteranalytik. Mit Hilfe dieser können bisher verwendete zeit- und kostenintensive Festphasenextraktionen (SPE) umgangen und PFAS-Extraktionseffizienzen gesteigert werden. Die methodische Bestimmungsgrenze (LOQ) war mit 10,30 μg/kg (Fluor pro Bodenprobe) ausreichend für alle 9 untersuchten Realbodenproben. KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - PFAS KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Extractable organically bound fluorine (EOF) KW - Solid-liquid extraction KW - Böden PY - 2022 UR - https://www.gdch.de/fileadmin/downloads/Netzwerk_und_Strukturen/Fachgruppen/Umweltchemie_Oekotoxikologie/mblatt/2022/Heft122.pdf SN - 1618-3258 VL - 28 IS - 1 SP - 12 EP - 15 PB - Gesellschaft Deutscher Chemiker AN - OPUS4-54417 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moufid, M. A1 - Tiebe, Carlo A1 - El Bari, N. A1 - Bartholmai, Matthias A1 - Bouchikhi, B. T1 - Combining of TD-GC-MS and home developed electronic nose for road traffic air monitoring N2 - In this work, we demonstrate the ability of an electronic nose system based on an array of six-semiconductor gas sensors for outdoor air quality monitoring over a day at a traffic road in downtown of Meknes city (Morocco). The response of the sensor array reaches its maximum in the evening of the investigated day which may due to high vehicular traffic or/and human habits resulting in elevated concentrations of pollutants. Dataset treatment by Principal Component Analysis and Discriminant Function Analysis shows a good discrimination between samples collected at different times of the day. Moreover, Support Vector Machines were used and reached a classification success rate of 97.5 %. Thermal Desorption-Gas Chromatography-Mass Spectrometry (TD-GC-MS) technique was used to validate the developed e-nose system by identifying the composition of the analyzed air samples. The discrimination obtained by e-nose system was in good agreement with the TD-GC-MS results. This study demonstrates the usefulness of TD-GC-MS and e-nose, providing high accuracy in discriminating outdoor air samples collected at different times. This demonstrates the potential of using the e-nose as a rapid, easy to use and inexpensive environmental monitoring system. T2 - 2021 IEEE International Conference on Design & Test of Integrated Micro & Nano-Systems (DTS) CY - Sfax, Tunisia DA - 07.06.2021 KW - GC-MS KW - Electronic nose KW - Gas sensors KW - Urban air monitoring PY - 2021 DO - https://doi.org/10.1109/DTS52014.2021.9498110 SP - 1 EP - 6 AN - OPUS4-54401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Martins, Ines T1 - Carbamazepine Dihydroxybenzoic Acid Cocrystals: Exploring Packing Interactions and Reaction Kinetics N2 - Herein, we present the mechanochemical formation of three new cocrystals containing the active pharmaceutical ingredient carbamazepine and dihydroxybenzoic acids as coformers (CBZ:2,4-DHBA 1:1, CBZ:2,5-DHBA 1:1, and CBZ:2,6-DHBA 1:1). Rietveld methods were used for three different purposes: (i) refining all structures solved using powder X-ray diffraction, (ii) performing a quantitative phase analysis of the diffraction data collected from ex situ mechanochemical reactions at different milling times, and (iii) determining the cocrystallization kinetic profiles. The rate of cocrystallization was found to be higher for the formation of CBZ:2,4-DHBA and CBZ:2,6-DHBA, reaching an equilibrium after 600 s of milling. In the case of CBZ:2,5-DHBA a short induction period of 20 s was detected prior to the start of the reaction and an equilibrium was reached after 1200 s. An empirical trend between the rate of cocrystallization and the structural complexity of the cocrystal product was found. The slowest cocrystallization rate observed for CBZ:2,5-DHBA corresponds to the crystal structure deviating substantially from the hydrogen-bonding motif found in the reactants. KW - Mechanochemistry KW - In situ real-time monitoring KW - Kinetics PY - 2021 DO - https://doi.org/10.1021/acs.cgd.1c00902 VL - 21 IS - 12 SP - 6961 EP - 6970 PB - ACS Publications AN - OPUS4-54407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blind, K. A1 - Krüger, M. A1 - Kinne, J. A1 - Mirtsch, Mona ED - Jacobs, K. T1 - Organisation Innovation in the Digital Layer: Exploring the Adoption of the Management System Standard ISO/IEC 27001 N2 - Despite the increasing relevance of cybersecurity for companies’ performance, there is limited research on the adoption of ISO/IEC 27001, an international information security management standard. The aim of our study is to expand this limited body of literature. First, we analyse the influence of companies’ networks on the adoption of ISO/IEC 27001 as an organisational innovation based on firm website data and their hyperlinks, using the entire population of ISO/IEC 27001 certified firms identified via web mining. Second, we validate the method of constructing and analysing companies’ “digital layer” following the call for new methodological approaches to study the organisational adoption of innovations. Our findings reveal that companies' decision to adopt ISO/IEC 27001 increases significantly with their number of linkages to other companies and to those having the same certificate. Finally, their cognitive and organisational distances to linked partners have the expected inverted u-shaped influence on their own adoption decision. T2 - 11th International Conference on Standardisation and Innovation in Information Technology (SIIT 2021) CY - Aachen, Germany DA - 06.09.2021 KW - Information Security KW - Hyperlinks KW - Management system standard KW - Digital Layer PY - 2021 SN - 978-3-95886-421-4 SP - 95 PB - Verlagshaus Mainz GmbH Aachen CY - Mainz AN - OPUS4-54411 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rautenberg, Max T1 - Ca-MOFs with varying fluorination degree N2 - In current Li-ion batteries electrode materials consist typically of inorganic materials, such as LiCoO2, LiNixCoyMn1-zO2, LiFePO4, Li4Ti5O12. These materials struggle with toxicity or limited mineral resources, making them expensive. Therefore, eco-friendly, sustainable, and low-cost alternatives are researched for in recent years. A series of organic compounds were investigated as electrode materials for alkali-ion batteries. Among them organic carbonyl-based materials show reversible storage of lithium- or sodium-ions. Metal terephthalates stand out with their easy synthesis, moderate operational voltage and enhanced dissolution stability compared to other organic compounds. One degradation pathway consists of the dissolution of the electrode material by HF, formed in a side reaction by water and the fluorous electrolyte. Fluorinated metal terephthalates could offer higher dissolution stability against HF and less contamination by water due to their increased hydrophobicity. The goal of this project is the synthesis and the investigation of the formation mechanism of a series of calcium-based MOFs with increasing fluorine content. For this purpose, we aimed for the construction of calcium-based MOFs with terephthalic acid (H2-pBDC), 2-fluoro-terephthalic acid (H2-2F-pBDC), 2,3,4,5-tetrafluoroterephthalic acid (H2-pBDC-F4), isophthalic acid (H2-mBDC) and 5-fluoro-isophthalic acid (H2-5F-mBDC). T2 - SFB 1349 Wintersymposium 2022 CY - Berlin, Germany DA - 15.03.2022 KW - Mechanochemistry KW - Electrode materials KW - Fluorinated MOFs KW - In situ PXRD PY - 2022 AN - OPUS4-54478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schwaar, Timm T1 - Entwicklung von multidimensionalen Hochdurchsatzmethoden zur Analyse von partikelbasierten Peptidbibliotheken N2 - Ziel dieser Arbeit war die Entwicklung einer Methode zur Hochdurchsatzanalyse von partikelgebundenen Split-and-Mix-Peptidbibliotheken. Dabei wurde ein System entwickelt, das Partikelbibliotheken in kurzer Zeit auf ihre Bindung zu einem Zielmolekül hin untersucht und im nächsten Schritt eine direkte „Ein-Partikel“-Sequenzierung der Peptide von der festen Phase ermöglicht. Die Analyse der Bindung eines Zielmoleküls an ein selektiv bindendes Peptid wurde dabei in einem Modellsystem simuliert. Dazu wurde FITC-markiertes Neutravidin 3 mit festphasengebundenen biotinylierten und nicht-biotinylierten Peptiden inkubiert. Die Bindung von Neutravidin-FITC an die biotinylierten Peptide konnte erfolgreich mittels eines Fluoreszenzmikroskops nachgewiesen werden, wobei diese Methode für eine Hochdurchsatzanalyse ungeeignet war. So wurde die Analyse des Fluoreszenzassays auf einen Microarrayscanner übertragen (siehe Abbildung 33). Dies gelang erfolgreich wobei die hohe Eigenfluoreszenz des Tentagel-Harzes zu falsch positiven Ergebnissen führte. Mit einem Wechsel zum längerwelligen Fluoreszenzfarbstoff ATTO-633 konnten falsch positive Ergebnisse vermieden werden. Somit wurde die zeitintensive Fluoreszenzanalyse von einem Fluoreszenzmikroskop erfolgreich auf einen Microarrayscanner übertragen, welcher in kurzer Zeit (ca. 5 min pro Objektträger) eine Vielzahl an peptidbeladenen Partikeln gleichzeitig analysieren kann. KW - Peptide KW - OBOC library KW - MALDI-TOF-MS KW - Sequencing KW - Ladder sequencing KW - Solid-phase peptide synthesis KW - SPPS KW - Microarray KW - Fluorescence label KW - Polymer beads KW - Tentagel KW - Merrifield KW - Split and mix technology PY - 2015 SP - 1 EP - 80 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54644 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Paul, Martin T1 - Microarrays for the screening of monoclonal antibodies from supernatants N2 - In this thesis a protocol based on a direct competitive and non-competitive immunoassay using the microarray format was developed to screen emulated hybridoma supernatants against the drug carbamazepine (CBZ). As support, epoxy slides were manufactured by coating microscope glass slides with epoxy silanes. The manufactured epoxy slides showed similar capacity for protein immobilization as commercially available NEXTERION slides, but showed a higher autofluorescence background. On the epoxy slides, protein A, Cys-A, G and Cys-G were immobilized as antibody capturing coating. It could be shown that the Cys-tag considerably increased the immobilization of all compared proteins, especially of protein G. Protein Cys-G immobilized at pH 8-9 was considered the most suitable protein for antibody immobilization due to good spot uniformity and a high binding capacity for IgG. Additionally, in immobilization experiments it could be shown, that 10-500 fold excess of bovine IgG, introduced by two different fetal bovine serum (FBS) products, showed no significant competition on the immobilization of mice or goat IgG on protein Cys-G. To examine the captured antibodies for affinity to CBZ, the CBZ-TOTA-DY654 tracer was custom synthesized. It could be demonstrated, that the tracer antibody interaction was competitive with the tracer precursor, CBZ-TOTA-NH2 and CBZ. Furthermore, the synthesized tracer was also successfully used by externals to evaluate CBZ affine hybriodoma cells in flow cytometry. In the simulated screening, five antibodies with known affinity to CBZ were diluted in a cell culture medium. The screening method allowed to differentiate between affine antibodies (IC50 < 20 µg/ml) and unaffine antibodies (IC50 > 20 µg/ml), when concentrations of 0.1 µg/ml IgG or greater have been used. Of five applied antibodies, all highly affine clones (CE2 and B3212M) were reported as positives while no false-positive samples were observed. The screening included competitive, with around 89500 fold excess of CBZ, and non-competitive tracer incubation on different segments of the same chip, which resulted in total signal suppression on the competitive segment. The screening was performed in 20 hours, only a few nanoliters, of each simulated supernatant, were consumed in the screening process, furthermore in the method standard 96 well MTPs were used and no cleanroom facilities were required. KW - Carbamazepine KW - Microscopic slides KW - Protein A cys KW - Competition KW - Epoxy silanes KW - Supernatant KW - Antibody immobilization PY - 2017 SP - 1 EP - 96 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54645 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bienwald, Frank T1 - Optimierung der Aminosäureanalytik aromatischer Aminosäuren mittels HPLC N2 - Ausgehend von dem in der Literatur beschriebenen Verfahren zur Bestimmung aromatischer Aminosäuren konnte eine Analysemethode zur Proteinbestimmung über die optische Detektion von Tyrosin und Phenylalanin nach chromatographischer Trennung der Protein-Hydrolysate entwickelt werden, die gegenüber dem Verfahren aus der Literatur erhebliche Vorteile besitzt. Der Einsatz von Rundbodenvials stellt eine Neuerung und kostengünstige Alternative zu der konventionellen Hydrolyse in Vakuumhydrolyseröhrchen wie auch zu den Mikrowellenvials der Mikrowellenhydrolyse dar, die das Potential für Miniaturisierungen der Proben hat und sich zudem für große Probendurchsätze eignet. Anstelle der Mikrowellenheizungen wurde ein konventionelles Ölbad als Heizquelle verwendet. Somit ergibt sich eine Verbesserung auch darin, dass diese Methode geringere Geräteinvestitionen erfordert. Wie die Ergebnisse nahelegen, sind sowohl Salzsäure als auch Bromwasserstoffsäure geeignete Reagenzien, die bei der sauren Hydrolyse von Proteinen verwendet werden können. Mit Hilfe antioxidativer Zusätze können Nebenreaktionen erfolgreich vermieden werden. Hier haben sich L-Cystein und Oxalsäure als wirkungsvolle Additive herausgestellt. Wichtige Verbesserungen betreffen vor allem die Zeitersparnis bei der Hydrolyse, die Aufarbeitung der Hydrolysate und die chromatographischen Separationen. Erstere konnte gegenüber der konventionellen Methode von 22 Stunden auf 45 Minuten reduziert werden. Die chromatographische Trennung wurde so weit optimiert, dass die Laufzeit von 64 auf 35 Minuten verkürzt werden konnte. Zudem konnte auf das zeitraubende und kontaminationsanfällige Eindampfen der Hydrolysate verzichtet werden. Während der Aufarbeitung der Hydrolysate konnten die Menge eingesetzter Chemikalien reduziert und damit mögliche Störungen während der optischen Detektion verringert werden. Letztere wurde zum einen durch das Einbeziehen der UV-Absorption bei 260 nm erweitert, sodass eine Alternative zur Absorption bei 215 nm vorliegt, die ebenere Basislinien im Chromatogramm ermöglicht. Zum anderen wurde gezeigt, dass mit Hilfe der Fluoreszenz die Empfindlichkeit der Methode gegenüber der UV-Absorption erheblich verbessert werden kann. Anhand der Probe eines Birkenpollenextraktes ließ sich die Anwendbarkeit der optimierten Methode auf Realproben demonstrieren. KW - Aromatische Aminosäuren KW - Aromatic amino acid analysis KW - AAAA KW - Phenylalanine KW - Tyrosine KW - Hydrochloric acid KW - Hydrobromic acid KW - HCl KW - HBr KW - Chromatographie KW - Reversed-phase KW - Hydrolysis KW - AdvanceBio Peptide Map KW - PRP-C18 PY - 2017 SP - 1 EP - 71 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54650 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien T1 - Thermographic testing using 2D pseudo-random illumination and photothermal super resolution reconstruction N2 - Due to the diffusive nature of heat propagation in solids, the detection and resolution of internal defects with active thermography based non-destructive testing is commonly limited to a defect-depth-to-defect-size ratio greater than or equal to one. In the more recent past, we have already demonstrated that this limitation can be overcome by using a spatially modulated illumination source and photothermal super resolution-based reconstruction. Furthermore, by relying on compressed sensing and computational imaging methods we were able to significantly reduce the experimental complexity to make the method viable for investigating larger regions of interest. In this work we share our progress on improving the defect/inhomogeneity characterization using fully 2D spatially structured illumination patterns instead of scanning with a single laser spot. The experimental approach is based on the repeated blind pseudo-random illumination using modern projector technology and a high-power laser. In the subsequent post-processing, several measurements are then combined by taking advantage of the joint sparsity of the defects within the sample applying 2D-photothermal super resolution reconstruction. Here, enhanced nonlinear convex optimization techniques are utilized for solving the underlying ill-determined inverse problem for typical simple defect geometries. As a result, a higher resolution defect/inhomogeneity map can be obtained at a fraction of the measurement time previously needed. T2 - Thermosense: Thermal Infrared Applications XLIV CY - Orlando, FL, USA DA - 05.04.2022 KW - Thermography KW - Super resolution KW - NDT KW - Material testing KW - Internal defects KW - DMD KW - DLP PY - 2022 AN - OPUS4-54667 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Getenet, M. A1 - Garcia-Ruiz, J. M. A1 - Otálora, F. A1 - Emmerling, Franziska A1 - Al-Sabbagh, Dominik A1 - Verdugo-Escamilla, E. T1 - A comprehensive methodology for monitoring evaporitic mineral precipitation and hydrochemical evolution of saline lakes: The case of Lake Magadi soda brine (East African Rift Valley, Kenya) N2 - Lake Magadi, East African Rift Valley, is a hyperalkaline and saline soda lake highly enriched in Na+, K+, CO32–, Cl–, HCO3–, and SiO2 and depleted in Ca2+ and Mg2+, where thick evaporite deposits and siliceous sediments have been forming for 100 000 years. The hydrogeochemistry and the evaporite deposits of soda lakes are subjects of growing interest in paleoclimatology, astrobiology, and planetary sciences. In Lake Magadi, different hydrates of sodium carbonate/bicarbonate and other saline minerals precipitate. The precipitation sequence of these minerals is a key for understanding the hydrochemical evolution, the paleoenvironmental conditions of ancient evaporite deposits, and industrial crystallization. However, accurate determination of the precipitation sequence of these minerals was challenging due to the dependency of the different hydrates on temperature, water activity, pH and pCO2, which could induce phase transformation and secondary mineral precipitation during sample handling. Here, we report a comprehensive methodology applied for monitoring the evaporitic mineral precipitation and hydrochemical evolution of Lake Magadi. Evaporation and mineral precipitations were monitored by using in situ video microscopy and synchrotron X-ray diffraction of acoustically levitated droplets. The mineral patterns were characterized by ex situ Raman spectroscopy, X-ray diffraction, and scanning electron microscopy. Experiments were coupled with thermodynamic models to understand the evaporation and precipitation-driven hydrochemical evolution of brines. Our results closely reproduced the mineral assemblages, patterns, and textural relations observed in the natural setting. Alkaline earth carbonates and fluorite were predicted to precipitate first followed by siliceous sediments. Among the salts, dendritic and acicular trona precipitate first via fractional crystallization─reminiscent of grasslike trona layers of Lake Magadi. Halite/villiaumite, thermonatrite, and sylvite precipitate sequentially after trona from residual brines depleted in HCO3–. The precipitation of these minerals between trona crystals resembles the precipitation process observed in the interstitial brines of the trona layers. Thermonatrite precipitation began after trona equilibrated with the residual brines due to the absence of excess CO2 input. We have shown that evaporation and mineral precipitation are the major drivers for the formation of hyperalkaline, saline, and SiO2-rich brines. The discrepancy between predicted and actual sulfate and phosphate ion concentrations implies the biological cycling of these ions. The combination of different in situ and ex situ methods and modeling is key to understanding the mineral phases, precipitation sequences, and textural relations of modern and ancient evaporite deposits. The synergy of these methods could be applicable in industrial crystallization and natural brines to reconstruct the hydrogeochemical and hydroclimatic conditions of soda lakes, evaporite settings, and potentially soda oceans of early Earth and extraterrestrial planets. KW - Crystallization KW - Precipitation KW - Crystals KW - Evaporation KW - Minerals PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546712 DO - https://doi.org/10.1021/acs.cgd.1c01391 SN - 1528-7483 VL - 22 IS - 4 SP - 2307 EP - 2317 PB - ACS Publications CY - Washington, DC AN - OPUS4-54671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramin, Steffen T1 - Antibody-based SAW sensor for the detection of explosives N2 - One of the important analytical challenges is the fast and reliable trace detection of explosives in the context of security issues, ammunition disposal, and environmental pollution. Antibodies (Ab) are a promising tool for this purpose and the combination with a surface acoustic wave (SAW) sensor opens the opportunity of highly selective and fast, label-free detection. A robust and sensitive method for the detection of the explosive trinitrotoluene (TNT) was developed. The detection limit was determined to be around 0.5 μg/L. The fast signal response of less than 1 minute shows that this approach is suitable for security and other time-critical applications. In addition, the very low crossreactivity highly reduces the number of false-positives in relation to competing techniques, including sniffer dogs. Due to the multianalyte ability of the SAW system, several explosives might be detected in parallel. Terminal amino groups were functionalized with trinitrophenyl (TNP) groups by reaction with trinitrobenzene sulfonic acid (TNBS). In less than 1 minute, a good signal response was obtained. 50 μL of sample was used. No non-specific interaction with the SAM surface was observed. A complete measuring cycle needed 19 minutes including a surface regeneration step with 50 μL of acetonitrile/water/propionic acid (50:50:1) and 150 μL of SDS solution (0.1 %, pH 1 with 100 mM glycine and 100 mM NaCl). A good long-term stability could be shown for at least 6 hours. Two polyclonal antibodies (R1, R2, affinity purified with Protein A) and a monoclonal antibody (A1.1.1) were tested successfully. A commercially available SAW sensor (sam5 blue, SAW Instruments) was used for liquid handling and detection. Self-assembled monolayers (SAM) of alkanethiol derivatives were prepared on gold surfaces leading to non-fouling and hydrophilic properties, due to attached polyethylene glycol (PEG) residues. A continuous flow of buffer (phosphate-buffered saline, PBS plus Tween 20) of 100 μL/min was applied to the sensor system. TNT antibodies were pre-incubated with the samples containing traces of explosives. Polyclonal and monoclonal antibodies were tested. The limit of detection (LOD) was determined to 0.5 μg/L for all three antibodies (3s from 12 replicates). T2 - ANAKON 2013 CY - Essen, Germany DA - 04.03.2013 KW - Surface acoustic wave sensor KW - SAW KW - Explosives KW - TNT KW - Trinitrotoluene KW - SAM KW - Self-assembled monolayer KW - Gold surface KW - Hexadecanethiol KW - PEG KW - Polyethylene glycol KW - TNBS KW - Hapten KW - Amino-PEG PY - 2013 UR - https://f1000research.com/posters/5-1352 DO - https://doi.org/https://doi.org/10.7490/f1000research.1112309.1 AN - OPUS4-54677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahmadi, Samim A1 - Kästner, L. A1 - Hauffen, Jan Christian A1 - Jung, P. A1 - Ziegler, Mathias T1 - Photothermal-SR-Net: A customized deep unfolding neural network for photothermal super resolution imaging N2 - This article presents deep unfolding neural networks to handle inverse problems in photothermal radiometry enabling super-resolution (SR) imaging. The photothermal SR approach is a well-known technique to overcome the spatial resolution limitation in photothermal imaging by extracting high-frequency spatial components based on the deconvolution with the thermal point spread function (PSF). However, stable deconvolution can only be achieved by using the sparse structure of defect patterns, which often requires tedious, handcrafted tuning of hyperparameters and results in computationally intensive algorithms. On this account, this article proposes Photothermal-SR-Net, which performs deconvolution by deep unfolding considering the underlying physics. Since defects appear sparsely in materials, our approach includes trained block-sparsity thresholding in each convolutional layer. This enables to super-resolve 2-D thermal images for nondestructive testing (NDT) with a substantially improved convergence rate compared to classic approaches. The performance of the proposed approach is evaluated on various deep unfolding and thresholding approaches. Furthermore, we explored how to increase the reconstruction quality and the computational performance. Thereby, it was found that the computing time for creating high-resolution images could be significantly reduced without decreasing the reconstruction quality by using pixel binning as a preprocessing step. KW - Deep unfolding KW - Defect reconstruction KW - Elastic net KW - Inverse problems KW - Iterative shrinkage thresholding KW - Neural network KW - Nondestructive testing (NDT) KW - Photothermal imaging KW - Super resolution (SR) KW - Thermography PY - 2022 DO - https://doi.org/10.1109/tim.2022.3154803 SN - 1557-9662 VL - 71 SP - 1 EP - 9 PB - IEEE AN - OPUS4-54678 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Fischer, Janina T1 - Suspensionsarray-Fluoreszenzimmunoassay zur Multiplexbestimmung von SARS-CoV-2-Antikörpern N2 - Übergeordnetes Ziel der Arbeit war die Entwicklung und Optimierung eines Suspensionsarray-Fluoreszenzimmunoassays (SAFIA) für die simultane Bestimmung verschiedener gegen SARS-CoV-2-Proteine gerichtete Antikörper mittels Multiplexdetektion in komplexen Matrices wie humanen Blutserumproben. KW - SARS-CoV-2 KW - Corona KW - COVID-19 KW - Coronavirus KW - Virus KW - Spike-Protein KW - Nucleocapsid-Protein KW - RBD KW - SAFIA KW - LFIA KW - ELISA KW - Partikel KW - Mutationen KW - Neutralisierende Antikörper KW - Durchflusszytometrie KW - ACE2 PY - 2022 SP - 1 EP - 99 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54722 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfender, Max T1 - Einführung in das Leitthema: Prüfprobleme bei Verbundwerkstoffen N2 - Die Prüfprobleme bei Verbundwerkstoffen sind im wesentlichen bestimmt durch die Zweckbestimmung des betreffenden Gegenstandes, die materielle und organisatorische Basis für die Verwirklichung des Vorhabens, die untersuchende und vergleichende Auswahl geeigneter Stoffe und Verarbeitungsverfahren und durch die bestätigende und deshalb meist komplexe Prüfung seiner Funktion mit vorgegebenem Leitwert und darauf bezogenen Variablen bei oft nicht als Konstanten beherrschbaren Parametern. Die erfolgreiche Lösung einer solchen Aufgabe setzt voraus die ausreichende Kenntnis physikalischer, chemischer, mechanischer und technologischer Eigenschaften von verfügbaren und preiswürdigen Stoffen und Stoffzuständen, deren Beeinflußbarkeit und deren Auswirkungen auf den angestrebten Zweck einschließlich erwünschter belangloser oder auch unerwünschter aber erträglicher oder zusätzlich zu kompensierender Nebenwirkungen. Dafür wiederum braucht man ausreichende qualitative und quantitative Vorstellungen über die mit der angestrebten Funktion zusammenhängenden physikalischen Vorgänge, mechanischen Anstrengungen und chemischen Einwirkungen in dem so bedingten Verbundsystem von Werkstoffen entsprechender Eigenschaften. Aufgaben dieser Art sind z. B. Konstruktionen für die Wandlung, Verteilung, Nutzung oder Abwehr von Energie für die Herstellung, die Verarbeitung und den Transport von Stoffen, für die Darstellung von Wohnung, Kleidung und Nahrung sowie jener materiellen und organisatorischen Voraussetzungen, die dem Menschen als Gesellschaftswesen und über den physischen Bereich hinaus dienen. Hinweisende Beispiele zeigen, daß die Problematik der Prüfung von Verbundwerkstoffen am zuverlässigsten erfaßt und beherrscht werden kann, wenn die Kenntnis der Eigenschaften von Stoffen und Materialien dem konstruktiv zu behandelnden Funktionszweck entspricht, dadurch eine souveräne Auswahl im Sinne einer weiter reichenden Kombination einzelner hervorragender Eigenschaften möglich ist und das Geplante als geschaffene Wirklichkeit durch den prüfenden Versuch und die beobachtete Bewährung bestätigt wird. T2 - DVM-Tag 1967 CY - Würzburg, Germany DA - 20.04.1967 PY - 1967 AN - OPUS4-54751 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altenburg, T. A1 - Giese, S. A1 - Wang, S. A1 - Muth, Thilo A1 - Renard, B.Y. T1 - Ad hoc learning of peptide fragmentation from mass spectra enables an interpretable detection of phosphorylated and cross-linked peptides N2 - Mass spectrometry-based proteomics provides a holistic snapshot of the entire protein set of living cells on a molecular level. Currently, only a few deep learning approaches exist that involve peptide fragmentation spectra, which represent partial sequence information of proteins. Commonly, these approaches lack the ability to characterize less studied or even unknown patterns in spectra because of their use of explicit domain knowledge. Here, to elevate unrestricted learning from spectra, we introduce ‘ad hoc learning of fragmentation’ (AHLF), a deep learning model that is end-to-end trained on 19.2 million spectra from several phosphoproteomic datasets. AHLF is interpretable, and we show that peak-level feature importance values and pairwise interactions between peaks are in line with corresponding peptide fragments. We demonstrate our approach by detecting post-translational modifications, specifically protein phosphorylation based on only the fragmentation spectrum without a database search. AHLF increases the area under the receiver operating characteristic curve (AUC) by an average of 9.4% on recent phosphoproteomic data compared with the current state of the art on this task. Furthermore, use of AHLF in rescoring search results increases the number of phosphopeptide identifications by a margin of up to 15.1% at a constant false discovery rate. To show the broad applicability of AHLF, we use transfer learning to also detect cross-linked peptides, as used in protein structure analysis, with an AUC of up to 94%. KW - Mass spectrometry KW - Machine learning KW - Deep learning KW - Peptide identification PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547580 DO - https://doi.org/10.1038/s42256-022-00467-7 SN - 2522-5839 VL - 4 SP - 378 EP - 388 PB - Springer Nature CY - London AN - OPUS4-54758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska T1 - Charakterisierung von Salzbeton und alkali-aktivierten Material basierend auf der Schallemissionsanalyse N2 - Nach einer kurzen Einführung in die Schallemissionsprüfung und -Analyse wird ein Versuchsstand vorgestellt, der im Rahmen des Themenfeldprojektes Seal Waste Safe installiert wurde. Schwerpunkt des Vortrages sind die Schallemissionsmessungen an einem 150 l Demonstrator aus Salzbeton und einem weiteren aus alkali-aktiviertem Material. Neben der konventionellen Schallemissionsanaylse mit Aktivitäts- und Intensitätsparametern der Zeitsignale, werden auch frequenzbasierte Parameter zur Analyse andiskutiert. N2 - After a brief introduction to acoustic emission testing and analysis, an experimental test setup is presented, which was part of the Seal Waste Safe project (internal BAM project 2019-2022). Herein, the acoustic emission measurements of a 150 l demonstrator made of salt concrete and another one made of alkali-activated material are focused. In addition to the conventional acoustic emission analysis regarding the activity and intensity parameters of the detected time signals, also frequency-based parameters were discussed for analysis. T2 - Dauerhafte Verschlussbauwerke für Endlager CY - Online meeting DA - 14.2.2022 KW - Acoustic Emission KW - Schallemission KW - Salzbeton KW - Alkali aktiviertes Material KW - Geopolymer PY - 2022 AN - OPUS4-54937 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Veico, V. P. A1 - Karlagina, Yu. Yu. A1 - Samokhvalov, A. A. A1 - Polyakov, D. S. A1 - Manokhin, S. S. A1 - Radaev, M. M. A1 - Odintsova, G. V. A1 - Gornushkin, Igor B. T1 - Surface Structuring and Reverse Deposition of Nanoporous Titanium Oxides by Laser Ablation of Titanium in Air N2 - The deposition of titanium oxides during titanium laser ablation in air has been experimentally and numerically investigated. A titanium sample was irradiated by nanosecond pulses from an Yb-fber laser with a beam scanned across the sample surface for its texturing. As a result, the hierarchical structure was observed consisting of a microrelief formed by the laser ablation and a nanoporous coating formed by the reverse deposition from the laser induced plasma plume. The chemical and phase composition of the nanoporous coating, as well as the morphology and structure of the surface, were studied using scanning electron microscopy, atomic force microscopy, and X-ray microanalysis. It was found that the deposit consists mostly of porous TiO2 with 26% porosity and inclusions of TiO, Ti2O3, and Ti2O3N. Optical emission spectroscopy was used to control the plasma composition and estimate the effective temperature of plasma plume. The chemical-hydrodynamic model of laser induced plasma was developed to get a deeper insight into the deposition process. The model predicts that condensed titanium oxides, formed in peripheral plasma zones, gradually accumulate on the surface during the plasma plume evolution. A satisfactory agreement between the experimental and calculated chemical composition of the plasma plume as well as between the experimental and calculated composition and thickness of the deposited film was demonstrated. This allows a cautious conclusion that the formation of condensed oxides in the plasma and their consequent deposition onto the ablation surface are among the key mechanisms of formation of porous surface films. KW - Laser ablation KW - Laser induced plasma deposition KW - Surface coating KW - Titanium dioxide KW - Hydrodynamic model KW - Plasma chemistry KW - Emission spectroscopy PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548555 DO - https://doi.org/10.1007/s11090-022-10256-0 VL - 42 IS - 4 SP - 923 EP - 937 PB - Springer AN - OPUS4-54855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Veiko, V. P. A1 - Karlagina, Y. Y. A1 - Samokhvalov, A. A. A1 - Polyakov, D. S. T1 - Equilibrium model of titanium laser induced plasma in air with reverse deposition of titanium oxides N2 - A chemical-hydrodynamic model of laser induced plasma is developed to study a process of deposition of titanium oxides from titanium laser induced plasma to the titanium target surface. The model is relevant to texturing and coating of titanium bone implants that is done by scanning the ablation laser across implant surfaces. Such the procedure improves the biocompatibility and durability of the implants. The model considers plasma chemical reactions, formation of condensed species inside the plasma plume, and deposition and accumulation of these species on the ablation surface. A chemical part of the model is based on minimization of Gibbs free energy of the chemical system; it is used to calculate the chemical composition of the plasma. A hydrodynamic part uses the 2D fluid-dynamic equations that model a 3D axisymmetric plasma plume and assumes the mass and energy exchange between the plasma and the surface. The initial parameters for the model are inferred from experiment. The model shows that condensed titanium oxides, mostly TiO2, form in a peripheral plasma zone and gradually adhere to the surface during the plasma plume evolution. The model predicts the major component and thickness of the deposit and can be applied for the optimization of experiments aimed at surface modification. KW - Fluid dynamic model KW - Plasma chemistry KW - Laser ablation KW - Laser induced plasma deposition KW - Surface coating KW - Titanium dioxide PY - 2022 DO - https://doi.org/10.1016/j.sab.2022.106449 SN - 0038-6987 SN - 0584-8547 VL - 193 SP - 1 EP - 7 PB - Elsevier CY - Amsterdam AN - OPUS4-54866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hüllmann, Dino A1 - Winkler, Nicolas P. A1 - Schugardt, Jan ED - Rudnitskaya, A. T1 - Remote Drone-to-Drone Gas Sensing: A Feasibility Study N2 - Remote gas sensors mounted on mobile robots enable the mapping of gas distributions in large or poorly accessible areas. A challenging task however, is the generation of three-dimensional distribution maps from these spatially sparse gas measurements. To obtain high-quality reconstructions, the choice of optimal measuring poses is of great importance. Remote gas sensors, that are commonly used in Robot Assisted Gas Tomography (RAGT), require reflecting surfaces within the sensor’s range, limiting the possible sensing geometries, regardless of whether the robots are ground-based or airborne. By combining ground and aerial robots into a heterogeneous swarm whose agents are equipped with reflectors and remote gas sensors, remote inter-robot gas measurements become available, taking RAGT to the next dimension – releasing those constraints. In this paper, we demonstrate the feasibility of drone-to-drone measurements under realistic conditions and highlight the resulting opportunities. T2 - 19th International Symposium on Olfaction and Electronic Nose CY - Aveiro, Portugal DA - 29.05.2022 KW - Aerial robot KW - TDLAS KW - Inter-robot measurements KW - Gas tomography KW - Plume PY - 2022 SN - 978-1-6654-5860-3 DO - https://doi.org/10.1109/isoen54820.2022.9789627 SP - 1 EP - 3 PB - IEEE CY - USA AN - OPUS4-54926 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Remote Drone-to-Drone Gas Sensing: A Feasibility Study N2 - Remote gas sensors mounted on mobile robots enable the mapping of gas distributions in large or poorly accessible areas. A challenging task however, is the generation of three-dimensional distribution maps from these spatially sparse gas measurements. To obtain high-quality reconstructions, the choice of optimal measuring poses is of great importance. Remote gas sensors, that are commonly used in Robot Assisted Gas Tomography (RAGT), require reflecting surfaces within the sensor’s range, limiting the possible sensing geometries, regardless of whether the robots are ground-based or airborne. By combining ground and aerial robots into a heterogeneous swarm whose agents are equipped with reflectors and remote gas sensors, remote inter-robot gas measurements become available, taking RAGT to the next dimension – releasing those constraints. In this paper, we demonstrate the feasibility of drone-to-drone measurements under realistic conditions and highlight the resulting opportunities. T2 - 19th International Symposium on Olfaction and Electronic Nose CY - Aveiro, Portugal DA - 29.05.2022 KW - Aerial robot KW - TDLAS KW - Inter-robot measurements KW - Gas tomography KW - Plume PY - 2022 AN - OPUS4-54927 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moufid, M. A1 - Tiebe, Carlo A1 - El Bari, N. A1 - Hamada, D. A. A1 - Bartholmai, Matthias A1 - Bouchikhi, B. T1 - Pollution parameters evaluation of wastewater collected at different treatment stages from wastewater treatment plant based on E-nose and E-tongue systems combined with chemometric techniques N2 - Wastewater contains harmful chemicals and heavy metals that are known to cause various environmental and health problems. Therefore, the water quality control using sensitive, simple, fast, accurate, and portable tools is of great importance. This study aimed to evaluate the pollution parameters of wastewaters collected at different treatment stages from a wastewater treatment plant (WWTP) that treats domestic and industrial wastewaters by using an electronic nose (E-nose) and a voltammetric electronic tongue (E-tongue) combined with chemometric techniques. Water and wastewater pollution parameters determination were performed using inductively coupled plasma optical emission spectrometry for the determination of cations, and anions by using ion chromatography. Chemometric techniques, such as Principal Component Analysis (PCA), Discriminant Function Analysis (DFA), Support Vector Machines (SVMs), and Hierarchical Cluster Analysis (HCA), were used to process the E-nose and E-tongue datasets to describe the similarities between the samples. In addition, Partial Least Squares Regression (PLSR) model was constructed using electronic sensing data to simultaneously predict the concentration values of physicochemical parameters. The obtained correlation coefficient, for training and testing sets, is higher than 0.91 for the prediction of the concentration of all physicochemical parameters, except for iron (Fe) which remains 0.84. These results suggest that simple, portable, and inexpensive tools such as electronic nose and tongue are suitable for wastewater analysis. KW - Wastewater KW - Electronic nose KW - Voltammetric electronic tongue KW - Water quality control KW - Chemometric techniques KW - Gas sensing PY - 2022 DO - https://doi.org/10.1016/j.chemolab.2022.104593 VL - 227 SP - 1 EP - 12 PB - Elsevier B.V. AN - OPUS4-55652 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - A Long Way of Plasma Modeling: Personal Experience N2 - Modeling is an important tool for understanding a physical phenomenon. It helps to interpret results of experiments and optimize experimental parameters for obtaining a desirable result. Modeling laser induced plasma is beneficial for many scientific and industrial fields, e.g., analytical chemistry, pulsed laser deposition, plasma enhanced chemical vapor deposition, laser welding, additive manufacturing etc. In this presentation, a personal experience in development of a physical model of laser induced plasma will be given in a chronological sequence starting from early 2000th and until now. Over the time, the model evolved from its simple analytical form that described plasma emission spectra to its current numerical form that describes plasma dynamics, chemistry, and interaction with a substrate surface. Several examples will be given for the application of the model to practical problems such as spectroscopic chemical analysis, plasma enhanced chemical vapor deposition, and surface modification by laser ablation. T2 - XII World Conference on Laser Induced Breakdown Spectroscopy CY - Bari, Italy DA - 05.09.2022 KW - Laser induced plasma KW - CFD computational fluid dynamic KW - Plasma modeling KW - Plasma chemistry PY - 2022 AN - OPUS4-55669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kazlagić, Anera A1 - Vogl, Jochen T1 - Investigating the differences in 87Sr/ 86Sr isotope ratio measurements between MC-ICP-MS and MC-TIMS in cement RMs N2 - Thirteen laboratories participated in an international interlaboratory comparison for the determination of 87Sr/86Sr isotope ratios in four cement reference materials (RM) using the conventional method for 87Sr/86Sr isotope ratios analyses. Sample dissolution and Sr isolation via ion exchange chromatography were required since the cement samples were distributed as powders. Analytical preparation included the use of various digestion methods including mixed mineral acids, microwave/acid, bomb/acid digestion or borate fusion, followed by Sr separation using ion exchange chromatography. In this study, we evaluated whether any statistically significant differences were attributable to instrumental differences (i.e., MC-ICP-MS and MC-TIMS), or to laboratory-specific techniques (different sample preparation techniques, Sr isolation and the procedures for correcting the data outputs). To evaluate these effects, consensus values for cement RMs and associated standard uncertainties were estimated by fitting a linear, Gaussian mixed effects model using the R function “lmer” defined in package “lme4”. No statistically significant effects (SSE) attributable to instrumental differences regardless of whether the materials are considered together or separately were evident. There were SSE attributable to differences between laboratories for three cement RMs when the individual cements were considered separately. Since consideration or disregard for such differences does not induce significant changes in the estimate of the consensus values for the 87Sr/86Sr isotope ratios in cement RMs, these effects can safely be neglected when calculating the best estimates for the true values of 87Sr/86Sr isotope ratios in these RMs. T2 - ICP-MS Anwender*innentreffen 2022 CY - Leoben, Austria DA - 05.09.2022 KW - Conventional isotope ratio KW - Reference material KW - Metrology KW - Traceability KW - Uncertainty PY - 2022 AN - OPUS4-55682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Aktuelles aus der Normung N2 - Es wird ein Überblick über die aktuellen Aktivitäten im Bereich der Normung und Standardisierung der Wirbelstromprüfung und der ZfP im Allgemeinen bei DIN, ISO, IIW, ASTM und in den Fachausschüssen Wirbelstromprüfung und ZfP 4.0 der DGZfP gegeben. T2 - 2. Fachseminar Wirbelstromprüfung CY - Schweinfurt, Germany DA - 14.09.2022 KW - ZfP KW - Normung KW - Wirbelstrom PY - 2022 AN - OPUS4-55712 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cordsmeier, Leo A1 - Hahn, Marc Benjamin T1 - DNA Stability in Biodosimetry, Pharmacy and DNA Based Data-Storage: Optimal Storage and Handling Conditions N2 - DNA long-term stability and integrity is of importance for applications in DNA based bio-dosimetry, data-storage, pharmaceutical quality-control, donor insemination and DNA based functional nanomaterials. Standard protocols for these applications involve repeated freeze-thaw cycles of the DNA, which can cause detrimental damage to the nucleobases, as well as the sugar-phosphate backbone and therefore the whole molecule. Throughout the literature three hypotheses can be found about the underlying mechanisms occurring during freeze-thaw cycles. It is hypothesized that DNA single-strand breaks during freezing can be induced by mechanical stress leading to shearing of the DNA molecule, by acidic pH causing damage through depurination and beta elimination or by the presence of metal ions catalyzing oxidative damage via reactive oxygen species (ROS). Here we test these hypotheses under well defined conditions with plasmid DNA pUC19 in high-purity buffer (1xPBS) at physiological salt and pH 7.4 conditions, under pH 6 and in the presence of metal ions in combination with the radical scavengers DMSO and Ectoine. The results show for the 2686 bp long plasmid DNA, that neither mechanical stress, nor pH 6 lead to degradation during repeated freeze-thaw cycles. In contrast, the presence of metal ions (Fe2+) leads to degradation of DNA via the production of radical species. KW - DNA KW - DNA stability KW - Pharmacy KW - Reference material KW - pUC19 KW - Strand break KW - SSB KW - Dosimetry KW - Biodosimetry KW - Biologisches Dosimeter KW - DNA Dosimeter KW - Quality control KW - Plasmid DNA KW - DNA data storage KW - Nucleobase KW - Base damage KW - Base loss KW - DNA degradation KW - Metal ions KW - ROS KW - OH radical KW - Fenton Reaction KW - H2O2 KW - DNA based data storage KW - Freezing KW - Thawing KW - Mechanical stress KW - pH KW - Beta elimination KW - Ectoine KW - Ectoin KW - THP(B) KW - Radical scavenger KW - DMSO KW - Buffer KW - lN2 KW - DNA vortexing KW - AGE KW - SYBR Gold KW - Gel electrophoresis KW - DNA long term storage KW - DNA reference material PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557148 DO - https://doi.org/10.1002/cbic.202200391 SP - 1 EP - 9 PB - Wiley-VCH GmbH AN - OPUS4-55714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat T1 - Coherent heterodyne OTDR based on geometric phase N2 - Results showing a Distributed Acoustic Sensing setup based on Geometric Phase as opposed to the traditionally measured Dynamic Phase. T2 - Meeting on PhD progress CY - Online Meeting DA - 09.08.2022 KW - Coherent Heterodyne KW - Distributed Acoustic Sensing KW - Geometric Phase PY - 2022 AN - OPUS4-55717 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hicke, Konstantin T1 - Distributed fiber optic sensing @BAM N2 - Research and developement activities of BAM regarding Distributed Fiber Optic Sensing are portrayed using exemplary previous and current projects. Shown results pertain to distributed acoustic sensing (DAS), distributed temperagture sensing (DTS) and distributed strain sensing (DSS). T2 - Seismic seminar FU Berlin (group Prof. Shapiro) CY - Online meeting DA - 15.09.2022 KW - Distributed fiber optic sensing KW - Distributed acoustic sensing KW - Distributed temperature sensing KW - Distributed strain sensing KW - Infrastructure monitoring PY - 2022 AN - OPUS4-55721 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat T1 - Earthquake Monitoring N2 - A brief introduction of my previous research experince involving design of Photonic Crystal Fiber followed by introduction to my current PhD project at BAM involving earthquake monitoring. First results of my original setup for measuring geometric Phase are included. T2 - Intro to PhD project on Earthquake Monitoring CY - Berlin, Germany DA - 01.04.2022 KW - Earthquake Monitoring KW - Geometric Phase PY - 2022 AN - OPUS4-55707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat T1 - Geometric phase in distributed fiber sensing N2 - Introduction to Geometric Phase in time and space domain. Results showing successful detection of Geometric Phase using a distributed fiber optic sensor setup are presented. T2 - Detecting Geometric Phase CY - Online Meeting DA - 10.05.2022 KW - Coherent Heterodyne KW - Geometric Phase KW - Distributed Fiber Optic Sensor PY - 2022 AN - OPUS4-55708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat T1 - Measurement of Geometric Phase using a φ-OTDR setup N2 - Geometric phase showing sensitivity to changes in polarisation state (SOP) and intensity of backscattered light is measured using a novel φ-OTDR setup based on coherent heterodyne detection. Principle is demonstrated using a polarisation scrambler inline a fiber-under-test. T2 - 27th Optical Fiber Sensors conference CY - Alexandria, United States DA - 29.08.2022 KW - Coherent Heterodyne KW - Geometric Phase KW - Distributed Fiber Optic Sensor PY - 2022 AN - OPUS4-55710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Procop, Mathias A1 - Terborg, R. T1 - Measurement and calculation of x-ray production efficiencies for copper, zirconium, and tungsten N2 - Electron probe microanalysis (EPMA) is based on physical relations between measured X-ray intensities of characteristic lines and their Xray production efficiency, which depends on the specimen composition. The quality of the analysis results relies on how realistically the physical relations describe the generation and emission of X-rays. Special experiments are necessary to measure X-ray production efficiencies. A challenge in these experiments is the determination of the detection efficiency of the spectrometer as a function of the photon energy. An energy-dispersive spectrometer was used in this work, for which the efficiency was determined at metrological synchrotron beamlines with an accuracy of ±2%. X-ray production efficiencies for the L series and the Kα series of copper and zirconium and for the M and L series of tungsten were determined at energies up to 30 keV in a scanning electron microscope. These experimental values were compared with calculated X-ray production efficiencies using physical relations and material constants applied in EPMA. The objective of the comparison is the further improvement of EPMA algorithms as well as extending the available database for X-ray production efficiencies. Experimental data for the X-ray production efficiency are also useful for the assessment of spectrum simulation software. KW - Copper KW - Electron probe microanalysis KW - Tungsten KW - X-ray production efficiency KW - Zirconium PY - 2022 DO - https://doi.org/10.1017/S1431927622012351 VL - 28 IS - 6 SP - 1865 EP - 1877 PB - Oxford University Press CY - Oxford AN - OPUS4-55711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Tobias T1 - Application of LIBS to identify construction and demolition waste for circular economy N2 - Responsible treatment of the environment and resources is a key element of sustainability. The building and construction industry is one of the largest consumers of natural resources. Consequently, there is a particular need for regulations and technologies that help to create closed material cycles. From the technological point of view, such efforts are complicated by the growing material diversity and the amount of composites contained in present and future construction and demolition waste (CDW). Nowadays, simple but proven techniques like manual sorting are mainly used. However, this practice not only poses health risks and dangers to the staff performing the work, but also relies on merely obvious, visually striking differences. Automated, sensor-based sorting of these building materials could complement or replace this practice to improve processing speed, recycling rates, sorting quality, and prevailing health conditions. The preliminary results for the identification of a wide variety of building materials with LIBS are presented. T2 - XII Laser Induced Breakdown Spectroscopy (LIBS 2022) CY - Bari, Italy DA - 04.09.2022 KW - LIBS KW - Construction and demolition waste KW - Circular economy PY - 2022 AN - OPUS4-55679 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Tobias T1 - Interlaboratory comparison for quantitative chlorine analysis in cement pastes with LIBS N2 - Concrete structures often show severe damage during their lifetime. One such damage is pitting corrosion of the steel reinforcement caused by chloride ingress into the porous concrete structure. Laser-induced breakdown spectroscopy (LIBS) is a promising method in civil engineering, which is used for detection of chlorine in concrete structures in addition to conventional methods of wet chemistry. To assess LIBS as a trustful analytical technique, its accuracy and robustness is carefully tested. The presentation will outline the results of the interlaboratory comparison of chlorine quantification in cement paste samples, which was carried out by 12 laboratories in 10 countries. Two sets of samples with chloride content ranging from 0.06-1.95 wt.% in the training set and 0.23-1.51 wt.% in the test sample set (“unknowns”), with additional variations in the type of cement and chlorine source (salt type) were sent to the laboratories. The overall result demonstrates that LIBS is suitable for the quantification of the investigated sample compositions: average relative bias was mostly below 15 %. Considering that the laboratories did not receive instructions on how to perform the analysis or how to process the data, the results can be evaluated as a true status quo of the LIBS technique for this type of analysis. T2 - XII Laser Induced Breakdown Spectroscopy (LIBS 2022) CY - Bari, Italy DA - 04.09.2022 KW - LIBS KW - Chlorine KW - Cement pastes KW - Interlaboratory comparison PY - 2022 AN - OPUS4-55680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen A1 - Oelze, Marcus T1 - Isotope reference materials N2 - The variation of isotope ratios is increasingly used to unravel natural and technical questions. In the past, the investigation and interpretation of such variations was the field of a limited number of experts. With new upcoming techniques and research topics in the last decades, such as provenance or food authenticity studies, the number of published isotope data strongly increased. Instrumental developments such as the enhancement of inductively coupled plasma mass spectrometers (ICP-MS) from an instrument for simple quantitative analysis to highly sophisticated isotope ratio machines influenced this process significantly. While in former times only experts in mass spectrometry were able to produce reliable isotope data, nowadays many laboratories, never been in touch with mass spectrometry before, produce isotope data with an ICP-MS. Isotope reference materials (iCRM) are indispensable to enable a reliable method validation or in rare cases even SI-traceability. The fast development and the broad availability of ICP-MS also lead to an expansion of the classical research areas and new elements are under investigation. Irrespective of the investigated element or the knowledge of the user all isotope ratio applications require reference materials either for correction of instrumental isotope fractionation, for method validation or to provide a common accepted basis as needed for delta measurements. This presentation will outline the basic principles and illustrate the urgent need for new iCRMs. Consequently, the production and certification of iCRMs will be discussed and illustrated by examples of already completed certification projects. Finally, plans for future iCRMs to be produced at BAM will be presented. T2 - ICP-MS Anwender*innentreffen 2022 CY - Leoben, Austria DA - 05.09.2022 KW - Absolute isotope ratio KW - Traceability KW - Metrology KW - Comparability KW - Uncertainty KW - Isotope reference materials KW - Delta scale PY - 2022 AN - OPUS4-55681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Even, Morgane T1 - Development of a procedure for the analysis of the emissions of VVOCs – Results of a research project N2 - Since 1997, the Committee for Health-related Evaluation of Building Products (AgBB) has been developing the basis for building regulations for protection against indoor health risks that may arise when building products are used. In 2009, the AgBB decided to include relevant VVOCs in the assessment procedure. The ISO 16000-6 (2021) states that the use of the thermal desorption gas chromatography technique is appropriate for VVOCs, if adaptations are considered. However, a suitable method for the trustworthy quantification of VVOC emissions from building products and in the indoor air is still missing. This webinar will present the results of a research project on the development of a procedure for VVOC analysis: • identification of the gaps towards standardization • investigations on gas standards and the suitability of chromatography columns • investigations on sorbent combinations and water management • validation of the method and screening of VVOC emissions from building products. T2 - Webinar organized by Umweltbundesamt and BAM CY - Online meeting DA - 13.09.2022 KW - Analytical method KW - EN 16516 KW - ISO 16000-6 KW - VVOCs PY - 2022 AN - OPUS4-55693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deumer, J. A1 - Pauw, Brian Richard A1 - Marguet, S. A1 - Skroblin, D. A1 - Taché, O. A1 - Krumrey, M. A1 - Gollwitzer, C. T1 - Small-angle X-ray scattering: characterization of cubic Au nanoparticles using Debye’s scattering formula N2 - A versatile software package in the form of a Python extension, named CDEF (computing Debye’s scattering formula for extraordinary form factors), is proposed to calculate approximate scattering profiles of arbitrarily shaped nanoparticles for small-angle X-ray scattering (SAXS). CDEF generates a quasi-randomly distributed point cloud in the desired particle shape and then applies the open-source software DEBYER for efficient evaluation of Debye’s scattering formula to calculate the SAXS pattern (https://github.com/j-from-b/CDEF). If self-correlation of the scattering signal is not omitted, the quasi-random distribution provides faster convergence compared with a true-random distribution of the scatterers, especially at higher momentum transfer. The usage of the software is demonstrated for the evaluation of scattering data of Au nanocubes with rounded edges, which were measured at the four-crystal monochromator beamline of PTB at the synchrotron radiation facility BESSY II in Berlin. The implementation is fast enough to run on a single desktop computer and perform model fits within minutes. The accuracy of the method was analyzed by comparison with analytically known form factors and verified with another implementation, the SPONGE, based on a similar principle with fewer approximations. Additionally, the SPONGE coupled to McSAS3 allows one to retrieve information on the uncertainty of the size distribution using a Monte Carlo uncertainty estimation algorithm. KW - X-ray scattering KW - SAXS KW - Non-spherical nanoparticles KW - Nanoparticles KW - Nanomaterials KW - Debye scattering equation KW - Simulation KW - Data fitting PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557652 DO - https://doi.org/10.1107/S160057672200499X VL - 55 IS - Pt 4 SP - 993 EP - 1001 PB - International Union of Crystallography CY - Chester, England AN - OPUS4-55765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat T1 - Distributed fiber optic sensing for earthquake monitoring N2 - Earthquake monitoring using geometric phase. Planned foeld measurements at Horstwalde (BAM TTS) are discussed with Professor Serge Shapiro of Free University for a possible collaboration. T2 - Invitation for coolaboration on Earthquake Monitoring project CY - Online Meeting DA - 15.09.22 KW - Coherent Heterodyne KW - Geometric Phase KW - Distributed Fiber Optic Sensor PY - 2022 AN - OPUS4-55767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - VIDEO A1 - Pauw, Brian Richard T1 - Just a minute: X-ray scattering N2 - An extremely brief summary of what X-ray scattering can do for you (X-ray scattering encompasses small-angle X-ray scattering (SAXS), and wide-angle X-ray scattering (WAXS/XRD), amongst others). See my other videos for more detailed explanations on sample selection, data correction, data analysis, etc. KW - X-ray scattering KW - Introduction KW - Materials science KW - Nanostructure investigation KW - MOUSE PY - 2022 UR - https://www.youtube.com/watch?v=jWWNQyaCTHA DO - https://doi.org/10.26272/opus4-55768 PB - YouTube, LLC CY - San Bruno, CA, USA AN - OPUS4-55768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Analytical Challenges for PFAS in Environmental Samples - Methods, Approaches and Applicability N2 - Per- and polyfluoroalkyl substances (PFAS) are anionic, cationic and zwitterionic synthetic products, in which the hydrogen atoms on the carbon skeleton of at least one carbon atom have been completely replaced by fluorine atoms and which include up to 1.7 M compounds, depending on the definition. As a result of continuous and prolific use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil, groundwater and surface water. Furthermore, because of the continuous contamination through PFAS containing commercial products, effluents and sewage sludge from WWTPs have been shown to be an important source of PFAS discharge into the aquatic environment. In the last few years, legacy PFAS (≥C4) have been found in various environments, including soil, water and wastewater, and their environmental pathways have been partly described. Several long-chain PFAS species, and their respective salts are considered as persistent organic pollutants by the United Nations Stockholm Convention. These pollutants have been linked to altered immune and thyroid function, liver disease, lipid and insulin dysregulation, kidney disease, adverse reproductive and developmental outcomes, and cancer. A significant shift in the chemical industry towards production of short (C4-C7) and ultrashort (C1-C3) alternatives was observed in response to recently intensified regulations and restrictions on the use of long-chain (≥C8) PFAS. PFAS analysis in environmental samples is currently mainly done by liquid chromatography tandem mass spectrometry (LC-MS/MS). This efficient method is conducted in a targeted fashion analyzing a small subset of PFAS. The US EPA method for analysis of PFAS using LC-MS/MS for example currently lists 40 PFAS (≥C4). However, to get a better overview of the amount of “total PFAS,” sum parameter methods like total oxidizable precursor (TOP) assay and methods based on combustion ion chromatography (CIC) are in development. CIC results in data regarding the sum of absorbable organic fluorine (AOF) or extractable organic fluorine (EOF), which can also quantify other organically bound fluorine compounds such as fluorinated pesticides and pharmaceutical. Moreover, non-target and suspect screening mass spectrometry can be used to identify novel emerging PFAS and partly unknown fluorinated compounds in environmental samples. Furthermore, to analyze ultrashort PFAS (C1-C3), supercritical fluid chromatography (SFC), hydrophilic interaction chromatography (HILIC) and gas chromatography-mass spectrometry (GC-MS) are available, but further research is needed to develop reliable and accurate methods to quantify several ultrashort PFAS in environmental samples. Additionally, for research purpose several spectroscopical methods like X-ray photoelectron spectroscopy (XPS), fluorine K-edge X-ray absorption near-edge structure (XANES)spectroscopy, particular induced gamma-ray emission (PIGE) spectroscopy and 19F nuclear magnetic resonance (NMR) spectroscopy are available. T2 - CleanUp 2022 CY - Adelaide, Australia DA - 11.09.2022 KW - PFAS KW - Combustion ion chromatography KW - XANES spectroscopy PY - 2022 AN - OPUS4-55741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Mechanochemical Remediation of Per- and Polyfluoroalkyl Substanzes (PFAS) in Soils N2 - Per- and polyfluoroalkyl substances (PFAS) are a large group of anionic, cationic, or zwitterionic organofluorine surfactants used in the formulations of thousands of products and consumer goods, including aqueous film-forming foams (AFFF) used to suppress aviation fires in training scenarios, non-stick cookware, fast-food wrappers, water-repellent fabrics, medical equipment. Because PFAS have been extensively used in a variety of AFFF products they can be found in soils from industrial and military installations. Current decontamination strategies of PFAS-burdened soils mainly consist of adsorption methods using adsorbents for fixation of PFAS in the ground. A second option is the utilization of a “pump and treat” process, cycling polluted soils through a washing plant leading to the concentration of the pollutants in the fine fraction. Only a subsequent, high-energy consuming pyrolysis process guarantees the total destruction of all fluorinated organic contaminants. Both approaches are cost-intensive and not intended for the direct decomposition of all PFAS contaminants. Hence, there is a great demand for innovative developments and chemical treatment technologies, dealing with new strategies of tackling the PFAS problem. Previously, mechanochemical treatment of polychlorinated organic compounds in soils showed an efficient dechlorination. Thus, we investigated mechanochemical treatment of PFAS contaminated soils with various additives in a ball mill and analyzed the PFAS defluorination with gas chromatography mass spectrometry (GCMS) and liquid chromatography tandem mass spectrometry (LC-MS/MS), respectively, as well es the fluoride mineralization by ion chromatography (IC) and fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy. T2 - CleanUp 2022 CY - Adelaide, Australia DA - 11.09.2022 KW - PFAS KW - Mechanochemical treatment KW - XANES spectroscopy PY - 2022 AN - OPUS4-55742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - PFAS Sum Parameter and Structural Analysis N2 - Per- and polyfluoroalkyl substances (PFAS) are anionic, cationic and zwitterionic synthetic products, in which the hydrogen atoms on the carbon skeleton of at least one carbon atom have been completely replaced by fluorine atoms (see Figure 1) and which include more than 4730 compounds, depending on the definition. As a result of continuous and prolific use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil, groundwater and surface water. Furthermore, because of the continuous contamination through PFAS containing commercial products, effluents and sewage sludge from WWTPs have been shown to be an important source of PFAS discharge into the aquatic environment. In the last few years, legacy PFAS (≥C4) have been found in various environments, including soil, water and wastewater, and their environmental pathways have been partly described. To get a better overview of the amount of “total PFAS,” sum parameter methods like total oxidizable precursor (TOP) assay and methods based on combustion ion chromatography (CIC) are in development. CIC results in data regarding the sum of absorbable organic fluorine (AOF) or extractable organic fluorine (EOF), which can also quantify other organically bound fluorine compounds such as fluorinated pesticides and pharmaceutical. Additionally, for research purpose several spectroscopical methods like X-ray photoelectron spectroscopy (XPS), fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy, particular induced gamma-ray emission (PIGE) spectroscopy and 19F nuclear magnetic resonance (NMR) spectroscopy are available. Therefore, an overview is given on various analytical techniques for PFAS in environmental samples and their application possibilities discussed for different kind of PFAS compounds T2 - CleanUp 2022 CY - Adelaide, Australia DA - 11.09.2022 KW - PFAS KW - Combustion ion chromatography KW - XANES spectroscopy KW - Soil PY - 2022 AN - OPUS4-55743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Rienitz, O. A1 - Pramann, A. A1 - Flierl, L. T1 - Scale Conversion and Uncertainty Calculations in Isotope Delta Measurements N2 - Isotope ratio applications are on the increase and a major part of which are delta measurements, because they are easier to perform than the determination of absolute isotope ratios while offering lower measurement uncertainties. Delta measurements use artefact-based scales and therefore scale conversions are required due to the lack of the scale defining standards. Such scale conversions often form the basis for comparing data being generated in numerous projects andtherefore need to be as accurate as possible. In practice, users are tempted to apply linear approximations, which are not sufficiently exact, because delta values are defined by nonlinear relationships. The bias of such approximations often is beyond typical measurement uncertainties and its extent can hardly be predicted. Therefore, exact calculations are advised. Here, the exact equations and the bias of the approximations are presented, and calculations are illustrated by real-world examples. Measurement uncertainty is indispensable in this context and therefore, its calculation is described as well for determining delta values but also for scale conversions. Approaches for obtaining a single delta measurement and for repeated measurements are presented. For the latter case, a new approach for calculating the measurement uncertainty is presented, which considers covariances between the isotope ratios. KW - Delta isotope standard KW - Delta scale KW - In-house calibration solution KW - Isotope ratios KW - Isotope reference material KW - Measurement uncertainty KW - Scale conversion PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557254 DO - https://doi.org/10.1111/ggr.12450 SN - 1639-4488 VL - 46 IS - 4 SP - 773 EP - 787 PB - Wiley AN - OPUS4-55725 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hahn, Marc Benjamin T1 - BioSAXS models for TOPAS/Geant4 N2 - Models for TOPAS/Geant4 to estimate the microscopic dose received by biomolecules during bioSAXS experiments. The C++ classes in this repository extend the functionality of the TOPAS (http://www.topasmc.org/) Monte-Carlo program, which is itself a wrapper of the Geant4 MCS Toolkit (http://geant4.org). KW - TOPAS KW - TOPAS-nBio KW - Geant4 KW - Geant4-DNA KW - MCS KW - Microdosimetry KW - Protein KW - Proteins KW - Particle scattering KW - G5P KW - GV5 KW - SAXS KW - Monte-Carlo simulation KW - Dosimetry KW - Micorscopic dose-damage relation PY - 2022 UR - https://github.com/MarcBHahn/TOPAS-bioSAXS-dosimetry DO - https://doi.org/10.26272/opus4-55751 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-55751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - VIDEO A1 - Pauw, Brian Richard T1 - How to run a (lab) SAXS instrument efficiently N2 - Here I talk about our holistic approach to X-ray scattering, and what improvements we made to our methodology to make measuring with us a very streamlined process. KW - Laboratory management KW - MOUSE KW - X-ray scattering KW - Instrument utilization KW - Research efficiency KW - Automation KW - Metadata collection KW - Laboratory automation PY - 2022 UR - https://www.youtube.com/watch?v=ncadUQ43Uwc DO - https://doi.org/10.26272/opus4-55761 PB - YouTube, LLC CY - San Bruno, CA, USA AN - OPUS4-55761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruna, F. G. A1 - Prokop, M. A1 - Bystron, T. A1 - Loukrakpam, R. A1 - Melke, J. A1 - Lobo, C. M. S. A1 - Fink, M. A1 - Zhu, M. A1 - Voloshina, E. A1 - Kutter, M. A1 - Hoffmann, H. A1 - Yusenko, Kirill A1 - de Oliveira Guilherme Buzanich, Ana A1 - Röder, B. A1 - Bouzek, K. A1 - Paulus, B. A1 - Roth, C. T1 - Following adsorbed intermediates on a platinum gas diffusion electrode in H3PO3‑containing electrolytes using in situ X‑ray absorption spectroscopy N2 - One of the challenges of high-temperature polymer electrolyte membrane fuel cells is the poisoning of the Pt catalyst with H3PO4. H3PO4 is imbibed into the routinely used polybenzimidazole-based membranes, which facilitate proton conductivity in the temperature range of 120−200 °C. However, when leached out of the membrane by water produced during operation, H3PO4 adsorbs on the Pt catalyst surface, blocking the active sites and hindering the oxygen reduction reaction (ORR). The reduction of H3PO4 to H3PO3, which occurs at the anode due to a combination of a low potential and the presence of gaseous H2, has been investigated as an additional important contributing factor to the observed poisoning effect. H3PO3 has an affinity toward adsorption on Pt surfaces even greater than that of H2PO4 −. In this work, we investigated the poisoning effect of both H3PO3 and H3PO4 using a half-cell setup with a gas diffusion electrode under ambient conditions. By means of in situ X-ray absorption spectroscopy, it was possible to follow the signature of different species adsorbed on the Pt nanoparticle catalyst (H, O, H2PO4 −, and H3PO3) at different potentials under ORR conditions in various electrolytes (HClO4, H3PO4, and H3PO3). It was found that H3PO3 adsorbs in a pyramidal configuration P(OH)3 through a Pt−P bond. The competition between H3PO4 and H3PO3 adsorption was studied, which should allow for a better understanding of the catalyst poisoning mechanism and thus assist in the development of strategies to mitigate this phenomenon in the future by minimizing H3PO3 generation by, for example, improved catalyst design or adapted operation conditions or changes in the electrolyte composition. KW - H3PO4 life cycle KW - XAS KW - In situ coupling KW - High-temperature fuel cells KW - Δμ XANES KW - H3PO3 PY - 2022 DO - https://doi.org/10.1021/acscatal.2c02630 SN - 2155-5435 VL - 12 IS - 18 SP - 11472 EP - 11484 PB - ACS CY - Washington, DC AN - OPUS4-55815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rautenberg, Max A1 - Bhattacharya, Biswajit A1 - Witt, Julia A1 - Jain, Mohit A1 - Emmerling, Franziska T1 - In situ time-resolved monitoring of mixed-ligand metal–organic framework mechanosynthesis N2 - The mechanism of mixed-ligand metal–organic framework (MOF) formation, and the possible role of intermediate single-ligand metal complexes during mechanosynthesis, have not been explored yet. For the first time, we report here in situ real-time monitoring of the mechanochemical formation mechanism of mixed-ligand MOFs. Our results show that binary phases can act as intermediates or competing products in one-pot and stepwise synthesis. KW - Mechanochemistry KW - Metal-organic-frameworks KW - In situ X-ray diffraction KW - Mixed-ligand MOFs PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558167 DO - https://doi.org/10.1039/D2CE00803C SP - 1 EP - 4 PB - Royal Society of Chemistry AN - OPUS4-55816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim T1 - Overview of NDT techniques for moisture measurements in building materials N2 - Overview of NDT techniques for moisture measurements in building materials used in department 8 of BAM. T2 - ENBRI Expert Workshop "Hygrothermal testing - a necessity to guarantee durable buildings" CY - Brussels, Belgium DA - 21.09.2022 KW - Moisture KW - Building materials KW - GPR KW - NMR KW - Microwave PY - 2022 AN - OPUS4-55817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - An improved method for the determination of PFAS using HR-CS-GFMAS via GaF detection N2 - Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate realistic PFAS pollution levels. PFAS sum parameters display the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a Ga pretreatment as described by Gawor et al. resulting in overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analyzed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for EOF determination in soils. T2 - ESAS - CSSC CY - Brno, Czech Republic DA - 04.09.2022 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2022 AN - OPUS4-55782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - An improved method for the determination of PFAS using HR-CS-GFMAS via GaF detection N2 - Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate realistic PFAS pollution levels. PFAS sum parameters display the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a Ga pretreatment as described by Gawor et al. resulting in overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analyzed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for EOF determination in soils. T2 - SALSA - Communicating Make and Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2022 AN - OPUS4-55783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Völker, Tobias T1 - Intrinsic Performance of Monte Carlo Calibration-Free Algorithm for Laser-Induced Breakdown Spectroscopy N2 - The performance of the Monte Carlo (MC) algorithm for calibration-free LIBS was studied on the example of a simulated spectrum that mimics a metallurgical slag sample. The underlying model is that of a uniform, isothermal, and stationary plasma in local thermodynamical equilibrium. Based on the model, the algorithm generates from hundreds of thousands to several millions of simultaneous configurations of plasma parameters and the corresponding number of spectra. The parameters are temperature, plasma size, and concentrations of species. They are iterated until a cost function, which indicates a difference between synthetic and simulated slag spectra, reaches its minimum. After finding the minimum, the concentrations of species are read from the model and compared to the certified values. The algorithm is parallelized on a graphical processing unit (GPU) to reduce computational time. The minimization of the cost function takes several minutes on the GPU NVIDIA Tesla K40 card and depends on the number of elements to be iterated. The intrinsic accuracy of the MC calibration-free method is found to be around 1% for the eight elements tested. For a real experimental spectrum, however, the efficiency may turn out to be worse due to the idealistic nature of the model, as well as incorrectly chosen experimental conditions. Factors influencing the performance of the method are discussed. KW - Laser induced breakdown spectroscopy KW - Calibration-free analysis KW - Monte Carlo algorithm PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558016 DO - https://doi.org/10.3390/s22197149 VL - 22 IS - 19 SP - 7149 PB - MDPI AN - OPUS4-55801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Gornushkin, Igor B. T1 - Importance of physical units in the Boltzmann plot method N2 - The Boltzmann plot is one of the most widely used methods for determining the temperature in different types of laboratory plasmas. It operates on the logarithm as a function of the dimensional argument, which assumes that the correct physical units are used. In many works using the Boltzmann method, there is no analysis of the dimension of this argument, which may be the cause of a potential error. This technical note offers a brief description of the method and shows how to correctly use physical units when using transcendental functions like the logarithm. KW - Boltzmann plot KW - Laser induced plasma PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558039 DO - https://doi.org/10.1039/d2ja00241h SP - 1 EP - 3 PB - Royal Society of Chemistry AN - OPUS4-55803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Application of 3,3’,5,5’-Tetramethylbenzidine (TMB) in Amperometric Immunoassays for Mycotoxin Detection N2 - Electrochemical methods make great promise to meet the demand for user-friendly on-site devices for monitoring important parameters. Food industry often runs own lab procedures, e.g., for mycotoxin analysis, but it is a major goal to simplify analysis, linking analytical methods with miniaturized technologies. Enzyme-linked immunosorbent assays, with photometric detection of the horseradish peroxidase (HRP) substrate 3,3’,5,5’-tetramethylbenzidine (TMB), form a good basis for sensitive detection. To provide a straight-forward approach for the miniaturization of the detection step, we have studied the pitfalls of the electrochemical TMB detection. By cyclic voltammetry, it could be shown that TMB electrochemistry is strongly dependent on the pH and the electrode material. It was found that screen-printed gold electrodes and a very low pH value (pH 1) are well-suited to perform the electrochemical detection of TMB, due to the reversible character of the redox reaction under these conditions. Under these conditions, a good signal stability over several measuring cycles is achieved, providing the basis for analyzing multiple samples. In contrast to this, for carbon screen-printed electrodes, it was found that the signal response has changed after the electrochemical reaction with TMB at pH 1. At moderately acidic conditions (pH 4), neither with carbon nor with gold electrodes a reproducible electrochemical detection of TMB could be achieved. Based on these findings, we created a smartphone-based, electrochemical, immunomagnetic assay for the detection of ochratoxin A (OTA) and ergometrine in food samples. A competitive assay is performed on magnetic beads using HRP and TMB/H2O2 to generate the signal. Enzymatically oxidized TMB is quantified after addition of H2SO4 by amperometry with screen-printed gold electrodes in a custom-made wall-jet flow cell. The results are in good correlation with the established photometric detection method, providing a solid basis for sensing of further analytes in HRP-based assays using the newly developed miniaturized smartphone-based, electrochemical, immunomagnetic assay. T2 - 73rd Annual Meeting of the ISE CY - Online meeting DA - 12.09.2022 KW - Cylic Voltammetry KW - Immunoassay KW - Mycotoxins KW - Amperometry KW - Electrochemistry PY - 2022 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-55793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Singh, S. A1 - Palani, I. A. A1 - Paul, C. P. A1 - Funk, Alexander A1 - Gokuldoss, P. K. T1 - Wire Arc Additive Manufacturing of NiTi 4D Structures: Influence of Interlayer Delay N2 - Shape memory alloy structures for actuator and vibration damper applications may be manufactured using wire arc additive manufacturing (W AAM), which is one of the additive manufacturing technologies. Multilayer deposition causes heat accumulation during W AAM, which rises the preheat temperature of the previously created layer. This leads to process instabilities, which result in deviations from the desired dimensions and mechanical properties changes. During W AAM deposition of the wall structure, a systematic research is carried out by adjusting the interlayer delay from 10 to 30 s. When the delay period is increased from 10 to 30 s, the breadth decreases by 45% and the height increases by 33%. Grain refinement occurs when the interlayer delay duration is increased, resulting in better hardness, phase transformation temperature, compressive strength, and shape recovery behavior. This study shows how the interlayer delay affects the behavior of W AAM-built nickel-titanium alloy (NiTi) structures in a variety of applications. KW - Wire are additive manufacturing KW - Shape memory alloy KW - Nitinol KW - Interlayer delay PY - 2022 DO - https://doi.org/10.1089/3dp.2021.0296 SN - 2329-7662 SP - 1 EP - 11 PB - Liebert CY - New Rochelle, NY AN - OPUS4-55795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brence, Blaž T1 - Interdigital Transducers for Structural Health Monitoring N2 - Interdigital transducers (IDTs) are a well-known tool for excitation of surface acoustic waves. The use of IDTs is versatile, but they are most commonly employed as actuators for excitation of ultrasonic guided waves (UGWs). However, they are still a relatively new technology, which leaves many possibilities for future research, especially in the scope of newly emerging structural health monitoring (SHM) systems. IDTs offer low weight, design flexibility and beam directivity, which make them ideal candidates for employment in such systems. Due to the IDTs’ and waves’ complexity, problems often cannot be described analytically, therefore they require numerical solutions and experimental validations. In this contribution, a novel, simple use of IDTs, in the scope of SHM is described. Firstly, numerical findings acquired with finite element method are presented. To validate those results, experiments in a plate-like waveguide are carried out. A good agreement between them is found. The results show the potential of the IDTs in yet another prospective application, which could be attractive for adoption in the future. T2 - DAGA 2022 - Jahrestagung für Akustik CY - Stuttgart, Germany DA - 21.03.2022 KW - Lamb waves KW - Ultrasonic Guided Waves KW - Selective excitation PY - 2022 AN - OPUS4-55500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brence, Blaž A1 - Lugovtsova, Yevgeniya A1 - Prager, Jens T1 - Interdigital Transducers for Structural Health Monitoring N2 - Interdigital transducers (IDTs) are a well-known tool for excitation of surface acoustic waves. The use of IDTs is versatile, but they are most commonly employed as actuators for excitation of ultrasonic guided waves (UGWs). However, they are still a relatively new technology, which leaves many possibilities for future research, especially in the scope of newly emerging structural health monitoring (SHM) systems. IDTs offer low weight, design flexibility and beam directivity, which make them ideal candidates for employment in such systems. Due to the IDTs’ and waves’ complexity, problems often cannot be described analytically, therefore they require numerical solutions and experimental validations. In this contribution, a novel, simple use of IDTs, in the scope of SHM is described. Firstly, numerical findings acquired with finite element method are presented. To validate those results, experiments in a plate-like waveguide are carried out. A good agreement between them is found. The results show the potential of the IDTs in yet another prospective application, which could be attractive for adoption in the future. T2 - 48. Jahrestagung für Akustik (DAGA) CY - Stuttgart, Germany DA - 21.03.2022 KW - Lamb waves KW - Ultrasonic Guided Waves KW - Selective excitation PY - 2022 SP - 221 EP - 224 AN - OPUS4-55501 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brence, Blaž T1 - Determination of a notch depth using ultrasonic guided waves N2 - In non-destructive testing and structural health monitoring, ultrasonic guided waves (UGWs) are of great interest for finding and characterizing structural flaws. The interaction of the waves with the flaws can often not be described analytically due to waves’ complexity. This makes numerical simulations and experiments indispensable. However, mentioned field of research is still relatively young and most of the methods focus on flaw localization, using time of flight of the reflected signal. This leaves many possibilities for further research, especially when it comes to separate analysis of different propagating modes. It is well-known that ultrasonic wave modes convert when interacting with flaws. When a fundamental mode (A0 or S0) encounters a notch, it interacts and converts to another fundamental mode. In this contribution, this effect is used to analyze the depth of a notch. Firstly, numerical simulations are presented, which show notch depth proportionality to amplitude ratio of fundamental modes. To validate these results, experiments were carried out on a metal plate with a shallow notch which was gradually deepened. UGWs were excited using a polymer-based interdigital transducer (IDT) and detected with a 3D laser Doppler vibrometer. The IDT is employed to ensure excitation of a single mode and thus to reduce the complexity of the analysis. Good agreement between numerical and experimental results has been found. The results show the potential of UGWs not only for defect reconstruction and localization, but also its precise sizing. T2 - 10th European Workshop on Structural Health Monitoring (EWSHM 2022) CY - Palermo, Italy DA - 04.07.2022 KW - Lamb waves KW - Numerical simulation KW - Selective excitation PY - 2022 AN - OPUS4-55502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Spallanzani, Roberta A1 - Koga, K. A1 - Cichy, S. A1 - Wiedenbeck, M. A1 - Schmidt, B. A1 - Oelze, Marcus A1 - Wilke, M. T1 - Lithium and boron difusivity and isotopic fractionation in hydrated rhyolitic melts N2 - Lithium and boron are trace components of magmas, released during exsolution of a gas phase during volcanic activity. In this study, we determine the difusivity and isotopic fractionation of Li and B in hydrous silicate melts. Two glasses were synthesized with the same rhyolitic composition (4.2 wt% water), having diferent Li and B contents; these were studied in difusion-couple experiments that were performed using an internally heated pressure vessel, operated at 300 MPa in the temperature range 700–1250 °C for durations from 0 s to 24 h. From this we determined activation energies for Li and B difusion of 57±4 kJ/mol and 152±15 kJ/mol with pre-exponential factors of 1.53 × 10–7 m2/s and 3.80× 10–8 m2 /s, respectively. Lithium isotopic fractionation during difusion gave β values between 0.15 and 0.20, whereas B showed no clear isotopic fractionation. Our Li difusivities and isotopic fractionation results difer somewhat from earlier published values, but overall confrm that Li difusivity increases with water content. Our results on B difusion show that similarly to Li, B mobility increases in the presence of water. By applying the Eyring relation, we confrm that B difusivity is limited by viscous fow in silicate melts. Our results on Li and B difusion present a new tool for understanding degassing-related processes, ofering a potential geospeedometer to measure volcanic ascent rates. KW - Hydrated silicate melts KW - Stable isotopes KW - Diffusion KW - Isotopic fractionation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554496 DO - https://doi.org/10.1007/s00410-022-01937-2 VL - 177 IS - 8 SP - 1 EP - 17 PB - Springer AN - OPUS4-55449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hauffen, J. C. A1 - Kästner, L. A1 - Ahmadi, Samim A1 - Jung, P. A1 - Caire, G. A1 - Ziegler, Mathias T1 - Learned block iterative shrinkage thresholding algorithm for photothermal super resolution imaging N2 - Block-sparse regularization is already well known in active thermal imaging and is used for multiple-measurement-based inverse problems. The main bottleneck of this method is the choice of regularization parameters which differs for each experiment. We show the benefits of using a learned block iterative shrinkage thresholding algorithm (LBISTA) that is able to learn the choice of regularization parameters, without the need to manually select them. In addition, LBISTA enables the determination of a suitable weight matrix to solve the underlying inverse problem. Therefore, in this paper we present LBISTA and compare it with state-of-the-art block iterative shrinkage thresholding using synthetically generated and experimental test data from active thermography for defect reconstruction. Our results show that the use of the learned block-sparse optimization approach provides smaller normalized mean square errors for a small fixed number of iterations. Thus, this allows us to improve the convergence speed and only needs a few iterations to generate accurate defect reconstruction in photothermal super-resolution imaging. KW - Thermography KW - Laser KW - Machine learning KW - Optimization KW - Non-destructive testing KW - NDT KW - Neural network KW - Defect reconstruction KW - Block-sparsity KW - Active thermal imaging KW - Regularization KW - Laser thermography PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554598 DO - https://doi.org/10.3390/s22155533 SN - 1424-8220 VL - 22 IS - 15 SP - 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-55459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Standardized workflow for checking the performance of an EDS X-ray spectrometer at a Scanning Electron Microscope N2 - For test laboratories operating under accreditation schemes like ISO/IEC 17025 (ISO/IEC 17025), as the international reference for testing and calibration laboratories wanting to demonstrate their capacity to deliver reliable results, a periodical control of the critical instrumental parameters of an Energy-Dispersive X-ray Spectrometer (EDS) is required. This periodical check of an EDS is specified with exact procedures and materials in the ISO 15632:2021 ”Microbeam Analysis – Selected instrumental performance parameters for the specification and checking of energy-dispersive X-ray spectrometers for use in electron probe microanalysis” (ISO 15632). The EDS check can be simplified to the acquisition of only one 10 kV spectrum from a dedicated test material, EDS-TM002, which is made available by BAM since 2009 (https://webshop.bam.de/webshop_en/). The optional BAM software “EDX spectrometer check” is destined to automatically evaluate this spectrum and determine the performance of the EDS in terms of energy resolution and calibration, as well as possible alteration of low-energy efficiency due to detector contamination. Nearly 200 laboratories have the EDS-TM and associated software package in use. Practical examples based on various types of artifacts occurred in the EDS spectra and a long-term (>10 years) meticulous observation of the own spectrometers will be discussed. Different types of EDS spectrometers are considered, e.g. Si(Li) and SDD, of various window types (AP, the recent one Si3N4 or even windowless), and with different front contact layers (Au and Ni) (Hodoroaba and Procop, 2014). Evaluation of other parameters or effects such as the deadtime at different count rates or pileup effects is also explained with examples. T2 - Workshop "Automated Mineralogy" @ GEOANALYSIS 2022 CY - Freiberg, Germany DA - 06.08.2022 KW - EDS KW - X-ray spectrometer KW - Performance check KW - Test material KW - Standardized check KW - EDS-TM002 PY - 2022 UR - https://geoanalysis2021.de/en/workshops/automated-mineralogy AN - OPUS4-55460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholtz, Lena T1 - Luminescence Encoding of Polymer Microbeads during Polymerization N2 - Differently sized, luminescent polymer beads encoded with QDs were prepared with a simple, optimized procedure. The optical properties of the resulting particles were studied to ensure sufficient fluorescence and to evaluate the influence of the polymerization on QD fluorescence. T2 - 84th Prague Meeting on Macromolecules - Frontiers of Polymer Colloids CY - Prague, Czech Republic DA - 24.07.2022 KW - Polymerization KW - Fluorescence KW - Quantum dots KW - Microbeads PY - 2022 AN - OPUS4-55447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - Application of Temperature Compensation Strategies for Ultrasonic Guided Waves to Distributed Sensor Networks N2 - The application of temperature compensation strategies is crucial in structural health monitoring approaches based on guided waves. Actually, the varying temperature influences the performance of the inspection system inducing false alarms or missed detection, with a consequent reduction of reliability and impact on probability of detection (POD). This paper quantitatively describes two different methods to compensate the temperature effect, namely the optimal baseline selection (OBS) and the baseline signal stretch (BSS) extending their application to the case of a distributed sensor networks (DSN). This latter introduces a number of possible data to explore compensation strategies which do not necessarily returns univocal results. Hence, a decision framework is needed, which takes into consideration multiple ultrasonic time traces with different arrival times and amplitude. In detail, the effect of temperature separation between baseline time-traces in OBS are investigated considering multiple couples of sensors employed in the DSN. A combined strategy that uses both OBS and a frequent value warning is introduced to find the more probable temperature with increasing reliability of the assessment. The same procedure is applied using the BSS algorithm. Finally, the use of both approaches is introduced, comparing the capability of the mixed algorithm to correctly sort temperature information from OBS and then apply the BSS combining the frequent value warning to have a unique correction all over the DSN. Theoretical results are compared, using data from two several experiments, which use different frequency analysis with either predominantly A0 mode or S0 mode data or both. The focus is given on the fact that different paths are available in a sensor network and several possible combinations of results are available. Nonetheless, introducing a frequent value warning it is possible to increase the efficiency of the OBS and BSS approaches making use of fewer signal processing algorithms. These confirm that the performance of OBS quantitatively agrees with predictions. In addition, the possibility to combine BSS approached also demonstrates that the use of compensation strategies improves detectability and localization of damage even in a DSN. This result can be used to improve the SHM system reliability, with promising perspectives in increasing POD. T2 - ASME 2022 49th Annual Review of Progress in Quantitative Nondestructive Evaluation (QNDE2022) CY - San Diego, CA, USA DA - 25.07.2022 KW - Performance assessment KW - Elastic waves KW - Structural Health Monitoring PY - 2022 AN - OPUS4-55427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reuter, T. A1 - Plotzki, David A1 - Borges de Oliveira, F. A1 - Wohlgemuth, F. A1 - Bauer, F. A1 - Ballach, F. A1 - Kimmig, W. A1 - Wagner, G. A1 - Watzl, C. A1 - Weiß, D. A1 - Hausotte, T. T1 - Numerical measurement uncertainty evaluation for X-ray computed tomography using simulations – A first approach to build a digital twin N2 - The ability of industrial X-ray computed tomography (CT) to scan an object with several internal and external features at once causes increasing adoption in dimensional metrology. In order to evaluate the quality of a measurement value, the task-specific measurement uncertainty has to be determined. Currently, VDI/VDE 2630 part 2.1 gives a guideline to determine the uncertainty of CT measurements experimentally by conducting repeated measurements. This is costly and time-consuming. Thus, the aim is to determine the task-specific measurement uncertainty numerically by simulations (e. g. according to the guide to expression of uncertainty in measurement (GUM) Supplement 1). To achieve that, a digital twin is necessary. This contribution presents a simple first approach how a digital twin can be built. In order to evaluate this approach, a study comparing measurements and simulations of different real CT systems was carried out by determining the differences between the measurement results of the digital twin and of the measurement results of the real-world CT systems. The results have shown a moderate agreement between real and simulated data. To improve on this aspect, a standardized method to characterize CT systems and methods to implement CT parameters into the simulation with sufficient accuracy will be developed. N2 - Die industrielle Röntgencomputertomografie (CT) wird durch ihre Fähigkeit, ein Messobjekt mit unterschiedlichen inneren und äußeren Merkmalen auf einmal zu messen, immer häufiger auch in der dimensionellen Messtechnik eingesetzt. Um die Güte eines Messwertes beurteilen zu können, muss die aufgabenspezifische Messunsicherheit ermittelt werden. Mit der Richtlinie VDI/VDE 2630 Blatt 2.1 kann derzeit die aufgabenspezifische Messunsicherheit von CT-Messungen experimentell durch eine Vielzahl an Wiederholmessungen ermittelt werden. Diese Vorgehensweise ist allerdings kosten- und zeitintensiv. Daher wird die Bestimmung der aufgabenspezifischen Messunsicherheit numerisch durch Simulationen angestrebt (z. B. Leitfaden zur Angabe der Unsicherheit beim Messen (GUM) Supplement 1). Um dieses Ziel zu erreichen, ist es notwendig, einen Digitalen Zwilling von der Messung mit dem verwendeten CT-System zu erstellen. Dieser Beitrag stellt einen ersten Ansatz zur Erstellung eines Digitalen Zwillings vor. Um diesen anschließend zu testen, wurden in einem ersten Test mehrere CT-Scans auf verschiedenen Anlagen durchgeführt und anschließend anhand der verfügbaren Parameter simuliert. Um die Qualität des jeweiligen Digitalen Zwillings einschätzen zu können, wurden die Abweichungen der resultierenden Messwerte von ihren jeweiligen Sollwerten miteinander verglichen. Die Ergebnisse zeigten eine bedingte Übereinstimmung zwischen realen und simulierten Daten. Um diese zu verbessern, wird eine standardisierte Methode zur Charakterisierung der realen CT-Systeme angestrebt. Darüber hinaus sollten Methoden entwickelt werden, die Charakterisierungsparameter in einer Simulationsumgebung hinreichend genau umzusetzen. KW - Computed tomography KW - Measurement uncertainty KW - Simulation KW - Digital twin PY - 2022 DO - https://doi.org/10.1515/teme-2022-0025 SP - 1 EP - 16 PB - De Gruyter CY - Berlin AN - OPUS4-55428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - Towards Characterisation of Elastic Constants of Composite Materials by means of Ultrasonic Guided Waves N2 - The availability of non-destructive methods is particularly important for composites, e.g., carbon or glass fiber-reinforced polymers because their properties strongly depend on the manufacturing process and in-service conditions. Composites are mostly used in thin-walled components which are perfectly suited for the characterisation with ultrasonic guided waves (UGWs). In this contribution, we demonstrate sensitivities of UGW to different elastic constants of a composite material. Then we present a characterisation procedure which can be used to in-fer elastic properties. Our approach is based on an inverse procedure in which the numeri-cally calculated dispersion curves are fitted to the measured curves. The acquisition is done by applying a broadband piezoelectric transducer (PZT) to excite various UGW modes and a 3D laser Doppler vibrometer (3D LDV) to record them. Compared to the approaches based on laser excitation, the PZT provides a better signal-to-noise ratio because more energy is brought into the structure. Whereas the 3D LDV compared to a 1D LDV or a PZT allows cap-turing in-plane and out-of-plane components giving more dispersion information for a better characterisation. Since the inverse procedure requires many iterations before elastic prop-erties are retrieved, an efficient tool for the calculation of the dispersion curves is necessary. For this, the Scaled Boundary Finite Element Method is used. All in all, a good agreement be-tween theoretical and experimental curves is demonstrated. T2 - ASME 2022 49th Annual Review of Progress in Quantitative Nondestructive Evaluation (QNDE2022) CY - San Diego, CA, USA DA - 25.07.2022 KW - Carbon fibre reinforced polymer KW - Glass fibre reinforced polymer KW - Inverse procedure PY - 2022 AN - OPUS4-55425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Sending and receiving acoustic waves using atmospheric pressure plasmas N2 - Atmospheric pressure plasmas interact in various physical ways with their surroundings. They release heat and generate charge carriers, which leads to two effects. The first effect is the generation of acoustic waves due to heat release, known as the thermoacoustic effect, and the second effect is the perturbation of the resting fluid provoked by the release of charge carriers, called “ionic wind”. The direct connection between the charge carrier production of the discharge arrangement and the surroundings also allows the detection of acoustic waves by tracking the electrical current of the arrangement. This contribution introduces a multi-fluid model approach to describe the acoustic interaction of atmospheric plasmas. In addition, we present experimental results on commercially available and in-house fabricated discharge arrangements for either emitting or receiving acoustic waves. T2 - DAGA 2020 - 46. Jahrestagung für Akustik CY - Stuttgart, Germany DA - 22.03.2022 KW - Luftgekoppelte Ultraschallprüfung KW - Plasma KW - Ultraschallwandler PY - 2022 AN - OPUS4-54616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Döring, Sarah T1 - Vergleichende Darstellung SARS-CoV-2-spezifischer Nanobodys aus unterschiedlichen Wirtsorganismen N2 - Aufgrund der anhaltenden COVID-19-Pandemie werden neutralisierende Therapeutika benötigt. Eine Möglichkeit zur Behandlung stellt die Verwendung monoklonaler Anti-SARS-CoV-2-Immun-globuline dar. Ihre Produktion in Säugetierzellen ist jedoch schwer skalierbar, um den weltweiten Bedarf zu decken. VHH-Antikörper, auch Nanobodys genannt, bieten hierfür eine Alternative, da sie eine hohe Temperaturstabilität aufweisen und eine kostengünstige Produktion in prokaryotischen Wirtsorganismen ermöglichen. KW - E. coli KW - Corona KW - Virus KW - Spike-Protein KW - Nanobody KW - Antikörper KW - Expression KW - Fingerprint KW - Vhh KW - RBD KW - COVID-19 KW - SARS-CoV-2 KW - ELISA KW - MST KW - Halomonas elongata KW - Periplasma KW - SDS-PAGE KW - ACE2-Rezeptor PY - 2021 SP - 1 EP - 111 PB - Technische Universität Berlin CY - Berlin AN - OPUS4-54624 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kittner, Maria A1 - Kerndorff, A. A1 - Ricking, M. A1 - Bednarz, M. A1 - Obermaier, N. A1 - Lukas, M. A1 - Asenova, M. A1 - Bordós, G. A1 - Eisentraut, Paul A1 - Hohenblum, P. A1 - Hudcova, H. A1 - Humer, F. A1 - István, T. G. A1 - Kirchner, M. A1 - Marushevska, O. A1 - Nemejcová, D. A1 - Oswald, P. A1 - Paunovic, M. A1 - Sengl, M. A1 - Slobodnik, J. A1 - Spanowsky, K. A1 - Tudorache, M. A1 - Wagensonner, H. A1 - Liska, I. A1 - Braun, U. A1 - Bannick, C. G. T1 - Microplastics in the Danube River Basin: A First Comprehensive Screening with a Harmonized Analytical Approach N2 - In this study, carried out within the Joint Danube Survey 4, a comprehensive microplastic screening in the water column within a large European river basin from its source to estuary, including major tributaries, was realized. The objective was to develop principles of a systematic and practicable microplastic monitoring strategy using sedimentation boxes for collection of suspended particulate matter followed by its subsequent analysis using thermal extraction desorption-gas chromatography/mass spectrometry. In total, 18 sampling sites in the Danube River Basin were investigated. The obtained suspended particulate matter samples were subdivided into the fractions of >100 μm and <100 μm and subsequently analyzed for microplastic mass contents. The results showed that microplastics were detected in all samples, with polyethylene being the predominant polymer with maximum contents of 22.24 μg/mg, 3.23 μg/mg for polystyrene, 1.03 μg/mg for styrene-butadiene-rubber, and 0.45 μg/mg for polypropylene. Further, polymers such as different sorts of polyester, polyacrylates, polylactide, and natural rubber were not detected or below the detection limit. Additional investigations on possible interference of polyethylene signals by algae-derived fatty acids were assessed. In the context of targeted monitoring, repeated measurements provide more certainty in the interpretation of the results for the individual sites. Nevertheless, it can be stated that the chosen approach using an integrative sampling and determination of total plastic content proved to be successful. KW - Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS), monitoring KW - Microplastics KW - River KW - Suspended particulate matter (SPM) KW - Sedimentation box (SB) PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551444 DO - https://doi.org/10.1021/acsestwater.1c00439 VL - 2 IS - 7 SP - 1174 EP - 1181 PB - ACS Publications AN - OPUS4-55144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steglich, P. A1 - Rabus, D. G. A1 - Sada, C. A1 - Paul, Martin A1 - Weller, Michael G. A1 - Mai, C. A1 - Mai, A. T1 - Silicon Photonic Micro-Ring Resonators for Chemical and Biological Sensing: A Tutorial N2 - Silicon photonic micro-ring resonators (MRR) developed on the silicon-on-insulator (SOI) platform, owing to their high sensitivity and small footprint, show great potential for many chemical and biological sensing applications such as label-free detection in environmental monitoring, biomedical engineering, and food analysis. In this tutorial,we provide the theoretical background and give design guidelines for SOI-based MRR as well as examples of surface functionalization procedures for label-free detection of molecules. After introducing the advantages and perspectives of MRR, fundamentals of MRR are described in detail, followed by an introduction to the fabrication methods, which are based on a complementary metal-oxide semiconductor (CMOS) technology. Optimization of MRR for chemical and biological sensing is provided, with special emphasis on the optimization of waveguide geometry. At this point, the difference between chemical bulk sensing and label-free surface sensing is explained, and definitions like waveguide sensitivity, ring sensitivity, overall sensitivity as well as the limit of detection (LoD) of MRR are introduced. Further, we show and explain chemical bulk sensing of sodium chloride (NaCl) in water and provide a recipe for label-free surface sensing. KW - Biosensors KW - Biophotonics KW - Chemosensor KW - Biosensor KW - Microresonator KW - Nanophotonics KW - Optical sensors KW - Photonic sensors KW - Optoelectronic KW - Ring resonator KW - Silicon photonics KW - Miniaturization KW - Lab-on-a-chip KW - Lab-on-chip KW - Waveguide KW - Surface chemistry KW - Silanization KW - Glutaraldehyde KW - Affinity immobilization KW - Antibody KW - Oriented immobilization KW - Real-time measurement PY - 2022 DO - https://doi.org/10.1109/JSEN.2021.3119547 SN - 1530-437X VL - 22 IS - 11 SP - 10089 EP - 10105 PB - IEEE AN - OPUS4-55147 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Coplen, T. B. A1 - Holden, N. E. A1 - Ding, T. A1 - Meijer, H. A. J. A1 - Vogl, Jochen A1 - Zhu, X. T1 - The Table of Standard Atomic Weights—An exercise in consensus N2 - The present Table of Standard Atomic Weights (TSAW) of the elements is perhaps one of the most familiar data sets in science. Unlike most parameters in physical science whose values and uncertainties are evaluated using the “Guide to the Expression of Uncertainty in Measurement” (GUM), the majority of standard atomic weight values and their uncertainties are consensus values, not GUM-evaluated values. The Commission on Isotopic Abundances and Atomic Weights of the International Union of Pure and Applied Chemistry (IUPAC) regularly evaluates the literature for new isotopic-abundance measurements that can lead to revised standard atomic-weight values, Ar(E) for element E. The Commission strives to provide utmost clarity in products it disseminates, namely the TSAW and the Table of Isotopic Compositions of the Elements (TICE). In 2016, the Commission recognized that a guideline recommending the expression of uncertainty listed in parentheses following the standard atomic-weight value, for example, Ar(Se) = 78.971(8), did not agree with the GUM, which suggests that this parenthetic notation be reserved to express standard uncertainty, not the expanded uncertainty used in the TSAW and TICE. In 2017, to eliminate this noncompliance with the GUM, a new format was adopted in which the uncertainty value is specified by the “±” symbol, for example, Ar(Se) = 78.971 ± 0.008. To clarify the definition of uncertainty, a new footnote has been added to the TSAW. This footnote emphasizes that an atomic-weight uncertainty is a consensus (decisional) uncertainty. Not only has the Commission shielded users of the TSAW and TICE from unreliable measurements that appear in the literature as a result of unduly small uncertainties, but the aim of IUPAC has been fulfilled by which any scientist, taking any natural sample from commerce or research, can expect the sample atomic weight to lie within Ar(E) ± its uncertainty almost all of the time. KW - Atomic weight KW - Standard atomic weight KW - Uncertainty PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551299 DO - https://doi.org/10.1002/rcm.8864 SN - 1097-0231 VL - 36 IS - 15 SP - 1 EP - 15 PB - Wiley AN - OPUS4-55129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - El-Athman, Rukeia T1 - The BAM Data Store – an institutional RDM framework for Materials Science and Engineering N2 - In view of the increasing digitization of research and the use of data-intensive measurement and analysis methods, research institutions and their staff are faced with the challenge of documenting a constantly growing volume of data in a comprehensible manner, archiving them for the long term, and making them available for discovery and re-use by others in accordance with the FAIR principles. At BAM, we aim to facilitate the integration of research data management (RDM) strategies during the whole research cycle from the creation and standardized description of materials datasets to their publication in open repositories. To this end, we present the BAM Data Store, a central system for internal RDM that fulfills the heterogenous demands of materials science and engineering labs. The BAM Data Store is based on openBIS, an open-source software developed by the ETH Zurich that has originally been created for life science laboratories but that has since been deployed in a variety of research domains. The software offers a browser-based user interface for the digital representation of lab inventory entities (e.g., samples, chemicals, instruments, and protocols) and an electronic lab notebook for the standardized documentation of experiments and analyses. To investigate whether openBIS is a suitable framework for the BAM Data Store, we carried out a pilot phase during which five research groups with employees from 16 different BAM divisions were introduced to the software. The pilot groups were chosen to represent a diverse array of domain use cases and RDM requirements (e.g., small vs big data volume, heterogenous vs structured data types) as well as varying levels of prior IT knowledge on the users’ side. Overall, the results of the pilot phase are promising: While the creation of custom data structures and metadata schemas can be time-intensive and requires the involvement of domain experts, the system offers specific benefits in the form of a simplified documentation and automation of research processes, as well as constituting a basis for data-driven analysis. In this way, heterogeneous research workflows in various materials science research domains could be implemented, from the synthesis and characterization of nanomaterials to the monitoring of engineering structures. In addition to the technical deployment and the development of domain-specific metadata standards, the pilot phase also highlighted the need for suitable institutional infrastructures, processes, and role models. An institute-wide rollout of the BAM Data Store is currently being planned. T2 - Analytica Conference 2022 CY - Munich, Germany DA - 21.06.2022 KW - BAM Data Store KW - Forschungsdatenmanagement KW - Research data management KW - OpenBIS PY - 2022 AN - OPUS4-55139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - IRWG strategy update N2 - This talk presents a strategy update of the Isotope Ratio Working Group of CCQM. The focus is on future comparisons and the promotion of international comparability. T2 - IRWG Meeting CY - Online meeting DA - 12.05.2022 KW - Isotope ratio KW - Traceability KW - Metrology PY - 2022 AN - OPUS4-55160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Plan for comparison on absolute Cu isotope ratios by applying the isotope mixture approach N2 - Based on a previously circulated questionnaire, the plan for a key comparison is presented which focuses on the determination of absolute copper isotope ratios by the means of synthetic isotope mixtures. T2 - IRWG Meeting CY - Online meeting DA - 12.05.2022 KW - Absolute isotope ratio KW - Traceability KW - CCQM PY - 2022 AN - OPUS4-55161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - CCQM-P213: BAM procedure for obtaining Cu delta values N2 - BAM participated in the CCQM pilot study P213 for obtaining copper isotope delta values. This presentations provides details on the MC-ICP-MS based measruement procedure, which has been applied to obtain such copper delta values. T2 - IRWG Meeting CY - Online meeting DA - 12.05.2022 KW - Isotope delta value KW - Copper KW - Metrology KW - Traceability PY - 2022 AN - OPUS4-55162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling, Diagnostics and Applications of Laser Induced Plasma N2 - Laser-induced plasmas are widely used in many areas of science and technology; examples include spectrochemical analysis, thin film deposition, and material processing. Several topics will be addressed. First, general phenomenology of laser-induced plasmas will be discussed. Then, a chemical model will be presented based on a coupled solution of Navier-Stokes, state, radiative transfer, material transport, and chemical equations. Results of computer simulations for several chemical systems will be shown and compared to experimental observations obtained by optical imaging, spectroscopy, and tomography. The latter diagnostic tools will also be briefly discussed. Finally, a prospective application of laser-induced plasma and plasma modeling will be illustrated on the example of chemical vapor deposition of molybdenum borides and micro processing and coating of titanium dental implants. T2 - University of Saragossa, Department of Chemistry CY - Saragossa, Spain DA - June 30, 2022 KW - Laser ablation KW - Laser induced plasma KW - Plasma modeling KW - Plasma diagnostics KW - Surface coating PY - 2022 AN - OPUS4-55166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim T1 - Laser-based sorting of construction and demolition waste for the circular economy N2 - Closed material cycles and unmixed material fractions are required to achieve high recovery and recycling rates in the building industry. The growing diversity of construction and demolition waste is leading to increasing difficulties in separating the individual materials. Manual sorting involves many risks and dangers for the executing staff and is merely based on obvious, visually detectable differences for separation. An automated, sensor-based sorting of these building materials could complement or replace this practice to improve processing speed, recycling rates, sorting quality, and prevailing health conditions. A joint project of partners from industry and research institutions approaches this task by investigating and testing the combination of laser-induced breakdown spectroscopy (LIBS) and visual (VIS)/ near-infrared (NIR) spectroscopy. Joint processing of information (data fusion) is expected to significantly improve the sorting quality of various materials like concrete, main masonry building materials, organic components, etc., and may enable the detection and separation of impurities such as SO3-containing building materials (gypsum, aerated concrete, etc.). Focusing on Berlin as an example, the entire value chain will be analyzed to minimize economic/technological barriers and obstacles at the cluster level and to sustainably increase recovery and recycling rates. First LIBS measurements show promising results in distinguishing various material types. A meaningful validation shall be achieved with further practical samples. Future works will investigate the combination of LIBS and VIS/NIR spectroscopy in a fully automated measurement setup with conveyor belt speeds of 3 m/s. T2 - 6th fib Congress 2022 CY - Oslo, Norway DA - 12.06.2022 KW - LIBS KW - Recycling KW - Construction and demolition waste KW - Sorting PY - 2022 AN - OPUS4-55120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Thermographic super resolution reconstruction using 2D pseudo-random pattern illumination N2 - Thermographic non-destructive testing is based on the interaction of thermal waves with inhomogeneities. The propagation of thermal waves from the heat source to the inhomogeneity and to the detection surface according to the thermal diffusion equation leads to the fact that two closely spaced defects can be incorrectly detected as one defect in the measured thermogram. In order to break this spatial resolution limit (super resolution), the combination of spatially structured heating and numerical methods of compressed sensing can be used. The improvement of the spatial resolution for defect detection then depends in the classical sense directly on the number of measurements. Current practical implementations of this super resolution detection still suffer from long measurement times, since not only the achievable resolution depends on performing multiple measurements, but due to the use of single spot laser sources or laser arrays with low pixel count, also the scanning process itself is quite slow. With the application of most recent high-power digital micromirror device (DMD) based laser projector technology this issue can now be overcome. T2 - ICPPP21: International Conference on Photoacoustic and Photothermal Phenomena CY - Bled, Slovenia DA - 19.06.2022 KW - Thermography KW - Super resolution KW - NDT KW - Inspection KW - Internal defects KW - DMD KW - DLP PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551224 UR - https://indico.ung.si/event/5/contributions/237/ AN - OPUS4-55122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - A fast and simple PFAS extraction method for soil sample analysis using HR-CS-GFMAS N2 - Per- and polyfluorinated alkyl substances (PFASs) are a substance class of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their different chemical and physical properties as well as the high number of target substances. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate a realistic PFAS pollution level. PFAS sum parameters compromise the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for indirect fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. Here, we describe a fast and simple extraction method for the determination of the EOF using HR-CS-GFMAS in soil samples. Common approaches for the EOF determination use solid phase extraction (SPE). To omit the bias of this time consuming and expensive step we optimized a fast and simple SPE-free extraction method. The developed extraction method consists of a liquid-solid extraction using acidified methanol. Comparison of the method with and without an SPE clean-up step revealed a drastic underestimation of EOF concentrations using SPE. In the next step, the applicability of our method was tested for other solid matrices. In view of steadily increasing numbers of PFASs, our method will make an important contribution in assessing the pollution situation as well as support policy makers in deriving exposure limits for PFASs in the future. T2 - Analytica conference CY - München, Germany DA - 21.06.2022 KW - PFAS KW - HR-CS-GFMAS KW - Soil KW - Fluorine KW - SPE PY - 2022 AN - OPUS4-55124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Hodoroaba, Vasile-Dan A1 - Kraehnert, R. A1 - Hertwig, Andreas T1 - Multilevel effective material approximation for modeling ellipsometric measurements on complex porous thin films N2 - Catalysts are important components in chemical processes because they lower the activation energy and thus determine the rate, efficiency and selectivity of a chemical reaction. This property plays an important role in many of today’s processes, including the electrochemical splitting of water. Due to the continuous development of catalyst materials, they are becoming more complex, which makes a reliable evaluation of physicochemical properties challenging even for modern analytical measurement techniques and industrial manufacturing. We present a fast, vacuum-free and non-destructive analytical approach using multi-sample spectroscopic ellipsometry to determine relevant material parameters such as film thickness, porosity and composition of mesoporous IrOx–TiOy films. Mesoporous IrOx–TiOy films were deposited on Si wafers by sol–gel synthesis, varying the composition of the mixed oxide films between 0 and 100 wt%Ir. The ellipsometric modeling is based on an anisotropic Bruggeman effective medium approximation (a-BEMA) to determine the film thickness and volume fraction of the material and pores. The volume fraction of the material was again modeled using a Bruggeman EMA to determine the chemical composition of the materials. The ellipsometric fitting results were compared with complementary methods, such as scanning electron microscopy (SEM), electron probe microanalysis (EPMA) as well as environmental ellipsometric porosimetry (EEP). KW - Electrochemical catalysts KW - Mixed metal oxide KW - Multi-sample analysis KW - Spectroscopic ellipsometry KW - Thin mesoporous films PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-551026 DO - https://doi.org/10.1515/aot-2022-0007 SN - 2192-8584 SN - 2192-8576 VL - 11 IS - 3-4 (Topical issue: Ellipsometry) SP - 137 EP - 147 PB - De Gruyter CY - Berlin AN - OPUS4-55102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Olaf A1 - Seeger, Stefan A1 - Brödner, Doris A1 - Erdmann, Kerstin A1 - Rasch, Fabian T1 - Chemical characterization of ultra-fine particles released from laser printers N2 - 11 laser printers from 5 manufacturers were purchased in 2017 and tested for their UFP emissions. Size resolved sampling of the emitted particles was done with a 13 stage (30 nm to 10 µm) low pressure cascade impactor. The sampled particles were analysed for their chemical composition by thermal extraction (vaporization at 290°C) followed by GC-MS analysis. High boiling cyclic siloxanes (D10 to D16) were detected as constituents of UFP from laser printers. In comparison to measurements in 2008, aliphatic long-chain alkanes (C22 to C34) were detected additionally as chemical constituents of UFP from most of the tested printers and their amounts were higher than for cyclic siloxanes. Printers of one manufacturer showed very low UPF emissions compared to the other manufacturers. T2 - Indoor Air Conference 2022 CY - Kuopio, Finland DA - 12.06.2022 KW - UFP KW - Thermal extraction KW - Cascade impactor PY - 2022 SP - 1 EP - 4 AN - OPUS4-55106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Olaf T1 - Chemical characterization of ultra-fine particles released from laser printers N2 - 11 laser printers from 5 manufacturers were purchased in 2017 and tested for their UFP emissions. Size resolved sampling of the emitted particles was done with a 13 stage (30 nm to 10 µm) low pressure cascade impactor. The sampled particles were analysed for their chemical composition by thermal extraction (vaporization at 290°C) followed by GC-MS analysis. High boiling cyclic siloxanes (D10 to D16) were detected as constituents of UFP from laser printers. In comparison to measurements in 2008, aliphatic long-chain alkanes (C22 to C34) were detected additionally as chemical constituents of UFP from most of the tested printers and their amounts were higher than for cyclic siloxanes. Printers of one manufacturer showed very low UPF emissions compared to the other manufacturers. T2 - Indoor Air Conference 2022 CY - Kuopio, Finland DA - 12.06.2022 KW - UFP KW - Thermal extraction KW - Cascade impactor PY - 2022 AN - OPUS4-55107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinmuth-Selzle, K. A1 - Tchipilov, Teodor A1 - Backes, A. T. A1 - Tscheuschner, Georg A1 - Tang, K. A1 - Ziegler, K. A1 - Lucas, K. A1 - Pöschl, U. A1 - Fröhlich-Nowoisky, J. A1 - Weller, Michael G. T1 - Determination of the protein content of complex samples by aromatic amino acid analysis, liquid chromatography-UV absorbance, and colorimetry N2 - Fast and accurate determination of the protein content of a sample is an important and non-trivial task of many biochemical, biomedical, food chemical, pharmaceutical, and environmental research activities. Different methods of total protein determination are used for a wide range of proteins with highly variable properties in complex matrices. These methods usually work reasonably well for proteins under controlled conditions, but the results for non-standard and complex samples are often questionable. Here, we compare new and well-established methods, including traditional amino acid analysis (AAA), aromatic amino acid analysis (AAAA) based on the amino acids phenylalanine and tyrosine, reversed-phase liquid chromatography of intact proteins with UV absorbance measurements at 220 and 280 nm (LC-220, LC-280), and colorimetric assays like Coomassie Blue G-250 dye-binding assay (Bradford) and bicinchoninic acid (BCA) assay. We investigated different samples, including proteins with challenging properties, chemical modifications, mixtures, and complex matrices like air particulate matter and pollen extracts. All methods yielded accurate and precise results for the protein and matrix used for calibration. AAA, AAAA with fluorescence detection, and the LC-220 method yielded robust results even under more challenging conditions (variable analytes and matrices). These methods turned out to be well-suited for reliable determination of the protein content in a wide range of samples, such as air particulate matter and pollen. KW - Air particulate matter KW - Aromatic amino acid analysis KW - Atmospheric aerosol KW - Chemical protein modification KW - Derivatization KW - Nitration KW - Nitrotyrosine KW - LC-UV absorbance KW - Pollen extract KW - Protein quantification KW - Protein test KW - Kjeldahl KW - Tyrosine KW - Phenylalanine KW - Hydrolysis KW - Bradford KW - BCA test KW - 280 nm KW - Air filter samples KW - Fluorescence KW - HPLC KW - Chromatography KW - Protein content KW - 150th anniversary of BAM KW - Topical collection: Analytical Methods and Applications in the Materials and Life Sciences PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545924 UR - https://pubmed.ncbi.nlm.nih.gov/35320366/ DO - https://doi.org/10.1007/s00216-022-03910-1 SP - 1 EP - 14 PB - Springer Nature Limited CY - New York, Heidelberg AN - OPUS4-54592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Heidt, Heinrich A1 - Mundry, Eberhard T1 - "Klassische" Methoden der zerstörungsfreien Materialprüfung N2 - Mit Hilfe der zerstörungsfreien Prüfung (ZfP) sind i.a. verborgene Ungänzen oder Mängel in Werkstoffen, Bauteilen oder Konstruktionen zu finden, und zwar mit Verfahren, deren Anwendung am Prüfobjekt keinesfalls seine Verwendbarkeit schädigende Veränderungen hervorrufen dürfen. Dabei sind Verfahrensauswahl und -anwendung auf das Prüfobjekt, seine Verwendung und das dabei bestehende Sicherheitsbedürfnis so abzustimmen, daß das angestrebte Prüfziel mit ausreichender Zuverlässigkeit bei einem Minimum an Prüfaufwand erreicht wird. PY - 1968 SP - 1 EP - 16 PB - Bundesanstalt für Materialprüfung (BAM) CY - Berlin AN - OPUS4-54705 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Denkler, Tilman T1 - Comparison of the Operation of Accreditation Bodies in Europe - Final Report 2nd Round N2 - In 2019 the Bundesanstalt für Materialforschung und –prüfung (BAM) conducted a benchmarking to compare the operations of European accreditation bodies and to identify best practices, with the aim of improving key processes in accreditation. Ten European accreditation bodies attended the comparison, four of which had already taken part in the pilot phase of the benchmarking project, which was conducted in 2017 by the German accreditation body Deutsche Akkreditierungsstelle GmbH (DAkkS) and BAM. The study, designed to examine and compare the operation of accreditation bodies in Europe, used a management tool called Process Maturity Benchmarking Tool, which was especially elaborated and validated for this purpose in the pilot phase, in order to determine the values of indicators, thus enabling a comparison of the accreditation bodies despite different operational processes and organizational forms. The management tool is based on the analysis of selected processes with high relevance for the operation of accreditation bodies. The processes are derived from a process map designed for accreditation bodies in a universally applicable way. The indicators used to characterize the processes come from two sources: The first source relates to data already available from internal databases, reports, financial audits, and others. The second source is derived from the self-evaluation of process maturity performed by the accreditation bodies. The criteria for evaluating process maturities were designed by applying the criteria of the EFQM excellence model 2013 of the European Foundation for Quality Management (EFQM) to the processes identified in the process map. The results of the analysis were presented to and discussed with representatives of the ten accreditation bodies at a Results-Workshop that took place at BAM on 21/22 January 2020. KW - Akkreditierung KW - Accreditation KW - Benchmarking KW - EFQM Excellence Modell KW - Quality Infrastructure KW - Total Quality Management PY - 2020 SP - 1 EP - 70 AN - OPUS4-54712 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hieu, D.T. A1 - Kosslick, H. A1 - Riaz, M. A1 - Schulz, A. A1 - Springer, A. A1 - Frank, M. A1 - Jäger, Christian A1 - Minh Thu, N.T. A1 - Son, L.T. T1 - Acidity and Stability of Bronsted Acid Sites in Green Clinoptilolite Catalysts and Catalytic Performance in the Etherification of Glycerol N2 - Natural zeolite clinoptilolite CLIN with a framework ratio of Si/Al ≥ 4 containing mainly potassium and calcium ions in its internal channel system was used as a starting material. The acidic HCLIN catalysts were prepared under soft conditions avoiding the use of environmental less benign mineral acids. The starting material was ion exchanged using a 0.2 M aqueous ammonium nitrate solution at a temperature 80 ◦C for 2 h. The obtained NH4CLIN was converted into the acid HCLIN catalyst by calcination at 300–600 ◦C. The obtained samples were characterized by XRD, FTIR, SEM/TEM, AAS, and EDX element mapping. The state of aluminium and silicon was studied by 27Al- and 29SiMAS NMR spectroscopy. The textural properties of the catalysts were investigated by nitrogen adsorption and desorption measurements. The Brønsted acidity of the HCLIN catalysts was studied by temperature-programmed decomposition of the exchanged ammonium ions releasing ammonia as well as 1H MAS NMR, {1H–27Al} Trapdor, and {1H–27Al} Redor experiments. The strongly agglomerated samples were crystalline and thermally stable up to >500 ◦C. Although a part of the clinoptilolite framework is maintained up to 600 ◦C, a loss of crystallinity is already observed starting from 450 ◦C. The specific surface areas of the starting CLIN and ammonium exchanged NH4CLIN are low with ca. 26 m2/g. The pores are nearly blocked by the exchangeable cations located in the zeolite pores. The thermal decomposition of the ammonium ions by calcination at 400 ◦C causes an opening of the pore entrances and a markable increase in the specific micropore area and micropore volume to ca. 163 m2/g and 0.07 cm3/g, respectively. It decreases with further rising calcination temperature indicating some structural loss. The catalysts show a broad distribution of Brønsted acid sites (BS) ranging from weak to strong sites as indicated the thermal decomposition of exchanged ammonium ions (TPDA). The ammonium ion decomposition leaving BS, i.e., H+ located at Al–O–Si framework bridges, starts at ≥250 ◦C. A part of the Brønsted sites is lost after calcination specifically at 500 ◦C. It is related to the formation of penta-coordinated aluminium at the expense of tetrahedral framework aluminium. The Brønsted sites are partially recreated after repeated ammonium ion exchange. The catalytic performance of the acidic HCLIN catalysts was tested in the etherification of glycerol as a green renewable resource with different C1 -C4 alcohols. The catalysts are highly active in the etherification of glycerol, especially with alcohols containing the branched, tertiary alkyl groups. Highest activity is observed with the soft activated catalyst HCLIN300 (300 ◦C, temperature holding time: 1 min). A total of 78% conversion of glycerol to mono and di ether were achieved with tert-butanol at 140 ◦C after 4 h of reaction. The mono- and di-ether selectivity were 75% and 25%, respectively. The catalyst can be reused. KW - Etherification KW - Glycerol KW - Zeolite KW - Clinoptilolite KW - Bronsted acidity KW - Dehydroxylation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546982 DO - https://doi.org/10.3390/catal12030253 VL - 12 IS - 3 SP - 1 EP - 24 PB - MDPI AN - OPUS4-54698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Tscheuschner, Georg T1 - Entwicklung einer Methode zur schnellen Identifikation von Antikörpern mittels MALDI-TOF-MS N2 - Im Vergleich zu anderen Proteinen ist die Identifizierung von Antikörpern anhand ihrer Sequenz zum Beispiel mittels "peptide mass fingerprinting" schwierig. Da die Sequenzinformation eines Antikörpers aufgrund der hypersomatischen Mutation während der Affinitätsreifung nicht im Genom eines Organismus gespeichert ist, kann die Aminosäuresequenz nicht auf einfachem Weg der DNA-Sequenzierung gewonnen werden. Das ist nur in seltenen Fällen möglich, wenn dem Endanwender der Zellklon der Antikörper-produzierenden Zelle zugänglich ist. Eine Sequenzierung auf Protein-Ebene ist sehr aufwändig und teuer und wird daher fast nie für die Charakterisierung von analytischen Antikörpern verwendet. Der Mangel an Validierung dieser analytischen Antikörper, die bei Experimenten verwendeten werden, löst aber eine Reihe Probleme aus, die die Wiederholbarkeit dieser Experimente schwierig und in einigen Fällen unmöglich macht. Das sorgt jährlich für verschwendete Forschungsgelder in Milliardenhöhe und hindert den wissenschaftlichen Fortschritt. Ziel der vorliegenden Arbeit war die Entwicklung einer einfachen und schnellen Methode, die es trotzdem ermöglicht, die Identifikation von Antikörpern sicherzustellen. Dazu wurde eine Methode basierend auf dem "peptide mass fingerprinting" gewählt. Das Problem der unbekannten Aminosäuresequenz der Antikörper wurde gelöst, indem lediglich die Peptidmuster der entstehenden Fingerprint-Spektren zur Identifikation herangezogen wurden. MALDI wurde dabei als Ionisationsmethode für die Massenspektrometrie gewählt, da die resultierenden Spektren im Gegensatz zu ESI-MS einfach auszuwerten sind. Auch kann auf eine vorige Trennung der Peptide mittels LC verzichtet werden, was zusätzlich Analysenzeit spart. Für die Proteinspaltung wurde eine simple saure Hydrolyse mittels Ameisensäure gewählt. Im Vergleich zum herkömmlichen Trypsin-Verdau konnten auf zeitraubende Arbeitsschritte wie Denaturierung, Reduktion und Alkylierung der Antikörper verzichtet werden. Die Hydrolyse mittels Ameisensäure wurde bisher nur auf kleine und mittelgroße Proteine angewendet, sodass im ersten Teil dieser Arbeit mehrere Schritte optimiert wurden bevor zufriedenstellende Fingerprint-Spektren von Antikörpern erhalten wurden. KW - Peptide KW - Fingerprint KW - Peptide mass fingerprinting KW - Massenspektrometrie KW - Saure Hydrolyse KW - Festphasenextraktion KW - Protein G KW - Ameisensäure KW - ABID KW - Korrelationsmatrix PY - 2019 SP - 1 EP - 116 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54626 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hirschberg, L. A1 - Bake, Friedrich A1 - Knobloch, K. A1 - Hulshoff, S. A1 - Hirschberg, A. T1 - Experimental investigations of indirect noise due to modulation of axial vorticity and entropy upstream of a choked nozzle N2 - An experimental cold-gas study of the response of a choked convergent–divergent nozzle to swirl perturbations is presented. The perturbations were obtained by means of upstream unsteady tangential injections into initially steady flows with different values of steady background swirl. The swirl perturbations induced changes in the axial mass-flow rate, due to either their ingestion or evacuation by the nozzle. This in turn caused a downstream acoustic response. For low-intensity background swirl the responses were found to be similar to those obtained without steady background swirl. Perturbations of a high-intensity background swirl led to different effects. For long injection times, the negative mass-flow rate modulation occurred in two stages. The first stage was similar to that of the background-swirl free case. The second stage occurred after a short time delay, and induced a much stronger negative acoustic response. This unexpected behavior suggests that a significant part of the tangentially injected fluid flows upstream inducing an accumulation of swirl, which is – after tangential injection is ceased – suddenly cleared out through the nozzle. A scaling rule for the amplitudes of these acoustic responses is reported. Furthermore, quasi-steady models, based on steady-state measurements are proposed. These models predict the downstream acoustic response amplitude within a factor two. Additionally, preliminary empirical evidence of the effect of swirl on the downstream acoustic response due to the interaction of entropy patches with a choked nozzle is reported. This was obtained by comparison of sound produced by abrupt radial or tangential sonic injection, upstream from the choked nozzle, of air from a reservoir at room temperature to that from a reservoir with a higher stagnation temperature. Because the mass flow through the nozzle does not increase instantaneously, the injected higher-enthalpy air accumulates upstream of the injection-port position in the main flow. This eventually induces a large downstream acoustic pulse when tangential injection is interrupted. The magnitude of the resulting sound pulse can reach that of a quasi-steady response of the nozzle to a large air patch with a uniform stagnation temperature equal to that of the upstream-injected heated air. This hypothesis is consistent with the fact that the initial indirect-sound pulse is identical to one obtained with unheated air injection. The authors posit that – given all of the insight gleaned from them in this case – acoustic measurements of indirect sound appear to be a potentially useful diagnostic tool. KW - Aeroacoustics KW - Indirect combustion noise KW - Vorticity noise KW - Entropy noise KW - Swirl PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548331 DO - https://doi.org/10.1016/j.jsv.2022.116989 SN - 0022-460X VL - 532 SP - 1 EP - 22 PB - Elsevier Ltd. AN - OPUS4-54833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lecompagnon, Julien A1 - Ahmadi, Samim A1 - Hirsch, Philipp Daniel A1 - Rupprecht, C. A1 - Ziegler, Mathias T1 - Thermographic detection of internal defects using 2D photothermal super resolution reconstruction with sequential laser heating N2 - Thermographic photothermal super resolution reconstruction enables the resolution of internal defects/inhomogeneities below the classical limit, which is governed by the diffusion properties of thermal wave propagation. Based on a combination of the application of special sampling strategies and a subsequent numerical optimization step in post-processing, thermographic super resolution has already proven to be superior to standard thermographic methods in the detection of one-dimensional defect/inhomogeneity structures. In our work, we report an extension of the capabilities of the method for efficient detection and resolution of defect cross sections with fully two-dimensional structured laser-based heating. The reconstruction is carried out using one of two different algorithms that are proposed within this work. Both algorithms utilize the combination of several coherent measurements using convex optimization and exploit the sparse nature of defects/inhomogeneities as is typical for most nondestructive testing scenarios. Finally, the performance of each algorithm is rated on reconstruction quality and algorithmic complexity. The presented experimental approach is based on repeated spatially structured heating by a high power laser. As a result, a two-dimensional sparse defect/inhomogeneity map can be obtained. In addition, the obtained results are compared with those of conventional thermographic inspection methods that make use of homogeneous illumination. Due to the sparse nature of the reconstructed defect/inhomogeneity map, this comparison is performed qualitatively. KW - Thermography KW - Super resolution KW - NDT KW - Inspection KW - Internal defects PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548351 DO - https://doi.org/10.1063/5.0088102 SN - 1089-7550 VL - 131 IS - 18 SP - 1 EP - 12 PB - AIP Publishing AN - OPUS4-54835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufschläger, Daniel A1 - Gaal, Mate T1 - Sending and receiving acoustic waves using atmospheric pressure plasmas N2 - Atmospheric pressure plasmas interact in various physical ways with their surroundings. They release heat and generate charge carriers, which leads to two effects. The first effect is the generation of acoustic waves due to heat release, known as the thermoacoustic effect, and the second effect is the perturbation of the resting fluid provoked by the release of charge carriers, called “ionic wind”. The direct connection between the charge carrier production of the discharge arrangement and the surroundings also allows the detection of acoustic waves by tracking the electrical current of the arrangement. This contribution introduces a multi-fluid model approach to describe the acoustic interaction of atmospheric plasmas. In addition, we present experimental results on commercially available and in-house fabricated discharge arrangements for either emitting or receiving acoustic waves. T2 - DAGA 2022 - 48. Jahrestagung für Akustik CY - Stuttgart, Germany DA - 21.03.2022 KW - Plasma acoustics KW - Atmospheric pressure discharges KW - Ait-coupled ultrasound PY - 2022 SN - 978-3-939296-20-1 VL - 48 SP - 923 EP - 926 CY - Berlin AN - OPUS4-54681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chambers, M. S. A1 - Hunter, R. D. A1 - Hollamby, M. J. A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Danks, A. E. A1 - Schnepp, Z. T1 - In Situ and Ex Situ X‑ray Diffraction and Small-Angle X‑ray Scattering Investigations of the Sol−Gel Synthesis of Fe3N and Fe3C N2 - Iron nitride (Fe3N) and iron carbide (Fe3C) nanoparticles can be prepared via sol−gel synthesis. While sol−gel methods are simple, it can be difficult to control the crystalline composition, i.e., to achieve a Rietveld-pure product. In a previous in situ synchrotron study of the sol−gel synthesis of Fe3N/Fe3C, we showed that the reaction proceeds as follows: Fe3O4 → FeOx → Fe3N → Fe3C. There was considerable overlap between the different phases, but we were unable to ascertain whether this was due to the experimental setup (side-on heating of a quartz capillary which could lead to thermal gradients) or whether individual particle reactions proceed at different rates. In this paper, we use in situ wide- and small-angle X-ray scattering (wide-angle X-ray scattering (WAXS) and small-angle X-ray scattering (SAXS)) to demonstrate that the overlapping phases are indeed due to variable reaction rates. While the initial oxide nanoparticles have a small range of diameters, the size range expands considerably and very rapidly during the oxide−nitride transition. This has implications for the isolation of Rietveld-pure Fe3N, and in an extensive laboratory study, we were indeed unable to isolate phasepure Fe3N. However, we made the surprising discovery that Rietveld-pure Fe3C nanoparticles can be produced at 500 °C with a sufficient furnace dwell time. This is considerably lower than the previous reports of the sol−gel synthesis of Fe3C nanoparticles. KW - Small-angle X-ray Scattering KW - SAXS KW - Diffraction KW - XRD KW - Scattering KW - Sol-gel KW - Iron nitride KW - Nanoparticles KW - Iron carbide KW - Catalyst KW - In-situ KW - Ex-situ KW - Synthesis KW - Synchrotron PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548226 DO - https://doi.org/10.1021/acs.inorgchem.1c03442 VL - 61 IS - 18 SP - 6742 EP - 6749 PB - ACS Publications CY - Washington AN - OPUS4-54822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Microspectroscopy reveals dust-derived apatite grains in highly-weathered soils from the Kohala climosequence on Hawaii N2 - Dust deposition is an important source of phosphorus (P) to many ecosystems. However, there is little evidence of dust-derived P-containing minerals in soils. Here we studied P forms along a well-described climatic gradient on Hawaii, which is also a dust deposition gradient. Soil mineralogy and soil P forms from six sites along the climatic gradient were analyzed with bulk (X-ray diffraction and P K-edge X-ray absorption near edge structure) and microscale (X-ray fluorescence, P K-edge X-ray absorption near edge structure, and Raman) analysis methods. In the wettest soils, apatite grains ranging from 5 to 30 μm in size were co-located at the micro-scale with quartz, a known continental dust indicator suggesting recent atmospheric deposition. In addition to colocation with quartz, further evidence of dust-derived P included backward trajectory modeling indicating that dust particles could be brought to Hawaii from the major global dust-loading areas in central Asia and northern Africa. Although it is not certain whether the individual observed apatite grains were derived from long-distance transport of dust, or from local dust sources such as volcanic ash or windblown fertilizer, these observations offer direct evidence that P-containing minerals have reached surface layers of highly-weathered grassland soils through atmospheric deposition. T2 - BESSY Science Seminar CY - Online meeting DA - 01.04.2022 KW - Phosphorus KW - Soil KW - X-ray diffraction KW - X-ray absorption near-edge structure (XANES) spectroscopy KW - Fertilizer KW - Raman spectroscopy KW - infrared spectroscopy PY - 2022 AN - OPUS4-54584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pech May, Nelson Wilbur T1 - Robot-assisted laser thermography for surface breaking crack detection on complex shaped components N2 - Laser thermography using a focused (spot or line) beam has proved to be effective for detection of surface breaking cracks on planar samples. In this work, we use the same principle, but applied to complex shaped components, like a rail cross-section, a gear, and a gas turbine blade. We use a six-axis robot to move the sample in-front of our thermographic setup. Several scanning-path and thermographic parameters are explored: scanning speed, density of points in each scanning slice, laser power, camera framerate. Additionally, we explore semi-automatic evaluation algorithms for crack detection, as well as 2D-to-3D registration of the found indications. T2 - SPIE Future Sensing Technologies 2023 CY - Yokohama, Japan DA - 18.04.2023 KW - Flying line thermography KW - Crack-detection algorithms PY - 2023 UR - https://www.spiedigitallibrary.org/conference-proceedings-of-spie/12327/1232715/Robot-assisted-infrared-thermography-for-surface-breaking-crack-detection-on/10.1117/12.2666757.short AN - OPUS4-57594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Phased-Array-Prüfköpfe für luftgekoppelte Ultraschallprüfung auf Basis von zellulären Kunststoffen N2 - Luftgekoppelte Ultraschallprüfung setzt sich immer häufiger gegen die konventionelle Ultraschallprüfung von Leichtbaukomponenten durch, und zwar in vielen Industriezweigen von der Holzindustrie bis zur Luftfahrt. aWährend die Phased-Array-Technik mittlerweile zu dem industriellen Standard im Bereich der Prüfung mit Ankopplung gehört, wird luftgekoppelte Ultraschallprüfung meist mit zwei Wandlern in Durchschallung durchgeführt. Deswegen werden Vorteile der Phased-Array-Technik wie beispielsweise elektronische Fokussierung oder Schwenkung des Einschallwinkels für luftgekoppelte Prüfung selten genutzt. In diesem Beitrag werden die laufenden Arbeiten an der Entwicklung eines neuen Phased-Array-Geräts vorgestellt, mit dem Schwerpunkt an der Charakterisierung der Prüfköpfe und ihrer Schallfelder. Das Gerät besteht aus einem linearen Phased-Array-Prüfkopf, einer Sende- und einer Empfangseinheit. Die Hauptinnovation unserer Arbeit ist die Anwendung von zellulären Kunststoffen für den Bau eines Arrays, wobei der Sender mit Hochspannung von ca. 1500 V angeregt wird. Geladene zelluläre Polymere werden auch Ferroelektrete oder Piezoelektrete genannt. Sie weisen einen sehr niedrigen Elastizitätsmodul und dadurch eine niedrige akustische Impedanz auf, so dass auf den Einbau von Anpassschichten verzichtet werden kann. Eine sehr niedrige mechanische Kreuzkopplung bei Ferroelektreten ermöglicht eine unabhängige Anregung einzelner Elemente, was bei Piezokompositen deutlich schwieriger wäre. Die Entwicklung der Array-Prüfköpfe wurde durch Berechnungen des Schallfeldes unterstützt, die auf Punktquellensynthese basieren. Die beabsichtigte Anwendung von Phased-Array-Prüfköpfen und des Prüfsystems sind die Durchschallung mit Fokussierung, elektronischer Scan und die Schwenkung des Einschallwinkels zur Anregung von geführten Wellen, angewandt an carbonfaserverstärkten Kunststoffen und ähnlichen Materialien. Die Anwendung von geführten Wellen bietet die Perspektive, Bauteile mit einseitiger Zugänglichkeit zu prüfen. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Luftgekoppelte Ultraschallprüfung KW - Ferroelektret KW - Ultraschallwandler KW - Phased Array PY - 2023 AN - OPUS4-57609 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. A1 - Johann, Sergej A1 - Kohlhoff, Harald A1 - Neumann, Patrick P. T1 - Revisiting Environmental Sensing Nodes: Lessons Learned and Way Forward N2 - Setting up sensors for the purpose of environmental monitoring should be a matter of days, but often drags over weeks or even months, preventing scientists from doing real research. Additionally, the newly developed hardware and software solutions are often reinventing existing wheels. In this short paper, we revisit the design of our environmental sensing node that has been monitoring industrial areas over a span of two years. We share our findings and lessons learned. Based on this, we outline how a new generation of sensing node(s) can look like. T2 - SMSI 2023 Conference Sensor and Measurement Science International CY - Nuremberg, Germany DA - 08.05.2023 KW - Sensing node KW - Sensor network KW - Environmental monitoring KW - Low-cost KW - LoRaWAN PY - 2023 SN - 978-3-9819376-8-8 DO - https://doi.org/10.5162/SMSI2023/C5.1 SP - 173 EP - 174 PB - AMA Service GmbH CY - Wunstorf AN - OPUS4-57454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. T1 - Revisiting Environmental Sensing Nodes: Lessons Learned and Way Forward N2 - Setting up sensors for the purpose of environmental monitoring should be a matter of days, but often drags over weeks or even months, preventing scientists from doing real research. Additionally, the newly developed hardware and software solutions are often reinventing existing wheels. In this short paper, we revisit the design of our environmental sensing node that has been monitoring industrial areas over a span of two years. We share our findings and lessons learned. Based on this, we outline how a new generation of sensing node(s) can look like. T2 - SMSI 2023 Conference Sensor and Measurement Science International CY - Nuremberg, Germany DA - 08.05.2023 KW - Sensing node KW - Sensor network KW - Environmental monitoring KW - Low-cost KW - LoRaWAN PY - 2023 AN - OPUS4-57455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - An improved method for the determination of PFASs using HR CS GFMAS via GaF detection N2 - Introduction Per- and polyfluorinated alkyl substances (PFASs) are a group of over 4730 individual compounds. Several PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate realistic PFAS pollution levels. Methods For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. In our study we used high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) which is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. Results Here, we present an improved method for the determination of PFASs using HR-CS-GFMAS via GaF detection. The optimized method includes a modifier pretreatment step using a mixture of Mg, Pd and Zr and a correction measurement using perfluorooctanoic acid. The combination of both resulted in increased accuracy and precision as well as overall lower detection limits. Furthermore, during optimization the influence of species-specific responses during HR-CS-GFMAS analysis was reduced resulting in a more accurate determination of PFAS sum parameters. To test the applicability of the improved method, we analysed soil samples from a former fire-fighting training area combining the improved method for detection with our previously optimized extraction method for extractable organically bound fluorine (EOF) determination in soils. Innovative aspects • Highly sensitive and selective method for fluorine/PFASs analysis based on HR-CS-GFMAS • Increased accuracy for the determination of EOF • Reduction of PFAS species-specific responses by optimized modifier conditions T2 - ANAKON23 CY - Vienna, Austria DA - 11.04.2023 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine PY - 2023 AN - OPUS4-57409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ermilova, Elena A1 - Weise, Matthias A1 - Hertwig, Andreas T1 - Application of imaging ellipsometry and white light interference microscopy for detection of defects in epitaxially grown 4H-SiC layers N2 - Critical defects, also known as device killers, in wide bandgap semiconductors significantly affect the performance of power electronic devices. We used the methods imaging ellipsometry (IE) and white light interference microscopy (WLIM) in a hybrid optical metrology study for fast and non-destructive detection, classification, and characterisation of defects in 4H–SiC homoepitaxial layers on 4H–SiC substrates. Ellipsometry measurement results are confirmed by WLIM. They can be successfully applied for wafer characterisation already during production of SiC epilayers and for subsequent industrial quality control. T2 - EOS Annual Meeting (EOSAM 2022) CY - Porto DA - 12.09.2022 KW - Imaging ellipsometry KW - White light interference microscopy KW - 4H–SiC KW - Defects PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-574209 DO - https://doi.org/10.1051/jeos/2023018 SN - 1990-2573 VL - 19 IS - 1 SP - 1 EP - 8 PB - EDP Sciences AN - OPUS4-57420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Valdestilhas, Andre A1 - Bayerlein, Bernd A1 - Moreno Torres, Benjami A1 - Zia, Ghezal Ahmad Jan A1 - Muth, Thilo T1 - The Intersection Between Semantic Web and Materials Science N2 - The application and benefits of Semantic Web Technologies (SWT) for managing, sharing, and (re-)using of research data are demonstrated in implementations in the field of Materials Science and Engineering (MSE). However, a compilation and classification are needed to fully recognize the scattered published works with its unique added values. Here, the primary use of SWT at the interface with MSE is identified using specifically created categories. This overview highlights promising opportunities for the application of SWT to MSE, such as enhancing the quality of experimental processes, enriching data with contextual information in knowledge graphs, or using ontologies to perform specific queries on semantically structured data. While interdisciplinary work between the two fields is still in its early stages, a great need is identified to facilitate access for nonexperts and develop and provide user-friendly tools and workflows. The full potential of SWT can best be achieved in the long term by the broad acceptance and active participation of the MSE community. In perspective, these technological solutions will advance the field of MSE by making data FAIR. Data-driven approaches will benefit from these data structures and their connections to catalyze knowledge generation in MSE. KW - Linked open data KW - Materials science KW - Ontology KW - Semantic web PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575506 DO - https://doi.org/10.1002/aisy.202300051 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-57550 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat A1 - Hicke, Konstantin A1 - Krebber, Katerina T1 - phi-g OTDR utilizing geometric phase N2 - Geometric phase measured per beat period in a ϕ-OTDR based on coherent heterodyne detection is used to measure strain. Proposed method is robust to polarisation mismatch fading as a polarisation mismatch between interfering beams is not a hindrance to the measurement of the geometric phase. The Geometric phase is a function of the intensities of the interfering beams as well as the envelope of the beat signal. Its calculation does not require phase unwrapping and accordingly does not suffer the phase unwrapping errors. It is required to be equated with the traditionally measured phase by applying a scaling factor. The spatial resolution of the measured strain is reduced as it is calculated per beat period. Results are verified using a piezo-electric transducer inline a fiber-under-test. T2 - European Workshop on Optical Fibre Sensors (EWOFS 2023) CY - Mons, Belgium DA - 23.05.23 KW - Coherent Heterodyne KW - Geometric Phase KW - Distributed Fiber Optic Sensor PY - 2023 DO - https://doi.org/10.1117/12.2678295 SP - 1 EP - 5 PB - SPIE AN - OPUS4-57551 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Hufschläger, Daniel A1 - Gohlke, Dirk A1 - Weise, Matthias A1 - Ilse, D. A1 - Hillger, W. A1 - Szewieczek, A. T1 - Thermoakustische und Ferroelektret-Wandler als Phased-Array-Sender für luftgekoppelte Ultraschallprüfung N2 - Die üblichen Verfahren der zerstörungsfreien Prüfung mit Ultraschall basieren auf der Verwendung von flüssigen Koppelmitteln. Luftgekoppelte Prüfung setzt sich gegen die konventionellen Verfahren durch, wenn die Flüssigkeit nicht erwünscht oder den Prüfling gar beschädigen kann. Zwei Technologien für Erzeugung von Ultraschallsignalen sind vielversprechend: thermoakustische Wandler und Ferroelektret-Wandler. Basierend auf diesen beiden Technologien wurden Array-Sender gebaut und in diesem Beitrag miteinander verglichen. Thermoakustische Wandler basieren auf Dünnschichttechnologie und bieten eine resonanzfreie Erzeugung von Ultraschall. Sie bestehen aus einer dünnen elektrisch leitenden Schicht und werden mit kurzen elektrischen Pulsen angeregt. Die Erhöhung der thermischen Energie führt zur Erzeugung von akustischen Wellen in der umgebenden Luft. Bei Ferroelektret-Wandlern handelt es sich um polarisierte zelluläre Kunststoffe, die für den Bau eines Array-Senders besonders gut geeignet sind. Einige Ferroelektrete weisen eine hervorragende an Luft angepasste akustische Impedanz auf, so dass auf den Einsatz von Anpassschichten verzichtet werden kann. Ein sehr niedriges mechanisches Übersprechen zwischen einzelnen Elementen ermöglicht eine unabhängige Anregung einzelner Elemente, was bei Piezokompositen deutlich schwieriger wäre. Mit der Phased-Array-Technik können elektronische Fokussierung oder Schwenkung des Einschallwinkels für eine luftgekoppelte Prüfung genutzt werden. Die Schallfelder von diesen beiden Technologien wurden berechnet, gemessen und miteinander verglichen. Die Vorteile und Nachteile der beiden Technologien werden dargestellt. T2 - DAGA 2023 Jahrestagung für Akustik CY - Hamburg, Germany DA - 06.03.2023 KW - Luftgekoppelte Ultraschallprüfung KW - Thermoakustik KW - Ferroelektret KW - Phased Array PY - 2023 UR - https://pub.dega-akustik.de/DAGA_2023 SN - 978-3-939296-21-8 SP - 1594 EP - 1597 AN - OPUS4-57554 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Thermoakustische und Ferroelektret-Wandler als Phased-Array-Sender für luftgekoppelte Ultraschallprüfung N2 - Die üblichen Verfahren der zerstörungsfreien Prüfung mit Ultraschall basieren auf der Verwendung von flüssigen Koppelmitteln. Luftgekoppelte Prüfung setzt sich gegen die konventionellen Verfahren durch, wenn die Flüssigkeit nicht erwünscht oder den Prüfling gar beschädigen kann. Zwei Technologien für Erzeugung von Ultraschallsignalen sind vielversprechend: thermoakustische Wandler und Ferroelektret-Wandler. Basierend auf diesen beiden Technologien wurden Array-Sender gebaut und in diesem Beitrag miteinander verglichen. Thermoakustische Wandler basieren auf Dünnschichttechnologie und bieten eine resonanzfreie Erzeugung von Ultraschall. Sie bestehen aus einer dünnen elektrisch leitenden Schicht und werden mit kurzen elektrischen Pulsen angeregt. Die Erhöhung der thermischen Energie führt zur Erzeugung von akustischen Wellen in der umgebenden Luft. Bei Ferroelektret-Wandlern handelt es sich um polarisierte zelluläre Kunststoffe, die für den Bau eines Array-Senders besonders gut geeignet sind. Einige Ferroelektrete weisen eine hervorragende an Luft angepasste akustische Impedanz auf, so dass auf den Einsatz von Anpassschichten verzichtet werden kann. Ein sehr niedriges mechanisches Übersprechen zwischen einzelnen Elementen ermöglicht eine unabhängige Anregung einzelner Elemente, was bei Piezokompositen deutlich schwieriger wäre. Mit der Phased-Array-Technik können elektronische Fokussierung oder Schwenkung des Einschallwinkels für eine luftgekoppelte Prüfung genutzt werden. Die Schallfelder von diesen beiden Technologien wurden berechnet, gemessen und miteinander verglichen. Die Vorteile und Nachteile der beiden Technologien werden dargestellt. T2 - DAGA 2023 Jahrestagung für Akustik CY - Hamburg, Germany DA - 06.03.2023 KW - Luftgekoppelte Ultraschallprüfung KW - Thermoakustik KW - Ferroelektret KW - Phased Array PY - 2023 AN - OPUS4-57555 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Hufschläger, Daniel A1 - Gohlke, Dirk A1 - Weise, Matthias A1 - Ilse, D. A1 - Hillger, W. A1 - Szewieczek, A. T1 - Phased-Array-Prüfköpfe für luftgekoppelte Ultraschallprüfung auf Basis von zellulären Kunststoffen N2 - Luftgekoppelte Ultraschallprüfung setzt sich immer häufiger gegen die konventionelle Ultraschallprüfung von Leichtbaukomponenten durch, und zwar in vielen Industriezweigen von der Holzindustrie bis zur Luftfahrt. Während die Phased-Array-Technik mittlerweile zu dem industriellen Standard im Bereich der Prüfung mit Ankopplung gehört, wird luftgekoppelte Ultraschallprüfung meist mit zwei Wandlern in Durchschallung durchgeführt. Deswegen werden Vorteile der Phased-Array-Technik wie beispielsweise elektronische Fokussierung oder Schwenkung des Einschallwinkels für luftgekoppelte Prüfung selten genutzt. In diesem Beitrag werden die laufenden Arbeiten an der Entwicklung eines neuen Phased-Array-Geräts vorgestellt, mit dem Schwerpunkt an der Charakterisierung der Prüfköpfe und ihrer Schallfelder. Das Gerät besteht aus einem linearen Phased-Array-Prüfkopf, einer Sende- und einer Empfangseinheit. Die Hauptinnovation unserer Arbeit ist die Anwendung von zellulären Kunststoffen für den Bau eines Arrays, wobei der Sender mit Hochspannung von ca. 1500 V angeregt wird. Geladene zelluläre Polymere werden auch Ferroelektrete oder Piezoelektrete genannt. Sie weisen ein sehr niedriges Elastizitätsmodul und dadurch eine niedrige akustische Impedanz auf, so dass auf den Einbau von Anpassschichten verzichtet werden kann. Eine sehr niedrige mechanische Kreuzkopplung bei Ferroelektreten ermöglicht eine unabhängige Anregung einzelner Elemente, was bei Piezokompositen deutlich schwieriger wäre. Die Entwicklung der Array-Prüfköpfe wurde durch Berechnungen des Schallfeldes unterstützt, die auf Punktquellensynthese basieren. Die beabsichtigte Anwendung von Phased-Array-Prüfköpfen und des Prüfsystems sind die Durchschallung mit Fokussierung, elektronischer Scan und die Schwenkung des Einschallwinkels zur Anregung von geführten Wellen, angewandt an carbonfaserverstärkten Kunststoffen und ähnlichen Materialien. Die Anwendung von geführten Wellen bietet die Perspektive, Bauteile mit einseitiger Zugänglichkeit zu prüfen. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Luftgekoppelte Ultraschallprüfung KW - Ferroelektret KW - Ultraschallwandler KW - Phased Array PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575564 SP - 1 EP - 6 AN - OPUS4-57556 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Thermoakustische Gruppenstrahler: Theorie und Anwendungen N2 - Bei der Prüfung von Werkstücken mit empfindlichen Oberflächen oder auch hydrophilen Werkstoffen sind traditionelle ultraschallbasierte zerstörungsfreie Prüfmethoden wie die Kontakttechnik oder die Tauchtechnik in vielen Anwendungsfällen aufgrund der Flüssigkeitsankopplung nicht anwendbar. Die luft-gekoppelte Ultraschallprüfung umgeht diese Problematik und eröffnet neue Prüfszenarien. Derzeit werden zwei Varianten der Schallerzeugung als vielversprechend angesehen: ferroelektrische Folien und thermoakustische Dünnschichtwandler. Thermoakustische Wandler ermöglichen die resonanzfreie Erzeugung von Ultraschall und somit kurze zeitliche Impulse sowie eine sehr breitbandige Anregung. Durch die Verwendung von gekrümmten Substraten ist sowohl eine Herstellung von planaren als auch fokussierten Wandlern möglich. Dieser Beitrag präsentiert die letzten Forschungsergebnisse im Bezug auf thermoakustischen Wandlern, welche derzeit in einen thermoakustischen Gruppenstrahler münden. Gruppenstrahler erlauben die simultane Änderung des Einschallwinkels, sowie die Verschiebung des Fokuspunktes während der Verwendung. Durch die Verbindung beider Schlüsseltechnologien, der thermoakustischen Anregung und des Gruppenstrahlerprinzips, wird das Spektrum der klassischen ZfP-Anwendungen, sowie moderner Ansätze wie der Anregung von geführten Wellen oder der Strukturüberwachung erheblich erweitert und bereichert. Dabei soll innerhalb dieses Beitrages auf die Modellierung des Schallfeldes, die elementweise Charakterisierung und verschiedene Anwendungsszenarien eingegangen werden. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Luftgekoppelte Ultraschallprüfung KW - Thermoakustik KW - Ultraschallwandler KW - Phased Array PY - 2023 AN - OPUS4-57558 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufschläger, Daniel A1 - Gohlke, Dirk A1 - Weise, Matthias A1 - Bente, K. A1 - Gaal, Mate T1 - Thermoakustische Gruppenstrahler: Theorie und Anwendungen N2 - Bei der Prüfung von Werkstücken mit empfindlichen Oberflächen oder auch hydrophilen Werkstoffen sind traditionelle ultraschallbasierte zerstörungsfreie Prüfmethoden wie die Kontakttechnik oder die Tauchtechnik in vielen Anwendungsfällen aufgrund der Flüssigkeitsankopplung nicht anwendbar. Die luft-gekoppelte Ultraschallprüfung umgeht diese Problematik und eröffnet neue Prüfszenarien. Derzeit werden zwei Varianten der Schallerzeugung als vielversprechend angesehen: ferroelektrische Folien und thermoakustische Dünnschichtwandler. Thermoakustische Wandler ermöglichen die resonanzfreie Erzeugung von Ultraschall und somit kurze zeitliche Impulse sowie eine sehr breitbandige Anregung. Durch die Verwendung von gekrümmten Substraten ist sowohl eine Herstellung von planaren als auch fokussierten Wandlern möglich. Dieser Beitrag präsentiert die letzten Forschungsergebnisse im Bezug auf thermoakustischen Wandlern, welche derzeit in einen thermoakustischen Gruppenstrahler münden. Gruppenstrahler erlauben die simultane Änderung des Einschallwinkels, sowie die Verschiebung des Fokuspunktes während der Verwendung. Durch die Verbindung beider Schlüsseltechnologien, der thermoakustischen Anregung und des Gruppenstrahlerprinzips, wird das Spektrum der klassischen ZfP-Anwendungen, sowie moderner Ansätze wie der Anregung von geführten Wellen oder der Strukturüberwachung erheblich erweitert und bereichert. Dabei soll innerhalb dieses Beitrages auf die Modellierung des Schallfeldes, die elementweise Charakterisierung und verschiedene Anwendungsszenarien eingegangen werden. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Luftgekoppelte Ultraschallprüfung KW - Thermoakustik KW - Ultraschallwandler KW - Phased Array PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575599 SP - 1 EP - 6 AN - OPUS4-57559 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmitt, M. A1 - Casperson, Ralf A1 - Baensch, F. T1 - Ein Überblick über die Normung in der zerstörungsfreien Prüfung N2 - Normung und Standardisierung in der zerstörungsfreien Prüfung finden auf nationaler, europäischer und internationaler Ebene statt. Durch die Übernahme von Leitungsfunktionen in diesen Gremien kann ein deutlicher steuernder Einfluss auf Themen und Inhalte der Normen genommen werden. Unabdingbar für den Erfolg ist zusätzlich das persönliche Engagement der Fachexpert*innen in den nationalen Gremien und den europäischen und internationalen Arbeitsgruppen. Denn wer nicht normt wird genormt und muss letztlich Regeln verwenden, die andere entsprechend ihrer eigenen Interessen gestalten. Voraussetzung für die Teilnahme in europäischen und internationalen Normungsgremien ist die Mitwirkung in den entsprechenden nationalen Spiegelgremien der nationalen Normungsinstitute, welche die europäischen und internationalen Aktivitäten spiegeln und die Fachexperten für die Mitarbeit autorisieren. Gezeigt werden die relevante Gremienstruktur auf internationaler Ebene (ISO/TC 135 “Non-destructive testing”, ISO/TC 44/SC 5 “Testing and inspection of welds”), auf europäischer Ebene (CEN/TC 138 “Zerstörungsfreie Prüfverfahren”), die Struktur der nationalen deutschen Spiegelgremien, das Zusammenspiel der Gremien, und die Einflussmöglichkeiten. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Normung PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575759 UR - https://jahrestagung.dgzfp.de/Portals/jt2023/bb/P4.pdf VL - 2023 SP - 1 EP - 6 PB - DGZfP CY - Berlin AN - OPUS4-57575 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nerger, Tino T1 - Passive Smart Dust: A versatile low-cost sensor platform N2 - Beschichtete Zellulose Partikel als kolorimetrische passive Sensoren, die mittels optische Kamerasystem einer Drohne erfasst werden. Somit können Gefahrenstoffe, in ersten Versuchen z. B. Säuren aus sicherer Entfernung, kostengünstig und umweltverträglich detektiert werden. T2 - SMSI 2023 Sensor and Measurement Science International CY - Nuremberg, Germany DA - 08.05.2023 KW - Passive Smart Dust KW - Drone KW - Colorimetric sensor particles PY - 2023 AN - OPUS4-57526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nerger, Tino A1 - Neumann, Patrick P. A1 - Weller, Michael G. T1 - Passive Smart Dust a versatile low-cost sensor platform N2 - Coated cellulose particles as colourimetric passive sensors that are detected by the optical camera system of a drone. In this way, hazardous substances, e.g. acids, can be detected from a safe distance in a cost-effective and environmentally friendly way. N2 - Beschichtete Zellulose Partikel als kolorimetrische passive Sensoren, die mittels optische Kamerasystem einer Drohne erfasst werden. Somit können Gefahrenstoffe, in ersten Versuchen zB Säuren aus sicherer Entfernung, kostengünstig und umweltverträglich detektiert werden. T2 - SMSI 2023 Sensor and Measurement Science International CY - Nuremberg, Germany DA - 08.05.2023 KW - Passive Smart Dust KW - Drone KW - Colorimetric sensor particles KW - Remote detection PY - 2023 DO - https://doi.org/10.5162/SMSI2023/C5.3 SP - 1 EP - 2 AN - OPUS4-57527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat T1 - ɸgOTDR utilizing Geometric Phase for Earthquake Monitoring N2 - Geometric phase measured per beat period1 in a ɸ-OTDR based on coherent heterodyne detection2 is used to measure strain3, instead of the traditionally measured dynamic phase. The new setup is referred to as a ɸgOTDR. Results are verified using a piezo-electric transducer inline a fiber-undertest. T2 - European Workshop on Optical Fibre Sensors (EWOFS 2023) CY - Mons, Belgium DA - 23.05.2023 KW - Geometric Phase KW - Distributed Fiber Optic Sensor KW - Coherent Heterodyne PY - 2023 AN - OPUS4-57607 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Raysyan, Anna A1 - Zwigart, S. A1 - Eremin, S. A. A1 - Schneider, Rudolf T1 - BPA Endocrine Disruptor Detection at the Cutting Edge: FPIA and ELISA Immunoassays N2 - BPA is a chemical commonly used in the production of polymer-based materials that can have detrimental effects on the thyroid gland and impact human reproductive health. Various expensive methods, such as liquid and gas chromatography, have been suggested for detecting BPA. The fluorescence polarization immunoassay (FPIA) is an inexpensive and efficient homogeneous mix-and-read method that allows for high-throughput screening. FPIA offers high specificity and sensitivity and can be carried out in a single phase within a timeframe of 20–30 min. In this study, new tracer molecules were designed that linked the fluorescein fluorophore with and without a spacer to the bisphenol A moiety. To assess the influence of the C6 spacer on the sensitivity of an assay based on the respective antibody, hapten–protein conjugates were synthesized and assessed for performance in an ELISA setup, and this resulted in a highly sensitive assay with a detection limit of 0.05 µg/L. The lowest limit of detection was reached by employing the spacer derivate in the FPIA and was 1.0 µg/L, working range from 2 to 155 µg/L. The validation of the methods was conducted using actual samples compared to LC–MS/MS, which served as the reference method. The FPIA and ELISA both demonstrated satisfactory concordance. KW - Fluorescence Polarization KW - Enzyme-Linked Immunosorbent Assay KW - Endokriner Disruptor KW - Bisphenol A KW - Freisetzung PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579497 DO - https://doi.org/10.3390/bios13060664 VL - 13 IS - 6 SP - 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-57949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien T1 - Thermographic Detection of Internal Defects using Photothermal Super Resolution Reconstruction and 2D structured Illumination Patterns N2 - For a long time, the rule of thumb for active thermography as a non-destructive testing method was that the resolution of internal defects/inhomogeneities is limited to a ratio of defect depth/defect size ≤ 1. This is due to the diffusive nature of thermal conduction in solids. So-called super resolution approaches have recently allowed this physical limit to be overcome many times over. This offers the attractive possibility of developing thermography from a purely near surface-sensitive testing method to one with improved depth range. How far this development can be pushed is the subject of current research. We have already been able to show that this classical limitation for one- and two-dimensional defect geometries can be overcome by illuminating the test object sequentially in a structured manner with individual laser spots and thus subsequently calculating a defect map from the resulting measurement data by applying photothermal super resolution reconstruction, which allows significantly improved separation of individual closely spaced defects. As a result, this method benefits strongly from the combination of sequential spatially structured illumination and modern numerical optimization methods, which come at the expense of higher experimental complexity. This leads to long measurement times, large data sets, and tedious numerical analysis, in contrast to the application of established standard thermographic methods with homogeneous illumination. In this work, we report on the application of full-area spatially structured two-dimensional illumination patterns, which, by applying state-of-the-art laser projector technology in conjunction with a high-power laser, makes it possible to achieve an efficient implementation of photothermal super-resolution reconstruction even for larger test areas in the first place. T2 - 13th European Conference on Non-destructive Testing CY - Lisbon, Portugal DA - 03.07.2023 KW - Thermography KW - Super resolution KW - Digital light processing KW - Material testing KW - Internal defects KW - DMD PY - 2023 AN - OPUS4-57909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Given, Joseph T1 - An automatic system for categorizing and quantifying human factors N2 - Human factors (HF) are little understood, and particularly in non-destructive testing (NDT) experimental data is rare, samples are often small, and statistical methods are rarely used to evaluate results. HF have been widely implicated in major occurrences of technical failure, for example at North Anna Power Plant and on United Airlines Flight 232. Understanding HF is vital for reliable detection and prevention of failures. Reliability assessments, though known to be affected by intrinsic capability, application factors, and HF, have thus far only concentrated to a sufficient degree on intrinsic capability. The addition of HF to that assessment has proven difficult due to the lack of a method of quantifying HF. This paper presents the first attempt from a psychological perspective to quantify HF from qualitative data. HF data was derived from qualitative human-oriented Failure Modes and Effects Analysis (Human-FMEA) workshops for visual inspection of tunnels by laser scanning and for ultrasonic testing of welds. Data was collected on human failure modes, causes, consequences and preventive measures, as well as eliciting a risk priority number (RPN). Using this data, a system of quantitative weightings was created to allocate errors to inductively derived HF categories for further allocation to existing HF categorisation models. This weighting model proved useful for creating quantitative summaries of HF, informing and validating qualitative FMEA results, and comparing existing HF categorisation models. Further potential lies within a planned interface to quantitative reliability assessment methods such as POD (Probability of Detection). While providing quantifications, the method retains a qualitative and holistic nature, can, thus, bridge the gap between psychological and engineering concerns of HF and reliability, contributing to future interdisciplinary work. T2 - SPIE Smart Structures + Nondestructive Evaluation, 2023 CY - Long Beach, CA, USA DA - 12.03.2023 KW - Quantification KW - Human-FMEA KW - Human Factors PY - 2023 DO - https://doi.org/10.1117/12.2658407 SN - 0277-786X VL - 12491 SP - 1 EP - 15 PB - SPIE (The International Society for Optical Engineering) CY - Bellingham, Wash. AN - OPUS4-57928 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN T1 - Forschungsprogramm 2009 - 2010 N2 - In den Zeiten der Globalisierung und der beschleunigten technologischen Entwicklungen lassen sich in den Industrieländern nur mit einer entsprechenden Innovationsdynamik und -dichte die Herausforderungen im Hinblick auf Wachstum, Beschäftigung und Strukturwandel erfüllen. Grundvoraussetzung hierfür ist eine leistungsfähige Forschung. Um die Forschungsinfrastruktur in der Bundesrepublik zu erhalten und global wettbewerbsfähig zu bleiben, sind verstärkte Investitionen des Staates und der Wirtschaft notwendig. Mit den Investitionen im Rahmen der Hightech-Strategie hat die Bundesregierung einen wichtigen Schritt zur Förderung des wissenschaftlich-technischen Fortschritts in Deutschland getan. Die Investitionen in die Forschungsinfrastruktur des Landes sind nun von den Forschungseinrichtungen und Universitäten effektiv und effizient zu nutzen. Für einen möglichst wirksamen Einsatz der Forschungsetats sind Forschungsprogramme sowohl für die Forschungseinrichtung als auch für die Mittelgeber ein wichtiges Instrument im Hinblick auf die Darstellung der Aktivitäten. Dies gilt insbesondere für die Ressortforschungseinrichtungen des Bundes, zu denen die Bundesanstalt für Materialforschung und -prüfung (BAM) zählt. Diese Einrichtungen verfügen über einen klaren Auftrag und ihre Forschung ist mit der Wahrnehmung öffentlicher Aufgaben verbunden. Forschungsprogramme dienen daher besonders in diesen Einrichtungen dazu, Perspektiven im Bereich ihres Aufgabenfeldes sowie ihre Forschungsaktivitäten transparent darzustellen und politisch vertretbar zu machen. Das vorliegende Forschungsprogramm der BAM gibt einen Überblick über die in den nächsten Jahren aktuellen Forschungsthemen und die hierfür erforderlichen Ressourcen und Rahmenbedingungen. PY - 2009 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578814 SP - 1 EP - 38 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-57881 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nowatzky, Yannek A1 - Benner, Philipp A1 - Reinert, K. A1 - Muth, Thilo T1 - Mistle: bringing spectral library predictions to metaproteomics with an efficient search index N2 - Motivation: Deep learning has moved to the forefront of tandem mass spectrometry-driven proteomics and authentic prediction for peptide fragmentation is more feasible than ever. Still, at this point spectral prediction is mainly used to validate database search results or for confined search spaces. Fully predicted spectral libraries have not yet been efficiently adapted to large search space problems that often occur in metaproteomics or proteogenomics. Results: In this study, we showcase a workflow that uses Prosit for spectral library predictions on two common metaproteomes and implement an indexing and search algorithm, Mistle, to efficiently identify experimental mass spectra within the library. Hence, the workflow emulates a classic protein sequence database search with protein digestion but builds a searchable index from spectral predictions as an in-between step. We compare Mistle to popular search engines, both on a spectral and database search level, and provide evidence that this approach is more accurate than a database search using MSFragger. Mistle outperforms other spectral library search engines in terms of run time and proves to be extremely memory efficient with a 4- to 22-fold decrease in RAM usage. This makes Mistle universally applicable to large search spaces, e.g. covering comprehensive sequence databases of diverse microbiomes. Availability and implementation: Mistle is freely available on GitHub at https://github.com/BAMeScience/Mistle. KW - Mass spectrometry KW - Proteomics KW - Algorithms KW - Metaproteomics PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579373 DO - https://doi.org/10.1093/bioinformatics/btad376 SN - 1367-4811 VL - 39 IS - 6 SP - 1 EP - 12 PB - Oxford University Press CY - Oxford, Great Britain AN - OPUS4-57937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zweigle, J. A1 - Capitain, C. A1 - Simon, Fabian Michael A1 - Roesch, Philipp A1 - Bugsel, B. A1 - Zwiener, C. T1 - Non-extractable PFAS in functional textiles − Characterization by complementary methods: oxidation, hydrolysis, and fluorine sum parameters N2 - Per- and polyfluoroalkyl substances (PFAS) are widely used for durable water-repellent finishing of different fabrics and textiles like outdoor clothing, carpets, medical textiles and more. Existing PFAS extraction techniques followed by target analysis are often insufficient in detecting widely used side-chain fluorinated polymers (SFPs) that are barely or non-extractable. SFPs are typically copolymers consisting of a non-fluorinated backbone with perfluoroalkyl side-chains to obtain desired properties. We compared the accessible analytical information and performance of complementary techniques based on oxidation (dTOP assay, PhotoTOP), hydrolysis (THP assay), standard extraction, extractable organic fluorine (EOF), and total fluorine (TF) with five functional textiles and characterized 7 further textiles only by PhotoTOP oxidation. The results show that when applied directly to textile samples, oxidation by dTOP and PhotoTOP and also hydrolysis by the THP are able to capture large fractions of the TF in form of perfluoroalkyl side-chains present in the textiles while methods relying on extracts (EOF, target and non-target analysis) were much lower (e.g., factor ~25-50 lower). The conversion of large fractions of the measured TF into PFCAs or FTOHs from fluorinated side chains is in contrast to previous studies. Concentrations ranged from 2/ZnS Quantum Dots and Molecular Photosensitizers N2 - Antibacterial photodynamic therapy (a‐PDT) has emerged as a promising non‐invasive therapeutic modality that utilizes the combination of a photosensitive agent, molecular oxygen, and excitation light to generate reactive oxygen species (ROS), demonstrating remarkable activity against multidrug‐resistant bacterial infections. However, the effective use of conventional photosensitizers is significantly limited by a number of their shortcomings, namely, poor water solubility and low selectivity. Herein, we present a novel biocompatible water‐soluble nanocomposite based on hydrophobic tetraphenylporphyrin (TPP) molecules and hydrophilic ternary AgInS2/ZnS quantum dots incorporated into a chitosan matrix as an improved photosensitizer for a‐PDT. We demonstrated that TPP molecules could be successfully transferred into chitosan solution while remaining primarily in the form of monomers, which are capable of singlet oxygen generation. We performed a detailed analysis of the Förster resonance energy transfer (FRET) between quantum dots and TPP molecules within the nanocomposite and proposed the mechanism of the singlet oxygen efficiency enhancement via FRET. KW - Nano KW - Particle KW - Quantum dot KW - Fluorescence KW - Synthesis KW - Optical spectroscopy KW - Energy transfer KW - Quality assurance KW - Lifetime KW - Quantum yield PY - 2024 DO - https://doi.org/10.1002/cnma.202300469 SN - 2199-692X VL - 10 IS - 3 SP - 1 EP - 11 PB - Wiley AN - OPUS4-59728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raab, A. A1 - Solovyev, N. A1 - El-Kathib, Ahmed A1 - Vogl, Jochen A1 - Costas-Rodriguez, M. T1 - Isotope signature of iron, copper and zinc in mouse models (L66 and 5XFAD) and their controls used for dementia research N2 - Introduction: The influence of copper, iron and zinc concentrations on the formation of ß-amyloid plaques and neurofibrillary tangles in Alzheimer’s disease (AD) is widely discussed in the community. The results from human and animal studies so far are mixed with some studies showing a correlation and others not. From a number of studies, it is known that disease state and isotopic composition of essential elements can be coupled. Aim: The aim of the study was to identify changes in element content and isotopic composition in two transgenic mouse models used in AD research compared to their genetic WT relatives and to establish whether element content and isotopic signature between different laboratories is comparable. Methods: ß-amyloid (5xFAD) and tau overexpressing (L66) mice together with their matching wild-types were bred at dedicated facilities in accordance with the European Communities Council Directive (63/2010/EU). Serum and brain were sampled after sacrifice and the samples distributed among the participants of the study. The tissues were acid digested for total element determination and high-precision isotope ratio determination. Element content was determined by either sector-field or quadrupole-based inductively coupled plasma mass spectrometry (ICPMS). For the determination of isotope ratios multi-collector ICPMS was used. Results: Total copper content was significantly higher for L66 and their matched WT compared to 5xFAD and WT. Brains of L66 mice contained more Fe in brain than their WT, Zn and Cu were not significantly different between L66 and WT. Whereas 5xFAD mice had a slightly lower Cu and slightly higher Zn concentration in brain compared to WT. The isotopic signature in brain of L66 mice for Fe was different from their controls, whereas Zn isotope ratios were influenced in 5xFAD mice compared to their WT . The Cu isotopic ratio did not seem to be influenced in either strain. In serum, the shifts were less pronounced. Conclusion: Even though neither Tau-protein nor amyloid precursor protein are known to be metal-dependent / -containing proteins, the overexpression of both influences the Fe, Cu and Zn metabolism in brain and to some extent also in serum as can be seen not only using total element determination but probably more clearly studying the isotopic signature of Fe, Cu and Zn. T2 - International Conference of Trace Elements and Minerals CY - Aachen, Germany DA - 05.06.2022 KW - Isotope delta value KW - Copper KW - Zinc KW - Iron KW - Dementia PY - 2022 AN - OPUS4-58230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Everything SAXS Part 1: Introduction, Sample Requirements and Measurement "Space" N2 - This talk for the Swiss Society for Crystallography (SSCr) workshop on SAXS will introduce scattering from various angles, focusing in particular on: - Information content of X-ray scattering experiments, three entry points… - An introduction to Fourier Transforms - Sample criteria, compatibility, and selection - Key indicators of a measurement – where is the information? - Key indicators of measurement quality - Experiment planning, the basics T2 - Topical workshop of the Swiss Society for Crystallography CY - Zurich, Switzerland DA - 08.09.2023 KW - X-ray scattering KW - Data stewardship KW - Measurement science KW - MOUSE KW - Holistic experiment approaches PY - 2023 AN - OPUS4-58235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Everything SAXS Part 2: Data Processing, Workflow and Pitfalls N2 - The second talk for the Swiss Society for Crystallography (SSCr) workshop on SAXS will highlight the data processing challenges, holistic experimental workflow developments, and the pitfalls. In particular, the following items will be addressed: - The importance of data processing and estimating uncertainty - A universal correction pipeline – away with the headaches, at least for this step! - Experiment planning part 2, some tips and advice to improve your corrected data. - Sample preparation, background selection, some tips and advice to improve your corrected data. - Automate for your mental well-being; electronic logbooks, measurement catalogs and workflow management software - Life on the edge: several pitfalls to avoid… T2 - Topical workshop of the Swiss Society for Crystallography CY - Zurich, Switzerland DA - 08.09.2023 KW - X-ray scattering KW - MOUSE KW - Data processing KW - Uncertainties KW - Pitfalls PY - 2023 AN - OPUS4-58236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - 3D X-ray Imaging and residual stress analysis of materials N2 - The focus of the presentation focus will be on 3D imaging by means of X-ray Computed Tomography (XCT) at the lab and at synchrotron, and the non-destructive residual stress (RS) characterization by diffraction of different kind of materials in FB8.5 Micro-NDT BAM. For instance, the manufacturing defects and high RS are inherent of additively manufacturing techniques and affect structural integrity of the components. Using XCT the defects size and shape distribution as well as geometrical deviations can be characterized, allowing the further optimization of the manufacturing process. Diffraction-based RS analysis methods using neutron and synchrotron X-rays at large scale facilities offer the possibility to non-destructively spatially resolve both surface and bulk RS in complex components and track their changes following applied thermal or mechanical loads. T2 - Seminar at Applied Materials Group at PSI CY - Villigen, Switzerland DA - 13.09.2023 KW - Additive manufacturing KW - Residual stress KW - X-ray computed tomography PY - 2023 AN - OPUS4-58310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hantschke, Luisa Lamberta T1 - Comparison of three different TOP-Assay approaches for the determination of PFAS concentration in soil N2 - Per- and polyfluoroalkyl substances (PFAS) are a large, ever-growing and widely used class of chemicals. Due to the strength of the C-F bond, they do not decompose but accumulate in the environment posing a risk for nature and humans alike. While the use of some PFAS, like perfluorooctanoic acid (PFOA) is already regulated in the EU, new ‘precursor’ substances are used to replace them. However, these precursors may be equally harmful to the environment. In recent years, many ‘hot spot’ sites with high PFAS contaminations in soil have been distinguished, but no German-wide background values have been determined yet. Knowing these background values is crucial to understand the degree of PFAS contamination, underpinning future regulatory decisions. Due to the complexity and variety of different PFAS compounds, one needs to apply a broad spectrum of different techniques to capture most of the PFAS content in one sample. In the framework of this project, 600 soil samples are taken at different sites all over Germany. The concentration of 30 PFAS - 13 carboxylic acids (C4-C18), 5 sulfonic acids (C4-C10) and 12 precursor substances) - is determined in these soil samples using three different sample preparation approaches: 1) ultrasonic extraction of the soil samples with Methanol; 2) preparation of eluates to test the leaching behaviour of the PFAS and 3) TOP assays following the method published by Houtz & Sedlak. Targeted LC-MS/MS is used to determine PFAS concentration after all three preparation steps. For the TOP-assay, the concentration of all 30 PFAS is compared prior to and after the oxidation reaction. Besides the ‘classic’ TOP-Assay, two other TOP-Assay approaches, the dTOP Assay and the photoTOP-Assay, are tested and the results of all three approaches are compared. First, all three TOP-Assay approaches will be tested on a reference soil spiked with a solution including all 30 PFAS measured in the project. Later, soil samples taken in the frame of the priorly described project will be tested. This poster will focus on the results of the experiments comparing the three different TOP Assay approaches in spiked reference soil. Additionally, some of the results of the other sample preparation methods, extraction and eluate preparation will be presented. T2 - FLUOROS 2023 CY - Idstein, Germany DA - 31.08.2023 KW - PFAS TOP Assay soil contamination PY - 2023 AN - OPUS4-58267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Reliability reassessment of bridges with geometrical NDT results N2 - This presentation summarizes recent developments within the scope of the national pre-standardization project “ZfPStatik”, which aims to prepare a guideline about NDT-supported structural analyses. The focus is on the purposeful and explicit utilization of geometrical tendon and reinforcement bar positions measured on-site in reliability analysis — shown by means of a prestressed concrete bridge as case study. T2 - 13th German Japanese Bridge Symposium CY - Osaka, Japan DA - 28.08.2023 KW - Existing structures KW - Probabilistic methods KW - Data-supported assessment PY - 2023 AN - OPUS4-58268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan A1 - Kainz, C. A1 - Braml, T. T1 - Reliability assessment of existing concrete bridges with geometrical NDT results - Case studies N2 - The results of and the validity in reliability assessment of existing bridges essentially depend on the information available about the considered system. Information about the actual condition as well as structural and material characteristics can be observed on-site to refine the computation models used in assessment. Non-destructive testing (NDT) methods for concrete structures are capable of reconstructing missing, questioned, or inconsistent as-built plans. This contribution summarizes recent developments within the scope of the national pre-standardization project “ZfPStatik”, which aims to prepare a guideline about NDT-supported structural analyses. The focus is on the purposeful and explicit utilization of geometrical tendon and reinforcement bar positions (measured on-site using the ultrasound echo and ground penetrating radar (GPR) techniques) in probabilistic reliability analyses — shown by means of real case studies. The well-established first order reliability method is applied to different concrete bridges, which are typical for the German road bridge stock, to demonstrate the utility of incorporating quality-evaluated NDT-results in terms of changes in structural reliability. T2 - 13th German-Japanese Bridge Symposium CY - Osaka, Japan DA - 28.08.2023 KW - Non-destructive testing KW - Prestressed concrete KW - Data-informed reliability analysis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582727 SP - 29 EP - 40 PB - Osaka Metropolitan University CY - Osaka AN - OPUS4-58272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Birkholz, H. A1 - Bayerlein, Bernd T1 - PMD Core Ontology: A Community Driven Mid-Level Ontology in the MSE Domain N2 - Knowledge representation in the materials science and engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant and variant knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific. In this presentation, an approach how to maintain a comprehensive and intuitive MSE-centric terminology composing a mid-level ontology–the PMD core ontology (PMDco)–via MSE community-based curation procedures is shown. The PMDco is designed in direct support of the FAIR principles to address immediate needs of the global experts community and their requirements. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics, how the PMDco lowers development and integration thresholds, and how to fuel it from real-world data sources ranging from manually conducted experiments and simulations as well as continuously automated industrial applications. T2 - FEMS EUROMAT 2023 CY - Frankfurt a. M., Germany DA - 03.09.2023 KW - Knowledge Representation KW - Semantic Interioerability KW - Mid-Level Ontology for MSE KW - FAIR Data Management PY - 2023 AN - OPUS4-58201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Alexander T1 - Simulation of Eddy Current Rail Testing Data for Neural Networks N2 - The present work is part of the AIFRI project (Artificial Intelligence For Rail Inspection), where we and our project partners train a neural network for defect detection and classification. Our goal at BAM is to generate artificial ultrasound and eddy current training data for the A.I. This paper has an exploratory nature, where we focus on the simulation of eddy current signals for head check cracks, one of the most important rail surface defects. The goal of this paper is twofold. On the one hand, we present our general simulation setup. This includes geometric models for head check cracks with features like branching and direction change, a model for the HC10 rail testing probe, and the configuration of the Faraday simulation software. On the other hand, we use the Faraday software to simulate eddy current testing signals with a strong focus on the influence of the damage depth on the signal, while differentiating between different crack geometries. Here, we observe an early saturation effect of the test signal at a damage depth of 2 mm (at a crack angle of 25◦ to the surface). That is about 2 mm earlier than we would expect from measurements at a crack angle of 90◦. This behavior will be investigated further in a future paper. Finally, we interpolate the simulated signals in a two-step curve fitting process. With these interpolations we may generate eddy current test signals for any damage depth within the simulated range. T2 - 13th European Conference on Non-Destructive Testing 2023 CY - Lisbon, Portugal KW - Artificial Intelligence KW - Simulation KW - Eddy Current PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581918 DO - https://doi.org/10.58286/28179 SN - 1435-4934 VL - 28 IS - 8 SP - 1 EP - 6 PB - NDT.net CY - Kirchwald AN - OPUS4-58191 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Friedrich, Alexander T1 - Simulation of Eddy Current Rail Testing Data for Neural Networks N2 - The present work is part of the AIFRI project (Artificial Intelligence For Rail Inspection), where we and our project partners train a neural network for defect detection and classification. Our goal at BAM is to generate artificial ultrasound and eddy current training data for the A.I. This paper has an exploratory nature, where we focus on the simulation of eddy current signals for head check cracks, one of the most important rail surface defects. The goal of this paper is twofold. On the one hand, we present our general simulation setup. This includes geometric models for head check cracks with features like branching and direction change, a model for the HC10 rail testing probe, and the configuration of the Faraday simulation software. On the other hand, we use the Faraday software to simulate eddy current testing signals with a strong focus on the influence of the damage depth on the signal, while differentiating between different crack geometries. Here, we observe an early saturation effect of the test signal at a damage depth of 2 mm (at a crack angle of 25◦ to the surface). That is about 2 mm earlier than we would expect from measurements at a crack angle of 90◦. This behavior will be investigated further in a future paper. Finally, we interpolate the simulated signals in a two-step curve fitting process. With these interpolations we may generate eddy current test signals for any damage depth within the simulated range. T2 - 13th European Conference on Non-Destructive Testing 2023 CY - Lisbon, Portugal DA - 03.07.2023 KW - Simulation KW - Eddy Current KW - Artificial Intelligence PY - 2023 AN - OPUS4-58192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - PMDco - Platform MaterialDigital Core Ontology N2 - The PMD Core Ontology (PMDco) is a comprehensive set of building blocks produced via consensus building. The ontological building blocks provide a framework representing knowledge about fundamental concepts used in Materials Science and Engineering (MSE) today. The PMDco is a mid-level ontology that establishes connections between narrower MSE application ontologies and domain neutral concepts used in already established broader (top-level) ontologies. The primary goal of the PMDco design is to enable interoperability between various other MSE-related ontologies and other common ontologies. PMDco’s class structure is both comprehensive and extensible, rendering it an efficient tool to structure MSE knowledge. The PMDco serves as a semantic middle-layer unifying common MSE concepts via semantic mapping to other semantic representations using well-known key terms used in the MSE domain. The PMDco enables straight-forward documentation and tracking of science data generation and in consequence enables high-quality FAIR data that allows for precise reproducibility of scientific experiments. The design of PMDco is based on the W3C Provenance Ontology (PROV-O), which provides a standard framework for capturing the production, derivation, and attribution of resources. Via this foundation, the PMDco enables the integration of data from various data origins and the representation of complex workflows. In summary, the PMDco is a valuable advancement for researchers and practitioners in MSE domains. It provides a common MSE vocabulary to represent and share knowledge, allowing for efficient collaboration and promoting interoperability between diverse domains. Its design allows for the systematic integration of data and metadata, enabling seamless tracing of science data. Overall, the PMDco is a crucial step towards a unified and comprehensive understanding of the MSE domain in general. T2 - FEMS EUROMAT 2023 CY - Frankfurt a. M., Germany DA - 03.09.2023 KW - Knowledge Representation KW - Ontology KW - Semantic Interoperability KW - FAIR KW - Automation PY - 2023 AN - OPUS4-58197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - Reveal the unknown: Interfacing non-target and elemental speciation analysis N2 - The combination of non-target analysis (NTA) based on HPLC-ESI-MS with elemental fluorine speciation analysis based on HPLC-PARCI-MS for the identification and quantification of (unknown) organofluorines in environmental samples is associated with several advantages e.g., reduced non-target data treatment workflow and quantification. PFASs compromise persistent, bioaccumulative, and toxic properties and are hence, environmental contaminants of emerging concern. Thus, procedures for identifying potential sources of the entrance of these compounds into the environment, identification of new organofluorine species, and closing mass balances need urgent development. The intrinsic fluorine tag appears in a sizable fraction of these and other xenobiotics, making elemental speciation desirable for quantitative NTA in these areas. Current non-target approaches based on ESI-HRMS suffer from a lack of data mining algorithms for identification of PFASs with low fluorine mass percentages. Furthermore, low ionization efficiencies of the compounds hamper detection limits. Hence, the proposed combination of simultaneous HPLC-ESI-MS and HPLC-PARCI-MS via split-stream coupling is a promising approach for environmental PFAS monitoring. Furthermore, it could serve as an important analytical procedure to set up limiting values in compliance with the desired PFAS ban of the European Union. T2 - SALSA Make and Measure 2023: Interfaces CY - Berlin, Germany DA - 13.09.2023 KW - PFAS KW - HRMS KW - PARCI-MS KW - ESI-MS PY - 2023 AN - OPUS4-58405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - Breaking the Wall of Environmental Pollutants N2 - With the continuous release of anthropogenic pollutants into the environment, substantial risks for the human health arise. Concerning are especially persistent substances (e.g., PFAS) as they accumulate in food chains which inevitably result in the transgression of negative impact threshold levels. Environmental Analytical Chemsitry interfaces all disciplines of Risk Assessment. Therefore it is the important tool to identify, monitor, and remediate environmental pollutants. Based on the example of PFAS, a workflow to tackle environmental pollutants in a retro- and pro-spective way is shown. Within the project, the worldwide situation of environmental pollutants will be illustrated for the example of PFAS. As the major discipline to confront the problem, analytical chemistry will be shown as a key tool for contesting PFAS and creating safe-by-design materials in the future. T2 - Falling Walls Lab 2023 CY - Berlin, Germany DA - 21.09.2023 KW - PFAS KW - Analytical Chemistry KW - Environmental pollutants KW - Risk assessment PY - 2023 AN - OPUS4-58406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Retzmann, Anika A1 - Faßbender, Sebastian A1 - Rosner, M. A1 - von der Au, Marcus A1 - Vogl, Jochen T1 - Performance of second generation ICP-TOFMS for (multi-)isotope ratio analysis: a case study on B, Sr and Pb and their isotope fractionation behavior during the measurements N2 - The performance of second generation ICP-TOFMS, equipped with a micro-channel plate (MCP) enabling multi-isotope detection, in terms of isotope ratio precision and instrumental isotopic fractionation (IIF) for (multi-)isotope ratio analysis was thoroughly assessed for B, Sr and Pb. Experimental isotope ratio precision of 0.14 % for 11B/10B intensity ratio, 0.15 % for 87Sr/86Sr intensity ratio and 0.07% for 208Pb/206Pb intensity ratio were obtained at high signal levels ($500 mg L−1) which is comparable to first generation ICP-TOFMS. The long-term stability of isotope ratios, measured over several hours and expressed as repeatability, is between 0.05 % and 1.8 % for B, Sr and Pb. The observed IIF per mass unit is negative for B (i.e., −11 % for 11B/10B) which is in accordance with measurements using sector field (MC) ICP-MS. But the observed IIF per mass unit is positive for Sr (i.e., 2 % for 87Sr/86Sr) and Pb (i.e., 4.5 % for 208Pb/206Pb) which is not in accordance with measurements using sector field (MC) ICP-MS. Furthermore, different IIFs per mass unit were observed for different isotope pairs of the same isotopic system (i.e., Sr, Pb) and adjacent isotopic systems (i.e., Pb vs. Tl). This and the observations from three-isotope plots for Sr and Pb show that ion formation, ion extraction, ion transmission, ion separation and ion detection in second generation ICP-TOFMS is subject to IIF that does not follow the known mass dependent fractionation laws and is possibly caused by mass independent fractionation and/or multiple (contradictory) fractionation processes with varying contributions. The non-mass dependent IIF behavior observed for second generation ICP TOFMS has profound consequences for the IIF correction of isotope raw data, including application of multi-isotope dilution mass spectrometry (IDMS) using ICP-TOFMS. Hence, only IIF correction models that correct also for mass independent fractionation are applicable to calculate reliable isotope ratios using second generation ICP-TOFMS. In the present study, reliable d11B values, and absolute B, Sr and Pb isotope ratios could be determined using the SSB approach in single-element solutions as well as in a mixture of B, Sr and Pb, where the isotopes were measured simultaneously. KW - ICP-TOFMS KW - Isotope delta value KW - Isotope amount ratio KW - Conventional isotope ratio KW - Instrumental isotope fractionation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582239 DO - https://doi.org/10.1039/d3ja00084b SN - 0267-9477 VL - 38 IS - 10 SP - 2144 EP - 2158 PB - Royal Society of Chemistry AN - OPUS4-58223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Riedel, Soraya T1 - Development of electrochemical antibody-based and enzymatic assays for mycotoxin analysis in food N2 - Electrochemical methods are promising to meet the demand for easy-to-use devices monitoring key parameters in the food industry. Many companies run own lab procedures for mycotoxin analysis, but it is a major goal to simplify the analysis. The enzyme-linked immunosorbent assay using horseradish peroxidase as enzymatic label, together with 3,3',5,5' tetramethylbenzidine (TMB)/H2O2 as substrates allows sensitive mycotoxin detection with optical detection methods. For the miniaturization of the detection step, an electrochemical system for mycotoxin analysis was developed. To this end, the electrochemical detection of TMB was studied by cyclic voltammetry on different screen-printed electrodes (carbon and gold) and at different pH values (pH 1 and pH 4). A stable electrode reaction, which is the basis for the further construction of the electrochemical detection system, could be achieved at pH 1 on gold electrodes. An amperometric detection method for oxidized TMB, using a custom-made flow cell for screen-printed electrodes, was established and applied for a competitive magnetic bead-based immunoassay for the mycotoxin ochratoxin A. A limit of detection of 150 pM (60 ng/L) could be obtained and the results were verified with optical detection. The applicability of the magnetic bead-based immunoassay was tested in spiked beer using a handheld potentiostat connected via Bluetooth to a smartphone for amperometric detection allowing to quantify ochratoxin A down to 1.2 nM (0.5 µg/L). Based on the developed electrochemical detection system for TMB, the applicability of the approach was demonstrated with a magnetic bead-based immunoassay for the ergot alkaloid, ergometrine. Under optimized assay conditions a limit of detection of 3 nM (1 µg/L) was achieved and in spiked rye flour samples ergometrine levels in a range from 25 to 250 µg/kg could be quantified. All results were verified with optical detection. The developed electrochemical detection method for TMB gives great promise for the detection of TMB in many other HRP-based assays. A new sensing approach, based on an enzymatic electrochemical detection system for the mycotoxin fumonisin B1 was established using an Aspergillus niger fumonisin amine oxidase (AnFAO). AnFAO was produced recombinantly in E. coli as maltose-binding protein fusion protein and catalyzes the oxidative deamination of fumonisins, producing hydrogen peroxide. It was found that AnFAO has a high storage and temperature stability. The enzyme was coupled covalently to magnetic particles, and the enzymatically produced H2O2 in the reaction with fumonisin B1 was detected amperometrically in a flow injection system using Prussian blue/carbon electrodes and the custom-made wall-jet flow cell. Fumonisin B1 could be quantified down to 1.5 µM (≈ 1 mg/L). The developed system represents a new approach to detect mycotoxins using enzymes and electrochemical methods. N2 - Zur Entwicklung von einfach zu bedienenden Vor-Ort-Geräten, welche für die Analytik von wichtigen Parametern in der Lebensmittelindustrie eingesetzt werden können, sind elektrochemische Methoden besonders vielversprechend. Viele Unternehmen führen bereits Mykotoxinanalytik in eigenen Laboren am Produktionsstandort durch, dennoch gibt es große Bestrebungen Analysenmethoden weiter zu vereinfachen. Der Enzyme-linked Immunosorbent Assay (ELISA), welcher häufig mit der Meerrettichperoxidase als enzymatischem Label und 3,3',5,5'-Tetramethylbenzidine (TMB)/H2O2 als Enzymsubstraten arbeitet, ermöglicht den sensitiven Mykotoxinnachweis mithilfe optischer Detektionsmethoden. Zur Miniaturisierung des Detektionsschrittes wurde in dieser Arbeit der Aufbau von elektrochemischen Detektionssystemen für die Mykotoxinanalytik untersucht. Dazu wurde zunächst die elektrochemische Reaktion von TMB an verschiedenen Materialien siebgedruckter Elektroden (Kohlenstoff und Gold) sowie bei verschiedenen pH-Werten (pH 1 und pH 4) untersucht. Eine stabile Elektrodenreaktion, welche die Grundlage für den weiteren Aufbau des elektrochemischen Detektionssystems darstellt, konnte bei pH 1 an Goldelektroden erzielt werden. Basierend darauf wurde eine amperometrische Detektionsmethode für oxidiertes TMB entwickelt, wofür eine maßgefertigte Durchflusszelle verwendet wurde. Die amperometrische TMB-Detektion wurde für einen kompetitiven Magnetpartikel-basierten Immunoassay für Ochratoxin A eingesetzt. Mit diesem Assay wurde eine Nachweisgrenze von 150 pM (60 ng L-1) erreicht und die Ergebnisse konnten durch optische Detektion verifiziert werden. Die Anwendbarkeit des Assays konnte in Ochratoxin A dotiertem Bier demonstriert werden, wobei für die Detektion ein tragbarer Potentiostat verwendet wurde, welcher über Bluetooth mit einem Smartphone verbunden war. Hiermit konnten niedrige Ochratoxin A Konzentration von bis zu 1.2 nM (0.5 µg L-1) bestimmt werden. Aufbauend auf dem entwickelten elektrochemischen Detektionssystem für TMB wurde die Anwendbarkeit des Ansatzes auf einen Magnetpartikel-basierten Immunoassay für das Ergotalkaloid Ergometrine, evaluiert. Unter optimierten Bedingungen konnte mit dem Assay eine Nachweisgrenze von 3 nM (1 µg L-1) erreicht werden. In mit Ergometrin versetztem Roggenmehl konnten Konzentrationen von 25 bis 250 µg kg-1 nachgewiesen werden. Die entwickelte elektrochemische Nachweismethode für TMB bietet einen vielversprechenden Ansatz für den Einsatz in vielen anderen Meerrettichperoxidase-basierten Assays. Für das Mykotoxin Fumonisin B1, wurde ein neues sensorisches System entwickelt, welches auf einem enzymatischen elektrochemischen Nachweis basiert. Hierfür wurde eine Aspergillus niger Fumonisin Aminoxidase (AnFAO) rekombinant als Fusionsprotein mit dem Maltose-bindenden Protein exprimiert. AnFAO katalysiert die oxidative Deaminierung von Fumonisinen, wobei H2O2 gebildet wird. Es konnte gezeigt werden, dass AnFAO eine hohe Lagerungs- und Temperaturstabilität hat. Für den Nachweis von Fumonisin B1 wurde das Enzym kovalent an Magnetpartikel gekoppelt. Das enzymatisch produzierte H2O2 konnte anschließend amperometrisch mithilfe von Preußisch Blau/Kohlenstoff-Elektroden in der maßgefertigten Durchflusszelle detektiert werden. Fumonisin B1 konnte bis zu einer Konzentration von 1,5 µM (≈ 1 mg L-1) quantifiziert werden. Das entwickelte System stellt einen neuen Ansatz dar, um Mykotoxine unter Nutzung von Enzymen und elektrochemischen Methoden zu detektieren. KW - Mycotoxins KW - Biosensor KW - Antibodies KW - Electrochemical detection PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:517-opus4-607477 DO - https://doi.org/10.25932/publishup-60747 SP - 1 EP - 96 PB - Universität Potsdam CY - Potsdam AN - OPUS4-59189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Ecke, Alexander T1 - Integrated Diagnostics of Pharmaceutical Contaminants in Water Supply and Management Systems N2 - The contamination of drinking water with pharmaceuticals represents a severe health risk. In order to monitor the drinking water quality continuously and enable quick countermeasures in case of contamination, novel sensors are required. Here, immunoanalytical methods based on the binding of the analyte to highly selective antibodies can be helpful. In this work, magnetic bead-based immunoassays (MBBAs) have been developed for the detection of two relevant contaminants of drinking water: diclofenac (DCF) and amoxicillin (AMX). In case of the latter, not only the parent drug is of interest in the risk assessment but also its hydrolysis products (HPs). In a comprehensive study, the influence of external factors and intrinsic properties of the water on the rate of hydrolysis was investigated. As the hydrolysis of AMX further impacts the recognition by the antibody, a strategy to analyze samples with unknown hydrolysis degree of AMX was established employing the enzyme β-lactamase in sample preparation. For both analytes, the MBBAs enable the fast quantification with results obtained in less than one hour which represents a major improvement over conventional immunoassays like the enzyme-linked immunosorbent assay (ELISA). Compared to the respective ELISAs with the same antibodies, the MBBAs further exhibit improved analytical parameters such as a broader measurement range and lower limits of detection. Due to the magnetic properties of the beads that serve as a platform for the assays, they are suitable for the mobile and automated detection at the point-of-care. An integrated diagnostic system was designed in which electrochemical detection with chronoamperometry on a microfluidic chip allows for further miniaturization of the system to enable monitoring of the drinking water quality online in water supply pipes at waterworks. N2 - Die Kontamination von Trinkwasser mit Arzneimitteln stellt eine ernste Gesundheitsgefahr dar. Um die Trinkwasserqualität kontinuierlich überwachen und im Falle einer Verunreinigung zeitnah reagieren zu können, sind neuartige Sensoren erforderlich. Hier können immunanalytische Methoden, die auf der Bindung des Analyten an hochselektive Antikörper beruhen, hilfreich sein. In dieser Arbeit wurden magnetpartikelbasierte Immunoassays (MBBAs) für zwei relevante Kontaminanten des Trinkwassers entwickelt: Diclofenac (DCF) und Amoxicillin (AMX). Bei letzterem erwiesen sich neben der Ausgangsverbindung auch dessen Hydrolyseprodukte (HPs) als relevant für die Gefährdungsbeurteilung. In einer umfassenden Studie wurde der Einfluss von externen Faktoren und intrinsischen Eigenschaften des Wassers auf die Hydrolysegeschwindigkeit untersucht. Da die Hydrolyse von AMX auch die Erkennung durch den Antikörper beeinflusst, wurde eine Strategie zur Analyse von Proben mit unbekanntem Hydrolysegrad von AMX unter Verwendung des Enzyms β-Lactamase in der Probenvorbereitung entwickelt. Für beide Analyten ermöglichen die MBBAs eine schnelle Quantifizierung mit Ergebnissen in weniger als einer Stunde, was eine wesentliche Verbesserung gegenüber herkömmlichen Immunoassays wie dem Enzyme-linked Immunosorbent Assay (ELISA) darstellt. Im Vergleich zu den entsprechenden ELISAs mit denselben Antikörpern weisen die MBBAs zudem verbesserte analytische Parameter auf, wie einen breiteren Messbereich und niedrigere Nachweisgrenzen. Aufgrund der magnetischen Eigenschaften der Partikel, die als Plattform für die Assays dienen, eignen sie sich für den mobilen und automatisierten Einsatz vor Ort. Ein integriertes Diagnosesystem, bei dem die elektrochemische Detektion mittels Chronoamperometrie auf einem mikrofluidischen Chip eine weitere Miniaturisierung des Systems ermöglicht, wurde entworfen, um die Überwachung der Trinkwasserqualität online in Wasserwerken zu ermöglichen. KW - Antibiotics KW - Immunoassay KW - Amoxicillin KW - Diclofenac KW - Biosensor KW - Antibodies PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591901 DO - https://doi.org/10.18452/25853 SP - 1 EP - 129 CY - Berlin AN - OPUS4-59190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shaheen, Sabahat A1 - Hicke, Konstantin A1 - Krebber, Katerina T1 - Blast-Assisted Subsurface Characterisation Using a Novel Distributed Acoustic Sensing Setup Based on Geometric Phases N2 - A novel DAS setup based on geometric phases in coherent heterodyne detection is applied for the first time to the characterisation of the Earth’s subsurface. In addition, an optimisation of the proposed setup in terms of its spatial resolution is also presented for the first time. The surface waves are generated by strong blasts of 25 kg of explosives at a dedicated test site. A 10 km dark fiber link in the vicinity of the test site connected to the test setup records the resulting strain signals. The spike-free and low-noise strain data thus obtained minimize post-processing requirements, making the setup a candidate for real-time seismic monitoring. An analysis of the dispersion characteristics of the generated surface waves is performed using a recently reported optimised seismic interferometric technique. Based on the dispersion characteristics, the shear wave velocities of the surface waves as a function of the depth profile of the Earth’s crust are determined using an optimised evolutionary algorithm. KW - Geophysics KW - Geometric Phase KW - Distributed Fiber Optic Sensor KW - Distributed Acoustic Sensing KW - Earthquake Monitoring KW - Seismology PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591913 DO - https://doi.org/10.3390/s24010030 VL - 24 IS - 1 SP - 1 EP - 12 PB - MDPI AN - OPUS4-59191 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Pb isotope ratio analysis N2 - The determination of Pb isotope ratios by TIMS and ICP-MS is discussed and applications from archaeology are provided. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Isotope reference material KW - Provenance KW - Silver artefacts KW - Curse tablets PY - 2023 AN - OPUS4-59167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Sr isotope ratio analysis N2 - The measurment of Sr isotope ratios is described and examples from food authenticity, provenancing of cement and pietas are provided. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Conventional isotope ratios KW - Gypsum KW - Cement KW - Cheese PY - 2023 AN - OPUS4-59168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Measurement Uncertainty in Isotope Ratio Measurements N2 - The importance for measurement uncertainty in isotope ratio measurements is expalined and different approaches for calculating measurement uncertainty for absolute isotope ratios, isotope deltas and conventional isotope ratios are presented. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Isotope delta KW - Absolute isotope ratio KW - Conventional isotope ratio PY - 2023 AN - OPUS4-59169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Kazlagić, Anera T1 - Provenancing of cement by the means of isotope techniques N2 - Concrete is the most important human-made material because it serves as the basis of our built environment. Since the properties of concretes are dominated by their key compound, cement, devising a way to determine the cement’s origin, known as provenancing, is of great importance for answering different provenance-related questions. These questions range from liability issues when damage occurs to concrete-made structures, to forensic investigations where cement particles are found at crime scenes. This thesis showcases the use of isotope techniques to answer these provenance-related questions. Conventional 87Sr/86Sr and 143Nd/144Nd isotope and elemental ratios consisting of Ca, Sr, K, Mn, Mg, and Ti are used as fingerprints for ordinary Portland cement (OPC) provenancing. The first part of this thesis describes research previously conducted in fingerprinting cementitious materials, providing an overview of provenance studies of cement and the main approaches commonly used. In several studies, the origin of clinker for certain locations was determined via different approaches. However, clinker is an intermediate product, which is available only at the production site and therefore, the practical relevance is rather limited. Furthermore, the use of Sr and Nd isotope systems, together with elemental fingerprints are presented as state of the art in the field. Therein, the principal approach for the overall study is sketched. For the second part of the study, a sample preparation technique for Sr isotopes in Portland cement was developed. The aim was to find the most appropriate sample preparation procedure for cement provenancing and selection was realised by comparing the 87Sr/86Sr isotope ratios of differently treated OPCs with those of the corresponding clinkers. Based on these findings, the third part of the study focused on the measurements of Sr and Nd isotope ratios, together with elemental ratios, to establish a reliable technique for OPC provenancing. The outcomes of this final stage are then used to establish a procedure for fingerprinting cements. This becomes possible with the use of Sr and Nd isotope ratios and geochemical profiles. To perform isotope ratio measurements and obtain reliable data, it was necessary to establish a quality control procedure. Thus, an interlaboratory comparison (ILC) was organised to characterise 87Sr/86Sr isotope ratios in geological and industrial reference materials by applying the conventional method for 87Sr/86Sr isotope ratios. As reference material, four cements (VDZ 100a, VDZ 200a, VDZ 300a, IAG OPC-1), one limestone (IAG/CGL ML-3) and one slate (IAG OU-6) were selected, thus covering a wide range of Sr isotope signatures. KW - Isotope ratio KW - Strontium KW - Neodymium KW - Ordinary Portland cement PY - 2023 SP - 1 EP - 148 CY - Berlin AN - OPUS4-59172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bertovic, Marija A1 - Given, Joseph A1 - Rentala, V K A1 - Wall, M A1 - Kanzler, D A1 - Lehleitner, Johannes A1 - Heckel, Thomas A1 - Tkachenko, Viktoriya T1 - Methods for quantification and integration of human factors into probability of detection assessments N2 - Human factors (HFs) are a frequently mentioned topic when talking about the reliability of non-destructive testing (NDT). However, probability of detection (POD), the commonly used measure of NDT reliability, only looks at the technical capability of an NDT system to detect a defect. After several decades of research on the influence of HFs on NDT reliability, there is still no commonly accepted approach to rendering HFs visible in reliability assessment. This paper provides an overview of possible quantitative and qualitative methods for integrating HFs into the reliability assessment. It is concluded that reliability assessment is best carried out using both quantifiable and non-quantifiable approaches to HFs. KW - Materials Chemistry KW - Metals and Alloys KW - Mechanical Engineering KW - Mechanics of Materials KW - Non-Destructive Testing (NDT) KW - Human factors KW - Detection Assessments PY - 2023 DO - https://doi.org/10.1784/insi.2023.65.7.364 SN - 1354-2575 VL - 65 IS - 7 SP - 364 EP - 372 PB - British Institute of Non-Destructive Testing (BINDT) AN - OPUS4-59173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Vergin, Chantal Celine T1 - Entwicklung eines Extraktionsverfahrens für Mykotoxine aus Lebensmitteln für die Messung in immunanalytischen Assays und Sensoren N2 - Mykotoxine sind sekundäre Stoffwechselprodukte, die von Schimmelpilzen gebildet werden. Sie sind unvermeidliche Lebensmittelkontaminanten und stellen daher ein ernstes Gesundheitsrisiko für Mensch und Tier dar. Aus diesem Grund hat die Europäische Kommission Vorschriften erlassen, die Höchstwerte für Mykotoxine in bestimmten Lebensmitteln vorsehen. Um die gesetzlichen Grenzwerte einzuhalten, müssen in der Lebensmittelindustrie Mykotoxinanalysen der eingehenden Waren durchgeführt werden. Gegenwärtig umfasst die Analyse zeitaufwändige Probenvorbereitungsschritte, denen in der Regel eine chromatographische Analyse folgt. Immunoassays ermöglichen eine Vor-Ort-Analyse, aber in der Regel sind für feste Lebensmittelproben lösungsmittelbasierte Extraktionsschritte erforderlich. Da Immunoassays in der Regel nicht mit den hohen Lösungsmittelkonzentrationen kompatibel sind, die üblicherweise für die Mykotoxinextraktion verwendet werden (z.B. Acetonitril oder Methanol), war es das Ziel dieser Arbeit, ein Extraktionsverfahren für die Mykotoxine Deoxynivalenol und Ochratoxin A aus Weizenmehl und Getreide zu entwickeln, das für Immunoassays und -sensoren verwendet werden kann. Vier verschiedene Lösungsmittel, Methanol (10 %), Ethanol (5 %) und Acetonitril (10 %) sowie Milli-Q-Wasser wurden für die Extraktion des Analyten Deoxynivalenol getestet. Um negative Umweltaspekte zu vermeiden und aufgrund der vergleichbaren Extraktionseffizienz von Milli-Q-Wasser gegenüber den anderen Lösungsmitteln, wurde Milli-Q-Wasser als Extraktionslösung im optimierten Extraktionsprotokoll für Deoxynivalenol verwendet. Es wurden verschiedene Extraktionsbedingungen, wie die Extraktionszeit, das Lösungsmittel-Feststoff-Verhältnis, der Filtrationsschritt, der Zentrifugationsschritt sowie die Zusammensetzung des Wassers untersucht. Auf der Grundlage der Ergebnisse wurde ein Extraktionsprotokoll festgelegt, mit dem Wiederfindungsraten in einem Bereich von x bis x erzielt wurden. Das Extraktionsprotokoll umfasste die Extraktion von 2 g Weizenmehl mit 40 ml Milli-Q-Wasser für 30 Minuten, die anschließende Zentrifugation bei 3000 U/min für 15 Minuten bei 4 °C und die Filtration des Überstands. KW - Mykotoxine KW - ELISA KW - Probenvorbereitung PY - 2023 SP - 1 EP - 81 CY - Berlin AN - OPUS4-59199 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Advanced chemistry broadens the scope of antibody-based analytical methods N2 - Advanced chemistry, making haptens, chemical labels, particle labels, particle carriers, encoding particles, multiplexing, particles for hold/release, microfludics, electrode chemistry, DDI, WBE are the topics of this invited talk. T2 - Seminar des IQAC-CSIC (Institute for Advanced Chemistry of Catalonia) CY - Barcelona, Spain DA - 26.10.2023 KW - Labels KW - Particles KW - Sensors KW - Wastewater-based epidemiology PY - 2023 AN - OPUS4-59201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Von der Kläranlage in das Labor N2 - Im Vorhaben „MARKERIA - Bestimmung von anthropogenen Markerkonzentrationen für die SARS-CoV-2 Quantifizierung mittels eines Hochdurchsatzverfahrens (ELISA)“ geht es um die Bestimmung von Carbamazepin, Diclofenac, Koffein und einer endogenen Gallensäure als potentielle Marker für die Kalibrierung der SARS-CoV-2 Quantifizierung im Abwasser. Es ist ein Teilvorhaben des übergeordneten Projektes ESI-CorA und wird von der BAM im Auftrag des Umweltbundesamtes durchgeführt. Der Vortrag wurde gehalten im Rahmen der Abschlussveranstaltung des Projektes ESI-CorA. Er gab den Projektstand wieder, den UBA und BAM bis dahin erzielt hatten, das SARS-CoV-2 Virus und die anthropogenen Marker in 20 Kläranlagenzuläufen zu bestimmen und miteinander zu korrelieren. T2 - Abschlussveranstaltung des EU-Projekts ESI-CorA CY - Karlsruhe, Germany DA - 22.03.2023 KW - Wastewater-based epidemiology KW - Abwasser KW - ELISA KW - Coronavirus KW - COVID-19 PY - 2023 AN - OPUS4-59204 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Bestimmung von anthropogenen Markerkonzentrationen für die SARS-CoV-2 Quantifizierung mittels eines Hochdurchsatzverfahrens (ELISA) N2 - Im Vorhaben „MARKERIA - Bestimmung von anthropogenen Markerkonzentrationen für die SARS-CoV-2 Quantifizierung mittels eines Hochdurchsatzverfahrens (ELISA)“ geht es um die Bestimmung von Carbamazepin, Diclofenac, Koffein und einer endogenen Gallensäure als potentielle Marker für die Kalibrierung der SARS-CoV-2 Quantifizierung im Abwasser. Der Vortrag wurde gehalten im Rahmen der 22. Sitzung des Begleitkreises des übergeordneten Projektes ESI-CorA. Er gab den Projektstand wieder, den die BAM bis dahin erzielt hatte. Die Marker waren in sämtlichen untersuchten Abwasser-Zulaufproben enthalten und zeigten spezifische Trends. Weitere Korrelationen müsse die weitergehende Datenauswertung ergeben.A T2 - 22. Sitzung des Begleitkreises des Projektes ESI-CorA CY - Online meeting DA - 13.02.2023 KW - Wastewater-based epidemiology KW - ELISA KW - Abwasser KW - Antikörper KW - Antibody PY - 2023 AN - OPUS4-59205 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karafiludis, Stephanos A1 - Kochovski, Z. A1 - Scoppola, E. A1 - Retzmann, Anika A1 - Hodoroaba, Vasile-Dan A1 - ten Elshof, J. E. A1 - Emmerling, Franziska A1 - Stawski, Tomasz Maciej T1 - Nonclassical Crystallization Pathway of Transition Metal Phosphate Compounds N2 - Here, we elucidate nonclassical multistep crystallization pathways of transition metal phosphates from aqueous solutions. We followed precipitation processes of M-struvites, NH4MPO4·6H2O, and M-phosphate octahydrates, M3(PO4)2·8H2O, where M = Ni, Co, or NixCo1–x, by using in situ scattering and spectroscopy-based techniques, supported by elemental mass spectrometry analyses and advanced electron microscopy. Ni and Co phosphates crystallize via intermediate colloidal amorphous nanophases, which change their complex structures while agglomerating, condensing, and densifying throughout the extended reaction times. We reconstructed the three-dimensional morphology of these precursors by employing cryo-electron tomography (cryo-ET). We found that the complex interplay between metastable amorphous colloids and protocrystalline units determines the reaction pathways. Ultimately, the same crystalline structure, such as struvite, is formed. However, the multistep process stages vary in complexity and can last from a few minutes to several hours depending on the selected transition metal(s), their concentration, and the Ni/Co ratio. KW - Non-classical crystallization theory KW - Transition metals KW - Phosphates KW - Amorphous phases KW - Intermediate phases PY - 2023 DO - https://doi.org/10.1021/acs.chemmater.3c02346 SN - 1520-5002 VL - 35 IS - 24 SP - 10645 EP - 10657 PB - American Chemical Society (ACS) CY - Washington D.C. AN - OPUS4-59135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Metrology in Chemistry - Basics and international structure N2 - Basics in Metrology in Chemistry are explained and the international structure of the metrology network is presented. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Metrology in Chemistry KW - Traceability KW - Uncertainty PY - 2023 AN - OPUS4-59163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope Ratio Analysis N2 - Basic information on isotope ratio analysis is provided. Isotope fractionation is discussed and the measurement process is described. Additionally, practical examples are provided. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Isotope fractionation KW - Mass spectrometry KW - Terminology PY - 2023 AN - OPUS4-59164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope Ratio Measurement - Quantities and calibration N2 - The quantities and the terminoly in isotope ratio measurements is presented, followed by explaining calibration approaches for isotope ratio measurements. Sources of error and bias are presented and special focus is given on single detector mass spectrometry. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Isotope fractionation KW - Matrix separation KW - Interferences KW - Noise KW - Optimization PY - 2023 AN - OPUS4-59165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Detector deadtime N2 - Deadtime effects for counting detectors in ICP-MS and deadtime correction are discussed. Approaches for determining the deadtime are presented. T2 - Workshop & Training "Isotope Ratio Analysis" CY - Pathum Thani, Thailand DA - 06.12.2023 KW - Counting detector KW - Detector deadtime KW - Isotope ratio KW - Dual mode detector PY - 2023 AN - OPUS4-59166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Devi, Sarita T1 - Interaction of L-phenylalanine with Magnetic Metal-Organic Framework: Electrochemical Analysis N2 - As the basic units of proteins, the importance of amino acids in organisms is self-evident and therefore detection of the concentration of amino acids is significant in monitoring human health. For example, patients suffering from phenylketonuria should be able to monitor their phenylalanine (PHE) level in a rapid, decentralized, and affordable manner to avoid high levels of PHE in the body which can lead to a profound and irreversible mental disability. Herein, a magnetic and conductive Iron based metal–organic framework (MOF) is prepared using tetrahydroxyquinone and benzene dicarboxylic acid, dual ligands. The uncoordinated carboxyl groups provided the binding sites for PHE. Physicochemical properties of MOF were characterized by XRD, SEM, DLS and FTIR analyses. The effects of different operational parameters: pH (2, 4, 6, 7.2, 8.6, 10, 12), contact time and MOF concentration were optimized for best properties using cyclic voltametric technique. The 10 µl of 1mg/ml MOF (pH 8.6) in deionized water was used as working electrode on screen-printed gold electrode. The presence of new well-defined oxidation and reduction current peak in electrochemical signal of MOF-modified SPGE sensor vs. Ag/AgCl in phosphate buffer solution (pH 1.9) remarks the quantification of PHE. The analytical calibration curve for PHE showed a linear response with concentration in the oxidation and reduction peak current range from 50 to 1000 µM, with a limit of detection (LOD) of 35.16 µM. T2 - SALSA Conference Make & Measure: Interfaces CY - Berlin, Germany DA - 13.09.2023 KW - Electroanalysis KW - Metal-Organic Framework KW - L-phenylalanin KW - Cyclic Voltammetry PY - 2023 AN - OPUS4-59239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Expression of Aspergillus niger Fumonisin Amine Oxidase (AnFAO) for an Electrochemical Detection of the Mycotoxin N2 - The poster describes how molecular biology, especially recombinant expression of proteins, in this case, an enzyme, can underpin developments of biosensors. The fumonisin oxidase produced by the fungus Aspergillus niger (AnFAO) is highly selective for the toxic mycotoxin fumonisin. Its structure and sequence has been published before. We took this information and expressed the enzyme in E. coli. The enzyme proved active and could be employed in an amperometric biosensor for the detection of the mycotoxin. T2 - 30. Leibniz Conference of Advanced Science CY - Berlin, Germany DA - 06.10.2023 KW - Biosensor KW - Enyzme KW - Recombinant KW - Electrochemical detection PY - 2023 AN - OPUS4-59241 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bintz, Thilo A1 - Kruschwitz, Sabine T1 - Investigation of Capillary Water Absorption of Clinker-Reduced Binders by NMR Relaxometry N2 - To evaluate the durability of new alternative cement compositions, it is important to examine the internal transport of moisture through these materials. For this purpose, mortars were prepared from different types of cement and capillary suction experiments were carried out. The moisture transport was studied with an NMR tomograph and compared with weight measurements. With the tomograph, the total moisture input could be determined, as well as the moisture content within the samples non-destructively and spatially resolved. This allows precise observation of the moisture fronts. The tomograph was also used to determine the capillary transport coefficient. T2 - International Conference on Electromagnetic Wave Interaction with Water and Moist Substances of the International Society for Electromagnetic Aquametry (ISEMA) 2023 CY - Brisbane, Ausralia DA - 25.09.2023 KW - NMR relaxometry KW - Capillary suction KW - Capillary transport coefficient PY - 2023 SP - 1 EP - 3 AN - OPUS4-59217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Plasma Fundamentals and Diagnostics N2 - This course will provide an introduction to plasma diagnostic techniques. The major focus of the course will be on the discussions of the practical procedures as well as the underlying physical principles for the measurements of plasma fundamental characteristics (e.g., temperatures, thermodynamic properties, and electron number density). Particular emphasis will be placed on inductively coupled plasma–atomic emission spectrometry, but other analytical plasmas will also be used as examples when appropriate. Selected examples on how one can manipulate the operating conditions of the plasma source, based on the results of plasma diagnostic measurements, to improve its performance used for spectrochemical analysis will also be covered. Topics to be covered include thermal equilibrium, line profiles, temperatures, electron densities, excitation processes, micro reactions, pump and probe diagnostics, tomography, temporal and spatial resolution. Basis of plasma computer modeling will be presented. T2 - 2024 Winter Conference on Plasma Spectrochemistry CY - Tucson, Arizona, USA DA - 15.01.2024 KW - Plasma KW - Plasma fundamentals KW - Plasma diagnostics PY - 2024 AN - OPUS4-59430 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Laser-Induced Plasma for Spectroscopy and More N2 - An overview of personal experience with laser-induced plasma (LIP) will be given. The combination of LIP with laser-induced fluorescence, atomic absorption, Raman spectroscopy and spatial heterodyne spectroscopy for elemental and isotopic analysis will be discussed. Unusual applications of LIP will be covered, such as LIP-based lasers and LIP-based chemical reactors. T2 - 2024 Winter Conference on Plasma Spectrochemistry CY - Tucson, Arizona, USA DA - 15.01.2024 KW - Laser induced plasma KW - Laser ablation KW - LIP-LIF KW - LIP-AAS PY - 2024 AN - OPUS4-59431 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Häusler, F. A1 - Stührenberg, J. A1 - Neumann, Patrick P. ED - Sigalov, K. ED - Hagedorn, P. ED - Schönfelder, P. ED - Faltin, B. ED - Zentgraf, S. ED - Block, M. T1 - Gasquellenlokalisierung mit Drohnenschwärmen N2 - Gasquellenlokalisierungen (Gas Source Localization, GSL) tragen dazu bei, die Folgen von Industrieunfällen und Naturkatastrophen zu mildern. Während die GSL, wenn von Menschen durchgeführt, gefährlich und zeitaufwändig ist, können Schwärme von wendigen und kostengünstigen Nanodrohnen die Effizienz und Sicherheit der Suche erhöhen. Da die geringe Nutzlast von Nanodrohnen die Sensor- und Rechenressourcen einschränkt, werden Strategien zur Koordination des Roboterschwarms verwendet, die von biologischen Schwärmen, wie Kolonien sozialer Insekten, inspiriert sind. Die meisten Schwarm-GSL-Strategien verwenden das Maximum der Gaskonzentrationsverteilung zur Schätzung der Gasquellenposition. Experimente legen jedoch nahe, dass die Intermittenz der Gasverteilung vielversprechender ist. In diesem Beitrag wird eine neuartige GSL-Strategie für Schwärme vorgestellt, die auf Pheromonkommunikation und Intermittenz der Gasverteilung basiert. Die Agenten, d.h. die Nanodrohnen, emittieren Pheromonmarker in einer virtuellen Umgebung, wenn sie eine neue Gaswolke feststellen. Die Agenten werden durch virtuelle Kräfte gesteuert und nutzen abwechselnd das Wissen des Schwarms, indem sie dem Pheromongradienten folgen, oder erkunden den Suchraum, indem sie einen Zufallspunkt ansteuern. Zur Kollisionsvermeidung werden die Agenten durchgehend von anderen Agenten und Wänden abgestoßen. Die Strategie wurde auf drei Nanodrohnen implementiert und durch ein Experiment in einem Innenraum mit einer statischen Gasquelle validiert. Die Ergebnisse zeigen eine Verbesserung gegenüber maximabasierten Verfahren und geringe Lokalisierungsfehler in Windrichtung. T2 - 34. Forum Bauinformatik 2023 CY - Bochum, Germany DA - 06.08.2023 KW - Mobile Robotic Olfaction KW - Bouts KW - Mobile Sensorik KW - Nanodrohnen KW - Pheromonkommunikation KW - Schwarmrobotik PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594320 DO - https://doi.org/10.13154/294-10088 SP - 168 EP - 175 AN - OPUS4-59432 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - D.E.T.E.C.T. - Drohnengestützte Technologie zur Lokalisierung von Explosivstoffen mittels Chemosensoren N2 - Communities worldwide face significant threats from Explosive Remnants of War (ERW), which endanger lives and restrict land usage. From forest fires due to ERWs or in ERW-contaminated areas (e.g., in Jüterbog, Germany) to broader global challenges (e.g., the Ukrainian conflict), the need for efficient detection and removal of these remnants, especially for humanitarian demining, is paramount. Traditional methods, like manual demining, have severe limitations in safety and efficiency. Here, we introduce an innovative solution to these challenges: “Chemosensing Smart Dust.” This technology uses chemoselective dyes that change their fluorescence properties when exposed to explosives like 2,4,6-trinitrotoluene (TNT). Fluorescence-based detection offers superior sensitivity, reduced likelihood of false positives, and enhanced accuracy of explosive detection. Drones, equipped with excitation lasers or LEDs, deploy the Chemosensing Smart Dust over areas of interest and actively detect the fluorescence changes using high-resolution cameras, offering a rapid, safe, and adaptable detection method. Beyond demining, this innovative approach has potential applications in monitoring polluted areas, homeland security, and emergency response. T2 - Begutachtungskolloquium Schwerpunktprogramm “Messtechnik auf fliegenden Plattformen“ (SPP 2433/1) CY - Bonn, Germany DA - 22.01.2024 KW - Mobile Robotic Olfaction KW - Smart Dust KW - Source Localization PY - 2024 AN - OPUS4-59433 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Temgoua, Ranil C.T. A1 - Dontsi, Fabiola T. A1 - Lebègue, Estelle A1 - Thobie-Gautier, Christine A1 - Tonlé, Ignas K. A1 - Boujtita, Mohammed T1 - Understanding the behavior of phenylurazole-tyrosine-click electrochemical reaction using hybrid electroanalytical techniques N2 - In this work, the electrochemical behavior of 4-phenylurazole (Ph-Ur) was studied and the latter was used as a molecular anchor for the electrochemical bioconjugation of tyrosine (Y). Cyclic voltammetry (CV) and controlled potential coulometry (CPC) allowed the in-situ generation of the PTAD (4-phenyl-3 H-1,2,4-triazole-3,5(4 H)-dione) species from phenylurazole on demand for tyrosine electrolabeling. The chemoselectivity of the reaction was studied with another amino acid (lysine, Lys) and no changes in Lys were observed. To evaluate the performance of tyrosine electrolabeling, coulometric analyses at controlled potentials were performed on solutions of phenylurazole and the phenylurazole-tyrosine mixture in different proportions (2:1, 1:1, and 1:2). The electrolysis of the phenylurazole-tyrosine mixture in the ratio (1:2) produced a charge of 2.07 C, very close to the theoretical value (1.93 C), with high reaction kinetics, a result obtained here for the first time. The products obtained were identified and characterized by liquid chromatography coupled to high-resolution electrospray ionization mass spectrometry (LC-HRMS and LC- HRMS2). Two products were formed from the click reactions, one of which was the majority. Another part of this work was to study the electrochemical degradation of the molecular anchor 4-phenylazole (Ph-Ur). Four stable degradation products of phenylurazole were identified (C7H9N2O, C6H8N, C6H8NO, C14H13N4O2) based on chromatographic profiles and mass spectrometry results. The charge generated during the electrolysis of phenylurazole (two-electron process) (2.85 C) is inconsistent with the theoretical or calculated charge (1.93 C), indicating that secondary/parasitic reactions occurred during the electrolysis of the latter. In conclusion, the electrochemically promoted click phenylurazole-tyrosine reactions give rise to click products with high reaction kinetics and yields in the (1:2) phenylurazole-tyrosine ratios, and the presence of side reactions is likely to affect the yield of the click phenylurazole-tyrosine reaction. KW - Clinical Biochemistry KW - Spectroscopy KW - Drug Discovery KW - Pharmaceutical Science KW - Analytical Chemistry PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599267 DO - https://doi.org/10.1016/j.jpba.2024.116147 VL - 245 SP - 1 EP - 8 PB - Elsevier BV AN - OPUS4-59926 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Döring, Sarah T1 - Optimization of surface-functionalized particles for improved antibody digestion N2 - Therapeutic monoclonal antibodies are the fastest-growing group of biological agents which generated a yearly turnover of USD 210 billion in 2022 and whose sales are expected to grow by 10% annually over the next 10 years. With steadily increasing market importance, analytical methods for reliable quantification of therapeutic antibodies also become more and more relevant. Liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) has become the main technology for antibody quantification. This approach, however, requires enzymatic digestion of the intact protein into peptides, for which a wide range of different protocols exists that often lead to different results depending on the digestion procedure or trypsin variants used. In particular, the amount and type of detergents added for protein unfolding prior to digestion is known to create significant bias in measurement results. The overall goal of the presented project is the application of novel thermostable and surface-functionalized trypsin particles for improved antibody digestion. Specifically, a trypsin-variant described in the literature exhibiting increased activity and thermal stability above 80°C, will be examined. The application of this enzyme should allow to perform digestion at elevated temperatures where the protein is naturally unfolding thereby increasing enzyme accessibility without the need for detergents. Furthermore, we will immobilize the thermostable trypsin onto the surface to further enhance enzyme stability, prevent self-digestion, and enable separation of trypsin from target peptides before LC–MS/MS analysis. As an immobilization platform, cheap and non-porous corundum particles will be used as these show high chemical stability and low levels of interaction of matrix proteins with the functionalized surface. adsorption. In a multidisciplinary collaboration with the SALSA Photonics Lab, we will investigate the characteristics of covalent enzyme binding and unspecific peptide binding using an interface-sensitive analytical tool, vibrational sum-frequency generation (VSFG) spectroscopy. The insights gained will not only lead to new competencies in peptide and enzyme surface analysis using VSFG spectroscopy in SALSA but will also significantly contribute to optimizing antibody quantification. T2 - SALSA STF24 Kick-Off Meeting CY - Berlin, Germany DA - 11.04.2024 KW - Antibody Quantification KW - Vibrational Sum-Frequency Generation Spectroscopy KW - LC-MS/MS KW - Enzyme Immobilisation KW - Corundum PY - 2024 AN - OPUS4-59864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hiller, Lukas T1 - Herstellung und Charakterisierung eines rekombinanten Anti-Tetanus-Antikörpers aus verschiedenen Säugerzelllinien N2 - Antikörper sind in der medizinischen Welt nicht mehr wegzudenken. Ihr Einsatz-Repertoire als Therapeutika für die Behandlung diverser Krankheiten und Infektionen weitet sich von Jahr zu Jahr mehr aus. Dabei basiert ein Großteil der verwendeten Antikörper zu diesem Zeitpunkt auf monoklonalen Antikörpern auf Basis von Hybridomazellen. Doch hier könnten rekombinante Antikörper aufgrund ihrer Vektor-basierten Expression eine vielversprechende und womöglich sogar revolutionierende Alternative bieten. So ergeben sich neue Optimierungsoptionen für Merkmale wie Affinität, Stabilität und Kompatibilität über Anpassungen auf genetischer oder posttranslationaler Ebene. Allerdings ergibt sich kein Anwendungszweck ohne die vorhergehende detaillierte Charakterisierung der Antikörper. Denn nur mit spezifischem Wissen über die diversen Eigenschaften und Wechselwirkungen kann eine effektive und präzise Verwendung in der Diagnostik und Therapeutik gewährleistet werden und auf diese Weise Leben retten. Aus diesem Grund beschäftigt sich diese Masterarbeit mit der Vertiefung der rekombinanten Antikörper-Thematik. Dazu soll ein Anti-Tetanus-Antikörper erstmals rekombinant in verschiedenen Zelllinien hergestellt und anschließend über umfangreiche analytische Verfahren mit einem Fokus auf die Einflussanalyse der unterschiedlichen posttranslationalen Glykosylierungen charakterisiert werden. Zu diesem Zweck wurden als Grundlage einerseits zwei P1316-Dual-Expressions-Vektoren mit variierenden Insert-Positionen der schweren und leichten Kette durch Gibson-Assembly sowie individuellen pRK5-Plasmide für eine separiert Expression der Antikkörperketten mithilfe Restriktionsfragment-Ligation generiert. In einer Gegenüberstellung der der Expressionsausbeuten stellte sich die Überlegenheit der P1316-Plasmid-Konfiguration heraus, in der das Leichtketten-Insert an der ersten Expressionsstelle positioniert ist. Deshalb wurde dieser Vektor als Ausgangspunkt für die anschließende hochskalierten Herstellung des Anti-Tetanus-Antikörpers in Expi293F-GnTI- und ExpiCHO-S-Zellen verwendet. Ein ELISA bestätigte die Bindungsaktivität der rekombinanten Antikörper am Tetanus-Toxoid unabhängig vom Expressionssystem. Nach einer folgenden Optimierung der für die Aufreinigung verwendeten Protein-A-Affinitätschromatographie, wurde über weitere Charakterisierungsmethoden wie Größenausschlusschromatographie und dynamische Lichtstreuung eine vergleichbare Aggregation aufgrund der sauren Elution aufgezeigt. In diesem Kontext wurde die Notwendigkeit einer Zweistufen-Präparation mit Affinitäts- und Größenausschlusschromatografie für den Erhalt monodisperser Proben verdeutlicht. Zudem wurden die verschiedenen intakten Massen mitsamt ihrer spezifischen Glykan-abhängigen Streumaßen in Relation zum monoklonalen NISTmAB-Referenzantikörper bestimmt. Dabei konnte den Erwartungen nach sowohl die geringere Masse als auch die uniformere Glykosylierung der in Expi293 GnTI- exprimierten Immunoglobuline in Relation zum ExpiCHO-S-Antikörper nachgewiesen werden. Anschließend wurde das Stabilitätsverhalten mittels thermischer Entfaltung und dynamischer Lichtstreuung über einen ausgeweiteten Zeitraum sowie verschiedenen Temperaturen dokumentiert. Grundlegend wurde eine höhere thermische Stabilität der zweiten konstanten Schwerketten-Domäne des aus ExpiCHO-S-Zellen stammenden Antikörpers nachgewiesen. Außerdem konnte eine problemlose Lagerungsfähigkeit beider unterschiedlich glykosylierter Antikörper bei Raumtemperatur für mindestens 4 Wochen festgestellt werden. Des Weiteren wurde die Langzeitlagerung im Rahmen der Auswirkung von Gefrier-Auftau-Zyklen mit gleichbleibenden Methoden sowie zusätzlicher Größenausschlusschromatographie erprobt. Hierbei stellte sich der Erhalt der strukturellen Integrität nach bis zu 15 Zyklen heraus. Allerdings geht die Monodispersität bereits nach wenigen Zyklen verloren, wobei die geringfügiger glykosylierten Expi293F-GnTI-Anti-Tetanus-Antikörper eine stärkere Beeinträchtigung durch multiple Gefrier-Auftau-Zyklen aufwiesen. KW - Rekombinante Antikörper KW - Affinitätschromatographie KW - Größenausschlusschromatographie KW - MALDI-TOF-MS KW - Dynamische Lichtstreuung PY - 2024 SP - 1 EP - 120 CY - Berlin AN - OPUS4-59865 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vaupel, Otto T1 - 75 Jahre Röntgenstrahlen auch in der Materialprüfung N2 - Der Verfasser berichtet über Entstehung und Nachweis der Röntgenstrahlen sowie die Entwicklung und den heutigen Stand der Röntgentechnik in der Materialprüfung. KW - Röntgenstrahlung KW - Materialprüfung PY - 1970 SN - 0300-8592 VL - 23 IS - Oktober SP - 469 EP - 476 PB - Thieme CY - Stuttgart AN - OPUS4-59847 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dalgic, Mete-Sungur A1 - Weidner, Steffen T1 - Solvent-free sample preparation for matrix-assisted laserdesorption/ionization time-of-flight mass spectrometry ofpolymer blends N2 - Solvent-free sample preparation offers some advantages over solvent-based techniques, such as improved accuracy, reproducibility and sensitivity, for matrix-assisted laser desorption/ionization (MALDI) analysis. However, little or no information is available on the application of solvent-free techniques for the MALDI analysis of polymer blends. Solvent-free sample preparation by ball milling was applied with varying sample-to-matrix ratios for MALDI time-of-flight mass spectrometry analysis of various polymers, including polystyrenes, poly(methyl methacrylate)s and poly(ethylene glycol)s. The peak intensity ratios were compared with those obtained after using the conventional dried droplet sample preparation method. In addition, solvent-assisted milling was also applied to improve sample homogeneities. Depending on the sample preparation method used, different peak intensity ratios were found, showing varying degrees of suppression of the signal intensities of higher mass polymers. Ball milling for up to 30 min was required to achieve constant intensity ratios indicating homogeneous mixtures. The use of wet-assisted grinding to improve the homogeneity of the blends was found to be disadvantageous as it caused partial degradation and mass-dependent segregation of the polymers in the vials.The results clearly show that solvent-free sample preparation must be carefully considered when applied to synthetic polymer blends, as it may cause additional problems with regard to homogeneity and stability of the blends. KW - MALDI TOF MS KW - Sample preparation KW - Polymer blends KW - Solvent-free PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598570 DO - https://doi.org/10.1002/rcm.9756 SN - 0951-4198 VL - 38 IS - 12 SP - 1 EP - 9 PB - Wiley online library AN - OPUS4-59857 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Heidenreich, Sebastian A1 - Bär, Markus A1 - Klauenberg, Katy A1 - Elster, Clemens A1 - Harris, Peter A1 - Lines, Keith A1 - Hippolyte, Jean-Laurent A1 - George, Indhu A1 - Wright, Louise A1 - Cox, Maurice A1 - Rhodes, Susan A1 - Zilberti, Luca A1 - Manzin, Alessandra A1 - Pennecchi, Francesca A1 - Kok, Gertjan A1 - van der Veen, Adriaan A1 - Fischer, Nicolas A1 - Sousa, Joao Alves A1 - Vogel, Kristin A1 - Bosnjakovic, Alen A1 - Ellison, Stephen T1 - Strategic Agenda, European Metrology Network for Mathematics and Statistics N2 - This document constitutes the Strategic Research Agenda (SRA) for the European Metrology Network for Mathematics and Statistics in Metrology (EMN Mathmet). The EMN Mathmet is an alliance of European National Metrology Institutes (NMIs), Designated Institutes (DIs) and an EMN Partner that aims to strengthen research and cooperation in the field. The SRA has been developed within a European project (EMPIR 18NET05 MATHMET) to promote and support the network. The SRA was developed based on a consultation process with stakeholders and the strategies of individual NMIs and DIs, and in alignment with the EURAMET 2030 strategy. As a key result, the SRA defines a long-term research goal: the EMN Mathmet will coordinate research to strengthen the trust in algorithms, software tools and data to underpin digital transformation. For this purpose, new emerging research topics where algorithms, software tools and data play a significant role were identified: (i) Artificial Intelligence and Machine Learning, and (ii) Computational Modelling and Virtual Metrology. The foundation for the development of these new topics is given by the traditional focus on (iii) Data Analysis and Uncertainty Evaluation. The SRA characterises the future needs and challenges in the field of mathematics and statistics in metrology and provides an outline of how the EMN Mathmet can meet these new emerging requirements. KW - Research Agenda KW - Metrology KW - Mathematics and Statistics PY - 2023 UR - https://www.euramet.org/european-metrology-networks/mathmet/strategy/strategic-research-agenda SN - 978-3-942992-78-7 SP - 1 EP - 68 PB - EURAMET e.V. CY - Braunschweig AN - OPUS4-59526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mirtsch, Mona T1 - Adoption of the information security management system standard ISO/IEC 27001 - A study among German organizations N2 - Against the backdrop of numerous security breaches and cyber-attacks, organizations need to take measures to secure their data and information. However, the well-known management system standard ISO/IEC 27001 for information security has shown a lower adoption rate – in terms of annual ISO survey data – than was previously expected by scholars and practitioners. Through the lens of Rogers' diffusion of innovation theory, we consider the adoption of ISO/IEC 27001 as a 'preventive innovation' and aim to identify factors that help gain a better understanding of its adoption. Therefore, we conducted a survey among German organizations on the use and impact of management system standards, explicitly distinguishing between organizations that implement ISO/IEC 27001 and those that are additionally certified against this standard. This study provides insights and contributes to an advanced understanding of motives, impacts, barriers, and useful measures to increase adoption of ISO/IEC 27001. Our findings may be useful to organizations considering the adoption of this management system standard, to certification bodies providing certification services, and to policymakers seeking means to improve information security in organizations. KW - Management science and operations research KW - ISO/IEC 27001 KW - Management system standard KW - Information security KW - QI-FoKuS KW - Certification PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594704 UR - http://ijqr.net/paper.php?id=1098 DO - https://doi.org/10.24874/ijqr17.03-08 SN - 1800-6450 SN - 1800-7473 VL - 17 IS - 3 SP - 747 EP - 768 PB - Center for Quality, University of Montenegro CY - Podgorica AN - OPUS4-59470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taylor, Tristen L. A1 - Tukhmetova, Dariya A1 - Duong, Thi Phuong Thanh A1 - Böwe, Anna-Maria A1 - Meermann, Björn A1 - Gundlach-Graham, Alexander T1 - Comparative study of the vibrating capillary nebulizer (VCN) and commercially available interfaces for on-line coupling of capillary electrophoresis with ICP-MS N2 - Capillary electrophoresis (CE) is a powerful and sensitive tool for speciation analysis when combined with inductively coupled plasma mass spectrometry (ICP-MS); however, the performance of this technique can be limited by the nature of pneumatic nebulizers. This study compares two commercially available pneumatic nebulizers to a newly introduced vibrating capillary nebulizer (VCN) for on-line coupling of CE with ICP-MS. The VCN is a low-cost, non-pneumatic nebulizer that is based on the design of capillary vibrating sharp-edge spray ionization. As a piezoelectrically driven nebulization source, the VCN creates an aerosol independent of gas flows and does not produce a low-pressure region at the nebulizer orifice. To compare the systems, we performed replicate analyses of sulfate in river water with each nebulizer and the same CE and ICP-MS instruments and determined the figures of merit of each setup. With the CE-VCN-ICP-MS setup, we achieved around 2–4 times lower sensitivity compared to the commercial setups. However, the VCN-based setup provided lower noise levels and better linear correlation from the analysis of calibration standards, which resulted in indistinguishable LOD and LOQ values from the in-house-built VCN-based and commercial setups for CE-ICP-MS analysis. The VCN is found to have the highest baseline stability with a standard deviation of 3500 cts s−1, corresponding to an RSD of 2.7%. High reproducibility is found with the VCN with a peak area RSD of 4.1% between 3 replicate measurements. KW - Speciation analysis KW - Analytical chemistry KW - Surface water PY - 2024 DO - https://doi.org/10.1007/s00216-024-05162-7 SN - 1618-2650 SP - 1 EP - 9 PB - Springer CY - Berlin AN - OPUS4-59472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaytsev, D. A1 - Funk, Alexander T1 - On the crack evolutional in human dentin under uniaxial compression imaged by high resolution tomography N2 - An observation of the fracture process in front of the crack tip inside a dentin sample by means of ex-situ X-ray computed tomography after uniaxial compression at different deformation values was carried out in this work. This ex-situ approach allowed the microstructure and fracturing process of human dentin to be observed during loading. No cracks are observed up to the middle part of the irreversible deformation in the samples at least visible at 0.4μm resolution. First cracks appeared before the mechanical stress reached the compression strength. The growth of the cracks is realized by connecting the main cracks with satellite cracks that lie ahead of the main crack tip and parallel its trajectory. When under the stress load the deformation in the sample exceeds the deformation at the compression strength of dentin, an appearance of micro-cracks in front of the main cracks is observed. The micro-cracks are inclined (~60°) to the trajectory of the main cracks. The further growth of the main cracks is not realized due to the junction with the micro-cracks; we assume that the micro-cracks dissipate the energy of the main crack and suppressed its growth. These micro-cracks serve as additional stress accommodations, therefore the samples do not break apart after the compression test, as it is usually observed under bending and tension tests. KW - Dentin KW - Crack evolution KW - Compression strength KW - Mechanical properties KW - Microstructure KW - Ex-situ X-ray computed tomography PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594810 DO - https://doi.org/10.18149/MPM.5152023_5 SN - 1605-8119 VL - 51 IS - 5 SP - 38 EP - 51 PB - Advanced Study Center CY - St. Petersburg AN - OPUS4-59481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El-Athman, Rukeia A1 - Bresch, Harald A1 - Muth, Thilo A1 - Rädler, Jörg A1 - Rühle, Bastian T1 - Datenmanagement im Nanomaterial-Labor: Einsatz von ELN-Software zur digitalen Transformation des Laboralltags N2 - Angesichts der zunehmenden Digitalisierung und dem Einsatz datenintensiver Methodiken in der Wissenschaft stehen Forschende vor der Herausforderung, stetig wachsende Datenmengen nachvollziehbar zu dokumentieren, langfristig zu speichern und für Dritte nachnutzbar zu machen. Um diesen Anforderungen gerecht zu werden, bietet sich die Nutzung von Software-Lösungen an, welche Forschungsdatenmanagement mit der digitalen Dokumentation von Laborinventar und Experimenten in elektronischen Laborbüchern (engl. electronic lab notebooks (ELN)) verknüpfen. KW - NanoPlattform KW - BAM Data Store KW - OpenBIS KW - Forschungsdatenmanagement KW - Research data management KW - Elektronisches Laborbuch KW - Electronic lab notebook (ELN) PY - 2023 UR - https://analyticalscience.wiley.com/content/article-do/datenmanagement-im-nanomaterial-labor SN - 0016-3538 IS - 9 SP - 24 EP - 26 PB - Wiley Analytical Science CY - Weinheim AN - OPUS4-59600 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heilmann, V. A1 - Spitzer, S. A1 - Dufaud, O. A1 - Hohenberger, M. A1 - Jankuj, V. A1 - Prodan, M. A1 - Zakel, S. T1 - European round robin on safety characteristics of hybrid mixtures from vapors and dusts N2 - As part of the development of a new standard testing procedure, a round robin study was conducted by six participating laboratories. This study involved the measurement of both the maximum explosion pressure and the maximum rate of pressure rise for hybrid mixtures comprising dust and vapor. Measurements were performed using a modified 20L-sphere. The primary objective of this collaborative effort was to assess the accuracy, reliability, and consistency of analytical and measurement methods across multiple laboratories, thereby increasing confidence in the obtained results. The method and protocol were developed as part of the NEX-HYS project and documented in a technical specification by the German Institute for Standardization Registered Association (DIN). The study revealed that precise pre-ignition pressure rise (PIPR) measurements and the use of a leak-free test apparatus significantly influenced the results of the measured maximum explosion pressure and maximum pressure rise rate. KW - Hybrid Explosions KW - Safety characteristics KW - Round robin KW - 20L-sphere PY - 2024 DO - https://doi.org/10.1016/j.jlp.2024.105273 SN - 0950-4230 VL - 88 SP - 1 EP - 5 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-59534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Studt, Peter T1 - Massenspektrometrische Strukturgruppenanalysen von Kohlenwasserstoffgemischen (Schmierölen) N2 - Das Prinzip der Massenspektrometrie wird kurz erläutert. Anwendungsbereich und Grenzen der massenspektrometrischen Strukturuntersuchung werden am Beispiel von Massenspektren reiner Kohlenwasserstoffe demonstriert. Die Strukturgruppenanalyse von Mineralölen - Fragmentpeak-Methode, Molekülpeak-Methode - wird beschrieben. KW - Massenspektrometrie KW - Strukturuntersuchung KW - Kohlenwasserstoffe KW - Strukturgruppenanalyse KW - Mineralöle KW - Fragmentpeak-Methode KW - Molekülpeak-Methode PY - 1970 SN - 0036-6218 IS - 4 SP - 175 EP - 180 PB - Konradin CY - Stuttgart AN - OPUS4-59693 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chazeau, E. A1 - Fabre, C. A1 - Privat, M. A1 - Godard, A. A1 - Racoeur, C. A1 - Bodio, E. A1 - Busser, B. A1 - Wegner, Karl David A1 - Sancey, L. A1 - Paul, C. A1 - Goze, C. T1 - Comparison of the In Vitro and In Vivo Behavior of a Series of NIR-II-Emitting Aza-BODIPYs Containing Different Water-Solubilizing Groups and Their Trastuzumab Antibody Conjugates N2 - The development of new fluorescent organic probes effective in the NIR-II region is currently a fast-growing field and represents a challenge in the domain of medical imaging. In this study, we have designed and synthesized an innovative series of aza-boron dipyrromethenes emitting in the NIR-II region. We have investigated the effect of different water-solubilizing groups not only on the photophysical properties of the compounds but also on their in vitro and in vivo performance after bioconjugation to the antibody trastuzumab. Remarkably, we discovered that the most lipophilic compound unexpectedly displayed the most favorable in vivo properties after bioconjugation. This underlines the profound influence that the fluorophore functionalization approach can have on the efficiency of the resulting imaging agent. KW - NIR-II KW - In vivo imaging KW - Fluorescence KW - Spectroscopy KW - Antibody conjugates PY - 2024 DO - https://doi.org/10.1021/acs.jmedchem.3c02139 SN - 1520-4804 VL - 67 IS - 5 SP - 3679 EP - 3691 PB - ACS Publications CY - Washington, DC AN - OPUS4-59607 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lu, Xin A1 - Hicke, Konstantin A1 - Krebber, Katerina T1 - Distributed acoustic sensing to monitor ground motion/movement at multi-frequency bands N2 - A novel distributed acoustic sensing technique is proposed that exploits both phase and amplitude of the Rayleigh backscattered light to quantify the environmental variation. The system employs a wavelength-scanning laser and an imbalanced Mach-Zehnder interferometer to acquire the reflection spectra and the phase of the detected light, respectively. Fading-free and low-frequency measurements are realized via the crosscorrelation of the reflection spectra. The discrete crosscorrelation is used to circumvent the nonlinear frequency sweeping of the laser. Based on the phase of the backscattered light, it is possible to quantify fast environmental variations. The whole system requires no hardware modification of the existing system and its functionality is experimentally validated. The proposed system has the potential to monitor ground motion/movement at very low frequency band like subsidence around mining areas and at high frequency band like earthquakes and vibrations induced by avalanches. KW - Distributed acoustic sensing KW - DAS KW - Distributed fiber optic sensing KW - Ground motion detection KW - Subsidence monitoring PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596129 DO - https://doi.org/10.1109/JLT.2024.3358495 VL - 42 IS - 18 SP - 1 EP - 8 PB - Optical Society und IEEE Photonics Society AN - OPUS4-59612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilrich, Thomas A1 - Wilrich, Cordula T1 - Nachbarklage gegen einen Sauerstofftank N2 - Technische Regeln im Arbeitsschutz – wie TRBS für die Betriebssicherheitsverordnung und TRGS für die Gefahrstoffverordnung – sind nicht zwingendes Recht, sondern konkretisierende Empfehlungen mit Vermutungswirkung. In Gerichtsurteilen werden sie eher selten herangezogen. Wie diese – und Branchenregelungen von Verbänden – von der Rechtsprechung diskutiert werden, zeigt ein Urteil des Verwaltungsgerichts Münster. KW - Arbeitsschutz KW - Betriebssicherheitsverordnung KW - Branchenregelung KW - Gefahrstoffverordnung KW - Nachbarklage KW - Sauerstofftank KW - Sicherheitsabstand KW - TRBS KW - TRGS KW - Anlagensicherheit PY - 2024 UR - https://beprdigital.de/ce/nachbarklage-gegen-einen-sauerstofftank-1/detail.html DO - https://doi.org/10.37307/j.2365-7634.2024.01.12 SN - 2199-7330 IS - 1 SP - 45 EP - 47 PB - Erich Schmidt Verlag (ESV) CY - Berlin AN - OPUS4-59614 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard T1 - Trinamic TMCL IOC for exposing Trinamics motor controllers to EPICS CA N2 - Trinamic TMCL IOC is a Python package designed for controlling stepper motors connected to a Trinamic board using the TMCL language (all boards supported by PyTrinamic should now work, has been tested on the TMCM 6110 and the TMCM 6214). Since it is implementing the TMCL protocol, it should be easy to adapt to other Trinamic motor controller boards. This package assumes the motor controller is connected over a machine network via a network-to-serial converter, but the underlying PyTrinamic package allows for other connections too. This allows the control of attached motors via the EPICS Channel-Access virtual communications bus. If EPICS is not desired, plain Pythonic control via motion_control should also be possible. An example for this will be provided in the example.ipynb Jupyter notebook. This package leverages Caproto for EPICS IOCs and a modified PyTrinamic library for the motor board control, and interfaces between the two via an internal set of dataclasses. Configuration for the motors and boards are loaded from YAML files (see tests/testdata/example_config.yaml). The modifications to PyTrinamic involved extending their library with a socket interface. This was a minor modification that should eventually find its way into the official package (a pull request has been submitted). KW - Instrumentation KW - Motor controller KW - EPICS KW - Channel access KW - Instrument control KW - Laboratory automation PY - 2024 DO - https://doi.org/10.5281/zenodo.10792593 PB - Zenodo CY - Geneva AN - OPUS4-59624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena T1 - Hybrid measurement technique for defect characterisation in wide bandgap semiconductors N2 - Climate change and increasing demand for electricity require the use of power electronics based on new wide bandgap (WBG) compound semiconductors. Power electronics devices are used in numerous application areas to control and convert electric energy. These may include generation and distribution of renewable energy for green hydrogen, electrification of transport or 5G communication. WBG electronics have much higher efficiency than the silicon-based ones and can operate at higher power densities, voltages, temperatures and switching frequencies with low energy losses. However, defects in the semiconductors can considerably affect the performance of power electronic devices or make their operation even impossible. The presentation will show the application of spectroscopic and imaging ellipsometry as well as white light interference microscopy for defect characterisation in SiC, GaN and Ga2O3 over a wide wavelength range. We used parameterized modelling of ellipsometric transfer parameters to determine the dielectric properties of bulk materials and thin layers. Imaging ellipsometry offers more information and is an advanced variant of optical microscopy, combining the lateral resolution of optical microscopy with the extreme sensitivity to surface and interface effects of ellipsometry. Surface topography and morphology of different types of defects were additionally investigated with imaging white light interference microscopy. Modern electronic thin film components require complex surface analysis methodologies and hybrid metrology. Hybrid measurement techniques enable fast and non-destructive traceable characterisation of thin film compound semiconductors as well as accurate detection and identification of defects. This methodical approach leads to a better understanding of the materials themselves and of the defect formation mechanisms during manufacturing. This work aims to enable highly reproducible manufacturing of compound semiconductor power electronics as well as operation monitoring to ensure failure-safety of electronic systems in power electronic devices. T2 - Abteilungskolloquium 2023, BAM CY - Berlin, Germany DA - 09.02.2023 KW - Spectroscopic and imaging ellipsometry KW - White light interference microscopy KW - Wide bandgap semiconductors KW - Surface analysis, PY - 2023 AN - OPUS4-59443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kornev, Roman A1 - Gornushkin, Igor B. A1 - Shabarova, Lubov A1 - Kadomtseva, Alena A1 - Mochalov, Georgy A1 - Rekunov, Nikita A1 - Romanov, Sergey A1 - Medov, Vitaly A1 - Belousova, Darya A1 - Maleev, Nikita T1 - Plasma-Chemical Disposal of Silicon and Germanium Tetrachlorides Waste by Hydrogen Reduction N2 - The processes of hydrogen reduction of silicon and germanium chlorides under the conditions of high-frequency (40.68 MHz) counteracted arc discharge stabilized between two rod electrodes are investigated. The main gas-phase and solid products of plasma-chemical transformations are determined. Thermodynamic analysis of SiCl4 + H2 and GeCl4 + H2 systems for optimal process parameters was carried out. Using the example of hydrogen reduction of SiCl4 by the method of numerical modeling, gas-dynamic and thermal processes for this type of discharge are investigated. The impurity composition of gas-phase and solid reaction products is investigated. The possibility of single-stage production of high-purity Si and Ge mainly in the form of compact ingots, as well as high-purity chlorosilanes and trichlorogermane, is shown. KW - High-frequency arc discharge KW - Hydrogen reduction KW - Silicon chlorides KW - Germanium chlorides PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594454 DO - https://doi.org/10.3390/sci6010001 VL - 6 IS - 1 SP - 1 EP - 12 PB - MDPI AG AN - OPUS4-59445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Dell'Avvocato, Giuseppe A1 - Gohlke, Dirk A1 - Palumbo, Davide A1 - Galietti, Umberto T1 - Quantitative evaluation of the welded area in Resistance Projection Welded (RPW) thin joints by pulsed laser thermography N2 - A semi-automatic thermographic procedure for the assessment of the welded area of resistance projection welded joints has been developed. Currently, to assess the quality of RPW joints destructive tests are used and the more commonly used non-destructive technique is the ultrasonic one. The possibility for a quantitative evaluation of the welded area by thermographic technique has been proved by means of an innovative procedure applied on steel RPW joints with ‘as it’ surface conditions. Measurements obtained by thermography and ultrasound have been compared, to verify the developed procedure. T2 - Thermosense: Thermal Infrared Applications XLIV, CY - Orlando, USA DA - 03.04.2022 KW - Nondestructive evaluation KW - Ultrasonics KW - Contact area PY - 2022 DO - https://doi.org/10.1117/12.2618806 VL - 12109 SP - 1 EP - 14 PB - SPIE AN - OPUS4-59380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grundmann, Jana A1 - Ermilova, Elena A1 - Hertwig, Andreas A1 - Klapetek, Petr A1 - Pereira, Silvania F. A1 - Rafighdoost, Jila A1 - Bodermann, Bernd T1 - Optical and Tactile Measurements on SiC Sample Defects N2 - The different defect types on SiC samples are measured with various measurement methods including optical and tactile methods. The defect types investigated include particles, carrots and triangles and they are analyzed with imaging ellipsometry, coherent Fourier scatterometry and atomic force microscopy. Each of these methods measures different properties of the defects and they all together contribute to a complete analysis. T2 - SMSI 2023 - Sensor and Measurement Science International CY - Nuremberg, Germany DA - 08.05.2023 KW - Defects KW - Silicon carbide KW - Imaging ellipsometry KW - Atomic force microscopy KW - Coherent Fourier scatterometry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593397 SN - 978-3-9819376-8-8 DO - https://doi.org/10.5162/SMSI2023/D5.2 VL - 2023/D5 SP - 233 EP - 234 PB - AMA Service CY - Wunstorf AN - OPUS4-59339 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena T1 - Imaging spectroscopic ellipsometry for investigation of energy materials and materials for nano-electronics N2 - Ellipsometry is a very powerful tool used for accurate material investigation in a wide wavelength range. It is a non-destructive and fast method. Imaging ellipsometry as a combination of optical microscopy and ellipsometry enables spatially resolved measurements when determining the layer thickness and dielectric properties of thin layers. It is known for its high polarisation sensitivity and high contrast for the surface structures. In this contribution we show the application of the imaging ellipsometry for detection of defects in energy materials and quality validation of possible reference materials for nano-electronics. Defects in wide bandgap semiconductors, in homoepitaxial SiC and heteroepitaxial GaN layers on transparent SiC substrates, can be successfully detected and classified by means of imaging ellipsometry. Correlation of imaging ellipsometry results with results from complementary techniques such as white light interference microscopy as well as atomic force microscopy contribute to understanding of surface topography and defect formation mechanisms. We discuss the potential of different methods for analysing ellipsometric map data for monitoring the defect densities. Electric properties of materials at the nanoscale can be investigated by means of scanning probe microscopy methods such as scanning microwave microscopy and conductive atomic force microscopy. However, development of new robust and easy-to-use calibration methods and calibration standards is essential to increase the traceability of these methods and allow their broad application in industry. We show how imaging spectroscopic ellipsometry can be used for development and monitoring of processing quality of patterned reference samples based on indium tin oxide (ITO) layer with different thickness and conductivity. T2 - 12th Workshop on Spectroscopic Ellipsometry (WSE) CY - Prague, Czech Republic DA - 18.09.2023 KW - Ellipsometry KW - Thin Films KW - Transparent Conductive Oxides KW - Energy materials KW - White light interference microscopy KW - Nanoelectronics KW - Wide-bandgap semiconductors PY - 2023 AN - OPUS4-59340 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bayerlein, Bernd A1 - Schilling, Markus A1 - Birkholz, Henk A1 - Jung, Matthias A1 - Waitelonis, Jörg A1 - Mädler, Lutz A1 - Sack, Harald T1 - PMD Core Ontology: Achieving semantic interoperability in materials science N2 - Knowledge representation in the Materials Science and Engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant (consistent) and variant (context-specific) knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific. In this paper, an approach how to maintain a comprehensive MSE-centric terminology composing a mid-level ontology–the Platform MaterialDigital Core Ontology (PMDco)–via MSE community-based curation procedures is presented. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics. Additionally, it demonstrates how the PMDco lowers development and integration thresholds. Moreover, the research highlights how to fuel it with real-world data sources ranging from manually conducted experiments and simulations with continuously automated industrial applications. KW - Ontology KW - Materials science and engineering KW - Knowledge representation KW - Reproducibility KW - Semantic interoperability KW - Semantic data integration PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-592948 DO - https://doi.org/10.1016/j.matdes.2023.112603 SN - 0264-1275 VL - 237 SP - 1 EP - 12 PB - Elsevier CY - Amsterdam AN - OPUS4-59294 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghasem Zadeh Khorasani, Media T1 - Federated SHM: a Novel Collaborative ML Approach to Overcome Data Scarcity and Data Privacy Concerns in StructuralHealth Monitoring N2 - The deployment of machine learning (ML) and deep learning (DL) in structural health monitoring (SHM) faces multiple challenges. Foremost among these is the insufficient availability of extensive high-quality data sets essential for robust training. Within SHM, high-quality data is defined by its accuracy, relevance, and fidelity in representing real-world structural scenarios (pristine as well as damaged). Although methods like data augmentation and creating synthetic data can add to datasets, they frequently sacrifice the authenticity and true representation of the data. Sharing real-world data encapsulating true structural and anomalous scenarios offers promise. However, entities are often reluctant to share raw data, given the potential extraction of sensitive information, leading to trust issues among collaborating entities. Our study introduces a novel methodology leveraging Federated Learning (FL) to navigate these challenges. Within the FL framework, models are trained in a decentralized manner across different entities, preserving data privacy. In our research, we simulated several scenarios and compared them to traditional local training methods. Employing guided wave (GW) datasets, we distributed the data among different parties (clients) using IID (independent, identically distributed or in other words, statistically identical) mini batches of dataset, as well as non-IID configurations. This approach mirrors real-world data distribution among varied entities, such as hydrogen refueling stations. In our methodology, the initial round involves individualized training for each client using their unique datasets . Subsequently, the model parameters are sent to the FL server, where they are averaged to construct a global model. In the second round, this global model is disseminated back to the clients to aid in predictive tasks. This iterative process continues for several rounds to reach convergence. Our findings distinctly highlight the advantages of FL over localized training, evidenced by a marked improvement in prediction accuracy . This research underscores the potential of FL in GW-based SHM, offering a remedy to similar challenges tied to data scarcity in other SHM approaches and paving the way for a new era of collaborative, data-centric monitoring systems. T2 - QI Digital Forum CY - Berlin, Germany DA - 10.10.2023 KW - Machine learning KW - Federated learning KW - Structural health monitoring KW - Artificial intelligence KW - Hydrogen safety KW - Data privacy PY - 2023 AN - OPUS4-59415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Isleyen, Alper A1 - Can, Suleyman Z. A1 - Cankur, Oktay A1 - Engin, Betul Ari A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Horvat, Milena A1 - Jacimovic, Radojko A1 - Zuliani, Tea A1 - Fajon, Vesna A1 - Jotanovic, Aida A1 - Gaževic, Luka A1 - Milosevic, Milena A1 - Ochsenkuehn–Petropoulou, Maria A1 - Tsopelas, Fotis A1 - Lymberopoulou, Theopisti A1 - Tsakanika, Lamprini-Areti A1 - Serifi, Olga A1 - Ochsenkuehn, Klaus M. A1 - Bulska, Ewa A1 - Tomiak, Anna A1 - Kurek, Eliza A1 - Cakılbahçe, Zehra A1 - Aktas, Gokhan A1 - Altuntas, Hatice A1 - Basaran, Elif A1 - Kısacık, Barıs A1 - Gumus, Zeynep T1 - Certification of the total element mass fractions in UME EnvCRM 03 soil sample via a joint research project N2 - Soil certified reference material (CRM), UME EnvCRM 03 was produced by a collaborative approach among national metrology institutes, designated institutes and university research laboratories within the scope of the EMPIR project: Matrix Reference Materials for Environmental Analysis. This paper presents the sampling and processing methodology, homogeneity, stability, characterization campaign, the assignment of property values and their associated uncertainties in compliance with ISO 17034:2016. The material processing methodology involves blending a natural soil sample with a contaminated soil sample obtained by spiking elemental solutions for 8 elements (Cd, Co, Cu, Hg, Ni, Pb, Sb and Zn) to reach the level of warning risk monitoring values specified for metals and metalloids of soils in Europe. Comparative homogeneity and stability test data were obtained by two different institutes, ensuring the reliability and back up of the data. The certified values and associated expanded uncertainties for the total mass fractions of thirteen elements (As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sb, V and Zn) are established. The developed CRM can be used for the development and validation of measurement procedures for the determination of the total mass fractions of elements in soil and also for quality control/assurance purposes. The developed CRM is the first example of a soil material originating from Türkiye. KW - Total element content KW - Soil KW - CRM KW - Certification KW - Environmental pollution monitoring PY - 2024 DO - https://doi.org/10.1007/s00769-024-01597-8 SN - 1432-0517 VL - 29 SP - 293 EP - 301 PB - Springer Science and Business Media LLC AN - OPUS4-59954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lohrke, Heiko T1 - Robotic Measurement System Concept for Greenhouse Gas Tomography in Wastewater Treatment Plants N2 - This paper introduces a conceptual framework for a greenhouse gas (GHG) measurement system designed for wastewater treatment plants (WWTPs). The emphasis is on accurate gas tomography measurements of emissions, crucial for national emission assessments. The proposed system is movable, semi-autonomous, and employs a combination of ground and air robots equipped with integral remote gas sensors and in-situ sensors. The proposed two/two configuration ensures comprehensive coverage of WWTPs, overcoming obstacles. The system concept lays the foundation for future implementation and evaluation, addressing the need for enhanced understanding of GHG emissions from WWTPs. T2 - 39th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Siófok, Hungary DA - 26.09.2023 KW - Remote Gas Sensing KW - Greenhouse Gas Emissions KW - Robot-based Emission Measurements KW - Semi-autonomous Sensor Networks KW - Gas Tomography PY - 2023 AN - OPUS4-58883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. A1 - Kornev, R. A1 - Bulanov, A. A1 - Ermakov, A. T1 - Laser-Induced Dielectric Breakdown as a Novel Method for Obtaining Isotopically Enriched Nanoscale Substances N2 - The possibility of obtaining high-purity, isotopically modified and nanostructured elemental substances 29Si, 98Mo, and 100Mo, as well as 98Mox10By compounds from volatile halides under conditions of laser optical breakdown of a pulsed Nd:YAG laser is shown. Currently, research in the field of developing new methods for obtaining high-purity, isotopically modified and nanostructured substances is being actively conducted. Interest in Si and Mo combining these forms has noticeably increased. In nuclear medicine, 29Si-enriched nanoparticles can be used as contrast agents in magnetic resonance imaging (MRI), and 98Mo and 100Mo isotopes can be used to obtain the unstable 99mTc radioisotope. These applications do not require large amounts of isotopically modified Si and Mo. Their obtaining belongs to the problems of small chemistry. When obtaining isotopically modified Si and Mo, it is expedient to use their volatile fluorides, for which technologies of isotope enrichment and deep purification are well developed. These halides have high chemical and thermal stability; therefore, plasma-chemical methods based on the plasma of a pulsed discharge generated by laser breakdown can be promising for separating 29Si, 98Mo, and 100Mo from them. Laser breakdown in H2+Ar+SiF4 and H2+Ar+MoF6 mixtures in various stoichiometric ratios in the pressure range 30–760 Torr was carried out using a pulsed Nd:YAG laser. The pulse duration at a wavelength of 1064 nm was 15 ns, the repetition rate was 5 Hz. A pulse energy of 800 mJ was focused by a lens with a focal length of 5 cm. The energy density at the focus was 26 J/cm3 . It has been shown that when using a mixture based on 29SiF4, the sample contains a 29Si crystalline phase with an average grain size of 30–50 nm (Fig. 1a). When using a mixture based on 98MoF6, the sample contains a 98Mo crystalline phase with an average grain size of 70–100 nm (Fig. 1b). In this type of gas discharge, the possibility of forming superhard materials, isotopically modified molybdenum borides, was also studied. These substances in the form of nanosized particles have improved tribological properties. After ablation of metallic Mo in the H2 + BF3 mixture, the main phase was MoB2 in the form of a nanodispersed powder with an average grain size of 100 nm (Fig. 1c) [1]. A technique for modeling gas-dynamic and thermal conditions in a low-temperature chemically active plasma induced by laser breakdown is proposed. Using computational experiments, the features of gas mixture heating and the formation of nanoparticles in the LIBS reactor were studied T2 - 17the International Conference on Laser Applications in Life Sciences CY - Mugla, Turkey DA - 15.10.2023 KW - Laser induced plasma KW - Chemical vapor deposition KW - Isotopically enriched nanomaterials PY - 2023 AN - OPUS4-58888 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Gornushkin, Igor B. A1 - Kornev, R. A. A1 - Shabarova, L. V. A1 - Ermakov, A. A. A1 - Mochalov, G. M. A1 - Rekunov, N. V. A1 - Medov, V. A. A1 - Chaschina, A. D. A1 - Kalinina, A. A. T1 - Features of Plasma-Chemical Hydrogen Reduction of Volatile Silicon and Germanium Chlorides in RF-arc Discharge N2 - The processes of hydrogen reduction of silicon and germanium chlorides under the conditions of radio-frequency (40.68 MHz) counteracted arc discharge stabilized between two rod electrodes were investigated. The main gas-phase and solid products of plasma-chemical transformations were determined. Thermodynamic analysis of SiCl4 + H2 and GeCl4 + H2 systems was carried out. It is shown that under the implemented experimental conditions, equilibrium components of the products are established. The detected spectra of chemical activity were studied, which gave reason to assume that the molecular mechanism of the hydrogen reduction process is the main one. The impurity composition of gas-phase and solid reaction products was investigated. The possibility of single-stage production of high-purity Si and Ge mainly in the form of compact ingots, as well as high-purity chlorosilanes and trichlorogermane, was shown. KW - RF-arc discharge KW - Hydrogen reduction KW - Silicon chloride KW - Germanium chloride KW - Thermodynamic KW - Silicon KW - Germanium PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588909 DO - https://doi.org/10.20944/preprints202311.1412.v1 SP - 1 EP - 14 PB - MDPI CY - Basel AN - OPUS4-58890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - Wirbelstromprüfung für die additive Fertigung N2 - Überblick über die derzeitige Entwicklungen für das Online-Monitoring additiver Fertigungsverfahren für metallische Werkstoffe mittels der Wirbelstromprüfung. Hierbei wird eine Einführung in die Wirbelstromprüfung gegeben sowie erste Entwicklungen hinsichtlich eines Online-Monitoring thematisiert. T2 - BAM Akademie: Qualitätssicherung in der additiven Fertigung CY - Online meeting DA - 26.10.2023 KW - Wirbelstromprüfung KW - Additive Fertigung KW - Online Monitoring PY - 2023 AN - OPUS4-58917 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - The Dark Side of Science (2023 edition) N2 - An introductory lecture on the Dark Side of Science; what it is, why it exists, and what can be done to fight it. This lecture illuminates the increasing prevalence of fraudulent scientific work (e.g. faked data, manipulated images, paper mills) with plenty of examples and sources. The second section expands on the driving forces that caused this phenomenon to emerge, largely driven by pressures from management, peers and the researcher themselves. The third section expands on methods and tools that can be used to educate and arm oneself against this phenomenon. The 2023 edition includes new examples of larger fraudulent bodies of work emerging, and the problems posed by the arrival of LLMs. T2 - Lecture series on "Information management" CY - Berlin, Germany DA - 27.11.2023 KW - Research fraud KW - Scientific misconduct KW - Paper mills KW - Metrics-driven science KW - Image manipulation KW - Faked research PY - 2023 AN - OPUS4-58925 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Rühl, Isabel A1 - Westphalen, Tanja A1 - Simon, Fabian A1 - von der Au, Marcus A1 - Cossmer, Antje A1 - Meermann, Björn T1 - Investigating the uptake and fate of per- and polyfluoroalkylated substances (PFAS) in bean plants (Phaseolus vulgaris): comparison between target MS and sum parameter analysis via HR-CS-GFMAS N2 - AbstractIn this study, we present a screening method based on molecular absorption spectrometry to study PFAS uptake and fate in plants. To evaluate the suitability of this method we analyzed plant extracts with molecular absorption spectrometry (MAS) as well as liquid chromatography–tandem mass spectrometry (LC–MS/MS) for mass balance studies (w(F)). French bean plants (Phaseolus vulgaris) were grown on soil spiked using eight PFAS substances that vary in chain length and functional group composition. Specifically, these include three short-chained (C4–C5), five long-chained (C7–C10) carboxylic acids, one sulfonic acid and one sulfonic amide moieties. To investigate substance-specific PFAS uptake systematically, PFAS were spiked as single substance spike. Additionally, we studied one mixture of the investigated substances in equal proportions regarding w(F) and four PFAS mixtures of unknown composition. After 6 weeks, the plants were separated into four compartments. We analyzed the four compartments as well as the soil for extractable organically bound fluorine (EOF) by high resolution-continuum source-graphite furnace-molecular absorption spectrometry (HR-CS-GFMAS) as well as for sum of ten target-PFAS by LC–MS/MS. All three short-chained PFAS perfluorobutanoic acid (PFBA), perfluorobutanoic sulfonic acid (PFBS) and perfluoropentanoic acid (PFPeA) were determined in high concentrations mainly in the fruits of the investigated plants while long-chained PFAS perfluorononanoic acid (PFNA) and perfluorodecanoic acid (PFDA) were mainly determined in roots. PFBS was determined in remarkably high concentrations in leaves compartment by both quantification methods. Overall, comprehensive results of single substance spikes were in good agreement for both methods except for a few cases. Hence, two phenomena were identified: for mixed PFAS spikes of unknown composition huge differences between EOF and sum of target PFAS were observed with systematically higher EOF values. Overall, both methods indicate comparable results with MS being more reliable for known PFAS contamination and MAS being more valuable to identify PFAS exposure of unknown composition. Graphical Abstract KW - Pollution PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589394 DO - https://doi.org/10.1186/s12302-023-00811-7 VL - 35 IS - 104 SP - 1 EP - 13 PB - Springer Science and Business Media LLC AN - OPUS4-58939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bilsel, M. A1 - Gökçen, T. A1 - Binici, B. A1 - Isleyen, A. A1 - Piechotta, Christian A1 - Kar-wai, A. A1 - Krylov, A. A1 - Miheeva, A. A1 - Beliakov, M. A1 - Palagina, M. A1 - chenko, Irina Tka A1 - Perkola, N. A1 - Lewin, M. A1 - Hua, T. T1 - High polarity analyte(s) in aqueous media: determination of L-PFOA and L-PFOS in ground water N2 - The CCQM-K156 comparison was coordinated by TUBITAK UME on behalf of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) for National Measurement Institutes (NMIs) and Designated Institutes (DIs) which provide measurement services in organic analysis under the 'Comité International des Poids et Mesures' Mutual Recognition Arrangement (CIPM MRA). Perfluoro alkyl substances (PFAS) such as PFOS and PFOA have been used in numerous industrial applications and products. Because of their high stability and resistance to biodegradation, atmospheric photooxidation, direct photolysis and hydrolysis, they are extremely persistent in the environment. The European Union (EU) Water Framework Directive lists PFOS as a priority hazardous substance that poses a significant risk to the aquatic environment. The use of PFOS-containing Aqueous Film-Forming Foams (AFFFs) has been banned since June 2011 in the EU. As relatively water-soluble, effectively non-degradable compounds, PFOS and PFOA migrate to ground water. They are not removed in the conventional drinking water treatment, and therefore cause health risks in polluted areas. The EU Drinking Water Directive and the European Commission has proposed a limit value of 100 ng/L for the sum of 20 PFAS, including PFOS and PFOA. This study provides the means for assessing measurement capabilities for determination of high polarity measurands in a procedure that requires extraction, clean-up, analytical separation and detection. Successful participation in CCQM-K156 demonstrates measurement capabilities in determining mass fraction of organic compounds, with a molecular mass of 200 g/mol to 700 g/mol, having high polarity pKow -2, in a mass fraction range from 0.5 ng/kg to 500 ng/kg in aqueous media. Nine NMIs and DIs participated in the CCQM-K156 key comparison. Seven institutes reported their results. SPE was applied in the sample pre-treatment and LC-MS was applied for detection. All participating laboratories applied isotope dilution mass spectrometry (IDMS) techniques for quantification. Participants established the metrological traceability of their results using certified reference materials (CRMs) from NMIs with stated traceability; where commercially available high purity materials were used the purity was determined in-house. The CCQM-K156 results for L-PFOA and L-PFOS range from 2.75 ng/kg to 5.50 ng/kg with a % RSD of 19.5 % for L-PFOA and from 2.04 ng/kg to 4.45 ng/kg with a % RSD of 21.3 % for L-PFOS. The KCRV was assigned using a Hierarchical Bayesian Random Effects Model (HB REM) estimator from the values reported by six of the participants. One participant result of L-PFOS and one result of L-PFOA were excluded from the KCRV for technical reasons. The KCRV was 4.9 ng/kg ± 0.4 ng/kg for L-PFOA and 3.8 ng/kg ± 0.4 ng/kg for L-PFOS. The six institutes that were included in the assignment of consensus KCRV all agreed within their standard uncertainties. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - PFAS KW - Surface water KW - ILC KW - CCQM PY - 2022 DO - https://doi.org/10.1088/0026-1394/59/1A/08016 VL - 59 IS - 1A SP - 1 EP - 3 PB - IOP Publishing AN - OPUS4-58941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blotevogel, J. T1 - Thermal Destruction of PFAS N2 - Thermal treatment processes are currently the only full-scale option for thedestruction of per- and polyfluoroalkyl substances (PFAS) in large waste streams. While all organic molecules including PFAS are susceptible to thermal destruction, their decomposition rates are controlled by process variables such as temperature, reaction atmosphere, and residence time. Concerns exist about the formation of products of incomplete destruction and their emission from hazardous waste incinerators. This talk will summarize the current stateof-the-art of thermal PFAS destruction, identify research needs, and showcase future research designed to address critical knowledge gaps. T2 - Department of Defense's (DoD) Energy and Environment Innovation Symposium CY - Washington DC, USA DA - 28.11.2023 KW - Thermal treatment KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Remediation PY - 2023 AN - OPUS4-58974 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - PFAS analytics and their relation to PFAS remediation N2 - Per- and polyfluoroalkyl substances (PFAS) are a large group of more than 10,000 anionic, cationic, zwitterionic or neutral organofluorine surfactants. As a result of continuous and prolific use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil, groundwater and surface water. While liquid chromatography tandem mass spectrometry (LC-MS/MS) is commonly used technique to characterize targeted PFAS in environmental samples, there are more than 10,000 different PFAS known, which have various headgroups and properties. Therefore, several analytical techniques are available to analyse various groups or pools of PFAS or “all” PFAS as a sum parameter. Current decontamination strategies of PFAS-burdened soils mainly consist of adsorption methods using adsorbents for fixation of PFAS in the ground. A second option is the utilization of a “pump and treat” process, cycling polluted soils through a washing plant leading to the concentration of the pollutants in the fine fraction. Both approaches are cost-intensive and not intended for the direct decomposition of all PFAS contaminants. Hence, there is a great demand for innovative developments and chemical treatment technologies, dealing with new strategies of tackling the PFAS problem. Previously, mechanochemical treatment of polychlorinated organic compounds in soils showed an efficient dechlorination. Thus, we investigated mechanochemical treatment of PFAS contaminated soils with various additives in a ball mill and analyzed the PFAS defluorination with gas chromatography mass spectrometry (GC-MS) and liquid chromatography tandem mass spectrometry (LC-MS/MS), respectively, as well es the fluoride mineralization by ion chromatography (IC) and fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy. T2 - International workshop of CAR-PFAS (Consortium for analysis and remediation of per- and polyfluoroalkyl substances) Japan CY - Tokyo, Japan DA - 17.10.2023 KW - Mechanochemical treatment KW - Per- and Polyfluoroalkyl substances (PFAS) KW - XANES spectroscopy KW - Soil PY - 2023 AN - OPUS4-58609 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reynolds, Merilie A. A1 - Kamber, Balz S. A1 - McKenna, Cora A. A1 - Oelze, Marcus A1 - Gleeson, Sarah A. T1 - Repeat, fast, and high-resolution mapping of fine-scale trace element distribution in pyrite and marcasite by LA-Q-ICP-MS with the Aerosol Rapid Introduction System (ARIS) N2 - AbstractThe minor and trace element composition of minerals provides critical insights into a variety of geological processes. Multi-element mapping by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is an important technique applied for this purpose and although the method is rapidly advancing, there remains a fundamental compromise between spatial resolution, detection limit, and experiment duration when using sequential mass analyzers. To address the limitation of limited analyte selection for high spatial resolution maps imposed by the sequential nature of typical quadrupole (Q)-ICP-MS, we tested the Aerosol Rapid Introduction System (ARIS) for repeat mapping of the same area. The ARIS is a high-speed transfer tubing system that reduces aerosol washout times, permitting resolution of individual pulses at 40–60 Hz. Here, the ARIS was tested not for pulse resolution but with novel operating conditions optimized to perform fast, high spatial resolution mapping of minor and trace element distribution in pyrite and marcasite. For this purpose, ablation was conducted with a 5 µm beam aperture, a repetition rate of 50 Hz, and a continuous stage scan speed of 40 µm s−1. For each LA-Q-ICP-MS map, data were acquired for six elements with an acquisition time of 20 ms per element. This deliberately reduced the individual pulse resolution of the ARIS but instead exploited the spatial resolution and sensitivity gains afforded by the high-laser repetition rate combined with efficient aerosol transfer. The new method successfully mapped trace elements at single to double-digit parts per million levels, and the maps reveal fine-scale zoning of trace elements with an effective x and y resolution of 5 µm, while white light interferometry showed that for each experiment, only ca. 1 µm of the sample was removed. Repeated mapping of the same area showed excellent correspondence not only between element concentrations in successive experiments but also in the shape, dimension, and location of regions of interest defined by concentration criteria. The very good repeatability of the elemental maps indicates that for studies requiring more analytes, successive mapping of additional elements is possible. By contrast with conventional very small spot (i.e., 5 µm) analysis, fast repetition rate and stage scan speed mapping avoids down-hole fractionation effects and minimizes accidental analysis of buried invisible inclusions. Compared to conventional LA-ICP-MS mapping, the method reduces the experiment time by 4–8 times. KW - Geochemistry and Petrology KW - Geophysics PY - 2023 DO - https://doi.org/10.2138/am-2022-8168 SN - 0003-004X VL - 108 IS - 1 SP - 18 EP - 30 PB - Mineralogical Society of America AN - OPUS4-59038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rieger, Philip A1 - Magnall, Joseph M. A1 - Gleeson, Sarah A. A1 - Oelze, Marcus T1 - Pyrite chemistry records a multistage ore forming system at the Proterozoic George Fisher massive sulfide Zn-Pb-Ag deposit, Mount Isa, Australia N2 - Trace element (TE) analysis of pyrite via LA-ICP-MS can be used to reconstruct the conditions of pyrite formation in complex mineral systems. The Carpentaria province in northern Australia is host to some of the world’s highest value Zn-Pb (+Ag, Cu) deposits. The genesis of many of these deposits is controversial, with competing models of single-vs. multi-stage ore formation. In this study, LA-ICP-MS data of paragenetically constrained pyrite from the George Fisher Zn-Pb-Ag deposit has been analysed to investigate the chemistry of different stages of ore formation. Pyrite from correlative unmineralized host rocks has also been analysed to investigate evidence of distal hydrothermal anomalism. All LA-ICP-MS data have been statistically evaluated (principal component analysis) and interpreted together with whole rock lithogeochemical data of the same samples. Pre-ore diagenetic pyrite is compositionally similar to other Proterozoic diagenetic pyrite, with some evidence of minor hydrothermal anomalism that with further analysis could help define distal alteration. Pyrite from the different ore stages are compositionally distinct, consistent with a multi-stage system. Ore stage 1 pyrite exceeds background contents of Co, Cu, Zn, As, Ag, Sb, Tl, and Pb and has elevated Co/Ni ratios, whereas only Ni and Co are above background abundances in ore stage 2 and 3 pyrite, of which only ore stage 3 pyrite has high Co/Ni ratios. Ore stage 1 pyrite has a similar composition to hydrothermal pyrite in the undeformed northern Carpentaria CD-type deposits and was likely syn-diagenesis. Ore stage 2 was syn-deformation, and resulted in replacement and recrystallization of pre-existing pyrite, and the expulsion of incompatible TEs. Ore stage 3 formed via a later Cu-Zn-Pb mineralizing event that resulted in a new geochemically distinct generation of Co-rich pyrite. Overall, this study demonstrates the value of paragenetically-constrained pyrite TE data for refining genetic models in complex sediment hosted mineral systems. KW - General Earth and Planetary Sciences PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590407 DO - https://doi.org/10.3389/feart.2023.892759 VL - 11 SP - 1 EP - 19 PB - Frontiers Media SA AN - OPUS4-59040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Melzer, Michael T1 - Die Etablierung des DCC im akkreditierten Kalibrierlabor im Rahmen von QI-Digital N2 - In diesem Beitrag soll die Etablierung von digitalen Kalibrierscheinen als maschineninterpretierbare Ergebnisberichte in akkreditierten Kalibrierlaboren, am Beispiel der Kalibrierung von Widerstandsthermometern nach DKD-R 5-1 aufgezeigt werden. Der DCC-Entwurf basiert auf dem von der PTB entwickelten DCC-Schema für XML-Formate. Vorrangig sollen folgende Aspekte bei der Umsetzung in akkreditierten Kalibrierlaboren beleuchtet werden: Angepasste digitale Workflows und Prozessdarstellungen; Harmonisierung von DCCs nach DKD-R 5-1; Entwicklung der IT-Infrastruktur (Middleware) zur automatisierten Generierung von DCCs; Erfahrungen aus der Pilotierung der DAkkS-eAttestation zum digitalen Nachweis der Akkreditierung; Praktische Umsetzung im Rahmen von QI-Digital. Dieses Qualitätswerkzeug soll im Gesamtkonzept von QI-Digital zum UseCase Wasserstofftankstelle kurz vorgestellt werden. T2 - 11. VDI-Fachtagung Messunsicherheit und Prüfprozesse 2023 CY - Erfurt, Germany DA - 14.11.2023 KW - Digitaler Kalibrierschein KW - Digitalisierung KW - QI-Digital PY - 2023 UR - www.vdi-wissensforum.de/02TA152023 AN - OPUS4-59042 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Melzer, Michael A1 - Nattuveettil, Keerthana A1 - Brunner, Nanine A1 - Thomas, Marcus T1 - DCC´s im Praxistest: Rückführung auf Knopfdruck N2 - Eine online Live-Vorführung des DCC Demonstrators zur automatisierten Erstellung und Auswertung eines maschinenlesbaren digitalen Kalibrierscheins zur metrologischen Rückführung eines Pt 100 Temperaturfühlers. Workflow: DCC Vorlage für Kalibrierungen nach DKD-R 5-1; DCC Middleware zur Aufnahme der auftragsbezogenen Metadaten und Einfügen aller Daten, inkl. der Messdaten, in die DCC Vorlage; Validierung des befüllten DCCs gegen das DCC-Schema; Siegelung des DCCs mit dem digitalen Akkreditierungssymbol; Übertragung an den DCC-Nutzer; nutzerseitige Verifizierung des elektronischen Siegels zur Sicherstellung von Authentizität, Integrität und Akkreditierung; direktes auslesen der Sensordaten mit Messunsicherheit basierend auf Herstellerspezifikationen; Einlesen und Auswerten des DCCs auf Knopfdruck, damit automatisierte Erstellung einer Kalibrierfunktion und entsprechende Korrektur der Sensordaten, automatisches Auslesen der temperaturabhängigen Messunsicherheit und Erweiterung um relevante Beiträge zum Erreichen der metrologischen Rückführbarkeit der Temperaturmessung; qualitätsgesicherte Konformitätsaussage des Prozesses auf Basis der so korrigierten Temperaturmesswerte und deren Unsicherheiten. T2 - Virtuelle und interaktive Praxiswerkstätten: "Digitale QI für Prüf- und Kalibrierlabore" CY - Online meeting DA - 30.11.2023 KW - Live Demonstration KW - Digitalisierung KW - Digitaler Kalibrierschein KW - Metrologische Rückführbarkeit PY - 2023 UR - https://www.qi-digital.de/hauptmenue/begleitforschung/praxiswerkstaetten AN - OPUS4-59048 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tsamos, Athanasios T1 - CNN Architectures for Image Processing. N2 - Deep Convolutional Neural Networks (DCNNs) and their applications in (XCT) data conditioning and automatic segmentation. A case study in Al-Si MMCs with synthetic training data. T2 - EUROLAB-D Tagung: KI im Prüflabor: Chancen und Herausforderungen von Künstlicher Intelligenz für akkreditierte Stellen CY - Berlin, Germany DA - 14.11.2023 KW - Automatic Segmentation KW - XCT KW - Artificial Intelligence KW - Synthetic Training Data PY - 2023 AN - OPUS4-59093 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Melzer, Michael T1 - The digitalization of force metrology N2 - The transfer of data for the metrological traceability of measurement results is currently taking place in the form of paper-based calibration certificates, mostly. Especially accredited metrology services providers are often bound to paper certificates by regulatory constrictions and sometimes lack of IT-infrastructure. This analog form of metrology data transfer, however, implies hands-on work, in particular for the certificate receiver, as its key values need to be translated into the device- and quality management (QM) system, manually. With thousands of certificates transferred from accredited calibration labs until the industrial regime, this binds a significant amount of human resources and is a well-known source of errors, thus constricting cost-effective and secure workflows. This contribution highlights the status of the advancing digital transformation in metrology, on the example of force calibration. Although this appealing initiative is to a large extend driven by German stakeholders, it currently evolves to extend across all Europe and far beyond. T2 - 39TH DANUBIA-ADRIA SYMPOSIUM ON ADVANCES IN EXPERIMENTAL MECHANICS CY - Siofok, Hungary DA - 26.09.2023 KW - Digitalisierung KW - Metrologische Rückführung KW - Digitaler Kalibrierschein PY - 2023 UR - https://das2023.hu/ AN - OPUS4-59027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Inostroza, Manuel A1 - Fernandez, Bárbara A1 - Aguilera, Felipe A1 - Layana, Susana A1 - Walter, Thomas R. A1 - Zimmer, Martin A1 - Rodríguez-Díaz, Augusto A1 - Oelze, Marcus T1 - Physical and chemical characteristics of active sulfur flows observed at Lastarria volcano (northern Chile) in January 2019 N2 - Molten sulfur is found in various subaerial volcanoes. However, limited records of the pools and flows of molten sulfur have been reported: therefore, questions remain regarding the physicochemical processes behind this phenomenon. A suite of new sulfur flows, some of which active, was identified at the Lastarria volcano (northern Chile) and studied using satellite imagery, in situ probing, and temperature and video recording. This finding provides a unique opportunity to better understand the emplacement mechanisms and mineral and chemical compositions of molten sulfur, in addition to gaining insight into its origin. Molten sulfur presented temperatures of 124–158°C, with the most prolonged sulfur flow reaching 12 m from the source. Photogrammetric tools permitted the identification of levees and channel structures, with an estimated average flow speed of 0.069 m/s. Field measurements yielded a total volume of 1.45 ± 0.29 m3 of sulfur (equivalent to ∼2.07 tons) mobilized during the January 2019 event for at least 408 min. Solidified sulfur was composed of native sulfur with minor galena and arsenic- and iodine-bearing minerals. Trace element analysis indicated substantial enrichment of Bi, Sb, Sn, Cd, as well as a very high concentration of As (&gt;40.000 ppm). The January 2019 molten sulfur manifestations in Lastarria appear to be more enriched in As compared to the worldwide known volcanoes with molten sulfur records, such as the Shiretoko-Iozan and Poás volcanoes. Furthermore, their rheological properties suggest that the “time of activity” in events such as this could be underestimated as flows in Lastarria have moved significantly slower than previously thought. The origin of molten sulfur is ascribed to the favorable S-rich chemistry of fumarolic gases and changes in host rock permeability (fracture opening). Molten sulfur in Lastarria correlates with a peak in activity characterized by high emissions of SO2 and other acid species, such as HF and HCl, in addition to ground deformation. Consequently, molten sulfur was framed within a period of volcanic unrest in Lastarria, triggered by changes in the magmatic-hydrothermal system. The appearance of molten sulfur is related to physicochemical perturbations inside the volcanic system and is perhaps a precursor of eruptive activity, as observed in the Poás and Turrialba volcanoes. KW - General Earth and Planetary Sciences PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590331 DO - https://doi.org/10.3389/feart.2023.1197363 VL - 11 SP - 1 EP - 18 PB - Frontiers Media SA AN - OPUS4-59033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zhang, Tianyun T1 - Aufbau eines digitalen Zwillings für die mechanisierte Eisenbahnschienenprüfung für das Training von KI-Algorithmen N2 - Im Rahmen des Forschungsprojekts "Artificial Intelligence for Rail Inspection" (AIFRI) wird ein KI-Algorithmus entwickelt, um die Fehlererkennung bei der Auswertung von Schienenprüfungen zu verbessern. Der Prozess der mechanisierten Schienenprüfung wird analysiert und die Schienenfehler sowie Artefakte werden in einem digitalen Zwilling abgebildet, um in einem weiteren Schritt die automatische Fehlererkennung und Klassifizierung mit KI-Algorithmen trainieren zu können. Zu diesem Zweck werden Ultraschalldatensätze auf der Grundlage der Regelwerke und Informationen aus der Instandhaltung mit einer Simulationssoftware erstellt, die Anzeigen der verschiedenen Schienenschädigungen und Artefakte enthalten. Die Schienenfehler werden bei der Auswertung in Fehlerklassen eingeordnet, für das KI-Training priorisiert und auf Basis der von der DB Netz AG ausgewählten Informationen untersucht. Hierfür werden die Schienenfehler nach den für das KI-Training relevanten Merkmalen zerlegt und die Konfiguration der Parameter der Simulation entsprechend abgestimmt. Für die Grundstruktur des Datensatzes wird ein Schienenmodell mit einer Länge von einem Meter für die Simulation eingesetzt, auf dessen Basis alle bei der Schienenprüfung zu verwendenden Prüfköpfe für den jeweiligen Reflektortyp betrachtet werden. Die simulierten Daten werden auf einer Testschiene im Labormaßstab validiert. Mögliche Einflussparameter wie z. B. der Signal-Rausch-Abstand sowie die Fahrgeschwindigkeit werden in den Datensätzen herangezogen. Die Zusammenstellung eines Testdatensatzes mit lokal veränderlichen Einflussgrößen erfolgt aus den simulierten Daten unter Verwendung der skriptbasierten Programmierumgebung Python und Matlab. Das Projekt AIFRI wird im Rahmen der Innovationsinitiative mFUND unter dem Förderkennzeichen 19FS2014 durch das Bundesministerium für Digitales und Verkehr gefördert. T2 - Seminar des FA Ultraschallprüfung Konventionelle und innovative Anwendungen der Ultraschallprüfverfahren CY - Kassel, Germany DA - 14.11.2023 KW - Ultraschallprüfung KW - Simulation KW - Schienenprüfung PY - 2023 AN - OPUS4-59055 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Charmi, Amir A1 - Mustapha, Samir A1 - Yilmaz, Bengisu A1 - Heimann, Jan A1 - Prager, Jens T1 - A Machine Learning Based-Guided Wave Approach for Damage Detection and Assessment in Composite Overwrapped Pressure Vessels N2 - The applications of composite overwrapped pressure vessels (COPVs) in extreme conditions, such as storing hydrogen gases at very high pressure, impose new requirements related to the system's integrity and safety. The development of a structural health monitoring (SHM) system that allows for continuous monitoring of the COPVs provides rich information about the structural integrity of the component. Furthermore, the collected data can be used for different purposes such as increasing the periodic inspection intervals, providing a remaining lifetime prognosis, and also ensuring optimal operating conditions. Ultimately this information can be complementary to the development of the envisioned digital twin of the monitored COPVs. Guided waves (GWs) are preferred to be used in continuous SHM given their ability to travel in complex structures for long distances. However, obtained GW signals are complex and require advanced processing techniques. Machine learning (ML) is increasingly utilized as the main part of the processing pipeline to automatically detect anomalies in the system's integrity. Hence, in this study, we are scrutinizing the potential of using ML to provide continuous monitoring of COPVs based on ultrasonic GW data. Data is collected from a network of sensors consisting of fifteen Piezoelectric (PZT) wafers that were surface mounted on the COPV. Two ML algorithms are used in the automated evaluation procedure (i) a long short-term memory (LSTM) autoencoder for anomaly detection (defects/impact), and (ii) a convolutional neural network (CNN) model for feature extraction and classification of the artificial damage sizes and locations. Additional data augmentation steps are introduced such as modification and addition of random noise to original signals to enhance the model's robustness to uncertainties. Overall, it was shown that the ML algorithms used were able to detect and classify the simulated damage with high accuracy. T2 - 13th European Conference on Non-Destructive Testing (ECNDT) 2023 CY - Lisbon, Portugal DA - 03.07.2023 KW - Machine learning KW - Structural health monitoring KW - COPV KW - Guided waves KW - Damage localization PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590789 DO - https://doi.org/10.58286/28079 SN - 2941-4989 VL - 1 IS - 1 SP - 1 EP - 6 PB - NDT.net CY - Mayen AN - OPUS4-59078 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mustapha, S. A1 - Yilmaz, Bengisu A1 - Heimann, Jan A1 - Brence, Blaz A1 - Prager, Jens T1 - Guided Waves Propagation in Composite Overwrapped Pressure Vessel N2 - The application of composite overwrapped pressure vessels (COPV) to store hydrogen and other compressed gases, especially when operating at high pressures, imposed the need for an innovative and reliable approach to ensure the safe operation of the system. Continuous structural health monitoring (SHM) based on ultrasonic guided waves (GWs) is a promising approach due to the ability of the wave to propagate for long distances and go around complex structures, moreover the high sensitivity to various failure modes such as delamination, matrix cracking and debonding. In this study, we scrutinize the behavior of (GWs) within the COPV using a network of PZT elements that are used for excitation and sensing. A laser doppler vibrometer (LDV) was also used to scan the surface of the vessel in various directions. L(0,1) and L(0,2) were observed in the captured signal. The L(0, 2) appeared to be a dominant mode in the COPV and was capable of propagating along the entire length and maintaining a good signal-to-noise ratio. The L(0,2) mode maintained the same phase velocity when it is captured at various excitation angles (0, 45, and 90 degrees). The reduced effect of the orthotropy of the materials on the propagating waves is an important result as it will reduce the complexity in data processing when performing damage identification. T2 - 13th. European Conference on Non-Destructive Testing (ECNDT) CY - Lisbon, Portugal DA - 03.07.2023 KW - Composite Overwrapped Pressure Vessels KW - Guided Waves KW - Laser Doppler Vibrometer KW - Structural Health Monitoring KW - Sensors Placement PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591081 DO - https://doi.org/10.58286/28068 SN - 2941-4989 VL - 1 IS - 1 SP - 1 EP - 6 PB - NDT.net CY - Mayen AN - OPUS4-59108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yilmaz, Bengisu A1 - Heimann, Jan A1 - Mustapha, S. A1 - Charmi, Amir A1 - Prager, Jens T1 - Guided wave ultrasonic feature determination in Type IV composite overwrapped pressure vessels towards the digital twin N2 - The digitalization of quality control processes and the underlying data infrastructures for safety relevant components, such as hydrogen pressure vessels, plays a significant role in the transition towards Industry 4.0. In the current safety regulations for hydrogen pressure vessels, there is no established concept for structural health monitoring. The development of a reliable structural health monitoring methodology for monitoring the structural integrity of pressure vessels enables a fast-forward transition from personnel- and costintensive recurring inspections, a.k.a. periodic maintenance, to predictive maintenance. In the work presented; we investigated the application of ultrasonic guided wave propagation to monitor and assess the condition of Type IV composite overwrapped pressure vessel (COPV). A sensor network of fifteen piezo-electric wafers is placed on the carbon fibre reinforced composite cylinder. Five different artificial damage configurations are created by gluing two different weight blocks on three different locations. The database containing measured guided wave data sets is enriched by two different boundary conditions. We utilized an open-source software, openBIS labnotebook, to store and analyse experimental datasets. The guided wave ultrasonic signals were investigated and analysed by using commonly used ultrasonic features (e.g., amplitude, frequency, time of flight) as well as non-traditional time-series features (kurtosis, skewness, variance). The features were used to calculate damage index and the detection performance for the results has been evaluated. The results suggest that both traditional and non-traditional features assume significant importance in artificial damage detection. The future works will additionally involve the impacts of operational conditions, such as periodic pressure variations temperature loadings as well as material degradations. T2 - 13th European Conference on Non-Destructive Testing (ECNDT) CY - Lisbon, Portugal DA - 03.07.2023 KW - Industry 4.0 KW - Composite overwrapped pressure vessels KW - Structural health monitoring KW - Ultrasonic guided waves KW - Predictive maintenance PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591094 DO - https://doi.org/10.58286/28072 SN - 2941-4989 VL - 1 IS - 1 SP - 1 EP - 6 PB - NDT.net CY - Mayen AN - OPUS4-59109 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tsamos, Athanasios T1 - Denoising, Deblurring and Automatic Segmentation of XCT Data with Deep Learning and Synthetic XCT Training Data. A Case Study on Al-Si MMCs. N2 - We employ in-house generated synthetic Al-Si matrix composite XCT data for training deep convolutional neural networks for XCT data conditioning and automatic segmentation. We propose an in-house multilevel deep conditioning framework capable of rectifying noise and blur in corrupted XCT data sequentially. Furthermore, for automatic segmentation, we utilize a special in-house network coupled with a novel iterative segmentation algorithm capable of generalized learning from synthetic data. We report a consistent SSIM efficiency of 92%, 99%, and 95% for the combined denoising/deblurring, standalone denoising, and standalone deblurring, respectively. The overall segmentation precision was over 85% according to the Dice coefficient. We used experimental XCT data from various scans of Al-Si matrix composites reinforced with ceramic particles and fibers. T2 - 12th International Conference on Industrial Computed Tomography (iCT2023) CY - Fürth, Germany DA - 27.02.2023 KW - Automatic Segmentation KW - Denoising Deblurring Sharpening KW - Artificial Intelligence KW - DCNNs KW - Synthetic Training Data KW - XCT PY - 2023 AN - OPUS4-59095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hicke, Konstantin T1 - Approaching distributed ground motion sensing at high and low frequency ranges N2 - The phase and reflection spectrum of a standard distributed acoustic sensor based on an interferometer are used for fast and slow dynamic measurements, respectively, enabling the system to simultaneously measure various types of ground movement. T2 - 28th International Conference on Optical Fiber Sensors (OFS-28) CY - Hamamatsu, Japan DA - 20.11.2023 KW - Distributed acoustic sensing KW - Ground movement monitoring KW - Geomonitoring KW - Interferometer-based KW - DAS PY - 2023 AN - OPUS4-59097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lu, Xin A1 - Hicke, Konstantin A1 - Krebber, Katerina T1 - Approaching distributed ground motion sensing at high and low frequency ranges N2 - The phase and reflection spectrum of a standard distributed acoustic sensor based on an interferometer are used for fast and slow dynamic measurements, respectively, enabling the system to simultaneously measure various types of ground movement. T2 - 28th International Conference on Optical Fiber Sensors (OFS-28) CY - Hamamatsu, Japan DA - 20.11.2023 KW - Distributed acoustic sensing KW - Ground movement monitoring KW - Geomonitoring KW - Interferometer-based KW - DAS PY - 2023 SP - 1 EP - 4 PB - Optica CY - Washington D.C., USA AN - OPUS4-59098 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Seminar on Smelling Drones – Part 1: Introduction to Aerial Robot Olfaction N2 - This seminar series comprises three lectures on drones and ground robots capable of sensing chemical substances and two accompanying hands-on workshops on nano drones equipped with chemical sensors. In the first lecture, Dr. Neumann will talk on a summary of aerial robot olfaction and his research. In the second and third lectures, more details of the nano drones equipped with chemical sensors will be provided, and the participants can get hands on experience of the nano drones in the accompanying workshops. The lectures will be given in English. This seminar series is supported by FY2023 Researcher Exchanges Program in UEC. T2 - Seminar Series on Smelling Drones CY - Tokyo, Japan DA - 28.11.2023 KW - Mobile robotic olfaction KW - Aerial robot KW - Gas source localization KW - Gas distribution mapping PY - 2023 AN - OPUS4-59129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Seminar on Smelling Drones – Part 2: Design and Experimental Study of an Nano Aerial Robot for ARO Applications N2 - This seminar series comprises three lectures on drones and ground robots capable of sensing chemical substances and two accompanying hands-on workshops on nano drones equipped with chemical sensors. In the first lecture, Dr. Neumann will talk on a summary of aerial robot olfaction and his research. In the second and third lectures, more details of the nano drones equipped with chemical sensors will be provided, and the participants can get hands on experience of the nano drones in the accompanying workshops. The lectures will be given in English. This seminar series is supported by FY2023 Researcher Exchanges Program in UEC. T2 - Seminar Series on Smelling Drones CY - Tokyo, Japan DA - 28.11.2023 KW - Mobile robotic olfaction KW - Nano aerial robot KW - Gas source localization KW - Setup and Validation KW - Gas distribution mapping PY - 2023 AN - OPUS4-59130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Seminar on Smelling Drones – Part 3: Deep Dive: Bout-based Gas Source Localization using Aerial Robot Swarms N2 - This seminar series comprises three lectures on drones and ground robots capable of sensing chemical substances and two accompanying hands-on workshops on nano drones equipped with chemical sensors. In the first lecture, Dr. Neumann will talk on a summary of aerial robot olfaction and his research. In the second and third lectures, more details of the nano drones equipped with chemical sensors will be provided, and the participants can get hands on experience of the nano drones in the accompanying workshops. The lectures will be given in English. This seminar series is supported by FY2023 Researcher Exchanges Program in UEC. T2 - Seminar Series on Smelling Drones CY - Tokyo, Japan DA - 28.11.2023 KW - Mobile robotic olfaction KW - Nano aerial robot KW - Gas source localization KW - Bouts KW - Distributed robotics KW - Swarm PY - 2023 AN - OPUS4-59131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Lecompagnon, Julien T1 - Nondestructive defect characterization using full-frame spatially structured super resolution laser thermography N2 - Laser-based active thermography is a contactless non-destructive testing method to detect material defects by heating the object and measuring its temperature increase with an infrared camera. Systematic deviations from predicted behavior provide insight into the inner structure of the object. However, its resolution in resolving internal structures is limited due to the diffusive nature of heat diffusion. Thermographic super resolution (SR) methods aim to overcome this limitation by combining multiple thermographic measurements and mathematical optimization algorithms to improve the defect reconstruction. Thermographic SR reconstruction methods involve measuring the temperature change in an object under test (OuT) heated with multiple different spatially structured illuminations. Subsequently, these measurements are inputted into a severely ill-posed and heavily regularized inverse problem, producing a sparse map of the OuT’s internal defect structure. Solving this inverse problem relies on limited priors, such as defect-sparsity, and iterative numerical minimization techniques. Previously mostly experimentally limited to one-dimensional regions of interest (ROIs), this thesis aims to extend the method to the reconstruction of two-dimensionalROIs with arbitrary defect distributions while maintaining reasonable experimental complexity. Ultimately, the goal of this thesis is to make the method suitable for a technology transfer to industrial applications by advancing its technology readiness level (TRL). In order to achieve the aforementioned goal, this thesis discusses the numerical expansion of a thermographic SR reconstruction method and introduces two novel algorithms to invert the underlying inverse problem. Furthermore, a forward solution to the inverse problem in terms of the applied SR reconstruction model is set up. In conjunction with an additionally proposed algorithm for the automated determination of a set of (optimal) regularization parameters, both create the possibility to conduct analytical simulations to characterize the influence of the experimental parameters on the achievable reconstruction quality. On the experimental side, the method is upgraded to deal with two-dimensional ROIs, and multiple measurement campaigns are performed to validate the proposed inversion algorithms, forward solution and two exemplary analytical studies. For the experimental implementation of the method, the use of a laser-coupled DLP-projector is introduced, which allows projecting binary pixel patterns that cover the whole ROI, reducing the number of necessary measurements per ROI significantly (up to 20x). Finally, the achieved reconstruction of the internal defect structure of a purpose-made OuT is qualitatively and qualitatively benchmarked against well-established thermographic testing methods based on homogeneous illumination of the ROI. Here, the background-noise-free two-dimensional photothermal SR reconstruction results show to outclass all defect reconstructions by the considered reference methods. N2 - Die laserbasierte aktive thermografische Prüfung als berührungslose Methode der zerstörungsfreien Werkstoffprüfung (NDT) basiert auf der aktiven Erwärmung des Testobjekts (OuT) und Messung des resultierenden Temperaturanstiegs mit einer Infrarotkamera. Dadurch bedingt können systematische Abweichungen vom vorhergesagten Erwärmungsverhalten Aufschluss über dessen innere Struktur geben. Jedoch ist das Auflösungsvermögen für innenliegende Defekte durch die diffusive Natur der Wärmeleitung in Festkörpern begrenzt. Thermografische Super-Resolution (SR)-Methoden zielen darauf ab, diese Limitation durch die Kombination mehrerer Messungen mit jeweils unterschiedlicher strukturierter Erwärmung und mathematischer Optimierungsmethoden zu überwinden. Zur Rekonstruktion innerer Defekte mithilfe thermografischer SR-Rekonstruktionsmethodik wird für die Gesamtheit mehrerer Messungen ein schlecht gestelltes und stark regularisiertes inverses mathematisches Problem gelöst, was in einer dünnbesetzten Karte der internen Defektstruktur des OuTs resultiert. Die Inversion mittels iterativer numerischer Minimierungsverfahren profitiert dabei von einzelnen Annahmen wie der vergleichsweisen Seltenheit von Materialdefekten. Nachdem die Methode bisher experimentell fast ausschließlich auf eindimensionale Messbereiche (ROIs) beschränkt war, zielt diese Arbeit auf eine Erweiterung zur Prüfung zweidimensionaler ROIs mit arbiträren Defektverteilungen bei erträglicher experimenteller Komplexität ab. Ziel ist es, durch die Weiterentwicklung des Technologie-Reifegrades (TRL) den Technologietransfer zur industriellen Anwendung zu ermöglichen. Hierzu werden erst die numerische Erweiterung der SR-Rekonstruktionsmethodik für zweidimensionale ROIs erörtert und zwei neue Algorithmen zur Invertierung des zugrunde liegenden inversen Problems vorgestellt, sowie eine Vorwärtslösung des inversen Problems entwickelt. In Verbindung mit einem neuartigen Algorithmus zur automatisierten Bestimmung der (optimalen) Regularisierungsparameter wird erstmals die Möglichkeit geschaffen, analytische Simulationen zum Einfluss einzelner Parameter auf die erreichbare Rekonstruktionsqualität durchzuführen. Weiterhin wird der experimentelle Ansatz zur Prüfung zweidimensionaler ROIs erweitert. Mehrere Messkampagnen validieren die eingeführten Inversionsalgorithmen, die Vorwärtslösung und zwei exemplarische analytische Studien. Für die experimentelle Umsetzung wird erstmals die Verwendung lasergekoppelter DLP-Technologie für die makroskopische thermografische Prüfung nutzbar gemacht, welche die Projektion großflächiger binärer Pixelmuster ermöglicht. Dadurch kann die Anzahl der erforderlichen Messungen pro ROI ohne Qualitätseinbußen erheblich reduziert werden (bis zu 20x). Abschließend werden die erzielten Rekonstruktionsergebnisse der internen Defektstruktur eines speziell angefertigten OuTs qualitativ und quantitativ mit auf homogener Erwärmung basierenden etablierten Methoden der thermografischen Prüfung verglichen. Hier zeigt sich, dass die weitgehend rauschfreien SR-Rekonstruktionsergebnisse alle Defektrekonstruktionen der betrachteten Referenzmethoden deutlich übertreffen. KW - Nondestructive testing KW - Zerstörungsfreie Prüfung KW - Thermography KW - Thermografie KW - Super resolution KW - Structured illumination KW - Strukturierte Beleuchtung KW - Defect characterization KW - Defektcharakterisierung KW - DMD KW - DLP PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588296 DO - https://doi.org/10.14279/depositonce-19271 SP - 1 EP - 154 PB - Technische Universität Berlin CY - Berlin AN - OPUS4-58829 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Häusler, F. T1 - Bout-based Gas Source Localization using Aerial Robot Swarms N2 - Gas source localization (GSL) helps mitigate the impact of industrial accidents and natural disasters. While GSL may be dangerous and time-consuming when performed by humans, swarms of agile and inexpensive nano aerial robots may increase the safety and efficiency of gas source localizations. Since the small payloads of nano aerial robots limit the sensing and computing resources, strategies adapted from biological swarms, such as colonies of social insects, are used to coordinate robot swarms. Most swarm GSL strategies are based on the assumption that the maxima of gas concentrations are sufficiently close to the gas sources. However, prior studies have indicated that the occurrence of “bouts”, a metric for the intermittency of gas distributions, may advantageously be used as a more accurate gas source proximity indicator. This paper presents a swarm GSL strategy employing bouts as source proximity indicators and a bio-inspired pheromone system for communication. Nano aerial robots, deployed in this study, act as agents and emit pheromone markers in an artificial environment upon detecting bouts. Leveraging the concept of artificial potential fields, the agents switch between exploiting the knowledge of the swarm by following pheromone gradients and exploring the search space by targeting a random point. The agents are repelled by each other and by walls to avoid collisions. The swarm GSL strategy is implemented into three nano aerial robots and validated in a real-world experiment in an indoor environment with a single gas source. The results indicate that the the swarm GSL strategy presented in this paper is capable of GSL in indoor environments and that the intermittency of gas distributions is a better source proximity indicator than the mean concentration. T2 - IEEE Sensors 2023 CY - Vienna, Austria DA - 29.10.2023 KW - Mobile robotic olfaction KW - Nano aerial robot KW - Gas source localization KW - Bouts KW - Distributed robotics PY - 2023 AN - OPUS4-58779 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Haratsu, T. A1 - Sakaue, M. A1 - Matsukura, H. A1 - Ishida, H. T1 - Toward Robust Robotic Gas Source Localization in Outdoor Environments: Testing Search Algorithms with Real Outdoor Wind Spectrum N2 - This poster reports an improved outdoor gas source localization algorithm, showing promising results under simulations with a realistic gas plume. In the scenario assumed in this work, an unmanned ground vehicle searches for the location of a gas source in an open outdoor field. The simulated gas plume in this work consists of frequent and large meandering as a real outdoor plume. The source location is estimated using gas and wind measurements obtained from sensors fixed on a mobile platform. When a gas puff is detected, its source is likely to be in the upwind direction. Particle filter-based algorithms have been proposed in previous work to estimate the most likely source location from multiple gas detection events. In this work, the particle weight update function has been modified by adopting a 2D Gaussian plume model, to improve the accuracy in estimating the likelihood of the source location. We have evaluated the performance of this algorithm combined with an estimation-based route planning algorithm. The simulator uses wind data recorded outdoors to calculate transport of gas puffs allowing a formation of a gas plume containing large meandering, due to real fluctuations of outdoor wind. Simulations of the improved particle filter with the estimation-based route planning algorithm have yielded more accurate, stable and time-efficient results than the pre-modified version. T2 - IEEE Sensors 2023 CY - Vienna, Austria DA - 29.10.2023 KW - Mobile robotic olfaction KW - Sensor signal processing KW - Gas source localization KW - Particle filter KW - Unmanned ground vehicle PY - 2023 AN - OPUS4-58780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Barzegar, M. A1 - Lugovtsova, Yevgeniya A1 - Bulling, Jannis A1 - Mishurova, Tatiana A1 - Pasadas, D. A1 - Ribeiro, A. A1 - Ramos, H. T1 - Automatic improved-resolution imaging of composite adhesive joints using time-frequency-wavenumber filtering applied to ultrasonic guided wavefields N2 - This paper presents an automatic damage imaging technique by employing a signal processing approach based on applying hierarchically clustered filters across different domains. The technique involves time-frequency-wavenumber filter banks which are applied sequentially to ultrasonic guided wave (UGW) data. The study is conducted for a single lap joint composite specimen with a special focus on small voids which were formed due to manual adhesive component mixing. UGW data are acquired with a 3D Scanning Laser Doppler Vibrometer (LDV) over the scan area of the bonded plate. UGWs are excited at the central frequency of 100 kHz by a single piezoelectric transducer mounted on the surface of the single plate. Within each domain of time, frequency, and wavenumber, four filters are designed which results in 64 distinct filtered wavefields. From each filtered wavefield, an image is obtained by using root-mean-square (RMS) calculation of the signals. The obtained results are then combined to create a final, improved-resolution image of the scan area. The final image is compared to the image obtained through RMS calculation of full wavefield with interpolation through Delaunay triangulation and the image obtained by X-ray radiography. The results show that the smallest void that could be detected has a diameter of 2.14 mm. T2 - 2023 IEEE International Ultrasonics Symposium (IUS) CY - Montreal, QC, Canada DA - 03.09.2023 KW - Adhesive joints KW - Ultrasonic guided waves KW - Laser Doppler vibrometer KW - Damage imaging KW - Non-destructive testing KW - Porosity analysis PY - 2023 DO - https://doi.org/10.1109/IUS51837.2023.10307423 SP - 1 EP - 4 PB - IEEE AN - OPUS4-58795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Held, Mathias T1 - Determination of isotropic elastic constants from dispersion images based on ultrasonic guided wave propagation by using convolutional neuronal networks N2 - Detaillierte Kenntnisse der elastischen Materialeigenschaften sind in vielen ingenieurtechnischen Bereichen von grundlegender Bedeutung. Insbesondere für die Anwendung von Predictive Maintenance und Structural- Health-Monitoring Methoden mit Ultraschall ist die genaue Kenntnis der elastischen Materialkonstanten eine Grundvoraussetzung. Die von den Herstellern zur Verfügung gestellten Angaben zu den elastischen Materialkonstanten, insbesondere für Polymere und faserverstärkte Kunststoffe, sind jedoch oft unzureichend, da diese vom Produktionsprozess abhängig sind und sich zusätzlich aufgrund von Materialabbauprozessen oder Ermüdung ändern können. In der Praxis liegen polymere Werkstoffe, faserverstärkte Kunststoffe und Metalle oft als dünne, plattenförmige Strukturen vor, in welchen sich geführte Ultraschallwellen (UGWs) ausbreiten können. In der aktuellen Forschung sind bereits verschiedene Neuronale Modelle zur Bestimmung der elastischen Konstanten und der Materialcharakterisierung mittels UGWs bekannt. Ein einfaches neuronales Netz, mit aus Dispersionsbildern extrahierten Werten für Frequenz und Wellenzahl ausbeutungsfähiger Moden als Eingabe, zur Vorhersage der elastischen Konstanten wird in verwendet. Ein rekurrentes Neuronales Netz mit einem Zeit-Frequenz Vektor als Eingabe wird in angewandt, während in ein 1D- Convolutional-Neuronal-Networks (CNN) unter Verwendung der zeitlichen Auslenkung der Grundmoden und in ein 2D-CNN unter Verwendung einer polaren Gruppengeschwindigkeitsdarstellung zur Bestimmung der elastischen Konstanten verwendet wird. In diesem Vortrag wird ein Ansatz zur Bestimmung der isotropen elastischen Konstanten von dünnen Platten auf der Grundlage von UGWs unter Verwendung von Dispersionsbildern und 2D-CNNs vorgestellt. Dispersionsabbildungen aus numerischen Simulationen werden mithilfe verschiedener Methoden vorverarbeitet, um realistische Messdaten zu simulieren. Mit den modifizierten Daten wird das Modell trainiert und die Architektur optimiert. Anschließend wird die Genauigkeit des erzeugten Modells mit realen Messdaten validiert. Es wird gezeigt, dass 2D-CNNs in der Lage sind, die isotropen elastischen Konstanten anhand multimodaler Merkmale aus Dispersionsbildern vorherzusagen, ohne dass eine anfängliche Schätzung der Parameter oder manuelle Merkmalsextraktion erforderlich ist. T2 - Doktorandentreffen Akademie Biggesee CY - Attendorn, Germany DA - 16.10.2023 KW - Elastische Konstanten KW - Dispersion KW - Maschinelles Lernen PY - 2023 AN - OPUS4-58800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lohrke, Heiko A1 - Neumann, Patrick P. ED - Kossa, A. ED - Kiss, R. T1 - Robotic Measurement System Concept for Greenhouse Gas Tomography in Wastewater Treatment Plants N2 - This paper introduces a conceptual framework for a robotic greenhouse gas (GHG) measurement system designed for wastewater treatment plants (WWTPs). The emphasis is on accurate gas tomography measurement of emissions, crucial for national emission assessments. The proposed system is movable, semi-autonomous, and employs a combination of ground and air robots equipped with integral remote gas sensors and in-situ sensors. Employing a two/two configuration ensures comprehensive coverage of WWTPs, overcoming obstacles. The system concept lays the foundation for future implementation and evaluation, addressing the need for enhanced understanding of GHG emissions from WWTPs. T2 - 39th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Siófok, Hungary DA - 26.09.2023 KW - Remote Gas Sensing KW - Greenhouse Gas Emissions KW - Robot-based Emission Measurements KW - Semi-autonomous Sensor Networks KW - Gas Tomography PY - 2023 SN - 978-963-421-927-9 SP - 160 EP - 161 PB - Hungarian Scientific Society of Mechanical Engineering (GTE) CY - Siófok, Hungary AN - OPUS4-58880 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien T1 - Nondestructive defect characterization using full frame spatially structured super resolution laser thermography N2 - Laser-based active thermography is a contactless non-destructive testing method to detect material defects by heating the object and measuring its temperature increase with an infrared camera. Systematic deviations from predicted behavior provide insight into the inner structure of the object. However, its resolution in resolving internal structures is limited due to the diffusive nature of heat diffusion. Thermographic super resolution (SR) methods aim to overcome this limitation by combining multiple thermographic measurements and mathematical optimization algorithms to improve the defect reconstruction. Thermographic SR reconstruction methods involve measuring the temperature change in an object under test (OuT) heated with multiple different spatially structured illuminations. Subsequently, these measurements are inputted into a severely ill-posed and heavily regularized inverse problem, producing a sparse map of the OuT’s internal defect structure. Solving this inverse problem relies on limited priors, such as defect-sparsity, and iterative numerical minimization techniques. Previously mostly experimentally limited to one-dimensional regions of interest (ROIs), this thesis aims to extend the method to the reconstruction of twodimensional ROIs with arbitrary defect distributions while maintaining reasonable experimental complexity. Ultimately, the goal of this thesis is to make the method suitable for a technology transfer to industrial applications by advancing its technology readiness level (TRL). In order to achieve the aforementioned goal, this thesis discusses the numerical expansion of a thermographic SR reconstruction method and introduces two novel algorithms to invert the underlying inverse problem. Furthermore, a forward solution to the inverse problem in terms of the applied SR reconstruction model is set up. In conjunction with an additionally proposed algorithm for the automated determination of a set of (optimal) regularization parameters, both create the possibility to conduct analytical simulations to characterize the influence of the experimental parameters on the achievable reconstruction quality. On the experimental side, the method is upgraded to deal with two-dimensional ROIs, and multiple measurement campaigns are performed to validate the proposed inversion algorithms, forward solution and two exemplary analytical studies. For the experimental implementation of the method, the use of a laser-coupled DLP-projector is introduced, which allows projecting binary pixel patterns that cover the whole ROI, reducing the number of necessary measurements per ROI significantly (up to 20x). Finally, the achieved reconstruction of the internal defect structure of a purpose-made OuT is qualitatively and qualitatively benchmarked against well-established thermographic testing methods based on homogeneous illumination of the ROI. Here, the background-noise-free twodimensional photothermal SR reconstruction results show to outclass all defect reconstructions by the considered reference methods. T2 - Öffentliche wissenschaftliche Aussprache an der Technischen Universität Berlin CY - Berlin, Germany DA - 31.10.2023 KW - Thermography KW - Super resolution KW - NDT KW - Material testing KW - Internal defects KW - DMD KW - DLP PY - 2023 AN - OPUS4-58771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruyle, B. A1 - Pickard, H. A1 - Schultes, L. A1 - Fredriksson, F. A1 - Heffernan, A. A1 - Knappe, D. A1 - Lord, H. A1 - Meng, P. A1 - Mills, M. A1 - Ndungu, K. A1 - Roesch, Philipp A1 - Rundberget, J.T. A1 - Tettenhorst, D. A1 - Van Buren, J. A1 - Vogel, Christian A1 - Westerman, D. A1 - Yeung, L. A1 - Sunderland, E. T1 - Interlaboratory Comparison of Extractable Organofluorine Measurements in Groundwater and Eel (Anguilla rostrata): Recommendations for Methods Standardization N2 - Research on per- and polyfluoroalkyl substances (PFAS) frequently incorporates organofluorine measurements, particularly because they could support a class-based approach to regulation. However, standardized methods for organofluorine analysis in a broad suite of matrices are currently unavailable, including a method for extractable organofluorine (EOF) measured using combustion ion chromatography (CIC). Here, we report the results of an international interlaboratory comparison. Seven laboratories representing academia, government, and the private sector measured paired EOF and PFAS concentrations in groundwater and eel (Anguilla rostrata) from a site contaminated by aqueous film-forming foam. Among all laboratories, targeted PFAS could not explain all EOF in groundwater but accounted for most EOF in eel. EOF results from all laboratories for at least one replicate extract fell within one standard deviation of the interlaboratory mean for groundwater and five out of seven laboratories for eel. PFAS spike mixture recoveries for EOF measurements in groundwater and eel were close to the criterion (±30%) for standardized targeted PFAS methods. Instrumental operation of the CIC such as replicate sample injections was a major source of measurement uncertainty. Blank contamination and incomplete inorganic fluorine removal may introduce additional uncertainties. To elucidate the presence of unknown organofluorine using paired EOF and PFAS measurements, we recommend that analysts carefully consider confounding methodological uncertainties such as differences in precision between measurements, data processing steps such as blank subtraction and replicate analyses, and the relative recoveries of PFAS and other fluorine compounds. KW - Extractable organic fluorine KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Combustion ion chromatography (CIC) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587726 DO - https://doi.org/10.1021/acs.est.3c04560 SN - 0013-936X VL - 57 IS - 48 SP - 20159 EP - 20168 PB - American Chemical Society (ACS) AN - OPUS4-58772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Häusler, F. A1 - Stührenberg, J. A1 - Smarsly, K. A1 - Neumann, Patrick P. T1 - Bout-based Gas Source Localization using Aerial Robot Swarms N2 - Gas source localization (GSL) helps mitigate the impact of industrial accidents and natural disasters. While GSL may be dangerous and time-consuming when performed by humans, swarms of agile and inexpensive nano aerial robots may increase the safety and efficiency of gas source localizations. Since the small payloads of nano aerial robots limit the sensing and computing resources, strategies adapted from biological swarms, such as colonies of social insects, are used to coordinate robot swarms. Most swarm GSL strategies are based on the assumption that the maxima of gas concentrations are sufficiently close to the gas sources. However, prior studies have indicated that the occurrence of “bouts”, a metric for the intermittency of gas distributions, may advantageously be used as a more accurate gas source proximity indicator. This paper presents a swarm GSL strategy employing bouts as source proximity indicators and a bio-inspired pheromone system for communication. Nano aerial robots, deployed in this study, act as agents and emit pheromone markers in an artificial environment upon detecting bouts. Leveraging the concept of artificial potential fields, the agents switch between exploiting the knowledge of the swarm by following pheromone gradients and exploring the search space by targeting a random point. The agents are repelled by each other and by walls to avoid collisions. The swarm GSL strategy is implemented into three nano aerial robots and validated in a real-world experiment in an indoor environment with a single gas source. The results indicate that the the swarm GSL strategy presented in this paper is capable of GSL in indoor environments and that the intermittency of gas distributions is a better source proximity indicator than the mean concentration. T2 - IEEE Sensors 2023 CY - Vienna, Austria DA - 29.10.2023 KW - Mobile robotic olfaction KW - Nano aerial robot KW - Gas source localization KW - Bouts KW - Distributed robotics PY - 2023 SN - 979-8-3503-0387-2 DO - https://doi.org/10.1109/sensors56945.2023.10325109 SP - 1 EP - 4 PB - IEEE AN - OPUS4-58778 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Guerra, M.F. A1 - Martinón-Torres, M. A1 - Lemasson, Q. A1 - Moignard, B. A1 - Pacheco, C. A1 - Pichon, L. A1 - Macdonald, L. A1 - Hess, M. A1 - Tissot, I. ED - Guerra, M. F. ED - Martinón-Torres, M. ED - Quirke, S. T1 - Analytical approaches to Egyptian goldwork N2 - The structure and composition of ancient gold objects retain information about their long history of manufacture, from the exploitation of the ore to the finishing touches, as well as evidence of their use, deposition, and degradation. By developing an efficient analytical strategy, it is possible to retrieve that information. This chapter sets the necessary foundation 131to explore fully the analytical results presented in the following chapters of this volume. The techniques employed in the analyses of the Egyptian jewellery are described and the analytical parameters provided. For more established techniques, only brief introductions are presented, while more recent developments are presented in greater detail. KW - Gold KW - Synchrotron KW - D2XRF KW - Egypt PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586039 DO - https://doi.org/10.17863/CAM.99681 SP - 131 EP - 191 AN - OPUS4-58603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Enhancing efficiency at bamline: employing data science and machine learning for x-ray research N2 - This talk discusses how data science and machine learning techniques are being applied at the BAM Federal Institute for Materials Research and Testing to enhance efficiency and automation at the BAMLine synchrotron facility. The methods presented include Gaussian processes and Bayesian optimization for beamline adjustment and optimization of X-ray measurements. These statistical techniques allow automated alignment of beamline components and active learning scanning to reduce measurement time. Additional machine learning methods covered are neural networks for quantification of X-ray fluorescence (XRF) data and decoding coded apertures. T2 - 17th International Work-Conference on Artificial Neural Networks (IWANN2023) CY - Ponta Delgada, Portugal DA - 19.06.2023 KW - Bayesian Optimization KW - Gaussian Process KW - BAMline PY - 2023 AN - OPUS4-58605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Insights into materials with hard x-rays: capabilities of the bamline N2 - This contribution provides an overview of the BAMline synchrotron radiation beamline, which specializes in hard X-ray spectroscopy techniques for materials research. The BAMline offers X-ray absorption spectroscopy (XAS), x-ray fluorescence spectroscopy (XRF), and tomography to study materials' electronic structure, chemical composition, and structure. Key capabilities include standard and dispersive XAS for electronic structure, micro-XRF for elemental mapping, coded aperture imaging, and depth-resolved grazing exit XAS. The BAMline enables in situ characterization during materials synthesis and functions for energy, catalysis, corrosion, biology, and cultural heritage applications. Ongoing developments like the implementation of machine learning techniques for experiment optimization and data analysis will be discussed. For instance, Bayesian optimization is being used to improve beamline alignment and scanning. An outlook to the future, where the BAMline will continue pioneering dynamic and multi-scale characterization, aided by advanced data science methods, to provide unique insights into materials research, will be given. T2 - μ-XRF at Elettra 2.0: challenges and opportunities CY - Trieste, Italy DA - 11.09.2023 KW - Synchrotron KW - XRF KW - XANES KW - Bayes PY - 2023 AN - OPUS4-58607 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Radiation biophysics N2 - We give an overview about our work related to radiation damage to DNA, proteins, and DNA-protiren complexes damage. Hereby the focus lies on the combination of experiments and Geant4 particle scattering simulations to understand effects in plasmid DNA pUC19, Oligos, and G5P protein. T2 - Project overview CY - Berlin, Germany DA - 27.09.2023 KW - DNA KW - Dosimetry KW - Proteins KW - Radiation damage KW - G5P KW - Microdosimetry KW - Ionizing radiation KW - Geant4 KW - TOPAS KW - TOPAS-nBio KW - Geant4-DNA KW - LEE KW - OH KW - Hydroxyl radical PY - 2023 AN - OPUS4-58742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Radiation biophysics: a journey N2 - We give an overview about recent work concerning ionizing radiation damage to Oligonucleotides, plasmid DNA, DNA binding proteins (G5P), and DNA-protein complexes. We focus on combining new experimental setups with Geant4/TOPAS particle scattering simulations to understand the effets of ionizing radiation. T2 - Project update CY - Online meeting DA - 09.10.2023 KW - DNA KW - Proteins KW - G5P KW - Geant4 KW - Geant4-DNA KW - TOPAS KW - TOPAS-nBio KW - LEE KW - Dosimetry KW - Microdosimetry KW - Magnetism KW - Protein PY - 2023 AN - OPUS4-58744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien T1 - Overcoming the Spatial Resolution Limits imposed by the Thermal MTF with Thermographic Photothermal Super Resolution Reconstruction N2 - The achievable spatial resolution of active thermographic testing is inherently limited by the diffusive nature of heat conduction in solids. This degradation of the achievable spatial resolution for a semi-infinite body acting on a defect signal can be approximated by spatial convolution with the Green’s function of the heat PDE. As the degradation in spatial resolution is dependent on the depth 𝐿, a common rule of thumb specifies that for proper detection, any defect should feature a spatial extension greater or equal to the depth it is located at. However, as the exact shape of a defect can have a large impact on its severity, at best a proper reconstruction of the defect shape should be performed, which therefore must also deal with the aforementioned adverse effects of heat conduction. One recent method to overcome the spatial resolution limit of thermographic testing is the photothermal super resolution reconstruction method. It is based on performing multiple active thermographic measurements on the same region of interest (ROI) with varying spatially structured heating and subsequent numerical reconstruction of the measured defect signals by solving a severely ill-posed inverse reconstruction problem relying on heavy regularization. By extending the experimental implementation of the method to make use of random-pixel patterns projected onto the ROI using a laser-coupled DLP-projector, defect reconstructions can now be performed within a reasonable time frame (~15 min per ROI) at high accuracy. Compared to conventional thermographic testing methods, the photothermal super resolution reconstruction stands out by resulting in a sparse representation of the defect structure of the ROI, making it especially well-suited to further automatic defect classification and quality assurance measures in an Industry 4.0 context. T2 - INTERNATIONAL SCHOOL OF QUANTUM ELECTRONICS: 67th Course: Progress in Photoacoustic & Photothermal Phenomena CY - Erice, Italy DA - 24.09.2023 KW - Thermography KW - Super resolution KW - NDT KW - Internal defects KW - DLP PY - 2023 AN - OPUS4-58472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - In-situ hot isostatic pressing combined with x-ray imaging and diffraction of laser powder bed fusion ti-6al-4v N2 - Hot Isostatic Pressing (HIP) is often introduced to tackle the porosity issue in additively manufactured (AM) materials. For instance, HIP post-processing is recommended to improve fatigue resistance of Laser powder bed fusion (PBF-LB) manufactured parts [1, 2]. Even though HIP cannot completely remove porosity, it significantly decreases the defect population and its average size below the critical threshold value leading to early crack initiation. In the present study, in-situ investigation of HIP procedure of PBF-LB Ti-6Al-4V parts was carried out to gain further insights into the densification mechanism occurring during HIP. The in-situ observations at high pressure and high temperature are uniquely possible at the PSICHE beamline of the Soleil synchrotron (France), thanks to the Ultrafast Tomography on a Paris-Edinburgh Cell (UToPEC) and the combination of the fast phase-contrast tomography and energy-dispersive diffraction [3, 4]. A detailed methodology was developed to ensure that the correct pressure and temperature were maintained during the experiments. The results allowed an estimation of the global dentification rate during HIP of PBF-LB Ti-Al-4V material, as well as a detailed quantitative characterization of the influence of pore size and shape on the densification process, thereby understanding the effectiveness of HIP process on different pore categories. After 20 mins, 75% of porosity can be considered as closed or has size below the resolution of the XCT reconstruction. We also observed that the smallest defects showed higher densification rate, while the defect shape did not have significant effect on such rate. The current development of in-situ HIP experiment allows experimental quantification and validation of the simulation work. Ultimately it paves the road to tailoring the HIP procedure for different materials depending on the porosity and microstructure. T2 - AAMS 2023 CY - Madrid, Spain DA - 26.09.23 KW - Additive manufacturing KW - HIP KW - X-ray computed tomography PY - 2023 AN - OPUS4-58482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Detection, quantification, and treatment of per- and polyfluoroalkyl substances (PFAS) in groundwater (DFEAT-PFAS) N2 - Over the past century, a range of synthetic compounds have been produced to improve humanity’s quality of life. These include pharmaceuticals, plastics, and other chemical compounds that possess properties making them potentially harmful when released to the environment (e.g., ecological and health impacts to humans and animals). Per- and polyfluoroalkyl substances (PFAS) are a large group of chemicals used in the formulations of thousands of consumer goods, including aqueous film-forming foams used to suppress aviation fires in training scenarios, non-stick cookware, fast-food wrappers, water-repellent fabrics, medical equipment, and plastic and leather products. Because of the recent regulations and restrictions on the use of long chain (≥C8) PFAS a significant shift in the industry towards short (C4-C7) and ultrashort (C1-C3) chain alternatives has been recognized the last years. Due to the high polarity and water solubility of ultrashort PFAS, the potential for bioaccumulation is low. However, the high persistence of ultrashort-chain PFAS will result in environmental accumulation, especially in aquatic environments, leading to potential risks for aquatic organisms and increased human external exposure through drinking water. Ultrashort PFAS like trifluoroacetic acid (TFA) are low to moderately toxic to a range of organisms. In addition, ultrashort PFAS can penetrate natural and anthropogenic barriers and eventually reach drinking water sources. Because common drinking water treatment techniques do not sufficiently remove them, they may reach human consumption. In the project we are focusing on detecting and removing PFAS, especially ultrashort-chain PFAS from contaminated groundwater. We are designing passive sampling devices, which can collect and monitor the temporal profile of PFAS species in groundwater. This will allow us to analyze PFAS contaminations in German and Israeli groundwater using state-of-the-art and novel analytical techniques and understand the extent of contamination. In addition to quantification, PFAS contaminated groundwater will be treated via a two-stage process to produce PFAS-free drinking water. As ultrashort-chain PFAS are difficult to analyze with the current target (LC-MS/MS) and sum parameter (AOF, EOF) analysis methods, we additionally using gas chromatography – mass spectrometry (GC-MS). Therefore, an analytical method based on GC-MS is in development to analyze the volatile ultrashort-chain PFAS (TFA, PFPrA, TFMS, PFEtS, PFPrS, trifluoroethanol, pentafluoropropanol and hexafluoro isopropanol) directly in contaminated groundwater samples with the headspace technique and in eluates of organic solvents from the developed passive sampler after direct injection. Moreover, a two-stages process is designed to increase the low concentrations found in groundwater using novel membranes processes such as closed-circuit reverse osmosis (CCRO) and mixed matrix composite nanofiltration membranes (MMCM). Next, the rejected streams containing higher concentrations of PFAS will be treated by coagulation, and the remaining PFAS adsorbed onto carbonaceous nanomaterials (CNMs). The DEFEAT-PFAS project will result in the development of novel tools to detect, quantify, and remove PFAS, especially ultrashort-chain PFAS from contaminated groundwater, and will acquire a new understanding of the extent of these contaminations. T2 - Dioxin Konferenz CY - Maastricht, Netherlands DA - 10.09.2023 KW - Ground water KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Remediation PY - 2023 AN - OPUS4-58346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Melzer, Michael A1 - Nattuveettil, Keerthana T1 - Digital Calibration Certificates: Transforming Efficiency and Safety in Hydrogen Refuelling Station N2 - Digital Certificates have emerged as a pivotal element in automation and digitalisation. This presentation highlights the added value of a digitalised metrology, its impact on the workflows on the calibration service providing and receiving side as well as their significance in enhancing the quality infrastructure. An overview of digital calibration certificates (DCC) for temperature sensors, including their structure and role in establishing trust in hydrogen refuelling stations (HRS), will be discussed. Additionally, it explores the impact of DCC on optimising efficiency in the hydrogen refuelling process. Exploring the paradigm shift brought about by Industry 4.0, where machines possess the ability to autonomously interpret digital certificate data, leads to streamlined safety checks and reduced human intervention. We will discuss how automated verification of machine-readable certificates contributes to maintaining and elevating safety standards over human-readable certificates. Furthermore, we will take a deep dive into the application of DCCs in HRS, showcasing how they enhance operational efficiency, accuracy, and maintenance by enabling real-time monitoring and adjustment of process data. By exploring the interdependent relationship between digital certificates, machine-readable environments, and HRS optimisation, this presentation will provide valuable insights into harnessing cutting-edge technologies to create a safer, more efficient, and technologically empowered hydrogen refuelling process. T2 - H2Safety@BAM : Hydrogen Colloquium CY - Online meeting DA - 06.09.2023 KW - Digital Calibration Certificate KW - Digitalization KW - Digital Traceability KW - QI-Digital KW - Hydrogen Infrastructure PY - 2023 UR - https://www.bam.de/Content/DE/Standardartikel/Themen/Energie/Wasserstoff/wasserstoff.html AN - OPUS4-58353 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Ch’ng, A. C. W. A1 - Konthur, Zoltán A1 - Lim, T. S. T1 - Magnetic Nanoparticle-Based Semi-automated Panning for High-Throughput Antibody Selection N2 - Bio-panning is a common process involved in recombinant antibody selection against defined targets. The biopanning process aims to isolate specific antibodies against an antigen via affinity selection from a phage display library. In general, antigens are immobilized on solid surfaces such as polystyrene plastic, magnetic beads, and nitrocellulose. For high-throughput selection, semi-automated panning selection allows simul-taneous panning against multiple target antigens adapting automated particle processing systems such as the KingFisher Flex. The system setup allows for minimal human intervention for pre-and post-panning steps such as antigen immobilization, phage rescue, and amplification. In addition, the platform is also adaptable to perform polyclonal and monoclonal ELISA for the evaluation process. This chapter will detail the protocols involved from the selection stage until the monoclonal ELISA evaluation with important notes attached at the end of this chapter for optimization and troubleshooting purposes. KW - Phage display KW - Monoclonal antibody KW - Antibody library PY - 2023 DO - https://doi.org/10.1007/978-1-0716-3381-6_15 VL - 2702 SP - 291 EP - 313 PB - Springer US CY - New York, NY AN - OPUS4-58359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - PALUP: Phased-Array-Technik für Luftultraschall-Prüfungen N2 - Im Forschungsvorhaben PALUP werden luftgekoppelte Phased-Array-Sender und -Empfänger entwickelt. Die Wandler basieren auf geladenen zellulären Polymeren, auch Ferroelektrete genannt, die piezoelektrische Eigenschaften und eine sehr geringe spezifische akustische Impedanz aufweisen, womit sie sich für den Bau von luftgekoppelten Ultraschallwandlern sehr gut eignen. T2 - 10. Forum Leichtbau CY - Berlin, Germany DA - 28.09.2023 KW - Luftultraschall KW - Phased Array Technik PY - 2023 AN - OPUS4-58529 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - OITB Quality Assurance concept and minimum requirements for testing services offered on the Metabuilding platform N2 - A brief description of the Quality Assurance concept of the Metabuilding Labs Open Ivvovation Test Bed (OITB) and presentation of the minimum requirements for testing services offered on the Metabuilding platform, wehich were elaborated in 2 workshops in summer 2023. T2 - 4th General Meeting of the Metabuilding Labs project (Horizon 2020) CY - Valladolid, Spain DA - 10.10.2023 KW - Open Innovation Test Bed KW - Metabuilding Labs PY - 2023 AN - OPUS4-58566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - O3BET Quality Protocols N2 - Presentation of the process-oriented approach for the development of the quality protocolls (standard operation procedures and work instructions) for the O3BETs. O3BETs are innovative testing facilities for building envelopes which are developed in the course of the Metabuilding Labs EU Horizon 2020 project. T2 - 4th General Meeting of the Metabuilding Labs project (Horizon 2020) CY - Valladolid, Spain DA - 10.10.2023 KW - Open Innovation Test Bed KW - Metabuilding Labs KW - O3BET PY - 2023 AN - OPUS4-58567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Improved Data Processing for Accurate Plasma Diagnostics with Implications for Calibration-Free LIBS N2 - Many LIBS papers report the determination of plasma temperature using the Boltzmann plot method or the determination of electron density using the Stark line broadening relation. This requires measuring the integrated intensities of the spectral lines and the linewidth under the assumption of optical thinness. It is taken for granted that this can be easily done either by working with the raw spectra or by fitting the appropriate function to the observed spectral lines. However, extracting the necessary information from raw spectral data is not as easy as it might seem. The quality of such extraction will depend to a decisive extent on the type of spectral instrument used. The spectrum emitted by the plasma is distorted by the device; an example is shown in Fig. 1. The elimination of this distortion belongs to the class of inverse problems, the successful solution of which fundamentally depends on the quality of the available information. When it comes to spectroscopy, the quality of information primarily means high spectral resolution and low noise. Not all spectrometers used in LIBS can provide the quality needed to solve the inverse problem; this casts doubt on many published plasma measurements. This communication will be devoted to the general shortcomings of spectral data processing and the inaccuracies in determining the plasma parameters resulting from these shortcomings. The analysis is based on the use of synthetic spectra generated by plasma with known temperature, particle density and electron density. The estimation of errors caused by inadequate processing of spectral data is made by comparing the initial and measured plasma parameters from the spectra. Recommendations will be made for which analytic function best approximates the observed spectral lines, and how data processing errors affect the accuracy of calibration-free LIBS will be discussed. These issues were only partially covered in previously published works, for example [1, 2]. T2 - Colloquium Spectroscopicum Internationale XLIII, The 5th Asian Symposium on Laser Induced Breakdown Spectroscopy June 26-30, 2023 CY - Tokushima, Japan DA - 26.06.2023 KW - Laser induced breakdown spectroscopy KW - Calibration-free LIBS KW - Data processing PY - 2023 AN - OPUS4-58589 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Importance of Spectral Resolution for Accurate Plasma Diagnostics with Implications for Calibration-Free LIBS N2 - In the LIBS literature, almost every second article reports the determination of the plasma temperature using the Boltzmann plot method or the determination of the electron density using the Stark line broadening relation. The first requires the measurement of the integrated intensities of the spectral lines, and the second requires the measurement of the linewidth, under the same assumption of optical thinness. It is taken for granted that this can be easily done either by working with the raw spectra or by fitting an appropriate function to the observed spectral lines. As a rule, reported data are not verified either by an alternative method (e.g., Thomson scattering) or by computer simulations using synthetic spectra. However, the question of how to extract the necessary information from the raw spectral data is not as simple as it might seem. The quality of such an extraction will depend critically on the type of spectral instrument used, its resolution, and the noise superimposed on the data. The problem is that we do not see the spectrum emitted by the plasma, but the spectrum distorted by the measurement; an exaggerated example of such a distortion is shown in Fig. 1. The elimination of this distortion belongs to the class of inverse problems, the so-called ill-posed problems, whose successful solution crucially depends on the quality of the information available. When it comes to spectroscopy, quality of information primarily means high spectral resolution and low noise. Not all spectrometers used in LIBS can provide the quality needed to solve the inverse problem; this casts doubt on many published plasma measurements. The current presentation will be devoted to general shortcomings in the processing of spectral data and inaccuracies in the determination of plasma parameters resulting from these shortcomings. The analysis is based on the use of synthetic spectra produced by plasma with known characteristics, i.e., temperature, species densities, and electron density. The estimation of errors caused by inadequate processing of spectral data is made by comparing the initial and reconstructed plasma parameters. Recipes will be given for which the analytic function best approximates the observed spectral lines, and how data processing errors affect accuracy of calibration-free LIBS will be discussed. These issues were only partially covered in previously published works, for example [1, 2, 3]. T2 - EMS LIBS 2023 CY - Porto, Portugal DA - 04.09.2023 KW - Laser induced breakdown spectroscopy KW - Calibration-free analysis KW - Data processing PY - 2023 AN - OPUS4-58590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Improved Data Processing for Accurate Plasma Diagnostics and Calibration-Free LIBS N2 - Many applications of LIBS require the measurement of plasma temperature and electron density, which in turn requires knowledge of the integrated line intensity and the shape of the spectral lines. While the integral intensity is preserved as light passes through the spectrometer, the shape emitted by an individual atom or ion is greatly distorted. This is due, firstly, to the transfer of light through the plasma (self-absorption), secondly, to the influence of the instrumental function of the spectrometer, and, thirdly, to the aberrations of the optical system. In addition, processing of spectral information, such as background removal, noise reduction, deconvolution, and line fitting, introduces additional errors in the reconstructed linewidth and line integral, which leads to erroneous temperature and electron density values. This communication will be devoted to the general shortcomings of spectral data processing and the resulting inaccuracies in determining the plasma parameters. The analysis is based on the use of synthetic spectra generated by plasma with known temperature and particle density. The estimation of errors caused by inadequate processing of the spectral data is made by comparing the initial and determined plasma parameters. As a result, an improved data processing method will be proposed that takes into account the spectrum distortion by the instrumental function and integration on the pixel detector. The former is accounted for by convolution (instead of deconvolution) of the estimated line profile using a predetermined slit function, and the latter is achieved by piecewise integration of the line profile by the pixel detector, taking into account the pixel size and uniform or non-uniform pixel separation. Recommendations will be made for which analytic function best approximates the observed spectral lines and examples will be given for the application of this routine to calibration-free LIBS using both synthetic and experimental data. T2 - SciX 2023 CY - Sparks, USA DA - 08.10.2023 KW - Laser induced plasma KW - Calibration-free analysis KW - Plasma modeling KW - Emission spectroscopy PY - 2023 AN - OPUS4-58591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. A1 - Mendez, Cristina A1 - Bordel, Nerea T1 - Investigation of LIBS-RF Plasma for Analytical Spectroscopy N2 - Laser breakdown spectroscopy (LIBS) is a common tool for applications in various fields of science and technology. Originally an atomic analysis technique, LIBS was later extended to molecular analysis due to the transient nature of the laser-induced plasma, which develops from a hot dissociation stage on a nanosecond to several microsecond scale to a relatively cold recombination stage on a scale of 10 to 100 microseconds after breakdown. Molecules formed during the recombination stage or incompletely dissociated after ablation can be efficiently detected, allowing the analysis of "difficult" elements or even molecular isotopes. However, with a small amount of ablated material and a short lifetime of the luminous plasma, analytical signals, especially molecular ones, can be very weak. Several methods have been proposed for reheating the plasma and increasing its lifetime, for example, a two-pulse LIBS or a LIBS combined with microwave radiation or with an electric spark discharge. Here we propose another one, LIBS combined with a capacitively coupled RF discharge at 13.6 MHz. The advantages of this combination are an increase in the lifetime of atomic and molecular emission and operation in a low-pressure atmosphere, which significantly reduces pressure line broadening and allows high-resolution spectroscopy. Another major advantage is operating in a chemically controlled atmosphere that can predictably drive desired chemical reactions. In this presentation, we will show the first results obtained with RF-LIBS combination. These will include separate and joint characterization of LIBS and RF plasmas and evaluation of its potential for elemental and molecular analysis and for plasma enhanced chemical vapor deposition. T2 - SciX 2023 CY - Sparks, USA DA - 08.10.2023 KW - Laser induced breakdown spectroscopy KW - Capacitively coupled discharge KW - RF-LIBS combination KW - Plasma reheating PY - 2023 AN - OPUS4-58592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling laser-induced plasma in vacuum and low-pressure co2 atmosphere N2 - The aim of the project is to develop an adequate model of laser induced plasma for conditions expected in space missions, i.e., vacuum, or low-pressure CO2 atmosphere. Numerical modeling will help to find optimal experimental parameters for the laser ablation under artificial lunar or Martian environments and obtain both qualitative, in terms of a composition, and quantitative, in terms of an elemental abundance, information about interrogated samples based on spectral data generated by the model. The best operational conditions will be found at a low cost without conducting tedious and time-consuming optimization experiments. The modeling approaches will be supported by machine learning to accelerate the optimization. T2 - Workshop on DFG project CY - Brno, Czech Republic DA - 10.08.2023 KW - Laser induced plasma KW - CFD computational fluid dynamic KW - Plasma modeling PY - 2023 AN - OPUS4-58595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Combining DGT and 31P NMR spectroscopy to determine phosphorus species in soil N2 - The amount of plant-available phosphorus (P) in soil strongly influences the yield of plants in agriculture. Therefore, various simple chemical extraction methods have been developed to estimate the plant-available P pools in soil. More recently, several experiments with the DGT technique have shown that it has a much better correlation to plant-available P in soils than standard chemical extraction methods (e.g. calcium-acetate-lactate (CAL), Colwell, Olsen, water) when soils with different characteristics are considered. However, the DGT technique cannot give information on the plant-available P species in the soil. Therefore, we combined DGT with solution 31P nuclear magnetic resonance (NMR) spectroscopy. This was achieved by using a modified DGT device in which the diffusive layer had a larger pore size, the binding layer incorporated an adsorption material with a higher capacity, and the device had a larger exposure area. The spectroscopic investigation was undertaken after elution of the deployed DGT binding layer in a NaOH solution. Adsorption tests using solutions of known organic P compounds showed that a sufficient amount of these compounds could be adsorbed on the binding layer in order for them to be analyzed by solution 31P NMR spectroscopy. Furthermore, various intermediates of the hydrolysis of trimetaphosphate in soil could be also analyzed over time. T2 - DGT Konferenz CY - Paris, France DA - 11.10.2023 KW - Soil KW - Phosphorus KW - Plant-availability PY - 2023 AN - OPUS4-58574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Brierley, N. A1 - Casperson, Ralf A1 - Engert, D. A1 - Heilmann, S. A1 - Herold, F. A1 - Hofmann, D. A1 - Küchler, H. A1 - Leinenbach, F. A1 - Lorenz, S. A1 - Martin, J. A1 - Rehbein, J. A1 - Sprau, B. A1 - Suppes, A. A1 - Vrana, J. A1 - Wild, E. T1 - DICONDE in industrial inspection N2 - DICONDE (Digital Imaging and Communication in Non-Destructive Testing) is an open international standard for storing and exchanging industrial test data and process-related information. The DICONDE standard defines both the semantics for structured storage of data and the network-based communication between two endpoints. This allows many test processes to be mapped digitally and securely, while at the same time meeting normative requirements such as traceability to the tester and test object and reproducibility of test results. KW - DICONDE KW - NDT KW - Interoperability KW - Data storage KW - Communication PY - 2023 SN - 978-3-947971-32-9 N1 - Es gibt eine parallele Sprachausgabe (deutsch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (German), a link is in the field related identifier VL - Specification ZfP 4.0-01E SP - 1 EP - 13 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin ET - Edition August 2023 AN - OPUS4-58576 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Casperson, Ralf A1 - Engert, D. A1 - Heilmann, S. A1 - Herold, F. A1 - Hofmann, D. A1 - Küchler, H. A1 - Leinenbach, F. A1 - Lorenz, S. A1 - Martin, J. A1 - Rehbein, J. A1 - Sprau, B. A1 - Suppes, A. A1 - Vrana, J. A1 - Wild, E. T1 - DICONDE in der ZfP N2 - DICONDE (Digital Imaging and Communication in Non-Destructive Evaluation) ist ein offener internationaler Standard zur Speicherung und zum Austausch industrieller Prüfdaten und prozessbezogener Informationen. Der DICONDE-Standard definiert sowohl die Semantik für eine strukturierte Speicherung von Daten als auch die netzwerkbasierte Kommunikation zwischen zwei Endpunkten. Damit lassen sich viele Vorgänge von Prüfprozessen digital und sicher abbilden und gleichzeitig normative Anforderungen wie eine Rückführbarkeit zum Prüfer und Prüfobjekt sowie eine Reproduzierbarkeit von Prüfergebnissen erfüllen. KW - DICONDE KW - ZfP KW - Interoperabilität KW - Datenspeicherung KW - Kommunikation PY - 2023 SN - 978-3-947971-30-5 N1 - Es gibt eine parallele Sprachausgabe (englisch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (English), a link is in the field related identifier VL - Merkblatt ZfP 4.0-01 SP - 1 EP - 13 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin ET - Ausgabe Juni 2023 AN - OPUS4-58578 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Guideline on NDT-supported reliability assessment of existing structures N2 - The presentation summarizes the idea and the methodology of the ZfPStatik project and gives insight into three case studies, showing how non-destructive testing results can be utilized beneficially in the recalculation of existing prestressed concrete and reinforced concrete bridges. T2 - 2nd Conference of the European Association on Quality Control of Bridges and Structures – EUROSTRUCT2023 CY - Vienna, Austria DA - 26.09.2023 KW - Reliability KW - Assessment KW - Existing structures KW - Non-destructive testing PY - 2023 AN - OPUS4-58485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peters, Stefan A1 - Kunkel, Benny A1 - Cakir, Cafer Tufan A1 - Kabelitz, Anke A1 - Witte, Steffen A1 - Bernstein, Thomas A1 - Bartling, Stephan A1 - Radtke, Martin A1 - Emmerling, Franziska A1 - Abdel-Mageed, Ali Mohamed A1 - Wohlrab, Sebastian A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time-, space- and energy-resolved in situ characterization of catalysts by X-ray absorption spectroscopy N2 - A novel setup for dispersive X-ray absorption spectroscopy (XAS) with simultaneous resolution of space, time and energy for in situ characterization of solid materials is demonstrated. KW - Dispersive XAS KW - Catalysis KW - In situ KW - Structure analysis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584924 DO - https://doi.org/10.1039/d3cc03277a SN - 1359-7345 SP - 1 EP - 4 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Platform MaterialDigital Core Ontology (PMDco): A Community Driven Mid-Level Ontology in the MSE Domain N2 - Knowledge representation in the materials science and engineering (MSE) domain is a vast and multi-faceted challenge: Overlap, ambiguity, and inconsistency in terminology are common. Invariant and variant knowledge are difficult to align cross-domain. Generic top-level semantic terminology often is too abstract, while MSE domain terminology often is too specific. The PMDco is designed in direct support of the FAIR principles to address immediate needs of the global experts community and their requirements. The illustrated findings show how the PMDco bridges semantic gaps between high-level, MSE-specific, and other science domain semantics, how the PMDco lowers development and integration thresholds, and how to fuel it from real-world data sources ranging from manually conducted experiments and simulations as well as continuously automated industrial applications. T2 - Patents4Science CY - Berlin, Germany DA - 05.10.2023 KW - Knowledge Representation KW - Semantic Interoperability KW - FAIR data management KW - Knowledge graph and ontologies KW - PMD Core Ontology PY - 2023 AN - OPUS4-58507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - HR-CS-GFMAS a new screening tool for per- and polyfluoroalkyl substances (PFAS) in the environment N2 - Per- and polyfluorinated alkyl substances (PFASs) are a large group of anthropogenic contaminates. Concerning are especially their persistent, bioaccumulative and toxic properties. Mostly, target-based approaches (e.g., LC-MS/MS) are utilized for the analysis of PFASs in the environment. But these approaches are limited to the availability of analytical grade standards and therefore drastically underestimate the total PFAS burden. Analytical approaches based on total fluorine for PFAS sum parameter analysis become increasingly important to indicate realistic PFAS pollution levels. PFAS sum parameters display the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. Besides combustion ion chromatography (CIC), high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification in the low µg F L-1 range. Here, we present a comparison of total fluorine analysis methods – AOF vs. EOF and HR-CS-GFMAS vs. CIC. Therefore, surface water samples from the Spree River in Berlin, Germany were analyzed at 10 locations for total fluorine (TF), AOF and EOF. The AOF made up 0.14–0.81% of TF and the EOF 0.04–0.28% of TF while AOF concentrations were systematically higher. For the instrumental comparison, HR-CS-GFMAS was the more sensitive and precise method for fluorine analysis compared to CIC. T2 - ICOBTE / ICHMET 2023 CY - Wuppertal, Germany DA - 06.09.2023 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine KW - WWTP KW - SPE PY - 2023 AN - OPUS4-58245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Jens A1 - Hufgard, Josefin A1 - You, Yi T1 - LIBS at high duty-cycles: effect of repetition rate and temporal width on the excitation laser pulses N2 - Laser-induced breakdown spectroscopy (LIBS) is becoming a more mature technology every year with new variants such as laser ablation molecular isotopic spectrometry, reheating by various discharge techniques, and multiple pulse excitation schemes, in which sometimes lasers of different pulse lengths are used. However, lasers with inherent parameters like pulse length and repetition rate are still almost exclusively employed. Recent years have witnessed the advent of novel high-repetition-rate laser concepts for machining processes, like welding, milling, and engraving. Here, a comprehensive study of single-pulse LIBS spectra of a single aluminum target is presented to showcase the applicability of flexible high duty-cycle master oscillator power amplifier (MOPA) lasers. Although traditional flashlamp-pumped Fabry–Pérot lasers only permit a variation in the pulse energy and are operated at very low duty-cycles, MOPA lasers add repetition rate and pulse length as variable parameters. A thorough analysis of the temporal plasma behavior revealed the emission dynamic to closely match the excitation laser pulse pattern. An aluminum sample’s spectral response was shown to be significantly impacted by variations in both rate and length. Although the spectral emission strength of the elemental lines of Al, Sr, and Ca all peaked at slightly different parameter settings, the strongest impact was found on the relative abundance of molecular AlO bands. Unlike in previous laser ablation molecular isotopic spectrometry (LAMIS) publications, the latter could be readily detected with a good intensity and well-resolved spectral features without any temporal gating of the detector. This finding, together with the fact that MOPA lasers are both inexpensive and dependable, makes for a promising combination for future studies including the detection of diatomic band structures. KW - Laser-induced breakdown spectroscopy KW - LIBS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583300 DO - https://doi.org/10.3389/fphy.2023.1241533 SN - 2296-424X VL - 11 SP - 1 EP - 8 AN - OPUS4-58330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Xunyu A1 - Riedel, Jens A1 - You, Yi T1 - Determination of broadband-light atomic absorption through interferometric spectrometry with a spatial heterodyne spectrometer N2 - A spatial heterodyne spectrometer (SHS) was combined with a flame atomic absorption (FAA) setup to reveal the analytical potential of SHS to be used as a tool for high-resolution atomic absorption studies. Exploiting the advances in modern computational power, the spectral information encoded in the interferograms was extracted and separated. Consequently, unseeable interferometric ingredients corresponding to narrow-band absorption lines could be recognized. Namely, a single SHS absorption interferogram simultaneously contains both illumination background and absorption information, which can be distinguished through a series of computational steps. In the examples given by this work, we demonstrate the construction of Na absorbance spectra from a single image. The described single-image approach can be used to investigate highly dynamic systems, whereby background collections can be obviated. KW - Optical Spectrometry KW - Spatial Heterodyne Spectrometry KW - Atomic Absorption PY - 2023 DO - https://doi.org/10.1039/D2JA00367H VL - 38 IS - 5 SP - 1088 EP - 1096 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gupta, Kanhaiya T1 - Classification of pores from micro-XCT data of additively manufactured components prepared by laser powder bed fusion. N2 - Laser powder bed fusion (PBF-LB/M) is a metal-based additive manufacturing (AM) process that utilizes a laser to melt powder particles selectively and form the desired product through a layer-by-layer fabrication process. It allows access to a vast new design space and can produce parts with far greater geometrical complexity than traditional methods. However, PBF-LB/M induces inevitable microstructural defects, such as voids and pores, that can adversely affect the quality and performance of the manufactured components. Hence, knowledge of pore formation, types, and suppression is essential for successful future AM applications. This research investigates the formation of different types of pores and their quantification from X-ray micro-computed tomography images of a formerly reported sample. It also examines the influence of the volumetric energy density (VED) on the size, shape, and location of pores for 316L stainless steel parts produced by the PBF-LB/M process. T2 - FEMS EUROMAT 2023 CY - Frankfurt a. M., Germany DA - 03.09.2023 KW - Additive manufacturing KW - Laser Powder Bed Fusion KW - X-ray Computed Tomography PY - 2023 AN - OPUS4-58337 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - News from the working area - Semantic Interoperability N2 - This presentation provides a comprehensive overview of recent developments and the current status within the Semantic Interoperability work area, with a particular emphasis on the advancements related to the Platform MaterialDigital Core Ontology (PMDco). The presentation will delve into the collaborative and community-supported curation process that has been instrumental in shaping PMDco. Additionally, we will introduce the innovative Ontology Playground, showcasing its role in fostering experimentation and exploration within the realm of ontology development. T2 - MaterialDigital Vollversammlung CY - Karlsruhe, Germany DA - 21.09.2023 KW - Semantic Representation KW - FAIR data management KW - Semantic Interoperability KW - Knowledge graph and ontologies KW - PMD Core Ontology KW - MaterialDigital PY - 2023 AN - OPUS4-58422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim T1 - LIBS ConSort: Development of a sensor-based sorting method for constuction and demolition waste N2 - Closed material cycles and unmixed material fractions are required to achieve high recovery and recycling rates in the building industry. In construction and demolition waste (CDW) recycling, the preference to date has been to apply simple but proven techniques to process large quantities of construction rubble in a short time. This is in contrast to the increasingly complex composite materials and structures in the mineral building materials industry. Manual sorting involves many risks and dangers for the executing staff and is merely based on obvious, visually detectable differences for separation. An automated, sensor-based sorting of these building materials could complement or replace this practice to improve processing speed, recycling rates, sorting quality, and prevailing health conditions. A joint project of partners from industry and research institutions approaches this task by investigating and testing the combination of laser-induced breakdown spectroscopy (LIBS) with near-infrared (NIR) spectroscopy and visual imaging. Joint processing of information (data fusion) is expected to significantly improve the sorting quality of various materials like concrete, main masonry building materials, organic components, etc., and may enable the detection and separation of impurities such as SO3-cotaining building materials (gypsum, aerated concrete, etc.) Focusing on Berlin as an example, the entire value chain will be analyzed to minimize economic / technological barriers and obstacles at the cluster level and to sustainably increase recovery and recycling rates. We present current advances and results about the test stand development combining LIBS with NIR spectroscopy and visual imaging. In the future, this laboratory prototype will serve as a fully automated measurement setup to allow real-time classification of CDW on a conveyor belt. T2 - 21. International Conference on Building Materials (Ibausil) CY - Weimar, Germany DA - 13.09.2023 KW - Material classification KW - Data fusion KW - Circular economy KW - LIBS KW - Recycling PY - 2023 AN - OPUS4-58495 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat T1 - Earth‘s near surface characterisation using DAS based on geometric phase N2 - Results obtained from field measurements using a novel distributed acoustic sensor based on geometric phase. The target application is Seismology where we attempt to characterise the Earth's subsurface. T2 - Colaboration on Earthquake Monitoring project with Freue University CY - Berlin, Germany DA - 18.09.2023 KW - Geometric Phase KW - Distributed Fiber Optic Sensor KW - Seismology KW - Coherent Heterodyne KW - Subsurface KW - Earth KW - Surface waves KW - Geophysics PY - 2023 AN - OPUS4-58460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pech May, Nelson Wilbur A1 - Tabasco-Novelo, Carolina A1 - Quintana, Patricia A1 - Rodriguez-Gattorno, Geonel A1 - Alvarado-Gil, Juan J. T1 - Evidence of a Thermal Diffusivity Gap in Sintered Li–Co–Sb–O Solid Solutions N2 - In this work, the thermal properties of ternary Li₃ₓCo₇₋₄ₓSb₂₊ₓO₁₂ solid solutions are studied for different concentrations in the range 0 ≤ x ≤ 0.7. Samples are elaborated at four different sintering temperatures: 1100, 1150, 1200 and 1250 °C. The effect of increasing the content of Li⁺ and Sb⁵⁺, accompanied by the reduction of Co²⁺, on the thermal properties is studied. It is shown that a thermal diffusivity gap, which is more pronounced for low values of x, can be triggered at a certain threshold sintering temperature (around 1150 °C in this study). This effect is explained by the increase of contact area between adjacent grains. Nevertheless, this effect is found to be less pronounced in the thermal conductivity. Moreover, a new framework for heat diffusion in solids is presented that establishes that both the heat flux and the thermal energy (or heat) satisfy a diffusion equation and therefore highlights the importance of thermal diffusivity in transient heat conduction phenomena. KW - General Chemical Engineering KW - General Chemistry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593248 DO - https://doi.org/10.1021/acsomega.2c07557 SN - 2470-1343 VL - 8 IS - 8 SP - 7808 EP - 7815 PB - American Chemical Society (ACS) CY - Washington, DC AN - OPUS4-59324 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schade, U. A1 - Puskar, L. A1 - Golnak, R. A1 - Veber, A. A1 - Beckmann, Jörg T1 - Infrared Attenuate Total Reflection Cell with a Functionalized Surface N2 - ATR cell utilizing chips from silicon wafers is discussed. The cell can be used for wet-chemical analysis on functionalized surfaces. Here, silicon chips are exemplarily "functionalized" by silica layers to provide a hydrophilic or hydrophobic ATR surface in-situ. T2 - 48th International Conference on Infrared, Millimeter, and Terahertz Waves (IRMMW-THz) CY - Montreal, Quebec, Canada DA - 17.09.2023 KW - THz radiation KW - ATR KW - FTIR PY - 2023 DO - https://doi.org/10.1109/IRMMW-THz57677.2023.10298918 SP - 1 PB - IEEE CY - New York, NY AN - OPUS4-59326 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Aktueller Stand der Normung in der Thermografie N2 - Die Thermografie ist trotz ihrer ausgereiften wissenschaftlichen und technologischen Grundlagen ein noch relativ junges Mitglied in der Familie der zerstörungsfreien Prüfverfahren. Sie erschließt sich aufgrund einer Reihe von Vorzügen eine wachsende Anwendungsgemeinde. Für eine weitere Verbreitung insbesondere im industriellen Kontext spielen Normen, Standards und technische Regeln eine wichtige Rolle. In diesem Beitrag wird der aktuelle Stand der Normung in Deutschland vorgestellt. Wir zeigen, welche Normen und technischen Regeln es für die Thermografie in Deutschland und international gibt und wir wagen einen Blick in die Zukunft. Darüber hinaus lebt auch die Normierungsarbeit von der Beteiligung durch interessierte Kreise. Dies können industrielle und akademische Anwender*innen, Hersteller*innen von Geräten, Forschungseinrichtungen oder Dienstleistungsunternehmen sein. Sie können gern Ihre Bedarfe bezüglich Normierungsprojekten mitbringen und/oder direkt an die Autoren senden. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Thermografie KW - Zerstörungsfreie Prüfung KW - Normung KW - Standardisierung PY - 2023 AN - OPUS4-59250 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Aktueller Stand der Normung in der Thermografie N2 - Die Thermografie ist trotz ihrer ausgereiften wissenschaftlichen und technologischen Grundlagen ein noch relativ junges Mitglied in der Familie der zerstörungsfreien Prüfverfahren. Sie erschließt sich aufgrund einer Reihe von Vorzügen eine wachsende Anwendungsgemeinde. Für eine weitere Verbreitung insbesondere im industriellen Kontext spielen Normen, Standards und technische Regeln eine wichtige Rolle. In diesem Beitrag wird der aktuelle Stand der Normung in Deutschland vorgestellt. Wir zeigen, welche Normen und technischen Regeln es für die Thermografie in Deutschland und international gibt und wir wagen einen Blick in die Zukunft. Darüber hinaus lebt auch die Normierungsarbeit von der Beteiligung durch interessierte Kreise. Dies können industrielle und akademische Anwender*innen, Hersteller*innen von Geräten, Forschungseinrichtungen oder Dienstleistungsunternehmen sein. Sie können gern Ihre Bedarfe bezüglich Normierungsprojekten mitbringen und/oder direkt an die Autoren senden. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Thermografie KW - Zerstörungsfreie Prüfung KW - Normung KW - Standardisierung PY - 2023 AN - OPUS4-59251 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bente, Klaas A1 - Rus, J. A1 - Mooshofer, H. A1 - Gaal, Mate A1 - Grosse, C.U. T1 - Broadband air-coupled ultrasound emitter and receiver enable simultaneous measurement of thickness and speed of sound in solids N2 - Air-coupled ultrasound sensors have advantages over contact ultrasound sensors when a sample should not become contaminated or influenced by the couplant or the measurement has to be a fast and automated inline process. Thereby, air-coupled transducers must emit high-energy pulses due to the low air-to-solid power transmission ratios (10−3 to 10−8). Currently used resonant transducers trade bandwidth—a prerequisite for material parameter analysis—against pulse energy. Here we show that a combination of a non-resonant ultrasound emitter and a non-resonant detector enables the generation and detection of pulses that are both high in amplitude (130 dB) and bandwidth (2 µs pulse width). We further show an initial application: the detection of reflections inside of a carbon fiber reinforced plastic plate with thicknesses between 1.7 mm and 10 mm. As the sensors work contact-free, the time of flight and the period of the in-plate reflections are independent parameters. Hence, a variation of ultrasound velocity is distinguishable from a variation of plate thickness and both properties are determined simultaneously. The sensor combination is likely to find numerous industrial applications necessitating high automation capacity and opens possibilities for air-coupled, single-side ultrasonic inspection. KW - Thermoacoustic emitter KW - Optical microphone KW - Air-coupled ultrasound KW - Local resonance KW - Thickness measurement KW - Thickness resonance PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569533 DO - https://doi.org/10.3390/s23031379 VL - 23 IS - 3 SP - 1379 PB - MDPI AN - OPUS4-56953 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN T1 - Forschungsprogramm 2022 - 2024 N2 - Der Koalitionsvertrag der Bundesregierung betont in seiner Präambel zur Zukunft Deutschlands in Bezug auf die notwendige Modernisierung, dass „dieser Fortschritt auch mit einem Sicherheitsversprechen einhergehen muss“. Die Bundesanstalt für Materialforschung und -prüfung (BAM) stellt mit ihrem Auftrag „Sicherheit in Technik und Chemie“ und ihrer über 150-jährigen Kompetenz sicher, dass ein nachhaltiger technischer Fortschritt von einem Sicherheitsversprechen für die Bürger*innen begleitet ist. Durch ihre Interdisziplinarität, die thematische Breite, die langjährige Erfahrung und die unabhängige Rolle als Ressortforschungseinrichtung ist die BAM in einer herausragenden Lage, als zentraler Akteur die Entwicklung unterschiedlichster Technologien unter Berücksichtigung sicherheitstechnischer Aspekte voranzubringen, das Vertrauen der Gesellschaft in diese Technologien sicherzustellen und dadurch die Basis für erfolgreiche Innovationen zu schaffen. Der Fokus ihrer Arbeit liegt auf den fünf Themenfeldern Energie, Infrastruktur, Umwelt, Material und Analytical Sciences. Wichtige Themen betreffen dabei sowohl die Energiewende (Wasserstoff, elektrische Energiespeicher, Windenergie) als auch Bereiche der Technologiesouveränität wie die additive Fertigung, zuverlässige Materialdaten, Zustandsüberwachung und Kreislaufwirtschaft. Die Digitalisierung und den digitalen Wandel unterstützt die BAM in Bezug auf technologieübergreifende Rahmenbedingungen besonders in der Initiative Qualitätsinfrastruktur-Digital (QI-Digital), in der gemeinsam mit weiteren zentralen Akteuren der deutschen QI Lösungen für die Qualitätssicherung in einer digitalisierten Welt entwickelt werden. Grundvoraussetzung für sichere Technologien und Innovationen ist eine leistungsfähige Forschung und Entwicklung ebenso wie Wissens- und Technologietransfer zur Umsetzung von Forschungsergebnissen in marktfähige Produkte und Dienstleistungen. Dafür bildet die Arbeit der BAM eine wichtige Basis. Ihre Forschung ist mit der Wahrnehmung öffentlicher Aufgaben verbunden. Das Forschungsprogramm zeigt Perspektiven im Bereich ihres Aufgabenfeldes sowie ihrer damit verbundenen Forschungsaktivitäten transparent und politisch nutzbar auf und dient darüber hinaus der Koordinierung der Ressortforschung. Das Forschungsprogramm der BAM wird alle zwei Jahre aktualisiert. Es gibt einen Überblick über die aktuellen und zukünftigen Forschungsthemen und die hierfür erforderlichen Rahmenbedingungen. PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572758 SP - 1 EP - 40 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-57275 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Gornushkin, Igor B. T1 - Investigation of a method for the correction of self-absorption by Planck function in laser induced breakdown spectroscopy N2 - The electron density and temperature of a laser-induced plasma can be determined from the width and intensity of the spectral lines, provided that the corresponding optical transitions are optically thin. However, the lines in laser induced plasma are often self-absorbed. One of the methods of correction of this effect is based on the use of the Planck function and an iterative numerical calculation of the plasma temperature. In this study, the method is further explored and its inherent errors and limitations are evaluated. For this, synthetic spectra are used that fully correspond to the assumed conditions of a homogeneous isothermal plasma at local thermodynamic equilibrium. Based on the error analysis, the advantages and disadvantages of the method are discussed in comparison with other methods of self-absorption correction. KW - LIBS KW - Self-absorption KW - Planck function PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572677 DO - https://doi.org/10.1039/D2JA00352J SN - 0267-9477 SP - 1 EP - 6 PB - Royal Society of Chemistry (RSC) AN - OPUS4-57267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - ZfPStatik - Verbesserte Beurteilung von Bestandsbauwerken N2 - Vorgestellt werden - die Projektziele - das Konsortium - die allgemeine Vorgehensweise - und aktuelle Fortschritte im WIPANO-Projekt "ZfPStatik" (Stand: Februar 2023). T2 - 3. vierteljährliche Versammlung des Projektkonsortiums CY - Neubiberg, Germany DA - 07.02.2023 KW - Zerstörungsfreie Prüfung KW - Nachrechnung KW - Zuverlässigkeitsbewertung KW - Bestandsbauwerke PY - 2023 AN - OPUS4-57239 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Friedrich, Alexander T1 - The AIFRI Project - Artificial Intelligence For Rail Inspection N2 - The rails of modern railways face an enormous wear and tear from ever increasing train speeds and loads. This necessitates diligent non-destructive testing for defects of the entire railway system. Non-destructive testing of rail tracks is carried out by rail inspection trains equipped with ultrasonic and eddy current test devices. However, the evaluation of the gathered data is mainly done manually with a strong focus on ultrasonic data, and defects are checked on-site using hand-held testing equipment. Maintenance measures are derived based on these on-site findings. The aim of the AIFRI project (Artificial Intelligence For Rail Inspection) is to - increase the degree of automation of the inspection process, from the evaluation of the data to the planning of maintenance measures, - increase the accuracy of defect detection, - automatically classify detected indications into risk classes. These aims will be achieved by training a neural network for defect detection and classification. Since the current testing data is unbalanced, insufficiently labeled and largely unverified we will supplement fused, simulated eddy current and ultrasonic testing data in form of a configurable digital twin. T2 - PostDoc Day 2022 CY - Berlin, Germany DA - 03.11.2022 KW - Non-destructive testing KW - Artificial intelligence KW - Simulation KW - Eddy current KW - Ultrasound PY - 2022 AN - OPUS4-57240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M.F. A1 - Neri, E. A1 - Radtke, Martin T1 - Gold leaf tesserae: tracing the origins of gold using synchrotron-based techniques N2 - To gain insight into the possible origin of the gold used in the production of tesserae containing gold leaf less than 0.5 μm thick placed between two layers of glass, we propose a non-destructive synchrotron radiation (SR) XRF protocol based on sequential analysis under optimised analytical conditions. Using this protocol, trace element analysis is achieved with detection limits of 1–6 mg/kg. As Pt and Au have adjacent fluorescence energies, we tested the most challenging situation, when Pt is present in very low concentrations in gold. Data obtained by double-dispersive XRF (D2XRF) and μXRF for fourth–ninth-century mosaics decorating nine Eastern and Western religious buildings show that the Eastern and Western tesserae are made from different alloys. However, these alloys are identical to those used to make gold leaf for gilding, because plastic deformation requires the use of gold alloys with high ductility and malleability. Although trace element composition of gold used in the concerned period is only available for coins, by comparing the amounts of Pt contained in the tesserae and in the coins we show that Roman tesserae are made from Roman gold, as described in the documentary sources. We observe for the Byzantine period the use of a Byzantine gold and of gold supposedly from different stages of recycling, and we suggest the use of Umayyad and Abbasid gold for the production of Islamic tesserae. KW - Gold KW - XRF KW - Synchrotron KW - BAMline KW - D2XRF KW - Tesserae PY - 2023 DO - https://doi.org/10.1140/epjp/s13360-022-03638-y SN - 2190-5444 VL - 138 IS - 2 SP - 1 EP - 15 AN - OPUS4-57208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Friedrich, Alexander T1 - AI-based analysis of eddy current and ultrasonic rail testing data N2 - Non-destructive testing of rail tracks is carried out by using rail inspection cars equipped with ultrasonic and eddy current measurement. The evaluation of test data is mainly done manually, supported by a software tool which pre-selects relevant indications shown to the evaluators. The resulting indications have to be checked on-site using hand-held testing equipment. Maintenance interventions are then derived on the basis of these on-site findings. Overall aim of the AIFRI (Artificial Intelligence For Rail Inspection) project - funded by the German Federal Ministry of Digital and Transport (BMDV) as part of the mFUND programme under funding code 19FS2014 – is to increase the degree of automation of the inspection process from the evaluation of the data to the planning of maintenance interventions. The accuracy of defect detection shall be increased by applying AI methods in order to enable an automated classification of detected indications into risk classes. For this purpose, data from both eddy current inspections and ultrasonic inspections will be used in combination. Within the framework of this data-driven project, relevant defect patterns and artefacts present in the rail are analysed and implemented into a configurable digital twin. With the help of this digital twin virtual defects can be generated and used to train AI algorithms for detection and classification. With the help of reliability assessment trained AI algorithms will be evaluated with regard to the resulting quality in defect detection and characterisation. A particular aspect of the development of AI methods is the data fusion of different NDT data sources: Thereby, synergies are used that arise from linking eddy current and ultrasonic inspection data in a combined model. In the course of the project a demonstrator consisting of the developed IT-tool and an asset management system will be implemented and tested in the field using real-world data. T2 - NDT in Railway CY - Berlin, Germany DA - 26.09.2022 KW - NDT KW - Eddy current KW - Ultra sound KW - Simulation KW - Machine learning PY - 2022 UR - https://www.dgzfp.de/seminar/railway/#5 AN - OPUS4-57236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schnur, C. A1 - Moll, J. A1 - Lugovtsova, Yevgeniya A1 - Schütze, A. A1 - Schneider, T. ED - Kundu, T. ED - Reis, H. ED - Ihn, J.-B. ED - Dzenis, Y. T1 - Explainable Machine Learning for Damage Detection: in Carbon Fiber Composite Plates Under Varying Temperature Conditions N2 - Understanding on how a machine learning model interprets data is a crucial step to verify its reliability and avoid overfitting. While the focus of the scientific community is nowadays orientated towards deep learning approaches, which are considered as black box approaches, this work presents a toolbox that is based on complementary methods of feature extraction and selection, where the classification decisions of the model are transparent and can be physically interpreted. On the example of guided wave benchmark data from the open guided waves platform, where delamination defects were simulated at multiple positions on a carbon fiber reinforced plastic plate under varying temperature conditions, the authors could identify suitable frequencies for further investigations and experiments. Furthermore, the authors presented a realistic validation scenario which ensures that the machine learning model learns global damage characteristics rather than position specific characteristics. T2 - 2021 48th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Online meeting DA - 28.07.2021 KW - Explainable machine learning KW - Guided waves KW - Damage detection KW - Structural health monitoring KW - Composite structures PY - 2021 SN - 978-0-7918-8552-9 DO - https://doi.org/10.1115/QNDE2021-75215 VL - QNDE2021-75215 SP - 1 EP - 6 PB - The American Society of Mechanical Engineers (ASME) CY - New York, USA AN - OPUS4-56723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hicke, Konstantin A1 - Liao, Chun-Man A1 - Chruscicki, Sebastian A1 - Breithaupt, Mathias T1 - Vibration Monitoring of Large-Scale Bridge Model using Distributed Acoustic Sensing N2 - Results of DAS measurements along a large-scale concrete bridge model are presented. The improvement of measurable dynamic strain range is demonstrated. Vibration modes obtained by DAS correspond well to those determined from broadband seismometer measurements. T2 - 27th International Conference on Optical Fiber Sensors (OFS-27) CY - Alexandria, VA, USA DA - 29.08.2022 KW - Distributed acoustic sensing KW - Vibration modes KW - Bridge monitoring KW - WS-COTDR KW - Fiber-optic vibration monitoring PY - 2022 SP - 1 EP - 4 PB - Optica CY - Washington D.C., USA AN - OPUS4-56082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Muth, Thilo T1 - QI-CLOUD Perspektiven zur Entwicklung einer digitalen Qualitätsinfrastruktur N2 - In diesem Vortrag wird die Perspektive einer digitalen Qualitätsinfrastruktur (QI) auf informatischer Seite vorgestellt. Eine zu entwickelnde QI-Cloud ist die Grundlage einer verteilten IT-Plattform über die digitalisierte Prozesse der QI abgewickelt, Daten sicher vorgehalten und ausgetauscht sowie digitale Zertifikate ausgestellt werden können. Dazu werden Methoden wie die Distributed Ledger Technologie sowie Smart Standards beschrieben, die das Potential haben, essentielle technologische Bestandteile einer digital transformierten QI zu werden. T2 - VMPA Tagung CY - Nuremberg, Germany DA - 31.05.2022 KW - Digital quality infrastructure KW - QI-Digital KW - QI-Cloud KW - smart standards PY - 2022 AN - OPUS4-56680 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pollard, M. T1 - Functionalized Poly(ethylene glycol)s (PEGs) as a Reference Material for Detection of Polymeric end Groups via SEC Hyphenated with FTIR and 1H-NMR (80 MHz) N2 - With the online coupling (or hyphenation) of chemically-resolved spectroscopy detection with classical size-exclusion chromatography (SEC) it is possible to correlate polymer molecular size with chemical structure in a single in-situ or on-flow measurement. Medium-resolution 1H-NMR (60 MHz) spectroscopy (i.e., “desktop NMR”) and Fouriertransform Infrared Spectroscopy (FTIR) have both been developed as coupled methods (SEC-MR-NMR, SEC-FTIR) for the detection of polymer analytes by monitoring e.g. alkene or carbonyl functionality.1,2 Here, we have investigated the potential for the detection of polymer end groups, using a slightly higher field-strength spectrometer (80 MHz 1H Larmor frequency) and taking advantage of a columnless injection method that provides bulk spectra for reference. End-functionalized polymers were synthesized by reaction of PEG with toluene isocyanate, yielding ,-functionalized polymers with exactly 2 IR- and NMR-detectable functional groups per chain, as proven by MALD-TOF mass spectrometry. We have investigated the sensitivity (limit of detection) and spectral resolution for these functional groups in chloroform, THF, and water. Results have demonstrated a good feasibility for the simultaneous online detection of PEG backbone (M~4000 g/mol) and these end groups at the level of ca. 2 mol%. T2 - 33rd International Symposium on Chromatography CY - Budapest DA - 18.09.2022 KW - Size exclusion chromatography KW - Polyethyleneglycol KW - MALDI-TOF MS KW - NMR PY - 2022 AN - OPUS4-56716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Muth, Thilo T1 - Better data quality for man and machine in materials research and testing N2 - Applying data-driven AI systems makes it possible to extract patterns from given data, generate predictions and helps making decisions. Material research and testing holds a plethora of AI-based applications, for example, for the automatized search and synthesis of new materials, the detection of materials defects, or the prediction of process and materials parameters (inverse problems). However, AI algorithms can often only be as good as the training data from which the corresponding models are learned. Therefore, it is also indispensable to develop measures for the standardization and quality assurance of such data. For this purpose, we develop and implement methods from transferring data from various sources into a homogeneous data repository with uniform data descriptions. Through the standardization and corresponding machine-readable interfaces, research data can be made usable and reusable for further data analyses. In addition to the technical implementation of integrative platforms, it is crucial that quality-assured research data management is recognized and implemented as an integral part of daily scientific work. Finally, we provide a vision of how the Federal Institute for Materials Research and Testing can benefit from data-driven AI systems. We discuss early applications and take a peek at future research. T2 - BR50 AI Workshop CY - Online meeting DA - 13.12.2021 KW - Data quality KW - Machine learning KW - Research data management PY - 2021 AN - OPUS4-56681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Muth, Thilo T1 - The promise of mass spectrometry-based virus proteomics: taking a peek at current bioinformatics applications and limitations N2 - Driven by recent technological advances and the need for improved viral diagnostic applications, mass spectrometry-based proteomics comes into play for detecting viral pathogens accurately and efficiently. However, the lack of specific algorithms and software tools presents a major bottleneck for analyzing data from host-virus samples. For example, accurate species- and strain-level classification of a priori unidentified organisms remains a very challenging task in the setting of large search databases. Another prominent issue is that many existing solutions suffer from the protein inference issue, aggravated because many homologous proteins are present across multiple species. One of the contributing factors is that existing bioinformatic algorithms have been developed mainly for single-species proteomics applications for model organisms or human samples. In addition, a statistically sound framework was lacking to accurately assign peptide identifications to viral taxa. In this presentation, an overview is given on current bioinformatics developments that aim to overcome the above-mentioned issues using algorithmic and statistical methods. The presented methods and software tools aim to provide tailored solutions for both discovery-driven and targeted proteomics for viral diagnostics and taxonomic sample profiling. Furthermore, an outlook is provided on how the bioinformatic developments might serve as a generic toolbox, which can be transferred to other research questions, such as metaproteomics for profiling microbiomes and identifying bacterial pathogens. T2 - European Virus Bioinformatics Center in-silico lecture series CY - Online meeting DA - 28.02.2022 KW - Mass spectrometry KW - Data science KW - Virus detection KW - Bioinformatic algorithms PY - 2022 AN - OPUS4-56682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Muth, Thilo T1 - Benchmarking the current state of metaproteomics : a community driven evaluation of experimental and computational techniques N2 - Metaproteomics has substantially grown over the past years and supplements other omics approaches by bringing valuable functional information, enabling genotype- phenotype linkages and connections to metabolic outputs. Currently, a wide variety of metaproteomic workflows is available, yet their impact on the results remains to be thoroughly assessed. Here, we carried out the first community-driven, multi-lab comparison in metaproteomics: the critical assessment of metaproteome investigation (CAMPI) study. Based on well-established workflows, we evaluated the influence of sample preparation, mass spectrometry acquisition, and bioinformatic analysis using two samples: a simplified, lab-assembled human intestinal model and a human fecal sample. Although bioinformatic pipelines contributed to variability in peptide identification, wet-lab workflows were the most important source of differences between analyses. Overall, these peptide-level differences largely disappeared at the protein group level. Differences were observed between peptide- and protein-centric approaches for the predicted community composition but similar functional profiles were found across workflows. The CAMPI findings demonstrate the robustness of current metaproteomics research and provide a perspective for future benchmarking studies. T2 - ISMB/ECCB 2021 CY - Online meeting DA - 28.07.2021 KW - Mass spectrometry KW - Metaproteomics KW - Benchmarking KW - International lab study KW - Bioanalytics PY - 2021 AN - OPUS4-56685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Materialuntersuchungen zur Schadensanalyse an einem explodierten Umlaufkühler N2 - Ein Umlaufkühler ist im Betrieb explodiert. Splitter des zerborstenen Gehäuses aus Kunststoff wurden mit dem Kühlwasser in die Umgebung geschleudert, am Betriebsort entstand Personenschaden. Bei Funktionsprüfungen am beschädigten Gerät traten unerwartet - aber reproduzierbar - Knalleffekte bei Berührung der Außenoberfläche der Kupfer-Kühlschlange auf. Ein möglicher Mechanismus konnte im Labor durch Synthese von Kupferazid auf Kupferproben und Auslösung vergleichbarer Knalleffekte nachgestellt werden. Damit ist die Plausibilität des beschriebenen Schadensereignisses mit diesem oder einem ähnlich reagierenden Stoff belegt. Ein eindeutiger Nachweis darüber, dass bei dem aufgetretenen Schadensfall dieselbe chemische Reaktion stattgefunden hat, war nicht möglich, da die Belag-Überreste aus dem explodierten Kühlgerät für eine Analyse nicht mehr in ausreichender Menge verfügbar gewesen sind. T2 - BG RCI Präventionstagung, Teil 11 - Inkompatible Systeme – Wenn Chemikalien und Werkstoffe heftig reagieren CY - Online meeting DA - 19.01.2022 KW - Explosion KW - Gutachten KW - Kupferazid KW - Materialuntersuchung KW - Schadensanalyse KW - Umlaufkühler PY - 2022 AN - OPUS4-56686 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kister, Alexander T1 - Multi-Agent Neural Rewriter for Vehicle Routing with Limited Disclosure of Costs N2 - We interpret solving the multi-vehicle routing problem as a team Markov game with partially observable costs. For a given set of customers to serve, the playing agents (vehicles) have the common goal to determine the team-optimal agent routes with minimal total cost. Each agent thereby observes only its own cost. Our multi-agent reinforcement learning approach, the so-called multi-agent Neural Rewriter, builds on the single-agent Neural Rewriter to solve the problem by iteratively rewriting solutions. Parallel agent action execution and partial observability require new rewriting rules for the game. We propose the introduction of a so-called pool in the system which serves as a collection point for unvisited nodes. It enables agents to act simultaneously and exchange nodes in a conflict-free manner. We realize limited disclosure of agent-specific costs by only sharing them during learning. During inference, each agents acts decentrally, solely based on its own cost. First empirical results on small problem sizes demonstrate that we reach a performance close to the employed OR-Tools benchmark which operates in the perfect cost information setting. T2 - Gamification and Multiagent Solutions Workshop (ICLR 2022) CY - Online meeting DA - 29.04.2022 KW - Reinforcement learning KW - Deep Learning KW - Vehicle Routing PY - 2022 AN - OPUS4-56687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yablokov, A. A1 - Lugovtsova, Yevgeniya A1 - Serdyukov, A. T1 - Uncertainty quantification of multimodal surface wave inversion using artificial neural networks N2 - An inversion of surface waves dispersion curves is a non-unique and ill-conditioned problem. The inversion result has a probabilistic nature, which becomes apparent when simultaneously restoring the shear wave (S-wave) velocity and layer thickness. Therefore, the problem of uncertainty quantification is relevant. Existing methods through deterministic or global optimization approaches of uncertainty quantification via posterior probability density (PPD) of the model parameters are not computationally efficient since they demand multiple solutions of the inverse problem. We present an alternative method based on a multi-layer fully connected artificial neural network (ANN). We improve the current uni-modal approach, which is known from publications, to multi-modal inversion. The learned ANN maps the phase velocity dispersion curves to values of the S-wave velocity and layers thickness. To estimate the uncertainties, we adapt the Monte-Carlo simulation strategy and project onto the resulting velocity model both frequency-dependent data noise and inverse operator errors, which are evaluated by the prediction of the training data set. The proposed combination of surface waves data processing methods, configured with each other, provides a novel surface waves multi-modal dispersion data inversion and uncertainty quantification approach. We first test our approach on synthetic experiments for various velocity models: a positive velocity gradient, a low-velocity layer and a high-velocity layer. This is done considering uni-modal inversion at first and then compared to the multi-modal inversion. Afterwards, we apply our approach to field data and compare resulting models with the body S-wave processing by the generalized reciprocal method (GRM). The experiments show high-potential results – using ANN yields the possibility to accurately estimate PPD of restored model parameters without a significant computational effort. The PPD-based comparison demonstrates advantages of a multi-modal inversion over uni-modal inversion. The trained ANN provides reasonable model parameters predictions and related uncertainties in real-time. KW - Multi-layers KW - Multichannel analysis of surface waves (MASW) KW - Characterisation of soil sites KW - Monte Carlo simulation KW - Field data PY - 2023 DO - https://doi.org/10.1190/geo2022-0261.1 SN - 0016-8033 VL - 88 IS - 2 SP - 1 EP - 43 PB - Society of Exploration Geophysicists CY - Tulsa, Okla. AN - OPUS4-56624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Melzer, Michael T1 - Flexible GMR sensors for novel flux leakage testing capabilities N2 - In order to detect small and hidden material defects or micro-cracks, weak and localized magnetic stray fields need to be detected and characterized on the magnetic surface. Current flux leakage sensor elements are rigid and rely on air gaps to detect stray fields several hundred micrometers above the surface. Furthermore, the increasing complexity of critical components, enabled by novel fabrication technologies, primarily additive manufacturing, poses a significant challenge to the available flux leakage testing technologies. The emergence of flexible magneto-electronics paves the way to a compliant form of magnetic sensors that, on one hand, are able to adapt to highly curved surfaces, allowing these measurements to be conducted on irregularly formed components, which are inaccessible for nowadays electromagnetic NDT equipment and, on the other hand, could enhance the detection limit for small magnetic stray fields, by allowing the magneto-sensitive elements to approximate the object’s surface until only a few µm, mediated by thin and flexible packaging. T2 - 38th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Poros, Greece DA - 20.09.2022 KW - Non-destructive testing KW - Flux leakage testing KW - Flexible sensorics KW - GMR Sensors KW - Flexible electronics PY - 2022 AN - OPUS4-56628 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bauer, R. A1 - Pham, M. A1 - Becker, T. A1 - Melzer, Michael A1 - Pelkner, Matthias A1 - Böhle, B. A1 - op den Winkel, F. A1 - Kliche, K. A1 - Welker, F. A1 - Becker, P. A1 - Pfeffer, A. A1 - Gerber, J. A1 - Holzhey, R. A1 - Wenzel, B. A1 - Slatter, R. A1 - Grönefeld, M. A1 - Nasaruk, M. A1 - Buß, R. A1 - Hille, P. A1 - Bartos, A. A1 - Schreiner, I. T1 - Anforderungen an die technische Darstellung von magnetischen Maßverkörperungen in Konstruktionszeichnungen N2 - Dieses Dokument legt Anforderungen an die technische Darstellung von Geometrie und magnetischen Eigenschaften in Konstruktionszeichnungen von magnetischen Maßverkörperungen fest und definiert die dazu notwendige Terminologie. KW - Magnetische Maßverkörperungen KW - Konstruktionszeichnungen KW - Terminologie KW - Magnetische Messsysteme PY - 2022 DO - https://doi.org/10.31030/3359425 IS - DIN SPEC 91411:2022-08 SP - 1 EP - 48 PB - Beuth CY - Berlin AN - OPUS4-56631 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Melzer, Michael T1 - Taxonomie magnetischer Maßverkörperungen N2 - Darstellung der Taxonomie magnetischer Maßverkörperungen im Zusammenhang mit der DIN SPEC 91411 "Anforderungen an die technische Darstellung von magnetischen Maßverkörperungen in Konstruktionszeichnungen" KW - Magnetische Maßverkörperungen KW - Magnetische Messysteme KW - Taxonomie PY - 2022 UR - https://innomag.org/wp-content/uploads/2021/10/DIN-SPEC-Poster_final.pdf SP - 1 EP - 1 PB - Innovationsplattform Magnetische Mikrosysteme INNOMAG CY - Kaiserslautern AN - OPUS4-56633 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Gornushkin, Igor B. ED - Galbács, G. T1 - Calibration-Free Quantitative Analysis N2 - Calibration-free methods in laser-induced breakdown spectroscopy, CF LIBS, serve as an alternative to calibration-based LIBS techniques. Their major advantage is the ability for fast chemical analysis in situations where matrix-matched standards are not readily available (as, e.g., in the analysis of biological materials and remote analysis) or amount of samples are limited. Their main applications are in the industry, geology, biology, archeology, and even space exploration. This chapter overviews the principle of operation and performance of CF LIBS techniques. KW - Laser induced plasma KW - Calibration-free LIBS PY - 2022 SN - 978-3-031-14501-8 DO - https://doi.org/10.1007/978-3-031-14502-5 SP - 67 EP - 100 PB - Springer Nature Switzerland AG AN - OPUS4-56651 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nowatzky, Yannek T1 - Mistle: Metaproteomic index and spectral library search engine N2 - Introduction: With the introduction of accurate deep learning predictors, spectral matching applications might experience a renaissance in tandem mass spectrometry (MS/MS) driven proteomics. Deep learning models, e.g., Prosit, predict complete MS/MS spectra from peptide sequences and give the unprecedented ability to accurately predict mass spectra that may arise from any given proteome. However, the amount of spectral data is enormous when querying large search spaces, e.g., metaproteomes composed of many different species. Current spectral library search software, such as SpectraST, is not equipped to meet run time and memory constraints imposed by such large MS/MS databases, covering several millions of peptide spectrum predictions. Methods: Inspired by the fragment index data structure that had been introduced with MSFragger, we implement an efficient peak matching algorithm for computing spectral similarity between query and library spectra. Mistle (Metaproteomic index and spectral library search engine) uses index partitioning and SIMD (Single instruction, multiple data) intrinsics, which greatly improves speed and memory efficiency for searching large spectral libraries. Mistle is written in C++20 and highly parallelized. Results: We demonstrate the efficiency of Mistle on two predicted spectral libraries for the lab-assembled microbial communities 9MM and SIHUMIx. Compared to the spectral library search engine SpectraST, Mistle shows a >10-fold runtime improvement and is also faster than msSLASH, which uses locality-sensitive hashing. Although Mistle is slower than MSFragger, Mistle‘s memory footprint is an order of magnitude smaller. Furthermore, we find evidence that the spectral matching approach to predicted libraries identifies peptides with higher precision. Mistle detects peptides not found by database search via MSFragger and in turn uncovers unnoticed false discoveries among their matches. Conclusion: In this study, we show that predicted spectral libraries can enhance peptide identification for metaproteomics. Mistle provides the means to efficiently search large-scale spectral libraries, highlighted for the microbiota 9MM and SIHUMIx. T2 - HUPO2022 CY - Cancun, Mexico DA - 04.12.2022 KW - Proteomics KW - Mass spectrometry KW - Algorithms KW - Metaproteomics PY - 2022 AN - OPUS4-56695 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena T1 - Modell based ellipsometry standards for different application cases and their application for real non-ideal systems N2 - Ellipsometry enables the investigation of material properties over a broad spectral range. As a fast and non-destructive method, it is widely used in industry for quality assurance. Despite the wide application of ellipsometry and its high industrial relevance there are some material-specific standards and there have been no generally accepted standards dealing with model validation and measurement uncertainties. The first German standard DIN50989-1: 2018 Ellipsometry – Part1: Principles (currently international standard ISO 23131: 2021) marks the beginning of a 6-part standard series for ellipsometry, which was developed under consideration of GUM. T2 - International Conference on Spectroscopic Ellipsometry (ICSE-9) CY - Beijing, China DA - 22.05.2022 KW - Spectroscopic and imaging ellipsometry KW - Standards KW - Uncertainties PY - 2022 AN - OPUS4-56698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena T1 - Hybrid optical measurement technique for detection of defects in epitaxially grown 4H-SiC layers N2 - Recent developments in power electronics require the use of new wide bandgap compound semiconductors. Silicon carbide (SiC) is one of the most promising materials for power electronics due to its outstanding properties and commercial availability. Some types of defects in the SiC substrates or homoepitaxial SiC layers can affect the performance of electronic devices in a serious manner or make its operation even impossible. Optical methods such as imaging ellipsometry (IE) and white light interference microscopy (WLIM) were applied for fast and non-contact investigation of defects in the epitaxially grown 12 µm 4H-SiC layers on 4H- SiC substrates. T2 - EOS Annual Meeting (EOSAM 2022) CY - Porto, Portugal DA - 12.09.2022 KW - Imaging ellipsometry KW - White light interference microscopy KW - Epitaxially grown 4H-SiC layers KW - Wide bandgap compound semiconductors PY - 2022 AN - OPUS4-56705 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schade, U. A1 - Puskar, L. A1 - Ritter, E. A1 - Beckmann, Jörg T1 - Etalon effects in THz film measurements N2 - Etalon effects in THz transmittance spectra, either taken in time- domain or frequency-domain, often hamper or even hinder the interpretation of film properties. In this paper we discuss the transferability and applicability of spectroscopic methods typically employed in the near and mid infrared spectral range to eliminate the fringes in the transmittance spectra in the THz spectral range. T2 - 2020 45th International Conference on Infrared, Millimeter, and Terahertz Waves (IRMMW-THz) CY - Buffalo, NY, USA DA - 08.11.2020 KW - THz radiation KW - Total transmittance reflection technique KW - Etalon effects PY - 2020 SN - 978-1-7281-6620-9 DO - https://doi.org/10.1109/IRMMW-THz46771.2020.9370451 SN - 2162-2035 SN - 2162-2027 SP - 1 PB - IEEE CY - Buffalo, NY AN - OPUS4-56943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schade, U. T1 - Etalon effects in THz film measurements N2 - Etalon features in transmittance spectra of films arise due to the coherent superposition of waves caused by reflections multiple times at the inner film boundaries. The fringe maxima occur at i𝜆 = 2nd cos 𝜑 with i - being an integer, 𝜆 - the wavelength, d - the film thickness, 𝜑 - the angle of incidence in respect to the film normal and n - the refractive index of the film. It is obvious that such features can hinder the interpretation of absorption bands when fringe amplitude and period are in the same range as the expected bands. This poster discusses the suitability of two optical methods for the THz spectral range applied to Fourier Transform Spectroscopy. T2 - 2020 45th International Conference on Infrared, Millimeter, and Terahertz Waves (IRMMW-THz) CY - Buffalo, NY, USA DA - 08.11.2020 KW - THz radiation KW - Total transmittance reflection technique PY - 2020 AN - OPUS4-56945 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinmuth-Selzle, K. A1 - Bellinghausen, I. A1 - Leifke, A. L. A1 - Backes, A. T. A1 - Bothen, N. A1 - Ziegler, K. A1 - Weller, Michael G. A1 - Saloga, J. A1 - Schuppan, D. A1 - Lucas, K. A1 - Pöschl, U. A1 - Fröhlich-Nowoisky, J. T1 - Chemical modification by peroxynitrite enhances TLR4 activation of the grass pollen allergen Phl p 5 N2 - The chemical modification of aeroallergens by reactive oxygen and nitrogen species (ROS/RNS) may contribute to the growing prevalence of respiratory allergies in industrialized countries. Post-translational modifications can alter the immunological properties of proteins, but the underlying mechanisms and effects are not well understood. In this study, we investigate the Toll-like receptor 4 (TLR4) activation of the major birch and grass pollen allergens Bet v 1 and Phl p 5, and how the physiological oxidant peroxynitrite (ONOO–) changes the TLR4 activation through protein nitration and the formation of protein dimers and higher oligomers. Of the two allergens, Bet v 1 exhibited no TLR4 activation, but we found TLR4 activation of Phl p 5, which increased after modification with ONOO– and may play a role in the sensitization against this grass pollen allergen. We attribute the TLR4 activation mainly to the two-domain structure of Phl p 5 which may promote TLR4 dimerization and activation. The enhanced TLR4 signaling of the modified allergen indicates that the ONOO–-induced modifications affect relevant protein-receptor interactions. This may lead to increased sensitization to the grass pollen allergen and thus contribute to the increasing prevalence of allergies in the Anthropocene, the present era of globally pervasive anthropogenic influence on the environment. KW - Bet v 1 KW - Birch pollen allergen KW - Phl p 5 KW - Grass pollen KW - Phleum pratense KW - Betula pendula KW - Nitration KW - Nitrotyrosine KW - Protein nitration KW - Toll-like receptor 4 KW - Allergy KW - Enhancement KW - Oligomerization KW - Dimerization KW - TLR4 activation KW - Air pollution KW - Nitrogen oxides KW - Inflammation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570298 DO - https://doi.org/10.3389/falgy.2023.1066392 VL - 4 SP - 1 EP - 7 PB - Frontiers Media SA CY - Lausanne, Switzerland AN - OPUS4-57029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - van Wasen, S. A1 - You, Yi A1 - Beck, S. A1 - Riedel, Jens A1 - Volmer, D. A. T1 - Miniaturized Protein Digestion Using Acoustic Levitation with Online High Resolution Mass Spectrometry N2 - The combination of acoustically levitated droplets, mid-IR laser evaporation, and subsequent post-ionization by secondary electrospray ionization was applied for monitoring the enzymatic digestion of various proteins. Acoustically levitated droplets are an ideal, wall-free model reactor, readily allowing compartmentalized microfluidic trypsin digestions. Time-resolved interrogation of the droplets yielded real-time information on the progress of the reaction and thus provided insights into reaction kinetics. After 30 min of digestion in the acoustic levitator, the obtained protein sequence coverages were identical to the reference overnight digestions. Importantly, our results clearly demonstrate that the applied experimental setup can be used for the real-time investigation of chemical reactions. Furthermore, the described methodology only uses a fraction of the typically applied amounts of solvent, analyte, and trypsin. Thus, the results exemplify the use of acoustic levitation as a green analytical chemistry alternative to the currently used batch reactions. KW - Acoustic levitation KW - Protein analysis KW - Mass spectrometry PY - 2023 DO - https://doi.org/10.1021/acs.analchem.2c05334 VL - 95 SP - 4190 EP - 4195 PB - ACS Publications AN - OPUS4-57053 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lecompagnon, Julien A1 - Hirsch, Philipp Daniel A1 - Rupprecht, C. A1 - Ziegler, Mathias T1 - Nondestructive thermographic detection of internal defects using pixel-pattern based laser excitation and photothermal super resolution reconstruction N2 - In this work, we present a novel approach to photothermal super resolution based thermographic resolution of internal defects using two-dimensional pixel pattern-based active photothermal laser heating in conjunction with subsequent numerical reconstruction to achieve a high-resolution reconstruction of internal defect structures. With the proposed adoption of pixelated patterns generated using laser coupled high-power DLP projector technology the complexity for achieving true two-dimensional super resolution can be dramatically reduced taking a crucial step forward towards widespread practical viability. Furthermore, based on the latest developments in high-power DLP projectors, we present their first application for structured pulsed thermographic inspection of macroscopic metal samples. In addition, a forward solution to the underlying inverse problem is proposed along with an appropriate heuristic to find the regularization parameters necessary for the numerical inversion in a laboratory setting. This allows the generation of synthetic measurement data, opening the door for the application of machine learning based methods for future improvements towards full automation of the method. Finally, the proposed method is experimentally validated and shown to outperform several established conventional thermographic testing techniques while conservatively improving the required measurement times by a factor of 8 compared to currently available photothermal super resolution techniques. KW - Thermography KW - Super resolution KW - NDT KW - Inspection KW - Internal defects KW - DMD KW - DLP PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570551 DO - https://doi.org/10.1038/s41598-023-30494-2 SN - 2045-2322 VL - 13 SP - 1 EP - 13 PB - Nature Research AN - OPUS4-57055 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Lugovtsova, Yevgeniya T1 - Damage detection in multi-layered plates using ultrasonic guided waves N2 - This thesis investigates ultrasonic guided waves (GW) in multi-layered plates with the focus on higher order modes. The aim is to develop techniques for hybrid structures such as of adhesive bonds and composite pressure vessels (COPV) which are widely used in automotive and aerospace industries and are still challenging to inspect non-destructively. To be able to analyse GW, numerical methods and precise material properties are required. For this purpose, an efficient semi-analytical approach, the Scaled Boundary Finite Element Method, is used. The material properties are inferred by a GW-based optimisation procedure and a sensitivity study is performed to demonstrate the influence of properties on GW. Then, an interesting feature, called mode repulsion, is investigated with respect to weak and strong adhesive bonds. The results show that the coupling between two layers influences the distance between coupled modes in a mode repulsion region, thus allowing for the characterisation of adhesive bonds. At next, wave-damage interaction is studied in the hybrid structure as of the COPV. Results show that the wave energy can be concentrated in a certain layer enabling damage localisation within different layers. Further investigations are carried out on the hybrid plate with an impact-induced damage. Two well-known wavenumber mapping techniques, which allow to quantify the damage in three dimensions, are implemented and their comparison is done for the first time. KW - Lamb waves KW - Composites KW - Structural Health Monitoring KW - Inverse procedure KW - Scaled Boundary Finite Element Method PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:bsz:291--ds-382863 DO - https://doi.org/10.22028/D291-38286 SP - 1 EP - 131 PB - SciDok - Der Wissenschaftsserver der Universität des Saarlandes CY - Saarbrücken, Germany AN - OPUS4-57058 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Ectoine protects biomolecules from ionizing radiation: Molecular mechanisms N2 - The compatible solute and osmolyte ectoine is an effective protectant of biomolecules and whole cells against heating, freezing and high salinity. The protection of cells (human Keratinocytes) by ectoine against ultraviolet radiation was also reported by various authors, although the underlying mechanism is not yet understood. We present results on the irradiation of biomolecules (DNA) with ionizing radiation (high energy electrons) in fully aqueous environment in the presence of ectoine and high salt concentrations. The results demonstrate an effective radiation protection of DNA by ectoine against the induction of single strand breaks by ionizing radiation. The effect is explained by an increased in low-energy electron scattering at the enhanced free-vibrational density of states of water due to ectoine, as well as the action of ectoine as an OH-radical scavenger. This was demonstrated by Raman spectroscopy, electron paramagnetic resonance (EPR) and Monte-Carlo simulations (Geant4). T2 - #RSCposter 2023 CY - Online meeting DA - 28.02.2023 KW - Compatible solute KW - Dosimetry KW - Ectoine KW - Ectoin KW - Ectoine radiation protection KW - Ectoine radical scavenger KW - Geant4 KW - Geant4-DNA KW - Hydroxyectoine KW - Hydroxyl radical KW - Ionizing radiation KW - Low energy electrons KW - LEE KW - OH-radical KW - DNA KW - Osmolyte KW - Radiation damage KW - Radiation protection KW - Radical scavenger KW - Radiation therapy PY - 2023 AN - OPUS4-57061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hicke, Konstantin T1 - Using DAS for monitoring of infrastructures and for seismic sensing applications N2 - After describing the basics of distributed fiber optic sensing in general and distributed fiber optic acoustic sensing (DAS) in particular, several currently and previously investigated fields of application of DASin infrastructure monitoring and seismic monitoring are presented. A focus is placed on seismic measurements and DAS measurements determining the dynamic responses of concrete structures to certain stimuli. T2 - Meeting of the WAVE Initiative Hamburg CY - Online meeting DA - 09.02.2023 KW - Distributed acoustic sensing KW - DAS KW - Dynamic structural response KW - Seismic measurements KW - Bridge monitoring KW - Traffic monitoring PY - 2023 AN - OPUS4-57007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kader, A. A1 - Kaufmann, Jan Ole A1 - Mangarova, D. B. A1 - Moeckel, J. A1 - Adams, L. C. A1 - Brangsch, J. A1 - Heyl, J. L. A1 - Zhao, J. A1 - Verlemann, C. A1 - Karst, U. A1 - Collettini, F. A1 - Auer, T. A. A1 - Hamm, B. A1 - Makowski, M. R. T1 - Collagen-specific molecular magnetic resonance imaging of prostate cancer N2 - Constant interactions between tumor cells and the extracellular matrix (ECM) influence the progression of prostate cancer (PCa). One of the key components of the ECM are collagen fibers, since they are responsible for the tissue stiffness, growth, adhesion, proliferation, migration, invasion/metastasis, cell signaling, and immune recruitment of tumor cells. To explore this molecular marker in the content of PCa, we investigated two different tumor volumes (500 mm3 and 1000 mm3) of a xenograft mouse model of PCa with molecular magnetic resonance imaging (MRI) using a collagen-specific probe. For in vivo MRI evaluation, T1-weighted sequences before and after probe administration were analyzed. No significant signal difference between the two tumor volumes could be found. However, we detected a significant difference between the signal intensity of the peripheral tumor area and the central area of the tumor, at both 500 mm3 (p < 0.01, n = 16) and at 1000 mm3 (p < 0.01, n = 16). The results of our histologic analyses confirmed the in vivo studies: There was no significant difference in the amount of collagen between the two tumor volumes (p > 0.05), but within the tumor, higher collagen expression was observed in the peripheral area compared with the central area of the tumor. Laser ablation with inductively coupled plasma mass spectrometry further confirmed these results. The 1000 mm3 tumors contained 2.8 +- 1.0% collagen and the 500 mm3 tumors contained 3.2 +- 1.2% (n = 16). There was a strong correlation between the in vivo MRI data and the ex vivo histological data (y = 0.068x + 1.1; R2 = 0.74) (n = 16). The results of elemental analysis by inductively coupled plasma mass spectrometry supported the MRI data (y = 3.82x + 0.56; R2 = 0.79; n = 7). MRI with the collagen-specific probe in PCa enables differentiation between different tumor areas. This may help to differentiate tumor from healthy tissue, potentially identifying tumor areas with a specific tumor biology. KW - Molecular imaging KW - Magnetic resonance imaging KW - MRI KW - Prostate cancer KW - Collagen KW - Laser ablation-inductively coupled plasma-mass spectroscopy KW - EP-3533 KW - Peptide probe KW - Gd-DOTA KW - Contrast agent KW - Tumor PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568449 DO - https://doi.org/10.3390/ijms24010711 SN - 1422-0067 SN - 1661-6596 VL - 24 IS - 1 SP - 1 EP - 13 PB - MDPI CY - Basel AN - OPUS4-56844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kazlagić, Anera A1 - Rosner, M. A1 - Vogl, Jochen T1 - Investigating the differences between MC-ICP-MS and MC-TIMS using conventional 87Sr/86Sr isotope ratios in limestone and slate reference materials N2 - The Federal Institute for Materials Research and Testing (BAM) organised an interlaboratory comparison (ILC) for the characterisation of 87Sr/86Sr isotope ratios in limestone (IAG/CGL ML-3) and Penrhyn slate (IAG OU-6) reference materials by applying the conventional method for 87Sr/86Sr isotope ratios. Samples were sent to thirteen analytical laboratories . Since both samples are powdered, rock materials, dissolution of the sample and Sr isolation via ion exchange chromatography were mandatory. This was done using acid, microwave/acid, bomb/acid digestion or borate fusion and subsequent isolation of Sr by means of commercially available ion exchange resins. In this study, we present and discuss the potential effects that differences between laboratories, and between two instrumental measurement techniques (i.e., MC-ICP-MS and MC-TIMS), may have upon the dispersion of measurement results of the 87Sr/86Sr isotope ratio in the two aforementioned reference materials. We used a statistical mixed effects model to assess the potential effects of both the laboratory and the measurement technique. Consensus values for both materials and associated standard uncertainties {(IAG/CGL ML-3 (0.708245±0.000004) mol/mol; IAG OU-6 (0.729769±0.000008) mol/mol} were estimated by fitting a linear, Gaussian mixed effects model (Pinheiro and Bates 2000) using the R function “lmer” defined in package “lme4”. The statistical results showed that there is no significant effect attributable to differences between instrumental techniques when both materials are considered together, or separately. The p-value of the test of significance of the measurement technique effect is greater than 0.54. For both materials there were statistically significant effects attributable to differences between laboratories when the measurement results for both materials were considered together and separately. This effect is less than 0.00004 in absolute value. However, for neither material did consideration or disregard for such differences induce significant changes in the estimate of the consensus value for the 87Sr/86Sr isotope ratio. Therefore, the effects attributable to differences between instrumental techniques or between laboratories can safely be disregarded when computing the best estimate for the true value of 87Sr/86Sr isotope ratio in these materials, by the community of expert laboratories represented in this study. T2 - GeoAnalysis 2022 CY - Freiberg, Germany DA - 06.08.2022 KW - Isotope ratio KW - Conventional isotope ratio KW - ILC KW - Traceability KW - Uncertainty KW - Isotope reference materials PY - 2022 AN - OPUS4-56848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - 3D imaging and residual stress analysis for AM Materials N2 - The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique). T2 - Seminar at Integrated Additive Manufacturing center, Politecnico Torino CY - Turin, Italy DA - 14.02.2023 KW - Additive manufacturing KW - Laser powder bed fusion KW - Residual stress KW - Computed tomography KW - Synchrotron X-ray diffraction PY - 2023 AN - OPUS4-57047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Veh, G. A1 - Lützow, N. A1 - Tamm, J. A1 - Luna, L. V. A1 - Hugonnet, R. A1 - Vogel, Kristin A1 - Geertsema, M. A1 - Clague, J. J. A1 - Korup, O. T1 - Less extreme and earlier outbursts of ice-dammed lakes since 1900 N2 - Episodic failures of ice-dammed lakes have produced some of the largest floods in history, with disastrous consequences for communities in high mountains. Yet, estimating changes in the activity of ice-dam failures through time remains controversial because of inconsistent regional flood databases. Here, by collating 1,569 ice-dam failures in six major mountain regions, we systematically assess trends in peak discharge, volume, annual timing and source elevation between 1900 and 2021. We show that extreme peak flows and volumes (10 per cent highest) have declined by about an order of magnitude over this period in five of the six regions, whereas median flood discharges have fallen less or have remained unchanged. Ice-dam floods worldwide today originate at higher elevations and happen about six weeks earlier in the year than in 1900. Individual ice-dammed lakes with repeated outbursts show similar negative trends in magnitude and earlier occurrence, although with only moderate correlation to glacier thinning8. We anticipate that ice dams will continue to fail in the near future, even as glaciers thin and recede. Yet widespread deglaciation, projected for nearly all regions by the end of the twenty-first century9, may bring most outburst activity to a halt. KW - Outburst floods KW - Bayesian hierachical modelling KW - Trends in extreme events PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570529 DO - https://doi.org/10.1038/s41586-022-05642-9 VL - 614 IS - 7949 SP - 701 EP - 707 AN - OPUS4-57052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Inspired by Computed Tomography – Swarm-based Gas Tomography N2 - This talk gives an introduction to Mobile Robot Olfaction (MRO) and Robot-assisted Gas Tomography within the scope of the Idea-Workshop "Inspired by Science" @Startup Incubator Berlin. T2 - Inspired by Science: Idea-Workshop CY - Berlin, Germany DA - 13.02.2023 KW - Aerial robot KW - Gas tomography KW - Mobile Robot Olfaction PY - 2023 AN - OPUS4-56993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudert, R. A1 - Schulz, Burkhard A1 - Reck, Günter A1 - Vollhardt, D. A1 - Kriwanek, J. T1 - (Carboxymethyl)dimethylundecylammonium bromide N2 - The title compound, C₁₅H₃₂NO₂⁺.Br⁻, crystallizes to form layers with interdigitating hydrocarbon chains stabilized by Br⁻۰۰۰H—O hydrogen bonds and Br⁻۰۰۰N⁺ contacts. KW - (Carboxymethyl)dimethylundecylammonium bromide KW - Crystal structure PY - 1995 DO - https://doi.org/10.1107/s0108270194011443 SN - 0108-2701 VL - 51 SP - 768 EP - 770 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-56998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kohlbrecher, J. A1 - Breßler, Ingo T1 - Updates in SASfit for fitting analytical expressions and numerical models to small-angle scattering patterns N2 - Small-angle scattering is an increasingly common method for characterizing particle ensembles in a wide variety of sample types and for diverse areas of application. SASfit has been one of the most comprehensive and flexible curve-fitting programs for decades, with many specialized tools for various fields. Here, a selection of enhancements and additions to the SASfit program are presented that may be of great benefit to interested and advanced users alike: (a) further development of the technical basis of the program, such as new numerical algorithms currently in use, a continuous integration practice for automated building and packaging of the software, and upgrades on the plug-in system for easier adoption by third-party developers; (b) a selection of new form factors for anisotropic scattering patterns and updates to existing form factors to account for multiple scattering effects; (c) a new type of a very flexible distribution called metalog [Keelin (2016). Decis. Anal. 13, 243–277], and regularization techniques such as the expectation-maximization method [Dempster et al. (1977). J. R. Stat. Soc. Ser. B (Methodological), 39, 1–22; Richardson (1972) J. Opt. Soc. Am. 62, 55; Lucy (1974). Astron. J. 79, 745; Lucy (1994). Astron. Astrophys. 289, 983–994], which is compared with fits of analytical size distributions via the non-linear least-squares method; and (d) new structure factors, especially for ordered nano- and meso-scaled material systems, as well as the Ornstein–Zernike solver for numerical determination of particle interactions and the resulting structure factor when no analytical solution is available, with the aim of incorporating its effects into the small-angle scattering intensity model used for fitting with SASfit. KW - Small-angle scattering KW - Numerical models KW - Structure factors KW - Regularization KW - SAXS KW - SANS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565069 DO - https://doi.org/10.1107/S1600576722009037 SN - 0021-8898 SN - 1600-5767 VL - 55 IS - 6 SP - 1677 EP - 1688 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-56506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej A1 - Winkler, Nicolas P. A1 - Bartholmai, Matthias ED - Kourkoulis, S. K. T1 - Multi-sensor system for long-term monitoring with WiFi and LoRaWAN technology N2 - In many cases, science falls back on self-developed prototype systems, which are used and developed for the measurement and execution of the tasks. About 80 % of the development is based on the same hardware design, which is used in only one application scenario and then discarded. For the most part, there are also uncalibrated sensors, since it is costly to calibrate a complicated sensor measurement system or the entire measurement chain since access to the sensor systems is not always available. This paper describes a conceptual design to implement a versatile sensor system with the motivation to fuse the data recording and data reception, which can cover large areas with the help of LoRaWAN (Long Range Wide Area Network) technology. To overcome disadvantages of LoRaWAN, namely the slow data rates, the proposed sensor system can also cover smaller areas with the widespread WiFi technology. An enormous advantage over individual complete systems in the form of a prototype, is the rapid expansion, uncomplicated calibration of the individual sensors and the ecological relief. A modular design is used, where individual stacks with sensors and peripherals can be added separately. The stacks are standalone low-power systems and can be calibrated, maintained, and replaced separately and do not require the entire measurement chain. The measured and sent values are stored locally on the main stack and sent to the data collector (gateway) and evaluated by means of the automated selection between WiFi and LoRaWAN. T2 - 38th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Athens, Greece DA - 20.09.2022 KW - Multisensor system KW - LoRaWAN KW - WiFi KW - Long term monitoring PY - 2022 SP - 1 EP - 2 AN - OPUS4-56462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej T1 - Multi-sensor system for long-term monitoring with WiFi and LoRaWAN technology N2 - In many cases, science falls back on self-developed prototype systems, which are used and developed for the measurement and execution of the tasks. About 80 % of the development is based on the same hardware design, which is used in only one application scenario and then discarded. For the most part, there are also uncalibrated sensors, since it is costly to calibrate a complicated sensor measurement system or the entire measurement chain since access to the sensor systems is not always available. This paper describes a conceptual design to implement a versatile sensor system with the motivation to fuse the data recording and data reception, which can cover large areas with the help of LoRaWAN (Long Range Wide Area Network) technology [1, 2]. To overcome disadvantages of LoRaWAN, namely the slow data rates, the proposed sensor system can also cover smaller areas with the widespread WiFi technology. An enormous advantage over individual complete systems in the form of a prototype, is the rapid expansion, uncomplicated calibration of the individual sensors and the ecological relief. A modular design is used, where individual stacks with sensors and peripherals can be added separately. The stacks are standalone low-power systems and can be calibrated, maintained, and replaced separately and do not require the entire measurement chain. The measured and sent values are stored locally on the main stack and sent to the data collector (gateway) and evaluated by means of the automated selection between WiFi and LoRaWAN. T2 - 38th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Athens, Greece DA - 20.09.2022 KW - Multisensor system KW - LoRaWAN KW - WiFi KW - Long term monitoring PY - 2022 AN - OPUS4-56464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Held, Mathias T1 - Pre-colloquium: Inverse determination of elastic material parameters from the propagation behavior of guided ultrasonic waves using a convolutional neural network N2 - Geführte Ultraschallwellen sind für die Materialcharakterisierung hervorragend geeignet, da ihr Ausbreitungsverhalten abhängig von den Materialeigenschaften des untersuchten Werkstoffs ist. Um aus dem messtechnisch ermittelten Ausbreitungsverhalten geführter Ultraschallwellen Rückschlüsse auf die Materialparameter zu ziehen, werden in der aktuellen Forschung verschiedene inverse Methoden diskutiert. Dispersionsabbildungen im Frequenz-Wellenzahl-Bereich repräsentieren das Ausbreitungsverhalten geführter Ultraschallwellen. Maschinelles Lernen und insbesondere Convolutional-Neural-Networks (CNNs) sind eine Möglichkeit der automatisierten inversen Bestimmung der Materialparameter aus den Dispersionsabbildungen. In diesem Beitrag wird anhand synthetischer Daten gezeigt, wie das Ausbreitungsverhalten von geführten Ultraschallwellen unter Verwendung von CNNs und Dispersionsabbildungen genutzt werden kann, um die elastischen Konstanten einer isotropen plattenförmigen Struktur zu bestimmen. Anhand dieses Beispiels wird das generelle Vorgehen zur Anwendung maschineller neuronaler Lernverfahren aufgezeigt. Hierfür werden die verwendeten Daten analysiert, das Preprocessing erläutert und eine einfache CNN-Architektur gewählt. Im Rahmen der Auswertung wird insbesondere Wert auf die Erklärbarkeit und Zuverlässigkeit des verwendeten CNNs gelegt und so Grenzen und Möglichkeiten aufgezeigt. T2 - DAGA 2022 (Jahrestagung für Akustik) CY - Stuttgart, Germany DA - 21.03.2022 KW - Guided Waves KW - Maschinelles Lernen KW - Dispersionsabbildungen PY - 2022 AN - OPUS4-56566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Olbrich, Adelina-Elisa T1 - Deciphering microbiological influenced corrosion processes on steel with single cell-ICP-ToF-MS N2 - Microbiologically influenced corrosion (MIC) is a highly unpredictable process dictated by the environment, microorganisms, and the respective electron source. Interaction pathways between cells and the metal surface remain unclear. The development of this novel single cell-inductively coupled plasma-time of flight-mass spectrometry analytical method and a MIC-specific staining procedure facilitate the investigation of steel-MIC interactions. With this it is possible to analyze the multi-elemental fingerprint of individual cells. The detection method revealed elemental selectivity for the corrosive methanogenic archaeal strain Methanobacterium-affiliated IM1. The interface between material and environmental analysis thus receives special attention, e.g., when considering MIC on solid steel. Hence, the possible uptake of individual elements from different steel samples is investigated. Results showed the cells responded at a single-cell level to the different types of supplemented elements and displayed the abilities to interact with chromium, vanadium, titanium, cobalt, and molybdenum from solid metal surfaces. The information obtained will be used in the future to elucidate underlying mechanisms and develop possible material protection concepts, thus combining modern methods of analytical sciences with materials research. References. T2 - Future WiNS CY - Berlin, Germany DA - 07.12.2022 KW - Single cell KW - Microbiological influenced corrosion MIC KW - Sc-ICP-ToF-MS KW - Method development KW - Ir DNA staining approach KW - Carbon steel corrosion PY - 2022 AN - OPUS4-56567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Samaitis, V. A1 - Yilmaz, Bengisu A1 - Jasiuniene, E. T1 - Adhesive bond quality classification using machine learning algorithms based on ultrasonic pulse-echo immersion data N2 - In this study, we explored the detection of weak bonds (WBs) due to contamination and faulty curing (FC) using linear ultrasound and machine learning. For this purpose, aluminium single-lap adhesive joints containing three variants of bonding quality were investigated: perfect bond, WB due to release agent (RA) contamination, and WB due to FC. The data, according to the deviation of the bonding protocol, were arranged in two groups, creating two datasets: distinct and complete. Each dataset included all bonding conditions (perfect, RA, and FC), although the distinct dataset contained only marginal cases, which were expected to be well separable, whereas the complete dataset included data with minor deviations from the bonding protocol. Pulse-echo C-scan images were acquired for all prepared samples in the immersion tank, and 45 features were initially extracted from the time traces representing each bonding group. The initial data were analysed via a t-test and pairwise correlation analysis to reveal statistically significant features. Then, we performed dimensionality reduction using tree-based, recursive, sequential, and linear discriminant analysis (LDA) feature selectors to explore feature importance and classification accuracy with different feature subsets. Finally, the important features identified with the different feature selectors were fed to support vector machine (SVM) classifiers, and the classification accuracies were compared amongst the different feature subsets. The classification accuracy using a distinct dataset in some cases demonstrated nearly 99% accuracy, indicating that significant bonding protocol deviations could be easily detected. It was demonstrated that classification accuracy increased with the number of features. However, even in the case of the 2D feature space obtained using linear discriminant analysis, the bonding quality classification accuracy remained higher than 84%. The feature subspace reduction with LDA demonstrated sufficient classification accuracy and an improvement of nearly 40% in training time compared with that for the initial feature set. Thus, the classical ultrasonic pulse-echo C-scan with an LDA feature transformation and SVM classifier could be used to identify the deviations in the bonding protocol in aluminium single-lap adhesive joints. KW - Adhesive bonding KW - Defect characterisation KW - Machine learning KW - Ultrasonic imaging PY - 2023 DO - https://doi.org/10.1016/j.jsv.2022.117457 VL - 546 SP - 1 EP - 18 PB - Journal of Sound and Vibration AN - OPUS4-56569 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lecompagnon, Julien T1 - Detektion innenliegender Defekte mittels photothermischer Super-Resolution-Rekonstruktion und 2D-Beleuchtungsmustern N2 - Für die aktive Thermografie als zerstörungsfreie Prüfmethode galt lange Zeit die Faustformel, dass die Auflösung interner Defekte/Inhomogenitäten auf ein Verhältnis von Defekttiefe/Defektgröße ≤ 1 beschränkt ist. Die Ursache hierfür liegt in der diffusiven Natur der Wärmeleitung in Festkörpern. Sogenannte Super-Resolution-Ansätze erlauben seit Kurzem die Überwindung dieser physikalischen Grenze um ein Vielfaches. Damit ergibt sich die attraktive Möglichkeit die Thermografie von einem rein oberflächensensitiven Prüfverfahren hin zu einem Verfahren mit verbesserter Tiefenreichweite zu entwickeln. Wie weit diese Entwicklung getrieben werden kann, ist Gegenstand aktueller Forschung. Wir konnten bereits zeigen, dass diese klassische Einschränkung für ein- und zweidimensionale Defektgeometrien überwunden werden kann, indem das Prüfobjekt mit einzelnen Laserspots sequenziell strukturiert beleuchtet wird und damit anschließend aus den resultierenden Messdaten durch Anwendung photothermischer Super-ResolutionRekonstruktion eine Defektkarte berechnet werden kann, welche eine deutlich verbesserte Trennung einzelner naheliegender Defekte erlaubt. Dieses Verfahren profitiert dabei im Ergebnis stark von der Kombination von sequenzieller räumlich strukturierter Beleuchtung und modernen numerischen Optimierungsverfahren, was jedoch in Summe stark auf Kosten der experimentellen Komplexität geht. Dies führt im Gegensatz zur Anwendung von etablierten thermografischen Standardverfahren mit vollflächiger Beleuchtung zu langen Messzeiten, großen Datensätzen und langwieriger numerischer Auswertung. In dieser Arbeit berichten wir über die Anwendung vollflächig räumlichstrukturierter zweidimensionaler Beleuchtungsmuster, welche es durch den Einsatz modernster Laserprojektortechnik in Verbindung mit einem Hochleistungslaser überhaupt erst erlaubt, eine effiziente Umsetzung von photothermischer Super-ResolutionRekonstruktion auch für größere Prüfflächen zu erreichen. T2 - Thermographie-Kolloquium 2022 CY - Saarbrücken, Germany DA - 28.09.2022 KW - Thermografie KW - Super resolution KW - Eingeschlossene Defekte KW - ZfP KW - DLP KW - Projektor KW - DMD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565222 UR - https://www.dgzfp.de/Portals/thermo2022/BB178/Inhalt/13.pdf AN - OPUS4-56522 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Functional molecular chromophores and nanomaterials reporters, optical probes, and sensors N2 - •Overview of expertise of division Biophotonics •Functional molecular and nanoscale luminescent reporters, probes, and sensors including design principles available from division Biophotonics •Examples for pH and O2 responsive molecular probes and particle sensors •Surface group quantification Analytical methods and cleavable probes •Concepts & standards for the validation and traceability of optical measurements T2 - FU-Seminar CY - Berlin, Germany DA - 09.12.2022 KW - Particle sensors KW - Surface group quantification KW - Nanoscale luminescent reporters KW - Cleavable probes PY - 2022 AN - OPUS4-56526 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Alcalde-Vasquez, R. A1 - Moreno-Pedraza, A. A1 - Rosas-Román, I. A1 - Guillén-Alonso, H. A1 - Riedel, Jens A1 - Partida-Martínez, L. P. A1 - Winkler, R. T1 - MoBiMS: A Modular Miniature Mass Analyzer for the Real-Time 2 Monitoring of Gases and Volatile Compounds in Biological Systems N2 - Living organisms constantly interact with their environment, including through the exchange of gases. Respiration and the release and uptake of volatile organic compounds (VOCs) create dynamic microenvironments in biological systems. Studying the kinetics of volatiles in biological systems requires expensive instruments, and data analysis is challenging. Therefore, we aimed to design a minimal analytical device for measuring the composition of gaseous mixtures in realtime. We built the ‘Modular Biological Mass Spectrometer’ (MoBiMS) from 3D-printed parts and custom sensors to fit a wide array of experimental set-ups. We tested the chemical detection range and temporal resolution of the MoBiMS employing pure compounds and complex biological samples. Compounds with a higher than 0.4 mmHg vapor pressure and a molecular weight up to 154 g/mol were reliably sensed within seconds. The generated electron impact (EI) spectra were directly comparable with standard databases like the NIST EI library. Under a direct analysis approach, the MoBiMS identified the characteristic odor of banana (Musa sp.), that is, isoamyl acetate; tracked the dynamics of CO2 release while the Alka-Seltzer® reaction occurred showed the kinetics of the transient production and consumption of carbon dioxide during photosynthesis. MoBiMS also discriminated between volatile compounds ions coming from tobacco (Nicotiana benthamiana) leaves and the surrounding air through untargeted analysis. The small footprint of the MoBiMS and its relatively low energy consumption facilitate in situ analyses, as an additional gas supply is not necessary with EI ionization. The MoBiMS is easy to assemble, and its construction and operation are very cost-efficient compared to commercial devices. The analytical performance of the MoBiMS is suitable for real-time studies of biological systems, environmental monitoring, and medical diagnostics. KW - Mass spectrometry KW - Instrumentation KW - Miniaturization KW - Volatiles PY - 2022 DO - https://doi.org/10.1016/j.microc.2021.107090 SN - 0026-265X VL - 175 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-56528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - van Wasen, S. A1 - You, Yi A1 - Beck, S. A1 - Riedel, Jens A1 - Volmer, D. A. T1 - Laser Ablation Secondary Electrospray Ionization for In Situ Mass Spectrometric Interrogation of Acoustically-Levitated Droplets N2 - The composition of acoustically levitated droplets was probed by a novel combination of mid-IR laser evaporation and subsequent postionization via secondary electrospray ionization. The combination of microliter samples and subnanoliter sampling provided time-resolved interrogation of droplets and allowed for a kinetic investigation of the laser-induced release of the analyte, which was found to strongly depend on the analytes. The observed substancespecific delayed release of the analytes permitted baseline-separated discrimination of the analytes, ideal for the study of complex samples. The additionally applied postionization scheme was found to enable efficient detection of small volatile compounds as well as peptides. The detection of small molecules and peptides occurred under very different sampling geometries, pointing to two distinct underlying ionization mechanisms. Overall, our results suggest that the experimental setup presented in this study can serve as a widely applicable platform to study chemical reactions in acoustically levitated droplets as model reactors. KW - Acoustic levitation KW - Mass spectrometry KW - Electrospray KW - Laser ablation PY - 2022 DO - https://doi.org/10.1021/acs.analchem.2c03800 SN - 0003-2700 VL - 2022 SP - 1 EP - 5 PB - ACS Publications CY - Washington AN - OPUS4-56531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Application of LIBS in civil engineering – status, trends and challenges N2 - The main application of LIBS in civil engineering is the detection of harmful ions in concrete, which can penetrate the component through the porous concrete structure. The advantages of LIBS over standard methods are the possibility of multi-element analysis, measurement speed, spatially resolved measurements, and minimal sample preparation. The spatially resolved measurements of LIBS allow the assessment of the heterogeneity of the concrete by measuring separately the chemical composition of the aggregates and the binder matrix. The latter is particularly relevant because the determined elemental distribution can be directly related to the binder matrix. This is not possible with standard methods, since the material is homogenized to powder during sample preparation stage and the determined concentration is thus related to the total mass. In addition to the use of LIBS for the specific analysis of individual harmful ions, LIBS can also be used to estimate the concrete composition and thus determine, for example, the type of cement used. Corresponding information are relevant for the estimation of the remaining service life and for the preparation of a maintenance concept. In recent years, LIBS has been increasingly used in civil engineering. Currently, however, it is primarily used in research institutions and only occasionally in building materials laboratories. Special commercial devices have also been developed, which greatly simplify the application due to the high degree of automation. Mobile LIBS systems allow on-site application. A central point, which limits the use of LIBS in the commercial sector, is the lack of norms and standards. Therefore, within the framework of a project funded by the German government, work has been carried out on the preparation of a leaflet on quantitative chlorine determination in concrete, which will be published this year. In interlaboratory comparisons the robustness and accuracy for the practical application was demonstrated. LIBS also has great potential in the recycling of construction waste in conjunction with hyperspectral sensors. This issue is currently being addressed in a national project. During the presentation, the state of the art of LIBS in civil engineering will be presented, next steps will be discussed, and future challenges will be outlined. T2 - XII international conference on laser induced breakdown spectroscopy (LIBS 2022) CY - Bari, Italy DA - 04.09.2022 KW - LIBS KW - Concrete KW - Chlorine KW - Civil engineering PY - 2022 AN - OPUS4-56535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Condition assessment of concrete infrastructure with LIBS N2 - Due to the ageing of the infrastructure facilities, a reliable assessment of the condition of concrete structures is of great interest to plan timely and appropriate measures. In concrete structures, pittingcorrosion of the reinforcement is the predominant deterioration mechanism affecting serviceability and eventually structural performance. Determination of quantitative chloride ingress is not only necessary to obtain valuable information on the current condition of a structure, but the data obtained can also be used to predict future developments and the associated risks. An overview of the progress and the possibilities of the application of laser-induced breakdown spectroscopy for concrete analysis in daily civil engineering practice is given. High-resolution 2D measurements of drill cores to determine the penetration of harmful species into concrete is presented. Furthermore, the application of a mobile LIBS system in a parking garage is shown. The system consists of a diode-pumped low-energy laser (3 mJ, 1.5 ns, 100 Hz) and a compact NIR spectrometer. A scanner allows two-dimensional element mapping. Progress towards the establishment of LIBS in a leaflet for the analysis of chlorine ingress into concrete in civil engineering is presented. T2 - Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy 2021 CY - Gijón, Spain DA - 29.11.2021 KW - LIBS KW - Concrete KW - Chlorine KW - Civil engineering PY - 2021 AN - OPUS4-56536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hallier, Dorothea C. T1 - Inonizing Radiation Damage to Nucleoprotein Filaments . Literaturseminar N2 - Literaure Seminar on progress of doctoral thesis with title "ionizing radiation damage to nucleoprotein filaments involved in DNA recombination, replication and repair" T2 - Literaturseminar Uni Potsdam CY - Potsdam, Germany DA - 25.01.2022 KW - Radiation KW - Radiation damage KW - Nucleoprotein filaments KW - Radiation damage dosimetry KW - Gene-V Protein KW - Single-stranded DNA-binding protein KW - GVP G5P KW - Protein purification and expression KW - DNA PY - 2022 AN - OPUS4-56537 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hallier, Dorothea C. T1 - Jahresvortrag Ionizing radiation damage to nucleoprotein filaments N2 - Jahresvortrag AG Seitz Fraunhofer IZI BB Potsdam about progress of doctoral thesis with the title "Ionizing Radiation Damage to Nucleoprotein filaments involved in DNA recombination, replication and repair T2 - Jahresmeeting Fraunhofer IZI-BB Potsdam, AG Biomarkervalidierung und Assayentwicklung CY - Potsdam, Germany DA - 18.02.2022 KW - Radiation KW - Radiation damage KW - Nucleoprotein filaments KW - Single-stranded DNA-binding protein KW - Protein expression and purification KW - DNA KW - Radiation damage dosimetry PY - 2022 AN - OPUS4-56539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Laser Induced Breakdown Spectroscopy – A Tool for the Chemical Investigation of Concrete N2 - LIBS is a complementary method to XRF and can detect all elements without the need for vacuum conditions. Automated systems are already commercially available capable of scanning surfaces with a resolution of up to 0.1 mm within a few minutes. In addition to possible applications in R&D, LIBS is also used for practical applications in building materials laboratories and even on-site. In view of ageing infrastructure facilities, a reliable assessment of the condition of concrete structures is of increasing interest. For concrete structures, the ingress of potential harmful ions is affecting the serviceability and eventually structural performance. Pitting corrosion induced by penetrating chlorides is the dominant deterioration mechanism. Condition assessment based on frequently performed chloride profiling can be useful to identify the extent and evolution of chloride ingress. This could prove to be more economical than extensive repairs, especially for important infrastructure facilities. Currently the most common procedure for determining the chloride content is wet chemical analysis with standard resolution of 10 mm. The heterogeneity is not considered. LIBS is an economical alternative for determining the chloride content at depth intervals of 1 mm or less. It provides 2D distributions of multiple elements and can locate spots with higher concentrations. The results are directly correlated to the mass of binder and can also be performed on-site with a mobile LIBS-System. The application of a LIBS-system is presented. Calibration is required for quantitative analysis. Concrete cores were drilled, sliced and analyzed to determine the 2D-distribution of harmful elements. By comparing the chloride ingress and the carbonation, the interaction of both processes can be visualized in a measurement that takes less than 10 minutes for a 50 mm x 100 mm drill core. A leaflet on the use of LIBS for the chloride ingress assessment has been completed. T2 - NDT-CE 2022 - The International Symposium on Nendestructive Testing in Civil Engineering CY - Zurich, Switzerland DA - 16.08.2022 KW - Chlorides KW - Corrosion KW - Imaging KW - Service life KW - Damage assessment KW - LIBS PY - 2022 AN - OPUS4-56540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - On-line hyphenation of capillary electrophoresis with multicollector-ICP-MS (CE/MC-ICP-MS) for species-specific isotope ratio analysis of sulfur species N2 - In many scientific fields, isotopic analysis can offer valuable information, e.g., for tracing the origin of food products, environmental contaminants, forensic and archaeological samples (provenance determination), for age determination of minerals (geochronological dating) or for elucidating chemical processes. Up to date, typically bulk analysis is aimed at measuring the isotopic composition of the entire elemental content of the sample. However, the analyte element is usually present under the form of different elemental species. Thus, separating species of interest from one another and from matrix components prior to isotope ratio measurements can provide species-specific isotopic information, which could be used for tracing the origin of environmental pollutants and elucidation of (environmental) speciation. Using on-line hyphenations of separation techniques with multicollector-ICP-MS (MC-ICP-MS) can save time and effort and enables the analysis of different species during a single measurement. In this work, we developed an on-line hyphenation of CE with multicollector-ICP-MS (CE/MC-ICP-MS) for isotopic analysis of sulfur species. With this method, the isotopic composition of sulfur in sulfate originating from river water could be analyzed without sample preparation. The results were compared with data from off-line analysis of the same samples to ensure accuracy. The precision of the results of the on-line measurements was high enough to distinguish the rivers from one another by the isotopic signature of the river water sulfate. Next to environmental applications, a current field is species-specific isotopic analysis of biomolecules, as sulfur is the only covalently bound constituent of proteins which can be analyzed by MC-ICP-MS. Data analysis of transient signals in terms of isotope ratio determination is further issue - we developed a small free accessible App allowing for fast data analysis taking relevant aspects (e.g., mass bias correction, peak picking, …) into account. T2 - SCIX 2022 CY - Cincinnati, OH, USA DA - 02.10.2022 KW - CE KW - MC-ICP-MS KW - Speciation Analysis KW - Species-specific Isotope ratios PY - 2022 AN - OPUS4-56543 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hirsch, Philipp Daniel T1 - Roboterunterstütze Inspektion von stark gekrümmten Oberflächen mit Laserthermografie N2 - Zur Gewährleistung der Dauerhaftigkeit von Bauteilen sind regelmäßige Prüfungen notwendig. Für oberflächennahe Risse wurde bereits das Potenzial von Flying-Spot-Untersuchungen gezeigt, bei denen das Messfeld mit einem Laserpunkt, z.B. mittels eines Laserscanners, abgerastert wird. Eine Beschleunigung der Messung durch die Verwendung von Laserlinien ist möglich, wobei die Detektierbarkeit von Rissen u.a. von ihrer Ausrichtung zur Scanrichtung abhängt. Zudem können bei stark gekrümmten Oberflächen, wie z.B. denen von Turbinenschaufeln oder Maschinenteilen mit einem einzelnen stationären Messaufbau nur ein Teil der Oberfläche mit aktiver Thermografie auf Risse untersucht werden da die begrenzte Tiefenschärfe der optischen Systeme (Laser und Kamera)die mechanischen Nachführung innerhalb des Schärfentiefe-Bereichs erforderlich macht. Um eine vollständige Untersuchung der Oberfläche durchzuführen, sind daher mehrere Perspektiven notwendig. Die hier angewandte Laserthermografie erzeugt dabei die Relativbewegung durch die Manipulation des Prüfobjektes mit einem Roboterarm, welcher es erlaubt, komplexe Oberflächen abzuscannen. Es erfolgt ein systematisches Abfahren mit einer Laserlinie entlang zuvor geplanter Bahnen der gesamten erreichbaren Oberfläche. Da der Roboterarm das Prüfobjekt trägt, sind die eingesetzten Messsysteme unbeeinflusst. Die Bewegung des Prüfobjektes ist dabei mit vielen Freiheitsgraden möglich, was eine Optimierung für das Messproblem erlaubt. Es können unter anderem die Scangeschwindigkeit, Laserleistung, Laserspotgeometrie, Laserwellenlänge, Scanschema und Kamerabildrate variiert werden. Mithilfe der Positionsdaten des Roboterarms kann jedem Punkt auf dem Prüfkörper ein Temperaturverlauf zugeordnet werden, um einen ortsaufgelösten Temperaturverlauf zu erzeugen. Das Ziel ist es, die oberflächennahen Defekte zu detektieren und deren Position auf der Oberfläche des 3D Models positionsgenau darstellen zu können. In diesem Vortrag werden die Ergebnisse zur robotergestützten Thermografie an unterschiedlichsten Prüfkörpern vorgestellt. Vorteile gegenüber herkömmlichen Methoden werden erläutert und aktuelle Herausforderungen auf der Hard- und Softwareseite für den praktischen Einsatz diskutiert. T2 - Thermographie-Kolloquium 2022 CY - Saarbrücken, Germany DA - 28.09.2022 KW - Laserthermografie KW - Roboter KW - Risserkennung KW - Canny approach KW - Flying line thermography PY - 2022 AN - OPUS4-56545 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis A1 - Jurgelucks, B. A1 - Prager, Jens A1 - Walther, A. T1 - Defect Characterization in Plate Models Facilitated by Algorithmic Differentiation N2 - In non-destructive testing and structural health monitoring with ultrasonic waves, the quantification of damage in components is one of the main tasks. In many shell-like structures, such as plates, pipes, or laminate components, ultrasonic waves propagate as guided waves. Although guided waves enable the testing of large areas, their multimodal and dispersive properties make it challenging to analyze signals. So, there is a need for more advanced algorithms to handle these properties, especially when reconstructing damage position and geometry. The reconstruction can be formulated as an inverse problem where the measured signals are fitted with a simulative forward model. Due to the small wavelength of ultrasonic waves, classic forward models based on, e.g., the Finite Element Method are computationally intensive. In contrast, the authors use the semi-analytical Scaled Boundary Finite Element Method (SBFEM) to reduce the computational effort. The SBFEM approximates arbitrary long, undamaged parts of the structure with only a few degrees of freedom. This contribution summarizes a general inverse procedure based on algorithmic differentiation in combination with the SBFEM. Results are presented for damaged 2D cross-sectional models of waveguides. These results include an analysis of the robustness of the proposed algorithms against noise. T2 - DAGA 22 CY - Stuttgart, Germany DA - 21.03.2022 KW - Structural health monitoring KW - Inverse Methods KW - SBFEM KW - Algorithmic Differentiation KW - Non-destructive testing PY - 2022 VL - 2022 SP - 871 EP - 874 AN - OPUS4-56547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bulling, Jannis A1 - Jurgelucks, B. A1 - Prager, Jens A1 - Walther, A. T1 - Defect reconstruction in a two-dimensional semi-analytical waveguide model via derivative-based optimization N2 - This paper considers an indirect measurement approach to reconstruct a defect in a two-dimensional waveguide model for a non-destructive ultrasonic inspection via derivative-based optimization. The propagation of the mechanical waves is simulated by the scaled boundary finite element method that builds on a semi-analytical approach. The simulated data are then fitted to given data associated with the reflected waves from a defect which is to be reconstructed. For this purpose, we apply an iteratively regularized Gauss-Newton method in combination with algorithmic differentiation to provide the required derivative information accurately and efficiently. We present numerical results for three kinds of defects, namely, a crack, delamination, and corrosion. The objective function and the properties of the reconstruction method are investigated. The examples show that the parameterization of the defect can be reconstructed efficiently as well as robustly in the presence of noise. KW - Mechanical waves KW - Corrosion KW - Finite-element analysis KW - Ultrasonic testing KW - Nondestructive testing techniques KW - Symbolic computation KW - Materials analysis KW - MATLAB KW - Newton Raphson method PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565485 DO - https://doi.org/10.1121/10.0013574 VL - 152 IS - 2 SP - 1217 EP - 1229 PB - AIP Publ. CY - Melville, NY AN - OPUS4-56548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuner, Maximilian T1 - Quantification of ergot alkaloids - a glimpse into the future N2 - Mycotoxins (toxins formed by fungi) in food and have caused problems for mankind since the beginning of time. The group of ergot alkaloids plays a special role in human history. Several tens of thousands of deaths during the middle ages caused by to ergotism (the disease caused by continuous intake of ergot alkaloid contaminated food) underscore the importance of reliable analytical methods to ensure food safety. More than 50 compounds belong to the group of ergot alkaloids. The 12 most found structures – the major ergot alkaloids – are typically measured, when it comes to ergot alkaloid quantification. High performance liquid chromatography (HPLC) with a fluorescence detector (FLD) is typically used to quantify the ergot alkaloid content. The main disadvantage of this method are the high costs for calibration standards (12 different calibration substances are required). But also the time and effort required for the analysis of 12 peaks and overlapping signals that occur in complex food samples such as bread. As all ergot alkaloids share the ergoline structure and just differ in the substituents attached to this backbone, measurement of all ergot alkaloids in one sum parameter presents a time and cost saving alternative. The most important step for the development of such a sum parameter method is the reaction used to transfer all ergot alkaloids to one uniform structure. In the talk two promising reactions, the acidic esterification to lysergic acid methyl ester and hydrazinolysis to lysergic acid hydrazide, are examined for possible use in a routine analysis method. In addition to yield and reaction rate, factor such as the handling of the reaction and the possibility of parallelization play a role. Next to the current status of the ongoing research project, in this talk, current approaches to ergot alkaloid quantitation will be discussed. T2 - FOODMETNET MycoTWIN JOINT TRAINING COURSE 2022 CY - Gebze, Turkey DA - 22.11.2022 KW - Ergot alkaloids KW - Sum Parameter PY - 2022 AN - OPUS4-56586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Soraya A1 - Jaut, Valerie A1 - Schneider, Rudolf T1 - Ergometrine sensing in rye flour by a magnetic bead-based immunoassay followed by flow injection analysis with amperometric detection N2 - A certain group of mycotoxins, the ergot alkaloids, has caused countless deaths throughout human history. They are found in rye and other cereals and ingesting contaminated foods can cause serious health problems. To identify contaminated food exceeding the legal limits for ergot alkaloids, a portable and cost-effective test system is of great interest to the food industry. Rapid analysis can be achieved by screening for a marker compound, for which we chose ergometrine. We developed a magnetic bead-based immunoassay for ergometrine with amperometric detection in a flow injection system using a handheld potentiostat and a smartphone. With this assay a limit of detection of 3 nM (1 μg/L) was achieved. In spiked rye flour, ergometrine levels from 25 to 250 μg/kg could be quantified. All results could be verified by optical detection. The developed assay offers great promise to meet the demand for on-site ergometrine detection in the food industry. KW - Ergot alkaloids KW - Amperometry KW - Magnetic beads KW - Immunoassay KW - Food analysis KW - Fow injection analysis KW - Mycotoxins PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565906 DO - https://doi.org/10.1016/j.talanta.2022.124172 SN - 0039-9140 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. VL - 254 IS - 124172 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-56590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Memmolo, V. A1 - Lugovtsova, Yevgeniya A1 - Olino, M. A1 - Prager, Jens ED - Kundu, T. ED - Reis, H. ED - Ihn, J.-B. T1 - Application of Temperature Compensation Strategies for Ultrasonic Guided Waves to Distributed Sensor Networks N2 - Temperature compensation strategies play a key role in the implementation of guided wave based structural health monitoring approaches. The varying temperature influences the performance of the inspection system inducing false alarms or missed detection, with a consequent reduction of reliability. This paper quantitatively assesses two temperature compensation methods, namely the optimal baseline selection (OBS) and the baseline signal stretch (BSS), with the aim to extend their use to the case of distributed sensor networks (DSN). The effect of temperature separation between baseline time-traces in OBS and BSS are investigated considering multiple couples of sensors employed in the DSN. A decision strategy that uses frequent value warning to define the optimal baseline or stretching parameter is found to be effective analyzing data from two several experiments, which use different frequency analysis with either predominantly A0 mode or S0 mode data or both. The focus is given on the fact that different paths are available in a sensor network and several possible combinations of results are available. Nonetheless, introducing a frequent value warning it is possible to increase the efficiency of the OBS and BSS approach making use of fewer signal processing algorithms. In addition, the effectiveness of those approach is quantified using damage indicators as metric, which confirms that the performance of OBS and BSS quantitatively agree with predictions and also demonstrate that the use of compensation strategies improve detectability of damage with a higher reliability of the system. T2 - 2022 49th Annual Review of Progress in Quantitative Nondestructive Evaluation (QNDE 2022) CY - San Diego, CA, USA DA - 25.07.2022 KW - Ultrasound KW - Elastic waves KW - Structural Health Monitoring KW - Environmental Effects KW - Damage Detection PY - 2022 SN - 978-0-7918-8659-5 DO - https://doi.org/10.1115/QNDE2022-98534 SP - 1 PB - The American Society of Mechanical Engineers (ASME) CY - 2 Park Avenue, New York, NY 10016, USA AN - OPUS4-57074 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - EDC-WFD: A project to deliver reliable measurements for better monitoring survey and risks assessments. N2 - Monitoring programs should generate high-quality data on the concentrations of substances and other pollutants in the aquatic environment to enable reliable risk assessment. Furthermore, the need for comparability over space and time is critical for analysis of trends and evaluation of restoration of natural environment. Additionally, research work and exercises at the European level have highlighted that reliable measurements of estrogenic substances at the PNEC level are still challenging to achieve. The project EDC-WFD Metrology for monitoring endocrine disrupting compounds under the EU Water Framework Directive aims to develop traceable analytical methods for determining endocrine disrupting compounds and their effects, with a specific focus on three estrogens of the first watch list (17-beta-estradiol (17βE2), 17-alpha-ethinylestradiol (EE2), and estrone (E1)). Estrogens 17-alpha-estradiol (17E2) and estriol (E3) will be included to demonstrate the reliability of the developed methods and to support the requirements of Directive 2013/39/EC, Directive 2009/90/EC and Commission Implementation Decision (EU) 2018/840, hence improving the comparability and compatibility of measurement results within Europe. During the EDC-WFD project four selected effect-based methods (EBM) will be deeply investigated in order to improve their rationale use and their support in water quality assessment. In particular, the EBM sensitivity, specificity and accuracy on reference materials with single or mixture solutions of the five substances at a concentration of EQS values will be explored. This contribution will present the objectives and methods applied within the EDC-WFD project. T2 - EuChemS CY - Lisbon, Portugal DA - 29.08.2022 KW - WFD KW - Estrogens KW - Whole water samples KW - EQS PY - 2022 AN - OPUS4-57096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - A method for monitoring estrogens in whole surface waters by GC-MS/MS N2 - Natural and synthetic estrogens are key endocrine-disrupting chemicals. Despite occurring at ultra-trace levels (below ng L-1), it is believed that they are contributing to an increase in feminized fish and other endocrine disruptive effects, and hence, their inclusion in the Watch list was not unexpected. One of the main sources ofestrogens to surface waters is wastewater effluent. Once in surface waters, they can partition into different compartments, i.e., water and suspended particulate matter. For this reason, there is an urgent need for a methodology to monitor estrogen levels below the environmental quality standards (EQS) set by the Water Framework Directive requirements. In this study, a precise and accurate gas chromatography-mass spectrometry method (GC-MS/MS) for the analysis of estrone (E1), 17β-estradiol (17β-E2), 17α-estradiol (17α- E2), 17-alpha-ethinylestradiol (EE2), and estriol (E3) in whole water samples with ng L-1 limit of quantification (LOQ) was developed and validated in accordance with CEN/TS 16800:2020 guidelines. T2 - IMSC 2022 CY - Maastricht, Netherlands DA - 27.08.2022 KW - EDC KW - WFD KW - GC-MS PY - 2022 AN - OPUS4-57097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Wilsch, Gerd A1 - Gornushkin, Igor B. A1 - Kratochvilo, L. A1 - Pořízka, P. A1 - Kaiser, J. A1 - Millar, S. A1 - et al., T1 - Interlaboratory comparison for quantitative chlorine analysis in cement pastes with laser induced breakdown spectroscopy N2 - Concrete structures experience severe damage during service, for example due to pitting corrosion of rebars caused by the ingress of chlorine (Cl) into the porous concrete structure. The ingress can be monitored using laser-induced breakdown spectroscopy (LIBS), a recently introduced civil engineering technique used to detect Cl in concrete structures in addition to conventional wet chemistry methods. The key advantages of LIBS are high spatial resolution, which is important when analyzing heterogeneous concrete samples, as well as the almost complete absence of sample preparation. To assess LIBS as a reliable analytical method, its accuracy and robustness must be carefully tested. This paper presents the results of an interlaboratory comparison on the analysis of Cl in cement paste samples conducted by 12 laboratories in 10 countries. Two sets of samples were prepared with Cl content ranging from 0.06 to 1.95 wt% in the training set and 0.23–1.51 wt% in the test set, with additional variations in the type of cement and Cl source (salt type). The overall result shows that LIBS is suitable for the quantification of the studied samples: the average relative error was generally below 15%. The results demonstrate the true status quo of the LIBS method for this type of analysis, given that the laboratories were not instructed on how to perform the analysis or how to process the data. KW - LIBS KW - Interlaboratory comparison KW - Round robin test KW - Cement KW - Chlorine PY - 2023 DO - https://doi.org/10.1016/j.sab.2023.106632 SN - 0584-8547 VL - 202 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-57102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Bestimmung von anthropogenen Markerkonzentrationen für die SARS-CoV-2 Quantifizierung mittels eines Hochdurchsatzverfahrens (ELISA) N2 - Vortrag zum Kick-off des Projektes. Ziel des Projektes ist es, die Eignung der Bestimmung eines oder mehrerer der genannten anthropogenen Marker im Abwasser zur Volumenkorrektur („Kalibration“) im SARS-CoV-2-Monitoring von Abwässern auf der Basis eines von der BAM zu erhebenden Messdatensatzes zu evaluieren. T2 - Kick-off Meeting zum Projekt MARKERIA (VH1802) CY - Berlin, Germanyy DA - 01.04.2022 KW - Biosensoren KW - Immunoassay KW - SARS-CoV-2 PY - 2022 AN - OPUS4-57109 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Bestimmung von anthropogenen Markerkonzentrationen für die SARS-CoV-2 Quantifizierung mittels eines Hochdurchsatzverfahrens (ELISA) N2 - ESI-CorA ist ein nationales Verbundprojekt mit dem Ziel des Nachweises von SARS-CoV-2 im Abwasser. Das UBA hat als Teilprojekt das Projekt MARKERIA (VH1802) an die BAM vergeben. Ziel des Projektes ist es, die Eignung der Bestimmung eines oder mehrerer der genannten anthropogenen Marker im Abwasser zur Volumenkorrektur („Kalibration“) im SARS-CoV-2-Monitoring von Abwässern auf der Basis eines von der BAM zu erhebenden Messdatensatzes zu evaluieren. T2 - 12. Sitzung des Begleitkreises des nationalen Verbundprojektes ESI-CorA CY - Online meeting DA - 13.06.2022 KW - Biosensoren KW - Immunoassay KW - SARS-CoV-2 PY - 2022 AN - OPUS4-57110 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lozano, Daniel A1 - Bulling, Jannis A1 - Prager, Jens T1 - Quadtree decomposition as a meshing strategy for guided waves simulations using the scaled boundary finite element method N2 - Structural health monitoring techniques associate strongly with damage detection and characterization. Ultrasonic guided waves (UGW), for such scope, arise as one of the most promising methods for many reasons i.e. UGW are able to travel long distances and they have high sensitivity to damage. In this context, the necessity to model realistic wave-defect interaction occurs to be critical. Realistic damage scenarios can be modeled through the usage of image-based quadtree meshes. Images, such as the outcome from X-ray scans, C-scans, etc., can be converted into meshes for further integration in a computational domain. Quadtree meshes are created by converting the intensity of the pixels to quadrilateral cells. Homogeneous regions inside one image result in one quad, whereas fine features such as discontinuities can be described with smaller quads. This contribution proposes an efficient methodology to model wave defect interaction, using as a framework the scaled boundary finite element method (SBFEM) and quadtree meshes. Problems as non-conforming regions in the mesh due to the space tree decomposition can be easily avoided using SBFEM’s polygonal elements. Moreover, the semi-analytical nature of the SBFEM allows the modeling of arbitrarily long prismatic/undamaged regions of the waveguides without an increase in the computational burden. T2 - DAGA 2022 CY - Stuttgart, Germany DA - 21.03.2022 KW - Wave defect interaction KW - Scaled Boundary Finite Element Method KW - Quadtree meshes KW - Image-based models KW - Transient analysis PY - 2022 SP - 887 EP - 890 CY - Stuttgart AN - OPUS4-57153 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pramann, A. A1 - Vogl, Jochen A1 - Flierl, L. A1 - Rienitz, O. T1 - Determination of absolute (SI‐traceable) isotope ratios: The use of Gravimetric Isotope Mixtures N2 - The presentation is brief overview on how to use gravimetric isotope mixtures to determine SI traceable isotope ratios. There is no mass spectrometer on earth that directly measures isotope ratios. Mass spectrometers will always measure signal intensity ratios instead. The actual problem is that the measured intensity ratios differ more or less from the isotope ratios. The difference can be up to more than 10 % in case of lithium while it‘s below 1 % in case of the heavier elements like lead or uranium. Consequently, the signal intensity ratios are expressed for example in V/V depending on the type of mass spectrometer you are using, while the isotope ratios are expressed in mol/mol. This phenomenon is called Instrumental Isotopic Fractionation (or short IIF) but the more common name is still mass bias (even though this name is not entirely correct). To convert the measured into the isotope ratio usually a simple multiplication with a so-called correction (or short K) factor is done. Therefore, the problem is to determine the K factor. In absence of isotope reference materials the golden route is via gravimetric isotope mixtures, which will be explained within the presentation. T2 - CCRI-CCQM Workshop on the use of mass spectrometry in radionuclide metrology: Opportunities and challenges - Video Tutorial CY - Online meeting DA - 14.02.2023 KW - Absolute isotope ratio KW - Traceability KW - Uncertainty KW - Isotope mixtures PY - 2023 AN - OPUS4-57172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pollack, M. T1 - Functionalized poly(ethylene glycol)s (PEGs) as a reference material for detection of polymeric end groups via SEC hyphenated with FTIR and 1H-NMR (80 MHz) N2 - Benchtop 1H-NMR and FTIR have both been successfully developed for size-exclusion chromatography (SEC) applications. The latest implementations of these methods by Wilhelm and collaborators[1-3] have taken advantage of commerically available low-cost equipment, and a provide a means to obtain slice-by-slice spectra for the monitoring of functional groups in polymer separations. Demonstrated applications include the detection of highly diluted chains in a polymer blend (e.g., PS/PMMA), copolymer content determination (e.g., styrene-methyl methacrylate), and butadiene isomer detection. To synthesize and characterize an end-labelled low molecular wt. poly(ethylene glycol) as a model polymer to aid in the development and validation of spectroscopic detection (FTIR and 1H-NMR) for SEC applications. A particular focus is to improve quantitation and/or detection of highly diluted funtional groups (e.g., polymer chain ends or sparsely functionalized chains) In the first approach, an isocyanate with IR- and NMR-active functional groups was reacted with PEG (4000 and 10000 g/mol) to form end-functionalized chains by means of an addition reaction. The functionalization of the 10000 g/mol PEG was found to be non-homogeneous (not discussed further). The 4000 g/mol PEG was successfully functionalized to 100%, found to be homogeneous across the molecular weight distribution and could therefore serve as a model polymer for analysis by the coupled methods. T2 - 10th International Symposium on the Separation and Charcterization of Natural and Synthetic Macromolecules CY - Amsterdam, Netherlands DA - 01.02.2023 KW - PEG KW - Reference materials KW - NMR KW - MALDI-TOF MS PY - 2023 AN - OPUS4-57071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Bestimmung von anthropogenen Markerkonzentrationen für die SARS-CoV-2 Quantifizierung mittels eines Hochdurchsatzverfahrens (ELISA) N2 - 1. Projektreffen mit dem Umweltbundesamt für das Projekt MARKERIA (VH1802). Ziel des Projektes ist es, die Eignung der Bestimmung eines oder mehrerer der genannten anthropogenen Marker im Abwasser zur Volumenkorrektur („Kalibration“) im SARS-CoV-2-Monitoring von Abwässern auf der Basis eines von der BAM zu erhebenden Messdatensatzes zu evaluieren. T2 - 1. Projekttreffen mit dem UBA zum Projekt MARERIA (VH1802) CY - Berlin, Germany DA - 15.09.2022 KW - Biosensoren KW - Immunoassay KW - SARS-CoV-2 PY - 2022 AN - OPUS4-57111 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Bestimmung von anthropogenen Markerkonzentrationen für die SARS-CoV-2 Quantifizierung mittels eines Hochdurchsatzverfahrens (ELISA) N2 - 2. Projekttreffen mit dem Umweltbundesamt zum Projekt MARKERIA (VH1802). Ziel des Projektes ist es, die Eignung der Bestimmung eines oder mehrerer der genannten anthropogenen Marker im Abwasser zur Volumenkorrektur („Kalibration“) im SARS-CoV-2-Monitoring von Abwässern auf der Basis eines von der BAM zu erhebenden Messdatensatzes zu evaluieren. T2 - 2. Projekttreffen mit dem UBA zum Projekt MARKERIA (VH1802) CY - Berlin, Germany DA - 25.11.2022 KW - Biosensoren KW - Immunoassay KW - SARS-CoV-2 PY - 2022 AN - OPUS4-57112 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Becher, S. A1 - Dierckes, G. A1 - Langhammer, Nicole A1 - Cossmer, Antje A1 - von der Au, Marcus A1 - Göckener, B. A1 - Fliedner, A. A1 - Rüdel, H. A1 - Koschorreck, J. A1 - Meermann, Björn T1 - Quantification and characterization of PFASs in suspended particulate matter (SPM) of German rivers using EOF, dTOPA, (non-)target HRMS N2 - In this study, we compare analytical methods for PFAS determination–target analysis, non-target screening (NTS), direct total oxidizable precursor assay (dTOPA) and extractable organically bound fluorine (EOF). Therefore, suspended particulate matter (SPM) samples from German rivers at different locations in time series from2005 to 2020 were analyzed to investigate temporal and spatially resolved trends. In this study 3 PFAS mass balances approaches were utilized: (i) PFAA target vs. PFAS dTOPA, (ii) PFAS target vs. EOF and (iii) PFAS target vs. PFAS dTOPA vs. organofluorines NTS vs. EOF. Mass balance approach (i) revealed high proportions of precursor substances in SPM samples. For the time resolved analysis an increase from 94% (2005) to 97% in 2019 was observable. Also for the spatial resolved analysis precursor proportions were high with >84% at all sampling sites. Mass balance approach (ii) showed that the unidentified EOF (uEOF) fraction increased over time from82% (2005) to 99% (2019). Furthermore, along the river courses the uEOF increased. In the combined mass balance approach (iii) using 4 different analytical approaches EOF fractions were further unraveled. The EOF pattern was fully explainable at the sampling sites at Saar and Elbe rivers. For the time resolved analysis, an increased proportion of the EOF was now explainable. However, still 27% of the EOF for the time resolved analysis and 25% of the EOF for the spatial resolved analysis remained unknown. Therefore, in a complementary approach, both the EOF and dTOPA reveal unknown gaps in the PFAS mass balance and are valuable contributions to PFAS risk assessment. Further research is needed to identify organofluorines summarized in the EOF parameter. KW - PFAS KW - HR-CS-GFMAS KW - Fluorine KW - SPM KW - LC-MS/MS PY - 2023 DO - https://doi.org/10.1016/j.scitotenv.2023.163753 SN - 1879-1026 SN - 0048-9697 VL - 885 SP - 1 EP - 12 PB - Elsevier Science CY - Amsterdam AN - OPUS4-57429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope Ratio Measurements and Certification of iCRMs at BAM N2 - A short overview on isotope ratio measurements at BAM and related CRM activities is given. The current isotope CRM range offered by BAM and future iCRM projects are presented. T2 - CCQM IRWG Meeting CY - Sevres, France DA - 24.04.2023 KW - Absolute isotope ratio KW - Reference material KW - Metrology KW - Traceability PY - 2023 AN - OPUS4-57399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - IRWG strategy update N2 - An update of the IRWG strategy for the period 2023-2030 is given. The status and the futuere work of the task group on quantities, symbols and units is discussed. The present status of IRWG comparisons is shown and the need for specific key comparisons is discussed. T2 - CCQM IRWG Meeting CY - Sevres, France DA - 24.04.2023 KW - Isotope ratio KW - Traceability KW - Metrology PY - 2023 AN - OPUS4-57400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Plan for comparison on absolute Cu isotope ratios by applying the isotope mixture approach N2 - The reference method for obtaining absolute isotope ratios still is the isotope mixture approach. Due the huge efforts required the full isotope mixture approach is applied only by a few institutes worldwide. To enable an IRWG key comparison with a sufficiently large number of participants a proposal for absolute cu isotope ratios is presented where participants will be provided with the enriched isotopes, the isotope mixtures and the samples. In parallel a pilot study will be organized where alternative approaches for obtaining absolute Cu isotope ratios can be applied. T2 - CCQM IRWG Meeting CY - Sevres, France DA - 24.04.2023 KW - Absolute isotope ratio KW - Traceability KW - Metrology PY - 2023 AN - OPUS4-57401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - Analyse von PFAS mittels (Non-)Target HRMS, dTOPA und EOF in Schwebstoff-Proben aus Zeitreihen der Umweltprobenbank N2 - Per- und polyfluorierte Alkylverbindungen (PFAS) sind eine Substanzklasse bestehend aus mehreren tausenden Einzelverbindungen. Unter PFAS zählen alle Verbindungen, die mindestens eine perfluorierte Methyl- (-CF3) oder Methylen-Gruppe (-CF2-) besitzen.[1] Somit zählt auch ein großer Teil der fluorierten Medikamente, Pflanzenschutzmittel oder Biozide in die PFAS-Substanzklasse. Aufgrund der Persistenz, Bioakkumulation in Nahrungsketten, Toxizität und der ubiquitären Verbreitung von PFAS zählen sie zu den „emerging pollutants“.[2] Die PFAS-Analytik ist wegen ihrer vielfältigen physikalisch-chemischen Eigenschaften und der sehr hohen Anzahl an PFAS eine große Herausforderung. Da es für viele Anwendungen noch ungewiss ist, welche PFAS verwendet werden, wie sie in die Umwelt gelangen und welche Transformations- bzw. Abbauprodukte entstehen, stoßen analytische Ansätze, die nur auf Einzelsubstanzen abzielen, hier an ihre Grenzen. PFAS-Summenparameter-Methoden, die darauf abzielen ein möglichst vollständiges Abbild der PFAS-Belastungssituation widerzuspiegeln, werden daher immer wichtiger. T2 - Wasser 2023 CY - Augsburg, Germany DA - 14.05.2023 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine KW - SPM KW - Schwebstoffe KW - LC-HRMS PY - 2023 AN - OPUS4-57516 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Flierl, Lukas A1 - Rienitz, Olaf A1 - Vogl, Jochen A1 - Pramann, Axel T1 - An advancement of the gravimetric isotope mixture method rendering the knowledge of the spike purity superfluous N2 - The gravimetric isotope mixture method is the primary method to determine absolute isotope ratios. This method, however, depends on the existence of suitable spike materials and knowledge of their purities. Determining the purity of the spikes can be tedious and labour-intensive. In this publication, an advancement of the gravimetric isotope mixture method, rendering the determination of the purity of the spike materials unnecessary, is presented. The advancement combines mass spectrometry and ion chromatography leading to an approach being independent of the purity of the spike materials. In the manuscript the mathematical background and the basic idea of the novel approach are described using a two-isotope system like copper or lithium. KW - Isotope amount ratios KW - Metrology KW - Mass spectrometry KW - Ion chromatography PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608726 DO - https://doi.org/10.1007/s00216-024-05465-9 SP - 5325 EP - 5333 PB - Springer Science and Business Media LLC AN - OPUS4-60872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wulfes, Birte S. T1 - Rekombinante Herstellung und explorative Anwendung immobilisierter, thermostabiler Trypsin-Varianten für die Bottom-Up-Proteomik N2 - Die Erforschung des Proteoms, der Gesamtheit der Proteine eines Lebewesens, ist von großer Bedeutung für das Verständnis biologischer Systeme. Aufgrund dessen ist die Proteomik ist eines der bedeutendsten aktuellen Forschungsfelder der Biowissenschaften. In der Bottom-Up-Proteomik werden die Proteine einer Probe vor ihrer Analyse einem enzymatischen Verdau mit Proteasen unterzogen, was eine erleichterte Analyse mit hohem Durchsatz ermöglicht. Aufgrund seiner hohen Aktivität und Effektivität hat sich die Serinprotease Trypsin als Standard-Enzym der Proteomik etabliert. Die weitere Verbesserung ihrer Enzymcharakteristika, wie Thermostabilität und Aktivität, ist unter anderem durch Immobilisierung an ein Trägermaterial oder genetische Modifikation möglich. In der vorliegenden Arbeit wurde eine von Xiao et al. 2023 entwickelte thermostabile Trypsin-Variante mit erhöhter Oberflächen-Hydrophobizität rekombinant in E. coli hergestellt und sowohl immobilisiert als auch in Lösung hinsichtlich ihrer Enzymaktivität und Thermostabilität im Vergleich zum Wildtyp charakterisiert. Die vorliegende Arbeit stellt dabei eine Erstbeschreibung der Immobilisierung einer thermostabilen Trypsin-Spezies an ein Trägermaterial dar und untersucht somit erstmalig das Zusammenspiel der beiden Optimierungsstrategien Immobilisierung und genetische Modifikation. Das thermostabile Trypsin und sein Wildtyp wurden rekombinant als Zymogene hergestellt, wobei trotz verschiedener Strategien zum Erhalt der nativen Konformation, wie der Fusion mit dem Chaperon-ähnlichen Maltose-bindenden Protein (MBP), eine starke Aggregation in Einschlusskörperchen (inclusion bodies, IB) erfolgte. Im Zuge der Rückfaltung der fehlgefalteten Proteine wurden verschiedene Rückfaltungsbedingungen untersucht, wobei die Vorteile einer langsamen Absenkung des Gehalts der Denaturierungsreagenz in Kombination mit einem Cystein-Cystine- Redoxsystem dargelegt werden konnten. Es konnte keine Verbesserung der Aktivität und Thermostabilität des genetisch modifizierten Enzyms in freier Form festgestellt werden, jedoch eine erhöhte Substrataffinität. Durch Immobilisierung an Magnetbeads mit tosylfunktionalisierter Oberfläche konnte die Enzymaktivität der genetisch modifizierten Trypsin-Variante bei 80 °C vollständig erhalten werden, während die Aktivität des Wildtyps verringert wurde. Dies legt nahe, dass die erhöhte Oberflächen-Hydrophobizität der modifizierten Trypsin-Variante zu einer erhöhten Bindung an das Trägermaterial beiträgt, was eine Verbesserung der Stabilität bei thermischer Erhitzung bewirkt. KW - Rekombinante Proteine KW - Proteomik KW - Thermostabile Enzyme KW - Immobilisierung PY - 2024 SP - 1 EP - 149 PB - Technische Universität Berlin CY - Berlin AN - OPUS4-60885 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mangarova, Dilyana Branimirova T1 - A novel ADAMTS-specific MR peptide probe for characterization of atherosclerotic plaques in a murine model N2 - Motivation: A precise diagnosis of atherosclerosis is of clinical importance, since cardiovascular disease remain one of the leading causes of death worldwide. Goal(s): The goal of this study was to evaluate the feasibility of characterizing a disintegrin and metalloproteinase with thrombospondin motifs (ADAMTS4) using molecular magnetic resonance imaging in a preclnical model of atherosclerosis. Approach: Molecular magnetic resonance imaging using a novel probe targeted against ADAMTS4 was used in a high-fat murine model. Results: It was possible to image atherosclerotic lesions in a mouse model using an ADAMTS4- specific probe for magnetic resonance imaging. Impact: Using molecular MRI targeting ADAMTS4 is a promising method for characterization of plaque composition and could possibly impact plaque vulnerability assessment in the diagnosis and treatment of atherosclerosis in patients. N2 - Motivation: Eine genaue Diagnose der Atherosklerose ist von klinischer Bedeutung, da Herz-Kreislauf-Erkrankungen nach wie vor eine der häufigsten Todesursachen weltweit sind. Ziel(e): Ziel dieser Studie war es, die Durchführbarkeit der Charakterisierung einer Desintegrin- und Metalloproteinase mit Thrombospondin-Motiven (ADAMTS4) mittels molekularer Magnetresonanztomographie in einem präklinischen Modell der Atherosklerose zu untersuchen. Herangehensweise: Molekulare Magnetresonanztomographie mit einer neuartigen, gegen ADAMTS4 gerichteten Sonde wurde in einem fettreichen Mausmodell eingesetzt. Ergebnisse: Es war möglich, atherosklerotische Läsionen in einem Mausmodell mit einer ADAMTS4-spezifischen Sonde für die Magnetresonanztomographie abzubilden. Auswirkungen: Die Verwendung einer molekularen MRT, die auf ADAMTS4 abzielt, ist eine vielversprechende Methode zur Charakterisierung der Plaque-Zusammensetzung und könnte sich möglicherweise auf die Bewertung der Plaque-Anfälligkeit bei der Diagnose und Behandlung von Atherosklerose bei Patienten auswirken. T2 - 2024 ISMRM & ISMRT Annual Meeting & Exhibition CY - Singapore DA - 04.05.2024 KW - ADAMTS4 KW - Peptide probe KW - Peptide binder KW - Selective peptide KW - International Society for Magnetic Resonance in Medicine PY - 2024 AN - OPUS4-60865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, Philipp A1 - Vogel, Christian A1 - Schuck, G. A1 - Simon, Franz-Georg T1 - Speciation of copper and zinc compounds relevant for the hazard property (HP) 14 classification of municipal solid waste incineration bottom and fly ashes N2 - The analysis of the presence and content of substances that are toxic to aquatic life in waste is essential for classification of waste with regard to hazard property (HP) 14 ‘ecotoxic’. For the determination of HP14 classified copper (Cu) and zinc (Zn) compounds in various municipal solid waste incineration bottom ashes (IBA) and one fly ash (FA) from Germany we applied X-ray absorption near-edge structure (XANES) spectroscopy in combination with linear combination fitting. The analysis showed that approx. 50–70% of Cu in the IBA are Cu(I) compounds and elemental Cu(0), but these compounds were not equally distributed in the different IBA. In contrast, the majority (approx. 50–70%) of Zn in all IBA is elemental zinc, which originates from brass or other alloys and galvanized metals with a large content of zinc in the waste. The FA contain higher mass fraction on Zn and other toxic elements, but similar Cu and Zn species. Additional performed selective extraction at a pH of 4 with an organic acid of some IBA showed that the ecotoxic Zn fraction is mainly elemental zinc and zinc oxide. In contrast, for the ecotoxic Cu fraction within the IBA no specific compound could be identified. Furthermore, the XANES analysis showed that the HP14 properties of especially Cu in IBA is overestimated with current best-practice guidelines for sample processing for the current substance-related approach with the 0.1% cut-off rule for each substance. However, it should be considered whether it would not be better from an environmental point of view to take the ecotoxicologically leachable copper and zinc as a reference value. KW - Thermal waste treatment KW - XANES spectroscopy KW - Ecotoxicity KW - Incineration bottom ash PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609584 DO - https://doi.org/10.1016/j.wasman.2024.09.001 VL - 189 SP - 421 EP - 426 PB - Elsevier Ltd. AN - OPUS4-60958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wegner, Karl David A1 - Hildebrandt, N. T1 - Near infrared quantum dots for biosensing and bioimaging N2 - Quantum dots (QDs) possess unique optoelectronic properties, which make them very attractive to be used as optical probes in biosensing and bioimaging applications. The strong absorbance and light scattering of biological compounds like tissue and blood in the visible range pose a problem. However, if optical probes emitting in the near-infrared (NIR) range are used, scattering, absorption, and autofluorescence of biological components are strongly reduced. This allows for an increased light penetration depth and higher spatial and temporal resolution for the investigation of biological processes. The synthesis and application of NIR emitting QDs is a fast-growing research field and the benefits of using QDs were demonstrated for a variety of applications, such as photoelectrochemical biosensor, in vivo vascular imaging, and fluorescence-guided surgery. This article reviews the state-of-the-art developments in the preparation of NIR/IR QDs and highlights the latest research about their utilization in biosensing and bioimaging applications. KW - Quantum dots KW - Near-infrared KW - Biosensing KW - Bioimaging KW - NIR-II / SWIR KW - Advanced nanomaterials PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609708 SN - 0165-9936 DO - https://doi.org/10.1016/j.trac.2024.117922 VL - 180 SP - 1 EP - 19 PB - Elsevier B.V. AN - OPUS4-60970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sunderkötter, Jan T1 - Eurachem - a network and expert forum for young scientists N2 - Eurachem is an international network of national organisations having the objective of establishing a system for the international traceability of chemical measurements and the promotion of good quality practices. It also provides a forum for discussing common problems and exchanging information on quality assurance issues in analytical chemistry. The presentation will explain how Eurachem is organised, the requirements for participation and the opportunities for collaboration and networking. In particular, it will discuss why Eurachem offers an interesting network for young scientists to exchange experiences and further their own education. T2 - Doktorandenseminar der GDCh CY - Mannheim, Germany DA - 31.07.2024 KW - Eurachem KW - Network PY - 2024 AN - OPUS4-60923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Yi A1 - Danischewski, Julia A1 - Molnar, Brian A1 - Riedel, Jens A1 - Shelley, Jacob T1 - Manipulation of Gaseous Ions with Acoustic Fields at Atmospheric Pressure N2 - The ability to controllably move gaseous ions is an essential aspect of ion-based spectrometry (e.g., mass spectrometry and ion mobility spectrometry) as well as materials processing. At higher pressures, ion motion is largely governed by diffusion and multiple collisions with neutral gas molecules. Thus, high-pressure ion optics based on electrostatics require large fields, radio frequency drives, complicated geometries, and/or partially transmissive grids that become contaminated. Here, we demonstrate that low-power standing acoustic waves can be used to guide, block, focus, and separate beams of ions akin to electrostatic ion optics. Ions preferentially travel through the static-pressure regions (“nodes”) while neutral gas does not appear to be impacted by the acoustic field structure and continues along a straight trajectory. This acoustic ion manipulation (AIM) approach has broad implications for ion manipulation techniques at high pressure, while expanding our fundamental understanding of the behavior of ions in gases. KW - Ion mobility spectrometry KW - Acoustic KW - Mass spectrometry PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600704 DO - https://doi.org/10.1021/jacs.4c01224 SP - 1 EP - 6 PB - ACS Publications AN - OPUS4-60070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Janina A1 - Kaufmann, Jan Ole A1 - Weller, Michael G. T1 - Simple Determination of Affinity Constants of Antibodies by Competitive Immunoassays N2 - The affinity constant, also known as the equilibrium constant, binding constant, equilibrium association constant, or the reciprocal value, the equilibrium dissociation constant (Kd), can be considered as one of the most important characteristics for any antibody–antigen pair. Many methods based on different technologies have been proposed and used to determine this value. However, since a very large number of publications and commercial datasheets do not include this information, significant obstacles in performing such measurements seem to exist. In other cases where such data are reported, the results have often proved to be unreliable. This situation may indicate that most of the technologies available today require a high level of expertise and effort that does not seem to be available in many laboratories. In this paper, we present a simple approach based on standard immunoassay technology that is easy and quick to perform. It relies on the effect that the molar IC50 approaches the Kd value in the case of infinitely small concentrations of the reagents. A two-dimensional dilution of the reagents leads to an asymptotic convergence to Kd. The approach has some similarity to the well-known checkerboard titration used for the optimization of immunoassays. A well-known antibody against the FLAG peptide, clone M2, was used as a model system and the results were compared with other methods. This approach could be used in any case where a competitive assay is available or can be developed. The determination of an affinity constant should belong to the crucial parameters in any quality control of antibody-related products and assays and should be mandatory in papers using immunochemical protocols. N2 - Die Affinitätskonstante, auch bekannt als Gleichgewichtskonstante, Bindungskonstante, Gleichgewichtsassoziationskonstante oder der reziproke Wert, die Gleichgewichtsdissoziationskonstante (Kd), kann als eine der wichtigsten Eigenschaften für jedes Antikörper-Antigen-Paar angesehen werden. Zur Bestimmung dieses Wertes wurden zahlreiche Methoden auf der Grundlage verschiedener Technologien vorgeschlagen und verwendet. Da jedoch eine sehr große Anzahl von Veröffentlichungen und kommerziellen Datenblätter diese Information nicht enthalten, scheint es erhebliche Hindernisse bei der Durchführung solcher Messungen zu geben. In anderen Fällen, in denen solche Daten angegeben werden, haben sich die Ergebnisse häufig als unzuverlässig erwiesen. Diese Situation könnte darauf hindeuten, dass die meisten der heute verfügbaren Technologien ein hohes Maß an Fachwissen und Aufwand erfordern, das in vielen Labors nicht vorhanden zu sein scheint. In diesem Beitrag stellen wir einen einfachen Ansatz vor, der auf der Standard-Immunoassay-Technologie basiert und einfach und schnell durchführbar ist. Er beruht auf dem Effekt, dass sich der molare IC50 bei unendlich kleinen Reagenz-Konzentrationen dem Kd-Wert annähert. Eine zweidimensionale Verdünnung der Reagenzien führt zu einer asymptotischen Konvergenz zu Kd. Der Ansatz hat eine gewisse Ähnlichkeit mit der bekannten Checkerboard-Titration, die zur Optimierung von Immunoassays verwendet wird. Ein bekannter Antikörper gegen das FLAG-Peptid, Klon M2, wurde als Modellsystem verwendet, und die Ergebnisse wurden mit anderen Methoden verglichen. Dieser Ansatz kann überall dort angewendet werden, wo ein kompetitiver Assay verfügbar ist oder entwickelt werden kann. Die Bestimmung einer Affinitätskonstante sollte zu den entscheidenden Parametern bei der Qualitätskontrolle von Antikörperprodukten und -assays gehören und in Arbeiten, die immunchemische Protokolle verwenden, obligatorisch sein. KW - ELISA KW - Competitive immunoassay KW - IC50 KW - Test midpoint KW - Point of inflection KW - Equilibrium constant KW - Dissociation constant KW - Binding strength KW - Antibody antigen complex KW - Bio-interaction KW - SPR KW - Surface-plasmon resonance KW - FLAG peptide KW - Clone M2 KW - Antibody quality PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-605607 DO - https://doi.org/10.3390/mps7030049 SN - 2409-9279 VL - 7 IS - 3 SP - 1 EP - 11 PB - MDPI CY - Basel AN - OPUS4-60560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hill, Sarah A1 - Infante, Heidi Goenaga A1 - Entwisle, John A1 - Strekopytov, Stanislav A1 - Ward-Deitrich, Christian A1 - Cowen, Simon A1 - Rienitz, Olaf A1 - Roethke, Anita A1 - Goerlitz, Volker A1 - Schulz, Ursula A1 - Pape, Carola A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Jacimovic, Radojko A1 - Fisicaro, Paola A1 - Ren, Tongxiang A1 - Wang, Song A1 - Song, Panshu A1 - Li, Haifeng A1 - Linsky, Maré A1 - Sobina, Egor A1 - Lozano, Hernán Ezequiel A1 - Puelles, Mabel A1 - Yamani, Randa A1 - Haraldsson, Conny T1 - CCQM-K160: platinum group elements in automotive catalyst N2 - The platinum group elements (PGEs) play an important role in reducing emissions from automotive vehicles through their use in catalytic convertors but also for catalysis in the pharmaceutical industry. The immense economic value of platinum (Pt), palladium (Pd) and rhodium (Rh) highlights the importance of highly accurate measurements. Therefore, there is a need for National Metrology Institutes (NMIs) and Designated Institutes (DIs) to demonstrate measurement capability in this space. A pilot comparison (CCQM-P63) for precious metals in automotive catalyst took place in 2006, but with a limited number of institutes participating. Furthermore, this study was performed over 17 years ago. Therefore, there was a need to maintain existing capability and demonstrate new capability in a key comparison, in order to claim calibration and measurement capability claims (CMCs). With the core capability matrix, this study falls into the "Difficult to dissolve metals/metal oxides" which will support CMC categories 8 (Metal and metal alloys), 9 (Advanced materials) and 14 (Other materials). Eleven NMIs and DIs participated in the Key Comparison CCQM-K160 Platinum Group Elements in Automotive Catalyst. Participants were requested to evaluate the mass fractions of Pt, Pd and Rh in mg/kg in an unused autocatalyst material (cordierite ceramic base). The Key Comparison Reference Values (KCRVs) and Degrees of Equivalence (DoEs) were calculated utilising the NIST Decision Tree for the measurands. The participants utilised a number of sample preparation and analytical methods including hot plate digestion, microwave digestion and sodium fusion, followed by either atomic absorption spectroscopy (AAS), inductively coupled plasma optical emission spectroscopy (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS) detection. Several calibration techniques were used, namely external calibration, standard addition, isotope dilution mass spectrometry (IDMS) and an exact matching procedure. Additionally, one participant employed instrumental neutron activation analysis (INAA) with k0 standardisation which is a direct solid analysis method. The majority of participants claimed traceability to NIST primary calibrants or their own CRMs. Furthermore, several matrix CRMs were included or spiked samples for quality control. All institutes were required to determine the dry mass fraction using the stipulated protocol. The NIST decision tree was implemented for the calculation of the KCRVs and DoEs. The participant results overall showed good agreement with the KCRV, despite the variety of dissolution procedures and measurement techniques for this highly complex matrix and challenging measurands. Successful participation in CCQM-K160 demonstrated measurement capabilities for the determination of mass fraction of Pt, Pd and Rh in the mg/kg range and will support broad scope CMC claims for a wide range of challenging matrices. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA). KW - Metrology in Chemistry KW - Traceability KW - Uncertainty PY - 2024 DO - https://doi.org/10.1088/0026-1394/61/1A/08011 VL - 61 IS - 1A SP - 1 EP - 39 PB - IOP Publishing AN - OPUS4-60524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Fabian A1 - von der Au, Marcus A1 - Gehrenkemper, Lennart A1 - Meermann, Björn T1 - An optimized method for PFAS analysis using HR–CS–GFMAS via GaF detection N2 - The analysis of per- and polyfluoroalkyl substances (PFAS) via sum parameters like extractable organic fluorine (EOF) in combination with high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR–CS–GFMAS) is highly promising regarding fluorine sensitivity and selectivity. However, the HR–CS–GFMAS method includes several drying and heating steps which can lead to losses of volatile PFAS before the molecular formation step using e.g., GaF formation. Hence, the method leads to a strong discrimination of PFAS within the EOF depending on their physical/chemical properties and is therefore associated with reduced accuracy. To reduce this discrepancy and to indicate realistic PFAS pollution values, an optimization of the HR–CS–GFMAS method for PFAS analysis is needed. Hence, we determined fluorine response factors of several PFAS with different physical/chemical properties upon application of systematic optimization steps. We could therefore improve the method's sensitivity for PFAS analysis using a modifier drying pre-treatment step followed by a sequential injection of sample solutions. The highest improvement in sensitivity of volatile PFAS was shown upon addition of a Mg modifier during drying pre-treatment. Thereby, during optimization the relative standard deviation of fluorine response factors could be reduced from 55 % (initial method) to 27 % (optimized method) leading to a more accurate determination of organofluorine sum parameters. The method provides an instrumental LOD and LOQ of β(F) 1.71 μg/L and 5.13 μg/L, respectively. Further validation aimed to investigate several matrix effects with respect to water matrices. Here, substance-specific behavior was observed. For example, perfluorooctanoic acid (PFOA) which was used as calibrator, showed signal suppressions upon high chloride concentrations (>50 mg/L). Hence, a thorough separation of Cl from analytes during sample preparation is needed for accurate sum parameter analysis. KW - PFAS KW - GF-AAS KW - Method optimization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610522 DO - https://doi.org/10.1016/j.talanta.2024.126811 VL - 281 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-61052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chronakis, Michail Ioannis A1 - Meermann, Björn A1 - von der Au, Marcus T1 - The evolution of data treatment tools in single-particle and single-cell ICP-MS analytics N2 - Single-particle inductively coupled plasma-mass spectrometry (sp-ICP-MS) is one of the most powerful tools in the thriving field of nanomaterial analysis. Along the same lines, single-cell ICP-MS (sc-ICP-MS) has become an invaluable tool in the study of the variances of cell populations down to a per-cell basis. Their importance and application fields have been listed numerous times, across various reports and reviews. However, not enough attention has been paid to the immense and ongoing development of the tools that are currently available to the analytical community for the acquisition, and more importantly, the treatment of single-particle and single-cell-related data. Due to the ever-increasing demands of modern research, the efficient and dependable treatment of the data has become more important than ever. In addition, the field of single-particle and single-cell analysis suffers due to a large number of approaches for the generated data—with varying levels of specificity and applicability. As a result, finding the appropriate tool or approach, or even comparing results, can be challenging. This article will attempt to bridge these gaps, by covering the evolution and current state of the tools at the disposal of sp-ICP-MS users. Graphical Abstract KW - Trend Article KW - spICP-MS KW - Data Tools KW - scICP-MS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610539 DO - https://doi.org/10.1007/s00216-024-05513-4 SP - 1 EP - 7 PB - Springer Science and Business Media LLC AN - OPUS4-61053 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mangarova, Dilyana Branimirova A1 - Reimann, Carolin A1 - Kaufmann, Jan Ole A1 - Möckel, Jana A1 - Kader, Avan A1 - Adams, Lisa Christine A1 - Ludwig, Antje A1 - Onthank, David A1 - Robinson, Simon A1 - Karst, Uwe A1 - Helmer, Rebecca A1 - Botnar, Rene A1 - Hamm, Bernd A1 - Makowski, Marcus Richard A1 - Brangsch, Julia T1 - Elastin-specific MR probe for visualization and evaluation of an interleukin-1β targeted therapy for atherosclerosis N2 - Atherosclerosis is a chronic inflammatory condition of the arteries and represents the primary cause of various cardiovascular diseases. Despite ongoing progress, finding effective anti-inflammatory therapeutic strategies for atherosclerosis remains a challenge. Here, we assessed the potential of molecular magnetic resonance imaging (MRI) to visualize the effects of 01BSUR, an anti-interleukin-1β monoclonal antibody, for treating atherosclerosis in a murine model. Male apolipoprotein E-deficient mice were divided into a therapy group (01BSUR, 2 × 0.3 mg/kg subcutaneously, n = 10) and control group (no treatment, n = 10) and received a high-fat diet for eight weeks. The plaque burden was assessed using an elastin-targeted gadolinium-based contrast probe (0.2 mmol/kg intravenously) on a 3 T MRI scanner. T1-weighted imaging showed a significantly lower contrast-to-noise (CNR) ratio in the 01BSUR group (pre: 3.93042664; post: 8.4007067) compared to the control group (pre: 3.70679168; post: 13.2982156) following administration of the elastin-specific MRI probe (p < 0.05). Histological examinations demonstrated a significant reduction in plaque size (p < 0.05) and a significant decrease in plaque elastin content (p < 0.05) in the treatment group compared to control animals. This study demonstrated that 01BSUR hinders the progression of atherosclerosis in a mouse model. Using an elastin-targeted MRI probe, we could quantify these therapeutic effects in MRI. N2 - Atherosklerose ist eine chronische entzündliche Erkrankung der Arterien und die Hauptursache für verschiedene Herz-Kreislauf-Erkrankungen. Trotz kontinuierlicher Fortschritte ist es nach wie vor schwierig, wirksame entzündungshemmende Therapiestrategien für Atherosklerose zu finden. In dieser Studie haben wir das Potenzial der molekularen Magnetresonanztomographie (MRT) zur Visualisierung der Wirkung von 01BSUR, einem monoklonalen Anti-Interleukin-1β-Antikörper, zur Behandlung von Atherosklerose in einem Mausmodell untersucht. Männliche Apolipoprotein-E-defiziente Mäuse wurden in eine Therapiegruppe (01BSUR, 2 × 0,3 mg/kg subkutan, n = 10) und eine Kontrollgruppe (keine Behandlung, n = 10) aufgeteilt und erhielten acht Wochen lang eine fettreiche Diät. Die Plaquebelastung wurde mit einer auf Elastin ausgerichteten Kontrastmittelsonde auf Gadoliniumbasis (0,2 mmol/kg intravenös) auf einem 3-T-MRT-Scanner untersucht. Die T1-gewichtete Bildgebung zeigte ein signifikant niedrigeres Kontrast-Rausch-Verhältnis (CNR) in der 01BSUR-Gruppe (vorher: 3,93042664; nachher: 8,4007067) im Vergleich zur Kontrollgruppe (vorher: 3,70679168; nachher: 13,2982156) nach Verabreichung der Elastin-spezifischen MRT-Sonde (p < 0,05). Histologische Untersuchungen zeigten eine signifikante Verringerung der Plaque-Größe (p < 0,05) und eine signifikante Abnahme des Plaque-Elastin-Gehalts (p < 0,05) in der Behandlungsgruppe im Vergleich zu den Kontrolltieren. Diese Studie zeigte, dass 01BSUR das Fortschreiten der Atherosklerose in einem Mausmodell hemmt. Mit einer auf Elastin ausgerichteten MRT-Sonde konnten wir diese therapeutischen Effekte in der MRT quantifizieren. KW - Atherosclerosis KW - Molecular imaging KW - Elastin KW - Plaque KW - Interleukin-1beta PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610858 DO - https://doi.org/10.1038/s41598-024-71716-5 VL - 14 IS - 1 SP - 1 EP - 11 PB - Springer Science and Business Media LLC AN - OPUS4-61085 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Döring, Sarah T1 - Optimization of Polymer Interface: Novel Surface-functionalized Corundum Particles for Improved Antibody Digestion N2 - Therapeutic monoclonal antibodies are the fastest-growing class of biological agents and the development of reliable analytical methods for their quantification is becoming increasingly important. Liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) represents one of the leading technologies for antibody quantification. The serin protease trypsin has emerged as the gold standard enzyme for digesting intact protein into peptides for this approach. However, many protocols exist that often lead to different results. The talk will provide a brief introduction to the application of novel thermostable and surface-functionalized trypsin particles for improved antibody digestion as well as initial successes in polymer functionalization of the corundum surface to prevent nonspecific protein adsorption during the digestion procedure. T2 - SALSA Make and Measure 2024: Interfaces CY - Berlin, Germany DA - 11.09.2024 KW - Antibody Quantification KW - Recombinant Enzymes KW - LC-MS/MS KW - Enzyme Immobilisation KW - Surface Functionalisation KW - Corundum PY - 2024 AN - OPUS4-61041 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Temgoua, Ranil C. T. T1 - Voir les choses sous un autre angle : Comment l’électrochimie analytique aide à révolutionner l'analyse chimique N2 - As part of the "Journées de Chimie Analytique, JCA Dschang 2024", this plenary scientific conference will explore how analytical electrochemistry is fundamentally changing modern chemical analysis methods. We will highlight key innovations such as wearable/handheld sensors, lab-on-a-chip, lab-on-paper, lab-on-a-glove, integrated detection systems with artificial intelligence, and point-of-care (POC) technologies. We will also address the couplings between analytical electrochemistry and various analytical techniques such as mass spectrometry (EC-MS), chromatography (EC-LC), spectroscopy [EC-spectroscopy (UV-VIS, Raman, IR, NMR)], microscopy [EC-microscopy (EM, AFM)], and capillary electrophoresis (EC-CE). These advances enable faster, more accurate, and more accessible analyses, opening new perspectives for research and practical applications in environmental science, food and agriculture, public health, and advanced materials. T2 - Journées de Chimie Analytique 12th Edition CY - Dschang, Cameroon DA - 28.08.2024 KW - Organic Trace Analysis KW - Electrochemistry KW - Mass Spectrometry PY - 2024 AN - OPUS4-61064 LA - fra AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Isleyen, Alper A1 - Can, Suleyman Z. A1 - Cankur, Oktay A1 - Engin, Betul Ari A1 - Vogl, Jochen A1 - Koenig, Maren A1 - Horvat, Milena A1 - Jacimovic, Radojko A1 - Zuliani, Tea A1 - Fajon, Vesna A1 - Jotanovic, Aida A1 - Gaževic, Luka A1 - Milosevic, Milena A1 - Ochsenkuehn–Petropoulou, Maria A1 - Tsopelas, Fotis A1 - Lymberopoulou, Theopisti A1 - Tsakanika, Lamprini-Areti A1 - Serifi, Olga A1 - Ochsenkuehn, Klaus M. A1 - Bulska, Ewa A1 - Tomiak, Anna A1 - Kurek, Eliza A1 - Cakılbahçe, Zehra A1 - Aktas, Gokhan A1 - Altuntas, Hatice A1 - Basaran, Elif A1 - Kısacık, Barıs A1 - Gumus, Zeynep T1 - Correction: Certification of the total element mass fractions in UME EnvCRM 03 soil sample via a joint research project N2 - In this article the author’s name Betul Ari Engin was incorrectly written as Murat Tunc. The original article has been corrected. PY - 2024 DO - https://doi.org/10.1007/s00769-024-01611-z VL - 29 SP - 303 PB - Springer Science and Business Media LLC AN - OPUS4-60824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dobosy, Péter A1 - Nguyen, Hoang Thi Phuong A1 - Záray, Gyula A1 - Streli, Christina A1 - Ingerle, Dieter A1 - Ziegler, Philipp A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Endrédi, Anett A1 - Fodor, Ferenc T1 - Effect of iodine species on biofortification of iodine in cabbage plants cultivated in hydroponic cultures N2 - Iodine is an essential trace element in the human diet because it is involved in the synthesis of thyroid hormones. Iodine deficiency affects over 2.2 billion people worldwide, making it a significant challenge to find plant-based sources of iodine that meet the recommended daily intake of this trace element. In this study, cabbage plants were cultivated in a hydroponic system containing iodine at concentrations ranging from 0.01 to 1.0 mg/L in the form of potassium iodide or potassium iodate. During the experiments, plant physiological parameters, biomass production, and concentration changes of iodine and selected microelements in different plant parts were investigated. In addition, the oxidation state of the accumulated iodine in root samples was determined. Results showed that iodine addition had no effect on photosynthetic efficiency and chlorophyll content. Iodide treatment did not considerably stimulate biomass production but iodate treatment increased it at concentrations less than 0.5 mg/L. Increasing iodine concentrations in the nutrient solutions increased iodine content in all plant parts; however, the iodide treatment was 2–7 times more efficient than the iodate treatment. It was concluded, that iodide addition was more favourable on the target element accumulation, however, it should be highlighted that application of this chemical form in nutrient solution decreased the concetrations of selected micoelement concentration comparing with the control plants. It was established that iodate was reduced to iodide during its uptake in cabbage roots, which means that independently from the oxidation number of iodine (+ 5, − 1) applied in the nutrient solutions, the reduced form of target element was transported to the aerial and edible tissues. KW - BAMline KW - XANES KW - Synchrotron KW - Lodine PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608330 DO - https://doi.org/10.1038/s41598-024-66575-z VL - 14 IS - 1 SP - 1 EP - 12 PB - Springer Science and Business Media LLC AN - OPUS4-60833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Huang, Junhao A1 - Klahn, Marcus A1 - Tian, Xinxin A1 - Bartling, Stephan A1 - Zimina, Anna A1 - Radtke, Martin A1 - Rockstroh, Nils A1 - Naliwajko, Pawel A1 - Steinfeldt, Norbert A1 - Peppel, Tim A1 - Grunwaldt, Jan‐Dierk A1 - Logsdail, Andrew J. A1 - Jiao, Haijun A1 - Strunk, Jennifer T1 - Fundamental Structural and Electronic Understanding of Palladium Catalysts on Nitride and Oxide Supports N2 - The nature of the support can fundamentally affect the function of a heterogeneous catalyst. For the novel type of isolated metal atom catalysts, sometimes referred to as single‐atom catalysts, systematic correlations are still rare. Here, we report a general finding that Pd on nitride supports (non‐metal and metal nitride) features a higher oxidation state compared to that on oxide supports (non‐metal and metal oxide). Through thorough oxidation state investigations by X‐ray absorption spectroscopy (XAS), X‐ray photoelectron spectroscopy (XPS), CO‐DRIFTS, and density functional theory (DFT) coupled with Bader charge analysis, it is found that Pd atoms prefer to interact with surface hydroxyl group to form a Pd(OH)x species on oxide supports, while on nitride supports, Pd atoms incorporate into the surface structure in the form of Pd−N bonds. Moreover, a correlation was built between the formal oxidation state and computational Bader charge, based on the periodic trend in electronegativity. KW - BAmline KW - XANES KW - Catalyst PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608341 DO - https://doi.org/10.1002/anie.202400174 SN - 1433-7851 VL - 63 IS - 20 SP - 1 EP - 9 PB - Wiley AN - OPUS4-60834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Valentim Gelamo, Rogério A1 - Bueno Leite, Natália A1 - Amadeu, Nader A1 - Reis Pedreira Muniz Tavares, Michel A1 - Oberschmidt, Dirk A1 - Klemm, Sophie A1 - Fleck, Claudia A1 - Cakir, Cafer-Tufan A1 - Radtke, Martin A1 - Aparecido Moreto, Jéferson T1 - Exploring the Nb2O5 coating deposited on the Ti-6Al-4V alloy by a novel GE-XANES technique and nanoindentation load-depth N2 - This research group has been demonstrating the significant advantages of using Nb2O5 coatings for functionalizing titanium, aluminium, and stainless steels. Regarding the biomedical sector and considering Ti-6Al-4V alloy, the reactive sputtering technique improved the cell viability, the osteogenic performance of cells involved in the osseointegration process as well as the ability to delay bacterial proliferation. The characteristics of the Nb2O5 coatings were assessed before by using standard methods, which provide information only a few tens of nanometers depth. Given that the Nb2O5 coating fabricated in this work exhibits a thickness of approximately 300 nm, the GE-XANES technique emerges as the most suitable method for this analysis. Additional information was provided with the aid of nanoindentation load-depth (P-h) curves. GE-XANES results indicated the formation of a homogeneous layer of Nb2O5 coating on the Ti-6Al-4V surfaces. The deposition process improved the surface hardness of the Ti-6Al-4V alloy (4.38 GPa versus 5.62 GPa) considering the 2 mN load. KW - BAMline KW - GE-XANES KW - Synchrotron PY - 2024 DO - https://doi.org/10.1016/j.matlet.2023.135584 SN - 0167-577X VL - 355 SP - 1 EP - 4 PB - Elsevier B.V. AN - OPUS4-60835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Senges, Gene A1 - de Oliveira Guilherme Buzanich, Ana A1 - Lindič, Tilen A1 - Gully, Tyler A. A1 - Winter, Marlon A1 - Radtke, Martin A1 - Röder, Bettina A1 - Steinhauer, Simon A1 - Paulus, Beate A1 - Emmerling, Franziska A1 - Riedel, Sebastian T1 - Unravelling highly oxidized nickel centers in the anodic black film formed during the Simons process by in situ X-ray absorption near edge structure spectroscopy N2 - The electrofluorination after Simons has been used for the last century to produce everyday life materials. An in situ XANES investigation of the controversially debated black film apparent in the Simons process revealed high-valent nickel centers. KW - Synchrotron KW - BAMline KW - XANES PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608366 DO - https://doi.org/10.1039/d3sc06081k SN - 2041-6520 VL - 15 IS - 12 SP - 4504 EP - 4509 PB - Royal Society of Chemistry (RSC) AN - OPUS4-60836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moufid, M. A1 - Tiebe, Carlo A1 - El Bari, N. A1 - Bartholmai, Matthias A1 - Bouchikhi, B. T1 - Advance in electronic nose technology developed for the detection and discrimination of ethanol, ammonia, and hydrogen sulfide gases N2 - This work focuses on the design and fabrication of low-cost and fast-response of an electronic nose (E-nose) based on semiconductor gas sensors, for discriminating some synthetic gases such as ammonia (NH3), ethanol (C2H5OH), and hydrogen sulfide (H2S). Additionally, the capability of separating different concentration levels of each considered gases was checked. Dataset treatment of E-nose by using Principal Component Analysis (PCA) showed a good discrimination of the different synthetic gases. Furthermore, perfect classification was reached of different concentration levels of the analysed gases by using Discriminant Function Analysis (DFA). In the light of these results, it could be stated that the developed E-nose system constitutes an inexpensive, rapid, simple to use, and efficient tool for synthetic gases detection. T2 - IEEE International Symposium on Olfaction and Electronic Nose (ISOEN) CY - Aveiro, Portugal DA - 29.05.2022 KW - Electronic nose KW - Metal oxide semiconductor KW - Chemometric techniques KW - Environmental analysis PY - 2022 SN - 978-1-6654-5860-3 DO - https://doi.org/10.1109/ISOEN54820.2022.9789636 SP - 1 EP - 3 AN - OPUS4-56574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hohendorf, Stefan T1 - Medea und Jason, Eine Radiologische Untersuchung im Neuen Palais Potsdam N2 - Seit der Antike gehört die Medea-Sage zu den bekanntesten Geschichten der Weltliteratur. Der berühmte französische Künstler Carle Van Loo hat sich dieses Epos um 1759 angenommen und ein beeindruckendes Ölgemälde mit Abmessungen von 2,30x3,28m² erschaffen. Mit Mademoiselle Clairon als Medea und Henri Louis Le Kain als Jason ist ein Kunstwerk entstanden, das seitdem einige Veränderungen und Restaurierungen erfahren hat. Die Bundesanstalt für Materialforschung und -prüfung (BAM) hatte 2020 die Möglichkeit, dieses und ein zweites Kunstwerk, im Neuen Palais in Potsdam, für die Stiftung Preußische Schlösser und Gärten Berlin-Brandenburg, radiografisch zu untersuchen. Hierbei wurden sowohl technologisch als auch kunsthistorisch einige interessante Entdeckungen gemacht, die im vorliegenden Beitrag vorgestellt werden. T2 - DGZfP Jahrestatung 2022 CY - Kassel, Germany DA - 23.05.2022 KW - Röntgen KW - X-Ray KW - Kunsstechnologisch KW - Gemälde KW - Untermalung KW - Speicherfolie KW - Strahlenschutz PY - 2022 AN - OPUS4-56577 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jasiuniene, E. A1 - Yilmaz, Bengisu A1 - Smagulova, D. A1 - Bhat, G. A. A1 - Cicenas, V. A1 - Zukauskas, E. A1 - Mazeika, L. T1 - Non-Destructive Evaluation of the Quality of Adhesive Joints Using Ultrasound, X-ray, and Feature-Based Data Fusion N2 - The aim of this work is to achieve reliable nondestructive evaluation (NDE) of adhesively bonded aerospace components by developing novel multidimensional data fusion techniques, which would combine the information obtained by ultrasonic and X-ray NDE methods. Separately, both NDE techniques have their advantages and limitations. The integration of data obtained from pulse echo immersion ultrasound testing and radiography holds immense potential to help improve the reliability of non-destructive evaluation. In this study, distinctive features obtained from single techniques, traditional ultrasonic pulse echo testing, and radiography, as well as fused images, were investigated and the suitability of these distinctive features and fusion techniques for improving the probability of defect detection was evaluated. For this purpose, aluminum single lap joints with brass inclusions were analyzed using ultrasound pulse echo and radiography techniques. The distinctive features were extracted from the data obtained, and images of features obtained by both techniques were fused together. Different combinations of features and fusion algorithms were investigated, considering the desire to automate data evaluation in the future. KW - Data fusion KW - Ultrasonics KW - Radiography PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565789 DO - https://doi.org/10.3390/app122412930 VL - 12 IS - 24 SP - 1 EP - 20 PB - MDPI AN - OPUS4-56578 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat T1 - Photonic crystal fibers for microwave signal processing N2 - We present a novel design of an optical True Time Delay Line based on a 19-core Photonic Crystal Fiber that operates in a broad radiofrequency signal processing range from 1 to 67 GHz on a 10-km link, thus enabling simultaneous signal distribution and processing. T2 - 2021 IEEE Photonics Conference (IPC) CY - Vancouver, BC, Canada DA - 18.10.2021 KW - Delay lines KW - Photonic crytal fibers KW - Optical fibers PY - 2021 SN - 978-1-6654-1601-6 DO - https://doi.org/10.1109/IPC48725.2021.9592934 SP - 1 EP - 3 PB - IEEE AN - OPUS4-56582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias A1 - Ehlers, Henrik A1 - Casperson, Ralf A1 - Thewes, R. A1 - Jutkuhn, D. T1 - Hochauflösende online Wirbelstromprüfung von PBF LB/M Bauteilen mit GMR Arrays N2 - In den letzten Jahren haben additive Fertigungstechnologien an Bedeutung gewonnen. Für komplexe Funktionsbauteile oder die Produktion von Werkstücken in kleinen Stückzahlen kann das Laser-Pulverbettschmelzen eingesetzt werden. Hohe Sicherheitsanforderungen, z. B. in der Luft- und Raumfahrt, erfordern eine umfassende Qualitätskontrolle. Daher werden nach der Fertigung zerstörungsfreie Offline-Prüfverfahren wie die Computertomographie eingesetzt. In jüngster Zeit wurden zur Verbesserung der Rentabilität und Praktikabilität zerstörungsfreie Online-Prüfverfahren wie die optische Tomographie entwickelt. In diesem Beitrag wird die Anwendbarkeit der Wirbelstromprüfung mit GMR Sensoren für die online Prüfung von PBF-LB/M Teilen demonstriert. Die Ergebnisse einer online Wirbelstromprüfung mit GMR Sensoren und einer Ein-Draht-Anregung werden gezeigt. Während des Produktionsprozesses wird für jede Lage eine Wirbelstromprüfung durchgeführt. Trotz hochauflösender Arrays mit 128 Elementen wird durch eine angepasste Hardware die Prüfdauer geringgehalten. So kann die Messung während des Beschichtungsvorgangs durchgeführt werden, ohne den Fertigungsprozess signifikant zu verlangsamen. Eine online Wirbelstromprüfung eines stufenförmigen Testkörpers aus Haynes282 über 184 Lagen zeigt, dass die Kanten nicht nur in der aktuellen Lage detektiert werden können, sondern auch in einer Tiefe von 400 µm, wenn eine Anregungsfrequenz von 1,2 MHz gewählt wird. T2 - 2. Fachseminar Wirbelstromprüfung CY - Schweinfurt, Germany DA - 14.09.2022 KW - Wirbelstromprüfung KW - Additive Fertigung KW - Online Monitoring KW - GMR Arrays PY - 2022 AN - OPUS4-55895 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas T1 - Raman microspectroscopy elucidates Early Medieval art technology: high-fired gypsum mortar and Egyptian blue from the church St. Peter above Gratsch (South Tyrol, Northern Italy) N2 - Raman microspectroscopy enables imaging of the distributions of mineral phases as well as physical properties of materials, such as crystal orientations and crystallinities, with down to sub-micrometre resolution. In a combination with other spectroscopic and microscopic techniques, this approach was applied to the analysis and elucidation of ancient production technologies of stucco fragments made of high-fired gypsum mortar and Egyptian blue pigment discovered on a monochrome wall painting fragment originating from the Early Medieval (5th/6th century AD) construction phase of the church St. Peter above Gratsch in South Tyrol (Northern Italy). T2 - Analytica Conference 2022 CY - Munich, Germany DA - 21.06.2022 KW - Raman microspectroscopy KW - Gypsum KW - Pigments PY - 2022 AN - OPUS4-55896 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Raman focal point on Roman Egyptian blue elucidates disordered cuprorivaite, green glass phase and trace compounds N2 - The discussed comparative analyses of Roman Imperial pigment balls and fragmentary murals unearthed in the ancient cities of Aventicum and Augusta Raurica (Switzerland) by means of Raman microspectroscopy pertain to a predecessor study on trace compounds in Early Medieval Egyptian blue (St. Peter, Gratsch, South Tyrol, Northern Italy). The plethora of newly detected associated minerals of the raw materials surviving the synthesis procedure validate the use of quartz sand matching the composition of sediments transported by the Volturno river into the Gulf of Gaeta (Campania, Southern Italy) with a roasted sulphidic copper ore and a mixed-alkaline plant ash as fluxing agent. Thus, the results corroborate a monopolised pigment production site located in the northern Phlegrean Fields persisting over the first centuries A.D., this in line with statements of the antique Roman writers Vitruvius and Pliny the Elder and recent archaeological evidences. Beyond that, Raman spectra reveal through gradual peak shifts and changes of band width locally divergent process conditions and compositional inhomogeneities provoking crystal lattice disorder in the chromophoric cuprorivaite as well as the formation of a copper-bearing green glass phase, the latter probably in dependency of the concentration of alkali flux, notwithstanding that otherwise solid-state reactions predominate the synthesis. KW - Raman microspectroscopy KW - Egyptian blue KW - Cuprorivaite PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559028 DO - https://doi.org/10.1038/s41598-022-19923-w SN - 2045-2322 VL - 12 IS - 1 SP - 1 EP - 12 PB - Nature Publishing Group CY - London AN - OPUS4-55902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sechi, R. A1 - Fackeldey, K. A1 - Chewle, Surahit A1 - Weber, M. T1 - SepFree NMF: A toolbox for analyzing the kinetics of sequential spectroscopic data N2 - This work addresses the problem of determining the number of components from sequential spectroscopic data analyzed by non-negative matrix factorization without separability assumption (SepFree NMF). These data are stored in a matrix M of dimension “measured times” versus “measured wavenumbers” and can be decomposed to obtain the spectral fingerprints of the states and their evolution over time. SepFree NMF assumes a memoryless (Markovian) process to underline the dynamics and decomposes M so that M = WH, with W representing the components’ fingerprints and H their kinetics. However, the rank of this decomposition (i.e., the number of physical states in the process) has to be guessed from pre-existing knowledge on the observed process. We propose a measure for determining the number of components with the computation of the minimal memory effect resulting from the decomposition; by quantifying how much the obtained factorization is deviating from the Markovian property, we are able to score factorizations of a different number of components. In this way, we estimate the number of different entities which contribute to the observed system, and we can extract kinetic information without knowing the characteristic spectra of the single components. This manuscript provides the mathematical background as well as an analysis of computer generated and experimental sequentially measured Raman spectra. KW - Kinetics from experiments KW - Separability assumption KW - Sequential spectroscopic data PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559046 DO - https://doi.org/10.3390/a15090297 SN - 1999-4893 VL - 15 IS - 9 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-55904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fackeldey, K. A1 - Röhm, J. A1 - Niknejad, A. A1 - Chewle, Surahit A1 - Weber, M. T1 - Analyzing Raman spectral data without separabiliy assumption N2 - Raman spectroscopy is a well established tool for the analysis of vibration spectra, which then allow for the determination of individual substances in a chemical sample, or for their phase transitions. In the time-resolved-Raman-sprectroscopy the vibration spectra of a chemical sample are recorded sequentially over a time interval, such that conclusions for intermediate products (transients) can be drawn within a chemical process. The observed data-matrix M from a Raman spectroscopy can be regarded as a matrix product of two unknown matrices W and H, where the first is representing the contribution of the spectra and the latter represents the chemical spectra. One approach for obtaining W and H is the non-negative matrix factorization. We propose a novel approach, which does not need the commonly used separability assumption. The performance of this approach is shown on a real world chemical example. KW - Non-negative matrix factorization KW - NMF KW - Raman spectra KW - Separability condition KW - PCCA+ PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559051 DO - https://doi.org/10.1007/s10910-020-01201-7 SN - 1572-8897 VL - 59 SP - 575 EP - 596 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-55905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Multifaceted laser induced plasma: spectroscopy and beyond N2 - In this presentation, I will give a brief overview of my personal experience with laser induced plasma (LIP). I will start from my and colleagues’ early works, where we used LIP as an atomic reservoir for laser induced fluorescence (LIP). We applied LIP-LIF for a sensitive detection of trace elements in various materials and demonstrated that under certain conditions the technique can even be used for isotope analysis. Next, I will discuss the application of LIP spectroscopy, i.e., LIBS, to material identification that nowadays constitutes one of the best applications of this technique. In those early days, we used correlation analysis for spectra processing; it is now replaced by more powerful chemometric methods. Further, I will stop on our efforts in modeling LIP that we first intended for the improved quality of spectroscopic analysis and later extended to non-spectroscopic fields such as chemical vapor deposition and surface structuring. We developed a version of calibration-free LIBS, in which we iterated model-generated spectra until a close match was achieved between experimental and synthetic spectra to determine concentrations. Next, I will briefly overview our recent developments in plasma modeling that include plasma chemistry. This was important in view of widening application of LIBS as a molecular technique. I will also address several plasma diagnostics, e.g., Radon transform tomography that we developed to get more insight about LIP that was helpful for both analytic spectroscopy and modeling. Finally, I will mention several exotic applications of LIP such as LIP-based lasers and chemical reactors to illustrate a real multifaceted character of laser induced plasma and usefulness of its study for many science fields. T2 - SciX 2022, The Federation of Analytical Chemistry and Spectroscopy Societies (FACSS) CY - Cincinnati, OH, USA DA - 02.10.2022 KW - Emission spectroscopy KW - Laser ablation KW - Laser induced plasma deposition KW - Surface coating KW - Hydrodynamic model KW - Plasma chemistry PY - 2022 AN - OPUS4-55968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fritzsche, Sven T1 - Classification of defects in Direct Laser Writing N2 - Direct laser writing grows to an industry-ready manufacturing platform. A stable quality infrastructure is needed for robust processing. However, flaws, errors or impurities are neither described nor communicated in the community of two-photon polymerization. In contrast, additive manufacturing errors in metals manufacturing are described thoroughly. T2 - MNE EUROSENSORS 2022 CY - Leuven, Belgium DA - 19.09.2022 KW - Quality infrastructure KW - Direct laser writing KW - Two photon polymerisation PY - 2022 AN - OPUS4-55984 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Imaging of results in NDT-CE: Strength and limitations in the use of Radar vs. Ultrasonic Echo N2 - Presentation on behalf of the co-author specified in BAM-Publica. Study on capabilities of volume methods (GPR, Ultrasonic Echo) regarding lateral and depth localisation of reinforcement and tendons in concrete components. Varied boundary conditions: spacing and diameter of both the near surface rebars of the mesh, and the reflectors of interest, as well as component thickness and concrete cover. Please find corresponding references on slide 2. T2 - 6th International Conference on Concrete Repair, Rehabilitation and Retrofitting (ICCRRR2022) CY - Cape Town, South Africa DA - 03.10.2022 KW - Reinforcement KW - Tendon duct KW - Concrete KW - NDT KW - Localisation PY - 2022 AN - OPUS4-55987 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Per- and polyfluoroalkyl substances (PFAS) in sewage sludge and wastewater-based fertilizers and future PFAS remediation N2 - Per- and polyfluoroalkyl substances (PFAS) are a group of anionic, cationic and zwitterionic synthetic products, in which the hydrogen atoms on the carbon skeleton of at least one carbon atom have been completely replaced by fluorine atoms and which include more than 4730 compounds, depending on the definition. As a result of continuous and prolific use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil, groundwater and surface water. As a result of the perpetual use of PFAS containing products, effluents and sewage sludge from wastewater treatment plants (WWTPs) have been observed to be an important pathway for PFAS into the environment. In Germany, phosphorus and other nutrients from sewage sludge and wastewater should be recycled in WWTPs of cities with a large population. However, it is not clear if PFAS contamination from wastewater and sewage sludge end up in novel wastewater-based fertilizers. Normally, PFAS are analyzed using PFAS protocols typically with liquid chromatography tandem mass spectrometry (LC-MS/MS) quantification. To get a better overview of the amount of “total PFAS,” we applied sum parameter methods based on combustion ion chromatography (CIC) to screen the PFAS contaminations in various sewage sludge and wastewater-based fertilizers. Furthermore, current decontamination strategies of PFAS-burdened soils mainly consist of adsorption methods using adsorbents for fixation of PFAS in the ground. A second option is the utilization of a “pump and treat” process, cycling polluted soils through a washing plant leading to the concentration of the pollutants in the fine fraction. Only a subsequent, high-energy consuming pyrolysis process guarantees the total destruction of all fluorinated organic contaminants. Both approaches are cost-intensive and not intended for the direct decomposition of all PFAS contaminants. Hence, there is a great demand for innovative developments and chemical treatment technologies, dealing with new strategies of tackling the PFAS problem. T2 - Seminar of Ben-Gurion University CY - Midreshet Ben-Gurion, Israel DA - 02.11.2022 KW - PFAS KW - Sewage sludge KW - XANES spectroscopy PY - 2022 AN - OPUS4-56166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Costabel, S. A1 - Hiller, Thomas A1 - Dlugosch, R. A1 - Kruschwitz, Sabine A1 - Müller Petke, M. T1 - Evaluation of single-sided nuclear magnetic resonance technology for usage in geosciences N2 - Because of its mobility and ability to investigate exposed surfaces, single-sided (SiS) nuclear magnetic resonance (NMR) technology enables new application fields in geosciences. To test and assess its corresponding potential, we compare longitudinal (T1) and transverse (T2) data measured by SiS NMR with those of conventional geoscientific laboratory NMR. We use reference sandstone samples covering a broad range of pore sizes. Our study demonstrates that the lower signal-to-noise ratio of SiS NMR data generally tends to slightly overestimated widths of relaxation time distributions and consequently pore size distributions. While SiS and conventional NMR produce very similar T1 relaxation data, unbiased SiS NMR results for T2 measurements can only be expected for fine material, i.e. clayey or silty sediments and soils with main relaxation times below 0.05s. This limit is given by the diffusion relaxation rate due to the gradient in the primary magnetic field associated with the SiS NMR. Above that limit, i.e. for coarse material, the relaxation data is strongly attenuated. If considering the diffusion relaxation time of 0.2 s in the numerical data inversion process, the information content >0.2s is blurred over a range larger than that of conventional NMR. However, our results show that principle range and magnitudes of the relaxation time distributions are reconstructed to some extent. Regarding these findings, SiS NMR can be helpful to solve geoscientific issues, e.g. to assess the hydro-mechanical properties of the walls of underground facilities or to provide local soil moisture data sets for calibrating indirect remote techniques on the regional scale. The greatest opportunity provided by the SiS NMR technology is the acquisition of profile relaxation data for rocks with significant bedding structures at the µm scale. With this unique feature, SiS NMR can support the understanding and modeling of hydraulic and diffusional anisotropy behavior of sedimentary rocks. KW - Single-sided NMR KW - Geosciences KW - Nuclear magnetic resonance PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561676 DO - https://doi.org/10.1088/1361-6501/ac9800 SN - 0957-0233 VL - 34 IS - 1 SP - 1 EP - 13 PB - IOP Publishing AN - OPUS4-56167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ecke, Alexander A1 - Westphalen, Tanja A1 - Retzmann, Anika A1 - Schneider, Rudolf T1 - Factors affecting the hydrolysis of the antibiotic amoxicillin in the aquatic environment N2 - The environmental fate of the frequently used broad-spectrum β-lactam antibiotic amoxicillin (AMX) is of high concern regarding the potential evolution of antimicrobial resistance (AMR). Moreover, it is known that AMX is prone to hydrolysis, yielding a variety of hydrolysis products (HPs) with yet unknown effects. Studies to identify those HPs and investigate their formation mechanisms have been reported but a long-term study on their stability in real water samples was missing. In this regard, we investigated the hydrolysis of AMX at two concentration levels in four distinct water types under three different storage conditions over two months. Concentrations of AMX and four relevant HPs were monitored by an LC-MS/MS method revealing pronounced differences in the hydrolysis rate of AMX in tap water and mineral water on the one hand (fast) and surface water on the other(slow). In this context, the occurrence, relative intensities, and stability of certain HPs are more dependent on the water type than on the storage condition. As clarified by ICP-MS, the main difference between the water types was the content of the metals copper and zinc which are supposed to catalyze AMX hydrolysis demonstrating an effective method to degrade AMX at ambient conditions. KW - β-lactam KW - Stability KW - Degradation KW - Hydrolysis products KW - LC-MS/MS KW - ICP-MS PY - 2023 DO - https://doi.org/10.1016/j.chemosphere.2022.136921 SN - 0045-6535 VL - 311 SP - 136921 PB - Elsevier Ltd. AN - OPUS4-56124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Portesi, C. T1 - Creation of a European Metrology Network for Safe and Sustainable Food N2 - Safe food is a prerequisite for good human health, however currently almost one in ten people in the world fall ill after eating contaminated food. National food safety authorities need to be able to manage food safety risks along the entire food chain. The Official Controls Regulation (EU) 2017/625 was put in place to ensure that food and feed law stipulates the need for validated analytical methods. However, whilst method development for food control and proficiency testing are well established by European Union Reference Laboratories and National Reference Laboratories, validation of the measurements involved, certified reference materials and internationally recognised calibration and measurement capabilities are currently often (?) lacking. This may erode trust in the accuracy of the measurements. This poster presents Food-MetNet, a coordinated preparatory initiative to establish the European Metrology Network for Safe and Sustainable Food, recently approved by the European Association of National Metrology Institutes (EURAMET). Food-MetNet aims to establish an ongoing dialogue between the metrology community, reference laboratories and regulatory bodies, in order to (i) identify stakeholders’ needs, (ii) develop a sustainable knowledge-sharing programme and web-based platform for stakeholders and (iii) develop roadmaps and a strategic research agenda. Improved access to more reliable and accurate food safety measurements will enable reference laboratories to more confidently and effectively compare their measurement results and support accreditation. This is particularly important where national food safety authorities need to assess potential new contaminants, novel food ingredients and newly emerging food risks, and new measurements methods may be required as well as input into new documentary standards. The activities for sustainable food intend to boost the activity within the "EU green deal framework" to reduce food waste and losses, and the development of standards and methods that allow for the reuse of food waste. The support to new business opportunities and innovation will allow increasing the market competitiveness of EU food industries and the valorisation of waste by reducing environmental impacts. T2 - 10th International Symposium on RECENT ADVANCES IN FOOD ANALYSIS CY - Prague, Czech Republic DA - 06.09.2022 KW - Food KW - Analysis KW - EMN KW - Metrology KW - Network PY - 2022 AN - OPUS4-56133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ermilova, Elena A1 - Weise, Matthias A1 - Hertwig, Andreas T1 - Hybrid optical measurement technique for detection of defects in epitaxially grown 4H-SiC layers N2 - Recent developments in power electronics require the use of new wide bandgap compound semiconductor. We demonstrate the use of the ellipsometry and white light interference microscopy to detect defects in epitaxially grown SiC layers on SiC substrates. Such hybrid optical metrology methods can be used to better understand the mechanism of the development of the defects as well as their effects on the material´s optoelectronic properties. T2 - EOS Annual Meeting (EOSAM 2022) CY - Porto, Portugal DA - 12.09.2022 KW - Imaging ellipsometry KW - White light interference microscopy KW - Wide bandgap compound semiconductor KW - Epitaxially grown 4H-SiC layers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561113 DO - https://doi.org/10.1051/epjconf/202226610001 VL - 266 SP - 1 EP - 2 AN - OPUS4-56111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Shaheen, Sabahat A1 - Hicke, Konstantin T1 - Measurement of Geometric Phase using a φ-OTDR setup N2 - Geometric phase showing sensitivity to changes in polarisation state and intensity of backscattered light is measured using a novel φ-OTDR setup based on coherent heterodyne detection. Principle is demonstrated using a polarisation scrambler inline a fiber-under-test. T2 - Optical Fiber Sensors 2022 CY - Alexandria, Virginia, United States DA - 29.08.2022 KW - Coherent Heterodyne KW - Geometric Phase KW - Distributed Fiber Optic Sensor PY - 2022 SN - 978-1-957171-14-2 SP - W4.72 AN - OPUS4-56116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sieber, M. J. A1 - Wilke, M. A1 - Appelt, O. A1 - Oelze, Marcus A1 - Koch-Müller, M. T1 - Melting relations of Ca–Mg carbonates and trace element signature of carbonate melts up to 9 GPa – A proxy for melting of carbonated mantle lithologies N2 - The most profound consequences of the presence of Ca–Mg carbonates (CaCO3–MgCO3) in the Earth’s upper mantle may be to lower the melting temperatures of the mantle and control the melt composition. Low-degree partial melting of a carbonate-bearing mantle produces CO2-rich, silica-poor melts compositionally imposed by the melting relations of carbonates. Thus, understanding the melting relations in the CaCO3–MgCO3 system facilitates the interpretation of natural carbonate-bearing silicate systems. We report the melting relations of the CaCO3–MgCO3 system and the partition coefficient of trace elements between carbonates and carbonate melt from experiments at high pressure (6 and 9 GPa) and temperature (1300–1800 ◦C) using a rocking multi-anvil press. In the absence of water, Ca–Mg carbonates are stable along geothermal gradients typical of subducting slabs. Ca–Mg carbonates (∼ Mg0.1–0.9Ca0.9–0.1CO3) partially melt beneath mid-ocean ridges and in plume settings. Ca–Mg carbonates melt incongruently, forming periclase crystals and carbonate melt between 4 and 9 GPa. Furthermore, we show that the rare earth element (REE) signature of Group-I kimberlites, namely strong REE fractionation and depletion of heavy REE relative to the primitive mantle, is resembled by carbonate melt in equilibrium with Ca-bearing magnesite and periclase at 6 and 9 GPa. This suggests that the dolomite–magnesite join of the CaCO3–MgCO3 system might be useful to approximate the REE signature of carbonate-rich melts parental to kimberlites. KW - High pressure experiments KW - Laser Ablation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561197 DO - https://doi.org/10.5194/ejm-34-411-2022 SN - 0935-1221 VL - 34 IS - 5 SP - 411 EP - 424 PB - Copernicus Publications CY - Göttingen AN - OPUS4-56119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, U. A1 - Jaenisch, Gerd-Rüdiger A1 - Schumacher, David A1 - Bircher, B. A1 - Meli, F. A1 - Deresch, A. T1 - EMPIR-Projekt NanoXSpot: Neue Normentwürfe für die Brennfleckmessung an Röntgenröhren im Makro-, Mikro- und Nanometerbereich für Hersteller und Anwender N2 - Im Rahmen des EMPIR-Projektes NanoXSpot (Nanometre X-ray Focal Spot Measurement) werden rückführbare Messverfahren zur Bestimmung der Brennfleckgröße und -form von Röntgenröhren im Bereich von 100 nm bis 10 mm entwickelt, welche die Grundlage für die Erarbeitung mehrerer Normentwürfe bilden. Diese werden 2022 parallel bei ISO TC 135 (NDT) SC 5 (RT) und CEN TC 138 (NDT) WG 1 (RT) eingereicht. Entsprechende Normen werden auch bei ASTM vorgestellt. Die Norm EN 12543-4 (Kantenmethode) wird umgeschrieben für die Messung von Brennflecken von 1 μm – 10 mm durch Auswertung von Loch- oder Scheibenaufnahmen. Der im Rahmen des NanoXSpot-Projektes neu entwickelte NxS-Testkörper ist geeignet für den Bereich von 1 μm – 100 μm. Von 100 μm bis 10 mm können ASTM-Lochtestkörper verwendet werden, die bereits bei ASTM E 1165 beschrieben sind. Neu ist die Anwendung eines CT-Algorithmus zur Rekonstruktion der Brennflecke, um Lochblenden-basierte Brennfleckkameras, insbesondere im Bereich unter 100 μm, zu ersetzen. Ein neuer Normteil, EN 12543-6, wurde entworfen, um die Brennfleckmessung im Bereich 100 nm – 20 μm mit hoher Genauigkeit zu ermöglichen. Verschiedene Strichgruppen-Testkörper kommen hier zum Einsatz. Das sind die JIMAPrüfkörper, ein neuer Hochkontrast-Strichgruppentestkörper von YXLON (HiCo) und der neu entwickelte Testkörper NxS. Diese werden vorgestellt. Die Messprozedur für Röhrenhersteller wird auf einer numerischen Fit-Prozedur basieren, die über einen Ringversuch im Projekt validiert wurde. Beide Normen benötigen numerische Auswertealgorithmen zur korrekten Anwendung, die als kommerzielle Software und Public Domain – Software verfügbar gemacht werden. Es wird über die zu erwartenden Standardprozeduren und die erforderliche Hardware zur Anwendung der Normen informiert. T2 - DGZfP-Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Röntgenröhre KW - Brennfleckmessung KW - Normung PY - 2022 AN - OPUS4-56100 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, U. A1 - Jaenisch, Gerd-Rüdiger A1 - Schumacher, David A1 - Bircher, B. A1 - Meli, F. A1 - Deresch, A. T1 - EMPIR-Projekt NanoXSpot: Neue Normentwürfe für die Brennfleckmessung an Röntgenröhren im Makro-, Mikro- und Nanometerbereich für Hersteller und Anwender N2 - Im Rahmen des EMPIR-Projektes NanoXSpot (Nanometre X-ray Focal Spot Measurement) werden rückführbare Messverfahren zur Bestimmung der Brennfleckgröße und -form von Röntgenröhren im Bereich von 100 nm bis 10 mm entwickelt, welche die Grundlage für die Erarbeitung mehrerer Normentwürfe bilden. Diese werden 2022 parallel bei ISO TC 135 (NDT) SC 5 (RT) und CEN TC 138 (NDT) WG 1 (RT) eingereicht. Entsprechende Normen werden auch bei ASTM vorgestellt. Die Norm EN 12543-4 (Kantenmethode) wird umgeschrieben für die Messung von Brennflecken von 1 μm – 10 mm durch Auswertung von Loch- oder Scheibenaufnahmen. Der im Rahmen des NanoXSpot-Projektes neu entwickelte NxS-Testkörper ist geeignet für den Bereich von 1 μm – 100 μm. Von 100 μm bis 10 mm können ASTM-Lochtestkörper verwendet werden, die bereits bei ASTM E 1165 beschrieben sind. Neu ist die Anwendung eines CT-Algorithmus zur Rekonstruktion der Brennflecke, um Lochblenden-basierte Brennfleckkameras, insbesondere im Bereich unter 100 μm, zu ersetzen. Ein neuer Normteil, EN 12543-6, wurde entworfen, um die Brennfleckmessung im Bereich 100 nm – 20 μm mit hoher Genauigkeit zu ermöglichen. Verschiedene Strichgruppen-Testkörper kommen hier zum Einsatz. Das sind die JIMAPrüfkörper, ein neuer Hochkontrast-Strichgruppentestkörper von YXLON (HiCo) und der neu entwickelte Testkörper NxS. Diese werden vorgestellt. Die Messprozedur für Röhrenhersteller wird auf einer numerischen Fit-Prozedur basieren, die über einen Ringversuch im Projekt validiert wurde. Beide Normen benötigen numerische Auswertealgorithmen zur korrekten Anwendung, die als kommerzielle Software und Public Domain – Software verfügbar gemacht werden. Es wird über die zu erwartenden Standardprozeduren und die erforderliche Hardware zur Anwendung der Normen informiert. T2 - DGZfP-Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Röntgenröhre KW - Brennfleckmessung KW - Normung PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561029 SP - 1 EP - 10 AN - OPUS4-56102 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumacher, David A1 - Jaenisch, Gerd-Rüdiger A1 - Ewert, U. A1 - Bircher, B. A1 - Meli, F. A1 - Sofiienko, A. A1 - Steffen, J. P. A1 - Deresch, A. T1 - EMPIR-Projekt NanoXSpot: Ringversuch zur Untersuchung der neu entwickelten Methoden für die Brennfleckmessung an Röntgenröhren im Mikro- und Nanometerbereich N2 - Im Rahmen des EMPIR-Projektes NanoXSpot (Nanometre X-Ray Focal Spot Measurement) werden rückführbare Messverfahren zur Bestimmung der Brennfleckgröße und -form von Röntgenröhren mit Submikrometerauflösung (100 nm – 20 μm) entwickelt, die die Grundlage für die Erarbeitung eines Standardentwurfes bilden. Der Standardentwurf wird bei CEN TC 138 (Non-destructive testing) WG 1 (Radiographic testing) eingereicht und mit ISO und ASTM harmonisiert. Zur Untersuchung der entwickelten Methoden (Brennfleck-CT, Fit-Prozedur für Strichgruppenkörper) und des im Projekt NanoXSpot neu entworfenen Testkörpers, NxS, wurde ein Ringversuch durchgeführt. Dabei wurde sowohl der angestrebte Überlappungsbereich mit EN 12543 Teil 5 (Messung der effektiven Brennfleckgröße von Mini- und Mikrofokus-Röntgenröhren) und ASTM E 2903 (Standard Test Method for Measurement of the Effective Focal Spot Size of Mini and Micro Focus X-ray Tubes) für Brennflecke >5 μm als auch Brennflecke <5 μm untersucht. Im Mittelpunkt standen dabei Stabilität und Wiederholbarkeit der entwickelten Methoden zur Bestimmung der Brennfleckgröße. In diesem Beitrag werden die Ergebnisse des durchgeführten Ringversuches vorgestellt und diskutiert, um Schlussfolgerungen und Empfehlungen für die Vorbereitung eines erweiterten Ringversuchs mit Partnern und Stakeholdern abzuleiten. T2 - DGZfP-Jahrestagung CY - Kassel, Germany DA - 23.05.2022 KW - Brennfleckmessung KW - Computer-Tomografie KW - EMPIR KW - Normung PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561037 SP - 1 EP - 2 AN - OPUS4-56103 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Philipp, Rosemarie A1 - Lalere, B. A1 - Gantois, F. A1 - Sánchez, C. A1 - Sáez, A. A1 - Bebić, J. A1 - Banjanac, K. A1 - Alexopoulos, Ch. A1 - Kakoulides, E. A1 - Claramunt, A. V. A1 - Janko, P. A1 - Jotanovic, A. A1 - Hafner-Vuk, K. A1 - Buzoianu, M. A1 - Mihail, R. A1 - Fernández, M. M. A1 - Etcheverry, J. A1 - Mbithi Muendo, B. A1 - Muriira Karau, G. A1 - Silva, A. A1 - Almirón, F. A1 - Marajh, D. A1 - Makgatho, P. A1 - Visser, R. A1 - Alaskar, A. R. A1 - Alosaimi, A. A1 - Alrashed, M. A1 - Yılmaz, H. A1 - Ün, İ. A1 - Gündüz, S. A1 - Topal, K. A1 - Bilsel, M. A1 - Karasinski, J. A1 - Torres, J. T1 - Supplementary comparison study - measurement capabilities for the quantification of ethanol in water N2 - The accurate quantification of ethanol in water is essential for forensic applications such as blood and breath alcohol testing and for commercial applications such as the assessment of alcoholic beverages. The intercomparison EURAMET.QM-S14 is part of a capacity building project named ALCOREF “Certified forensic alcohol reference materials” that is running within the European Metrology Programme for Innovation and Research (EMPIR). The intercomparison should allow project partners and other interested National Metrology Institutes (NMIs) and Designated Institutes (DIs) to benchmark their analytical methods for the quantification of ethanol in water. The study plan was agreed by the European Association of National Metrology Institutes (EURAMET) Subcommittee Bio- and Organic Analysis (SCBOA) and the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) in February and April 2019, respectively. The intercomparison was coordinated by BAM. Two concentration levels relevant for the calibration and verification of evidential breath alcohol analysers were distributed to study participants. Fifteen institutes from 15 countries registered for the intercomparison and returned results. Participants mostly applied gas chromatography with flame ionisation detection (GC-FID) or mass spectroscopy (GC-MS), one participant used titrimetry and one participant employed a test bench for breath analyser calibration (“bubble train”). Participants did either in-house purity assessment of their commercial ethanol calibrants by Karl-Fischer titration, chromatographic methods, quantitative nuclear magnetic resonance spectroscopy (qNMR) and/or density measurements; or they used ethanol/water Certified Reference Materials (CRMs) from NMIs/DIs for calibration. CCQM OAWG agreed to use a consensus value from participants results that utilizes the reported uncertainties as Key Comparison Reference Value (KCRV). The Gaussian Random effects model with Hierarchical Bayesian solution (HB-REM) is a reasonable approach in this case. The KCRVs and Degrees of Equivalence (DoEs) were calculated with the NIST consensus builder version 1.2 Hierarchical Bayes procedure. Successful participation in the interlaboratory comparison has demonstrated the capabilities in determining the mass fraction of ethanol in aqueous matrices in the range 0.1 mg/g to 8 mg/g. Fourteen out of 15 participants have successfully quantified both samples, one participant successfully quantified only the lower-level (0.6 mg/g) sample. KW - Certified reference material KW - EURAMET KW - EMPIR KW - ALCOREF KW - Ethanol in water KW - Supplementary comparison PY - 2022 DO - https://doi.org/10.1088/0026-1394/59/1A/08015 VL - 59 IS - 1A SP - 08015 PB - IOP Publishing AN - OPUS4-55889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Burgmayer, R. A1 - Bake, Friedrich A1 - Enghardt, L. T1 - Design and Evaluation of a Zero Mass Flow Liner N2 - In this study, the concept of a zero mass flow liner is evaluated. The concept enables impedance control by theinduction of, acoustically actuated, periodic bias flowthrough the facing sheet of the liner. Bymeans of the periodic bias flow, the impedance of the liner is adapted to different grazing flowconditions.The equivalent fluid impedancemodel for perforated plates is modified to account for the effects of periodic bias and grazing flow. A generally applicable optimization routine, using the impedance of the lined surface as a boundary condition in a numeric calculation, is implemented. Based on the results of the optimization, a zero mass flow liner is manufactured and evaluated experimentally. The damping characteristics are assessed in the form of dissipated energy along the lined surface. Prediction and measurements show reasonable agreement. The zero mass flow liner delivers broadband dissipation of high peak value over a range of grazing flow Mach numbers. Under grazing flow, the effect of periodic bias flow is reduced. For a ratio of grazing to bias flow velocities larger than five, no appreciable effect is found. This poses considerable energy requirements on the actuation source for the application in high-Mach-number flow regimes. KW - Zero Massflow Liner KW - Acoustic Damping KW - Liner PY - 2022 DO - https://doi.org/10.2514/1.J062197 SN - 1533-385X SP - 1 EP - 12 PB - AIAA CY - Reston, Va. AN - OPUS4-56410 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haratsu, T. A1 - Neumann, Patrick P. T1 - Simulating a Gas Source Localization Algorithm with Gas Dispersion Produced by Recorded Outdoor Wind N2 - This presentation reports the use of the first gas dispersion simulator capable of generating large wind fluctuation, to test a modification to a gas source localization algorithm and study how the change affects it. Gas source localization at an outdoor environment is a challenging task mainly due to the complexity of the spreading gas caused by the unpredictable nature of constantly changing wind. Therefore, a novel use of outdoor wind in developing a gas source localization system by simulation will be shared. To consider the characteristic of sudden but large and unpredictable changes in wind direction, recorded outdoor wind was used to simulate a realistic outdoor gas dispersion which has been done for the first time. With the use of this simulator, a modification to a mobile robot-based gas source localization algorithm was evaluated. Multiple simulations of the modified and the original algorithm were done to study the effect of the tested modification. The results showed that a small difference in the algorithm can greatly impact the results. From this study, we consider the use of simulation consisting of the necessary traits to evaluate outdoor gas source localization, has the potential to accelerate the development of a reliable localization system. T2 - ROBOT2022: Fifth Iberian Robotics Conference CY - Zaragoza, Spain DA - 23.11.2022 KW - Gas Dispersion Simulator KW - Gas Source Localization KW - Mobile Robot Olfaction KW - Particle Filter PY - 2022 AN - OPUS4-56413 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. A1 - Kotlyar, O. A1 - Schaffernicht, E. A1 - Fan, H. A1 - Matsukura, H. A1 - Ishida, H. A1 - Neumann, Patrick P. A1 - Lilienthal, A. J. ED - Tardioli, D. ED - Matellán, V. ED - Heredia, G. ED - Silva, M. F. ED - Marques, L. T1 - Learning From the Past: Sequential Deep Learning for Gas Distribution Mapping N2 - To better understand the dynamics in hazardous environments, gas distribution mapping aims to map the gas concentration levels of a specified area precisely. Sampling is typically carried out in a spatially sparse manner, either with a mobile robot or a sensor network and concentration values between known data points have to be interpolated. In this paper, we investigate sequential deep learning models that are able to map the gas distribution based on a multiple time step input from a sensor network. We propose a novel hybrid convolutional LSTM - transpose convolutional structure that we train with synthetic gas distribution data. Our results show that learning the spatial and temporal correlation of gas plume patterns outperforms a non-sequential neural network model. T2 - ROBOT2022: Fifth Iberian Robotics Conference CY - Zaragoza, Spain DA - 22.11.2022 KW - Gas Distribution Mapping KW - Spatial Interpolation KW - Sequential Learning KW - Convolutional LSTM PY - 2023 SN - 978-3-031-21061-7 DO - https://doi.org/10.1007/978-3-031-21062-4_15 SP - 178 EP - 188 PB - Springer International Publishing AN - OPUS4-56414 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. T1 - Learning From the Past: Sequential Deep Learning for Gas Distribution Mapping N2 - To better understand the dynamics in hazardous environments, gas distribution mapping aims to map the gas concentration levels of a specified area precisely. Sampling is typically carried out in a spatially sparse manner, either with a mobile robot or a sensor network and concentration values between known data points have to be interpolated. In this paper, we investigate sequential deep learning models that are able to map the gas distribution based on a multiple time step input from a sensor network. We propose a novel hybrid convolutional LSTM - transpose convolutional structure that we train with synthetic gas distribution data. Our results show that learning the spatial and temporal correlation of gas plume patterns outperforms a non-sequential neural network model. T2 - ROBOT2022: Fifth Iberian Robotics Conference CY - Zaragoza, Spain DA - 22.11.2022 KW - Gas Distribution Mapping KW - Spatial Interpolation KW - Sequential Learning KW - Convolutional LSTM PY - 2022 AN - OPUS4-56415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haratsu, T. A1 - Sakaue, M. A1 - Matsukura, H. A1 - Neumann, Patrick P. A1 - Ishida, H. ED - Tardioli, D. ED - Matellán, V. ED - Heredia, G. ED - Silva, M. F. ED - Marques, L. T1 - Simulating a Gas Source Localization Algorithm with Gas Dispersion Produced by Recorded Outdoor Wind N2 - This paper reports the use of the first gas dispersion simulator capable of introducing large wind fluctuations into simulations. The proposed simulator enables testing of a modification made to a gas source localization algorithm in a realistic scenario in order to study how the change affects it. Gas source localization in an outdoor environment is a challenging task mainly due to the complexity of the gas spread caused by the unpredictable nature of constantly changing wind. Therefore, a novel use of outdoor wind in developing a gas source localization system by simulation is presented in this paper. To consider the characteristic of sudden but large and unpredictable changes in wind direction, we propose to use recorded outdoor wind to simulate a realistic outdoor gas dispersion which has been done for the first time to the best of our knowledge. With the use of this simulator, we have tested a modification to a mobile robot-based gas source localization algorithm. Multiple simulations of the modified and the original particle filter-based algorithm have been done to study the effect of the tested modification. The results showed that a small difference in the algorithm can greatly impact the results. From this study, we show that the use of simulation consisting of the necessary traits to evaluate outdoor gas source localization, has the potential to accelerate the development of a reliable localization system. T2 - ROBOT2022: Fifth Iberian Robotics Conference CY - Zaragoza, Spain DA - 23.11.2022 KW - Gas Dispersion Simulator KW - Gas Source Localization KW - Mobile Robot Olfaction KW - Particle Filter PY - 2023 SN - 978-3-031-21061-7 DO - https://doi.org/10.1007/978-3-031-21062-4_9 SP - 105 EP - 116 PB - Springer AN - OPUS4-56416 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Tchipilov, Teodor A1 - Meyer, Klas A1 - Weller, Michael G. T1 - Quantitative 1H nuclear magnetic resonance (qNMR) of aromatic amino acids for protein quantification N2 - qNMR is a valuable technique for metrological studies due to the uniformity of its signal response for all chemical species of an isotope of interest, which enables compound-independent calibration. However, protein quantification remained challenging as large molecules produce wide, low-intensity signals that reduce the already low sensitivity. Combining qNMR with the hydrolysis of protein samples into amino acids circumvents many of these issues and facilitates the use of NMR spectroscopy for absolute protein and peptide quantification.In this work, different conditions have been tested for quantifying aromatic amino acids and proteins. First, we examined the pH-based signal shifts in the aromatic region. The preferable pH depends on the selection of the amino acids for quantification and which internal standard substance should be used to avoid peak overlap. Several aromatic compounds, such as terephthalic acid, sulfoisophthalic acid, and benzene tricarboxylic acid, have been applied as internal standards. The quantification of amino acids from an amino acid standard, as well as from a certified reference material (bovine serum albumin), was performed. Using the first two suggested internal standards, recovery was ~ 97 % for histidine, phenylalanine, and tyrosine at a concentration of approximately 1 mM in solution. Acidic hydrolysis of a certified reference material (CRM) of bovine serum albumin (BSA) and subsequent quantification of Phe and Tyr yielded recoveries of 98 ± 2 and 88 ± 4 %, respectively, at a protein concentration of 16 g/L or 250 µM. KW - Amino acid analysis KW - AAA KW - Protein hydrolysis KW - Metrology KW - Traceability KW - Reference materials KW - Internal standards KW - Calibration PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564520 DO - https://doi.org/10.20944/preprints202211.0569.v1 SP - 1 EP - 13 PB - MDPI CY - Basel AN - OPUS4-56452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Linberg, Kevin T1 - Polymorphism in molecular cocrystals controlled by variable temperature ball milling N2 - Mechanochemistry offers a unique opportunity to modify or synthesize new crystal forms. Although the method is very promising, little is known about the mechanochemical means to control the synthesis of a solid form. Using an polymorphic organic cocrystal system, we show here that mechanochemistry can be used to obtain a polymorph transformation under the apparently conventional (thermal) transition point. T2 - Bessy User Meeting 2022 CY - Online meeting DA - 08.12.2022 KW - Mechanochemistry KW - Polymorphism KW - TRIS PY - 2022 AN - OPUS4-56473 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schleeh, T. A1 - Rötting, O. A1 - Bettge, Dirk A1 - Hinrichsen, G. T1 - Alkoxy-substituted liquid-crystalline aromatic copolyesters, 2 N2 - Number-average molecular weights and inherent viscosities were found for the soluble members of an alkoxy-substituted copolyester series. A liquid-crystalline (high-temperature) phase was distinguisehd by IR and wide-angle X-ray scattering on molten and quenched samples in form of a nematic sanidic phase. In this phase no relationship exists between the orientation of the aromatic polyester backbone and that of the laterally attracted alkoxy groups. Further, it was proven by IR that only the polyester backbone can be aligned by shear stress. If the applied shear stress is very strong, the orientation of the stiff backbone becomes sensitive to disturbance caused by mechanical forces. KW - Liquid-crystalline polymers PY - 1993 DO - https://doi.org/10.1002/macp.1993.021940304 VL - 194 IS - 3 SP - 791 EP - 798 PB - Hüthig & Wepf CY - Basel AN - OPUS4-56486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zabihi, Mohammadmasoud A1 - Krebber, Katerina T1 - Approach for Faster Signal Processing in Փ-OTDR Systems Based on Directional Measurement of Fiber Slices Interaction N2 - In this study, a signal processing approach for heterodyne Փ-OTDR and C-OTDR systems that can obtain external perturbation and its frequency content in a faster way is proposed. We can detect vibrations with the same or better SNR using this processing approach, only with a single step and fast calculation. Fig. 12 shows the comparison of the normalized measurement time for the gamma matrix method and the conventional method throughout the three experiments. The speed of processing using a gamma matrix is ~35%–50% faster compared to a conventional method in high frequency test (PZT), low frequency test (walking) and street monitoring test. The processing speed in low frequency test is normally a bit lower than the similar high frequency one, since we must use higher number of time frames. Also, in street test we have higher speed because we can select wider gauges. KW - Փ-OTDR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560492 DO - https://doi.org/10.1364/OPTCON.456421 VL - 1 IS - 8 SP - 1837 EP - 1847 PB - Optica Publishing Group CY - Washington, DC AN - OPUS4-56049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zabihi, Mohammadmasoud A1 - Krebber, Katerina T1 - Laser source frequency drift compensation in Φ-OTDR systems using multiple probe frequencies N2 - In this study, an approach for mitigation of LSFD in Φ-OTDR systems was proposed. By using one probe pulse as a reference in a system with two or more probe frequencies, we can remove unwanted low frequency noise that is originally caused by the laser source. Although LSFD is problematic issue, it is not the only source of low frequency noise. Change in temperature, humidity, physical surroundings, environment, etc., can result in such noises. The proposed method; however, is expected to highly suppresses all of these effects, regardless of their source, either in the time or frequency domain. For comparing reference and probe signals, there are sophisticated methods, rather than normal differentiation, available for use. Some of these methods have a close relationship with CPD methods and can further enhance the results. These methods can be further discussed in an independent research or future work. The proposed method is very helpful for increasing accuracy in passive and active seismic monitoring, reservoir monitoring, underwater monitoring, etc. It also helps using relatively simpler laser sources and make the whole system price-efficient, as well as processing data without lengthy compensation algorithms. KW - Frequency Drift KW - Փ-OTDR KW - LSFD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560517 DO - https://doi.org/10.1364/oe.460302 SN - 1094-4087 VL - 30 IS - 11 SP - 19990 EP - 19998 PB - Optica CY - Washington, DC AN - OPUS4-56051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - DICONDE für die Schienenprüfung N2 - Einführung in DICONDE und deren Verwendung bei der Prüfung verlegter Eisenbahnschienen im Projekt AIFRI. T2 - Projektmeeting AIFRI CY - Online meeting DA - 27.09.2022 KW - DICONDE KW - ZfP KW - I4.0 PY - 2022 AN - OPUS4-55940 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kaufmann, Jan Ole T1 - Finding the Ticking Timebomb - MRI probe for the detection of aneurysms N2 - Screening against ADAMTS4 reveals a specific peptide, which was turned into an MRI probe. The aneurysm in a mouse modal was visualized via MRI. A differentiation between stable and unstable aneurysm in an early state was performed. Using the probe as tool for an easy and non-invasive rupture assessment is possible. T2 - Adlershofer Forschungsforum 2022 CY - Berlin, Germany DA - 11.11.2022 KW - Magnetic resonance imaging KW - Peptide library KW - OBOC library KW - Synthetic peptides KW - Contrast agent KW - Imaging KW - ADAMTS4 KW - MALDI-TOF mass spectrometry KW - Cardiovascular diseases KW - Medicine KW - Diagnostic KW - Screening KW - Risk assessment KW - Aorta PY - 2022 AN - OPUS4-56313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard T1 - dataMerge V0.1 - A statistics-aware binning and merging backend N2 - A tool for merging and/or rebinning single or multiple datasets to achieve a lower point density with best possible statistics. highly scriptable, CLI, no GUI Version 0.1: works but could do with a cleanup. Weighting by uncertainty currently always on, but should be optional for use as an azimuthal or radial averager KW - X-ray science KW - Image averaging KW - Dataset merging KW - Photon counting detectors KW - SAXS KW - SANS KW - X-ray scattering KW - X-ray diffraction PY - 2022 DO - https://doi.org/10.6084/m9.figshare.21591360 PB - Digital Science CY - Cambridge, MA, USA AN - OPUS4-56340 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Vogel, Christian A1 - Roesch, Philipp A1 - Wittwer, Philipp A1 - Simon, Franz-Georg ED - Holm, O. ED - Thomé-Kozmiensky, E. ED - Quicker, P. ED - Kopp-Assenmacher, S. T1 - Per- und polyfluorierte Alkylsubstanzen (PFAS) im Klärschlamm N2 - Per- and polyfluoroalkyl substances (PFAS) are a group of more than 4700 anionic and cationic anthrophonic substances which have been used extensively in a variety of products and industries due to their inert chemical stability and resistance to degradation by heat or acids. As a result of continuous use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil and groundwater resources. However, because of the continuous use of fluorinated consumer products, also effluents and sewage sludge from wastewater treatment plants (WWTPs) have been shown to be an important source of PFAS contamination into the aquatic environment. Resulting from recent stricter regulations and restrictions in the last years on the use of long chain (≥C8) PFAS, there is a significant shift in the chemical industry towards production of short (C4-C7) and ultrashort (C1-C3) chain alternatives. With the amendment of the Sewage Sludge Ordinance in 2017 the German legislation banned sewage sludge application on agricultural land, and by 2029/2032 sewage sludge will be completely prohibited from agricultural application. While environmental exposure of organic pollutants like PFAS, pesticides and pharmaceuticals are no longer desirable, phosphorus (P) from sewage sludge must still be used to produce high-quality P-fertilizers for a circular economy. Currently, plant-available P-fertilizers from sewage sludge/wastewater can be produced using a variety of treatment approaches including precipitation, leaching, and thermal treatment. However, the fate of legacy and emerging PFAS compounds during P leaching, precipitation and treatment from sewage sludge and wastewater is for the most parts still unknown. KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Klärschlamm KW - Düngemittel PY - 2022 SN - 978-3-944310-65-7 SP - 270 EP - 279 PB - Thomé-Kozmiensky Verlag GmbH CY - Neuruppin AN - OPUS4-56290 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Per- und polyfluorierte Alkylsubstanzen (PFAS) im Klärschlamm - Analytische Methoden und Grenzwerte N2 - Per- und Polyfluoralkylsubstanzen (PFAS) sind eine Gruppe von mehr als 4700 anionischen und kationischen anthrophonen Stoffen, die aufgrund ihrer inerten chemischen Stabilität und ihrer Widerstandsfähigkeit gegen den Abbau durch Hitze oder Säuren in einer Vielzahl von Produkten verwendet werden. Infolge der ständigen Verwendung, vor allem in Feuerlöschschäumen für die Luftfahrt, wurden in Tausenden von Industrie- und Militäranlagen kontaminierte Böden und Grundwasservorkommen gefunden. Aufgrund der ständigen Verwendung von fluorierten Konsumgütern haben sich jedoch auch Abwässer und Klärschlamm aus Kläranlagen als Quelle für die Kontamination der aquatischen Umwelt mit PFAS erwiesen. Infolge der strengeren Vorschriften und Beschränkungen, die in den letzten Jahren für die Verwendung langkettiger (≥C8) PFAS erlassen wurden, findet in der chemischen Industrie eine deutliche Verlagerung hin zur Herstellung kurz- (C4-C7) und ultrakurzkettiger (C1-C3) Alternativen statt. Mit der Novellierung der Klärschlammverordnung im Jahr 2017 hat der deutsche Gesetzgeber die Ausbringung von Klärschlamm auf landwirtschaftlichen Flächen verboten, und bis 2029/2032 wird die Ausbringung von Klärschlamm in der Landwirtschaft vollständig verboten sein. Während die Belastung der Umwelt mit organischen Schadstoffen wie PFAS, Pestiziden und Arzneimitteln nicht mehr erwünscht ist, muss Phosphor (P) aus Klärschlamm weiterhin zur Herstellung hochwertiger P-Dünger für eine Kreislaufwirtschaft genutzt werden. Derzeit können pflanzenverfügbare P-Düngemittel aus Klärschlamm/Abwasser mit verschiedenen Behandlungsmethoden hergestellt werden, darunter Fällung, Auslaugung und thermische Behandlung. Der Verbleib von PFAS bei der Auslaugung, Ausfällung und Behandlung von Klärschlamm und Abwasser ist jedoch noch weitgehend unbekannt. T2 - Berliner Klärschlammkonferenz CY - Berlin, Germany DA - 14.11.2022 KW - Klärschlamm KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Phosphor KW - Düngemittel PY - 2022 AN - OPUS4-56291 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Energy Resolved Imaging with Coded Apertures N2 - Our aim is to develop a simple and inexpensive method for full field X-ray fluorescence imaging.We combine an energydispersive array detector with a coded aperture to obtain high resolut ion images. To obtain the information from the recorded image a reconstruction step is necessary. The reconstruction methods we have developed, were tested on simulated data and then applied to experimental data. The first tests were carried out at the BAMline @BESSY II. This method enables the simultaneous detection of multiple elements,which is important e.g. in the field of catalysis. T2 - SRI 2021 CY - Online meeting DA - 28.3.2022 KW - Synchrotron KW - BAMline KW - Machine Learning KW - Coded Aperture PY - 2022 AN - OPUS4-56298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Hampel, S. A1 - Fittschen, UEA A1 - Streli, C. A1 - Radtke, Martin T1 - Reconstruction for coded aperture full-field x-ray fluorescence imaging N2 - X-ray fluorescence imaging is a well-established tool in materials characterization. In this work, we present the adaption of coded aperture imaging to full-field X-ray fluorescence imaging at the synchrotron. Coded aperture imaging has its origins in astrophysics, and has several advantages: Coded apertures are relatively easy to fabricate, achromatic, allow a high photon throughput, and high angular acceptance. Coded aperture imaging is a two-step-process, consisting of the measurement process and a reconstruction step. Different programs have been written, for the raytracing/forward projection and the reconstruction. Experiments with coded aperture in combination with a Color X-ray Camera and an energy-dispersive area detector, have been conducted at the BAMline. Measured samples were successfully reconstructed, and gave a 9.1-fold increase in count rate compared to a polycapillary optic. KW - Synchrotron KW - BAMline KW - Coded Aperture PY - 2022 SN - 1097-0002 VL - 65 SP - 57 EP - 70 PB - Cambridge University Press CY - Cambridge AN - OPUS4-56350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steinhäuser, Lorin A1 - Piechotta, Christian A1 - Westphalen, Tanja A1 - Kaminski, Katja T1 - Evaluation, comparison and combination of molecularly imprinted polymer solid phase extraction and classical solid phase extraction for the preconcentration of endocrine disrupting chemicals from representative whole water samples N2 - Estrogens are endocrine disrupting chemicals and of high concerns due to demonstrated harmful effects on the environment and low effect levels. For monitoring and risk assessment, several estrogens were included in the "watch list" of the EU Water Framework Directive which sets very low environmental quality standard (EQS) levels for Estrone (E1) and 17β-Estradiol (E2) of 0.4 ng L−1 and for 17α-Ethinylestradiol (EE2) of 0.035 ng L−1 requiring sensitive detection methods, as well as extensive sample preparation. A sensitive, derivatization-free, isotope dilution calibration HPLC-MS/MS method for a panel of 5 selected estrogens (including the 3 estrogens of the EU WFD watchlist), and a procedure for the reproducible preparation of a representative whole water matrix including mineral water, humic acids and solid particulate matter are presented. These are used in a diligent comparison of classical solid phase extraction (SPE) on hydrophilic-lipophilic balanced (HLB) phase to SPE on an estrogen-specific molecularly imprinted polymer phase (MISPE) for ultra-trace levels of the analytes (1–10 ng L−1). Additionally, a two-step procedure combining HLB SPE disks followed by MISPE is evaluated. The tow-step procedure provides superior enrichment, matrix removal and sample throughput while maintaining comparable recovery rates to simple cartridge SPE. Estimated method quantification limits (MQLs) range from 0.109–0.184 ng L−1 and thus meet EQS-levels for E1 and E2, but not EE2. The representative whole water matrix provides a reproducible comparison of sample preparation methods and lays the foundation for a certified reference material for estrogen analysis. The presented method will serve as the basis for an extended validation study to assess its use for estrogen monitoring in the environment. KW - Estrogens KW - Whole water samples KW - Molecular imprinted polymers KW - EU-WFD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563547 DO - https://doi.org/10.1016/j.talo.2022.100163 SN - 2666-8319 VL - 6 SP - 1 EP - 5 PB - Elsevier B.V. CY - Amsterdam, Niederlande AN - OPUS4-56354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Fabian T1 - HR-CS-GFMAS as a new screening method for emerging pollutants – per- and polyfluoroalkyl substances (PFASs) in the environment N2 - Per- and polyfluorinated alkyl substances (PFASs) are a group of several thousand individual compounds. Many PFASs are extremely persistent, bioaccumulative and toxic. The analysis of PFASs is challenging because of their various chemical and physical properties as well as the high number of compounds. Target-based approaches (e.g., LC-MS/MS) are limited to the availability of analytical grade standards and are not suitable for the analysis of new/unknown PFASs and transformation products. Therefore, PFAS sum parameter methods become increasingly important to indicate realistic PFAS pollution levels. PFAS sum parameters display the proportion of organically bound fluorine that can either be extracted (EOF) or adsorbed to activated carbon (AOF). For the instrumental analysis of such sum parameters, a fluorine selective detector is needed. High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) is a sensitive and highly selective tool for fluorine determination. The method is based on the in situ formation of diatomic gallium-mono fluoride (GaF) in a graphite furnace at a temperature of 1550°C. The molecular absorption of GaF can be detected at its most sensitive wavelength at 211.248 nm providing limits of quantification of c(F) 2.7 µg/L. In the present work a HR-CS-GFMAS method for EOF analysis was utilized for suspended particulate matter (SPM) analysis in German rivers in time lines from 2005–2020. Therefore, time and spatial resolved trends were investigated. In addition, SPM samples were analyzed for the Σ41PFAS using target analysis based on UHPLC-HRMS. Overall, target analysis drastically underestimated the total PFAS burden in SPM of German rivers compared to the EOF HR-CS-GFMAS analysis. Using a fluorine mass balance approach, only 0.2% to 38.6% of the EOF was explainable using the Σ41PFAS determined with target analysis. Our study highlights the need to integrate PFAS sum parameters (e.g., EOF with HR-CS-GFMAS) in PFAS risk assessment strategies. T2 - Adlershofer Forschungsforum 2022 CY - Berlin, Germany DA - 11.11.2022 KW - PFAS KW - HR-CS-GFMAS KW - Fluorine KW - SPM PY - 2022 AN - OPUS4-56392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ehlers, Henrik A1 - Thewes, R. A1 - Pelkner, Matthias T1 - Online Process Monitoring for Additive Manufacturing Using Eddy Current Testing With Magnetoresistive Sensor Arrays N2 - The rising popularity of additive manufacturing processes leads to an increased interest in possibilities and methods for related process monitoring. Such methods ensure improved process quality and increase the understanding of the manufacturing process, which in turn is the basis for stable component quality, e.g., required in the aerospace industry or in the medical sector. For laser powder bed fusion, a handful of process monitoring tools already exist, such as optical tomography, thermography, pyrometry, imaging, or laser power monitoring. Although these tools provide helpful information about the process, more information is required for an accurate in-depth understanding. In this article, advanced approaches in eddy current testing (ET) are combined, such as single wire excitation, magnetoresistive (MR) sensor arrays, and heterodyning to build up a system that can be used for online process monitoring of laser powder bed fusion. In addition to detailed information about the developed ET system and underlying signal processing, the first results of magnetoresistance-basedonline ET during the laser powder fusion process are presented. While producing a step-shaped cuboid, each layer is tested during recoating. Test results show that not only the contours of the topmost layer are detected but also the contours of previous layers covered by powder. At an excitation frequency of 1 MHz, a penetration depth of approx. 400 μm is obtained. To highlight the possibilities of ET for online process monitoring of laser powder bed fusion, results are compared with postexposure images of the integrated layer control system (LCS). KW - Process monitoring KW - Eddy current testing KW - Giant magneto resistance (GMR) KW - Additive manufacturing KW - Laser powder bed fusion PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560881 DO - https://doi.org/10.1109/JSEN.2022.3205177 VL - 22 IS - 20 SP - 19293 EP - 19300 PB - IEEE CY - New York, NY AN - OPUS4-56088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nerger, Tino A1 - Neumann, Patrick P. A1 - Weller, Michael G. T1 - A New Approach: Passive Smart Dust for Detection of Hazardous Substances N2 - Remote sensing of hazardous substances is a key task that can be achieved with the help of remotely operated platforms equipped with specific sensors. A huge variety of methods and used vehicles have been developed for different purposes in recent years. The term smart dust refers to a science fiction novel and develop shortly after into a research proposal at UC Berkley funded by DARPA. Subsequently, the topic gained attraction but was overall considered as to complex for the technologies available at that time. In the launched passive smart dust project, we shift to a simple “chemical intelligent” passive sensor particle on the ground combined a read-out active sensor attached to an Unmanned Aerial Vehicle (UAV). The reactive particle surface can be preadjusted in the lab for exact desired properties regarding certain reactions to hazardous substances. Moreover, the aimed interaction with the active sensor can be modified. Planed applications allow for different materials e.g., for short time measurement, being ecologically degradable, or weather stable for long time monitoring. T2 - 38th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Poros, Greece DA - 20.09.2022 KW - Smart Dust KW - Drone KW - Remote Detection KW - Hazardous substances PY - 2022 SP - 1 EP - 2 CY - Athens, Greece AN - OPUS4-55925 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Baloh, P. A1 - Bauer, L. A1 - Bendová, A. A1 - Čermák, P. A1 - Fellner, K. A1 - Ghanathe, M. A1 - Hernández Alvarez, O. E. A1 - Hricov, Š. A1 - Jochum, J. K. A1 - Kotvytska, L. A1 - Kumar, S. A1 - Labh, A. A1 - Machovec, P. A1 - Pauw, Brian Richard A1 - Ramszová, K. A1 - Walz, E. A1 - Wild, P. T1 - An exercise in open data: Triple axis data on Si single crystal N2 - Efforts are rising in opening up science by making data more transparent and more easily available, including the data reduction and evaluation procedures and code. A strong foundation for this is the F.A.I.R. principle, building on Findability, Accessibility, Interoperability, and Reuse of digital assets, complemented by the letter T for trustworthyness of the data. Here, we have used data, which was made available by the Institute Laue-Langevin and can be identified using a DOI, to follow the F.A.I.R.+T. principle in extracting, evaluating and publishing triple axis data, recorded at IN3. KW - Open data KW - Neutron diffraction KW - Analysis KW - Open science PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562257 DO - https://doi.org/10.48550/arXiv.2010.12086 SN - 2331-8422 SP - 1 EP - 4 PB - Cornell University CY - Ithaca, NY AN - OPUS4-56225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bernhardt, Y. A1 - Császár, L. A1 - Dengiz, N. A1 - Fuchs, M. A1 - Gaal, Mate A1 - Gautzsch, T. A1 - Gohlke, Dirk A1 - Hahn-Jose, T. A1 - Heckel, Thomas A1 - Hillger, W. A1 - Hufschläger, Daniel A1 - Ilse, D. A1 - Kiel, M. A1 - Kornely, M. A1 - Labud, P. A. A1 - Marhenke, T. A1 - Schubert, F. A1 - Sommerhuber, R. A1 - Steinhausen, R. A1 - Szewieczek, A. A1 - Wachter, L. A1 - Waschkies, T. T1 - Characterization and verification of air-coupled ultrasonic probes N2 - This guideline was drafted following and complementing the norm ISO 22232-2:2020(E) to include air-coupled ultrasonic transducers. This document specifies the characteristics of probes used for non-destructive air-coupled ultrasonic testing with center frequencies above 20 kHz, with focusing or without focusing means. KW - Air-coupled ultrasound KW - Ultrasonic testing KW - Guideline KW - Probe KW - Characterization PY - 2022 SN - 978-3-947971-26-8 VL - Guideline US 08 SP - 1 EP - 23 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin ET - Edition September 2022 AN - OPUS4-56228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Iro, M. A1 - Ingerle, D. A1 - Radtke, Martin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Kregsamer, P. A1 - Streli, C. T1 - Investigation of polycapillary half lenses for quantitative confocal micro-X-ray fluorescence analysis N2 - The use of polycapillary optics in confocal micro-X-ray fluorescence analysis (CMXRF) enables the destruction-free 3D investigation of the elemental composition of samples. The energy-dependent transmission properties, concerning intensity and spatial beam propagation of three polycapillary half lenses, which are vital for the quantitative interpretation of such CMXRF measurements, are investigated in a monochromatic confocal laboratory setup at the Atominstitut of TU Wien, and a synchrotron setup on the BAMline beamline at the BESSY II Synchrotron, Helmholtz-Zentrum-Berlin. The empirically established results, concerning the intensity of the transmitted beam, are compared with theoretical values calculated with the polycap software package and a newly presented analytical model for the transmission function. The resulting form of the newly modelled energy-dependent transmission function is shown to be in good agreement with Monte Carlo simulated results for the complete energy regime, as well as the empirically established results for the energy regime between 6 keV and 20 keV. An analysis of possible fabrication errors was conducted via pinhole scans showing only minor fabrication errors in two of the investigated polycapillary optics. The energy-dependent focal spot size of the primary polycapillary was investigated in the laboratory via the channel-wise evaluation of knife-edge scans. Experimental results are compared with data given by the manufacturer as well as geometric estimations for the minimal focal spot size. Again, the resulting measurement points show a trend in agreement with geometrically estimated results and manufacturer data. KW - BAMline KW - Synchrotron KW - Capillary KW - confocal PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562430 DO - https://doi.org/10.1107/S1600577522009699 SN - 1600-5775 VL - 29 SP - 1376 EP - 1384 PB - International Union of Crystallography CY - Chester AN - OPUS4-56243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de O. Primo, J. A1 - Horsth, D.F. A1 - de S. Correa, J. A1 - Das, A. A1 - Bittencourt, C. A1 - Umek, P. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Yusenko, Kirill A1 - Zanetta, C. A1 - Anaissi, F.J. T1 - Synthesis and Characterization of Ag/ZnO Nanoparticles for Bacteria Disinfection in Water N2 - n this study, two green synthesis routes were used for the synthesis of Ag/ZnO nanoparticles, using cassava starch as a simple and low-cost effective fuel and Aloe vera as a reducing and stabilizing agent. The Ag/ZnO nanoparticles were characterized and used for bacterial dis- infection of lake water contaminated with Escherichia coli (E. coli). Characterization indicated the formation of a face-centered cubic structure of metallic silver nanoparticles with no insertion of Ag into the ZnO hexagonal wurtzite structure. Physicochemical and bacteriological analyses described in “Standard Methods for the Examination of Water and Wastewater” were used to evaluate the efficiency of the treatment. In comparison to pure ZnO, the synthesized Ag/ZnO nanoparticles showed high efficiencies against Escherichia coli (E. coli) and general coliforms present in the lake water. These pathogens were absent after treatment using Ag/ZnO nanoparticles. The results indicate that Ag/ZnO nanoparticles synthesized via green chemistry are a promising candidate for the treatment of wastewaters contaminated by bacteria, due to their facile preparation, low-cost synthesis,and disinfection efficiency. KW - Synchrotron KW - BAMline PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-562440 DO - https://doi.org/10.3390/nano12101764 SN - 2079-4991 VL - 12 IS - 10 SP - 1 EP - 18 PB - MDPI CY - Basel AN - OPUS4-56244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Soraya T1 - Tracing toxic fumonisins - Fumonisin sensing by Aspergillus niger Fumonisin Amine Oxidase (AnFAO) and amperometric hydrogen peroxide detection N2 - Fumonisins are a class of toxic secondary metabolites produced by various Fusarium species. The two most important producers of fumonisins are F. verticillioides and F. proliferatum but also Aspergillus niger is known to produce fumonisins. Most frequently they occur on maize, but also other grains can be contaminated with this group of mycotoxins. Exposure to fumonisins by dietary intake can have serious health effects on farm animals such as equine leukoencephalomalacia and porcine pulmonary oedema and is associated with neural tube defects and esophageal cancer in humans. Thus, the European Commission sets legal limits for fumonisins in foodstuffs. The detection of fumonisins is frequently performed in laboratories by chromatographic methods, which are costly and require trained personnel. Simplifying the analysis is therefore a major goal using portable detection systems. Electrochemical enzymatic biosensors offer great promise to meet this demand. Here we report for the first time an enzymatic fumonisin sensing approach with amperometric detection. For this purpose, an Aspergillus niger fumonisin amine oxidase (AnFAO) catalyzing the oxidative deamination of fumonisins, producing hydrogen peroxide, was recombinantly produced in E. coli. For the first time, the specific enzyme activity of AnFAO was determined using a horseradish peroxidase-based fluorescence assay. It was found that the specific activity of AnFAO using 20 μM Fumonisin B1 as substrate is higher than for 20 μM Fumonisin B2 with 0.122 U mg-1 and 0.058 U mg-1, respectively. It was possible to show a dependence of enzyme activity with enzyme – and substrate-concentration. For fumonisin B1 detection, the enzyme was coupled covalently to magnetic particles and the enzymatically produced H2O2 was detected amperometrically in a flow injection system using Prussian blue carbon electrodes. The developed method allows to quantify fumonisin B1 concentrations down to 1.5 µM and demonstrates that the recombinantly produced AnFAO was able to deaminate different concentrations of fumonisin even in immobilized form. Thus, this enzyme is well suited to develop an enzyme based electrochemical biosensor for fumonisin contaminated food and feed. T2 - Posterschau Adlershofer Forschungsforum CY - Berlin, Germany DA - 11.11.2022 KW - Biosensor KW - Amperometry KW - Mycotoxins KW - Electrochemical sensor KW - Recombinant protein expression PY - 2022 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-56248 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Big to Small - Getting Smarter@BAMline N2 - In this talk an overview about artificial intelligence/machine learning applications @BAMline is given. In the first part, the use of neural networks for the quantification of XRF measurements and the decoding of coded-aperture measurements are shown. Then it is shown how Gaussian processes and Bayesian statistics can be used to achieve an optimal alignment of the set-up and in general for optimization of measurements. T2 - Forschungsseminar Institut für Optik und Atomare Physik TU Berlin CY - Berlin, Germany DA - 25.10.2022 KW - Artificial Inelligence KW - Machine Learning KW - Bayesian Statistics KW - Gaussian process KW - Neural network KW - BAMline KW - Synchrotron PY - 2022 AN - OPUS4-56249 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Döring, Sarah T1 - Cost-effective method for full-length sequencing of monoclonal antibodies N2 - With the development of hybridoma technology, monoclonal antibodies are increasingly important in therapeutic and analytical applications. For recombinant expression in mammalian cells, knowledge of the variable regions of both, heavy (VH) and light (VL) chain, is a necessary prerequisite for generating expression plasmids. Furthermore, cloning antibody sequences including constant regions CH1 to CH3 and CL reduces impact of hybridoma cell loss and associated full natural antibody sequence leakage. Here, we show a cost-effective workflow for amplification of IgG antibody variable regions in combination with advanced methods for full-length cloning of monoclonal antibodies. T2 - Adlershofer Forschungsforum CY - Berlin, Germany DA - 11.11.2022 KW - Monoclonal Antibodies KW - DNA-Sequencing KW - PCR PY - 2022 AN - OPUS4-56275 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Getting more efficient – The use of Bayesian optimization and Gaussian processes at the BAMline N2 - For more than 20 years, BAM is operating the BAMline at the synchrotron BESSY II in Berlin Adlershof. During this time, the complexity of the setup and the amount of data generated have multiplied. To increase the effectiveness and in preparation for BESSY III, algorithms from the field of machine learning are increasingly used. In this paper, several examples in the areas of beamline alignment and measurement time optimization based on Bayesian optimization (BO) with Gaussian processes (GP) are presented. BO is a method for finding the global optimum of a function using a probabilistic model represented by a GP. The advantage of this method is that it can handle high-dimensional problems, does not depend on the initial estimate, and also provides uncertainty estimates. After a short introduction to BO and GP, the first example is the automatic alignment of our double multilayer monochromator (DMM). To achieve optimal performance, up to three linear and two angular motor positions have to be optimized. To achieve this with a grid scan, at least 100^5 measurement points would be required. Assuming that all positions can be aligned independently, 100*5 points are still necessary. We show that with BO and GP less than 100 points are sufficient to achieve equal or better results. The second example is the optimization of measurement time in XRF scanning. Here we will show the advantage of the BO GP approach over point-by-point scanning. As can be seen in Fig. 1, the number of points required and thus the measurement time can be reduced by a factor of 50, while the loss in image quality is acceptable. The advantages and limitations of this approach will be discussed. T2 - European Conference on X-ray Spectrometry 2022 CY - Bruges, Belgium DA - 26.06.2022 KW - Artificial Inelligence KW - Machine Learning KW - Bayesian Statistics KW - Gaussian process KW - Neural network KW - BAMline KW - Synchrotron PY - 2022 AN - OPUS4-56251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - From Egypt to Hiddensee – Analysis of Gold with Synchrotron Radiation IV N2 - Gold is one of the seven metals already known in antiquity and was used from time immemorial as a medium of exchange and for the production of jewelry because of its luster and rarity. In addition, it is easy to work and largely resistant to chemical influences. Investigations of gold using synchrotron radiation excited X-ray fluorescence analysis are non-destructive and provide information about the chemical elements present in the sample under investigation. The investigations presented here at BAMline focus on questions such as the origin, manufacturing process, and association of gold findings. The different questions are explained by a number of examples ranging from the Viking treasure from Hiddensee to the Nebra Sky Disk and finds from Egypt. The find from Bernstorf is discussed in detail. A Bayesian treatment of the authenticity is shown. T2 - Ringvorlesung Einführung in die Archäometrie CY - Berlin, Germany DA - 04.11.2022 KW - Synchrotron KW - BAMline KW - Bayesian Statistics KW - Gold KW - Röntgenfluoreszenz PY - 2022 AN - OPUS4-56252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - News from the BAMline N2 - A presentation of recent measurements at the BAMline with focus on AI and ML applications T2 - Seminar: Strahlenphysikalische Anwendungen in Technik und Medizin CY - Vienna, Austria DA - 18.05.2022 KW - Synchrotron KW - BAMline KW - Bayesian Statistics KW - Gold KW - X-ray fluorescence PY - 2022 AN - OPUS4-56253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Getting more efficient – The use of Bayesian optimization and Gaussian processes at the BAMline N2 - For more than 20 years, BAM is operating the BAMline at the synchrotron BESSY II in Berlin Adlershof. During this time, the complexity of the setup and the amount of data generated have multiplied. To increase the effectiveness and in preparation for BESSY III, algorithms from the field of machine learning are increasingly used. After a short introduction to BO and GP, the first example is the automatic alignment of our double multilayer monochromator (DMM). The second example is the optimization of measurement time in XRF scanning. T2 - SNI2022 conference CY - Berlin, Germany DA - 05.09.2022 KW - Artificial Inelligence KW - Machine Learning KW - Bayesian Statistics KW - Gaussian process KW - X-ray fluorescence KW - BAMline PY - 2022 AN - OPUS4-56255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - Denver X-ray Conference: DXC 2021 CY - Online meeting DA - 02.08.2021 KW - Dispersive XAS KW - Mechanochemistry KW - Time resolved KW - In situ PY - 2021 AN - OPUS4-56257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray absorption spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - European Conference on X-ray Spectrometry 2022 CY - Bruges, Belgium DA - 27.06.2022 KW - XAS KW - Mechanochemictry KW - Time resolved KW - In situ PY - 2022 AN - OPUS4-56258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray absorption spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - Advances X ray Analytics Seminar at TU Berlin CY - Berlin, Germany DA - 14.06.2022 KW - XAS KW - Mechanochemistry KW - Time resolved KW - In situ PY - 2022 AN - OPUS4-56259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krankenhagen, Rainer T1 - Comment on "Sizing the depth and width of ideal delaminations using modulated photothermal radiometry" [J. Appl. Phys. 131, 085106 (2022)] N2 - Comment on the article "Sizing the depth and width of ideal delaminations using modulated photothermal radiometry" by Agustín Salazar and Arantza Mendioroz, Journal of Applied Physics 131, 085106 (2022, https://doi.org/10.1063/5.0085178). KW - Ideal delamination KW - Modulated photothermal radiometry KW - Delamination depth KW - Delamination width PY - 2022 DO - https://doi.org/10.1063/5.0107603 VL - 132 SP - 1 PB - AIP CY - Melville, NY AN - OPUS4-56261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan T1 - High Speed for High Entropy Materials N2 - Time is the most valuable parameter in synchrotron experiments. This is costly and some of the experiments suffer from low efficiency due to low counting statistics. With today's high processing power long experiments are run in a shorter time and increase efficiency. With optimization algorithms time in "counting-hungry" experiments reduced by factor of 10. Our project is to develop a new method to analyze the chemical properties of complex materials non-destructively and efficiently, such as high entropy materials subjected to corrosion processes. A better understanding of the corrosion process will help to develop corrosion-resistant materials and reduce the cost of corrosion damage, which averages around 2.5 trillion USD annually. T2 - Berlin Science Week CY - Berlin, Germany DA - 01.11.2022 KW - GEXRF KW - High entropy alloys KW - XANES KW - High entropy materials KW - Grazing exit KW - XAS KW - Optimization PY - 2022 AN - OPUS4-56269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan T1 - Optimization of Depth Resolved X-Ray Absorption Spectroscopy in Grazing Emission Mode for Characterizing Compositionally Complex Alloys N2 - The components that are used in structural and in high temperature applications generally face significant challenges with respect to oxidation behaviours and metalworking processes. In most of the cases, harsh environmental conditions lead materials to degrade due to corrosion. To thoroughly investigate the corrosion processes and to determine oxidation states of metal components within the reaction products, we need special analytical tools. Grazing exit X-ray fluorescence (GEXRF) offers a non-destructive way to collect this information in sub-micrometre depth range. In order to obtain structural information, such as regarding oxidation states or atomic/molecular geometric arrangement, the GEXRF approach can also be combined with the X-ray absorption spectroscopy (XAS) method. The position and energy sensitive detector, with 264x264 pixel detector area, provides information regarding the signal emitted from the sample as a function of the emission angle and thus allows depth-sensitive analysis. Furthermore, the data collected from samples of an incidence energy which can be controlled with a resolution of 0.5 eV provides XANES data to determine oxidation states. We address the feasibility of our setup and provide a new optimization procedure (Bayesian Optimization and Gaussian Regression) to decrease measuring time. The results settle on a conceptual study on a reference sample (Cr-Oxide layer (300nm) on Cr layer (500nm) on Si wafer). T2 - XAFS 2022, The 19th International XAFS Conference CY - Sydney, Australia DA - 10.07.2022 KW - GEXRF KW - High entropy alloys KW - XANES KW - Grazing exit KW - High entropy materials KW - Optimization KW - XAS PY - 2022 AN - OPUS4-56270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan T1 - Scanning-Free Grazing Exit XANES Analysis of Stratified Samples and the Optimization of the Data Collection Process N2 - The components that are used in structural and in high temperature applications generally face significant challenges with respect to oxidation behaviours and metalworking processes. In most of the cases, harsh environmental conditions lead materials to degrade due to corrosion. To thoroughly investigate the corrosion processes and to determine oxidation states of metal components within the reaction products, we need special analytical tools. Grazing exit X-ray fluorescence (GEXRF) offers a non-destructive way to collect this information in sub-micrometre depth range. In order to obtain structural information, such as regarding oxidation states or atomic/molecular geometric arrangement, the GEXRF approach can also be combined with the X-ray absorption spectroscopy (XAS) method. The position and energy sensitive detector, with 264x264 pixel detector area, provides information regarding the signal emitted from the sample as a function of the emission angle and thus allows depth-sensitive analysis. Furthermore, the data collected from samples of an incidence energy which can be controlled with a resolution of 0.5 eV provides XANES data to determine oxidation states. We address the feasibility of our setup and provide a new optimization procedure (Bayesian Optimization and Gaussian Regression) to decrease measuring time. The results settle on a conceptual study on a reference sample (Cr-Oxide layer (300nm) on Cr layer (500nm) on Si wafer). T2 - Denver X-Ray Conference DXC 2022 CY - Washington D.C., USA DA - 07.08.2022 KW - GEXRF KW - High entropy alloys KW - High entropy materials KW - Optimization KW - XANES KW - Grazing exit KW - XAS PY - 2022 AN - OPUS4-56271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan T1 - Bayesian optimization for depth resolved analysis of complex alloys with grazing exit XANES N2 - Compositionally complex alloys (CCAs) are a new class of alloys containing at least 5 elements with concentrations between 5 and 35 atomic percent. Due to their adjustable composition, which enables modifications of mechanical properties (such as hardness, strength and ductility etc) and their stability at high temperatures, CCAs have been the focus of various studies [1,2]. Especially the corrosion behavior of CCAs has been a wide research interest. However, there are only few studies that deals with the degradation process on such materials, which is highly relevant for the safety aspect for future component design. To thoroughly investigate the corrosion processes and to determine oxidation states of metal components within the reaction products, we need special analytical tools. Since the grazing exit X-ray fluorescence (GEXRF) offers a non-destructive way to collect notable information regarding the high temperature oxidation, we consider it as a useful method to investigate how CCAs behave in corrosive environments. The main idea of grazing geometry is to enhance the fluorescence signal of the surface. This enables highly sensitive surface analyses of thin protective film on surface in sub-micrometer scale [3]. When compared to a conventional CCD-based camera, the advantage and most important feature of the detector system (Color X-Ray Camera (CXC)) is that each pixel is an energy sensitive detector. The position and area sensitive detector, with 264x264 pixel detector area, provides information regarding the signal emitted from the sample as a function of the emission angle and thus allows depth-sensitive analysis. Furthermore, the data collected from samples of an incidence energy which can be controlled with a resolution of 0.5 eV provides XANES data to determine oxidation states. In this contribution, we address the feasibility of our setup and new optimization procedure (Bayesian Optimization and Gaussian Regression). The results of a conceptual study regarding layer properties of the reference sample (Cr-Oxide layer (300nm) on Cr layer (500nm) on Si wafer) and CrCoNi (Cr-Oxide (>1µm) layer on CrCoNi substrate) medium entropy alloy. T2 - European Conference on X-ray Spectrometry. EXRS 2022 CY - Bruges, Belgium DA - 26.06.2022 KW - GEXRF KW - High entropy alloys KW - XANES KW - Grazing exit KW - High entropy materials KW - XAS KW - Optimization PY - 2022 AN - OPUS4-56272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis A1 - Jurgelucks, B. A1 - Prager, Jens A1 - Walther, A. T1 - Schadensrekonstruktion mittels geführter Wellen in Stahlplatten N2 - Ein Hauptziel der zerstörungsfreien Prüfung und der Strukturüberwachung (engl. Structural Health Monitoring - SHM) mit Ultraschallwellen ist die Charakterisierung von Schäden in Bauteilen. In vielen schalenförmigen Bauteilen, wie zum Beispiel Rohrleitungen, Laminaten und Platten, breitet sich der Ultraschall in Form geführter Wellen aus. Zwar erlauben geführte Wellen eine großflächige Prüfung durch das langsame Abklingen der Wellen. Jedoch breiten sich die Wellen in verschiedenen dispersiven Moden aus, was die Analyse der vom Schaden erzeugten Reflexionen erschwert. Eine Möglichkeit, die Messsignale zu interpretieren, um Schäden zu charakterisieren, ist der direkte Vergleich mit einem Simulationsmodell. Die Rekonstruktion des Schadens stellt ein inverses Problem dar. Das inverse Problem kann als Optimierungsproblem formuliert werden. Für die Optimierung werden mehrere Vorwärtsrechnungen gebraucht, um das Schadensmodell an die Messdaten anzupassen. Aufgrund der kurzen Wellenlängen von Ultraschallwellen sind klassische Methoden für die Vorwärtsrechnung, wie z.B. die Finite Elemente Methode (FEM), rechenintensiv. Eine Möglichkeit den Rechenaufwand zu reduzieren, bietet die Approximation der Wellenausbreitung mittels der semi-analytischen Scaled Boundary Finite Element Method (SBFEM). Frühere Untersuchungen haben gezeigt, dass die benötigten Freiheitsgrade im Vergleich zur FEM wesentlich geringer sind [1]. Im Beitrag wird eine Optimierung basierend auf einem Gradientenverfahren in Kombination mit der SBFEM vorgestellt und an verschiedenen Schadenstypen in 2D-Querschnittsmodellen von Stahlplatten getestet. Der Gradient des Vorwärtsmodells wird durch Algorithmisches Differenzieren berechnet, wodurch eine genaue und schnelle Optimierung ermöglicht wird. Es werden Untersuchungen zum inversen Problem und das Finden einer geeigneten Zielfunktion präsentiert. Es wird verdeutlicht, dass der entwickelte Algorithmus robust gegenüber von Rauscheinflüssen ist. In diesen Untersuchungen werden zunächst „Messdaten“ aus unabhängigen Simulationen verwendet [2]. Erste Schritte für die experimentelle Validierung und Erweiterung auf 3D Modelle werden anschließend vorgestellt. T2 - Doktorandenworkshop in Kloster Lehnin CY - Kloster Lehnin, Germany DA - 19.10.22 KW - SBFEM KW - Zerstörungsfreie Prüfung KW - Structural Health Monitoring KW - Ultraschallwellen PY - 2022 AN - OPUS4-56551 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von der Au, Marcus A1 - Meermann, Björn T1 - MDG-ICP-MS - A Versatile Tool for Quantification in the field of Single Particle ICP-MS Using Isotopic Dilution N2 - In the interest of exploring their potential in the field of single particle analysis, a Microdroplet Generator (MDG) was coupled to an ICP-ToF-MS. Isotopic Dilution Analysis was also incorporated for the size determination of three different Platinum Nanoparticles samples (50, 63 and 70 nm). The performance of the technique was validated by comparison to traditional size characterization techniques (sp-ICP-ToF-MS, TEM), while the robustness of the technique was proven by incorporating NaCl in the samples’ matrix, up to 100 mg/L. T2 - SciX 2022 CY - Cincinnati, OH, USA DA - 02.10.2022 KW - MDG KW - ICP-TOF-MS KW - Nanoparticle PY - 2022 AN - OPUS4-56554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bawadkji, O. A1 - Cherri, M. A1 - Schäfer, A. A1 - Herziger, S. A1 - Nickl, Philip A1 - Achazi, K. A1 - Donskyi, Ievgen A1 - Adeli, M. A1 - Haag, R. T1 - One-pot covalent functionalization of 2D black phosphorus by anionic ring opening polymerization N2 - In this work, a one-pot approach for the covalent functionalization of few-layer black phosphorus (BP) by anionic ring opening polymerization of glycidol to obtain multifunctional BP-polyglycerol (BP-PG) with high amphiphilicity for near-infrared-responsive drug delivery and biocompatibility is reported. Straightforward synthesis in combination with exceptional biological and physicochemical properties designates functionalized BP-PG as a promising candidate for a broad range of biomedical applications. KW - 2D nanomaterial KW - Amphiphilicity KW - Black phosphorus KW - Hyperbranched KW - Polyglycerol KW - Water dispersibility PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568833 DO - https://doi.org/10.1002/admi.202201245 SN - 2196-7350 VL - 9 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hong, H. A1 - Part, Florian A1 - Nowack, B. T1 - Prospective dynamic and probabilistic material flow analysis of graphene-based materials in Europe from 2004 to 2030 N2 - As industrial demand for graphene-based materials (GBMs) grows, more attention falls on potential environmental risks. The present article describes a first assessment of the environmental releases of GBMs using dynamic probabilistic material flow analysis. The model considered all current or expected uses of GBMs from 2004 to 2030, during which time there have already been significant changes in how the graphene mass produced is distributed to different product categories. Although the volume of GBM production is expected to grow exponentially in the coming years, outflow from the consumption of products containing GBMs shows only a slightly positive trend due to their long lifetimes and the large in-use stock of some applications (e.g., GBM composites used in wind turbine blades). From consumption and end-of-life phase GBM mass flows in 2030, estimates suggest that more than 50% will be incinerated and oxidized in waste plants, 16% will be landfilled, 12% will be exported out of Europe, and 1.4% of the annual production will flow to the environment. Predicted release concentrations for 2030 are 1.4 ng/L in surface water and 20 μg/kg in sludge-treated soil. This study’s results could be used for prospective environmental risk assessments and as input for environmental fate models. KW - Graphene KW - Graphene-based material (GBM) KW - Material flow analysis KW - Exposure modeling PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568843 DO - https://doi.org/10.1021/acs.est.2c04002 SN - 0013-936X SN - 1520-5851 VL - 56 SP - 13798 EP - 13809 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-56884 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zinke, R. A1 - Wothe, K. A1 - Dugarev, D. A1 - Götze, O. A1 - Köhler, F. A1 - Schalau, Sebastian A1 - Krause, U. T1 - Uncertainty consideration in CFD-models via response surface modeling: Application on realistic dense and light gas dispersion simulations N2 - Major accidents in the process industry often lead to the release of light or dense gases, which can mean a thread to employees, local residents or to the environment. Possible scenarios are therefore analyzed and evaluated in advance for approval issues. There is a trend, where simple empirical models are being replaced with more complex numerical models. Gaussian dispersion models or models based on dimensional analysis approaches are for example, increasingly replaced by CFD simulations. The main reason for this is the potentially higher accuracy. However, usually scenarios using sharp parameter values are calculated, since comprehensive consideration of parameter distributions via Monte Carlo or Latin Hypercube Sampling fails due to the numerical effort. This includes the risk that the influence of uncertainties on the simulation results is not taken into account. Response surface methods offer an alternative, with which the CFD problem can be mapped onto an algebraic surrogate model. If this is sufficiently precise, parameter sampling can also be carried out with the surrogate as well, as shown in some publications. Previous investigations only demonstrated the basic principle using trivial dispersion models. In this paper two realistic CFD simulations from the plant safety area are considered: VOC emissions from a storage tank and near-ground dense gas emissions. The entire procedure of response surface determination and parameter studies was automated and parallelized for high-performance-computing, and is carried out on the underlying CFD grids. For the CFD simulations as well as for all visualizations, the commercial software ANSYS CFX and the open source software OpenFOAM were used. The aim of this paper is to demonstrate the method using industry-relevant applications as well as to show how this can be used in practical engineering applications. The quality of surrogate modeling, the numerical effort and advantages that can result from the procedure are discussed as well as advantages which may result from taking parameter uncertainties into account in safety studies. KW - CFD KW - Accidental release KW - Response surface methods KW - Air dispersion modeling PY - 2022 DO - https://doi.org/10.1016/j.jlp.2021.104710 SN - 0950-4230 VL - 75 SP - 1 EP - 10 PB - Elsevier CY - Amsterdam AN - OPUS4-56887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Mobile Applications with Drones/Robots - Aerial- and Ground-based Gas Tomography N2 - Remote gas sensors mounted on mobile robots enable the mapping of gas distributions in large or poorly accessible areas. A challenging task however, is the generation of three-dimensional distribution maps from these spatially sparse gas measurements. To obtain high-quality reconstructions, the choice of optimal measuring poses is of great importance. Remote gas sensors, that are commonly used in Robot Assisted Gas Tomography (RAGT), require reflecting surfaces within the sensor’s range, limiting the possible sensing geometries, regardless of whether the robots are ground-based or airborne. By combining ground and aerial robots into a heterogeneous swarm whose agents are equipped with reflectors and remote gas sensors, remote inter-robot gas measurements become available, taking RAGT to the next dimension – releasing those constraints. In this paper, we demonstrate the feasibility of drone-to-drone measurements under realistic conditions and highlight the resulting opportunities. T2 - ISOCS Short Course Winter 2023 CY - Bormio, Italy DA - 16.01.2023 KW - Aerial robot KW - Ground robot KW - Gas tomography KW - Inter-robot measurements KW - Plume KW - TDLAS PY - 2023 AN - OPUS4-56872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tatzel, M. A1 - Frings, P. J. A1 - Oelze, Marcus A1 - Herwartz, D. A1 - Lünsdorf, K. A1 - Wiedenbeck, M. T1 - Chert oxygen isotope ratios are driven by Earth's thermal evolution N2 - The 18O/16O ratio of cherts (δ18Ochert) increases nearly monotonically by ~15‰ from the Archean to present. Two end-member explanations have emerged: cooling seawater temperature (TSW) and increasing seawater δ18O (δ18Osw). Yet despite decades of work, there is no consensus, leading some to view the δ18Ochert record as pervasively altered. Here, we demonstrate that cherts are a robust archive of diagenetic temperatures, despite metamorphism and exposure to meteoric fluids, and show that the timing and temperature of quartz precipitation and thus δ18Ochert are determined by the kinetics of silica diagenesis. A diagenetic model shows that δ18Ochert is influenced by heat flow through the sediment column. Heat flow has decreased over time as planetary heat is dissipated, and reasonable Archean-modern heat flow changes account for ~5‰ of the increase in δ18Ochert, obviating the need for extreme TSW or δ18Osw reconstructions. The seawater oxygen isotope budget is also influenced by solid Earth cooling, with a recent reconstruction placing Archean δ18OSW 5 to 10‰ lower than today. Together, this provides an internally consistent view of the δ18Ochert record as driven by solid Earth cooling over billion-year timescales that is compatible with Precambrian glaciations and biological. KW - Climate KW - Oxygen isotope ratios KW - Silica diagenesis KW - Early Earth KW - Heat flow PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569359 DO - https://doi.org/10.1073/pnas.2213076119 SN - 0027-8424 VL - 119 IS - 51 SP - 1 EP - 7 PB - National Academy of Sciences CY - Washington, DC AN - OPUS4-56935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Breuninger, Esther S. A1 - Tolu, Julie A1 - Aemisegger, Franziska A1 - Thurnherr, Iris A1 - Bouchet, Sylvain A1 - Mestrot, Adrien A1 - Ossola, Rachele A1 - McNeill, Kristopher A1 - Tukhmetova, Dariya A1 - Vogl, Jochen A1 - Meermann, Björn A1 - Sonke, Jeroen E. A1 - Winkel, Lenny H. E. T1 - Marine and terrestrial contributions to atmospheric deposition fluxes of methylated arsenic species N2 - Arsenic, a toxic element from both anthropogenic and natural sources, reaches surface environments through atmospheric cycling and dry and wet deposition. Biomethylation volatilizes arsenic into the atmosphere and deposition cycles it back to the surface, affecting soil-plant systems. Chemical speciation of deposited arsenic is important for understanding further processing in soils and bioavailability. However, the range of atmospheric transport and source signature of arsenic species remain understudied. Here we report significant levels ofmethylated arsenic in precipitation, cloudwater and aerosols collected under free tropospheric conditions at Pic du Midi Observatory (France) indicating long-range transport, which is crucial for atmospheric budgets. Through chemical analyses andmoisture source diagnostics, we identify terrestrial and marine sources for distinct arsenic species. Estimated atmospheric deposition fluxes of methylated arsenic are similar to reported methylation rates in soils, highlighting atmospheric deposition as a significant, overlooked source of potentially bioavailable methylated arsenic species impacting plant uptake in soils. KW - Arsenic KW - Speciation KW - Fluxes KW - Marine KW - Terrestrial KW - Sulfur isotopes PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615551 DO - https://doi.org/10.1038/s41467-024-53974-z SN - 2041-1723 VL - 15 IS - 1 SP - 1 EP - 13 PB - Springer Science and Business Media LLC AN - OPUS4-61555 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chan, George C.-Y. A1 - Engelhard, Carsten A1 - Wiley, Joshua S. A1 - Shoulds, Ayanna U. A1 - Cooks, R. Graham A1 - Hieftje, Gary M. A1 - Shelley, Jacob T. T1 - Characterization of a Low-Temperature Plasma (LTP) Ambient Ionization Source Using Temporally Resolved Monochromatic Imaging Spectrometry N2 - The low-temperature plasma (LTP) probe is a common plasma-based source used for ambient desorption–ionization mass spectrometry (MS). While the LTP probe has been characterized in detail with MS, relatively few studies have used optical spectroscopy. In this paper, two-dimensional (2D) imaging at selected wavelengths is used to visualize important species in the LTP plasma jet. First, 2D steady-state images of the LTP plume for N2+ (391.2 nm), He I (706.5 nm), and N2 (337.1 nm) emissions were recorded under selected plasma conditions. Second, time-resolved 2D emission maps of radiative species in the LTP plasma jet were recorded through the use of a 200 ns detection gate and varying gate delays with respect to the LTP trigger pulse. Emission from He I, N2+, and N2 in the plasma jet region was found to show a transient behavior (often referred to as plasma bullets) lasting only a few microseconds. The N2+ and He I maps were highly correlated in spatial and temporal structure. Further, emission from N2 showed two maxima in time, one before and one after the maximum emission for N2+ and He I, due to an initial electronic excitation wave and ion–electron recombination, respectively. Third, the interaction of the LTP probe with a sample substrate and an electrically grounded metallic needle was studied. Emission from a fluorophore on the sample substrate showed an initial photon-induced excitation from plasma-generated photons followed by electronic excitation by other plasma species. The presence of a grounded needle near the plasma jet significantly extended the plasma jet lifetime and also generated a long-lived corona discharge on the needle. The effect of LTP operating parameters on emission spectra was correlated with mass-spectral results including reagent-ion signals. Lastly, five movies provide a side-by-side comparison of the temporal behavior of emitting species and insights into the interactions of the emission clouds with a sample surface as well as an external needle. Temporally and spatially resolved imaging provided insights into important processes in the LTP plasma jet, which will help improve analyte ion sampling in LTP–MS. KW - Optical spectroscopy KW - Low-temperature plasma KW - Ambient ionization KW - Instrumentation PY - 2023 DO - https://doi.org/10.1177/00037028231184501 VL - 77 IS - 8 SP - 940 EP - 956 PB - SAGE Publications AN - OPUS4-61269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Sauer, Andreas T1 - Report on the interlaboratory validation trial of DIN 38407-53 N2 - DIN 38407-53 "German standard methods for the examination of water, waste water and sludge — Jointly determinable substances (group F) — Part 53: Determination of TFA in water — Method using liquid chromatography and mass spectrometric detection (LC-MS/MS) after direct injection (F 53)" was prepared by working group NA 119 01 03 02 16 AK "LC-MS/MS-Verfahren" of the Technical Committee NA 119 01 03 AA "Wasseruntersuchung" in the DIN-Normenausschuss Wasserwesen (NAW). The DIN 38407-53 was technically finalized as Draft on 2024-02, further versions have been editorially revised only. The interlaboratory validation trial was carried out according to the rules set by ISO 7013. They allowed adopting validation data from a working group internal ring test if they are scientifically accepted and fulfil the requirements of ISO 7013. Twelve German and Swiss participants declared to have strictly followed the instructions given in draft DIN 38407-53. The intercomparison was organised and operated by the Federal Institute for Materials Research and Testing BAM in 2024. The performance characteristics for the quantification of TFA were evaluated in different water types and evaluated according to ISO 5725-2. KW - TFA Trifluoroacetic acid KW - Water analysis KW - LC MSMS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615066 DO - https://doi.org/10.26272/opus4-61506 SP - 1 EP - 18 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-61506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xue, Boyang A1 - Wang, Zhangjun A1 - Zhu, Tao A1 - Gu, Yezhen A1 - Sun, Weihong A1 - Chen, Chao A1 - Li, Zhigang A1 - Riedel, Jens A1 - You, Yi T1 - High repetition-rate laser-induced breakdown spectroscopy combined with two-dimensional correlation method for analysis of sea-salt aerosols N2 - Laser-induced breakdown spectroscopy (LIBS) offers a tantalizing glimpse into real-time, on-the-spot aerosol analysis. Yet, the reliance on traditional lasers, with their limitations in energy and frequency, hampers optimal sample handling, dissociation, and excitation. To address those challenges, we propose a novel tactic: utilize a high repetition-rate (rep.-rate) laser with low pulse energy in combination with the two-dimensional correlation (2D-corr.) technique for sea-salt aerosols analyses. By examining the emission patterns from both the laser pulse train and individual pulses, we recognize distinctive analyte-specific rep.-rate responses, which allowed spectral reconstruction of analytes, avoiding background interferences. This discovery enabled the rep.-rate modulation for a 2D-corr. spectroscopy workflow. Consequently, we successfully differentiated between particle-related and air-species-related spectral components, obviating expensive spectrometers or intensified image detectors. For instance, the Na I at 589 nm stemming from aerosols exhibited an entirely different correlation contribution compared to O I at 777 nm, resulting in reconstructed clean aerosol-spectra without spectral peaks originated from air species. This 2D-corr. aerosol LIBS approach shows promising analytical potential streamlining aerosol particle analysis. KW - LIBS KW - Aerosol PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613392 DO - https://doi.org/10.1016/j.sab.2024.107048 SN - 0584-8547 VL - 221 SP - 1 EP - 8 PB - Elsevier AN - OPUS4-61339 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Xunyu A1 - Riedel, Jens A1 - You, Yi T1 - Practical high-resolution spectroscopy with a spatial heterodyne spectrometer: Determination of instrumental function for lineshape recovery N2 - The spatial heterodyne spectrometer (SHS) is a well-recognized platform for its high resolving power in various use cases of spectroscopy. Same as other spectrometer topologies, the SHS, unfortunately, also suffers from classical challenges such as distorted lineshape due to the instrumental function. The goal of this work is to tackle this persisting issue through a simple numerical approach. With the inherent characteristics of an SHS interferogram, we report the direct extraction and determination of the instrumental function in its numerical representation from an SHS interferogram; this instrumental function was further used for spectral data processing that enables significant improvements in spectral resolution through deconvolution algorithms.Here, we systematically discuss the recognition of the embedded instrumental function among various ingredients within an interferogram. To verify the numerical approach, lithium was chosen as the model sample, resembling the use of SHS in an isotopic analysis application. Specifically, the resonance transition of lithium D-lines (2P1/2,3/2 ← 2S1/2) was selected to assess the performance of the spectral processing. With the spectral deconvolution, the spectral features that represent the 6Li and 7Li were nearly baseline-separated, allowing for the accurate measure of the isotopic abundance without external references or algorithm adjustments (e.g., curve fitting). KW - SHS KW - Isotopic analysis KW - High Resolution PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613401 DO - https://doi.org/10.1016/j.sab.2024.107053 SN - 0584-8547 VL - 221 SP - 1 EP - 5 PB - Elsevier AN - OPUS4-61340 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Scheliga, Felix A1 - Kricheldorf, Hans R. T1 - Polycondensation, Cyclization and Disproportionation of Solid Poly(L-lactide) Trifluoroethyl Esters and the Simultaneous Formation of Extended Chain Crystals and Extended Ring Crystals N2 - Two poly(L-lactide)s (PLAs) with a degree of polymerization (DP) of 20 or 100 were prepared by trifluoroethanol-initiated ring-opening polymerization (ROP) catalyzed by tin(II) 2-ethyl hexanoate (SnOct2). These PLAs were annealed at 140 ◦C or at 160 ◦C in the presence of SnOct2, and the changes in topology and molecular weight distribution (MWD) were monitored by matrix-assisted laser desorption/ionization time-of flight (MALDI TOF) mass spectrometry and gel permeation chromatography (GPC). For the PLA with a DP 20, the main reaction was polycondensation combined with higher dispersities. In the case of the DP 100, PLA polycondensation was combined with disproportionation and the formation of a new MWD maximum around m/z 3500. In addition, extensive cyclization occurred, and the resulting cyclic PLAs crystallized separately from the linear chains in the form of extended ring crystals. These results also suggest that both extended chain and extended ring crystals posses the same crystal thickness as a result of thermodynamically controlled transesterification in the solid state. KW - Polycondensation KW - MALDI KW - Polylactide KW - Cyclization PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616441 DO - https://doi.org/10.1016/j.polymer.2024.127800 VL - 315 SP - 1 EP - 9 PB - Elsevier Ltd. AN - OPUS4-61644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Multigassensoren - Standardisierte Prüfanweisung und Prüfgase für VOC-Detektoren zur Innenraumluftgütemessung N2 - Flüchtige organische Verbindungen (VOC, "Volatile Organic Compounds") sind ein wichtiger Parameter zur Bewertung der Luftqualität speziell in Innenräumen. Deren Bestimmung ist vergleichsweise komplex, da VOC ein Oberbegriff für viele verschiedene Verbindungen ist. Die Richtlinie VDI/VDE 3518 Blatt 4[1] (Entwurf) beschreibt eine vom Messprinzip unabhängige Prüfung sowie sinnvolle Prüfgasmischungen für VOC-Detektoren. Die Richtlinie schafft die Basis für vergleichbare Messungen mit Sensoren und Messsystemen für die Bestimmung von VOC Konzentrationen in Innenräumen. T2 - 22. GMA/ITG- Fachtagung Sensoren und Messsysteme 2024 CY - Nuremberg, Germany DA - 11.06.2024 KW - Richtlinie KW - VOC KW - VOC-Detektion KW - Innenraumluftgüte PY - 2024 AN - OPUS4-61675 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vo, P. H.N. A1 - Vogel, Christian A1 - Nguyen, H. T.M. A1 - Hamilton, B. R. A1 - Thai, P. K. A1 - Roesch, Philipp A1 - Simon, Franz-Georg A1 - Mueller, J. F. T1 - µ-X-ray fluorescence (XRF) and fluorine K-edge µ-X-ray absorption near-edge structure (XANES) spectroscopy for detection of PFAS distribution in the impacted concrete N2 - An improved understanding of the distribution of per- and polyfluoroalkyl substances (PFAS) in PFAS-impacted concrete is important for risk management and decontamination of PFAS. This study incorporates µ-X-ray fluorescence (µ-XRF) and fluorine K-edge µ-X-ray absorption near-edge structure (µ-XANES) spectroscopy to gain non-destructive insights into PFAS distribution in the impacted concrete. The μ-XRF and μ-XANES spectroscopy provided additional details on the detection of PFAS, which were not detected by the desorption electrospray ionization (DESI) imaging method conducted previously. The shorter chain PFAS were found on the top part of the concrete core (0.5 cm), and longer chain PFAS were mostly at the bottom part of the concrete core (5 cm). The inorganic fluorine fraction was also detected, and it likely hampered the detection of organic fluorine such as PFAS in the concrete. Thus, this non-destructive technique is an complementary approach to detect PFAS in contaminated concrete. KW - Beton KW - Per- and Polyfluoroalkyl substances (PFAS) KW - XANES spectroscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-616711 DO - https://doi.org/10.1016/j.hazl.2024.100134 SN - 2666-9110 VL - 5 SP - 1 EP - 5 PB - Elsevier B.V. AN - OPUS4-61671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zuliani, T. T1 - Advancing Stable and Long-lived Radiogenic Isotope Ratio Measurements of Environmental Pollutants N2 - The isotopic compositions of elements vary in the environment due to processes such as radioactive decay, cosmic ray spallation, mass-dependent and mass-independent fractionation, and different anthropogenic sources such as industrial activities, nuclear weapon testing, nuclear accidents, as well as natural phenomena long-range atmospheric and water transport, climate change, etc. Isotope ratio data obtained by mass spectrometry now plays an important role as tracers of a multitude of processes in Earth and environmental sciences. Inductively coupled plasma mass spectrometry (ICP-MS) is a widely used technique for detecting variations in isotopic abundances in e.g., environmental samples. Recent advancements in mass spectrometric instrumentation have significantly enhanced sensitivity and precision, enabling the reliable detection of even minute variations in the isotopic composition of most elements with more than one natural isotope. However, to fully realize these new capabilities, a significant analytical challenge remains due to a vast number of analyte/matrix combinations, concomitant matrix effects, spectral interferences, and instrumental isotopic fractionation that must be characterized before and during the measurements. Success in developing new and improved methods for stable and long-lived radiogenic isotope ratio measurements by mass spectrometric methods depends on improvements in the reduction and quantification of uncertainties associated with sample preparation, instrumentation, and external calibration. The goal of this presentation is to show the key findings of the European Partnership on Metrology project “Metrology for the harmonisation of measurements of environmental pollutants in Europe” - MetroPOEM (https://www.npl.co.uk/euramet/metropoem), with a focus on the ICP-MS techniques used for isotope ratio measurements. Several elements were used as model systems for the development and optimisation of sample preparation and measurement procedures, including Li, B, Cr, Cd, Ni, Sb, Pb, and U. Isotope ratios of these elements determined by multi-collector ICP-MS, sector field ICPMS, quadrupole ICP-MS, and ICP-MS/MS will be assessed and compared. Data on their performance will be presented and assessed in terms of accuracy and precision. Comprehensive uncertainty budgets for the determination of the isotope ratios of the selected elements by different calibration approaches will be presented. The presented results will highlight the potential of recent advances in ICP-MS technology. T2 - 11th Nordic Conference on Plasma Spectrochemistry CY - Loen, Norway DA - 09.06.2024 KW - Isotope analysis KW - ICP-MS KW - Measurement uncertainty PY - 2024 AN - OPUS4-61599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trimpin, Sarah A1 - Yenchick, Frank S. A1 - Lee, Chuping A1 - Hoang, Khoa A1 - Pophristic, Milan A1 - Karki, Santosh A1 - Marshall, Darrell D. A1 - Lu, I-Chung A1 - Lutomski, Corinne A. A1 - El-Baba, Tarick J. A1 - Wang, Beixi A1 - Pagnotti, Vincent S. A1 - Meher, Anil K. A1 - Chakrabarty, Shubhashis A1 - Imperial, Lorelei F. A1 - Madarshahian, Sara A1 - Richards, Alicia L. A1 - Lietz, Christopher B. A1 - Moreno-Pedraza, Abigail A1 - Leach, Samantha M. A1 - Gibson, Stephen C. A1 - Elia, Efstathios A. A1 - Thawoos, Shameemah M. A1 - Woodall, Daniel W. A1 - Jarois, Dean R. A1 - Davis, Eric T.J. A1 - Liao, Guochao A1 - Muthunayake, Nisansala S. A1 - Redding, McKenna J. A1 - Reynolds, Christian A. A1 - Anthony, Thilani M. A1 - Vithanarachchi, Sashiprabha M. A1 - DeMent, Paul A1 - Adewale, Adeleye O. A1 - Yan, Lu A1 - Wager-Miller, James A1 - Ahn, Young-Hoon A1 - Sanderson, Thomas H. A1 - Przyklenk, Karin A1 - Greenberg, Miriam L. A1 - Suits, Arthur G. A1 - Allen, Matthew J. A1 - Narayan, Srinivas B. A1 - Caruso, Joseph A. A1 - Stemmer, Paul M. A1 - Nguyen, Hien M. A1 - Weidner, Steffen A1 - Rackers, Kevin J. A1 - Djuric, Ana A1 - Shulaev, Vladimir A1 - Hendrickson, Tamara L. A1 - Chow, Christine S. A1 - Pflum, Mary Kay H. A1 - Grayson, Scott M. A1 - Lobodin, Vladislav V. A1 - Guo, Zhongwu A1 - Ni, Chi-Kung A1 - Walker, J. Michael A1 - Mackie, Ken A1 - Inutan, Ellen D. A1 - McEwen, Charles N. T1 - New Processes for Ionizing Nonvolatile Compounds in Mass Spectrometry: The Road of Discovery to Current State-of-the-Art N2 - This Perspective covers discovery and mechanistic aspects aswell as initial applications of novel ionization processes for use in massspectrometry that guided us in a series of subsequent discoveries, instrumentdevelopments, and commercialization. Vacuum matrix-assisted ionization onan intermediate pressure matrix-assisted laser desorption/ionization sourcewithout the use of a laser, high voltages, or any other added energy wassimply unbelievable, at first. Individually and as a whole, the variousdiscoveries and inventions started to paint, inter alia, an exciting new pictureand outlook in mass spectrometry from which key developments grew thatwere at the time unimaginable, and continue to surprise us in its simplisticpreeminence. We, and others, have demonstrated exceptional analyticalutility. Our current research is focused on how best to understand, improve, and use these novel ionization processes throughdedicated platforms and source developments. These ionization processes convert volatile and nonvolatile compounds from solid orliquid matrixes into gas-phase ions for analysis by mass spectrometry using, e.g., mass-selected fragmentation and ion mobilityspectrometry to provide accurate, and sometimes improved, mass and drift time resolution. The combination of research anddiscoveries demonstrated multiple advantages of the new ionization processes and established the basis of the successes that lead tothe Biemann Medal and this Perspective. How the new ionization processes relate to traditional ionization is also presented, as wellas how these technologies can be utilized in tandem through instrument modification and implementation to increase coverage ofcomplex materials through complementary strengths. KW - Mass spectrometry PY - 2024 DO - https://doi.org/10.1021/jasms.3c00122 SN - 1879-1123 VL - 35 IS - 12 SP - 2753 EP - 2784 PB - American Chemical Society (ACS) AN - OPUS4-61417 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zweigle, J. A1 - Schmidt, A. A1 - Bugsel, B. A1 - Vogel, Christian A1 - Simon, Fabian A1 - Zwiener, C. T1 - Perfluoroalkyl acid precursor or weakly fluorinated organic compound? A proof of concept for oxidative fractionation of PFAS and organofluorines N2 - Organofluorine mass balance approaches are increasingly applied to investigate the occurrence of per- and polyfluoroalkyl substances (PFAS) and other organofluorines in environmental samples more comprehensively. Usually, complex samples prevent the identification and quantification of every fluorine-containing molecule. Consequently, large unidentified fractions between fluorine sum parameters such as extractable organic fluorine (EOF) and the sum of quantified analytes are frequently reported. We propose using oxidative conversion to separate (unidentified) weakly fluorinated compounds (e.g., pesticides, pharmaceuticals) from PFAA-precursors (perfluoroalkyl chain lengths ≥ C6). We show with three organofluorine model substances (flufenamic acid, diflufenican, pantoprazole) that CF3-groups or aromatic fluorine can be quantitatively converted to inorganic fluoride and trifluoroacetic acid (TFA) by applying PhotoTOP oxidation (UV/TiO2). The principle of fluorine separation in mixtures is demonstrated by the oxidation of the three weakly fluorinated compounds together with the PFAA-precursor 6:2/6:2 fluorotelomer mercaptoalkyl phosphate diester (FTMAP). After oxidation, the products F− and TFA were separated from PFCAs ( C4) by SPE, and the fractions were analyzed individually. Closed mass balances both with and without the addition of organic matrix were achieved. Eventually, the fluorine balance was verified by total fluorine measurements with combustion ion chromatography (CIC). The proposed methods should be considered a proof of concept to potentially explain unidentified fractions of the EOF, especially if compounds with low fluorine content such as pesticides, pharmaceuticals, and their transformation products contribute largely to the EOF. Future studies are needed to show the applicability to the complexity of environmental samples. Graphical Abstract KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613429 DO - https://doi.org/10.1007/s00216-024-05590-5 SP - 1 EP - 10 PB - Springer Science and Business Media LLC AN - OPUS4-61342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lancaster, Shaun T. A1 - Sahlin, Eskil A1 - Oelze, Marcus A1 - Ostermann, Markus A1 - Vogl, Jochen A1 - Laperche, Valérie A1 - Touze, Solène A1 - Ghestem, Jean-Philippe A1 - Dalencourt, Claire A1 - Gendre, Régine A1 - Stammeier, Jessica A1 - Klein, Ole A1 - Pröfrock, Daniel A1 - Košarac, Gala A1 - Jotanovic, Aida A1 - Bergamaschi, Luigi A1 - Di Luzio, Marco A1 - D’Agostino, Giancarlo A1 - Jaćimović, Radojko A1 - Eberhard, Melissa A1 - Feiner, Laura A1 - Trimmel, Simone A1 - Rachetti, Alessandra A1 - Sara-Aho, Timo A1 - Roethke, Anita A1 - Michaliszyn, Lena A1 - Pramann, Axel A1 - Rienitz, Olaf A1 - Irrgeher, Johanna T1 - Evaluation of X-ray fluorescence for analysing critical elements in three electronic waste matrices: A comprehensive comparison of analytical techniques N2 - As the drive towards recycling electronic waste increases, demand for rapid and reliable analytical methodology to analyse the metal content of the waste is increasing, e.g. to assess the value of the waste and to decide the correct recycling routes. Here, we comprehensively assess the suitability of different x-ray fluorescence spectroscopy (XRF)-based techniques as rapid analytical tools for the determination of critical raw materials, such as Al, Ti, Mn, Fe, Co, Ni, Cu, Zn, Nb, Pd and Au, in three electronic waste matrices: printed circuit boards (PCB), light emitting diodes (LED), and lithium (Li)-ion batteries. As validated reference methods and materials to establish metrological traceability are lacking, several laboratories measured test samples of each matrix using XRF as well as other independent complementary techniques (instrumental neutron activation analysis (INAA), inductively coupled plasma mass spectrometry (ICP-MS) and ICP optical emission spectrometry (OES)) as an inter-laboratory comparison (ILC). Results highlighted key aspects of sample preparation, limits of detection, and spectral interferences that affect the reliability of XRF, while additionally highlighting that XRF can provide more reliable data for certain elements compared to digestion-based approaches followed by ICP-MS analysis (e.g. group 4 and 5 metals). A clear distinction was observed in data processing methodologies for wavelength dispersive XRF, highlighting that considering the metals present as elements (rather than oxides) induces overestimations of the mass fractions when compared to other techniques. Eventually, the effect of sample particle size was studied and indicated that smaller particle size (<200 μm) is essential for reliable determinations. KW - XRF KW - WEEE KW - PCB KW - Battery KW - LED KW - Recycling PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614060 DO - https://doi.org/10.1016/j.wasman.2024.10.015 VL - 190 SP - 496 EP - 505 PB - Elsevier B.V. AN - OPUS4-61406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jurković, J. A1 - Kazlagić, Anera A1 - Sulejmanović, J. A1 - Smječanin, N. A1 - Karalija, E. A1 - Prkić, A. A1 - Nuhanović, M. A1 - Kolar, M. A1 - Albuquerque, A. T1 - Assessment of heavy metals bioaccumulation in Silver Birch (Betula pendula Roth) from an AMD active, abandoned gold mine waste N2 - Acid mine drainage (AMD) is generally outlined as one of the largest environmental concerns, characterized by very low pH value of mine waste, heavy metals and high sulphate content. This extremely hostile environment reduces plant ability to develop and grow. Present study focuses on a silver birch (Betula pendula Roth), a pioneer species that grows on an extremely hostile gold mine waste, to investigate the bioaccumulation of rare metals (thallium (Tl) and indium (In)), as well as nine other more common heavy metals (bismuth (Bi), cadmium (Cd), cobalt (Co), copper (Cu), lead (Pb), manganese (Mn), nickel (Ni), silver (Ag) and zinc (Zn)), and to asses phytoextraction and phytostabilization potential of silver birch. Additionally, parameters determining AMD process and overall contamination (pH, electrical conductivity (EC), sulphates (SO₄²⁻), arsenic (As), iron (Fe), oxidation–reduction potential (ORP), turbidity, dissolved oxygen (DO), total dissolved solids (TDS), acidity, hardness, X-ray diffraction (XRD) and radioactivity) were determined in mine waste and drainage water samples. To assess the heavy metals bioaccumulation and mine waste status, statistical geochemical indices were determined: bioaccumulation factor (BCF), pollution load index (PLI), geochemical abundance index (GAI) and exposure index (EI). The results show that silver birch bioaccumulates the essential elements Cu, Ni, Mn and Zn, and the nonessential elements Tl (average BCF = 24.99), In (average BC = 23.01) and Pb (average BCF = 0.84). Investigated mine waste was enriched by Bi, Ag and Cd according to positive values of GAI index. Present research provides a novel insight into bioaccumulation of nonessential heavy metals in silver birches who grow on the extremely hostile mine waste, and they exhibit significant phytoremediation potential. KW - Heavy metals KW - Acid mine drainage KW - Bioaccumulation KW - Silver birch KW - Thallium PY - 2023 DO - https://doi.org/10.1007/s10653-023-01774-7 SN - 1573-2983 SN - 0142-7245 VL - 45 SP - 9855 EP - 9873 PB - Springer Science and Business Media CY - Dordrecht AN - OPUS4-61835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kader, A. A1 - Snellings, J. A1 - Adams, L. C. A1 - Gottheil, P. A1 - Mangarova, D. B. A1 - Heyl, J. L. A1 - Kaufmann, Jan Ole A1 - Moeckel, J. A1 - Brangsch, J. A1 - Auer, T. A. A1 - Collettini, F. A1 - Sauer, F. A1 - Hamm, B. A1 - Käs, J. A1 - Sack, I. A1 - Makowski, M. R. A1 - Braun, J. T1 - Sensitivity of magnetic resonance elastography to extracellular matrix and cell motility in human prostate cancer cell line-derived xenograft models N2 - Prostate cancer (PCa) is a significant health problem in the male population of the Western world. Magnetic resonance elastography (MRE), an emerging medical imaging technique sensitive to mechanical properties of biological tissues, detects PCa based on abnormally high stiffness and viscosity values. Yet, the origin of these changes in tissue properties and how they correlate with histopathological markers and tumor aggressiveness are largely unknown, hindering the use of tumor biomechanical properties for establishing a noninvasive PCa staging system. To infer the contributions of extracellular matrix (ECM) components and cell motility, we investigated fresh tissue specimens from two PCa xenograft mouse models, PC3 and LNCaP, using magnetic resonance elastography (MRE), diffusion-weighted imaging (DWI), quantitative histology, and nuclear shape analysis. Increased tumor stiffness and impaired water diffusion were observed to be associated with collagen and elastin accumulation and decreased cell motility. Overall, LNCaP, while more representative of clinical PCa than PC3, accumulated fewer ECM components, induced less restriction of water diffusion, and exhibited increased cell motility, resulting in overall softer and less viscous properties. Taken together, our results suggest that prostate tumor stiffness increases with ECM accumulation and cell adhesion - characteristics that influence critical biological processes of cancer development. MRE paired with DWI provides a powerful set of imaging markers that can potentially predict prostate tumor development from benign masses to aggressive malignancies in patients. Statement of significance: Xenograft models of human prostate tumor cell lines, allowing correlation of microstructure-sensitive biophysical imaging parameters with quantitative histological methods, can be investigated to identify hallmarks of cancer. KW - Magnetic resonance elastography KW - Quantitative histology KW - Prostate cancer KW - Stiffness KW - Fluidity KW - Apparent diffusion coefficient KW - Collagen KW - Elastin KW - Nuclear shape PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618361 DO - https://doi.org/10.1016/j.bioadv.2024.213884 SN - 2772-9508 VL - 161 SP - 1 EP - 12 PB - Elsevier CY - Amsterdam AN - OPUS4-61836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wittwer, Philipp A1 - Roesch, Philipp A1 - Vogel, Christian A1 - Simon, Fabian A1 - Gehrenkemper, Lennart A1 - Feldmann, Ines A1 - Simon, Franz-Georg T1 - Less Is More: Influence of Cross-Linking Agent Concentration on PFOS Adsorption in Chitosan N2 - As a result of the continuous use of persistent per- and polyfluoroalkyl substances (PFAS), e.g., in aviation firefighting foams, contamination with PFAS has been found in soil, groundwater, and surface water around thousands of industrial and military installations. Due to their harmful (environmental) potential, further dispersion in the environment needs to be stopped, which can be achieved by appropriate absorption materials. In this work, the influence of the cross-linking agent epichlorohydrin (ECH) concentration on the perfluorooctanesulfonic acid (PFOS) adsorption capacity of chitosan gel was investigated. It was found that higher ECH concentration during the cross-linking step decreases the PFOS adsorption capacity of the cross-linked chitosan gel from 0% to 4% ECH solution by about 15%. Using a concentration of 1%, ECH resulted still in an acid-stable material, and a maximum PFOS loading capacity of 4.04 mmol/g was obtained, one of the highest described in the literature. Furthermore, we used a rapid small-scale column test to compare the PFOS adsorption capacity of chitosan and activated carbon, each in both milled and unmilled form. Unmilled chitosan showed the highest PFOS adsorption capacity considering adsorption material dry masses (>0.9 and <0.4 mmol/g for both types of chitosan and activated carbon, respectively). Milled activated carbon proved to be the better adsorption material, considering the fixed volume of the adsorber (>99.9% PFOS adsorbed). Overall, the cross-linking agent concentration in chitosan is a crucial factor influencing its PFOS absorption potential. Our results feature cross-linked chitosan as an effective economic and ecologic alternative for PFOS adsorption in aqueous solutions. KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Remediation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618406 DO - https://doi.org/10.3390/app142311145 VL - 14 IS - 23 SP - 1 EP - 13 PB - MDPI AN - OPUS4-61840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wittwer, Philipp T1 - Results of ILC Data Treatment N2 - Results of the interlaboratory comparison study for data treatment were presented. They show, that nearly all participants found all the problems in the data. However, only a few corrected the problems, therefore making it one possible point to focus on in the knowledge sharing program. T2 - AGM POLMO Meeting 2024 CY - Paris, France DA - 21.05.2024 KW - JNP POLMO KW - ILC KW - Ringversuch PY - 2024 AN - OPUS4-60166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bosc-Bierne, Gaby A1 - Ewald, Shireen A1 - Kreuzer, Oliver J. A1 - Weller, Michael G. T1 - Efficient Quality Control of Peptide Pools by UHPLC and Simultaneous UV and HRMS Detection N2 - Peptide pools consist of short amino acid sequences and have proven to be versatile tools in various research areas in immunology and clinical applications. They are commercially available in many different compositions and variants. However, unlike other reagents that consist of only one or a few compounds, peptide pools are highly complex products which makes their quality control a major challenge. Quantitative peptide analysis usually requires sophisticated methods, in most cases isotope-labeled standards and reference materials. Usually, this would be prohibitively laborious and expensive. Therefore, an approach is needed to provide a practical and feasible method for quality control of peptide pools. With insufficient quality control, the use of such products could lead to incorrect experimental results, worsening the well-known reproducibility crisis in the biomedical sciences. Here we propose the use of ultra-high performance liquid chromatography (UHPLC) with two detectors, a standard UV detector at 214 nm for quantitative analysis and a high-resolution mass spectrometer (HRMS) for identity confirmation. To be cost-efficient and fast, quantification and identification are performed in one chromatographic run. An optimized protocol is shown, and different peak integration methods are compared and discussed. This work was performed using a peptide pool known as CEF advanced, which consists of 32 peptides derived from cytomegalovirus (CMV), Epstein–Barr virus (EBV) and influenza virus, ranging from 8 to 12 amino acids in length. N2 - Peptidpools bestehen aus kurzen Aminosäuresequenzen und haben sich als vielseitige Werkzeuge in verschiedenen Forschungsbereichen der Immunologie und bei klinischen Anwendungen erwiesen. Sie sind in vielen verschiedenen Zusammensetzungen und Varianten im Handel erhältlich. Im Gegensatz zu anderen Reagenzien, die nur aus einer oder wenigen Verbindungen bestehen, sind Peptidpools jedoch hochkomplexe Produkte, was ihre Qualitätskontrolle zu einer großen Herausforderung macht. Die quantitative Peptidanalyse erfordert in der Regel ausgefeilte Methoden, in den meisten Fällen isotopenmarkierte Standards und Referenzmaterialien. Dies ist in der Regel sehr aufwändig und teuer. Daher wird ein Ansatz benötigt, der eine praktische und praktikable Methode zur Qualitätskontrolle von Peptidpools bietet. Bei unzureichender Qualitätskontrolle könnte die Verwendung solcher Produkte zu falschen Versuchsergebnissen führen, was das bekannte Problem der Reproduzierbarkeit in den biomedizinischen Wissenschaften noch verschärfen würde. Hier schlagen wir die Verwendung der Ultrahochleistungs-Flüssigkeitschromatographie (UHPLC) mit zwei Detektoren vor, einem Standard-UV-Detektor bei 214 nm für die quantitative Analyse und einem hochauflösenden Massenspektrometer (HRMS) für die Identitätsbestätigung. Um kosteneffizient und schnell zu sein, werden Quantifizierung und Identifizierung in einem einzigen chromatographischen Lauf durchgeführt. Es wird ein optimiertes Protokoll gezeigt, und es werden verschiedene Peak-Integrationsmethoden verglichen und diskutiert. Für diese Arbeit wurde ein Peptidpool verwendet, der als CEF advanced bekannt ist und aus 32 Peptiden besteht, die vom Cytomegalovirus (CMV), Epstein-Barr-Virus (EBV) und Influenzavirus stammen und zwischen 8 und 12 Aminosäuren lang sind. KW - Synthetic peptides KW - Quality control KW - Impurites KW - Byproducts KW - Degradation KW - Mass spectrometry KW - Orbitrap PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602299 DO - https://doi.org/10.3390/separations11050156 SN - 2297-8739 VL - 11 IS - 5 SP - 1 EP - 18 PB - MDPI CY - Basel AN - OPUS4-60229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pavasarytė, Lina A1 - Azevedo do Nascimento, Allana A1 - Cysne Barbosa, Ana Paula A1 - Trappe, Volker A1 - Melo, Daniel T1 - Effects of particle size and particle concentration of poly (ethylene-co-methacrylic acid) on properties of epoxy resin N2 - Self-healing polymers have been developed to improve durability and reduce costs associated with maintenance during service. The addition of thermoplastics to thermosets to produce mendable polymers appears as a promising selfhealing technique. In this study, poly (ethylene-co-methacrylic acid) (EMAA) was added to epoxy resin and the effects of EMAA addition on epoxy properties were evaluated. Specimens with two different contents of thermoplastic and particles sizes were manufactured. A two-level full factorial experimental design was used to evaluate the effect of particle size and particle content on properties of epoxy modified with addition of EMAA. Tensile tests and dynamic mechanical analysis (DMA) were used and the evaluated responses were tensile strength, modulus of elasticity, and glass transition temperature (Tg). X-ray computed tomography (XCT) was used to investigate particle size and concentration after manufacturing. It was found that the particle concentration has greater effects on stress–strain behavior of epoxy while Tg was not significantly affected by neither of the analyzed entrance variables. KW - Fracture KW - Self-healing KW - Epoxy KW - Thermoplastic PY - 2024 DO - https://doi.org/10.1002/app.55677 SN - 0021-8995 SP - 1 EP - 14 PB - Wiley online library AN - OPUS4-60205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Groschke, Matthias A1 - Becker, Roland T1 - Comparison of carrier gases for the separation and quantification of mineral oil hydrocarbon (MOH) fractions using online coupled high performance liquid chromatography-gas chromatography-flame ionisation detection N2 - On-line coupled high performance liquid chromatography-gas chromatography-flame ionisation detection (HPLC-GC-FID) was used to compare the effect of hydrogen, helium and nitrogen as carrier gases on the chromatographic characteristics for the quantification of mineral oil hydrocarbon (MOH) traces in food related matrices. After optimisation of chromatographic parameters nitrogen carrier gas exhibited characteristics equivalent to hydrogen and helium regarding requirements set by current guidelines and standardisation such as linear range, quantification limit and carry over. Though nitrogen expectedly led to greater peak widths, all required separations of standard compounds were sufficient and humps of saturated mineral oil hydrocarbons (MOSH) and aromatic mineral oil hydrocarbons (MOAH) were appropriate to enable quantitation similar to situations where hydrogen or helium had been used. Slightly increased peak widths of individual hump components did not affect shapes and widths of the MOSH and MOAH humps were not significantly affected by the use of nitrogen as carrier gas. Notably, nitrogen carrier gas led to less solvent peak tailing and smaller baseline offset. Overall, nitrogen may be regarded as viable alternative to hydrogen or helium and may even extend the range of quantifiable compounds to highly volatile hydrocarbon eluting directly after the solvent peak. KW - Mineral oil hydrocarobons KW - Food KW - Liquid chromatography KW - Gas chromatography KW - MOSH/MOAH PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601450 DO - https://doi.org/10.1016/j.chroma.2024.464946 SN - 0021-9673 VL - 1726 SP - 1 EP - 7 PB - Elsevier CY - New York, NY AN - OPUS4-60145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Gottlieb, Cassian A1 - Kapteina, Gesa A1 - Wilsch, Gerd A1 - Millar, Steven A1 - Reichling, Kenji T1 - Neues DGZfP-Merkblatt B14: Quantifizierung von Chlorid in Beton mittels LIBS N2 - Bei der Erhaltung von Stahlbetonbauwerken ist der Chloridgehalt im Beton ein wichtiger Parameter zur Festlegung geeigneter Instandsetzungsmaßnahmen. Die bisher etablierten Verfahren basieren auf der nasschemischen Analyse einer Probe, Bohrmehl oder aufgemahlener Segmente eines Bohrkerns. Das Verfahren liefert einen Chloridgehalt je Tiefensegment, was mit einer starken Homogenisierung der Probe einhergeht, wodurch detaillierte Informationen zu Chloridunterschieden im Millimeterbereich verloren gehen. Eine alternative Methode ist die laserinduzierte Plasmaspektroskopie (LIBS), die nicht nur die quantitative ortsaufgelöste Bestimmung des Chloridgehalts im Bezug zur Zementmasse ermöglicht, sondern auch simultan detaillierte Informationen über die Verteilung vieler anderer chemischer Elemente liefert. Die räumliche Auflösung liegt in der Regel im Bereich von einigen Millimetern, kann aber bei Bedarf auf 0,1 mm oder weniger erhöht werden. Das neue Merkblatt B14 „Quantifizierung von Chlorid in Beton mit der laserinduzierten Plasmaspektroskopie (LIBS)“ der Deutschen Gesellschaft für Zerstörungsfreie Prüfungen (DGZfP) regelt und vereinheitlicht erstmals die zuverlässige und reproduzierbare Ermittlung des Chloridgehalts mit LIBS. In diesem Beitrag wird das Merkblatt vorgestellt und anhand praktischer Anwendungsbeispiele das Potenzial von LIBS für Fragestellungen in der Betonerhaltung verdeutlicht. KW - LIBS KW - Chlor KW - Chlorid KW - Beton KW - Bauwerksdiagnostik PY - 2024 DO - https://doi.org/10.1002/best.202400014 SP - 1 EP - 7 AN - OPUS4-60005 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalgic, Mete-Sungur T1 - Lösemittelfreie Probenpräparation zur Untersuchung von Polymerblends mittels MALDI-TOF MS N2 - Die Probenpräparation ist ein wichtiger Schritt für die Qualität der Massenspektren in MALDI-TOF MS. Es werden Polymerproben, die lösungsmittelbasiert und lösungsmittelfrei präpariert worden sind, verglichen. Dabei werden die Intensitätsverhältnisse von ternären Mischungen von PEG-, PS- und PMMA-Polymeren beachtet. T2 - 28. Kolloquium - Massenspektrometrische Techniken zur Untersuchung synthetischer Polymere CY - Berlin, Germany DA - 14.05.2024 KW - Polymere KW - Massenspektrometrie KW - Probenpräparation PY - 2024 AN - OPUS4-60032 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leube, Peter T1 - Quantification of ultrashort per- and polyfluoroalkyl substances (PFAS) in water samples via headspace gas chromatography-mass spectrometry (GC-MS) - a method development N2 - Per- and polyfluoroalkyl substances (PFAS) were classified as a group of highly concerning chemicals over the last decades. Because of the high persistence of PFAS, their previous use led to contamination of the environment and human population. Due to ongoing use and incomplete remediation or destruction methods, the PFAS background in the environment is growing continuously. The presence of ultrashort PFAS (with ≤3 carbon atoms) in the environment is often overlooked despite their contributions to PFAS levels. These compounds may directly contaminate the environment and arise from degradation of polyfluorinated compounds as well as incomplete PFAS destruction in certain industrial processes. Nonetheless, few approaches for targeted analysis of ultrashort PFASs have been developed, except for trifluoroacetic acid (TFA). Beside liquid (LC-MS/MS), supercritical fluid (SFC-MS/MS), and ion chromatography (IC-MS)-based systems, gas chromatography coupled with mass spectrometry (GC-MS) is a promising method for detection and quantification of ultrashort PFAS. The goal of this study was to develop a simple headspace GC-MS method for the quantification of ultrashort perfluorocarboxylic acids (PFCAs) and polyfluorinated alcohols (PFOHs) in water samples. In contrast to PFOHs, functionalization of PFCAs was required for quantification. This was done by esterification with methanol at 80 °C, which can be carried out directly in the headspace GC-MS system. Moreover, several parameters were optimized to achieve a low limit of quantification (LOQ) for the analytes used: i) The ratio of the aqueous solution, methanol, and available gas phase within the analysis vessel, ii) the concentration of additional acid in esterification mixtures of PFCAs, iii) shaking frequency and iv) shaking time before analysis. After optimizing the procedure, we were able to quantify ultrashort PFCAs and PFOHs. Thus, our developed headspace GC-MS method has the potential to be used as an alternative target analysis for ultrashort-chain PFCAs and PFOHs in various water samples (groundwater, wastewater). T2 - SETAC Europe 34th Annual Meeting CY - Seville, Spain DA - 05.05.2024 KW - Ultrashort PFAS KW - Headspace GC-MS KW - Perfluorocarboxylic acid (PFCA) KW - Polyfluorinated alcohol (PFOH) PY - 2024 AN - OPUS4-60042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Stephan A1 - Hoffmann, Holger A1 - Garbe, Leif-Alexander A1 - Harrer, Andrea A1 - Steiner, Markus A1 - Himly, Martin A1 - Schneider, Rudolf T1 - Re-assessment of monoclonal antibodies against diclofenac for their application in the analysis of environmental waters N2 - The non-steroidal anti-inflammatory drug (NSAID) diclofenac (DCF) is an important environmental contaminant occurring in surface waters all over the world, because, after excretion, it is not adequately removed from wastewater in sewage treatment plants. To be able to monitor this pollutant, highly efficient analytical methods are needed, including immunoassays. In a medical research project, monoclonal antibodies against diclofenac and its metabolites had been produced. Based on this monoclonal anti-DCF antibody, a new indirect competitive enzyme-linked immunosorbent assay (ELISA) was developed and applied for environmental samples. The introduction of a spacer between diclofenac and the carrier protein in the coating conjugate led to higher sensitivity. With a test midpoint of 3 mg L−1 and a measurement range of 1–30 mg L−1, the system is not sensitive enough for direct analysis of surface water. However, this assay is quite robust against matrix influences and can be used for wastewater. Without adjustment of the calibration, organic solvents up to 5%, natural organic matter (NOM) up to 10 mg L−1, humic acids up to 2.5 mg L−1, and salt concentrations up to 6 g L−1 NaCl and 75 mg L−1 CaCl2 are tolerated. The antibody is also stable in a pH range from 3 to 12. Cross-reactivity (CR) of 1% or less was determined for the metabolites 40-hydroxydiclofenac (40-OH-DCF), 5-hydroxydiclofenac (5-OH-DCF), DCF lactam, and other NSAIDs. Relevant cross-reactivity occurred only with an amide derivative of DCF, 6-aminohexanoic acid (DCF-Ahx), aceclofenac (ACF) and DCF methyl ester (DCF-Me) with 150%, 61% and 44%, respectively. These substances, however, have not been found in samples. Only DCF-acyl glucuronide with a cross-reactivity of 57% is of some relevance. For the first time, photodegradation products were tested for cross-reactivity. With the ELISA based on this antibody, water samples were analysed. In sewage treatment plant effluents, concentrations in the range of 1.9–5.2 mg L−1 were determined directly, with recoveries compared to HPLC-MS/MS averaging 136%. Concentrations in lakes ranged from 3 to 4.4 ng L−1 and were, after pre-concentration, determined with an average recovery of 100% KW - Antikörper KW - Immunoassay KW - Wasser PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602280 DO - https://doi.org/10.1039/d3ay01333b VL - 16 IS - 21 SP - 3349 EP - 3363 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-60228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tatzel, Michael A1 - Oelze, Marcus A1 - Frick, Daniel A. A1 - Di Rocco, Tommaso A1 - Liesegang, Moritz A1 - Stuff, Maria A1 - Wiedenbeck, Michael T1 - Silicon and oxygen isotope fractionation in a silicified carbonate rock N2 - Silicon isotope fractionation during silicification is poorly understood and impedes our ability to decipher paleoenvironmental conditions from Si isotopes in ancient cherts. To investigate isotope fractionation during silica-for-carbonate replacement we analyzed the microscale Si and O isotope composition in different silica phases in a silicified zebra dolostone as well as their bulk δ18O and Δ’17O compositions. The subsequent replacement of carbonate layers is mimicked by decreasing δ18O and δ30Si. The textural relationship and magnitude of Si and O isotope fractionation is best explained by near-quantitative silica precipitation in an open system with finite Si. A Rayleigh model for silicification suggests positive Ɛ30/28Si during silicification, conforming with predictions for isotope distribution at chemical equilibrium from ab-initio models. Application of the modelled Ɛ30Si-T relationship yields silicification temperatures of approx. 50°C. To reconcile the δ18Ochert composition with these temperatures, the δ18O of the fluid must have been between -2.5 and -4 ‰, compositions for which the quartz phases fall close to the oxygen equilibrium fractionation line in three-isotope space. Diagenetic silica replacement appears to occur in O and Si isotopic equilibrium allowing reconstructions of temperatures of silicification from Si isotopes and derive the δ18O composition of the fluid – a highly desired value needed for accurate reconstructions of the temperature- and δ18O histories of the oceans. KW - Silicon isotopes PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-603430 DO - https://doi.org/10.1016/j.chemgeo.2024.122120 SN - 0009-2541 VL - 658 SP - 1 EP - 13 PB - Elsevier B.V. AN - OPUS4-60343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ronen, A. A1 - Panglisch, S. T1 - Detection, Quantification and Treatment of Per and Polyfluoroalkyl substances (PFAS) in Groundwater N2 - The research project focuses on tackling the detection, measurement, and elimination of per- and polyfluoroalkyl substances (PFAS) from polluted groundwater, with a particular emphasis on addressing short (C4-C7) and ultrashort (C1-C3) chain PFAS. Given the widespread use of PFAS in various products, they are commonly found in groundwater near industrial and military sites in Germany and Israel. Moreover, recent regulations limiting the use of long chain PFAS have led industries to shift towards shorter chain alternatives. Hence, our efforts are geared towards refining detection, quantification, and removal methods for short and ultrashort chain PFAS. In terms of detection, ww are developing passive sampling devices capable of collecting and tracking the temporal distribution of PFAS species in groundwater. This will enable us to analyze contaminations in German and Israeli groundwater using cutting-edge analytical techniques. Additionally, contaminated groundwater will undergo a two-stage treatment process aimed at concentrating the relatively low PFAS concentrations using innovative membrane technologies such as closed-circuit reverse osmosis and mixed matrix composite nanofiltration membrane adsorbers. Subsequently, the streams containing higher PFAS concentrations will be treated through coagulation, with the remaining PFAS being adsorbed onto carbonaceous nanomaterials. The outcome of this research will include the creation of advanced tools for detecting, measuring, and eliminating PFAS from polluted groundwater, while also enhancing our understanding of the scope of these contaminations. T2 - German Israeli Water Technology Status Seminar CY - Koblenz, Germany DA - 18.06.2024 KW - Ground water KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Remediation PY - 2024 AN - OPUS4-60328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Leube, Peter T1 - Quantification of ultrashort per- and polyfluoroalkyl substances (PFAS) in water samples via headspace gas chromatographymass spectrometry (GC-MS) - a method development N2 - Ultrashort PFAS (≤ 3 carbon atoms) were overlooked for a long time in analytical monitoring. Beside through the use of these substances, they contribute to the PFAS background in the environment through (environmental/ bio-) degradation and incomplete destruction3 of PFAS with longer carbon chains or other fluorinated compounds. As part of the German-Israeli Cooperation in Water Technology Research project „Detection, quantification, and treatment of per- and polyfluoroalkyl substances in groundwater“ (DEFEAT-PFAS), we are developing an as simple as possible direct headspace (HS-)GC-MS method to detect trifluoroacetic acid (TFA) and perfluoropropanioc acid (PFPrA), as well as trifluoroethanol (TFEtOH), pentafluoropropanol(PFPrOH) and hexafluoroiospropanol (HFIP) in water samples. Here we present the results of the PFAS mentioned in spiked ultrapure water solutions. T2 - German Israeli Water Technology Status Seminar CY - Koblenz, Germany DA - 18.06.2024 KW - Ground water KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Gas chromatography - mass spectrometry (GC-MS) PY - 2024 AN - OPUS4-60330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ronen, A. A1 - Vogel, Christian A1 - Leube, Peter A1 - Ben Efraim, R. A1 - Nir, O. A1 - Chaudhary, M. A1 - Futterlieb, M. A1 - Panglisch, S. T1 - DEFEAT-PFAS: Detection, Quantification, and Treatment of Per- and Polyfluoroalkyl Substances (PFAS) in Groundwater N2 - The research project focuses on tackling the detection, measurement, and elimination of per- and polyfluoroalkyl substances (PFAS) from polluted groundwater, with a particular emphasis on addressing short (C4-C7) and ultrashort (C1-C3) chain PFAS. Given the widespread use of PFAS in various products, they are commonly found in groundwater near industrial and military sites in Germany and Israel. Moreover, recent regulations limiting the use of long chain PFAS have led industries to shift towards shorter chain alternatives. Hence, our efforts are geared towards refining detection, quantification, and removal methods for short and ultrashort chain PFAS. In terms of detection, ww are developing passive sampling devices capable of collecting and tracking the temporal distribution of PFAS species in groundwater. This will enable us to analyze contaminations in German and Israeli groundwater using cutting-edge analytical techniques. Additionally, contaminated groundwater will undergo a two-stage treatment process aimed at concentrating the relatively low PFAS concentrations using innovative membrane technologies such as closed-circuit reverse osmosis and mixed matrix composite nanofiltration membrane adsorbers. Subsequently, the streams containing higher PFAS concentrations will be treated through coagulation, with the remaining PFAS being adsorbed onto carbonaceous nanomaterials. The outcome of this research will include the creation of advanced tools for detecting, measuring, and eliminating PFAS from polluted groundwater, while also enhancing our understanding of the scope of these contaminations. T2 - German Israeli Water Technology Status Seminar CY - Koblenz, Germany DA - 18.06.2024 KW - Ground water KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Remediation PY - 2024 UR - https://indico.scc.kit.edu/event/4029/attachments/7552/12045/Proceedings_Ger-Isr-Coop_Status-Seminar-2024.pdf SP - 33 EP - 36 AN - OPUS4-60331 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Simon, Franz-Georg T1 - Detektion, Quantifizierung und Entfernung von insbesondere ultrakurzkettigen PFAS in Grundwasser N2 - Da PFAS in großem Umfang in einer Vielzahl von Produkten verwendet wurde, sind sie im Grundwasser in der Nähe vieler industrieller und militärischer Anlagen weltweit zu finden. Darüber hinaus führten neue Vorschriften und Beschränkungen für die Verwendung von langkettigen PFAS zu einer vermehrten Produktion kurzkettiger Alternativen. Ultrakurzkettige PFAS (≥C3) können natürliche und anthropogene Barrieren durchdringen und schließlich in Trinkwasserquellen gelangen. Zudem entfernen die meisten gängigen Trinkwasser-aufbereitungsverfahren die ultrakurzkettigen PFAS nicht ausreichend. Im Kooperationsprojekt DEFEAT-PFAS wird daher das Ziel verfolgt, Wissenslücken über Nachweis, Quantifizierung und Entfernung von kurz- (C4-C7) und ultrakurzkettige (C1-C3) PFAS, in kontaminiertem Grundwasser zu schließen. Die israelischen und deutschen Projektpartner entwickeln dafür analytische Methoden and selektive Passivsammler, um das zeitliche Profil von PFAS-Spezies im Grundwasser zu erfassen und überwachen. Darüber hinaus ein zweistufiges Verfahren entwickelt, welches darauf ausgelegt ist, die relativ niedrigen PFAS-Konzentrationen im Grundwasser durch neuartige Membranverfahren, Umkehrosmose im Batchbetrieb mit geschlossenem Kreislauf sowie Verbund-Nanofiltrationsmembranen, zu konzentrieren. Anschließend werden die PFAS angereicherten Konzentrate mittels Koagulation behandelt und das verbleibende PFAS an kohlenstoffhaltigen Nanomaterialien adsorbiert. T2 - Workshop des Netzwerks Perflusan CY - Karlsruhe, Germany DA - 18.06.2024 KW - Grundwasser KW - Per- und Polyfluoroierte Alkylsubstanzen (PFAS) PY - 2024 AN - OPUS4-60334 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kaczmarek, D. A1 - Albert, T. J. A1 - Munz, Martin A1 - Sturm, Heinz A1 - Bonse, Jörn T1 - Erratum: “Structure formation on the surface of indium phosphide irradiated by femtosecond laser pulses” [J. Appl. Phys. 97, 013538 (2005)] N2 - This erratum publishes some corrections to the article “Structure formation on the surface of indium phosphide irradiated by femtosecond laser pulses” [J. Appl. Phys. 97, 013538 (2005)]. PY - 2024 DO - https://doi.org/10.1063/5.0222903 SN - 0021-8979 SN - 1089-7550 VL - 136 IS - 4 SP - 1 EP - 2 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-60690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gauglitz, Günter A1 - Bodensteiner, Michael A1 - Bohleber, Pascal A1 - Clases, David A1 - Dahms, Marcel A1 - Engelhard, Carsten A1 - Haider, Markus A1 - Hayen, Heiko A1 - Herbst‐Irmer, Regine A1 - Jäger, Martin A1 - Kramell, Annemarie E. A1 - Legner, Robin A1 - Matysik, Frank‐Michael A1 - Pöthig, Alexander A1 - Rädle, Matthias A1 - Seifert, Stephan A1 - Steinhauser, Georg A1 - Wolter, Kathrin T1 - Trendbericht Analytische Chemie 2024 N2 - Mehrdimensionale Trenntechniken sowie Kopplungstechniken verbessern weiter die Auflösung in der Analytik. In der Elementanalytik beeindrucken neue Entwicklungen der Massenspektrometrie mit induktiv gekoppeltem Plasma, in der Archäometrie zerstörungsfreie In‐situ‐Analysen. Der 3‐D‐Druck treibt die elektroanalytische Forschung voran, und die Prozessanalytik setzt auf Lab‐on‐a‐Chip und vermeldet Neues bei der Raman‐Spektroskopie mit Flüssigkernlichtleitern. KW - Analytische Chemie KW - Trenntechniken KW - Elementanalytik KW - Massenspektrometrie KW - Prozessanalytik PY - 2024 DO - https://doi.org/10.1002/nadc.20244139242 SN - 1868-0054 VL - 72 IS - 4 SP - 52 EP - 64 PB - Wiley CY - Weinheim AN - OPUS4-62155 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalgic, Mete-Sungur T1 - Discrimination effects in MALDI-MS of Ternary Polymer Mixtures N2 - MALDI-TOF MS is a viable method to determine molecular weights of polymers. However, quantification using MALDI-TOF MS presents specific challenges due to intensity biases caused by instrumental and sample-specific parameters. In this presentation, the influence of molar masses on MALDI-TOF mass spectra is explored. The intensities of a ternary PMMA blend with different mixture ratios are depicted in contour plots. T2 - SALSA Make and Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - MALDI-TOF MS KW - Ternary polymer blends KW - PMMA PY - 2022 AN - OPUS4-62212 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalgic, Mete-Sungur T1 - Einfluss der Konformation auf das Ionisationsverhalten in MALDI-TOF MS N2 - MALDI-TOF Massenspektrometrie ist eine wichtige Methode zur Bestimmung von Molekulargewichten von Polymeren. Jedoch wird die quantitative Analyse von Polymeren durch verschiedene Faktoren erschwert. In dieser Präsentation wird unter anderem der Einfluss der molaren Massen auf die Massenspektren näher betrachtet. Dabei werden Konturplots von ternären PMMA- und PS-Mischungen gezeigt. T2 - 27. Kolloquium - Massenspetrometrische von Polymeren CY - Berlin, Germany DA - 09.05.2023 KW - MALDI-TOF MS KW - Ternäre Polymermischungen KW - PMMA und PS PY - 2023 AN - OPUS4-62214 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Portesi, Chiara T1 - Metrology for food safety in the circular economy: targeted and screening methods for contaminants in food and recycled packaging N2 - Safeguarding consumers from potential harm caused by food contamination is of paramount importance to ensure food safety. The focus on safety is a central priority for European Commision lawmakers. Furthermore, as outlined in the EU circular economy action plan, the development of a sustainable food system is a critical objective. However, progress towards these goals can sometimes face obstacles, including the risk of eroding consumer confidence in food quality. Factors such as the increased use of recycled and sustainable packaging materials and the growing awareness of emerging contaminants necessitate immediate attention. To ensure a high level of food safety throughout production and distribution, it is crucial to improve and harmonise analytical techniques for contaminant quantification. This constitutes the basis for reliable data and compliance with regulations and for resolving disputes and minimising financial losses within the food industry. The ScreenFood project (June 2024 -May 2027) is funded by the European Metrology Partnership and aims to develop reference methods and reference materials for quantifying contaminants in both food and food packaging, with a specific emphasis on recycled materials. These metrological tools will aid industries and official food control in guaranteeing the delivery of safe food and sustainable packaging while adhering to regulatory requirements. Specific objectives of the project are i. To improve protocols for the quantification of the mineral oil aromatic hydrocarbons (MOAH) fraction and for the quantification of the fraction consisting of substances with three or more aromatic ring systems (3+MOAH); ii. To develop sensitive analytical procedures for detecting and quantifying per- and polyfluoroalkyl substances (PFAS) in selected matrices, in line with EU requirements; iii. To develop traceable and highly accurate reference materials for quality control and quality assurance purposes; iv. to develop screening methods addressing new/existing organic and inorganic contaminants, in virgin and recycled packaging, such as PET, and bio-based and reusable materials; v. To investigate the migration of contaminants from packaging into food simulants, as well as to foster the research in the discovery of Emerging and Novel PFAS through non-targeted screening. The consortium brings together 28 partners from EU metrological institutes, research centres, control laboratories, EU reference laboratories and industries. A large panel of collaborators and stakeholders is supporting the consortium in keeping the project aligned with EU and industrial priorities.  T2 - 11th International Symposium on RECENT ADVANCES IN FOOD ANALYSIS (RAFA) CY - Prague, Czech Republic DA - 05.11.2024 KW - Per- and Polyfluoroalkyl Substances (PFAS) KW - MOSH/MOAH KW - EU Project KW - Food KW - Food Contact Material (FCM) KW - ScreenFood PY - 2024 AN - OPUS4-62185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Schäferling, Michael T1 - Focus issue "Luminescent imaging with optical chemical sensors" N2 - Photoluminescent imaging techniques using chemical sensors are essential tools in many areas of science and technology because they enable the visualization of parameters which exhibit no intrinsic color or fluorescence, e.g. O₂, pH, CO₂, H₂O₂, Ca²⁺, K⁺, or temperature, just to name a few. The application of luminescent probes exhibit the advantage that these can be delivered directly into the sample, which can also be a living cell or tissue, and they can be detected in a remote monitoring mode. They are often encapsulated in polymer nanoparticles, however planar 2D luminescent sensor materials have also found numerous applications in biomedical imaging, marine research, process control, or aerodynamics. Furthermore, they can be integrated into fiber optic (micro)sensors, microwell plates, or sensor arrays. Sensing of oxygen by means of luminescent probes that are quenched by oxygen is a widely used method in biomedical research. The corresponding probes have been reviewed in numerous extensive review articles in the past years. Therefore, we think that it is overdue to feature a critical assessment of the applicability of different probes for oxygen sensing inside live cells and tissue. The other emphasis of this compilation of articles was to introduce brand-new developments in the field of chemical imaging that were not in the focus of previous review articles. These concern the design of new sensor nanomaterials based on photon upconversion crystals, and new miniaturized analytical applications, e.g. in microfluidic devices, microreactors and microelectrophoresis. KW - Chemical sensors KW - Fluorescence imaging KW - Optical sensors PY - 2015 UR - https://iopscience.iop.org/collections/2050-6120_focus_issue_Luminescent-imaging-with-optical-chemical-sensors SN - 2050-6120 VL - 3 IS - 3 SP - 034001-1 EP - 034004-22 PB - IOP Publ. CY - Bristol AN - OPUS4-62181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - PFAS analysis by fluorine K-edge XANES spectroscopy and thermal and mechanochemical treatment N2 - Per- and polyfluoroalkyl substances (PFAS) are a large group of more than 12,000 organofluorine surfactants. As a result of continuous and prolific use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil, groundwater and surface water. . Current decontamination strategies of PFAS-burdened soils mainly consist of adsorption methods using adsorbents for fixation of PFAS in the ground. A second option is the utilization of a “pump and treat” process, cycling polluted soils through a washing plant leading to the concentration of the pollutants in the fine fraction. Both approaches are cost-intensive and not intended for the direct decomposition of all PFAS contaminants. Furthermore, the contaminated adsorbants have to be safely thermal treated for recovery. Hence, there is a great demand for innovative developments, dealing with new strategies of tackling the PFAS problem. Previously, mechanochemical treatment of polychlorinated organic compounds in soils showed an efficient dechlorination. Thus, we investigated mechanochemical treatment of PFAS contaminated soils with various additives in a ball mill. T2 - SEMICON CY - Tokyo, Japan DA - 12.12.2024 KW - Mechanochemical treatment KW - Per- and Polyfluoroalkyl substances (PFAS) KW - XANES spectroscopy KW - Thermal treatment PY - 2024 AN - OPUS4-62183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heide, K. A1 - Nolze, Gert A1 - Völksch, G. A1 - Heide, G. T1 - Boracite Mg3[B7O13Cl] from the Zechstein salt deposits N2 - Among the borates in the Middle European Zechstein Salt Succession boracite Mg3[B7O13Cl] is the most common mineral in quantity and local distribution. An exceptional enrichment is observed in Stassfurt Serie Z2) in the Stassfurth seam K2H. Boracite is to be found in two varieties: individual crystals in cubic, tetrahedral or dodecahedral habit on the one hand and fibrous crystals so-called “stassfurtite” on the other hand. The formation conditions such widely spread borates in the salt succession are ambiguous in two respects. First of all the synthetic formation of boracites is to be made by hydrothermal or melt conditions. Both processes can be suspended for the salt succession. Furthermore the cubic modification is stable above 265°C for the Mg-boracite. The cubic, tetrahedral or dodecahedral habit could be used as a geothermometer, but such conditions can be exclude by the paragenetic minerals, esp. carnallite (MgKCl3 x 6H2O). The chemical composition of orthorhombic, pseudo-cubic boracite depends on the location. Pure Mg-boracite in hexahedral habit and in fibrous habit, so-called “stassfurtite”, occurs in the North Harz region, whereas the Fe-, Mn-, Mg-boracite appears in the South Harz region. Until now the source of boron, the time of formation of crystals, but also the reasons for the differences in habit of the single hexahedral crystals are still unclear. The formation during a diagenetic/metamorphic process is evident. However, the preferred formation in Stassfurt seam could be an indication for the boron enrichment in an early diagenetic process. Furthermore permit the determination of the thermal stability and the volatile content of crystals conclusions to the chemical composition of the fluid. The observed variation suggests that the condition of crystal growth as well as the chemical composition of fluid repeatedly changed over the time. Randomly occuring xenomorpheous anhydrite and magnesite inclusions within single boracite crystals have been interpreted as an indication to factors of chemical milieu during the formation of crystals. The reversible phase transition temperature of the boracite is a linearly function of the iron and manganese content and varies from 265°C for Mg-boracite to 330°C for Fe(Mn)-boracite. The thermal decomposition of boracite is determined by two processes. The decomposition started with a boron-chlorine release (BOCl?), having a maximum rate at 1050°C. Additionally to this release one observes a simultaneous emission of H2O, HCl, HF, CO2 , N2 , SO2 , H2 , and hydro carbons. The results give evidence for the aged approach of a secondary formation of boracite within the complete Stassfurt seam, possibly in connection with the formation of salt diapirs in the Jura and Cretaceous period. The wider environmental distribution of borates is an indication of chemical transport processes within the salt succession. This should be a more important issue in the discussion about the utilisation of salt diapirs for the storage of nuclear waste. KW - Borate KW - Boracite KW - Thermal behaviour KW - Electron backscatter diffraction KW - Energy-dispersive x-ray spectroscopy PY - 2013 DO - https://doi.org/10.1524/zkri.2013.1633 VL - 228 SP - 467 EP - 475 PB - Oldenbourg Wissenschaftsverlag, München AN - OPUS4-37982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. A1 - Link, T. A1 - Svetlov, I. L. A1 - Nolze, Gert A1 - Saliwan Neumann, Romeo A1 - Lucas, H. T1 - Mechanism of porosity growth during homogenisation in single crystal nickel-based superalloys N2 - Several mechanisms for porosity growth in single crystal nickel-based superalloys during homogenisation heat treatment have been proposed in the literature. They were carefully checked using different experimental methods, namely quantitative light microscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and density measurements. It is shown that the main mechanism is the Kirkendall–Frenkel effect, i.e. generation of voids due to uncompensated efflux of Al atoms from dissolving γ/γ′-eutectic areas. The Al diffusion is supported by the afflux of vacancies from surrounding γ-matrix which results in porosity growth. This conclusion is confirmed by the estimation of the vacancy afflux towards the dissolving eutectic. KW - Ni-base superalloy KW - Eutectic KW - Vacancies KW - Porosity PY - 2013 VL - 104 IS - 8 SP - 776 EP - 782 PB - Carl Hanser Verlag AN - OPUS4-37983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Payton, E. A1 - Winkelmann, Aimo T1 - Advanced EBSD Pattern Interpretation through Iterative Post-Processing N2 - Since the BSE signal depends on many factors, like the chemistry of the phase and the acceleration voltage, the size and position of the detector array is (slightly) different from phase to phase so that an (iterative) post-processing of the stored patterns is highly recommended. The derived BSE signal can be used for phase assignment in high resolution and high speed maps when EBSD fails and/or EDS (energy dispersive spectroscopy) needs too much time for a suitable and parallel signal acquisition. KW - Electron backscatter diffraction KW - Phase identification KW - Microstructure KW - SEM PY - 2013 DO - https://doi.org/10.1017/S1431927613005631 VL - 19 IS - Suppl. 2 SP - 728 EP - 729 AN - OPUS4-37986 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert T1 - Combination of colored patterns and cubes for crystallographic point group visualization N2 - A concept based on the application of a cube as a general polyhedron is presented for the visualization of point group symmetry. The cube is used to represent both the highest and lowest crystal symmetries, with differences observable as patterns characteristic to each point group. Patterns are generated using direction-specific color keys, which enable the recognition of point group-specific distribution of vectors in an external reference frame. For the visualization of the incoherent hexagonal crystal classes, two twinned cubes are applied in order to generate symmetry operators that would otherwise be missing. The resulting hexagonal dipyramid is described in the frame of a cube, reducing the number of used symmetry operators from 72 to 60. The complete set of 32 polyhedra are suitable, for example, as a visual aid for understanding the crystal symmetry and/or sub- and supergroup relationships. KW - Subgroup KW - Crystal class KW - Color key KW - Fundamental zone KW - Teaching PY - 2013 DO - https://doi.org/10.1002/crat.201300134 VL - 48 IS - 7 SP - 476 EP - 489 PB - WILEY-VCH AN - OPUS4-37988 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert T1 - Azimuthal Projections: Data Rotation and Projection Switching in Real Time N2 - Pole figures are often used to present crystal orientation data. The huge number of single orientation measurements acquired by electron backscatter diffraction (EBSD) poses a challenge for pole figure representation due to the large number of calculations required. This significantly reduces the speed at which the data may be rotated and affects the ability to switch between different projection types. In the present work, it will be shown that satisfactory representation of orientation data in different projection types can generally be achieved by an imaging of a spherical projection. With this approach, explicit calculation of the projections is no longer required, allowing for both real-time dataset rotation and real-time switching between all projection types relevant to materials science. The technique can be applied to any other directional property distribution, for example, not only for EBSD orientation presentation. KW - Stereographic projection KW - Equal area projection KW - Gnomonic projection KW - Azimuthal projection KW - Crystal orientation KW - Projection imaging KW - Coordinate transformation KW - Real-time rotation PY - 2013 DO - https://doi.org/10.1017/S1431927613001414 VL - 19 SP - 950 EP - 958 PB - Microscopy Society of America AN - OPUS4-37989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR T1 - Amts- und Mitteilungsblatt, Band 46, Heft 3 T3 - Amts- und Mitteilungsblatt der BAM - 3/2016 PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-379934 SN - 0340-7551 VL - 46 IS - 3 SP - 141 EP - 342 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-37993 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reith, F. A1 - Fairbrother, L. A1 - Nolze, Gert A1 - Wilhelmi, O. A1 - Clode, P. L. A1 - Gregg, A. O. A1 - Parsons, J. E. A1 - Wakelin, S. A. A1 - Pring, A. A1 - Hough, R. A1 - Southam, G. A1 - Brugger, J. T1 - Nanoparticle factories: Biofilms hold the key to gold dispersion and nugget formation N2 - Biofilms living on gold (Au) grains play a key role in the biogeochemical cycle of Au by promoting the dispersion of Au via the formation of Au nanoparticles as well as the formation of secondary biomorphic Au. Gold grains from Queensland, Australia, are covered by a polymorphic, organic-inorganic layer that is up to 40 μm thick. It consists of a bacterial biofilm containing Au nanoparticles associated with extracellular polymeric substances as well as bacterioform Au. Focused ion beam (FIB) sectioning through the biofilm revealed that aggregates of nanoparticulate Au line open spaces beneath the active biofilm layer. These aggregates (bacterioform Au type 1) resulted from the reprecipitation of dissolved Au, and their internal growth structures provide direct evidence for coarsening of the Au grains. At the contact between the polymorphic layer and the primary Au, bacterioform Au type 2 is present. It consists of solid rounded forms into which crystal boundaries of underlying primary Au extend, and is the result of dealloying and Ag dissolution from the primary Au. This study demonstrates that (1) microbially driven dissolution, precipitation, and aggregation lead to the formation of bacterioform Au and contribute to the growth of Au grains under supergene conditions, and (2) the microbially driven mobilization of coarse Au into nanoparticles plays a key role in mediating the mobility of Au in surface environments, because the release of nanoparticulate Au upon biofilm disintegration greatly enhances environmental mobility compared to Au complexes only. KW - Nanomaterial KW - Gold KW - Electron backscatter diffraction PY - 2010 DO - https://doi.org/10.1130/G31052.1 VL - 38 IS - 9 SP - 843 EP - 846 PB - Geological Society of America AN - OPUS4-37995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Improved quantitative XRF analysis of industrial thin film samples by calibration using thin film RMs certified by reference-free XRF enabling traceability to the SI N2 - Reference-free XRF is a SI traceable technique for the determination of the mass deposition (mass per unit area) of elements in films on the nano- and micro scale. The method is radiometrically calibrated instrumentation (PTB@BESSY II, Germany) and based on reliable knowledge of all relevant atomic fundamental, experimental and instrumental parameters. No calibration sample or reference materials are necessary. The approach had been validated in the CCQM-P140 pilot study and the K129 key comparison by determination of mole fractions in Cu(In,Ga)Se2 thin films. T2 - Annual Meeting of ISO TC 201 SC 10 XRR/XRF CY - Seoul, Korea DA - 12.10.2016 KW - Reference-free XRF KW - CIGS thin films PY - 2016 AN - OPUS4-38265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Testing lateral resolution and field of view in imaging and small area analysis: reference materials and standardization N2 - The certified reference material BAM-L200, a nanoscale stripe pattern for length calibration and specification of lateral resolution, is described. BAM-L200 is prepared from a cross-sectioned epitaxially grown layer stack of AlxGa1-xAs and InxGa1 xAs on a GaAs substrate. The surface of BAM-L200 provides a flat pattern with stripe widths ranging down to 1 nm. Calibration distances, grating periods and stripe widths have been certified by TEM with traceability to the length unit. The combination of gratings, isolated narrow stripes and sharp edges of wide stripes offers a plenty of options for the determination of lateral resolution, sharpness and calibration of length scale at selected settings of imaging surface analytical instruments. The feasibility of the reference material for an analysis of the lateral resolution is demonstrated in detail by evaluation of ToF-SIMS, AES and EDX images. Other applications developed in the community are summarized, too. BAM-L200 fully supports the implementation of the revised International Standard ISO 18516 (in preparation) which is based on knowledge outlined in the Technical Report ISO/TR 19319:2013. T2 - 7th International Symposium on Practical Surface Analysis(PSA-16) CY - Daejeon, Korea DA - 17.10.2016 KW - BAM L200 KW - SIMS KW - AES KW - XPS PY - 2016 AN - OPUS4-38266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Schwarz, F. A1 - Heinrich, Thomas A1 - Kaufmann, J. O. A1 - Lippitz, Andreas A1 - Puttreddy, R. A1 - Rissanen, K. A1 - Schalley, C. A. T1 - Photocontrolled on-surface pseudorotaxane formation with well-ordered macrocycle multilayers N2 - The photoinduced pseudorotaxane formation between a photoresponsive axle and a tetralactam macrocycle was investigated in solution and on glass surfaces with immobilized multilayers of macrocycles. In the course of this reaction, a novel photoswitchable binding station with azobenzene as the photoswitchable unit and diketopiperazine as the binding station was synthesized and studied by NMR and UV/Vis spectroscopy. Glass surfaces have been functionalized with pyridine-terminated SAMs and subsequently withmultilayers of macrocycles through layer-by-layer self assembly. A preferred orientation of the macrocycles could be confirmed by NEXAFS spectroscopy. The photocontrolled Deposition of the axle into the surface-bound macrocycle-multilayers was monitored by UV/Vis spectroscopy and led to an increase of the molecular order, as indicated by more substantial linear dichroism effects in angle-resolved NEXAFS spectra. KW - Well-ordered macrocycle multilayers KW - XPS KW - NEXAFS PY - 2016 DO - https://doi.org/10.1002/chem.201603156 SN - 0947-6539 SN - 1521-3765 VL - 22 IS - 40 SP - 14383 EP - 14389 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-38270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Pelster, A. A1 - Tyler, B.J. A1 - Kösgen, M. A1 - Kassenböhmer, R. A1 - Peterson, R.E. A1 - Stöver, M. A1 - Arlinghaus, H. F. T1 - Improved 3D-imaging of a sirolimus/probucol eluting stent coating using laser postionization secondary neutral mass spectrometry and time-of-flight secondary ion mass spectrometry N2 - Implantable drug delivery systems that provide controlled and sustained release of a therapeutic agent are used in a wide variety of applications. Drug eluting stents, which are used to treat coronary artery disease, are among the most widespread of these devices, with an estimated 3x10⁶ implants annually worldwide. Controlling the rate of drug release from these devices relies on precise control of the three dimensional (3D)-distribution of the drug, so methods for measuring this distribution are of great importance. The aims of this work were to determine how 3D-imaging of polymer-free sirolimus/probucol drug eluting stent coatings could be improved through the use of laser postionization secondary neutral mass spectrometry (Laser- SNMS) and Ar cluster sputtering with time-of-flight secondary ion mass spectrometry (ToF-SIMS) and to optimize conditions for this analysis. In this study, 3D-imaging of a sirolimus/probucol dual drug eluting stent has been investigated using Laser-SNMS and ToF-SIMS. Laser-SNMS studies of pure sirolimus and probucol were undertaken using 30 keV Bi₃⁺ primary Ions and a 157 nm excimer postionization laser. Under optimal conditions, a greater than 100-fold increase in detected ion yield was observed for Laser-SNMS when compared to ToF-SIMS, although ToF-SIMS provided equal or greater yields for higher mass characteristic ions. Although the optimal laser power density for detecting probucol (5x10⁶W/cm²) was significantly lower than the optimum for sirolimus(7x10⁷W/cm²), an intermediate laser power density of 1x10⁷W/cm² was sufficient to allow imaging of both drugs. Using individual selected ion signals, ToF-SIMS and Laser-SNMS produced similar images of the two drug species. When using, however, a multivariate approach (Maximum autocorrelation factors), Laser-SNMS provided significant improvements in image contrast and small area detection when compared to ToF-SIMS. Following optimization of the technique, 3D-images of the dual drug eluting stent coating were obtained using 10 keV Ar₂₀₀₀⁺ cluster ions for sputtering and 30 keV Bi₃⁺ cluster ions for Analysis for both ToF-SIMS and Laser-SNMS. This work demonstrates the advantages of Laser-SNMS for 3D-imaging of pharmaceutical devices, which has not been previously published. Both ToF-SIMS and Laser-SNMS revealed that the outermost surface of the drug eluting coating contained pure sirolimus to a depth of a few tens of nanometers, with a few channels of sirolimus extending to a depth of around 1 lm. Below about 1 lm, the two drugs were uniformly mixed. Using the 10 keV Ar₂₀₀₀⁺ sputter beam, the authors were able to sputter through the complete drug coating (~6 μm) without observing any accumulated damage in the organic layer. The two techniques showed complementary strengths: ToF-SIMS offers faster data collection and better detected ion yield for larger characteristic ions than Laser-SNMS, and Laser-SNMS offers significantly enhanced detected ion yield for smaller fragment ions, allowing for improved Image contrast and Resolution of smaller features. KW - Imaging ToF SIMS KW - Eluting stent PY - 2016 DO - https://doi.org/10.1116/1.4964687 SN - 1934-8630 SN - 1559-4106 VL - 11 IS - 4 SP - 041001-1 EP - 041001-10 PB - AVS: Science & Technology of Materials, Interfaces, and Processing AN - OPUS4-38272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Kalbe, Henryk A1 - Rades, Steffi T1 - Determining shell thicknesses in stabilised CdSe@ZnS core-shell nanoparticles by quantitative XPS analysis using an infinitesimal columns model N2 - A novel Infinitesimal Columns (IC) simulation model is introduced in this study for the quantitativeanalysis of core-shell nanoparticles (CSNP) by means of XPS, which combines the advantages of exist-ing approaches. The IC model is applied to stabilised Lumidot™CdSe/ZnS 610 CSNP for an extensiveinvestigation of their internal structure, i.e. calculation of the two shell thicknesses (ZnS and stabiliser)and exploration of deviations from the idealised CSNP composition. The observed discrepancies betweendifferent model calculations can be attributed to the presence of excess stabiliser as well as synthesisresidues, demonstrating the necessity of sophisticated purification methods. An excellent agreement isfound in the comparison of the IC model with established models from the existing literature, the Shardmodel and the software SESSA. KW - XPS KW - Quantum dot KW - Core shell nano particle PY - 2016 DO - https://doi.org/10.1016/j.elspec.2016.08.002 SN - 0368-2048 VL - 212 SP - 34 EP - 43 PB - Elsevier B.V. AN - OPUS4-38273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Swaraj, S. A1 - Dietrich, Paul M. T1 - X-ray spectromicroscopy of nanoparticulate iron oxide phases N2 - Soft x-ray spectromicroscopy techniques have seen great amount of development in the recent years, and with the development of new diffraction limited synchrotron source, many new nanoscale and mesoscale characterization opportunities of applied materials are foreseen. In this perspective, the authors present some examples that illustrate the capabilities of spectromicroscopy techniques, namely, 2D and 3D spatially resolved chemical quantification, surface and bulk sensitive measurements, and polarization dependent measurements as applied to iron oxide nanoparticulate materials of biological, geological, and other origins. KW - X-ray spectromicroscopy KW - STXM KW - Iron oxide PY - 2016 DO - https://doi.org/10.1116/1.4966654 SN - 1934-8630 SN - 1559-4106 VL - 11 IS - 4 SP - 04B402-1 EP - 04B402-6 PB - AVS: Science & Technology of Materials, Interfaces, and Processing AN - OPUS4-38274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Current activities to implement the technology roadmap „Process Sensors 4.0“ N2 - As presented at the NAMUR general meeting 2015, the technology roadmap "Process Sensors 4.0" identifies the necessary requirements as well as the communication abilities of such process sensors. We report on the progress of discussions in trialogue between users, software and device manufacturers as well as the research. An important key is the definition of an appropriate and uniform topology for such smart sensors, which will be driven forward in a new NAMUR AK 3.7 "smart sensors" in mutual exchange with device and software manufacturers and research institutions. T2 - NAMUR General Meeting 2016 CY - Bad Neuenahr, Germany DA - 10.11.2016 KW - Prozess-Sensoren KW - Prozess-Sensoren 4.0 KW - Prozess-Spektroskopie KW - Process analytical technology PY - 2016 AN - OPUS4-38228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Die Technologie-Roadmap „Prozess-Sensoren 4.0“ – Chancen für neue Automatisierungskonzepte und neue Geschäftsmodelle N2 - Die auf der NAMUR HS 2015 vorgestellte Technologie-Roadmap „Prozess-Sensoren 4.0“ zeigt die nötigen Anforderungen an Prozess-Sensoren sowie an deren Kommunikations-fähigkeiten auf. Eine Topologie für smarte Sensoren, das Zusammenwirken mit daten- und modellbasierte Steuerungen bis hin zur Softsensorik sowie weitere Anforderungen an Sensoren sind heute noch nicht angemessen beschrieben. Wir müssen jetzt schnell die Weichen für eine smarte und sichere Kommunikationsarchitektur stellen, um zu einer störungsfreien Kommunikation aller Sensoren auf Basis eines einheitlichen Protokolls zu kommen, welches alle Sensoren ausgeben und verstehen. KW - Prozess-Sensoren KW - Prozess-Sensoren 4.0 KW - Industrie 4.0 KW - OPC UA KW - Prozessanalytik KW - Prozessindustrie KW - Automatisierung PY - 2016 UR - https://www.di-verlag.de/de/atp-plus-Smart-Sensors SN - 2510-3911 VL - 01 IS - 1 SP - 12 EP - 21 PB - DIV Deutscher Industrieverlag GmbH CY - München AN - OPUS4-38229 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schönhals, Andreas A1 - Zorn, R. A1 - Frick, B. T1 - Inelastic neutron spectroscopy as a tool to investigate nanoconfined polymer systems N2 - The effect of a nanometer scale confinement (pore sizes 7.5 nm down to 2.5 nm) on the vibrational density of states (VDOS) and on the molecular dynamics of Poly(dimethyl siloxane) (PDMS) and Poly(-methyl phenyl siloxane) (PMPS) is studied by inelastic Neutron scattering. The high penetration depth of neutrons makes neutron scattering a suitable tool for the study of confined systems. Moreover, Neutrons are sensitive to light nuclei therefore the confined polymers can be investigated directly, more or less independently of the confining host. Resulting findings are firstly, a reduction of the low frequency contributions to the VDOS below the Boson Peak frequency for both polymers. Including literature data, this reduction can be regarded as a more general feature for glass-forming systems confined by hard walls. Secondly, clear deviations in the temperature dependence of the mean squared displacement of the confined molecules compared to the bulk were found close to the thermal glass transition temperature, whereas localized methyl group rotations were only weakly influenced. Furthermore, the molecular dynamics is accessed. The combination of neutron Time-of-Flight with neutron backscattering, thus covering a broad dynamical range from sub ps to ns, reveal clear influence from confinement on the intermediate incoherent scattering function S(q,t). The latter was obtained by combining the inverse Fourier transform of the individual dynamical structure factors measured by the both methods. The time and q dependence of S(q,t) are discussed in detail for the local methyl group rotations and the segmental dynamics, considering both the interaction of the segments with the pore walls and possible geometrical confinement effects. KW - Confinement KW - Density of states KW - Dynamic glass transition PY - 2016 DO - https://doi.org/10.1016/j.polymer.2016.06.006 SN - 0032-3861 SN - 1873-2291 VL - 105 SP - 393 EP - 406 PB - Elsevier AN - OPUS4-38256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, P. T1 - Evaluation of electron microscopy techniques for the purpose of classification of nanomaterials N2 - One current and much-debated topic in the characterization of nanomaterials (NM) is the implementation of the recently introduced recommendation on a definition of a nanomaterial by the European Commission. According to this definition, a material is a NM when for 50% or more of the particles in the number size distribution, one or more external dimensions is in the size range 1 nm-100 nm. The European NanoDefine Project was set up to develop and validate a robust, readily implementable and cost-effective measurement approach to obtain a quantitative particle size distribution and to distinguish between NMs and non-NMs according to the definition. All currently available sizing techniques able to address nanoparticles were systematically evaluated. It was demonstrated that particle sizing techniques like: analytical centrifugation, particle tracking analysis, single-particle inductively coupled plasma mass-spectrometry, differential electrical mobility analysis, dynamic light scattering, small angle X-ray scattering, ultrasonic attenuation spectrometry, but also gas adsorption analysis based on the BET-method can be applied for a screening classification. However, the quality of the results depends on the individual material to be classified. For well-dispersed, nearly spherical (nano)particles most of the sizing techniques can be applied in a quick and reliable way. In contrast, the classification of most real-world materials is a challenging task, mainly due to non-spherical particle shape, large polydispersity or strong agglomeration/aggregation of the particles. In the present study it was shown that these issues can be resolved in most cases by electron microscopy as a confirmatory classification technique. Electron microscopy techniques such as TEM, STEM, SEM or TSEM (transmission in SEM) are capable of assessing the size of individual nanoparticles accurately. Nevertheless the challenging aspect is sample preparation from powder or liquid form on the substrate, so that a homogeneous distribution of well-separated (deagglomerated) particles is attained. The systematic study in this work shows examples where the extraction of the critical, smallest particle dimension - as the decisive particle parameter for the classification as a NM - is possible by analysing the sample after its simple, dry preparation. The consequences of additional typical issues like loss of information due to screening of smaller particles by larger ones or the (in)ability to access the constituent particles in aggregates are discussed. By means of practical examples the inherent statistical evaluation of the particle size is highlighted together with all its pitfalls such as setting of a suitable threshold for delimitation of the particle . T2 - European Microscopy Congress EMC 2016 CY - Lyon, France DA - 28.08.2016 KW - Electron microscopy KW - Nanomaterial KW - Classification KW - Particle size distribution PY - 2016 AN - OPUS4-38258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hetti, M. A1 - Wei, Q. A1 - Casperson, Ralf A1 - Pohl, Rainer A1 - Bartusch, M. A1 - Neu, V. A1 - Pospiech, D. A1 - Voit, B. T1 - Magnetite core-shell nanoparticles in nondestructive flaw detection of polymeric materials N2 - Nondestructive flaw detection in polymeric materials is important but difficult to achieve. In this research, the application of magnetite nanoparticles (MNPs) in nondestructive flaw detection is studied and realized, to the best of our knowledge, for the first time. Superparamagnetic and highly magnetic (up to 63 emu/g) magnetite core-shell nanoparticles are prepared by grafting bromo-end group-functionalized poly(glycidyl methacrylate) (Br-PGMA) onto surface-modified Fe3O4 NPs. These Fe3O4-PGMA NPs are blended into bisphenol A diglycidylether (BADGE) based epoxy to form homogeneously distributed magnetic epoxy nanocomposites (MENCs) after curing. The core Fe3O4 of the Fe3O4-PGMA NPs endows the MENCs with magnetic property, which is crucial for nondestructive flaw detection of the materials, while the shell PGMA promotes colloidal stability and prevents NP aggregation during curing. The eddy current testing (ET) technique is firstly applied to detect flaws in the MENCs. Through the brightness contrast of the ET image, surficial and sub-surficial flaws in MENCs can be detected, even for MENCs with low content of Fe3O4-PGMA NPs (1 wt %). The incorporation of Fe3O4-PGMA NPs can be easily extended to other polymer and polymer-based composite systems and opens a new and very promising pathway toward MNP-based nondestructive flaw detection in polymeric materials. KW - Magnetite nanoparticles KW - Poly(glycidyl methacrylate) KW - Atom transfer radical polymerization KW - Magnetic nanocomposites KW - Nondestructive flaw detection PY - 2016 DO - https://doi.org/10.1021/acsami.6b09934 SN - 1944-8244 SN - 1944-8252 VL - 8 IS - 41 SP - 28208 EP - 28215 PB - American Chemical Society CY - Washington, DC AN - OPUS4-38300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ehlert, Christopher T1 - A detailed assignment of NEXAFS resonances of imidazolium based ionic liquids N2 - In Near Edge X-Ray Absorption Fine Structure (NEXAFS) spectroscopy X-Ray photons are used to excite tightly bound core electrons to low-lying unoccupied orbitals of the system. This technique offers insight into the electronic structure of the system as well as useful structural information. In this work, we apply NEXAFS to two kinds of imidazolium based ionic liquids ([CnC1im]+ [NTf2]− and [C4C1im]+ [I]−). A combination of measurements and quantum chemical calculations of C K and N K NEXAFS resonances is presented. The simulations, based on the transition potential density functional theory method (TP-DFT), reproduce all characteristic features observed by the experiment. Further, a detailed assignment of resonance features to excitation centers leads to a consistent interpretation of the spectra. T2 - 52nd Symposium on Theoretical Chemistry (STC2016) CY - Ruhr Universität Bochum, Germany DA - 26.9.2016 KW - NEXAFS KW - Simulation KW - Ionic liquid PY - 2016 AN - OPUS4-38276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobina, E. A1 - Zimathis, Anett A1 - Prinz, Carsten A1 - Emmerling, Franziska A1 - de Santis Neves, R. A1 - Galhardo, C. E. A1 - De Robertis, E. A1 - WANG, H. A1 - Mizuno, K. A1 - Kurokawa, A. A1 - Unger, Wolfgang T1 - Final report of CCQM-K136 measurement of porosity properties (specific adsorption, BET specific surface area, specific pore volume and pore diameter) of nanoporous Al2O3 N2 - The CCQM-K136 key comparison for determination of the porosity properties of aluminum oxide has been organized jointly by the surface and micro/nano analysis working groups of CCQM to test the abilities of the metrology institutes to measure the porosity properties (specific adsorption, BET specific surface area, specific pore volume and pore diameter) of nanoporous Al2O3. Ural Scientific Research Institute for Metrology (UNIIM) acted as the coordinating laboratory for this comparison with BAM Federal Institute for Materials Research and Testing (BAM) as co-coordinating laboratory. Five NMIs and one DI participated in this key comparison. All participants used a gas adsorption method, here nitrogen adsorption at 77.3 K, for analysis according to the international standards ISO 15901-2 and 9277. KW - BET specific surface area KW - Specific adsorption KW - Pore diameter KW - Specific pore volume KW - Nanoporous Al2O3 PY - 2016 UR - http://iopscience.iop.org/article/10.1088/0026-1394/53/1A/08014 DO - https://doi.org/10.1088/0026-1394/53/1A/08014 SN - 0026-1394 SN - 1681-7575 VL - 2016 IS - 53 Technical Supplement SP - Article 08014, 1 EP - 39 PB - IOPscience AN - OPUS4-38282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph A1 - Kruschwitz, Sabine A1 - Boller, C. A1 - Wiggenhauser, Herbert T1 - Feasibility study on adapting a machine learning based multi-sensor data fusion approach for honeycomb detection in concrete N2 - We present the results of a machine learning (ML)- inspired data fusion approach, applied to multi-sensory nondestructive testing (NDT) data. Our dataset consists of Impact-Echo (IE), Ultrasonic Pulse Echo (US) and Ground Penetrating Radar (GPR) measurements collected on large-scale concrete specimens with built–in simulated honeycombing defects. In a previous study we were able to improve the detectability of honeycombs by fusing the information from the three different sensors with the density based clustering algorithm DBSCAN. We demonstrated the advantage of data fusion in reducing the false positives up to 10% compared to the best single sensor, thus, improving the detectability of the defects. The main objective of this contribution is to investigate the generality, i.e. whether the conclusions from one specimen can be adapted to the other. The effectiveness of the proposed approach on a separate full-scale concrete specimen was evaluated. T2 - NDE/NDT for Highway and Bridges: Structural Materials Technology 2016 CY - Portland, Oregon, USA DA - 29.08.2016 KW - Data fusion KW - Concrete evaluation KW - Honeycombing KW - Machine learning KW - Clustering PY - 2016 SN - 978-1-57117-392-8 SP - 144 EP - 148 PB - The American Society for Nondestructive Testing, Inc CY - Portland, Oregon, USA AN - OPUS4-38288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Feasibility study on adapting a machine learning based multi-sensor data fusion approach for honeycomb detection in concrete N2 - We present the results of a machine learning (ML)- inspired data fusion approach, applied to multi-sensory nondestructive testing (NDT) data. Our dataset consists of Impact-Echo (IE), Ultrasonic Pulse Echo (US) and Ground Penetrating Radar (GPR) measurements collected on large-scale concrete specimens with built–in simulated honeycombing defects. In a previous study we were able to improve the detectability of honeycombs by fusing the information from the three different sensors with the density based clustering algorithm DBSCAN. We demonstrated the advantage of data fusion in reducing the false positives up to 10% compared to the best single sensor, thus, improving the detectability of the defects. The main objective of this contribution is to investigate the generality, i.e. whether the conclusions from one specimen can be adapted to the other. The effectiveness of the proposed approach on a separate full-scale concrete specimen was evaluated. T2 - NDE/NDT for Highway and Bridges: Structural Materials Technology 2016 CY - Portland, Oregon, USA DA - 29.08.2016 KW - Data fusion KW - Concrete evaluation KW - Honeycombing KW - Machine learning KW - Clustering PY - 2016 AN - OPUS4-38289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Iannarelli, L. T1 - Shape engineered TiO2 nanoparticles in Caenorhabditis elegans: a Raman imaging based approach to assist tissue-specific toxicological studies N2 - In vivo detailed spatial distribution of TiO2 NPs was here investigated for the first time using a 2D chemical imaging analysis based on Confocal Raman Spectroscopy. The invertebrate nematode C. elegans was employed as prototypical model of living organism. Rod, bipyramidal and quasi-spherical engineered TiO2 NPs with different primary particle sizes and agglomeration states were prepared, characterized and then administered to nematodes. Exploiting the typical fingerprint of TiO2 in the Raman spectrum, we monitored the biodistribution of NPs inside the worm using a non-invasive, label-free method. The high spatial resolution chemical imaging and the specificity of the Raman technique in the localization of TiO2 NPs helped in the design of behavioral C. elegans studies aimed at elucidating the relationship among the size, shape, and agglomeration state of NPs and their ability to induce specific toxic effects. T2 - 16th European Conference on Applications of Surface and Interface Analysis ECASIA'15 CY - Fortaleza, Brazil DA - 14.08.2016 KW - TiO2 KW - Nanoparticles KW - Raman imaging KW - Toxicological studies PY - 2016 AN - OPUS4-38240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Lazik, D. A1 - Bartholmai, Matthias T1 - Leak detection with linear soil gas sensors under field conditions - First experiences running a new measurement technique N2 - A 400 m² soil test field with gas injection system was built up, which enables an experimental validation of linear gas sensors for specific applications and gases in an application-relevant scale. Several injection and soil watering experiments with carbon dioxide (CO2) at different days with varying boundary conditions were performed indicating the potential of the method for, e.g., rapid leakage detection with respect to Carbon Capture and Storage (CCS) issues. T2 - IEEE Sensors 2016 CY - Orlando, FL, USA DA - 30.10.2016 KW - Soil test field KW - Membrane-based linear gas sensor KW - Leak detection KW - Field conditions PY - 2016 SN - 978-1-4799-8287-5 SN - 1930-0395 SP - B-3-65, 757 EP - 759 PB - IEEE AN - OPUS4-38244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Neumann, Patrick P. T1 - Leak detection with linear soil gas sensors under field conditions - First experiences running a new measurement technique N2 - A 400 m² soil test field with gas injection system was built up, which enables an experimental validation of linear gas sensors for specific applications and gases in an application-relevant scale. Several injection and soil watering experiments with carbon dioxide (CO2) at different days with varying boundary conditions were performed indicating the potential of the method for, e.g., rapid leakage detection with respect to Carbon Capture and Storage (CCS) issues. T2 - IEEE Sensors 2016 CY - Orlando, FL, USA DA - 30.10.2016 KW - Soil test field KW - Membrane-based linear gas sensor KW - Leak detection KW - Field conditions PY - 2016 AN - OPUS4-38247 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fretwurst, T. A1 - Buzanich, Günter A1 - Nahles, S. A1 - Woelber, J. P. A1 - Riesemeier, Heinrich A1 - Nelson, K. T1 - Metal elements in tissue with dental peri-implantitis: a pilot study N2 - Objectives: Dental peri-implantitis is characterized by a multifactorial etiology. The role of metal elements as an etiological factor for peri-implantitis is still unclear. The aim of this study was to investigate the incidence of metal elements in bone and mucosal tissues around dental Grade 4 CP titanium implants with signs of peri-implantitis in human patients. Methods: In this prospective pilot study, all patients were enrolled consecutively in two study centers. Bone and soft tissue samples of patients with peri-implantitis with indication for explantation were analyzed for the incidence of different elements (Ca, P, Ti, Fe) by means of synchrotron radiation X-ray fluorescence spectroscopy (SRXRF) and polarized light microscopy (PLM). The existence of macrophages and lymphocytes in the histologic specimens was analyzed. Results: Biopsies of 12 patients (seven bone samples, five mucosal samples) were included and analyzed. In nine of the 12 samples (75%), the SRXRF examination revealed the existence of titanium (Ti) and an associated occurrence with Iron (Fe). Metal particles were detected in peri- implant soft tissue using PLM. In samples with increased titanium concentration, lymphocytes were detected, whereas M1 macrophages were predominantly seen in samples with metal particles. Conclusion: Titanium and Iron elements were found in soft and hard tissue biopsies retrieved from peri-implantitis sites. Further histologic and immunohistochemical studies need to clarify which specific immune reaction metal elements/particles induce in dental peri-implant tissue. KW - Peri-implantitis KW - Metal elements KW - Synchrotron radiation X-ray fluorescence PY - 2016 DO - https://doi.org/10.1111/clr.12718 SN - 0905-7161 VL - 27 IS - 9 SP - 1178 EP - 1186 PB - WILEY-BLACKWELL CY - 111 RIVER ST, HOBOKEN 07030-5774, NJ USA AN - OPUS4-38641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Unger, Wolfgang T1 - Surfchem - Traceable quantitative surface chemical analysis for industrial applications N2 - The project addresses chemical and topographical metrology at surfaces. The new methodologies of measurements at surfaces will be developed as good practice guides and new work item proposals for industrial ISO standards. The objectives of the Joint research project (JRP) are to provide measurement standards and methods with traceability wherever it is practicable to do so for quantitative surface chemical analysis for industrial applications. KW - Method development KW - Surface chemical analysis KW - Analytical methods KW - Reference material PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-386319 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schukar, Vivien A1 - Gong, Xin A1 - Hofmann, Detlef A1 - Basedau, Frank A1 - Köppe, Enrico A1 - Bartholmai, Matthias A1 - Westphal, Anja A1 - Sahre, Mario A1 - Beck, Uwe ED - Berghmans, F. ED - Mignani, A. G. T1 - Modelling and simulation of a fibre Bragg grating strain sensor based on a magnetostrictive actuator principle N2 - A new concept for the self-diagnosis of embedded fiber Bragg grating (FBG) strain sensors was developed, simulated and experimentally tested. This concept is based on a magnetostrictive metallic layer directly coated on the fibre cladding over the grating segment of the FBG sensor, so that an on-demand external magnetic field in a millitesla scale can produce a controllable artificial strain as an indication signal for the remote optical interrogator. The relationship between the pre-defined magnetic field and its induced Bragg wavelength shift characterizes this validation concept. Any deviation of the local bonding state of the interfaces from the initial or/and any change of shear strain transferring mechanism from composite matrix to the optical fibre core will result in alterations in this sensitive relationship, and thus triggers an immediate alert for a further inspection. The finite element method is used to simulate the strain of this configuration as result of different values of the magnetic field in order to optimize the geometrical sensor parameters. The simulations are verified by experiments results. © (2016) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE). Downloading of the abstract is permitted for personal use only. T2 - Optical Sensing and Detection IV CY - Brüssel, Belgium DA - 03.04.2016 KW - Fiber Bragg gratings KW - Actuators KW - Modeling and simulation KW - Finite element methods PY - 2016 SN - 9781510601444 DO - https://doi.org/10.1117/12.2224728 SN - 0277-786X SN - 1996-756X VL - 9899 SP - 9899-39 PB - SPIE Digital Library AN - OPUS4-38634 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Zientek, Nicolai A1 - Rump, Doreen A1 - Fischer, Franziska A1 - Maiwald, Michael A1 - Emmerling, Franziska T1 - Make and break - Facile synthesis of cocrystals and comprehensive dissolution studies N2 - Mechanochemistry is increasingly used as a ‘green alternative’ for synthesizing various materials including pharmaceutical cocrystals. Herein, we present the mechanochemical synthesis of three new cocrystals containing the API carbamazepine (cocrystals CBZ:Indometacin 1:1, CBZ:Benzamide 1:1, and CBZ:Nifedipine 1:1). The mechanochemical reaction was investigated in situ documenting a fast and complete reaction within one minute. Online NMR spectroscopy proved the direct influence of the dissolution behaviour of the coformers to the dissolution behaviour of the API carbamazepine. The dissolution behaviour of the organic cocrystals is compared to the behaviour of the pure drug indicating a general applicability of this approach for detailed cocrystal dissolution studies. KW - Cocrystals KW - Carbamazepine KW - Mechanochemistry KW - Powder diffraction KW - Online NMR spectroscopy PY - 2017 DO - https://doi.org/10.1016/j.molstruc.2016.11.063 SN - 0022-2860 SN - 1872-8014 VL - 1133 SP - 18 EP - 23 AN - OPUS4-38664 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koegler, M. A1 - Paul, Andrea A1 - Alborch, K. P. A1 - Birkholz, M. A1 - Junne, S. A1 - Neubauer, P. T1 - Raman on-line monitoring approach for bioprocess and bio-pharmaceutical manufacturing N2 - There is a high demand of monitoring in the era of QbD in industrial scale require new approaches to gain data rapidly and of sufficient quality in real time. Raman spectroscopy technology has great potential but not yet shown it fully in process on-line monitoring due to limitations such as i) uncomplete separation between cells and growth media alone, ii) general weak Raman signals of analytes in complex solutions and iii) strong background signals such as the auto-fluorescence, cosmic rays and surrounding lights overlapping the weak Raman signals. Here we demonstrate a Proof-of-Concept on an the example lactic acid bacteria process using a Streptococcus thermophiles fermentation. Results from three different Raman approaches are presented: 1) Time-Gated Raman Spectroscopy (TG-Raman), 2) Surface Enhanced Raman Spectroscopy (SERS) and 3) Raman process spectroscopy with NIR excitation combined with multivariate data analysis (MVDA) using Principal Component Analysis (PCA) and Partial Least Squares Regression (PLSR). T2 - 12. Kolloquium Arbeitskreis Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Raman KW - Chemometrics KW - SERS KW - TimeGate PY - 2016 SP - 91 EP - 93 CY - Berlin AN - OPUS4-38673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kern, Simon A1 - Meyer, Klas A1 - Maiwald, Michael T1 - NMR-Spektroskopie im Feld - Eine neue Online-Methode für die Prozesskontrolle N2 - Flexible, modulare Produktionsanlagen auf der Basis von verfahrenstechnischen Teilmodulen stellen einen vielversprechenden Ansatz für die kontinuierliche Produktion von Fein- und Spezialchemikalien dar. Der Schwerpunkt des Horizont-2020-Projekts der Europäischen Kommission CONSENS (Integrated Control and Sensing) liegt in der Implementierung von innovativen Sensorkonzepten zur Prozessüberwachung und -regelung innerhalb von containerbasierten modularen Produktionsan lagen. In diesem Artikel wird die Feldintegration eines Online-NMR-Sensors als smartes Modul für die Prozesskontrolle beschrieben. Dieses Modul basiert auf einem kommerziell erhältlichen Niederfeld-NMRSpektrometer, das zurzeit für die Anwendung im Laborbereich erhältlich ist. Für die Feldintegration wurde ein ATEX-zertifiziertes, explosionsgeschütztes Gehäuse entwickelt sowie Automationsschemen für den unbeaufsichtigten Betrieb und für die spektrale Datenauswertung erstellt. Nachdem die Machbarkeit und Leistungsfähigkeit des Sensorkonzeptes in Laborexperimente an einer aromatischen Substitutionsreaktion bereits erfolgreich demonstriert wurde, ist die Inbetriebnahme des NMR-Sensormoduls in industrieller Umgebung für 2017 geplant. KW - Prozessanalytik KW - Reaction monitoring KW - Industrie 4.0 KW - Online-NMR-Spektroskopie KW - CONSENS KW - Prozess-Sensoren PY - 2016 SN - 2190-4111 VL - 58 IS - 12 SP - 21 EP - 25 PB - DIV Deutscher Industrieverlag GmbH CY - München AN - OPUS4-38675 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauli, Jutta A1 - Pochstein, Marieke A1 - Haase, A. A1 - Napp, J. A1 - Luch, A. A1 - Resch-Genger, Ute T1 - Influence of label and charge density on the association of the therapeutic monoclonal antibodies trastuzumab and cetuximab conjugated to anionic fluorophores N2 - The design of bright and functional dye–protein conjugates requires hydrophilic and stable fluorophores with high molar absorption coefficients and high fluorescence quantum yields,which must not be prone to dimerization, as well as conservation of protein function and suppression of protein association. Although many synthetic dyes meet these needs, the influence of dye charge on bioconjugate performance is commonly neglected. This encouraged us to assess the spectroscopic properties, antibody functionality, binding behavior, folding, and association of conjugates of the therapeutic antibodies trastuzumab and cetuximab with the red cyanine dyes S0586, S2381,and 6SIDCC (bearing two, three, and six sulfonate Groups respectively. Our results demonstrate a negligible effect of dye labeling on antibody folding, yet a strong influence of Label charge and density on antibody isoelectric points and association.Especially 6SIDCC decreased strongly the isoelectric points of both antibodies and their heavy or light chains even at low labeling degrees, thus favoring protein association. Although an increasingly negative dye charge reduces Antigen affinity as shown in a competitive immunoassay, all conjugates still bound to cells overexpressing the target of the respective antibody. Obviously, dyes that cause minimum dimerization with a small number of charged groups are best for conjugate brightness, minimum protein association, and strong target binding. This underlines the need to consider dye Charge for the rational design of conjugates with Optimum performance. KW - Fluorophore KW - Antibody KW - 2D gel electrophoresis KW - Isoelectric point KW - Protein association PY - 2016 DO - https://doi.org/10.1002/cbic.201600299 SN - 1439-7633 SN - 1439-4227 VL - 18 IS - 1 SP - 101 EP - 110 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-38573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Applicability of CCQM-P149 to support CMCs N2 - The presentation describes the limitations of CCQM-P149 to be used for supporting CMCs and it gives possibilities and applications where CCQM-P149 can provide additional Support. T2 - CCQM IAWG Meeting CY - Daejeon, South Korea DA - 04.10.2016 KW - CCQM KW - CMC KW - Purity assessment PY - 2016 AN - OPUS4-38586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fittschen, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Böttger, S. A1 - Rosenberg, D. A1 - Menzel, M. A1 - Jensen, W. A1 - Busker, M. A1 - Gotlib, Z. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Wobrauschek, P. A1 - Streli, C. ED - de Oliveira Guilherme Buzanich, Ana T1 - A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline N2 - An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml⁻¹ to μg ml⁻¹). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NISTwater 1640. Low limits of detection of less than 100 fg absolute (10 pg ml⁻¹) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state. KW - TXRF KW - TXRF-XANES KW - Sample changer KW - BAMline KW - Re-XANES PY - 2016 DO - https://doi.org/10.1107/S1600577516001995 SN - 1600-5775 VL - 23 IS - 3 SP - 820 EP - 824 PB - International Union of Crystallography AN - OPUS4-38656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwarz, F. A1 - Heinrich, Thomas A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Schalley, C. T1 - A photoswitchable rotaxane operating in monolayers on solid support N2 - A novel photoswitchable rotaxane was synthesised and its switching behaviour in solution was analysed with NMR and UV-Vis. A monolayer of rotaxanes was deposited on glass surfaces and the on-surface photoswitching was investigated. Angle-resolved NEXAFS spectra revealed a preferential orientation that reversibly changes upon switching. KW - XPS KW - NEXAFS KW - Photoswitchable rotaxane KW - Self assembly PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-386814 DO - https://doi.org/10.1039/c6cc08586e SN - 0022-4936 SN - 1364-548X SN - 0009-241x SN - 1359-7345 VL - 52 IS - 100 SP - 14458 EP - 14461 PB - Royal Society of Chemistry (RSC) AN - OPUS4-38681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - NEXAFS and XPS analysis of functionalized graphene surfaces for bio applications N2 - Graphene prepared from Graphene oxide (GO) is used as a platform for functional 2D nanomaterials with diverse applications ranging from bios ensors to antimicrobial surfaces. C and N K-edge NEXAFS and XPS spectroscopies at BESSY’s HE-SGM beamline have been used to prove and control covalent functionalization of graphenic materials at ambient conditions for the synthesis of functional 2D-surfaces. T2 - 8th Jouint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 7.12.2016 KW - XPS KW - NEXAFS KW - Graphene PY - 2016 AN - OPUS4-38683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - MetVBadBugs - XRF and NAP-XPS characterization of drug uptake in multi-resistant bacteria N2 - Multi-resistant bacteria embedded in infectious biofilms are one of the largest future threats in human healthcare. The mechanism of drug uptake and the origin of resistancy is quantitatively not well characterized and understood. Modern X-ray and synchrotron excited spectroscopic methods like XRF and NAP-XPS under ambient pressure conditions and liquid media will add new insights into this field. T2 - 8th Jouint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 7.12.2016 KW - XPS KW - XRF KW - Biofilm PY - 2016 AN - OPUS4-38684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Nele T1 - Nuclease activity of copper(II)phenanthroline complexes immobilized on silicon nitride films N2 - Copper(II)phenanthroline complexes intercalate into DNA and induce DNA cleavage. Here, we investigate the nuclease activity of copper(II)phenanthroline complexes on Silicon nitride films. 1,10-phenanthroline-5-carboxylic acid is immobilized at Si-NHx bonds via amide coupling followed by the formation of copper(II)phenanthroline complexes. XPS and NEXAFS were carried out at the HE-SGM beamline. T2 - 8th Jouint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 7.12.2016 KW - XPS KW - NEXAFS KW - Copper(II) - phenanthroline - complexe filmss PY - 2016 AN - OPUS4-38685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Seewald, G. T1 - 2PM FlySCAN: Innovative approach for wide field high resolution imaging of skin tissue volumes N2 - Two Photon Microscopy (2PM) is an innovative Technology for high resolution imaging of human skin in vivo and ex vivo. Up to now the method is limited by its interdependence between the field of view and the attainable resolution. The new FlySCAN Technology overcomes these boundaries and enable images sizes of many millimeters by resolutions in the submicrometer range revealing very specific information on clinically and biologically relevant tissue and cell structures. The advantages of the new approach are demonstrated by excellent in vivo and ex vivo tissue images. T2 - EPIC Biophotonics Workshop “Translating Biophotonics Technologies to Clinical Oncology: Perspectives & Challenges” CY - Paris, France DA - 01.12.2016 KW - Two photon microscopy KW - Wide field KW - Skin tissue PY - 2016 AN - OPUS4-38687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Neuartige Wandler für Luftultraschallprüfung N2 - Es werden die neuesten Wandler für Luftultraschallprüfung dargestellt. Sie basieren auf zellulären Kunststoffen und auf dem thermoakustischen Prinzip. Zu den typischen Anwendungen gehört die Prüfung von Verbundwerkstoffen und Klebeverbindungen. T2 - DGZfP Arbeitskreis Dresden CY - Dresden, Germany DA - 22.9.2016 KW - Thermoakustik KW - Zelluläres Polypropylen KW - Luftultraschall KW - Zerstörungsfreie Prüfung PY - 2016 AN - OPUS4-38688 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Philipp, Rosemarie T1 - Traceable measurements for monitoring critical pollutants under the European Water Framework Directive (WFD) 2000/60/EC N2 - The European Water Framework Directive (WFD) 2000/60/EC specifies a list of 33 priority water pollutants. For these substances, Environmental Quality Standards (EQS), equivalent to the maximum allowable concentrations, had been defined at very low levels. EQS values refer to the whole water body, i.e. include contaminants which are associated to suspended solids or colloids present in the natural water. For several priority pollutants primary analytical methods capable of measuring the target analytes at EQS level in natural water are still missing. The project has developed and validated such methods for three selected compounds, namely Tributyltin (TBT), Polybrominated Diphenylether (PBDE) and Polycyclic Aromatic Hydrocarbons (PAH). KW - Water polluntants KW - Monitoring KW - Water analysis KW - Tributyltin KW - Polybrominated diphenylether KW - Polycyclic aromatic hydrocarbons PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-386230 SP - 1 EP - 3 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Roadmap for purity determination N2 - A Roadmap for the purity Determination of pure metallic elements is presented. The roadmap distinguishes between different approaches for the purity determination and list theindividual steps for each Approach which are necessary to successfully apply These approaches. T2 - CCQM IAWG Meeting CY - Daejeon, South Korea DA - 04.10.2016 KW - Traceability KW - Purity determination PY - 2016 AN - OPUS4-38590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Development of an online-analysis technique for the determina-tion of plant essential nutrients in soils using XRF and LIBS N2 - The main task of BAM in the I4S project is the development of online analytics for reliable monitoring of major and minor nutrients like K, P, Ca in soil using mobile-XRF (X-ray fluorescence spectroscopy) and mobile-LIBS (laser-induced breakdown spectroscopy). Each method provides fast and simultaneous multi-element analyses which are neccessary for mapping agricultural cropland. The first objective was to design a combined measurement setup for XRF and LIBS. The centerpiece is the rotatable sample plate which enables the measurement of moving samples. Current steps are the optimisation of the parameters for the analysis of soils. T2 - 12. Kolloquium Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - RFA KW - Agricultural KW - LIBS KW - Online KW - Soil KW - Monitoring PY - 2016 AN - OPUS4-38591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Establishment of reference values for sensor based soil analysis N2 - Production of soil reference materials (for project partners) is integrated into the project „X-ray fluorescence, laser-induced breakdown spectroscopy (and Raman spectroscopy) as tools for a site-specific management of soil fertility“. BAM provides good analytics which is necessary for measuring the right values. Why is it important to have reference values? They enable the connection of own measuring results to the SI (international system of units) and the comparison with results from other laboratories. The soil reference materials are also needed for the calibration of the matrix dependent methods laser-induced breakdown spectroscopy (LIBS) and X-ray fluorescence analysis (XRF). For the production of soil reference materials different steps are required, for example drying, sieving and homogenisation. T2 - BonaRes Statusseminar CY - Leipzig, Germany DA - 14.11.2016 KW - LIBS KW - Reference KW - Homogenisation KW - Calibration KW - RFA KW - Soil PY - 2016 AN - OPUS4-38593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Büchele, Dominique T1 - Mobile-XRF and -LIBS analysis of soils N2 - The main task of BAM in the I4S project is the development of online analytics for reliable monitoring of major and minor nutrients like K, P, Ca in soil using mobile-XRF (X-ray fluorescence spectroscopy) and mobile-LIBS (laser-induced breakdown spectroscopy). Each method provides fast and simultaneous multi-element analyses which are neccessary for mapping agricultural cropland. The first objective was to design a combined measurement setup for XRF and LIBS. The centerpiece is the rotatable sample plate which enables the measurement of moving samples. Current steps are the optimisation of the parameters for the analysis of soils. T2 - BonaRes Statusseminar CY - Leipzig, Germany DA - 14.11.2016 KW - RFA KW - Agricultural KW - LIBS KW - Online KW - Soil KW - monitoring PY - 2016 AN - OPUS4-38594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Zwei neue Normprojekte für die Instrumentierte Eindringprüfung: „Linear elastische dynamische Eindringprüfung“ und Eindringkriechen und zeitabhängige Eigenschaften N2 - Mechanische Eigenschaften von Materialien im Mikro- und Nanobereich werden heute mit der Instrumentierten Eindringprüfung bestimmt. Das Verfahren ist bereits umfangreich in der DIN EN ISO 14577 Teil 1-4 genormt. Im Ergebnis des EU EMRP Projekts Dynamic mechanical properties and long-term deformation behavior of viscous materials (MEPROVISC)“ wurden die zwei neuen Normprojekte für die Instrumentierte Eindringprüfung „Linear elastische dynamische Eindringprüfung“ und „Eindringkriechen und zeitabhängige Eigenschaften“ vorgeschlagen und mit deren Bearbeitung im ISO/TC 164/SC3 Hardness Testing begonnen. Ausgehend von der Darstellung der wesentlichen Ergebnisse des Projekts MEPROVISC werden die Grundzüge der neuen Normen in Bezug auf Kalibrierung, Methodik, Auswertung und Bestimmung der Messunsicherheit erläutert. Weiterhin werden die Möglichkeiten der aktiven Mitarbeit an diesen Normprojekten aufgezeigt. T2 - Tagung Werkstoffprüfung 2016 CY - Neu-Ulm, Germany DA - 01.12.2016 KW - Instrumentierte Eindringprüfung KW - Dynamische Materialeigenschaften KW - Kriechen KW - Normung PY - 2016 AN - OPUS4-38597 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael ED - Maiwald, Michael T1 - Trends in der Prozessanalytik N2 - Aktuell wird von der Prozessindustrie die Weiterentwicklung einiger Messaufgaben und Technologien als sehr bedeutend eingeschätzt. Dazu zählen Infrarot-Kaskadenlaser, die Online-Analyse von Partikeln und Emulsionen, neuartige NIR/MIR-Spektroskopiemodule und deren Miniaturisierung sowie die Weiterentwicklung und Kostenvergünstigung der Raman-Spektroskopie. Heute wie morgen müssen Prozess-Sensoren zuerst die Aufgabe des robusten Messens und der Generierung von Prozessinformationen erfüllen. KW - Prozessanalytik KW - Sensoren KW - Trends KW - Process Analytical Technology PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/cite.201690036/full DO - https://doi.org/10.1002/cite.201690036 SN - 0009-286X VL - 88 IS - 6 SP - 683 EP - 683 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-38090 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkelmann, Aimo A1 - Nolze, Gert T1 - Channeling-enhanced EDX for polarity resolved crystal orientation determination N2 - Using channeling-enhanced energy-dispersive X-ray spectroscopy (EDX), we demonstrate polarity sensitive orientation determination of a non-centrosymmetric crystal in the scanning electron microscope. The authors observe a characteristic asymmetry in the channeling-enhanced, angle-dependent EDX data of a GaAs sample, which is in good agreement to simulations using the dynamical theory of diffraction for the incident electron beam. This allows us to assign the orientation of the GaAs crystal according to the non-centrosymmetric point group. The method shown here overcomes the limitation of a reduced point-group sensitivity of electron backscatter diffraction Patterns and electron channeling patterns for crystalline phases that contain atoms of approximately equal electron scattering cross sections. KW - Channeling KW - EDX KW - EDS KW - Composition KW - GaAs KW - GaP PY - 2016 DO - https://doi.org/10.1002/crat.201600258 SN - 0232-1300 SN - 0023-4753 VL - 51 IS - 12 SP - 752 EP - 756 AN - OPUS4-38098 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert T1 - Interphase boundary characterization in duplex steel and iron meteorites using EBSD technique N2 - The properties of materials are mainly described by the orientation distribution of the crystalline phases in a material. Beside the so considered anisotropy also the grain as well as phase boundaries are of extreme importance for a whole string of properties, e.g. the strength of a material. On the example of the interface between fcc and bcc iron the discovered and derived models are discussed. Although the common models are based on the crystal lattice description, the atomic configuration on the interface is analysed. Since experimentally a wide spread of orientations data appears the consideration of the frequency distribution is proposed to find at least the main orientation relationship between fcc and bcc. High-indexed pole figures as well as the Euler subspace are introduced in order to increase the accuracy and to compare different measurements. For the sake of simplicity EBSD measurements on iron meteorites are used since they commonly consist of large fcc single crystals which transformed to a low and very specific number of bcc grains. In special cases the described procedure could also be used for steels. KW - Orientation relationships KW - Electron backscatter diffraction KW - Steel KW - Iron meteorites KW - Kurdjumov-Sachs KW - Nishiyama-Wassermann PY - 2006 SN - 1733-3490 SN - 0004-0770 SN - 0860-7052 VL - 51 IS - 1 SP - 15 EP - 22 AN - OPUS4-38030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Glowacka, A. A1 - Wozniak, M. J. A1 - Nolze, Gert A1 - Swiatnicki, W. A. T1 - Hydrogen induced phase transformations in austenitic-ferritic steel N2 - The hydrogen influence on the microstructure of the austenitic-ferritic Cr22-Ni5-Mo3 stainless steel was investigated. Cathodic hydrogen charging was performed electrochemically from aqueous solution of 0.1M H2SO4 with hydrogen entry promoter addition. The aim of this study was to reveal microstructural changes appearing during the hydrogen charging and particularly to clarify the occurrence of phase transformations induced by hydrogen. The specific changes in both phases of steel were observed. In the ferritic phase, strong increase of dislocation density was noticed. Longer time of hydrogen charging leaded also to the strips and twin plates formation in ferrite phase. In the austenitic phase, the generation of stacking faults, followed by the formation of α' martensite was remarked. KW - Steel KW - Hydrogen KW - Embrittlement KW - Electron backscatter diffraction KW - SEM PY - 2006 DO - https://doi.org/10.4028/www.scientific.net/SSP.112.133 SN - 1662-9779 VL - 112 SP - 133 EP - 140 AN - OPUS4-38031 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Geist, V. T1 - A new method for the investigation of orientation relationships in meteoritic plessite N2 - The orientation relationship (OR) between the bcc and fcc phase in the plessite microstructure of the iron meteorites Watson, Agpalilik and Gibeon has been analysed in a scanning electron microscope using electron back-scattered diffraction (EBSD). A very strong OR exists, independently on the analysed plessite type and the observed spreading of single orientation data. The agreement between the experimental orientation distribution and existing models varies for each meteorite. The black plessite in the Agpalilik corresponds to the Nishiyama-Wassermann model whereas the Duplex plessite of the Gibeon meteorite shows an OR close to the Kurdjumov-Sachs model. The Watson meteorite is strongly deformed so that a general OR is difficult to determine due to the blurred experimental orientation distribution. KW - Meteorite KW - Orientation relationship KW - Steel KW - Electron backscatter diffraction KW - Kurdjumov-Sachs KW - Nishiyama-Wassermann PY - 2004 DO - https://doi.org/10.1002/crat.200310193 SN - 0023-4753 SN - 0232-1300 VL - 39 IS - 4 SP - 343 EP - 352 AN - OPUS4-38032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraus, Werner A1 - Nolze, Gert T1 - POWDER CELL-A Program for the representation and manipulation of crystal structure and calculation of the resulting X-ray powder pattern N2 - The main component of this program is a simultaneous representation of the unit cell and the calculated powder pattern. It allows the manipulation of the Crystal structure by moving selected atoms of the asymmetric unit. The resulting powder pattern can be directly compared to experimental data in order to obtain reliable starting values for further computations in refinement programs. KW - XRD KW - Simulation KW - PowderCell KW - Programming KW - Crystal structure KW - Refinement PY - 1996 SN - 0021-8898 VL - 29 SP - 301 EP - 303 AN - OPUS4-38033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Nolze, Gert ED - Sen Gupta, S. P. ED - Chatterjee, P. T1 - PowderCell : a mixture between crystal structure visualizer, simulation and refinement tool N2 - The program PowderCell is a crystallographic tool for visualization of Crystal structures. However, it offers also non-conventional features like the fulautomatical generation of subgroups or the consideration of non-standard settings of space-group types. On the one Hand the program is very useful for non-crystallographers who like to get an impression of the atomic arrangement within the unit cell. But also for crystallographers it is recommendable because it contains a lot of additional information which can be extracted and used like data given in the International Tables for Crystallography, Vol. A. However, the most important advantage of the program is the simultaneous calculation of the X-ray or neutron diffraction powder patterns for a mixture of up to 10 crystalline phases. Between more than 7 different characteristic radiations can be chosen and their influence on the resulting powder pattern can be studied. Furthermore, experimental diffractograms can be analysed using a refinement procedure. The implemented LeBail-algorithm allows the investigation of unknown phases. In combination with the refinement algorithm an interface to Shelx offers the possibility for a step by step ab initio structure analysis. Certainly, the user-friendly shell is one reason that especially users who are not so familar with space-group symmetry, crystal structure data or diffractometry use this powerful tool for the solution of scientific or analytical problems as well as in teaching. KW - XRD KW - Simulation KW - Crystal structure KW - Neutron diffraction PY - 2002 SN - 8177642626 SN - 9788177642629 SP - 146 EP - 155 PB - Allied Publishers CY - Kolkata, India AN - OPUS4-38035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Nolze, Gert ED - Sen Gupta, S. P. ED - Chatterjee, P. T1 - The determination of residual stress N2 - X-ray stress analysis on crystalline materials is based on the determination of elastic lattice strains. The strains described by the shift of peak positions are converted to stresses by the means of theory of elasticity. The development of the sin2ψ-method of X-ray stress analysis introduced an enormous progress in X-ray stress analysis during the last decades. This report outlines some important elements of X-ray physics and fundamentals of theory of elasticity. The Standard measuring procedure are described and special experimental differences to the common powder diffractometry are outlined. KW - XRD KW - Residual stress PY - 2002 SN - 81-7764-262-6 SN - 9788177642629 SP - 77 EP - 83 PB - Allied Publishers CY - Kolkata, India AN - OPUS4-38036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Kraus, Werner T1 - PowderCell 2.0 for Windows N2 - PowderCell contains a comfortable, user friendly visualization and modification tool for crystal structures. It provides on-line calculation of the corresponding powder diffraction patterns simulating a variety of experimental conditions. The common ICSD and Shelx file formats are supported for importing crystal structure information. It has control of automatic cell transformation and also derivation of subgroups. More than 740 different settings of the 230 space-group types are supported. Up to ten crystal structures can be considered simultaneously. A full pattern refinement enables the direct comparison with experimental diffractograms for quantitative phase analysis, lattice parameter refinement, polynomial background estimation, etc. KW - XRD KW - Simulation KW - Powdercell KW - Software KW - Programming KW - Phase mixtures KW - Crystal structure KW - Subgroup PY - 1998 SN - 0885-7156 VL - 13 IS - 4 SP - 256 EP - 259 PB - Cambridge University Press AN - OPUS4-38037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maierhofer, Christiane A1 - Röllig, Mathias A1 - Krankenhagen, Rainer A1 - Myrach, Philipp T1 - Comparison of quantitative defect characterization using pulse-phase and lock-in thermography N2 - Using optical excitation sources for active thermography enables a contactless, remote, and non-destructive testing of materials and structures. Currently, two kinds of temporal excitation techniques have been established: pulse or flash excitation, usingmostly flash lamps; and periodic or lock-in excitation, using halogen lamps, LED, or laser arrays. From the experimental point of view, both techniques have their advantages and disadvantages. Concerning the comparison of the testing results of both techniques, only very few studies have been performed in the past. In this contribution, the phase values obtained at flat bottom holes in steel and CFRP and the spatial resolution measured at crossed notches in steel using flash and lock-in excitation are compared quantitatively. KW - Nondestructive testing KW - Thermal imaging KW - Infrared imaging KW - Phase measurement KW - Metals KW - Polymers PY - 2016 DO - https://doi.org/10.1364/AO.55.000D76 SN - 1559-128X SN - 0003-6935 SN - 1539-4522 VL - 55 IS - 34 SP - D76 EP - D86 PB - Optical Society of America (OSA) CY - Washington, DC AN - OPUS4-38184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Broadband dielectric spectroscopy as an orthogonal tool to mechanical analysis – From theory to applications N2 - The basics of broadband dielectric spectroscopy were introduced in detail. The analysis of the data was discussed. As application of broadband dielectric spectroscopy the alpha-relaxation (dynamic glass transition), the chain dynamics of polymers, and the behavior of a high performance polymer were illustrated. T2 - Geesthachter Polymertage CY - Geesthcht, Germany DA - 08.11.2016 KW - Broadband dielectric spectroscopy PY - 2016 AN - OPUS4-38185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madkour, Sherif T1 - Evidence of a three-layred structure in ultrathin PVME and PVME-PS blend films by nanosized relaxation spectroscopy N2 - In the course of miniaturizing modern technology down to the molecular scale, much remain unknown about the materials behavior and the deviations from the bulk that might arises from confinement effects. Here, a combination of nano-sized relaxation spectroscopies (Broadband dielectric spectroscopy (BDS) and Specific heat spectroscopy (SHS); employing AC nanochip calorimetry) were utilized to investigate the glassy dynamics of ultra-thin films of Poly (vinyl methyl ether) (PVME) and of blends PVME / Polystyrene (PS) 50:50 wt-%,, which are miscible in bulk (thicknesses: ca. 8 nm – 160 nm, film thickness was controlled by ellipsometry, film topography by AFM). Both methods are sensitive to different probes; where SHS senses entropy fluctuations while BDS measures dipole fluctuations. For BDS measurements, a recently developed nano-structured electrode sample arrangement is employed, where ultra-thin films are spin-coated on an ultra-flat highly conductive silicon wafer, sandwiched between a wafer with nanostructured SiO2 nano-spacers with heights between 35 nm and 70 nm. For PVME films, two thickness independent processes were observed and interpreted to be the α-processes of a bulk-like layer and a process due to an absorbed layer to the substrate. This adsorbed layer further undergoes a confinement effect that results in the localization of the segmental dynamics, which results in an Arrhenius-like temperature dependence. A detailed analysis of the dielectric strengths of both processes reveals that the thickness of the adsorbed layer decreases with increasing temperature, while that of the bulk-like layer increases. For the blend system, by measuring the dynamic Tg in dependence of the film thickness, SHS showed that the Tg of the whole film was strongly influenced by a nanometer-thick surface layer at the polymer/air interface due to a self-assembling process. The dynamic Tg obtained from the SHS measurements decreased with decreasing film thickness. On the other hand, BDS measurements showed a completely different behavior. At high temperatures, the temperature dependence of the relaxation times of the films follows that of bulk-like PS/PVME; obeying the VFT-law. With decreasing temperature, the temperature dependence deviates from the VFT to an Arrhenius law; where the apparent activation energy decreases with decreasing film thickness. This is the first example where confinement induced changes were observed by BDS for ultra-thin films. All results were analyzed in detail in a comprehensive discussion. T2 - Polydays 2016 CY - Potsdam, Germany DA - 28.09.2016 KW - Ultra-Thin films PY - 2016 AN - OPUS4-38188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rothbart, Nick A1 - Maierhofer, Christiane A1 - Goldammer, M. A1 - Hohlstein, F. A1 - Koch, J. A1 - Kryukov, I. A1 - Mahler, G. A1 - Stotter, B. A1 - Walle, G. A1 - Oswald-Tranta, B. A1 - Sengebusch, M. T1 - Probability of detection analysis of round robin test results performed by flash thermography N2 - Within the scope of a standardisation research project, a flash thermography round robin test that evaluates reliability, comparability and efficiency of different testing situations was performed. Data recorded at metal test specimens with flat bottom holes (FBHs) were analysed by calculating the signal-to-noise ratio (SNR) of the defect signatures in the thermograms as well as in the phase images as a function of defect parameters. A new multi-parameter probability of detection (POD) model was developed, where an â versus a continuous signal analysis was based on the linear relationship between the SNR and a multi-parameter a. This linear relationship was verified by comparison to data obtained from an analytical model that is considering lateral thermal heat diffusion as well as to data obtained by numerical simulation. The resulting POD curves for the thermograms and phase images give an estimation for the detectability of the FBHs with known geometry in steel using different equipment and obtained by different participants. By comparing the SNRs of FBHs with similar geometries, this POD model was transferred to aluminium and copper as well. KW - Active thermography KW - Flash excitation KW - Signal-to-noise ratio KW - Round robin test KW - Multi-parameter POD PY - 2016 UR - http://www.tandfonline.com/doi/full/10.1080/17686733.2016.1229246 DO - https://doi.org/10.1080/17686733.2016.1229246 SN - 1768-6733 SN - 2116-7176 VL - 14 IS - 1 SP - 1 EP - 23 PB - Taylor and Francis CY - Abingdon, UK AN - OPUS4-38192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Ritz-Test: Evaluierung und Stand der Normung N2 - Der Vortrag widmet sich dem „RITZ-TEST: EVALUIERUNG UND STAND DER NORMUNG“ und beschreibt die Komponenten, Ergebnis und Messgrößen, nicht registrierende Prüfgeräte, Evaluierung Ritz-Test (Makrobereich), den Atlas der Versagensformen, Geräte für den instrumentierten Ritz-Test und die Normung des Ritz-Tests (ASTM) zur Bewertung der Haftfestigkeit“ im Einzelnen. T2 - EFDS, 17. Wörlitzer Workshop "Schichthaftung - Anwendungsbeispiele aus der Praxis" CY - Oranienbaum-Wörlitz, Germany DA - 06.06.2016 KW - Kratzfestigkeit KW - Haftfestigkeit KW - Ritztest KW - Instrumentierte Eindringprüfung KW - Normung PY - 2016 AN - OPUS4-38105 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kormunda, M. A1 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Beck, Uwe A1 - Sebik, M. A1 - Esser, N. T1 - Preparation of pulsed DC magnetron deposited Fe-doped SnO2 coatings N2 - Iron-doped SnO2 coatings were deposited in a 50 kHz DC-pulsed magnetron sputtering discharge. The pulses had a duration of 4 µs in selected gas mixtures from pure argon up to 60% of oxygen at a constant total pressure of 0.2 Pa. A single target of SnO2 with Fe inset was used. The mass spectrometry study detected the gas-related ions Ar+, O2+ and O+, where the last one becomes the dominant positive ion at higher oxygen contents. Atomic oxygen ions had a higher energy as it resulted from the collision-caused dissociation on the target surface. The tin-related species were detected as Sn+ and SnO+. SnO2+ species were not detected. The deposition rate decreased by using gas mixtures with oxygen as well as the corresponding amount of Sn-related species in the plasma. The increase of oxygen also increased significantly the sheet resistance of the films. The XPS study showed that the iron concentration decreased by using additional oxygen. But the O/Sn ratio in the coatings was constant, contrary to the increased FeO/Fe ratio in the films. An additional analysis of the coatings by spectroscopic ellipsometry has shown a dependence of the polarizability and the permittivity on the amount of oxygen used during the deposition. In contrast, the study has found no such dependence for the absorption of the layers. KW - Coatings KW - Magnetron sputtering KW - Optical properties KW - Sheet resistivity KW - SnO2 PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/pssa.201532882/full DO - https://doi.org/10.1002/pssa.201532882 SN - 0031-8965 SN - 1862-6300 VL - 213 IS - 9 SP - 2303 EP - 2309 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-38106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosu, Dana-Maria T1 - The accuracy and reproducibility in thickness determination of thin films using SE N2 - Maintaining a consistent product quality is critical for the thin film industry. Therefore, the development of highly accurate protocols able to detect variations and nonidealities in manufactured thin film devices is essential and helps improve production quality and decrease manufacturing costs. The present work will discuss the accuracy and reproducibility in the determination of the thickness of thin films relevant for optoelectronic industry using spectroscopic ellipsometry, starting with the importance of set-up calibration, the need for very well defined calibration standards suitable for real devices and not least, the importance of accurate data analysis. As ellipsometry is an indirect method and theoretical modelling is needed to obtain the desired information regarding the investigated samples (e.g. thickness, roughness, optical constants), the model uncertainty has to be discussed and taken into account. If for ideal samples consisting of single layers with well-known optical constants the determination of thickness and roughness is straight forward and pretty accurate, for real samples, more complex theoretical models are needed and extracting accurate information regarding the samples can be very challenging. With careful calibration and a multidisciplinary approach, a combined measurement methodology can be developed enabling reliability, comparability, and accuracy. For production-relevant operation, maintaining the ease of use and scalability of ellipsometry as a technique can also be retained. T2 - EOSAM (European Optical Society Annual Meeting) CY - Berlin, Germany DA - 26.09.2016 KW - Spectroscopic ellipsometry KW - Thin films KW - Film thickness determination KW - Uncertainty PY - 2016 AN - OPUS4-38109 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kim, K. J. A1 - Kim, A. S. A1 - Jang, J. S. A1 - Suh, J. K. A1 - Wirth, Thomas A1 - Hodoroaba, Vasile-Dan A1 - Unger, Wolfgang A1 - Araujo, J. R. A1 - Archanjo, B. S. A1 - Galhardo, C. E. A1 - Damasceno, J. A1 - Achete, C. A. A1 - Wang, H. A1 - Wang, M. A1 - Bennett, J. A1 - Simons, D. A1 - Kurokawa, A. A1 - Terauchi, S. A1 - Fujimoto, T. A1 - Streeck, C. A1 - Beckhoff, B. A1 - Spencer, S. A1 - Shard, A. T1 - Measurement of mole fractions of Cu, In, Ga and Se in Cu(In,Ga)Se2 films N2 - CCQM key comparison K-129 for the quantitative analysis of Cu(In,Ga)Se2 (CIGS) films has been performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The objective of this key comparison is to compare the equivalency of the National Metrology Institutes (NMIs) and Designated Institutes (DIs) for the measurement of mole fractions of Cu, In, Ga and Se in a thin CIGS film. The measurand of this key comparison is the average mole fractions of Cu, In, Ga and Se of a test CIGS alloy film in the unit of mole fraction (mol/mol). Mole fraction with the metrological unit of mol/mol can be practically converted to atomic fraction with the unit of at%. In this key comparison, a CIGS film with certified mole fractions was supplied as a reference specimen to determine the relative sensitivity factors (RSFs) of Cu, In, Ga and Se. The mole fractions of the reference specimen were certified by isotope dilution - inductively coupled plasma/mass spectrometry (ID-ICP/MS) and are traceable to the SI. A total number counting (TNC) method was recommended as a method to determine the signal intensities of the constituent elements acquired in the depth profiles by Secondary Ion Mass Spectrometry (SIMS), X-ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES). Seven NMIs and one DI participated in this key comparison. The mole fractions of the CIGS films were measured by depth profiling based-SIMS, AES and XPS. The mole fractions were also measured by non-destructive X-Ray Fluorescence (XRF) Analysis and Electron Probe Micro Analysis (EPMA) with Energy Dispersive X-ray Spectrometry (EDX). In this key comparison, the average degrees of equivalence uncertainties for Cu, In, Ga and Se are 0.0093 mol/mol, 0.0123 mol/mol, 0.0047 mol/mol and 0.0228 mol/mol, respectively. These values are much smaller than that of Fe in a Fe-Ni alloy film in CCQM K-67 (0.0330 mol/mol). This means that the quantification of multi-element alloy films is possible by depth profiling analysis using the TNC method. KW - CIGS KW - Key comparison KW - CCQM KW - SIMS KW - XPS KW - AES KW - XRF KW - EPMA PY - 2016 UR - http://iopscience.iop.org/article/10.1088/0026-1394/53/1A/08011 DO - https://doi.org/10.1088/0026-1394/53/1A/08011 SN - 0026-1394 SN - 1681-7575 VL - 53, Technical Supplement SP - Article 08011, 1 EP - 19 PB - IOP Publishing AN - OPUS4-38110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Segundo, M. T1 - Microsphere biofunctionalization for meso/microfluidic-based automated immunoassays N2 - Immunochromatography and enzyme-linked immunosorbent assay (ELISA) represent selective and sensitive procedures based on solid-phases for separation/detection and quantification of anthropogenic pollutants in the aquatic environment. In contrast with batch-wise procedures, such as microplate-based platforms, automated methods reduce manual handling of reagents, thus increasing overall precision and decreasing time-to-result. Microparticles have been shown to be an adequate support for carrying out immunoassays in meso and microfluidic systems. They offer a wide range of coupling sites for biomolecules such as antibodies, combined with specialised anti-fouling surfaces to prevent non-specific binding and high compressibility for optimum fluidics. In this work we investigated the protein-coupling behaviour of two commercially available microsphere supports (Tentagel® polystyrene-PEG-COOH and PolyAn® PMMA beads with 3D antifouling surface) using DCC/EDC and NHS/S-NHS activation chemistry. The study of coupling conditions (pH, proportion of reagents and type of buffering system) was addressed. The success of the biomodification of the supports was demonstrated by using self-prepared fluorophore-protein conjugates (Fig. 1). Laser-scanning microscopy and flow cytometry were applied for further characterization of the functionalized particles. The applicability of the developed particles will be demonstrated through the design of suspension multiplex assays for the detection, quantification and preconcentration of bioactive substances such as caffeine and carbamazepine, using Lab-on-valve (LOV) platforms. T2 - XXII Encontro Luso-Galego de Química CY - Bragança, Portugal DA - 09.11.2016 KW - Immunoassay KW - Carbamazepine KW - Antibody immobilization KW - Lab-on-valve KW - Microbeads PY - 2016 AN - OPUS4-38208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Jungnickel, R. A1 - Neuhaus, B. A1 - Riedel, Jens A1 - Kneipp, Janina A1 - Lüter, C. T1 - Raman spectroscopy as a tool for the collection management of microscope slides N2 - Throughout the history of preparation of biological samples for microscopy the choice of the mounting medium was sometimes dictated merely by availability of the used media. Thus, a plethora of resins and other organic polymers as well as complex mixtures are found to serve as mounting agents in microscope slide collections of museums of natural history, impeding the work for both curators and conservators. Dramatically, in some cases the used mounting media can already be observed to have undergone crystallization and other decomposition processes within few years of mounting demanding immediate action in restoring as well as an imminent precaution in conservation. Therefore, an unambiguous chemical identification of the used agent as well as its current aging stage is of great interest for the biologist community. The technical demands on the analytical approach to obtain this information can be straightforwardly identified. Any used technique has to be non-destructive, yield in molecular information allowing for a chemical identification of the used mounting agents and allow for a spatially well-defined interrogation in a thin sample slice, typically through a transparent cover slip. In this contribution we present a thorough study of the applicability of Raman spectroscopy for the described task. The obtained results clearly demonstrate the successful feasibility of the chosen method for a) a clear distinction between different media, b) the elucidation of the chemical composition of a multicomponent medium and c) an unambiguous identification of real unknown samples by a distinct assignment to a previously recorded spectral library. This library database was built up by recording pure mounting agents and will be provided to the general public. In combination with a Raman spectrometer, it can be an invaluable tool for future curation and conservation endeavors devoted to microscope slide collections at natural history museums. KW - Taxonomy KW - Mounting medium KW - Coverslip seal PY - 2016 DO - https://doi.org/10.1016/j.jcz.2016.07.002 SN - 0044-5231 VL - 265 SP - 178 EP - 190 PB - Elsevier AN - OPUS4-38210 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bienge, J.-E. A1 - Illerhaus, Bernhard A1 - Epperlein, J. ED - Szallies, agrathaer GmbH, Isabell T1 - Blick in den Boden N2 - Computertomographische Untersuchungen in einer Studie zum vergleichenden Wurzelwachstum von Raps unter verschiedenen Bedingungen der Bodenbearbeitung. T2 - 20 Jahre Praxisversuch Lietzen Ackerbau und Forschung auf dem Weg in die Zukunft Feldtag in der Komturei Lietzen CY - Komturei Lietzen, Germany DA - 19.5.2016 KW - Computer Tomographie PY - 2016 SP - 28 EP - 29 AN - OPUS4-38144 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Veliz Montes, Cinthya T1 - Addressable immunoarrays: Enhancing the stability of short DNA - directed immobilization surfaces N2 - By using this method it is possible to have a platform that can be used for a multiplex diagnostic immuno-array formed by stable short ODNs. T2 - Biosensors 2016 CY - Gothenburg, Sweden DA - 25.05.2016 KW - DNA KW - Antibody PY - 2016 AN - OPUS4-38553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Veliz Montes, Cinthya T1 - Addressable immunoarrays: Implementation of 1O2 generator and applications N2 - The demand for sensitive and cost-effective diagnostics Analysis is steadily increasing. Addressable immunoarrays based on matching oligo-deoxynucleotide (ODN) strands have been described before 1,2. Short ODNs (e.g. 10 mers) could be used for addressing but are not stable enough to resist washing steps which lead to a sensitivity reduction. T2 - Analytica 2016 CY - Munich, Germany DA - 08.11.2016 KW - DNA KW - Antibody PY - 2016 AN - OPUS4-38554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Veliz Montes, Cinthya T1 - Adressable immunoarrays - Implementation of 1O2 generator and applications N2 - The demand for sensitive and cost-effective diagnostic tools is steadily increasing. Short ODNs (e.g. 10mers) could be used for addressable immunoarrays 1,2 but are not stable enough to resist washing steps which lead to a sensitivity reduction. Our aim is to establish a new platform for addressable immuno-arrays using shorter ODNs by increasing their stability via covalent linking. The main strategy consisted in the use of furan-modified ODNs that can be selectively oxidized leading to the formation of a site-specific interstrand cross-link (ICL) Comparison of the surface plasmon resonance (SPR) response shows successful ICL of short DNA duplex on surface. After ICL formation only the binding of the cross-linked DNA duplex with the recognition antibody is stable after regeneration using Na2CO3 (Fig. 1). Figure1. Method for detection of DNA ICL formation using an FITC labeled ODN and an anti-FITC antibody as model system a) Hybridized ODNs are efficiently separated after using Na2CO3 for regeneration b) Oxidation of the furan using 1O2 results in the formation of a stable ICL, which makes the short ODN duplex stable after regeneration T2 - Singlet Oxygen Strategy CY - Gent, Belgium DA - 17.06.2016 KW - DNA KW - Antibody PY - 2016 AN - OPUS4-38555 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tahri, K. A1 - Tiebe, Carlo A1 - El Bari, N. A1 - Hübert, Thomas A1 - Bouchikhi, B. T1 - Geographical provenience differentiation and adulteration detection of cumin by means of electronic sensing Systems and SPME-GC-MS in combination with different chemometric approaches N2 - The detection of the aroma and flavour volatile compounds of spices is key in product quality control. Accordingly, it is necessary to develop new electronic sensing systems for food adulteration control and authenticity assessment for protecting customer's health. In this work, the capability of the E-nose and VE-tongue in combination with SPME-GC-MS to correctly discriminate between several cumin samples of different geographical origins and to detect their adulteration, by using unsupervised and supervised chemometric tools, was evaluated. Regarding the aroma profile, eleven volatile compounds were characterized by SPME-GC-MS; all of them were found in cumin powder while only eight are found in cumin seeds. The main volatile compounds detected were b-pinene, m-cymene, g-terpinene, cuminaldehyde and cuminic alcohol, in different proportions depending on the cumin sample form (seed or powder). In summary, the results obtained are sufficiently encouraging as a starting point for the development of new electronic sensing systems with more improvement in the reliability of the sensor's performance as well as chemometric tools in order to deal with a complex dataset. KW - Voltammetric electronic tongue KW - Electronic nose KW - SPME-GC-MS KW - Chemometric tool KW - Cumin discrimination KW - Geographical origins KW - Adulteration detection PY - 2016 DO - https://doi.org/10.1039/c6ay01906d SN - 1759-9660 VL - 8 IS - 42 SP - 7638 EP - 7649 PB - RCS AN - OPUS4-38558 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Döge, N. T1 - In situ wide-field two photon microscopy of human hair follicles N2 - In a standard high magnification two-photon microscopy (2PM) setup the scan is achieved by moving the excitation beam inside the beam path limits of the microscope. Thus, the scanning area of the focus is limited by the field of view of the objective lens. As a consequence, the maximum scanning area is optically restricted to a diameter of 0.5 to 0.7 mm which impairs the application in biological and biomedical research. Herein, wide-field 2PM was used to image every dimension of the human hair follicle in whole tissue samples in situ. Therefore, a 2P microscope with a new approach called 2PM FlySCAN was applied. The 2P microscope moves the scan lens in a flying optics setup: The focus of the excitation laser beam is always concentric and collinear with the scan lens. The laser focus is in a fixed axial position to the scan lens. This approach allows to scan a large field of view (7×10 mm2) up to a resolution of 500 nm2 and a scan depth ~ 500 µm without vignetting or distortion. Further, a new en bloc longitudinal imaging mode was implemented which allows to image hair follicles in full length at a glance in a histomorphological correlation without further processing or sectioning. In situ labelling was successfully applied to investigate certain cell populations in the hair follicle which is of highly clinical relevance for various issues. Our results demonstrate that the here used wide-field 2P microscope combined with the en bloc longitudinal imaging mode is a promising approach for the preclinical assessment of the human hair follicle addressing the demand for an appropriate sample preparation and analysis techniques. T2 - Workshop "Advanced microscopy in life sciences" CY - Potsdam, Germany DA - 30.11.2016 KW - Two photon microscopy KW - Imaging KW - Tissue KW - Hair follicles KW - 2PM Fly Scan PY - 2016 AN - OPUS4-38535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bleeker, E. A1 - Visser, M. A1 - Groenewold, M. A1 - Blab, G. A1 - Brouwer, D. A1 - Sultan, Y. A1 - Gagnon, C. A1 - Wilkinson, K. A1 - Doa, M. A1 - Boyes, W. A1 - Kiyota, Y. A1 - Yanase, K. A1 - Holmqvist, J. A1 - Rasmussen, K. A1 - Sumrein, A. A1 - Clancy, S. A1 - Brown, S. A1 - Carlander, D. A1 - Murphy, L. A1 - Bresch, Harald A1 - Hund-Rinke, K. A1 - Igarashi, T. A1 - Riego-Sintes, J. A1 - Tentschert, J. T1 - Physical-chemical properties of nanomaterials: Evaluation of methods applied in the OECD-WPMN Testing Programme N2 - The Sponsorship Programme for the Testing of Manufactured Nanomaterials (further referred to as “the Testing Programme”) was concluded in March 2013, and the publication of the dossiers via the OECD website (www.oecd.org/science/nanosafety) started in June 2015. As indicated in the “Guidance manual for the testing of manufactured nanomaterials: OECD’s sponsorship programme”, after conclusion of the Testing Programme a next step is to consider “the status, need for, and coordination of further test development”. Parallel to concluding the final stages of the Testing Programme, a series of workshops have taken place, in which for different topics the applicability of existing OECD test guidelines for nanomaterials was discussed and the need for new ones analysed. One workshop focussed on physico-chemical methods, addressing in detail the relevance of each physico-chemical endpoint proposed in the Testing Programme for the regulation of nanomaterials. The methods were discussed in more general terms. However, as most of the proposed endpoints are new to the OECD Test Guidelines Programme, a much more detailed evaluation of the applied methods would be highly relevant. To this extent,the Netherlands volunteered to lead an initial detailed evaluation of the applicability of the test methods applied to determine the physico-chemical properties of different types of nanomaterials in the Testing Programme. This initial focus on physico-chemical properties was prompted by the essential need for an adequate and complete characterisation of nanomaterials to enable a further evaluation of their (toxicological) properties. A number of experts from several delegations volunteered to review and evaluate the methods applied to determine the physico-chemical properties of the nanomaterials in the Testing Programme. KW - Nanomaterialien KW - Nano KW - Nanopartikel KW - Charakterisierung KW - OECD KW - Nanomaterials PY - 2016 UR - http://www.oecd.org/env/ehs/nanosafety/publications-series-safety-manufactured-nanomaterials.htm IS - 65 SP - 1 EP - 43 CY - Paris AN - OPUS4-38495 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pieres, A. A1 - Almeida, Ângela A1 - Correia, J. A1 - Calisto, V. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Freitas, R. T1 - Long-term exposure to caffeine and carbamazepine: Impacts on the regenerative capacity of the polychaete Diopatra neapolitana N2 - The toxicity induced in non-target organisms by pharmaceutical drugs has been the focus of several studies. In the aquatic environment, most of the studies have been devoted to fish and bivalves, while little is known on the impacts induced in polychaetes. The present study evaluated the impacts of carbamazepine and caffeine on the regenerative capacity of Diopatra neapolitana, a polychaete species with high ecological and economic relevance. Under laboratory controlled conditions polychaetes were exposed, during 28 days, to carbamazepine (Ctl-0.0; 0.3; 3.0; 6.0; 9.0 mg/L) and caffeine (Ctl-0.0; 0.5; 3.0; 18.0 mg/L). During the experiment, at days 11, 18, 25, 32, 39 and 46 after amputation, for each specimen, the percentage of the body width regenerated was determined and the number of new segments was counted. The regenerative capacity was assessed considering the number of days needed to achieve full regeneration and the total number of new segments. The obtained results revealed that with the increase of drugs concentrations organisms regenerated less new segments and took longer to completely regenerate. KW - Diopatra neapolitana KW - Pollution KW - Pharmaceutical drugs KW - Regenerative capacity PY - 2016 DO - https://doi.org/10.1016/j.chemosphere.2015.12.035 SN - 0045-6535 VL - 146 SP - 565 EP - 573 PB - Elsevier AN - OPUS4-38497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beyer, Sebastian T1 - Surface functionality independent conjugation of biomolecules to colloidal metal-organic frameworks and their exemplified application in immuno-assays N2 - Metal-organic framework (MOF) colloids hold great potential for bioanalytical and biomedical applications due to their unique features. These include responsive luminescent properties and exceptionally high loading capacities for small molecular drugs. However, currently the lack of a surface functionality independent method for biomolecule conjugation is strongly limiting the advancement of colloidal MOFs in bioanalytical or biomedical applications. Bioanalytical methods, especially for environmental analysis, would benefit dramatically when responsive luminescent properties of MOFs could be coupled with a specific antibody interaction. Targeted drug delivery in biomedical applications often requires specificity towards tissues of interest in addition to a high drug loading capacity. Thus, both envisioned applications require biomolecules and in particular antibodies to be conjugated to colloidal MOFs. Here, we propose a robust and easy to handle method that is suitable for a wide range of MOF templates and that allows reliable conjugation of biomolecules. Colloidal ZIF-8 MOFs with particle size between 300nm and 5µm were used as templates to adsorb polymeric multilayer through a Layer-by-Layer self-assembly process. Multilayer build up was confirmed by the change in zeta-potential of particles upon polyelectrolyte adsorption as well as dynamic light scattering experiments and SEM/TEM microscopy. Subsequent biomolecule conjugation to functional groups of the polymeric multilayer on the surface of colloidal MOFs was achieved by established carbodiimide/succinimide conjugation chemistry. Successful and stable conjugation was confirmed by employing fluorescent labeled biomolecules. Subsequently, colloidal MOF-antibody (IgG) conjugates were utilized in a solid-phase immuno assay using antibodies against carbamazepine and lithocholic acid, two interesting markers in environmental analysis. In brief, mouse anti-CBZ (Carbamazepine) and rabbit anti-lithocholic acid were separately and covalently immobilized on 2D polystyrene surfaces to form a small micro spot array. Two separate populations of colloidal MOF particles were conjugated with goat anti mouse IgG and goat anti rabbit IgG, respectively. The different fluorescent labels of the two MOF colloid populations allowed the determination of binding selectivity and strength of the colloidal MOF-antibody conjugates to the immobilized binding partners. The ability to coat MOFs in solution independent of their surface charge with polymers and subsequently to conjugate biomolecules to their surface makes this method a powerful tool to foster bioanalytical, biomedical as well as other applications. T2 - MOF-2016 Conference Long Beach, California CY - Long Beach, California, USA DA - 11.09.2016 KW - Immunoassay PY - 2016 AN - OPUS4-38498 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Freitas, R. A1 - Almeida, Ângela A1 - Calisto, V. A1 - Velez, C. A1 - Moreira, A. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Wrona, F. J. A1 - Figueira, E. A1 - Soares, A. M. V. M. T1 - The impacts of pharmaceutical drugs under ocean acidification: Newdata on single and combined long-term effects of carbamazepine on Scrobicularia plana N2 - Ocean acidification and increasing discharges of pharmaceutical contaminants into aquatic systems are among key and/or emerging drivers of environmental change affecting marine ecosystems. A growing body of evidence demonstrates that ocean acidification can have direct and indirect impacts on marine organisms although combined effects with other stressors, namely with pharmaceuticals, have received very little attention to date. The present study aimed to evaluate the impacts of the pharmaceutical drug Carbamazepine and pH 7.1, acting alone and in combination, on the clamScrobicularia plana. For this, a long-termexposure (28 days)was conducted and a set of oxidative stress markers was investigated. The results obtained showed that S. plana was able to develop mechanisms to prevent oxidative damage when under low pH for a long period, presenting higher survival when exposed to this stressor compared to CBZ or the combination of CBZ with pH 7.1. Furthermore, the toxicity of CBZ on S. plana was synergistically increased under ocean acidification conditions (CBZ + pH 7.1): specimens survival was reduced and oxidative stress was enhanced when compared to single exposures. These findings add to the growing body of evidence that ocean acidification will act to increase the toxicity of CBZ to marine organisms,which has clear implications for coastal benthic ecosystems suffering chronic pollution from pharmaceutical drugs. KW - Ocean acidification KW - Pharmaceuticals KW - Biomarkers KW - Oxidative stress KW - Clams KW - Long-term exposures PY - 2016 DO - https://doi.org/10.1016/j.scitotenv.2015.09.138 VL - 541 SP - 977 EP - 985 PB - Elsevier B.V. AN - OPUS4-38502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fernandez, L. A1 - Esteves, V. I. A1 - Cunha, A. A1 - Schneider, Rudolf A1 - Tome, J. P. C. T1 - Photodegradation of organic pollutants in water by immobilized porphyrins and phthalocyanines N2 - New methods for water treatment are required as a result from an increasing awareness in the reduction of the pollution impact in the environment. In the perspective of the photo-oxidation of organic pollutants present in water, the principal incentive for the preparation of heterogeneous photocatalysts is their easy recovery from the reaction mixture, which allows their reuse in successive runs, minimizing the loss of their original photocatalytic properties. Different types of supports can be used in the immobilization of photoactive species, such as porphyrins (Pors) and phthalocyanines (Pcs). This mini-review will consider the different methodologies for the immobilization of Pors and Pcs and their photocatalytic performance in the photodegradation of organic pollutants in water, addressing also their recycling ability in successive water treatments. KW - Porphyrins KW - Phthalocyanines KW - Water treatment KW - Organic pollutants KW - Advanced oxidation processes KW - Heterogeneous photocatalysis KW - TiO2 KW - Microporous KW - Nanoparticles PY - 2016 DO - https://doi.org/10.1142/S108842461630007X VL - 2016 IS - 20 SP - 150 EP - 166 PB - World Scientific Publishing AN - OPUS4-38503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pires, A. A1 - Almeida, Ângela A1 - Calisto, V. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Wrona, F. J. A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Freitas, R. T1 - Long-term exposure of polychaetes to caffeine: Biochemical alterations induced in Diopatra neapolitana and Arenicola marina N2 - In the last decade studies have reported the presence of several pharmaceutical drugs in aquatic environments worldwide and an increasing effort has been done to understand the impacts induced on wildlife. Among the most abundant drugs in the environment is caffeine, which has been reported as an effective chemical anthropogenic marker. However, as for the majority of pharmaceuticals, scarce information is available on the adverse effects of caffeine on marine benthic organisms, namely polychaetes which are the most abundant group of organisms in several aquatic ecossystems. Thus, the present study aimed to evaluate the biochemical alterations induced by environmentally relevant concentrations of caffeine on the polychaete species Diopatra neapolitana and Arenicola marina. The results obtained demonstrated that after 28 days exposure oxidative stress was induced in both species, especially noticed in A. marina, resulting from the incapacity of antioxidant and biotransformation enzymes to prevent cells from lipid peroxidation. The present study further revealed that D. neapolitana used glycogen and proteins as energy to develop defense mechanisms while in A. marina these reserves were maintained independently on the exposure concentration, reinforcing the low capacity of this species to fight against oxidative stress. KW - Invertebrates KW - Pharmaceuticals KW - Oxidative stress biomarkers KW - Energy reserves PY - 2016 DO - https://doi.org/10.1016/j.envpol.2016.04.031 VL - 2016 IS - 214 SP - 456 EP - 463 PB - Elsevier Ltd. AN - OPUS4-38505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cruz, D. A1 - Almeida, Ângela A1 - Calisto, V. A1 - Esteves, V. I. A1 - Schneider, Rudolf A1 - Wrona, F. J. A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Freitas, R. T1 - Caffeine impacts in the clam Ruditapes philippinarum: Alterations on energy reserves, metabolic activity and oxidative stress biomarkers N2 - Caffeine is known to be one of the most consumed psychoactive drugs. For this reason, caffeine is continuously released into the environment with potential impacts on inhabiting organisms. The current study evaluated the biochemical alterations induced in the clam species Ruditapes philippinarum after exposure for 28 days to caffeine (0.5, 3.0 and 18.0 mg/L). The results obtained showed that, with the increasing caffeine concentrations, an increase in clams defense mechanisms (such as antioxidant and biotransformation enzymes activity) was induced which was accompanied by an increase in protein content. Nevertheless, although an increase on defense mechanisms was observed, clams were not able to prevent cells from lipid peroxidation that increased with the increase of caffeine concentration. Furthermore, with the increase of exposure concentrations, clams increased their metabolic activity (measured by electron transport activity), reducing their energy reserves (glycogen content), to fight against oxidative stress. Overall, the present study demonstrated that caffeine may impact bivalves, even at environmentally relevant concentrations, inducing oxidative stress in organisms. The present study is an important contribution to address knowledge gaps regarding the impacts of long-term exposures to pharmaceuticals since most of the studies assessed the effects after acute exposures, most of them up to 96 h. KW - Bivalves KW - Oxidative stress KW - Pharmaceuticals KW - Long-term exposure KW - Environmentally relevant concentrations PY - 2016 DO - https://doi.org/10.1016/j.chemosphere.2016.06.068 VL - 2016 IS - 160 SP - 95 EP - 103 PB - Elsevier Ltd. AN - OPUS4-38508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pires, A. A1 - Almeida, Ângela A1 - Calisto, V. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Wrona, F. J. A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Freitas, R. T1 - Hediste diversicolor as bioindicator of pharmaceutical pollution: Results from single and combined exposure to carbamazepine and caffeine N2 - Several environmental stressors have been identified as key and/or emerging drivers of habitat change that could significantly influence marine near-shore ecosystems. These include increasing discharges of pharmaceutical contaminants into the aquatic coastal systems. Pharmaceutical drugs are often detected in aquatic environments but still information on their toxicity impacts on inhabiting species is scarce, especially when acting in combination. Furthermore, almost no information is available on the impacts of pharmaceuticals in polychaetes, often the most abundant taxon in benthic communities and commonly used as indicator species of environmental conditions. Therefore, the present study aimed to evaluate the biochemical alterations induced in the polychaete Hediste diversicolor, from a low contaminated area at the Ria de Aveiro lagoon (Portugal), by the antiepileptic drug carbamazepine (0.0 - control, 0.3, 3.0, 6.0 and 9.0 μg/L) and the stimulant caffeine (0.0 - control, 0.5, 3.0, and 18.0 μg/L), acting alone and in combination (0.3 CBZ + 0.5 CAF and 6.0 CBZ + 3.0 CAF). Glutathione Stransferases (GSTs), superoxide dismutase (SOD) and catalase (CAT) activities was determined in Hediste diversicolor from each condition. Lipid peroxidation (LPO), glutathione reduced and oxidized (GSH and GSSG), glycogen and electron transport system (ETS) were also measured. The results obtained clearly revealed that both drugs induced oxidative stress in H. diversicolor, shown by the increase on LPO levels and decrease on total glutathione and GSH/GSSG ratio with the increase of exposure concentrations. Furthermore, the present findings demonstrated that polychaetes biotransformation capacity as well as antioxidant defense mechanisms were not sufficiently efficient to fight against the excess of reactive oxygen species (ROS) leading to LPO when organisms were exposed to both drugs. Our results also demonstrated that polychaetes tended to decrease the activity of ETSwhen exposed to drugs, avoiding energy expenditurewhich may prevent them fromgreater damages. The present study further revealed that the impacts induced by the combination of both drugswere similar to those obtained at the highest drugs concentrations acting alone. KW - Invertebrates KW - Pharmaceuticals KW - Oxidative stress biomarkers KW - Energy reserves PY - 2016 DO - https://doi.org/10.1016/j.cbpc.2016.06.003 VL - 2016 IS - 188 SP - 30 EP - 38 PB - Elsevier Inc. AN - OPUS4-38509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Asadujjaman, Asad T1 - Temperature sensitive aggregation behavior of poly(acrylamide-co-acrylonitrile) in water N2 - Thermoresponsive polymers have shown great potential in applications such as bioseparation, drug delivery and diagnostic. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range have been reported so far. Moreover, the most studied UCST type polymers namely polybetaines are difficult to use under physiological conditions, which significantly restricts their potential applications. Therefore, UCST polymers with sharp and robust phase transition in physiological conditions (in the presence of salts, ions etc.) are highly needed in order to extend the range of applications of this class of polymers. Herein, a robust UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain transfer (RAFT) polymerization[4] and its thermo-induced aggregation behavior in aqueous media was studied. At temperature below the UCST, the copolymer chains were aggregated together. The aggregate size was found to be larger with increasing AN contents and became smaller upon dilution of the copolymer solutions. While above the UCST, the copolymer chains were expanded and weekly associated in solution. The association between the copolymer chains formed smaller aggregates with increasing the AN contents or the dilution of the solutions. A model is proposed to explain such aggregation behavior. T2 - Polydays Konferenz 2016 CY - Potsdam, Germany DA - 28.09.2016 KW - Thermoresponsive polymer KW - UCST KW - Copolymer KW - RAFT PY - 2016 AN - OPUS4-38511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reier, T. A1 - Schultze, J. W. A1 - Österle, Werner A1 - Buchal, C. T1 - Nucleation and growth of AlN nanocrystallites prepared by N+2 implantation N2 - The formation of AlN films prepared by N+2 ion implantation into aluminium was investigated using X-ray and Auger photoelectron spectroscopy ( XPS, AES) as well as cross-sectional transmission electron microscopy (XTEM). After 100-keV N+2 implantation of low doses (1×1017 cm−2), the formation of hexagonal AlN nanocrystals (crystal size <5 nm, Ncrystal=1017 cm−3) was observed. Their orientation is strongly correlated with the aluminium matrix. With the dose increasing to 3×1017 cm−2, crystal growth follows, finally forming a homogeneous AlN-layer. Furthermore, the diffraction patterns show an increasing amount of misorientation with increasing dose. From the crystal size distribution, we conclude that continuous nucleation takes place. Samples implanted with an energy of 3 keV exhibit analogous behaviour. Nitride growth was further investigated using microstructured AlN formed by 3-keV implantation through movable TEM-masks (structure size: 15–150 mm). In the case of high N+2 doses (D&5×1017 cm−2), AlN is detected by AES in the shielded area at a distance of up to 10 mm from the exposed region. The Diffusion coefficient was calculated to be 10−10 cm2 s−1. The formation of AlN proceeds in two steps. After a continuous nucleation, diffusion-assisted Crystal growth takes place until a homogeneous AlN layer results. KW - Aluminium nitride KW - Ion implantation KW - Nanocrystallites KW - Surface analysis KW - XTEM PY - 1998 SN - 0257-8972 VL - 103-104 SP - 415 EP - 420 PB - Elsevier AN - OPUS4-38539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuhmann, J. F. A1 - Chiang, C. H. A1 - Harde, P. A1 - Reier, F. A1 - Österle, Werner A1 - Urban, Ingrid A1 - Klein, A. T1 - Pt thin-film metallization for FC-bonding using SnPb60/40 solder bump metallurgy N2 - Platinum does not form any adherent oxides and can be easily wetted by tin-based solders. Platinum is also an available metallization in semiconductor laboratories. Therefore we investigated the diffusion of platinum thin-film metallizations into eutectic tin–lead solder by using a high-resolution secondary ion mass spectroscopy (SIMS) profiling from the back side. It is shown that an intermetallic phase (PtSn4) is formed during soldering, which controls the consumption of platinum during soldering and in operation. The consumption of platinum follows the well-known parabolic diffusion law. The activation energy of this process is 0.63 eV. Even at extended heating cycles of 2 min at 250°C, 190 nm from the original 300 nm of the platinum film remain undissolved. This high stability makes platinum a very attractive thin-film metallization for flip-chip (FC) bonding of new microsystems. KW - Pt thin film metallization KW - FC solder bonding KW - Diffusion KW - SIMS PY - 1998 SN - 0921-5093 VL - A242 SP - 22 EP - 25 PB - Elsevier AN - OPUS4-38540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Österle, Werner A1 - Urban, Ingrid A1 - Severin, D. A1 - Trepte, S. T1 - Analyse von Reibschichten auf Bremsbelägen N2 - Die volle Leistung einer auf Reibung basierenden Bremse wird erst nach einem Einlaufvorgang erreicht. Dieser ist notwendig, um auf Belag und Scheibe eine sogenannte Reibschicht aufzubauen. Da diese Zwischenschicht das Reibungsverhalten des Systems maßgeblich bestimmt, ist es wichtig, sich Klarheit über ihre chemische Zusammensetzung, Mikrostruktur und die daraus resultierenden Eigenschaften zu verschaffen. Als Basismaterial diente ein phenolharzgebundener Belag Jurid 57-62, der mit verschiedenen Parametern (Flächenpressung und Umdrehungsgeschwindigkeit) gegen eine Stahlscheibe getestet wurde. Es wurden Dauerbremsungen von jeweils einer Stunde bzw. bis zu einem maximalen Belagverschleiß von 1 mm simuliert, wobei die Entwicklung der Reibzahl und die Oberflächentemperatur der Scheibe registriert wurde. Zur Analyse der Reibschichten auf dem Bremsbelag wurden mehrere Methoden parallel angewandt. So wurden Verschleißpartikel, die aus der Reibschicht stammen, gesammelt bzw. abgekratzt und nach Dispergieren auf Kohlefolien direkt im Transmissionselektronenmikros-kop (TEM) untersucht. Ferner wurden von einigen ausgesuchten Belagproben Mikrotom-schnitte sowie dünne Querschnittsfolien für die TEM-Untersuchung präpariert, um den Verbund Reibschicht-Grundmaterial darstellen zu können. Als Ergänzung wurden ferner oberflächenmorphologische und –analytische Verfahren wie REM/EDX und ESCA eingesetzt. Die Ergebnisse deuten darauf hin, dass die Reibschicht nanokristallin ist, und dass fast alle anorganischen Bestandteile des Bremsbelags sowie Eisenoxid von der Bremsscheibe in sehr fein verteilter Form vorliegen. Bei Belägen ohne Metallanteil bildet eine Barium-Eisen-Sulfatphase offenbar die Grundstruktur der Reibschicht, während auf eisenhaltigen Belägen Eisenoxid dominierend ist. Die nanokristalline Mikrostruktur entsteht, ähnlich wie beim mechanischen Legieren, durch einen Mahlvorgang von Verschleißpartikeln zwischen den Reibpartnern. Bei Überlastung des Belags tritt Zersetzung der Polymer-Bindephase ein, was zu einem raschen Anstieg der Verschleißrate führt. KW - Bremsbelag KW - Reibschicht KW - Reibungskoeffizient KW - Oberflächenanalyse KW - Transmissionselektronenmikroskopie PY - 2000 SN - 0933-5137 VL - 31 SP - 708 EP - 711 PB - Whiley VCH CY - Weinheim AN - OPUS4-38542 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nebauer, E. A1 - Österle, Werner A1 - Hilsenbeck, J. A1 - Würfl, J. A1 - Klein, A. T1 - XTEM and TFXRD investigations of ohmic Ti/Al/Ti/Au/WSiN contacts on AlGaN/GaN HFET layer systems N2 - The microstructural features of the high-temperature-stable ohmic contact system Ti/Al/Ti/Au/WSiN on AlGaN/GaN were investigated using analytical transmission electron microscopy and thin film x-ray diffraction. For two typical rapid thermal annealing steps at 750 ◦C (non-ohmic behaviour) and 850 ◦C (ohmic behaviour) the intermetallic phases at the metal–semiconductor interface are presented. Increased annealing leads to the transformation of an Al2Au-AlAuTi phase mixture to a mixture of Al2Au-Al3Au8 phases and the formation of Ti-Al-nitride layers at the interfaces. In light of these results the electrical contact properties are discussed. KW - Ohmic contact KW - WSiN diffusion barrier KW - Rapid thermal annealing KW - Intermetallic phases KW - AlGaN/GaN heterostructure PY - 2002 SN - 0268-1242 VL - 17 SP - 249 EP - 254 PB - IOP Publishing Ltd AN - OPUS4-38543 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Natte, Kishore A1 - Friedrich, Jörg Florian A1 - Wohlrab, Sebastian A1 - Lutzki, J. A1 - von Klitzing, R. A1 - Österle, Werner A1 - Orts-Gil, Guillermo T1 - Impact of polymer shell on the formation and time evolution of nanoparticle-protein corona N2 - The study of protein corona formation on nanoparticles (NPs) represents an actual main issue in colloidal, biomedical and toxicological sciences. However, little is known about the influence of polymer shells on the formation and time evolution of protein corona onto functionalized NPs. Therefore, silicapoly(ethylene glycol) core–shell nanohybrids (SNPs@PEG) with different polymer molecular weights (MW) were synthesized and exhaustively characterized. Bovine serum albumin (BSA) at different concentrations (0.1–6 wt%) was used as model protein to study protein corona formation and time evolution. For pristine SNPs and SNPs@PEG (MW = 350 g/mol), zeta potential at different incubation times show a dynamical evolution of the nanoparticle–protein corona. Oppositely, for SNPs@PEG with MW ≥2000 g/mol a significant suppression of corona formation and time evolution was observed. Furthermore, AFM investigations suggest a different orientation (side-chain or perpendicular) and Penetration depth of BSA toward PEGylated surfaces depending on the polymer length which may explain differences in protein corona evolution. KW - Nanoparticles KW - Silica KW - PEGylation KW - Protein corona KW - BSA KW - Biointerface PY - 2013 DO - https://doi.org/10.1016/j.colsurfb.2012.11.019 SN - 0927-7765 VL - 104 SP - 213 EP - 220 PB - Elsevier AN - OPUS4-38547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Natte, Kishore A1 - Österle, Werner A1 - Friedrich, Jörg Florian A1 - von Klitzing, R. A1 - Orts-Gil, Guillermo T1 - Tuning interfacial properties and colloidal behavior of hybrid nanoparticles by controlling the polymer precursor N2 - A facile and versatile synthetic route for controlling the size and surface potential of organic–inorganic hybrid silica nanoparticles (NPs) is introduced in this paper. For polymer-grafted NPs, the density of polymer chains on the surface is strongly affected by the concentration of precursor. Nevertheless, for condensed NPs, the precursor concentration determines the particle size but not the density of polymer chains on the surface or the adsorption of bovine serum albumin (BSA). Results presented here may have Major implications in biomedical and colloidal chemistry since interfacial and colloidal properties are known to drive several processes associated with nanoparticles in biological media. KW - BSA KW - Bio-interface KW - Nanosilica hybrids KW - PEG KW - Protein corona PY - 2012 DO - https://doi.org/10.1002/macp.201200148 SN - 0025-116X SN - 1022-1352 SN - 1521-3935 VL - 213 IS - 22 SP - 2412 EP - 2419 PB - Whiley-VCH CY - Weinheim AN - OPUS4-38549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Villatoro, J. A1 - Zühlke, M. A1 - Riebe, D. A1 - Beitz, T. A1 - Weber, M. A1 - Riedel, Jens A1 - Löhmannsröben, H.-G. T1 - IR-MALDI ion mobility spectrometry: physical source characterization and application as HPLC detector N2 - Infraredmatrix-assisted laser dispersion and ionization(IR-MALDI) in combination with on mobility (IM) spectrometry enables the direct Analysis of biomolecules in aqueous solution. The release of ions directly from an aqueous solution is based on a phase explosion, induced by the Absorption of an IR laser pulse, which disperses the liquid as vapor, nano- and micro-droplets. The ionization process is characterized initially by a broad spatial distribution of the ions, which is a result of complex fluid dynamics and desolvation kinetics. These processes have a profound effect on the shape and width of the peaks in the IM spectra. In this work, the Transport of ions by the phase explosion-induced shockwave could be studied independently from the transport by the electric field. The shockwave-induced mean velocities of the ions at different time scales were determined through IM spectrometry and shadowgraphy. The results show a deceleration of the Ions from 118m∙s−1 at a distance of 400 μm from the liquid surface to 7.1 m∙s−1 at a distance of 10 mm, which is caused by a pileup effect. Furthermore, the desolvation kinetics were investigated and a first-order desolvation constant of 325 ± 50 s−1 was obtained. In the second part, the IR-MALDI-IM spectrometer is used as an HPLC detector for the twodimensional separation of a pesticide mixture. KW - Ion mobility spectrometry KW - IR-MALDI KW - Shadowgraphy KW - Laser PY - 2016 DO - https://doi.org/10.1007/s12127-016-0208-1 VL - 2016 IS - 4 SP - 197 EP - 207 PB - Springer-Verlag Berlin CY - Heidelberg AN - OPUS4-38467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kanje, S. A1 - Hober, S. A1 - Mueller, L. A1 - Herrmann, Antje Jutta T1 - Next generation of labeling reagents for quantitative and multiplexing immunoassays by the use of LA-ICP-MS N2 - Immuno imaging by the use of Laser Ablation Inductively Coupled Mass Spectrometry (LA-ICP-MS) is a growing research field in life sciences such as biology and biomedicine. Various element labeling strategies for antibodies have been developed for the application of multiplex immunoassays analyzed by the use of LA-ICP-MS. High multiplexing capabilities, a wide linear dynamic range and the possibility of absolute quantification are the main advantages of ICP-MS. But in the context of immuno imaging by the use of LA-ICP-MS, quantification of analytes is limited due to non-controllable antibody labeling chemistry. In the presented proof-of-principle a novel antibody labeling technique has been investigated which results in a controlled labeling degree. A small affinity protein based on the C2 domain of protein G was modified with conventional metal coded tags (MeCAT) after introducing a cysteine into the C-terminus of the protein. The modified C2 domain photo-crosslinks to the Fc or Fab region of the IgG and allows specific and covalent labeling of antibodies for multiplex immunoassay analysis by the use of LA-ICP-MS. In combination with a house-made calibration membrane the amount of labeled antibody–antigen complexes in a multiplex western blot immunoassay was determined by LA-ICP-MS. KW - LA-ICP-MS based immunoassays KW - Antibody labeling PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-384712 DO - https://doi.org/10.1039/c6an01878e SN - 0003-2654 SN - 1364-5528 VL - 141 IS - 23 SP - 6374 EP - 6380 PB - The Royal Society of Chemistry AN - OPUS4-38471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - Tagungsband - 12. Kolloquium Prozessanalytik Berlin N2 - Das 12. Kolloquium würdigt mit dem diesjährigen Schwerpunkt auf der Pharma- und Lebensmittel-technologie zwei technisch-wissenschaftliche Bereiche, die sich zum einen die Aufgabe gestellt haben, für jeden und jede Krankheit etwas parat zu haben, und zum anderen daran arbeitet, nicht nur den Hunger zu bekämpfen, sondern täglich auch eine unermessliche Auswahl an Lebensmitteln für eine ausgewogene Ernährung zu liefern. In beiden Arbeitsgebieten bestehen nach wie vor große Herausforderungen. Phamaka etwa stehen bei weitem nicht überall auf der Welt in gleichmäßiger Qualität und bezahlbar zur Verfügung. Auch die noch immer schnell wachsende Bevölkerung sowie der fortschreitende Klimawandel stellen die Lebensmittel-produzierende Industrie sowie die Erzeuger vor die immer größer werdende Aufgabe, nachhaltigere und insbesondere ergiebigere Verfahren zu entwickeln und umzusetzen. Die Pro-zessanalytik kann und wird an diesen Stellen ihren Beitrag leisten. Die Anforderungen an die Prozessanalytik für die Pharma- und Lebensmittelproduktion weisen viele Parallelen auf. So sind beide Bereiche heutzutage regulatorischen Anforderungen unterworfen, die auf der Basis einer risikobasierten Vorgehensweise beruhen, womit Entwicklungs-, Herstellungs- und Qualitätssicherungsprozesse sowohl für die Produzenten als auch für die überwachenden Behörden deutlich verbessert und beschleunigt worden sind. Diese erfreuliche Entwicklung hat ihr Ende aber noch lange nicht gefunden und die die Verfahren befinden sich noch immer in einem starken Wandel. Dennoch haben sie bereits jetzt dazu beigetragen, dass zum Beispiel viele Produktionsmaschinen und Teilanlagen ihre Prozessanalytik bereits an Bord haben, wie etwa der Mähdrescher mit eingebauter Online-Spektroskopie und GPS-Kartierung für das Precision Farming oder die Gefriertrocknungsanlage mit 100%-Trocknungskontrolle am vereinzelten Produkt. Das 12. Kolloquium greift die wichtigsten Herausforderungen auf und spannt eine Diskussionslinie entlang der technologie- und verbrauchergetriebenen Herstellungsverfahren, von Phenotyping und Digital Farming über rote und grüne Biotechnologie bis hin zur Laborautomation unter Einsatz der Hochdurchsatz-Experimentation. Die in der Pharma- und Lebensmittelherstellung gesteckten Ziele sind hoch und entsprechend groß sind die zu erwartenden Vorteile: Im sogenannten Real Time Release wird die Qualität des finalen (Zwischen-)Produktes ausschließlich aus In-Prozess-Kontrollen oder Prozessdaten abgeleitet. Für jede produzierte Charge lässt sich die Konformität zu akzeptierten Qualitätsmerkmalen aufzeigen und diese damit ohne weitere Endkontrolle freigeben. Der konsequente Einsatz von Real Time Release ist eine der wesentlichen Voraussetzungen für die kontinuierliche Produktion (Continuous Manufacturing), die die Pharmazeutische Industrie eines Tages adaptieren wird. Im historischen Rückblick haben sich fast ausnahmslos alle Zweige der Produktion in der Prozessindustrie mehr und mehr hin zu einer kontinuierlichen Produktion gewandelt. Man kann davon ausgehen, dass die Qualitätssicherungskosten bei konsequenter Implementierung von PAT von derzeit ca. 30 % in zukünftig einen kleinen einstelligen Prozentbereich der COGS gesenkt werden können. Gleichzeitig führt der Erkenntnisgewinn zur Verbesserung der Produkte selbst sowie ihrer Herstellungsprozesse. Die Qualität wird sozusagen intrinsisch eingebaut. So kann die Sicherheit für den Verbraucher sogar noch gesteigert werden und der Kostenanstieg im Gesundheitssystem wird deutlich gedämpft. T2 - 12. Kolloquium Arbeitskreis Prozessanalytik CY - Berlin, Germany DA - 28.12.2016 KW - Kolloquium Prozessanalytik KW - Process Analytical Technology KW - Prozessanalytik KW - Pharmazeutische Chemie KW - Lebensmitteltechnologie KW - Lebensmittelproduktion KW - Medikamente PY - 2016 SP - 1 EP - 104 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38560 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Die Technologie-Roadmap „Prozess-Sensoren 4.0“ – Chancen für neue Automatisierungskonzepte und neue Geschäftsmodelle N2 - Die auf der NAMUR HS 2015 vorgestellte Technologie-Roadmap „Prozess-Sensoren 4.0“ zeigt die nötigen Anforderungen an Prozess-Sensoren sowie an deren Kommunikations-fähigkeiten auf. Wir berichten über den Stand der Diskussionen im Trialog zwischen Anwendern, Software- und Geräteherstellern sowie der Forschung. Ein wichtiger Schlüssel ist die Definition einer bedarfsgerechten und einheitlichen Topologie für solche smarten Sensoren, die in einem Arbeitskreis „Smarte-Sensorik“ ohne im wechselseitigen Austausch mit Geräte- und Softwareherstellern und Forschungseinrichtungen vorangetrieben werden soll. T2 - 1. Forum Embedded Spektroskopie CY - Berlin, Germany DA - 01.12.2016 KW - Roadmap KW - Prozess-Sensoren 4.0 KW - Prozessanalytik KW - Embedded spectroscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-385611 AN - OPUS4-38561 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana A1 - Meyer, Klas T1 - Process monitoring of an intensified continuous production unit with compact NMR spectroscopy N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and relatively inexpensive analyzers, which feature advantages like low cost, low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, sufficient robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Recently, promising benchtop NMR instruments with acceptable performance came to market and process integrated sensors developed on basis of such laboratory instruments are on their way. Intensified continuous processes are in focus of current research. Compared to traditional batch processes, these are giving admittance to new and difficult to produce compounds, leading to better product uniformity, and dras-tically reducing the consumption of raw materials and energy. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns, and quick introduction of new products to the market. Typically, such plants have smaller scale than big size facilities for production of basic chemicals but are still capable to produce kilograms to tons of specialty products each day. Such flexible (modular) plants can be provided in the size of 20 ft freight containers and represent a promising approach by their ability of easy transfer to production sites as well as the possibility of increasing production capacity by a simple numbering-up-approach. However, full automation is a prerequisite to realize such benefits of intensified continuous production. In continu-ous flow processes steady automated measurements and tight closed-loop control of the product quality are mandatory. If these are not available, there is a huge risk of producing large amounts of out-of-spec (OOS) prod-ucts. This is addressed in the European Union’s Research Project CONSENS (Integrated Control and Sensing) by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. T2 - 12. Kolloquium des Arbeitskreises Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Low field NMR spectroscopy KW - Modular production units KW - Online NMR spectroscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-385628 AN - OPUS4-38562 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Harald T1 - OECD-WPMN sponsorship programme dossiers - a review of the results for particle size N2 - The Organization for Economic Co-operation and Development (OECD) established the Working Party on Manufactured Nanomaterials (WPMN) in 2006. The OECD-WPMN initiated the "Sponsorship Programme for the Testing of Manufactured Nanomaterials", where a defined set of manufactured nanomaterials is tested for their physical/chemical properties, their toxicological potential and their environmental fade. The results of this program have been declassified in June 2015. Having a big set of independent measurements for one endpoint/measurand, has the advantage of really independent comparision of methods. It is surprising what these few data sets already delivered. Nevertheless the amount of data in the OECD-dossiers is still not enough. While we have a lot of data for titanium dioxide, we have only one data set for zinc oxide and very weak data sets for silver nanoparticles. This limits the useablility of the data sets. Regarding the quality of the data, we have seen a very good agreement of TEM and SMPS. This leads to the advice that we should have results for these two methods for each nanomaterial in the sponsorship programme. Another outcome of this draft review is, that currently we cannot compare measurements of agglomerates. This also prohibits the use of DLS as a standard method for size determination. T2 - European Aerosol Conference CY - Tours, France DA - 05.09.2016 KW - OECD KW - Nanopartikel KW - Nano KW - Nanoparticle KW - Nanomaterials PY - 2016 AN - OPUS4-38568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mielke, Johannes A1 - Babick, F. A1 - Uusimäki, T. A1 - Müller, P. A1 - Verleysen, E. A1 - Hodoroaba, Vasile-Dan T1 - Evaluation of electron microscopy techniques for the purpose of classification of nanomaterials N2 - Electron microscopy techniques such as TEM, STEM, SEM or TSEM (transmission in SEM) are capable of assessing the size of individual nanoparticles accurately. Nevertheless, the challenging aspect is sample preparation from powder or liquid form on the substrate, so that a homogeneous distribution of well-separated (deagglomerated) particles is attained. The systematic study in this work shows examples where the extraction of the critical, smallest particle dimension - as the decisive particle parameter for the classification as a NM - is possible by analysing the sample after ist simple, dry preparation. The consequences of additional typical issues like loss of information due to screening of smaller particles by larger ones or the (in)ability to access the constituent particles in aggregates are discussed. KW - Nanomaterial KW - Electron microscopy KW - Particle size distribution KW - Classification PY - 2016 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/evaluation-of-electron-microscopy-techniques-for-the-purpose-of-classification-of-nanomaterials/0B66A25EA7F7A5A3622C02A359C8304F DO - https://doi.org/10.1017/S1431927616005523 SN - 1431-9276 SN - 1435-8115 VL - 22 IS - Suppl. 3 SP - 936 EP - 937 PB - Cambridge AN - OPUS4-38445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Avishai, N. A1 - Avishai, A. A1 - Hodoroaba, Vasile-Dan T1 - What is the effective geometrical collection efficiency of your XEDS detector? A routine procedure applied in a SEM laboratory. N2 - In this contribution, two large-area EDS detectors were tested according to the procedure proposed recently by Procop et al. In a first step, the optimal working distance (WD) in the two different SEM chambers was determined by moving the sample stage in the Z direction and monitoring the count rates from a field of view of 25.6 μm. The WD at which the highest intensity was measured was selected as the optimal position. Next the Cu Kα peak was measured at different relative EDS positions while it was partially removed from the fully inserted position. The spectrum at each location was collected for 10 sec using the highest pulse rate and intermediate current (2.3 nA) to minimize pile up effects (13% dead time). The ‘inverse squared normalized intensities vs. relative EDS position’ used to extract the true detector – specimen distance shows a non-linear relationship even at the minimal relative positions, which indicates shadowing due to obstruction or use of an unsuitable and/or off-centered collimator. The normalized count rates measured as a function of the EDS distances, results in a too low GCE (too low true solid angles) for both tested detectors. The search for sources of losses of signal due to possible shadowing effects is in progress. KW - EDS Geometrical Detection Efficiency KW - EDS Solid Angle KW - EDS net active sensor area KW - EDS detector PY - 2016 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/what-is-the-effective-geometrical-collection-efficiency-of-your-xeds-detector-a-routine-procedure-applied-in-a-sem-laboratory/40A1A25C97916CA4D9FA365249CFC36C DO - https://doi.org/10.1017/S1431927616002919 SN - 1431-9276 SN - 1435-8115 VL - 22 IS - Suppl. 3 SP - 412 EP - 413 PB - Cambridge AN - OPUS4-38446 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - Certified forensic alcohol reference materials N2 - The poster presents a project proposal for the production and certification of ethanol/water reference materials suitable for the calibration and type approval of breath alcohol analysers. T2 - EURAMET EMPIR Research Potential Review Conference 2016 CY - Rotterdam, The Netherlands DA - 23.11.2016 KW - Reference material KW - Breath alcohol analyser KW - Interlaboratory comparison PY - 2016 AN - OPUS4-38455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Quantifizierung der Festigkeit von Kunststoffklebungen & -beschichtungen: Vorbehandeln, Kleben und Prüfen im OKTETT N2 - Der Vortrag widmet sich der „Quantifizierung der Festigkeit von Kunststoffklebungen & -beschichtungen: Vorbehandeln, Kleben und Prüfen im OKTETT“ und beschreibt das Mehr-Proben-Konzept zur Herstellung und Prüfung von Klebeverbunden. Vorgestellt werden die Mehr-Proben-Klebevorrichtung sowie die Centrifugal Adhesion Testing (CAT) Technologie zur Bestimmung der Haft- und Klebefestigkeit von Beschichtungen (Al auf PP, SiO2 auf CR39). T2 - SKZ Das Kunststoff-Zentrum Würzburg 2016 CY - Würzburg, Germany DA - 21.11.2016 KW - Klebfestigkeit KW - Haftfestigkeit KW - Multiple Sample Bonding (MSB) KW - Centrifugal Adhesion Testing (CAT) PY - 2016 AN - OPUS4-38461 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bierstedt, Andreas A1 - Riedel, Jens T1 - High-repetition rate laser ablation coupled to dielectric barrier discharge postionization for ambient mass spectrometry N2 - Most ambient sample introduction and ionization techniques for native mass spectrometry are highly selective for polar agents. To achieve a more general sensitivity for a wider range of target analytes, a novel laser ablation dielectric barrier discharge (LA DBD) ionization scheme was developed. The Approach employs a two-step mechanism with subsequent sample desorption and post-ionization. Effective Ablation was achieved by the second harmonic output (λ = 532 nm) of a diode pumped Nd:YVO₄ laser operating at a high-repetition rate of several kHz and pulse energies below 100 μJ. The ejected analytecontaining aerosol was consecutively vaporized and ionized in the afterglow of a DBD plasma jet. Depending on their proton affinity the superexcited Helium species in this afterglow produced analyte ions as protonated and ammoniated species, as well as radical cations. The optimization procedure could corroborate underlying conceptual consideration on the ablation, desorption and ionization mechanisms. A successful detection of a variety of target molecules could be shown from the pharmaceutical ibuprofen, urea, the amino acids L-arginine, L-lysine, the polymer polyethylene glycol, the organometallic compound ferrocene and the technical mixture wild mint oil. For a reliable evaluation of the introduced detection procedure spectra from the naturally abundant alkaloid capsaicin in dried capsicum fruits were recorded. KW - Laser ablation KW - High-repetition rate laser KW - Dielectric barrier discharge KW - Ambient mass spectrometry PY - 2016 DO - https://doi.org/10.1016/j.ymeth.2016.02.002 SN - 1046-2023 IS - 104 SP - 3 EP - 10 PB - Elsevier CY - Oxford AN - OPUS4-36730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Carl, Peter A1 - Westad, Frank A1 - Voss, J.-P. A1 - Maiwald, Michael T1 - Towards process spectroscopy in complex fermentation samples and mixtures N2 - Supernatants from a fermentation process of Pichia pastoris were investigated by Raman spectroscopy. Using partial least squares regression, the principal substrates glycerol and methanol could be predicted, however not the expressed protein. To gain further insight, a priori prepared calibration samples were studied by vibrational-, UV/Vis-, and fluorescence spectroscopy. For the quantification of glycerol and methanol, Raman spectroscopy was identified as the most sensitive technique, and superior to near-infrared spectroscopy, but not for protein contents below 1 g L–1. Both UV/Vis absorption and fluorescence spectroscopy are well suited for the quantification of protein, however, best results were obtained with UV/Vis absorption. KW - Fluorescence KW - NIR spectroscopy KW - Partial least squares regression KW - Pichia pastoris KW - Raman spectroscopy KW - UV/VIS spectroscopy PY - 2016 DO - https://doi.org/10.1002/cite.201500118 SN - 0009-286X SN - 1522-2640 VL - 88 IS - 6 SP - 756 EP - 763 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim, Germany AN - OPUS4-36755 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Anwendung chemometrischer Methoden in der Prozessanalysentechnik N2 - Der Einsatz moderner Prozessanalysentechnik führt zu einer Datenflut, deren Verarbeitung und Nutzung häufig nicht ohne den Einsatz von Chemometrie zu realisieren ist. Dafür stehen zahlreiche multivariate Verfahren, wie z.B. Hauptkomponentenanalyse (PCA) und Regressionsanalyse (PLSR) für die Klassifizierung und für die quantitative Analyse zur Verfügung. Darüber hinaus können in Spezialfällen, insbesondere in der Spektroskopie, Methoden des „Indirect Hard Modeling“ eingesetzt werden. Anhand einer Industrie-relevanten Reaktion, der Hydroformylierungsreaktion zur Bildung langkettiger Aldehyde aus der Reaktion von Alkenen und Synthesegas, die sowohl im Labormaßstab als auch in einer Miniplant in Kooperation mit der TU Berlin untersucht wurde, werden Kalibrationsstrategien (Design of Experiment, DoE) und Auswertungsansätze mittels PLSR prozessbegleitender Raman Spektren dargelegt. Auf Grundlage des chemometrischen Ansatzes ist eine on-line Überwachung der Reaktion hinsichtlich der Hauptreaktanden, 1-Dodecene und 1-Tridecanal, möglich. Weiterhin konnte mittels Raman Spektroskopie die Bildung eines unerwünschten Nebenprodukts nachgewiesen werden. T2 - Automatisierungsforum Westküste CY - Heide, Germany DA - 09.02.2016 KW - Online KW - PLS KW - DoE KW - Hydroformylierung PY - 2016 AN - OPUS4-36760 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hübert, Thomas A1 - Tiebe, Carlo A1 - Detjens, Marc A1 - Majewski, J. T1 - On-site calibration system for trace humidity sensors N2 - A portable device for calibration of trace humidity sensors and an adopted calibration procedure have been developed. The calibration device is based on humidity generation by permeating water through polymeric membrane tubes. Water vapour transmission rates for various polymers were experimentally determined in order to select the most suitable polymeric material. The developed trace humidity generator consists of a gas-flow polymeric hose immersed in a water reservoir thermostated by a sensorcontrolled heater. Mole fractions of water vapour between 1 µmol/ molˉ¹ and 350 µmol/molˉ¹ (equivalent to frost-point temperatures from -76 °C to -31 °C) were generated by varying either the operating temperature or gas flow. The operating temperature can be varied from 20 °C to 60 °C and kept stable within 0.1 K. Uncertainty analysis indicated that the trace humidity generator produces gas flows of constant humidity amounts with a relative expanded uncertainty less than 3.4% (k = 2) of the generated value. KW - Polymeric tubes KW - Measurements KW - Trace Humidity KW - Sensor calibration KW - Water vapour permeation PY - 2016 DO - https://doi.org/10.1016/j.measurement.2016.05.013 SN - 0263-2241 VL - 91 IS - 9 SP - 251 EP - 257 PB - Elsevier Ltd. AN - OPUS4-36762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Spranger, Holger A1 - Beckmann, Jörg A1 - Boehm, Rainer T1 - THz-ToF techniques for the detection of inherent discontinuities in dielectric materials based on a SAFT – and an optical layer reconstruction algorithm N2 - Electromagnetic waves with frequencies between 0.1 and 10 THz are described as THz-radiation (T-ray). The ability to penetrate dielectric materials makes T-rays attractive to reveal discontinuities in polymer and ceramic materials. THz-Time Domain Spectroscopy Systems (THz-TDS) are available on the market today which operates with THz-pulses transmitted and received by optically pumped semiconductor antennas. In THz-TDS the travelling time (ToF) and shape of the pulse is changed if it interacts with the dielectric material and its inherent discontinuities. A tomogram of the object under the test can be reconstructed from time of flight diffraction (ToFD) scans if a synthetic focusing aperture (SAFT) algorithm is applied. Otherwise, planar discontinuities like cracks in plastics or delaminated layers in composites can be abstracted as layers located at any angle in relation to the outer sample surface direction. A tomogram from the scanned sample can then be reconstructed in case the interactions of electromagnetic pulses with the existing inherent interfaces are detectable and a model is assumed which describes the device under the test as multilayer structure composed of thin layers with different dielectric properties. A short description of both the SAFT – and Optical Layer algorithm for the reconstruction of the inherent structure is initially given. Measurements on representative samples with a variety of artificially produced small and large scale. Reconstructed tomograms are presented to discuss and evaluate the benefits and limits of the two different reconstruction approaches. T2 - 19th World Conference on Non-Destructive Testing 2016 CY - Munich, Germany DA - 13.06.2016 KW - THz SAFT Optical layer reconstruction PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-365866 SN - 978-3-940283-78-8 VL - 158 SP - 1 EP - 10 AN - OPUS4-36586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas A1 - Maierhofer, Christiane T1 - Entwicklung eines innovativen Bodenradars zur Ortung von Objekten im Baugrund N2 - Das Projektziel war die Vermeidung von Schäden bei Erdarbeiten und Ausschachtungen durch Entwicklung eines innovativen Bodenradarsystems mit wesentlicher Verbesserung des räumlichen Auflösungsvermögens bei der zerstörungsfreien Ortung von folgenden Objekten im Untergrund: Gasleitungen, Frisch- und Abwasserleitungen, Leitungen zur Elektrizitäts- und Kommunikationsversorgung aus verschiedenen Materialien und umgeben mit unterschiedlichen Böden mit variierendem Feuchtegehalt. Darüber hinaus ging es um die Reduzierung der Kosten und Erhöhung der Akzeptanz des Verfahrens durch eine schnelle Echtzeit-Interpretation der Messdaten. T2 - Fachtagung Bauwerksdiagnose - Praktische Anwendungen Zerstörungsfreier Prüfungen CY - Leipzig, Germany DA - 25.10.2001 KW - räumliches Auflösungsvermögen KW - zerstörungsfreie Ortung KW - Echtzeit-Interpretation PY - 2001 AN - OPUS4-36559 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hosseini, Seyed T1 - Characterization and optimization of ultrasonic tests for the inspection of fiber-reinforced plastic composites N2 - Applications of fibre reinforced plastic (FRP) composites in modern industries are increasing due to their considerable advantages such as light weight and excellent mechanical properties. Accordingly, importance of operational safety of modern structures made of advanced composites by ensuring the material quality has led to increasing demands for development of non-destructive evaluation (NDE) systems. In the context of a European project entitled “Validated Inspection Techniques for Composites in Energy Applications” (VITCEA), the aim is to develop and validate traceable procedures for novel NDE techniques with contrasting damage detection capabilities in energy related applications such as wind and marine turbine blades, nacelles, oil and gas flexible risers. Accordingly, VITCEA focuses on optimization of ultrasonic tests (UTs) for quantitative defect detection and quality characterization of FRP structures. In this context, the present study describes the ultrasound field in heterogeneous composite materials. The theoretical predictions are compared with simulation results obtained from CIVA a software package dedicated to NDT simulations based on the asymptotic ray theory. T2 - WCNDT 2016 CY - München, Germany DA - 13.06.2016 KW - analytical approach KW - ultrasonic tests KW - composite KW - wave propagation PY - 2016 AN - OPUS4-36563 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mielentz, Frank T1 - Zerstörungsfreie Risscharakterisierung in Betonbauteilen mit Ultraschall N2 - Die Risstiefenbestimmung in Festen Fahrbahnen ist hinsichtlich der Dauerhaftigkeit der Konstruktion von wesentlichem Interesse. Im Rahmen eines gemeinsamen Forschungsvorhabens mit der DB AG wurden aus der Literatur bekannte Ansätze bewertet und darauf aufbauend ein Verfahren zur bildgebenden Rissdarstellung entwickelt. Rissüberbrückende Bewehrung sowie Kontaktstellen zwischen den Rissflanken wirken als Schallbrücken und erschweren die Risscharakterisierung, wie bei einem Einsatz an einer Betriebserprobungsstrecke festgestellt wurde. Ein aus der Literatur bekanntes Verfahren der einfachen Laufzeitmessung erwies sich für die Tiefenbestimmung von realen verunreinigten Rissen als ungeeignet. T2 - Fachtagung Bauwerksdiagnose - Praktische Anwendungen Zerstörungsfreier Prüfungen CY - Leipzig, Germany DA - 25.10.2001 KW - Risstiefenbestimmung KW - Laufzeitmessung KW - bildgebende Rissdarstellung PY - 2001 AN - OPUS4-36564 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram T1 - Homogeneity and stability testing of (C)RM N2 - The paper describes approaches to homogeneity and stability testing of (certified) reference materials which meet the requirements of ISO 17034. T2 - IDMS Training at BAM CY - BAM, Berlin, Germany DA - 22.02.2016 KW - Reference materials KW - Homogeneity KW - Stabilty PY - 2016 AN - OPUS4-36820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Multivariate statistics applied to MALDI-TOF MS data of pollen samples N2 - Pollen represent one major cause for human allergic diseases. Currently the characterization and identification of pollen is time-consuming since it mainly relies on the microscopic determination of the genus-specific pollen morphology. A variety of new analytical approaches, like Raman - and fluorescence spectroscopy have been proposed in order to develop fast and reliable pollen identification. Recently matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) was initially applied for the rapid investigation of such complex biological samples. Taxonomic differences and relations of single pollen grains could be identified. Both commercially available lyophilized pollen and fresh pollen acquired from biological samples collected in parks and in the Botanical Garden Berlin in the years 2013-2015 were investigated. The samples were prepared by formic acid extraction in the gas phase and spotted with HCCA matrix. A variety of new approaches, like a newly developed MALDI target with micrometer sample spots sizes, were tested for their suitability. The obtained mass spectral data were investigated by principal component analysis (PCA). The applicability of MALDI-TOF mass spectrometry for the classification of pollen according to their taxonomic relationships was proven. Specifically, chemical differences in the mass spectra at the levels of plant order, genus and in many cases even of species could be identified. Based on these results, further investigations have been undertaken to optimize the sample preparation for the classification of single pollen grains in mixtures of pollens. A novel MALDI-target design was developed to enhance the phenotypic information of pollens in their mass spectra. The combination of mass spectral patterns and multivariate statistics provide a powerful tool for the investigation of structural correlations within mixtures. The results can be used to improve the reconstruction of taxonomic relations of single species in various mixtures and might be useful for the development of a fast routine method to identify pollen based on mass spectrometry. T2 - 64th ASMS Conference on Mass Spectrometry and Allied Topics CY - San Antonio, TX, USA DA - 05.06.2016 KW - Pollen KW - MALDI-TOF Mass Spectrometry KW - Multivariate statistics PY - 2016 AN - OPUS4-36837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, Nele A1 - Dietrich, Paul M. A1 - Lippitz, Andreas A1 - Kulak, N. A1 - Unger, Wolfgang T1 - New azidation methods for the functionalization of silicon nitride and application in copper-catalyzed azide-alkyne cycloaddition (CuAAC) N2 - In this study, a new direct functionalization method of silicon nitride (Si3N4) using azidation and click chemistry is presented. First, amino groups (NHx) were created on a Si3N4 substrate by fluoride etching. These NHx-terminated Si3N4 surfaces were analyzed by chemical derivatization X-ray photoelectron spectroscopy (CD-XPS) with 4-trifluoromethylbenzaldehyde (TFBA) and a derivatization yield of 20% was concluded. In the second step freshly prepared NHx surfaces were transformed into azides which were used immediately in a click reaction with halogenated alkynes. The presented combination of amination, azidation and click reaction is a promising alternative for common silane-based Si3N4 functionalization methods. T2 - 16th European Conference on Applications of Surface and Interface Analysis CY - Granada, Spain DA - 28.09.2015 KW - XPS KW - Azidation KW - Click chemistry KW - Silicon nitride KW - Chemical derivatization PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/sia.5950/full DO - https://doi.org/10.1002/sia.5950 VL - 48 SP - 621 EP - 625 PB - John Wiley & Sons, Ltd AN - OPUS4-36841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Möhlmann, Lennart T1 - Investigation on the photocatalytic degradation of toluene, butyl acetate and limonene under UV and visible light irradiation N2 - The photocatalytic degradation of three indoor air relevant volatile organic compounds (VOC), namely toluene, butylacetate (BuAc) and limonene was investigated both under UV and visible light using modified TiO2 as photcatalyst. The new materials feature a high reactivity under UV light and, compared to pure TiO2, a significantly enhanced reactivity under blue light irradiation for the decomposition of BuAc (up to 39% degradation). T2 - 9th European meeting on Solar Chemistry and Photocatalysis: Environmental Applications (SPEA) CY - Straßburg, France DA - 13.06.2016 KW - Photocatalysis KW - TiO2 KW - VOC degradation KW - Air purification PY - 2016 AN - OPUS4-36824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Gottlieb, Cassian A1 - Millar, Steven A1 - Wiggenhauser, Herbert T1 - Laser induced breakdown spectroscopy (LIBS) – automated 2D chemical analysis of concrete N2 - Laser-induced breakdown spectroscopy (LIBS) is a combination of laser ablation and optical emission spectroscopy. Due to the possibility of direct measurements on the sample surface with a minimum of sample preparation investigations of building materials can be conducted quite fast. In combination with a scanning technique (translation stage or scanning mirrors head) 2D element distributions of harmful species like chlorides and alkalis are evaluated with a sub-mm resolution. By scanning a surface of typically 100 mm x 100 mm the heterogeneity of the material may be considered. LIBS is capable to identify hot spots in element concentration with a resolution of 0.1 mm or even smaller. A LIBS-system for the on-site application on building materials is, in cooperation with system developers and companies which will use this technique for investigation on real structures, under test at BAM. We present an example. Further work will focus on providing guidelines to establish LIBS as a standard procedure for chemical investigations of building materials. T2 - NDE / NDT for Highway and Bridges: Structural Materials Technology CY - Portland, Oregon, USA DA - 29.08.2016 KW - LIBS KW - Concrete KW - Chloride KW - Chemical analysis PY - 2016 SN - 978-1-57117-392-8 SP - 155 EP - 160 PB - The American Society for Nondestructive Testing, Inc. CY - Columbus, OH 43228-0518, USA AN - OPUS4-37679 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel T1 - Measurement of hydrogen distributions in metals by neutron radiography and tomography N2 - In recent years, the optimization of the imaging stations at research reactors and especially the further development of the neutron detectors allowed the measurement of hydrogen distributions with increasing spatial and temporal resolution at lower detection limits at the same time. Hydrogen has compared to iron a high total neutron cross section, which allows with basic radiographic methods the visualization of hydrogen in two and three dimensions inside the microstructure of components. This enables the in situ measuring of hydrogen mass flows inside cm thick steel samples with a temporal resolution of 20 s as well as the quantitative measurement of hydrogen accumulations at the crack’s inner surfaces in hydrogen embrittled iron samples. For the first time, we detected directly gaseous hydrogen in the crack cavities and we could measure the gas pressure. This new quality of the information on a micrometer scale allows new insights for the analysis of damage mechanisms, e.g. of hydrogen embrittlement. Further, this method is non-destructive and provides local information in situ and in three dimensions with a spatial resolution of 20-30 µm, which is not accessible with common methods as e.g. thermal desorption spectroscopy. In this contribution, we show examples that demonstrate the spatial and temporal resolution of the neutron radiography and tomography method in order to visualize and quantify hydrogen accumulations at cracks. The measurements were performed at the research reactor BER II of HZB in Berlin and at the FRM II reactor of the neutron source Heinz Maier-Leibnitz in Garching. T2 - 2016 International Hydrogen Conference CY - Moran, Wyoming, USA DA - 11.09.2016 KW - Neutron imaging KW - Hydrogen embrittlement KW - Neutron tomography KW - Neutron radiography PY - 2016 AN - OPUS4-37700 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Galindo Guerreros, Julio Cesar A1 - Mackens, S. A1 - Niederleithinger, Ernst A1 - Fechner, T. ED - Manzanal, D. ED - Sfriso, A. O. T1 - Numerical simulations of crosshole and downhole seismic measurements as quality control tool for jet grout columns N2 - Sealing and strengthening of the subsoil by injection is a major issue in the field of geotechnical engineering. This involves also jet grouting, which allows creating columns of grouted soil by eroding and mixing the in-situ soil with a thin cement suspension. A general difficulty of this method is to predict the column diameter and its material strength. Here, we present two-dimensional finite-difference numerical simulation results of a promising non-destructive quality assurance testing tool to evaluate the diameter of jet grout columns. This approach incorporates crosshole and downhole seismic measurements. Preliminary tests showed that this tool is applicable under real site conditions. T2 - 15th Pan-American Conference on Soil Mechanics and Geotechnical Engineering CY - Buenos Aires, Argentina DA - 15.11.2015 KW - Jet grout KW - Diameter KW - Seismic KW - Crosshole KW - Downhole KW - FD KW - Quality control tool PY - 2015 SN - 978-1-61499-603-3 SN - 978-1-61499-602-6 DO - https://doi.org/10.3233/978-1-61499-603-3-985 SP - Part 1, 985 EP - 992 PB - IOS Press AN - OPUS4-37706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hartmann, S. A1 - Shaporin, A. A1 - Hermann, S. A1 - Bonitz, J. A1 - Heggen, M. A1 - Meszmer, P. A1 - Sturm, Heinz A1 - Hölck, O. A1 - Blaudeck, T. A1 - Schulz, S. E. A1 - Mehner, J. A1 - Gessner, T. A1 - Wunderle, B. T1 - Towards nanoreliability of CNT-based sensor applications: Investigations of CNT-metal interfaces combining molecular dynamics simulations, advanced in situ experiments and analytics N2 - In this paper we present results of our recent efforts to understand the mechanical interface behaviour of single-walled carbon nanotubes (CNTs) embedded in metal matrices. We conducted experimental pull-out tests of CNTs embedded in Pd or Au and found Maximum forces in the range 10 - 102 nN. These values are in good agreement with forces obtained from molecular Dynamics simulations taking into account surface functional Groups (SFGs) covalently linked to the CNT material. The dominant failure mode in experiment is a CNT rupture, which can be explained with the presence of SFGs. To qualify the existence of SFGs on our used CNT material, we pursue investigations by means of fluorescence labeling of surface species in combination with Raman imaging. We also report of a tensile test system to perform pull-out tests inside a transmission electron microscope to obtain in situ images of CNT-metal interfaces under mechanical loads at the atomic scale. T2 - 2015 16th International Conference on Thermal, Mechanical and Multi-Physics Simulation and Experiments in Microelectronics and Microsystems CY - Budapest, Hungary DA - 20.4.2015 KW - Carbon nanotube CNT KW - Metal matrix KW - Pull-out test KW - Molecular dynamics simulation KW - Surface functional groups KW - Fluorescence labeling KW - Raman imaging KW - Tensile test inside a TEM PY - 2015 SN - 978-1-4799-9950-7 VL - 2015 SP - 1 EP - 8 PB - IEEE AN - OPUS4-37625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Polymer characterisation by multidimensional techniques with focus on LC - MALDI/ESI-TOF-MS N2 - Since the first LC/ ESI-MS experiment of the Nobel prize winner John B. Fenn in 1984, the coupling of liquid chromatographic to mass spectrometric techniques gained a continuous rapid development. The lecture will give a general survey of different LC separation techniques as size exclusion chromatography (SEC), liquid adsorption chromatography (LAC), liquid chromatography at critical conditions (LCCC) and gradient elution liquid chromatography (GELC) combined with Matrix assisted Laser Desorption Ionization (MALDI) respectively Electrospray Ionization (ESI) Time of Flight (TOF) mass spectrometry. Often the deficiencies of stand-alone methods can be bridged. LC, blind to structural information needs mass spectrometry as one of the most powerful detectors able to give detailed information on e.g. the repeat units, functionalization or copolymer composition of the chromatographic separated constituents. A separation prior to MS reduces the polydispersity which is one of the reasons for failing of MS. Also problems with different ionization probabilities in complex mixtures can partly be overcame. On the basis of different examples on- and offline coupling principles will be compared and the pros and cons of both mass spectrometric techniques will be discussed. Recently, MALDI imaging techniques in coupling with chromatography have become interesting e.g. for visualization of copolymer composition. T2 - International Symposium GPC/SEC and Related Techniques CY - Amsterdam, The Netherlands DA - 26.09.2016 KW - Polymers KW - Liquid chromatography KW - MALDI-TOF-MS KW - ESI-TOF-MS PY - 2016 AN - OPUS4-37629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Epping, Ruben T1 - Characterization of statistical EO-PO copolymers containing different end groups by UPLC/ESI-MS N2 - Commercial statistical ethylene oxide (EO) and propylene oxide (PO) copolymers of different monomer compositions and different average molar masses were studied by liquid chromatography under critical conditions (LCCC). Theoretical predictions of the existence of a critical adsorption point (CPA) for statistical copolymers with a given chemical and sequence distribution, could be studied and confirmed. An improved way to determine these critical conditions in a copolymer, alongside the inevitable chemical composition distribution (CCD), with the aid of mass spectrometric detection is described. Shift of the critical eluent composition with the monomer composition of the polymers could be observed. Due to the relatively low average molecular weight, broad molecular weight distribution (MWD) and the presumed existence of different end group functionalities as well as sequence distribution, gradient separation only by CCD was not possible. Therefore isocratic separations at the CPA of definite CCD’s were applied. Although the various present distributions partly superimposed the separation process the goal of separation by end group functionality could still be achieved on the basis of the additional dimension of ESI-MS. The existence of HO-H besides the desired AllylO-H end group functionalities could be confirmed and their amount could be estimated. T2 - International Symposium GPC/SEC and Related Techniques CY - Amsterdam, The Netherlands DA - 26.09.2016 KW - Polymers KW - UPLC KW - ESI-TOF-MS PY - 2016 AN - OPUS4-37632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schade, U. T1 - Estimation of THz waveforms for material characterization of stratified objects N2 - The poster discusses theoretically and exemplarily the influence of the materials and experimentally selected situation on the shape and size deformation of a detected pulse signal previously reflected on a three layer sheet. T2 - 41st International Conference on Infrared, Millimeter, and Terahertz Waves (IRMMW-THz 2016) CY - Copenhagen, Denmark DA - 25.09.2016 KW - THz spectroscopy KW - Pulse reflection KW - Pulse shape analysis KW - Optical layer model PY - 2016 AN - OPUS4-37639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Esche, E. A1 - Müller, D. A1 - Maiwald, Michael A1 - Wozny, G. T1 - Raman-based advanced control of an absorption desorption system N2 - For absorption processes with fluctuating feed gas compositions it is vital to continuously adjust the operation point to achieve energy efficiency. In this contribution a Raman-based advanced process control (APC) is introduced for the absorption of carbon dioxide (CO2) using an aqueous solution of monoethanolamine (MEA). The APC is based on a Raman spectroscopic analysis of the composition and CO2 load of the scrubbing liquid and a non-linear model predictive control (NMPC) to adjust the scrubbing liquid cycle. In addition, an outer real-time optimization loop is set in place to update the set points for the absorption process depending on the current feed gas composition minimizing the energy consumption of the process. Implementation and testing of the APC have been carried out in a mini-plant at TU Berlin. During a plant operation of more than 160 hours robustness and stability of the APC were shown. T2 - 12th International Symposium on Process Systems Engineering and 25th European Symposium on Computer Aided Process Engineering CY - Kopenhagen, Denmark DA - 31.05.2015 KW - Raman spectroscopy KW - Advanced process control KW - CO2 KW - Carbon dioxide KW - Absorption KW - Process analytical technology PY - 2015 UR - https://www.elsevier.com/books/12th-international-symposium-on-process-systems-engineering-and-25th-european-symposium-on-computer-aided-process-engineering/author/978-0-444-63429-0 SN - 9780444634290 SN - 9780444634450 VL - 37 SP - 1523 EP - 1528 PB - Elsevier CY - Amsterdam AN - OPUS4-37669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schukar, Vivien A1 - Köppe, Enrico A1 - Hofmann, Detlef A1 - Westphal, Anja A1 - Sahre, Mario A1 - Gong, Xin A1 - Bartholmai, Matthias A1 - Beck, Uwe T1 - Magnetic field detection with an advanced FBG-based sensor device N2 - A high-performance fiber Bragg grating-based (FBG) sensor device has been developed for the detection of small magnetic fields. Based on a smart multilayer jacket around the fibre over the physical length of the FBG, magnetic fields generated by rotating machine parts, power generators or power cable can be easily detected, analysed and evaluated. Consequently, this innovative, on-line and non-contact inspection method results in an increase in quality and reliability of high-performing machine parts, devices and cables. The basic physical principle is based on a magnetostrictive multilayer system that strains the high-resolution FBG element in presence of magnetic fields. Subsequently, a fixed relationship between induced magnetic field and wavelength change of the FBG element describes the characteristic sensitivity curve. Intensive tests regarding characterisation of this magnetic field FBG sensor have been carried out and its performance has been evaluated. T2 - 30th Eurosensors Conference, EUROSENSORS 2016 CY - Budapest, Hungary DA - 04.09.2016 KW - Fiber Bragg grating KW - Magnetostriction KW - Strain KW - Magnetic field PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-376703 DO - https://doi.org/10.1016/j.proeng.2016.11.445 SN - 1877-7058 VL - 168 SP - 1270 EP - 1274 PB - Elsevier Ltd. AN - OPUS4-37670 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Marc Benjamin A1 - Uhlig, F. A1 - Solomun, Tihomir A1 - Smiatek, J. A1 - Sturm, Heinz T1 - Combined influence of ectoine and salt: spectroscopic and numerical evidence for compensating effects of aqueous solutions N2 - Ectoine is an important osmolyte, which allows microorganisms to survive in extreme environmental salinity. The hygroscopic effects of ectoine in pure water can be explained by a strong water binding behavior whereas a study on the effects of ectoine in salty solution is yet missing. We provide Raman spectroscopic evidence that the influence of ectoine and NaCl are opposing and completely independent of each other. The effect can be explained by the formation of strongly hydrogen-bonded water molecules around ectoine which compensate the influence of the salt on the water dynamics. The mechanism is corroborated by first principles calculations and broadens our understanding of zwitterionic osmolytes in aqueous solution. Our findings allow us to provide a possible explanation for the relatively high osmolyte concentrations in halotolerant bacteria. KW - Ectoine KW - Aqueous solution KW - Biological structure KW - Organic osmolytes KW - Raman spectroscopy KW - Water structure PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-376761 UR - http://pubs.rsc.org/en/content/articlelanding/2016/cp/c6cp05417j#!divAbstract DO - https://doi.org/10.1039/c6cp05417j VL - 18 IS - 41 SP - 28398 EP - 28402 PB - Royal Society of Chemistry CY - UK AN - OPUS4-37676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Coda wave interferometry used for monitoring of concrete constructions N2 - Ultrasonic transmission measurements on concrete; embedded transducers; coda wave interferometry to check for subtle chnages in velocity as indicator for various loads or deterioration. T2 - 76. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Münster, Germany DA - 14.03.2016 KW - Ultrasound KW - Transmission KW - Coda wave interferometry KW - Concrete KW - Load PY - 2016 AN - OPUS4-37721 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Electronic Reference Images for Flaw Indications in Welds and Castings N2 - The state of art in electronic flaw catalogues is discussed. The conversion to digital radiography is in full progress. A series of catalogues with reference images of flaw indications are on the way at ASTM, IIW and DGZfP. All are supported by hi-res film digitization at BAM Berlin. T2 - WCNDT 2016 CY - Munich, Germany DA - 13.06.2016 KW - Castings KW - NDT KW - RT KW - Radiography KW - Discontinuities KW - Catalogues KW - Welds PY - 2016 AN - OPUS4-37729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zscherpel, Uwe A1 - Ewert, Uwe T1 - Electronic reference images for flaw indications in welds and castings N2 - Since decades the evaluation of flaw indications on radiographs from welds or castings are based on well accepted reference film catalogues from organizations like IIW (weldments), ASTM (castings) or DGZfP (D5 recommendation on heavy steel castings). Today, the transformation of classical film radiography to the digital world is in full progress. Some ASTM standards do not permit the evaluation of digital radiographs in reference to film catalogues. Therefore, these reference film catalogues have to be converted into the digital age too. BAM is supporting this transition by high definition film scanning. The result is a corresponding reference image catalogue. The different standard organizations selected different ways to distribute the digital data. ASTM used high definition film scanning at 10 μm pixel size and distribution of a huge amount of high-res data via DVD. The user sub-samples these high-res data during catalogue import to the resolution of his system. The comparison is done by synchronized image viewing on the computer work station. IIW recently decided to distribute their ISO 5817 reference images installed on tablets, which are used for image viewing too. The tablet image has to be compared with the digital image on the system monitor. DGZfP transformed their D5 reference radiographs into a PDF for monitor viewing. This is the simplest and cheapest solution, but still allows the full usage of the catalogue in the digital era. The status of ongoing work in progress will be discussed. T2 - WCNDT 2016 CY - Munich, Germany DA - 13.06.2016 KW - Castings KW - NDT KW - RT KW - Radiography KW - Discontinuities KW - Catalogues KW - Welds PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-377306 UR - http://ndt.net/?id=19310 SN - 1435-4934 VL - 21 IS - 7 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-37730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zscherpel, Uwe A1 - Poeppl, J. T1 - Mit digitaler Radiologie verborgenen Fehlern auf der Spur N2 - Der Stand der Technik beim digitalen Filmersatz in der Gussteilpruefung in Giessereien wird betrachtet.Eine Reihe von Normen fuer den Ersatz des Roentgenfilms durch neue digitale Detektoren wurde in den letzten Jahren veroeffentlicht. Die verschiedene Fehlertypen werden mit Fehlerkatalogen bewertet, die ebenfalls digital verfuegbar sind. Die Bildverarbeitung gestattet eine einfachere Bewertung der Anzeigen. Eine automatische Bewertung von Gussteilen durch den Computer erlaubt vollautomatische Anlagen, die 10 000 Teile pro Tag pruefen. KW - Film replacement KW - NDT KW - RT KW - Radiography KW - Discontinuities KW - Catalogues KW - Castings KW - Durchstrahlungsprüfung KW - Automatische Bildbewertung KW - Bildverarbeitung KW - Gussteilprüfung KW - Standardisierung KW - Filmersatz durch digitale Detektoren KW - Zerstörungsfreie Prüfung PY - 2016 VL - 103 IS - 6 SP - 85 EP - 87 PB - GIESSEREI-Verlag GmbH CY - Düsseldorf AN - OPUS4-37731 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mery, D. A1 - Riffo, V. A1 - Zscherpel, Uwe A1 - Mondragon, G. A1 - Lillo, I. A1 - Zuccar, I. A1 - Lobel, H. A1 - Carrasco, M. T1 - GDXray: The Database of X-ray Images for Nondestructive Testing N2 - In this paper, we present a new dataset consisting of 19,407 X-ray images. The images are organized in a public database called GDXray that can be used free of charge, but for research and educational purposes only. The database includes five groups of X-ray images: castings, welds, baggage, natural objects and settings. Each group has several series, and each series several X-ray images. Most of the series are annotated or labeled. In such cases, the coordinates of the bounding boxes of the objects of interest or the labels of the images are available in standard text files. The size of GDXray is 3.5 GB and it can be downloaded from our website. We believe that GDXray represents a relevant contribution to the X-ray testing community. On the one hand, students, researchers and engineers can use these X-ray images to develop, test and evaluate image analysis and computer vision algorithms without purchasing expensive X-ray equipment. On the other hand, these images can be used as a benchmark in order to test and compare the performance of different approaches on the same data. Moreover, the database can be used in the training programs of human inspectors. KW - Data base KW - NDT KW - RT KW - Digital image catalogues KW - Security PY - 2015 DO - https://doi.org/10.1007/s10921-015-0315-7 SN - 0195-9298 VL - 34 IS - 4 SP - 34 EP - 42 PB - Springer Verlag CY - Heidelberg AN - OPUS4-37732 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe A1 - Ewert, Uwe T1 - Filmersatz in der radiographischen Schweißnahtprüfung: Neue ISO-Standards und Erfahrungen im praktischen Einsatz digitaler Detektoren N2 - Der Ersatz von Röntgenfilmen durch digitale Detektoren in der zerstörungsfreien Prüfung wurde in den letzten 10 Jahren kontrovers diskutiert. Nach der Erfolgsgeschichte der digitalen Photographie und der fast vollständigen Ablösung der Filmtechnik in der optischen Bilderfassung wurde erwartet, dass sich der Übergang von der Filmradiographie zur digitalen Radiographie schnell vollziehen sollte. Dieser Trend ist derzeit so noch nicht zu beobachten. Zur mobilen Prüfung wird in Europa immer noch vorrangig die Filmradiographie und nur teilweise die Speicherfolientechnik eingesetzt. Im Bereich der stationären Prüftechnik haben sich die Matrixdetektoren (DDA) weitgehend durchgesetzt, wobei es auch hier noch alternative Detektoren wie Bildverstärker und Fluoroskope gibt. Mit Einführung der DIN EN ISO 17636-2 wird seit 2013 erstmalig geregelt, wie man einen digitalen Detektor für die technische Radiographie auswählen soll, um im Vergleich zur Filmradiographie eine äquivalente Bildqualität zu erhalten. Essentielle Parameter bestimmen, ob die geforderte Bildgüte erreicht werden kann. Es wird ein Überblick gegeben, welche Parameter zum praktischen Einsatz wichtig sind und wie sie ermittelt werden. Erste Erfahrungen im praktischen Einsatz werden diskutiert. T2 - Sondertagung "Schweissen im Anlagen- und Behälterbau" 2016 CY - Munich, Germany DA - 23.02.2016 KW - Welds KW - RT KW - Radiography KW - NDT KW - Discontinuities KW - Catalogues KW - Zerstörungsfreie Prüfung KW - Praktische Erfahrungen KW - Standardisierung KW - Durchstrahlungsprüfung KW - Filmersatz durch digitale Detektoren PY - 2016 SN - 978-3-945023-59-4 VL - 322 SP - 55 EP - 58 PB - DVS Media CY - Düsseldorf AN - OPUS4-37733 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Filmersatz in der radiographischen Schweißnahtprüfung: Neue ISO-Standards und Erfahrungen im praktischen Einsatz digitaler Detektoren N2 - Der Ersatz von Röntgenfilmen durch digitale Detektoren in der zerstörungsfreien Prüfung wurde in den letzten 10 Jahren kontrovers diskutiert. Nach der Erfolgsgeschichte der digitalen Photographie und der fast vollständigen Ablösung der Filmtechnik in der optischen Bilderfassung wurde erwartet, dass sich der Übergang von der Filmradiographie zur digitalen Radiographie schnell vollziehen sollte. Dieser Trend ist derzeit so noch nicht zu beobachten. Zur mobilen Prüfung wird in Europa immer noch vorrangig die Filmradiographie und nur teilweise die Speicherfolientechnik eingesetzt. Im Bereich der stationären Prüftechnik haben sich die Matrixdetektoren (DDA) weitgehend durchgesetzt, wobei es auch hier noch alternative Detektoren wie Bildverstärker und Fluoroskope gibt. Mit Einführung der DIN EN ISO 17636-2 wird seit 2013 erstmalig geregelt, wie man einen digitalen Detektor für die technische Radiographie auswählen soll, um im Vergleich zur Filmradiographie eine äquivalente Bildqualität zu erhalten. Essentielle Parameter bestimmen, ob die geforderte Bildgüte erreicht werden kann. Es wird ein Überblick gegeben, welche Parameter zum praktischen Einsatz wichtig sind und wie sie ermittelt werden. Erste Erfahrungen im praktischen Einsatz werden diskutiert. T2 - Sondertagung "Schweissen im Anlagen- und Behälterbau" 2016 CY - Munich, Germany DA - 23.02.2016 KW - Standardss KW - NDT KW - RT KW - Radiography KW - Discontinuities KW - Catalogues KW - Welds KW - Zerstörungsfreie Prüfung KW - Gussteilprüfung KW - Standardisierung KW - Filmersatz durch digitale Detektoren KW - Durchstrahlungsprüfung KW - Bildverarbeitung KW - Automatische Bildbewertung PY - 2016 AN - OPUS4-37734 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane T1 - Comparison of concepts for a point-shaped energy density detector after flash lamp excitation N2 - The paper describes investigations and Research work in order to develop a simple sensor for the quantification of spectral broadband energy Dissipation of flash lamps at any point in space. Such Flash lamps are often used as energy source during active thermography testing (TT). Here, the temperature transient of the sensor surface has to be recorded by the infrared camera that is already present. During the following data evaluation, the energy input into the investigated specimen can be determined. Two opposite concepts were considered: thermal thick and thermal thin probes. The direct comparison shows advantages for thermal thick probes based on the physics of thermal balance processes. KW - Flash thermography KW - Non-destructive testing KW - Flash lamp KW - Energy dissipation KW - Energy sensor PY - 2016 DO - https://doi.org/10.3139/120.110939 SN - 0025-5300 VL - 58 IS - 10 SP - 887 EP - 893 PB - Carl Hanser Verlag CY - München AN - OPUS4-37650 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kästner, Claudia A1 - Thünemann, Andreas T1 - Tracking silver nanoparticles: ultra-small silver refunctionalizable with fluorescent biopolymers N2 - We report on the synthesis of ultra-small silver nanoparticles and their quantitative characterization by small-angle X-ray scattering. The size distribution was derived by utilizing a Monte-Carlo data evaluation procedure reported by Pauw et al. Mean volume-weighted sizes are 3 nm with a size distribution width of 18 %. The particles should be used as reference materials for comparison of the result of different analytical methods among which are field-flow fractionation (FFF), dynamic light scattering (DLS), nanoparticle tracking analysis (NTA) and electron microscopy (EM). In addition further use of the particles is foreseen for comparison of studies on the toxicology of nanoparticles. Therefore the silver nanoparticles are transfunctionalized with fluorescent marked albumin (BSA-FITC) and also thoroughly characterized. With this it is possible to track silver nanoparticles and their behavior in interaction with cells. T2 - Polydays 2016 CY - Potsdam, Germany DA - 28.09.2016 KW - SAXS KW - Biological application KW - Ligand exchange KW - Toxicity PY - 2016 AN - OPUS4-37651 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Werner, Klaus-Dieter A1 - Petrov, Sergej A1 - Bartholmai, Matthias A1 - Lazik, D. ED - Puente León, F. ED - Zagar, B. T1 - Aufbau eines großflächigen Testfeldes für verteilte Bodengassensorik und Untersuchung einer Monitoringmethode basierend auf Tomographie T1 - Setup of a large-scale test field for distributed soil gas sensors and testing of a monitoring method based on tomography N2 - A 400 m² soil test field with gas injection system was built up for the purpose of large-scale validation, optimization, and characterization of a novel comprehensive monitoring method for underground gas storage areas. The method combines gas sensing technology with linear form factor for in-situ monitoring of gases in soil with the mapping capabilities of Computed Tomography (CT) to reconstruct time-series of gas distribution maps based on samples of orthogonally-aligned linear gas sensors. Several injection experiments with carbon dioxide (CO2) at different days with varying boundary conditions indicates the potential of the method for, e.g., rapid leakage detection with respect to Carbon Capture and Storage (CCS) issues. N2 - Zur Validierung, Optimierung und praxisnahen Demonstration eines flächendeckenden Monitoringverfahrens für Untergrundgasspeichern wurde ein 400 m² großes Testfeld mit Gasinjektionssystem auf dem BAM Testgelände Technische Sicherheit aufgebaut. Die Methode kombiniert verteilte, linienförmige Gassensorik für die In-situ-Überwachung von Gasen im Boden mit den Mapping-Fähigkeiten der Computertomographie (CT). Auf Basis von orthogonal zueinander ausgerichteten linearen Gassensoren können mit diesem Verfahren so Zeitreihen der Gasverteilung rekonstruiert werden. Experimente mit Kohlendioxid (CO2) zeigen das Potential des Verfahrens zur schnellen Lokalisierung von Leckagen auf. KW - Soil test field KW - Distributed linear sensor KW - Membrane-based gas sensing KW - Subsurface monitoring KW - Gas storage areas KW - Computed tomography PY - 2016 DO - https://doi.org/10.1515/teme-2016-0015 SN - 2196-7113 SN - 0171-8096 VL - 83 IS - 10 SP - 606 EP - 615 PB - Walter de Gruyter GmbH CY - Berlin, Deutschland AN - OPUS4-37653 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rietz, U. A1 - Lange, Thorid A1 - Hielscher, Stefan A1 - Beck, Uwe A1 - Kavianpour, D. A1 - Lerche, D. T1 - Quantitative determination of adhesive tape properties by CAT-technology (centrifugal adhesion testing) N2 - The future commercial prospects for adhesive tapes are very good and its application range is very broad. From every-day-use in office, packaging, maintenance, and quick repair in workshops, it ranges from handicraft work, medical purposes and cosmetics up to workmanship. The study describes a new multi-sample approach in adhesive tape testing from theoretical background, preparation of test specimen for tensile as well as shear testing, detailed measurement procedures up to analysis and result interpretation. Various types of single and double-sided pressure sensitive adhesive tapes supplied by different manufacturers were investigated and compared T2 - EURADH 2016 Adhesion ´16 CY - Glasgow, UK DA - 21.09.2016 KW - Tensile KW - Shear KW - Peel KW - Strength KW - Analytical centrifugation KW - Adhesive tapes PY - 2016 SP - 352 EP - 355 AN - OPUS4-37664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Worldwide BAM Certification of Radigraphic Image Detectors for the NDT Market – Status of 2016 N2 - Der Status der weltweiten BAM Zertifizierung im Bereich Zerstörungsfreie Prüfung für radiographisch Bilddetektoren wird dargestellt sowie die an der BAM geschaffenen normativen Grundlagen dazu. N2 - The Poster shows the status of 2016 in BAM certification of radiographic image detectors for industrial radiology for nondestructive testing. BAM was generating first the basis by worldwide standardization activities and released later certificates on request of the device manufacturers using these Standards a base for certification. T2 - BAM-Evaluierung durch den Wissenschaftsrat 2016 CY - Berlin, Germany DA - 16.02.2016 KW - Castings KW - NDT KW - RT KW - Radiography KW - Discontinuities KW - Catalogues KW - Welds PY - 2016 AN - OPUS4-37735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weller, Michael G. T1 - Methods for immunoaffinity extraction – Setup and characterization N2 - Affinity extraction is one of the most powerful separation methods. Regarded to be indispensable in some research fields, such as proteomics, the application in other fields is still scarce or even waning. Many researchers fear the perceived complexity, cost and unreliability of this approach. The presentation gives a broad overview of the most important methods and discusses some important points for their implementation. Having considered these aspects, it should be easier to establish an affinity separation approach to resolve challenging analytical questions. T2 - Seminar des Max-Planck-Instituts für Chemie (MPIC) CY - Mainz, Germany DA - 28.09.2016 KW - affinity chromatography KW - immunoaffinity KW - antibodies KW - sample preparation KW - bioanalysis PY - 2016 AN - OPUS4-37736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lühr, T. A1 - Winkelmann, Aimo A1 - Nolze, Gert A1 - Krull, D. A1 - Westphal, C. T1 - Direct Atom Imaging by Chemical-Sensitive Holography N2 - In order to understand the physical and chemical properties of advanced materials, functional molecular adsorbates, and protein structures, a detailed knowledge of the atomic arrangement is essential. Up to now, if subsurface structures are under investigation, only indirect methods revealed reliable results of the atoms’ spatial arrangement. An alternative and direct method is three-dimensional imaging by means of holography. Holography was in fact proposed for electron waves, because of the electrons’ short wavelength at easily accessible energies. Further, electron waves are ideal structure probes on an atomic length scale, because electrons have a high scattering probability even for light elements. However, holographic reconstructions of electron diffraction patterns have in the past contained severe image artifacts and were limited to at most a few tens of atoms. Here, we present a general reconstruction algorithm that leads to high-quality atomic images showing thousands of atoms. Additionally, we show that different elements can be identified by electron holography for the example of FeS₂ . KW - holography KW - electron diffraction KW - atomic imaging KW - photoemission KW - electron backscattering PY - 2016 DO - https://doi.org/10.1021/acs.nanolett.6b00524 VL - 16 IS - 5 SP - 3195 EP - 3201 PB - American Chemical Society AN - OPUS4-37739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietrich, D. A1 - Nolze, Gert A1 - Mehner, T. A1 - Nickel, D. A1 - Lampke, T. T1 - EDS/EBSD studies and HR-EBSD pattern analysis on pre-Inca ceramic fragments recovered during San José de Moro Archaeology Program N2 - Pre-Inca civilizations like the coastal cultures Moche and Nazca (Early Intermediate) and the inland culture Wari (Middle Horizon) were agrarian societies which supported indigenous elites of impressive wealth, power, and organization. With the expansion of the Wari Empire, the polychrome style and technique of Nazca propagated to the other cultures. High status burials, most of the Late Moche Fine Line ceramics and a large corpus of ceramics with Wari-derived decoration have been recovered in San José de Moro since 1991. The degree of transfer of procedures in this highly interactive scenario is of special interest: is there a limitation to decoration or is it adopted by the local potters also regarding the formulation of the ceramic bodies? In this context the relative amount, size and type of incorporated non-plastic inclusions as temper are important. T2 - The 16th European Microscopy Congress 2016 CY - Lyon, France DA - 28.08.2016 KW - EBSD KW - EDX KW - Ceramic KW - Phase distribution KW - Microstructure KW - Texture KW - Phase identification KW - SEM PY - 2016 DO - https://doi.org/10.1002/9783527808465.EMC2016.4462 SP - 4462 PB - John Wiley & Sons AN - OPUS4-37740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Hielscher, R. ED - Hielscher, Ralf T1 - Orientations - perfectly colored N2 - The inverse pole figure (IPF) coloring for a suitable evaluation of crystal orientation data is discussed. The major goal is a high correlation between encoding color and crystal orientation. Revised color distributions of the fundamental sectors are introduced which have the advantages of (1) being applicable for all point groups, (2) not causing color discontinuities within grains, (3) featuring carefully balanced regions for red, cyan, blue, magenta, green and yellow, and (4) an enlarged gray center in opposition to a tiny white center. A new set of IPF color keys is proposed which is the result of a thorough analysis of the colorization problem. The discussion considers several topics: (a) the majority of presently applied IPF color keys generate color discontinuities for specifically oriented grains; (b) if a unique correlation between crystal direction and color is requested, discontinuity-preventing keys are possible for all point groups, except for 4, 3 and 1; (c) for a specific symmetry group several IPF color keys are available, visualizing different features of a microstructure; and (d) for higher symmetries a simultaneous IPF mapping of two or three standard reference directions is insufficient for an unequivocal orientation assignment. All color keys are available in MTEX, a freely available MATLAB toolbox. KW - Electron backscatter diffraction KW - Color coding KW - Symmetry groups KW - Orientation description PY - 2016 DO - https://doi.org/10.1107/S1600576716012942 SN - 0021-8898 SN - 1600-5767 VL - 49 IS - 5 SP - 1786 EP - 1802 AN - OPUS4-37741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, L. A1 - Han, M. A1 - Nolze, Gert T1 - The determination of lattice parameters using single EBSD patterns N2 - A typical electron backscatter diffraction (EBSD) pattern usually contains more than a hundred of Kikuchi poles that formed by intersecting dozens of visible Kikuchi bands. The poles correspond to zone axes in real space or lattice planes in reciprocal space. The band widths are inversely proportional to the interplanar spacings of diffracting lattice planes, and the angle formed by the beam source and two band center-lines approximately corresponds to angle between two lattice planes. However, EBSD patterns always suffer from gnomic distortions. In addition, the band width measurement has a relative error of 5-20% due to the complex profile. Thus, an EBSD pattern always provides abundant crystallographic information but disappointingly low accuracy. T2 - Microscopy & MicroAnalysis 2016 CY - Columbus, Ohio, USA DA - 24.07.2016 KW - Electron backscatter diffraction KW - Lattice parameter determination PY - 2016 UR - https://www.cambridge.org/core/services/aop-cambridge-core/content/view/S1431927616004025 SN - 1431-9276 SN - 1435-8115 VL - 22 SP - Suppl. 3, 634 EP - 635 AN - OPUS4-37742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkelmann, Aimo A1 - Nolze, Gert T1 - Orientation analysis of non-centrosymmetric crystal structures using electron backscatter diffraction N2 - Crystal structures that show a broken symmetry in their cubic and hexagonal modifications are of great relevance for optoelectronic and photonic applications. This is why methods which are sensitive to non-centrosymmetric structures are important for analysis of these materials in technological applications. T2 - 24th Annual Conference of the german Crystallographic Society CY - Stuttgart, Germany DA - 14.03.2016 KW - Electron backscatter diffraction KW - Non-centrosymmetry KW - Friedel's rule KW - Pattern matching KW - GaN KW - GaP PY - 2016 VL - 36 Supplement SP - 22 PB - Walter de Gruyter GmbH & Co KG AN - OPUS4-37743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Franziska A1 - Wenzel, Klaus-Jürgen A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Quantitative determination of activation energies in mechanochemical reactions N2 - Mechanochemical reactions often result in 100% yields of single products, making purifying procedures obsolete. Mechanochemistry is also a sustainable and eco-friendly method. The ever increasing interest in this method is contrasted by a lack in mechanistic understanding of the mechanochemical reactivity and selectivity. Recent in situ investigations provided direct insight into formation pathways. However, the currently available theories do not predict temperature T as an influential factor. Here, we report the first determination of an apparent activation energy for a mechanochemical reaction. In a temperaturedependent in situ study the cocrystallisation of ibuprofen and nicotinamide was investigated as a model system. These experiments provide a pivotal step towards a comprehensive understanding of milling reaction mechanisms. KW - Mechanochemistry KW - Cocrystal KW - Activation energy KW - Milling PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-377444 DO - https://doi.org/10.1039/c6cp04280e SN - 1463-9076 SN - 1463-9084 VL - 18 IS - 33 SP - 23320 EP - 23325 AN - OPUS4-37744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzweber, Markus T1 - Ionische Flüssigkeiten als Referenzmaterial in der Oberflächenanalytik N2 - Die Bestimmung der chemischen Zusammensetzung einer Oberfläche und deren Quantifizierung mit wichtig für die Qualitätssicherung vieler industrieller Produkte und Materialien. Die chemische Beschaffenheit von Oberflächen bzw. Grenzflächen muss genau kontrolliert werden um die Produktqualität zu garantieren. Diese Prüfung ist oft auch für individuelle Prozessschritte durchzuführen. Referenzmaterialien sind unverzichtbar, wenn es darum geht, die Richtigkeit und Zuverlässigkeit von Messergebnissen zu gewährleisten. Falsche Messwerte können zu erheblichen Mehrkosten führen. Referenzmaterialien gewährleisten die Rückführung von Messergebnissen auf anerkannte Bezugsgrößen (Standards), dienen der Ermittlung der Messunsicherheit von analytischen Verfahren und wer-den zur Kalibrierung verwendet. Für zertifizierte/akkreditierte (ISO 9000 und ISO 17025) Prüf- und Kalibrierlaboratorien ist der Einsatz von Referenzmaterialien in der Qualitätssicherung obligatorisch. Ionischen Flüssigkeiten (IL) sind vielversprechende Kandidaten für die Verwendung als Referenzmaterial in oberflächenanalytischen Verfahren wie Energie-dispersive Röntgenspektroskopie (EDX) und Röntgenphotoelektronenspektroskopie (XPS). In zwei Machbarkeitsstudien wurde eine geeignete Klasse von ILs als Referenzmaterial getestet: Für die Anwendung in EDX wurde die Eignung von ILs als Referenzmaterial zur routinemäßigen Überprüfung der Energieskala, der Energieauflösung und der Spektrometer-Effizienz untersucht. Es kann gezeigt werden, dass mit einer einzigen Messung an einem einzigen Referenzmaterial mehrere Geräteparameter überprüft werden können. Damit ist es im niederenergetischen Bereich möglich, regelmäßige Funktionsprüfungen von Spektrometern durchzuführen, aber auch die Leistungsfähigkeit verschiedener Spektrometer zu vergleichen Für Die Anwendung in XPS wurde die Eignung von ILs als Referenzmaterial zur Bestimmung der Transmissionsfunktion T(E) von Photoelektronenspektrometern getestet. Dazu wurde die Auswertesoftware UNIFIT entsprechend adaptiert und erlaubt nun T(E) anhand der bekannten Stöchiometrie der IL zu ermitteln. Es wird gezeigt, dass durch die Verwendung ausgewählter ILs als Referenzmaterial die Genauigkeit der Quantifizierung von XPS Daten unter Nutzung einer experi-mentell bestimmten T(E) wesentlich verbessert werden kann. T2 - 19. Arbeitstagung Angewandte Oberflächenanalytik CY - Soest, Germany DA - 05.09.2016 KW - Ionische Flüssigkeiten KW - Referenzmaterial KW - REM-EDX KW - XPS PY - 2016 AN - OPUS4-37640 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Schukar, Vivien T1 - Intelligent automatic validation of structure-integrated fibre optic strain sensors N2 - Identification of physical faulty fibre optic strain sensors embedded in safety-relevant structures or systems and detection of abnormal measurement data to prevent misinterpretation of critical operating parameters and misleading of management and control systems. T2 - 33rd Danubia- Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Fiber bragg grating KW - Magnetic field KW - Magnetostrictive metal coating KW - Self-diagnostic fiber optical sensor PY - 2016 AN - OPUS4-37642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Neumann, Patrick P. T1 - Validation of membrane-based linear soil gas sensors – results from repetitive CO2 injection experiments performed in the field N2 - This work presents first results from repeti-tive CO2 injection experiments performed on a recently built-up 400 m² soil test field with gas injection system. The test field contains 48 membrane-based linear gas sensors that were installed in several depths of the test field. Sensors for measuring meteorological parameters (e.g., wind / rain) and the parameters soil temperature, soil moisture, and groundwater level were installed additionally. A more de-tailed description of the test field setup can be found in. A short description of the mem-brane-based linear gas sensors’ functional prin-ciple can be found in. T2 - 33rd Danubia- Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Distributed linear sensor KW - Gas distribution mapping and gas source localization KW - Gas storage areas KW - Membrane-based gas sensing KW - Subsurface monitoring PY - 2016 AN - OPUS4-37643 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Lazik, D. A1 - Bartholmai, Matthias ED - Aulova, Alexandra ED - Rogelj Ritonja, A. ED - Emri, I. T1 - Validation of membrane-based linear soil gas sensors – results from repetitive CO2 injection experiments performed in the field N2 - This work presents first results from repetitive CO2 injection experiments performed on a recently built-up 400 m² soil test field with gas injection system. The test field contains 48 membrane-based linear gas sensors that were installed in several depths of the test field. Sensors for measuring meteorological parameters (e.g., wind / rain) and the parameters soil temperature, soil moisture, and groundwater level were installed additionally. T2 - 33rd Danubia- Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Distributed linear sensor KW - Gas distribution mapping and gas source localization KW - Gas storage areas KW - Membrane-based gas sensing KW - Subsurface monitoring PY - 2016 SN - 978-961-94081-0-0 SP - 174 EP - 175 CY - Ljubljana AN - OPUS4-37644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schukar, Vivien A1 - Köppe, Enrico A1 - Hofmann, Detlef A1 - Westphal, Anja A1 - Sahre, Mario A1 - Beck, Uwe A1 - Gong, Xing A1 - Bartholmai, Matthias ED - Aulova, Alexandra ED - Rogelj Ritonja, A. ED - Emri, I. T1 - A contribution to intelligent automatic validation of structure-integrated fibre optic strain sensors N2 - Sensors integrated into devices and structures provide essential data to control, optimize or manage machines and structural components. In the last years, processes, applications and machine parts became more and more intelligent. Consequently, the need for sensor validation increased significantly in order to rely on sensor data and measurement results. Structure-integrated fibre optic strain sensors, such as fiber Bragg gratings (FBG), are of special interest in the composite manufacturing industry. This type of sensor makes it possible to gain information and to collect measurement data about entire production processes and whole life-time cycles of composite-made machine parts and structures. However, validation concepts and approaches for this type of sensors are barely reported in literature. Furthermore, all the reported activities have the drawback that the sensor diagnosis strategy is implemented as limited mathematical models and/or complex time-consuming spectral analysis tools which are applied in data post-processing loops. However, to automate sensor validation and to apply real-time and in-field sensor fault detection, it is necessary to acquire measurement data and information about the measurement reliability at the same time. T2 - 33rd Danubia- Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Fiber bragg grating KW - Magnetic field KW - Magnetostrictive metal coating KW - Self-diagnostic fiber optical sensor PY - 2016 SN - 978-961-94081-0-0 SP - 180 EP - 181 CY - Ljubljana AN - OPUS4-37645 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst A1 - Ertel, Jens-Peter A1 - Sochor, M. A1 - Unseld, H. T1 - Nachbestimmung von Pfahllängen am Beispiel von Masten N2 - Im Rahmen der Lebensdauerverlängerung oder der Umnutzung von Bauwerken (z. B. Brücken, Bürogebäude oder Maste) müssen diese zum Teil neu bewertet werden. Dafür ist eine Nachrechnung für statische und dynamische Lastfälle erforderlich. Dies betrifft zum einen die Struktur selbst, die gegebenenfalls verstärkt werden muss. Aber auch die Gründung (oft Pfähle verschiedenster Typen) muss neu beurteilt werden. Nach mehreren Jahrzehnten sind jedoch für einige Bauwerke keine zuverlässigen Bestandsunterlagen verfügbar. Eine vollständige Freilegung der Pfähle verbietet sich aus Kostengründen sowie Verlust an Widerstand gegen Zug. Lediglich der Pfahlanschluss kann visuell begutachtet werden, um Pfahlzahl, -typ und Durchmesser zu bestimmen. Für die Bestimmung der Pfahllänge müssen zerstörungsfreie Verfahren eingesetzt werden. In einer Machbarkeitsstudie wurden von den Autoren teils im Blindversuch drei Verfahren evaluiert: die klassische Pfahlintegritätsprüfung nach der Hammerschlagmethode, eine mehrkanalige Variante hierzu und das Parallel-Seismik-Verfahren. Die ersten beiden Methoden lieferten an den untersuchten Pfählen nur in Einzelfällen verwertbare Ergebnisse. Die Parallel-Seismik-Methode lieferte auch im Blindversuch an Fundamenten, bei denen die Pfahllänge dem Eigentümer bekannt war, Ergebnisse mit einer Abweichung von max. 0,5 m. Diese Toleranz lässt sich bei der Standfestigkeitsbeurteilung berücksichtigen. Die Mehrkosten des Verfahrens (anders als bei den anderen Verfahren wird ein verrohrtes Bohrloch im Boden nahe dem Pfahl benötigt) halten sich in Grenzen, wenn man es in die geotechnische Untersuchung integriert. Daher wurde es inzwischen auch in der Praxis eingesetzt. Auch liegen die Gesamtkosten für die Untersuchung deutlich unter denen für eventuell notwendigen Ersatz – oder Verstärkungsmaßnahmen, die notwendig werden, wenn keine Daten zur Pfahllänge verfügbar sind. Der Vortrag erläutert die Ergebnisse der Machbarkeitsstudie, zeigt erste Praxisfälle und weist auf Möglichkeiten hin, das Parallel-Seismik Verfahren in Zukunft noch genauer und effizienter einzusetzen. T2 - 34. Baugrundtagung CY - Bielefeld, Germany DA - 15.09.2016 KW - Mast KW - Pfahl KW - Länge KW - Parallel-Seismik KW - Integritätsprüfung PY - 2016 SN - 9783946039013 SP - 31 EP - 36 PB - DGGT CY - Essen AN - OPUS4-37648 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiele, T. A1 - Borcherding, H. A1 - Carl, Peter A1 - Schedler, U. T1 - Mastering the Challenge of Fluorescence Intensity Calibration N2 - The calibration of fluorescence signals in assays as well as in biological systems is a key requirement. Especially for quantitative studies of living cells, e.g. expression of biomolecules the generation of concentration-proportional analytical statements obtained by the fluorescence intensity plays a significant role. This also applies for cell assays like immunofluorescence assays. Also, the determination of local concentrations of target proteins within cells or within their environment is a major challenge in modern biology. Proper calibration of the fluorescence imaging systems is the prerequisite to ensure that test results from different instruments and different test environments are comparable. The existing calibration solutions for fluorescence imaging systems, however, mostly depend on simple instrument calibration without reference to absolute physical standards or with insufficient stability for multiple measurements. In order to obtain the necessary quantitative information, it is required to calibrate both instruments and the corresponding assays, ideally with one calibrating system. We present several new calibration tools for the most commonly used platforms for cytometry, i.e. fluorescence microscope based systems and flow cytometry based systems. They are comprised of ultra-stable fluorophores that are encapsulated in bio- and cell-compatible polymer matrices. Each tool is tailored to the specific requirements of the different read-out platforms. Both re-usable single-color calibration slides for fluorescence microscopes as well as new multi-color calibration beads are presented. The traceability of the calibration tools to international standards and the wide calibration range of the fluorescence intensity are illustrated. They are thus suitable for calibration of the signal over concentration and quantum yield to that of the targets. T2 - DGFZ 26th Annual Meeting CY - Berlin, Germany DA - 05.10.2016 KW - Flow Cytometry KW - Fluoresence KW - Calibration PY - 2016 AN - OPUS4-37714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Die Technologie-Roadmap „Prozess-Sensoren 4.0“ – Chancen für neue Automatisierungskonzepte und neue Geschäftsmodelle N2 - Derzeit finden gravierende Veränderungen im Umfeld der Informations- und Kommunikationstechnik statt, die eine große Chance für die optimierte Prozessführung und Wertschöpfung mit darauf abgestimmten vernetzt kommunizierenden Sensoren bieten. Diese Art „smarte“ Sensoren stellen Dienste innerhalb eines Netzwerks bereit und nutzen Informationen daraus. Dieses ist die Voraussetzung für die Realisierung von Cyber Physical Systems (CPS) innerhalb zukünftiger Automatisierungskonzepte für die Prozessindustrie, wie sie auch durch das Zukunftsprojekt „Industrie 4.0“ adressiert werden. Smarte Prozess-Sensoren ermöglichen neue Geschäftsmodelle für Anwender, Gerätehersteller, Dienstleister. T2 - SICK Prozessindustrie-Tage 2016 CY - Gelsenkirchen, Germany DA - 22.09.2016 KW - Roadmap KW - Prozess-Sensoren 4.0 KW - Prozessanalytik KW - Smart Sensors KW - Automatisierung KW - Prozessindustrie PY - 2016 AN - OPUS4-37390 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - 9. Interdisziplinäres Doktorandenseminar N2 - Das interdisziplinäre Doktorandenseminar, das unter den Teilnehmerinnen und Teilnehmern mittlerweile als echter Geheimtipp gehandelt wird, startete dieses Mal gleich in medias res mit einem Design-Thinking-Workshop zum Thema "Prozessanalytik für Industrie 4.0". Das Thema ist derzeit in aller Munde, erfährt eine eigene Dynamik und es wird hierzulande kräftig an Roadmaps und White Papers gestrickt. So kam aus Fachkreisen der VDI/GMA und NAMUR der Vorschlag, die Generation der zukünftigen Kolleginnen und Kollegen zu dem Thema zu befragen, die die heute verbrochenen Konzepte zukünftig selber ausbaden müssen. Die Vorträge der nächsten beiden Tage umfassten wieder ein sehr breites und interdisziplinäres Themen-, Methoden- und Anwendungsspektrum. Neben lumineszenten Temperatursensoren in Mikrochipreaktoren, Mikromischer NMR-Detektion und in Arbeitsschutzkleidung integrierte Chemosensorik folgten einige Vorträge zu Verbesserungen und neunen Konzepten von Biosensoren sowie für Immuno-Micorarray-Verfahren. Die ebenfalls diskutierten Identifizierungs- und Quantifizierungsverfahren reichten von der Kokskohle bis zur Arzneitablette. Desweiteren wurde der Bogen von lumineszenten Nanopartikeln zu Kalibrationsstandards für Trübungssonden gespannt. Neben den Erzeugen der Daten ist ein intelligentes Datenmanagement notwendig um die Informationen auch zu verarbeiten und entsprechend dem User zu präsentieren. Die interdisziplinäre Ausrichtung und Vielfalt der verschiedenen Forschungsbereiche spiegelte sich auch in den Postersession wieder. Die Themen umfassten etwa Softsensoren für die Regelung von CHO-Zellkultivierungen, Prozessanalytik für die Reaktivabsorption von CO2 aus industriellen Gasströmen oder Alkoholmarker in menschlichem Haar, um nur einige zu nennen. T2 - 9. Interdisziplinäres Doktorandenseminar CY - Berlin, Germany DA - 22.02.2015 KW - Doktorandentagung KW - Prozess-Sensoren KW - Elektrochemie KW - Chemometrie KW - Prozessanalytik PY - 2015 SN - 978-3-9817267-0-1 SP - 1 EP - 40 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-37391 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - 8. Interdisziplinäres Doktorandenseminar N2 - Auch dieses Jahr war das interdisziplinäre Doktorandenseminar, organisiert von den Arbeitskreisen Prozessanalytik, Chemometrik und Qualitätssicherung, Chemo- und Biosensoren und Elektrochemische Analysenmethoden der Fachgruppe für Analytische Chemie der GDCh und erstmals in Kooperation mit den kreativen jungen Verfahrensingenieuren (kjVIs), wieder gut besucht und für alle Teilnehmer eine ausgezeichnete Gelegenheit zum interdisziplinären Wissensaustausch. Das Seminar fand wie bereits in den vergangenen zwei Jahre in Berlin statt, in der Eventpassage Nähe Bahnhof Zoo, grossartig vorbereitet und geleitet von Dr. Michael Maiwald und Grit Seifert, von der BAM Bundesanstalt für Materialforschung und -prüfung. Die Vorträge der nächsten beiden Tage umfassten ein breites Themen-, Methoden- und Anwendungsspektrum von Applikationen im Mikrobereich, wie etwa der Entwicklung eines Chips als Leitfähigkeitssensor zur Bestimmung des CO2-Partialdrucks am Oxygenatorausgang während extrakorporaler Membranoxygenierung bis hin zu grossen Massstäben wie etwa der Sortierung von Altholz mit Nahinfrarotspektroskopie. Die vielen hoch interessanten Vorträge aus verschiedenen Bereichen und Technologien, wie NMR-Spektroskopie, Elektrochemie, Fluoreszenz-Spektroskopie, Surface enhanced Raman scattering (SERS), regten zu konstruktiven Diskussionen an und gaben Einblicke in wissenschaftliche Bereiche und deren Anwendung, die über den eigenen Themenbereich hinaus gehen. Die interdisziplinäre Ausrichtung und Vielfalt der verschiedenen Forschungsbereiche spiegelte sich auch in der Postersession wieder. Die Themen umfassten etwa den Versuch zur Diskriminierung einer Lungenkrebszelllinie durch Honigbienen, die parallelen Analyse von Mikroschadstoffen in Wasser, sowie die Kombination von faser-optischer Methoden zur Inline Multiparameterprozessanalytik, um nur einige zu nennen. T2 - 8. Doktorandentagung CY - Berlin, Germany DA - 23.02.2014 KW - Doktorandentagung KW - Smart Sensors KW - Elektrochemie KW - Chemometrie KW - Prozessanalytik PY - 2014 SN - 978-3-9816380-1-1 SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-37392 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - 7. Interdisziplinäres Doktorandenseminar N2 - Niedriglegierte warmfeste Mn-Mo-Ni und Cr-Mo-V Stähle bilden einen wesentlichen Beitrag gegenwärtig eingesetzter Werkstoffe für druck- und temperaturführende Komponenten im Kraftwerksbau. Dies sind beispielsweise Kesselkomponenten wie Membranwände und Druckbehälter. Dabei kommen die Hauptmerkmale dieser Werkstoffgruppe (sehr gute mechanische Hochtemperatureigenschaften, Verarbeitbarkeit und niedrige Legierungskosten) zum Tragen. Die weitere Erhöhung des thermischen Wirkungsgrades ist dabei das wichtigste Ziel, der Werkstoffauswahl für die nähere Zukunft, unabhängig vom Kraftwerkskonzept. Dies trifft jedoch im Besonderen bei fossil-befeuerten Kraftwerken im Rahmen der notwendigen Reduzierung der CO2 Emissionen zu. Die schweißtechnische Komponentenfertigung ist dabei das maßgebliche Fertigungsverfahren. Das Einbringen der Schweißwärme bedingt dabei metallurgische und Gefügeveränderungen in der wärmebeeinflussten Zone des Grundwerkstoffes (WEZ) als auch im niedergeschmolzenen Schweißgut. Die Schweißverbindung kann dabei zusätzlich während oder nach dem Schweißen Wasserstoff aufnehmen. Wasserstoff hat dabei eine degradierende Wirkung auf die mechanischen Eigenschaften, die sich im Worst-Case als wasserstoffunterstützte Kaltrisse zeigen, dies vor allem auch zeitverzögert (delayed cracking) durch die temperaturabhängige Wasserstoffdiffusion. Dabei zeigt jede Schweißmikrostruktur spezifische Wasserstoffdiffusions- und Lösungscharakteristika. Die Degradation ist daher als eine Kombination sich gegenseitig beeinflussender Faktoren aus lokaler Wasserstoffkonzentration, Mikrogefüge und mechanischer Beanspruchung zu sehen. Wie aktuelle Schadensfälle in der jüngeren Vergangenheit belegten (Rissbildung bei Schweißnähten an T24 Rohr-Rohr-Verbindungen), ist Wasserstoff dabei eine potentiell zu berücksichtigende Schadensursache. Zur weiterführenden Früherkennung möglicher Schäden, ist es daher notwendig, den gefügespezifischen Wasserstoffeffekt in Schweißnähten an niedriglegierten Stählen festzustellen und zu bewerten. Die Interdependenz der mechanischen Beanspruchung und des Verbleibens einer potentiell degradierenden Wasserstoffkonzentration muss dabei für jedes Gefüge separiert werden. Daher wurden für die Charakterisierung der mechanischen Eigenschaften gefügespezifische Untersuchungen an wasserstoffbeladenen Zugproben aus Grundwerkstoffen und thermisch simulierten WEZ Gefügen untersucht. Das Diffusionsverhalten wurde mit der elektrochemischen Permeationsmethode bei Raumtemperatur und über die Interpretation des Wasserstoffeffusions-verhaltens mittels Trägergasheißextraktion bei erhöhten Temperaturen bis 400°C untersucht. Zur realistischen Abbildung des Diffusionsverhaltens, wurde dabei eine optimierte Prozedur aus Probenaufheizung und Wasserstoffeffusion entwickelt. Diese wurde zusätzlich auf ein Wasserstoffmessgerät mit gekoppeltem Massen-spektrometer (MS) übertragen. Gleichzeitig, wurden die korrespondierende getrappte, sowie die Gesamtwasserstoff-konzentration bestimmt. Die Ergebnisse zeigten, dass die WEZ eine generell erhöhte Anfälligkeit für die Degradation besitzt (im Gegensatz zum Grundwerk-stoff), unabhängig von der verwendeten Legierungsroute. Dabei nimmt die martensitische Grobkornzone die Stellung als anfälligste Mikrostruktur ein. Aus den gewonnenen Daten, konnten erstmals durchgängige gefügespezifische Kriterien(Hüllkurven) für das Versagen mit quantifizierbaren Wasserstoffkonzentrationen generiert werden. Dazu erfolgten Untersuchungen an Mn-Mo-Ni legierten Stählen (16MND5 und 20MND5 / 20MnMoNi5-5) sowie an kriechfesten Stählen T24 (7CrMoVTiB1010) und T22 (10CrMo9-10). Generell, zeigten Mn-Mo-Ni Grundwerk-stoffe eine bessere Beständigkeit als Cr-Mo(-V) Stähle. Im Fall des Cr-Mo-V Legierungskonzeptes, konnte zusätzlich die positive Wirkung von Vanadium als Legierungselement zur Erhöhung der Beständigkeit gegenüber einer Degradation bestätigt werden. Die Untersuchungen des Diffusions- und Lösungs-vermögens zeigten, dass die WEZ generell niedrigere Diffusionskoeffizienten besitzt als der Grundwerk-stoff. Dies wird durch stärkeres Trapping des Wasserstoffs beeinflusst und steigert dabei die Lösungs-fähigkeit der Mikrostruktur. Oberhalb von 100°C konnte dabei kein nennenswertes Trapping festgestellt werden, außer im Fall des T24 infolge der Zulegierung von Vanadium. Unterhalb von 100°C, zeigte sich ein deutlicher Abfall der Diffusion infolge des weiter ansteigenden Trappings. Für den betrachteten Temperatur-bereich wurden dabei effektive Wasserstoffdiffusions-koeffizienten berechnet, die zum Teil höher liegen, im Vergleich zu Literaturwerten. Dies liegt zum großen Teil in der optimierten Aufheizprozedur der Proben begründet und, daran gekoppelt, der beschleunigten Wasserstoffeffusion. Die weiterführende Bedeutung der Ergebnisse liegt in drei Bereichen begründet. Erstens, besteht jetzt die Möglichkeit der quantifizierbaren Vergleichbarkeit des gefüge-spezifischen Wasserstoff-einflusses auf die Degradation. Zweitens, wurden aus den experimentellen Daten, Kriterien für das Versagen für der spezifischen Schweißnahtgefüge abgeleitet. Drittens, stehen realistischere Diffusionskoeffizienten für eine Vielzahl von Schweißnahtgefügen zur Verfügung. Aus wissenschaftlicher Sicht ergeben sich wichtige Beiträge zur Interpretation des Wasserstoffeinflusses auf die makroskopischen mechanischen Eigenschaften hinsichtlich der Legierung bzw. Phasenzusammensetzung, wie oben angeführt. Weiterhin konnte gezeigt werden, dass Berechnungsalgorithmen in Kombination mit bestimmten experimentellen Randbedingungen, großen Einfluss auf die effektiven Wasserstoffdiffusions-koeffizienten haben. Dies kann speziell bei erhöhten Temperaturen zu Abweichungen führen, die einen weiteren Ansatz zur Erklärung (der in der Literatur) genannten Streubänder ergeben. Aus ökonomischer Sicht leisten die präsentierten Ergebnisse Beiträge zur sicheren und zuverlässigen Verarbeitung der Werkstoffe. So können anhand der identifizierten Temperaturstufen des Wasserstofftrappings Mindestvorwärm-, Zwischenlagen- bzw. Nachwärmtemperaturen für das Wasserstoffarmglühen identifiziert werden. Die Verwendung der Diffusionskoeffizienten ermöglicht zusätzlich die Abschätzung bzw. Anpassung von notwendigen Haltezeiten. Für die weitere Zukunft ist die Einbindung der mechanischen Daten in vorhandene Modelle zur numerischen Simulation und der verbesserten Vorhersage wasserstoffunterstützter Degradation von Schweißmikrostrukturen vorgesehen. T2 - 7. Interdisziplinäres Doktorandenseminar CY - Berlin, Germany DA - 24.02.2013 KW - Doktorandentagung KW - Sensoren KW - Elektrochemie KW - Chemometrie KW - Prozessanalytik PY - 2013 SN - 978-3-9815360-9-6 SP - 1 EP - 52 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-37393 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - 6. Interdisziplinäres Doktorandenseminar N2 - Das 6. Interdisziplinäre Doktorandenseminar ist 2012 von Attendorn nach Berlin umgezogen. Es bot wieder reichlich Gelegenheit zum Kennenlernen, Wiedersehen und fachlichen Gedankenaustausch. Insgesamt kamen über 30 Teilnehmerinnen und Teilnehmer von Hochschulen, Forschungseinrichtungen und der Industrie zusammen. T2 - 6. Interdisziplinäres Doktorandenseminar CY - Berlin, Germany DA - 26.02.2012 KW - Doktorandentagung KW - Sensoren KW - Elektrochemie KW - Chemometrie KW - Prozessanalytik PY - 2012 SN - 978-3-9814634-5-3 SP - 1 EP - 42 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-37394 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - 8. Kolloquium Prozessanalytik Berlin N2 - Themenschwerpunkt "Spektroskopie und Sensorik in der Prozessanalytik" Am 03. und 04. Dezember fand das 8. Kolloquium des Arbeitskreises Prozessanalytik statt, diesmal in Berlin. Wie bekannt ist ein wichtiger Aspekt dieser Konferenz, Grenzen zwischen Fachgebieten sowie technischen Anwendungsbereichen zu überschreiten und einen interdisziplinären Austausch zu ermöglichen. Diesem Gedanken wurde bereits mit dem diesjährigen Themenschwerpunkt „Spektroskopie und Sensorik in der Prozessanalytik“ deutlich Rechnung getragen. Wie wichtig diese Themen für den Produktionsstandort Deutschland sind, zeigt die rege Beteiligung der Industrie. Neben insgesamt sieben industriellen Sponsoren und Ausstellern kam weit über die Hälfte der Teilnehmer aus der Industrie. Neben den Vorträgen bot die Veranstaltung noch zahlreiche Posterbeiträge, die ebenfalls neue Einblicke in prozessanalytische Themen und natürlich auch Anlässe für anregende Fachdiskussionen boten. Die Veranstalter hatten darauf geachtet, dass der fachliche Austausch in den Pausen, insbesondere aber auch während der Postersessions nicht zu kurz kam. T2 - 8. Kolloquium Arbeitskreis Prozessanalytik CY - Berlin, Germany DA - 03.12.2012 KW - Kolloquium Prozessanalytik KW - Prozessanalytik KW - Arbeitskreis Prozessanalytik PY - 2012 SN - 978-3-9815360-1-0 SP - 1 EP - 48 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-37395 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - 9. Kolloquium Prozessanalytik Ludwigshafen N2 - Die Geschichte der Prozessanalysentechnik begann mit Paul Gmelin, Mitarbeiter im physikalischen Laboratorium der Badischen Anilin und Soda Fabrik in Ludwigshafen und einer großen Aufgabe: Bei den Versuchen zur Ammoniaksynthese war deutlich geworden, dass die großen Gasdurchflüsse hinsichtlich ihrer Zusammensetzung überwacht werden mussten. Gmelin entwickelte den sogenannten Pfeifenanalysator, der das Verhältnis der Gase Stickstoff und Wasserstoff für die Ammoniaksynthese messtechnisch erfassen und so den Produktionsprozess steuern konnte. Im Mai 1913 erhielt er hierfür das Patent – die Prozessanalysentechnik war geboren. Heute sind Chemieanlagen, Raffinerien und nahezu alle Anlagen der verfahrenstechnischen Industrie ohne die vielfältigen Messmethoden der PAT nicht mehr wirtschaftlich zu betreiben. Die direkte Messung von Substanzeigenschaften, Konzentrationen und Zusammensetzungen erlaubt die Überwachung von Produktionsprozessen sowie die Einhaltung hoher Sicherheitsstandards und ermöglicht eine optimierte, zielproduktorientierte Produktion. Begünstigt durch den Innovationsschub im Bereich der Automatisierungstechnik etablierte sich die PAT als hochinnovatives, interdisziplinäres Arbeitsfeld. Mit der Verkürzung der Zeitkonstanten bei der Erfassung von online Messergebnissen gelang der Sprung von einer reinen Überwachungsfunktion hin zur Führungsgröße innerhalb der Prozesssteuerung. Das diesjährige Kolloquium des Arbeitskreises Prozessanalytik der DECHEMA und der GDCh mit dem Schwerpunkt „Prozessführung und -automatisierung“ steht deshalb ganz im Zeichen des „Trialogs“ .zwischen Forschern, Geräteherstellern und Anwendern, um gemeinsam hierfür interdisziplinäre Lösungsansätze zu entwickeln und Innovationen auf diesem Gebiet voranzutreiben. Die technische Entwicklung von einer indirekten zur direkten Messgröße ermöglicht bereits heute den Einsatz von PAT-Methoden in ressourcenschonenenden, energieeffizienten und nachhaltigen Regelungskonzepten. Dies ist ein wichtiger Schritt auf dem Weg zu Operational Excellence in der Prozessführung. Dieser Herausforderung wird sich die Prozessanalysentechnik selbstbewusst und gegründet auf 100 Jahren Erfahrung und Expertise stellen und die erfolgreiche interdisziplinäre Zusammenarbeit auch in Zukunft weiter fortsetzen. T2 - 9. Kolloquium Arbeitskreis Prozessanalytik CY - Ludwigshafen, Germany DA - 28.11.2013 KW - Kolloquium Prozessanalytik KW - Prozessanalytik KW - 100 Jahre Prozessanalytik KW - Fankhänel PY - 2013 SP - 1 EP - 87 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-37396 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - 10. Kolloquium Prozessanalytik Berlin N2 - Dieses jährliche Netzwerktreffen hat sich als Diskussionsplattform zu allen Themen rund um die Prozessanalysenmesstechnik etabliert und es erwarten uns spannende Vorträge und Diskussionen. Wir freuen uns dieses Jahr Ihr Gastgeber zu sein. Endress+Hauser ist ein weltweit tätiger Anbieter von Automatisierungslösungen. Als Kompetenzzentrum für Flüssigkeitsanalyse bietet Endress+Hauser Conducta mit eigenen Produktionsstandorten in Deutschland, Asien und den USA ein breites Spektrum von Sensoren und Messsystemen für die Prozessanalysentechnik (PAT). Exzellente Produkte und zukunftsweisende Dienstleistungen und Lösungen unterstützen die Prozesse der Kunden seit über 60 Jahren. Das diesjährige Kolloquium hat den Schwerpunkt „Prozessanalytik in der Biotechnologie“. Erste biotechnologische Verfahren wurden bereits vor mehreren 1000 Jahren angewandt zur Herstellung von Brot oder auch Bier und Wein aus Hefen. Heute treiben biotechnologische Verfahren Innovationen auf vielen Gebieten und deren Bedeutung in der Produktion von Lebensmitteln, landwirtschaftlichen Produkten, Arzneimitteln und Impfstoffen sowie Chemikalien steigt überproportional an. Biotechnologische Prozesse erlauben es zum Beispiel Proteine, Antikörper oder Vakzine maßgeschneidert und gezielt für den therapeutischen Einsatz herzustellen. Die Wirtschaftlichkeit der biologischen Prozesse hängt in hohem Maße davon ab, dass die richtigen Bedingungen geschaffen werden, damit die Mikroorganismen oder Zellkulturen optimal wachsen und die Erträge stabil und vorhersagbar maximiert werden können. Dieses stellt neue Anforderungen an die Sensorik und auch an die prozessanalytischen Werkzeuge für die Prozessautomatisierung. Darüber hinaus fördert die PAT-Initiative der FDA und das Streben nach Operational Excellence den Einsatz der Prozessanalysentechnik. Intelligente digitale pH und Sauerstoffsensoren ermöglichen eine zuverlässige Steuerung von biotechnologischen Verfahren bei gleichzeitig intuitiver Bedienung und sicherer Diagnose des Sensorzustandes. Biotechnologische Hochdurchsatzanalytik wird zur Optimierung in der modernen Pflanzenzüchtung eingesetzt. Innovative Modelle helfen die biotechnologischen Prozesse und deren Analytik zu verstehen und zu beschreiben. Wir wünschen Ihnen ein erfolgreiches Kolloquium mit vielen anregenden Diskussionen im TRIALOG zwischen den Forschern, Geräteherstellern und Anwendern. T2 - 10. Kolloquium Arbeitskreis Prozessanalytik CY - Gerlingen, Germany DA - 25.11.2014 KW - Kolloquium Prozessanalytik KW - Prozessanalytik KW - Tagungsband PY - 2014 SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-37397 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - 11. Kolloquium Prozessanalytik Wien N2 - Themenschwerpunkt des 11. Kolloquiums war „Vom Sensor zur Prozessintelligenz“. Diskutiert wurde damit über die neusten Fortschritte in der Messtechnik und deren Implementierung sowie über neue Aspekte der Modellierung und das Umsetzen, also das Leben des daraus generierten Wissens im Prozess. Das 11. Kolloquium Prozessanalytik in Wien startete mit einem Konferenzvorkurs zum Thema Ressourcenanalytik. Bei der Erschließung, Förderung und Umsetzung von natürlichen Rohstoffen gewinnen analytische Online-Verfahren eine immer größere Bedeutung. Gleichzeitig liegen die Analyte jedoch in sehr heterogenen Matrizes vor, sodass die Ressourcenanalytik ein sehr herausforderndes, für Fachleute damit aber auch sehr spannendes Thema ist. Für diesen interdisziplinären Brückenschlag fanden an den beiden Hauptveranstaltungstagen vier Sessions mit jeweils drei Fachvorträgen und anschließender Diskussion statt: Im ersten Vortragsblock Sensoren – „messen“ wurden beispielhaft neue Messtechniken sowie übergeordnet deren Einbindung in die digitale Welt über Zukunftstrends wie Industrie 4.0 oder die Technologieroadmap Prozess-Sensoren 4.0 beschrieben. Mit Automatisierung – „implementieren“ wurden in einer zweiten Session Herausforderungen aber auch konkrete Lösungswege bei der Implementierung von Messtechnik im industriellen Umfeld aufgezeigt. Die Vortragsreihe Modelle – „erkennen“ widmete sich am zweiten Veranstaltungstag der Fragestellung, wie Messergebnisse in Wissen transferiert werden können, wobei insbesondere entsprechende Erfahrungen aus der Bioprozesstechnik zugänglich gemacht wurden. Ebenfalls am zweiten Tag war schließlich Life-Cycle-Management – „leben“ Titel der „österreichischen Session“ zum Schwerpunktthema des Kolloquiums. In den drei Vorträgen wurde gezeigt, wie einmal generiertes Prozesswissen durch gutes Wissensmanagement und dessen Werkzeuge nicht nur tradiert sondern auch transferiert werden kann. Besondere Berücksichtigung fanden beim diesjährigen Kolloquium auch die fast 40 hochqualitativen Posterbeiträge. Neben den ausgedehnten Postersessions an beiden Veranstaltungstagen erhielten die Autoren in zwei Posterslams jeweils eineinhalb Minuten Zeit, ihre Arbeit vorzustellen und das Fachpublikum zu vertiefenden Gesprächen im Anschluss einzuladen. Damit rückten nicht nur diese wertvollen Beiträge noch mehr ins Zentrum der Aufmerksamkeit, auch das Auditorium hatte so Gelegenheit, die Posterausstellung noch gezielter wahrzunehmen. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Wien, Austria DA - 30.11.2015 KW - Kolloquium Prozessanalytik KW - Prozessanalytik KW - Tagungsband PY - 2015 SP - 1 EP - 96 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-37398 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Esche, E. A1 - Kraemer, B. A1 - Müller, D. A1 - Meyer, Klas A1 - Zientek, Nicolai A1 - Maiwald, Michael A1 - Wozny, G. T1 - Improved desorption control via Raman spectroscopy N2 - In this contribution a Raman spectrometer based control structure for the heating of a desorption column is proposed. For this purpose calibration experiments for the absorption of carbon dioxide using monoethanolamine solutions are carried out and calibration models are developed to measure both carbon dioxide liquid loads and monoethanolamine mass fractions. The calibration experiments are supported by online NMR spectroscopy to accurately measure the appearance of all species in the electrolyte system. Both models are tested during the plant operation of a mini-plant for the oxidative coupling of methane and the proof of concept for the control structure is given. The Raman spectroscopy implemented in the ATEX conform mini-plant shows a reliable and robust performance being even indifferent to impurities hindering the GC analysis. T2 - 20th International Conference of Process Engineering and Chemical Plant Design CY - Berlin, Germany DA - 15.10.2014 KW - Absorption KW - Carbon capture KW - Raman spectroscopy KW - desorption control KW - Prozessanalytik KW - Process analytical technology PY - 2014 UR - https://www.verfahrenstechnik.tu-berlin.de/fileadmin/fg158/Dokumente/Manuskripte/2014/20th-ICPEPD-Proceedings.pdf SN - 978-3-00-047364-7 SP - 223 EP - 233 PB - Technische Universität Berlin CY - Berlin AN - OPUS4-37399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wiggenhauser, Herbert A1 - Wilsch, Gerd A1 - Schaurich, Dieter A1 - Wöstmann, Jens T1 - Application of LIBS in civil engineering for the analysis of concrete N2 - Our aim is the application of LIBS as a simple, quasi on-line method for the non-destructive testing of concrete. Concrete is naturally inhomogeneous. Therefore we must take into account the local variation of the element composition using a statistical analysis. Depending on how much cement and aggregate is measured with each laser pulse, a scan on the surface of a concrete specimen produces a distribution of points in the Rankin diagram which is used to characterise the concrete. T2 - First International Conference on Laser Induced Plasma Spectroscopy and Applications CY - Tirrenia, Italy DA - 08.10.2000 KW - Element composition KW - Statistical analysis KW - Rankin diagramm PY - 2000 AN - OPUS4-36539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Schaurich, Dieter A1 - Wöstmann, Jens A1 - Wiggenhauser, Herbert T1 - Nachweis von Hydrophobierungsmitteln mit Laser Induced Breakdown Spectroscopy N2 - Die Eignung des Verfahrens der Laser Induzierten Breakdown Spectroscopy (LIBS) zur Kontrolle einer ausreichenden Beschichtung und zur Bestimmung der Schichtdicke von Hydrophobierungsschichten auch im Rahmen wiederholender Messungen sollte untersucht werden. Mit LIBS kann die Elementverteilung orts- und tiefenaufgelöst in oberflächennahen Bereichen quasi on-line bestimmt werden. Es ist keine Probenpräparation notwendig. Wiederholende Messungen würden das vorzeitige Erkennen beschädigter Beschichtungen ermöglichen, wodurch kostspielige Sanierungsmaßnahmen vermieden werden. T2 - Fachtagung Bauwerksdiagnose - Praktische Anwendungen Zerstörungsfreier Prüfungen CY - Leipzig, Germany DA - 25.10.2001 KW - Beschichtung KW - Schichtdicke KW - Elementverteilung PY - 2001 AN - OPUS4-36540 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane A1 - Wöstmann, Jens T1 - Ortung von Hohlstellen in Mauerwerk und Betonstrukturen mit dem Impulsradar N2 - In den letzten Jahren hat sich das Impulsradar als zerstörungsfreies Prüfverfahren im Bauwesen insbesondere zur Ortung von metallischen Einbauteilen wie z. B. schlaffer und vorgespannter Bewehrung in Betonbauteilen immer stärker durchgesetzt. Systematische Laboruntersuchungen und Fallstudien zeigen aber auch, dass das Verfahren sehr gut zur Ortung von Hohlstellen sowohl in Mauerwerk als auch in Betonstrukturen geeignet ist. Das Radarverfahren arbeitet nach dem Impuls-Echo Prinzip. Dabei wird von der Sendeantenne ein sehr kurzer elektromagnetischer Impuls ausgesendet (ca. 3 Halbwellen), der an Grenzflächen im Material (Änderung der Dielektrizitätskonstanten) und bei nicht zu dicken Bauteilen auch an der Rückseite reflektiert und von der Empfangsantenne detektiert wird. Bei den hier vorgestellten Messergebnissen wurden eine 900 MHz sowie eine 1,5 GHz Antenne in Kombination mit einem kommerziellen Radargerät eingesetzt. T2 - DGZfP-Jahrestagung CY - Berlin, Germany DA - 21.05.2001 KW - Metallische Einbauteile KW - Impuls-Echo Prinzip KW - Bodemuseum Berlin PY - 2001 AN - OPUS4-36541 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tahri, K. A1 - Tiebe, Carlo A1 - Bougrini, M. A1 - Saidi, T. A1 - El Alami-El Hassani, N. A1 - El Bari, N. A1 - Hübert, Thomas A1 - Bouchikhi, B. T1 - Determination of safranal concentration in saffron samples by means of VE-tongue, SPME-GC-MS, UV-vis spectrophotometry and multivariate analysis N2 - An experimental investigation has been carried out to characterize and discriminate seven saffron samples and to verify their declared geographical origin using a voltammetric electronic tongue (VE-tongue). The ability of multivariable analysis methods such as Principal Component Analysis (PCA), Hierarchical Cluster Analysis (HCA) to classify the saffron samples according to their geographical origin have been investigated. A good discrimination has reached using PCA and HCA in the VE-tongue characterization case. Furthermore, cross validation and Partial Least Square (PLS) techniques were applied in order to build suitable management and prediction models for the determination of safranal concentration in saffron samples based on SPME-GC-MS and UV-Vis Spectrophotometry. The obtained results reveals that some relationships were established between the VE-tongue signal, SPMEGC-MS and UV-Vis spectrophotometry methods to predict safranal concentration levels in saffron samples by using the PLS model. In the light of these results, we can say that the proposed electronic system offer a fast, simple and efficient tool to recognize the declared geographical origin of the saffron samples. T2 - IEEE Sensor 2015 CY - Busan, South Korea DA - 01.11.2015 KW - Chemometrics KW - Voltammetric electronic tongue KW - SPME-GC-MS KW - UV-vis Spectrometry KW - Saffron KW - Geographic differentiation PY - 2015 SN - 978-1-4799-8202-8 VL - CFP15SEN-USB SP - 68 EP - 71 PB - IEEE CY - Piscataway AN - OPUS4-36545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geißler, Daniel A1 - Hildebrandt, N. T1 - Recent developments in Förster resonance energy transfer (FRET) diagnostics using quantum dots N2 - The exceptional photophysical properties and the nanometric dimensions of colloidal semiconductor quantum dots (QD) have strongly attracted the bioanalytical community over the last approximately 20 y. In particular, the integration of QDs in the analysis of biological components and interactions, and the related diagnostics using Förster resonance energy transfer (FRET), have allowed researchers to significantly improve and diversify fluorescence-based biosensing. In this TRENDS article, we review some recent developments in QD-FRET biosensing that have implemented this technology in electronic consumer products, multiplexed analysis, and detection without light excitation for diagnostic applications. In selected examples of smartphone-based imaging, single- and multistep FRET, steady-state and time-resolved spectroscopy, and bio/chemiluminescence detection of QDs used as both FRET donors and acceptors, we highlight the advantages of QD-based FRET biosensing for multiplexed and sensitive diagnostics. KW - Fluorescence spectroscopy and imaging KW - Multiplexing immunoassay KW - Nanoparticle KW - DNA/RNA KW - BRET/CRET PY - 2016 DO - https://doi.org/10.1007/s00216-016-9434-y SN - 1618-2642 SN - 1618-2650 VL - 408 IS - 17 SP - 4475 EP - 4483 PB - Springer-Verlag CY - Berlin, Heidelberg AN - OPUS4-36546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schäfer, N. A1 - Chahine, G. A. A1 - Wilkinson, A. J. A1 - Schmid, Thomas A1 - Rissom, T. A1 - Schülli, T. U. A1 - Abou-Ras, D. T1 - Microstrain distributions in polycrystalline thin films measured by X-ray microdiffraction N2 - Microstrain distributions were acquired in functional thin films by high-resolution X-ray microdiffraction measurements, using polycrystalline CuInSe2 thin films as a model system. This technique not only provides spatial resolutions at the submicrometre scale but also allows for analysis of thin films buried within a complete solar-cell stack. The microstrain values within individual CuInSe2 grains were determined to be of the order of 10^-4. These values confirmed corresponding microstrain distribution maps obtained on the same CuInSe2 layer by electron backscatter diffraction and Raman microspectroscopy. KW - Microstrain distribution KW - X-ray microdiffraction KW - Polycrystalline thin films KW - Raman microscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-366592 DO - https://doi.org/10.1107/S1600576716003204 SN - 1600-5767 VL - 49 SP - 632 EP - 635 AN - OPUS4-36659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Dariz, P. T1 - Chemical imaging of historical mortars by Raman microscopy N2 - Raman microspectroscopic imaging was just recently introduced into the analysis of cement stone. Here, we demonstrate this approach on 19th-century Roman and Portland cement mortars and extend it to gypsum-based samples originating from a medieval stucco sculpture (high-burnt gypsum) and a stucco ornament prefabricated at the beginning of the 20th century (plaster of Paris). Furthermore, the distributions of dolomite and Calcite were mapped in an accessory mineral grain with approx. 500 nm lateral Resolution demonstrating the ability for studying alteration processes such as dedolomitisation. As we would like to make this approach accessible to other researchers, we discuss its present status, advantages, limitations and pitfalls. KW - Raman microscopy KW - Chemical imaging KW - Cement clinker KW - Gypsum KW - Dedolomite PY - 2016 DO - https://doi.org/10.1016/j.conbuildmat.2016.03.153 SN - 0950-0618 VL - 114 SP - 506 EP - 516 PB - Elsevier Science CY - Oxford, UK AN - OPUS4-36661 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik A1 - Kreutzbruck, M. A1 - Ziegler, Mathias T1 - Laser projected photothermal thermography for characterizing hidden defects N2 - For the last 20 years active thermography has developed into a standard method in non-destructive material testing. It has become possible to detect defects such as cracks, voids, or even material inhomogeneities. Until now, it is still difficult to quantify subsurface or hidden defects in size due to the diffusive nature of heat flow within a solid. Facing this issue, lockin thermography and other photothermal techniques have been established. They are based on exciting a sample periodically (e.g. with a halogen lamp), causing a controlled periodical heat flow and thereby representing strongly damped thermal waves. These techniques make use of interference and reflection of thermal waves which allow enhancing depth resolution. So far, only the temporal component of the light source was modified to achieve a defined vertical heat flow – In contrast, we propose a novel technique in which we are able to control both: time and space. This technique enables us to exploit the possibilities of coherent thermal wave shaping. We achieve that by combining a spatial light modulator (SLM) with a high power laser. This approach allows us to launch a set of individually controlled and fully coherent high energy thermal waves into the sample volume. That means, we intentionally use wave propagation throughout the sample’s material in both - vertical and lateral direction. As one possible application, we use a thermal waves’ interference effect of two phase shifted wave patterns to detect the position of hidden defects. The wave patterns are positioned with a certain distance and a 180° phase shift to each other creating an amplitude depletion zone right in the middle of the two patterns. When a defect is brought unsymmetrically into the depletion zone, the lateral heat flow is disturbed. If the sample is now moved through the depletion zone, a defect can be easily characterized. Exciting periodically while controlling simultaneously phase and amplitude enables us to have a defined thermal wave propagation throughout the sample which means thermal waves can be controlled almost like acoustical or optical waves. This offers the opportunity to transfer known technologies from wave shaping techniques to thermography methods. T2 - 19th World Conference of Non-Destructive Testing 2016 CY - München, Germany DA - 13.06.2016 KW - Thermal waves KW - DMD KW - Active thermography KW - SLM PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-365702 SP - Th.4.I.2 - 1 EP - Th.4.I.2 - 6 AN - OPUS4-36570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik T1 - Laser projected photothermal thermography for characterizing hidden defects N2 - For the last 20 years active thermography has developed into a standard method in non-destructive material testing. It has become possible to detect defects such as cracks, voids, or even material inhomogeneities. Until now, it is still difficult to quantify subsurface or hidden defects in size due to the diffusive nature of heat flow within a solid. Facing this issue, lockin thermography and other photothermal techniques have been established. They are based on exciting a sample periodically (e.g. with a halogen lamp), causing a controlled periodical heat flow and thereby representing strongly damped thermal waves. These techniques make use of interference and reflection of thermal waves which allow enhancing depth resolution. So far, only the temporal component of the light source was modified to achieve a defined vertical heat flow – In contrast, we propose a novel technique in which we are able to control both: time and space. This technique enables us to exploit the possibilities of coherent thermal wave shaping. We achieve that by combining a spatial light modulator (SLM) with a high power laser. This approach allows us to launch a set of individually controlled and fully coherent high energy thermal waves into the sample volume. That means, we intentionally use wave propagation throughout the sample’s material in both - vertical and lateral direction. As one possible application, we use a thermal waves’ interference effect of two phase shifted wave patterns to detect the position of hidden defects. The wave patterns are positioned with a certain distance and a 180° phase shift to each other creating an amplitude depletion zone right in the middle of the two patterns. When a defect is brought unsymmetrically into the depletion zone, the lateral heat flow is disturbed. If the sample is now moved through the depletion zone, a defect can be easily characterized. Exciting periodically while controlling simultaneously phase and amplitude enables us to have a defined thermal wave propagation throughout the sample which means thermal waves can be controlled almost like acoustical or optical waves. This offers the opportunity to transfer known technologies from wave shaping techniques to thermography methods. T2 - 19th World Conference of Non-Destructive Testing 2016 CY - München, Germany DA - 13.06.2016 KW - Thermal waves KW - DMD KW - Active thermography KW - SLM PY - 2016 AN - OPUS4-36577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane T1 - A round robin test on flash thermography N2 - A round robin test on flash thermography was organized within the scope of a standardization research project. This test gives information on reliability, comparability and efficiency of different testing situations. Data recorded on metal and CFRP test specimens with flat bottom holes (FBH) were analysed by evaluating the detectability and by calculating the signal-to-noise ratio (SNR) of the defect signatures as a function of defect parameters. For the investigation of the influence of material properties on the spatial resolution as well as on penetration depth, test specimens made of steel and copper with crossed notches and a notch ramp were constructed and investigated. Here, the minimum resolvable notch distance and the maximum detectable depth of the ramp were analysed. T2 - 19th World Conference on Non-destructive Testing (WCNDT) CY - Munich, Germany DA - 13.06.2016 KW - Active thermography KW - Flash excitation KW - Round robin test KW - Standardisation PY - 2016 AN - OPUS4-36684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rothbart, Nick A1 - Maierhofer, Christiane A1 - Goldammer, M. A1 - Hohlstein, F. A1 - Koch, J. A1 - Kryukov, I. A1 - Mahler, G. A1 - Stotter, B. A1 - Walle, G. A1 - Oswald-Tranta, B. A1 - Sengebusch, M. T1 - A round robin test on flash thermography N2 - A round robin test on flash thermography was organized within the scope of a standardization research project. This test gives information on reliability, comparability and efficiency of different testing situations. Data recorded on metal and CFRP test specimens with flat bottom holes (FBH) were analysed by evaluating the detectability and by calculating the signal-to-noise ratio (SNR) of the defect signatures as a function of defect parameters. For the investigation of the influence of material properties on the spatial resolution as well as on penetration depth, test specimens made of steel and copper with crossed notches and a notch ramp were constructed and investigated. Here, the minimum resolvable notch distance and the maximum detectable depth of the ramp were analysed. T2 - 19th World Conference on Non-destructive Testing (WCNDT) CY - Munich, Germany DA - 13.06.2016 KW - Active thermography KW - Flash excitation KW - Round robin test KW - Standardisation PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-366853 SN - 978-3-940283-78-8 VL - BB 158 SP - We.3.D.4., 1 EP - 8 PB - DGZfP CY - Berlin AN - OPUS4-36685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaenisch, Gerd-Rüdiger T1 - Influence of scattered radiation on the efficiency of dual high-energy X-Ray imaging for material characterization N2 - In this contribution, we discuss the influence of scattered radiation on materials’ effective attenuation coefficients at higher X-ray energies. The selected X-ray spectra for the dual-energy experiments correspond to 3 MV and 7.5 MV acceleration potential of the used betatron. Experiments were performed on a test phantom containing step wedges of different low- and high-Z materials. We evaluated the ratio between low- and high-energy X-ray attenuation coefficients quantitatively based on simulated poly-energetic high-energy X-ray source spectra and the detector sensitivity using the “analytical Radiographic Testing inspection simulation tool” (aRTist) developed at BAM. Furthermore, the influence of scattered radiation is evaluated using an efficient Monte-Carlo simulation. The simulation results are compared quantitatively with experimental investigations. Finally, important applications of the proposed technique in the context of aviation security are discussed. T2 - 19th World Conference on Nondestructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Monte Carlo methods KW - Dual-energy imaging KW - Experiments KW - Simulation PY - 2016 AN - OPUS4-36607 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard A1 - Maenz, S. A1 - Bischoff, S. A1 - Bungartz, M. A1 - Bossert, J. A1 - Kunisch, E. A1 - Kinne, R. ED - Maenz, S. T1 - Micro computer tomography (μCT) set-up for long-term serial measurements, image evaluation, and subsequent compressive strength tests on frozen sheep vertebrae for osteoporosis research N2 - Injection of poly(methyl methacrylate) cements, one standard Treatment for osteoporotic vertebral body fractures, may lead to critical loads and subsequent fractures in adjacent vertebral bodies. Biodegradable calcium phosphate cements (CPC) with bioinductive growth factors may be an alternative, since they have a Young’s modulus comparable to that of cancellous bone. Non-destructive tests with μCT and quantitative Image evaluation are used to assess new bone growth and material resorption following intravertebral injection of CPC. Immediate deep-freezing of excised bone prevents shrinkage or tissue disintegration and the samples have to be kept frozen for all following steps, including transport, μCT measurements, and subsequent biomechanical tests. Here we will report on a set-up to preserve the frozen state of the material and allow stable long-term serial μCT measurements. In addition, the image processing technique for the evaluation of bone growth and selected results on subsequently carried out compressive strength tests will be presented. T2 - WCNDT2016 CY - München, Germany DA - 13.6.2016 KW - Computed tomography KW - Osteoporosis KW - CT PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-366410 UR - https://www.ndt.net/?id=19382 VL - BB 158 SP - 1 EP - 7 PB - DGZfP CY - Berlin AN - OPUS4-36641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Granulierte Hochofenschlacke als Mörtelzuschlag im 19. Jahrhundert in der Schweiz N2 - Als schweizweit einziger Hersteller produzierte die Gesellschaft der Ludwig von Roll'schen Eisenwerke seit den 1870er Jahren granulierte Hochofenschlacke. Im Blashochofen von Choindez im Schweizer Jura wird bis Mitte der 1920er Jahre Bohnerz aus dem Delsberger Becken, das kontemporär publizierten Analysen zufolge als Spuren- bzw. Schwermetalle Titan, Chrom, Blei und Vanadium enthält, zu grauem Roheisen verhüttet. In zementgebundenen Mörtelmischungen des 19. und frühen 20. Jahrhunderts aus verschiedenen Regionen der Schweiz finden sich neben reliktischen Hüttensandsplittern vereinzelt bis zu fünfhundert Mikrometer große scharze Kugeln mit grünlichem Schimmer, wohl nicht gemahlener Schlackensand. Deren mittels Ramanmikroskopie (Phasenbestand) und energiedispersiver Röntgenspektroskopie am Rasterelektronenmikroskop (Elementanalytik) ermittelte Mineralogie ergibt in Form von Plattnerit PbO2, Rutil TiO2 und vermitlich Chromit Fe(II)Cr2O4 bzw. Nichromit (Ni,Co,Fe(II))(Cr,Fe(III),Al)2)4 Übereinstimmungen mit den nur die Elementzusammensetzung berücksichtigenden historischen Resultaten. Ebenfalls im Zusammenhang mit dem das Bohnerz begleitenden Boluston samt Huppererde zu sehen sind die Minerale Coelestin SrSO4 und Zirkon ZrSiO4, des Weiteren der Siliciumcarbidpolymorph Moissanit SiC als Reaktionsprodukt von Quarzsand und Brennstoff. Die Kohärenz zwischen um die Jahrhundertwende durchgeführten Analysen von Rohmaterial als auch Ofenbruch aus dem in Choindez betriebenen Hochofen und den in diesem Beitrag diskutierten Resultaten moderner analytischer Methoden spricht für den Gebrauch von granulierter Schlacke aus dem Hause Ludwig von Roll als Mörtelzuschlag. Die Hüttensandkörner, eigentlich latent hydraulisch, sind aufgrund der fehlenden Aufbereitung zu grob für eine effektive Hydratation und deshalb trotz reaktiver Glasphase und Klinkermineralien (Belit Ca2SiO4 und Monocalciumaluminat CaAl2O4) intakt in der Bindemittelmatrix erhalten. N2 - From the 1870s the Ludwig von Roll ironworks produced granulated blast furnace slag in Choindez (Jura, Switzerland) as a by-product of the smelting of bean ore excavated until 1926 in the Delsberg Basin. According to historical analyses, this iron ore deposit contais heavy and trace metals such as titanium, chromium, lead and vanadium. In mortar samples from different regions of Switzerland originating from the 19th and early 20th centuries, residues of granulated blast furnace slag are observable as angular glassy particles in the binder matrix. In addition, black spherical grains with greenish lustre (up to 500 micrometres in diameter), probably not ground granulated blast furnace slag, can be distinguished sporadically in thin sections. Raman microscopy as well as scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM-EDX) measurements have revealed, inter alia, the presence of the crystalline components plattnerite PbO2, rutile TiO2 and presumably chromite Fe(II)Cr2O4 or nichromite (Ni,Co,Fe(II))(Cr,Fe(III),Al)2O4. These findings are consistent with historical analyses, which were restricted to the determination of the elemental (not phase) composition of the raw material processed by the Ludwig von Roll ironworks. Furthermore the minerals celestine SrSO4 and zircon ZrSiO4 can be linked to bean ore and bole from Delsberg, and likewise the silicon carbide moissanite SiC, which is a reaction product of quartz sand and coke. The coherence if the results of historical chemical analyses and of modern microscopic imaging and spectroscopy methods described here pinpoints the Ludwig von Roll ironworks as the most probable supplier of the granulated blast furnace slag that was added to the mortars under investigation. The unreacted remnants exhibit defined boundaries; no hydration rims are observable despite the glassy nature of the latent hydraulic aggregate, which contains cement clinker minerals (belite and calcium aluminate) as crystalline components. Not finely ground, the spheroids are too coarse for an effective hydration reaction and act as inert filler. KW - Granulierte Hochofenschlacke KW - Raman Mikroskopie KW - REM-EDX KW - Granulated blast furnace slag KW - Raman microscopy KW - SEM-EDX PY - 2015 VL - 29 IS - 2 SP - 293 EP - 304 PB - Wernersche Verlagsgesellschaft mbH CY - Worms AN - OPUS4-36651 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Daschewski, Maxim A1 - Bartusch, Jürgen A1 - Schadow, Florian A1 - Dohse, Elmar A1 - Kreutzbruck, Marc A1 - Weise, Matthias A1 - Beck, Uwe T1 - Novel air-coupled ultrasonic transducer combining the thermoacoustic with the piezoelectric effect N2 - In recent years, there has been an increasing industrial demand for one-sided inspection of various structures by means of air-coupled ultrasonic technique. Lightweight structures based on carbon-fibre-reinforced polymers may have very complex shapes, making air-coupled transmission difficult or even impossible. The inspection of concrete structures is another example where one-sided inspection is required. To address these challenges a new type of transducer for air-coupled pulse-echo inspection was developed, which unites two principles: thermoacoustic emission and piezoelectric reception. The thermoacoustic emitter is a titanium electrode with a thickness of several tens of nanometer. This electrode was deposited onto charged cellular polypropylene, which serves as a piezoelectric receiver. The thermoacoustic transmission is based on a transformation of the thermal energy of an electrically heated electrode into the acoustic energy of an ultrasonic wave. Thermoacoustic emitters provide resonance-free behaviour and thus extremely broadband pulses. Charged cellular polypropylene is piezoelectric due to the polarization of its cells and it is well matched to air, with a Young modulus in the order of magnitude of MPa. In this contribution we present some pulse-echo measurements with the first prototypes of the combined thermoacoustic-piezoelectric transducer. T2 - World Conference of Non-Destructive Testing CY - Munich, Germany DA - 13.6.2016 KW - Thermoacoustic KW - Piezoelectric KW - Ultrasonic transducer KW - Ferroelectret PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-367151 VL - 158 SP - Mo.1.F.4, 1 EP - 6 AN - OPUS4-36715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, D. T1 - Hydroformylation of long-chained alkenes in microemulsions: Raman-spectrometer assisted mini-plant operation N2 - Hydroformylation in microemulsions under mild reaction conditions is investigated using a Rhodium-based catalyst yields high selectivity of 98:2 of the desired linear product. A successful mini-plant operation for over 130 hours was performed. Online concentration monitoring of the system was done using 785nm Raman spectrometer. T2 - Conference: 9th International Symposium on Catalysis in Multiphase Reactors CY - Lyon, France DA - 07.12.2014 KW - Hydroformylierung KW - Reaction monitoring KW - Raman spectroscopy KW - Online monitoring KW - Prozessanalytik PY - 2014 AN - OPUS4-37400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Editorial: Es ist Arznei, nicht Gift, was ich dir reiche N2 - Im Rahmen der Herstellung und Überwachung von Arzneimitteln käme wohl niemand – außer dem alten Paracelsus – auf die Idee, diese Aussage in irgendeiner Form anzuzweifeln. Zeit, der Pharmazeutischen Industrie endlich einmal ein Kompliment zu machen. Danke zu sagen, für die technisch, wissenschaftliche Kultur, die fast für jede Krankheit etwas parat hat und uns, unserer Familie, unseren Freunden ein unbeschwertes und langes Leben ermöglicht. Leute, verkauft Euch doch nicht immer so schlecht! KW - Editorial KW - Nathan der Weise KW - Lessing KW - Quality by design KW - Real time release KW - PAT/QbD KW - Prozessanalytik PY - 2012 SN - 2191-8341 VL - 2 IS - 3 SP - 161 PB - Editio-Cantor-Verlag für Medizin und Naturwissenschaften (ECV) CY - Aulendorf AN - OPUS4-37401 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Ugly spectra and lousy interfaces – challenges for compact NMR spectroscopy in process control N2 - With the introduction of advanced process analytical technology, the closeness of key process variables to their limits can be directly controlled and the product can be classified or even released in real time. Compact NMR instruments can make NMR spectroscopy accessible in industrial and harsh environments for process control. T2 - ProcessNet-Jahrestagung und 32. DECHEMA-Jahrestagung der Biotechnologen 2016 CY - Aachen, Germany DA - 12.09.2016 KW - Industrie 4.0 KW - Online NMR spectroscopy KW - Reaction monitoring KW - Smart sensors PY - 2016 AN - OPUS4-37405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schäferling, Michael T1 - Editorial: Luminescent imaging with optical chemical sensors N2 - The intention of this compilation of articles was to introduce brand-new developments in the field of chemical imaging which have not been discussed in previous review articles. These include the design of new sensor nanomaterials based on photon uponversion crystals which convert near-infrared excitation light into sensor signals in the visible wavelength range highlighted by Christ and Schäferling. Sun, Ungerböck and Mayr describe the state of the art in oxygen imaging in microreactors and microfluidic devices. Miniaturized sensors for the imaging of oxygen, pH and temperature in microchips, microfluidic platforms and microbioreactors are reviewed by Pfeiffer and Nagl. Furthermore, Dmitriev and Papkovsky present a critical assessment of the applicability of probes for intracellular oxygen sensing. I hope these articles provide an interesting insight into advanced luminescent sensor materials and the applications of optical micro- and nanosensors in fluorescence imaging today and will be inspiring for the reader. Finally, I would like to thank all authors and referees for spending their time to enable this collection of articles. KW - Optical sensors KW - Fluorescence imaging KW - Chemical sensors PY - 2015 DO - https://doi.org/10.1088/2050-6120/3/4/040202 VL - 3 IS - 4 SP - 1 PB - IOP Publ. CY - Bristol AN - OPUS4-37444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Álvarez-García, J. A1 - Izquierdo-Roca, V. A1 - Pistor, P. A1 - Schmid, Thomas A1 - Pérez-Rodríguez, A. ED - Abou-Ras, D. ED - Kirchartz, T. ED - Rau, U. T1 - Raman spectroscopy on thin films for solar cells N2 - In the present chapter, the capabilities of Raman spectroscopy for the advanced characterisation of thin films for solar cells are reviewed. Raman spectroscopy is an optical, nondestructive technique based on the inelastic scattering of photons with elemental vibrational excitations in the material. The line shape and position of the Raman bands are determined by the crystalline structure and chemical composition of the measured samples, being sensitive to the presence of crystalline defects, impurities and strain. Presence of peaks characteristic of different phases also allows for the identification of secondary phases that are strongly related to the growth and process conditions of the films. All these aspects account for a strong interest in the analysis of the Raman spectra, providing a powerful nondestructive analytical tool for the structural and chemical assessment of the films. In addition, the combination of a Raman spectrometer with an optical microscope also allows for achieving a high spatial resolutions (of below 1 µm) when mapping surfaces and analyzing depth-resolved phase distributions in thin films. The present chapter is divided into four main sections: The two first ones are devoted to a revision of the Fundamentals of Raman spectroscopy (Section 17.2) and Vibrational modes in crystalline materials (Section 17.3). Section 17.4 deals with the main experimental considerations involved in the design and implementation of a Raman scattering setup. This is followed by a detailed description of the application of Raman scattering for the structural and chemico-physical analysis of thin film photovoltaic materials (Section 17.5), with the identification of crystalline structure and secondary phases, evaluation of film crystallinity, analysis of chemical composition of semiconductor alloys, characterisation of nanocrystalline and amorphous layers, stress effects and crystal orientations. This includes the description of corresponding state of the art and recent case examples that illustrate the capabilities of the Raman technique for the advanced characterisation of layers and process monitoring in thin-film photovoltaic technologies. KW - Thin-film solar cells KW - Polycrystalline materials KW - Raman spectroscopy KW - Raman microscopy PY - 2016 UR - http://eu.wiley.com/WileyCDA/WileyTitle/productCd-3527339922.html SN - 978-3-527-33992-1 SP - 469 EP - 499 PB - Wiley & Sons, Ltd. CY - Oxford, UK AN - OPUS4-37451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schäfer, N. A1 - Wilkinson, A. J. A1 - Schmid, Thomas A1 - Winkelmann, Aimo A1 - Chahine, G. A. A1 - Schülli, T. U. A1 - Rissom, T. A1 - Marquardt, J. A1 - Schorr, S. A1 - Abou-Ras, D. T1 - Microstrain distribution mapping on CuInSe2 thin films by means of electron backscatter diffraction, X-ray diffraction, and Raman microspectroscopy N2 - The investigation of the microstructure in functional, polycrystalline thin films is an important contribution to the enhanced understanding of structure–property relationships in corresponding devices. Linear and planar defects within individual grains may affect substantially the performance of the device. These defects are closely related to strain distributions. The present work compares electron and X-ray diffraction as well as Raman microspectroscopy, which provide access to microstrain distributions within individual grains. CuInSe₂ thin films or solar cells are used as a modelsystem. High-resolution electron backscatter diffraction and X-ray microdiffraction as well as Ramanmicrospectroscopy were applied for this comparison. Consistently, microstrain values were determined of the order of 10⁻⁴ by these three techniques. However,only electron backscatter diffraction, X-ray microdiffraction exhibit sensitivities appropriate for mapping local strain changes at the submicrometer level within individual grains in polycrystalline materials. KW - Microstrain KW - Thin film KW - X-ray microdiffraction KW - EBSD KW - Raman microspectroscopy PY - 2016 DO - https://doi.org/10.1016/j.ultramic.2016.07.001 SN - 0304-3991 SN - 1879-2723 VL - 169 SP - 89 EP - 97 PB - Elsevier B.V. AN - OPUS4-37453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Haftung und Haftfestigkeit: Grundlagen, Einflussgrößen, Prüfverfahren – Eine Übersicht N2 - Der Vortrag widmet sich Haftung und Haftfestigkeit bezüglich Grundlagen, Einflussgrößen sowie Prüfverfahren und beschreibt die Punkte: Generische und spezifische Motivation, Einflussgrößen auf Haftfestigkeit und Haftung von Beschichtungen, Prüfverfahren zur quantitativen Bestimmung der Haftfestigkeit und zur qualitativen Klassifizierung bzw. semi-quantitativen Bewertung der Haftung im Einzelnen. T2 - EFDS, 17. Wörlitzer Workshop "Schichthaftung - Anwendungsbeispiele aus der Praxis" CY - Oranienbaum-Wörlitz, Germany DA - 06.06.2016 KW - Haftfestigkeit KW - Klebfestigkeit KW - Verbundfestigkeit PY - 2016 AN - OPUS4-37479 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Production of inorganic RM N2 - Beschrieben wird anhand von Beispielen die Vorgehensweise der BAM bei der Zertifizierung von Referenzmaterialien T2 - I4S-Projekttreffen CY - Berlin, Germany DA - 22.09.2016 KW - Reference materials KW - Ceramics KW - Non-ferrous metals KW - Iron and steel PY - 2016 AN - OPUS4-37480 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Determination of perfluordecalin in consume care products by use of GF-HR-CS-MAS N2 - The introduction of HR-CS-MAS instrumentation, as it is shown in Fig. 1, provides a new way for the determination of non-metals including fluorine via molecular absorption. We present a sensitive and fluorine-specific method for total fluorine determination in fifteen consume care products in which perfluordecalin were declared (nail polishes, eye shadows and body creams). After pyrohydrolytic digestion of samples, fluorine content was determined by GF-HR-CS-MAS. Calcium was used as a molecule forming element and the molecular absorption of calcium monofluoride (CaF) at the wavelength 606.440 nm was used for its quantification. No matrix effect was observed. Analytical signal depends only on the fluorine concentration and therefore pure sodium fluoride NaF was used as calibration standard. The use of zirconium oxide nanoparticles as permanent modifier improves the limit of detection (from 0.2 to 0.1 ng) and characteristic mass (from 0.10 to 0.05 ng) from a previous reported method. These results were also compared with ISE method (standard DIN 51-084) and no significant difference was found T2 - Bremen Flourine Days CY - Bremerhafen, Germany DA - 03.07.2016 KW - Perfluordecalin KW - Consume care products KW - High resolution continuum source absorption spectrometry PY - 2016 AN - OPUS4-37481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Prozessanalytik für die moderne Verfahrenstechnik – Online-NMR- und -Raman-Spektroskopie im mizellaren Stoffsystem N2 - Homogen katalysierte Reaktionsschritte sind ein wichtiges Werkzeug in der chemischen Industrie. Durch die milden Reaktionsbedingungen hinsichtlich Temperatur und Druck bei gleichzeitig hoher Selektivität bieten diese die Möglichkeit energieeffizienter und ressourcenschonender Produktionsschritte. Eine der wichtigsten industriellen Anwendungen bildet die Hydroformylierung. Hier besteht das Katalysatorsystem meist aus Übergangsmetallkomplexen, vorwiegend Kobalt und Rhodium, die zur Steuerung der Selektivität und Löslichkeit mit mehrzähnigen Liganden koordiniert sind. Diese Komplexe liegen für eine effiziente Katalysator-rückführung in wässriger Lösung vor, was jedoch die Anwendbarkeit auf kurzkettige Edukte mit hinreichender Wasserlöslichkeit beschränkt. Ein möglicher Lösungsansatz für die Verwendung langkettiger Alkene ist die Umsetzung der Reaktion in einer Mikroemulsion. Durch die gesteigerte Phasen-grenzfläche besteht ein effektiver Kontakt von Katalysator und Reaktanden bei gleichzeitiger Möglichkeit der Produktseparation durch Phasentrennung, während der Katalysator dem Reaktionsschritt zurückgeführt wird und das Verfahren damit wirtschaftlich macht.[1] Am Beispiel der Reaktion von 1-Dodecen zu Tridecanal wird der Einsatz von Online-NMR- und -Raman-Spektroskopie für die Prozessanalytik (sowie Applikation von komplexen Regelungskonzepten) innerhalb eines mizellaren Systems demonstriert. Ein speziell konzipierter Laboraufbau ermöglicht die Durchführung von Experimenten unter Prozessbedingungen für die in Mikroemulsionen äußerst anspruchsvolle Entwicklung und Kalibrierung von multivariaten Modellen für die Raman-Spektroskopie. Diese konnten anschließend im Rahmen einer mehrtägigen Betriebs-studie einer Miniplant am realen technischen System erprobt werden. T2 - ProcessNet-Jahrestagung CY - Aachen, Germany DA - 12.09.2016 KW - Hydroformylierung KW - Prozessanalytik KW - Online-NMR-Spektroskopie KW - Online-Raman-Spektroskopie PY - 2016 N1 - Deutscher Vortrag mit englischsprachigen Folien AN - OPUS4-37385 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Broadband Dielectric Spectroscopy - Basics and Selected Applications N2 - The basics of broadband dielectric spectroscopy were introduced in detail. The analysis of the data was discussed. As application of broadband dielectric spectroscopy the alpha-relaxation (dynamic glass transition) and the chain dynamics of polymers were ilustrated. T2 - 9th International Conference on Broadband Dielectric Spectroscopy and its Applications CY - Pisa, Italy DA - 11.09.2016 KW - Broadband Dielectric Spectroscopy PY - 2016 AN - OPUS4-37386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Behavior of Ultra-Thin Films of Blends of Polystyrene/ Poly(vinyl methyl ether) by Nanosized Relaxation Spectroscopy N2 - In the course of miniaturizing modern technology down to the molecular scale, understanding the materials behavior has to be investigated and deviations from the bulk that might arises from confinement effects has to be understood. Here, a combination of nano-sized relaxation spectroscopies (Broadband dielectric spectroscopy (BDS) and Specific heat spectroscopy (SHS); employing AC nanochip calorimetry) were utilized to investigate the glassy dynamics of ultra-thin films of blends of Poly (vinyl methyl ether) (PVME) / Polystyrene (PS) 50:50 wt-%, which are miscible bulk (thicknesses: 8nm - 200nm, film thickness was controlled by ellipsometry, film topography by AFM). Both methods are sensitive to different probes; where SHS senses entropy fluctuations while BDS measures dipole fluctuations. For BDS measurements, a recently developed nano-structured electrode sample arrangement is employed; where ultra-thin films are spin-coated on an ultra-flat highly conductive silicon wafer, sandwiched between a wafer with nanostructured SiO2 nano-spacers with heights between 35 nm and 70 nm. The method was applied for film thicknesses up to 50 nm. For thicker films, the samples were prepared between crossed electrodes. It was proven that, for 50 nm films, both contact methods will lead to identical results. By measuring the dynamic Tg in dependence of the film thickness, SHS showed that the Tg of the whole film was strongly influenced by a nanometer-thick surface layer at the polymer/air interface due to a self-assembling process [1]. The dynamic Tg obtained from the SHS measurements decrease with decreasing film thickness, evidencing the importance of a mobile surface layer at the polymer/air interface for the glass transition of the whole film. Compared to the SHS results, the BDS measurements show a completely different behavior. At high temperatures, the temperature dependence of the relaxation times of the films follows that of bulk-like PS/PVME; obeying the VFT-law. With decreasing temperature, the temperature dependence deviates from the VFT to an Arrhenius law; where the apparent activation energy decreases with decreasing film thickness. This is the first example where confinement induced changes were observed by BDS for ultra-thin films. All results were analyzed in details in a comprehensive discussion. T2 - 9th International Conference on Broadband Dielectric Spectroscopy and its Applications CY - Pisa, Italy DA - 11.09.2016 KW - Ultra-Thin films KW - Broadband Dielectric Spectrscopy KW - Nanostructured Electrodes PY - 2016 AN - OPUS4-37387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Prozessanalytik für die moderne Verfahrenstechnik – Online-NMR- und -Raman-Spektroskopie im mizellaren Stoffsystem N2 - Homogen katalysierte Reaktionen sind wichtige Werkzeuge der chemischen Industrie. Milde Reaktionsbedingungen und hohe Selektivitäten führen zu einer energie- und ressourcenschonenden Produktion. Ein bedeutender Prozessschritt ist die Hydroformylierung. Hier kommen Kobalt- und Rhodiumkomplexe mit mehrzähnigen Liganden zum Einsatz, die zumeist in wässriger Lösung vorliegen. Die Anwendbarkeit beschränkt sich demnach auf kurzkettige Edukte mit hinreichender Wasserlöslichkeit. T2 - ProcessNet-Jahrestagung und 32. DECHEMA-Jahrestagung der Biotechnologen 2016 CY - Aachen, Germany DA - 12.09.2016 KW - Hydroformylierung KW - Mizellen KW - NMR-Spektroskopie KW - Raman-Spektroskopie KW - Chemometrie KW - Prozesssensoren KW - Prozessanalytik KW - Industrie PY - 2016 AN - OPUS4-37388 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Ugly Spectra and Lousy interfaces – Challenges for Compact NMR Spectroscopy in Process Control N2 - With the introduction of advanced process analytical technology, the closeness of key process variables to their limits can be directly controlled and the product can be classified or even released in real time. Compact NMR instruments can make NMR spectroscopy accessible in industrial and harsh environments for process control. T2 - ProcessNet-Jahrestagung und 32. DECHEMA-Jahrestagung der Biotechnologen 2016 CY - Aachen, Germany DA - 12.09.2016 KW - Industrie 4.0 KW - CONSENS KW - Reaction Monitoring KW - Smart Sensors KW - Online NMR Spectroscopy KW - Lithiation PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-373895 AN - OPUS4-37389 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roussel, N. A1 - Gram, A. A1 - Cremonesi, M. A1 - Ferrara, L. A1 - Krenzer, K. A1 - Mechtcherine, V. A1 - Shyshko, S. A1 - Skocec, J. A1 - Spangenberg, J. A1 - Svec, O. A1 - Thrane, L. N. A1 - Vasilic, Ksenija T1 - Numerical simulations of concrete flow: A benchmark comparison N2 - First, we define in this paper two benchmark flows readily usable by anyone calibrating a numerical tool for concrete flow prediction. Such benchmark flows shall allow anyone to check the validity of their computational tools no matter the numerical methods and parameters they choose. Second, we compare numerical predictions of the concrete sample final shape for these two benchmark flows obtained by various research teams around the world using various numerical techniques. Our results show that all numerical techniques compared here give very similar results suggesting that numerical simulations of concrete filling ability when neglecting any potential components segregation have reached a technology readiness level bringing them closer to industrial practice. KW - Casting KW - Fresh Concrete KW - Rheology KW - Workability KW - Modeling PY - 2016 UR - http://www.sciencedirect.com/science/article/pii/S0008884615002604 DO - https://doi.org/10.1016/j.cemconres.2015.09.022 SN - 0008-8846 VL - 2016/79 SP - 265 EP - 271 PB - Elsevier Ltd. AN - OPUS4-37440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Vasilic, Ksenija A1 - Geiker, M. A1 - Hattel, J. A1 - Martinie, L. A1 - Martys, N. A1 - Roussel, N. A1 - Spangenberg, J. ED - Roussel, N. ED - Gram, A. T1 - Advanced methods and future perspectives N2 - The one-phase methods described in Chapter 2 were shown to be able to predict casting to some extent, but could not depict segregation, sedimentation and blockage occurring during flow. On the other hand, the distinct element methods described in Chapter 3 did not take into account the presence of two phases in the system and describes concrete as distinct elements interacting through more or less complex laws. A reliable numerical model of a multiphase material behaviour shall take into account both phases (solid and liquid). From the numerical point of view, concrete flow shall be seen therefore as the free surface flow of a highly-concentrated suspension of rigid grains. KW - SCC KW - Numerical simulation PY - 2014 SN - 978-94-017-8883-0 DO - https://doi.org/10.1007/978-94-017-8884-7_5 VL - 15 SP - 125 EP - 146 PB - Springer Netherlands AN - OPUS4-37443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Raman Spektroskopie zur kontinuierlichen Überwachung einer Hydroformylierungsreaktion N2 - Der Beitrag beinhaltet die Vorstellung eines gemeinsamen Projekts zwischen der BAM und der TU Berlin (Process Dynamics and Operations Group). Mittels Raman Spektroskopie werden Hydroformylierungsreaktionen in einer Miniplant der TU prozessbegleitend untersucht. Kalibrationsstrategien, Laboruntersuchungen sowie Vorhersagen von Prozessmessungen basierend auf chemometrischen Modellen werden vorgestellt. Zum gegenwärtigen Zeitpunkt wird die Strategie als erfolgsversprechend bewertet, jedoch sind weitere Untersuchungen insbesondere zum Einfluss der Microemulsion auf die Ramanspektren notwendig. T2 - 12. PAT ERFA CY - Mainz / Ingelheim, Germany DA - 20.09.2016 KW - Raman Spektroskopie KW - Online KW - Multivariate Datenanalyse KW - Miniplant PY - 2016 AN - OPUS4-37469 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Bräuer, Bastian A1 - Nieuwenkamp, G. A1 - Ent, H. A1 - Bremser, Wolfram T1 - A validated near-infrared spectroscopic method for methanol detection in biodiesel N2 - Abstract. Biodiesel quality control is a relevant issue as biodiesel properties influence diesel engine performance and integrity. Within the European Metrology Research Program (EMRP) ENG09 project “Metrology for Biofuels”, an on-line /at-site suitable near-infrared spectroscopy (NIRS) method has been developed in parallel with an improved EN14110 headspace GC analysis method for methanol in biodiesel. Both methods have been optimized for a methanol content of 0.2 mass% as this represents the maximum limit of methanol content in FAME according to EN 14214:2009. The NIRS method is based on a mobile NIR spectrometer equipped with a fiber-optic coupled probe. Due to the high volatility of methanol, a tailored air-tight adaptor was constructed to prevent methanol evaporation during measurement. The methanol content of biodiesel was determined from evaluation of NIRS spectra by Partial Least Squares Regression (PLS). Both GC analysis and NIRS exhibited a significant dependence on biodiesel feedstock. The NIRS method is applicable to a content range of 0.1 % (m/m) to 0.4 % (m/m) of methanol with uncertainties at around 6% relative for the different feedstocks. A direct comparison of headspace GC and NIRS for samples of FAMEs yielded that the results of both methods are fully compatible within their stated uncertainties. KW - FAME KW - Headspace GC KW - NIR KW - PLSR KW - EMRP PY - 2016 DO - https://doi.org/10.1088/0957-0233/27/6/065002 SN - 0957-0233 SN - 1361-6501 VL - 27 IS - 6 SP - 065002, 1 EP - 9 PB - IOP Publishing Ltd CY - UK AN - OPUS4-37471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - On-site carbon analysis of coal using a mobile LIBS system N2 - The information about the chemical composition of coal is of great interest during mining, sorting and processing. Due to great variations of the soil layers the quality of coal suffers great fluctuations during mining because of adjoining rocks [1-6]. To provide on-site analysis of coal the application of LIBS as a multi-element method has been tested. Therefore different qualities of coal have been chemically analyzed to get reference values for the water content as well as for the major (carbon) and minor components (ash = Ca, Mg, S, Si). For the LIBS analysis a system using a low energy laser with a wavelength of 1064 nm, pulse energy of 3 mJ, pulse length of 1.5 ns and a repetition rate of 100 Hz have been used. A compact czerny turner spectrometer operating in the UV range (Δλ = 170 nm – 350 nm) have been applied. To provide quantitative concentrations different calibration curves have been evaluated using chemometrics. The system has been validated using internal cross-validation as well as an external set of samples. For the evaluation of the method different figures of merit will be presented. After applying LIBS for coal analysis in the laboratory a LIBS system for the on-site analysis has been tested during the mining process. T2 - 9th International Conference on Laser Induced Breakdown Spectroscopy (LIBS2016) CY - Chamonix, Switzerland DA - 12.09.2016 KW - LIBS KW - On-site LIBS KW - Coal PY - 2016 AN - OPUS4-37420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - 2D evaluation of heterogenous building materials using cluster algorithm N2 - In civil engineering the information about the quantitative ingress of harmful species like Cl⁻, Na⁺ and SO²⁻₄ is of great interest to evaluate the remaining life time of structures. These species are triggering different damage processes like the alkali-silica reaction (ASR) or the chloride-induced corrosion of the reinforcement. For the evaluation of the heterogeneous concrete it is necessary to discriminate between the different phases mainly cement matrix and aggregates. The transport processes are only proceeding in the cement matrix therefore the measured concentrations should be regarded to the cement content. For the 2D evaluation of element distributions different multivariate cluster-algorithms like k-means and Expectation-Maximization-algorithm (EM-algorithm) have been tested. The methods are compared and different figures of merit will be presented. After phase separation non-relevant information of the aggregates can be excluded. The ingress of harmful species is then quantified using chemometrics. Due to concrete cores from a parking deck the methods have been validated and verified with standard methods of wet-chemistry. T2 - 9th International Conference on Laser Induced Breakdown Spectroscopy (LIBS2016) CY - Chamonix, France DA - 12.09.2016 KW - LIBS KW - Building materials KW - Heterogeneity KW - Clustering PY - 2016 AN - OPUS4-37421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Anwendung von RFA und FOES zur Homogenitätsuntersuchung von Referenzmaterialien N2 - Die Bundesanstalt für Materialforschung und -prüfung (BAM) produziert seit vielen Jahren zertifizierte Referenzmaterialien und ist seit 2016 auch als Referenzmaterialhersteller nach ISO Guide 34 akkreditiert. Vor jeder Zertifizierungskampagne eines zukünftigen Referenzmaterials, welches im Batch zertifiziert wird, steht ein Homogenitätstest. Dabei spielt die Richtigkeit des verwendeten Analysenverfahrens nur eine untergeordnete Rolle. Viel wichtiger ist, dass ein Verfahren mit möglichst hoher Präzision eingesetzt wird. Wichtig ist außerdem, dass die für den Homogenitätstest eingesetzte Probemenge der Mindestmenge des ZRMs bei der zukünftigen analytischen Nutzung des Materials entspricht. Für kompaktes Material bieten sich Röntgenfluoreszenzanalyse (RFA) und Funkenemissionsspektrometrie (FOES) als Analysenverfahren an. Die RFA kann darüber hinaus auch für pulverförmige Materialien eingesetzt werden. Im Vortrag werden verschiedene Beispiele für die Verwendung der genannten Analysenmethoden für Homogenitätsuntersuchungen aus der Praxis eines Referenzmaterialherstellers beschrieben. T2 - 23. Anwendertreffen Röntgenfluoreszenz- und Funkenemissionsspektrometrie CY - Dortmund, Germany DA - 01.03.2016 KW - Referenzmaterial KW - Funkenemission KW - Röntgenfluoreszenzanalyse PY - 2016 AN - OPUS4-37426 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Zentrifugentechnologie in der Beanspruchung auf Zug und Druck; Zug-und Zugscherprüfung von CFK N2 - Der Vortrag widmet sich der Zentrifugentechnologie und beschreibt die Punkte der Beanspruchung auf Zug und Druck, Zug- und Zugscherprüfung von geklebten CFK-Platten im Einzelnen. T2 - Videokonferenz CY - Dingolfing, Germany DA - 13.06.2016 KW - Zentrifugentechnologie KW - Klebfestigkeit KW - Härteprüfung KW - CFK PY - 2016 AN - OPUS4-37494 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ortel, Erik A1 - Häusler, Ines A1 - Österle, Werner A1 - Narbey, S. A1 - Oswald, F. A1 - Andersen, I. H. A1 - Holzweber, Markus A1 - Unger, Wolfgang A1 - Hodoroaba, Vasile-Dan T1 - In-depth structural and chemical characterization of engineered TiO2 films N2 - Analytical routines for a comprehensive in-depth morphological, structural, and chemical characterization of functionalized TiO2 films by using different state-of-the-art analytical techniques are presented and discussed with the main objective to identify potential reference TiO2 coating parameters able to be certified at a later stage. TiO2 films fabricated by two different synthetic procedures as representative for two main large-scale applications were selected: (i) pulsed d.c. magnetron sputtering for photocatalytic applications and (ii) screen printing from preformed anatase nanoparticles. The screen-printed films were further loaded with a sensitizing dye for application as a dye-sensitized solar cell. Film properties such as microstructure and crystallographic texture of pulsed d.c. magnetron sputtering synthesized films were systematically studied by means of scanning nanobeam electron diffraction in a transmission electron microscope and the surface and inner morphology by scanning electron microscopy. The dye distribution over the depth of screen-printed TiO2 layers was analyzed before and after dye-loading by means of energy dispersive X-ray spectroscopy at scanning electronmicroscope, Auger electron spectroscopy and time-of-flight secondary ion mass spectrometry. The long-term goal of the present study is the improvement of quality of the TiO2 film parameters as measured by using different types of reference TiO2 coatings having specific parameters certified. T2 - 16th European Conference on Applications of Surface and Interface Analysis ECASIA'15 CY - Granada, Spain DA - 28.09.2015 KW - Mapping KW - Line scan KW - Depth profiling KW - TiO2 films KW - Crystallinity KW - Ru dye sensitizer PY - 2016 DO - https://doi.org/10.1002/sia.5966 SN - 0142-2421 SN - 1096-9918 VL - 48 SP - 664 EP - 669 PB - John Wiley & Sons, Ltd. AN - OPUS4-36791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Babick, F. A1 - Mielke, Johannes A1 - Wohlleben, W. A1 - Weigel, St. A1 - Hodoroaba, Vasile-Dan T1 - How reliably can a material be classified as a nanomaterial? Available particle-sizing techniques at work N2 - Currently established and projected regulatory frameworks require the classification of materials (whether nano or non-nano) as specified by respective definitions, most of which are based on the size of the constituent particles. This brings up the question if currently available techniques for particle size determination are capable of reliably classifying materials that potentially fall under these definitions. In this study, a wide variety of characterisation techniques, including counting, fractionating, and spectroscopic techniques, has been applied to the same set of materials under harmonised conditions. The selected materials comprised well-defined Quality control materials (spherical, monodisperse) as well as industrial materials of complex shapes and considerable polydispersity. As a result, each technique could be evaluated with respect to the determination of the number-weighted median size. Recommendations on the most appropriate and efficient use of techniques for different types of material are given. KW - Nanomaterial classification KW - Nanoparticle KW - Number-weighted median size KW - Tiered KW - Particle size analysis KW - Nanometrology KW - Characterisation techniques PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-367922 UR - http://link.springer.com/article/10.1007/s11051-016-3461-7 DO - https://doi.org/10.1007/s11051-016-3461-7 SN - 1388-0764 SN - 1572-896X VL - 18 IS - 6 SP - Article 158, 1 EP - 40 PB - Springer AN - OPUS4-36792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc T1 - Coulometric trace humidity measurement in industrial gases N2 - Coulometric sensors are applied for trace humidity measurements in various technical gases. The use of this sensor type is demanded in some standards by the European Pharmacopoeia for medical gases. Coulometric sensors allow the measurement of water vapour in gases such as e.g. air, Cl2, H2, N2, N2O, CH4 between the concentration ranging from 0.1 to 2,500 µmol∙mol-1 which corresponds to frost point temperature -90 °C to -10 °C, respectively. The sensing principle is based on Faraday’s law of electrolysis whereby water is decomposed to hydrogen and oxygen. The sensor signal is the measured electrical current which is proportional to the mass of water that is absorbed on the hygroscopic phosphorous pentoxide layer. The signal is dependent on the gas flow at a given voltage, gas pressure and temperature. The sensors need to be calibrated to measure the accurate signal for humidity in air. However, the signal is dependent on the type of gas matrix. This dependency has not been quantified so far. Therefore, the impact of reactive gases such as hydrogen and nitrous oxide on the calibration curve was investigated. Furthermore, a possible rationale in relation to the interaction of water with the gas matrix and its impact on the electrode reactions is suggested. The experimental setup consists of a gas supply, dryer, humidifier, test chamber and reference hygrometer. The test gas is generated by mixing the dry and the wet gas flow. First the carrier gas is dried by an activated carbon filter and then split into two flows. One flow is dried again with a molecular sieve. The other flow is humidified by passing it through a bubbler filled with pure water. After this, the rate of both flows is controlled by mass flow controllers and then mixed with the test gas. A calibrated precision chilled mirror dew-point hygrometer is used as a reference instrument. The coulometric sensors were exposed to different humidified gases and the sensor signal was recorded till a constant value was obtained. Calibration curves were calculated for the frost point temperature in the range of about -70 °C to -10 °C according to the equation, tf = A + B∙ln(I), (I is the electrolysis current and A, B are constants) followed with a linear regression fit. Comparison of the results of air and nitrogen showed no significant differences. In contrast, there are remarkable differences for humidified hydrogen and nitrous oxide, respectively. The difference might be due to increased recombination of hydrogen with the produced oxygen to form new water molecules in humidified hydrogen. In conclusion, coulometric trace humidity sensor is a robust hygrometer for various technical applications. However it needs to be calibrated for the specific gas matrix. T2 - Tempmeko 2016 CY - Zakopane, Poland DA - 27.06.2016 KW - Trace humidity KW - Coulometric sensor KW - Industrial gases PY - 2016 AN - OPUS4-36793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carvalho, Margarida T1 - Addressable Immunoarrays: Protein-Nucleic Acid Conjugate Production N2 - Immunoassays are analytical methods used to track both clinical and environmental parameters. Antibodies or other proteins with similar recognizing activity, are employed, often immobilized onto a modified surface. Addressable microarrays are based on single-stranded DNA oligonucleotides which are normally used to detect aptamers or relevant gene sequences. The use of antibody-oligonucleotide conjugates allows non-directed antibody immobilization from an immunoassay to be converted into DNA hybridization events on the array. Consequently, the diagnostics platform is multiplexed and addressable. Figure 1 is a model representation of the whole biosensor construct. In brief, a surface is coated with streptavidin, and decorated with biotin-modified oligonucleotides of a controlled size and known sequence. These oligonucleotides on the surface also contain a furan motif, which upon irradiation and in the presence of a photosensitizer, is oxidized via single oxygen to a reactive intermediate which crosslinks the immediate opposing base when hybridized with its complementary strand [1]. Antibody-oligonucleotides conjugates still display several concerns due to their heterogeneicity, difficulty of characterization and high price [2]. The being the case, we aim at developing stable, robust, reproducible and well characterized quimeras for the application on te above described immunoarray. Mild chemical conditions are crucial for the antibody stability, therefore bivalent crosslinkers have been employed [2]. Even though the use of these bilinkers is standard for other substrate conjugation (i.e., enzymes, drug payloads, etc.), there is no literature available on the conjugation of small oligonucleotides (< 30 mer) to antibodies using this method. Several protein-nucleic acid conjugates have been therefore developed, and successfully characterized using MALDI-ToF and gel electrophoresis techniques. T2 - SO2S - The singlet Oxygen Strategy - Final Network Meeting CY - Gent, Belgium DA - 14.06.2016 KW - Antibodies KW - Immunoarrays KW - Nucleic acids PY - 2016 AN - OPUS4-36680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fréjafon, E. A1 - Salvi, O. A1 - Hazebrouck, B. A1 - Le Feber, M. A1 - López de Ipiña Peña, J. A1 - Unger, Wolfgang T1 - Creation of the European centre for risk management and safe innovation in nanomaterials & nanotechnologies (EC4SafeNano) N2 - Safe innovation & sustainable production with MNMs need that we: Understand risks and benefits (diagnostic, assessment) Identify and implement risk reduction strategies (manage) Communicate on residual risks (acceptance) Huge knowledge on characterization, hazards, diagnostic (science) Little effective use of it for operational risk management (expertise) Objectives of the centre: Bridge the gap between research and application (public, private), Bridge the gap between knowledge on risks and risk management, Balance between Science and Appliance, in a sustainable way: Efficient & Sustainable structure Collective, harmonized, shared expertise EU scale, internationally connected. T2 - Workshop "NanoSafety: from research to implementation" CY - Amsterdam, The Netherlands DA - 22.06.2016 KW - Nano materials KW - Risk management KW - Safe innovation PY - 2016 UR - http://nanomile.eu-vri.eu/news.aspx?lan=230&tab=2361&nid=991#n991 AN - OPUS4-36966 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Novel air-coupled ultrasonic transducer combining the thermoacoustic with the piezoelectric effect N2 - In recent years, there has been an increasing industrial demand for one-sided inspection of various structures by means of air-coupled ultrasonic technique. Lightweight structures based on carbon-fibre-reinforced polymers may have very complex shapes, making air-coupled transmission difficult or even impossible. The inspection of concrete structures is another example where one-sided inspection is required. To address these challenges a new type of transducer for air-coupled pulse-echo inspection was developed, which unites two principles: thermoacoustic emission and piezoelectric reception. The thermoacoustic emitter is a titanium electrode with a thickness of several tens of nanometer. This electrode was deposited onto charged cellular polypropylene, which serves as a piezoelectric receiver. The thermoacoustic transmission is based on a transformation of the thermal energy of an electrically heated electrode into the acoustic energy of an ultrasonic wave. Thermoacoustic emitters provide resonance-free behaviour and thus extremely broadband pulses. Charged cellular polypropylene is piezoelectric due to the polarization of its cells and it is well matched to air, with a Young modulus in the order of magnitude of MPa. In this contribution we present some pulse-echo measurements with the first prototypes of the combined thermoacoustic-piezoelectric transducer. T2 - World Conference of Non-Destructive Testing CY - Munich, Germany DA - 13.6.2016 KW - Ferroelectret KW - Thermoacoustic KW - Piezoelectric KW - Ultrasonic transducer PY - 2016 AN - OPUS4-36716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meiling, T. A1 - Cywinski, P. A1 - Bald, Ilko T1 - White carbon: Fluorescent carbon nanoparticles with tunable quantum yield in a reproducible green synthesis N2 - In this study, a new reliable, economic, and environmentally-friendly one-step synthesis is established to obtain carbon nanodots (CNDs) with well-defined and reproducible photoluminescence (PL) properties via the microwave-assisted hydrothermal treatment of starch and Tris-acetate-EDTA (TAE) buffer as carbon sources. Three kinds of CNDs are prepared using different sets of above mentioned starting materials. The as-synthesized CNDs: C-CND (starch only), N-CND 1 (starch in TAE) and N-CND 2 (TAE only) exhibit highly homogenous PL and are ready to use without need for further purification. The CNDs are stable over a long period of time (>1 year) either in solution or as freeze-dried powder. Depending on starting material, CNDs with PL quantum yield (PLQY) ranging from less than 1% up to 28% are obtained. The influence of the precursor concentration, reaction time and type of additives on the optical properties (UV-Vis absorption, PL emission spectrum and PLQY) is carefully investigated, providing insight into the chemical processes that occur during CND formation. Remarkably, upon freeze-drying the initially brown CND-solution turns into a non-fluorescent white/slightly Brown powder which recovers PL in aqueous solution and can potentially be applied as fluorescent marker in bio-imaging, as a reduction agent or as a photocatalyst. KW - Carbon dots KW - Quantum yield KW - Fluorescence KW - Nanoparticles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-367204 DO - https://doi.org/10.1038/srep28557 VL - 6 SP - Article 28557, 1 EP - 9 PB - Nature Publishing Group AN - OPUS4-36720 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ehlert, Christopher A1 - Holzweber, Markus A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Saalfrank, Peter T1 - A detailed assignment of NEXAFS resonances of imidazolium based ionic liquids N2 - In Near Edge X-Ray Absorption Fine Structure (NEXAFS) spectroscopy X-Ray photons are used to excite tightly bound core electrons to low-lying unoccupied orbitals of the system. This technique offers insight into the electronic structure of the system as well as useful structural information. In this work, we apply NEXAFS to two kinds of imidazolium based ionic liquids ([CnC₁im]⁺[NTf₂]⁻ and [C₄C₁im]⁺[I]⁻). A combination of measurements and quantum chemical calculations of C K and N K NEXAFS resonances is presented. The simulations, based on the transition potential density functional theory method (TP-DFT), reproduce all characteristic features observed by the experiment. Furthermore, a detailed assignment of resonance features to excitation centers (carbon or nitrogen atoms) leads to a consistent interpretation of the spectra. KW - Ionic liquids KW - NEXAFS KW - DFT spectrum simulations PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-367223 DO - https://doi.org/10.1039/c5cp07434g SN - 1463-9076 SN - 1463-9084 VL - 18 IS - 12 SP - 8654 EP - 8661 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-36722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Advanced surface chemical analysis of plasma modified polymers and plasma-polymers N2 - A comprehensive characterization of plasma modified polymer surfaces or plasma-polymerized thin films needs access to parameters as - concentration of saturated/unsaturated carbon species (e.g. aromaticity) or other double bonds as C=N or C=O, - branching, and - losses of crystallinty or other degrees of structural order. Furthermore the complex ageing phenomena of plasma modified polymers/plasma-polymers and the measurement of an in-depth distribution of chemical species are challenges for the analyst. The talk will display selected examples where such challenges have been met by using advanced methods of surface chemical analyses as Photoelectron Spectroscopy with variable excitation energy (“SyncXPS”), X-ray Absorption Spectroscopy (NEXAFS) at C, N and O K-edges and Time-of-Flight Secondary Mass Spectroscopy (ToF-SIMS) combined with Principal Component analysis (PCA). T2 - IAP workshop – IAP 2016 "Organic surface modifications by plasmas and plasma-polymers" CY - Nancy, France DA - 08.06.2016 KW - XPS KW - NEXAFS KW - SIMS KW - Plasmapolymer PY - 2016 AN - OPUS4-36725 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sieg, H. T1 - Impact of (artificial) digestion on Al-containing nanomaterials and their physico-chemical characteristics N2 - Aluminium and its chemical derivatives are highly abundant in food, food contact materials and consumer products. Up to now little is known about its derivatization and uptake during digestion and its impact on human health. As part of the SolNanoTOX project, different aluminium species were investigated during an artificial digestion process that mimics the saliva, the stomach and the intestine regarding pH-values, duration time, chemical environment and enzymatic composition. Two different nanomaterials (Al, Al2O3) and a soluble ionic AlCl3 control were digested and investigated by different analytical methods regarding core radius, hydrodynamic diameter, agglomeration and dissolution behavior in biological media. The fate of nanoparticles during typical pH-values of saliva, gastric and intestinal juice was studied with dynamic light scattering (DLS), small angle X-ray scattering (SAXS) and ICP-MS in the single particle mode. After disappearance at pH 2 the nanoparticles were detected again in the intestinal fluid, as measured by DLS. During all artificial digestion stages Al nanoparticles had a constant average SAXS radius. In contrast, the radii of Al2O3 nanoparticles changed concentration-dependently. Highest radii were observed in the stomach fluid while intestinal fluid was found to cause full recovery of the primary particles. Dissolution of digested nanoparticles in cell culture media showed a bimodal size distribution of primary particles and aggregates. In summary, simulation of the gastrointestinal tract, mainly the change of pH settings, has provided evidence that the bioavailability of Al is likely to increase during the passage of the gut after oral uptake of aluminium-containing food products. T2 - 8th International Nanotoxicology Congress CY - Boston, MA, USA DA - 01.06.2016 KW - Artificial digestion KW - SAXS KW - DLS PY - 2016 AN - OPUS4-36919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sieg, H. T1 - Toxicological effects of artificially digested Al-containing nanomaterials on intestinal cell lines in vitro N2 - Although aluminium is one of the most common elements in the biosphere, little is known about its impact on human health. Since aluminium derivatives are highly abundant in food its oral uptake route is of toxicological relevance. Recently aluminium-containing nanomaterials are considered to be linked to cancer and neurodegenerative disorders. Within the frame of the european SolNanoTOX project, we therefore investigated the toxicological effects of Al-containing species in different intestinal cell lines that represent the first biological barrier for food components prior to systemic distribution. In our in vitro digestion system, nanomaterials have been exposed to different physiological, chemical and biochemical conditions characteristic for saliva, gastric juice and the intestinal fluid. In vitro toxicity assays and cellular impedance measurements demonstrated the absence of cytotoxic effects of nanoparticles during a period of 48h after incubation. This was also observed after the digestion procedure. In contrast, aluminium ions from high concentrations of AlCl3 showed larger effects on cell viability after the digestion procedure. In summary, the toxicological potential of aluminium-containing nanoparticles and ions to healthy intestinal cells appears to be low. Artificial digestion of these particles does not increase their toxic potential. Only for high doses of ionic aluminium, an increase of toxicity after artificial digestion was observed. Hence, we suggest that the release of Al ions from nanoparticles may lead to toxicity. Due to these observations, other cellular effects of Al-containing nanomaterials are required to be investigated. T2 - 8th International Nanotoxicology Congress CY - Boston, MA, USA DA - 01.06.2016 KW - Artificial digestion KW - Cytotoxicity KW - Caco-2 cells PY - 2016 AN - OPUS4-36920 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sieg, H. T1 - Cellular effects of Al-, Ti- and Zn-containing nanomaterials on intestinal cell lines in vitro N2 - Aluminium-, titanium- and zinc-containing chemicals are highly abundant in food, food contact materials and consumer products. Physical and chemical conversion might lead to a certain amount of nanoscaled particles that can be taken up by the gastrointestinal tract. Nanospecific effects such as higher reactivity, increased surface or altered uptake can increase hazardous potential for human health. The aim of this study as part of the european SolNanoTOX project is to characterize toxicological effects of Al-, Zn- and Ti-containing nanomaterials on intestinal cell lines. While toxicological potential of zinc species has been well studied, little is known about the effects of aluminium- and titanium-species. We have performed toxicological experiments on the human intestinal cell line Caco-2 for numerous endpoints: Cellular ATP and glutathione levels, apoptosis, necrosis, vesicular uptake, oxidative stress, growth rate and cell cycle modification. While zinc-containing controls showed toxic responses, our utilized aluminium- (elementary Al, γ-Al2O3) and titanium-species (TiO2, rutile) did not. Nevertheless, we detected some differences between both different aluminium nanoparticle species and aluminium ions with regard to cell viability. We also provide strong evidence for particle-specific uptake of aluminium and titanium in the intestinal cell line Caco-2. In summary, among the different tested endpoints, Al- and Ti-containing nanomaterials did not show any toxicity in intestinal cell lines in vitro. Nevertheless, this absence of effect was not due to an absence of exposure, since particle-specific uptake was reported. Metal particle uptake over a long time might therefore be relevant for risk assessment of aluminium- and titanium-containing food products. T2 - 8th International Nanotoxicology Congress CY - Boston, MA, USA DA - 01.06.2016 KW - Artificial digestion KW - SAXS KW - Cell viability KW - Toxicity PY - 2016 AN - OPUS4-36921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kästner, Claudia T1 - Artificial Digestion of Colloidal Silver Monitored by Small-Angle X-Ray Scattering N2 - In the last decade the utilization of silver nanoparticles in consumer related products is enhanced. Therefore, many studies focus on investigations regarding their toxicological potential. This includes investigations concerning uptake, distribution and excretion of the particles. So far, little attention was paid to changes of physical and chemical properties in the human body. During processes like digestion, the question arises whether they can pass this barrier in a nanoscale form. In this study we analytically monitored the changes in the size distribution of colloidal silver during an artificial digestion process with the help of small angle x-ray scattering (SAXS). Therefore, we synthesized polyacrylic acid stabilized ultra-small silver nanoparticles with a radius of 3 nm and a size distribution width of 18%. The artificial digestion process mimics the gastro-intestinal passage and simulates the oral, gastric and small intestinal conditions. Additionally, food components like oil, starch, glucose and skimmed milk powder are used to provide a preferably realistic environment. In absence of any food components the low pH initiates aggregation of the particles in the stomach. However, the particles unexpectedly stabilize in a defined cluster form with a mean radius of 12 nm. By the use of the food components oil and starch we observed that the particles are dispersed again. Now we found a bimodal size distribution of primary particles and aggregates. In contrast to that, with skimmed milk powder only a slight aggregation occurs in the stomach. In the gastric tract the particle distribution is stabilized at a mean volume weighted radius of 5 nm. Hence, skimmed milk powder acts as a colloidal stabilizer. For comparison we also used silver nitrate as a control substance. Surprisingly, we observed a formation of nanoparticles already in the saliva. During the digestion process the distribution narrows and finally in the intestine it shows a stable distribution with a mean volume weighted radius of 3 nm and a small fraction of aggregates. These results indicate that the silver nanoparticles can pass the digestion process in a nanoscale form but undergo a transformation in the size distribution. However, even from pure silver nitrate nanoparticle formation can be observed. This sketches a complex mechanism in which not only food components but also silver ions cause changes in nanoparticle size and aggregation. T2 - 6th International Colloids Conference CY - Berlin, Germany DA - 19.06.2016 KW - SAXS KW - Artificial digestion KW - Silver nanoparticles PY - 2016 AN - OPUS4-36888 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Avishai, N. A1 - Avishai, A. A1 - Hodoroaba, Vasile-Dan T1 - What is the effective geometrical collection efficiency of your XEDS detector? Routine procedure applied in a SEM laboratory N2 - In this contribution, two large-area EDS detectors were tested according to the procedure proposed by Procop et al. (2015). In a first step, the optimal working distance (WD) in the two different SEM chambers was determined by moving the sample stage in the Z direction and monitoring the count rates at a magnification of 10,000 and a field of view of 25.6 µm. The WD at which the highest intensity was measured was selected as the optimal position, corresponding to the crossover between the EDS detector optical axis and electron beam optical axis. Next the Cu Kα peak was measured at different relative EDS positions while it was partially removed from the fully inserted position. The spectrum at each location was collected for 10 sec using the highest pulse rate and intermediate current to minimize pile up effects. The ‘inverse squared normalized intensities vs. relative EDS position’ used to extract the true detector – specimen distance shows a non-linear relationship even at the minimal relative positions, which indicates shadowing due to obstruction or use of an unsuitable and/or off-centered collimator. The normalized count rates measured as a function of the EDS distances, results in a too low GCE (too low true solid angles) for both tested detectors. The source of losses of signal was shadowing caused by collimators. T2 - Microscopy & Microanalysis 2016 Meeting CY - Columbus, Ohio, USA DA - 24.07.2016 KW - EDS KW - Solid angle KW - Net effective sensor area KW - X-ray yields PY - 2016 AN - OPUS4-36982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altenburg, Simon T1 - Thickness determination of semitransparent isolated solids using the flash method and an analytical model N2 - As groundwork for thickness determination of polymeric surface protection systems for concrete, we present a method for measuring the thickness of isolated semitransparent solids using pulse thermography both in transmission and reflection configuration. An advanced analytical model by Salazar et al. capturing semitransparency is applied. After calibration with samples of well-known thickness, the unknown thickness of samples of the same material can be obtained by fitting. T2 - QIRT 2016 CY - Gdansk, Poland DA - 04.07.2016 KW - Thermography KW - Analytical model KW - Surface protection KW - Concrete KW - Semitransparency KW - Thickness KW - Flash thermography PY - 2016 AN - OPUS4-36983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zeegers, G. P. T1 - Evidence for laser-induced redox reactions between added trifluoroacetate salts and substrate material during polystyrene/DCTB MALDI N2 - Polymers, such as polystyrene, have been successfully analyzed with matrix-assisted laser desorption/ionization (MALDI) through the addition of e.g. copper or silver salts. This method is often used to establish the polydispersity index of polymer blends. However, the mechanism of cation addition and the possible interactions between the added salts and the chosen target material are still points of interest. Therefore, the addition of several trifluoroacetate salts to a mixture of polystyrene and matrix on a range of different target plate materials was systematically investigated, revealing several new interesting aspects of MALDI. Polystyrene (Mw 1,920 Da) was mixed with a range of trifluoroacetate salts (Li, Na, K, Cs, Ba, Cr, Pd, Cu, Ag, Zn, Al and In, as well as trifluoroacetic acid) and analyzed with MALDI using 2 -[2E-3-4-tert-butylphenyl)- 2- methylprop-2-enylidene]ma lononitrile DCTB) as matrix on different target plate materials (chrome, copper, silver, gold, Ti90/Al6/V4, Inconel® 625, Zinc and stain less steel) to evaluate the occurrence of redox-reactions. Polystyrene/salt/matrix solutions were deposited through pneumatic-assisted spraying on microscope slide -shaped target plate insets of varying material, which, secured with copper tape, fitted a milled out structure from the original target plate. Spectra, obtained on a Bruker Autoflex I MALDI-Time -of-Flight mass spectrometer, were processed with MATLAB to obtain polystyrene-and matrix -adduct ion signal intensities for direct comparison between chosen conditions. The resulting spectra shed light on the MALDI adduct formation process and the cation-polystyrene interactions. It was found that the following cation -polystyrene adducts were formed on stainless steel: Al, Li, Na, Cu and Ag, where the yield was found to depend on the sample layer thickness and possibly the cation’s ability to form a complex with either one or two of polystyrene’s phenyl rings, based on the ligand-field and the valence bond theory. With the exception of Al, these salts also formed adducts and in case of Cu and Ag also sandwich adducts with DCTB. Some alkali salts (e.g. potassium) formed clusters rather than interacting with polystyrene or DCTB, which can be explained with the HSAB theory. Application of TFA salts on a copper surface led to copper cation formation, resulting in DCTB and polystyrene copper-adduct formation. The same effect occurred for silver substrate. In the absence of copper or silver salts, it is therefore still possible to form their respective adducts by choosing the proper alternative salt (e.g. Li, Cs, Ba, Cr) in combination with either a silver or a copper substrate surface. Incubation tests with copper beads in various salt solutions, before matrix and polystyrene addition, support that copper ions are not generated during the deposition process before the MALDI experiment is carried out, except when trifluoroacetic acid, indium and aluminium trifluoroacetate are used. For all other salts used on a copper plate, it can therefore be concluded that these copper cation forming redox-reactions are enabled by the input of laser photon energy. Furthermore, it was discovered that copper beads can successfully sequester polystyrene from the sample mixture, indicating the strong bonding of polystyrene to the copper surface. These findings support that the redox-reactions occur (almost) instantaneously with laser pulse impact at the sample-coated substrate surface. T2 - Jahrestagung der DGMS 2016 CY - Hamburg, Germany DA - 28.02.2016 KW - MALDI KW - Redox-reactions KW - Substrate KW - Cations PY - 2016 AN - OPUS4-36937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkelmann, Aimo A1 - Nolze, Gert A1 - Voss, M. A1 - Salvat-Pujol, F. A1 - Werner, W. S. M. T1 - Physics-based simulation models for EBSD: advances and challenges N2 - EBSD has evolved into an effective tool for microstructure investigations in the scanning electron microscope. The purpose of this contribution is to give an overview of various simulation approaches for EBSD Kikuchi patterns and to discuss some of the underlying physical mechanisms. T2 - EMAS 2015 - 14th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS CY - Portoroz, Slovenia DA - 03.05.2015 KW - Electron backscatter diffraction KW - Simulation KW - Dynamical theory KW - Kinematic theory PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-377469 DO - https://doi.org/10.1088/1757-899X/109/1/012018 VL - 109 SP - 012018-1 EP - 012018-13 AN - OPUS4-37746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grunwald, Daniel T1 - Determining the influence of preparation and measurement conditions on bonding strength using CAT-Technology N2 - The paper addresses the ‘Determining the influence of preparation and measurement conditions on bonding strength using CAT-Technology’ and the follow points are discussed in more detail: Motivation, CAT – Technology, Influence of bonding area on bonding strength, Influence of storing & measurement temperatures and Influence of substrate thickness and coating support. T2 - LUM, International Workshop Dispersion Analysis & Materials Testing 2016 CY - Berlin, Germany DA - 26.10.2016 KW - Tensile strength KW - Centrifuge technology KW - Bonding KW - Composite KW - Substrate PY - 2016 AN - OPUS4-37856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - Introduction to PowderCell N2 - The presentation give a short introduction into the free-available software PowderCell (BAM)for the simulation of X-ray diffraction patterns of polycrystalline materials. T2 - PowderCell Users meeting CY - Joinville, Brazil DA - 19.10.2015 KW - X-ray diffraction KW - Simulation KW - Structure viewer KW - Subgroup relationships PY - 2015 AN - OPUS4-37791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - EBSD: more reliable and accurate N2 - The presentation discusses numerous new approaches in order to increase precision and accuracy of electrom backscatter diffraction measurements. T2 - 1st EBSD Workshop CY - Belo Horizonte, Brazil DA - 17.09.2015 KW - Orientation mapping KW - Electron backscatter diffraction KW - Lattice parameter determination KW - Orientation precision KW - Orientation noise PY - 2015 AN - OPUS4-37797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schallschmidt, Kristin A1 - Becker, Roland A1 - Jung, Christian A1 - Bremser, Wolfram A1 - Nehls, Irene A1 - Leschber, G. A1 - Frese, S. A1 - Walles, T. A1 - Neudecker, J. T1 - Comparison of volatile organic compounds from lung cancer patients and healthy controls—challenges and limitations of an observational study N2 - The design and operation of an observational study on the profiles of volatile organic compounds (VOC) in the breath of 37 lung cancer patients and 23 healthy controls of similar age is outlined. The necessity to quantify each VOC considered as potential disease marker on basis of individual calibration is elaborated and the quality control measures required to maintain reproducibility in breath sampling and subsequent instrumental trace VOC analysis using SPME-GC-MS over a study period of 14 months are described. 24 VOC were quantified on basis of their previously suggested potential as cancer markers. The breath concentration levels of aromatic compounds was expectedly increased in smokers while lung cancer patients displayed significantly increased levels of oxygenated VOC such as aldehydes, 2-butanone and 1-butanol. Though sets of selected oxygenated VOC displayed sensitivities and specificities between 80 and 90% using linear discriminant analysis with leave-one-out cross validation the effective selectivity of the breath VOC approach with regard to cancer detection is clearly limited. Results were discussed against the background of the literature on volatile cancer marker investigations and the prospects to link increased VOC levels in patients’ breath with approaches to employ sniffer dogs. Experiences from this study and the literature suggest that the current state of breath VOC based discrimination between cancer patients and healthy controls is hardly improvable. Observational studies tend to observe significant differences mostly in levels of certain oxygenated VOC but without resolution required for practical application. Any step towards practicable exploitation of VOC profile differences for illness detection would have to solve current restrictions set by the low and variable VOC concentrations. Further challenges are the technical complexity of studies involving breath sampling and possibly the limited capability of current analytical procedures to detect instable marker candidates. KW - Breath KW - Volatile organic compounds KW - Marker KW - Cancer KW - Gas chromatography KW - Solid phase microextraction KW - Volatilome PY - 2016 DO - https://doi.org/10.1088/1752-7155/10/4/046007 SN - 1752-7155 SN - 1752-7163 VL - 10 IS - 4 SP - Article 046007, 1 EP - 17 PB - IOP Publishing AN - OPUS4-37801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - High-pressure qNMR spectroscopy in condensed- and gas-phase towards determination of impurities and compositions of gas mixtures N2 - Recent technical developments of NMR instruments such as in acquisition electronics and probe design allow detection limits of components in liquid mixtures in the lower ppm range (approx.. 5–10 ppm amount of substance). The major advantage of quantitative NMR spectroscopy (qNMR) is that it is a direct ratio method of analysis without the need of calibration. This means that the signal for a specific NMR-active nucleus (e.g., a proton) in an analyte can be compared and quantified by reference to a different nucleus of a separate compound, comparable to a counting of spins in the active volume of the spectrometer. A special application of qNMR in technical mixtures is the observation in the gas phase, which is rarely applied compared to liquid and solid NMR studies. Because of the low density it results in a reduced sensitivity, which can be improved by applying pressure. Therefore a high-pressure NMR setup was developed based on a commercially available NMR tube made of zirconia. This is currently tested up to 20 MPa, but can be extended up to 100 MPa with regard to pressure rating of its components. This work shows results of gas-phase application on natural-gas like reference gas mixtures produced at BAM, as well as investigations on liquefied petroleum gas mixtures (LPG) with high accuracy provided in constant-pressure piston cylinders. T2 - 35th Meeting of the CCQM-Gas Analysis Working Group, Workshop "Cutting edge research for gas metrology" CY - Caparica, Portugal DA - 13.10.2016 KW - Quantitative NMR spectroscopy KW - Gas-phase NMR KW - Reference gas mixtures KW - Liquefied petroleum gas PY - 2016 AN - OPUS4-37803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Characterization of Materials: Uncertainty Budgets in Measurement and Testing N2 - The comprehensive knowledge of material properties as engineered and the material behavior in use is of huge importance for the functionality and reliability of processes and products. Hence, the accurate determination of material properties is a prerequisite for the applicability of a given material. Nowadays, macroscopic product features are originated by material properties on the microscopic and nanoscopic scale. This is a general challenge for uncertainty budgets in measurement and testing based on a conformity assesment. Testing labs accreditated according to DIN EN ISO/IEC 17025 have to meet these demands. This paper focuses on the measurement of physical quantities (measurand with value and unit) and on the testing of material properties (qualitative, semi-quantitative or quantitative characteristics) of solid state materials. For both measurement and testing, the expression of uncertainty according to GUM is essential. Regarding the object/sample one has to subdivide in surface and bulk features, from the measurement/testing point of view destructive vs. nondestructive procedures have to be distinguished. Moreover, direct mesurement/testing and model-based determination of quantities/properties of interest require different approaches regarding the expression of uncertainty. For surface quantities and properties as discussed here, further considerations have to be made with respect to localized (lateral extension, native or artificial) or stratified (homogeneity and isotropy) material features vs. mapping (integration area) and imaging (lateral resolution and field of analysis) specifications of the measurement/testing procedure. The concept of uncertainty budgets and the expression of uncertainty is introduced and discussed in more detail for the nondestructive model-based determination of thickness by spectroscopic ellipsometry (SE), the destructive determination of adhesion by means of centrifugal adhesion testing (CAT). It is shown that the expression of uncertainty for these examples and real materials requires different approaches resulting in either quantitity values with unit or qualitative/quantititative attributes with calculated/estimated uncertainties in agreement with GUM. T2 - The 4th International Conference on Competitive Materials and Technology Processes, ic-cmtp4, 2016 CY - Miskolc-Lillafüred, Hungary DA - 03.10.2016 KW - Measurement and testing KW - Uncertainty budgets KW - Expression of uncertainty PY - 2016 AN - OPUS4-37841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. I. A1 - Petrushin, N. V. A1 - Link, T. A1 - Nolze, Gert A1 - Loshchinin, Yu. V. A1 - Gerstein, G. T1 - Thermal stability of the structure of a heat-resistant cobalt alloy hardened with intermetallic γ'-phase precipitates N2 - The thermal stability of the microstructure of a heat-resistant cobalt alloy, which consists of a γ solid solution strengthened with γ'-phase precipitates, has been studied. The temperature behavior of the dissolution of the hardening γ' phase and the kinetics of its coarsening at 700 and 800°C have been determined. It is found that, during prolonged annealing at 800°C, the γ' → β phase transformation occurs. KW - Superalloy KW - Microstructure KW - Hardening KW - Electron backscatter diffraction KW - TEM PY - 2016 DO - https://doi.org/10.1134/S0036029516040078 SN - 0036-0295 VL - 2016 IS - 4 SP - 286 EP - 291 PB - Pleiades Publishing AN - OPUS4-37768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - Microstructure characterization of the Treysa meteorite N2 - Microstructure descripton of heat-affected zone, fusion crust and main metal of the Treysa iron using scanning electron microscopy, EBSD and EDS. T2 - 8. Deutsches Meteoriten Kolloquium, CY - Zella Willingshausen, Germany DA - 02.04.2016 KW - Electron backscatter diffraction KW - EDX KW - Light microscopy KW - Microstructure KW - Oxidation PY - 2016 DO - https://doi.org/10.13140/RG.2.1.3387.8161 AN - OPUS4-37769 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert A1 - Saliwan Neumann, Romeo A1 - Buchheim, Michaela T1 - Microstructure investigations of iron meteorites by EBSD and EDS analyses N2 - Meteorites are a unique and inspiring material for microstructural studies because if their very specific genesis. Iron meteorites have been formed under unimaginable cooling rates of a few ten Kelvins per million years so that the observable transformation of the formerly huge Fe-Ni single crystals of taenite occurred under nearly-equilibrium conditions. Octahedrites (meteorites having a Ni content between 6...15%) are characterized by ribbons of the low-temperature Fe-Ni phase kamacite separated by rims of residual taenite. This very specific feature is known as Widmanstaetten structure and has been investigated by synchrotron radiation in order to cover a higher volume fraction for a statistically relevant description of orientation relationships. However, plessite – a microstructure mainly consisting of the same phases – reflects the orientation relationship between kamacite and taenite as well. For their characterization, a scanning electron microscope is very suitable in order to investigate crystal orientations or identify phases. Despite the apparently ideal formation circumstances of iron meteorites, Ni concentration profiles prove non-equilibrium conditions. Combined EDS (energy dispersive spectroscopy) and EBSD (electron backscatter diffraction) measurements at a selected plessitic region of the Cape York iron shows that a correlation exists between Ni-concentration and the locally detected orientation relationship. T2 - 15th European Microscopy Congress CY - Manchester, UK DA - 16.09.2012 KW - Phase identification KW - Corrosion KW - Chloride KW - Dermbach PY - 2012 SP - 90 AN - OPUS4-37775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert A1 - Winkelmann, Aimo T1 - The challenge of band detection N2 - The presentation demonstrates different traps which are related to the detection of Kikuchi bands in EBSD patterns. T2 - EBSD 2015 CY - Glasgow, UK DA - 30.03.2015 KW - Electron backscatter diffraction KW - Image processing KW - Pseudo symmerty KW - Crystal lattice KW - Pyrite KW - Pattern matching KW - Misindexing PY - 2015 AN - OPUS4-37805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Höhne, Patrick T1 - Optimization of ceramic slurries for spray drying yielding non-hollow granules N2 - Economic industrial spray drying of ceramic slurries aims for as high as possible solids content. Investigated slurries of up to 80 wt% solids content were analyzed regarding stability while staying processable for granule production via spray drying. Preliminary stability examinations were carried out on the one hand via zeta potential measurements and on the other hand by optical centrifuge analysis for determination of suitable additive type, quantity and composition while even allowing the detection of potential side effects. The processability of the slurry for spraying has primarily been quantified by viscosity measurements. Early spray dried granules turned out to have internal voids and/or hard shells leading to defective sinter bodies and low density. Focusing on the root of these voids, the “hollow hard granules”, a controlled destabilization and flocculation was initiated by weakening electrostatic repulsion and approaching the isoelectric point. Destabilization, quantifiable by optical centrifugation, leaded to a change in speed of clarification as well as packing density, influencing movement speed of the phase boundary and the final height of the sediment, respectively. For sufficient destabilization, the solids content needed to be reduced in order to keep the viscosity suitable for the following spray drying procedure. The versatile controlled destabilization of the ceramic slurry finally leaded to a significantly reduced fraction of hollow granules featuring a sinter body of higher density with smaller pores and a narrower pore size distribution, additionally this destabilization approach has shown to be transferrable with excellent results to zirconia and even ZTA (zirconia toughened alumina) composite materials. T2 - International Workshop Dispersion Analysis & Materials Testing 2016 CY - Berlin, Germany DA - 26.09.2016 KW - ceramics KW - slurry KW - granulation KW - spray drying KW - microstructure PY - 2016 AN - OPUS4-37778 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vos, M. A1 - Winkelmann, Aimo A1 - Nolze, Gert T1 - Element-specific Kikuchi patterns of Rutile N2 - The kinetic energy of keV electrons backscattered from a rutile (TiO2) surface depends measurably on the mass of the scattering atom. This makes it possible to determine separately the angular distribution of electrons backscattered elastically from either Ti or O. Diffraction effects of these backscattered electrons inside the rutile crystal lead to the formation of Kikuchi patterns. The element-resolved Kikuchi patterns of Ti and O differ characteristically, but each can be described fairly well in terms of the dynamical theory of diffraction. Qualitatively, much of the differences can be understood by considering the relative arrangement of the Ti and O atoms with respect to planes defined by the crystal lattice. KW - Electron Rutherford backscattering KW - TiO2 KW - Kikuchi pattern KW - EBSD pattern KW - Simulation PY - 2015 DO - https://doi.org/10.1016/j.ultramic.2015.04.018 SN - 0304-3991 VL - 156 SP - 50 EP - 58 AN - OPUS4-37787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - SEM-TKD: Signal formation, practical challenges and related applications N2 - TKD and EBSD will be compared and benefits as well as limitations of TKD will be discussed. T2 - XIV Brazilian MRS Meeting CY - Rio de Janeiro, Brazil DA - 27.09.2015 KW - TKD KW - EBSD KW - Kikuchi diffraction KW - Nanoanalytic KW - Orientation mapping PY - 2015 AN - OPUS4-37788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - Simulation of powder diffraction patterns N2 - The theory of powder diffraction simulation is explained at the example of PowderCell, a free-available software of BAM. T2 - PowderCell Users meeting CY - Joinville, Brazil DA - 21.09.2015 KW - Powder diffraction KW - X-ray diffraction KW - Phase analysis KW - Simulation PY - 2015 AN - OPUS4-37789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weller, Michael G. T1 - Trennschärfe: Robustheit, Selektivität und Spezifität N2 - Zusammenfassung Selektivität 1. Widersprüchliche Definitionen in unterschiedlichen Bereichen 2. Analytische Definition (pragmatisch): Selektivität ist die Fähigkeit einer Methode zur Unterscheidung aller interessierender Stoffe in der Probe. 3. Tests: Blindwerte, Leerwerte, Blank Values; Peakform 4. Wichtige Einflussgrößen: Trennleistung, Auflösung, Peakkapazität, Trennkapazität 5. Verbesserung durch: Kopplungsverfahren, Änderung der chromatographischen „Selektivität“, Orthogonalität 6. Wichtig ist auch die Komplexität der Probe(n) 7. Selektivität in der Immunchemie/Biochemie wird oft als Kreuzreaktion gemessen. Zusammenfassung Robustheit 1. Sehr individuelle Kriterien – sinnvolle Auswahl notwendig! 2. Wichtige Testphasen: a)Änderung von Methodenparametern b)Stabilität über die Zeit c)Überführung in die Routine 3. Ringversuche bzw. Laborvergleichsmessungen 4. Wichtigstes Vergleichskriterium: Relative Verfahrensstandardabweichung 5. Extratipp: Maximale Diversität der Testproben sicherstellen (besonders bezüglich der Matrix) T2 - BAM Sommerschule 2016 "Qualitätssicherung in der analytischen Chemie" CY - Berlin, Germany DA - 04.07.2016 KW - Selektivität KW - Spezifität KW - Robustheit KW - Sommerschule KW - Blindwert KW - Peakkapazität KW - Kreuzreaktion PY - 2016 AN - OPUS4-37760 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. I. A1 - Link, T. A1 - Nolze, Gert A1 - Svetlov, I. L. A1 - Bokshtein, B. S. A1 - Rodin, A. O. A1 - Saliwan Neumann, Romeo A1 - Oder, Gabriele T1 - Diffusion processes in multicomponent nickel-base superalloy-nickel system N2 - Optical and scanning electron microscopy, as well as electron microprobe analysis and electron backscatter diffraction, have been used to study diffusion processes that occur in a diffusion pair that consistsof a single-crystal CMSX-10 nickel-base superalloy and polycrystalline nickel, at temperatures of 1050–1250°C. It has been found that, in this system, the distributions of γ-stabilizing elements (Cr, Co, W, and Re) are described by the Boltzmann solution for diffusion between two semiinfinite plates of a binary alloy. The processing of these distributions has shown that the diffusion coefficients of Cr, Co, W, and Re in the multicomponent system are close to those in binary alloys of these elements with Ni. The diffusion redistribution of the elements leads to the dissolution of the γ′ phase in the nickel-base superalloy, growth of nickel grains toward the superalloy constituent of the diffusion pair, and the formation of porosity on both sides of the migrating interface, which is determined from a crystal misorientation of the alloy single crystal and nickel grains. KW - Ni-base superalloy KW - Interface KW - Diffusion KW - Phase transformation KW - Porosity PY - 2014 SN - 0031-918X VL - 115 IS - 1 SP - 21 EP - 29 AN - OPUS4-37980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Payton, E. T1 - Messengers from Space: A Scanning Electron Microscopy Investigation N2 - The macro- and microstructure of iron meteorites provide valuable insights into both the inner structure of our planet and the history of our solar system. High speed collision events in the asteroid belt send the meteorites careening toward Earth. The collisions produce unique deformation microstructures. With cooling rates on the scale of a few degrees per million years, iron meteorites can consist of crystal sizes on the order of meters prior to the collision events. These extremely slow cooling rates result in phase transformations occurring at conditions near thermodynamic equilibrium. Preserving meteorite fragments is important for future studies of phase transformations, material behavior at high strain rates, and the origin of the universe. KW - Meteorite KW - Phase identification KW - Hibbingite KW - Orientation relationship KW - Electron backscatter diffraction KW - Energy dispersive x-ray spectroscopy KW - EDX PY - 2013 IS - 3 SP - 2 EP - 4 PB - GIT Verlag AN - OPUS4-37981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert T1 - Irrational orientation relationship derived from rational orientation relationships using EBSD data N2 - The determination of the orientation relationship (OR) between α-Fe matrix (bcc) and γ-Fe precipitates (fcc) is discussed using orientation data collected by electron backscatter diffraction (EBSD). The comparatively low accuracy of EBSD is compensated by the high number of measurements what allows a general statement regarding to the mean OR existing in a sample. The representation and discussion is realized on a part of the Bain zone in a {001} pole figure. A discussion of some selected rational OR which are commonly used for the phase boundary characterization between α and γ shows that the pole figures describing a transformation from γ → α are different to those for α → γ. A technique is proposed based on at least three misorientation angles between the experimental OR to the rational OR's as reference. For the misorientation angle distribution a refinement is applied to extract the mean values. They are used to detect the mean OR, what is also possible for only a few or even a single precipitate if the number of measurements describing the phase boundary is sufficiently high. KW - Orientation mapping KW - Orientation relationship KW - Electron backscatter diffraction KW - Kurdjumov-Sachs KW - Nishiyama-Wassermann KW - Misorientation PY - 2008 DO - https://doi.org/10.1002/crat.200711058 VL - 43 IS - 1 SP - 61 EP - 73 PB - WILEY-VCH AN - OPUS4-38009 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik T1 - The VCSEL-Array - a Novel High-Power Light Source for (Photo) Thermal Imaging N2 - Within the field of optically excited thermography, full-field thermal imaging is used to characterize materials, to determine thicknesses of layers or to find inhomogeneities such as voids or cracks. Classical light sources, such as flash lamps (impulse heating) or halogen lamps (modulated heating), are hereby specifically used. This has led to the different testing methods lock-in and flash thermography. The VCSEL array promises to merge these excitation methods. Vertical Cavity Surface Emitting Lasers (VCSELs) are laser diodes emitting light perpendicular to their surface. Due to the vertical structure they can be arranged in large arrays of many thousand individual lasers and still be controlled like ordinary diode lasers. Recently a high-power albeit very compact version of such a VCSEL-array became available which offers both the fast timing behavior of lasers and large illumination areas. Moreover, it allows a spatial and temporal control of the heating because individual parts of the VCSEL-array can be controlled arbitrarily in frequency, amplitude, and phase. Although the VCSEL-array has a high potential for a new range of applications, it is too early to proclaim them. As one out of very few labs, we already adopted to this new VCSEL technology and show a thorough characterization and first results obtained with a 2.4 kW device. Specifically, we will discuss - the linearity between control voltage and optical output - the minimal pulse duration - the maximal applicable modulation frequency - optical projection and its influence on the optical output - spatial control of the illumination and thermal wave shaping Our results indicate that a VCSEL-array can be used for conventional impulse (aka flash) thermography whereas pulse duration and power are instantaneously accessible compared to flash lamp excitation. In case of lock-in thermography, we can apply frequencies in excess of 200 Hz without a loss in amplitude or an after glowing of the source, making it attractive for photo thermal applications. Consequently, this means that the VCSEL-array is able to merge the two main excitation methods lock-in and impulse thermography. T2 - 57th Course on Photoacoustic & Photothermal Phenomena CY - Erice, Italy DA - 19.10.2016 KW - VCSEL KW - Thermal Wave KW - Active Thermography PY - 2016 AN - OPUS4-37952 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik T1 - Spatial and temporal control of thermal waves using spatial light modulators N2 - Active thermography has been developed into a well-established non-destructive testing method and is used to detect cracks, voids, or material properties. The spatial-temporal structure of the external heating: spatially: planar (e.g., halogen lamp) or local (e.g., focused laser), and temporally: pulsed (e.g., flash lamp) or periodical (e.g., halogen lamp), has led to different testing modalities, as for instance flash and lock-in thermography. In this work, we combine a high-power laser with a spatial light modulator (SLM) allowing us to merge all degrees of freedom into a spatially and temporally controlled heat source. This approach allows us to launch a set of individually controlled and fully coherent high-energy thermal waves into the sample volume. As one possible application, we demonstrate the interference of two phase shifted thermal wave patterns in order to detect the position and depth of hidden defects, which is still a challenging task in thermographic and photothermal techniques. The patterns are positioned with a certain distance and a phase shift of pi to each other, creating an amplitude depletion zone that is centered between them. Now, when a defect is brought into the depletion zone, the destructive interference is disturbed and the defect can be recognized. This approach means that we intentionally exploit the vertical and lateral propagation directions of the thermal waves. In a more general view, controlling simultaneously control of phase and amplitude of a set of thermal waves enables us to have a defined propagation of the thermal wave field within the sample, which means that thermal waves can be controlled almost like acoustical or optical waves. However, in contrast to optical or acoustical waves, thermal waves are highly damped due to the diffusive character of the thermal heat flow and therefore limited in penetration depth in relation to the achievable spatial resolution. Nevertheless, the coherence length of thermal waves can be chosen in the mm-range for modulation frequencies below 10 Hz which is perfectly met by present SLM technology. Eventually, this offers the opportunity to transfer known technologies from wave shaping techniques to thermography methods and to exploit the possibilities of coherent thermal wave shaping. T2 - 57th Course on Photoacoustic & Photothermal Phenomena CY - Erice, Italy DA - 19.10.2016 KW - Infrared thermography KW - Thermal Wave KW - DMD PY - 2016 AN - OPUS4-37954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Plasma Germany, Fachausschuss Normung, Herbstsitzung 2016 N2 - Der Stand der Normung im Bereich der Oberflächentechnik wird zusammengefasst. Aktuelle Normungsvorhaben zur chemischen Oberflächenanalyse, Rastersondenmikroskopie, Nanotechnologie, Oberflächenmesstechnik im Mikro- und Nanobereich, für Anwendungen von Kohlenstoffschichten sowie von Mess- und Prüfverfahren für metallische und anorganische Überzüge werden vorgestellt. Ein Ringversuch zur Klassifizierung von Kohlenstoffschichten mittels Ellipsometrie wird diskutiert. Abschließend wird das DIN-Terminologie Portal erläutert. T2 - Lenkungsausschuss von Plasma Germany, Fachausschuss Normung, Herbstsitzung 2016 CY - Stuttgart, Germany DA - 27.10.2016 KW - Stand der Normung KW - Oberflächentechnik KW - Schichttechnik PY - 2016 AN - OPUS4-38068 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Imrie, F. T1 - Biocompatibility of DC magnetron-sputtered TiO2 N2 - SETNanoMetro, a European Seventh Framework project, seeks to develop standard synthetic routes and metrological characterisation methods for the development and production of TiO₂ nanoparticles and nano-sized coatings with highly-defined, homogeneous and reproducible characteristics, including bulk structure, size, shape and surface structure. These materials are being tested for their potential in selected technological applications, including as coatings on bone-substituting prostheses. The objective of this study was to assess how variations in morphology and chemistry of nano-sized TiO₂ coatings affect their biocompatibility in vitro. T2 - Bioceramics 28 CY - Charlotte, NC, USA DA - 18.10.2016 KW - TiO2 KW - Coating KW - Biocompatibility PY - 2016 AN - OPUS4-38077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sitzman, S. D. A1 - Nolze, Gert A1 - Nowell, M. M. T1 - EBSD Pattern Quality and its Use in Evaluating Sample Surface Condition N2 - Modern EBSD systems perform diffraction pattern “quality” (PQ) calculations, essentially measurements of the contrast of the brighter bands in the pattern above background, for every pattern analyzed. Since the calculations are independent of EBSD indexing, data are generated from all points on the analyzed sample surface, regardless of indexability or the state of the material beneath. EBSD maps generated from PQ data are like microstructurally sensitive SEM images, collected at EBSD speeds and grid resolutions, with contrast arising from phase density, crystal structure, crystallographic orientation, grain boundary location, near-surface plastic strain, coating density/thickness, and to some extent topography. Grain boundaries and other aspects of sample microstructure are readily revealed, so the PQ map is a very useful characterization tool in its own right, and serves as a reference for EBSD maps generated from indexing-derived data, such as orientation, grain boundary character, phase distribution and strain maps. KW - Electron backscatter diffraction KW - Sample preparation KW - Pattern quality PY - 2010 DO - https://doi.org/10.1017/S143192761005467X VL - 16 IS - Suppl. 2 SP - 698 EP - 699 PB - Microscopy Society of America AN - OPUS4-37997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Winkelmann, Aimo T1 - Progress in dynamic EBSD pattern simulation N2 - EBSD is nowadays a common technique for the characterization of crystalline microstructures in scanning electron microscopy. The diffraction patterns are often interpreted by superimposing individual Kikuchi bands which are geometrically described by band edges derived from Braggs law. For the typically very simple crystal structures of technically applied materials, such a simplification of the Kikuchi pattern interpretation works sufficiently well, especially for orientation determinations as a main application of EBSD. The more complex crystal structures, however, are a challenge for EBSD indexing routines which in such cases often fail unpredictably. The use of only the intensities of single reflectors for a description of the Kikuchi band intensity and as a cut-off criterion for a pre-selection of the strongest bands are not satisfactory. Often the result will match too many phases, or there are certain deviations in the intensity prediction which must be adapted manually. This is already problematic if one is absolutely sure that the patterns are originating from the expected phase and it becomes a very questionable procedure for an unknown phase. KW - Electron backscatter diffraction KW - Dynamical simulation KW - Geometrical model KW - Kinematic approach KW - Intensity PY - 2010 DO - https://doi.org/10.1017/S1431927610063324 VL - 16 IS - Suppl. 2 SP - 62 EP - 63 PB - Microscopy Society of America AN - OPUS4-38000 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Salge, T. A1 - Nolze, Gert T1 - Innovations in EDS and EBSD Microanalysis: Hyperspectral Imaging for Planetological Applications Using Silicon Drift Detectors (SDD) and EBSD N2 - Within the last decade, silicon drift detectors (SDD) systems have become more and more popular in the field of energy-dispersive spectroscopy (EDS). The main characteristic of the SDDs is their extremely high pulse load capacity of up to 750,000 counts per second at good or reasonable energy resolution (<123eV Mn-Kα, <46eV C-Kα at 100.000 cps). These properties in conjunction with electron backscatter diffraction (EBSD) techniques and modern data processing make a range of innovative analysis options possible, not only high speed mapping but also hyperspectral imaging techniques. T2 - 72nd Annual Meeting of the Meteoritical Society CY - Nancy, France DA - 13.07.2009 KW - Electron backscatter diffraction KW - Energy dispersive x-ray spectroscopy KW - Method combination PY - 2009 VL - Suppl. SP - 5270 AN - OPUS4-38002 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abou-Ras, D. A1 - Gibmeier, J. A1 - Nolze, Gert A1 - Gholinia, A. A1 - Konijnenberg, P. T1 - On the capability of revealing the pseudosymmetry of the chalcopyrite-type crystal structure N2 - The tetragonal crystal- structure type of chalcopyrites (chemical formula AIBIIICVI2) is a superstructure of sphalerite type. The c/a ratio differs generally from the ideal value 2, i.e., the crystal structure is pseudocubically distorted. For CuInSe2 and CuGaSe2 thin films, simulations demonstrate that it is theoretically possible to reveal the tetragonality in electron backscatter-diffraction (EBSD) patterns for CuGaSe2, whereas it may not be possible for CuInSe2. EBSD experiments on CuGaSe2 thin films using the ”Advanced Fit” band-detection method show that it is possible to extract accurate misorientation-angle distributions from the CuGaSe2 thin film. Pole figures revealing the texture of the CuGaSe2 thin film are shown, which agree well with X-ray texture measurements from the same layer. KW - Pseudosymmetry KW - Chalcopyrite KW - Electron backscatter diffraction KW - Pattern simulation KW - Pattern matching KW - Sphalerite PY - 2008 DO - https://doi.org/10.1002/crat.200711082 VL - 43 IS - 3 SP - 234 EP - 239 PB - WILEY-VCH AN - OPUS4-38003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lexow, Jürgen T1 - Materials Properties - Acquisition and Treatment of Data at BAM N2 - Following to a brief introduction of BAM the procedures are explained how to prepare reference materials in analytical chemistry. Examples are given for collecting and presenting data in welding, thermomechanical properties and tribology. The use of data for modelling safety in technology and chemistry is demonstrated. Finally there is in outlook on the World Materials Research Institut Forum (WMRIF) and recommendations for action. T2 - NCSRD-Workshop CY - Daejon, South Korea DA - 28.10.2008 KW - Materials Data KW - Werkstoffdaten KW - Referenzmaterial KW - Fügetechnik KW - Modellierung KW - Werkstoffmechanik KW - Korea KW - National Center for Standards and Reference Data (NCSRD) KW - Tribologie KW - Industrielle Sicherheit KW - WMRIF PY - 2008 AN - OPUS4-38022 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wendt, U. A1 - Nolze, Gert T1 - Correlation between Crystal Orientation, Channeling Contrast and Topography during FIB Milling of Cu Studied by FIB, EBSD, SEM, and AFM N2 - We have studied the anisotropic milling of Cu with respect to the milling rate and the milling topography, as well. The background is twofold: i) anisotropic milling has to be taken into account during the preparation of TEM specimens and in the manufacturing of micro parts from crystalline materials, and ii) the orientation depending milling behaviour can be used to generate topographies with specific properties with respect to, for example, adsorption, wear, and corrosion. KW - FIB KW - AFM KW - Crystal orientation KW - SEM PY - 2007 VL - 44 IS - 5 SP - 236 EP - 238 PB - Carl Hanser Verlag AN - OPUS4-38026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wendt, U. A1 - Nolze, Gert A1 - Heyse, H. T1 - Effect of crystal orientation on imaging contrast and sputter results during focused ion beam milling of Cu studied by FIB, EBSD, SEM, and AFM N2 - During focused ion beam microscopy (FIB) of crystalline materials imaging contrast and milling result are effected by orientation of the crystals with respect to the incident ion beam. This is due to the possibility of ion channeling along preferred crystal directions which effects the depth at which interaction between ions and specimen atoms takes place. As a result of channeling emission of ion induced secondary electrons (iiSE) and secondary ions (SI) as well as the sputter rate decreases. Theoretical channeling orientations and critical angles can be calculated. These effects have been studied quantitatively for polycrystalline recrystallized Cu as a typical model case. KW - Electron backscatter diffraction KW - FIB KW - AFM KW - Crystal orientation PY - 2006 DO - https://doi.org/10.1017/S1431927606061812 SN - 1431-9276 SN - 1435-8115 VL - 12 IS - Suppl. 2 SP - 1302 EP - 1303 AN - OPUS4-38027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epishin, A. I. A1 - Nolze, Gert T1 - Investigation of the competitive grain growth during solidification of single crystals of nickel-based superalloys N2 - The competitive growth of columnar grains in a single-grain selector, which is used for directional solidification of single-crystal blades from nickel-based superalloys, has been investigated by electron backscattered diffraction and local X-ray diffraction analysis. It has been found that the competitive grain growth in a starter block is determined by the crystallographic factor: rapidly growing grains with the axial orientation close to the [001] direction dominate in this part of the casting. For the competitive grain growth in a helicoidal separator, the geometric factor (the position of a grain at the input of the separator) is also important. The results obtained suggest that an appropriate geometry of the single-grain selector was chosen. In addition, the distribution of the orientations of columnar grains obtained by electron backscattered diffraction, can be used for approximate estimation of the yield of suitable (i.e., with the deviation of the axial orientation from the [001] direction within a specified tolerance) single-crystal blades. KW - Electron backscatter diffraction KW - Single crystal KW - Growth competition KW - Nickel alloy PY - 2006 DO - https://doi.org/10.1134/S1063774506040298 SN - 1063-7745 SN - 1562-689X VL - 51 IS - 4 SP - 710 EP - 714 AN - OPUS4-38028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Glowacka, A. A1 - Nolze, Gert A1 - Swiatnicki, W. A. T1 - EBSD study of corrosion fatigue of austenitic-ferritic steel N2 - Fatigue crack propagation investigations have been performed in austenitic-ferritic duplex stainless steel H22N5M3 in air and during hydrogen charging, using various frequencies of loading. Strong differences of crack propagation velocity depending on the test conditions were noticed. Lower frequency with applied hydrogen charging led to the huge increase of crack propagation velocity compared to the tests performed in air. To understand such a behaviour in each case and characterize crack mode, the samples were observed using electron back-scattered diffraction (EBSD). It was shown that in air, the fatigue crack propagation involved plastic deformation and the resulting cracks had ductile character. The presence of hydrogen led to more brittle mode of cracking. This effect was also connected with frequency of loading: lower frequency, which assured longer time for hydrogen-crack tip interaction, resulted in the highest crack propagation velocity and the brittle cracking mode with lower amount of plastic deformation. The performed observations indicated that the path of the crack went mostly transgranularly through both austenite and ferrite phases. Phase and grain boundaries were not the preferred paths for crack propagation. KW - Hydrogen KW - Embrittlement KW - Electron backscatter diffraction KW - Steel PY - 2006 SN - 1733-3490 SN - 0004-0770 SN - 0860-7052 VL - 51 IS - 1 SP - 7 EP - 10 AN - OPUS4-38029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraus, Werner A1 - Nolze, Gert T1 - PowderCell as teaching tool N2 - PowderCell represents a user friendly program which supports the solution of scientific problems as well as teaching and education. Especially for the last one the program offers a lot of information regarding the space-group type as well as crystal structure used. Therefore, on some universities the program is used successfully to make students familiar with x-ray crystallography. The quasi-simultaneous diffraction pattern simulation visualized the changes caused by the respective crystal structure. However, it is also possible to vary different diffraction parameters and investigate the resulting changes in the interference intensity or the reflection position. In principle, the aim of the program is the intuitive generation of structure models. Therefore, special tools have been implemented to move (rotate or shift) or transform the crystal structure. KW - Simulation KW - PowderCell KW - Crystal structure KW - XRD KW - Neutron KW - Programming PY - 1998 VL - 20 SP - 27 EP - 29 AN - OPUS4-38055 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rades, Steffi T1 - Analysis of functionalization of TiO2 nanoparticles and various substrates by means of SEM-EDX, AES and ToF-SIMS N2 - The physico-chemical characteristics of TiO2 coatings can greatly influence their final performance. In SETNanoMetro, different deposition procedures are being set for applying films of TiO2 NPs with defined and homogenous thickness on supports of interest for the applications studied in the project. The selected substrates are the following: (i) Silica glasses for photocatalytic measurements, (ii) Ti-alloys for orthopedic and/or dental prostheses, and for cell cultures, and (iii) Conductive glasses (e.g. Fluorine doped Tin Oxide, FTO) for dye-sensitized solar cells. From the different film deposition procedures studied within the project Self-assembly of TiO2 NPs in multiple layers was selected. For this, surface modification of the substrate and of TiO2 nanoparticles (NPs) with e.g. silane coupling agents is a prerequisite. First attempts to prepare the self-assembled coating on the functionalized glass substrates seem to indicate that the functionalized NPs adhere to the substrates, even if the final coatings were not homogenous and presented agglomerates. ToF-SIMS results support this outcome. In order to use the layer-by-layer deposition technique for the formation of TiO2 films by controlled self-assembly of the TiO2 NPs, the proper complementary moieties for the functionalization of the NPs were chosen. A first set of NPs has been produced by reaction with (3-aminopropyl)phosphonic acid (APPA) in order to functionalize the surface with free amino-groups. Then, the complementary NP set can be obtained from an aliquot of the first one, through the conversion of free surface amino-groups to aldehydes by reaction with glutaraldehyde. A proper approach for the functionalization of two types of TiO2, commercial P25 (Evonik) and SETNanoMetro-sample labelled UT001, with APPA was developed. A second set of NPs consisting of three types of TiO2 NPs, P25 and SETNanoMetro NPs (TiO2 NPs with high specific surface area > 150 m2/g and TiO2 NPs with low size < 20 nm) was functionalized with (3-aminopropyl)triethoxysilane (APTS). As for the previous set of NPs, the complementary NP set was obtained through the conversion of free surface amino-groups to aldehydes by reaction with glutaraldehyde. EDX, AES and ToF-SIMS spectra were collected and analyzed to demonstrate the presence of the surface functionalization of the different types of TiO2 NPs. T2 - Nanoscience meets Metrology - Synthesis, Characterization, Testing and Applications of Validated Nanoparticles - International Summer School CY - Turin, Italy DA - 04.09.2016 KW - Time-of-flight secondary-ion mass spectrometry KW - X-ray spectroscopy KW - Auger electron spectroscopy KW - Electron microscopy KW - Nanoparticles KW - Thin films PY - 2016 UR - http://www.setnanometro.eu/events/ AN - OPUS4-38064 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Ringversuch zur Klassifizierung von Kohlenstoffschichten mittels Ellipsometrie N2 - Der Vortrag widmet sich dem „Ringversuch zur Klassifizierung von Kohlenstoffschichten mittels Ellipsometrie“ und beschreibt die experimentellen Eckdaten, die Ellipsometrie als Messmethode am Beispiel DLC auf Stahl, Proben vs. n-k Ebene vs. Ergebnisse des Ringversuches, messtechnische Bewertung des Ringversuches und normative Bewertung des Ringversuches sowie Schlussfolgerungen. T2 - 9. Sitzung DIN NA 062-01-64 „Kohlenstoffschichten“ CY - Berlin, Deutschland DA - 09.05.2016 KW - Amorphe Kohlenstoffschichten KW - Optische Konstanten KW - Ellipsometrie KW - Klassifizierungssystem PY - 2016 AN - OPUS4-38041 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fankhänel, J. A1 - Silbernagl, Dorothee A1 - Ghasem Zadeh Khorasani, Media A1 - Daum, B. A1 - Kempe, A. A1 - Sturm, Heinz A1 - Rolfes, R. T1 - Mechanical properties of Boehmite evaluated by Atomic Force Microscopy experiments and Molecular Dynamic Finite Element simulations N2 - Boehmite nanoparticles show great potential in improving mechanical properties of fiber reinforced polymers. In order to predict the properties of nanocomposites, knowledge about the material parameters of the constituent phases, including the boehmite particles, is crucial. In this study, the mechanical behavior of boehmite is investigated using Atomic Force Microscopy (AFM) experiments and Molecular Dynamic Finite Element Method (MDFEM) simulations. Young’s modulus of the perfect crystalline boehmite nanoparticles is derived from numerical AFM simulations. Results of AFM experiments on boehmite nanoparticles deviate significantly. Possible causes are identified by experiments on complementary types of boehmite, that is, geological and hydrothermally synthesized samples, and further simulations of imperfect crystals and combined boehmite/epoxy models. Under certain circumstances, the mechanical behavior of boehmite was found to be dominated by inelastic effects that are discussed in detail in the present work.The studies are substantiated with accompanying X-ray diffraction and Raman experiments. KW - AFM KW - MDFEM KW - Nanocomposite KW - Epoxy KW - X-ray diffraction KW - Raman spectroscopy KW - Young’s modulus KW - Slippage of weakly linked layers PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-384230 UR - https://www.hindawi.com/journals/jnm/2016/5017213/#B26 DO - https://doi.org/10.1155/2016/5017213 VL - 2016 IS - Article ID 5017213 SP - 1 EP - 13 PB - Hindawi Publishing Corporation AN - OPUS4-38423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weller, Michael G. T1 - Antibody quality - a never-ending story? N2 - Deficiencies in research antibody quality lead to economic losses up to several billions of Euros annually. Poorly documented antibody experiments lead to a flood of publications without any chance to be reproduced and without any scientific value.The dominance of antibody specifications in complex analytical procedures is often highly underestimated. Most journals and funding agencies lack the expertise to identify major flaws in antibody experiments and their documentation. Most companies sell insufficiently characterized and documented antibodies. Recombinant antibodies are not the solution for antibody validation. T2 - Seminar des Instituts für Analytische Chemie der Universität Wien CY - Wien, Austria DA - 17.11.2016 KW - Antibodies KW - Reproducibility KW - Crisis KW - Antibody ID PY - 2016 AN - OPUS4-38424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Imrie, F. E. T1 - Biocompatibility of DC magnetron-sputtered TiO2 coatings with nano-scale morphology and controlled phase composition on glass substrates N2 - SETNanoMetro, a European Seventh Framework project, seeks to develop standard synthetic routes and metrological characterisation methods for the development and production of TiO2 nanoparticles and nano-sized coatings with highly-defined, homogeneous and reproducible characteristics. These materials are being tested for their potential in selected technological applications, including as biomaterials, specifically as coatings on dental or orthopaedic metallic prostheses. This study aimed to assess how variations in nano-scale morphology and phase composition of TiO2 coatings affect their biocompatibility in vitro. Pulsed DC magnetron sputtering was used to deposit a layer of Ti metal followed by a layer of TiO¬2 on standard glass microscope slides. The substrate bias voltage was varied during deposition to control the morphology and phase composition of the TiO2 layers. In order of increasing substrate bias voltage, the phase compositions of the TiO2 layers were: predominantly anatase, mixed anatase/rutile, and predominantly rutile, as confirmed by XRD. Examination of the coating cross-sections by SEM revealed feather-like columnar structures in the thin (950 nm thick) and thick (1550 nm thick) anatase coatings and in the mixed anatase/rutile coating (900 nm thick). In the rutile coating (730 nm thick), the columns were denser and had largely lost their feather-like structure. Top-view SEM showed square-pyramidal morphology of the columns in the anatase coatings, with columns generally 100 nm or smaller in size (thin coating) or up to 200 nm across (thick coating). In the mixed anatase/rutile coating, the top-view showed less regular columnar morphology with more elongated columns (up to approx. 100 nm by 200 nm). In the rutile coating, the top-view showed a less ordered, pebble-like morphology. MG-63 human osteoblast-like cells and RAW 264.7 murine macrophage cells were cultured on the TiO2-coated substrates for 24 or 72 h before quantification of cell proliferation using the WST-1 cell proliferation assay. A toxic response was defined as a reduction in cell viability of greater than 30%. After 24 h culture, proliferation of MG-63 cells was significantly greater than the control (p < 0.05) on the thin anatase and mixed anatase/rutile coatings. After 72 h of culture no significant difference to the control was observed. For RAW 264.7 cells, proliferation was non-significantly decreased compared to the control on all coatings except the rutile coating after 24 h. After 72 h, RAW 264.7 proliferation was significantly decreased (p < 0.01) to 68% and 61% of the control for the thick and thin anatase coatings, respectively, indicating a toxic response. The results indicate that nano-sized TiO2 coatings show different biocompatibility to different test cell types, with a dependence upon coating phase composition and morphology. T2 - 2016 MRS (Materials Research Society) Fall Meeting CY - Boston, MA, USA DA - 27.11.2016 KW - Biocompatibility KW - TiO2 coating KW - In vitro KW - Cell proliferation KW - Toxicity PY - 2016 AN - OPUS4-38427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belsey, N. A. A1 - Cant, D. J. H. A1 - Minelli, C. A1 - Araujo, J. R. A1 - Bock, B. A1 - Brüner, P. A1 - Castner, D. G. A1 - Ceccone, G. A1 - Counsell, J. D. P. A1 - Dietrich, Paul M. A1 - Engelhardt, M. H. A1 - Fearn, S. A1 - Galhardo, C. E. A1 - Kalbe, H. A1 - Kim, J. W. A1 - Lartundo-Rojas, L. A1 - Luftman, H. S. A1 - Nunney, T. S. A1 - Pseiner, J. A1 - Smith, E. F. A1 - Spampinato, V. A1 - Sturm, J. M. A1 - Thomas, A. G. A1 - Treacy, J. P. W. A1 - Veith, L. A1 - Wagstaffe, M. A1 - Wang, H. A1 - Wang, M. A1 - Wang, Y.-C. A1 - Werner, W. A1 - Yang, L. A1 - Shard, A. G. T1 - Versailles Project on Advanced Materials and Standards Interlaboratory Study on Measuring the Thickness and Chemistry of Nanoparticle Coatings Using XPS and LEIS N2 - We report the results of a Versailles Project on Advanced Materials and Standards (VAMAS) interlaboratory study on the measurement of the shell thickness and chemistry of nanoparticle coatings. Peptide-coated gold particles were supplied to laboratories in two forms: a colloidal suspension in pure water and particles dried onto a silicon wafer. Participants prepared and analyzed these samples using either X-ray photoelectron spectroscopy (XPS) or low energy ion scattering (LEIS). Careful data analysis revealed some significant sources of discrepancy, particularly for XPS. Degradation during transportation, storage, or sample preparation resulted in a variability in thickness of 53%. The calculation method chosen by XPS participants contributed a variability of 67%. However, variability of 12% was achieved for the samples deposited using a single method and by choosing photoelectron peaks that were not adversely affected by instrumental transmission effects. The study identified a need for more consistency in instrumental transmission functions and relative sensitivity factors since this contributed a variability of 33%. The results from the LEIS participants were more consistent, with variability of less than 10% in thickness, and this is mostly due to a common method of data analysis. The calculation was performed using a model developed for uniform, flat films, and some participants employed a correction factor to account for the sample geometry, which appears warranted based upon a simulation of LEIS data from one of the participants and comparison to the XPS results. KW - VAMAS KW - Interlaboratory Study KW - Nanoparticle coating KW - XPS KW - LEIS KW - shell thicknss and chemistry PY - 2016 UR - http://pubs.acs.org/doi/pdf/10.1021/acs.jpcc.6b06713 DO - https://doi.org/10.1021/acs.jpcc.6b06713 IS - 120 SP - 24070 EP - 24079 PB - ACS Publications AN - OPUS4-38428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mielke, Johannes A1 - Dohányosová, P. A1 - Lopez, S. A1 - Hodoroaba, Vasile-Dan T1 - Electrospray deposition of nanoparticles on TEM grids N2 - The authors have tested the prototype of an electrospray deposition system developed by the company RAMEM under its trademark IONER. To test the prototype and assess its performance, several materials have been sprayed onto TEM grids and the resulting particle distributions were compared to more traditional sample preparation strategies like the “drop on grid” method. Operation parameters such as the sample flow-rate, capillary – substrate distance, electric field strength and sampling period length have been optimized. It was found that the particles deposited by electrospray generally show a much more homogeneous spatial distribution on the substrate and a substantial increase of the number of single particles, which are much better suited to an automatic image evaluation procedure than the agglomerated particles observed otherwise. The applicability of the technique to a broad range of materials is demonstrated by various examples, but also the influence of the substrate, the choice of the particular TEM grid, on the obtained spatial particle distribution is assessed. KW - Electrspray deposition KW - Electron microscopy KW - Nanoparticles KW - Sample preparation PY - 2016 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/electrospray-deposition-of-nanoparticles-on-tem-grids/459E634B7F74D474A19E15E69DA82E5D DO - https://doi.org/10.1017/S1431927616010072 SN - 1431-9276 SN - 1435-8115 VL - 22 IS - Suppl 3 SP - 1846 EP - 1847 PB - Cambridge AN - OPUS4-38436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Daschewski, Maxim T1 - Thermophony in real gases - Theory and applications N2 - A thermophone is an electrical device for sound generation. The advantages of thermophones over conventional sound transducers such as electromagnetic, electrostatic or piezoelectric transducers are their operational principle which does not require any moving parts, their resonance-free behavior, their simple construction and their low production costs. In this PhD thesis, a novel theoretical model of thermophonic sound generation in real gases has been developed. The model is experimentally validated in a frequency range from 2 kHz to 1 MHz by testing more than fifty thermophones of different materials, including Carbon nano-wires, Titanium, Indium-Tin-Oxide, different sizes and shapes for sound generation in gases such as air, argon, helium, oxygen, nitrogen and sulfur hexafluoride. Unlike previous approaches, the presented model can be applied to different kinds of thermophones and various gases, taking into account the thermodynamic properties of thermophone materials and of adjacent gases, degrees of freedom and the volume occupied by the gas atoms and molecules, as well as sound attenuation effects, the shape and size of the thermophone surface and the reduction of the generated acoustic power due to photonic emission. As a result, the model features better prediction accuracy than the existing models by a factor up to 100. Moreover, the new model explains previous experimental findings on thermophones which cannot be explained with the existing models. The acoustic properties of the thermophones have been tested in several gases using unique, highly precise experimental setups comprising a Laser-Doppler-Vibrometer combined with a thin polyethylene film which acts as a broadband and resonance-free sound-pressure detector. Several outstanding properties of the thermophones have been demonstrated for the first time, including the ability to generate arbitrarily shaped acoustic signals, a greater acoustic efficiency compared to conventional piezoelectric and electrostatic airborne ultrasound transducers, and applicability as powerful and tunable sound sources with a bandwidth up to the megahertz range and beyond. Additionally, new applications of thermophones such as the study of physical properties of gases, the thermo-acoustic gas spectroscopy, broad-band characterization of transfer functions of sound and ultrasound detection systems, and applications in non-destructive materials testing are discussed and experimentally demonstrated. N2 - Ein Thermophon ist ein elektrisches Gerät zur Schallerzeugung. Aufgrund der fehlenden beweglichen Teile verfügen Thermophone über mehrere Vorteile gegenüber den herkömmlichen elektromagnetischen, elektrostatischen oder piezoelektrischen Schallwandlern. Besonders bemerkenswert sind das resonanz- und nachschwingungsfreie Verhalten, die einfache Konstruktion und die niedrigen Herstellungskosten. Im Rahmen dieser Doktorarbeit wurde ein neuartiges theoretisches Modell der thermophonischen Schallerzeugung in Gasen entwickelt und experimentell verifiziert. Zur Validierung des Modells wurden mehr als fünfzig Thermophone unterschiedlicher Größen, Formen und Materialien, darunter Kohlenstoff-Nanodrähte, Titan und Indium-Zinnoxid zur Erzeugung von Schall in Gasen wie Luft, Argon, Helium, Sauerstoff, Stickstoff und Schwefelhexafluorid in einem Frequenzbereich von 2 kHz bis 1 MHz eingesetzt. Das präsentierte Modell unterscheidet sich von den bisherigen Ansätzen durch seine hohe Flexibilität, wobei die thermodynamischen Eigenschaften des Thermophons und des umgebenden Gases, die Freiheitsgrade und das Eigenvolumen der Gasatome und Moleküle, die Schallschwächungseffekte, die Form und Größe des Thermophons, sowie die Verringerung der erzeugten akustischen Leistung aufgrund der Photonenemission berücksichtigt werden. Infolgedessen zeigt das entwickelte Modell eine um bis zu einem Faktor 100 höhere Vorhersagegenauigkeit als die bisher veröffentlichten Modelle. Das präsentierte Modell liefert darüber hinaus eine Erklärung zu den Ergebnissen aus den Vorarbeiten, die von den bisherigen Modellen nicht abschließend geklärt werden konnten. Die akustische Eigenschaften der Thermophone wurden unter Verwendung von einzigartigen hochpräzisen Versuchsaufbauten getestet. Dafür wurde ein Laser-Doppler-Vibrometer in Kombination mit einer dünnen Polyethylenfolie verwendet, welche als breitbrandiger und resonanzfreier Schalldruckdetektor fungiert. Somit konnten mehrere herausragende akustische Eigenschaften der Thermophone zum ersten Mal demonstriert werden, einschließlich der Möglichkeit, beliebig geformte akustische Signale zu erzeugen, eine größere akustische Wirksamkeit im Vergleich zu herkömmlichen Luftultraschallwandlern und die Anwendbarkeit als leistungsfähige beliebig abstimmbare Schallquellen mit einer Bandbreite bis in den Megahertz-Bereich. Zusätzlich werden neue Anwendungen von Thermophonen wie die Untersuchung der physikalischen Eigenschaften von Gasen, die thermoakustische Gasspektroskopie, eine breitbandige Charakterisierung der Übertragungsfunktionen von Schall- und Ultraschallmesssystemen und Anwendungen in der zerstörungsfreien Materialprüfung demonstriert. KW - Acoustic actuator KW - Thermoacoustics KW - Sound source PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:517-opus4-98866 SP - 1 EP - 85 PB - Universität Potsdam CY - Potsdam AN - OPUS4-38344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zeegers, G. P. T1 - Evidence for laser-induced redox reactions between added trifluoroacetate salts and substrate material during polystyrene/DCTB MALDI N2 - The cation addition mechanism to polystyrene and the possible interactions between the target plate material and the cationization agent have been studied. A range of different trifluoroacetate salts mixed with DCTB and polystyrene, deposited on several different target plate materials, have been systematically investigated with MALDI mass spectrometry. MALDI-MS yielded polystyrene-­ and DCTB-­Cu adducts when sample solutions were applied on a copper substrate. For silver the same effect was observed. Control experiments showed that these species could only result from laser‐induced redoxreactions between the added salt and the substrate material. Reversed redoxreactions between added salts and target plate material are enabled by laser photon energy input during MALDI experiments. T2 - 21st International Mass Spectrometry Conference (IMSC) CY - Toronto, Canada DA - 20.08.2016 KW - MALDI-TOF MS KW - Redoxreactions PY - 2016 AN - OPUS4-38418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Kabelitz, Anke A1 - Gorelik, T. E. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Kolb, U. A1 - Rademann, K. A1 - Emmerling, Franziska T1 - The crystallisation of copper(II) phenylphosphonates N2 - The crystal structures and syntheses of four different copper(II) phenylphosphonates, the monophenylphosphonates α-, β-, and γ-Cu(O3PC6H5)·H2O (α-CuPhPmH (1) β-CuPhPmH (2) and γ-CuPhPmH (3)), and the diphosphonate Cu(HO3PC6H5)2·H2O (CuPhP2mH (4)), are presented. The compounds were synthesized from solution at room temperature, at elevated temperature, under hydrothermal conditions, and mechanochemical conditions. The structures of α-CuPhPmH (1) and CuPhP2mH (4) were solved from powder X-ray diffraction data. The structure of β-CuPhPmH (2) was solved by single crystal X-ray analysis. The structures were validated by extended X-ray absorption fine structure (EXAFS) and DTA analyses. Disorder of the crystal structure was elucidated by electron diffraction. The relationship between the compounds and their reaction pathways were investigated by in situ synchrotron measurements. KW - Mechanochemistry KW - Metal phosphonate KW - In situ PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-384217 DO - https://doi.org/10.1039/C6DT02904C SN - 1477-9226 SN - 1477-9234 VL - 45 IS - 43 SP - 17453 EP - 17463 PB - The Royal Society of Chemistry AN - OPUS4-38421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter A1 - Paul, Andrea A1 - Maiwald, Michael T1 - Spektroskopische Untersuchungen an Bioprozess- Simulationsproben N2 - Zur Onlineüberwachung von Fermentationsprozessen werden zunehmend schwingungsspektroskopische (Raman-, Mittel- und Nahinfrarotspektroskopie (NIRS) und UV-/VIS- Methoden(Absorptions- und Fluoreszenzspektroskopie) in Kombination mit multivariater Auswertung eingesetzt. Anliegen dieser Arbeit war es, zu testen, welche Verfahren für die spektroskopische On- und Offlineüberwachung des Fermentationsprozesses zur biotechnologischen Herstellung einer Malariavaccine grundlegend geeignet sind und welche Messbereiche und Genauigkeiten der Vorhersage im Idealfall bei der Abwesenheit von Hefezellen erzielt werden können. T2 - 10. Kolloquium Arbeitskreis Prozessanalytik CY - Gerlingen, Germany DA - 25.11.2014 KW - Prozessanalytik KW - Prozess-Sensoren KW - Bioprozess KW - Prozess-Spektroskopie KW - Raman-Spektroskopie KW - Nahinfrarot-Spektroskopie KW - Fluoreszenz-Spektroskopie PY - 2014 UR - http://arbeitskreis-prozessanalytik.de/images/stories/Veranstaltungen/Kolloquien/10_kolloquium_2014/tagungsband_10_kolloquium_ak_prozessanalytik_2014_hq-druck_f.pdf SP - P13, 35 EP - 35 PB - BAM Bundesanstalt für Materialforschung und -prüfung CY - Berlin AN - OPUS4-38362 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ analysis of mechanochemical reactions using combined X-ray diffraction and Raman spectroscopy N2 - Mechanochemistry is increasingly used for synthesizing various materials including metal organic compounds and cocrystals. Although this synthesis approach offers a fast and pure synthesis in high yields, there is a lack in understanding the mechanisms of milling reactions. The necessary data can only be obtained in in situ experiments, which were only recently established for milling reactions. Herein, we present a novel setup enabling a combined in situ investigation of mechanochemical reactions using synchrotron XRD and Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. Besides well-known MOFs like ZIF-8, the formation process of new metal phosphonates and model cocrystals could be studied in detail. The syntheses pathway of the different compounds could be revealed. The results prove that the presented method combination is applicable for a wide range of materials and will provide the necessary understanding to tune and optimize mechanochemically synthesized compounds. T2 - 3oth Meeting of the European Crystallographic Association CY - Basel, Switzerland DA - 28.08.2016 KW - Mechanochemistry KW - In situ PY - 2016 AN - OPUS4-38363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Kern, Simon A1 - Gräßer, Patrick A1 - Maiwald, Michael ED - Maiwald, Michael T1 - Process monitoring of an intensified continuous production unit with compact NMR spectroscopy N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and relatively inexpensive analyzers, which feature advantages like low cost, low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, sufficient robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are cur-rently not available off the rack. Recently, promising benchtop NMR instruments with acceptable performance came to market and process integrated sensors developed on basis of such laboratory instruments are on their way. T2 - 12. Kolloquium des Arbeitskreises Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Online NMR spectroscopy KW - Modular production units KW - Low field NMR spectroscopy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-383646 SP - P17, 75 EP - 77 AN - OPUS4-38364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kricheldorf, H. R. T1 - Cyclization and dispersity of polyesters N2 - Starting out from Flory`s most probable Distribution concept, correct and incorrect evaluations of SEC measurements are discussed. Using the correct mode, polyesters prepared by irreversible and reversible polycondensation methods were studied. Polyesters of α,ω−alkanediols and isophthalic acid or polyesters of diphenols and sebacic acid were prepared by three different irreversible polyconcensation methods. Formation of cyclic oligo and polyesters was monitored by MALDI-TOF mass spectrometry and dispersities were measured by SEC. The results are compared with the theories of Flory and Odian. Eqilibrated polyesters were prepared by reversible polycondensation of ethyl 6-hydroxycaproate or by alcohol-initiated ring-opening polymerization of ε-caprolactone. Various catalysts were compared. The influence of dilution and of di- or multifunctional initiators was evaluated. Furthermore, equilibrated polylactides were prepared from L- or meso-lactide at 120, 160 and 180°C. A fast even-odd equilibration was discovered in addition to reversible cyclization and intermolecular transesterification. The influence of these different equilibration mechanisms on the dispersity was investigated. The preparative and theoretical consequences are discussed. T2 - Polycondensation 2016 CY - Moscow, Russia DA - 11.09.2016 KW - Polyester KW - Cyclization KW - MALDI-TOF MS KW - SEC PY - 2016 AN - OPUS4-38365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brieger, C. A1 - Melke, J. A1 - van der Bosch, N. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - de Oliveira Guilherme Buzanich, Ana A1 - Krishna Kayarkatte, M. A1 - Derr, I. A1 - Schökel, A. A1 - Roth, C. ED - de Oliveira Guilherme Buzanich, Ana T1 - A combined in-situ XAS–DRIFTS study unraveling adsorbate induced changes on Pt nanoparticle structure N2 - The adsorption behavior of Platinum nanoparticles was studied for the as-received catalyst (under inert gas), under hydrogen and CO atmosphere using our newly designed in-situ cell. X-ray Absorption Spectroscopy (XAS) and Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) experiments were performed simultaneously with high data quality. Structural information and the type of adsorbate could be revealed via Extended X-ray Absorption Fine Structure (EXAFS) analysis, Δμ X-ray Absorption Near Edge Structure analysis (Δμ XANES) and in-situ DRIFTS. The as-received catalyst showed sub-surface oxygen and O(n-fold). Under CO atmosphere only CO(atop) was found. Reversible adsorbate induced changes of the Pt nanoparticle structure were derived from changes in the Pt-Pt coordination number and the corresponding bond distance. Under reducing conditions (H2, CO) a significant increase in both values occurred. Temperature dependent desorption of CO revealed a gradual shift from Pt-CO to Pt-O. Reoxidation was clearly assigned to strong metal support interaction from the SiO2 support. KW - X-ray absorption spectroscopy KW - DRIFTS KW - XANES KW - CO adsoprtion KW - Platinum KW - String metal support interaction KW - Silica support KW - Adsorbates KW - Infrared spectroscopy PY - 2016 DO - https://doi.org/10.1016/j.jcat.2016.03.034 SN - 0021-9517 VL - 339 SP - 57 EP - 67 PB - Elsevier AN - OPUS4-38367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prinz, J. A1 - Matkovic, A. A1 - Pesic, J. A1 - Gajic, R. A1 - Bald, Ilko T1 - Hybrid structures for surface-enhanced Raman scattering: DNA origami/gold nanoparticle dimer/graphene N2 - A combination of three innovative materials within one hybrid structure to explore the synergistic interaction of their individual properties is presented. The unique electronic, mechanical, and thermal properties of graphene are combined with the plasmonic properties of gold nanoparticle (AuNP) dimers, which are assembled using DNA origami nanostructures. This novel hybrid structure is characterized by means of correlated atomic force microscopy and surface-enhanced Raman scattering (SERS). It is demonstrated that strong interactions between graphene and AuNPs result in superior SERS performance of the hybrid structure compared to their individual components. This is particularly evident in efficient fluorescence quenching, reduced background, and a decrease of the photobleaching rate up to one order of magnitude. The versatility of DNA origami structures to serve as interface for complex and precise arrangements of nanoparticles and other functional entities provides the basis to further exploit the potential of the here presented DNA origami–AuNP dimer–graphene hybrid structures. KW - DNA origami KW - Gold nanoparticles KW - Graphene KW - Surface-enhanced Raman scattering PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/smll.201601908/full DO - https://doi.org/10.1002/smll.201601908 SN - 1613-6810 SN - 1613-6829 VL - 12 IS - 39 SP - 5458 EP - 5467 AN - OPUS4-38369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska ED - de Oliveira Guilherme Buzanich, Ana T1 - Time- and spatial-resolved X-ray absorption fine structure (XAFS) spectroscopy in a single-shot: new analytical possibilities for in situ material characterization N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ-2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 µm is achieved. KW - Single-shot XAFS KW - Time resolution KW - Spatial resolution KW - Divergent XAFS PY - 2016 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 VL - 23 SP - 769 EP - 776 PB - International Union of Crystallography AN - OPUS4-38370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Würth, Christian T1 - Absolute fluorescence measurements > 1000 nm: setup design, calibration and standards N2 - Bright emitters with photoluminescence in the spectral region of 800 – 1600 nm are increasingly important as optical reporters for molecular imaging, sensing, and telecommunication and as active components in electrooptical and photovoltaic devices. Their rational design is directly linked to suitable methods for the characterization of their signal-relevant properties, especially their photoluminescence quantum yield. Aiming at the development of bright semiconductor nanocrystals with emission > 1000 nm, we designed a new NIR/IR integrating sphere setup for the wavelength region of 600 – 1600 nm. We assessed the performance of this setup by acquiring the corrected emission spectra and quantum yield of the organic dyes Itrybe, IR140, and IR26 and several infrared (IR)-emissive Cd1-xHgxTe and PbS semiconductor nanocrystals and comparing them to data obtained with two independently calibrated fluorescence instruments absolutely or relatively to previously evaluated reference dyes. Our results highlight special challenges of photoluminescence studies in the IR ranging from solvent absorption to the lack of spectral and intensity standards together with quantum dot-specific challenges like photobrightening and photodarkening and the size-dependent air stability and photostability of differently sized oleate-capped PbS colloids. These effects can be representative for lead chalcogenides. Moreover, we redetermined the quantum yield of IR26, the most frequently used IR reference dye, to 1.1×10-3 in 1,2-dichloroethane DCE with a thorough sample reabsorption and solvent absorption correction. T2 - SPIE CY - San Francisco, USA DA - 11.02.2016 KW - Ir KW - Quantum yield PY - 2016 AN - OPUS4-38405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Einblick auf die Computertomographie N2 - Ein kurzes Blick in die Computertomographie (CT) im Rahmen des RT3 Kurs der DGZfP ist gegeben. Die Radontransformation ist bildlich erklärt, und die Grundlagen der Technik mit Vergleich zu der Radiographie sind auch erwähnt. Die typische Rekonstruktionsfehler und deren Beseitigung sind behandelt. Am Ende Beispiele der Anwendungen der CT sind gegeben, aus der zerstörungsfreie Prüfung, der Materialwissenschaft und der Metrologie. T2 - DGZfP RT3 Kurs CY - BAM, Berlin, Germany DA - 01.11.2016 KW - Computertomographie KW - Metrologie KW - 3D Mikrostruktur KW - Zerstörungsfreie Prüfung KW - TF Material PY - 2016 AN - OPUS4-38329 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weller, Andreas A1 - Zhang, Z. A1 - Slater, L. A1 - Kruschwitz, Sabine A1 - Halisch, M. T1 - Induced polarization and pore radius — A discussion N2 - Permeability estimation from induced polarization (IP) measurements is based on a fundamental premise that the characteristic relaxation time τ is related to the effective hydraulic radius reff controlling fluid flow. The approach requires a reliable estimate of the diffusion coefficient of the ions in the electrical double layer. Others have assumed a value for the diffusion coefficient, or postulated different values for clay versus clay-free rocks. We have examined the link between a widely used single estimate of τ and reff for an extensive database of sandstone samples, in which mercury porosimetry data confirm that reff is reliably determined from a modification of the Hagen-Poiseuille equation assuming that the electrical tortuosity is equal to the hydraulic tortuosity. Our database does not support the existence of one or two distinct representative diffusion coefficients but instead demonstrates strong evidence for six orders of magnitude of variation in an apparent Diffusion coefficient that is well-correlated with reff and the specific surface area per unit pore volume Spor. Two scenarios can explain our findings: (1) the length scale defined by τ is not equal to reff and is likely much longer due to the control of pore-surface roughness or (2) the range of diffusion coefficients is large and likely determined by the relative proportions of the different minerals (e.g., silica and clays) making up the rock. In either case, the estimation of reff (and hence permeability) is inherently uncertain from a single characteristic IP relaxation time as considered in this study. KW - Spectral induced polarisation KW - Pore radius KW - Permeability KW - Specific surface KW - Mercury intrusion PY - 2016 DO - https://doi.org/10.1190/GEO2016-0135.1 SN - 0016-8033 SN - 1942-2156 VL - 81 IS - 5 SP - D519 EP - D526 AN - OPUS4-38393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Industrie 4.0 aus Sicht der NAMUR - Die Technologie-Roadmap "Prozess-Sensoren 4.0" und danach ... N2 - Es wurde die Anforderungen an die Kommunikatoion von Analysengeräten für eine zukünftige Topologie nach Industrie 4.0 gemeinsam mit dem ZVEI-Arbeitskreis "Kommunikationstechnik für Analysatoren" (KfA) diskutiert. Ziel des Arbeitskreises ist es, kommunikationstechnische Trends für Prozess-Analysengeräte zu beobachten und zu bewerten. Im Bedarfsfall hat dieser Arbeitskreis die Aufgabe, Analysatoren für neue Kommunikationstechniken tauglich zu machen und die dafür notwendige Anschlusstechnik (inkl. Hardware-Interface und Software) zu entwickeln. Die Arbeiten werden in der Regel im Rahmen eines Firmenkonsortiums in gemeinschaftlichen Entwicklungsprojekten durchgeführt. Eine enge Zusammenarbeit mit verschiedenen Bus-Nutzerorganisationen mit der VDI/VDE-Gesellschaft Mess- und Automati-sierungstechnik (GMA)und mit der Interessengemeinschaft Prozessleittechnik der chemischen und pharmazeutischen Industrie (NAMUR) ist hierfür Grundvoraussetzung. T2 - Kolloquium des ZVEI-Arbeitskreises "Kommunikationstechnik für Analysatoren" CY - Reute, Germany DA - 17.11.2016 KW - Industrie 4.0 KW - ZVEI KW - Kommunikation für Analysengeräte KW - Kommunikation KW - Prozessanalytik KW - Prozess-Sensoren PY - 2016 AN - OPUS4-38358 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Kraemer, B. A1 - Zientek, Nicolai A1 - Esche, E. A1 - Müller, D. A1 - Wozny, G. A1 - Maiwald, Michael T1 - Eine robuste Prozessanalytik für die Reaktivabsorption von CO2 aus industriellen Gasströmen basierend auf Online-NMR- und -Raman-Spektroskopie N2 - Die Abtrennung von CO2 aus industriellen Gasströmen ist eine großtechnisch wichtige Trennaufgabe. Neben der Aufarbeitung von Erdgas werden diese Verfahren zur Verminderung der CO2-Emission durch industrielle Rauchgase, insbesondere für alternativlose Prozesse wie die Stahl- und Zementproduktion diskutiert. T2 - 10. Kolloquium Arbeitskreis Prozessanalytik CY - Gerlingen, Germany DA - 25.11.2014 KW - Prozessanalytik KW - Quantitative NMR-Spektroskopie KW - Raman spectroscopy KW - CO2-Absorption KW - CCS PY - 2014 UR - http://arbeitskreis-prozessanalytik.de/images/stories/Veranstaltungen/Kolloquien/10_kolloquium_2014/tagungsband_10_kolloquium_ak_prozessanalytik_2014_hq-druck_f.pdf SP - P03, 23 EP - 23 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38359 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zientek, Nicolai A1 - Laurain, Clement A1 - Meyer, Klas A1 - Paul, Andrea A1 - Engel, D. A1 - Guthausen, G. A1 - Kraume, M. A1 - Maiwald, Michael T1 - Automated data evaluation and modeling of simultaneous 19F-1H medium resolution NMR spectra for online reaction monitoring N2 - Medium resolution nuclear magnetic resonance spectroscopy (MR-NMR) currently develops to an important analytical tool for both quality control and process monitoring. One of the fundamental acceptance criteria for online MR-MNR spectroscopy is a robust data treatment and evaluation strategy with the potential for automation. The MR-NMR spectra were treated by an automated baseline and phase correction using the minimum entropy method. The evaluation strategies comprised direct integration, automated line fitting, indirect hard modeling, and partial least squares regression. T2 - 10. Kolloquium Arbeitskreis Prozessanalytik CY - Gerlingen, Germany DA - 25.11.2014 KW - Online NMR spectroscopy KW - Data evaluation KW - Reaction monitoring KW - Indirect hard modeling PY - 2014 UR - http://arbeitskreis-prozessanalytik.de/images/stories/Veranstaltungen/Kolloquien/10_kolloquium_2014/tagungsband_10_kolloquium_ak_prozessanalytik_2014_hq-druck_f.pdf SP - P04, 24 EP - 25 PB - BAM Bundesanstalt für Materialforschung und -prüfung CY - Berlin AN - OPUS4-38360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea A1 - Müller, D. A1 - Esche, E. A1 - Wozny, G. A1 - Maiwald, Michael T1 - Chemometric modeling of on-line Raman spectra from miniplant operation N2 - The project InPROMPT aims to establish a robust hydroformylation reaction process of the alkene n-dodecene to the aldehyde n-tridecanal using a rhodium complex as catalyst in the presence of syngas. This industrial relevant production process demands further research for optimization and expansion. For that purpose, the fiber optic coupled probe of a process Raman spectrometer is directly introduced in the product stream, which enables the recording of spectra within short control intervals. T2 - 10. Kolloquium Arbeitskreis Prozessanalytik CY - Gerlingen, Germany DA - 25.11.2014 KW - Reaction monitoring KW - Chemometrics KW - Raman spectroscopy KW - Hydroformylation PY - 2014 UR - http://arbeitskreis-prozessanalytik.de/images/stories/Veranstaltungen/Kolloquien/10_kolloquium_2014/tagungsband_10_kolloquium_ak_prozessanalytik_2014_hq-druck_f.pdf SP - P12, 34 EP - 34 PB - BAM Bundesanstalt für Materialforschung und -prüfung CY - Berlin AN - OPUS4-38361 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen A1 - Büchele, Dominique A1 - Schmid, Thomas A1 - Ostermann, Markus T1 - Development of an online-analysis technique for the determination of plant essential nutrients in soils using XRF and LIBS N2 - Currently, there is almost no comprehensive mapping of agricultural cropland because of the lack of fast and affordable mapping methods for important soil properties. Arable land of some hectares in size show a broad range of different nutrient compositions. Because of this heterogeneity wrong fertilization can occur and can cause environmental pollution or lead to smaller harvests and this is simply a waste of resources. The goal of I4S (intelligence for soil) is to develop an integrated system for site-specific soil fertility management. The I4S consortium consists of 10 different institutions, which are testing various sensors for their suitability for the requested applications. Besides the preparation of reference materials, the main task of the Federal Institute for Materials Research and Testing (BAM) in this project is the method development for online-XRF (x-ray fluorescence spectroscopy) and for online-LIBS (laser-induced breakdown spectroscopy) sensor systems. Both methods have the advantage that there is no or only little sample preparation necessary. Each method provides a fast and simultaneous multi-element analysis. Both measurement setups can be utilized for a mobile application which is fundamental for reaching the goals of I4S. Having finally a set of some reference materials, further work will focus on the online-XRF and online-LIBS methods in order to obtain useable calibration models. The calibration models will then be tested using stationary and moving samples. T2 - 12. Kolloquium Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - RFA KW - LIBS KW - Soil KW - Agricultural KW - Online KW - Sensor system PY - 2016 SP - P12, 63 EP - 65 AN - OPUS4-38377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, X.-d. A1 - Meier, R.J. A1 - Schäferling, Michael A1 - Bange, S. A1 - Lupton, J.M. A1 - Sperber, M. A1 - Wegener, J. A1 - Ondrus, V. A1 - Beifuss, U. A1 - Henne, U. A1 - Klein, C. A1 - Wolfbeis, Otto S. T1 - Two-photon excitation temperature nanosensors based on a conjugated fluorescent polymer doped with an Europium probe N2 - A strongly fluorescent organic semiconducting polymer doped with a highly temperature dependent fluorescent europium(III) complex is converted into a nanosized material that is capable of optically sensing temperature (T) in the range from 0 to 50 °C via two-photon excitation at 720 nm. The nanosensors are prepared from a blue-fluorescent polyfluorene that acts as both a lightharvesting antenna (to capture two-photon energy) and an energy donor in a fluorescence resonance energy transfer (FRET) system. The photonic energy absorbed by the polymer is transferred to the T-sensitive red-luminescent europium complex contained in the nanoparticles. The close spatial proximity of the donor and the acceptor warrants efficient FRET. A poly(ethylene glycol)- co-poly(propylene oxide) block copolymer is also added to render the particles biocompatible. It is shown that T can be calculated from a) the intensity of the luminescence of the europium complex, b) the ratio of the intensities of the red and blue luminescence, or c) the T-dependent luminescence lifetime of the Eu(III) complex. KW - Optical sensor KW - Temperature sensor KW - Nanosensor KW - FRET system PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/adom.201600601/abstract DO - https://doi.org/10.1002/adom.201600601 SN - 2195-1071 VL - 4 IS - 11 SP - 1854 EP - 1859 PB - Wiley-VCH CY - Weinheim AN - OPUS4-38737 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Schäferling, Michael ED - Meyers, R.A. T1 - Fluorescence-based biosensors N2 - Biosensors, as defined by Pure and Applied Chemistry, are ‘chemical sensors in which the recognition System utilizes a biochemical mechanism. The biological recognition system translates information from the biochemical domain, usually an analyte concentration, into a chemical or physical output signal with a defined sensitivity’.(1) It is also appointed that chemical or biological sensors contain two basic components connected in series: a chemical or biomolecular recognition System (receptor) and a physicochemical transducer. According to this prerequisite, this overlook is confined to sensor devices that combine a biomolecular recognition element with an optical signal transducer. Homogeneous or intracellular assays using fluorescent molecular probes or nanoparticles are not considered, although they are frequently termed as molecular sensors or nanosensors in the literature. Fluorescence-based biosensors are generalized as those devices that derive an analytical signal from a photoluminescent (either fluorescence or phosphorescence) emission process. Chemi- or bioluminescent detection systems are only briefly discussed in this review. Biosensors are used for a wide variety of tasks, including detection of compounds of biomedical, environmental or defense interest; on-line monitoring for process control; quality control of foodstuffs; selective detection of compounds undergoing a chemical separation; and screening of drug compounds. Advantages of such devices include high selectivity, rapid response times, reusability, amenability to remote analysis, and immunity to electrical interferences. The selective nature of complexation between biomolecule and analyte and the small size of sensor devices can be combined with advanced detection techiques such as total internal reflection (TIR) spectroscopy. This results in an ability to measure analytes in complex matrices with unsurpassed sensitivity. Such samples may include highly scattering components such as milk or whole blood,(11) or relatively inaccessible locations such as groundwater wells, or even intracellular environments. The key limitation of such devices mainly centers on the poor stability of biological compounds, which can lead to a substantial drift in instrumental response over time. The so-called Cambridge Definition appoints another characteristic property of sensors. Therein, they are defined as ‘miniaturized devices which can deliver real-time and on-line information on the presence of specific compounds or ions in even complex samples’. Accordingly, a sensor is expected to respond reversibly and continuously. With the exception of some enzymatic sensors, these conditions are not fulfilled in case of most biosensors. Particularly, in devices where immunological reagents or DNA are used as recognition elements, they show a lack of reversibility and operate only as a ‘one-shot’ screen, without the potential for continuous, quantitative analysis. Nevertheless, the designations immunosensors or DNA sensors became accepted for such analytical or diagnostic tools. KW - Biosensor KW - Fluorescence KW - Immunoassay KW - Enzyme sensor KW - DNA sensor PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/9780470027318.a0206.pub3/abstract SN - 9780470027318 DO - https://doi.org/10.1002/9780470027318.a0206.pub3 SP - 1 EP - 51 PB - John Wiley & Sons AN - OPUS4-38741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hübert, Thomas T1 - H2Sense - Cost-effective and reliable Hydrogen Sensors for Facilitating the Safe Use of Hydrogen N2 - The H2SENSE (Cost-effective and reliable hydrogen sensors for facilitating the safe use of hydrogen) project promoted hydrogen primarily, but not exclusively, for its use as an alternative fuel. It brought together different stakeholders including sensor manufacturers, end-users, certification bodies and independent evaluators to ensure the optimum use of low-cost and reliable hydrogen sensors. Project partners analysed sensor performance in real-life applications in industrial environments and identified increased requirements for sensors and for regulations, codes and standards. H2SENSE also facilitated the safe use and implementation of hydrogen as an alternative fuel by ensuring the correct use of effective hydrogen detection devices. European scientists worked together with colleagues from the National Renewable Energy Laboratory (NREL) in Colorado, USA. They pooled their knowledge of developments in hydrogen sensor technology as well as deployment and commercialisation strategies. These benefits will be continued through trans-Atlantic inter-laboratory sensor testing programmes in which EU and US laboratories perform complementary tests and exchange results. KW - Sensors KW - Hydrogen KW - Renewable energy PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-387484 SP - 1 EP - 3 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38748 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Searching for harmony in metrology: Examples from SAXS N2 - General SAXS introductory talk given at Keele University (UK) on the 30th of November, 2016. T2 - Invited talk, special seminar CY - Staffordshire, UK DA - 30.11.2016 KW - SAXS KW - Metrology KW - Small-angle X-ray scattering PY - 2016 AN - OPUS4-38701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Beiranvand, Z. A1 - Kakanejadifard, A. A1 - Donskyi, Ievgen A1 - Faghani, A. A1 - Tu, Z. A1 - Lippitz, Andreas A1 - Sasanpour, P. A1 - Maschietto, F. A1 - Paulus, B. A1 - Haag, R. A1 - Adeli, M. T1 - Functionalization of fullerene at room temperature: toward new carbon vectors with improved physicochemical properties N2 - In this work, fullerene has been functionalized with cyanuric Chloride at room temperature by a nitrene mediated [2 + 1] cycloaddition reaction. The adduct after functionalization is inherently in the form of azafulleroid and shows broad UV absorption in the wavelength range of 200–800 nm, as well as photothermal conversion and fluorescence with a high quantum yield. KW - Functionalization of fullerenes KW - XPS KW - NEXAFS PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-387076 DO - https://doi.org/10.1039/c6ra23419d SN - 2046-2069 VL - 6 IS - 114 SP - 112771 EP - 112775 PB - Royal Society of Chemistry (RSC) AN - OPUS4-38707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Franziska T1 - In situ investigation of the mechanochemical formation of cocrystals unsing combined PXRD and Raman spectroscopy N2 - We present an in situ investigation of the mechanochemical formation of cocrystals using synchrotron XRD and Raman spectroscopy. This combination allows to study milling processes on the level of the molecular and crystalline structure thus obtaining reliable data for mechanistic studies. Thereby, mechanochemical syntheses can be optimized to isolate new crystal structures. T2 - Joint BER II and BESSY II User Meeting 2016 CY - Berlin, Germany DA - 07.12.2016 KW - Intermediate KW - Mechanochemistry KW - Cocrystal KW - In situ KW - Milling PY - 2016 AN - OPUS4-38722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Niederleithinger, Ernst T1 - State-of-the-art of Ultrasonic Monitoring of Concrete N2 - Ultrasonic methods are well established in various aspects of concrete testing. They are used for imaging the interior geometry of constructions, estimation of concrete strength or monitoring lab investigations. However, so far the detection of distributed damages, especially in an early stage, has been almost impossible. The arrival of new technologies as deep penetration ultrasonic echo devices, new imaging techniques, embedded transducers for permanent monitoring and sensitive data processing techniques adopted from seismology have opened new fields of work. Recent research has been focused to detect changes in concrete elements induced by stress, temperature, moisture or chemical attacks. KW - Ultrasound KW - Concrete KW - Monitoring KW - Imaging PY - 2016 IS - 10 SP - 15 EP - 18 AN - OPUS4-38728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - State-of-the-art ultrasonic monitoring of concrete N2 - Ultrasonic methods are well established in various aspects of concrete testing. They are used for imaging the interior geometry of constructions, estimation of concrete strength or monitoring lab investigations. However, so far the detection of distributed damages, especially in an early stage, has been almost impossible. The arrival of new technologies as embedded transducers and sensitive data processing techniques adopted from seismology has opened new field of work. Recent research has been focused to detect changes in concrete elements induced by stress, temperature, moisture or chemical attacks by permanent monitoring. Techniques as Coda Wave Interferometry can resolve changes in ultrasonic velocity in the order of 1*10-5. In addition, many researchers believe that the investigation of nonlinear effects can be used to characterize damages. The presentation will give a wrap up of ultrasonic techniques currently used in practice. This will include echo based methods as multi-channel/multi-offset imaging of structural elements using commercial and prototype devices. Imaging methods as SAFT and RTM will be shortly discussed. The focus will be on the emerging techniques used for monitoring. New types of sensors will be presented as well as the devices used in laboratory and field applications. Insight will be given on the various influence factors on ultrasonic signals and various ways of feature extraction and data processing. The results of lab experiments will be shown to demonstrate the detection of various kind of damages from mechanical load, ASR, corrosion to fatigue. The experiences with or first installations in real constructions (bridges, tunnel) will also be presented. T2 - CBIR Research Seminar, University of Technology Sydney CY - Sydney, Australia DA - 05.12.2016 KW - Ultrasound KW - Concrete KW - Monitoring KW - Imaging PY - 2016 AN - OPUS4-38730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Progress in non-destructive testing and monitoring of concrete N2 - The presentation will give an overview on non-destructive testing techniques being developed at the Federal Institute for Materials Research and Testing, Germany (BAM). This includes ultrasonic methods, ground penetration radar, Laser-Induced Breakdown Spectroscopy (LIBS), infrared thermography, pile testing, sensor technology and building scanner. A focus of the talk will be ultrasonic methods, which are well established in various aspects of concrete testing. They are used for imaging the interior geometry of constructions, estimation of concrete strength or monitoring lab investigations. However, so far the detection of distributed damages, especially in an early stage, has been almost impossible. The arrival of new technologies as embedded transducers and sensitive data processing techniques adopted from seismology has opened new field of work. Recent research has been focused to detect changes in concrete elements induced by stress, temperature, moisture or chemical attacks by permanent monitoring. Techniques as Coda Wave Interferometry can resolve changes in ultrasonic velocity in the order of 1*10-5. In addition, many researchers believe that the investigation of nonlinear effects can be used to characterize damages. The presentation will give a wrap up of ultrasonic techniques currently used in practice. This will include echo based methods as multi-channel/multi-offset imaging of structural elements using commercial and prototype devices. Imaging methods as SAFT and RTM will be shortly discussed. The focus will be on the emerging techniques used for monitoring. New types of sensors will be presented as well as the devices used in laboratory and field applications. Insight will be given on the various influence factors on ultrasonic signals and various ways of feature extraction and data processing. The results of lab experiments will be shown to demonstrate the detection of various kind of damages from mechanical load, ASR, corrosion to fatigue. The experiences with our first installations in real constructions (bridges, tunnel) will also be presented. T2 - CIE Research Seminar, University of Western Sydney, New South Wales CY - Sydney, Australia DA - 15.12.2016 KW - Ultrasound KW - Concrete KW - Monitoring KW - Imaging PY - 2016 AN - OPUS4-38732 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Prost, J. T1 - Cr, Cu and Zn K-edge SR-TXRF-XANES of indoor aerosol samples at BESSY II and ELETTRA N2 - Airborne particulate matter is an issue of growing concern in industrialized countries. Particles with diameters of less than 10 μm (especially those smaller than 2.5 μm) can enter the human respiratory system and contribute to various diseases depending on their chemical composition and the chemical bonding state, in which elements are present. This chemical speciation can be obtained using X-ray absorption near-edge structure analysis (XANES), which requires a tunable excitation source and therefore has to be carried out at synchrotron facilities. Our special interest lies on the analysis of indoor airborne particulate matter, as particle composition and health effects of outdoor particles have been studied abundantly. For this work, samples were collected in various office rooms in the Atominstitut (ATI) building. The BAMline at BESSYII features a double-multilayer monochromator (DMM) and a double-crystal monochromator (DCM). The DCM offers an energy resolution E/ΔE of around 103, which makes it suitable for XANES applications. The ATI SR-TXRF vacuum chamber, formerly located at HASYLAB, Beamline L, is now available at the BAMline. The chamber offers a sample changer for up to 8 quartz reflectors and a 30 mm² silicon drift detector (SDD) was used. Aerosol samples were produced using a modified three-stage Dekati™ impactor. For this work, only the coarse (2.5 to 10 μm) and the fine particle fraction (1 to 2.5 μm), were of interest. XANES results of Cr, Cu and Zn will be presented on this poster. The X-ray Fluorescence beamline at ELETTRA operates in partnership with the IAEA an ultra-high vacuum instrument with a 7-axis manipulator suitable for a variety of X-ray analytical techniques, such as grazing incidence and total reflection X-ray fluorescence analysis (GI-XRF and TXRF), X-ray reflectometry (XRR) and XANES. Samples were produced using a four-stage Sioutas Personal Cascade Impactor. With this impactor, it is possible to produce size-fractionated samples down to the sub-μm range (Stages: A > 2.5 μm, B 1 to 2.5 μm, C 0.5 to 1 μm and D 0.25 to 0.5 μm). Direct sampling was performed on siliconized 25 mm Si wafers suitable for TXRF. Cu-K edge SR-TXRF-XANES analysis was carried out for samples of all impactor stages. Results of these experiments will be shown. T2 - European Conference on X-Ray Spectrometry (EXRS) CY - Gothenburg, Sweden DA - 19.06.2016 KW - Synchrotron KW - BAMline KW - BESSY KW - Aerosol KW - XANES PY - 2016 AN - OPUS4-38764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rauwolf, M. T1 - Zinc distribution in human bone: Sr-micro X-ray fluorescence imaging of osteoporotic samples N2 - Zn is known to be located in the reactive centers of various enzymes, which play a major role in the mineralization process at sites where new bone formation occurs. In addition, elevated Zn levels are supposed to increase the proliferation rate of osteoblasts [1] and may lead to a stimulation of bone formation in vitro and in vivo [2]. Consequently, Zn seems to play an essential role in bone formation and mineralization through various pathways. We thus expected Zn levels to be altered at sites of extensive bone formation like in the case of fracture healing. We measured the same areas on human bone samples with both a scanning confocal synchrotron radiation induced micro X-ray fluorescence (SR-μXRF) at the FLUO beamline (ANKA) and a full-field Color X-ray Camera at the BAMline (Bessy II) setup in order to find the ideal SR-μXRF imaging method to investigate trace element distributions in bone samples. As zinc is a trace element of special interest in bone, the setups were optimized for Zn detection. The setups were compared concerning count rate, required measurement time and resolution. We could show that the ideal method is depending on the element of interest. While for Ca (a major constituent of the bone with a low energy of 3.69keV for K) the Color X-ray Camera provided us with a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-μXRF was able to sufficiently image the distribution. Biopsies of healing osteoporotic fractures (Vertebral compression fractures (VCFs)) were investigated in regard to their Zn distribution. The samples were measured with a confocal SR-μXRF setup with a 10 μm x 15 μm resolution at the FLUO beamline at ANKA. As we found increased Zn levels, which seemed to be accumulated in narrow structures between bone packages we also investigated thin cuts (4 μm thick) of two sample areas with a higher resolution of 1 μm x 1 μm (monochromatic beam with E= 17 keV) at B16 at Diamond SR facility. We will present the advantages and disadvantages of all three SR-μXRF setups (ANKA FLUO beamline, Bessy II BAMline, and Diamond B16) for imaging elemental distributions in bone with a focus on Zn. We will also show the distribution of Zn in healing VCFs. T2 - XRM2016: 13th International Conference on X-Ray Microscopy CY - Oxford, UK DA - 15.08.2016 KW - Synchrotron KW - BAMline KW - XRF PY - 2016 AN - OPUS4-38765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Investigation on fire gilding using XRF and NAA N2 - Fire-gilding or amalgam gilding is a historical technique for the gilding of objects. The object to be gilded is coated with an amalgam (a solution of gold (Au) in mercury (Hg)). By heating, the largest part of the Hg is subsequently evaporated and there remains a gold layer, containing still detectable amounts of Hg. The information on the used gilding technique might be crucial for the conservation and preservation of archaeological objects. Therefore, the main objective of this work is the detailed understanding of the behaviour of Hg under conditions of fire gilding. I.e. the understanding of the diffusion and evaporating behaviour of Hg, depending on parameters like substrate material (silver, copper, bronze, brass...), heating temperature and duration, and the resulting Hg depth profiles under these conditions. Secondary objective is the establishment of a measurement protocol for the unambiguous identification of different types of gilding, based solely on non-destructive methods, which can be applied to historical samples. In a first step, fire-gilded samples have been prepared on Cu and Ag sheet metal, respectively. Some of the gildings were produced by a professional goldsmith; another set of samples was produced under laboratory conditions. These samples have been examined with NAA (neutron activation analysis) and SR-XRF (synchrotron radiation induced X-ray fluorescence). First results of these measurements will be presented and discussed. T2 - Synchrotron Radiation and Neutrons in Art & Archaeology (SR2A) CY - Chicago, IL, USA DA - 06.09.2016 KW - Synchrotron KW - BAMline KW - XRF KW - Archaeometry PY - 2016 AN - OPUS4-38766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strub, E. T1 - Investigation on fire gilding using XRF and NAA N2 - Fire-gilding or amalgam gilding is a historical technique for the gilding of objects. The object to be gilded is coated with an amalgam (a solution of gold (Au) in mercury (Hg)). By heating, the largest part of the Hg is subsequently evaporated and there remains a gold layer, containing still detectable amounts of Hg. The information on the used gilding technique might be crucial for the conservation and preservation of archaeological objects. Therefore, the main objective of this work is the detailed understanding of the behaviour of Hg under conditions of fire gilding. I.e. the understanding of the diffusion and evaporating behaviour of Hg, depending on parameters like substrate material (silver, copper, bronze, brass...), heating temperature and duration, and the resulting Hg depth profiles under these conditions. Secondary objective is the establishment of a measurement protocol for the unambiguous identification of different types of gilding, based solely on non-destructive methods, which can be applied to historical samples. In a first step, fire-gilded samples have been prepared on Cu and Ag sheet metal, respectively. Some of the gildings were produced by a professional goldsmith; another set of samples was produced under laboratory conditions. These samples have been examined with NAA (neutron activation analysis) and SR-XRF (synchrotron radiation induced X-ray fluorescence). First results of these measurements will be presented and discussed. T2 - NRC-9 CY - Helsinki, Finland DA - 29.08.2016 KW - Synchrotron KW - BAMline KW - Archaeometry PY - 2016 AN - OPUS4-38767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shabanov, Sergej V. A1 - Gornushkin, Igor B. T1 - Anions in laser-induced plasmas N2 - The equation of state for plasmas containing negative atomic and molecular ions (anions) is modeled. The model is based on the assumption that all ionization processes and chemical reactions are at local thermal equilibrium and the Coulomb interaction in the plasma is described by the Debye–Hu¨ckel theory. In particular, the equation of state is obtained for plasmas containing the elements Ca, Cl, C, Si, N, and Ar. The equilibrium reaction constants are calculated using the latest experimental and ab initio data of spectroscopic constants for the molecules CaCl2, CaCl, Cl2, N2, C2, Si2 , CN, SiN, SiC, and their positive and negative ions. The model is applied to laserinduced plasmas (LIPs) by including the equation of state into a fluid dynamic numerical model based on the Navier–Stokes equations describing an expansion of LIP plumes into an ambient gas as a reactive viscous flow with radiative losses. In particular, the formation of anions Cl-, C-, Si-, Cl2, Si2, C2 , CN-, SiC-, and SiN- in LIPs is investigated in detail. KW - Plasma modeling KW - Plasma KW - LIBS PY - 2016 DO - https://doi.org/10.1007/s00339-016-0175-8 VL - 2016 SP - Article Number: 676 PB - Applied Physics A, Springer AN - OPUS4-38771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Plasma fundamentals and diagnostics N2 - Short 4-hour course on plasma physics and plasma diagnostics T2 - January 8-13, Winter Plasma Conference CY - Tucson, USA DA - 08.01.2016 KW - PLasma physics KW - Plasma diagnostics PY - 2016 AN - OPUS4-38772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling chemical reactions in laser induced plasmas N2 - Under the assumption of local thermal equilibrium, a numerical algorithm is proposed to find the equation of state for laser-induced plasmas (LIPs) in which chemical reactions are permitted in addition to ionization processes. The Coulomb interaction in plasma is accounted for by the Debye–Hückel method. The algorithm is used to calculate the equation of state for LIPs containing carbon, silicon, calcium, chlorine, nitrogen, and argon. The equilibrium reaction constants are calculated using the latest experimental and ab initio data of spectroscopic constants for the molecules N2, C2, Si2, CN, Cl2, SiN, SiC, CaCl, CaCl2 and their positive and (if existed) negative ions. The algorithm is incorporated into a fluid dynamic numerical model based on the Navier–Stokes equations describing an expansion of LIP plumes into an ambient gas. The dynamics of LIP plumes obtained by the ablation of SiC, CaCl2, solid silicon, or solid carbon in an ambient gas containing N2 and Ar is simulated to study formation of molecules and molecular ions. A particular attention is paid to formation of anions Cl−, Cl2−, Si2−, C2−, CN−, and SiN− in LIPs. T2 - Winter Plasma Conference, January 8-13 2016 CY - Tucson, USA DA - 08.01.2016 KW - Plasma KW - Plasma modeling PY - 2016 AN - OPUS4-38774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosner, M. T1 - Intercomparison of delta26Mg Values in Mg Isotope RMs and Standards N2 - Accurate measurements of stable isotope abundance ratio variations are often reported using artifact based delta-scales, which rely on suitable isotopic reference materials (iRM) for their realization. For example, variations in the 26Mg/24Mg isotope abundance ratio in natural systems are typically reported as delta26Mg values that represents the relative difference between the 26Mg/24Mg ratio measured in a sample relative to its measurement preferably in an iRM. In the past, such delta26Mg measurements were referenced to NIST SRM 980, the initial zero of the delta26Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. It was then replaced by a Mg solution (DSM3), the new zero of the delta26Mg scale. A potential replacement iRM for DSM3 has been developed, ERM-AE143. This iRM has also been measured for its absolute isotope amount ratios1,2 making it traceable to the SI. The results of an delta26Mg intercomparison experiment include the Mg iRMs SRM 980, IRMM-009, ERM-AE143, AE144, AE145 standards DSM3 and Cambridge-1. The intercomparison involved 5 expert laboratories, consisting of 3 national metrological institutes (BAM, NIST, PTB) and 2 scientific research laboratories (GFZ Potsdam, UBremen). The iRMs were measured relative to AE143 and cover a range of ≈5 ‰ in delta26Mg. IRMM-009 has the lowest delta26Mg value while DSM3 has the highest, spanning a range in values that covers natural Mg isotope variations. The 2SD reproducibilities of the individual values from the different laboratories range from 0.02 to 0.26 ‰. The mean delta26Mg values, calculated from the laboratory means however show 2SD reproducibilities varing between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for delta26Mg determinations. 1 JAAS, 2015, 31,179; 2JAAS, 2016, 31, 1440 T2 - Goldschmidt Conference 2017 CY - Paris, France DA - 13.08.2017 KW - Magnesium delta scale KW - Isotope reference material KW - Intercalibration PY - 2017 AN - OPUS4-43995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruhe, L. A1 - Ickert, Stefanie A1 - Hochkirch, U. A1 - Hofmann, J. A1 - Beck, S. A1 - Thomale, J. A1 - Linscheid, M. W. T1 - Comprehensive molecular characterization of a cisplatin-specific monoclonal antibody N2 - Despite their immense and rapidly increasing importance as analytical tools or therapeutic drugs, the detailed structural features of particular monoclonal antibodies are widely unknown. Here, an antibody already in use for diagnostic purposes and for molecular dosimetry studies in cancer therapy with very high affinity and specificity for cisplatin-induced DNA modifications was studied extensively. The molecular structure and modifications as well as the antigen specificity were investigated mainly by mass spectrometry. Using nano electrospray ionization mass spectrometry, it was possible to characterize the antibody in its native state. Tandem-MS experiments not only revealed specific fragments but also gave information on the molecular structure. The detailed primary structure was further elucidated by proteolytic treatment with a selection of enzymes and high resolution tandem-MS. The data were validated by comparison with known antibody sequences. Then, the complex glycan structures bound to the antibody were characterized in all detail. The Fc-bound oligosaccharides were released enzymatically and studied by matrix-assisted laser desorption/ionization mass spectrometry. Overall 16 different major glycan structures were identified. The binding specificity of the antibody was investigated by applying synthetic single and double stranded DNA oligomers harboring distinct Pt adducts. The antibody− antigen complexes were analyzed by mass spectrometry under native conditions. The stability of the complex with double stranded DNA was also investigated. KW - Antibody KW - Native MS KW - Cisplatin KW - PTM PY - 2017 DO - https://doi.org/10.1021/acs.molpharmaceut.7b00575 SN - 1543-8384 SN - 1543-8392 VL - 14 IS - 12 SP - 4454 EP - 4461 AN - OPUS4-43997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruhe, L. A1 - Ickert, Stefanie A1 - Beck, S. A1 - Linscheid, M. W. T1 - A new strategy for metal labeling of glycan structures in antibodies N2 - Quantitative analysis of complex proteins is a challenging task in modern bioanalytical chemistry. Commonly available isotope labels are still suffering from limitations and drawbacks, whereas new metal labels open numerous possibilities in mass spectrometric analyses. In this work, we have developed a newmetal labeling strategy to tag glycan structures of proteins, more particularly antibodies. The oligosaccharide glycans were selectively trimmed to the last N-acetylglucosamine to which an artificial azide containing galactose residue was bound. This azide can be used for subsequent cycloaddition of an alkyne. Therefore, we developed a lanthanide-containing macrocyclic reagent to selectively connect to this azido galactose. In summary, the glycan structures of an antibody can be labeled with a metal functionality using this approach. Furthermore, the functionality of the antibodies can be fully maintained by labeling the Fc glycans instead of using labeling reagents that target amino or thiol groups. This approach enables the possibility of using elemental, besides molecular mass spectrometry, for quantitative analyses or imaging experiments of antibodies in complex biological samples. KW - Antibody KW - Metal labeling KW - Glycans KW - DOTA KW - Lanthanide PY - 2018 DO - https://doi.org/10.1007/s00216-017-0683-1 SN - 1618-2650 SN - 1618-2642 VL - 410 IS - 1 SP - 21 EP - 25 PB - Springer AN - OPUS4-44000 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Zscherpel, Uwe A1 - Ewert, Uwe ED - Russo, Paolo T1 - Handbook of X-ray imaging: Physics and technology N2 - Industrial Radiology is used for volumetric inspection of industrial objects. By penetration of these objects (typically weldments, pipes or castings) with X-ray or Gamma radiation the 3D-volume is projected onto a 2D image detector. The X-ray film is the oldest radiographic image detector and still in wide use in industry. The industrial X-ray film systems used today differ from these used in medicine. Medical film systems are described well in the literature, but industrial film systems not. So we start with a description of the properties and standards for industrial film systems. The requirements on image quality are defined by several standards and can be verified with different image quality indicators (IQIs). They describe the ability of the human being to detect small and low contrast indications in a noisy image background. The essential parameters for digital industrial radiology are described. Since about 30 years electronic image detectors are gradually replacing the industrial film. These detectors are based on storage phosphor imaging plates in combination with Laser scanners (“Computed Radiography”, CR) or a variety of different digital detector arrays (DDA). Typical applications of CR and DDAs are discussed as well as new possibilities by digital image processing, which is enabled by the computer based image handling, processing and analysis. KW - Industrial radiology KW - Industrial radiography KW - NDT films KW - Computed radiography KW - Digital detector arrays PY - 2018 SN - 978-1-4987-4152-1 SP - Chapter 30, 595 EP - 617 PB - CRC Press CY - Boca Raton, FL, USA AN - OPUS4-44026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Progress Talk 3 / Investigating the dimensions of core|shell nanoparticles using scanning transmission X-ray microscopy (STXM) N2 - This presentation deals with the progress between month twelve and nineteen of my PhD thesis. I prepared it, in order to update my supervisor Prof. Kemnitz and my colleagues from the department of chemistry at the Humboldt-Universität zu Berlin (HU). T2 - Working Group Meeting of Prof. Erhard Kemnitz CY - Humboldt-Universität zu Berlin (HU), Germany DA - 30.01.2018 KW - Core-shell nanoparticles KW - Metrology KW - PS KW - PTFE KW - Polymers KW - SEM KW - STXM PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-43981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reuther, R. T1 - A new tiered analytical approach and e-Tool for material classification to support the implementation of the EU Nano-Definition N2 - The EC recommendation for the definition of nanomaterial [2011/696/EU] requires the quantitative size determination of constituent particles in samples down to 1 nm. Accordingly, a material is a nanomaterial if 50 % or more of the particles are in the size range 1-100 nm. The fact that engineered nanomaterials already exist in many industrial and consumer products challenges the development of measurement methods to reliably identify, characterize and quantify their occurrence as substance and in various matrices. The EU FP7 NanoDefine project [www.nanodefine.eu] has addressed this challenge by developing a robust, readily implementable and cost-effective measurement strategy to obtain quantitative particle size distributions and to distinguish between nano and non-nano materials according to the EU definition. Based on a comprehensive evaluation of existing methodologies and intra- and inter-lab comparisons, validated measurement methods and instrument calibration procedures have been established to reliably measure the size of particles within 1-100 nm, and beyond, including different shapes, coatings and chemical compositions in industrial materials and consumer products. Case studies prove their applicability for various sectors, including food, pigments and cosmetics. Main outcome is the establishment of an integrated tiered approach including rapid screening (tier 1) and confirmatory methods (tier 2), and a user manual to guide end-users, such as manufacturers, in selecting appropriate methods. Another main product is the “NanoDefiner” e-Tool allowing the standardised / semi-automated selection of appropriate methods for material classification according to the EU definition. Results also contribute to standardization efforts, such as CEN TC 352 or ISO TC 229. T2 - EuroNanoForum 2017 CY - Valletta, Malta DA - 21.06.2017 KW - Nanomaterial classification KW - Nanoparticles KW - EC definition of nanomaterial KW - Tiered approach PY - 2017 UR - http://euronanoforum2017.eu/ AN - OPUS4-43993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Swaraj, Sufal T1 - Core-shell nanoparticles investigated with scanning transmission X-ray microscopy N2 - A scanning transmission x-ray microscopy (STXM) based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core-shell nanoparticles which exhibit a strong x-ray absorption contrast and a sharp interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less x-ray beam induced damage of the sample is achieved by recording STXM images only at two predetermined energies of maximum absorption contrast instead of recording a stack of images across the whole absorption edge. A model core-shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, investigated at the HERMES beamline is presented for demonstration. This STXM based methodology yields particle dimensions in good agreement with the scanning electron microscopy (SEM) results (deviation equal or less than 10%). Extension of this methodology to core-shell nanoparticles with inorganic core and organic shell will also be presented and the challenges encountered will be highlighted. T2 - 13th SOLEIL Users' Meeting CY - Saint-Aubin, France DA - 18.01.2018 KW - STXM KW - SEM KW - PTFE KW - PS KW - Core-shell nanoparticles KW - Polymers PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-43883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Nehls, Irene T1 - Volatile hydrocarbons in contaminated soil: Robustness of fractional quantification using headspace gas chromatography-mass-spectrometry N2 - Fuel contamination of soils display complex and variable hydrocarbon mixtures with different volatility and toxicity characteristics. A recently suggested headspace procedure for the structure-based quantification of volatile hydrocarbons is evaluated regarding repeatability, reproducibility, and practical robustness. Three aliphatic and three aromatic fractions covering the boiling range between 69 and 216°C were defined as summation parameters by their respective equivalent carbon number ranges. A standard mixture of 35 aliphatic and aromatic hydrocarbons was used for calibration on basis of selected mass fragments specific for the aliphatics and aromatics, respectively. Two standard soils were fortified with the standard mixture or different fuels, respectively, and submitted to the analytical procedure. Limit of detection (LOD) and limit of quantification (LOQ) were for all fractions lower than 0.1 and 0.3 mg/kg, respectively. Analyte recovery was linear up to between 20 and 110 mg hydrocarbons/kg soil depending on the fraction. Hydrocarbon recovery ranged between 80% and 110% depending on the fraction and the repeatability was typically better than 10%. Finally, the impact of extraction solvent variation, column solid-phase polarity, and alternative summation of fractions were investigated. The procedure was applied to liner samples taken from a site contaminated with aviation fuel and its practicability is discussed. KW - Gasoline KW - Contaminated site KW - Equivalent carbon number KW - Fuel KW - Static headspace PY - 2018 DO - https://doi.org/10.1080/15320383.2018.1418287 SN - 1532-0383 SN - 1549-7887 VL - 27 IS - 1 SP - 1 EP - 12 PB - Taylor & Francis AN - OPUS4-43889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, R. T1 - SEM or TEM for the characterization of nanoparticles? N2 - Scanning Electron Microscopy (SEM) or Transmission Electron Microscopy (TEM) ? This is a question, nowadays discussed in EM labs of research and industry involved in the characterization and metrology of nanoparticles. The Scanning principle is adapted to TEM, the Transmission mode is adapted to Ultra High Resolution SEM. Can modern SEM replace TEM, reach atomic resolution even without Cs corrector or nm lateral resolution for energydispersive X-ray spectroscopy (EDX)? Due to the development of a New Cold Field Emission (NCFE) electron source Hitachi SEMs SU9000 and SU8200 can deliver routinely sub-nm image resolution and EDX mappings at very high count rates and a lateral EDX resolution of a few nm. A TiO2 sample provided by BAM was analysed at 30kV using low kV STEM – simultaneously with the Through-the-lens (TTL) SE detector, the Bright Field transmitted and Dark Field transmitted signals. By this method a pixel precise information of the particles surface using SE, its chemical nature using DF-STEM and its crystalline structure using Bright Field signal is given in one 40sec scan. The advantage of this observation mode compared to Ultra Low Voltage imaging is outlined. T2 - Microscopy Conference 2017 CY - Lausanne, Switzerland DA - 21.08.2017 KW - SEM KW - TEM KW - Nanoparticles PY - 2017 UR - http://www.mc2017.ch/ AN - OPUS4-43890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Czarnecki, Sebastian A1 - Bertin, Annabelle T1 - Hybrid silicon-based organic/inorganic block copolymers with sol-gel active moieties: Synthetic advances, self-assembly and applications in biomedicine and material science N2 - Abstract: Hybrid silicon-based organic/inorganic (multi)block copolymers are promising polymeric precursors to create robust nano-objects and nanomaterials due to their sol–gel active moieties via self-assembly in solution or in bulk. Such nano-objects and nanomaterials have great potential in bio-medicine as nanocarriers or scaffolds for bone regeneration as well as in materials science as Pickering emulsifiers, pho- tonic crystals or coatings/films with antibiofouling, antibac- terial or water- and oil-repellent properties. Thus, this Review outlines recent synthetic efforts in the preparation of these hybrid inorganic/organic block copolymers, gives an overview of their self-assembled structures and finally presents recent examples of their use in the biomedical field and material science. KW - Organic/inorganic block copolymer KW - Robust nano objects KW - Self-assembly KW - Synthesis KW - Biomedical application KW - Material science PY - 2018 DO - https://doi.org/10.1002/chem.201705286 SN - 1521-3765 SN - 0947-6539 VL - 24 IS - 14 SP - 3354 EP - 3373 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-43953 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Preliminary work item (PWI) 23131 on standardization of ellipsometry N2 - The paper addresses the PRELIMINARY WORK ITEM (PWI) 23131 ON STANDARDIZATION OF ELLIPSOMETRY and the following points are discussed in more detail: Historical background of ellipsometry, Technical/industrial importance of ellipsometry and Standardization activities on ellipsometry. T2 - ISO TC 107 and JWG 4 meeting CY - Levi, Finland DA - 23.01.2018 KW - Standardization KW - Ellipsometrie KW - Modelling KW - Accreditation PY - 2018 AN - OPUS4-43959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Hahn, Marc Benjamin T1 - Quantifizierung der Schädigung von DNA in wässriger Lösung unter direkter Elektronenbestrahlung N2 - Bei der Behandlung von Krebs wird Strahlentherapie zur Zerstörung von Tumorzellen eingesetzt. Der zugrunde liegende Wirkmechanismus ist die durch ionisierende Strahlung verursachte Schädigung an Biomolekülen. Dabei kommt den Schädigungsprozessen an DNA aufgrund ihrer zentralen Rolle in Mutation und Zelltod eine besondere Bedeutung zu. Durch den hohen Wasseranteil in menschlichen Zellen findet ein Großteil der inelastischen Streuprozesse an Wassermolekülen statt und führt zur deren Radiolyse. Die so entstehenden Radiolyseprodukte sind für einen Großteil des Schadens an DNA verantwortlich. Ein detailliertes Verständnis der zugrunde liegenden molekularen Interaktion ist die Voraussetzung um effizientere Therapien zu entwickeln. Ziel dieser Arbeit ist es, die Schädigung von DNA durch ionisierende Strahlung in Abhängigkeit der inelastischen Streuevents und des Energieeintrags innerhalb des biologisch relevanten mikroskopischen Treffervolumens zu quantifizieren. Die Bestrahlungen müssen dazu in Flüssigkeit, unter Berücksichtigung der chemischen Umgebung durchgeführt werden, welche die indirekten Schäden vermittelt. Deshalb wurde eine neuartige Kombination aus Experiment und Monte- Carlo-Simulationen entworfen und angewandt. Um Elektronenbestrahlung flüssiger Lösungen innerhalb eines Rasterelektronenmikroskops zu ermöglichen, wurde ein Probenhalter mit einer für Elektronen durchlässigen Nanomembran entwickelt. So können Bestrahlungen an DNA, Proteinen, und Zellen bei verschiedenen pH-Werten, Salzkonzentrationen oder in Anwesenheit von Kosoluten durchgeführt werden. Für ein Modellsystem aus Plasmid-DNA in Wasser wurde damit die mittlere letale Dosis aus der Kombination der experimentellen Daten, Partikelstreusimulationen (Geant4-DNA) und Diffusionsberechnungen zu D1/2 = 1.7 ± 0.3 Gy bestimmt. Aus der Konvolution der Plasmidpositionen mit dem durch Elektronenstreusimulationen bestimmten ortsaufgelösten Energieeintrag wurde dessen Häufigkeitsverteilung im Targetvolumen der Plasmide sowie der mittlere mikroskopische letale Energieeintrag berechnet als E1/2 = 6 ± 4 eV . Es wurde gefolgert, dass weniger als zwei Ionisationsprozesse im sensitiven Targetvolumen der DNA im Mittel zu einem Einzelstrangbruch führen. Das für mikrodosimetrische Modellierungen wichtige Verhältnis von Einzelstrangbrüchen (SSB) zu Doppelstrangbrüchen (DSB) wurde als SSB : DSB = 12 : 1 bestimmt. Die vorgestellte Methode zur Bestimmung mikroskopischer Schaden-Dosis Relationen wurde auf weitere Klassen von Bestrahlungsexperimenten verallgemeinert. Dadurch ist die Methode unabhängig von der verwandten Primärstrahlung, der Probengeometrie und den Diffusionseigenschaften der untersuchten Moleküle anwendbar. So wird eine Vergleichbarkeit experimenteller Systeme mit inhomogenen Energieverteilungen erreicht, die bei ausschließlicher Betrachtung makroskopischer, gemittelter Größen nicht gegeben ist. Des weiteren wurden die Strahlenschutzfunktionen des kompatiblen Soluts Ectoine und sein Einfluss auf Wasser und Biomoleküle untersucht. Mittels Ramanspektroskopie wurde ein kon-zentrationsabhängiger Anstieg des Anteils der Kollektivmoden des Wassers der OH-Streckschwingungen und dessen Unabhängigkeit von der Natriumchloridkonzentration beobachtet. Molekulardynamik-Simulationen zeigten, dass die zwitterionischen Eigenschaften zur Bildung einer half-chair Konformation Ectoines führen. Die Wasserstoffbrückenbindungen in der ersten Hydrationshülle sind signifikant stabiler und besitzen höhere Lebensdauern als das Bulk-Wasser. Bestrahlung von DNA in Anwesenheit von 1 M Ectoine führt zu einer Erhöhung der Überlebensrate um den Faktor 1,41. Die Schutzfunktion wurde auf die Erhöhung des Streuquerschnitts niederenergetischer Elektronen an den akustischen Vibrationsmoden des Wasser durch Ectoine und seine Wirkung als OH-Radikalfänger zurückgeführt. Dies wurde mittels Ramanspektroskopie und Elektronenspinresonanzmessungen (ESR) nachgewiesen. N2 - To cure cancer radiation therapy is used to kill tumor cells. It is based on radiation induced damage to biomolecules. Especially DNA damage is of key interest due to its central role in apoptosis and mutation. Because of the high amount of water in biological tissue, most of the damage is caused by the secondary particles produced by the inelastic scattering of ionizing radiation and water. A detailed understanding of the underlying molecular processes under physiological conditions is the prerequisite to develop more efficient therapies. Goal of this work is to quantify the DNA damage caused by ionizing radiation in dependence of the inelastic scattering events and the energy deposit within the microscopic target volume of biological relevance. The irradiations have to be performed in liquid, under consideration of the chemical environment. Therefore, a new combination of experiment and Monte-Carlo simulations was developed and tested. To make it possible to irradiate liquids with electrons within scanning electron microscopes a new sample holder was constructed incorporating an electron transparent nanomembrane. It makes it possible to irradiate DNA, proteins or cells at different pH, salinity and in the presence of cosolutes. The median lethal dose for a model system of plasmid DNA and water was determined by the combination of experimental data, particle scattering simulations (Geant4-DNA) and Diffusion calculations as D1/2 = 1.7 ± 0.3 Gy. From the convolution of plasmid positions and the spatially resolved energy deposit, as determined by electron scattering simulations, the histogram of the energy deposit within the target volume of the plasmids and the microscopic median lethal energy deposit was calculated as E1/2 = 6 ± 4 eV . It could be deduced that on average less than two ionization events are sufficient to cause a single-strand-break. The relation of single- strand-breaks (SSB) to double-strand-breaks (DSB), which is of importance for microdosimetric modeling, was determined as SSB : DSB = 12 : 1. The presented method for the determination of microscopic dose-damage relations was further extended to be applicable for general irradiation experiments. It becomes independent of the type of primary radiation used, the experimental geometry, and the diffusional properties of the molecules under investigation. This way different experimental systems with varying, inhomogeneous energy deposit characteristics become comparable with each other, which is not possible when only macroscopic averaged values are taken into account. In addition, the radiation protection properties of the compatible solute ectoine, as well as ist influence on the water properties and biomolecules were investigated. Raman spectroscopy revealed a concentration dependent increase of the collective water modes in the OH-stretching region, which was found to be independent of the sodium chloride concentration. Molecular dynamic simulations showed that the zwitterionic properties of ectoine lead to its half-chair conformation. The hydrogen bonds in the first hydration shell are more stable and have an increased lifetime compared to the bulk water. Irradiation experiments with DNA in the presence of 1 M ectoine revealed an increase of the survival rate by a factor of 1.41 as compared to the absence of ectoine. The protective properties of ectoine result from the increase of the inelastic scattering probabilities of low energy electrons at the acoustic vibrational modes of water and its properties as OH-radical scavenger. This was shown by Raman spectroscopy and electron paramagnetic resonance measurements (EPR). KW - DNA KW - Radiation KW - Radiation damage KW - Dosimetry KW - Microdosimetry KW - DNA damage KW - DNA radiation damage KW - Low energy electrons KW - Electron irradiation KW - Hydroxyl radicals KW - Ectoine KW - Ectoine protein interaction KW - Ectoine DNA interaction KW - Ectoine radiation protection KW - Ectoine salt KW - Cancer therapy KW - Radiation therapy KW - Ectoin PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:188-fudissthesis000000106497-4 UR - http://www.diss.fu-berlin.de/diss/receive/FUDISS_thesis_000000106497 SP - 1 EP - 108 CY - Berlin AN - OPUS4-44510 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Titschack, J. A1 - Baum, D. A1 - Matsuyama, K. A1 - Boos, K. A1 - Färber, C. A1 - Kahl, W.-A. A1 - Ehrig, Karsten A1 - Meinel, Dietmar A1 - Soriano, C. A1 - Stock, S.R. T1 - Ambient occlusion – A powerful algorithm to segment shell and skeletal intrapores in computed tomography data N2 - During the last decades, X-ray (micro-)computed tomography has gained increasing attention for the description of porous skeletal and shell structures of various organism groups. However, their quantitative analysis is often hampered by the difficulty to discriminate cavities and pores within the object from the surrounding region. Herein, we test the ambient occlusion (AO) algorithm and newly implemented optimisations for the segmentation of cavities (implemented in the software Amira). The segmentation accuracy is evaluated as a function of (i) changes in the ray length input variable, and (ii) the usage of AO (scalar) field and other AO-derived (scalar) fields. The results clearly indicate that the AO field itself outperforms all other AO-derived fields in terms of segmentation accuracy and robustness against variations in the ray length input variable. The newly implemented optimisations improved the AO field-based segmentation only slightly, while the segmentations based on the AOderived fields improved considerably. Additionally, we evaluated the potential of the AO field and AO-derived fields for the separation and classification of cavities as well as skeletal structures by comparing them with commonly used distance-map-based segmentations. For this, we tested the zooid separation within a bryozoan colony, the stereom classification of an ophiuroid tooth, the separation of bioerosion traces within a marble block and the calice (central cavity)-pore separation within a dendrophyllid coral. The obtained results clearly indicate that the ideal input field depends on the three-dimensional morphology of the object of interest. The segmentations based on the AO-derived fields often provided cavity separations and skeleton classifications that were superior to or impossible to obtain with commonly used distance-map-based segmentations. The combined usage of various AO-derived fields by supervised or unsupervised segmentation algorithms might provide a promising target for future research to further improve the results for this kind of high-end data segmentation and classification. Furthermore, the application of the developed segmentation algorithm is not restricted to X-ray (micro-)computed tomographic data but may potentially be useful for the segmentation of 3D volume data from other sources. KW - Micro-computed tomography KW - Pore segmentation KW - Skeletal classification KW - Image analysis PY - 2018 DO - https://doi.org/10.1016/j.cageo.2018.03.007 SN - 0098-3004 SN - 1873-7803 VL - 115 SP - 75 EP - 87 PB - Elsevier Ltd. AN - OPUS4-44511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul A1 - Müller, C. A1 - Kauss, N. A1 - Halle, T. T1 - Einfluss der Wärmebehandlung auf Mikrostruktur und Korrosionsverhalten kohlenstoffhaltiger nichtrostender Stähle N2 - Das Korrosionsverhalten von kohlenstoffhaltigen martensitischen nichtrostenden Stählen variiert in Abhängigkeit der Wärmebehandlung (WB) und der damit eingestellten Mikrostruktur deutlich stärker als bei kohlenstoffarmen ferritischen und austenitischen nichtrostenden Stählen. Bei erhöhtem Kohlenstoffgehalt bestimmt die diffusionsgesteuerte Bildung und Auflösung von Chromkarbiden die Verteilung von Chrom und Kohlenstoff im Gefüge. Bisher lag der Fokus von Forschungsarbeiten zum Einfluss der WB auf dem Anlassen im allgemein bekannten Sensibilisierungsbereich dieser Werkstoffgruppe zwischen 200 °C und 700 °C und der dort auftretenden Chromverarmung. Mit der gezielten WB des X46Cr13 (1.4034) wird gezeigt, dass Temperatur und Dauer beim Austenitisieren sowie die anschließende Abkühlung beim Härten das Korrosionsverhalten schon vor dem Anlassen signifikant beeinflussen. Auf der Basis von thermodynamischen Berechnungen wurden definierte WB ausgewählt, um gezielt unterschiedliche Volumengehalte von Chromkarbiden im Gefüge und somit auch unterschiedliche Chrom bzw. Kohlenstoffgehalte im Mischkristall zu erzeugen. Anschließend wurden die resultierenden Gefügezustände hinsichtlich Chromkarbidanteil und Härte verglichen und das Korrosionsverhalten mit der elektrochemisch potentiodynamischen Reaktivierung (EPR) sowie durch einen Schnelltest mit der KorroPad-Prüfung untersucht. Dabei konnte ein direkter Zusammenhang zwischen WB, Mikrostrukturänderungen und Korrosionsverhalten festgestellt werden. Mit steigender Austenitisierungstemperatur wird der Anteil an Chromkarbiden reduziert und der Kohlenstoff- und Chromgehalt der Matrix erhöht, bis eine vollständige Auflösung der Chromkarbide gegeben und die chemische Nennzusammensetzung der Legierung im Mischkristall erreicht ist. In der direkten Folge wird die Ausbildung der für nichtrostende Stähle charakteristischen Passivschicht erleichtert und das Lochkorrosionsverhalten verbessert. Die Abkühlrate hat neben den Austenitisierungsparametern ebenfalls einen großen Einfluss auf das Korrosionsverhalten. So führt eine langsame Abkühlung an Luft zu einer Chromverarmung im Gefüge, die eine deutlich erhöhte Lochkorrosionsanfälligkeit zur Folge hat. In Abhängigkeit der WB von kohlenstoffhaltigen nichtrostenden Stählen können Mikrostruktur, Härte und Korrosionsbeständigkeit in einem weiten Bereich variieren. T2 - 20. Werkstofftechnisches Kolloquium CY - Chemnitz, Germany DA - 14.03.2018 KW - Nichtrostender Stahl KW - Wärmebehandlung KW - EPR KW - KorroPad KW - Korrosionsbeständigkeit KW - ThermoCalc KW - Sensibilisierung KW - Martensitischer nichtrostender Stahl KW - Passivschicht PY - 2018 SN - 978-3-00-058901-0 SN - 1439-1597 VL - 72 SP - 711 EP - 720 PB - Eigenverlag CY - Chemnitz AN - OPUS4-44559 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Bestimmung des mikroskopischen Energiedeposits an DNA in komplexen Geometrien N2 - Mikrodosimetrie zum Einsatz in der Charakterisierung von per 3D Druck erstellen medizinischen Röntgenphantomen. T2 - Charite PhantomX CY - Charite Campus Berlin, Germany DA - 21.03.2018 KW - Dosimetrie KW - Phantome KW - Strahlentherapie KW - Computertomographie KW - Medizintechnik KW - Geant4 KW - Monte-Carlo Simulationen PY - 2018 AN - OPUS4-44564 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Combination of Monte-Carlo simulations and experimental results to determine the microscopic energy depoit at DNA N2 - The quantification of radiation induced damage to DNA in aqueous en- vironment is of fundamental interest for dosimetry and its application in radiation-therapy and protection. We present a combined experi- mental and simulational approach to quantify and compare radiation induced damage to biomolecules in liquid environment for a wide range of primary radiation sources e. g. photons, electrons or ions and tar- gets, such as DNA, proteins or cells.[1] To show its viability, we will apply this method to an experimentally challenging systems, the di- rect irradiation of plasmid DNA (pUC19) in water with electrons as primary particles. Here we combine Geant4 electron-scattering simula- tions with calculations concerning the diffusion and convection induced movement of the biomolecules, within a coarse-grained model of the irradiated liquid. Additionally a microscopic target model for the plas- mid DNA based on the relation of lineal energy and radiation quality is used to calculate the effective target volume. T2 - DPG-Frühjahrstagung der Sektion Kondensierte Materie gemeinsam mit der EPS CY - Berlin, Germany DA - 11.03.2018 KW - DNA KW - Radiation damage KW - Dosimetry KW - Microdosimetry KW - Low energy electrons KW - Hydroxyl radicals KW - Monte-Carlo simulation KW - Geant4 KW - Electron scattering KW - Target volume KW - DNA damage KW - DNA radiation damage PY - 2018 AN - OPUS4-44565 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - DNA strand break yields by OH-radicals, low energy electrons and prehydrated electrons N2 - Universität Berlin Radiation damage to biomolecules such as DNA, is the reason to treat cancer via radiation therapy. The understanding of the molecular processes and the quantification of the underlying damaging mechanisms is necessary to develope more efficient irradiation protocols for cancer therapy. Thereby damage to DNA is of key interest due to its central role in reproduction and mutation. Due to the high amount of water in biological tissue, most of the damage is caused by the secondary particles which are produced by the interaction of ionizing radiation with water. Thereby a multitude of species are produced, e.g. kinetic low energy electrons, prehydrated electrons, OH-radicals and ions. The quantification of the contribution to DNA damage by the various species is of interest. Here we present an experimental approach to disentangle their relative DNA strand break yields. Plasmid DNA (pUC19 ) is irradiated in water with electrons under the presence of different scavengers. The presented preliminary results reveal the relative contributions of OH-radicals, low energy electrons and prehydrated electrons and their DNA single and double strand break yields. T2 - DPG-Frühjahrstagung der Sektion Kondensierte Materie gemeinsam mit der EPS CY - Berlin, Germany DA - 11.03.2018 KW - DNA KW - Radiation damage KW - Dosimetry KW - Low energy electrons KW - Hydroxyl radicals KW - Geant4 KW - Prehydrated electrons KW - Scavenger KW - Radiation damage to DNA KW - Plasmid DNA KW - Strand breaks KW - Double strand breaks KW - Single strand breaks PY - 2018 AN - OPUS4-44566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scherz, Franziska A1 - Krop, U. A1 - Monks, K. A1 - Weller, Michael G. T1 - Antikörperreinigung mit Glasmonolithen - Vereinfachung von Affinitätstrennungen mit HPLC-Systemen N2 - Druckstabile Glasmonolithen ermöglichen eine schnelle und unkomplizierte Reinigung von Antikörpern, z.B. aus Serum oder Zellkulturüberständen. Die sehr gute Regenerierbarkeit lässt eine lange Lebensdauer der Säulen erwarten, was die Kosten pro Probe niedrig hält. KW - Borosilicatglas KW - Immunglobuline KW - IgG KW - Serum KW - Plasma KW - Protein A KW - Protein G KW - Affinitätschromatographie KW - Agarose KW - Carrier-Material KW - Stationäre Phase KW - Immobilisierung KW - Highspeed KW - Trennung KW - Reinigung KW - Downstream Processing PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-445330 UR - http://www.git-labor.de/forschung/materialien/antikoerperreinigung-mit-glasmonolithen SN - 0016-3538 VL - 62 IS - 3 SP - 24 EP - 25 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-44533 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Detjens, Marc A1 - Banach, Ulrich T1 - Messunsicherheiten von Feuchtesensoren N2 - Inhalt dieses Seminarbeitrags sind Hygrometer und Kenngrößen der Hygrometrie, Anforderungen an ein Prüflabor sowie die Bestimmung der Messunsicherheit bei der Prüfung von Feuchtesensoren wie auch Prüfung auf signifikante Abweichungen. T2 - 308. PTB-Seminar Berechnung der Messunsicherheit – Empfehlungen für die Praxis CY - Berlin, Germany DA - 15.03.2018 KW - Messunsicherheit KW - Feuchtesensor KW - Prüflabor PY - 2018 UR - https://www.ptb.de/cms/fileadmin/internet/fachabteilungen/abteilung_8/8.4_mathematische_modellierung/308._PTB_Seminar/Vortraege/4PraxisII/Messunsicherheiten_von_Feuchtesensoren.pdf AN - OPUS4-44546 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Plasma Fundamentals and Diagnostics N2 - This course will provide an introduction to plasma diagnostic techniques. The major focus of the course will be on the discussions of the practical procedures as well as the underlying physical principles for the measurements of plasma fundamental characteristics (e.g., temperatures, thermodynamic properties, and electron number density). Particular emphasis will be placed on inductively coupled plasma–atomic emission spectrometry, but other analytical plasmas will also be used as examples when appropriate. Selected examples on how one can manipulate the operating conditions of the plasma source, based on the results of plasma diagnostic measurements, to improve its performance used for spectrochemical analysis will also be covered. Topics to be covered include thermal equilibrium, line profiles, temperatures, electron densities, excitation processes, microreactions, pump and probe diagnostics, tomography, temporal and spatial resolution. Basis of plasma computer modeling will be presented. T2 - Winter Plasma Conference CY - Amelia Island, FL, USA DA - 08.01.2018 KW - Plasma diagnostics KW - Plasma physics PY - 2018 AN - OPUS4-44497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling chemical reactions in laser-induced plasmas at local thermodynamic equilibrium N2 - Laser induced plasma (LIP) is a dynamic, short living event which presents significant difficulty for modeling. In this report, a collisional-dominated chemical model developed earlier* is expanded by the inclusion of a new method for calculation of chemical reactions. The model consists of the coupled Navier-Stokes, state, radiative transfer, material transport, and chemical equations. The latter are written in terms of atomic and molecular partition functions rather than reaction rates. Typically, a solution of such the system of chemical equations is difficult for the entire range of plasma temperatures and densities because reaction constants may vary by hundreds orders of magnitude owing to extreme plasma conditions. No numerical solver of non-linear systems of equations handles this situation with ease. We resolve the problem by using a hierarchical approach. First, we rank the reactions according to their ascendancy. Second, we exploit either the contraction or Newton-Raphson algorithms to solve the system of chemical equations. We illustrate the approach by performing a series of calculations for reacting species Si, C, N, Ca, Cl and their molecules in laser induced plasmas. T2 - Winter Plasma Conference CY - Amelia Island, FL, USA DA - 08.01.2018 KW - Plasma physics KW - Plasma diagnostics PY - 2018 AN - OPUS4-44499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina T1 - Dynamics of nanoscopically confined PVME in thin films of an asymmetric PVME/PS blend N2 - In recent years, substantial efforts have been devoted to investigating nanoscopic confinement of polymers, and its effect on glassy dynamics. Broadband Dielectric Spectroscopy (BDS) was used to study the dynamics of ultra-thin films of PVME/PS 50/50 wt% blend, employing a novel nano-structured capacitor sample arrangement. The investigated system shows a complex dynamic behavior. First, an α-relaxation, related to a bulk-like layer was found. Second, an α’-relaxation was observed, characteristic for dynamically asymmetric blends, where the out of equilibrium dynamics is attributed to weakly-cooperative PVME segments relaxing within a frozen environment of PS segments. Thirdly, for thinnest films, an Arrhenius-like process was dominant in the dielectric spectra, indicating localized fluctuations of the segments. Relaxation rates of this process resembled that of the degenerated α-relaxation of the adsorbed layer, found for pure PVME, thus it was assigned accordingly. For thinnest films, this process undergoes a further confinement, due to the topological constraints, introduced by PS. Such multiple confinement effect has not been reported for ultra-thin films of polymer blends, before this study. T2 - Spring Meeting of German Physical Society CY - Berlin, Germany DA - 12.03.2018 KW - Thin polymeric films PY - 2018 AN - OPUS4-44502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Boehm, Rainer T1 - Kegel-Phased-Array für die schnelle Ultraschallprüfung von längsgebohrten Eisenbahnradsatzwellen N2 - Durch die Verwendung von Ultraschall - Phased Arrays lässt sich in vielen Fällen sowohl die Prüfgeschwindigkeit als auch die Zuverlässigkeit der Prüfung erhöhen. Für die Prüfung von Eisenbahnradsatzwellen ist die Phased Arraytechnik schon verbreitet, jedoch vor allem für die Prüfung von Vollwellen. Die Prüfung von längsgebohrten Eisenbahnrad¬satzwellen erfolgt typischerweise mit einer Anzahl von konventionellen Prüfköpfen, die rotierend durch die Längsbohrung bewegt werden. Dabei werden weder die Achsen und Räder noch die Bremsscheiben demontiert. Ein neuer Ansatz für die Prüftechnik ist die Verwendung eines rotations-symmetrischen kegelförmigen Phased Arrays in Tauchtechnik. Die Abtastung in Umfangs-richtung erfolgt durch elektronische Rotation des Schallfeldes, was viel höhere Prüfge-schwindigkeiten ermöglicht und den mechanischen Aufwand des Prüfsystems erheblich reduziert. Nur die Bewegung des Sensorsystems in axialer Richtung innerhalb der Bohrung erfolgt mechanisch. Senkrecht zur Bauteilachse kann das Schallbündel durch die Phased Arraysteuerung in Umfangsrichtung exakt ausgerichtet und im Abstand der Prüfbereiche nahe der Außenoberfläche der Radsatzwelle fokussiert werden. Die Konstruktionsparameter des Kegelarrays wurden speziell optimiert zum Auffinden von rissartigen Querfehlern in und in der Nähe der äußeren Oberfläche von längsgebohrten Eisenbahnradsatzwellen von Hochgeschwindigkeitszügen. Die Fehlerfläche liegt dabei in der Querschnittsfläche des Bauteils. Im Beitrag werden der Prototyp des neuen Sensorsystems und erste Prüfergebnisse gezeigt. Die Arbeiten wurden durchgeführt im Rahmen des Europäischen Projektes “Whole Life Rail Axle Assessment and Improvement Using Ultrasonic Phased array and Corrosion Inspection Systems“ (RAAI). T2 - 10. Fachtagung ZfP im Eisenbahnwesen, 13. – 15. März 2018 CY - Wittenberge, Germany DA - 13.03.2018 KW - Eisenbahn KW - Ultraschallprüfung KW - Radsatzwellen KW - Phased Array KW - Kegelarray KW - Rotationsscanner PY - 2018 AN - OPUS4-44523 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moldenhauer, Laura A1 - Helmerich, Rosemarie A1 - Köppe, E. A1 - Wittmann, J. ED - Cosmi, F. T1 - Experimental modeling approach for determining the moisture damping exponent of a Bluetooth Low Energy signal in moist building material N2 - The presented development of a damping model is a research component of an experimental feasibility study about moisture in building materials measured with Bluetooth® Low Energy (BLE) signals. This study may be part of a structural health monitoring aiming on early damage detection in the built infrastructure and is increasingly focusing on wireless sensor Network technology. It is investigated, how the Received Signal Strength Indicator (RSSI) of a BLE signal, transmitted from the BLE-module embedded in building materials with changing moisture content is damped. The BLE-module communicates with a mobile Smart Device as tablet or mobile phone via 2.45 GHz-ISMfrequency band where water dipoles start to oscillate. If the BLE-signal transfers through a moist material, the moisture Content influences the RSS-Indicator. The damping model demonstrates this damping effect on RSSI by the abstraction of the reality observed in a real system. T2 - 34th Danube Adria Symposium CY - Trieste, Italy DA - 19.09.2017 KW - Moisture damping coefficient, KW - Buliding materials KW - Bluetooth Low Energy KW - RSSI KW - Experimental approach PY - 2017 SN - 978-88-8303-863-1 DO - https://doi.org/https://www.openstarts.units.it/handle/10077/14834 SP - 141 EP - 142 CY - Trieste, Italy AN - OPUS4-44528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Coelho Lima, Isabela A1 - Grohmann, Maria A1 - Niederleithinger, Ernst T1 - Alternative imaging conditions for reverse-time migration N2 - Poster on the evaluation of several imaging conditions for reverse time migration, applied to ultrasonic echo data, tested with synthetic (simulated) dat and real data from a polyamide model. T2 - Jahrestagung der Deutschen geophysikalischen Gesellschaft CY - Leoben, Austria DA - 12.2.2018 KW - Ultrasound KW - Reverse time migration KW - Imaging condition KW - Concrete KW - Polyamide PY - 2018 AN - OPUS4-44583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian T1 - Additiv gefertigte Kunststoffteile: Untersuchung der Beständigkeit durch künstliche Bewitterung und zerstörungsfreie Charakterisierung N2 - Es wird ein Verfahren zur Charakterisierung der Beständigkeit und Langzeitstabilität von additiv gefertigten Kunststoff-Bauteilen vorgestellt. Dabei sollen die Prüfkörper über 2000 Stunden künstlich bewittert und währenddessen die Änderungen der Eigenschaften der Bauteile zerstörungsfrei untersucht werden. Die Erkenntnisse dienen für die Entwicklung einer Strategie für eine Qualitätskontrolle von additiv gefertigten Kunststoffteilen. T2 - 47. Jahrestagung der GUS CY - Stutensee-Blankenloch, Germany DA - 21.03.2018 KW - Additive Fertigung KW - Additive manufacturing KW - Beständigkeit von Kunststoffen KW - Zerstörungsfreie Prüfung KW - Künstliche Bewitterung PY - 2018 AN - OPUS4-44589 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramos, I. I. T1 - Automated bead-based immunoassay for the determination of carbamazepine in wastewater N2 - The improvement of immunoanalytical methods for the determination of pharmaceuticals in wastewaters is a crucial yet challenging endeavor. In this work, the development of an automated miniaturized ELISA based on micro-Bead Injection Spectroscopy (μ-BIS) [1] for the determination of carbamazepine, a widely employed anti-epileptic drug and emergent pollutant [2], was pursued. The experimental workflow comprised the offline functionalization of Sepharose beads with specific anti-CBZ antibodies via affinity immobilization using protein G, and 3 online steps inside the microfluidic analyzer lab-on-valve (LOV): I) packing of the bead column into the detection unit; II) sequential percolation of sample and a CBZ competitor- labeled with horseradish peroxidase (tracer) through the bead column; and III) on-column colorimetric detection employing the enzyme substrate 3,3’,5,5’-tetramethylbenzidine. After each analysis, the bead column was discarded, and the flow cell was washed before receiving new beads. The elimination of manual washing steps is a novel feature compared to batch-wise ELISA, making the method less error-prone and therefore more robust. The replacement of the solid support prevents memory effects and cross-contamination between runs. The use of microparticles as solid support for the molecular recognition elements accounts for high area-to-volume ratios, and low molecular diffusion distances. For that reason, time-to-result was reduced from several hours to less than 10 min. The consumption of reagents was also very low. For instance, only ca. 200 μg of solid support and 900 ng of anti-CBZ antibody were required per determination. At last, the versatility of the LOV platform offers the possibility of adapting the assay to other relevant pharmaceuticals and anthropogenic markers in water. Acknowledgements: Inês I. Ramos thanks FCT (Fundação para a Ciência e a Tecnologia) and POPH (Programa Operacional Potencial Humano) for her grant (SFRH/BD/97540/2013). This work received financial support from the European Union (FEDER funds POCI/01/0145/FEDER/007265) and National Funds (FCT/MEC - Ministério da Educação e Ciência) under the Partnership Agreement PT2020 UID/QUI/50006/2013. Financial support from Deutscher Akademischer Austauschdienst and from Fundação das Universidades Portuguesas under the protocol CRUP-DAAD (Ações Integradas Luso-Alemãs nºE-20/16) is also acknowledged. [1] Gutzman, Y.; Carrol, A. D. Analyst 2006, 131, 809. [2] Murray, K. E.; Thomas, S. M.; Bodour, A. A. Environ. Pollut. 2010, 158, 3462. T2 - ANALÍTICA – 2018 CY - Porto, Portugal DA - 26.03.2018 KW - Lab-on-valve KW - Emerging pollutants KW - Immunoassay KW - Automation PY - 2018 AN - OPUS4-44592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica T1 - Nanocrystals as labeling reagents for bioimaging of clinical cell assays N2 - Imaging of elemental distributions in single cell assays as well as tissue sections can be performed by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). This powerful technique offers precise spatially resolved measurements at the trace and ultratrace level and has been established as an excellent tool to answer analytical, biological and biomedical questions. To date, imaging mass cytometry is already able to simultaneously detect up to 40 cellular targets due to conjugation of isotopically pure lanthanides to affinity binders, e.g. antibodies. To further enhance the ability of multiparametric analysis to more than 100 analytes at once, we investigated lanthanide nanocrystals as new, highly sensitive metal tags for identification of targets in clinical cell assays and tissue samples. Multiparametric analysis will be possible by encoding the lanthanide composition of nanocrystals associated to the affinity binders. Nanocrystals showed remarkable potential for sensitive detection in MS due to high stability and signal amplification compared to e.g. polymer tags, carrying fewer metal atoms. Synthesis of functionalized lanthanide nanocrystals for further bioconjugation was performed with high reproducibility and monodisperse size distribution. For proof of principle, the uptake and distribution of these nanocrystals within the monolayered cell line A549 were investigated by mapping the intensities at subcellular resolution using LA-ICP-MS. It could be shown, that the cells were efficiently labeled with the nanocrystals and mostly accumulate near the nucleus. Additionally, the bioconjugation of the nanocrystals to antibodies and particularly the preservation of the antibody specificity was investigated using Dot Blot experiments. All in all, the results imply high sensitivity and the possibility of multiparametric analysis by doting various lanthanides into the nanocrystals. T2 - ESAS & CANAS 2018 CY - Berlin, Germany DA - 20.03.2018 KW - Bioimaging KW - Nanoparticle KW - Immuno-assay KW - Lanthanide PY - 2018 AN - OPUS4-44593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ickert, Stefanie T1 - Vacuum ultraviolet light as a new Tandem MS method N2 - Tandem MS techniques are widely used for both, structure and sequence elucidation of biopolymers. Thereby, fragmentation activation is realized by various methods, for example with lasers or collisions with neutral gases. In this study, we present a new Tandem MS system using a commercially available vacuum ultraviolet lamp. On the one hand, this approach provides efficient fragmentation in both ionization modes, positive as well as negative. On the other hand, it enables an additional previously not achieved post ionization of the fragments. While the first results in atypical fragment patterns and, thus provides orthogonal information, the second is crucial especially to identify low abundant ions. T2 - European Mass Spectrometry Conference CY - Saarbrücken, Germany DA - 10.03.2018 KW - Tandem MS KW - Vacuum Ultraviolet PY - 2018 AN - OPUS4-44484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gawek, Marcel T1 - Growth Kinetics and Molecular Mobility of Irreversibly Adsorbed Layers in Thin Polymer Films N2 - In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is expected to form. These adsorbed layers have shown great potential for technological applications. However, their growth kinetics and molecular dynamics are still not fully understood. This is partially due to the hard accessibility of these layers in thin films. Here, the irreversibly adsorbed layers of homopolymer thin films are revealed by solvent-leaching experiments. First, the growth kinetics of these layers is investigated as a function of annealing times and original film thickness. The thickness, topography and quality of the adsorbed layer is controlled with Atomic Force Microscopy (AFM). Secondly, the molecular mobility of the adsorbed layer is investigated with Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor is employed to measure the adsorbed layers with a free surface layer. The results are quantitatively compared and discussed with respect to recently published work. T2 - Meeting of the American Physical Society CY - Los Angeles, CA, USA DA - 05.03.2018 KW - Thin polymeric films KW - Adsorbed layer PY - 2018 AN - OPUS4-44488 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gawek, Marcel T1 - Growth Kinetics and Molecular Mobility of Irreversibly Adsorbed Layers in Thin Polymer Films N2 - In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is expected to form. These adsorbed layers have shown great potential for technological applications. However, their growth kinetics and molecular dynamics are still not fully understood. This is partially due to the hard accessibility of these layers in thin films. Here, the irreversibly adsorbed layers of homopolymer thin films are revealed by solvent-leaching experiments. First, the growth kinetics of these layers is investigated as a function of annealing times and original film thickness. The thickness, topography and quality of the adsorbed layer is controlled with Atomic Force Microscopy (AFM). Secondly, the molecular mobility of the adsorbed layer is investigated with Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor is employed to measure the adsorbed layers with a free surface layer. The results are quantitatively compared and discussed with respect to recently published work. T2 - Spring Meeting of German Physical Society CY - Berlin, Germany DA - 12.03.2018 KW - Thin polymeric films KW - Dielectric spectroscopy PY - 2018 AN - OPUS4-44489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bierstedt, Andreas T1 - Laser-spark ionization mass spectrometry N2 - A versatile ionization scheme for atmospheric pressure MS is presented. It is based on a quasi-continuous laser-induced plasma (LIP), generated by a 26 kHz pulsed DPSS-laser, which is ignited in front of the MS inlet. Analytes are determined with different sampling regimes, comprising either an ambient desorption/ionization mechanism, a liquid-phase or gas-phase sample introduction. The MS signal closely resembles the ionization behavior of APCI-like plasma-based sources, such as DBD or DART. Though LIPs are known to efficiently atomize/ionize any sample material, mass spectra of intact molecular ions are recorded, exhibiting low fragment-ion content. To understand this contradictory behavior, the plasma properties are investigated that lead to the formation of molecular ions. Comprehensive studies include optical emission spectroscopy, shadowgraph imaging and mass spectrometry diagnostics. The results show that the ionization of analyte does not occur in the plasma itself, but in the cold adjacent gas layer. The pulsed character of LIPs induces an expanding shockwave, which concentrically expands around the plasma core and sweeps the molecules toward the plasma edges, where they are ionized either directly by the self-emission of the hot core or via interaction with secondary reactants. However, this unidirectional transport causes a rarefaction inside the plasma center, which leads to a decrease in plasma intensity and number density. Thus, a restoration of the former gaseous medium by other dynamically equilibrated diffusion processes would be favorable. Besides gas replenishing, we demonstrate the beneficial use of an acoustical standing wave inside an ultrasonic resonator on the performance of the LIP. T2 - European Mass Spectrometry Conference 2018 CY - Saarbrücken, Germany DA - 11.03.2018 KW - Laser-spark ionization KW - Laser-induced plasma KW - Ambient mass spectrometry KW - DPSS laser PY - 2018 AN - OPUS4-44492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - van Wasen, Sebastian T1 - Airborne laser-spark for ambient desorption/ionization of liquids N2 - The development and enhancement of new ionization techniques for mass spectrometry often needs to be custom-tailored for specific sampling approaches. Here, a direct sampling ionization technique is presented for ambient mass spectrometry. Ambient mass spectrometry based techniques are typically used to analyze samples in their native states without sample pretreatment. This new design is based on a quasi-continuous airborne plasma which is ignited inside the particulate air via a focused laser irradiation. Desorption and ionization of the analyte molecules are achieved by the laser plasma without reaching the plasma. The ionization process is induced by interaction with nascent ionic fragments, electrons and ultraviolet photons in the plasma vicinity. Previously, this method was solely used for the characterization of solid and gaseous analytes. The sample introduction was occurred via thermal desorption and headspace analysis. This study focuses on the potential applicability of liquid samples. In comparison to previous approaches, the usage of liquid samples has an impact on the stability of typically used plasma of 532 nm. It was necessary to realize an alternative plasma using light of the fundamental wavelength of 1064 nm. That new plasma resulted in a significant more stable and bright plasma and the first laser plasma ionization spectrum was recorded for an analyte in the condensed phase with a mass spectrometer of type LCQ DecaXP. T2 - European Mass Spectrometry Conference 2018 CY - Saarbrücken, Germany DA - 11.03.2018 KW - Laser-spark KW - Laser-induced plasma KW - Ambient mass spectrometry KW - Ambient desorption/ionization KW - DPSS laser PY - 2018 AN - OPUS4-44493 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina T1 - Unexpected behavior of thin PVME/PS blend films investigated by specific heat spectroscopy N2 - The structure and molecular dynamics of thin polymer films are of topical interest of soft matter-physics. Commonly, spatial structural heterogeneities of 1D confined thin films (surface, bulk-like and adsorbed layer), are expected to alter the glassy dynamics, compared to the bulk. Here, Specific Heat Spectroscopy (SHS) was used, to investigate the glassy dynamics of thin films of an asymmetric miscible PVME/PS 25/75 wt% blend. SHS measurements showed a non-monotonous thickness dependence of the dynamic Tg, on the contrary to the previously investigated PVME/PS 50/50 wt%. For PVME/PS 25/75 wt% thin films (> 30 nm), due to the presence of PVME-rich adsorbed and surface layers, the bulk-like layer experienced a thickness dependent increase of PS concentration. This led to a systematic increase of dynamic Tg. Further decrease of the film thickness (< 30 nm), resulted in a decrease of dynamic Tg, ascribed to the influence of the surface layer, which has a high molecular mobility. This is the first study, which shows deviations of dynamic Tg of thin films, compared to the bulk, resulting from the counterbalance of the free surface and adsorbed layer. T2 - Spring Meeting of German Physical Society CY - Berlin, Germany DA - 12.03.2018 KW - Thin polymeric films PY - 2018 AN - OPUS4-44494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Die Zentrifuge als universelles Prüfsystem für Beanspruchungen auf Zug und Druck N2 - Mit der Zentrifugentechnologie ist seit einigen Jahren ein neuartiges Mehr-Proben-Prüf-verfahren auf dem Markt etabliert, welches die klassische Zugprüfung in den Trommelrotor einer Tischzentrifuge überträgt. In der Beanspruchung auf Zug ist die Prüfung der Verbundfestigkeit mittels CAT-Technologie (centrifugal adhesion testing) an der BAM seit 2017 nach DIN EN ISO/IEC 17025 akkreditiert, wobei die Verbundfestigkeit von Klebungen direkt bestimmt wird und in Abhängigkeit von den Versagensformen Rückschlüsse auf die Klebfestigkeit von Klebstoffen/Klebebändern oder die Haftfestigkeit von Beschichtungen gezogen werden können. T2 - 13. ThGOT Thementage Grenz- und Oberflächentechnik und 11. Thüringer Biomaterial-Kolloquium CY - Zeulenroda, Germany DA - 13.03.2018 KW - Zentrifugentechnologie KW - Haftfestigkeit KW - Härteprüfung KW - Mehr-Proben-Prüfung KW - Beanspruchung auf Zug und Druck PY - 2018 AN - OPUS4-44570 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hielscher, Stefan A1 - Beck, Uwe A1 - Lange, Thorid A1 - Grunwald, Daniel A1 - Stockmann, Jörg M. A1 - Lerche, D. A1 - Rietz, U. T1 - Die Zentrifuge als universelles Prüfsystem für Beanspruchungen auf Zug und Druck N2 - Mit der Zentrifugentechnologie ist seit einigen Jahren ein neuartiges Mehr-Proben-Prüf-verfahren auf dem Markt etabliert, welches die klassische Zugprüfung in den Trommelrotor einer Tischzentrifuge überträgt. In der Beanspruchung auf Zug ist die Prüfung der Verbundfestigkeit seit 2017 nach DIN EN ISO/IEC 17025 akkreditiert, wobei die Verbundfestigkeit von Klebungen direkt bestimmt wird und in Abhängigkeit von den Versagensformen Rückschlüsse auf die Klebfestigkeit von Klebstoffen/Klebebändern oder die Haftfestigkeit von Beschichtungen gezogen werden können. Bei der zerstörenden Beanspruchung auf Zug ist zu beachten, dass es sich bei der Verbundfestigkeit um eine Systemeigenschaft handelt, d.h. nicht nur die chemischen und topografischen Oberflächeneigenschaften, sondern auch die plasto-elastischen Volumeneigenschaften des Klebstoffes und der Fügeteile haben Einfluss auf die ermittelten Kennwerte. Dabei ist eine qualitative Bestimmung der Versagensformen und Bruchbilder nach DIN EN ISO 10365 zwingend erforderlich, um eine Aussage über die Art des Versagens treffen zu können. Mit der Erweiterung der Zentrifugentechnologie um Beanspruchungen auf Druck wurde dann der Nachweis erbracht, dass auch die klassische Härteprüfung in einer Zentrifuge als Mehr-Proben-Prüfung durchgeführt werden kann. Im Verbundvorhaben QUO VADIS PLUS werden derzeit invasive Beanspruchungen auf Druck zur Bestimmung der Härte von Materialien, der Kompressibilität von Metallschäumen sowie der Kompaktierbarkeit von Pulvern untersucht, was das Anwendungspotential der Zentrifugentechnologie nochmals erweitert. Dazu gehören auch kombinierte Beanspruchungen wie Zug-Scher- und Druck-Scher-Prüfungen. Die Verbundfestigkeit von CFK-Platten in Abhängigkeit der Beanspruchungsart (Zug vs. Zug-Scher) bzw. der Faserorientierung (0°, 45°, 90°), die Klebfestigkeit von Klebstoffen bzw. Klebebändern auf unterschiedlichen Fügeteilwerkstoffen in Abhängigkeit von der Vorbehandlung, die Haftfestigkeit optischer Schichten auf Kunststoffen, die Bestimmung der Vickers-, Brinell- bzw. Kugeldruck-Härte sowie die Kompressibilität von metallischen Schäumen und Federn werden als ausgewählte Beispiele diskutiert. T2 - 13. ThGOT Thementage Grenz- und Oberflächentechnik und 11. Thüringer Biomaterial-Kolloquium CY - Zeulenroda, Germany DA - 13.03.2018 KW - Zentrifugentechnologie KW - Haftfestigkeit KW - Härteprüfung KW - Mehr-Proben-Prüfung KW - Beanspruchung auf Zug und Druck PY - 2018 SN - 978-3-00-058187-8 SP - 1 EP - 5 CY - Jena AN - OPUS4-44572 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donskyi, Ievgen A1 - Drüke, M. A1 - Silberreis, K. A1 - Lauster, D. A1 - Ludwig, K. A1 - Kühne, C. A1 - Unger, Wolfgang A1 - Böttcher, C. A1 - Herrmann, A. A1 - Dernedde, J. A1 - Adeli, M. A1 - Haag, R. T1 - Interactions of fullerene-polyglycerol sulfates at viral and cellular interfaces N2 - Understanding the mechanism of interactions of nanomaterials at biointerfaces is a crucial issue to develop new antimicrobial vectors. In this work, a series of water-soluble fullerene-polyglycerol sulfates (FPS) with different fullerene/polymer weight ratios and varying numbers of polyglycerol sulfate branches are synthesized, characterized, and their interactions with two distinct surfaces displaying proteins involved in target cell recognition are investigated. The combination of polyanionic branches with a solvent exposed variable hydrophobic core in FPS proves to be superior to analogs possessing only one of these features in preventing interaction of vesicular Stomatitis virus coat glycoprotein (VSV-G) with baby hamster kidney cells serving as a model of host cell. Interference with L-selectin-ligand binding is dominated by the negative charge, which is studied by two assays: a competitive surface plasmon resonance (SPR)-based inhibition assay and the leukocyte cell (NALM-6) rolling on ligands under flow conditions. Due to possible intrinsic hydrophobic and electrostatic effects of synthesized compounds, pico- to nanomolar half maximal inhibitory concentrations (IC50) are achieved. With their highly antiviral and anti-inflammatory properties, together with good biocompatibility, FPS are promising candidates for the future development towards biomedical applications. KW - Fullerene-Polyglycerol Sulfates KW - Fullerene KW - Biointerfaces KW - XPS PY - 2018 DO - https://doi.org/10.1002/smll.201800189 SN - 1613-6829 SN - 1613-6810 VL - 14 IS - 17 SP - 1800189, 1 EP - 7 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-44573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Untersuchung der akustischen Eigenschaften von Plasmalautsprechern auf Basis einer dielektrischen gehemmten Oberflächenentladung (SDBD) N2 - Analog zu Blitz und Donner können elektrische Entladungen innerhalb eines Gasvolumens als akustische Quellen agieren und haben daher eine starke Verbreitung als diagnostische Methode (bspw. in der Raumakustik und bei der Ortung von Teilentladungen). Diese auf dem Prinzip der Thermoakustik beruhende Möglichkeit der Schallerzeugung und die damit verbundenen physikalischen Wechselwirkungen machen die Notwendigkeit einer mechanisch ausgelenkten Membran überflüssig. Dabei wird dem hochfrequenten Träger das Nutzsignal aufgeprägt, welches eine Volumenänderung des umliegenden Gases um seinen Ruhezustand verursacht. Durch die somit hervorgerufene zyklische thermische Wechselwirkung mit dem umliegenden Gasgemisch bedarf es daher ebenfalls keiner akustischen Anpassung. In den vorgestellten Ergebnissen wurde das Übertragungsverhalten eines Oberflächenplasmas (SDBD, surface dielectric barrier discharge) untersucht. Als Maß für den Wirkungsgrad und das Übertragungsverhalten des Aktuators wurden Klirrfaktor- und THD-Messungen und unter Variation der Eingangsleistungen durchgeführt. Durch die positiven akustischen Eigenschaften eröffnen sich neue Applikationen für den Einsatz von Plasmahochtönern wie bspw. zerstörungsfreie Werkstoffprüfung von Verbundsystemen und Klebeverbindungen im Automobilsektor oder im Bauwesen. T2 - DAGA - Jahrestagung für Akustik CY - Munich, Germany DA - 19.03.2018 KW - Atmospheric pressure plasma KW - Gas discharges KW - Surface dielectric barrier discharge KW - Plasma speaker PY - 2018 AN - OPUS4-44579 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Online Raman spectroscopy for the quantitative evaluation of a Ralstonia cultivation N2 - Spectroscopic methods possess important advantages for the observation of bioprocesses: they are robust, gain many data within a short time scale, and allow for the measurement of multiple relevant information at the same time. Next to Near-infrared spectroscopy, Raman spectroscopy is increasingly applied as a powerful online tool to monitor bioprocesses. However, Raman spectra may be obscured by straylight, cosmic rays and fluorescence. To achieve the best performance, optimal conditions for spectral quality and stability should be pursued. This comprises not only the choice of highly-sensitive equipment, but also the way of implementation into the process. Here we compared the potential of introducing a sterilized fiber optical Raman probe, and a flow-through cell into the bypass of a stirred tank reactor to monitor an autotrophic cultivation of Ralstonia eutropha where gasses are the energy and carbon sources. Raman spectra were continuously recorded over seven days and 22 samples were taken for the reference analytics of biomass, optical density, and protein. In addition, data for of phosphate and ammonium were available. The quantitative Evaluation of Raman spectra by Partial Least Squares Regression (PLSR) yielded comparable results for both approaches, however, there was a general trend of lower prediction errors with the immersion probe. The better performance of the non-contact optic may be either related to a more representative interaction of the measurement optics with the probe or simply to the absence of probe-fouling, which was observed with the immersion optic in the interstice between window and metal frame. T2 - 5th BioProScale Symposium CY - Berlin, Germany DA - 20.03.2018 KW - Raman spectroscopy KW - Bioprocess KW - Chemometrics PY - 2018 UR - www.bioproscale-conference.org AN - OPUS4-44580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Ellipsometric imaging of low-contrast surface modifications and depolarization contrast imaging (DCI) of particulate accumulations N2 - Imaging of surfaces regarding topographical, morphological, micro-structural, and chemical features is a key requirement for quality control for the identification of contaminated, degraded, damaged or deliberately modified surface areas vs. clean, virgin, undamaged or unmodified regions. As optical functions may represent any of these changes on the micro- and nano-scale, imaging ellipsometry (IE) is the technique of choice using either intensity, phase, or/and amplitude contrast for visualization of low-contrast surface modifications [1, 2]. Defects or surface and film features whether native or artificial, intended or unintended, avoidable or unavoidable as well as surface pattern are of interest for quality control. In contrast to microscopic techniques operated at normal incidence, ellipsometry as oblique-incidence technique provides improved contrast for vertically nano-scaled add-on or sub-off features such as ultra-thin transparent films, metallic island films, carbon-based thin films, laser modification or laser induced damage, dried stain, cleaning agent or polymeric residue. Two-sample reference techniques, i.e. referenced spectroscopic ellipsometry (RSE) may further increase sensitivity and decrease measurement time. In case of particulate accumulations depolarization contrast imaging (DCI) may improve the lateral resolution beyond the Abbe limit. This has been proven for silica spheres as reference in terms of single particles, particulate accumulations or particulate monolayers and layer stacks. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were used for reference measurements of particle diameter, particle height, or particulate layer/accumulation thickness. It has been shown that single silica particles of 250 nm in diameter, i.e. at least a factor of 4 better than the lateral resolution limit as of now, can be visualized on even substrates. However, the ellipsometric measurement of particle diameters of this size needs further efforts interpretation. T2 - Workshop Ellipsometry 2018 CY - Chemnitz, Germaný DA - 19.03.2018 KW - Low-contrast surface modifications KW - Particulate distributions KW - Imaging ellipsometry(IE) KW - Depolarization contrast imaging (DCI) PY - 2018 AN - OPUS4-44548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul T1 - KorroPad-Prüfung - Neue Anwendungen aus Industrie und Forschung N2 - Mit der KorroPad-Prüfung kann die Lochkorrosionsbeständigkeit nichtrostender Stähle auf sehr einfache, schnelle und kostengünstige Weise eingeschätzt werden. Das KorroPad ist damit für Hersteller, Verarbeiter und Anwender nichtrostender Stähle eine interessante Alternative zu zeitintensiven Langzeitversuchen und komplexen elektrochemischen Untersuchungsmethoden. Die prinzipiellen Funktionsweise der KorroPad-Prüfung wird im Vortrag beschrieben, um anschließend verschiedene Anwendungen aus Industrie und Forschung vorzustellen. Exemplarisch werden dazu die Bewertung von Schleif- und Passivierungsprozessen, die Qualitätskontrolle der Wärmebehandlung und Oberflächenbearbeitung von Schneidwaren vorgestellt. Mit der KorroPad-Prüfung lassen sich aber auch werkstoff- und gefügebedingte Einflüsse auf die Lochkorrosionsbeständigkeit gezielt untersuchen. Dies wird an Beispielen aus aktuellen Forschungsarbeiten dargestellt. T2 - Forschungsseminar des MDZWP e. V. CY - Magdeburg, Germany DA - 13.03.2018 KW - Korrosion KW - Nichtrostender Stahl KW - KorroPad KW - Wärmebehandlung KW - Korrosionsbeständigkeit KW - Lochkorrosion KW - Schneidwaren KW - Korrosionsprüfung PY - 2018 AN - OPUS4-44549 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul T1 - Visualisierung werkstoffbedingter Lochkorrosionsanfälligkeit durch die KorroPad-Prüfung N2 - Mit der KorroPad-Prüfung können lochkorrosionsanfällige Oberflächenbereiche einfach, schnell und kostengünstig nachgewiesen werden. Das KorroPad ist damit für Hersteller, Verarbeiter, Anwender und Forscher eine interessante Alternative zu zeitintensiven Auslagerungsversuchen und elektrochemischen Untersuchungsmethoden, die normalerweise bei der Charakterisierung nichtrostender Stähle zur Anwendung kommen. Mit der KorroPad-Prüfung können auch werkstoff- und gefügebedingte Einflussfaktoren sichtbar gemacht werden, die Lochkorrosionsanfälligkeit verursachen. Um dies zu veranschaulichen, wird die Nachweisgrenze des KorroPads an Referenzlegierungen mit abgestuftem Chromgehalt aufgezeigt. Darauf aufbauend wird dargestellt, wie die Sensibilisierung nichtrostender Stähle durch Chromverarmung mit einer gezielten Verschärfung der KorroPad-Prüfung nachgewiesen werden kann. T2 - 20. Werkstofftechnischen Kolloquium CY - Chemnitz, Germany DA - 14.03.2018 KW - Korrosion KW - Nichtrostender Stahl KW - KorroPad KW - Korrosionsschutz KW - Korrosionsbeständigkeit KW - Lochkorrosion KW - Passivschicht PY - 2018 AN - OPUS4-44550 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Olaf T1 - VOC-Emissions from thermoplastic filaments for 3-D-printing N2 - Summary: A screening test for potential emissions of volatile organic compounds (VOC) was run on different thermoplastic filaments used for 3D printing. The method of direct thermal desorption was used to simulate the high temperatures during the 3D printing process and to identify the main compounds emitted from the filaments. A large number of unexpected compounds were detected that might affect the user’s health and have an impact on indoor air chemistry. Introduction: The use of desktop 3D printers is increasing. Compared to other devices with known emissions, e.g. laser printers, there is still a lack of information on possible emissions of VOC and ultrafine particles during operation and the effect on indoor air quality. Most of the commercially available desktop 3D printers operate with a molten polymer deposition. For this process a solid thermoplastic filament is heated in an extrusion nozzle. Most filaments for desktop 3D printers use either acrylonitrile butadiene styrene (ABS) or polylactic acid (PLA) as filament. Alternatives are polyvinyl alcohol (PVA) or polycarbonate (PC). Method: Eight different thermoplastic filaments for 3D printers were analysed by direct thermal desorption followed by GC-MS identification of the emitted substances. Direct thermal desorption was done by desorbing 5 mg of the feedstock for 1 minute at a temperature of 210°C. This is an average temperature for 3D printing with thermoplastic filaments. Results and conclusions: The comparison of the 4 different filament groups showed the highest overall emissions from ABS, followed by PLA, PC and PVA. Filament ABS 2 emitted mainly SVOCs and triphenyl phosphate, the latter has the highest emission for a single compound from all evaluated filaments. Thermoplastic filaments are a new source of VOC emissions due to the high temperatures associated with 3D printing, which can reach up to 270°C. Some of the detected compounds like lactic acid, lactide and bisphenol A have never been described before in the indoor environment. Additionally some of the main substances could not be identified and some others might have the potential to affect the indoor air chemistry. The appearance of some newly detected compounds raises concerns about potential health effects for the users of 3D printers at home. T2 - 20th Conference | Odour and Emissions of Plastic Materials CY - Kassel, Germany DA - 20.03.2018 KW - VOC KW - Emissions KW - 3D printing KW - Thermoplastic filaments PY - 2018 AN - OPUS4-44551 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul T1 - Einfluss der Oberflächen-Nachbearbeitung auf die Korrosionsbeständigkeit von Schweißnähten N2 - Der nichtrostende Duplexstahl 1.4062 (X2CrNiN22-2) hat sich im Bauwesen als Werkstoffalternative zu den nichtrostenden Austeniten etabliert. Die Korrosionsbeständigkeit von Schweißverbindungen aus 1.4062 wird, neben dem Grundwerkstoff, dem Schweißzusatzwerkstoff und dem Schweißverfahren, auch sehr stark von der Oberflächennachbehandlung der Schweißnaht beeinflusst. Je nach zukünftigem Anwendungsbereich und geforderter Korrosionsbeständigkeit wird die Schweißnaht geschliffen, gebeizt, elektropoliert oder gestrahlt, um die beim Schweißen entstandenen Anlauffarben zu entfernen. Gestrahlte Oberfläche sind in der industriellen Praxis häufig anzutreffen, da sie deutlich einfacher und kostengünstiger herzustellen sind als gebeizte oder elektropolierte Oberflächen. Die Auswahl des Strahlmittels bestimmt auch die Prozesskosten, wobei das Strahlen mit Korund effektiver als das Strahlen mit Glasperlen ist. In den letzten Jahren wurden korrosionsanfällige Oberflächen bei nichtrostenden Stählen beobachtet, wenn diese mit Korund geschliffen wurden. Daher wird nun auch beim Strahlen kritisch hinterfragt, ob Korund als Strahlmittel die Korrosionsbeständigkeit verändert. Diese Fragestellung wird im Vortrag beantwortet indem geschliffene, gebeizte, mit Korund gestrahlte und mit Glasperlen gestrahlte Schweißverbindungen vergleichend untersucht werden. Die Ergebnisse der Untersuchungen von den Strahlmitteln und den gestrahlten Oberflächen werden mit den Ergebnissen der Salzsprühnebelprüfung, den kritischen Lochkorrosionspotentialen und der KorroPad-Prüfung korreliert. T2 - Sitzung des Ausschusses Marketing der Informationsstelle Edelstahl Rostfrei CY - Düsseldorf, Germany DA - 22.03.2018 KW - Korrosion KW - Nichtrostender Stahl KW - Korrosionsprüfung KW - Lochkorrosion KW - Strahlen KW - Oberflächenbearbeitung KW - Schweißen KW - KorroPad KW - Passivschicht KW - Duplexstahl PY - 2018 AN - OPUS4-44552 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul A1 - Kauss, N. T1 - Visualisierung werkstoffbedingter Lochkorrosionsanfälligkeit durch die KorroPad-Prüfung N2 - Mit der KorroPad-Prüfung können lochkorrosionsanfällige Oberflächenbereiche einfach, schnell und kostengünstig nachgewiesen werden. Das KorroPad ist damit für Hersteller, Verarbeiter, Anwender und Forscher eine interessante Alternative zu zeitintensiven Auslagerungsversuchen und elektrochemischen Untersuchungsmethoden, die normalerweise bei der Charakterisierung nichtrostender Stähle zur Anwendung kommen. Mit der KorroPad-Prüfung können auch werkstoff- und gefügebedingte Einflussfaktoren sichtbar gemacht werden, die Lochkorrosionsanfälligkeit verursachen. Um dies zu veranschaulichen, wird die Nachweisgrenze des KorroPads an Referenzlegierungen mit abgestuftem Chromgehalt aufgezeigt. Darauf aufbauend wird dargestellt, wie die Sensibilisierung nichtrostender Stähle durch Chromverarmung mit einer gezielten Verschärfung der KorroPad-Prüfung nachgewiesen werden kann. T2 - 20. Werkstofftechnisches Kolloquium CY - Chemnitz, Germany DA - 14.03.2018 KW - KorroPad KW - Korrosion KW - Nichtrostender Stahl KW - Lochkorrosion KW - Korrosionsbeständigkeit KW - Korrosionsschutz KW - Passivschicht PY - 2018 SN - 978-3-00-058901-0 SN - 1439-1597 VL - 72 SP - 67 EP - 73 PB - Eigenverlag CY - Chemnitz AN - OPUS4-44557 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Zhiyang A1 - Merk, V. A1 - Müller, Anja A1 - Unger, Wolfgang A1 - Kneipp, Janina T1 - Role of metal cations in plasmon-catalyzed oxidation: A case study of p-aminothiophenol dimerization N2 - The mechanism of the plasmon-catalyzed reaction of p-aminothiophenol (PATP) to 4,4′-dimercaptoazobenzene (DMAB) on the surface of metal nanoparticles has been discussed using data from surface-enhanced Raman scattering of DMAB. Oxides and hydroxides formed in a plasmon-catalyzed process were proposed to play a central role in the reaction. Here, we report DMAB formation on gold nanoparticles occurring in the presence of the metal cations Ag+, Au3+, Pt4+, and Hg2+. The experiments were carried out under conditions where formation of gold oxide or hydroxide from the nanoparticles can be excluded and at high pH where the formation of the corresponding oxidic species from the metal ions is favored. On the basis of our results, we conclude that, under these conditions, the selective oxidation of PATP to DMAB takes place via formation of a metal oxide from the ionic species in a plasmon-catalyzed process. By evidencing the necessity of the presence of the metal cations, the reported results underpin the importance of metal oxides in the reaction. KW - Metal ions KW - Plasmonic catalysis KW - p-aminothiophenol KW - 4,4'-dimercaptoazobenzene KW - Surface-enhanced Raman scattering PY - 2017 UR - http://pubs.acs.org/doi/abs/10.1021/acscatal.7b02700 DO - https://doi.org/10.1021/acscatal.7b02700 SN - 2155-5435 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. VL - 7 IS - 11 SP - 7803 EP - 7809 PB - American Chemical Society CY - Washington AN - OPUS4-43001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wachtendorf, Volker A1 - Barthel, Anne-Kathrin A1 - Geburtig, Anja A1 - Trubiroha, P. ED - Reichert, T. T1 - Low-Temperature Irradiation Experiments for PE, PA, and PC Matrices N2 - In this paper, we demonstrate the effects of radiation exposures of polymeric materials with UV-A 340 nm lamps (ISO 4892-3, Type 1A) at -10 °C in comparison to an irradiation at +50 °C using a Global UV Test 200 fluorescent lamp device from Weiss Umwelttechnik GmbH, which incorporates an active cooling appliance. While the effects at -10 °C actually are lower than at + 50°C their extent was clearly beyond expectations. T2 - 8th European Weathering Symposium CY - Vienna, Austria DA - 20.09.2017 KW - Artificial weathering KW - Irradiation KW - Low-temperature KW - Photo-oxidation KW - Polyamide KW - Polycarbonate KW - Polyethylene PY - 2017 SN - 978-3-9818507-1-0 VL - 18 SP - Paper 22, 319 EP - 329 PB - Thomas Würtz Grafik Design CY - Karlsruhe AN - OPUS4-42130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred T1 - Determination of lost paint layers by scanning electron microskopy N2 - The identification of external paint layers on medieval stained glass windows in Lincoln Cathedral is not only of interest for art historians but is also important for the development of conservation proposals. For the gradual reduction and removal of corrosion layers conservators have to take care to preserve any remaining paint layers which are hidden underneath these corrosion and weathering crusts. T2 - Aspects of Glass - Stained Glass - Art at the Glass Surface CY - Cambridge, Great Britain DA - 02.09.2017 KW - Medieval glass composition KW - SEM/EDX KW - Glass conservation PY - 2017 AN - OPUS4-42131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas T1 - Einfluss der Heterogenität von Beton auf Radarmessungen und deren mögliche Nutzen N2 - Der Einfluss der Heterogenität von Beton auf Radarmessungen im Rahmen einer zerstörungsfreien Prüfung von Stahlbetonbauwerken wird beschrieben und ein möglicher Nutzen für die Zerstörungsfreie Prüfung im Bauwesen wird aufgezeigt. T2 - 12. Georadar Rundtisch Gespräch 2017 CY - Aachen, Germany DA - 21.09.2017 KW - Radar KW - Beton KW - Heterogenität KW - Zerstörungsfreie Prüfung KW - Schwache Streuung PY - 2017 AN - OPUS4-42134 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stockmann, Jörg M. A1 - Hertwig, Andreas A1 - Beck, Uwe T1 - Visualization of low-contrast surface modifications: Thin films, printed pattern, laser-induced changes, imperfections, impurities, and degradation N2 - Visualization of surface modifications may be very challenging for coating/substrate systems of either almost identical optical constants, e.g. transparent films on substrates of the same material, or minor film thickness, substance quantity and affected area, e.g. ultra-thin or island films. Methods for visualization are optical microscopy (OM), imaging ellipsometry (IE), and referenced spectroscopic ellipsometry (RSE). Imaging ellipsometry operates at oblique incidence near Brewster angle of the bare, clean or unmodified substrate. In this configuration, reflected intensities are rather weak. However, the contrast to add-on and sub-off features may be superior. Referenced spectroscopic ellipsometry operates in a two-sample configuration but with much higher intensities. In many cases, both ellipsometric techniques reveal and visualize thin films, printed-pattern, laser-induced changes, and impurities better than optical microscopy. In particular for stratified homogeneous modifications, ellipsometric techniques give access to modelling and hence thickness determination. Modifications under investigation are polymer foil residue on silicon, laser-induced changes of ta-C:H coatings on 100Cr6 steel, imperfections of ta-C:H on thermal silicon oxide, degradation of glass, thin film tin oxide pattern on silicon, printed and dried pattern of liquids such as deionized water, cleaning agents, and dissolved silicone. © 2016 Elsevier B.V. All rights reserved. T2 - International Conference on Spectroscopic Ellipsometry (ICSE-7) CY - Berlin, Germany DA - 06.06.2016 KW - Optical microscopy (OM) KW - Imaging ellipsometry (IE) KW - Referenced spectroscopic ellipsometry (RSE) KW - Thin films KW - Impurities KW - Degradation PY - 2016 DO - https://doi.org/10.1016/j.apsusc.2016.10.145 SN - 0196-4332 VL - 2017 IS - 421 SP - 807 EP - 812 PB - Elsevier B.V. AN - OPUS4-42136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN T1 - Forschungsprogramm 2015 - 2017 N2 - Globalisierung und die beschleunigte technologische Entwicklung bringen heute für die Industrieländer Herausforderungen im Hinblick auf Wachstum, Beschäftigung und Strukturwandel mit sich, denen nur mit einer entsprechenden Innovationsdynamik und -dichte begegnet werden kann. Grundvoraussetzung hierfür ist eine leistungsfähige Forschung und Entwicklung ebenso wie Wissens- und Technologietransfer zur Umsetzung von Forschungsergebnissen in marktfähige Produkte und Dienstleistungen. Europa hat sich im Rahmen des Lissabon-Prozesses zum Ziel gesetzt, den Anteil der Forschungsausgaben am Bruttoinlandsprodukt auf 3 % zu steigern. Um die Forschungsinfrastruktur in der Bundesrepublik zu stärken und global wettbewerbsfähig zu bleiben, hat die Bundesregierung mit der Hightech-Strategie einen weiteren wichtigen Schritt zur Förderung des wissenschaftlich-technischen Fortschritts in Deutschland getan. Forschungsprogramme sind sowohl für Forschungseinrichtungen als auch für Mittelgeber ein wichtiges Instrument für die Darstellung und Steuerung ihrer Aktivitäten. Dies gilt auch für die Bundeseinrichtungen mit Forschungs- und Entwicklungsaufgaben, zu denen die Bundesanstalt für Materialforschung und -prüfung (BAM) zählt. Die BAM verfügt über einen klaren gesetzlichen Auftrag für die Sicherheit in Technik und Chemie. Ihre Forschung ist mit der Wahrnehmung öffentlicher Aufgaben verbunden. Das Forschungsprogramm zeigt Perspektiven im Bereich ihres Aufgabenfeldes sowie ihrer damit verbundenen Forschungsaktivitäten transparent und politisch nutzbar auf und dient darüber hinaus der Koordinierung der Ressortforschung. Das Forschungsprogramm der BAM wird alle zwei Jahre aktualisiert. Es gibt einen Überblick über die aktuellen und zukünftigen Forschungsthemen und die hierfür erforderlichen Rahmenbedingungen. PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-421401 SP - 1 EP - 40 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-42140 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Von der Antike in die Zukunft: Materialanalyse mit Synchrotronstrahlung N2 - Die Eigenschaften und die Verlässlichkeit von Materialien jeglicher Art sind seit jeher die Grundlagen der Technik einer Gesellschaft. Tiefgreifende Kenntnisse über sie sind deshalb eine Voraussetzung um neue Produkte zu entwickeln, Verlässlichkeit zu gewährleisten, oder aber auch, wie in der Archäometrie, Kenntnisse über die Vergangenheit zu gewinnen. Ein Schlüssel zum Verständnis ist das Wissen über die chemische Zusammensetzung und die Struktur von Materialien Die Analyse mit Synchrotronstrahlung bietet hierfür herausragende Werkzeuge an, die zerstörungsfrei und hochsensitiv sind. Mit Röntgenfluoreszenzanalyse kann die elementare Zusammensetzung in winzigen Proben bis auf μg/g bestimmt werden. Anwendungsbeispiele aus verschiedenen Themengebieten, aber besonders von archäologischen Fragestellungen wie z.B. dem Goldfund von Bernstorf werden im Vortrag vorgestellt. T2 - Berliner Industriegespräch CY - Berlin, Germany DA - 05.04.2017 KW - Gold KW - Synchrotron KW - XRF KW - BESSY KW - Archeometry KW - BAMline PY - 2017 AN - OPUS4-42979 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - News from the BAMline N2 - In this talk, the newest developments at the BAMline and examples of applications are presented. T2 - Seminar: STRAHLENPHYSIKALISCHE ANWENDUNGEN IN TECHNIK UND MEDIZIN CY - Vienna, Austria DA - 18.01.2017 KW - XANES KW - Synchrotron KW - XRF KW - BESSY PY - 2017 AN - OPUS4-42981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Prost, J. T1 - Trace element analysis of airborne particulate matter with TXRF and SR-TXRF-XANES N2 - Airborne particulate matter is a topic of growing interest. Particles with aerodynamic diameters less than 10 μm (PM 10) and especially the fine fraction below 2.5 μm (PM2.5) are of particular importance, as they can enter the human respiratory system and cause acute and chronic respiratory or cardiovascular diseases. The mass distribution of airborne particles in dependence of their diameters is well-known, but also the abundance and temporal variation of trace elements in air (mass concentrations down to the pg/m³ range) are crucial. These elements originate from various natural (abrasion, erosion) and anthropogenic sources (combustion, road traffic), which complicate the discrimination between harmless and toxic emissions. Some new methods of investigation are therefore needed and X-ray fluorescence spectroscopy has ascertained ist huge potential in this matter, thanks to the possibility to determine simultaneously, in a time-resolved manner, the mass concentrations of critical elements which can be considered as markers of a potential toxic source. A method for the quantitative Analysis of airborne particles directly collected on sample substrates (30 mm quartz reflectors and 1" Si wafers suited for total-reflection X-ray fluorescence analysis (TXRF) will be presented. Samplings were performed using a three- stage Dekati™ PM10 impactor (>10 μm, 2.5 to 10 μm and 1 to 2.5 μm) and a four-stage Sioutas Personal Cascade Impactor (>2.5 μm, 1 to 2.5 μm,0.5 to 1 μm and 0.25 to 0.5 μm) at indoor and outdoor sites at the Atominstitut (Vienna, Austria). Quantitative results of two outdoor test sampling campaigns (July 2016 and January 2017) will be presented and discussed. Low detection limits were assessed via TXRF and range from several 10 to several 100 pg/m³ depending on the element and particle size fraction. T2 - Denver X-ray Conference CY - Big Sky, Montana, USA DA - 31.07.2017 KW - XANES KW - Synchrotron KW - TXRF KW - BAMline PY - 2017 AN - OPUS4-42982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Improved traceability chain of nanoparticle size measurements N2 - The overall objective of project Improved traceability chain of nanoparticle size measurements is to improve the traceability chain for nanoparticle size measurements. The main impact will be achieved by manifold contributions to standard documents for CEN/TC 352 “Nanotechnologies”, which directly addresses the research needs of CEN, CENELEC and ETSI mandated by EC to develop standards for methods and reference materials to accurately measure the size and size distribution of nanoparticles. This will take place in collaboration with ISO/TC229 ‘Nanotechnologies’, ISO/TC24/SC4 ‘Particle characterization’ and ISO/TC201 ‘Surface analysis’/ SC9 ‘Scanning probe microscopy’. T2 - EMPIR 2017 Review Conference CY - Monaco DA - 9.11.2017 KW - Nanoparticles KW - Traceability KW - Electron micrsocopy KW - Size KW - Shape PY - 2017 AN - OPUS4-43019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Muelow-Stollin, Ulrike A1 - Lehnik-Habrink, Petra A1 - Kluge, Stephanie A1 - Bremser, Wolfram A1 - Piechotta, Christian T1 - Efficiency Evaluation of Extraction Methods for Analysis of OCPs and PCBs in Soils of Varying TOC N2 - Organochlorine pesticides and polychlorinated biphenyls are toxic, carcinogenic, and have a high potential for bioaccumulation. Due to their stability, they are still considered an environmental problem even though the use of most of them has been phased out several decades ago. Soil is a matrix which can retain these contaminants to a great extent. This ability is often associated with the total organic carbon content (TOC). In order to judge the pollution status of soil and to make monitoring data more easily comparable a simple, yet robust extraction method is needed. Agitation solid-liquid-extraction is well suited for this purpose. However, the influence of TOC on the analyte recovery has to be known. For the presented study, 12 organochlorine pesticides and 7 polychlorinated biphenyls were spiked into four model soils with organic carbon contents between 1.6% - 13.3%. The matrices were extracted using solid-liquid extraction between 45 minutes and 16 hours. For comparison, all soils were also extracted using pressurised liquid extraction and Soxhlet extraction. After clean-up the extracts were measured using a gas chromatography-mass spectrometry (GC-MS) system. Statistical analysis of the results implied that the TOC content of the soils did not have significant influence on the extraction efficiency. A longer solid-liquid extraction time did not necessarily increase analyte recovery: Extraction for one hour resulted in 88% recovery while 16 hour extraction led to 89%. Thus, the efficiency of all the methods was comparable for all model soils. Additional investigations regarding GC liner performance highlighted the need for isotopically labelled standards during the analysis of thermolabile pesticides. KW - POP KW - Soil organic matter KW - Solid-liquid-extraction KW - Pressurised liquid extraction PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-430238 DO - https://doi.org/10.4236/jep.2017.86045 SN - 2152-2219 VL - 08 IS - 06 SP - Article ID:77202, 693 EP - 713 PB - Scientific Research Publishing AN - OPUS4-43023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martynenko, Irina A1 - Litvin, A.P. A1 - Purcell-Milton, F. A1 - Baranov, A. V. A1 - Fedorov, A.V. A1 - Gun´ko, Y.K. T1 - Application of semiconductor quantum dots in bioimaging and biosensing N2 - In this review we present new concepts and recent progress in the application of semiconductur quantum dots (QD) as labels in two important areas of biology, bioimaging and biosensing. We analyze the biologically relevant properties of QDs focusing on the following topics: QD surface treatment and stability labeling of cellular structures and receptors with QDs, incorporation of QDs in living cells, cytotoxicity of QDs and influence of the biolocical environment on the biological and optical properties of QDs. Initially, we consider utilization of QDs as agants in high-resolution bioimaging techniques that can provide information at the molecular levels. The deverse range of modern live-cell QD-based imaging techniques with resolution far beyond the diffraction limit of light is examined. In each technique, we discuss the pros and cons of QD use and deliberate how QDs can be further engineered to facilitate their application in the respective imaging techniques and to produce significant improvements in resolution. Then we review QD-based point-of-care bioassays, bioprobes, and biosensors designed in different formats ranging from analytic biochemistry assays and ELISA, to novel point-of-care smartphone integrated QD-based biotests. Here, a wide range of QD-based fluorescence bioassays with optical transduction, electrochemiluminescence and photoelectrochemical assays are discussedc. Finally, this review provides an analysis of the prospects of application of QDs in selected important Areas of biology. KW - Fluorescence KW - Semiconductor quantum dot KW - Imaging KW - Quantification KW - Nanoparticle KW - NIR KW - IR KW - Quantum yield KW - Method KW - Microscopy KW - Assay KW - Bioconjugate PY - 2017 DO - https://doi.org/10.1039/c7tb01425b VL - 5 IS - 33 SP - 6701 EP - 6727 PB - Royal Society of Chemistry AN - OPUS4-43027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Jens A1 - Warschat, Carsten T1 - Studying the field induced breakup of acoustically levitated drops N2 - Coulomb fission of charged droplets (The terms drop and droplet are often used synonymous. Throughout this manuscript, to avoid confusion, the terms drop and droplet will be used for liquid spheres with radii in the millimeter range and the micrometer range, respectively. In our experiments, the first correspond to the parent drop while the latter describes the ejected progeny droplets.) is a wellstudied natural phenomenon. Controlled droplet fission is already successfully employed in several technological applications. Still, since the occurring surface rupture relies on the exact understanding and description of the liquid gas boundary, some details are still under debate. Most empirical systematic studies observe falling micrometer droplets passing through the electric field inside a plate capacitor. This approach, although easily applicable and reliable, limits the experimental degrees of freedom regarding the observable time and the maximum size of the drops and can only be performed in consecutive individual observations of different subsequent drops. Here we present a novel setup to study the field induced breakup of acoustically levitated drops. The design does not bear any restrictions towards the temporal window of observation, and allows handling of drops of a tunable radius ranging from 10 µm to several millimeters and a real-time monitoring of one single drop. Our comprehensive study includes a time resolved visual inspection, laser shadowgraphy, laser induced fluorescence imaging, and ambient mass spectrometric interrogation of the nascent Taylor cone. The results shown for a millimeter sized drop, previously inaccessible for Coulomb fission experiments, are mostly comparable with previous results for smaller drops. The major difference is the time scale and the threshold potential of the drop rupture. Both values, however, resemble theoretically extrapolations to the larger radius. The technique allows for a systematic study of breakup behavior of drops of different charge, material, and size. KW - Droplet fission KW - Levitated droplets KW - Taylor limit KW - Spray PY - 2017 DO - https://doi.org/10.1063/1.5004046 SN - 0034-6748 SN - 1089-7623 VL - 88 IS - 10 SP - 105108-1 EP - 105108-6 PB - AIP publishing AN - OPUS4-42940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Monks, Melissa-Jane T1 - Rare earth strontium fluoride nanocrystals prepared via sol gel synthesis - Spectroscopic study of upconversion luminescence properties N2 - Obtaining high quality upconverting nanocrystals with only little crystal defects and hence, a high luminescence, affords a reliable synthesis route. Only this guarantees the reproducibility of the material and its spectroscopic properties required for future application. The fluorolytic sol-gel synthesis appears to be a convenient attempt, as this is a method with only few steps influencing the material properties, which can be well controlled. Also creating bright upconverting nanocrystals requires a profound understanding of the interplay of photophysical processes like multiphoton absorption, radiative and non-radiative pathways, and energy transfer in the material. Based on steady-state and time resolved luminescence measurements at different excitation power densities, the influence of the lanthanide doping ratio and synthesis parameters such as the annealing process on SrF2-nanocrystals obtained via the fluorolytic sol-gel synthesis was systematically studied. T2 - GDCh Wissenschaftsforum Chemie CY - Berlin, Germany DA - 10.09.2017 KW - Upconversion KW - Strontiumfluoride KW - Annealing study KW - Doping study KW - Luminescence PY - 2017 AN - OPUS4-42944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kjaervik, Marit A1 - Müller, Anja A1 - Dietrich, P. A1 - Thissen, A. A1 - Bahr, S. A1 - Ritter, B. A1 - Kemnitz, E. A1 - Unger, Wolfgang T1 - Detection of suspended nanoparticles with near-ambient pressure x-ray photoelectron spectroscopy N2 - Two systems of suspended nanoparticles have been studied with near-ambient pressure x-ray photoelectron spectroscopy: silver nanoparticles in water and strontium fluoride—calcium fluoride core-shell nanoparticles in ethylene glycol. The corresponding dry samples were measured under ultra high vacuum for comparison. The results obtained under near-ambient pressure were overall comparable to those obtained under ultra high vacuum, although measuring silver nanoparticles in water requires a high pass energy and a long acquisition time. A shift towards higher binding energies was found for the silver nanoparticles in aqueous Suspension compared to the corresponding dry sample, which can be assigned to a change of surface potential at the water-nanoparticle interface. The shell-thickness of the core-shell nanoparticles was estimated based on simulated spectra from the National Institute of Standards and Technology database for simulation of electron spectra for surface analysis. With the instrumental set-up presented in this paper, nanoparticle suspensions in a suitable Container can be directly inserted into the analysis chamber and measured without prior sample preparation. KW - Nanoparticles KW - Suspensions KW - Core-shell nanoparticles KW - NAP-XPS PY - 2017 DO - https://doi.org/10.1088/1361-648X/aa8b9d SN - 1361-648X SN - 0953-8984 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. VL - 29 IS - 47 SP - 474002, 1 EP - 474002, 9 PB - IOP Publishing CY - UK AN - OPUS4-42951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Zur Röntgenfluoreszenzanalyse von Kulturgütern - Von Nebra bis Ägypten N2 - Im Vortag werden die Möglichkeiten der Synchrotronstrahlungsinduzierten Röntgenfluoreszenzanalayse (SRXRF) dargestellt. Insbesondere werden bei einer Reihe von Beispielen die Vorteile der SRXRF erläutert und der mögliche Einsatz eines portablen Messgeräts für die Analse von Glas diskutiert. T2 - Workshop: Ritter, Goethe, ihre Prismen und die Polarität CY - Jena, Germany DA - 19.05.2017 KW - Gold KW - Synchrotron KW - XRF KW - BESSY KW - Archeometry KW - BAMline PY - 2017 AN - OPUS4-42976 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - The Bernstorf Gold - A challenge to the flexibility of SRXRF N2 - The gold finds from Bernstorf, in the Freising district of Bavaria, were discovered in 1998, in the area of a Bronze Age settlement. First analyses with X-ray fluorescence (XRF) revealed gold of an unusually high purity grade, which was explained by using cementation techniques. A newer analysis with laser ablation inductively coupled plasma mass spectrometry (LA–ICP–MS) indicated an even higher purity. These analytical results were the starting point of an ongoing discussion. The amount and type of the detected contaminants were highly controversial and led to contradictory interpretations. We reanalysed 11 gold samples with synchrotron radiation induced X-ray fluorescence (SRXRF) at the BAMline at BESSY-II. To reach the desired detection limits a thorough analysis with three different excitation energies and detection conditions were applied to confirm or disprove the previous results. In this contribution we will get into the details for the need of the different measurement conditions and the virtues of the use of synchrotron radiation. The use and effectiveness of cementation techniques will be addressed. Finally we will present the achieved results and their impact on the discussion. T2 - ICXOM 24 CY - Trieste, Italy DA - 25.10.2017 KW - Gold KW - Synchrotron KW - XRF KW - BESSY KW - Archeometry PY - 2017 AN - OPUS4-42977 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - TXRF and XANES at the BAMline N2 - The BAMline at the synchrotron BESSY II in Berlin supplies users with up to date analytical x-ray methods for the energy range between 5 and 50 keV. Additional to XRF with micron Resolution it provides amongst other things the possibility to use TXRF and XANES. Especially the use of the so-called Color X-Ray Camera (CXC) opens the possibility to use new and effective detection schemes, which allow to measure simultaneously distributions of elements or Absorption spectra in a motionless mode. In this talk the analytical possibilities at the BAMline for samples with biological Background will be introduced. The available methods will be presented and discussed for various examples. A perspective for the future use for XANES in grazing emission and TXRF geometries for plant materials will be given. T2 - TXRF 2017 CY - Brescia, Italy DA - 19.09.2017 KW - XANES KW - Synchrotron KW - XRF KW - BESSY PY - 2017 AN - OPUS4-42978 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baldofski, Stefanie A1 - Canitz, C. A1 - Garbe, L.-A. A1 - Schneider, Rudolf T1 - Studies on the development of antibodies for the highly hydrophobic plasticizers DINCH and DEHT N2 - Diisononylcyclohexane-1,2-dicarboxylate (DINCH) and di-2-ethylhexyl terephthalate (DEHT), two of the most important substitutes for phthalate plasticizers, are used for a wide range of applications. Consequently, an increasing occurrence in urine and environmental samples is reported. Reliable and fast analytical methods for the quantification of these plasticizers are needed. So far, mainly GC-MS or LC-MS methods are used. We aimed to develop the first antibodies and immunoassays allowing for high-throughput analysis of samples. We designed two DINCH hapten structures and one DEHT hapten structure and employed hapten-protein conjugates for the immunization of rabbits. Sensitive competitive enzyme-linked immunosorbent assays (ELISAs) against each hapten using the produced polyclonal antibodies were established. Yet, binding of DINCH to the respective antibodies was not observed in neither direct nor indirect assay formats, even when using protein conjugates with the heterologous haptens and different carrier proteins in the indirect format. The use of surfactants and solvents in the sample buffer did not result in recognition of the plasticizers. Also, no binding of DEHT in ELISA employing the respective antibodies was detected. We speculate that the production of antibodies against these highly hydrophobic molecules is not possible via our route, however a different hapten design could overcome this obstacle. KW - Weichmacher KW - Phthalate KW - Antikörper KW - Selektivität KW - Ersatzstoffe KW - Polyclonal antibodies KW - Phthalate substitutes KW - Antibody production for hydrophobic molecules KW - DEHT KW - DINCH KW - Hapten design PY - 2018 DO - https://doi.org/10.1016/j.ab.2017.12.006 SN - 0003-2697 VL - 543 SP - 90 EP - 96 PB - Elsevier Inc. CY - Amsterdam, NL AN - OPUS4-44015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohsin, G. F. A1 - Schmitt, F.-J. A1 - Kanzler, C. A1 - Epping, J. D. A1 - Flemig, Sabine A1 - Hornemann, A. T1 - Structural characterization of melanoidin formed from D-glucose and L-alanine at different temperatures applying FTIR, NMR, EPR, and MALDI-ToF-MS N2 - The aim of this study was to identify specific chemical bonds and characteristic structures in melanoidins formed from D-glucose and L-alanine between 130 and 200 °C. The results might be used to control the type and amount of melanoidin produced during food processing. For this purpose, complementary techniques, such as FTIR, NMR, EPR, and MALDI-ToF, were employed. At 160 °C color, solubility and UV/Vis absorption change characteristically and consequently, structural transformations could be observed in FTIR and NMR spectra. For example, sharp signals of N-H, C-N, and C-H oscillations in the L-alanine spectrum are prone to inhomogeneous broadening in melanoidins prepared above 150 °C. These changes are caused due to formation of heterogeneous macromolecular structures and occur during condensation reactions that lead to an increasing loss of water from the melanoidins with increasing temperatures. Additionally, MALDI-ToF-MS indicates the polymerization of glyoxal/glyoxylic acid and EPR shows the formation of radical structures. KW - MALDI-ToF-MS KW - Melanoidine KW - Konjugate KW - Lebensmittel KW - MALDI-ToF-MS KW - L-alanine KW - D-glucose KW - Maillard reaction KW - FTIR spectroscopy KW - EPR spectroscopy KW - Melanoidin KW - NMR spectroscopy PY - 2018 DO - https://doi.org/10.1016/j.foodchem.2017.11.115 SN - 0308-8146 VL - 245 SP - 761 EP - 767 PB - Elsevier Science CY - Amsterdam, NL AN - OPUS4-44018 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - In situ monitoring of a mechanochemical Knoevenagel condensation N2 - Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions. T2 - BESSY II User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Mechanochemistry KW - In situ KW - Knoevenagel condensation KW - C-C coupling PY - 2017 AN - OPUS4-44142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Homann, Tobias T1 - Mehrdimensionale Bestimmung der Schallschnelle auf Festkörperoberflächen mittels Einpunkt-Laservibrometrie im MHz-Bereich N2 - Die zerstörungsfreie Prüfung von austenitischen Mischnähten, wie sie beispielsweise im Primärkreislauf von Kernkraftwerken vorkommen, stellt besondere Anforderungen an die eingesetzte Ultraschallprüfung. Voraussetzung für die positions- und größenrichtige Darstellung von Bauteilfehlern, insbesondere bei bildgebenden Ultraschallverfahren, ist die genaue Kenntnis der Materialparameter auf dem gesamten Schalllaufweg vom Sender zum Empfänger. Im Rahmen eines Forschungsprojekts entwickeln wir ein zerstörungsfreies, inverses Verfahren, das die Schweißnahtparameter entsprechend des Ogilvy-Modells aus der Schallschnelleverteilung bestimmt, die eine Longitudinalwelle an der Oberfläche erzeugt, nachdem sie durch die Schweißnaht gelaufen ist. T2 - Workshop des Fachausschusses Ultraschall der DEGA e.V „Schallfeldbasierte Messverfahren – vom Transducer bis zur praktischen Anwendung“ CY - Kloster Drübeck, Germany DA - 10.07.2017 KW - Austenit KW - Ultraschall KW - Zerstörungsfreie Prüfung ZfP KW - Schweißnaht KW - Mischnaht PY - 2017 AN - OPUS4-44144 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jüngert, A. A1 - Dugan, S. A1 - Homann, Tobias A1 - Mitzscherling, Steffen A1 - Prager, Jens A1 - Pudovikov, S. A1 - Schwender, T. T1 - Advanced ultrasonic techniques for nondestructive testing of austenitic and dissimilar welds in nuclear facilities N2 - Austenitic stainless steel welds as well as dissimilar metal welds with nickel alloy filler material, used in safety relevant parts of nuclear power plants, still challenge the ultrasonic inspection. The weld material forms large oriented grains which lead on the one hand to high sound scattering and on the other hand – to inhomogeneity and to the acoustic anisotropy of the weld structure. The ultrasonic wave fronts propagate not linearly, as in ferritic weld joints, but along the curves, which depend on the specific grain structure of the weld. Due the influence of these phenomena, it is difficult to analyze the inspection results and to classify the ultrasonic indications, which could be both from the weld geometry and from the material defects. A correct flaw sizing is not possible. In an ongoing research project, different techniques to improve the reliability of ultrasonic testing at these kinds of welds are investigated. In a first step (in the previous research project) two ultrasonic inspection techniques were developed and validated on plane test specimens with artificial and realistic flaws. In the ongoing project, these techniques are applied to circumferential pipe welds with longitudinal and transverse flaws. The technique developed at the Federal Institute for Materials Research and Testing (BAM) in Germany uses a combination of ray tracing and synthetic aperture focusing technique (SAFT). To investigate the unknown grain structure, the velocity distribution of weld-transmitting ultrasound waves is measured and used to model the weld by ray tracing. The second technique, developed at the Fraunhofer Institute for Nondestructive Testing (IZFP) in Germany, uses Sampling Phased Array (Full Matrix Capture) combined with the reverse phase matching (RPM) and the gradient elastic constant descent algorithm (GECDM). This inspection method is able to estimate the elastic constants of the columnar grains in the weld and offers an improvement of the reliability of ultrasonic testing through the correction of the sound field distortion. The unknown inhomogeneity and anisotropy are investigated using a reference indication and the special optimization algorithm. Both reconstruction techniques give quantitative inspection results and allow the defect sizing. They have been compared to conventional ultrasonic testing with techniques, which are state of the art for components in nuclear power plants. The improvement will be quantified by the comparison of the probability of detection (POD) of each technique. T2 - 44th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Utah Valley Convention Center, Provo, Utah, USA DA - 15.07.2017 KW - Austenitic stainless steel KW - Nuclear power plants KW - Dissimilar welds KW - Nondestructive testing KW - Ultrasonic testing PY - 2018 SN - 978-0-7354-1644-4 SN - 0094-243X VL - 1949 SP - UNSP 110002, 1 EP - 9 AN - OPUS4-44148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jüngert, A. T1 - Advanced ultrasonic techniques for nondestructive testing of austenitic and dissimilar welds in nuclear facilities N2 - Austenitic stainless steel welds as well as dissimilar metal welds with nickel alloy filler material, used in safety relevant parts of nuclear power plants, still challenge the ultrasonic inspection. The weld material forms large oriented grains which lead on the one hand to high sound scattering and on the other hand – to inhomogeneity and to the acoustic anisotropy of the weld structure. The ultrasonic wave fronts propagate not linearly, as in ferritic weld joints, but along the curves, which depend on the specific grain structure of the weld. Due the influence of these phenomena, it is difficult to analyze the inspection results and to classify the ultrasonic indications, which could be both from the weld geometry and from the material defects. A correct flaw sizing is not possible. In an ongoing research project, different techniques to improve the reliability of ultrasonic testing at these kinds of welds are investigated. In a first step (in the previous research project) two ultrasonic inspection techniques were developed and validated on plane test specimens with artificial and realistic flaws. In the ongoing project, these techniques are applied to circumferential pipe welds with longitudinal and transverse flaws. The technique developed at the Federal Institute for Materials Research and Testing (BAM) in Germany uses a combination of ray tracing and synthetic aperture focusing technique (SAFT). To investigate the unknown grain structure, the velocity distribution of weld-transmitting ultrasound waves is measured and used to model the weld by ray tracing. The second technique, developed at the Fraunhofer Institute for Nondestructive Testing (IZFP) in Germany, uses Sampling Phased Array (Full Matrix Capture) combined with the reverse phase matching (RPM) and the gradient elastic constant descent algorithm (GECDM). This inspection method is able to estimate the elastic constants of the columnar grains in the weld and offers an improvement of the reliability of ultrasonic testing through the correction of the sound field distortion. The unknown inhomogeneity and anisotropy are investigated using a reference indication and the special optimization algorithm. Both reconstruction techniques give quantitative inspection results and allow the defect sizing. They have been compared to conventional ultrasonic testing with techniques, which are state of the art for components in nuclear power plants. The improvement will be quantified by the comparison of the probability of detection (POD) of each technique. T2 - 44th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Utah Valley Convention Center, Provo, Utah, USA DA - 15.07.2017 KW - Austenitic stainless steel KW - Nuclear power plants KW - Dissimilar Welds KW - Nondestructive Testing KW - Ultrasonic Testing PY - 2018 AN - OPUS4-44151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - White light interference microscopy, ellipsometry, and instrumented indentation testing as reference procedures N2 - The paper addresses “WHITE LIGHT INTERFERENCE MICROSCOPY, ELLIPSOMETRY, AND INSTRUMENTED INDENTATION TESTING AS REFERENCE PROCEDURES“ and is subdivided in the following sections: 1. Measurement vs. testing vs. reference procedures, 2. White light interference microscopy (WLIM) for determination of step height h, 3. Spectroscopic ellipsometry (SE) for determination of layer thickness d and 4. Instrumented indentation testing (IIT) for determination of indentation hardness HIT. The following points are discussed in more detail: methodology of measurement and testing, uncertainty budgets for direct (WLIM), model-based (SE) and formula-based (IIT) reference procedures by means of specific examples. It is shown that standardization efforts are connected to reference procedures. T2 - Referenzverfahren CY - BAM, Berlin, Germany DA - 21.02.2018 KW - Reference procedures KW - Uncertainty budgets KW - White light interference microscopy KW - Spectroscopic ellipsometry KW - Instrumented indentation testing PY - 2018 AN - OPUS4-44256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Stephan A1 - Hoffmann, Holger A1 - Garbe, L.-A. A1 - Schneider, Rudolf T1 - Liquid chromatography-tandem mass spectrometry detection of diclofenac and related compounds in water samples N2 - A frequently studied environmental contaminant is the active substance diclofenac, which is removed insufficiently in sewage treatment plants. Since its inclusion in the watch list of the EU Water Framework Directive, the concentrations in surface waters will be determined throughout Europe. For this, still, more precise analytical methods are needed. As a reference, HPLC-MS is frequently employed. One of the major metabolites is 4’-hydroxydiclofenac (4’-OH-DCF). Also, diclofenac lactam is important for assessing degradation and transformation. Aceclofenac (ACF), the glycolic acid ester of diclofenac is used as a drug, too, and could potentially be cleaved to yield diclofenac again. In various sewage treatment plant influent samples, diclofenac, 4’-OH-DCF, DCF lactam and ACF could be determined with detection limits of 3 µg/L, 0.2 µg/L, 0.17 µg/L and 10 ng/L, respectively. KW - Diclofenac KW - Festphasenextraktion KW - HPLC-MS KW - Probenvorbereitung KW - Kläranlage KW - Abwasser KW - Zyklisierung KW - Diclofenac KW - Solid-phase extraction KW - Sewage treatment plant KW - Cyclization KW - Sample treatment KW - HPLC–MS PY - 2018 DO - https://doi.org/10.1016/j.chroma.2018.01.037 SN - 0021-9673 SN - 1873-3778 VL - 1538 SP - 112 EP - 116 PB - Elsevier B.V. CY - Amsterdam, NL AN - OPUS4-44183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, Uwe T1 - International Standardization on Digital Industrial Radiography and CT N2 - Overview on state of the art of worldwide standardization in digital industrial radiography and industrial computed tomography T2 - Annual Fall Conference of KSNT - 2017 CY - Seoul, South Korea DA - 26.10.2017 KW - Industrial radiography KW - NDT KW - DIR KW - CT PY - 2017 AN - OPUS4-44184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja A1 - Schneider, Markus T1 - Surface chemical analysis of engineered nanoparticles by means of transmission x-ray microscopy and mass spectrometry N2 - PTFE/PS core-shell-nanoparticles were characterised by STXM, T-SEM, and ToF-SIMS. Shell-thicknesses were calculated and compared. Preliminary results from ToF-SIMS showed the capabilities of this method. T2 - BAM-BfR Seminar CY - Berlin, Germany DA - 15.02.2018 KW - STXM KW - NEXAFS KW - ToF-SIMS KW - SEM KW - Nanoparticles PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-44181 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - Messdatenauswertung mittels Origin in der Nanopartikelanalyse N2 - Die Anwendung der Software Origin zur Datenauswertung in der Nanopartikelanalyse wird anhand eines Beispiels vom Importieren der Daten über deren Verarbeitung bis zur graphischen Ausgabe demonstriert. T2 - ADDITIVE Origin Anwendertage 2018 CY - Berlin, Germany DA - 12.03.2018 KW - Silbernanopartikel KW - Origin KW - SAXS PY - 2018 AN - OPUS4-44458 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Heritage Lecture N2 - After finishing my diploma thesis in plasma physics in 1981, I dreamt of a future in a research lab to develop novel fusion reactors for energy production or to study universal plasmas and their emission in the cosmos. This dream never became real, however I found my first job in a team to build up a new museum dedicated to “Energy”, and this first part of my career was already finished after a year, because the funding was not extended. So, I found immediately a new job as a young scientist in the institute for analytical sciences (originally ISAS: Institute for Plasmachemistry and Applied Spectroscopy) in 1982 to develop novel plasma ion sources for inorganic mass spectrometry. The first source of interest was based on a glow discharge for direct analysis of conducting solids (technically supported by Finnigan MAT, Bremen). Here I adopted the design of the Grimm type discharge for the first time, which was well known in optical emission spectroscopy, and coupled it to a quadrupole mass analyzer. The advantage of this design was that flat craters are produced by sputtering which made this source very powerful for in-depth analysis of technical layers. This then became the topic of my PhD, which was not originally planned, and I had to learn a lot about surface analysis. However, since the first project was too successful we established a small team (in cooperation with Jose Broekaert - an expert in ICP-OES) which started with the development of our own inductively coupled plasma ion source in 1986 coupled to a quadrupole and in 1989 to a sector field mass spectrometer (funded by the Minister of Science and Technology; again in cooperation with Finnigan MAT). The latter device was launched to the market in 1993 as the Element 1. The second decade of my career was still related to instrumental development but mainly of glow discharge sources. In an EU funded project first an automated glow discharge sector field instrument was developed where the Grimm type geometry was combined with a fast flow concept (in cooperation with Volker Hoffmann at IFW in Dresden). This was done in cooperation with VG (which became later a part of Thermo Fisher Scientific together with Finnigan MAT), so that it is not surprising that this concept for the Element GD. This project was later continued in the third phase of my career, again funded by the EU and in cooperation with the group of Alfredo Sanz-Medel (Rosario Pereiro and Jorge Pisonero), to develop a fast flow, but now rf-powered GD ion source in combination with a time-of-flight mass spectrometer, which was later launched to the market commercially by Horiba Jobin Yvon (France) for in-depth profiling of thin layers even of non-conducting materials. In the first decade of my career I started to study already “analytical chemistry” from the scratch because the instruments developed have been applied now for direct analysis of solid materials, technical layers and environmental samples. In case of environmental applications our ICP-MS (the quadrupole and the sector field instrument) was coupled with separation techniques, so that this period of instrumental development was dominated in the second decade by development of high efficiency sample introduction systems in combination with speciation studies of Pt group elements, arsenic, selenium and phosphorus (in DNA and phosphorylated proteins), Ni and Cr. Additionally, we continued with the analysis of solid ceramic materials (Al2O3, SiC, SiN) and ambient air-born particles. At the end of the second decade we complemented our instrumental pool by a collision and reaction cell instrument in cooperation with Micromass and used this instrument for speciation studies of peptides and proteins and demonstrated that by ICP-HEX-MS quantitative proteomics is feasible. Therefore, we more and more focused in the following years on metalloproteins and published a famous paper on “Metallobiomolecules: The basis of life, the challenge of atomic spectroscopy” (together with Luc Moens and Ryszard Lobinski). For detection of metalloproteins we applied typical workflows of biochemistry and proteomics, for which I had to extend my knowledge about biochemistry and proteomics. As a new analytical tool, we used a homemade laser ablation cell for sample introduction of metalloproteins after their separation by gel electrophoresis and extended this work by applying metal-tagging of antibodies for Western blot assays. For this purpose, proteins were separated in SDS-PAGE and electroblotted onto membranes. Specific detection of proteins even not containing any metal could be performed by laser ablation ICP-MS using the metal tagged antibodies for indirect detection. This research was interrupted in 2009 by a movement from ISAS (where atomic spectroscopy was declining) to BAM (the Federal Institute for Materials Research and Testing, Berlin) where this research direction was fostered. The experience we achieved at ISAS in the previously mentioned projects were now used here at BAM in the fourth decade for materials research and the development of a quantitative elemental microscope with cellular resolution. So, at the end of my career I am trying to apply all my knowledge and expertise to develop analytical methods and to apply multimodal spectroscopies to decipher the construction code of the cellular machinery, which is the most precise and complex machinery I have ever seen. If we were able to understand how this machinery works, we can better diagnose and treat a malfunction in case of the development of a disease. Finally, I can conclude that lifelong learning starts before school but does not end at the end of this lecture. It looks like this heritage lecture will be focused on my career only, but this is not the case because some highlights of my career will be used to illustrate a few universal principles: how to have fun, how to find friends and how this all leads to an increase of joy and joy is the basis of new ideas (which must not always be related to your profession) and novel ideas are essential for a successful and satisfying career. So, this heritage lecture wants to answer the most important question of a life which was dedicated to plasma spectrochemistry: 1) Is it possible - at all - to have fun in this research direction? 2) Can we learn already today what we need tomorrow? 3) How can we still realize our scientific dreams of cutting edge research in times of cutting budgets? Which automatically leads to the next question: 4) Is necessity the mother of invention? All questions will be answered! Controversial discussions (for angry or disappointed colleagues) will be stimulated and my visions of future research (for students and postdocs) and instrumental developments (for manufacturer) will be presented. Finally, conclusions will be drawn by the auditorium (everybody) and thanks will be given to Ramon Barnes (by me) already in advance! T2 - 2018 Winter Conference on Plasma Spectrochemistry CY - Amelia Island, FL, USA DA - 08.01.2018 KW - History of the research work of Norbert Jakubowski KW - Glow Discharge Mass Spectrometry KW - Inductively Coupled Plasma Mass Spectrometry KW - Laser Ablation PY - 2018 AN - OPUS4-44461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Heritage Lecture N2 - After finishing my diploma thesis in plasma physics in 1981, I dreamt of a future in a research lab to develop novel fusion reactors for energy production or to study universal plasmas and their emission in the cosmos. This dream never became real, however I found my first job in a team to build up a new museum dedicated to “Energy”, and this first part of my career was already finished after a year, because the funding was not extended. So, I found immediately a new job as a young scientist in the institute for analytical sciences (originally ISAS: Institute for Plasmachemistry and Applied Spectroscopy) in 1982 to develop novel plasma ion sources for inorganic mass spectrometry. The first source of interest was based on a glow discharge for direct analysis of conducting solids (technically supported by Finnigan MAT, Bremen). Here I adopted the design of the Grimm type discharge for the first time, which was well known in optical emission spectroscopy, and coupled it to a quadrupole mass analyzer. The advantage of this design was that flat craters are produced by sputtering which made this source very powerful for in-depth analysis of technical layers. This then became the topic of my PhD, which was not originally planned, and I had to learn a lot about surface analysis. However, since the first project was too successful we established a small team (in cooperation with Jose Broekaert - an expert in ICP-OES) which started with the development of our own inductively coupled plasma ion source in 1986 coupled to a quadrupole and in 1989 to a sector field mass spectrometer (funded by the Minister of Science and Technology; again in cooperation with Finnigan MAT). The latter device was launched to the market in 1993 as the Element 1. The second decade of my career was still related to instrumental development but mainly of glow discharge sources. In an EU funded project first an automated glow discharge sector field instrument was developed where the Grimm type geometry was combined with a fast flow concept (in cooperation with Volker Hoffmann at IFW in Dresden). This was done in cooperation with VG (which became later a part of Thermo Fisher Scientific together with Finnigan MAT), so that it is not surprising that this concept for the Element GD. This project was later continued in the third phase of my career, again funded by the EU and in cooperation with the group of Alfredo Sanz-Medel (Rosario Pereiro and Jorge Pisonero), to develop a fast flow, but now rf-powered GD ion source in combination with a time-of-flight mass spectrometer, which was later launched to the market commercially by Horiba Jobin Yvon (France) for in-depth profiling of thin layers even of non-conducting materials. In the first decade of my career I started to study already “analytical chemistry” from the scratch because the instruments developed have been applied now for direct analysis of solid materials, technical layers and environmental samples. In case of environmental applications our ICP-MS (the quadrupole and the sector field instrument) was coupled with separation techniques, so that this period of instrumental development was dominated in the second decade by development of high efficiency sample introduction systems in combination with speciation studies of Pt group elements, arsenic, selenium and phosphorus (in DNA and phosphorylated proteins), Ni and Cr. Additionally, we continued with the analysis of solid ceramic materials (Al2O3, SiC, SiN) and ambient air-born particles. At the end of the second decade we complemented our instrumental pool by a collision and reaction cell instrument in cooperation with Micromass and used this instrument for speciation studies of peptides and proteins and demonstrated that by ICP-HEX-MS quantitative proteomics is feasible. Therefore, we more and more focused in the following years on metalloproteins and published a famous paper on “Metallobiomolecules: The basis of life, the challenge of atomic spectroscopy” (together with Luc Moens and Ryszard Lobinski). For detection of metalloproteins we applied typical workflows of biochemistry and proteomics, for which I had to extend my knowledge about biochemistry and proteomics. As a new analytical tool, we used a homemade laser ablation cell for sample introduction of metalloproteins after their separation by gel electrophoresis and extended this work by applying metal-tagging of antibodies for Western blot assays. For this purpose, proteins were separated in SDS-PAGE and electroblotted onto membranes. Specific detection of proteins even not containing any metal could be performed by laser ablation ICP-MS using the metal tagged antibodies for indirect detection. This research was interrupted in 2009 by a movement from ISAS (where atomic spectroscopy was declining) to BAM (the Federal Institute for Materials Research and Testing, Berlin) where this research direction was fostered. The experience we achieved at ISAS in the previously mentioned projects were now used here at BAM in the fourth decade for materials research and the development of a quantitative elemental microscope with cellular resolution. So, at the end of my career I am trying to apply all my knowledge and expertise to develop analytical methods and to apply multimodal spectroscopies to decipher the construction code of the cellular machinery, which is the most precise and complex machinery I have ever seen. If we were able to understand how this machinery works, we can better diagnose and treat a malfunction in case of the development of a disease. Finally, I can conclude that lifelong learning starts before school but does not end at the end of this lecture. It looks like this heritage lecture will be focused on my career only, but this is not the case because some highlights of my career will be used to illustrate a few universal principles: how to have fun, how to find friends and how this all leads to an increase of joy and joy is the basis of new ideas (which must not always be related to your profession) and novel ideas are essential for a successful and satisfying career. So, this heritage lecture wants to answer the most important question of a life which was dedicated to plasma spectrochemistry: 1) Is it possible - at all - to have fun in this research direction? 2) Can we learn already today what we need tomorrow? 3) How can we still realize our scientific dreams of cutting edge research in times of cutting budgets? Which automatically leads to the next question: 4) Is necessity the mother of invention? All questions will be answered! Controversial discussions (for angry or disappointed colleagues) will be stimulated and my visions of future research (for students and postdocs) and instrumental developments (for manufacturer) will be presented. Finally, conclusions will be drawn by the auditorium (everybody) and thanks will be given to Ramon Barnes (by me) already in advance! T2 - BAM-Doktorandenseminar CY - Berlin, Germany DA - 07.02.2018 KW - History of the research work of Norbert Jakubowski KW - Glow Discharge Mass Spectrometry KW - Inductively Coupled Plasma Mass Spectrometry KW - Laser Ablation PY - 2018 AN - OPUS4-44462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer-Tenhagen, C. A1 - Johnen, D. A1 - Nehls, Irene A1 - Becker, Roland T1 - A Proof of Concept: Are Detection Dogs a Useful Tool to Verify Potential Biomarkers for Lung Cancer? N2 - Early and reliable diagnostic test is essential for effective therapy of lung cancer. Volatile organic compounds that are characteristic for cancer could serve as valuable biomarkers in cancer diagnosis. Both trace analytical and detection dog approaches give some evidence for the existence of such biomarkers. In this proof of concept, study dogs and trace analysis were implemented in combination to gain more information concerning cancer biomarkers. Two dogs were trained to distinguish between absorbed breath samples of lung cancer patients and healthy persons and succeeded with correct identification of patients with 9/9 and 8/9 and correct negative indications from of 8/10 and 4/10 samples from healthy individuals. A recent observational study found that breath samples from lung cancer patients showed an increase in 1-butanol, 2-butanone, 2-pentanone, and hexanal. Synthetic air samples were therefore fortified with these compounds and adsorbed to a fleece. Tested against breath samples from healthy probands, on presentation to the dogs these synthetic samples provoked an indication in three out of four samples. We were able to demonstrate that a combination of the natural nose of a dog and a trace analytic technique can be a valuable concept in the search for cancer biomarkers. KW - Lung cancer KW - Breath KW - Detection dog KW - Biomarkers KW - Sampling KW - Synthetic air PY - 2018 DO - https://doi.org/10.3389/fvets.2018.00052 SN - 2297-1769 VL - 5 SP - Article 52,1 EP - 6 PB - Frontiers Research Foundation CY - Lausanne AN - OPUS4-44466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ickert, Stefanie A1 - Hofmann, J. A1 - Riedel, Jens A1 - Beck, S. A1 - Pagel, K. A1 - Linscheid, M. W. T1 - Charge-induced geometrical reorganization of DNA oligonucleotides studied by tandem mass spectrometry and ion mobility N2 - Mass spectrometry is applied as a tool for the elucidation of molecular structures. This premises that gas-phase structures reflect the original geometry of the analytes, while it requires a thorough understanding and investigation of the forces controlling and affecting the gas-phase structures. However, only little is known about conformational changes of oligonucleotides in the gas phase. In this study, a series of multiply charged DNA oligonucleotides (n¼15–40) has been subjected to a comprehensive tandem mass spectrometric study to unravel transitions between different ionic gas-phase structures. The nucleobase sequence and the chain length were varied to gain insights into their influence on the geometrical oligonucleotide organization. Altogether, 23 oligonucleotides were analyzed using collision-induced fragmentation. All sequences showed comparable correlation regarding the characteristic collision energy. This value that is also a measure for stability, strongly correlates with the net charge density of the precursor ions. With decreasing charge of the oligonucleotides, an increase in the fragmentation energy was observed. At a distinct charge density, a deviation from linearity was observed for all studied species, indicating a structural reorganization. To corroborate the proposed geometrical change, collisional cross-sections of the oligonucleotides at different charge states were determined using ion mobility-mass spectrometry. The results clearly indicate that an increase in charge density and thus Coulomb repulsion results in the transition from a folded, compact form to elongated structures of the precursor ions. Our data show this structural transition to depend mainly on the charge density, whereas sequence and size do not have an influence. KW - Ion mobility KW - Collision-induced dissociation KW - Mass spectrometry KW - Oligonucleotide KW - Fragmentation KW - Tandem-MS PY - 2018 DO - https://doi.org/10.1177/1469066717746896 SN - 1469-0667 SN - 1751-6838 VL - 24 IS - 2 SP - 225 EP - 230 PB - Sage AN - OPUS4-44429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ickert, Stefanie A1 - Riedel, Jens A1 - Beck, S. A1 - Linscheid, M. W. T1 - Negative nucleotide ions as sensitive probes for energy specificity in collision‐induced fragmentation in mass spectrometry N2 - Rationale: The most commonly used fragmentation methods in tandem mass spectrometry (MS/MS) are collision‐induced dissociation (CID) and higher energy collisional dissociation (HCD). While in CID the preselected ions in the trap are resonantly (and m/z exclusively) excited, in HCD the entire m/z range experiences the dissociative acceleration. The different excitation is reflected in different fragment distributions. Methods: As a test‐bed for particularly pronounced fragmentation specificity, here MS/MS experiments on several 4‐mer oligonucleotides were conducted employing both collision methods and the results were thoroughly compared. Oligonucleotides are shown to be sensitive probes to subtle changes, especially in the negative ion mode. A detailed analysis of these differences reveals insight into the dissociation mechanics. Results: Thedifferencesarerepresentedinheat‐maps,whichallowforadirectvisualinspection oflargeamountsofdata.Inthesefalsecolourrepresentationsthe,sometimessubtle,changesinthe individual dissociation product distributions become distinct. Another advantage of these graphic plots can be found in the formation of systematic patterns. These patterns reflect trends in dissociation specificity which allow for the formulation of general rules in fragmentation behavior. Conclusions: Instruments equipped with two different excitation schemes for MS/MS are today widely available. Nonetheless, direct comparisons between the individual results are scarcely made. Such comparative studies bear a powerful analytical potential to elucidate fragmentation reaction mechanism. KW - DNA KW - Tandem MS KW - HCD KW - CID PY - 2018 DO - https://doi.org/10.1002/rcm.8062 SN - 0951-4198 SN - 1097-0231 VL - 32 IS - 7 SP - 597 EP - 603 PB - Wiley & Sons, Ltd. AN - OPUS4-44430 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weller, Michael G. T1 - Ten Basic Rules of Antibody Validation N2 - The quality of research antibodies is an issue for decades. Although several papers have been published to improve the situation, their impact seems to be limited. This publication makes the effort to simplify the description of validation criteria in a way that the occasional antibody user is able to assess the validation level of an immunochemical reagent. A simple, 1-page checklist is supplied for the practical application of these criteria. KW - Replication KW - Reproducibility KW - Documentation KW - Open Science KW - Quality Control KW - Biochemistry KW - Biotechnology KW - Bioanalysis PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444322 UR - https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5813849/ DO - https://doi.org/10.1177/1177390118757462 SN - 11773901 VL - 13 SP - 1 EP - 5 PB - Sage CY - Los Angeles, USA AN - OPUS4-44432 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Leonhard, H. T1 - Korrosionsgefahr schnell aufdecken: Zerstörungsfreier Oberflächentest für nichtrostende Stähle N2 - Eine Passivschicht schützt die Oberflächen nichtrostender Stähle vor Korrosion. Ist diese unvollständig ausgebildet oder beschädigt, sind Anlagenkomponenten in Gefahr, durch Materialauflösung zerstört zu werden. KorroPads geben schnell Aufschluss über den Zustand der Passivschicht. In nur 15 Minuten liegt ein valides Prüfergebnis vor. KW - Nichtrostender Stahl KW - Korrosionsschnelltest KW - KorroPad KW - Passivschicht PY - 2018 SN - 1869-0149 VL - 2018 IS - 1 SP - 14 EP - 14 PB - KCI GmbH CY - Kleve AN - OPUS4-44482 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Quantification of silver nanoparticles at single cell level by mass cytometry N2 - Silver nanoparticles (AgNPs), have a high scientific and commercial impact due to their important antibacterial properties. However, there are serious concerns about their toxicological adverse effects as a consequence of their broad range of applications. Particularly, the impact of AgNPs on cells is not very well understood yet and there is a current demand to develop analytical methodologies providing information about the interaction and distribution of AgNPs at a single cell level. In this research, mass cytometry was used to introduce a new quantitative approach to study the uptake of AgNPs by individual THP-1 macrophages as a cell model system. Here, we show that this methodology provides not only multi-variate phenotypic information of individual cells but enables the quantitative analysis of AgNPs associated to cells in a single measurement by performing an external calibration using AgNPs suspension. Using differentiated THP-1 cells, we monitored and quantified the uptake of 50 nm AgNPs in a time and dose-dependent manner by mass cytometry. 7 to 120 AgNPs per cell (2 to 89 fg Ag/cell) were determined after exposure of differentiated THP-1 cells to low AgNPs concentrations of 0.1 and 1.0 mg L-1, at time points of 4 and 24 h. The results were validated by mass cytometric analysis of digested cells working as a conventional inductively coupled plasma mass spectrometry, ICP-MS. This study demonstrates the power of single cell analysis by mass cytometry even for low doses experiments as a new analytical tool for hitherto unaddressed questions in nanotoxicology. T2 - 1st German Mass Cytometry User Forum CY - Berlin, Germany DA - 01.02.2018 KW - Silver nanoparticles KW - Single cell KW - Mass cytometry PY - 2018 AN - OPUS4-44408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Quantification of silver nanoparticles at single cell level by mass cytometry N2 - Silver nanoparticles (AgNPs), have a high scientific and commercial impact due to their important antibacterial properties. However, there are serious concerns about their toxicological adverse effects as a consequence of their broad range of applications. Particularly, the impact of AgNPs on cells is not very well understood yet and there is a current demand to develop analytical methodologies providing information about the interaction and distribution of AgNPs at a single cell level. In this research, mass cytometry was used to introduce a new quantitative approach to study the uptake of AgNPs by individual THP-1 macrophages as a cell model system. Here, we show that this methodology provides not only multi-variate phenotypic information of individual cells but enables the quantitative analysis of AgNPs associated to cells in a single measurement by performing an external calibration using AgNPs suspension. Using differentiated THP-1 cells, we monitored and quantified the uptake of 50 nm AgNPs in a time and dose-dependent manner by mass cytometry. 7 to 120 AgNPs per cell (2 to 89 fg Ag/cell) were determined after exposure of differentiated THP-1 cells to low AgNPs concentrations of 0.1 and 1.0 mg L-1, at time points of 4 and 24 h. The results were validated by mass cytometric analysis of digested cells working as a conventional inductively coupled plasma mass spectrometry, ICP-MS. This study demonstrates the power of single cell analysis by mass cytometry even for low doses experiments as a new analytical tool for hitherto unaddressed questions in nanotoxicology. T2 - BAM-BfR Seminar CY - Berlin, Germany DA - 15.02.2018 KW - Silver nanoparticles KW - Single cell KW - Mass cytometry PY - 2018 AN - OPUS4-44410 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Hertwig, Andreas ED - Esser, N. ED - Hinrichs, K. ED - Beck, Uwe T1 - 7th International Conference on Spectroscopic Ellipsometry (ICSE-7) N2 - The 7th International Conference on Spectroscopic Ellipsometry (ICSE-7) was held in Berlin in June 2016, jointly organised by ICSE and BAM. The publication of the proceedings special issue in Applied Surface Science follows this event. In the special issue, about 100 articles on current topics of optics and surface science related to ellipsometry, polarimetry, and similar techniques are presented, underpinning the high significance of these techniques for many fields of materials science. T2 - 7th International Conference on Spectroscopic Ellipsometry CY - Berlin, Germany DA - 06.06.2016 KW - Spectroscopic ellipsomety PY - 2017 UR - https://www.sciencedirect.com/journal/applied-surface-science/vol/421/part/PB DO - https://doi.org/10.1016/j.apsusc.2017.04.081 SN - 0169-4332 VL - 421 Part B SP - 269 EP - 916 PB - Elsevier B.V CY - Amsterdam AN - OPUS4-44412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Unraveling the dynamics of thin films of a miscible PVME/PS blend N2 - Dielectric spectroscopy (BDS) was employed to investigate the dynamics of thin films (7 – 200 nm) of a Poly (vinyl methyl ether) (PVME) / Polystyrene (PS) blend (50:50 wt%). For the BDS measurements Nano-Structured Capacitors (NSC) were employed, where films have a free surface. This method was applied for film thicknesses up to 36 nm. Thicker films were prepared between Crossed Electrodes Capacitors (CEC). The spectra of the films showed multiple processes. The first process was assigned to the -relaxation of a bulk-like layer. For films measured by NSC, its rates were higher compared to that of the bulk blend. This behavior was related to a PVME-rich free-surface layer. A second process was observed for films measured by CEC (process X) and the 36 nm film measured by NSC (process X2). This process was assigned to fluctuations of PVME constraint by PS. Its activation energy was found to be thickness dependent, due to the evidenced thickness dependency of the compositional heterogeneity. Finally, a third process with an activated temperature-dependence was observed for all films measured by NSC (process X1). It resembled the molecular fluctuations in an adsorbed layer found for films of pure PVME. T2 - Anual Meeting of the American Physical Society CY - Los Angeles, CA, USA DA - 05.03.2018 KW - Thin polymeric films PY - 2018 AN - OPUS4-44414 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Örnek, C. A1 - Léonard, Fabien A1 - McDonald, S. A1 - Prajapati, A A1 - Withers, P. J. A1 - Engelberg, D. T1 - Time-dependent in situ measurement of atmospheric corrosion rates of duplex stainless steel wires N2 - Corrosion rates of strained grade UNS S32202 (2202) and UNS S32205 (2205) duplex stainless steel wires have been measured, in situ, using time-lapse X-ray computed tomography. Exposures to chloride-containing (MgCl2) atmospheric environments at 50 °C (12–15 M Cl− and pH ~5) with different mechanical elastic and elastic/plastic loads were carried out over a period of 21 months. The corrosion rates for grade 2202 increased over time, showing selective dissolution with shallow corrosion sites, coalescing along the surface of the wire. Corrosion rates of grade 2205 decreased over time, showing both selective and pitting corrosion with more localised attack, growing preferentially in depth. The nucleation of stress corrosion cracking was observed in both wires. KW - X-ray computed tomography KW - Time-lapse X-ray computed tomography PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444153 UR - https://www.nature.com/articles/s41529-018-0030-9 DO - https://doi.org/10.1038/s41529-018-0030-9 SN - 2397-2106 VL - 2 SP - Article 10, 1 EP - 15 PB - Nature CY - London AN - OPUS4-44415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Already Producing or Still Calibrating? – Advances of Model-Based Data Evaluation Concepts for Quantitative Online NMR Spectroscopy N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example. Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). Based on concentration measurements of reagents and products by the NMR analyzer a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (“Integrated CONtrol and SENsing”, www.consens-spire.eu). T2 - Practical Applications of NMR in Industry Conference (PANIC) 2018 CY - La Jolla, California, USA DA - 04.03.2018 KW - Process Monitoring KW - Process Control KW - Process analytical technology KW - Spectral Modeling KW - Smart Sensors KW - CONSENS KW - Industrie 4.0 PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444357 AN - OPUS4-44435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Novel Flow Cell Designs for Process Monitoring with Compact NMR Spectroscopy N2 - Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction characterization and process control. Robust field integration of NMR systems have to face explosion protection or integration into process control systems with short set-up times. This paves the way for industrial automation in real process environments. The design of failsafe, temperature and pressure resistant flow through cells along with their NMR-specific requirements is an essential cornerstone to enter industrial production plants and fulfill explosion safety requirements. Additionally, if fast reactions are monitored, suitable mixing devices need to be placed in close vicinity to the measuring volume to mix the reactants properly. NMR-specific requirements aim at full quantitative pre-magnetization and acquisition with maximum sensitivity while reducing sample transfer times and dwell-times. All parameters are individually dependent on the applied NMR instrument. Luckily, an increasing number of applications are reported together with an increasing variety of commercial equipment. However, these contributions have to be reviewed thoroughly. The performance of sample flow cells commonly used in online analytics and especially for low-field NMR spectroscopy was experimentally and theoretically investigated by 1H-NMR experiments and numerical simulations. Especially, the applicability of 3D printed zirconium dioxide for innovative flow cell designs was of interest. Here, we demonstrate and discuss an automated test method to determine the critical parameters of flow through cells for quantitative online NMR spectroscopy. The setup is based on randomized setpoints of flow rates in order to reduce temperature related effects. Five flow cells and tubing were assessed and compared for high-field as well as low-field NMR spectrometers. T2 - Practical Applications of NMR in Industry Conference ​(PANIC) 2018 CY - La Jolla, California, USA DA - 04.03.2018 KW - Process Monitoring KW - Process Control KW - Flow Cell KW - Online NMR Spectroscopy KW - Additive Manufacturing KW - CONSENS PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444364 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-44436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana T1 - Process Monitoring with Online NMR Spectroscopy – An Enabler for Industrial Internet of Things (IIoT) N2 - Improvement in deep process understanding is a mandatory prerequisite for the application of modern concepts like Industrial Internet of Things (IIoT) or “Industrie 4.0”. This is particularly relevant in new process concepts such as intensified production in modularized plants. The direct hyphenation with online methods of process analytical technology (PAT) allows profound insights into the actual reactions within chemical and pharmaceutical production steps and provides necessary information for associated advanced control strategies. While the industrial application of online Raman spectroscopy has already been successfully demonstrated, low-field NMR spectroscopy is not yet adequately developed as an online method for use in process industry. The high information content combined with the low calibration effort makes NMR spectroscopy a highly promising method for modern process automation with a high flexibility due to short set-up times and novel calibration concepts. This is a major advantage especially within multi-purpose production plants, as well as for processes suffering from fluctuating quality of raw materials. The concept was evaluated on several example processes of pharmaceutical and chemical industry. The one presented here represents a stage of the synthesis of the industrially important solvent tetrahydrofuran consisting of the catalytic hydrogenation of 2-butine-1,4-diol was monitored. This reaction is proceeding via an intermediate product and suffers from competitive reaction paths. In this application, different spectroscopic methods were combined with the data obtained from classical process sensors, e.g., pressure, temperature, and flow transducers for the development of innovative control concepts. T2 - Practical Applications of NMR in Industry Conference ​(PANIC) 2018 CY - La Jolla, California, USA DA - 04.03.2018 KW - Online NMR Spectroscopy KW - Process Control KW - Industrie 4.0 KW - Indirect Hard Modeling KW - Industrial Internet of Things (IIoT) KW - CONSENS KW - Hydrogenation KW - Lithiation PY - 2018 AN - OPUS4-44437 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Sustainable and Flexible Production of High Quality Chemicals and Pharmaceuticals Using Smart Sensors and Modular Production Units N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. The talk also generally covers current aspects of high-field and low-field online NMR spectroscopy for reaction monitoring and process control and gives also an overview on direct dissolution studies of API cocrystals. T2 - Chemistry Group Seminar Pfizer Inc. CY - La Jolla, California, USA DA - 09.03.2018 KW - Process Monitoring KW - Online NMR Spectroscopy KW - Smart Sensors KW - Indirect Hard Modeling KW - Modular Production KW - CONSENS PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444382 AN - OPUS4-44438 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Quantitative NMR Spectroscopy Uncertainty Analysis Workshop N2 - qNMR provides the most universally applicable form of direct concentration or purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. The workshop presents basic terms of statistics and uncertainty analysis, which are the basis for qNMR spectroscopy and data analysis such as, e.g., standard deviations, linear regression, significance tests, etc. and gives typical examples of applications in qNMR spectroscopy. T2 - Practical Applications of NMR in Industry Conference ​(PANIC) Validation Workshop 2018 CY - La Jolla, California, USA DA - 08.03.2018 KW - qNMR KW - NMR Validation KW - Basic Statistics KW - Linear Regression PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444395 AN - OPUS4-44439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Thorid T1 - HARFE: Haftfestigkeit Reproduzierbarkeit Festigkeit „Nanoskalige Haftvermittler zur Erhöhung der Haft- bzw. Klebfestigkeit unter Verwendung von ALD-Hybridprozessen“ N2 - Das Poster „HARFE: Haftfestigkeit Reproduzierbarkeit Festigkeit“ widmet sich den nanoskaligen Haftvermittlern zur Erhöhung der Haft- bzw. Klebfestigkeit unter Verwendung von ALD-Hybridprozessen. T2 - Netzwerksymposium “Schützen und Veredeln von Oberflächen”, Wildau CY - TH Wildau, Germany DA - 01.03.2018 KW - Verbundfestigkeit KW - Oberflächenenergie KW - ALD-Beschichtung PY - 2018 AN - OPUS4-44399 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trimpin, S. A1 - Lee, C. A1 - Weidner, Steffen A1 - El-Baba, T. A1 - Lutomski, C. A1 - Inutan, E. A1 - Foley, C. A1 - Ni, C.-K. A1 - McEwen, C. T1 - Unprecedented Ionization Processes in Mass SpectrometryProvide Missing Link between ESI and MALDI N2 - In the field of mass spectrometry,producing intact, highly-charged protein ions from surfaces is a conundrum with significant potential payoff in application areas ranging from bio-medical to clinical research. Here, we report on the ability to form intact, highly-charged protein ions on high vacuum time-of-flight mass spectrometers in the linear and reflectron modes achievable using experimental conditions that allow effective matrix removal from both the sample surfaces and from the charged clusters formed by the laser Ablation event. The charge states are the highest reported on high vacuum mass spectrometers, yet they remain at only around athird of the highest charge obtained using laser ablation with a suitable matrix at atmospheric pressure. Other than physical instrument modifications, the key to forming abundant and stable highly-charged ions appears to be the volatility of the matrix used. Cumulative results suggest mechanistic links between the ionization process reported here and traditional ionization methods of electrospray ionization and matrix-assisted laser desorp-tion/ionization. KW - MALDI KW - Electrospray KW - Mass spectrometry KW - Ionization PY - 2018 DO - https://doi.org/10.1002/cphc.201701246 SN - 1439-4235 SN - 1439-7641 VL - 19 IS - 5 SP - 581 EP - 589 PB - Wiley-VCH AN - OPUS4-44404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Acoustical analysis of DCSBD and MHC discharges N2 - Due to the multi-physical appearance of gas discharges the possibilities of interaction with their surrounding environment are very wide. Some of the most common applications are the surface or material modification and acting as an ion source for mass spectroscopy applications. Since atmosphere plasma generates a massive amount of thermal energy caused by collisions in the sheath, this temperature alternation is also able to produce acoustic waves in the ambient gas volume (as lightning and thunder), which is called thermoacoustic effect. This talk presents an overview of the experimental acoustic analysis of surface dielectric barrier and micro hollow cathode discharges. Regarding other methods of acoustic excitation, the thermoacoustic approach benefits of its massless working principle and the proper impedance matching. In addition to the characterisation, possible applications (e.g. plasma acoustic loudspeaker or transducer for air-coupled ultrasonic testing) concerning these discharge types are presented. T2 - DPG Frühjahrstagung (SAMOP) CY - Erlangen, Germany DA - 04.03.2018 KW - Gas discharges KW - Micro hollow cathode discharge KW - Surface dielectric barrier discharge KW - Atmospheric pressure plasma PY - 2018 AN - OPUS4-44443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Banach, Ulrich A1 - Hübert, Thomas T1 - VDI/VDE-Richtlinie für Multigassensoren N2 - Technische Richtlinien enthalten Empfehlungen sowie Anforderungen zum Stand der Technik zur Aufstellung von Bewertungskriterien und Behandlung wissenschaftlich-technischer Fragen. Sie fördern den Erfahrungsaustausch und Technologietransfer zwischen Entwicklern und Anwendern. In unserem Beitrag stellen wir die Richtlinie VDI/VDE 3518 vor. Diese Richtlinienreihe definiert Begriffe, beschreibt den Aufbau und klassifiziert Multigassensoren (Blatt 1), befasst sich mit den Anforderungen für das Unterscheiden, Erkennen und mengenmäßige Bestimmen von Gemischen gasförmiger Stoffe und die Prüfung von Multigassensoren (Blatt 2) und gibt Anleitung für geruchsbezogene Messungen mit „Elektronischen Nasen“ (Blatt 3). Multigassensoren können als elektronische Nasen in Anlehnung an den biologischen Geruchssinn zur Wahrnehmung und Charakterisierung von Gerüchen eingesetzt werden. Die Spezifik von Multigassensoren besteht darin, dass durch die Wahl und Betriebsweise der Sensoren eine Vielzahl von geeigneten Messsignalen erzeugt werden, aus denen mit mathematischen Verfahren die für die Anwendung gewünschten Informationen extrahiert werden. Dazu ist ein Training der Messeinrichtung mit Proben bekannter Eigenschaften notwendig. Diese Richtlinie soll Herstellern, Anbietern und Nutzern als ein Leitfaden Informationen und Erläuterungen für die korrekte und sichere Arbeit mit Multigassensoren liefern. Sie soll Prüflaboratorien und Anwendern helfen, bei der Beurteilung von Qualitätsmerkmalen einheitlich vorzugehen und dafür gemeinsame Randbedingungen anzugeben T2 - 7. Anwendertreffen Ionenmobilitätsspektrometrie CY - Reutlingen, Germany DA - 06.03.2018 KW - Elektronische Nase KW - Multigassensorik KW - Richtlinie PY - 2018 AN - OPUS4-44452 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Zerstörungsfreie Prüfung von Komposit-Druckbehältern und ferromagnetischen Kunststoffen unter Verwendung von Wirbelstromprüfgeräten N2 - Metallische Druckgefäße werden aus Gründen der Gewichtseinsparung zunehmend durch Composite-Druckgefäße ersetzt. Während der Alterungsprozess bei metallischen Druckgefäßen durch Wöhlerkurven hinreichend beschrieben wird, ist der Alterungsmechanismus bei Composite-Druckgefäßen noch nicht vollständig geklärt. Im Rahmen des BAM-interne Themenfeldprojekts COD-AGE werden mit diversen Verfahren alterungsbegleitende, zerstörungsfreie Prüfungen an Composite-Druckgefäßen durchgeführt. Nach einem kurzen Überblick über die BAM und den FB 8.4 werden zunächst die allgemeine Funktionsweise der Wirbelstromprüfung und die bildgebende Wirbelstromprüfung erklärt. Anschließend werden Ergebnisse der konventionellen und hochfrequenten Wirbelstromprüfung vorgestellt. Der letzte Teil des Vortrages beschäftigt sich mit der Prüfbarkeit von Kunststoffen aus Kunstharz und 3D-Druck mit dem Wirbelstromverfahren durch Zugabe ferromagnetischer Nanopartikel bzw. Verwendung von ferromagnetischem Filament. T2 - DGZfP Arbeitskreis Magdeburg CY - Magdeburg, Germany DA - 17.01.2018 KW - CFK KW - COD-AGE KW - Druckbehälter KW - Ferromagnetischer Kunststoff KW - Wirbelstromprüfung PY - 2018 AN - OPUS4-43809 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica T1 - Nanocrystals as tagging reagents for imaging mass cytometry N2 - Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining importance for bioimaging cytometry to answer analytical, biological and biomedical questions. High sensitivity and spatial resolution make it an excellent tool for imaging of metal and heteroelement distribution in single cells. Comparable to CyTOF imaging mass cytometry, metal coded antibodies can be used for multiparametric analysis as well as quantification. In this project, nanocrystals are investigated as new highly sensitive metal tags for identification and quantification of biomarkers, like Alzheimer’s or breast cancer, in clinical cell assays and tissue samples. Of high significance is the simultaneous analysis of several biomarkers at once, which is possible by special coding of lanthanide tags on the biomarker associated antibody. Nanocrystals show potential for sensitive measurement in MS due to high stability and signal amplification compared to tags with fewer metal atoms. For proof of principle, synthesis and characterization of lanthanide doped nanocrystals was performed by a nanoPET pharma GmbH with great reproducibility and homogenous size. In A549 cell cultures, the uptake and distribution of these nanocrystals within the monolayered cells was investigated by LA-ICP-MS measurements using subcellular resolution. The nanocrystals showed high sensitivity and the possibility of multiparametric analysis by doting different lanthanides. Additionally, stability of the bioconjugation of the nanocrystals and target antibodies was investigated using Dot Blot experiments and LA-ICP-MS. T2 - CyTOF User Forum 2018 CY - Berlin, Germany DA - 01.02.2018 KW - Nanocrystal KW - Imaging mass cytometry KW - LA-ICP-MS KW - Bioconjugation KW - Metal-Tag KW - Multimodal PY - 2018 AN - OPUS4-44106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laux, P. A1 - Tentschert, J. A1 - Riebeling, Ch. A1 - Braeuning, A. A1 - Creutzenberg, O. A1 - Epp, A. A1 - Fessard, V. A1 - Haas, K.-H. A1 - Haase, A. A1 - Hund-Rinke, K. A1 - Jakubowski, Norbert A1 - Kearns, P. A1 - Lampen, A. A1 - Rauscher, H. A1 - Schoonjans, R. A1 - Störmer, A. A1 - Thielmann, A. A1 - Mühle, U. A1 - Luch, A. T1 - Nanomaterials: certain aspects of application, risk assessment and risk communication N2 - Development and market introduction of new nanomaterials trigger the need for an adequate risk assessment of such products alongside suitable risk communication measures. Current application of classical and new nanomaterials is analyzed in context of regulatory requirements and standardization for chemicals, food and consumer products. The challenges of nanomaterial characterization as the main bottleneck of risk assessment and regulation are presented. In some areas, e.g., quantification of nanomaterials within complex matrices, the establishment and adaptation of analytical techniques such as laser ablation inductively coupled plasma mass spectrometry and others are potentially suited to meet the requirements. As an example, we here provide an approach for the reliable characterization of human exposure to nanomaterials resulting from food packaging. Furthermore, results of nanomaterial toxicity and ecotoxicity testing are discussed, with concluding key criteria such as solubility and fiber rigidity as important parameters to be considered in material development and regulation. Although an analysis of the public opinion has revealed a distinguished rating depending on the particular field of application, a rather positive perception of nanotechnology could be ascertained for the German public in general. An improvement of material characterization in both toxicological testing as well as end-product control was concluded as being the main obstacle to ensure not only safe use of materials, but also wide acceptance of this and any novel technology in the general public. KW - Nanomaterials KW - Toxicity KW - Ecotoxicity KW - Standardization KW - Exposure PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-441096 DO - https://doi.org/10.1007/s00204-017-2144-1 VL - 92 IS - 1 SP - 121 EP - 141 PB - Springer AN - OPUS4-44109 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, S. A1 - López-Serrano, Ana A1 - Mitze, H. A1 - Jakubowski, Norbert A1 - Schwerdtle, T. T1 - Single-cell analysis by ICP-MS/MS as a fast tool for cellular bioavailability studies of arsenite N2 - Single-cell inductively coupled plasma mass spectrometry (SC-ICP-MS) has become a powerful and fast tool to evaluate the elemental composition at a single-cell level. In this study, the cellular bioavailability of arsenite (incubation of 25 and 50 μM for 0-48 h) has been successfully assessed by SC-ICP-MS/MS for the first time directly after re-suspending the cells in water. This procedure avoids the normally arising cell membrane permeabilization caused by cell fixation methods (e.g. methanol fixation). The reliability and feasibility of this SC-ICP-MS/MS approach with a limit of detection of 0.35 fg per cell was validated by conventional bulk ICP-MS/MS analysis after cell digestion and parallel measurement of sulfur and phosphorus. KW - Single-cell analysis KW - ICP-MS/MS KW - Arsenite PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-441105 DO - https://doi.org/10.1039/c7mt00285h SN - 1756-5901 VL - 10 IS - 1 SP - 73 EP - 76 PB - RSC Publ. CY - Cambridge AN - OPUS4-44110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Mobile robot olfaction with flying platforms N2 - This presentation gives an introduction to the gas-sensitive aerial robots developed at BAM, including various application examples in the field of mobile robot olfaction: gas source localization and gas distribution mapping T2 - Networked Environmental Monitoring – from sensor principles to novel services CY - BAM, Berlin, Germany DA - 06.02.2018 KW - Localization of gas sources KW - Mobile Robot Olfaction KW - Tomographic reconstruction of gas plumes KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - UAV-REGAS PY - 2018 AN - OPUS4-44086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mielke, Johannes A1 - Babick, F. A1 - Uusimäki, T. A1 - Müller, P. A1 - Verleysen, E. A1 - Hodoroaba, Vasile-Dan T1 - Evaluation of electron microscopy techniques for the purpose of classification of nanomaterials N2 - One current and much-debated topic in the characterization of nanomaterials (NM) is the implementation of the recently introduced recommendation on a definition of a nanomaterial by the European Commission. All currently available sizing techniques able to address nanoparticles were systematically evaluated. It was demonstrated that particle sizing techniques like: analytical centrifugation, particle tracking analysis, single-particle inductively coupled plasma mass-spectrometry, differential electrical mobility analysis, dynamic light scattering, small angle X-ray scattering, ultrasonic attenuation spectrometry, but also gas Adsorption analysis based on the BET-method can be applied for a screening classification. However, the quality of the results depends on the individual material to be classified. For well-dispersed, nearly spherical (nano)particles most of the sizing techniques can be applied in a quick and reliable way. In contrast, the classification of most real-world materials is a challenging task, mainly due to non-spherical particle shape, large polydispersity or strong agglomeration/ aggregation of the particles. In the present study it was shown that these issues can be resolved in most cases by electron microscopy as a confirmatory classification technique. Electron microscopy techniques such as TEM, STEM, SEM or TSEM transmission in SEM) are capable of assessing the size of individual nanoparticles accurately (see Figures 1 and 2). Nevertheless the challenging aspect is sample preparation from powder or liquid form on the substrate, so that a homogeneous distribution of well-separated (deagglomerated) particles is attained. The systematic study in this work shows examples where the extraction of the critical, smallest particle dimension - as the decisive particle parameter for the classification as a NM - is possible by analysing the sample after its simple, dry preparation. The consequences of additional typical issues like loss of information due to Screening of smaller particles by larger ones or the (in)ability to access the constituent particles in aggregates are discussed. T2 - European Microscopy Congress emc 2016 CY - Lyon, France DA - 28.08.2016 KW - Nanomaterial classification KW - Nanoparticles KW - Electron microscopy PY - 2016 SN - 9783527808465 DO - https://doi.org/10.1002/9783527808465.EMC2016.5767 SP - 13 EP - 14 PB - Wiley-VCH AN - OPUS4-44087 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schütze, A. A1 - Tiebe, Carlo T1 - Gas sensor characterization and calibration N2 - This seminar contribution contains the topics: 3S - sensitivity, selectivity and stability; sensor drift, aging and poisoning; influence of ambient conditions; gas mixing systems for sensor characterization and on-site field (re)calibration. T2 - Networked Environmental Monitoring – from sensor principles to novel services CY - BAM, Berlin, Germany DA - 06.02.2018 KW - Gas sensor KW - Gas mixing systems KW - Sensor characterization PY - 2018 AN - OPUS4-44088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Schütze, A. T1 - Sensor network deployment N2 - Content • Fixed monitoring stations • Mobile monitoring stations (on trams, buses, cars) • Personal mobile monitoring systems • Environmental monitoring for agriculture and beyond • Sensors on flying platforms T2 - Networked Environmental Monitoring – from sensor principles to novel services CY - BAM, Berlin, Germany DA - 06.02.2018 KW - Environmental monitoring KW - Gas sensors PY - 2018 AN - OPUS4-44073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Neumann, Patrick P. A1 - Tiebe, Carlo T1 - KonSens - Kommunizierende Sensorsysteme für die Bauteil- und Umweltüberwachung N2 - Im Projekt KonSens werden für die Anwendungsbei- spiele bauteilintegrierte Sensorik für Betonkomponen- ten und mobile Multigassensorik Sensorsysteme in Form von Funktionsmustern entwickelt, validiert und angewendet. Schwerpunkte liegen einerseits in der Detektion und Bewertung von Korrosionsprozessen in Beton und andererseits in der Detektion und Quantifi- zierung sehr geringer Konzentrationen toxischer Gase in der Luft. Dabei ist die Adaption der sensorischen Methoden aus dem Labor in reale Messumgebungen inklusive geeigneter Kommunikationstechnik ein wichtiger Aspekt. T2 - Networked Environmental Monitoring – from sensor principles to novel services CY - BAM, Berlin, Germany DA - 06.02.2018 KW - Umweltmonitoring KW - Bauwerksüberwachung PY - 2018 AN - OPUS4-44074 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Neumann, Patrick P. A1 - Tiebe, Carlo A1 - Johann, Sergej T1 - Adaptable multi-sensor device for gas detection N2 - Innovation is the catalyst for the technology of the future. It is important to develop new and better technologies that can continuously monitor the environmental impact, e.g., for air Quality control or emission detection. In the recently at BAM developed Universal Pump Sensor Control (UPSC3) module, different components and sensors are fused. The combination of the individual components makes the UPSC3 module an excellent monitoring and reference system for the development and characterization of gas specific sensors. Measurements over long periods are possible, for mixed gas loads or for certain gas measurements. The System is part of a mobile sensor network of several sensor units, which can also be used as standalone systems. T2 - Networked Environmental Monitoring – from sensor principles to novel services CY - BAM, Berlin, Germany DA - 06.02.2018 KW - Environmental monitoring PY - 2018 AN - OPUS4-44077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Visualization of automated multi sensor NDT assessment of concrete structures N2 - This talk demonstrates the results of the IGSTC-project entitled "NDT-Data Fusion". Project approach: Nondestructive testing (NDT) of concrete buildings allows to coordinate efficient repair measures. Multi-sensor platforms collect large data sets. Nevertheless, data analysis is typically performed manually. Data Fusion uses the full potential of a multi-sensory data set in order to: improve information quality (reliability, robustness, accuracy, clarity, completeness) and enables automated algorithm based data analysis. We present the project achievements, namely: - Development of building scanner system for multisensory NDT - Laboratory multi sensor investigations - Development of data fusion concept for honeycombing and pitting corrosion - Field testing T2 - IGSTC-Partners Meeting 2017 CY - Jodhpur, India DA - 22.10.2017 KW - Machine learning KW - Data fusion KW - NDT KW - Concrete KW - Corrosion KW - Honeycombs PY - 2017 AN - OPUS4-44097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Data fusion for non-destructive testing N2 - This talk introduces the "mechanisms" behind data fusion and demonstrates how to effectively use them for NDT-data. Common fusion strategies are introduced to explain what is required to enter (publishing-) practice. T2 - NDE2017 Pre-Conference Workshop CY - Chennai, India DA - 12.12.2017 KW - Data fusion KW - NDT KW - Concrete KW - Validation KW - Machine learning PY - 2017 AN - OPUS4-44100 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stajanca, Pavol A1 - Topolniak, Ievgeniia A1 - Pötschke, Samuel A1 - Krebber, Katerina T1 - Solution-mediated cladding doping of commercial polymer optical fibers N2 - Solution doping of commercial polymethyl methacrylate (PMMA) polymer optical fibers (POFs) is presented as a novel approach for preparation of custom cladding-doped POFs (CD-POFs). The presented method is based on a solution-mediated diffusion of dopant molecules into the fiber cladding upon soaking of POFs in a methanol-dopant solution. The method was tested on three different commercial POFs using Rhodamine B as a fluorescent dopant. The dynamics of the diffusion process was studied in order to optimize the doping procedure in terms of selection of the most suitable POF, doping time and conditions. Using the optimized procedure, longer segment of fluorescent CD-POF was prepared and its performance was characterized. Fiber’s potential for sensing and illumination applications was demonstrated and discussed. The proposed method represents a simple and cheap way for fabrication of custom, short to medium length CD-POFs with various dopants. KW - Polymer optical fiber KW - Solution doping KW - Polymethyl methacrylate KW - Rhodamine B KW - Dye-doped fiber KW - Fluorescent optical fiber PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-441045 DO - https://doi.org/10.1016/j.yofte.2018.02.008 SN - 1068-5200 SN - 1095-9912 VL - 41 SP - 227 EP - 234 PB - Elsevier Inc. AN - OPUS4-44104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Epping, Ruben T1 - Characterization of small heterogeneities in polymers by analysis of UPLC/ESI-MS reconstructed ion chromatograms N2 - From simple molar mass disperse homopolymers over copolymers to functionalized, 3-dimensional structures containing various distributions, the complexity of polymeric materials has become more and more sophisticated in recent years. With applications in medicine, pharmacy, smart materials or for the semiconductor industry the requirements for the characterization have risen with the complexity of the used polymers. For each additional distribution, an additional dimension in analysis is needed. Small, often isobaric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector. Instead of a complicated, time consuming and/or expensive 2d-chromatography or ion mobility spectrometry (IMS) method, that also has its limitations, here a simple approach using size exclusion chromatography (SEC) coupled with electrospray ionization mass spectrometry (ESI) is proposed. We used SEC for the separation because unlike other separation modes the separation in this mode solely should occur due to the hydrodynamic volume with no interference of other interactions. This simplifies the interpretation and the above mentioned heterogeneities should show a slight difference in hydrodynamic volume. ESI mass spectrometry can offer more than an access to mass dependent information like MMD, end group masses or CCD in polymer analysis. The online coupling to SEC allows the analysis of reconstructed ion chromatograms (RIC) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities in microstructure or topology, that are otherwise inaccessible or accessible only by time consuming or expensive methods. Because these heterogeneities might vary with the molar mass, analysis of the whole MMD-Peak (here the total ion current (TIC)) would not lead to the desired information. The broadening of the chromatographic peaks in this case does not origin from the already well known band broadening factors in chromatography from diffusion. This band broadening is attributed to the nature and composition of the analyte itself. Surprisingly there is very little investigation into the peak width or peak shape due to analyte structure itself found in literature. It is also shown, that with proper calibration even quantitative information could be obtained. This method is suitable to detect small differences in e. g. branching, topology, monomer sequence or tacticity and could potentially be used in production control of oligomeric products or other routinely done analyses to quickly indicate deviations from set parameters. Based on a variety of examples we demonstrate the possibilities and limitations of this approach. T2 - HTC-15 CY - Cardiff, UK DA - 24.01.2018 KW - UPLC/ESI-MS KW - Reconstructed chromatograms KW - Polymer analysis KW - Microstructure PY - 2018 AN - OPUS4-44137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - In situ monitoring of mechanochemical Knoevenagel condensations N2 - Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions. T2 - Adlershofer Forschungsforum CY - Berlin, Germany DA - 10.11.2017 KW - Mechanochemistry KW - Knoevenagel condensation PY - 2017 AN - OPUS4-44140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - In situ investigation of a mechanochemical Knoevenagel condensation N2 - Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions. T2 - PRORA CY - Berlin, Germany DA - 30.11.2017 KW - C-C coupling KW - Knoevenagel condensation KW - In situ PY - 2017 AN - OPUS4-44141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Streeck, C. A1 - Wirth, Thomas A1 - Unger, Wolfgang A1 - Beckhoff, B. T1 - Qualifying calibration samples for advanced thin film materials characterisation N2 - In this article the question of the certification of calibration samples for the characterisation of advanced thin film materials is addressed within the framework of reliable process control or quality management purposes. Reference measurement techniques can be used in order to address the gap in appropriate certified reference materials (CRMs) for thin film analyses. They allow for qualifying out-of-production samples originating from an operating production line as calibration samples. As a template for this procedure, CIGS [Cu(In,Ga)Se2] layers, that are absorber layers for high efficiency thin-film solar cells, have been used for establishing and validating reference-free X-ray fluorescence (XRF) analysis and Auger-electron spectroscopy (AES) as reference measurement techniques. The focus was on determining the average mole fractions in the CIGS layers obtaining results traceable to the SI unit system. Reference-free XRF is physically traceable and is based upon radiometrically calibrated instrumentation and knowledge of atomic fundamental data. Sputter-assisted AES can be established as a chemically traceable method after careful calibration using a certified reference material (CRM) based on a total number counting method. KW - CIGS KW - X-ray fluorescence (XRF) KW - Auger-electron spectroscopy (AES) PY - 2018 UR - https://www.spectroscopyeurope.com/article/qualifying-calibration-samples-advanced-thin-film-materials-characterisation VL - 30 IS - 1 SP - 11 EP - 14 PB - John Wiley & Sons Ltd CY - Chichester, West Sussex PO19 8SQ, UK AN - OPUS4-44260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nagli, L. A1 - Gaft, M. A1 - Raichlin, Y. A1 - Gornushkin, Igor B. T1 - Cascade generation in Al laser induced plasma N2 - We found cascade IR generation in Al laser induced plasma. This generation includes doublet transitions 3s25s 2S1∕2→ 3s24p 2P1∕2,3∕2 → 3s24s 2S1∕2; corresponding to strong lines at 2110 and 2117 nm, and much weaker lines at 1312–1315 nm. The 3s25s2S 1∕2 starting IR generation level is directly pumped from the 3s23p 2P3∕2 ground level. The starting level for UV generation at 396.2 nm (transitions 3s24s 2S1∕2 → 4p 2P3∕2) is populated due to the fast collisional processes in the plasma plume. These differences led to different time and special dependences on the lasing in the IR and UV spectral range within the aluminum laser induced plasma. KW - Plasma diagnostics KW - Laser induced plasma KW - LIBS KW - Plasma modeling PY - 2018 DO - https://doi.org/10.1016/j.optcom.2018.01.041 VL - 415 SP - 127 EP - 129 PB - Elsevier B.V. AN - OPUS4-44274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kästner, Claudia A1 - Lampen, A. A1 - Thünemann, Andreas T1 - What happens to the silver ions? – Silver thiocyanate nanoparticle formation in an artificial digestion N2 - An artificial digestion of silver nitrate is reported. It is shown that AgSCN nanoparticles emerge from ionic silver in saliva and remain present during the entire digestion process. The particles were characterized by infrared spectroscopy and small- and wide-angle X-ray scattering (SAXS/WAXS) regarding their composition and size distribution. KW - SAXS KW - WAXS KW - Artificial digestion PY - 2018 DO - https://doi.org/10.1039/c7nr08851e SN - 2040-3364 SN - 2040-3372 VL - 10 IS - 8 SP - 3650 EP - 3653 PB - RSC Publ. CY - Cambridge AN - OPUS4-44277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Quantifizierung der Schädigung von DNA in wässriger Lösung unter direkter Elektronenbestrahlung N2 - To cure cancer radiation therapy is used to kill tumor cells. It is based on radiation induced damage to biomolecules. Especially DNA damage is of key interest due to its central role in apoptosis and mutation. Because of the high amount of water in biological tissue, most of the damage is caused by the secondary particles produced by the inelastic scattering of ionizing radiation and water. A detailed understanding of the underlying molecular processes under physiological conditions is the prerequisite to develop more efficient therapies. Goal of this work is to quantify the DNA damage caused by ionizing radiation in dependence of the inelastic scattering events and the energy deposit within the microscopic target volume of biological relevance. The irradiations have to be performed in liquid, under consideration of the chemical environment. Therefore, a new combination of experiment and Monte-Carlo simulations was developed and tested. To make it possible to irradiate liquids with electrons within scanning electron microscopes a new sample holder was constructed incorporating an electron transparent nanomembrane. It makes it possible to irradiate DNA, proteins or cells at different pH, salinity and in the presence of cosolutes. %The most important results of this work are as follows: The median lethal dose for a model system of plasmid DNA and water was determined by the combination of experimental data, particle scattering simulations (Geant4-DNA) and diffusion calculations as D0.5=(1.7+-0.3) Gy. From the convolution of plasmid positions and the spatially resolved energy deposit, as determined by electron scattering simulations, the histogram of the energy deposit within the target volume of the plasmids and the microscopic median lethal energy deposit was calculated as E0.5=6+-4eV. It could be deduced that on average less than two ionization events are sufficient to cause a single-strand-break. The relation of single-strand-breaks (SSB) to double-strand-breaks (DSB), which is of importance for microdosimetric modeling, was determined as SSB:DSB = 12:1. The presented method for the determination of microscopic dose-damage relations was further extended to be applicable for general irradiation experiments. It becomes independent of the type of primary radiation used, the experimental geometry, and the diffusional properties of the molecules under investigation. This way different experimental systems with varying, inhomogeneous energy deposit characteristics become comparable with each other, which is not possible when only macroscopic averaged values are taken into account. In addition, the radiation protection properties of the compatible solute ectoine, as well as its influence on the water properties and biomolecules were investigated. %In addition, the influence of the compatible solute ectoine on water, biomolecules and its radiation protection properties were investigated. Raman spectroscopy revealed a concentration dependent increase of the collective water modes in the OH-stretching region, which was found to be independent of the sodium chloride concentration. Molecular dynamic simulations showed that the zwitterionic properties of ectoine lead to its half-chair conformation. The hydrogen bonds in the first hydration shell are more stable and have an increased lifetime compared to the bulk water. Irradiation experiments with DNA in the presence of 1M ectoine revealed an increase of the survival rate by a factor of 1.41 as compared to the absence of ectoine. The protective properties of ectoine result from the increase of the inelastic scattering probabilities of low energy electrons at the acoustic vibrational modes of water and its properties as OH-radical scavenger. This was shown by Raman spectroscopy and electron paramagnetic resonance measurements (EPR). T2 - Vortrag CY - Freie Universität Berlin, Germany DA - 14.02.2018 KW - DNA KW - Radiation damage KW - Ionizing radiation KW - DNA strand break KW - Dosimetry KW - Microdosimetry KW - Ectoine KW - Ectoine radiation protection KW - Salt KW - Water PY - 2018 AN - OPUS4-44280 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Ellipsometrische Klassifizierung von Kohlenstoffschichten N2 - Der Vortrag widmet sich der „ELLIPSOMETRISCHE KLASSIFIZIERUNG VON KOHLENSTOFFSCHICHTEN“ und beschreibt die Punkte: 1. Anwendungen Kohlenstoffschichten–Carbon–based films (DLC) aus dem Vortrag N. Ohtakeet. al. (ISO TC 107, Tokyo 2017),2. Präparation der Kohlenstoffschichten für ISO TC 107 Ringversuch aus Vortrag M. Hiratsuka et. al. (ISO TC 107, Tokyo 2017), 3. Ellipsometrische Charakterisierung von Kohlenstoffschichten, Ergebnisse des Ringversuchs (ISO TC 107, Tokyo 2017) Vortrag Beck et. al. und 4.Deutsche Normungsaktivitäten national/international zur Ellipsometrie DIN NA 062-01-061 (DIN 50989-1)/TC 107 (PWI DE)“ im Einzelnen. T2 - Netzwerksymposium “schützen und Veredeln von Oberflächen”, Wildau CY - TH Wildau, Germany DA - 01.03.2018 KW - Anwendung von Kohlenstoffschichten KW - Klassifizierung von Kohlenstoffschichten KW - Ringversuch Ellipsometrie KW - Normung Ellipsometrie PY - 2018 AN - OPUS4-44340 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Using Smart Sensors and Modular Production Units - For Sustainable and Flexible Production of High Quality Chemicals and Pharmaceuticals N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. The talk also generally covers current aspects of high-field and low-field online NMR spectroscopy for reaction monitoring and process control giving also an overview on direct dissolution studies of API cocrystals. T2 - Pfizer Analytical Chemistry Seminar CY - Pfizer Global Research & Development, Groton, CT, USA DA - 01.03.2018 KW - Online NMR Spectroscopy KW - Process sensors KW - Process analytical technology KW - Indirect Hard Modeling KW - Dissolution studies KW - CONSENS PY - 2018 AN - OPUS4-44347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Already Producing or Still Calibrating? – Online NMR Spectroscopy as Smart Field Device. N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. The talk also generally covers current aspects of high-field and low-field online NMR spectroscopy for reaction monitoring and process control giving an overview from direct dissolution studies of API cocrystals to studies of emulsions for a hydroformylation. T2 - Boston and Cambridge NMR community seminar CY - Cambridge, MS, USA DA - 02.03.2018 KW - Process Monitoring KW - Process Control KW - Pprocess analytical technology KW - Indirect Hard Modeling KW - Spectral Modeling KW - CONSENS PY - 2018 AN - OPUS4-44348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lasri, J. A1 - Chulvi, Katherine A1 - Eltayeb, N. E. T1 - Crystal structures of (E)-1-naphthaldehyde oxime and (E)-phenanthrene-9-carbaldehyde oxime N2 - The aldoximes C11H9NO (I) and C15H11NO (II), synthesized in ca 90%yield, by treatment of 1-naphthaldehyde or phenanthrene-9-carbaldehyde, respectively, with hydroxylamine hydrochloride and sodium carbonate, have been characterized by IR, 1H, 13C and DEPT-135 NMR spectroscopies, and also by singlecrystal X-ray diffraction analysis. The molecules of (I) and (II) are conformationally similar, with the aldoxime substituent groups lying outside the planes of the naphthalene or phenanthrene rings, forming dihedral angles with them of 23.9 (4) and 27.9 (6)°, respectively. The crystal structures of both (I) and (II) are similar with a single intermolecular O—H...N hydrogenbonding interaction, giving rise to the formation of one-dimensional polymeric chains extending along the 21 (b) screw axes in each. KW - Crystal structure KW - Aromatic aldehydes KW - E-aldoximes KW - Hydrogen bonding PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-443351 DO - https://doi.org/10.1107/S2056989018002116 SN - 2056-9890 VL - 74 SP - 332 EP - 336 PB - International Union of Crystallography CY - Chester AN - OPUS4-44335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dudek, Gabriele T1 - Die neue ISO/IEC 17025 - Was ändert sich für Prüf- und Kalibrierlaboratorien? N2 - Die Revision der ISO/IEC 17025 ist abgeschlossen. Der Vortrag gibt einen Überblick über die Einflüsse auf die neue Norm und die Veränderungen, die die neue Ausgabe mit sich bringt. T2 - DGUV-Workshop CY - St. Augustin, Germany DA - 01.03.2018 KW - Konformitätsbewertung KW - ISO/IEC 17025 KW - Prüflaboratorien KW - Akkreditierung PY - 2018 AN - OPUS4-44358 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tumanova, N. A1 - Tumanov, N. A1 - Robeyns, K. A1 - Fischer, Franziska A1 - Fusaro, L. A1 - Morelle, F. A1 - Ban, V. A1 - Hautier, G. A1 - Filinchuk, Y. A1 - Wouters, J. A1 - Leyssens, T. A1 - Emmerling, Franziska T1 - Opening Pandora’s Box: Chirality, Polymorphism, and Stoichiometric Diversity in Flurbiprofen/Proline Cocrystals N2 - Proline has been widely used for various cocrystallization applications, including pharmaceutical cocrystals. Combining enantiopure and racemic flurbiprofen and proline, we discovered 18 new crystal structures. Liquid-assisted grinding proved highly efficient to explore all the variety of crystal forms. A unique combination of stateof-the-art characterization techniques, comprising variable temperature in situ X-ray diffraction and in situ ball-milling, along with other physicochemical methods and density functional theory calculations, was indispensable for identifying all the phases. Analyzing the results of in situ ball-milling, we established a stepwise mechanism for the formation of several 1:1 cocrystals via an intermediate 2:1 phase. The nature of the solvent in liquidassisted grinding was found to significantly affect the reaction rate and, in some cases, the reaction pathway. KW - Mechanochemistry KW - Polymorphs KW - In situ PY - 2018 UR - https://pubs.acs.org/doi/abs/10.1021/acs.cgd.7b01436 DO - https://doi.org/10.1021/acs.cgd.7b01436 VL - 18 IS - 2 SP - 954 EP - 961 PB - American Chemical Society AN - OPUS4-44365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, G. A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - Strontium-coordination polymers based on tetrafluorophthalic and phthalic acids: mechanochemical synthesis, ab initio structures determination, and spectroscopic characterization N2 - Two strontium-based dicarboxylate systems [Sr(oBDC-F4)(H2O)2] (1) and [{Sr(oBDC)(H2O)2)·H2O] (2) were synthesized mechanochemically via milling of Sr(OH)2·8H2O with tetrafluorophthalic acid (H2oBDC-F4) or phthalic acid (H2oBDC), respectively. The new structures were determined ab initio from the powder X-ray diffraction (PXRD) data. Both compounds 1 and 2 crystallize in the monoclinic space group P21 /c as two-dimensional coordination polymers (2D-CPs). The determined structures were validated by extended X-ray absorption (EXAFS) data. Compounds 1 and 2 show different thermal stabilities. The fluorinated CP 1 is decomposed at 300 °C while the nonfluorinated CP 2 transforms into a new phase after thermal treatment at 400 °C. The two hydrated CPs exhibit small surface areas which increase after the thermal posttreatment for 1 but remains unchanged for the dehydrated sample of 2. Dynamic vapor sorption (DVS) experiments indicate that both the dehydrated and hydrated samples of 2 depict no significant differences in their adsorption isotherms. The DVS of water indicates that the phase transition after thermal posttreatment of 2 is irreversible. KW - Mechanochemistry KW - XRD KW - NMR PY - 2017 DO - https://doi.org/10.1039/c7dt02564e SN - 1477-9226 SN - 1477-9234 VL - 46 IS - 37 SP - 12574 EP - 12587 PB - The Royal Society of Chemistry CY - Cambridge AN - OPUS4-42261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Hertwig, Andreas A1 - Heidari, M. A1 - von Klitzing, R. A1 - Napolitano, S. A1 - Sferrazza, M. A1 - Schönhals, Andreas T1 - Decoupling of dynamic and thermal glass transition in thin films of a PVME/PS blend N2 - The discussions on the nanoconfinement effect on the glass transition and glassy dynamics phenomena have yielded many open questions. Here, the thickness dependence of the thermal glass transition temperature of thin films of a PVME/PS blend is investigated by ellipsometry. Its thickness dependence was compared to that of the dynamic glass transition (measured by specific heat spectroscopy), and the deduced Vogel temperature (T0). While and T0 showed a monotonous increase, with decreasing the film thickness, the dynamic glass transition temperature () measured at a finite frequency showed a non-monotonous dependence that peaks at 30 nm. This was discussed by assuming different cooperativity length scales at these temperatures, which have different sensitivities to composition and thickness. This non-monotonous thickness dependence of disappears for frequencies characteristic for T0. Further analysis of the fragility parameter, showed a change in the glassy dynamics from strong to fragile, with decreasing film thickness. KW - Thin polymeric films KW - Ellipsometry KW - Specific heat spectroscopy PY - 2017 DO - https://doi.org/10.1021/acsmacrolett.7b00625 SN - 2161-1653 VL - 6 IS - 10 SP - 1156 EP - 1161 PB - ACS Publications AN - OPUS4-42266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Shabanov, Sergej V. T1 - Geometrical effects in data collection and processing for calibration-free laser-induced breakdown spectroscopy N2 - Data processing in the calibration-free laser-induced breakdown spectroscopy (LIBS) is usually based on the solution of the radiative transfer equation along a particular line of sight through a plasma plume. The LIBS data processing is generalized to the case when the spectral data are collected from large portions of the plume. It is shown that by adjusting the optical depth and width of the lines the spectra obtained by collecting light from an entire spherical homogeneous plasma plume can be leastsquare fitted to a spectrum obtained by collecting the radiation just along a plume diameter with a relative error of 10−11 or smaller (for the optical depth not exceeding 0.3) so that a mismatch of geometries of data processing and data collection cannot be detected by fitting. Despite the existence of such a perfect least-square fit, the errors in the line optical depth and width found by a data processing with an inappropriate geometry can be large. It is shown with analytic and numerical examples that the corresponding relative errors in the found elemental number densities and concentrations may be as high as 50% and 20%, respectively. Safe for a few found exceptions, these errors are impossible to eliminate from LIBS data processing unless a proper solution of the radiative transfer equation corresponding to the ray tracing in the spectral data collection is used. KW - Plasma KW - LIBS KW - Plasma modeling PY - 2017 DO - https://doi.org/10.1016/j.jqsrt.2017.09.018 SN - 0022-4073 SN - 1879-1352 VL - 204 SP - 190 EP - 205 PB - Elsevier CY - New York, NY AN - OPUS4-42287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej A1 - Noske, Reinhard A1 - Feller, Viktor A1 - Bartholmai, Matthias ED - Vonau, Winfried ED - Cruvinel, P. ED - Chilibon, I. ED - Carvalho, V. ED - Sophocleous, M. T1 - Gas detection using a multi-sensor device with pump control and VOC sensor N2 - This paper deals with the development and investi-gation of a volatile organic compound (VOC) system for differ-ent scenarios. The integrated multi-sensor unit can detect dif-ferent gases through the integrated 3-fold VOC sensor, where-by a continuous measurement takes place. The system-integrated flow control, with pump and flow sensor, allows the gas molecules to be transported directly to the VOC sensor. The entire measurement is permanently stored on an integrat-ed Secure Digital (SD) card. If the previously determined limit range is exceeded, an alarm is generated. Due to the combina-tion of different components, numerous applications are possi-ble. The system is the first step or a tool towards further devel-opments in the field of gas sensors and is primarily used for the validation of chemically based gas sensors, and it is still largely extended by application-specific influences. T2 - Sensordevices 2017 - The Eighth International Conference on Sensor Device Technologies and Applications CY - Rome, Italy DA - 2017-09-10 KW - Gas detection KW - VOC KW - Pump control KW - Multi sensor device PY - 2017 SN - 978-1-61208-581-4 SP - 1 EP - 4 CY - Rome, Italy AN - OPUS4-42097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej T1 - Gas detection using a multi-sensor device with pump control and VOC sensor N2 - This paper deals with the development and investi-gation of a volatile organic compound (VOC) system for differ-ent scenarios. The integrated multi-sensor unit can detect dif-ferent gases through the integrated 3-fold VOC sensor, where-by a continuous measurement takes place. The system-integrated flow control, with pump and flow sensor, allows the gas molecules to be transported directly to the VOC sensor. The entire measurement is permanently stored on an integrat-ed Secure Digital (SD) card. If the previously determined limit range is exceeded, an alarm is generated. Due to the combina-tion of different components, numerous applications are possi-ble. The system is the first step or a tool towards further devel-opments in the field of gas sensors and is primarily used for the validation of chemically based gas sensors, and it is still largely extended by application-specific influences. T2 - Sensordevices 2017 - The Eighth International Conference on Sensor Device Technologies and Applications CY - Rome, Italy DA - 2017-09-10 KW - Gas detection KW - VOC KW - Pump control KW - Multi sensor device PY - 2017 AN - OPUS4-42098 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tatzel, Michael A1 - von Blanckenburg, F. A1 - Oelze, M. A1 - Bouchez, J. A1 - Hippler, D. T1 - Late Neoproterozoic seawater oxygenation by siliceous sponges N2 - The Cambrian explosion, the rapid appearance of most animal phyla in the geological record, occurred concurrently with bottom seawater oxygenation. Whether this oxygenation Event was triggered through enhanced nutrient supply and organic carbon burial forced by increased continental weathering, or by species engaging in ecosystem engineering, remains a fundamental yet unresolved question. Here we provide evidence for several simultaneous developments that took place over the Ediacaran–Cambrian transition: expansion of siliceous sponges, decrease of the dissolved organic carbon pool, enhanced organic carbon burial, increased phosphorus removal and seawater oxygenation. This evidence is based on Silicon and carbon stable isotopes, Ge/Si ratios, REE-geochemistry and redox-sensitive elements in a chert-shale succession from the Yangtze Platform, China. According to this reconstruction, sponges have initiated seawater oxygenation by redistributing organic carbon oxidation through filtering suspended organic matter from seawater. The resulting increase in dissolved oxygen levels potentially triggered the diversification of eumetazoans. KW - Oxygenation KW - Carbon cycle KW - Silicon stable isotopes PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-422339 DO - https://doi.org/10.1038/s41467-017-00586-5 SN - 2041-1723 VL - 8 SP - Article 621, 1 EP - 10 AN - OPUS4-42233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauw, Brian Richard A1 - Kästner, Claudia A1 - Thünemann, Andreas T1 - Nanoparticle size distribution quantification: results of a small-angle X-ray scattering inter-laboratory comparison N2 - This paper presents the first worldwide inter-laboratory comparison of small-angle X-ray scattering (SAXS) for nanoparticle sizing. The measurands in this comparison are the mean particle radius, the width of the size distribution and the particle concentration. The investigated sample consists of dispersed silver nanoparticles, surrounded by a stabilizing polymeric shell of poly(acrylic acid). The silver cores dominate the X-ray scattering pattern, leading to the determination of their radius size distribution using (i) the generalized indirect Fourier transformation method, (ii) classical model fitting using SASfit and (iii) a Monte Carlo fitting approach using McSAS. The application of these three methods to the collected data sets from the various laboratories produces consistent mean number- and volume-weighted core radii of Rn = 2.76 (6) nm and Rv = 3.20 (4) nm, respectively. The corresponding widths of the lognormal radius distribution of the particles were σn = 0.65 (1) nm and σv = 0.71 (1) nm. The particle concentration determined using this method was 3.0 (4) g l−1 or 4.2 (7) × 10−6 mol l−1. These results are affected slightly by the choice of data evaluation procedure, but not by the instruments: the participating laboratories at synchrotron SAXS beamlines, commercial and in-house-designed instruments were all able to provide highly consistent data. This demonstrates that SAXS is a suitable method for revealing particle size distributions in the sub-20 nm region (at minimum), out of reach for most other analytical methods. KW - SAXS KW - Small-angle X-ray scattering KW - Silver nanoparticles PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-422800 DO - https://doi.org/10.1107/S160057671701010X SN - 1600-5767 VL - 50 IS - 5 SP - 1280 EP - 1288 PB - (IUCr) International Union of Crystallography AN - OPUS4-42280 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Ultrafast spectroscopy - Femtosecond electron diffraction N2 - Currently, two main high speed processes can be investigated: electromagnetic absorption and electromagnetic scattering. At the summer university of the School of Analytical Sciences Adlershof (SALSA-HU), a series of 5 articles were presented to ilustrate the potential of ultrafast spectroscopy, from IR band assignment to monitoring time resolved structural changes. First, by studying light absorption is possible to do assignment and interpretation of IR bands in small molecules and to study the influence of ligands or labeled molecules in protein structures. Second, by studying light scattering is possible to monitoring photoinduced structural changes in solid materials. This presentation contains a study of photoinduced structural changes monitored by light scattering in condensed matter. T2 - SALSA Summer University 2017 CY - Berlin, Germany DA - 19.09.2017 KW - Ultrafast spectroscopy KW - Femtosecond electron diffraction KW - Spin crossover KW - Photoexcitation KW - Structural dynamics PY - 2017 AN - OPUS4-42120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Niels A1 - Hüllmann, Dino A1 - Kohlhoff, Harald A1 - Neumann, Patrick P. ED - Cosmi, F. T1 - A concept for an aerial-based landfill monitoring system N2 - Aerial based robots constitute a safe and suitable approach to remote gas-sensing. This paper describes a new concept , incorporating existing UAVs and newly developed gas sensors. The presented autonomous system is able to perform gas source localization and gas distribution mapping. T2 - 34th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Trieste, Italy DA - 19.09.2017 KW - Gassensor KW - Multicopter KW - UAV KW - Olfaction PY - 2017 SN - 978-88-8303-863-1 SP - 179 EP - 181 PB - University of Trieste, Italy CY - Trieste, Italy AN - OPUS4-42122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Niels T1 - Concept for an aerial-based landfill monitoring system N2 - Aerial based robots constitute a safe and suitable approach to remote gas-sensing. This paper describes a new concept , incorporating existing UAVs and newly developed gas sensors. The presented autonomous system is able to perform gas source localization and gas distribution mapping. T2 - 34th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Trieste, Italy DA - 19.09.2017 KW - Gassensing KW - Multicopter KW - UAV KW - Olfaction PY - 2017 AN - OPUS4-42128 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pavlovic, Mato T1 - Achieving a more comprehensive POD using both simulation and measurements N2 - Today, it is an established fact that the capability of the non-destructive testing (NDT) to find flaws can be properly addressed only in terms of probability of detection (POD). The probabilistic, signal-response model, introduced in 1980s, was developed with experimental observation of eddy-current inspections of flat plate samples, containing surface breaking cracks. A linearity between the peak voltage measured by the testing system, and the crack depth was observed. The influence of the crack depth was therefore seen as the major influencing factor for the POD, whereas other factors merely caused the variability in the measurement. This model has proven itself valid for those inspection cases where there is only one main influencing factor on the POD (usually the flaw size) and other factors have a lesser influence. But with increasing requirements to quantify the capability of NDT systems in complex inspection situations, where several factors have a major influence on the POD, it has become clear that the applicability of this simple model has reached its limits. In disregard to its limitations, this model is regularly applied to those situations in which its fundamental assumptions are invalid, forcing evaluators and NDT researchers into attempts to fit the data to an unsuitable model, instead of fitting an appropriate model to the data. The multiparameter POD model, developed in the early 2010s, enables more factors that influence detection to be simultaneously analysed, making the POD a function of multiple factors. The model is based on the inspection’s physical model, to describe the influence of different factors on the response signal. Measurement variability is obtained from the experiment. Using this model assisted determination of the POD, the necessary number of flaws for evaluation is reduced and a more comprehensive understanding of the inspection is obtained. Several examples of the successful application of the multi-parameter POD model in different fields will be presented. T2 - 7th European-American Workshop on Reliability of NDE CY - Potsdam, Germany DA - 04.09.2017 KW - POD KW - Multi-parameter KW - Reliability KW - NDT PY - 2017 AN - OPUS4-42078 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkelmann, Aimo A1 - Nolze, Gert A1 - Vespucci, S. A1 - Gunsekar, N.-K. A1 - Trager-Cowan, C. A1 - Vilalta-Clemente, A. A1 - Wilkinson, A. J. A1 - Voss, M. T1 - Diffraction effects and inelastic electron transport in angle-resolved microscopic imaging applications N2 - We analyse the signal formation process for scanning electron microscopic imaging applications on crystalline specimens. In accordance with previous investigations, we find nontrivial effects of incident beam diffraction on the backscattered electron distribution in energy and momentum. Specifically, incident beam diffraction causes angular changes of the backscattered electron distribution which we identify as the dominant mechanism underlying pseudocolour orientation imaging using multiple, angle-resolving detectors. Consequently, diffraction effects of the incident beam and their impact on the subsequent coherent and incoherent electron transport need to be taken into account for an in-depth theoretical modelling of the energy- and momentum distribution of electrons backscattered from crystalline sample regions. Our findings have implications for the level of theoretical detail that can be necessary for the interpretation of complex imaging modalities such as electron channelling contrast imaging (ECCI) of defects in crystals. If the solid angle of detection is limited to specific regions of the backscattered electron momentum distribution, the image contrast that is observed in ECCI and similar applications can be strongly affected by incident beam diffraction and topographic effects from the sample surface. As an application, we demonstrate characteristic changes in the resulting images if different properties of the backscattered electron distribution are used for the analysis of a GaN thin film sample containing dislocations. KW - EBSD KW - Channeling-in KW - Background processing KW - Center of mass KW - Backscattered electrons PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-422063 DO - https://doi.org/10.1111/jmi.12571 SN - 0022-2720 VL - 267 IS - 3 SP - 330 EP - 346 PB - Wiley & Sons, Ltd. AN - OPUS4-42206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian T1 - Synchrotron-Absorptionskantentomographie zur dreidimensionalen Gefügeuntersuchung von Mg-Y-Zn Legierungen T1 - Synchrotron absorption edge tomography for three-dimensional microstructure characterisation of Mg-Y-Zn alloys N2 - Absorptionskantentomographie, auch bekannt als differentielle Tomographie an Kanten, ist ein Verfahren, bei dem ausgenutzt wird, dass sich die Schwächung von Röntgenstrahlen beim Übergang der Photonenenergie über die Absorptionskanten sprunghaft ändert. Die Verwendung von Synchrotronstrahlung ermöglicht die Anwendung der Absorptionskantentomographie für nahezu jedes Element, da sie eine intensive, durchstimmbare Strahlenquelle mit kleiner Bandbreite darstellt. Der Mikrotomographieaufbau der BAM am Elektronenspeicherring BESSY II eignet sich mit einem Energiebereich von 5 keV bis über 60 keV und einer Ortsauflösung besser als 0.5 µm zur differentiellen Tomographie an den K-Kanten der Elemente von Chrom bis zu den Lanthaniden, bei Einbeziehung der L-Kante bis zu Uran. In dieser Arbeit wird die Absorptionskantentomographie ausgenutzt, um das Gefüge von Legierungen dreidimensional und nichtdestruktiv zu vermessen. Als Beispiel wird eine Legierung zwischen Magnesium, Yttrium und Zink analysiert, die sich gegenüber unlegiertem Magnesium durch größere Festigkeit und geringere Korrosionsanfälligkeit auszeichnet. Der Grund dafür liegt in der Bildung einer kristallographisch hochgeordneten Phase (long period stacking ordered - LPSO) der Legierungsbestandteile, die die Matrix in Form von Fasern durchzieht. Anhand ihres Yttriumgehaltes wird die dreidimensionale Verteilung der LPSO-Phase in der Matrix für verschiedene Proben bestimmt und mit Schnittbildern und Korrosionstests verglichen. Die Absorptionskantentomographie erweist sich als eine geeignete Methode, um die dreidimensionale Mikrostruktur von Legierungen zu charakterisieren. T2 - 51. Metallographie-Tagung Materialographie CY - Aalen, Germany DA - 13.09.2017 KW - Tomographie KW - Absorptionskante KW - Legierung KW - Synchrotron PY - 2017 AN - OPUS4-42216 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian A1 - Cabeza, Sandra A1 - Garces, G. ED - Petzow, G. T1 - Synchrotron-Absorptionskantentomographie zur dreidimensionalen Gefügeuntersuchung von Mg-Y-Zn Legierungen N2 - Absorptionskantentomographie, auch bekannt als differentielle Tomographie an Kanten, ist ein Verfahren, bei dem ausgenutzt wird, dass sich die Schwächung von Röntgenstrahlen beim Übergang der Photonenenergie über die Absorptionskanten sprunghaft ändert. Die Verwendung von Synchrotronstrahlung ermöglicht die Anwendung der Absorptionskantentomographie für nahezu jedes Element, da sie eine intensive, durchstimmbare Strahlenquelle mit kleiner Bandbreite darstellt. Der Mikrotomographieaufbau der BAM am Elektronenspeicherring BESSY II eignet sich mit einem Energiebereich von 5 keV bis über 60 keV und einer Ortsauflösung besser als 0.5 µm zur differentiellen Tomographie an den K-Kanten der Elemente von Chrom bis zu den Lanthaniden, bei Einbeziehung der L-Kante bis zu Uran. In dieser Arbeit wird die Absorptionskantentomographie ausgenutzt, um das Gefüge von Legierungen dreidimensional und nichtdestruktiv zu vermessen. Als Beispiel wird eine Legierung zwischen Magnesium, Yttrium und Zink analysiert, die sich gegenüber unlegiertem Magnesium durch größere Festigkeit und geringere Korrosionsanfälligkeit auszeichnet. Der Grund dafür liegt in der Bildung einer kristallographisch hochgeordneten Phase (long period stacking ordered - LPSO) der Legierungsbestandteile, die die Matrix in Form von Fasern durchzieht. Anhand ihres Yttriumgehaltes wird die dreidimensionale Verteilung der LPSO-Phase in der Matrix für verschiedene Proben bestimmt und mit Schnittbildern und Korrosionstests verglichen. Die Absorptionskantentomographie erweist sich als eine geeignete Methode, um die dreidimensionale Mikrostruktur von Legierungen zu charakterisieren. T2 - 51. Metallographie-Tagung Materialographie CY - Aalen, Germany DA - 13.09.2017 KW - Tomographie KW - Absorptionskante KW - Synchrotron KW - Legierung PY - 2017 SN - 978-3-88355-415-0 SP - 177 EP - 178 PB - Deutsche Gesellschaft für Materialkunde eV AN - OPUS4-42218 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Leonhard, H. T1 - Sichere Werkstoffauswahl - Korrosionsschnelltest für nichtrostende Stähle N2 - Anlagenkomponenten aus nichtrostendem Stahl sind durch eine Passivschicht auf der Oberfläche vor Korrosion geschützt. Ist diese unvollständig ausgebildet oder beschädigt, geht der Schutz verloren. Hohe Investitionen für Reparaturen und Instandhaltung können die Folge sein. TÜV Süd Chemie Service beteiligte sich an der Prüfung eines von der Bundesanstalt für Materialforschung und -prüfung (BAM) entwickelten Verfahrens zur Charakterisierung der Korrosionsbeständigkeit der Passivschicht. Der KorroPad-Schnelltest liefert in nur 15 Minuten ein valides Prüfergebnis. KW - Nichtrostender Stahl KW - Korrosionsschnelltest KW - KorroPad KW - Passivschicht PY - 2017 SN - 0720-5953 VL - 69 IS - 11-12 SP - IW10 EP - IW11 PB - Springer-VDI-Verlag GmbH & Co. KG CY - Düsseldorf AN - OPUS4-43228 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Rauscher, H. A1 - Mech, A. A1 - Gaillard, C. A1 - Stintz, M. A1 - Wohlleben, W. A1 - Weigel, St. A1 - Ghanem, A. A1 - Hodoroaba, Vasile-Dan A1 - Babick, F. A1 - Mielke, Johannes T1 - Recommendations on a Revision of the EC Definition of Nanomaterial Based on Analytical Possibilities N2 - In October 2011 the European Commission (EC) published a "Recommendation on the definition of nanomaterial" (2011/696/EU), to promote consistency in the interpretation of the term "nanomaterial" for legislative and policy purposes in the EU. The EC NM Definition includes a commitment to its review in the light of experience and of scientific and technological developments. This review is ongoing in 2015 and as a contribution to the review the Joint Research Centre of the European Commission (JRC) has already developed a series of three scientific-technical reports with the title: “Towards a review of the EC Recommendation for a definition of the term nanomaterial” which provides to the EC policy services science-based options on how the definition could be revised or supported with additional guidance. The overarching nature and wide scope of the EC NM Definition, as it does not exclude a priori any particulate material regardless the state, form and size, creates many analytical challenges in its imple-mentation for all stakeholders, including enterprises and regulators. The NanoDefine project has as core objective to support the implementation of the EC NM Definition. In this report key aspects of the EC NM Definition are addressed, with the goal to improve the implement-ability of the EC NM Definition. These aspects are presented and discussed based on the results of two years of research performed within the framework of the project. As a result this report assesses how well the requirements of the EC NM Definition can be fulfilled with currently available analytical possi-bilities. It presents recommendations and options on a revision of the EC NM Definition to improve the implementability of the definition based on currently available analytical possibilities, according to the state of the art of mid-2015. Of the technical issues considered in this report, the following seem to deserve the most attention in terms of clarification of the definition and/or provision of additional implementation guidance:  The term ‘external dimension’. A clear definition of 'External dimension' should be included in the text of the EC NM definition and more precise guidance on what is considered as an external dimension and how to properly character-ise it should be provided.  The ‘number based particle size distribution‘. The EC NM Definition uses a threshold related to the number based size distribution of particles. Yet most of the easily available techniques provide a mass-, volume- or scattered light intensity-based size distribution which needs to be converted into a number based distribution to be used for regulatory pur-poses. A specific guidance on the conditions under which these methods can be used to identify a na-nomaterial by employing appropriate quantity or metrics conversion should be provided.  The ‘polydispersity‘ and ‘upper size limit‘ Polydispersity is a challenge for the measurement of particle size distribution for the EC NM definition, specifically for materials with high polydispersity index and broad size distribution especially when the volume or mass of the fraction containing particles below 100 nm is very small. Therefore a dedicated guidance should be provided that allows applying an upper size limit in measurements and particle statistics. KW - Nanomaterial KW - EU Definition of nanomaterial KW - Nanoparticles PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-432339 UR - http://www.nanodefine.eu/publications/reports/NanoDefine_TechnicalReport_D7.10.pdf SP - 1 EP - 68 PB - The NanoDefine Consortium CY - Wageningen, The Netherlands AN - OPUS4-43233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Terril, N. J. A1 - Thünemann, Andreas T1 - The modular small-angle X-ray scattering data correction sequence N2 - Data correction is probably the least favourite activity amongst users experimenting with small-angle X-ray scattering: if it is not done sufficiently well, this may become evident only during the data analysis stage, necessitating the repetition of the data corrections from scratch. A recommended comprehensive sequence of elementary data correction steps is presented here to alleviate the difficulties associated with data correction, both in the laboratory and at the synchrotron. When applied in the proposed order to the raw signals, the resulting absolute scattering cross section will provide a high degree of accuracy for a very wide range of samples, with its values accompanied by uncertainty estimates. The method can be applied without modification to any pinhole-collimated instruments with photon-counting direct-detection area detectors. KW - Small-angle X-ray scattering KW - SAXS KW - Accuracy KW - Methodology KW - Data correction PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-432114 DO - https://doi.org/10.1107/S1600576717015096 SN - 1600-5767 VL - 50 IS - 6 SP - 1800 EP - 1811 PB - International Union of Crystallography AN - OPUS4-43211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gunella, F. A1 - Kunisch, E. A1 - Bungartz, M. A1 - Maenz, S. A1 - Horbert, V. A1 - Xin, L. A1 - Mika, J. A1 - Borowski, J. A1 - Bischoff, S. A1 - Schubert, H. A1 - Hortschansky, P. A1 - Sachse, A. A1 - Illerhaus, Bernhard A1 - Günster, Jens A1 - Bossert, J. A1 - Jandt, K. D. A1 - Plöger, F. A1 - Kinne, R. W. A1 - Brinkmann, O. T1 - Low-dose BMP-2 is sufficient to enhance the bone formation induced by an injectable, PLGA fiber-reinforced, brushite-forming cement in a sheep defect model of lumbar osteopenia N2 - BACKGROUND CONTEXT: Bioresorbable calcium phosphate cement (CPC) may be suitable for vertebroplasty/kyphoplasty of osteoporotic vertebral fractures. However, additional targeted de- livery of osteoinductive bone morphogenetic Proteins (BMPs) in the CPC may be required to counteract the augmented local bone catabolism and support complete bone regeneration. PURPOSE: This study aimed at testing an injectable, poly (l-lactide-co-glycolide) acid (PLGA) fiber-reinforced, brushite-forming cement (CPC) containing low-dose bone morphogenetic Protein BMP-2 in a sheep lumbar osteopenia model. STUDY DESIGN/ SETTING: This is a prospective experimental animal study. METHODS: Bone defects (diameter 5 mm) were generated in aged, osteopenic female sheep and filled with fiber-reinforced CPC alone (L4; CPC+ fibers) or with CPC containing different dosages of BMP-2 (L5; CPC+ fibers + BMP-2; 1, 5, 100, and 500g BMP-2; n=5 or 6 each). The results were compared with those of untouched controls (L1). Three and 9 months after the operation, structural and functional effects of the CPC (±BMP-2) were analyzed ex vivo by measuring (1) bone Mineral density (BMD); (2) bone structure, that is, bone volume/total volume (assessed by micro-computed tomography [micro-CT] and histomorphometry), trabecular thickness, and trabecular number; (3) bone formation, that is, osteoid volume/bone volume, osteoid surface/bone surface, osteoid thickness, mineralizing surface/bone surface, mineral Apposition rate, and bone formation rate/bone surface; (4) bone resorption, that is, eroded surface/bone surface; and (5) compressive strength. RESULTS: Compared with untouched controls (L1), CPC+ fibers (L4) and/or CPC+ fibers + BMP-2(L5) significantly improved all parameters of bone formation, bone resorption, and bone structure. These effects were observed at 3 and 9 months, but were less pronounced for some parameters at 9 months. Compared with CPC without BMP-2, additional significant effects of BMP-2 were demonstrated for bone structure (bone volume/total volume, trabecular thickness, trabecular number) and formation (osteoid surface/bone surface and mineralizing surface/bone surface), as well as for the compressive strength. The BMP-2 effects on bone Formation at 3 and 9 months were dose-dependent, with 5–100g as the optimal dosage. CONCLUSIONS: BMP-2 significantly enhanced the bone formation induced by a PLGA fiber-reinforced CPC in sheep lumbar osteopenia. A single local dose as low as ≤100g BMP-2 was sufficient to augment middle to long-term bone formation. The novel CPC+ BMP-2 may thus represent an alternative to the bioinert, supraphysiologically stiff polymethylmethacrylate cement presently used to treat osteoporotic vertebral fractures by vertebroplasty/kyphoplasty. KW - Bone regeneration KW - Computed tomography KW - Calcium phosphat cement KW - Large animal model sheep KW - Osteoporotic vertebral fracture PY - 2017 DO - https://doi.org/10.1016/j.spinee.2017.06.005 SN - 1529-9430 SN - 1878-1632 VL - 17 IS - 11 SP - 1699 EP - 1711 PB - Elsevier Inc. AN - OPUS4-43237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Detjens, Marc A1 - Hübert, Thomas T1 - Messunsicherheit coulometrischer Spurenfeuchtesensoren N2 - Die Spurenfeuchte von technischen Gasen kann zuverlässig mit coulometrischen Feuchtesensoren bestimmt werden. Das Prinzip dieser Sensoren basiert auf der Absorption von Wasser in einer hygroskopischen Schicht und anschließenderelektrolytischer Zersetzung. Die Kalibrierung der Sensoren erfolgte mit einem Spurenfeuchtegenerator bei Frostpunkttemperaturen kleiner als -30 °C bzw. einem Volumenanteil kleiner als 376 µL·L-1. Die generierte Feuchte wurde zusätzlich zu den coulometrischen Sensoren mit einem Taupunktspiegelhygrometer, welches als Referenz diente, gemessen. Zwischen dem coulometrischen Sensorsignal und der gemessenen Referenzfeuchte wurde eine empirische nichtlinare Funktion gefunden. Die resultierende Kalibrierungsfunktion, die aus zwei Parametern besteht, wurde hinsichtlich ihrer Messunsicherheit bewertet. Zusätzlich erfolgt die Überprüfung der Kalibrierparameter mittels einfaktorieller Varianzanalyse (ANOVA). Die ANOVA zeigte, dass eine gemittelte Funktion für die Feuchtigkeitbestimmung in Stickstoff, Helium und synthetischer Luft für mehrere Sensoren angewendet werden kann. Mit coulmetrischen Sensoren ist es möglich, die Spurenfeuchte in technischen Gasen mit einer erweitereten Unsicherheit hinsichtlich der Frostpunkttemperatur kleiner als 2,1 K zu ermitteln. T2 - 8. VDI-Fachtagung Messunsicherheit CY - Erfurt, Germany DA - 15.11.2017 KW - Spurenfeuchte KW - Messunsicherheit KW - Gasfeuchte PY - 2017 AN - OPUS4-43238 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc A1 - Hübert, Thomas A1 - Tiebe, Carlo A1 - Banach, Ulrich T1 - Temperature influence on coulometric trace humidity measurement N2 - Planar coulometric sensors were tested in humidified synthetic air at various gas temperatures. Generated frost point temperature in the gas ranged from -30 °C to -60 °C and were measured by coulometric sensors and in addition by a calibrated dew point hygrometer. The gas temperatures, which were measured by a calibrated Pt100 sensor, were set to -20 °C, 0 °C, 23 °C, 40 °C, 50 °C, and 60 °C during the experiments. Empiric nonlinear functions were calculated between the generated humidity and the sensor signals. In comparison to the measured signals at 23 °C, the sensor signals were lower at the other gas temperatures. The measurements at 60 °C showed indistinct results due to a great signal noise. The response behavior of the sensors was similar at 23 °C, 40 °C and 50 °C. In contrast to that, the sensors reacted slowly at a gas temperature of -20 °C and 0 °C. In summary, with coulometric sensors it was possible to measure continuously trace humidity with an expanded uncertainty below 2 K. T2 - IEEE Sensors 2017 CY - Glasgow, Scotland, UK DA - 30.10.2017 KW - Response behavior KW - Coulometric sensors KW - Trace humidity measurement KW - Temperature influence KW - Chemical reaction PY - 2017 SN - 978-1-5386-4056-2 SP - 1308 EP - 1310 PB - IEEE CY - Piscataway, NJ, USA AN - OPUS4-43241 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gürlich, L. A1 - Kruschwitz, Sabine A1 - Halisch, M. A1 - Weller, Andreas T1 - SIP Messungen an Fontainebleau Sandsteinen N2 - Die Methode der Spektral Induzierten Polarisation (SIP) wird eingesetzt, um hydraulische Parameter wie Porosität und Permeabilität von Gesteinen abzuleiten. Dabei wird ein Wechselstrom im Bereich von 1 mHz bis 45 kHz in das Gestein eingespeist und die Phasenverschiebung zwischen elektrischem Strom und Spannung gemessen, woraus die komplexe Leitfähigkeit berechnet wird. In dieser Arbeit werden die komplexen Leitfähigkeiten von Fontainebleau Sandsteinen mittels einer am Leibnitz-Institut für Angewandte Geophysik (LIAG) hergestellten Messzelle und einer SIP Apparatur des Forschungszentrums Jülich (FZJ) gemessen. Die Fontainebleau Sandsteine stammen aus Frankreich, südlich von Paris und zeichnen sich durch eine nahezu homogene Zusammensetzung aus Quartz aus. Für die Messungen wurden vier Blöcke mit jeweils vier Proben ausgewählt, die in Porosität und Permeabilität variieren. Für die SIP-Messungen werden die Gesteinsproben mit Natriumchlorid Lösung unterschiedlicher Leitfähigkeiten gesättigt, um die Abhängigkeit der IP-Spektren von der Leitfähigkeit des Porenfluids zu untersuchen. Die Messungen werden mit anderen petrophysikalischen Untersuchungen ergänzt, wie z.B. der Bestimmung der Porenradienverteilung mittels Quecksilberporosimetrie und der spezifischen inneren Oberfläche mit Gassorption (BET). Mit dem Raster-Ektronen-Mikroskop werden hochauflösende Bilder der inneren Gesteinsstruktur erzeugt und ausgewertet. Erste Ergebnisse der SIP-Messungen zeigen deutliche Phasenmaxima im niederfrequenten Bereich, die hinsichtlich ihrer Amplitude und Frequenzlage zwischen den Blöcken variieren. Ziel der Arbeit ist eine systematische Untersuchung der Polarisationseigenschaften bezüglich der Variabilität von Porosität, Porenradienverteilung, spezifischen inneren Oberfläche und Fluidleitfähigkeit, um die Zusammenhänge qualitativ und quantitativ zu charakterisieren. T2 - 77. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Potsdam, Germany DA - 27.03.2017 KW - Spektral Induzierte Polarisation KW - Fontainebleau Sandstein PY - 2017 AN - OPUS4-43243 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Büchele, Dominique T1 - Herausforderungen bei der Quantifizierung von Nährstoffgehalten in Böden mittels RFA N2 - Mit wachsenden Bevölkerungszahlen steigt auch der Rohstoffkonsum, und der nachhaltigere und effizientere Umgang mit knappen Ressourcen wie Wasser und Boden rückt in den Fokus. Im Rahmen der vom Bundesministerium für Bildung und Forschung (BMBF) geförderten Forschungsinitiative BonaRes werden Strategien entwickelt, um Boden als nachhaltige Ressource in der Bioökonomie zu nutzen. Das interdisziplinäre Teilprojekt I4S – Intelligence for soil – ist dabei für die Entwicklung eines integrierten Systems zum ortsspezifischen Management der Bodenfruchtbarkeit zuständig. Hierfür wird eine Plattform gebaut, auf der verschiedene Sensoren installiert werden sollen, deren in Echtzeit erhaltene Messdaten in Modelle und Entscheidungsalgorithmen zur Steuerung der Düngung und dementsprechend Verbesserung der Bodenfunktionen einfließen sollen. Einer dieser Sensoren, auf dessen Grundlage ein robustes Online-Verfahren zur Bestimmung der Makro- und Mikronährstoffe, wie Ca oder K in Böden entwickelt werden soll, ist die Röntgenfluoreszenzanalyse (RFA). Um Messungen auf einem Feld zu simulieren, wurde in einen Laboraufbau ein Probenteller installiert, der sich bei verschiedenen Winkelgeschwindigkeiten bewegen lässt und so dynamisches Messen der als Spur aufgetragenen Probe ermöglicht. So kann der Aufwand der Probenvorbereitung minimiert werden. Gerade bei einer komplexen Matrix wie Boden, die eine breite Elementverteilung aufweist, ist die Datenauswertung ein wichtiger Faktor. Die bisher verwendete univariate Datenanalyse liefert gute Ergebnisse und zeigt, dass durch Kalibrierung der RFA mit 14 Referenzmaterialien große Ackerflächen ausgewertet werden können. Dies funktioniert aber nur, solange die Elementgehalte der Proben mit denen der Referenzmaterialien vergleichbar sind. Die zusätzlich verwendete multivariate Datenanalyse bietet hingegen die Möglichkeit, Modellrechnungen der Böden durchzuführen und Böden mithilfe der Hauptkomponentenanalyse (PCA) besser zu klassifizieren. Des Weiteren können basierend auf der Partial Least Squares Regression (PLSR) Kalibriermodelle erstellt werden, welche Prognosen zu den Elementgehalten unbekannter Ackerböden ermöglichen. Zusätzlich bietet die multivariate Datenanalyse die Möglichkeit, Störgrößen wie unterschiedliche Korngrößenverteilung und Feuchtigkeitsgrad der Probe in das Modell miteinzubeziehen. Beide Auswertemethoden sollen anhand statisch gemessener Proben verglichen werden und durch Messung einer Vielzahl realer Bodenproben von unterschiedlichen Standorten erweitert werden. Im weiteren Verlauf müssen beide Modelle auf dynamisch bewegte Proben übertragen werden. T2 - PRORA CY - Berlin, Germany DA - 30.11.2017 KW - RFA KW - Boden KW - Nährstoffe KW - PCA KW - PLSR PY - 2017 AN - OPUS4-43159 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Krop, U. A1 - Scherz, Franziska A1 - Weller, Michael G. A1 - Monks, K. T1 - Fast and robust purification of antibodies from human serum with a new monolithic protein A column N2 - The use of antibodies is becoming more and more important. Therewith the need for fast and robust methods for their purification and columns with a long lifetime is growing. In this application, we describe a fast and robust protein A affinity chromatography method with a new monolithic column. Antibodies were successfully purified in less than 1.5 minutes with a flowrate of 5 mL/min highlighting the advantages of this column and method. KW - Antibodies KW - Protein A KW - MNPQ KW - Technology transfer KW - Human serum KW - Purification KW - IgG KW - SDS PAGE KW - Regeneration PY - 2017 UR - http://www.knauer.net/en/application/fast_and_robust_purification_of_antibodies_from_human_serum_with_a_new_monolithic_protein_a_column.html SP - 1 EP - 2 PB - Knauer CY - Berlin AN - OPUS4-43163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stroh, Julia T1 - In situ cement hydration in levitated droplets N2 - Building materials consist of cement, water and chemical admixtures, which adjust cement paste properties. They can act beyond their aimed functions causing changes in hydration course. The mechanisms are still under investigation. We investigate cement hydration in levitated droplets using an ultrasonic levitator. Hydrate phase formation is followed in situ by synchrotron XRD. The data allows detailed conclusions about the mechanisms of the admixture action in the ongoing hydration reactions. T2 - 7th GACM Colloquium on Computational Mechanics CY - Stuttgart, Germany DA - 11.10.2017 KW - Portland cement KW - Hydration KW - Levitation KW - Admixtures PY - 2017 AN - OPUS4-43165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stroh, Julia T1 - Direct insight into the admixture activity during cement hydration using levitated droplets N2 - Chemical admixtures are widely used to adjust properties of the cementitious mixtures. Different superplasticizers (SP) are typically added to improve the flowability of the fresh cement paste. Their working period is the initial stage of the cement hydration from its beginning until stiffening. Currently, polycarboxylate-based SP (PCE-SP) are the most effective ones. They can act beyond their aimed function causing changes in the hydration course, e. g. retardation effects. The exact mechanisms and influencing factors are still under investigation. However, the occurrence of the retardation effect indicates the involvement of PCE in the hydration reactions. Some observations indicate, that the retardation depends on the type, molecular structure and concentration of PCE, and the presence of other admixtures (stabiliser, ST). These factors influence further the working time of admixture and its amount related efficacy in the flow improvement. We investigate the cement hydration process in situ in levitated droplets. High resolution synchrotron X-ray diffraction allows gathering temporal course of the hydration reactions. The measurement setup is based on an ultrasonic levitator allowing in situ investigation of the temporal changes of the phase composition in the hydrating cementitious system. Further, the hydration can be followed ab initio avoiding the time loss for the sample preparation and filling in the sample holder. The collected data allows to conclude about the mechanisms of the admixture action and their involvement into the ongoing hydration process. T2 - 2nd International Conference on Polycarboxylate Superplasticizers (PCE 2017) CY - München, Germany DA - 27.09.2017 KW - Portland cement KW - Initial hydration KW - Acoustic levitator KW - Admixtures KW - Time resolution PY - 2017 AN - OPUS4-43166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stroh, Julia A1 - Emmerling, Franziska ED - Plank, J. ED - Lei, L. T1 - Direct insight into the admixture activity during cement hydration using levitated droplets N2 - Chemical admixtures are widely used to adjust properties of the cementitious mixtures. Different superplasticizers (SP) are typically added to improve the flowability of the fresh cement paste. Their working period is the initial stage of the cement hydration from its beginning until stiffening. Currently, polycarboxylate-based SP (PCE-SP) are the most effective ones. They can act beyond their aimed function causing changes in the hydration course, e. g. retardation effects. The exact mechanisms and influencing factors are still under investigation. However, the occurrence of the retardation effect indicates the involvement of PCE in the hydration reactions. Some observations indicate, that the retardation depends on the type, molecular structure and concentration of PCE, and the presence of other admixtures (stabiliser, ST). These factors influence further the working time of admixture and its amount related efficacy in the flow improvement. We investigate the cement hydration process in situ in levitated droplets. High resolution synchrotron X-ray diffraction allows gathering temporal course of the hydration reactions. The measurement setup is based on an ultrasonic levitator allowing in situ investigation of the temporal changes of the phase composition in the hydrating cementitious system. Further, the hydration can be followed ab initio avoiding the time loss for the sample preparation and filling in the sample holder. The collected data allows to conclude about the mechanisms of the admixture action and their involvement into the ongoing hydration process. T2 - 2nd International Conference on Polycarboxylate Superplasticizers (PCE 2017) CY - München, Germany DA - 28.09.2017 KW - Portland cement KW - Initial hydration KW - Acoustic levitator KW - Admixtures KW - Time resolution PY - 2017 SN - 978-3-9816240-6-9 SP - 185 EP - 193 AN - OPUS4-43167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tvrdoňová, M. A1 - Ascher, Lena T1 - A new strategy of reagents labeling (NPs) used in immunoassay with LA-ICP-MS N2 - Laser ablation with inductively coupled plasma is still more used in life science as biology and biomedicine and the utilization of metals and proteins determination simultaneously is also growing up. We have developed a new strategy of labeling of antibody (it can specific binds to proteins) by nanoparticles and quantum dots which is composed of thousands of atoms and thus increases the sensitivity enormously and of course decreases the Limit of detection, compare to lanthanoids labeling. The ability of successfully tagged antibodies bound to Antigen (protein) was proved by dot blot on membrane imaged by LA-ICP-MS. T2 - Euroanalysis 2017 CY - Stockholm, Sweden DA - 28.08.2017 KW - Immunoassay KW - LA-ICP-MS KW - Labeling KW - Nanoparticle PY - 2017 AN - OPUS4-43168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hiller, Th. A1 - Costabel, S. A1 - Müller-Petke, M. A1 - Kruschwitz, Sabine T1 - Evaluation of different laboratory NMR devices in a tripartite round robin test N2 - Nuclear magnetic resonance (NMR) is a well established laboratory / borehole method to characterize the storage and transport properties of rocks due to its direct sensitivity to the corresponding pore fluid saturation (water or oil) and pore sizes. For petrophysical applications there are several different NMR laboratory devices commercially available varying over a wide range of e.g. magnetic field strength / frequency (2 MHz to 30 MHz), applicable measurement protocols (T1, T2, T1-T2, T2-D, etc.) and sample sizes (2.5 cm to 10 cm in diameter). In this work we present NMR measurements, layed out in a round robin like manner, on a set of 20 sandstone samples. We use three different NMR devices containing two standard setups with homogenous magnetic fields (LIAG and RWTH) and one single-sided setup with gradient field (BGR) to measure T1 and T2 relaxation data. In our evaluation we especially focus on the comparison of the individually inverted relaxation time distributions to quantify the differences arising from different laboratory setups. Diverging results can be deduced on the one hand to the inherit differences between homogeneous and gradient fields but on the other hand also due to quality differences between the two homogeneous setups. Additionally, we also examine the influence of the individually chosen inversion parameters (signal processing, distribution sampling points, error weighting, regularization, etc.) to establish a general standardized best practice recommendation for future petrophysical NMR laboratory measurements. T2 - 77. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Potsdam, Germany DA - 27.03.2017 KW - Nuclear Magnetic Resonance KW - Sandstone PY - 2017 AN - OPUS4-43244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zhang, Zeyu A1 - Kruschwitz, Sabine A1 - Prinz, Carsten A1 - Halisch, M. A1 - Weller, Andreas T1 - Porenraumanalyse mittels MIP, NMR, SIP, BET, CT und Auflichtmikroskopie N2 - In der Vergangenheit wurde immer wieder diskutiert, ob die Porenhalsverteilung poröser silikatischer Medien maßgeblich die Relaxationszeit in Messergebnissen der Spektralen Induzierten Polarisation (SIP) bestimmt und dementsprechend auch neuere Ansätze, Porenweitenverteilungen aus diesen Daten abzuleiten, zuverlässig sein können. Systematische Studien an Gesteinen mit sehr unterschiedlichen Porenverteilungen zeigten, dass in Materialien mit engen Porenhälsen (z.B. < 5 μm) vor allem oder zusätzlich zum vermuteten Porenhalspeak niederfrequente Relaxationen zu beobachten sind, deren Ursache noch unklar ist. Unter Einbeziehung der Methoden Röntgen-Computertomografie (μ-CT), Quecksilberporosimetrie (MIP), Stickstoffabsortion, Nukleare Magnetische Resonanz, SIP und Auflichtmikroskopie untersuchen wir den Porenraum hinsichtlich der Parameter Porosität, Permeabilität und innere Oberfläche und bestimmen die geometrischen Eigenschaften wie Porenweitenverteilungen oder fraktale Dimension durch verschiedene Algorithmen. Dabei ist zu berücksichtigen, dass sich die Methoden hinsichtlich der Grenzen ihres Auflösungsvermögens unterscheiden. Mit einer Zusammenführung der Ergebnisse aller Methoden kann eine mehrere Längenskalen überdeckende Charakterisierung der Porenraumgeometrie erfolgen. Die Anwendung und Auswertung der verschiedenen Methoden werden am Beispiel von Baumberger Kalksandstein und Bentheimer Sandstein verglichen und diskutiert. T2 - 77. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Potsdam, Germany DA - 27.03.2017 KW - Spektral Induzierte Polarisation KW - Fraktale Dimension KW - MIP KW - Sandstein PY - 2017 AN - OPUS4-43246 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Zeyu A1 - Weller, Andreas A1 - Kruschwitz, Sabine T1 - Pore radius distribution and fractal dimension derived from spectral induced polarisation N2 - The pore size distribution provides a suitable description of the pore space geometry that can be used to investigate the fractal nature of the pore space or to determine a fractal dimension. Fractal dimension describes the size of geometric objects as a function of resolution. It can be integrated into models of permeability prediction. We investigated the fractal dimension of the pore volume of 11 Eocene sandstone samples from China. This study describes an approach to use spectral induced polarisation spectra to estimate the pore size distribution and to determine the fractal dimension of the pore volume. Additionally, the fractal dimension was derived from data of the capillary pressure curves from mercury intrusion and the transversal relaxation time distribution of nuclear magnetic resonance. For samples with an effective pore radius larger than 1 μm, good agreement exists between the values of fractal dimension derived from the three different methods, which implies the identification of similar pore structures. Spectral induced polarisation can be a non-invasive laboratory technique for the estimation of the pore size distribution, but the application of the methodology for field measurements remains a challenging problem considering the limited frequency range. KW - Pore radius distribution KW - Fractal dimension KW - Spectral induced polarization PY - 2017 DO - https://doi.org/10.3997/1873-0604.2017035 SN - 1569-4445 VL - 15 IS - 6 SP - 625 EP - 632 PB - Wiley AN - OPUS4-43250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Gräßer, Patrick A1 - Wander, Lukas A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Kern, Simon T1 - Innen hui und außen pfui – Smarte Prozess-Sensoren in der gegenwärtigen Automatisierungslandschaft der Prozessindustrie N2 - Der Wandel von der aktuellen Automation zum smarten Sensor ist im vollen Gange. Automatisierungstechnik, sowie die Informations- und Kommunikationstechnik (IKT) verschmelzen zunehmend. Eine Topologie für smarte Sensoren, die das Zusammenwirken mit daten- und modellbasierten Steuerungen bis hin zur Softsensorik beschreibt gibt es bis heute jedoch noch nicht. Um zu einer störungsfreien Kommunikation aller Komponenten auf Basis eines einheitlichen Protokolls zu kommen sollte die Prozessindustrie die Weichen für eine smarte und sichere Kommunikationsarchitektur stellen. Sie verwehrt stattdessen die Entwicklungen ihrer Zulieferer und wartet lieber ab. Der Beitrag greift die Anforderungen der Technologie-Roadmap „Prozess-Sensoren 4.0“ auf und zeigt Möglichkeiten zu ihrer Realisierung am Beispiel eines Online-NMR-Analysators, der im Rahmen eines EU-Projekts entwickelt wurde. T2 - 13. Dresdner Sensor Symposium CY - Dresden, Germany DA - 04.12.2017 KW - Smarte Feldgeräte KW - Process Control KW - Modulare Produktion KW - Online-NMR-Spektroskopie KW - Indirect Hard Modeling KW - Industrie 4.0 PY - 2017 UR - https://www.ama-science.org/proceedings/details/2717 SN - 978-3-9816876-5-1 DO - https://doi.org/10.5162/13dss2017/2.1 SP - 61 EP - 66 PB - AMA Service GmbH CY - Berlin AN - OPUS4-43252 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Wander, Lukas A1 - Paul, Andrea A1 - Maiwald, Michael T1 - Mathematical and statistical tools for online NMR spectroscopy in chemical processes N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied, which require excessive calibration effort. NMR spectroscopy has a high potential for direct loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environments for advanced process Monitoring and control, as demonstrated within the European Union’s Horizon 2020 project CONSENS. We present a range of approaches for the automated spectra analysis moving from conventional multivariate statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). By using the benefits of traditional qNMR experiments data analysis models can meet the demands of the PAT community (Process Analytical Technology) regarding low calibration effort/calibration free methods, fast adaptions for new reactants or derivatives and robust automation schemes. T2 - 13. Dresdner Sensor Symposium CY - Dresden, Germany DA - 04.12.2017 KW - Online NMR spectroscopy KW - Process control KW - Partial least squares regression KW - Indirect hard modeling KW - Quantum mechanics KW - First principles PY - 2017 UR - https://www.ama-science.org/proceedings/details/2748 SN - 978-3-9816876-5-1 DO - https://doi.org/10.5162/13dss2017/P2.07 SP - P2, 209 EP - 212 PB - AMA Service GmbH CY - Berlin AN - OPUS4-43254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Leonhard, H. T1 - Schnelltest auf Korrosionsgefahr - KorroPad N2 - Rostfreie Stähle werden in prozesstechnischen Anlagen oft extremen Umgebungsbedingungen ausgesetzt. Eine schützende Passivschicht an der Oberfläche nichtrostender Stähle sorgt dafür, dass es zu keiner Materialauflösung kommt. Wenn diese unvollständig oder beschädigt ist, kann es zu Komplikationen kommen. Lesen Sie im Artikel, wie die von TÜV SÜD Chemie Service erprobte Methode funktioniert, mit der die Passivschicht überprüft werden kann. KW - Nichtrostender Stahl KW - Korrosionsschnelltest KW - KorroPad KW - Passivschicht PY - 2017 SN - 2198-0691 IS - 4 SP - 84 EP - 85 PB - Fachwelt Verlag CY - Stuttgart AN - OPUS4-43185 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haas, Marko T1 - Steuerung von Risiken N2 - Der Vortrag skizziert die Herausforderungen bei der Einführung und Umsetzung des Risikomanagements in öffentlichen Institutionen. Exemplarisch wird dabei auf die Erfahrungen bei der Einführung des Risikomanagements bei der BAM eingegangen. T2 - Tagung des Arbeitskreises Steuerung und Controlling in öffentlichen Institutionen CY - Berlin, Germnany DA - 08.11.2017 KW - Risikomanagement KW - Strategisches controlling KW - Erfahrungsbericht PY - 2017 AN - OPUS4-43188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Application of LIBS for the chemical investigation of concrete infrastructure N2 - The majority of the built infrastructure is made of concrete, which is a multiphase system made of cement, aggregates, water and pores (every year nearly 4 billion tons of cement are produced which is largest mass flow generated by mankind). Concrete is often used in combination with steel as reinforced concrete. Environmental influences, especially the ingress of harmful ions in combination with the ingress of water, trigger different damage processes which reduce the designed lifetime of a structure. The ingress of chlorides from de-icing salt or sea water leads to corrosion of the reinforcement. Also the carbonation of the concrete may trigger the corrosion of the reinforcement. The ingress of alkalis from de-icing salts may cause the expansion of the amorphous silica aggregates (alkali-silica reaction) through formation of a swelling gel of calcium silicate hydrate if water is present. The ingress of sulfates may cause spalling of the concrete surface due to ett-ringite formation. For the standard procedure in civil engineering cores are taken, cut in slices, grinded and the obtained homogenized powder is solved in acid and investigated by standard procedures. BAM has developed the LIBS technique for the 2D evaluation of the chemical composition of concrete [1-5]. The technique is established for automated laborato-ry use with high numbers of samples to investigate transport processes of harmful species (Cl-, CO2, SO42- and alkalis) in concrete. Information about ingress depth and the quantitative values are important to estimate the remaining lifetime of the infrastructure. LIBS is a surface technique. To get information about the ingress depth, a core has to be taken and cut in the middle. The measurements are carried out at the cross section. The main advantages of LIBS are the direct measure-ment on the surface of the concrete, fast analysis (sample rate 100 Hz) with a spatial resolution of up to 100 μm, the consideration of the heterogeneity of the concrete and the possibility of automated measurements which save a lot of man-power and time. As an example the investigation of ingress profiles for standard diffusion and migration tests in civil engi-neering takes hours in comparison to just a few minutes using LIBS. At the same time a 2D-evaluation provides information about hot spots of elemental concentration which may not be found by standard methods. The state of the art of LIBS technique for applications in civil engineering will be presented, including typical results of 2D investigation of concrete in laboratory. The performance is also demonstrated by examples for on-site applications using a mobile LIBS system. The road map to standardization is presented as well. T2 - 9th Euro-Mediterranean Symposium on LIBS / Colloquium Spectroscopicum Internationale XL CY - Pisa, Italy DA - 12.06.2017 KW - ASR KW - LIBS KW - Concrete KW - Chlorid KW - Carbonation PY - 2017 AN - OPUS4-43194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Bartholmai, Matthias A1 - Neumann, Patrick P. T1 - Multifunktionaler Sensor zur Überwachung von Untergrundspeichern durch flächendeckendes ortsaufgelöstes Monitoring von Gasen, Temperatur und Gefügebewegungen im Boden N2 - Untergrundspeicher für Roh- und Abfallstoffe gewinnen zunehmend an Bedeutung. Verwendet werden sie vor allem für Stoffe wie Erdgas, Wasserstoff, Erdöl und neuerdings auch für Kohlen-stoffdioxid (CO2). Diese Stoffe werden meist unter Druck in Kavernen- oder Porenspeichern einge-lagert. Die Speicher dienen einerseits zum Ausgleich von Ungleichgewichten zwischen Ange-bot/Förderung und Nachfrage/Verbrauch und zur Erhöhung der Versorgungssicherheit. Anderer-seits bestehen Konzepte Abfallstoffe oder Gefahrstoffe für die Umwelt (aktuell CO2-Speicherung) dort für lange Zeiträume einzulagern. Mit den Einlagerungsstoffen verbunden ist ein signifikantes Gefahrenpotential für Mensch und Umwelt, falls es trotz aller Sicherheitsmaßnahmen zu einem unkontrollierten Austritt dieser Stoffe kommen sollte. Daher kommt dem Monitoring derartiger Untergrundspeicher und den darüber befindlichen Bodenstrukturen eine extrem hohe Bedeutung zu. Ein hochaktuelles Beispiel, das die Überwachung entsprechender Bodenflächen fordert, ist die unterirdische CO2-Speicherung im Rahmen der CO2-Abscheidung und -Speicherung (Carbon Dioxide Capture and Storage, CCS). CCS gilt als wichtige Brückentechnologie der Energiewirtschaft und wird weltweit vorangetrieben, während die Sicherheit von Bevölkerung und Biosphäre noch kont-rovers diskutiert wird. Auch die EU setzt auf CCS und gibt in der EU-Richtlinie 2009/31 als Ziel-setzung bis 2015 vor, 15 Pilotanlagen zu bauen und in Betrieb zu nehmen. Als Bedingung für die Genehmigung der CO2-Speicherung ist explizit die Überwachung der Speicheranlagen durch Monito-ring vorgeschrieben, wobei die technisch besten Lösungen zum Einsatz kommen sollen. Das zu entwickelnde Messsystem adressiert neben den o.g. Anwendungsfeldern weitere, bei denen insbesondere die Emission von Gasen ein Risiko für Mensch und Umwelt darstellt oder wirt-schaftlichen Schaden verursachen kann. Hierzu zählen die Überwachung von Abfalldeponien, Ge-fahrgutlagerstätten, kontaminierten Altlastengebieten, Moor-, Torf-, Kohleflözen (präventive Branderkennung) und geodynamisch aktiven Regionen. Auch moderne Fördertechnologien, wie das Hot-Dry-Rock-Verfahren (HDR) zur Energiegewinnung durch Einpressen von überkritischem CO2 in den Erdkörper, das die Beweglichkeit eines Gases mit der Dichte einer Flüssigkeit kombiniert und Wärmeaustausch im Erdinneren bewirkt, bergen das Risiko unkontrollierter Gasemissionen und bedürfen der umfassenden Überwachung. KW - Verteilte Sensorik KW - Gassensor KW - CCS KW - Gasspeicher PY - 2015 DO - https://doi.org/10.2314/GBV:867138327 SP - 1 EP - 13 AN - OPUS4-43195 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - SILAMARK – Qualitätssicherung einer Tiefenhydrophobierung vor-Ort N2 - Stahlbetonbauwerke der Verkehrsinfrastruktur sind nutzungsbedingt Expositionen ausgesetzt, die zu Schä-den an der Konstruktion führen können. Dabei ist in erster Linie die Einwirkung von tausalzhaltigen Wässern im Winter zu nennen, die durch den Beton kapillar und über Diffusionsvorgänge aufgenommen werden. Ein Weg, die kapillare Wasseraufnahme zu unterbinden, ist eine Tiefenhydrophobierung der Werkstoffoberflä-chen durch siliziumorganische Verbindungen. Die Wirksamkeit und die Dauerhaftigkeit dieser Tiefenhydro-phobierungen werden im Wesentlichen durch die Eindringtiefe und den Wirkstoffgehalt in der Betonrandzone bestimmt. Diese beiden Parameter gilt es also in der Qualitätssicherung zu überprüfen. Bisherige Verfahren zur Qualitätssicherung einer hydrophobierenden Maßnahme sind mit einer Bohrkernent-nahme verbunden, da die Analysen im Labor durchgeführt werden müssen. Andere Verfahren arbeiten zwar zerstörungsfrei und können am Objekt durchgeführt werden, liefern aber keine Informationen über die Ein-dringtiefe und die Wirkstoffverteilung. Das Fehlen eines geeigneten Qualitätssicherungs-Verfahrens hat eine breite praktische Anwendung der als technisch sehr leistungsfähig geltenden Tiefenhydrophobierungen bisher verhindert. Im Rahmen eines vom BMBF geförderten Forschungsvorhabens wurde ein Verfahren entwickelt mit dem direkt vor Ort das Vorhandensein der Tiefenhydrophobierung nachgewiesen und die Wirkstoffverteilung in der Betonrandzone detektiert werden kann. Da der chemische Kontrast einer Tiefenhydrophobierung zum Beton gering ist mussten „reaktive Marker“ entwickelt werden, die an das eigentliche Hydrophobierungsmittel chemisch gebunden wurden. Mit dem Verfahren der „Laser Induced Breakdown Spetroscopy“ (LIBS) konnte dann die Verteilung des als Marker verwendeten Elementes, und damit der Wirkstoffgehalt in der Betonrand-zone qualitativ und quantitativ bestimmt werden. Das Vorhaben SILAMARK wurde als Verbundprojekt unter Beteiligung der Sto SE & Co. KGaA, der Bundes-anstalt für Materialforschung und –prüfung, der Hochschule Karlsruhe – Technik und Wirtschaft (HsKa), der Aqua Stahl GmbH und der Specht Kalleja + Partner Beratende Ingenieure GmbH realisiert. T2 - Deutscher Beton- und Bautechnik-Verein E.V. Tag der Forschung CY - Berlin, Germany DA - 13.10.2017 KW - Beton KW - Tiefenhydrophobierung KW - LIBS KW - Dauerhaftigkeit PY - 2017 AN - OPUS4-43196 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - LIBS vom Labor zum Produkt (Laser induced Breakdown spectroscopy) N2 - Präsentation der Entwicklung des mobilen LIBS-Systems T2 - FA ZfP im Bauwesen der DGZfP CY - Berlin, Germany DA - 11.05.2017 KW - LIBS KW - Beton KW - Chlorid KW - Dauerhaftigkeit PY - 2017 AN - OPUS4-43198 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Application of laser-induced breakdown spectroscopy for the chemical investigation of concrete infrastructure N2 - The majority of the built infrastructure is made of concrete, which is a multiphase system made of cement, aggregates, water and pores (every year nearly 4 billion tons of cement are produced which is largest mass flow generated by mankind). Concrete is often used in combination with steel as reinforced concrete. Environmental influences, especially the ingress of harmful ions in combination with the ingress of water, trigger different damage processes which reduce the designed lifetime of a structure. The ingress of chlorides from de-icing salt or sea water leads to corrosion of the reinforcement. Also the carbonation of the concrete may trigger the corrosion of the reinforcement. The ingress of alkalis from de-icing salts may cause the expansion of the amorphous silica aggregates (alkali-silica reaction) through formation of a swelling gel of calcium silicate hydrate if water is present. The ingress of sulfates may cause spalling of the concrete surface due to ettringite formation. For the standard procedure in civil engineering cores are taken, cut in slices, grinded and the obtained homogenized powder is solved in acid and investigated by standard procedures. BAM has developed the LIBS technique for the 2D evaluation of the chemical composition of concrete [1-11]. The technique is established for automated laboratory use with high numbers of samples to investigate transport processes of harmful species (Cl-, CO2, SO42- and alkalis) in concrete. Information about ingress depth and the quantitative values are important to estimate the remaining lifetime of the infrastructure. LIBS is a surface technique. To get information about the ingress depth, a core has to be taken and cut in the middle. The measurements are carried out at the cross section. The main advantages of LIBS are the direct measurement on the surface of the concrete, fast analysis (sample rate 100 Hz) with a spatial resolution of up to 100 µm, the consideration of the heterogeneity of the concrete and the possibility of automated measurements which save a lot of manpower and time. As an example the investigation of ingress profiles for standard diffusion and migration tests in civil engineering takes hours in comparison to just a few minutes using LIBS. At the same time a 2D-evaluation provides information about hot spots of elemental concentration which may not be found by standard methods. Ingress of chlorides due to a crack in a repair mortar. Left: Photo of the cross section of a concrete core and the surface investigated by LIBS (area 70 mm x 70 mm). Right: Color coded chlorine intensity on the cross section of a concrete core, dark red represents high chlorine content. The state of the art of LIBS technique for applications in civil engineering will be presented, including typical results of 2D investigation of concrete in laboratory. The performance is also demonstrated by examples for onsite applications using a mobile LIBS system. The road map to standardization is presented as well. T2 - Optics and photonics international congress - Laser Solutions for Space and the Earth CY - Yokohama, Japan DA - 18.04.2017 KW - LIBS KW - Beton KW - On-site KW - Chloride PY - 2017 AN - OPUS4-43199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Absolute Fluorescence Measurements > 800 nm - Setup Design, Challenges, and Characterization of Semiconductor and Lanthanide-based Nanocrystals N2 - There is an increasing interest in optical reporters like semiconductor and lanthanide-based nanocrystals with emission > 800 nm and recently also > 1000 nm for bioanalysis, medical diagnostics, and safety barcodes. Mandatory for the comparison of different emitter classes and the rational design of the next generation of reporters for the short wavelength infrared (SWIR) region are reliable and quantitative photoluminescence measurements in this challenging wavelength region. This is of special relevance for nanocrystalline emitters like semiconductor quantum dots and rods as well as for upconversion and downconversion nanocrystals, where surface states and the accessibility of emissive states by quenchers largely control accomplishable quantum yields and hence, signal sizes and detection sensitivities from the reporter side. Such measurements are currently hampered by the lack of suitable methods and standards for instrument calibration and validation as well as by the lack of quantum yield standards with emission > 800 nm and especially > 1000 nm. In this respect, we present the design of integrating sphere setups for absolute and excitation power densitydependent measurements of emission spectra and quantum yields in the wavelength region of 650 to 1650 nm including calibration strategies and first candidates for potential fluorescence standards. Subsequently, the photoluminescence properties of different types of nanocrystals are presented and discussed including absolute photoluminescence measurements of upconversion and down conversion emission in different solvents. T2 - MRS 2017 CY - Boston, MA, USA DA - 26.11.2017 KW - Upconversion KW - Nanoparticle KW - Absolute fluorometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Fluorescence KW - Surface chemistry KW - Deactivation pathways KW - Semiconductor quantum dot KW - SWIR KW - Quantum yield KW - Energy transfer KW - Size PY - 2017 AN - OPUS4-43202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Innen hui und außen pfui – Smarte Prozess-Sensoren in der gegenwärtigen Automatisierungslandschaft der Prozessindustrie N2 - Prozess-Sensoren 4.0 vereinfachen ihre Einbindung über Plug and Play, obwohl sie komplexer werden. Sie bieten Selbstdiagnose, Selbstkalibrierung und erleichterte Parametrierung. Über die Konnektivität ermöglichen die Prozess-Sensoren den Austausch ihrer Informationen als Cyber-physische Systeme mit anderen Prozess-Sensoren und im Netzwerk. Der Wandel von der aktuellen Automation zum smarten Sensor ist im vollen Gange. Automatisierungstechnik und Informations- und Kommunikationstechnik (IKT) verschmelzen zunehmend. Eine Topologie für smarte Sensoren, die das Zusammenwirken mit daten- und modellbasierte Steuerungen bis hin zur Softsensorik beschreibt gibt es heute jedoch noch nicht. Wir müssen jetzt schnell die Weichen für eine smarte und sichere Kommunikationsarchitektur stellen, um zu einer störungsfreien Kommunikation aller Komponenten auf Basis eines einheitlichen Protokolls zu kommen. Unnötiges Schnickschnack ist nicht erwünscht. Wenn die Prozessindustrie dieses nicht definiert, tun es andere. Für die weitere Entwicklung von der Ist‐Situation zu einer Industrie-4.0-Welt in der Prozessindustrie werden mehrere Szenarien diskutiert. Diese reichen vom erleichterten Abruf sensorbezogener Daten über zusätzliche Kommunikationskanäle zwischen Sensor und mobilen Endgeräten über vollständig bidirektionale Kommunikation bis hin zur Einbindung der Cloud und des Internets in virtualisierte Umgebungen. Um zu einer störungsfreien Kommunikation aller Komponenten untereinander zu kommen, muss mindestens ein einheitliches Protokoll her, das alle sprechen und verstehen. Der derzeit greifbarste offengelegte Standard, der moderne Kommunikationsanforderungen erfüllt, ist OPC Unified Architecture (OPC-UA). Viele halten das Sortieren der Kommunikationsstandards für eines der wesentlichen Errungenschaften von Industrie 4.0. Der Vortrag greift die Anforderungen der Technologie-Roadmap „Prozess-Sensoren 4.0“ auf und zeigt Möglichkeiten zu ihrer Realisierung am Beispiel eines Online-NMR-Analysators, der im Rahmen des EU-Projekts „CONSENS“ (www.consens-spire.eu) entwickelt wurde. Aktuelle und zukünftige öffentliche Förderung von Industrie 4.0-Projekten sind eine gute Investition. Wegen der hohen Komplexität und Interdisziplinarität gelingt die Umsetzung nur gemeinsam zwischen Anwendern aus der Prozessindustrie, Software- und Geräteherstellern sowie Forschungsgruppen. Anwender sind gefragt, diese neue Technologie durch eine beschleunigte Validierung und Akzeptanz umzusetzen. Sie erhalten die einzigartige Chance, ihre Prozesse und Anlagen wettbewerbsfähig zu halten. Kooperativ betriebenen F&E-Zentren und gemeinsam anerkannten Applikationslaboren kommt dafür eine hohe Bedeutung zu. T2 - 13. Dresdner Sensor Symposium CY - Dresden, Germany DA - 04.12.2017 KW - Prozessanalytik KW - Prozess-Sensoren 4.0 KW - Online-NMR-Spektroskopie KW - Continuous Manufacturing KW - Process Analytical Technology KW - CONSENS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-432056 AN - OPUS4-43205 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya T1 - Functional group analysis on 3D carrier materials with simple optical assays N2 - Carboxy, amino, and thiol groups play a critical role in a variety of physiological and biological processes and are frequently used for bioconjugation reactions. Moreover, they enable size control and tuning of the surface during the synthesis of particle systems. Especially, thiols have a high binding affinity to noble metals and semiconductors (SC). Thus, simple, inexpensive, robust, and fast methods for the quantification of surface groups and the monitoring of reactions involving ligands are of considerable importance for the characterization of modified or stabilized nanomaterials including polymers. We studied the potential of the Ellman’s assay, recently used for the quantification of thiol ligands on SC nanocrystals by us1 and the 4-aldrithiol assay for the determination of thiol groups in molecular systems and on polymeric, noble and SC nanomaterials. The results were validated with ICP-OES and reaction mechanisms of both methods were studied photometrically and with ESI-TOF-MS. The investigation of the reaction mechanisms of both methods revealed the influence of different thiols on the stoichiometry of the reactions2, yielding different mixed disulfides and the thiol-specific products spectroscopically detected. The used methods can quantify freely accessible surface groups on nanoparticles, e.g., modified polystyrene nanoparticles. For thiol ligands coordinatively bound to surface atoms of, e.g., noble or SC nanomaterials, depending on the strength of the thiol-surface bonds, particle dissolution prior to assay performance can be necessary. We could demonstrate the reliability of the Ellman’s and aldrithiol assay for the quantification of surface groups on nanomaterials by ICP-OES and derived assay-specific requirements and limitations. Generally, it is strongly recommended to carefully control assay performance for new samples, components, and sample ingredients to timely identify possible interferences distorting quantification. T2 - Colloquium of Optical Spectrometry (COSP) 2017 CY - Berlin, Germany DA - 27.11.2017 KW - Nanoparticle KW - Surface groups KW - Optical assays KW - Carboxy and amin PY - 2017 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-43207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Mathematical and statistical tools for online NMR spectroscopy in chemical processes N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied, which are calibration intensive. NMR spectroscopy has a high potential for direct loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environments for advanced process monitoring and control. Within the European Union’s Research Project CONSENS (Integrated CONtrol and SENsing, www.consens-spire.eu) by development and integration of a smart NMR module for process monitoring was designed and delivers online spectra of various reactions. The presented NMR module is provided in an explosion proof housing of 57 x 57 x 85 cm module size and involves a compact spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction), and evaluation. For reaction monitoring and process control using NMR instruments after acquisition of the FID the data needs to be corrected in real-time for common effects using fast interfaces and automated methods. When it comes to NMR data evaluation under industrial process conditions, the shape of signals can change drastically due to nonlinear effects. Additionally, the multiplet structure becomes more dominant because of the comparably low-field strengths which results in overlapping of multiple signals. However, the structural and quantitative information is still present but needs to be extracted by applying predictive models. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). By using the benefits of traditional qNMR experiments data analysis models can meet the demands of the PAT community (Process Analytical Technology) regarding low calibration effort/calibration free methods, fast adaptions for new reactants, or derivatives and robust automation schemes. T2 - 13. Dresdner Sensor Symposium CY - Dresden, Germany DA - 04.12.2017 KW - Process Monitoring KW - Process sensors KW - Process analytical technology KW - Online NMR spectroscopy KW - Direct loop control KW - Numerical methods KW - Spectral modeling KW - Indirect hard modeling KW - CONSENS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-432085 AN - OPUS4-43208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Theory of the Photoluminescence Quantum Yield and its Measurement for Different Emitters N2 - Mandatory for the comparison of different emitter classes and the rational design of the next generation of molecular and nanoscale reporters are reliable and quantitative photoluminescence measurements. This is of special relevance for all fluorescence applications in the life and material sciences. In the following, proccedures for the determination of this spectroscopic key parameter are presented including material-specific effects related to certain emitters T2 - COST 2017 CY - Turku, Finland DA - 03.04.2017 KW - Instrument calibration KW - Standard KW - Flourescence KW - Reference material KW - Absolute fluorometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Photophysics KW - Quantum yield KW - Dye PY - 2017 AN - OPUS4-43175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Effect of Particle Size and Excitation Power Density on the Luminescence Efficiency of Upconversion Nanocrystals in Different Dispersion Media N2 - Upconversion nanoparticles (UCNPs) offer new strategies for luminescence-based sensing and imaging. One of the best studied materials are ..-NaYF4 UCNPs doped with 20 % Yb3+ and 2 % Er3+, which efficiently convert 976 nm light to photons emitted at 540 nm, 655 nm, and 845 nm, respectively, reveal long luminescence lifetimes (> 100 µs), are photostable and chemically inert. Their upconversion (UC) luminescence (UCL) properties are, however, strongly influenced by particle size, surface chemistry, and microenvironment. In addition, the multiphotonic absorption processes responsible for UCL render UCL excitation power density (..) dependent. This makes quantitative UCL measurements as well as the determination of UC quantum yields (.UC) very challenging. The rational design of brighter UCNPs particle architectures and the interest in identifying optimum particle architectures for FRET-based sensing and imaging schemes, which often rely on core-only UCNPs to minimize donor-acceptor distances, encouraged us to assess the influence of particle size and P on UCL. Here, we present the photophysical properties of a series of hexagonal NaYF4 UCNPs with sizes from 10 to 43 nm with different surface ligands dispersed in organic solvents and water studied by steady state and time-resolved fluorometry as well as quantitatively by integrating sphere spectrometry with P varied over about three orders of magnitude. Our results underline the need for really quantitative luminescence studies for mechanistic insights and the potential of high P to compensate for UCL quenching due to high energy phonons and surface effects. T2 - 15th Conference on Methods and Applications in Fluorescence CY - Bruges, Belgium DA - 10.09.2017 KW - Upconversion KW - Nanoparticle KW - Absolute fluorometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Fluorescence KW - Surface chemistry KW - Deactivation pathways KW - Photophysics KW - Quantum yield PY - 2017 AN - OPUS4-43181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Leonhard, H. T1 - Fehlstellen im Visier - KorroPads N2 - Rohrsysteme und Behälter aus nichtrostendem Stahl sind mit einer Passivschicht vor Korrosion geschützt. Ist diese jedoch unvollständig ausgebildet oder beschädigt, geht der Schutz verloren. Das KorroPad-Verfahren ist ein Schnelltest zur Überprüfung der Passivschicht. Im Vergleich mit bisher üblichen Bewertungsmethoden ist die Anwendung sehr einfach und nimmt nur 15 Minuten in Anspruch. KW - Nichtrostender Stahl KW - Korrosionsschnelltest KW - KorroPad KW - Passivschicht PY - 2017 SN - 0946-2856 VL - 24 IS - 11/12 SP - 66 EP - 67 PB - Vogel Business Media GmbH & Co. KG CY - Würzburg AN - OPUS4-43184 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Büchele, Dominique T1 - Entwicklung einer online-RFA Analyse zur Bestimmung von Bodennährstoffen N2 - Mit wachsenden Bevölkerungszahlen steigt auch der Rohstoffkonsum, und der nachhaltigere und effizientere Umgang mit knappen Ressourcen wie Wasser und Boden rückt in den Fokus. Im Rahmen der vom Bundesministerium für Bildung und Forschung (BMBF) geförderten Forschungsinitiative BonaRes werden Strategien entwickelt, um Boden als nachhaltige Ressource in der Bioökonomie zu nutzen. Das interdisziplinäre Teilprojekt I4S – Intelligence for soil – ist dabei für die Entwicklung eines integrierten Systems zum ortsspezifischen Management der Bodenfruchtbarkeit zuständig. Hierfür wird eine Plattform gebaut, auf der verschiedene Sensoren installiert werden sollen, deren in Echtzeit erhaltene Messdaten in Modelle und Entscheidungsalgorithmen zur Steuerung der Düngung und dementsprechend Verbesserung der Bodenfunktionen einfließen sollen. So wären Untersuchungen in engmaschigen, dynamischen Rastern und schnelle Analysen großer Flächen möglich, um höhere Erträge zu erwirtschaften. Einer dieser Sensoren, auf dessen Grundlage ein robustes Online-Verfahren zur Bestimmung der Makro- und Mikronährstoffe, wie Ca, K und Mn in Böden entwickelt werden soll, ist die Röntgenfluoreszenzanalyse (RFA). Die RFA eignet sich vor allem durch ihre schnelle, kontaktlose, simultane Multielementanalyse und wird bereits zur Bestimmung von Schwermetallen in Böden eingesetzt. Ein weiterer Vorteil der RFA ist die geringe Probenvorbereitung. Um Messungen auf einem Feld zu simulieren, wurde in einen Laboraufbau ein Probenteller installiert, der sich bei verschiedenen Winkelgeschwindigkeiten bewegen lässt und so dynamisches Messen der als Spur aufgetragenen Probe ermöglicht. Gerade bei einer komplexen Matrix wie Boden, die eine breite Elementverteilung aufweist, ist die Datenauswertung ein wichtiger Faktor. Die bisher verwendete univariate Datenanalyse liefert gute Ergebnisse und zeigt, dass durch Kalibrierung der RFA mit 14 Referenzmaterialien große Ackerflächen ausgewertet werden können. Dies funktioniert aber nur, solange die Elementgehalte der Proben mit denen der Referenzmaterialien vergleichbar sind. Die zusätzlich verwendete multivariate Datenanalyse bietet hingegen die Möglichkeit, Modellrechnungen der Böden durchzuführen und Böden mithilfe der Hauptkomponentenanalyse (PCA) besser zu klassifizieren. Des Weiteren können basierend auf der Partial Least Squares Regression (PLSR) Kalibriermodelle erstellt werden, welche Prognosen zu den Elementgehalten unbekannter Ackerböden ermöglichen. Zusätzlich bietet die multivariate Datenanalyse die Möglichkeit, Störgrößen wie unterschiedliche Korngrößenverteilung und Feuchtigkeitsgrad der Probe in das Modell miteinzubeziehen. Beide Auswertemethoden sollen anhand statisch gemessener Proben verglichen werden und durch Messung einer Vielzahl realer Bodenproben von unterschiedlichen Standorten erweitert werden. Im weiteren Verlauf müssen beide Modelle auf dynamisch bewegte Proben übertragen werden. T2 - 13. Herbstkolloquium AK Prozessanalytik CY - Esslingen-Berkheim, Germany DA - 20.11.2017 KW - PCA KW - Nährstoffe KW - Boden KW - RFA KW - PLSR PY - 2017 AN - OPUS4-43150 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Bestimmung von Nährstoffen in Böden mittels LIBS – Univariate vs. multivariate Datenanalyse N2 - LIBS (laserinduzierte Plasmaspektroskopie) ist bekannt für eine schnelle, simultane Multielementanalyse, welche kaum bis keine Probenvorbereitung benötigt. Im Hinblick dessen ist das Interesse an LIBS als Online-Analysentechnik für den Einsatz auf Agrarflächen in den letzten Jahren stark gestiegen. Im Rahmen des Projekts I4S (engl. für: intelligence for soil) soll mithilfe von LIBS der Elementgehalt von Makro- und Mikronährstoffen in Böden in Echtzeit bestimmt werden. I4S gehört zu den zehn interdisziplinären Forschungsprojekten des Innovationsprogramms BonaRes und arbeitet an der Entwicklung einer Sensorplattform für ein ortsspezifisches Management der Bodenfruchtbarkeit. BonaRes ist vom Bundesministerium für Bildung und Forschung (BMBF) gefördert und beschäftigt sich mit Boden als nachhaltige Ressource für die Bioökonomie. Für die Anwendung von LIBS an Böden wurde ein spezieller Aufbau konstruiert. Die Probenzufuhr erfolgt über einen drehbaren Probenteller, auf den der lose Boden in Form einer Spur aufgetragen oder als gepresste Tablette platziert werden kann. Der Probenteller kann in unterschiedlichen Geschwindigkeitsstufen betrieben werden, um die Anwendung auf dem Feld zu simulieren. Für eine höhere Signalintensität und eine bessere Reproduzierbarkeit wird eine Doppel-Puls (DP) Nd:YAG Lasereinheit verwendet. Weiterhin besitzt der LIBS-Messkopf eine integrierte Absaugvorrichtung, um bei dem Ablationsprozess entstehende Stäube zu minimieren und eine störungsfreie Detektion des Signals zu gewährleisten. Da es sich bei LIBS um eine Relativmethode handelt, muss das System für eine absolute Quantifizierung hinsichtlich der Zielanalyten kalibriert werden. Hierfür werden realitätsnahe Proben benötigt. Es wurden 16 freiverkäufliche, zertifizierte Referenzmaterialien gemessen und für die Kalibrierung verwendet. Aufgrund der komplexen Bodenmatrix und Einflüsse, wie Korngrößeneffekte und Feuchtigkeit, stellt die absolute Quantifizierung mittels LIBS eine Herausforderung dar. Für die Kalibrierung wurde sowohl ein univariater als auch ein multivariater Analyseansatz (Partial least square regression) verwendet. Mittels der multivariaten Auswertung konnte ein robusteres Kalibriermodell aufgrund einer besseren Korrelation zwischen Signalintensität und Elementkonzentration erstellt werden. Innerhalb des I4S-Verbundes gibt es eine Vielzahl von Bodenproben von unterschiedlichen Testackerflächen mit bereits bekannten Informationen über die chemische Zusammensetzung, Textur und Korngrößenverteilung. Diese Bodenproben sollen im nächsten Schritt für weitere Berechnungen und zu Validierungszwecken verwendet werden. T2 - 13. Herbstkolloqium AK Prozessanalytik CY - Esslingen, Germany DA - 20.11.2017 KW - Analyse KW - Nährstoffe KW - Boden KW - LIBS KW - Multivariat PY - 2017 AN - OPUS4-43151 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Determination of plant essential nutrients in soils using DP-LIBS N2 - LIBS (laser-induced breakdown spectroscopy) is known as a fast and simultaneous multi-element analysis with little or no sample preparation. In the last few years there has been a growing interest in applications of LIBS in the field of agriculture. As part of the National Research Strategy BioEconomy 2030 the German Federal Ministry of Education and Research (BMBF) started an innovation programme called BonaRes. BonaRes consists of ten interdisciplinary research project associations which are dealing with soil as a sustainable resource for the bio-economy. One of these research projects is I4S (intelligence for soil) which has the goal to develop an integrated system for site-specific soil fertility management. This system includes a sensor platform, which contains different sensors, like XRF, VIS-NIR, Gamma and LIBS. The main task of LIBS measurements in this project is the real time determination of the elemental contents of nutrients in soils, like calcium, magnesium, potassium. For this purpose, a special setup has been designed. The sample uptake operates with the help of a rotatable sample plate which circulates with different velocities to simulate the application on the field. To provide a higher intensity and a better reproducibility of the obtained signal, a double-pulse Nd:YAG laser was used. In order to minimize dust formation from the soil during the operation of the laser, a dust removal by suction has been integrated. When using relative methods such as LIBS, a suitable calibration curve is needed for absolute quantification. With the help of 16 certified reference soils, calibration curves for different elements were initially calculated and used for the quantification of seven soil samples from different testing grounds in Germany. The complex matrix of soils, as well as the influence of moisture and grain size in soils makes the absolute quantification by LIBS challenging. To overcome these influences, a calibration curve based on multivariate analysis (partial least square regression) was generated. T2 - Adlershof Forschungsforum CY - Berlin, Germany DA - 10.11.2017 KW - Fertility management KW - Multivariate KW - Soil KW - LIBS PY - 2017 AN - OPUS4-43154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Büchele, Dominique T1 - Entwicklung einer Online-RFA Methode zur Bestimmung der Makro- und Mikronährstoffe im Boden N2 - Die vom Bundesministerium für Bildung und Forschung (BMBF) geförderte Forschungsinitiative BonaRes hat sich zum Ziel gesetzt Strategien zu erarbeiten um Boden als nachhaltige Ressource für die Bodenökonomie zu nutzen. Sie ist in 10 interdisziplinären Forschungskonsortien eingeteilt, wobei das Teilprojekt „Intelligence for soil“ (I4S) für die Entwicklung eines integrierten Systems zum ortsspezifischen Management der Bodenfruchtbarkeit zuständig ist. Das System soll sowohl verschiedene Bodensensoren sowie Modelle und Entscheidungsalgorithmen zur Steuerung der Düngung und dementsprechend Verbesserung der Bodenfunktionen vereinen. So kann die Umweltbelastung durch die im Dünger enthaltenen Nitrate reduziert werden und die durch Überdüngung entstehenden Kosten für die Landwirte minimiert werden. Hierzu ist eine flächendeckende Kartierung der Ackerflächen hinsichtlich der für Pflanzen wichtigen Makro- und Mikronährstoffe, wie Calcium nötig. Ziel der Bundesanstalt für Materialforschung und -prüfung (BAM) innerhalb von I4S ist die Optimierung eines auf der Röntgenfluoreszenzanalyse (RFA) basierenden Sensors für die mobile online-Applikation auf dem Feld. Diese zerstörungsfreie und kontaktlose Methode eignet sich besonders für den Feldeinsatz dank minimaler Probenvorbereitung und vor allem schneller, simultaner Multielementanalyse. Hauptkomponente der robusten und transportablen Messstation ist neben dem Sensor ein drehbarer Probenteller um das Messen während der Fahrt bei verschiedenen Geschwindigkeiten auf einem Feld unter Laborbedingungen zu simulieren. Der energiedispersive RFA-Sensor besitzt ein mit Helium gespültes Messvolumen womit auch die für diese Aufgabenstellung interessanten, leichten Elemente detektiert werden können. Schwierigkeiten beim Einsatz der RFA liegen in der Kalibrierung des Geräts um richtige und präzise Ergebnisse zu erhalten. Der Fokus zu Beginn richtet sich somit auf die Entwicklung eines Kalibriermodells, welches die verschiedenen Hauptbodenarten berücksichtigt. Gerade die zu untersuchenden Makro- und Mikronährstoffe wie Schwefel liegen im Vergleich zu SiO2 in sehr geringen Konzentrationen im Boden vor. Die Optimierung der Parameter wie Leistung oder auch Messzeit können an dieser Stelle die erhaltenen Signalintensitäten deutlich beeinflussen. Zusätzlich sind gerade bei einer komplexen Matrix wie Boden genaue Untersuchungen verschiedener Störgrößen wichtig. Hierzu zählen unter anderem der Feuchtigkeitsgrad der Probe, aber auch Korngrößeneffekte haben einen entscheidenden Einfluss. Beide Parameter müssen hinsichtlich ihrer Auswirkungen auf die Messergebnisse der mobilen-RFA sowohl bei stationären, als auch bei bewegten Bodenproben betrachtet werden. T2 - Anakon CY - Tübingen, Germany DA - 03.04.2017 KW - Nährstoffe KW - RFA KW - Boden PY - 2017 AN - OPUS4-43156 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Entwicklung eines Online-LIBS-Systems für die Bestimmung von Nährstoffgehalten in Böden N2 - Die Gehalte von für das Pflanzenwachstum relevanten Nährstoffen divergieren innerhalb einer landwirtschaftlichen Nutzfläche sehr stark. Für eine ertragssteigernde Bewirtschaftung ist daher eine gezielte Düngung unabdingbar. Die Nachfrage nach einer kostengünstigen, flächendeckenden Kartierung von Ackerflächen in Bezug auf die im Boden enthaltenen Nährstoffe steigt demnach. Hierzu werden schnelle, mobil einsetzbare und verlässliche Messmethoden benötigt. Eine geeignete Methode stellt die laserinduzierte Plasmaspektroskopie (kurz: LIBS aus dem Englischen für laser-induced breakdown spectroscopy) dar. Die LIBS ermöglicht eine schnelle und simultane Multielementanalyse und ist dabei nahezu zerstörungsfrei. Des Weiteren bedarf es für die Analyse kaum bis keine Probenvorbereitung was den Einsatz auf dem Feld begünstigt. Die Methode beruht auf der Ionisierung des Probenmaterials (Plasmabildung) durch den Beschuss dieser mit kurzen Laserpulsen. Während der Expansion des Plasmas wird Strahlung emittiert, welche charakteristisch für die in der Probe enthaltenen Elemente ist. Das hier verwendete LIBS-System verfügt über einen Doppelpuls-Laser, bei dem zwei Laserpulse im kurzen Abstand hintereinander ausgesendet werden. Der erste Laserpuls ist für die “Vorbehandlung“ der Probe und der zweite Laserpuls für die Erwärmung des Plasmas. Dadurch können die Nachweisgrenzen im Vergleich zu einem einfach gepulsten Laser deutlich verbessert werden. Die Probenzufuhr findet durch einen drehbaren Probenteller statt auf dem der lose Boden in Form einer Spur aufgetragen wird. Der Probenteller kann in verschiedenen Geschwindigkeiten betrieben werden, um die Anwendung auf dem Feld zu simulieren. Da es sich bei der LIBS um eine Relativmethode handelt, ist eine Kalibrierung mit exakten Referenzwerten von verschiedenen Bodenproben notwendig. Böden weisen eine sehr komplexe Matrix auf, was die verlässliche Analyse mittels LIBS erschwert. Daher ist zunächst das Ziel die verschiedenen Messparameter des LIBS-Systems für unterschiedliche Böden zu optimieren und mögliche Störeffekte, wie Korngrößen und Feuchtigkeitsgrad, durch eine geeignete Probenkonditionierung zu eliminieren. T2 - Anakon 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Multivariat KW - Boden KW - LIBS KW - Nährstoffe KW - Analyse PY - 2017 AN - OPUS4-43157 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram A1 - Paul, Andrea T1 - Ordinal sequences and their uncertainties N2 - Ordinal (alpha-numeric) number sequences may characterise structure and identity of substances. A simple approach to handling the spread between different determinations (both repeatability and reproducibility) is proposed. T2 - 22. General Assembly of COOMET TC 1.12 CY - Kasan, Russia DA - 11.09.2017 KW - Measurement uncertainty KW - Ordinal numbers KW - Sequence PY - 2017 AN - OPUS4-42475 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram T1 - The new Guide 35 – Where are the major changes? N2 - The fully revised ISO/REMCO Guide 35 comprehensively covers most of the aspects of preparing, homogenising, and characterising reference materials. Special attention is paid to certified RM and the expression of their traceability, as well as the evaluation of the measurement uncertainty of the assigned value(s). T2 - EUROLAB/D EDAC meeting CY - Berlin, Germany DA - 26 April 2017 KW - Reference materials KW - RM production KW - Homogeneity and stability testing KW - Characterisation PY - 2017 AN - OPUS4-42477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram A1 - Paul, Andrea T1 - Peculiarities of qualitative RM and accreditation of their producers N2 - With a more and more general acceptance of accreditation in the field of reference materials production, and an ever increasing number of RMP accredited, accreditation bodies face applications from RMP active in the field of qualitative RM production. While (the still valid and used for accreditation purposes) ISO Guides 34 and 35 describe in detail requirements applicable to RMP dealing with quantitative RM, accreditation bodies normally claim lack of normative requirements with respect to quantitative RM. The new ISO 17034:2016 which will be introduced in the accreditation practice over the next two to three years solves the problem pragmatically, allowing strategies for RM certification other than those for (purely) quantitative materials. In fact, both ISO Guide 34 and the new ISO 17034 are written in a form that, at least for the overwhelming majority of requirements, may be applied to RMP of both qualitative and quantitative RM. Peculiarities may occur in homogeneity and stability testing, and the uncertainty of a purely qualitative result is still under discussion. The problem of traceability might be solved for most of the application fields considered. The talk gives an overview of the specific problems encountered, and provides some possible solutions both for homogeneity and stability testing, the expression of uncertainty, and the statement of traceability in certificates. T2 - Advanced Mathematical and Computational Tools for Metrology; AMCTM (XI) CY - Glasgow, Scotland, UK DA - 29 August 2017 KW - Nominal values KW - Qualitative RM KW - Ordinal sequences PY - 2017 AN - OPUS4-42466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram A1 - Paul, Andrea T1 - Approaches to measurement uncertainty estimates for nominal properties N2 - Qualitative reference materials (RM) cover a wide range of the overall RM market. Proficiency testing providers attract up to a thousand of participants in PT schemes purely oriented on qualitative results. The RM used for these kinds of PT are poorly regulated, nevertheless with a more and more general acceptance of accreditation in the field of RM production and PT provision, there is an ever increasing interest in assessing producers and providers according to rules already well accepted in the field of quantitative analysis. The basic governing document, ISO 17034:2016, is written in a form that, at least for the overwhelming majority of requirements, may be applied to both qualitative and quantitative RM. However, problems remain. In particular, the expression of uncertainty of a purely qualitative result is still unresolved, and under discussion, the latter now lasting already dozens of years. Some handles would be needed. In the poster, existing approaches and some pragmatic, new ways to tackle the problem are displayed and discussed. T2 - Advanced Mathematical and Computational Tools for Metrology; AMCTM (XI) CY - Glasgow, Scotland, UK DA - 29 August 2017 KW - Nominal properties KW - Qualitative RM PY - 2017 AN - OPUS4-42467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram T1 - 2016/2017 Activities of REMCO N2 - The very active work of ISO/REMCO on the revision and updating of Guides is revised. Special attention is paid to the development of ISO 17034:2016, the guiding line for the assessment of competence of RM producers. T2 - 22. General Assembly of COOMET TC 1.12 CY - Kasan, Russia DA - 11 September 2017 KW - RM producers KW - Competence PY - 2017 AN - OPUS4-42468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mielke, Johannes A1 - Dohányosová, P. A1 - Müller, P. A1 - Lopez, S. A1 - Hodoroaba, Vasile-Dan T1 - Electrospray as a sample preparation tool for electron microscopic investigations: Toward quantitative evaluation of nanoparticles N2 - The potential of electrospray deposition, for the controlled preparation of particles for imaging in electron microscopes, is evaluated on various materials: from mono-modal suspensions of spherical particles to multimodal suspensions and to real-world industrial materials. It is shown that agglomeration is reduced substantially on the sample carrier, compared with conventional sample preparation techniques. For the first time, it is possible to assess the number concentration of a tri-modal polystyrene suspension by electron microscopy, due to the high deposition efficiency of the electrospray. We discovered that some suspension stabilizing surfactants form artifact particles during electrospraying. These can be avoided by optimizing the sprayed suspension. KW - Electrospray deposition KW - Nanoparticles KW - SEM KW - TEM KW - Sample preparation PY - 2017 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/electrospray-as-a-sample-preparation-tool-for-electron-microscopic-investigations-toward-quantitative-evaluation-of-nanoparticles/483B212FF290B7EC001A212A19E4E72A DO - https://doi.org/10.1017/S1431927617010145 SN - 1435-8115 SN - 1431-9276 VL - 23 IS - S1 (July) SP - 1896 EP - 1897 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-42453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Ortel, Erik A1 - Wirth, Thomas A1 - Holzweber, Markus A1 - Pellegrino, F. A1 - Martra, G. A1 - Hodoroaba, Vasile-Dan T1 - Analysis of fluorine traces in TiO2 nanoplatelets by SEM/EDX, AES and TOF-SIMS N2 - Hydrothermal synthesis of anatase TiO2 nanosheets with a high fraction of exposed {001} facets and related high photocatalytic activity - as an alternative to bipyramidal anatase TiO2 nanoparticles mainly exposing the {101} facets. The scope of the material preparation work is the thermal reduction of residual fluorides from HF (capping agent) induced during the synthesis of TiO2 nanosheets by calcination at 873K. The analytical task consists of detection and localization of fluorine present at the surface and/or in the bulk of TiO2 nanosheets before and after calcination by SEM/EDX, Auger electron spectroscopy and ToF-SIMS. KW - Fluorine KW - SEM/EDX KW - TiO2 nanoplatelets KW - Auger electron spectroscopy KW - TOF-SIMS PY - 2017 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/analysis-of-fluorine-traces-in-tio2-nanoplatelets-by-semedx-aes-and-tofsims/91EA2C0666B7927FCA57D2AD114910F6 DO - https://doi.org/10.1017/S1431927617010200 SN - 1435-8115 SN - 1431-9276 VL - 23 IS - S1 (July) SP - 1908 EP - 1909 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-42455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Hodoroaba, Vasile-Dan A1 - Ortel, Erik A1 - Wirth, Thomas A1 - Borghetti, P. A1 - Garcia, S. A1 - Gómez, E. A1 - Blanco, M. A1 - Alberto, Gabriele A1 - Martra, G. T1 - Organic surface modification and analysis of titania nanoparticles for self-assembly in multiple layers N2 - Parameters of TiO2 coatings can greatly influence their final performance in largescale applications such as photocatalytic measurements, orthopedic and/or dental prostheses, cell cultures, and dye-sensitized solar cells. From different film deposition procedures, self-assembly of TiO2 NPs in multiple layers was selected for systematic characterization. EDX, AES and ToF-SIMS analysis have been carried out in order to evaluate the functionalization of several types of TiO2 NPs differing in size, shape and surface area. KW - TiO2 KW - Nanoparticles KW - Surface modification KW - Functionalization PY - 2017 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/organic-surface-modification-and-analysis-of-titania-nanoparticles-for-selfassembly-in-multiple-layers/66776A4CA7FD059CE39041A99A922D90 DO - https://doi.org/10.1017/S1431927617010029 SN - 1431-9276 SN - 1435-8115 VL - 23 IS - S1 (July) SP - 1872 EP - 1873 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-42457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Jakob, C. A1 - Ectors, D. A1 - Neubauer, J. A1 - Schmid, Thomas T1 - Measuring the Burning Temperatures of Anhydrite Micrograins in a High-Fired Medieval Gypsum Mortar N2 - Typical feature of high-fired medieval gypsum mortars is a compact microstructure of squat gypsum crystals containing firing products as remains of the calcination process. So far, the burning history of the binder is estimated based on morphological characteristics of the latter. A novel Raman microspectroscopy approach provides access to the calcination temperatures of individual anhydrite grains based on quantifiable spectroscopic changes appearing due to gradual variations of crystallinity, as independently confirmed by X-ray diffraction analysis of anhydrites synthesised at temperatures between 500°C and 900°C. The approach was successfully applied to the high-fired gypsum mortar of a South Tyrolean stucco sculpture of a pieta dated around 1420. Microparticles of burned anhydrite II with firing temperatures scattered around 650°C and clusters of thermally damaged natural anhydrite II crystals from the raw material were identified and imaged. KW - Analytical methods KW - Gypsum technology KW - High-fired gypsum mortar KW - Raman microspectroscopy KW - Thermal anhydrite PY - 2017 DO - https://doi.org/10.1002/slct.201701260 VL - 2 IS - 28 SP - 9153 EP - 9156 PB - Wiley VCH Verlag AN - OPUS4-42458 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Investigation of core-shell nanoparticles using scanning transmission x-ray microscopy (STXM) N2 - A scanning transmission x-ray microscopy (STXM) based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core-shell nanoparticles which exhibit a strong x-ray absorption contrast and a well-defined interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less x-ray beam induced damage of the sample is achieved by recording STXM images only at two predetermined energies of maximum absorption contrast, instead of recording a stack of images across the whole absorption edge. A model core-shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, is used for demonstration. Near edge x-ray absorption fine structure (NEXAFS) spectroscopy confirms the significant difference in x-ray absorption behavior between PTFE and PS. Additionally, due to the insolubility of styrene in PTFE a well-defined interface between particle core and shell is expected. In order to validate the STXM results, both the naked PTFE cores as well as the complete core-shell nanoparticles are examined by scanning electron microscopy (SEM). The introduced STXM based methodology yields particle dimensions in good agreement with the SEM results (deviation equal or less than 10%) and provides additional information such as the position of the particle core which cannot be extracted from a SEM micrograph. T2 - European conference on applications of surface and interface analysis 2017 (ECASIA'17) CY - Montpellier, France DA - 24.09.2017 KW - STXM KW - SEM KW - PTFE KW - PS KW - Core-shell nanoparticles KW - Polymers KW - Metrology PY - 2017 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-42427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Determining the shell thickness of PTFE@PS core@shell nanoparticles using scanning transmission x-ray microscopy (STXM) N2 - A scanning transmission x-ray microscopy (STXM) based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core-shell nanoparticles which exhibit a strong x-ray absorption contrast and a well-defined interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less x-ray beam induced damage of the sample is achieved by recording STXM images only at two predetermined energies of maximum absorption contrast, instead of recording a stack of images across the whole absorption edge. A model core-shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, is used for demonstration. Near edge x-ray absorption fine structure (NEXAFS) spectroscopy confirms the significant difference in x-ray absorption behavior between PTFE and PS. Additionally, due to the insolubility of styrene in PTFE a well-defined interface between particle core and shell is expected. In order to validate the STXM results, both the naked PTFE cores as well as the complete core-shell nanoparticles are examined by scanning electron microscopy (SEM). The introduced STXM based methodology yields particle dimensions in good agreement with the SEM results (deviation equal or less than 10%) and provides additional information such as the position of the particle core which cannot be extracted from a SEM micrograph. T2 - BAM PhD Day 2017 CY - Berlin, Germany DA - 21.09.2017 KW - STXM KW - SEM KW - PTFE KW - PS KW - Core-shell nanoparticles KW - Polymers KW - Metrology PY - 2017 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-42430 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, Rudolf A1 - Carvalho, A. M. A1 - Manicardi, A. A1 - Montes, C. V. A1 - Gunnoo, S. B. A1 - Madder, A. T1 - Decoration of trastuzumab with short oligonucleotides: synthesis and detailed characterization N2 - Trastuzumab (Herceptin) is an FDA-approved therapeutic antibody currently employed in the treatment of metastatic stages of breast cancer. Herein, we propose a simple, fast and cost-effective methodology to conjugate trastuzumab with 22-mer 5' thiol-modified oligonucleotides using a bifunctional crosslinker. The conjugates were successfully characterized by MALDI-ToF MS and SDS-PAGE, obviating the need for enzymatic digestion and difficult chromatographic separations. Furthermore, ELISA was performed to ensure that trastuzumab activity is not affected by oligonucleotide conjugation. KW - MALDI-ToF KW - ELISA PY - 2017 DO - https://doi.org/10.1039/c7ob02216f SN - 1477-0539 VL - 15 IS - 42 SP - 8923 EP - 8928 AN - OPUS4-43328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, Rudolf A1 - Korsak, B. A1 - Almeida, G. M. A1 - Rocha, S. A1 - Pereira, C. A1 - Mendes, N. A1 - Osorio, H. A1 - Pereira, P. M. A1 - Rodrigues, J. M. M. A1 - Sarmento, B. A1 - Tome, J. P. C. A1 - Oliveira, C. T1 - Porphyrin modified trastuzumab improves efficacy of HER2 targeted photodynamic therapy of gastric cancer N2 - Gastric cancer (GC) is the 3rd deadliest cancer worldwide, due to limited treatment options and late diagnosis. Human epidermal growth factor receptor-2 (HER2) is overexpressed in similar to 20% of GC cases and anti-HER2 antibody trastuzumab in combination with conventional chemotherapy, is recognized as standard therapy for HER2-positive metastatic GC. This strategy improves GC patients' survival by 2-3 months, however its optimal results in breast cancer indicate that GC survival may be improved. A new photoimmunoconjugate was developed by conjugating a porphyrin with trastuzumab (Trast: Porph) for targeted photodynamic therapy in HER2-positive GC. Using mass spectrometry analysis, the lysine residues in the trastuzumab structure most prone for porphyrin conjugation were mapped. The in vitro data demonstrates that Trast: Porph specifically binds to HER2-positive cells, accumulates intracellularly, co-localizes with lysosomal marker LAMP1, and induces massive HER2-positive cell death upon cellular irradiation. The high selectivity and cytotoxicity of Trast: Porph based photoimmunotherapy is confirmed in vivo in comparison with trastuzumab alone, using nude mice xenografted with a HER2-positive GC cell line. In the setting of human disease, these data suggest that repetitive cycles of Trast: Porph photoimmunotherapy may be used as an improved treatment strategy in HER2-positive GC patients. KW - Photoimmunotherapy KW - Photoimmunoconjugate KW - Gastric cancer PY - 2017 DO - https://doi.org/10.1002/ijc.30844 SN - 0020-7136 VL - 141 IS - 7 SP - 1478 EP - 1489 PB - International Journal of Cancer AN - OPUS4-43315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, Rudolf A1 - Schmidt, S. A1 - Hanelt, S. A1 - Canitz, C. A1 - Hoffmann, H. A1 - Garbe, L.-A. T1 - Synthetic Strategies for the Modification of Diclofenac N2 - For many heterogeneous sensor applications as well as the synthesis of hapten antigens to produce antibodies, protein conjugates of the target substance are essential. A requirement is that the target substance already offers or is modified to contain a functionality that allows for coupling to a protein, that is, an amino acid residue. Ideally, to avoid shielding of the compound by the carrier protein, a sufficient distance to the protein surface should be provided. With its carboxyl function diclofenac (DCF) allows for direct binding to lysine residues after in situ synthesis of the NHS ester. One problem is that diclofenac as free acid tends to autocondensation, which results in low yields. Here we describe the 'insertion' of a C6 spacer via synthesis of the amide with 6-aminohexanoic acid. To carry out the reaction in solution, first the methyl ester of the amino acid had to be produced. Due to otherwise low yields and large cleaning efforts, solid-phase synthesis on Fmoc Ahx Wang resin is recommended. The crude product is mainly contaminated by cleavage products from the resin which were removed by chromatography. The structure of the highly pure hapten was completely determined by nuclear magnetic resonance (NMR) spectroscopy. KW - Diclophenac KW - Hapten synthesis KW - Solid-phase synthesis PY - 2017 DO - https://doi.org/10.1055/s-0036-1588858 SN - 0936-5214 VL - 28 IS - 15 SP - 1984 EP - 1989 PB - Georg Thieme Verlag AN - OPUS4-43316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seidel, R. A1 - Kraffert, K. A1 - Kabelitz, Anke A1 - Pohl, M.N. A1 - Kraehnert, R. A1 - Emmerling, Franziska A1 - Winter, B. T1 - Detection of the electronic structure of iron-(III)-oxo oligomers forming in aqueous solutions N2 - The nature of the small iron-oxo oligomers in iron-(III) aqueous solutions has a determining effect on the chemical processes that govern the formation of nanoparticles in aqueous phase. Here we report on a liquid-Jet photoelectron-spectroscopy experiment for the investigation of the electronic structure of the occurring iron-oxo oligomers in FeCl3 aqueous solutions. The only iron species in the as-prepared 0.75 M solution are Fe3+ monomers. Addition of NaOH initiates Fe3+ hydrolysis which is followed by the formation of iron-oxo oligomers. At small enough NaOH concentrations, corresponding to approximately [OH]/[Fe] = 0.2–0.25 ratio, the iron oligomers can be stabilized for several hours without engaging in further aggregation. Here, we apply a combination of non-resonant as well as iron 2p and Oxygen 1s resonant photoelectron spectroscopy from a liquid microjet to detect the electronic structure of the occurring species. Specifically, the oxygen 1s partial electron yield X-ray absorption (PEY-XA) spectra are found to exhibit a peak well below the onset of liquid water and OH (aq) absorption. The iron 2p absorption gives rise to signal centered between the main absorption bands typical for aqueous Fe3+. Absorption bands in both PEY-XA spectra are found to correlate with an enhanced photoelectron Peak near 20 eV binding energy, which demonstrates the sensitivity of resonant photoelectron (RPE) spectroscopy to mixing between iron and ligand orbitals. These various signals from the iron-oxo oligomers exhibit Maximum intensity at [OH]/[Fe] = 0.25 ratio. For the same ratio, we observe changes in the pH as well as in complementary Raman spectra, which can be assigned to the Transition from monomeric to oligomeric species. At approximately [OH]/[Fe] = 0.3 we begin to observe particles larger than 1 nm in radius, detected by small-angle X-ray scattering. KW - Iron-oxo oligomers KW - XPS KW - Electronic structure PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-433468 DO - https://doi.org/10.1039/c7cp06945f SN - 1463-9076 SN - 1463-9084 VL - 19 IS - 48 SP - 32226 EP - 32234 AN - OPUS4-43346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szczerba, Wojciech A1 - Schneider, M. A1 - Żukrowski, J. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Riesemeier, Heinrich A1 - Sikora, M. A1 - Mandel, K. T1 - Spectroscopic Study of the Role of Metal Ions in the Adsorption Process of Phosphate in Nanoscaled Adsorbers Based on Metal (Zn/ Fe/Zr) Oxyhydroxides N2 - Currently great effort is made to find materials and technologies for the recycling of phosphate from wastewater. Herein, we present an in-depth study of the Phosphate adsorption mechanism of a promising adsorber material, a Zn−Fe−Zr oxyhydroxide-based nanostructured precipitate. The behavior of the multicomponent nanomaterial, consisting of both crystalline and amorphous parts, is investigated via X-ray absorption fine structure spectroscopy and Mössbauer spectroscopy, revealing the importance of the nanostructured composition for the phosphate adsorption. We found evidence that adsorption takes place especially in the vicinity of iron sites in the amorphous part of the material. KW - Zn-Fe-Zr nanoparticles KW - Adsorption of phosphate KW - XAFS KW - Catalysis PY - 2017 DO - https://doi.org/10.1021/acs.jpcc.7b04773 SN - 1932-7447 VL - 121 IS - 45 SP - 25033 EP - 25042 PB - ACS Publications AN - OPUS4-43348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Otto, S. A1 - Moll, J. A1 - Förster, C. A1 - Geißler, Daniel A1 - Wang, Cui A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Three-in-One Crystal: The Coordination Diversity of Zinc Polypyridine Complexes N2 - The syntheses, structures, and photophysical properties of two new zinc(II) complexes bearing the tridentate N,N′-dimethyl-N,N′-dipyridin-2-ylpyridine-2,6-diamine (ddpd) ligand are presented. Structural investigations through single-crystal X-ray diffractometry, NMR spectroscopy, and density functional theory calculations revealed a diverse coordination behavior that depends on the counterion. Spectroscopic (UV/Vis and emission spectroscopy) and theoretical techniques (DFT and time-dependent DFT calculations) were employed to explore the photophysical properties of the complexes. KW - Zinc(II) complexes KW - X-ray diffractometry (XRD) KW - NMR spectroscopy KW - Density functional theory (DFT) KW - UV/Vis and emission spectroscopy PY - 2017 DO - https://doi.org/10.1002/ejic.201700948 SN - 1434-1948 SN - 1099-0682 VL - 43 SP - 5033 EP - 5040 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-43274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - Eddy current testing of compsite pressure vessels N2 - An internal project at BAM (Bundesanstalt für Materialforschung und -prüfung) pursue the goal to develop methods and models to investigate ageing of CFRP (carbon fiber reinforced plastic) composites pressure vessels. One main challenge is the application of appropriate testing methods for detecting the influences of pressure cycles and creep behavior on the material. This contribution presents results we achieved using conventional eddy current testing (ET) and high frequency ET. Before investigating pressure vessels, we studied test samples with artifcial defects. Here, we could show that also conventional ET with low frequencies are useable for CFRP samples which have at bottom holes of different size and depth. On the basis of the received results we deployed conventional ET besides high-frequency applications in order to investigate pressure vessels of different material combinations like steel-CFRP, Aluminum-CFRP and synthetics-CFRP. The thickness of the CFRP varies from 4 mm up to 8 mm. Here, we could detect both defects in the metal liner and in the CFRP. T2 - ISEM 2017 CY - Chamonix, France DA - 03.09.2017 KW - CFRP KW - Eddy current testing high frequency PY - 2017 AN - OPUS4-43279 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - qNMR spectroscopy has grown up to an original discipline – a review of recent international activities N2 - Quantitative NMR Spectroscopy (qNMR) provides the most universally applicable form of direct purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. Broadly accepted validation methods of qNMR spectroscopy will give users the tools to exploit qNMR more easily and enable them to speed up analytical method development and reduce the time and financial burden. The first initiative towards a worldwide agreement goes back to a panel discussion at PANIC 2014 (Practical Applications of NMR in Industry Conference) in Chicago. Since that, the Validation Workshop takes place following the PANIC Conference each year, last in 2017 with a turnout of over 50 people. The group aims at identifying a network of NMR people concerned with validation that can ultimately assist each other through the validation process, harmonize the terminology and a standard approach for NMR validations and position the guidelines produced by consensus of the NMR community so that accreditation agencies can use this process. T2 - qNMR Minisymposium CY - Baveno, Italy DA - 21.09.2017 KW - qNMR KW - Quantitative NMR Spectroscopy KW - Purity Analysis KW - SMASH KW - qNMR Summit PY - 2017 AN - OPUS4-42148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR T1 - Amts- und Mitteilungsblatt, Band 47, Heft 3 T3 - Amts- und Mitteilungsblatt der BAM - 3/2017 KW - Zulassungen KW - Zertifikate KW - Richtlinien KW - Ausnahmegenehmigungen KW - Festlegungen PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-421619 SN - 0340-7551 VL - 47 IS - 3 SP - 455 EP - 512 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-42161 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Advanced methods for nanomaterial characterization N2 - At the Final Outreach Event of the European FP7 NanoDefine project the results achieved during 4 years of intensive research and development work (2013-2017) with relevant stakeholders and wider community, and their practical implications and impact are presented and discussed. The newly developed particle-size related measurement tools and their practical suitability and applicability to classify materials, formulations and products according to the EC recommendation on the definition of a nanomaterial (2011/696/EU) are demonstrated. T2 - Final Outreach Event “Classification of nanomaterials according to the EU definition” CY - Brüssel, Belgium DA - 19.09.2017 KW - Nanomaterial KW - Nanoparticles KW - Particle sizing techniques KW - Nanomaterial classification PY - 2017 AN - OPUS4-42390 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Rauscher, H. T1 - Role of the volume specific surface area in the NanoDefine decision flow scheme N2 - In this lecture the VSSA concept is explained, and VSSA as measured by BET. Results of the NanoDefine evaluation based on selected examples on real-world materials are presented. Recommendations for consideration of the VSSA concept for the implementation of the EC definition of nanomaterial for powder materials are given. T2 - Final Outreach Event “Classification of nanomaterials according to the EU definition” CY - Brüssel, Belgium DA - 19.09.2017 KW - Volume specific surface area (VSSA) KW - Nanomaterial KW - Nanomaterial classification KW - BET PY - 2017 AN - OPUS4-42391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Deposition of nanoparticles by electrospray for improved analysis by SEM/TEM and EDX N2 - Of many experimental techniques for measuring particle sizes and size distributions, electron microscopy (EM) is still considered as the gold standard, especially in the nano range (1–100 nm). Furthermore, high-resolution X-ray spectroscopy (EDX) in conjunction with EM can be applied to individul NPs. Preparation of an EM sample for generic particulate materials is a difficult task. Usually, the particles in a suspension are deposited on a support. However, this procedure includes the drying of larger solvent amounts on the substrate itself, and this can affect the spatial distribution of the deposited particles. One possibility to overcome this is the use of an electrospray system, where the suspension of particles is sprayed onto the substrate in charged droplets that are so small that they either dry off on the substrate immediately without affecting the position of particles, or even already during their flight time to the substrate. Additionally, the charging of particles minimizes agglomeration and aggregation, maximizing the collection of the EM grids. The prototype of an electrospray deposition System was tested. Electrospray is theoretically described since a long time, but no dedicated commercial instruments are available for the preparation of TEM grids yet, apart from electrostatic deposition of aerosols. Several materials have been sprayed onto TEM grids and the resulting particle distributions were evaluated. Operation parameters such as the sample flow-rate, capillary – substrate distance, electric field strength and sampling period length have been optimized. It was found that the particles deposited by electrospray generally show a much more homogeneous spatial distribution on the substrate and a substantial increase of the number of single particles (suited to automatic analysis). T2 - 17th European Conference on Applications of Surface and Interface Analysis (ECASIA 2017) CY - Montpellier, France DA - 24.09.2017 KW - Electrospray deposition KW - Nanoparticles KW - SEM KW - TEM KW - TEM grid PY - 2017 AN - OPUS4-42393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane A1 - Ziegler, Mathias T1 - Neue Normen und Richtlinien für die Thermografie in der zerstörungsfreien Prüfung N2 - Da die Thermografie als zerstörungsfreies Prüfverfahren noch vergleichsweise neu in der Anwendung ist, beziehen sich die aktuell veröffentlichten und überarbeiteten Normen und Richtlinien im Wesentlichen auf die grundlegenden Prinzipien des Verfahrens und die verschiedenen Anregungs- und Auswertungstechniken, auf die Begriffe und auf die Gerätetechnik. Die grundlegenden Normen zum Prinzip des Prüfverfahrens, zu den Geräten und zu den Begriffen wurden in 2016 grundlegend überarbeitet und als CEN-Normen neu veröffentlicht. Im Anschluss dazu wird in 2017 der überarbeitete Normentwurf zur aktiven Thermografie veröffentlicht. Mit der Bearbeitung einer europäischen Norm zur Laserthermografie wurde begonnen. Auf nationaler Ebene werden zur Zeit Normen zu den verschiedenen Anregungstechniken erarbeitet. Anfang 2017 wurde der Normentwurf zur Impuls-Thermografie mit optischer Anregung veröffentlicht. Geplant sind weiterhin Entwurfsveröffentlichungen zur induktiv angeregten Thermografie sowie zur Lock-in-Thermografie mit optischer Anregung. Parallel dazu wurde die Überarbeitung der Norm zur Thermografischen Prüfung elektrischer Anlagen publiziert. Mit der Richtlinie VDI/VDE 3511 Blatt 4 bis 4.4 gibt es ein anerkanntes Regelwerk für die rückführbare Temperaturmessung und Kalibrierung von Strahlungsthermometern, die bisher für Thermografiekameras fehlte. In 2016 wurde daher die VDI/VDE Richtlinie 5585 Blatt 1 zur messtechnischen Charakterisierung von Thermografiekameras als Entwurf veröffentlicht. In Bearbeitung ist momentan Blatt 2 zur Kalibrierung von Thermografiekameras mit dem Ziel, auch für Thermografiekameras anerkannte Regeln zur rückführbaren Temperaturmessung zu erstellen. Im Beitrag werden die Anwendungsbereiche dieser Normen und Richtlinien vorgestellt und neue zukünftige Anwendungsbereiche in der Fertigung und Instandhaltung diskutiert. T2 - Thermografie-Kolloquium 2017 CY - Berlin, Germany DA - 28.9.2017 KW - Zerstörungsfreie Prüfung KW - Aktive Thermografie KW - Normung PY - 2017 AN - OPUS4-42396 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane T1 - Quantitative Fehlstellencharakterisierung mit Puls- und Lock-in-Thermografie N2 - Seit dem Beginn der Anwendung der aktiven Thermografie für die zerstörungsfreie Prüfung werden für die optische Anregung zwei alternative Anregungstechniken eingesetzt: die Puls- oder Blitzthermografie und die Lock-in-Thermografie. Bei der Puls-Thermografie ist der Anregungspuls wesentlich kürzer als die Zeit, die für die Wärmediffusion in das Bauteil hinein benötigt wird. Die Auswertung der erfassten Abkühlsequenzen wird zurzeit im Wesentlichen mit zwei Verfahren durchgeführt. Für die Auswertung im Zeitbereich werden verschiedene Auswertungsmodi des TSR-Verfahrens (TSR: thermal signal reconstruction) und Verfahren zur möglichst frühzeitigen Detektion des Intensitäts- oder Temperaturkontrastes der Fehlstellen herangezogen. Alternativ kann die Auswertung im Frequenzbereich nach dem Verfahren der Puls-Phasen-Thermografie (PPT) erfolgen. Dabei wird die Abkühlsequenz als Überlagerung vieler Einzelschwingungen betrachtet (Fouriersynthese). Die entsprechenden Phasenkontraste können unter bestimmten Umständen zur Abschätzung der Fehlstellentiefe genutzt werden. Bei der Lock-in Anregung wird das zu untersuchende Prüfobjekt periodisch mit einer bestimmten Frequenz erwärmt und die Wärmestrahlung von der Oberfläche zeitgleich mit der Infrarotkamera erfasst. Für jede Anregungsfrequenz ist daher eine Einzelmessung erforderlich. Die Auswertung bezieht sich in den meisten Fällen allein auf die Berechnung des Phasen- und Amplitudenbildes bei der Anregungsfrequenz. Diese Berechnung kann bereits während der Messung (on-line) oder erst nach der Erfassung der Thermogrammsequenz (off-line) erfolgen. Gemäß dem Superpositionsprinzip, das wegen des linearen Charakters der Wärmeleitungsgleichung für alle Lösungen der Differentialgleichung gilt, besteht Äquivalenz zwischen einer monofrequenten Anregung bei Lock-in-Thermografie und einer entsprechenden Komponente gleicher Frequenz bei der Puls-Thermografie. Daher sollten die Puls-Thermografie und die Lock-in-Thermografie in den Phasenbildern für die gleichen Fehlstellen die gleichen Phasenkontraste ergeben. Die experimentelle Bestätigung dieser Äquivalenz für unterschiedliche Fehlstellenarten ist der Schwerpunkt dieses Beitrages. Mögliche Gründe für Abweichungen werden benannt und sind Grundlage für weitere Diskussionen. T2 - Thermografie-Kolloquium 2017 CY - Berlin, Germany DA - 28.09.2017 KW - Zerstörungsfreie Prüfung KW - Aktive Thermografie KW - Impuls-Thermografie KW - Lock-in-Thermografie PY - 2017 AN - OPUS4-42397 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Hydrodynamic model of laser induced plasma including equilibrium chemistry N2 - Hydrodynamic model of laser induced plasma including plasma chemistry T2 - 6.07.2017, ITMO University, St. Petersburg, Russia CY - ITMO University, St. Petersburg, Russia DA - 5.07.2017 KW - Plasma KW - LIBS KW - Plasma modeling PY - 2017 AN - OPUS4-42294 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Predicting molecules in laser induced plasma based on equilibrium plasma model N2 - New development in modeling reactive flows in laser induced plasma T2 - 09.10.2017, SciX, Reno, NV, USA CY - Reno, NV, USA DA - 08.10.2017 KW - Laser induced plasma KW - LIBS KW - Plasma modeling PY - 2017 AN - OPUS4-42295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabe, Torsten T1 - Improved microstructure and strength of dry-pressed advanced ceramics by controlled slurry destabilization and ultrasonic atomization N2 - Spray drying of ceramic slurries aims for soft and free-flowing granules with homogenous microstructure neither containing voids nor hard shells suitable for uniaxial and isostatic pressing. The controlled destabilization of the slurries was introduced, since the unwanted formation of hard granules with voids donut-like shape could be drastically reduced. Spray drying of such modified slurries resulted in soft granules and finally leaded to sintered bodies with improved microstructure, density and strength. Optimized slurries were atomized in a laboratory spray dryer (Hi-Tec, Niro, Denmark) both with a commercial two stream nozzle and an adapted ultra sound atomization unit. Potential advantages of the ultra sound nebulization are investigated for model systems of alumina, zirconia and a ZTA composite while focusing on solids content of slurries, yield, and granule properties (size distribution, flowability, shape, microstructure, pressability) as well as the final sinter body properties (density, microstructure, strength). Using ultrasound nozzles in spray drying of identical slurries, as before tested and optimized for a two stream nozzle atomization process, resulted in a more suitable size distribution for dry pressing (less particles below 20 µm), a better flowability and a higher yield. Furthermore the sinter bodies produced of the ultra sound granules have higher sintered density, more homogenous microstructure without large pores and higher strength. T2 - EUROMAT, European Congress and Exhibition on Advanced Materials and Processes CY - Thessaloniki, Greece DA - 17.09.2017 KW - Granulation KW - Dry-pressing KW - Slurry KW - Ultrasonic atomization PY - 2017 AN - OPUS4-42299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Detlefsen, Malte A1 - Hüllmann, Dino A1 - Kohlhoff, Harald ED - Cosmi, Francesca T1 - A low-cost cable-suspended parallel manipulator for testing 3D olfaction algorithms N2 - Cable-suspended parallel manipulators have been a topic of research for multiple decades and called special attention in the fields of simulations. However, they are also well-suited for the simple evaluation of aerial-based mobile robot olfaction (MRO) algorithms, such as gas source localization and gas distribution mapping. Based on an open source framework for 3D printers, we designed a low-cost underconstrained, cable-suspended parallel manipulator. Computations are carried out purely on an Atmel ATmega2560 microcontroller. T2 - 34rd Danubia - Adria Symposium on Advances in Experimental Mechanics CY - Trieste, Italy DA - 19.09.2017 KW - Cable-suspended parallel manipulator KW - 3D KW - Mobile Robot Olfaction PY - 2017 SN - 978-88-8303-863-1 SP - 171 EP - 172 CY - Trieste AN - OPUS4-42316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Horn, Wolfgang A1 - Wilke, Olaf A1 - Mull, B. A1 - Richter, Matthias A1 - Brödner, Doris A1 - Mölders, N. A1 - Renner, M. T1 - Reproducibly emitting reference material for quality assurance/quality control of emission test chamber measurements N2 - Volatile Organic Compounds (VOC) are ubiquitous in the indoor air, since they emit from materials used indoors. Investigations of these materials are mostly carried out in test chambers under controlled climatic conditions. Quality control of these test chamber measurements is important but there is a lack of commercially available homogenous reference materials as required for round robin tests or quality assurance of laboratories. The approach of the present study is the impregnation of a supporting material with VOC, which are reproducibly released in measurable chamber air concentrations under standardised test conditions. A polymer made of Thermoplastic Polyurethane (TPU) was chosen as carrier material. It was impregnated with the VOC trimethyl pentanediol isobutyrat (texanol). T2 - Healthy Buildings 2017 Europe CY - Lublin, Poland DA - 02.07.2017 KW - Emissions testing KW - Volatile organic compounds KW - Polymeric material KW - CO2 assisted impregnation PY - 2017 SN - 978-83-7947-232-1 SP - Paper 0172, 1 EP - 2 AN - OPUS4-42348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shabanov, Sergej V. A1 - Gornushkin, Igor B. T1 - Geometrical effects in data collection and processing for calibration-free laser-induced breakdown spectroscopy N2 - Data processing in the calibration-free laser-induced breakdown spectroscopy (LIBS) is usually based on the solution of the radiative transfer equation along a particular line of sight through a plasma plume. The LIBS data processing is generalized to the case when the spectral data are collected from large portions of the plume. It is shown that by adjusting the optical depth and width of the lines the spectra obtained by collecting light from an entire spherical homogeneous plasma plume can be least-square fitted to a spectrum obtained by collecting the radiation just along a plume diameter with a relative error of 10 −11 or smaller (for the optical depth not exceeding 0.3) so that a mismatch of geometries of data processing and data collection cannot be detected by fitting. Despite the existence of such a perfect least-square fit, the errors in the line optical depth and width found by a data processing with an inappropriate geometry can be large. It is shown with analytic and numerical examples that the corresponding relative errors in the found elemental number densities and concentrations may be as high as 50% and 20%, respectively. Safe for a few found exceptions, these errors are impossible to eliminate from LIBS data processing unless a proper solution of the radiative transfer equation corresponding to the ray tracing in the spectral data collection is used. KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2018 DO - https://doi.org/10.1016/j.jqsrt.2017.09.018 SN - 0022-4073 SN - 1879-1352 VL - 204 SP - 190 EP - 205 PB - Elsevier AN - OPUS4-43131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Research and development in material and life sciences and quality assurance at BAM N2 - Research and development activities at BAM are presented with Special Focus on bioanalysis and biophotonics. This includes Topics from the Focus Areas Material, Environment, and Analytical Sciences. Also, Job opportunities at BAM are emphasized. T2 - MPI CY - Göttingen, Germany DA - 26.10.2017 KW - Analytics KW - Materials KW - Fluorometry KW - Sensors KW - Biophotonics KW - Microbiology KW - Reference material KW - Standard KW - Calibration KW - Nanoparticle PY - 2017 AN - OPUS4-43132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Semiconductor nanocrystals with VIS and NIR/IR emission - spectroscopy properties and surface chemistry N2 - Semiconductor nanocrystals with a spherical (QDs) core and a spherical or a rod-shaped Shell, u.a., so-called Quantum dot-Quantum rods (QDQRs) are increasingly used as fluorescent Reporters or optically active components in the life and material science, e.g., in solid state lightening including Plasma Displays. (1,2) Morever, there is an increasing interest in materials with emission >800 nm for bioanalysis, medical diagnostics, and safety barcodes. Prerequisites for the mechanistic understanding of nonradiativ decay channels needed for the rational design of improved nanomaterials and the comparison of material Performance are reliable fluorescence measurements and validated methods for the assessment of their surface chemistry. (3,4) The latter is of particular importance for nanocrystalline Emitters, where surface states and the accessibility of emissive states by quenchers largely control photoluminescence properties. (5) Here, we present results from systematic spectroscopic studies including absolutely measured photolumunescence Quantum yields of different vissible and NIR emisisve QD and QDQRs Systems of varying particle architecture size and surface chemistries in Dispersion and embedded in salt crystals. (6,7) T2 - MCare 2017 CY - Jeju, South Korea DA - 20.02.2017 KW - Semiconductor quantum dot KW - Nanoparticle KW - Absolute fluorometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Fluorescence KW - Surface chemistry KW - Photophysics KW - Quantum yield KW - Single particle PY - 2017 AN - OPUS4-43133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pavlovic, Mato T1 - The importance of determining the POD of the NDT system when designing a safe component N2 - Non-Destructive Testing (NDT) is routinely used in aerospace, nuclear, railway and automotive industries. The most common use of NDT is to find flaws in components. In dynamically loaded components, flaws grow, and if they are not detected in time and no corrective measures are taken they can reach critical sizes. When a flaw reaches a critical size, it endangers the structural integrity of the component and will likely cause the component to fail. To detect flaws before they reach a critical size, components are inspected in fixed time intervals with non-destructive testing systems. In order to determine the amount of time between inspections, three variables are necessary: the critical size of the flaw, the flaw propagation speed and the size of the flaw that can be reliably detected by NDT. All three variables are, to a certain extent, stochastic. The critical size of the flaw and flaw propagation speed are questions of fracture mechanics. The size of the flaw that can be reliably detected by NDT is predicted by POD curves. The POD is determined for a given inspection scenario. The inspection scenario includes the NDT system, the component geometry and the type of the flaw. If one of these changes, the POD will also change and needs to be recalculated. As a result, the design of a dynamically loaded safety-relevant components is an iterative process in which a geometry is sought that provides an optimum between structural integrity and inspectability. A model that describes the iterative process for the design of the safe components with examples from praxis will be presented. T2 - 15th ASIA PACIFIC CONFERENCE FOR NON-DESTRUCTIVE TESTING (APCNDT) CY - Singapore DA - 13.11.2017 KW - Safety KW - Mechanical design KW - Fracture mechanics KW - Nondestructive testing KW - POD PY - 2017 AN - OPUS4-43134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Analysis of the Operation of Accreditation Bodies - Conduction and Results from the first benchmarking Round with 8 Accreditation Bodies N2 - In autumn 2014 the German accreditation body Deutsche Akkreditierungsstelle GmbH (DAkkS) and the German federal institute Bundesanstalt für Materialforschung und –prüfung (BAM) initiated a project to compare the operations of accreditation bodies by developing and implementing a tailor-made management tool. Eight European Accreditation Bodies attended the first benchmarking round. By means of the Process Maturity Benchmarking Tool (PMBT) a set of relevant processes was identified and analyzed using indicators based on data from data records and the maturity of the investigated processes. A Results-Workshop was conducted with experts from the accreditation bodies to identify best practices and discuss different modes of operation. T2 - 40. Genaral Assembly der European Cooperation for Accreditation (EA) CY - Berlin, Germany DA - 22.11.2017 KW - Accreditation KW - Benchmarking PY - 2017 AN - OPUS4-43135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas T1 - Keramikdurchflusszellen für das industrielle Reaktionsmonitoring mit Niederfeld-NMR-Spektroskopie N2 - Derzeit verfügbare Niederfeld-NMR-Spektrometer sind oft für Laborapplikationen konzipiert. Für den Einsatz im industriellen Prozessmonitoring müssen deshalb Anpassungen vorgenommen werden. Ein wichtiger Aspekt ist die Gestaltung der Messzelle. Sie muss über eine hohe thermische-, chemische und vor allem mechanische Beständigkeit verfügen. Hinzu kommt die Besonderheit des NMR-Experiments, das auf die Durchlässigkeit von Radiofrequenzen angewiesen ist. Keramik ist ein in der Hochfeld-NMR-Spektroskopie bewährtes Material das diese Eigenschaften vereint. Um im Prozessmonitoring die Interessen kleiner Bypass-Volumina, großer Durchflussgeschwindigkeit und großes Signal-zu-Rausch-Verhältnis mit der nötigen Vormagnetisierungszeit in Einklang zu bringen, ist eine im Messbereich aufgeweitete Zellgeometrie vorteilhaft. Die Fertigung einer Keramikmesszelle für die Niederfeld-NMR-Spektroskopie für Drücke bis 7 MPa mit dieser besonderen Geometrie wurde mit Hilfe eines modernen additiven Fertigungsverfahrens realisiert. Quantitative NMR-Messungen an konstant durch das Spektrometer strömenden Flüssigkeiten werden durch eine maximale Durchflussgeschwindigkeit limitiert. Diese wird von vielen Einflussgrößen bestimmt und sollte vor jeder quantitativen Messreihe experimentell für das individuelle System ermittelt werden. Zu diesem Zweck wurde eine automatisierte Laboranordnung konzipiert. Der Vergleich der neuen NMR-Keramikzelle mit bestehenden Messzellen u. a. anhand dieses Parameters untermauert ihre Eignung für das industrielle Prozessmonitoring. T2 - 13. Herbstkolloquium Arbeitskreis Prozessanalytik CY - Esslingen, Germany DA - 20.11.2017 KW - Keramikdurchflusszelle KW - Niederfeld-NMR KW - Online-NMR PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-430918 AN - OPUS4-43091 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Simple calibration concept of an online NMR module demonstrated in a modularised production plant N2 - Monitoring specific information (such as physico-chemical properties, chemical re-actions, etc.) is the key to chemical process control. Within the CONSENS Project, the challenge to adapt a commercially available benchtop NMR spectrometer to the full requirements of an automated chemical production environment was tack-led. The developed online NMR module was provided in an explosion proof housing and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit, a programmable logic controller for automated triggering, flow con-trol, as well as data communication. First results of an aromatic coupling reaction in lab scale showed a general feasibil-ity according to the signal information in the acquired NMR spectra even though with a considerable overlap. Due to the comparatively low field strength of the NMR spectrometer multivariate methods had to be considered for the prediction of con-centration profiles based on spectral data. Typically, for industrial application of those methods, e.g. Partial Least Squares Regression (PLS-R) as well as Indirect Hard Modeling, large amount of calibration data is demanded, which must be ac-quired in time consuming lab-scale experiments and offline analytics. When it comes to changes in raw materials (e.g., varying functional groups, additional stabi-lizing agents) calibration experiments and data evaluation models are developed again. Here we present an approach of automated data analysis tools for low field NMR spectra with minimal calibration effort. The algorithms are based on Indirect Hard Modeling, whereby each component in each mixture spectra can be rep-resented by several flexible peak functions (pure component models). This means, that only pure component NMR spectra are needed to generate a first evaluation model. The flexibility of peak functions in the spectral model can be adjusted via constraints of peak parameters. The area of any pure component model can either be converted to concentrations based on a one-point calibration on raw material concentration or even neat solvent signals. In several cases it has been shown, the IHM works almost independently of the matrix of the real samples. Such a calibration can be repeated daily in the beginning of each process run with minimal time effort. Moreover, additional pure components can be added to the model or even substitut-ed while keeping the previously adjusted peak function constraints. The proposed method exhibited good agreement of resulting concentration data from low field NMR spectra, when compared to an online high field NMR spectrometer as refer-ence instrument. T2 - 13. Kolloquium des Arbeitskreises Prozessanalytik der DECHEMA und der GDCh-Fachgruppe Analytische Chemie CY - Esslingen, Germany DA - 20.11.2017 KW - Online monitoring KW - Online NMR spectroscopy KW - Modularised production PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-430999 AN - OPUS4-43099 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Laser-Thermografie – Von der flächigen zur strukturierten Anregung N2 - Im Bereich der optisch angeregten Thermografie haben sich Blitzlampen (impulsförmig-flächige Erwärmung) und Halogenlampen (moduliert-flächige Erwärmung) für die spezifischen Regime Impuls- und Lockin-Thermografie etabliert. Mittels eines rasternden fokussierten Lasers wird die Flying-spot Laserthermografie z.B. zur Risserkennung (Dauerstrichbetrieb) und die photothermische Materialcharakterisierung (hochfrequent moduliert)implementiert. Durch die Verfügbarkeit neuer Technologien (schnelle und hochauflösende IR-Kameras, brillante innovativer Lichtquellen und performante Datenakquisitions- und Verarbeitungstechnik) wird ein Paradigmenwechsel von den getrennt voneinander stehenden photothermischen und thermografischen Techniken hin zu einer einheitlichen quantitativen Mess-und Prüftechnik ermöglicht, die schneller und präziser ist. Ähnlich wie ein LED-Array, jedoch mit einer um zwei Größenordnungen höheren Bestrahlungsstärke, steht jetzt eine neuartige brillante Laserquelle, das VCSEL-Array (vertical-cavity surface-emitting laser) zur Verfügung, welches die starke Beschränkung der zeitlichen Dynamik der etablierten Lichtquellen aufhebt und gleichzeitig spektral sauber von der Detektionswellenlänge getrennt ist. Es vereint somit das schnelle zeitliche Verhalten eines Diodenlasers mit der hohen optischen Bestrahlungsstärke und dem großen Beleuchtungsbereich von Blitzlampen. Darüber hinaus kann die Erwärmung auch strukturiert vorgenommen werden, da einzelne Bereiche des VCSEL-Arrays unabhängig voneinander angesteuert werden können. Dieser neue Freiheitsgrad ermöglicht die Entwicklung ganz neuer thermografischer ZfP-Verfahren. T2 - Thermographie-Kolloquium 2017 CY - Berlin, Germany DA - 28.09.2017 KW - Thermografie KW - Laser KW - Zerstörungsfreie Prüfung KW - VCSEL KW - Photothermisch PY - 2017 AN - OPUS4-43115 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias A1 - Thiel, Erik A1 - Studemund, Taarna T1 - Laser-Thermografie – Von der flächigen zur strukturierten Anregung N2 - Im Bereich der optisch angeregten Thermografie haben sich Blitzlampen (impulsförmig-flächige Erwärmung) und Halogenlampen (moduliert-flächige Erwärmung) für die spezifischen Regime Impuls- und Lockin-Thermografie etabliert. Mittels eines rasternden fokussierten Lasers wird die Flying-spot Laserthermografie z.B. zur Risserkennung (Dauerstrichbetrieb) und die photothermische Materialcharakterisierung (hochfrequent moduliert)implementiert. Durch die Verfügbarkeit neuer Technologien (schnelle und hochauflösende IR-Kameras, brillante innovativer Lichtquellen und performante Datenakquisitions- und Verarbeitungstechnik) wird ein Paradigmenwechsel von den getrennt voneinander stehenden photothermischen und thermografischen Techniken hin zu einer einheitlichen quantitativen Mess-und Prüftechnik ermöglicht, die schneller und präziser ist. Ähnlich wie ein LED-Array, jedoch mit einer um zwei Größenordnungen höheren Bestrahlungsstärke, steht jetzt eine neuartige brillante Laserquelle, das VCSEL-Array (vertical-cavity surface-emitting laser) zur Verfügung, welches die starke Beschränkung der zeitlichen Dynamik der etablierten Lichtquellen aufhebt und gleichzeitig spektral sauber von der Detektionswellenlänge getrennt ist. Es vereint somit das schnelle zeitliche Verhalten eines Diodenlasers mit der hohen optischen Bestrahlungsstärke und dem großen Beleuchtungsbereich von Blitzlampen. Darüber hinaus kann die Erwärmung auch strukturiert vorgenommen werden, da einzelne Bereiche des VCSEL-Arrays unabhängig voneinander angesteuert werden können. Dieser neue Freiheitsgrad ermöglicht die Entwicklung ganz neuer thermografischer ZfP-Verfahren. T2 - Thermographie-Kolloquium 2017 CY - Berlin, Germany DA - 28.09.2017 KW - Thermografie KW - Laser KW - Zerstörungsfreie Prüfung KW - Lock-in KW - VCSEL KW - Photothermisch PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-431170 UR - https://www.dgzfp.de/Portals/thermo2017/BB/6.pdf SN - 978-3-940283-88-7 VL - 163 SP - 1 EP - 15 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-43117 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Colson, K. A1 - Schönberger, T. T1 - The q in NMR – a review of recent international activities N2 - Quantitative NMR Spectroscopy (qNMR) provides the most universally applicable form of direct purity determination without need for reference materials of impurities or the calculation of response factors for all samples exhibiting suitable NMR properties. Broadly accepted validation methods of qNMR spectroscopy gives users tools to exploit qNMR more easily and enables rapid analytical method development and reduce time and financial burdens. The first initiative towards a worldwide agreement goes back to a panel discussion at PANIC 2014 (Practical Applications of NMR in Industry Conference) in Chicago. Since that time, the Validation Workshop takes place each year following the PANIC Conference, last in 2017 with a turnout of over 65 people. The group aims to identifying a network of NMR people concerned with validation that can ultimately assist each other through the validation process, harmonize the terminology and a standard approach for NMR validations and position the guidelines produced by consensus of the NMR community so that accreditation agencies can use this process. The talk briefly summarises the outcome of the former PANIC Validation Workshops (2015, 2016, and 2017) as well as the recent satellite meetings including the qNMR meeting held at Spectral Service in Cologne, Germany (June 2016), a validation workshop at SMASH (La Jolla, USA, September 2016), the qNMR Summit with USP in Rockville, USA (October 2016), the qNMR Summit at BAM in Berlin, Germany (March 2017), and the qNMR Minisymposium at SMASH in Baveno, Italy (September 2017). Upcoming activities will be a qNMR Summit held by JP and JEOL in Tokyo, Japan (January 29th-30th, 2018) and a qNMR Summit at the University of Würzburg, Germany (planned for October 2018). The next PANIC takes place March 4th-8th, 2018 in La Jolla (San Diego), CA, USA. Further Information can be found under: http://www.validnmr.com T2 - qNMR Day CY - Politecnico di Bari, Bari, Italy DA - 24.11.2017 KW - qNMR KW - Quantitative NMR Spectroscopy KW - NMR validation KW - qNMR Summit KW - Direct purity determination PY - 2017 UR - http://www.gidrm.org/index.php/activities/workshops/2017-workshops/qnmr-day-a-gidrm-organized-in-cooperation-with-girm AN - OPUS4-43118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - qNMR metrology and current "primary" reference material activities N2 - In general, most quantitative organic chemical measurements rely on the availability of highly purified compounds to act as calibration standards. The traceability and providence of these standards is an essential component of any measurement uncertainty budget and provides the final link of the result to the units of measurement, ideally the SI. The more recent increase in the use of qNMR for the direct assessment of chemical purity however can potentially improve the traceability and reduce the uncertainty of the measured chemical purity at a reduced cost and with less material. For example, the method has beneficially been used by National Metrology Institutes for comparisons including comparisons on CCQM (Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology, www.bipm.org). First comparisons started 1998 with CCQM-P3 (Organics in solution) or CCQM-P35 (2002, EtOH in solution), were underpinned by a broad range of polarity and molecular size (CCQM–K55 series of purity studies including Valine, Aldrin, or Folic acid) and were continued with the recent pilot studies CCQM-P150 (2014, purity of Dimethyl sulfone) or CCQM-P150b (2017, purity of Pyributicarb). Traditional ‘indirect’ methods of purity analysis require that all impurities are identified and quantified, leading to a minimum of four individual analytical methods (organic impurities, water, solvents, inorganic residue). These multiple technique approaches measure an array of different chemical impurities normally present in purified organic chemical compounds. As many analytical methodologies have compound-specific response factors, the accuracy and traceability of the purity assessment is dependent on the availability of reference materials of the impurities being available. qNMR provides the most universally applicable form of direct purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. The development of CRMs addressing qNMR specific measurement issues will give analysts compounds ideally suited for the analytical method and also provide full characterisation of qNMR related parameters to enable more realistic uncertainty budgets. These materials will give users the tools to exploit qNMR more easily and enable them to speed up analytical method development and reduce the time and financial burden of multiple analytical testing. Due to recent advances in technical developments of NMR instruments such as acquisition electronics and probe design, detection limits of components in liquid mixtures were improved into the lower ppm range (approx. 5–10 ppm amount of substance) qNMR studies increasingly attract broader interest. T2 - qNMR Day CY - Politecnico di Bari, Bari, Italy DA - 24.11.2017 KW - qNMR KW - Quantitative NMR spectroscopy KW - qNMR metrology KW - Primary reference material KW - Comparison study KW - Direct purity determination PY - 2017 UR - http://www.gidrm.org/index.php/activities/workshops/2017-workshops/qnmr-day-a-gidrm-organized-in-cooperation-with-girm AN - OPUS4-43119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Leonhard, H. T1 - Korrosionsschutz bekennt Farbe - Schnelltest auf Korrosionsgefahr bei nicht rostenden Stählen N2 - In Chemieanlagen ist die Passivschicht von Rohrsystemen und Behältern aus nichtrostendem Stahl nicht nur durch den rauen Produktionsalltag gefährdet. Auch im Neuzustand können Schäden entstehen, bspw. durch Schleifvorgänge oder eine unvollständige Entfernung von Anlauffarben nach dem Schweißen. TÜV SÜD Chemie Service beteiligte sich an der Prüfung eines von der Bundesanstalt für Materialforschung und -prüfung (BAM) entwickelten Korrosionsschnelltests. KorroPads liefern in nur 15 Minuten eine valide Aussage zum Zustand der Passivschicht auf den Werkstoffoberflächen. KW - Nichtrostender Stahl KW - Korrosionsschnelltest KW - KorroPad KW - Passivschicht PY - 2017 SN - 0340-9961 VL - 46 IS - 11 SP - 46 EP - 48 PB - Hüthig GmbH CY - Heidelberg AN - OPUS4-43120 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Halisch, Matthias A1 - Kruschwitz, Sabine A1 - Weller, Andreas A1 - Mensching, Bernadette A1 - Gürlich, Lucinda T1 - Maximizing the core value – joint investigations with special emphasis on complex electrical conductivity give new insights into Fontainebleau Sandstone N2 - Within this study we have shown, that spectral induced polarization is a reliable method for the enhanced characterization of the Fontainebleau sandstone in general, and for its related stratigraphical units in particular. Due to its high sensitivity towards pore network and pore surface changes, different stratigraphical units can be clearly differentiated and probably even classified. We have observed a good correlation between the maximum of the SIP phase shift and the dominant pore throat radius for this rock type, as it has been reported for others sandstones before [20]. T2 - Annual Symposium of the Society of Core Analysts CY - Vienna, Austria DA - 27.08.2017 KW - Spectral induced polarization KW - µ-CT KW - ESEM KW - Fontainebleau Sandstone PY - 2017 SP - 035, 1 EP - 035, 9 AN - OPUS4-43079 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Senoner, Mathias A1 - Wirth, Thomas A1 - Bütefisch, S. A1 - Busch, I. T1 - Lateral resolution delivered by imaging surface-analytical instruments as SIMS, AES and XPS: Application of the BAM-L200 Certified Reference Material and related ISO Standards N2 - The certified reference material BAM-L200, a nanoscale stripe pattern for length calibration and specification of lateral resolution, is described. BAM-L200 is prepared from a cross-sectioned epitaxially grown layer stack of AlxGa1-xAs and InxGa1 xAs on a GaAs substrate. The surface of BAM-L200 provides a flat pattern with stripe widths ranging down to 1 nm. Calibration distances, grating periods and stripe widths have been certified by TEM with traceability to the length unit. The combination of gratings, isolated narrow stripes and sharp edges of wide stripes offers a plenty of options for the determination of lateral resolution, sharpness and calibration of length scale at selected settings of imaging surface analytical instruments. The feasibility of the reference material for an analysis of the lateral resolution is demonstrated in detail by evaluation of ToF-SIMS, AES and EDX images. Other applications developed in the community are summarized, too. BAM-L200 fully supports the implementation of the revised International Standard ISO 18516 (in preparation) which is based on knowledge outlined in the Technical Report ISO/TR 19319:2013. KW - Standardization KW - AES KW - XPS KW - SIMS KW - Lateral resolution KW - Certified reference material PY - 2017 SN - 1341-1756 VL - 24 IS - 2 SP - 123 EP - 128 AN - OPUS4-43138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul T1 - KorroPad-Prüfung - Anwendungen aus Industrie und Forschung - N2 - Mit der KorroPad-Prüfung kann die Lochkorrosionsbeständigkeit nichtrostender Stähle auf sehr einfache, schnelle und kostengünstige Weise eingeschätzt werden. Das Kor-roPad ist damit für Hersteller, Verarbeiter und Anwender nichtrostender Stähle eine interessante Alternative zu zeitintensiven Langzeitversuchen und komplexe elektrochemischer Untersuchungsmethoden. Die prinzipiellen Funktionsweise der KorroPad-Prüfung wird im Vortrag beschrieben, um anschließend verschiedene Anwendungen aus Industrie und Forschung vorzustellen. Exemplarisch werden dazu die Bewertung von Schleif- und Passivierungsprozessen, die Qualitätskontrolle der Wärmebehandlung und Oberflächenbearbeitung von Schneidwaren sowie die Optimierung der Schweißnaht-Nachbehandlung vorgestellt. Mit der KorroPad-Prüfung lassen sich aber auch werkstoff- und gefügebedingte Einflüsse auf die Lochkorrosionsbeständigkeit gezielt untersuchen. Dies wird an Beispielen aus aktuellen Forschungsprojekten dargestellt. Die abschließend dargestellte Charakterisierung vom Sensibilisierungsverhalten mit der KorroPad-Prüfung ist verdeutlicht das breite Anwendungsspektrum bei der Charakterisierung von nichtrostenden Stählen. T2 - Arbeitskreissitzung „Korrosionsuntersuchung und -überwachung“ des GfKORR e. V. CY - Magdeburg, Germany DA - 21.11.2017 KW - Korrosion KW - Nichtrostender Stahl KW - KorroPad KW - Schneidwaren KW - Oberflächenbehandlung KW - Lochkorrosion KW - Wärmebehandlung KW - Sensibilisierung KW - EPR PY - 2017 AN - OPUS4-43141 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul T1 - Referenzmaterialien für die Charakterisierung nichtrostender Stähle N2 - Im Vortrag wird ein innovativer Ansatz zur Herstellung von Referenzmaterialien für systematische Grundlagenuntersuchungen und Methodenentwicklungen vorgestellt. Dieser Ansatz basiert auf der Verwendung eines Lichtbogenschmelzofens (Arc-Melter), der zur Legierungsvariation bei nichtrostenden Stählen verwendet wurde. In Abhängigkeit vom Chromgehalt wurden zunächst Ergebnisse der elektrochemisch potentiodynamischen Reaktivierung (EPR) und der KorroPad-Prüfung vorgestellt, die neue Einblicke zur Nachweisgrenze beider Verfahren liefern. Anschließend wurde der Einfluss vom Schwefelgehalt auf die Lochkorrosionsbeständigkeit dargestellt und dabei gezeigt, dass die in den Normen festgeschriebenen Grenzwerte deutlich zu hoch sind. Darüber hinaus wurden zukünftig geplante Arbeiten vorgestellt, die mit diesem Ansatz möglich sind. T2 - Arbeitskreissitzung „Korrosionsuntersuchung und -überwachung“ des GfKORR e. V. CY - Magdeburg, Germany DA - 21.11.2017 KW - Referenzmaterialien KW - Lichtbogenschmelzofen KW - Nichtrostender Stahl KW - Korrosion KW - KorroPad KW - EPR KW - Nachweisgrenze KW - Lochkorrosion PY - 2017 AN - OPUS4-43142 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - Preparation and certification of ethanol/water CRMs at BAM N2 - The presentation describes the preparation and certification of ethanol/water certified reference materials for the calibration of evidential breath alcohol analysers at BAM. T2 - ALCOREF kick-off meeting and training CY - Berlin, Germany DA - 16.10.2017 KW - Certified Reference Material KW - Breath alcohol analyser KW - Calibration PY - 2017 AN - OPUS4-43057 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - BAM GC-FID method for the quantification of ethanol in water N2 - The talk presents an analytical method for the quantification of ethanol in water. The method is based on gas chromatography with flame ionisation detection and on-column injection. It is used at BAM for the certification and quality assurance of reference materials for the calibration of evidential breath alcohol analysers. T2 - ALCOREF kick-off meeting and training CY - Berlin, Germany DA - 16.10.2017 KW - GC-FID KW - Certified reference material KW - Breath alcohol analysis PY - 2017 AN - OPUS4-43061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, Jenny A1 - Bald, Ilko T1 - Low‐energy electron‐induced strand breaks in telomere‐derived DNA sequences—influence of DNA sequence and topology N2 - During cancer radiation therapy high‐energy radiation is used to reduce tumour tissue. The irradiation produces a shower of secondary low‐energy (<20 eV) electrons, which are able to damage DNA very efficiently by dissociative electron attachment. Recently, it was suggested that low‐energy electron‐induced DNA strand breaks strongly depend on the specific DNA sequence with a high sensitivity of G‐rich sequences. Here, we use DNA origami platforms to expose G‐rich telomere sequences to low‐energy (8.8 eV) electrons to determine absolute cross sections for strand breakage and to study the influence of sequence modifications and topology of telomeric DNA on the strand breakage. We find that the telomeric DNA 5′‐(TTA GGG)2 is more sensitive to low‐energy electrons than an intermixed sequence 5′‐(TGT GTG A)2 confirming the unique electronic properties resulting from G‐stacking. With increasing length of the oligonucleotide (i.e., going from 5′‐(GGG ATT)2 to 5′‐(GGG ATT)4), both the variety of topology and the electron‐induced strand break cross sections increase. Addition of K+ ions decreases the strand break cross section for all sequences that are able to fold G‐quadruplexes or G‐intermediates, whereas the strand break cross section for the intermixed sequence remains unchanged. These results indicate that telomeric DNA is rather sensitive towards low‐energy electron‐induced strand breakage suggesting significant telomere shortening that can also occur during cancer radiation therapy. KW - DNA radiation damage KW - Telomere KW - DNA origami KW - Electron PY - 2018 DO - https://doi.org/10.1002/chem.201705889 SN - 1521-3765 SN - 0947-6539 VL - 24 IS - 18 SP - 4680 EP - 4688 PB - Wiley AN - OPUS4-44702 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ribar, A. A1 - Huber, S. E. A1 - Smiałek, M. A. A1 - Tanzer, K. A1 - Neustetter, M. A1 - Schürmann, Robin A1 - Bald, Ilko A1 - Denifl, S. T1 - Hydroperoxyl radical and formic acid formation from common DNA stabilizers upon low energy electron attachment N2 - 2-Amino-2-(hydroxymethyl)-1,3-propanediol (TRIS) and ethylene-diaminetetraacetic acid (EDTA) are key components of biological buffers and are frequently used as DNA stabilizers in irradiation studies. Such surface or liquid phase studies are done with the aim to understand the fundamental mechanisms of DNA radiation damage and to improve cancer radiotherapy. When ionizing radiation is used, abundant secondary electrons are formed during the irradiation process, which are able to attach to the molecular compounds present on the surface. In the present study we experimentally investigate low energy electron attachment to TRIS and methyliminodiacetic acid (MIDA), an analogue of EDTA, supported by quantum chemical calculations. The most prominent dissociation channel for TRIS is through hydroperoxyl radical formation, whereas the dissociation of MIDA results in the formation of formic and acetic acid. These compounds are well-known to cause DNA modifications, like strand breaks. The present results indicate that buffer compounds may not have an exclusive protecting effect on DNA as suggested previously. KW - DEA KW - DNA KW - Low energy electrons KW - Mass spectrometry PY - 2018 UR - http://pubs.rsc.org/en/content/articlepdf/2018/cp/c7cp07697e DO - https://doi.org/10.1039/c7cp07697e VL - 20 IS - 8 SP - 5578 EP - 5585 PB - Royal Society of Chemistry AN - OPUS4-44703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotschate, Daniel A1 - Gaal, Mate A1 - Kersten, H. T1 - Acoustic emission by self-organising effects of micro-hollow cathode discharges N2 - We designed micro-hollow cathode discharge prototypes under atmospheric pressure and investi-gated their acoustic characteristics. For the acoustic model of the discharge, we correlated the self-organisation effect of the current density distribution with the ideal model of an acoustic membrane. For validation of the obtained model, sound particle velocity spectroscopy was used to detect and analyse the acoustic emission experimentally. The results have shown a behaviour similar to the ideal acoustic membrane. Therefore, the acoustic excitation is decomposable into its eigenfrequencies and predictable. The model was unified utilising the gas exhaust velocity caused by the electrohydrodynamic force. The results may allow a contactless prediction of the current density distribution by measuring the acoustic emission or using the micro-discharge as a tunable acoustic source for specific applications as well. KW - Micro hollow cathode discharge KW - Atmospheric pressure plasma KW - Gas discharges KW - Plasma acoustics PY - 2018 DO - https://doi.org/10.1063/1.5024459 SN - 0003-6951 VL - 112 IS - 15 SP - Article 154102, 1 EP - 4 PB - AIP Publishing AN - OPUS4-44659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lauer, Franziska T1 - A graphical user interface for a fast multivariate classification of MALDI-TOF MS data of pollen grains N2 - The common characterization and identification of pollen is a time-consuming task that mainly relies on microscopic determination of the genus-specific pollen morphology. A variety of spectroscopic and spectrometric approaches have been proposed to develop a fast and reliable pollen identification using specific molecular information. Amongst them, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) shows a high potential for the successful investigation of such complex biological samples. Based on optimized MALDI sample preparation using conductive carbon tape, the application of multivariate statistics (e.g. principal components analysis, PCA) yields an enormous improvement concerning taxonomic classification of pollen species compared to common microscopic techniques. Since multivariate evaluation of the recorded mass spectra is of vital importance for classification, it’s helpful to implement the applied sequence of standard Matlab functions into a graphical user interface (GUI). In this presentation, a stand-alone application (GUI) is shown, which provides multiple functions to perform fast multivariate analysis on multiple datasets. The use of a GUI enables a first overview on the measured dataset, conducts spectral pretreatment and can give classification information based on HCA and PCA evaluation. Moreover, it can be used to improve fast spectral classification and supports the development of a simple routine method to identify pollen based on mass spectrometry. T2 - 12. Interdisziplinäres Doktorandenseminar, GDCh AK Prozessanalytik CY - BAM, AH, Berlin, Germany DA - 25.03.2018 KW - MALDI KW - GUI KW - Pollen PY - 2018 AN - OPUS4-44661 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc A1 - Tiebe, Carlo A1 - Banach, Ulrich A1 - Ritter, U. T1 - Ionic Liquid Based Coulometric Trace Humidity Sensors N2 - This work presents a first attempt to use ionic liquids as a new coating for planar coulometric sensors. These sensors are used for the measurement of trace humidity in various gases. Usually, the coating of the sensors is tetraphosphorus decaoxide and its hydrolysis products. Instead, a hygroscopic ionic liquid was used as sensor coating in this work. Generated frost point temperatures tf in the gas ranged from -80 °C to -30 °C, which is equivalent to vapour mole fractions xv from 0.5 μmol·mol-1 to 376 μmol·mol-1. In addition to the coulometric sensors, the generated humidity is determined by a precision dew point hygrometer as reference. First results show that it is possible to measure humidity with ionic liquid based coulometric sensors. T2 - ALLSENSOR 2018 CY - Rom, Italy DA - 25.03.2018 KW - Ionic liquids. KW - Coulometric sensors KW - Sensor coating KW - Trace humidity measurement PY - 2018 SN - 978-1-61208-621-7 SP - 13 EP - 14 PB - IARIA AN - OPUS4-44609 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schwaar, Timm T1 - Multidimensional high throughput methods for the analysis of particle-based peptide libraries N2 - Screening of one-bead-one-peptide libraries is a useful procedure for the identification of protein ligands. The demand for binders with high affinity and high specificity towards various target proteins has surged in the biomedical field in the recent years. The 1 traditional peptide screening procedure involves tedious steps as selection, sequencing, and characterization. Herein, we developed a high-throughput – “all in one chip” system to avoid time-consuming separation steps. T2 - Chemistry and Biology of Peptides Gordon Research Conference CY - Ventura, CA, USA DA - 10.02.2018 KW - Lab-on-a-chip KW - Combinatorial peptide library PY - 2018 AN - OPUS4-44611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schwaar, Timm T1 - MALDI-Supported Screening of Large Peptide Libraries for Identification of Protein Binders N2 - Screening of one-bead-one-peptide libraries is a useful procedure for the identification of protein ligands. The demand for binders with high affinity and high specificity towards various target proteins has surged in the biomedical field in the recent years. The traditional peptide screening procedure involves tedious steps as selection, sequencing, and characterization. Herein, we developed a high-throughput – “all in one chip” system to avoid time-consuming separation steps. T2 - European Mass Spectrometry Conference (EMSC) 2018 CY - Saarbrücken, Germany DA - 11.02.2018 KW - Lab-on-a-chip KW - Combinatorial peptide library PY - 2018 AN - OPUS4-44612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abbas, Ioana M. T1 - Troubleshooting for the clinical measurement of iron biomarkers using LC-MS/MS: Suppression of sample losses in autosampler vials N2 - We developed a rapid and robust HPLC-MS/MS (QqQ) method for the quantification of hepcidin-25, a promising new biomarker in iron metabolism, in human samples. The novelty of the method is the use of special HPLC vials to avoid adsorptive losses due to the basic character of the peptide that causes interaction with the silanol groups of the vial’s glass surface. Up to 90% decrease in the MS/MS signal was observed, when commercial HPLC vials were used, while vials treated with 3-(2-aminoethylamino)propylmethyldimethoxysilane or 1H,1H,2H,2H-perfluorooctyltriethoxysilane, leading to no losses in the range of physiological hepcidin-25 mean serum levels (10-20 µg/L). T2 - MSACL 2017 EU CY - Salzburg, Austria DA - 10.09.2017 KW - Peptide losses KW - Adsorption KW - Silanization PY - 2017 AN - OPUS4-44613 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abbas, Ioana M. T1 - Analytical strategies for the clinical assessment of the peptide hepcidin-25, a potential diagnostic tool in iron related disorders N2 - Hepcidin-25 has attracted much attention ever since its discovery in 2001. It is widely recognized that this liver produced peptide hormone plays a major role in the regulation of iron levels in mammals and can reveal important clinical information about several pathological states in patients suffering from iron-related disorders. With the aim to tackle the current difficulties in hepcidin quantification and improve the status of this promising biomarker in the clinical field, we developed a rapid and robust analytical strategy for the quantification of hepcidin-25 in human samples based on HPLC-MS/MS (QqQ) to be implemented in routine laboratories. The novelty of the method is the use of special HPLC vials to avoid adsorptive losses due to the basic character of the peptide that causes interaction with the silanol groups of the vial’s glass surface. Up to 90% decrease in the MS/MS signal was observed, when commercial HPLC vials were used, while vials treated with 3-(2-aminoethylamino)propylmethyl-dimethoxysilane or 1H,1H,2H,2H-perfluorooctyltriethoxysilane, leading to no significant losses in the dynamic range of physiological hepcidin-25 mean serum levels (10-20 µg/L). Careful analytical validation was performed for determining the reproducibility, repeatability, limit of quantification (0.5 µg/L) and linearity (0.5-40 µg/L) of the method. Serum samples from 9 healthy volunteers were analyzed with a median hepcidin-25 level of 3.3 µg/L, comparable to results reported in the literature. T2 - Australian Peptide Conference 2017 CY - Noosa Heads, Australia DA - 15.10.2017 KW - Validation KW - Hepcidin-25 KW - LC-MS/MS quantification PY - 2017 AN - OPUS4-44614 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernevic, Bogdan A1 - El-Khatib, Ahmed H. A1 - Jakubowski, Norbert A1 - Weller, Michael G. T1 - Online immunocapture ICP‑MS for the determination of the metalloprotein ceruloplasmin in human serum N2 - The human copper-protein ceruloplasmin (Cp) is the major copper-containing protein in the human body. The accurate determination of Cp is mandatory for the reliable diagnosis of several diseases. However, the analysis of Cp has proven to be difficult. The aim of our work was a proof of concept for the determination of a metalloprotein-based on online immunocapture ICP-MS. The immuno-affinity step is responsible for the enrichment and isolation of the analyte from serum, whereas the compound-independent quantitation with ICP-MS delivers the sensitivity, precision, and large dynamic range. Off-line ELISA (enzyme-linked immunosorbent assay) was used in parallel to confirm the elution profile of the analyte with a structure-selective method. The total protein elution was observed with the 32S mass trace. The ICP-MS signals were normalized on a 59Co signal. The human copper-protein Cp could be selectively determined. This was shown with pure Cp and with a sample of human serum. The good correlation with off-line ELISA shows that Cp could be captured and eluted selectively from the anti-Cp affinity column and subsequently determined by the copper signal of ICP-MS. KW - ELISA KW - Affinity chromatography KW - Affinity extraction KW - IgY KW - Chicken antibodies KW - Immunoaffinity extraction KW - Copper KW - Diagnostics PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-446157 UR - https://bmcresnotes.biomedcentral.com/articles/10.1186/s13104-018-3324-7 UR - https://static-content.springer.com/esm/art%3A10.1186%2Fs13104-018-3324-7/MediaObjects/13104_2018_3324_MOESM1_ESM.pdf UR - https://static-content.springer.com/esm/art%3A10.1186%2Fs13104-018-3324-7/MediaObjects/13104_2018_3324_MOESM2_ESM.pdf DO - https://doi.org/10.1186/s13104-018-3324-7 SN - 1756-0500 VL - 11 IS - 1 SP - Article 213, 1 EP - 5 PB - Springer Nature CY - Heidelberg AN - OPUS4-44615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abbas, Ioana M. T1 - An LC-MS/MS based reference method candidate for the clinical assessment of the promising iron biomarker hepcidin-25 in serum N2 - Hepcidin-25 has attracted much attention ever since its discovery in 2001. It is widely recognized that this peptide hormone plays a major role in the regulation of iron levels in mammals and can reveal important clinical information about several iron-related disorders. However, the development of a reliable assay to quantify hepcidin proved to be problematic and serum hepcidin-25 concentrations determined by various assays differ substantially. Challenges arise in the MS analysis of hepcidin due to the “sticky” character of the peptide and the lack of suitable standards. With the aim to tackle the current difficulties in hepcidin quantification and improve the status of this promising biomarker in the clinical field, we developed a rapid and robust analytical strategy for the quantification of hepcidin-25 in human samples based on HPLC-MS/MS (QqQ) as a reference method candidate to be implemented in routine laboratories. The novelty of the method is the use of amino- and fluoro-silanized autosampler vials to reduce hepcidin interaction to laboratory glassware surfaces. Furthermore, we have investigated two sample preparation strategies and two chromatographic separation conditions where the use of acidic mobile phases was compared with a novel approach involving solvents at high pH containing 0.1% of ammonia. Both methods were carefully validated and applied to clinical samples in an intra-laboratory comparison of two LC-MS/MS methods using the same hepcidin-25 calibrators with very good correlation of the results. T2 - European Mass Spectrometry Conference 2018 CY - Saarbrücken, Germany DA - 11.03.2018 KW - Validation KW - LC-MS/MS peptide quantification KW - Clinical samples PY - 2018 AN - OPUS4-44616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Broadband dielectric spectroscopy to study soft matter systems N2 - The basics of broadband dielectric spectroscopy were introduced in detail. The analysis of the data was discussed. As application of broadband dielectric spectroscopy the alpha-relaxation (dynamic glass transition) and the chain dynamics of polymers were ilustrated. Further the application of dielectric spectroscopy to polymerbased nanocomposites and high preformance polymers was discussed in detail. T2 - Kolloquiumsvotrag am Karlsruher Instiut of Technology CY - Karlsruhe, Germany DA - 05.12.2018 KW - Broadband dielectric spectroscopy PY - 2018 AN - OPUS4-46910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler T1 - Röntgencomputertomographie für betonspezifische Anwendungen: Verwendung von In-situ und Ex-situ Prüfverfahren, um wesentliche Einblicke in das Betonverhalten zu gewinnen N2 - Beton ist das meistbenutzte Baumaterial der Welt. Sein Herstellungsprozess ist auch für schätzungsweise 5% der globalen Kohlenstoffemissionen verantwortlich. Daher können selbst kleine Verbesserungen in der Festigkeit oder Haltbarkeit zu einer erheblichen Verringerung der Bau- und Wartungskosten, der Umweltschäden und der Gefahr für die Menschen führen. Um das grundlegende Verhalten dieses Materials zu verstehen, ist es notwendig, seine Leistung während thermischer, chemischer und mechanischer Prozesse (d. h. in-situ) zu beobachten. Es wird eine zerstörungsfreie Messmethode benötigt, die in der Lage ist, nicht nur Änderungen des Materials wie Feuchtigkeitsumverteilung, Korrosion und Dehnung zu messen, sondern auch die innere Struktur des Materials im Dreidimensionalen aufzulösen, so dass Versagensmechanismen und Transportphänomene direkt auf bestimmte Eigenschaften der heterogenen Materialstruktur bezogen werden können (wie z.B. die Übergangszone zwischen Gesteinskörnungen und Zementstein oder die Orientierung von eingebetteten Fasern). Die Röntgencomputertomographie (CT) hat sich als ideal für solche Zwecke erwiesen. Neuere Forschungen an der BAM werden vorgetragen, die die Fähigkeiten der CT zur Identifizierung quantitativer Materialeigenschaften wie Faserorientierung, Rissoberfläche, Korrosionsverteilung und Änderungen des volumetrischen Feuchtigkeitsanteils demonstrieren. Der Nutzen dieser leistungsstarken Analysewerkzeuge wird dann anhand der Ergebnisse einer Reihe von Ex-situ und In-situ Testprogrammen für Bedingungen wie mechanische Belastung, Wassertransport und thermische Exposition gezeigt. Speziell entwickelte In-situ Testmaschinen für diese verschiedenen Testprogramme werden ebenfalls beschrieben. Die von der CT gelieferten quantitativen Charakterisierungsinformationen haben sich als ideale Grundlage für die Kalibrierung bzw. Validierung von numerischen Simulationen erwiesen. CT ist auch wesentlich für die Beantwortung von vielen anwendungsspezifischen Fragen, u.a. wie sich verschiedene Gießverfahren auf die Materialleistung auswirken, welche Mineralien sich als Zuschlagstoffe anfällig für langfristige chemische und hydraulische Prozesse erweisen und wie Polymerfasern den Druckaufbau in Beton während der thermischen Belastung beeinflussen. T2 - Abteilungsseminar 8. Zerstörungsfreie Prüfung CY - Berlin, Germany DA - 12.11.2018 KW - Feuchtigkeitsmessung KW - Röntgencomputertomographie (CT) KW - In-situ Prüfverfahren KW - Faserverstärkter Beton (FRC) KW - Digitale Bildkorrelation (DVC) PY - 2018 AN - OPUS4-46912 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Tumanov, N. A1 - Tumanova, N. A1 - Fischer, Franziska A1 - Morelle, F. A1 - Ban, V. A1 - Robeyns, K. A1 - Filinchuk, Y. A1 - Wouters, J. A1 - Leyssens, T. T1 - Exploring polymorphism and stoichiometric diversity in naproxen/proline cocrystals N2 - We present naproxen/proline cocrystals discovered when combining enantiopure and racemic naproxen and proline. Using liquid-assisted grinding as the main method to explore the variety of crystal forms in this system, we found 17 cocrystals, of which the structures of only four of them were previously known. The naproxen/proline system exhibited multiple polymorphs of 1 : 1 stoichiometry as well as more rare cocrystals with 1 : 2 and 2 : 3 stoichiometries, two cocrystal hydrates and one cocrystal solvate. In situ ballmilling, used to monitor liquid-assisted grinding reactions, revealed that the solvent dictates the reaction intermediates even if the final reaction product stays the same. Synchrotron X-ray diffraction data collected in situ upon heating allowed us to monitor directly the phase changes upon heating and gave access to pure diffraction patterns of several cocrystals, thus enabling their structure determination from powder X-ray diffraction data; this method also confirmed the formation of a conglomerate in the RS-naproxen/DL-proline system. Proline in cocrystals kept its ability to form charge-assisted head-to-tail N-H⋯O hydrogen bonds, typical of pure crystalline amino acids, thus increasing the percentage of strong chargeassisted interactions in the structure and consequently providing some of the cocrystals with higher melting points as compared to pure naproxen. The majority of drugs are chiral, and hence, these data are of importance to the pharmaceutical industry as they provide insight into the challenges of chiral cocrystallization. KW - In situ KW - Mechanochemistry KW - XRD PY - 2018 UR - https://pubs.rsc.org/en/Content/ArticleLanding/CE/2018/C8CE01338A#!divAbstract DO - https://doi.org/10.1039/c8ce01338a SN - 1466-8033 VL - 20 IS - 45 SP - 7308 EP - 7321 PB - Royal Society of Chemistry CY - London AN - OPUS4-46913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hinrichs, R. A1 - Zen Vasconcellos, M.A. A1 - Österle, Werner A1 - Prietzel, C. T1 - Amorphization of graphite flakes in gray cast iron under tribological load N2 - A gray cast iron disc, which had been submitted to a heavy duty automotive brake test, was examined with energy filtered transmission electron microscopy. A graphite flake in a convenient angular position showed the shear interaction of graphite layers with the iron matrix in nano-scale resolution. Atomic layers of graphite were wedged into the ferritic bulk, allowing the entrance of oxygen and the subsequent formation of magnetite. The exfoliated few-layer graphene batches deformed heavily when forced into the matrix. When Raman spectra from the disc surface, which show distinctive carbonaceous bands, were compared with Raman spectra from graphite subjected to deformation in a shaker mill with different milling times, it could be seen that the shear stress on the brake surface was much more effective to induce disorder than the milling, where compressive and impact forces had been additionally exerted on the sample. During shear load the high anisotropy of elastic modulus in the graphite crystalline structure and the low adhesion between graphite basal planes allowed the exfoliation of wrinkled few-layer grapheme batches, causing the formation of more defect related Raman bands than the mechanical stress during high-energy milling. KW - Graphite KW - Shear load KW - Amorphization KW - EFTEM KW - Raman spectroscopy PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-469227 DO - https://doi.org/10.1590/1980-5373-MR-2017-1000 SN - 1516-1439 SN - 1980-5373 VL - 21 IS - 4 SP - e20171000, 1 EP - 6 PB - Universidade Federal de São Carlos CY - São Carlos AN - OPUS4-46922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simoes, R. A1 - Bernades, C. A1 - Joseph, A. A1 - Piedade, F. A1 - Kraus, Werner A1 - Emmerling, Franziska A1 - Diogo, H. A1 - da Piedade, M. T1 - Polymorphism in simvastatin: Twinning, disorder, and enantiotropic phase transitions N2 - : Simvastatin is one of the most widely used active pharmaceutical ingredients for the treatment of hyperlipidemias. Because the compound is employed as a solid in drug formulations, particular attention should be given to the characterization of different polymorphs, their stability domains, and the nature of the phase transitions that relate them. In this work, the phase transitions delimiting the stability domains of three previously reported simvastatin forms were investigated from structural, energetics, and dynamical points of view based on single crystal X-ray diffraction (SCXRD), hot stage microscopy (HSM), and differential scanning calorimetry (DSC) experiments (conventional scans and heat capacity measurements), complemented with molecular dynamics (MD) simulations. Previous assignments of the crystal forms were confirmed by SCXRD: forms I and II were found to be orthorhombic (P212121, Z′/Z = 1/4) and form III was monoclinic (P21, Z′/Z = 2/4). The obtained results further indicated that (i) the transitions between different forms are observed at 235.9 ± 0.1 K (form III → form II) and at 275.2 ± 0.2 K (form II → form I) in DSC runs carried out at 10 K min−1 and close to these values when other types of techniques are used (e.g., HSM). (ii) They are enantiotropic (i.e., there is a transition temperature relating the two phases before fusion at which the stability order is reversed), fast, reversible, with very little hysteresis between heating and cooling modes, and occur under single crystal to single crystal conditions. (iii) A nucleation and growth mechanism seems to be followed since HSM experiments on single crystals evidenced the propagation of an interface, accompanied by a change of birefringence and crystal contraction or expansion (more subtle in the case of form III → form II), when the phase transitions are triggered. (iv) Consistent with the reversible and small hysteresis nature of the phase transitions, the SCXRD results indicated that the molecular packing is very similar in all forms and the main structural differences are associated with conformational changes of the “ester tail”. (v) The MD simulations further suggested that the tail is essentially “frozen” in two conformations below the III → II transition temperature, becomes progressively less hindered throughout the stability domain of form II, and acquires a large conformational freedom above the II → I transition. Finally, the fact that these transitions were found to be fast and reversible suggests that polymorphism is unlikely to be a problem for pharmaceutical formulations employing crystalline simvastatin because, if present, the III and II forms will readily convert to form I at ambient temperature. KW - Polymorphism KW - Twinning KW - Disorder KW - Simvastatine PY - 2018 DO - https://doi.org/10.1021/acs.molpharmaceut.8b00818 SN - 1543-8384 SN - 1543-8392 VL - 15 IS - 11 SP - 5349 EP - 5360 PB - American Chemical Society CY - Washington, DC AN - OPUS4-46927 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Improved algorithm for calibration-free laser induced breakdown spectroscopy N2 - An improved algorithm for calibration-free laser induced breakdown spectroscopy (CF LIBS) will be presented which includes several novel features in comparison with previously proposed similar algorithms. In particular, it allows using spectral lines with arbitrary optical thickness for the construction of Saha-Boltzmann plots, retrieves the absorption path length (plasma diameter) directly from a spectrum, replaces the Lorentzian line profile function by the Voigt function, and allows for self-absorption correction using pre-calculated and tabulated data rather than approximating functions. The tabulated data embody the solutions of the radiative transfer equation for numerous combinations of optical thicknesses and line widths. The algorithm is thoroughly verified using synthetic spectra. T2 - LIBS 2018 at SciX 2018 CY - Atlanta, GA, USA DA - 21.10.2018 KW - Plasma diagnostics KW - Laser induced plasma KW - LIBS KW - Plasma modeling PY - 2018 AN - OPUS4-46930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramos, I. I. T1 - Lab-on-valve platform for real-time automated immunosensing N2 - The talk presents results of collaborative work on implementing antibody-based, immunoanalytical methods on a lab-on-valve platform. T2 - Biosensors 2018 CY - Miami, FL, USA DA - 12.07.2018 KW - Antikörper KW - Immunoassay KW - Automation PY - 2018 AN - OPUS4-47049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schenderlein, Matthias T1 - Monitoring early stage corrosion processes during biofilm formation N2 - To investigate early stage corrosion processes of stainless steel 1.4301 taking place during the biofilm formation of the organism Shewanella putrefaciens electrochemical impedance spectroscopy (EIS) in a multielectrode approach has been used. The multielectrode array consisted of up to 25 electrically isolated electrodes made of stainless steel wires of diameters ranging from 100 µm to 500 µm. They were connected to a multichannel microelectrode analyzer (MMA) electrically coupled through zero resistance ammeters. Current flow between electrodes in the array as well as changes in impedance of individual electrodes over time were recorded and analyzed with respect to the onset of localized corrosion and biofilm formation. The results were complemented by optical microscopy, SEM and AFM images which were taken immediately after the respective experiment. To verify that the multielectrode arrays correctly indicated the initial stages of the corrosion process and of biofilm formation they were introduced in a flow cell reaction vessel containing test specimens made from stainless steel 1.4301, which were checked regularly for signs of localized corrosion and biofilms. Preceding results with the multielectrode array in solutions containing high amounts of chloride ions and hydrogen peroxide at low pH also showed that it is possible with the MMA to monitor individual electrodes becoming local anodes as local corrosion set in, while the remaining electrodes predominantly acted as cathodes. T2 - 69th Annual Meeting of the International Society of Electrochemistry CY - Bologna, Italy DA - 02.09.2018 KW - Corrosion KW - Multielectrode KW - Biofilm KW - Monitoring KW - Stainless steel PY - 2018 AN - OPUS4-47095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hüllmann, Dino A1 - Paul, Niels A1 - Kohlhoff, Harald A1 - Neumann, Patrick P. A1 - Lilienthal, A. J. ED - Eberhardsteiner, J. ED - Růžička, M. ED - Cosmi, F. T1 - Measuring rotor speed for wind vector estimation on multirotor aircraft N2 - For several applications involving multirotor aircraft, it is crucial to know both the direction and speed of the ambient wind. In this paper, an approach to wind vector estimation based on an equilibrium of the principal forces acting on the aircraft is shown. As the thrust force generated by the rotors depends on their rotational speed, a sensor to measure this quantity is required. Two concepts for such a sensor are presented: One is based on tapping the signal carrying the speed setpoint for the motor controllers, the other one uses phototransistors placed underneath the rotor blades. While some complications were encountered with the first approach, the second yields accurate measurement data. This is shown by an experiment comparing the proposed speed sensor to a commercial non-contact tachometer. T2 - 34th Danubia Adria Symposium on Advances in Experimental Mechanics CY - Trieste, Italy DA - 19.09.2017 KW - Wind vector estimation KW - Rotor speed KW - UAV KW - Tachometer PY - 2018 UR - https://www.sciencedirect.com/science/article/pii/S2214785318321114 DO - https://doi.org/10.1016/j.matpr.2018.08.139 SN - 2214-7853 VL - 5 IS - 13 SP - 26703 EP - 26708 PB - Elsevier CY - Amsterdam, Netherlands AN - OPUS4-47097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gulikers, J. A1 - Millar, Steven A1 - Wilsch, Gerd T1 - Practical application of Laser Induced Breakdown Spectroscopy for determinafion of the chioride content in concrete structures N2 - This paper will address the relevance of chloride measurements in practice for durability condition assessment and a description of the working principle of LIBS will be given. Examples of chloride profiles obtained by the common wet chemical analysis will be shown and compared with results from LIBS measurements as to demonstrate the accuracy of the LIBS-technique. The latter will be supported by clear graphs. In addition examples on the extra information resulting from measurements performed with LIBS for improvement of condition assessment and prediction will be shown. T2 - CONFERENCE IN HONOR OF Centennial of LABORATORY OF CONSTRUCTION MATERIALS CY - Lausanne, Switzerland DA - 19.08.2018 KW - LIBS KW - Concrete KW - Chloride KW - Condition assesment PY - 2018 SP - 80 EP - 83 CY - Lausanne AN - OPUS4-47108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gulikers, J. T1 - Practical application of Laser Induced Breakdown Spectroscopy for determination of the chloride content in concrete structures N2 - The relevance of chloride measurements in practice for durability condition assessment and a description of the working principle of LIBS will be given. A comparison of chloride profiles obtained by the common wet chemical analysis and results from LIBS measurements are shown to demonstrate the accuracy of the LIBS-technique. In addition, an example on the extra information resulting from measurements performed with LIBS for improvement of condition assessment and prediction will be shown. T2 - Conference celebrating the Laboratory of Construction Materials (EPFL) Centennial CY - Lausanne, Switzerland DA - 19.08.2018 KW - LIBS KW - Concrete KW - Chlorride KW - Condition assesment PY - 2018 AN - OPUS4-47109 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Alternative Möglichkeiten zur Bestimmung der Chlorid-Migration in Parkhausbauten (LIBS) N2 - Vorstellung von LIBS. Demonstration der Möglichkeiten zur Untersuchung des Chlorid-Gehaltes im Beton in Parkbauten. Darstellung von Praxisbeispielen zur Bestimmung des Zustandes eines Parkhauses. T2 - Fachtagung "Parkhäuser und Tiefgaragen" CY - Hamburg, Germany DA - 27.11.2018 KW - LIBS KW - Beton KW - Chlorid KW - Parkbauten KW - Qualitätssicherung PY - 2018 AN - OPUS4-47114 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Transformation of the antidiabetic drug metformin N2 - For years there have been more and more reports on the presence of drugs in the aquatic environment. Due to the demographic change, the consumption of pharmaceuticals has risen sharply. After taking the drugs, they are partly metabolized in the human body. However, the metabolism is not complete so that both the metabolites and non-metabolized amounts of the parent compounds are excreted. These compounds reach the waste water and afterwards the sewage treatment plants. In sewage treatment plants transformation products can be formed by the oxidative conditions during wastewater treatment processes. The transformation products may have a higher toxicity than the actual environmental pollutants and are often only partly removed during the waste water treatment. Since a lot of these compounds are still unknown, the transformation products are not detected by target analysis used in sewage treatment plants and are often released undetected in the aquatic ecosystems. The released substances may be subject to additional transformation processes in the environment. Pharmaceuticals produced in high amounts can be already detected in the μg/L range in water bodies worldwide. Metformin and its major transformation product guanylurea are one of the main representatives. Metformin is the drug of choice for treating type 2 diabetes. The drug therapy for diabetes mellitus has increased significantly in recent years. In the year 2015 1500 tons of metformin were prescribed in Germany (for statutory insured persons). Metformin is not metabolized in the human body and is excreted unchanged therefore concentrations between 57 μg/L and 129 μg/L are found in German waste water treatment plants influents. In this work the transformation of the antidiabetic drug metformin is investigated. The degradation of metformin is initialize by commercial water treatment techniques like UV-radiation or noncommercial techniques like heterogenous photocatalysis based on titanium dioxide. The degradation of metformin and resulting transformation products are analyzed by LC-MS/MS and LC-HRMS. T2 - SPEA 10 CY - Almeria, Spain DA - 04.06.2018 KW - Metformin KW - Photocatalysis PY - 2018 AN - OPUS4-47030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul T1 - Einfluss der Schweißnaht-Nachbehandlung auf die Korrosionsbeständigkeit des Duplex-Stahls 1.4062 N2 - Die Korrosionsbeständigkeit von Schweißverbindungen aus dem Duplex-Stahl 1.4062 wird, neben dem Grundwerkstoff, dem Schweißzusatzwerkstoff und dem Schweißverfahren, auch sehr stark von der Oberflächennachbehandlung der Schweißnaht beeinflusst. Je nach zukünftigem Anwendungsbereich und geforderter Korrosionsbeständigkeit wird die Schweißnaht geschliffen, gebeizt, elektropoliert oder gestrahlt, um die beim Schweißen entstandenen Anlauffarben zu entfernen. Gestrahlte Oberfläche sind in der industriellen Praxis häufig anzutreffen, da sie deutlich einfacher und kostengünstiger herzustellen sind als gebeizte oder elektropolierte Oberflächen. Die Auswahl des Strahlmittels bestimmt auch die Prozesskosten, wobei das Strahlen mit Korund effektiver als das Strahlen mit Glasperlen ist. Ziel der Untersuchungen war es festzustellen, ob das Strahlen aus Sicht der Korrosionsbeständigkeit äquivalent zu anderen Nachbehandlungsverfahren ist. Diese Fragestellung wird im Vortrag beantwortet indem geschliffene, gebeizte, mit Korund gestrahlte und mit Glasperlen gestrahlte Schweißverbindungen vergleichend untersucht werden. Die Ergebnisse der Untersuchungen von den Strahlmitteln und den gestrahlten Oberflächen werden mit den Ergebnissen der Salzsprühnebelprüfung, den kritischen Lochkorrosionspotentialen und der KorroPad-Prüfung korreliert. T2 - Sitzung des Arbeitskreises "Korrosion und Korrosionsschutz von Eisen und Stahl" der Gesellschaft für Korrosionsschutz e.V. CY - Duisburg, Germany DA - 12.12.2018 KW - Korrosion KW - Korosionsschutz KW - Duplexstahl KW - KorroPad KW - Nichtrostender Stahl KW - Lochkorrosion KW - Schweißen KW - Oberflächen KW - Strahlen PY - 2018 AN - OPUS4-47036 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Temperaturindikatoren in mittelalterlichen Hochbrandgipsen: Eine Ramanmikrospektroskopische Studie N2 - Infolge der beschränkten Kontrollmöglichkeiten über die in einem Meiler oder Feldofen herrschenden Parameter konstituiert mittelalterliche Hochbrandgipse ein Gemisch aus verschiedenen Anhydritstufen. Basierend auf modernen Versuchsbränden dienen in der gealterten Gipsmatrix nicht oder nur teilweise hydratisiert erhaltene Brenngutkörner üblicherweise anhand der morphologischen Eigenschaften der Anhydritkristalle der groben Einschätzung der zumindest lokal im Ofen bzw. im stückigen Brenngut erreichten Temperaturwerte. Die bildgebende Ramanmikroskopie ermöglicht die kornspezifische Bestimmung der Hitzeeinwirkung über den Grad der sich im Ramanspektrum abbildenden thermischen Beeinträchtigung der Thermoanhydritphasen, als auch deren Unterscheidung von primärem Anhydrit aus der Gipslagerstätte, da diesen eine höhere Kristallinität kennzeichnet. Hier beispielhaft diskutierte Ramananalysen an zwei reliktischen Brenngutkörnern lassen auf Brenntemperaturen von 650°C bzw. 800°C schließen. Pyrometamorphe Phasenneubildungen der natürlichen Verunreinigungen des Rohgipses liefern aufgrund ihres Bildungs- und Stabilitätsbereiches zusätzliche Hinweise. Im Beitrag erörtert werden die an die Dehydratation von magnesiumreichem Chlorit korrelierte Genese von Forsterit sowie die Zersetzung von Dolomit zu Calcit und Periklas, welcher beim Anmachen des Mörtels zu Brucit gelöscht wird und im Laufe der Zeit in der Gipsmatrix zu Magnesit carbonatisiert; beide pyrometamorphen Reaktionen erfordern Temperaturen von über 800°C. KW - Ramanmikrospektroskopie KW - Mineralthermometer KW - Gips PY - 2018 SN - 0931-7198 VL - 32 IS - 1 SP - 69 EP - 78 PB - Wernersche Verlagsgesellschaft mbH CY - Worms AN - OPUS4-47041 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bosc-Bierne, Gaby T1 - Development of an HPLC-HRMS method for quality control of peptide pools N2 - Synthetic peptide pools are used in antigen-specific T-cell assays, which are an important part in vaccine and immunotherapeutic clinical trials. As the analytical characterization is challenging due to the similarity of the single peptides or is expensive due to isotope labeled standards, usually only a pre-characterization of the single peptides is performed. However, a regular quality control of the peptide mix would be highly desirable. Therefore, a cost-efficient high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) method for quality control of a model peptide pool is developed. Peptides were synthesized using peptides&elephants proprietary libraries of individual peptides (LIPS) technology and purified by reversed-phase chromatography to > 90% each. The lyophilized single peptides were combined to a model peptide pool and analyzed by reversed-phase high-performance capillary liquid chromatography coupled to an orbitrap mass spectrometer. Separation was performed on a capillary reversed phase column (2 μm, ID x L 300 μm x 150 mm) with a linear gradient of acetonitrile + 0,05% trifluoroacetic acid. For the separation of a model peptide pool the additive, additive concentration, the gradient elution and the temperature were optimized. Different quantification approaches were tested. Identification was performed by high resolution mass spectrometry in which extracted ion chromatograms (XIC) were used to confirm exact masses. In line with the development of a new cost-efficient quality control method for the separation and identification of complex synthetic peptide pools, varied HPLC parameters highlighted their influence on chromatographic resolution and peptides were identified with high mass accuracy. T2 - 8th Austrian Peptide Symposium CY - Salzburg, Austria DA - 13.12.2018 KW - LC-MS KW - Peptide pools KW - Quality control PY - 2018 AN - OPUS4-47058 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Millar, Steven A1 - Kruschwitz, Sabine A1 - Wilsch, Gerd T1 - Determination of total chloride content in cement pastes with laser-induced breakdown spectroscopy (LIBS) N2 - The presented work discusses the accuracy of Laser Induced Breakdown Spectroscopy (LIBS) in determining the total chloride content in cement pastes. LIBS as an emission spectroscopy method is used to detect simultaneously several elements present in cement-based materials. By scanning surfaces the variability in the spatial distribution of elements can be visualised. However, for a quantification of the results, studies are necessary to characterise possible influences due to the wide variation of the chemical compositions in which cement can occur. It is shown how the calibration can be done, how the calibration samples were produced, and which statistical parameters are necessary to describe the precision of the regression. The performance of LIBS is estimated by detecting chloride in validation samples. Therefore, 55 samples and 7 ets with changing mix ompositions were produced. The presented study deals with possible influences of different mix compositions, ncluding different cations of chloride, varying w/c-ratios and the artial replacement of Portland cement with last furnace slag (50% BFS) and limestone (30% LS). Comparing the LIBS results with otentiometric titration, n accuracy of±0.05 wt%/total has been determined. KW - Spectroscopy KW - LIBS KW - Chloride KW - Quantification KW - Cement PY - 2019 DO - https://doi.org/10.1016/j.cemconres.2018.12.001 SN - 0008-8846 VL - 117 IS - March SP - 16 EP - 22 PB - Elsevier CY - Amsterdam AN - OPUS4-47059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dzierliński, M. A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias ED - Zagrobelny, Maciej ED - Suś-Ryszkowska, Małgorzata T1 - Wykrywanie wycieków gazu za pomocą bezzałogowych pojazdów powietrznych T1 - Detection of gas leaks by unmanned aerial vehicles N2 - Wyciek metanu (CH4) z infrastruktury takiej jak rurociągi czy zbiorniki magazynowe ma kluczowe znaczenie dla środowiska oraz stwarza zagrożenie dla bezpieczeństwa ludzi i mienia. Obecnie, po okresie bezawaryjnej eksploatacji, można zaobserwować wzrost liczby incydentów spowodowanych nieszczelnościami rurociągów przesyłowych. W Polsce szczególnie problematyczne okazują się gazociągi, które powstały dekady temu. W tamtym czasie normy techniczne i przepisy budowlane były łagodniejsze niż obecnie obowiązujące. Integralność tych gazociągów jest trudna do skontrolowania, gdyż na etapie budowy nie zostały one przystosowane do badania tłokami pomiarowymi. Aby sprostać temu wyzwaniu, UDT poszukuje metod umożliwiających szybkie i niezawodne wykrywanie oraz lokalizowanie nieszczelności gazociągów na duże odległości. N2 - Methane leakage (CH4) from infrastructure such as pipelines or storage tanks is crucial for the environment and poses a threat to the safety of people and property. Today, after a period of failure-free operation, an increase in the number of incidents caused by leaks in transmission pipelines can be observed. In Poland, gas pipelines created decades ago turn out to be particularly problematic. At that time, technical standards and building regulations were milder than those currently in force. The integrity of these pipelines is difficult to control, as they were not adapted for testing with measuring pigs at the construction stage. To meet this challenge, UDT is looking for methods to quickly and reliably detect and locate leaks in pipelines over long distances. KW - Aerial robot KW - Mobile robot olfaction KW - Tomographic reconstruction of gas plumes KW - Tunable diode laser absorption Spectroscopy (TDLAS) KW - UAV-REGAS PY - 2018 UR - https://www.udt.gov.pl/inspektor-on-line VL - 4 SP - 19 EP - 21 PB - Urząd Dozoru Technicznego CY - Warszawa, Polska AN - OPUS4-47062 LA - pol AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wasmer, Paul A1 - Krome, Fabian A1 - Bulling, Jannis A1 - Prager, Jens T1 - A fluid model for the simulation of fluid‐structure interaction in the Scaled Boundary Finite Element Method for prismatic structures N2 - The Scaled Boundary Finite Element Method is known as an efficient method for the simulation of ultrasonic wave propagation. As to investigate acoustic wave behavior in case of fluid‐structure interaction, a fluid model is implemented in the SBFEM for prismatic structures. To omit coupling terms a displacement‐based formulation is used. Spurious modes, which occur in the solution, are suppressed using a penalty parameter. To verify this formulation dispersion curves obtained with Comsol Multiphysics are compared to results of SBFEM. The results of both methods are in very good agreement T2 - GAMM 2018 CY - Munich, Germany DA - 19.03.2018 KW - Scaled Boundary Finite Element Method KW - Penalty Parameter KW - Fluid-Structure Interaction KW - Guided Waves PY - 2018 DO - https://doi.org/10.1002/pamm.201800139 VL - 18 IS - 1 SP - e201800139 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-47063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hein, Sebastian T1 - Qualitätsmanagement im Wissenschaftsbereich N2 - Die Empfehlungen der Deutschen Forschungsgemeinschaft (DFG) zur Sicherung guter wissenschaftlicher Praxis werden dargestellt und mit Maßnahmen der Qualitätssicherung ergänzt. T2 - Herbstschule 2018 Qualitätssicherung in der analytischen Chemie CY - Berlin, Germany DA - 29.10.2018 KW - Gute wissenschaftliche Praxis KW - Qualitätsmanagement PY - 2018 AN - OPUS4-47065 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kok, H. T. T1 - 2D nanomaterials with switchable pathogen binding N2 - Graphene and its derivatives have recently attracted much attention for sensing and deactivating pathogens. However, mechanism of multivalent interactions at the graphene-pathogen interface are not fully understood. Since different physicochemical parameters of graphene play a role at this interface, control over graphene’s structure is necessary to study the mechanism of these interactions. In this work, zwitterionic graphene nanomaterials (ZGNMs) were synthesized with defined isoelectric points and exposure, in terms of polymer coverage and functionality. Then, the switchable interactions of ZGNMs with E. coli were investigated to study the validity of the generally proposed “trapping” mechanism for inactivating pathogens by functionalized graphene derivatives. The ZGNMs were able to controllably trap and release E. coli by crossing their isoelectric points. T2 - 4th Erlangen Symposium on Synthetic Carbon Allortopes 2017 CY - Erlangen, Germany DA - 25.09.2017 KW - Graphene KW - XPS KW - NEXAFS KW - Zwitterionic graphene nanomaterials PY - 2017 AN - OPUS4-47084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Donskyi, Ievgen T1 - Inhibition of Herpes Virus by Specific and Non-specific Interactions With Graphene Conjugates N2 - Herpes viruses (HSV) are global, host-adapted pathogens that cause a widespread diversity of diseases. The frequency of HSV infections all over the world has amplified over the last years, making it a major concern in the area of public health. Therefore, synthesis of systems that can inhibit development of these viruses is required. Various compounds already have shown inhibition of HSV, but concentration of these inhibitors is relatively high and resistance against those drugs is challenging. Combination of biological knowledge, about structure of the active site on the surface of HSV that is responsible for inhibition of the pathogen, with the chemistry of graphene results in 2D systems with the ability of specific and nonspecific interactions with HSV. In this work, 2D nanomaterials with picomolar IC50 against HSV are synthesized by conjugation of peptides to the surface of graphene. 2D nanomaterials are characterized by various methods, including XPS, AFM and IR. Biological evaluation showed high potency of synthesized nanomaterials to inhibit HSV and therefore underlined possibility to use such materials in future biomedical applications. T2 - Jubiläumskongress 150 Jahre GDCh Wissenschaftforum Chemie CY - Berlin, Germany DA - 12.09.2017 KW - Graphene KW - Graphene 2D nanomaterial KW - XPS KW - Inhibition of HSV virus PY - 2017 AN - OPUS4-47085 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Donskyi, Ievgen T1 - Gram-scale production of high quality nanographene under mild conditions and doping via non-destructive covalent functionalization N2 - We report a new method for top-down one-pot, gram-scale production of high-quality nanographene from graphite under mild conditions. The nanographene sheets had a very low oxygen content, comparable to that of nanographene grown by chemical vapor deposition. This method is easily scalable and comparatively mild, opening the door to an environmentally friendly process to produce high-quality nanographenes. Nanographene sheets were further covalently functionalized using a non-destructive [2+1] cycloaddition reaction that left the π-conjugated system intact. T2 - 10th Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 05.12.2018 KW - Nano graphene KW - X-ray Photoelectron Spectroscopy (XPS) KW - NEXAFS KW - Raman spectroscopy PY - 2018 AN - OPUS4-47086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trog, S. A1 - El-Khatib, Ahmed A1 - Beck, S. A1 - Makowski, M. A1 - Jakubowski, Norbert A1 - Linscheid, M. T1 - Complementarity of molecular and elemental mass spectrometric imaging of Gadovist™ in mouse tissues N2 - Drug biodistribution analyses can be considered a key issue in pharmaceutical discovery and development. Here, mass spectrometric imaging can be employed as a powerful tool to investigate distributions of drug compounds in biologically and medically relevant tissue sections. Both matrix-assisted laser desorption ionization–mass spectrometric imaging as molecular method and laser ablation inductively coupled plasma–mass spectrometric imaging as elemental detection method were applied to determine drug distributions in tissue thin sections. Several mouse organs including the heart, kidney, liver, and brain were analyzed with regard to distribution of Gadovist™, a gadolinium-based contrast agent already approved for clinical investigation. This work demonstrated the successful detection and localization of Gadovist™ in several organs. Furthermore, the results gave evidence that gadolinium-based contrast agents in general can be well analyzed by mass spectrometric imaging methods. In conclusion, the combined application of molecular and elemental mass spectrometry could complement each other and thus confirm analytical results or provide additional information. KW - Laser ablation inductively coupled plasma–mass spectrometry imaging (LA-ICP-MSI) KW - Gadolinium-based contrast agents (GBCAs) KW - Matrix-assisted laser desorption ionization–mass spectrometry imaging (MALDI-MSI) PY - 2019 DO - https://doi.org/10.1007/s00216-018-1477-9 SN - 1618-2642 SN - 1618-2650 VL - 411 IS - 3 SP - 629 EP - 637 PB - Springer AN - OPUS4-47371 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Neue Entwicklungen im Bereich der luftgekoppelten Ultraschallprüfung N2 - Es wird über Ferroelektret-Wandler, thermoakustische Wandler und Plasma-Wandler für luftgekoppelte Ultraschallprüfung berichtet. T2 - Sitzung des Arbeitskreises Berlin der DGZfP CY - Berlin, Germany DA - 12.02.2019 KW - Luftultraschall KW - Ferroelektret KW - Thermoakustik KW - Plasma PY - 2019 AN - OPUS4-47375 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Ultraschallprüfung in der BAM (Fachbereich 8.4 - Zerstörungsfreie Prüfung - Akustische und elektromagnetische Verfahren) N2 - Vorstellung des Fachbereichs 8.4 mit dem Schwerpunkt Ultraschallprüfung. T2 - Sitzung des DFG-Schwerpunktprogramms Zyklische Schädigungsprozesse in Hochleistungsbetonen im Experimental-Virtual-Lab2020 CY - Berlin, Germany DA - 6.2.2019 KW - Luftultraschall KW - Ultraschall KW - Phased Array KW - Simulation KW - Wirbelstrom KW - Magnetfeldsensoren PY - 2019 AN - OPUS4-47376 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, L. M. A1 - Diaz Cubas, D. A1 - Colmenares, M. G. A1 - Schmidt, J. A1 - Bekheet, M. F. A1 - Pauw, Brian Richard A1 - Gurlo, A. A1 - Simon, U. T1 - High specific surface area ordered mesoporous silica COK-12 with tailored pore size N2 - Ordered mesoporous silica materials such as COK-12, analogous to the well-known SBA-15, are characterized by high surface areas and unique features such as defined pore sizes in the meso-size range and high pore ordering. The aim of this work was to prove the washing step and choice of calcination and aging temperature during the COK-12 synthesis as effective tools in tailoring, markedly improving the specific surface area, pore size, and pore volume. By controlling the aging temperature, the pore size was linearly adjusted between 5.7 and 8.1 nm, while preserving the hexagonal ordering of the pores. The synthesized COK-12 powders possess pore volumes and specific surface areas up to 1.23 cm3 g−1 and 860m2 g−1, respectively, which is markedly higher than what has previously been reported about COK-12. The presented results and the environmentally friendly character of the synthesis will make COK-12 more interesting for future adaption to the industrial processes, for example in catalysis, adsorption, or drug delivery. KW - Ordered mesoporous silica KW - Pore size tailoring KW - High specific surface area KW - SAXS KW - Small angle scattering PY - 2019 DO - https://doi.org/10.1016/j.micromeso.2019.01.050 SN - 1387-1811 VL - 280 SP - 133 EP - 143 PB - Elsevier AN - OPUS4-47378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, R. A1 - Braun, Ulrike A1 - Fankhänel, J. A1 - Daum, B. A1 - Arash, B. A1 - Rolfes, R. T1 - Molecular modelling of epoxy resin crosslinking experimentally validated by near-infrared spectroscopy N2 - Reliable simulation of polymers on an atomistic length scale requires a realistic representation of the cured material. A molecular modelling method for the curing of epoxy systems is presented, which is developed with respect to efficiency while maintaining a well equilibrated system. The main criterion for bond formation is the distance between reactive groups and no specific reaction probability is prescribed. The molecular modelling is studied for three different mixing ratios with respect to the curing evolution of reactive Groups and the final curing stage. For the first time, the evolution of reactive groups during the curing process predicted by the molecular modelling is validated with near-infrared spectroscopy data, showing a good agreement between simulation results and experimental measurements. With the proposed method, deeper insights into the curing mechanism of epoxy systems can be gained and it allows us to provide reliable input data for molecular Dynamics simulations of material properties. KW - Epoxy KW - NIR spectroscopy KW - Modelling PY - 2019 DO - https://doi.org/10.1016/j.commatsci.2019.01.054 SN - 0927-0256 VL - 161 SP - 223 EP - 235 PB - Elsevier AN - OPUS4-47431 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klöckner, P. A1 - Reemtsma, T. A1 - Eisentraut, Paul A1 - Braun, Ulrike A1 - Ruhl, A. S. A1 - Wagner, S. T1 - Tire and road wear particles in road environment e Quantification and assessment of particle dynamics by Zn determination after density separation N2 - In this study, a method for the determination of tire and road wear particle (TRWP) contents in particulate samples from road Environment was developed. Zn was identified as the most suitable elemental marker for TRWP, due to its high concentration in tire tread and the possibility of separation from other Zn sources. The mean concentration of 21 tire samples was 8.7 ± 2.0 mg Zn/g. Before quantification in samples from road environment, TRWP were separated from the particulate matrix by density separation. Method development was conducted using shredded tread particles (TP) as a surrogate for TRWP. Recovery of TP from spiked sediment was 95 ± 17% in a concentration range of 2 - 200 mg TP/g. TP determination was not affected by other Zn containing solids or spiked Zn-salts. By adjusting the density of the separation solution to 1.9 g/cm3, more than 90% of total TRWP were separated from the sample matrix. TRWP concentrations in particulate matter collected in two road runoff treatment Systems ranged from 0.38 to 150 mg TRWP/g. Differences in quantified TRWP contents of the two Systems indicate changes in particle dynamics due to ageing and aggregation processes. The developed method allows TRWP determination in road runoff and in environments that are influenced by road traffic. The validated separation procedure can also be applied for TRWP characterization in future studies. KW - Zinc analysis KW - Microplastics KW - Tire particles PY - 2019 VL - 222 SP - 714 EP - 721 PB - Elsevier AN - OPUS4-47433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Domonov, D.P. A1 - Pechenyuk, S.I. A1 - Semushina, Y.P. A1 - Yusenko, Kirill T1 - Solid state transformation in inner coordination sphere of [Co(NH3)6][Fe(C2O4)3]·3H2O as a route to access catalytically active Co-Fe materials N2 - Thermal decomposition of [Co(NH₃)₆][Fe(C₂O₄)₃]∙3H₂O in argon atmosphere, at a low heating rate (3°/min), and in large amounts of the initial complex (~0.1 mole), has been studied. It was possible to distinguish four decomposition steps upon heating: In the temperature range of 50⁻100 °C-the loss of crystal water; 100⁻190 °C-stability region of dehydrated complex; 230⁻270 °C-the range of stability of intermediate phase with the formula CoFe(NH₃)₂(C₂O₄)₂; 270⁻350 °C-thermal decomposition of the intermediate with the formation of metallic products and further air oxidation with the formation of Co1.5Fe1.5O₄. Catalytic properties of thermolysis products were tested in the decomposition reaction of H₂O₂ (inactive), oxidation of acetone (average activity), and decomposition of ammonium perchlorate (highly active). KW - Double complex salts KW - Catalysts KW - Single-source precursors PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474014 DO - https://doi.org/10.3390/ma12020221 SN - 1996-1944 VL - 12 IS - 2 SP - 221, 1 EP - 10 PB - mdpi CY - Zürich AN - OPUS4-47401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baek, W. A1 - Gromilov, S. A1 - Kuklin, A. A1 - Kovaleva, E. A1 - Fedorov, A. A1 - Sukhikh, Alex A1 - Hanfland, M. A1 - Pomogaev, V. A1 - Melchakova, Y. A1 - Avramov, P. A1 - Yusenko, Kirill T1 - Unique Nanomechanical Properties of Diamond-Lonsdaleite Biphases: Combined Exp and Theor consideration of popigai impact diamonds N2 - For the first time, lonsdaleite-rich impact diamonds from one of the largest Popigai impact crater (Northern Siberia) with a high concentration of structural defects are investigated under hydrostatic compression up to 25 GPa. It is found that, depending on the nature of a sample, the bulk modulus for lonsdaleite experimentally obtained by X-ray diffraction in diamond-anvil cells is systematically lower and equal to 93.3−100.5% of the average values of the bulk moduli of a diamond matrix. Density functional theory calculations reveal possible coexistence of a number of diamond/lonsdaleite and twin diamond biphases. Among the different mutual configurations, separate inclusions of one lonsdaleite (001) plane per four diamond (111) demonstrate the lowest energy per carbon atom, suggesting a favorable formation of single-layer lonsdaleite (001) fragments inserted in the diamond matrix. Calculated formation energies and experimental diamond (311) and lonsdaleite (331) powder X-ray diffraction patterns indicate that all biphases could be formed under high-temperature, high-pressure conditions. Following the equation of states, the bulk modulus of the diamond (111)/lonsdaleite (001) biphase is the largest one among all bulk moduli, including pristine diamond and lonsdaleite. KW - Compressibility KW - Lonsdaleite KW - Impact diamonds PY - 2019 DO - https://doi.org/10.1021/acs.nanolett.8b04421 VL - 19 IS - 9 SP - 1570 EP - 1576 PB - ACS AN - OPUS4-47403 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zeise, I. A1 - Heiner, Z. A1 - Holz, S. A1 - Joester, Maike A1 - Buttner, C. A1 - Kneipp, Janina T1 - Raman imaging of plant cell walls in sections of cucumis sativus N2 - Raman microspectra combine information on chemical composition of plant tissues with spatial information. The contributions from the building blocks of the cell walls in the Raman spectra of plant tissues can vary in the microscopic sub-structures of the tissue. Here, we discuss the analysis of 55 Raman maps of root, stem, and leaf tissues of Cucumis sativus, using different spectral contributions from cellulose and lignin in both univariate and multivariate imaging methods. Imaging based on hierarchical cluster analysis (HCA) and principal component analysis (PCA) indicates different substructures in the xylem cell walls of the different tissues. Using specific signals from the cell wall spectra, analysis of the whole set of different tissue sections based on the Raman images reveals differences in xylem tissue morphology. Due to the specifics of excitation of the Raman spectra in the visible wavelength range (532 nm), which is, e.g., in resonance with carotenoid species, effects of photobleaching and the possibility of exploiting depletion difference spectra for molecular characterization in Raman imaging of plants are discussed. The reported results provide both, specific information on the molecular composition of cucumber tissue Raman spectra, and general directions for future imaging studies in plant tissues. KW - Raman KW - Imaging KW - Pants PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474610 DO - https://doi.org/10.3390/plants7010007 SN - 2223-7747 VL - 7 IS - 1 SP - 7, 1 EP - 16 PB - MDPI, ST ALBAN-ANLAGE 66, CH-4052 BASEL, SWITZERLAND AN - OPUS4-47461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Stefanie A1 - Ebel, Kenny A1 - Schürmann, Robin M. A1 - Miloavljevic, A. R. A1 - Guliani, A. A1 - Bald, Ilko T1 - Vacuum-UV induced DNA strand breaks – influence of the radiosensitizers 5-bromouracil and 8-bromoadenine N2 - Radiation therapy is a basic part of cancer treatment. To increase the DNA damage in carcinogenic cells and preserve healthy tissue at the same time, radiosensitizing molecules such as halogenated nucleobase analogs can be incorporated into the DNA during the cell reproduction cycle. In the present study 8.44 eV photon irradiation induced single strand breaks (SSB) in DNA sequences modified with the radiosensitizer 5-bromouracil (5BrU) and 8-bromoadenine (8BrA) are investigated. 5BrU was incorporated in the 13mer oligonucleotide flanked by different nucleobases. It was demonstrated that the highest SSB cross sections were reached, when cytosine and thymine were adjacent to 5BrU, whereas guanine as a neighboring nucleobase decreases the activity of 5BrU indicating that competing reaction mechanisms are active. This was further investigated with respect to the distance of guanine to 5BrU separated by an increasing number of adenine nucleotides. It was observed that the SSB cross sections were decreasing with an increasing number of adenine spacers between guanine and 5BrU until the SSB cross sections almost reached the level of a non-modified DNA sequence, which demonstrates the high sequence dependence of the sensitizing effect of 5BrU. 8BrA was incorporated in a 13mer oligonucleotide as well and the strand breaks were quantified upon 8.44 eV photon irradiation in direct comparison to a non-modified DNA sequence of the same composition. No clear enhancement of the SSB yield of the modified in comparison to the non-modified DNA sequence could be observed. Additionally, secondary electrons with a maximum energy of 3.6 eV were generated when using Si as a substrate giving rise to further DNA damage. A clear enhancement in the SSB yield can be ascertained, but to the same degree for both the non-modified DNA sequence and the DNA sequence modified with 8BrA. KW - Vacuum-UV KW - 5-bromouracil KW - 8-bromoadenine PY - 2019 DO - https://doi.org/10.1039/c8cp06813e SN - 1463-9084 VL - 21 IS - 4 SP - 1972 EP - 1979 PB - RSC AN - OPUS4-47462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Song, L. A1 - You, Yi A1 - Evans-Nguyen, T. T1 - Surface acoustic wave nebulization with atmospheric-pressure chemical ionization for enhanced ion signal N2 - Many ambient desorption/ionization mass spectrometry (ADI-MS) techniques rely critically on thermal desorption. Meanwhile, the analyte classes that are successfully studied by any particular ADI-MS methods are strongly dependent on the type of ionization source. Generally, spraybased ionization sources favor polar analytes, whereas plasmabased sources can be used for more hydrophobic analytes and are more suitable for molecules with small molar masses. In the present work, classic atmospheric-pressure chemical ionization (APCI) is used. To provide improved desorption performance for APCI, a surface acoustic wave nebulization (SAWN) device was implemented to convert liquid analytes into fine airborne particles. Compared to conventional SAWN that is used solely as an ionization source for liquid samples, the coupling of SAWN and APCI significantly improves ion signal by up to 4 orders of magnitude, reaching comparable ion abundances to those of electrospray ionization (ESI). Additionally, this coupling also extends the applicable mass range of an APCI source, conventionally known for the ionization of small molecules <500 Da. Herein, we discuss cursory evidence of this applicability to a variety of analytes including both polar and nonpolar small molecules and novel peptides that mimic biomolecules upward of 1000 Da. Observed species are similar to ESI-derived ions including doubly charged analyte ions despite presumably different charging mechanisms. SAWN−APCI coupling may thus involve more nuanced ionization pathways in comparison to other ADI approaches. KW - Nebulization KW - Ionization KW - Atomspheric-Pressure KW - Acoustic PY - 2018 DO - https://doi.org/10.1021/acs.analchem.8b03927 SN - 0003-2700 SN - 1520-6882 VL - 91 IS - 1 SP - 912 EP - 918 PB - American Chemical Society AN - OPUS4-47463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Stefanie A1 - Ebel, Kenny A1 - Schürmann, Robin M. A1 - Heck, Christian A1 - Meiling, T. A1 - Milosavljevic, A. A1 - Giuliani, A. A1 - Bald, Ilko T1 - Vacuum-UV and low-energy electron induced DNA strand breaks - Influence of the DNA sequence and substrate N2 - DNA is effectively damaged by radiation, which can on the one hand lead to cancer and is on the other hand directly exploited in the treatment of tumor tissue. DNA strand breaks are already induced by photons having an energy below the ionization energy of DNA. At high photon energies, most of the DNA strand breaks are induced by low-energy secondary electrons. In the present study we quantified photon and electron induced DNA strand breaks in four different 12mer oligonucleotides. They are irradiated directly with 8.44 eV vacuum ultraviolet (VUV) photons and 8.8 eV low energy electrons (LEE). By using Si instead of VUV transparent CaF2 as a substrate the VUV exposure leads to an additional release of LEEs, which have a maximum energy of 3.6 eV and can significantly enhance strand break cross sections. Atomic force microscopy is used to visualize strand breaks on DNA origami platforms and to determine absolute values for the strand break cross sections. Upon irradiation with 8.44 eV photons all the investigated sequences show very similar strand break cross sections in the range of 1.7 - 2.3 x 10-16 cm2. The strand break cross sections for LEE irradiation at 8.8 eV are one to two orders of magnitude larger than the ones for VUV photons, and a slight sequence dependence is observed. The sequence dependence is even more pronounced for LEEs with energies < 3.6 eV. The present results help to assess DNA damage by photons and electrons close to the ionization threshold. KW - Vacuum-UV KW - Low-Energy KW - DNA KW - DNA-Sequence PY - 2019 DO - https://doi.org/10.1002/cphc.201801152 SN - 1439-7641 VL - 20 IS - 6 SP - 823 EP - 830 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-47464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wack, Yannick T1 - Simulation der Schallausbreitung in Eisenbahnschienen mit FEM und SAM N2 - Die Simulation von Ultraschallausbreitung ist ein wesentliches Hilfsmittel zur Optimierung von Prüfanordnungen und wird zunehmend in der Prüfvorbereitung eingesetzt. Eisenbahnschienen sind Bauteile mit komplexer Geometrie und im eingebauten Zustand eingeschränkter Zugänglichkeit. Bei der Prüfung im Feld entstehen aus der Schienengeometrie komplexe Echosignale mit Formanzeigen, die schwer zu interpretieren sind. Für das bessere Verständnis der Schallausbreitung in der Eisenbahnschiene wird diese in einem ersten Schritt mit Hilfe verschiedener Ansätze modelliert. Hierbei werden Finite Elemente Methoden und semi-analytischen Modelle verwendet. In einem zweiten Schritt werden die Ergebnisse der Simulationsmodelle einander gegenübergestellt und mit Messungen an realen Schienen verglichen. Ziel dieser Untersuchungen ist die Validierung von Simulationsverfahren mit Hilfe von Messdatensätzen und Überprüfung der Anwendbarkeit bei der Bewertung von Ergebnissen der Schienenprüfung. T2 - DGZfP-Jahrestagung 2018 CY - Leibzig, Gemany DA - 07.05.2018 KW - Ultraschall KW - FEM KW - Eisenbahn KW - Simulation KW - SAM PY - 2018 AN - OPUS4-47412 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wack, Yannick T1 - Simulation der Schallausbreitung in Eisenbahnschienen mit FEM und SAM N2 - Die Simulation von Ultraschallausbreitung ist ein wesentliches Hilfsmittel zur Optimierung von Prüfanordnungen und wird zunehmend in der Prüfvorbereitung eingesetzt. Eisenbahnschienen sind Bauteile mit komplexer Geometrie und im eingebauten Zustand eingeschränkter Zugänglichkeit. Bei der Prüfung im Feld entstehen aus der Schienengeometrie komplexe Echosignale mit Formanzeigen, die schwer zu interpretieren sind. Für das bessere Verständnis der Schallausbreitung in der Eisenbahnschiene wird diese in einem ersten Schritt mit Hilfe verschiedener Ansätze modelliert. Hierbei werden Finite Elemente Methoden und semi-analytischen Modelle verwendet. In einem zweiten Schritt werden die Ergebnisse der Simulationsmodelle einander gegenübergestellt und mit Messungen an realen Schienen verglichen. Ziel dieser Untersuchungen ist die Validierung von Simulationsverfahren mit Hilfe von Messdatensätzen und Überprüfung der Anwendbarkeit bei der Bewertung von Ergebnissen der Schienenprüfung. T2 - 10. Fachtagung - ZfP im Eisenbahnwesen 2018 CY - Wittenberge, Germany DA - 13.03.2018 KW - Ultraschall KW - FEM KW - Eisenbahn KW - Simulation KW - SAM PY - 2018 AN - OPUS4-47415 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Career talk & lab tour - Working at BESSY II, a large scale research facility in Adlershof N2 - What exactly does a postdoc do at a research institute? What scientific questions does he or she want to address? What is their daily work routine? During our regular Lab Tours, female postdocs provide insight into their jobs. They also tell us about their career path: How did they get there? And what do they envision for their professional future? This time, Dr. Ana Guilherme Buzanich, a scientist from the Structure Analysis division at the Bundesanstalt für Materialforschung und -prüfung (BAM), will give an overview of her Research areas. She works at the electron storage ring BESSY-II where she conducts experiments at two hard X-ray beamlines (BAMline and µSpot). The tour includes a guided visit of the research facility. T2 - Lab Tour & Career Talk, WiNS CY - Berlin, Germany DA - 11.02.2019 KW - Women in STEM KW - X-ray Spectroscopy KW - Synchrotron KW - Beamline KW - Material characterization PY - 2019 AN - OPUS4-47418 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Manso, M. A1 - Pessanha, S. A1 - Guerra, M. A1 - Reinholz, Uwe A1 - Afonso, C. A1 - Radtke, Martin A1 - Lourenco, H. A1 - Carvalho, M. L. A1 - de Oliveira Guilherme Buzanich, Ana T1 - Assessment of Toxic Metals and Hazardous Substances in Tattoo Inks Using Sy-XRF, AAS, and Raman Spectroscopy N2 - Synchrotron radiation X-ray fluorescence spectroscopy, in conjunction with atomic absorption and Raman spectroscopy, was used to analyze a set of top brand tattoo inks to investigate the presence of toxic elements and hazardous substances. The Cr, Cu, and Pb contents were found to be above the maximum allowed levels established by the Council of Europe through the resolution ResAP(2008)1 on requirements and criteria for the safety of tattoos and permanent makeup. Raman analysis has revealed the presence of a set of prohibited substances mentioned in ResAP(2008)1, among which are the pigments Blue 15, Green 7, and Violet 23. Other pigments that were identified in white, black, red, and yellow inks are the Pigment White 6, Carbon Black, Pigment Red 8, and a diazo yellow, respectively. The present results show the importance of regulating tattoo ink composition. KW - Synchrotron KW - Tattoo inks KW - XRF KW - Toxic metals KW - Hazardous substances PY - 2019 DO - https://doi.org/10.1007/s12011-018-1406-y VL - 187 IS - 2 SP - 596 EP - 601 PB - Springer AN - OPUS4-47369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Mirtsch, Mona ED - Mangelsdorf, Axel ED - Weiler, Petra T1 - Konformitätsbewertung im Bereich Cybersicherheit N2 - Das Ziel dieses Kapitels besteht darin, die Rolle von Konformitätsbewertung für die Erhöhung der Cybersicherheit von Produkten, Dienstleistungen und Prozessen zu betrachten. Dazu wird der Begriff Cybersicherheit beleuchtet sowie ausgewählte Cybersicherheitsnormen kurz vorgestellt. Im Folgenden wird der regulative europäische Rahmen für die Konformitätsbewertung aus ordnungspolitischer Sicht sowie der aktuelle Verordnungsentwurf zum Cybersecurity Act dargestellt und kritsch beleuchtet. KW - Cybersicherheit KW - Konformitätsbewertung KW - Cybersecurity Act KW - Normen PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473829 UR - https://www.degruyter.com/downloadpdf/books/9783110629057/9783110629057-009/9783110629057-009.pdf SN - 978-3-11062-905-7 DO - https://doi.org/10.1515/9783110629057 SP - 141 EP - 164 PB - De Gruyter CY - Berlin, Boston ET - 1 AN - OPUS4-47382 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Goenaga-Infante, H A1 - Malinovskiy, D. A1 - Hill, S. A1 - Ren, T. A1 - Wang, J. A1 - Vocke, R. D. A1 - Murphy, K. E. A1 - Nonose, N. A1 - Rienitz, O. A1 - Noordmann, J. T1 - Certification of ERM-EB400, the first matrix reference material for lead isotope amount ratios, and ERM-AE142, a lead solution providing a lead isotopic composition at the edge of natural variation N2 - Lead isotope amount ratios are commonly used in diverse fields such as archaeometry, geochemistry and forensic science. Currently, five reference materials with certified lead isotope amount ratios are available, namely NIST SRM 981, 982 and 983, GBW-04442 and NMIJ 3681-a. Only NIST SRM 981 and NMIJ 3681-a have approximately natural isotopic compositions, and NIST SRM 981 is predominantly used for correcting mass discrimination/mass fractionation in the applied mass spectrometric procedures. Consequently, there is no other certified reference material available to be used for validation and/or quality control of the analytical procedures applied to lead isotope amount ratio measurements. To fill this gap, two new reference materials have been produced and certified for their lead isotope amount ratios. For both certified reference materials, complete uncertainty budgets have been calculated and SI traceability has been established. This provides the users with independent means for validating and verifying their analytical procedures and for conducting quality control measures. ERM-EB400 is a bronze material with a nominal lead mass fraction of 45 mg kg-1 and certified lead isotope amount ratios of n(206Pb)/n(204Pb) = 18.072(17) mol mol-1, n(207Pb)/n(204Pb) = 15.578(18) mol mol-1 and n(208Pb)/n(204Pb) = 38.075(46) mol mol-1 with the associated expanded uncertainties (k = 2) given in brackets. ERM-AE142 is a high-purity solution of lead in 2% nitric acid with a nominal mass fraction of 100 mg kg-1 and certified Pb isotope amount ratios of n(206Pb)/n(204Pb) = 21.114(17) mol mol-1, n(207Pb)/n(204Pb) = 15.944(17) mol mol-1 and n(208Pb)/n(204Pb) = 39.850(44) mol mol-1 with the associated expanded uncertainties (k = 2) given in brackets. Both materials are specifically designed to fall within the natural lead isotopic variation and to assist users with the validation and verification of their analytical procedures. Note that while one of these reference materials requires the chemical separation of Pb from its matrix (ERM-EB400), the other does not (ERM-AE142). As additional information, δ208/206PbNIST SRM981 values are provided for both materials. For ERM-AE142, a delta value of δ208/206PbNIST SRM981 = -28.21(30) ‰ was obtained, and for ERM-EB400, a delta value of δ208/206PbNIST SRM981 = -129.47(38) ‰ was obtained, with the associated expanded uncertainties (k = 2) given in brackets. KW - Lead isotope variations KW - Radiogenic isotopes KW - Isotope reference material KW - Metrology in chemistry KW - Measurement uncertainty PY - 2019 DO - https://doi.org/10.1111/ggr.12253 SN - 1751-908X SN - 1639-4488 VL - 43 IS - 1 SP - 23 EP - 37 PB - John Wiley & Sons AN - OPUS4-47383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - MALDI-TOF MS und MALDI-MSI zur Identifikation und Klassifizierung von Pollen N2 - Es werden die letzten Ergebnisse präsentiert, die es ermöglichen, einzelne Pollenkörner unterschiedlicher Arten in Mischungen mittels MALDI-TOF Massenspektrometrie bzw. MALDI-TOF Imaging zu messen und unter Zuhilfenahme multivariater Auswertemethoden zu klassifizieren. T2 - 24. Bruker MALDI Anwendertreffen CY - Leipzig, Germany DA - 18.02.2019 KW - MALDI-TOF Massenspektrometrie KW - Pollenkörner KW - Klassifizierung KW - MALDI Imaging KW - Multivariate Analyse PY - 2019 AN - OPUS4-47441 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler T1 - In-situ Röntgencomputertomographie für mechanische, thermische und hydraulische Prozesse N2 - Die Präsentation demonstriert die Fähigkeiten der Röntgencomputertomographie (CT) zur Identifizierung quantitativer Materialeigenschaften wie Faserorientierung und Korrosionsverteilung sowie die Implementierung von CT-Daten innerhalb numerischer Simulationen. Die besondere Stärke der CT, als zerstörungsfreies Prüfverfahren, ermöglicht es, das Materialverhalten und den Versagensprozess während mechanischer, hydraulischer und thermischer Prozesse zu beobachten. Die Ergebnisse einer Reihe von Ex-situ und In-situ Testprogrammen unter Bedingungen wie mechanische Belastung, Wassertransport und thermische Exposition, stellen die Nutzungsmöglichkeiten dieser Verfahren in Kombination mit der CT in eindrucksvoller Weise dar. T2 - InnoTesting Konferenz CY - Wildau, Germany DA - 21.02.2019 KW - Röntgencomputertomographie (CT) KW - In-situ Prüfverfahren KW - Feuchtigkeitsmessung KW - Digitale Bildkorrelation (DVC) KW - Faserverstärkter Beton (FRC) PY - 2019 AN - OPUS4-47442 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kunz, Valentin T1 - Surface chemical transformations of nanoparticles N2 - Nanomaterials are a relatively new class of materials for which a regulatory framework still has to be established and regulators require comprehensive datasets of well characterized nanomaterials for the implementation. Especially information about the surface chemistry of nanoparticles is crucial, since it largely determines their biological and environmental fate. How the surface chemistry changes under relevant ageing conditions is of particular interest, because exposure will normally occur not to the pristine material but to a nanoform that underwent some kind of transformation. In this talk, first a short overview about the contributions of division 6.1 to multiple European-funded projects will be presented, in which surface analytical techniques are used to improve the physical-chemical characterization of nanomaterials. Secondly, a study investigating the surface-chemical transformations of a representative set of titanium dioxide nanoparticles is discussed in more detail. The ageing has partly been performed at the BAM division 7.5, and the surface chemistry was analyzed using time-of-flight secondary ion mass spectrometry (ToF-SIMS) and X-ray photoelectron spectroscopy (XPS). By analyzing the complex mass spectra with principal component analysis (PCA), it was possible to identify even subtle changes that occur upon ageing. T2 - Abteilungsseminar CY - BAM, Berlin, Germany DA - 25.2.2019 KW - Nanoparticles KW - Surface Chemistry KW - Ageing KW - Titanium Dioxide KW - ToF-SIMS PY - 2019 AN - OPUS4-47444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - CAT-Technologie zur Bestimmung der Klebfestigkeit N2 - Der Vortrag widmet sich der „ CAT-TECHNOLOGIE ZUR BESTIMMUNG DER KLEBFESTIGKEIT“ und beschreibt die Punkte „Motivation –CAT-Technologie (Centrifugal Adhesion Testing), Klebfestigkeit ( Materialscreening verschiedener Werkstoffklassen, Klebstoffscreening fürV2A gegenV2A als Referenz, Klebstoffscreening für Niedrigenergie-Polymere und Oberfächenmodifizierung von Niedrigenergie-Polymeren) und Verbundfestigkeit (“Stirnabzug vs. Zug-Scher-Prüfung an CFK) im Einzelnen. T2 - 17. Praxisseminar KLEBEN CY - IWF Jena, Germany DA - 30.01.2019 KW - CAT-Technologie KW - Klebfestigkeit KW - Verbundfestigkeit KW - Niedrigenergie-Polymeren PY - 2019 AN - OPUS4-47466 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Sekine, R. A1 - Steckenmesser, D. A1 - Lombi, E. A1 - Herzel, Hannes A1 - Zuin, L. A1 - Wang, D. A1 - Felix, R. A1 - Adam, Christian T1 - Combining diffusive gradients in thin films (DGT) and spectroscopic techniques for the determination of phosphorus species in soils N2 - A wide range of methods are used to estimate the plant-availability of soil phosphorus (P). Published research has shown that the diffusive gradients in thin films (DGT) technique has a superior correlation to plant-available P in soils compared to standard chemical extraction tests. In order to identify the plantavailable soil P species, we combined DGT with infrared and P K- and L2,3-edge X-ray adsorption near edge structure (XANES) spectroscopy. This was achieved by spectroscopically investigating the dried binding layer of DGT devices after soil deployment. All three spectroscopic methods were able to distinguish between different kinds of phosphates (poly-, trimeta-, pyro- and orthophosphate) on the DGT binding layer. However, infrared spectroscopy was most sensitive to distinguish between different types of adsorbed inorganic and organic phosphates. Furthermore, intermediates of the time-resolved hydrolysis of trimetaphosphate in soil could be analyzed. KW - Phosphorus plant-availability KW - X-ray adsorption near-edge structure (XANES) spectroscopy KW - Infrared spectroscopy KW - Diffusive gradients in thin films (DGT) PY - 2019 DO - https://doi.org/10.1016/j.aca.2019.01.037 SN - 0003-2670 VL - 1057 SP - 80 EP - 87 PB - Elsevier AN - OPUS4-47471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Loewer, M. A1 - Guenther, T. A1 - Igel, J. A1 - Kruschwitz, Sabine A1 - Martin, T. A1 - Wagner, N. T1 - Ultra-broad-band electrical spctroscopy of soils and sediments - a combined permittivity and conductivity model N2 - We combined two completely different methods measuring the frequency-dependent electrical properties of moist porous materials in order to receive an extraordinary large frequency spectrum. In the low-frequency (LF) range, complex electrical resistivity between 1 mHz and 45 kHz was measured for three different soils and sandstone, using the spectral induced polarization (SIP) method with a four electrode cell. In the high-frequency (HF) radio to microwave range, complex dielectric permittivity was measured between 1MHz and 10 GHz for the same samples using dielectric spectroscopy by means of the coaxial transmission line technique. The combined data sets cover 13 orders of magnitude and were transferred into their equivalent expressions: the complex effective dielectric permittivity and the complex effective electrical conductivity.We applied the Kramers-Kronig relation in order to justify the validity of the data combination. A new phenomenological model that consists of both dielectric permittivity and electrical conductivity terms in a Debye- and Cole–Cole-type manner was fitted to the spectra. The combined permittivity and conductivity model accounts for the most common representations of the physical quantities with respect to the individual measuring method. A maximum number of four relaxation processes was identified in the analysed frequency range. Among these are the free water and different interfacial relaxation processes, the Maxwell-Wagner effect, the counterion relaxation in the electrical double layer and the direct-current electrical conductivity. There is evidence that free water relaxation does not affect the electrical response in the SIP range. Moreover, direct current conductivity contribution (bulk and interface) dominates the losses in the HF range. Interfacial relaxation processes with relaxations in the HF range are broadly distributed down to the LF range. The slowest observed process in the LF range has a minor contribution to the HF response. KW - Electrical properties KW - Permeability KW - Porosity KW - Hydrogeophysics PY - 2017 DO - https://doi.org/10.1093/gji/ggx242 VL - 210 IS - 3 SP - 1360 EP - 1373 PB - Oxford University Press CY - Oxford AN - OPUS4-42598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Vergleich der Arbeitsweise von Akkreditierungsstellen in Europa N2 - Das übergeordnete Ziel des Projekts ist es, ein Werkzeug bereitzustellen, mit dem die Arbeitsweise von Akkreditierungsstellen auf objektiver Grundlage und kennzahlenbasiert analysiert werden kann. Durch Anwendung auf mehrere Akkreditierungsstellen soll zudem eine vergleichende Analyse verschiedener Akkreditierungsstellen ermöglicht werden, die zur Harmonisierung der Arbeitsweise der Akkreditierungsstellen in Europa beiträgt. In der ersten Phase des Projekts wurden die Tätigkeiten von Akkreditierungsstellen und ihre auf gesetzlichen und normativen Anforderungen beruhenden Verpflichtungen systematisch analysiert. Es wurde eine mit Kennzahlen unterlegte Prozesslandschaft entwickelt, die ein Modell bildet, dem die implementierten Abläufe und eingesetzten Ressourcen der Akkreditierungsstelle zugeordnet werden können. In der zweiten Phase wurden die Prozesse der Deutschen Akkreditierungsstelle DAkkS dem Modell zugeordnet. Die Übertragbarkeit des so erstandenen Modells wurde in einem dritten Schritt durch die Erweiterung auf sieben weitere Akkreditierungsstellen im europäischen Raum untersucht. Im Rahmen eines Abteilungsseminars wurden die Ergebnisse der Datenerhebung der acht teilnehmenden Akkreditierungsstellen in anonymisierter Form präsentiert. T2 - Abteilungsseminar der Abteilung S CY - BAM Berlin, Germany DA - 10.10.2017 KW - Akkreditierung KW - Benchmarking PY - 2017 AN - OPUS4-42715 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Götschel, S. T1 - Simulation und Identifizierung von Delaminationen in kohlenstofffaserverstärkten Kunststoffen N2 - Kohlenstofffaserverstärkte Kunststoffe werden häufig in sicherheitsrelevanten Gebieten wie im Automobilbau und in der Luftfahrt eingesetzt. Hier besteht ein zunehmender Bedarf an zerstörungsfreien Prüfmethoden um die Sicherheit und Zuverlässigkeit der eingesetzten Bauteile gewährleisten zu können. Aktive Thermographieverfahren ermöglichen die effiziente Prüfung großer Flächen mit hoher Auflösung in wenigen Arbeitsschritten. Ein wichtiges Teilgebiet ist die Ortung und Charakterisierung von Delaminationen, die sowohl bereits in der Fertigung als auch während der Nutzung eines Bauteils auftreten und dessen strukturelle Integrität schwächen können. In diesem Beitrag beschäftigen wir uns mit der Modellierung und effizienten Finite-Elemente-Simulation solcher Delaminationen, sowie ihrer Rekonstruktion aus gemessenen Oberflächentemperaturen. Dabei sollen die Rekonstruktionsergebnisse nicht nur eine Ortung der Fehlstellen, sondern auch eine quantitative Beschreibung der geometrischen Abmessungen und des Umfangs der Schädigungen ermöglichen. Hier erlauben numerische Rekonstruktionsverfahren basierend auf der Simulation des dreidimensionalen Wärmetransports eine Defektrekonstruktion unter Berücksichtigung lateraler Wärmeleitungsprozesse sowie von anisotropen thermischen Materialeigenschaften. Da solche Verfahren sehr rechenaufwändig sind diskutieren wir schnelle heuristische Rekonstruktionsverfahren für die Anwendung in der Praxis. T2 - Thermografie-Kolloquium 2017 CY - Berlin, Germany DA - 28.09.2017 KW - Aktive Thermografie KW - Simulation KW - Rekonstruktion KW - CFK PY - 2017 AN - OPUS4-42717 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abbas, Ioana M. A1 - Schwaar, Timm A1 - Bienwald, Frank A1 - Weller, Michael G. T1 - Predictable Peptide Conjugation Ratios by Activation of Proteins with Succinimidyl Iodoacetate (SIA) N2 - The small heterobifunctional linker succinimidyl iodoacetate (SIA) was examined for the preparation of peptide–protein bioconjugates with predicable conjugation ratios. For many conjugation protocols, the protein is either treated with a reductant to cleave disulfide bonds or is reacted with thiolation chemicals, such as Traut’s reagent. Both approaches are difficult to control, need individual optimization and often lead to unsatisfactory results. In another popular approach, a heterobifunctional linker with a N-hydroxysuccinimide (NHS) and a maleimide functionality is applied to the protein. After the activation of some lysine ε-amino groups with the NHS ester functionality, a cysteine-containing peptide is attached to the activated carrier protein via maleimide. Particularly, the maleimide reaction leads to some unwanted byproducts or even cleavage of the linker. Many protocols end up with conjugates with unpredictable and irreproducible conjugation ratios. In addition, the maleimide-thiol addition product should be assumed immunogenic in vivo. To avoid these and other disadvantages of the maleimide approach, we examined the known linker succinimidyl iodoacetate (SIA) in more detail and developed two protocols, which lead to peptide–protein conjugates with predefined average conjugation ratios. This holds potential to eliminate tedious and expensive optimization steps for the synthesis of a bioconjugate of optimal composition. KW - Bioconjugate KW - Carrier protein KW - Immunogen KW - Hapten KW - Linker KW - Antibody drug conjugate KW - ADC KW - Drug-to-antibody ratio KW - DAR KW - Conjugation ratio KW - Conjugation density KW - Carrier load KW - Click reaction KW - Click chemistry PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-427188 UR - http://www.mdpi.com/2409-9279/1/1/2 DO - https://doi.org/10.3390/mps1010002 SN - 2409-9279 VL - 1 SP - 1 EP - 14 PB - MDPI CY - Basel, Schweiz AN - OPUS4-42718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Analysis of Fluorine Traces in TiO2 Nanoplatelets by SEM/EDX, AES and TOF-SIMS N2 - The synthesis of TiO2 nanoplatelets with fluorine-containing reactants is carried out using Ti (IV) butoxide as precursor and concentrated HF as shape controller, the final product requires a working up in order to eliminate or at least to reduce the amount of residual fluorides, which is realized here by well-defined thermal treatment. Qualitative investigation of the bulk elemental composition by means of EDX of TiO2 nanoparticles (NPs) has identified fluorine in case of the as-synthesized samples. EDX spectra of thermally treated products exhibit either a fluorine content close to the limit of detection. The latter holds also true for the reference sample, TiO2 NPs of bipyramidal shape and prepared by a different synthesis route. For differentiation whether fluorine is present in the bulk or at the surface of the TiO2 nanoplatelets, top-surface sensitive AES and ToF-SIMS has been applied. Secondary ions of fluorine are detected in ToF-SIMS spectra of all samples, but could be roughly quantified by measurement of same reference sample as for EDX, namely TiO2 nano-bipyramids. This revealed that the amount of fluorine within1 nm depth beneath the surface is reduced in the thermally treated specimen compared to the raw product down to a content about as low as in the reference sample. AES allows analyzing analysis of the first few nanometers from the top-surface of individual NPs by point analysis. An F KLL peak has been detected at the surface of samples of as-prepared TiO2 nanoplatelets under optimized measurement conditions, but was not detectable after their calcination, which is in agreement with ToF-SIMS results. Moreover, high resolution AES on single TiO2 nanoplatelets elucidated that the surface atomic layers surrounding the TiO2 nanopaltelet contain fluorides before thermal treatment of the NPs. T2 - 17th European Conference on Applications of Surface and Interface Analysis ECASIA 2017 CY - Montpellier, France DA - 24.09.2017 KW - Titania KW - Nanoparticles KW - Fluorine KW - SEM/EDX KW - Auger Electron Spectroscopy KW - Nanoplatelets PY - 2017 AN - OPUS4-42656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Functionalization of TiO2 Nanoparticles and supports for Assembly of Multiple Porous Layers N2 - Self-assembly of TiO2 nanoparticles in multiple layers by layer-by-layer deposition has been selected of different deposition procedures usually applied for fabrication of TiO2 thin films with defined and homogeneous thickness on supports of interest for the large-scale applications. The substrates tested were: conductive (FTO) glass, silica glass and titanium alloy. The selected film fabrication technique consists of the deposition of alternating layers of oppositely charged, i.e. functionalized, TiO2 nanoparticle layers with wash steps in between. The controlled assembly of TiO2 nanoparticles on the supports surface requires both a proper functionalization of the supports to promote the adhesion of the TiO2 film to the substrates and proper functionalization of TiO2 nanoparticles to allow attachment to substrate and subsequent reaction between different NP layers. The current study focusses on the analytical control of the functionalization of the substrates with 3-Aminopropyltriethoxysilane (APTS) and glutaraldehyde (GA) by means of surface sensitive methods, XPS, Auger Electron Spectroscopy (AES) and ToF-SIMS. Chemical composition of surface of functionalized substrates shows differences in the degree and type of modification in dependence on substrate. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2017 CY - Montpellier, France DA - 24.09.2017 KW - Functionalization KW - Substrates KW - Titania KW - Nanoparticles KW - SEM/EDX KW - XPS KW - Auger Electron Spectroscopy KW - ToF-SIMS PY - 2017 AN - OPUS4-42658 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Morphological and surface analytical long-term investigations of a CH3NH3PbI3/TiO2 perovskite solar cell N2 - Long-term investigations over 20 weeks of a organic-inorganic hybrid solar cell with SEM/EDX and XPS will be presented. T2 - Kratos User Meeting 2017 CY - Stuttgart, Germany DA - 17.10.2017 KW - Perovskite solar cell KW - SEM with EDX KW - XPS PY - 2017 AN - OPUS4-42626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sankat, Nina A1 - Wilsch, Gerd A1 - Gottlieb, Cassian A1 - Millar, Steven T1 - Analysis of concrete structures using Laser-Induced Breakdown Spectroscopy N2 - The Laser-Induced Breakdown Spectroscopy (LIBS) is a laser spectroscopic method which allows a time efficient, minor-destructive, chemical analysis of materials. In principle all elements on the periodic table can be simultaneously analysed by using LIBS, regardless of the state of aggregation. LIBS offers numerous applications in the field of civil engineering; most importantly the analysis of building materials. This work will focus on the evaluation of concrete structures and harmful substances which can penetrate the concrete. A variety of information can be collected through LIBS. Determining the concentration of harmful substances like chloride, sodium or sulphur, the examination of the carbonation depth and the distinction between varying layers of materials (e.g. aggregates, cement paste, metals, etc.) are possible applications. All this information can be provided through one LIBS measurement in the form of a high resolution 2D element map, with resolutions up to 0.1 mm x 0.1 mm. To scan a concrete surface only an optical access is needed. To create a depth profile of an intruding substance the extraction of a drill core is necessary. Onsite measurements via LIBS can be conducted by using a mobile version of the LIBS system. Through using calibration curves LIBS allows not only the qualitative but also quantitative analysis of element concentrations. All those prospects make LIBS a trendsetting method to secure the integrity of infrastructures in a sustainable manner. A variety of examples which show the performance and results of LIBS analysis will be presented. T2 - CoMS 2017 CY - Zadar, Croatia DA - 19.04.2017 KW - Testing method KW - Concrete KW - LIBS KW - Harmful substances PY - 2017 SN - 978-953-8168-04-8 VL - 1 SP - 334 EP - 340 AN - OPUS4-42630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sankat, Nina T1 - Analysis of concrete structures using Laser-Induced Breakdown Spectroscopy N2 - The Laser-Induced Breakdown Spectroscopy (LIBS) is a laser spectroscopic method which allows a time efficient, minor-destructive, chemical analysis of materials. In principle all elements on the periodic table can be simultaneously analysed by using LIBS, regardless of the state of aggregation. LIBS offers numerous applications in the field of civil engineering; most importantly the analysis of building materials. This work will focus on the evaluation of concrete structures and harmful substances which can penetrate the concrete. A variety of information can be collected through LIBS. Determining the concentration of harmful substances like chloride, sodium or sulphur, the examination of the carbonation depth and the distinction between varying layers of materials (e.g. aggregates, cement paste, metals, etc.) are possible applications. All this information can be provided through one LIBS measurement in the form of a high resolution 2D element map, with resolutions up to 0.1 mm x 0.1 mm. To scan a concrete surface only an optical access is needed. To create a depth profile of an intruding substance the extraction of a drill core is necessary. Onsite measurements via LIBS can be conducted by using a mobile version of the LIBS system. Through using calibration curves LIBS allows not only the qualitative but also quantitative analysis of element concentrations. All those prospects make LIBS a trendsetting method to secure the integrity of infrastructures in a sustainable manner. T2 - CoMS 2017 CY - Zadar, Croatia DA - 19.04.2017 KW - Testing method KW - LIBS KW - Concrete KW - Harmful substances PY - 2017 AN - OPUS4-42632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Juling, S. A1 - Niedzwiecka, A. A1 - Böhmert, L. A1 - Lichtenstein, D. A1 - Selve, S. A1 - Braeuning, A. A1 - Thünemann, Andreas A1 - Krause, E. A1 - Lampen, A. T1 - Protein Corona Analysis of Silver Nanoparticles Links to Their Cellular Effects N2 - The breadth of applications of nanoparticles and the access to food-associated consumer products containing nanosized materials lead to oral human exposure to such particles. In biological fluids nanoparticles dynamically interact with biomolecules and form a protein corona. Knowledge about the protein corona is of great interest for understanding the molecular effects of particles as well as their fate inside the human body. We used a mass spectrometry-based toxicoproteomics approach to elucidate mechanisms of toxicity of silver nanoparticles and to comprehensively characterize the protein corona formed around silver nanoparticles in Caco-2 human intestinal epithelial cells. Results were compared with respect to the cellular function of proteins either affected by exposure to nanoparticles or present in the protein corona. A transcriptomic data set was included in the analyses in order to obtain a combined multiomics view of nanoparticle-affected cellular processes. A relationship between corona proteins and the proteomic or transcriptomic responses was revealed, showing that differentially regulated proteins or transcripts were engaged in the same cellular signaling pathways. Protein corona analyses of nanoparticles in cells might therefore help in obtaining information about the molecular consequences of nanoparticle treatment. KW - Silver nanoparticles KW - Protein KW - Small-angle X-ray scattering KW - SAXS PY - 2017 DO - https://doi.org/10.1021/acs.jproteome.7b00412 SN - 1535-3893 SN - 1535-3907 VL - 16 IS - 11 SP - 4020 EP - 4034 PB - Americal Chemical Society AN - OPUS4-42688 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Beck, Uwe A1 - Negendank, Detlef A1 - Lohse, Volkmar A1 - Kormunda, M. A1 - Esser, N. T1 - Dependence of the optical constants and the performance in the SPREE gas measurement on the thickness of doped tin oxide over coatings N2 - In this study, thickness related changes of the optical properties of doped tin oxide were studied. Two different sets of samples were prepared. The first set was doped with iron or nickel on silicon substrate with thicknesses of 29–56 nm, the second was iron doped on gold/glass substrate with 1.6–6.3 nm. The optical constants were determined by using spectral ellipsometry (SE) followed by modelling of the dielectric function with an oscillator model using Gaussian peaks. The analysis of the optical constants shows a dependence of the refraction and the absorption on the thickness of the doped tin oxide coating. In addition to the tin oxide absorption in the UV, one additional absorption peak was found in the near-IR/red which is related to plasmonic effects due to the doping. This peak shifts from the near-IR to the red part of the visible spectrum and becomes stronger by reducing the thickness, probably due to the formation of metal nanoparticles in this layer. These results were found for two different sets of samples by using the same optical model. Afterwards the second sample set was tested in the Surface Plasmon Resonance Enhanced Ellipsometric (SPREE) gas measurement with CO gas. It was found that the thickness has significant influence on the sensitivity and thus the adsorption of the CO gas. By increasing the thickness from 1.6 nm to 5.1 nm, the sensing ability is enhanced due to a higher coverage of the surface with the over coating. This is explained by the high affinity of CO molecules to the incorporated Fe-nanoparticles in the tin oxide coating. By increasing the thickness further to 6.3 nm, the sensing ability drops because the layer disturbs the SPR sensing effect too much. T2 - 7th International Conference on Spectroscopic Ellipsometry (ICSE-7) DA - 06.06.2016 KW - Surface plasmon resonance KW - Spectroscopic ellipsometry KW - Doped tin oxide KW - Gas sensing KW - Plasmonic absorption PY - 2017 DO - https://doi.org/10.1016/j.apsusc.2016.11.188 SN - 0169-4332 VL - 421, Teil B SP - 480 EP - 486 PB - Elsevier B.V. AN - OPUS4-42692 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wilsch, Gerd T1 - Fast Quantitative Chemical Analysis of Cencrete using LIBS N2 - Non-destructive testing of concrete based on laser induced breakdown spectroscopy in civil engineering. KW - LIBS KW - Concrete KW - Chloride PY - 2017 SP - 289 EP - 325 CY - Berlin, Germany AN - OPUS4-42648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - DNA strand break induction by secondary radiation products: damage yields of OH-radicals, low energy electrons and prehydrated electrons N2 - The damage caused by ionizing radiation to biomolecules, especially DNA, is the reason to treat cancer via radiation therapy. A better understanding of the molecular processes and the quantification of the various damaging mechanisms is the prerequisit to develope efficient therapies. Hereby the understanding of the processes involved in the damage to DNA are of key interest due to its central role in reproduction and mutation. Due to the high amount of water in biological tissue, most of the damage is caused by the secondary particles produced by the interaction of the IR with water. Thereby a multitude of species are produced, e.g. kinetic low energy electrons, prehydrated electrons, OH-radicals and ions. The quantification of the contribution to DNA damage of the various species is of interest. Here we present an experimental approach to disentangle their relative DNA strand break yield. Plasmid DNA is irradiated in water with electrons under the presence of different scavengers. With the presented method it will be possible to reveal the relative contributions of OH-radicals, low energy electrons and prehydrated electrons to the DNA single and double strand break yield. T2 - Radiation Research Conference 2017 CY - Cancun, Mexico DA - 15.10.2017 KW - DNA KW - Dosimetry KW - Radiation damage KW - low energy electrons KW - OH radicals KW - Prehydrated electrons KW - LEE KW - Geant4 KW - Hydroxyl radicals KW - Radiation protection KW - Biomolecules KW - Microdosimetry PY - 2017 AN - OPUS4-42617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - From sensing to dosimetry: Immobilized single-stranded DNA on surfaces as versatile sensor for protein activity and irradiation damage N2 - We report on the design, preparation and application of immobilized Oligonucleotides as biological sensors for dosimetry and protein activity. Oligonucleotides can be custom tailored in terms of sequence and length to the needs of the specific application. The preparation can be scaled from small lab-scales to higher output via spotting technology on various surfaces such as glass, silicon-dioxide or gold. They can be applied for the sensing of DNA-protein interaction and surface-plasmon resonance to detect the influence of cosolutes on the protein activity. This can be applied in the testing of pharmaceutical or cosmsetic applications and incorporated in microfluidic devices. Other important use cases are the usage in dosimetric application where the oligonucleotides are subjected to ionizing radiation. They can directly act as a sensor for biological damage which is detected and quantified by the subsequent hybridization of complementary strands who carry a fluorescence dye. The quantification can be performed by an array scanner or fluorescence microscope. Investigation on a molecular level can be performed with the AFM-IR technique. Applications are calibration of radiation sources and the investigation of interaction of ionizing radiation with biomolecules. T2 - Euromat 2017 CY - Thessaloniki, Greece DA - 17.09.2017 KW - DNA KW - Protein KW - Dosimetry KW - Radiation damage KW - SPR KW - Surface modification PY - 2017 AN - OPUS4-42619 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Direct electron irradiation of DNA in fully aqueous environment: Microscopic dose determination in combination with Monte-Carlo simulations N2 - Introduction: Ionizing radiation & DNA damage Experimental setup: Direct electron irradiation of DNA in liquid Monte-Carlo simulations: Electron scattering & diffusion Application: Radiation protection by compatible solutes T2 - Seminarvortrag im Joint Ultrafast Dynamics Laboratory in Solution and at Interfaces CY - Helmholtz-Zentrum Berlin, Germany DA - 14.06.2017 KW - DNA KW - Ectoine KW - Microdosimetry KW - Dosimetry KW - Radiation damage KW - Compatible solutes KW - Low energy electrons KW - Ionizing radiation KW - OH radical KW - Hydroxyl radicals KW - Prehydrated electrons KW - Radiation therapy KW - Cancer KW - Cancer therapy KW - Radiation protection KW - Proteins KW - Monte carlo simulations KW - Geant4 KW - Electron scattering PY - 2017 AN - OPUS4-42620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Size effects in electrodeposited Ni-coatings N2 - Polycrystalline Ni materials with grain sizes less than 100 nm (nano crystalline NC) and with grain sizes in the micrometer range (micro crystalline MC) in form of thin films have become important in many technologies due to their improved physical, chemical and mechanical properties. Usual the mechanical properties of such coatings are described by a Hardness value and a Young´s modulus measured by Instrumented Indentation Testing (IIT).The behavior of such coatings during indentation test is influenced by different size effects having their representative length scale – grain size, coating thickness, length that characterizes the depth dependence of the hardness (Indentation Size Effect ISE). To estimate realistic values for the intrinsic coating Hardness and Young´s modulus all size effects have to be considered. For this work thin nano crystalline Ni – coatings (average grain size 30 nm) with thickness from 1 μm to 5 μm were electrodeposited on brass substrates. Indentation tests in the continuous stiffness measurement (CSM) mode were provided on as prepared Ni – coatings using a G200 Nanoindentation system (Fa. Keysight). For estimation of the intrinsic hardness of the coatings from composite hardness values calculated from the measured force –displacement curve using the Oliver & Pharr method, the model described by Z.S. Ma [1] was used. It was found that the experimental data can be well described by the model. The fitted values for the intrinsic hardness and the fitting parameters will be given. The different values of intrinsic hardness and of length characterizing depth dependence of the hardness for different coating thickness are discussed as results of changes in the coating structure because of changes in deposition parameters. [1] Z.S. Ma, Y.C. Zhou, S.G. Long, C. Lu: On the intrinsic hardness of a metallic film/substrate system: Indentation size and substrate effects. International Journal of Plasticity 34 (2012) 1-11. This work is supported by European Metrology Program for Innovation and Research (EMPIR) (JRP 14IND03 Strength – ABLE) T2 - Conference: Nanomechanical Testing in Materials Research and Development CY - Dubrovnik, Croatia DA - 01.10.2017 KW - Size effect KW - Substrate effect KW - Electrodeposited Ni - coatings KW - Instrumented indentation testing PY - 2017 AN - OPUS4-42664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poppenberg, J. A1 - Richter, S. A1 - Traulsen, Ch. H.-H. A1 - Darlatt, Erik A1 - Baytekin, B. A1 - Heinrich, Thomas A1 - Deutinger, P. M. A1 - Huth, K. A1 - Unger, Wolfgang A1 - Schalley, Ch. T1 - Programmable multilayers of nanometer-sized macrocycles on solid support and stimuli-controlled on-surface pseudorotaxane formation N2 - Mechanically interlocked molecules (MIMs) such as rotaxanes and catenanes are capable of mechanical motion on the nanoscale and are therefore promising prototypes for molecular machines in recent nanotechnology. However, most of the existing examples are isotropically distributed in solution, which prohibits concerted movement and with it the generation of macroscopic effects. Thus, arranging them in ordered arrays is of huge interest in recent research. We report the deposition of quite densely packed multilayers of tetralactam macrocycles on gold surfaces by metal-coordinated layer-by-layer self-assembly. Linear dichroism effects in angle-resolved NEXAFS spectra indicate a preferential orientation of the macrocycles. The sequence of the metal ions can be programmed by the use of different transition metal ions at each deposition step. Additionally, reversible on-surface pseudorotaxane formation was successfully realized by repeated uptake and release of axle molecules inside the macrocycles cavities. KW - NEXAFS KW - XPS KW - Supramolecular Chemistry KW - Multilayers KW - Pyridine KW - UV/Vis KW - Macrocycles KW - Pseudorotaxanes PY - 2013 DO - https://doi.org/10.1039/c3sc50558h VL - 4 IS - 8 SP - 3131 EP - 3139 AN - OPUS4-42668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - van de Kreeke, Johannes T1 - EPTIS and COMAR in support of international PT/RM trade T1 - EPTIS和COMAR为支持国际PT/RM贸易 N2 - The presentation shows how the PT/RM markets worldwide develop. It hints at a number of pitfalls in international trade and then describes how COMAR and EPTIS can aid trade by increasing RMP/PTP visibility. The presentation has a focus on EU/China. T2 - International Conference on Reference Materials and Proficiency Testing CY - Xiamen, China DA - 17.10.2017 KW - Reference materials (RM) KW - Proficiency testing (PT) KW - COMAR KW - EPTIS KW - Trade PY - 2017 AN - OPUS4-42673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neuhaus, Birger A1 - Schmid, Thomas A1 - Riedel, Jens T1 - Collection management and study of microscope slides: Storage, profiling, deterioration, restoration procedures, and general recommendations N2 - A wide range of aspects concerning microscope slides, their preparation, long-time storage, curatorial measures in collections, deterioration, restoration, and study is summarized based on our own data and by analyzing more than 600 references from the 19th century until 2016, 15 patents, and about 100 Materials Safety Data Sheets. Information from systematic zoology, conservation sciences, chemistry, forensic sciences, pathology, paleopathology, applied sciences like food industry, and most recent advances in digital imaging are put together in order to obtain a better understanding of which and possibly why mounting media and coverslip seals deteriorate, how slides can be salvaged, which studies may be necessary to identify a range of ideal mounting media, and how microscope studies can benefit from improvements in developmental biology and related fields. We also elaborate on confusing usage of concepts like that of maceration and of clearing. The chemical ingredients of a range of mounting media and coverslip seals are identified as much as possible from published data, but this information suffers in so far as the composition of a medium is often proprietary of the manufacturer and may vary over time. Advantages, disadvantages, and signs of deterioration are documented extensively for these media both from references and from our own observations. It turns out that many media degrade within a few years, or decades at the latest, except Canada balsam with a documented life-time of 150 years, Euparal with a documented life-time of 50 years, and glycerol-paraffin mounts sealed with Glyceel, which represents almost the only non-deteriorating and easily reversible mount. Deterioration reveals itself as a yellowing in natural resins and as cracking, crystallization, shrinkage on drying or possibly on loss of a plasticizer, detachment of the coverslip, segregation of the ingredients in synthetic polymers, as well as continued maceration of a specimen to a degree that the specimen virtually disappears. Confusingly, decay does not always appear equally within a collection of slides mounted at the same time in the same medium. The reasons for the deteriorative processes have been discussed but are controversial especially for gum-chloral media. Comparing data from conservation sciences, chemical handbooks, and documented ingredients, we discuss here how far chemical and physical deterioration probably are inherent to many media and are caused by the chemical and physical properties of their components and by chemicals dragged along from previous preparation steps like fixation, chemical maceration, and physical clearing. Some recipes even contain a macerating agent, which proceeds with its destructive work. We provide permeability data for oxygen and water vapor of several polymers contained in mounting media and coverslip seals. Calculation of the penetration rate of moisture in one example reveals that water molecules reach a specimen within a few days up to about a month; this lays to rest extensive discussions about the permanent protection of a mounted specimen by a mounting medium and a coverslip seal. Based on the ever growing evidence of the unsuitable composition and application of many, and possibly almost all, mounting media, we strongly encourage changing the perspective on microscope slides from immediate usability and convenience of preparation towards durability and reversibility, concepts taken from conservation sciences. Such a change has already been suggested by Upton (1993) more than 20 years ago for gum-chloral media, but these media are still encouraged nowadays by scientists. Without a new perspective, taxonomic biology will certainly lose a large amount of its specimen basis for its research within the next few decades. Modern non-invasive techniques like Raman spectroscopy may help to identify mounting media and coverslip seals on a given slide as well as to understand ageing of the media. An outlook is given on potential future studies. In order to improve the situation of existing collections of microscope slides, we transfer concepts as per the Smithsonian Collections Standards and Profiling System, developed for insect collections more than 25 years ago, to collections of slides. We describe historical and current properties and usage of glass slides, coverslips, labels, and adhesives under conservational aspects. In addition, we summarize and argue from published and our own experimental information about restorative procedures, including re-hydration of dried-up specimens previously mounted in a fluid medium. Alternatives to microscope slides are considered. We also extract practical suggestions from the literature concerning microscope equipment, cleaning of optical surfaces, health risks of immersion oil, and recent improvements of temporary observation media especially in connection with new developments in digital software. KW - Re-hydration KW - Mounting medium KW - Coverslip seal KW - Fixation KW - Maceration KW - Clearing KW - Immersion oil KW - Permeability PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-423322 SN - 978-1-77670-222-0 SN - 978-1-77670-223-7 DO - https://doi.org/10.11646/zootaxa.4322.1.1 SN - 1175-5326 VL - 4322 IS - 1 SP - 1 EP - 173 PB - Magnolia Press CY - Auckland, Neuseeland AN - OPUS4-42332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lichtenstein, D. A1 - Meyer, T. A1 - Böhmert, L. A1 - Juling, S. A1 - Fahrenson, C. A1 - Selve, S. A1 - Thünemann, Andreas A1 - Meijer, J. A1 - Estrela-Lopis, I. A1 - Braeuning, A. A1 - Lampen, A. T1 - Dosimetric quantification of coating-related uptake of silver nanoparticles N2 - The elucidation of mechanisms underlying the cellular uptake of nanoparticles (NPs) is an important topic in nanotoxicological research. Most studies dealing with silver NP uptake provide only qualitative data about internalization efficiency and do not consider NP-specific dosimetry. Therefore, we performed a comprehensive comparison of the cellular uptake of differently coated silver NPs of comparable size in different human intestinal Caco-2 cell-derived models to cover also the influence of the intestinal mucus barrier and uptake-specialized M-cells. We used a combination of the Transwell system, transmission electron microscopy, atomic absorption spectroscopy, and ion beam microscopy techniques. The computational in vitro sedimentation, diffusion, and dosimetry (ISDD) model was used to determine the effective dose of the particles in vitro based on their individual physicochemical characteristics. Data indicate that silver NPs with a similar size and shape show coating-dependent differences in their uptake into Caco-2 cells. The internalization of silver NPs was enhanced in uptake-specialized M-cells while the mucus did not provide a substantial barrier for NP internalization. ISDD modeling revealed a fivefold underestimation of dose–response relationships of NPs in in vitro assays. In summary, the present study provides dosimetry-adjusted quantitative data about the influence of NP coating materials in cellular uptake into human intestinal cells. Underestimation of particle effects in vitro might be prevented by using dosimetry models and by considering cell models with greater proximity to the in vivo situation, such as the M-cell model. KW - Silver nanoparticles KW - Small-angle X-ray scattering KW - Saxs PY - 2017 DO - https://doi.org/10.1021/acs.langmuir.7b01851 SN - 0743-7463 VL - 33 IS - 45 SP - 13087 EP - 13097 PB - Americal Chemical Society AN - OPUS4-42875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hupatz, H. T1 - Deposition of redox-switchable rotaxanes on surfaces N2 - Deposition of Redox-switchable rotaxanes on surfaces Nature has created molecular machines which can perform a variety of different tasks. They exhibit defined operational pathways and order, resulting in directed macroscopic effects. Within the last decades researchers have been developing numerous artificial molecular machines which are so far mostly operating in solution. However, this represents a major obstacle for the generation of a macroscopic output, due to the random orientation of molecules in solution. As a general approach to this problem, interfaces have been used to generate ordered arrays of functional molecules. Recently, we developed a new class of redox-switchable crown ether/ammonium-based [2]- and [3]rotaxanes which incorporate redox-active tetrathiafulvalene and naphthalene diimide units in their wheels resulting in emergent optoelectronic properties. Electrochemical stimuli influence the interactions between the two macrocycles of [3]rotaxanes and induce conformational changes. In a proof-of-principle study [2]pseudorotaxanes were deposited on gold surfaces by “click”-reaction to azide-terminated self-assembled monolayers to generate ordered arrays of redox-active rotaxanes on-surface. X-ray photoelectron spectroscopy (XPS) confirms the successful deposition of a rotaxane monolayer, though angle-resolved near-edge X-ray absorption fine structure spectroscopy (NEXAFS) exhibits poor order of the rotaxanes. Following, new terpyridine-stoppered rotaxanes will be synthesised opening a pathway for the deposition of [2]- and [3]rotaxanes in a layer-by-layer metal-mediated self-assembly procedure. This approach would allow for a programmed sequence of different rotaxanes in multilayers. Electrochemical on-surface switching will be investigated by angle-resolved NEXAFS spectroscopy, XPS, cyclic voltammetry and UV/Vis spectroscopy. A more detailed understanding of the electron-transfer between the surface and the different rotaxane layers as well as of the on-surface switching could give rise to potential applications like optoelectric data-storage devices or potential-driven molecular motors. T2 - Gordon Research Conference - Artificial Molecular Switches & Motors CY - Holderness, NH, USA DA - 11.06.2017 KW - Rotaxane KW - Immobilization KW - XPS KW - NEXAFS PY - 2017 AN - OPUS4-42843 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hupatz, H. T1 - Redox-Switchable Rotaxanes on Surfaces N2 - Nature has created molecular machines which can perform a variety of different tasks. They exhibit defined operational pathways and order, resulting in directed macroscopic effects. Within the last decades researchers have been developing numerous artificial molecular machines which are so far mostly operating in solution. However, this represents a major obstacle for the generation of a macroscopic output, due to the random orientation of molecules in solution. As a general approach to this problem, interfaces have been used to generate ordered arrays of functional molecules. Recently, we developed a new class of redox-switchable crown ether/ammonium-based [2]- and [3]rotaxanes which incorporate redox-active tetrathiafulvalene and naphthalene diimide units in their wheels resulting in emergent optoelectronic properties. Electrochemical stimuli influence the interactions between the two macrocycles of [3]rotaxanes and induce conformational changes. In a proof-of-principle study [2]pseudorotaxanes were deposited on gold surfaces by “click”-reaction to azide-terminated self-assembled monolayers to generate ordered arrays of redox-active rotaxanes on-surface. X-ray photoelectron spectroscopy (XPS) confirms the successful deposition of a rotaxane monolayer, though angle-resolved near-edge X-ray absorption fine structure spectroscopy (NEXAFS) exhibits poor order of the rotaxanes. Following, new terpyridine-stoppered rotaxanes will be synthesised opening a pathway for the deposition of [2]- and [3]rotaxanes in a layer-by-layer metal-mediated self-assembly procedure. This approach would allow for a programmed sequence of different rotaxanes in multilayers. Electrochemical on-surface switching will be investigated by angle-resolved NEXAFS spectroscopy, XPS, cyclic voltammetry and UV/Vis spectroscopy. A more detailed understanding of the electron-transfer between the surface and the different rotaxane layers as well as of the on-surface switching could give rise to potential applications like optoelectric data-storage devices or potential-driven molecular motors. T2 - GDCh-Wissenschaftsforum Chemie CY - Berlin, Germany DA - 10.09.2017 KW - NEXAFS KW - Rotaxane KW - XPS KW - Surface characterization PY - 2017 AN - OPUS4-42848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Helmerich, Rosemarie T1 - Active thermography N2 - Active thermography is introduced as tool for diagnostics in civil engineering structures. Aside from basic information, examples for applications of active thermography in different types of structures was presented. Active thermography was applied in historic structures to reveal former components or even ancient openings. Other examples present active thermography as a tool for nondestructive detection of debonding in CFRP strengthened structures. The way is explained, how the system was optimized for different materials. T2 - NDT&E Advanced Training Workshop CY - Berlin, Germany DA - 05.07.2017 KW - Active thermography KW - Strengthening KW - Nondestructive testing KW - Civil structures PY - 2017 AN - OPUS4-42920 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jemian, P. T1 - NXcanSAS: standard to store reduced SAS data of any dimension N2 - The communication of experimental results is common to scientific investigation. The method of presentation varies widely across investigation technique, and may stymie fundamental scientific goals such as sharing of results and replication of experiments. Even within a limited community, such as small-angle scattering, the choice of how to organize stored information is fragmented, with the result that often, the data are deposited in ad hoc form. To increase access to data produced from publicly-funded research, funding agencies are now requiring that proposals describe how data will be made available. With the increases in data volume due to higher-efficiency collection, increased experimental complexity, and larger and faster detectors, the plethora of ad hoc formats is a burden to the scientific community. Reliance on a few, well-considered standards facilitates automated processes for analysis and correlation of scientific data. Furthermore, it leads to development of common tools for data visualization and analysis, and data catalogues for access, reference, and data mining. The Worldwide Protein Data Bank is such an example where, by the provision of a standardized data format, scientific data and metadata from a vast range of methods has become available for research on the structures of proteins. Guidelines for structural modelling of smallangle scattering data from biomolecules in solution were adopted by the IUCr Commission on Small-Angle Scattering in 2012. NXcanSAS is a standard to store reduced small-angle scattering data of any dimension. It is sufficiently general that it may be used for any form of reduced SAS data in different scientific applications. The hierarchical structure of the canSAS (http://www.cansas.org) standard has been designed within the NeXus (http://www.nexusformat.org) data format. This presentation will describe the NXcanSAS standard, underlying concepts, and will give some examples. T2 - 24th Congress and General Assembly of the International Union of Crystallography CY - Hyderabad, India DA - 21.08.2017 KW - Small-angle scattering KW - Data standard KW - NeXus KW - Archival format PY - 2017 AN - OPUS4-42917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik T1 - Novel thermographic methods for non-destructive testing using structured illumination N2 - Photothermal imaging is commonly used for the characterization of material properties, the determination of layer thicknesses or the detection of inhomogeneities such as voids or cracks. For this purpose, the solid specimen is externally heated, e.g. by using a light source. The resulting transient heat flows interact with the inner structures of the specimen, which in turn is measured as a transient temperature distribution at the surface. Novel array-shaped, high-power laser light sources allow to control the heating of the surface arbitrarily, both temporally and spatially. This enables us to shape the heat flows within the material in a very specific way. In a first application, we demonstrate how to apply destructively interfering thermal wave fields in order to detect subsurface defects with a very high sensitivity. A similar technique, although originating from a very different physical domain, is already in use for medical 3D imaging showing the high potential of this approach. T2 - Adlershofer For­schungs­forum 2017 CY - Berlin, Germany DA - 10.11.2017 KW - Active thermography KW - Photothermal KW - Crack detection KW - Thermal wave KW - Structured heating PY - 2017 AN - OPUS4-42835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumacher, David A1 - Ewert, Uwe A1 - Zscherpel, Uwe T1 - Influencing parameters on image quality using photon counting detectors for laminography N2 - Classical film radiography is a well-established NDT technique and it is most commonly used for testing weld seams and corroded pipes e.g. in oil and gas industry or in nuclear power plants. In the course of digitization, digital detector arrays (DDA) are finding their way into industrial applications and are replacing film radiography step by step. This study deals with the latest generation of DDAs, the photon counting and energy resolving detectors (PCD), and their characteristics compared to charge integrating detectors (CID). No matter which technology to use, radiography still lacks a general issue: A three-dimensional object is projected onto a two dimensional image. Of course, advanced computed tomography (CT) algorithms exist since many years, but if the object to investigate is too large to fit into the manipulation system or its shape is not appropriate, CT is not feasible or sensible to be applied. To overcome this limitation, numerous laminographic algorithms have been developed in the past. In this study, photon counting detectors are used in combination with co-planar translational laminography to gain reconstructed three-dimensional volumes. Both laminographic testing and PCDs require a serious knowledge of many parameters that can influence the image quality in the resulting datasets. These are e.g. the detector efficiency and calibration procedure, setting of energy thresholds, exposure data, number of projections, beam length correction and spatial resolution. The use of PCDs yields more variables to be considered compared to CIDs. The most important parameters in laminographic testing and in the use of PCDs are described in this study and limits are discussed. T2 - 7th European-American Workshop on Reliability of NDE CY - Potsdam, Germany DA - 05.09.2017 KW - X-ray imaging KW - Digital radiography KW - Co-planar translational laminography KW - Reliability KW - Photon counting detectors PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-428912 UR - http://www.nde-reliability.de/portals/nde17/BB/31.pdf SP - Paper 31, 1 EP - 11 AN - OPUS4-42891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pignatelli, Giuseppe T1 - Effects of nanoparticles on laser ablation N2 - Introduction: Laser Induced Breakdown Spectroscopy (LIBS) is an atomic emission analytical technique, wide spreading in laboratories and industries. One way to dramatically increase its analytical results is to deposit metal NPs on the sample surface, resulting in an better version called Nanoparticle Enhanced LIBS (NELIBS). In order to better know and use this technique, the evolution of the plasma has been studied with Tomography. T2 - CHESS 2017 CY - Florence, Italy DA - 27.11.2017 KW - LIBS KW - Nanoparticles PY - 2017 AN - OPUS4-43476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Advanced codicology: including instrumental analysis into N2 - Investigation of physical properties and chemical composition of writing materials generates important data that we add to the results of the codicological analysis of the manuscripts. In its individual materiality, each manuscript is the result of a wide variety of influences. The “life” of a manuscript starts with its production that includes preparation of the writing surfaces and inks; it is followed by the use and storage, and finally characterized by treatment during restoration. Using instrumental analysis we record the characteristics that still exist. Combining our data with those obtained from the palaeographical and codicological analysis produces a new powerful tool for reconstruction of the history of a manuscript. T2 - Manuscripts East and West – Towards Comparative and General Codicology CY - Hamburg, Germany DA - 17.10.2017 KW - Ink KW - Hebrew manuscripts PY - 2017 AN - OPUS4-43479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Ultrasonic Inspection and Data Analysis of Glass- and Carbon-Fibre-Reinforced Plastics N2 - Non-destructive testing (NDT) helps to find material defects without having an influence on the material itself. It is applied as a method of quality control, for online structural health monitoring, and for inspection of safety related components. Due to the ability of automation and a simple test setup ultrasonic testing is one major NDT technique next to several existing options. Whereas contact technique allows the use of higher frequencies of some MHz and phased array focusing, air-coupled ultrasonic testing (ACUT) shows different advantages. Most significant for ACUT is the absence of any coupling fluid and an economical test procedure respective time and costs. Both contact technique and ACUT have been improved and enhanced during the past years. One important enhancement is the development of airborne transducers based on ferroelectrets, like charged cellular polypropylene (cpp), which makes the application of any matching layers being mandatory in conventional piezoelectric transducers unnecessary. In this contribution we show ultrasonic inspection results of specimens made of carbon- and glass-fibre-reinforced plastic. These specimens include defects represented by drill holes and artificial delaminations of various size and depth. We compare inspection results achieved by using contact technique to those achieved by ACUT. For ACUT, conventional piezoelectric transducers and transducers based on cpp were used, both focused as well as non-focused types. Contact inspections were performed with a multi-channel matrix array probe. Once the inspection data is recorded it can be analysed in order to detect and evaluate defects in the specimen. We present different analysing strategies and compare these regarding detection rate and sizing of defects. T2 - 3rd International Symposium on Fatigue Design and Material Defects, FDMD 2017 CY - Lecco, Italy DA - 19.09.2017 KW - Ultrasonic testing KW - Air-coupled KW - Carbon-fibre-reinforced plastic KW - Glass-fibre-reinforced KW - Defect sizing KW - Material inspection PY - 2017 AN - OPUS4-43482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waiblinger, H. U. A1 - Bartsch, D. A1 - Brockmeyer, J. A1 - Bruenen-Nieweler, C. A1 - Busch, U. A1 - Haase, I. A1 - Hahn, A. A1 - Haarmann, M. A1 - Hauser, W. A1 - Huber, I. A1 - Jany, K. D. A1 - Kirmse, N. A1 - Lindeke, S. A1 - Neumann, K. A1 - Naumann, H. A1 - Paschke, A. A1 - Pietsch, K. A1 - Pöpping, B. A1 - Reiting, R. A1 - Schroeder, U. A1 - Schwägele, F. A1 - Weller, Michael G. A1 - Zagon, J. T1 - Methods of differentiating animal species in food - Status quo N2 - In the field of animal species differentiation, work on standardizing methods has been intensified in Germany in recent years, not least due to the horsemeat scandal in 2013. Even though there are now hardly ever any positive findings anymore in examinations to detect horse adulterations in foods such as lasagne, animal species differentiation altogether ranks high in detecting adulteration of foods. This article, therefore, summarises the current status of analytical techniques used in Germany with standardization at German level. It has been established by the working group "Biochemical and Molecular Biological Analytics" of the Lebensmittelchemische Gesellschaft (Food Chemistry Society within the German Chemical Society) with support of experts in the working group “Molecular biology techniques for differentiating plant and animal species" (§64 of the German Food and Feed Code - LFGB) and the "Immunology and molecular biology" task force of the food hygiene and food of animal origin working group (ALTS), both from Germany. KW - Animal species differentiation KW - Fish species KW - PCR KW - ELISA KW - LC-MS/MS PY - 2017 IS - 3 SP - 29 EP - 36 PB - Deutscher Fachverlag GmbH CY - Frankfurt am Main AN - OPUS4-43485 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kästner, Claudia T1 - Highly enhanced catalytic activity of silver N2 - Silver nanoparticles are one of the most widespread consumer related nanoparticles worldwide. Since the particles show special optical and antibacterial properties they are used for a wide range of applications from biological investigations over medical applications and catalysis. Especially the outstanding question of applicable alternatives for catalysts in diverse reactions can be addressed with the design of versatile system of small silver nanoparticles. In this study we present the synthesis and application of ultra-small silver nanoparticles with a narrow size distribution (R = 3.1 nm, σ = 0.6 nm). The particles are thoroughly characterized by small angle X-ray scattering, dynamic light scattering and UV/Vis spectroscopy. As a representative test reaction the reduction of 4-nitrophenol to 4-aminophenol was chosen. The particles show a catalytic activity of (436 ± 24) L g-1 s-1, which is two orders of magnitude higher than for other silver particles in the literature. The particles surrounding shell, composed of poly(acrylic acid), provides the particles with a good accessibility for the reactants. Since the catalytic activity strongly depends on the surrounding ligand, the particles shell can also be exchanged by other ligands enabling a tuning of the catalytic activity to a desired value. This shows the high flexibility of this system which can also be applied for other catalytic reactions. T2 - 5th Nano Today Conference CY - Waikoloa Village, HI, USA DA - 06.12.2017 KW - SAXS KW - Catalysis KW - Silver nanoparticles KW - Reduction 4-nitrophenol PY - 2017 AN - OPUS4-43496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - Do non-thermal effects exist? - Microwave-assisted acceleration of silver nanoparticle synthesis and particle growth N2 - Ever since increasing a reaction’s yield while shortening the reaction time is the main objective in synthesis optimization. Microwave reactors meet these demands. In literature however their usage is under discussion due to claims of the existence of non-thermal effects resulting from the microwave radiation. Especially for nano-material syntheses it is of crucial importance to be aware of influences on the reaction pathway. Therefore, we compare ultra-small silver nanoparticles with mean radii of 3 nm, synthesized via conventional and microwave heating. We employed a versatile one-pot polyol synthesis of poly(acrylic acid) (PAA) stabilized silver nanoparticles, which display superior catalytic properties. No microwave specific effects in terms of particle size distribution characteristics, as derived by small-angle X-ray scattering (SAXS) and dynamic light scattering (DLS), are revealed. Due to the microwave reactor’s characteristics of a closed system, syntheses can be carried out at temperatures beyond the solvent’s boiling point. Particle formation was accelerated by a factor of 30 by increasing the reaction temperature from 200 °C to 250 °C. The particle growth process follows a cluster coalescence mechanism. A post-synthetic incubation step at 250 °C induces a further growth of the particles while the size distribution broadens. Thus, utilization of microwave reactors enables an enormous decrease of the reaction time as well as the opportunity of tuning the particles’ size. Possibly, decomposition of the stabilizing ligand at elevated temperatures results in reduced yields. A temperature of 250 °C and a corresponding reaction time of 30 s represent a compromise between short reaction times and high yields. T2 - 5th Nano Today Conference CY - Waikoloa Village, HI, USA DA - 06.12.2017 KW - Microwave synthesis KW - Small-angle scattering KW - Silver nanoparticles PY - 2017 AN - OPUS4-43497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kästner, Claudia T1 - What does your gut see? – Silver nanoparticles in an artificial digestion N2 - Over the last decade nanoparticles are progressively included in products of our daily life. Due to their antimicrobial properties, silver nanoparticles are used in a high variety of consumer products ranging from food containers over medicine and textiles. Therefore, research on the toxicological potential of nanosilver becomes increasingly important. This includes investigations concerning uptake, distribution and excretion of the particles. However, little attention was paid to changes of physical and chemical properties of the particles in the human body. One of the most important questions is if the particles can pass the digestion process without altering their shape and size. In this study we report on a versatile system of ultra-small silver nanoparticles with a mean volume weighted radius of 3.1 nm and a narrow size distribution width of 20%. The nanoparticles’ coating of poly (acrylic acid) can easily be exchanged by biocompatible ligands like albumin or glutathione. The particles are thoroughly characterized by small angle X-ray scattering (SAXS), DLS, IR and UV/Vis spectroscopy. We used the particles in an artificial digestion procedure which mimics the gastro-intestinal passage (Figure 1). Thereby the changes in the size distribution during the digestion process were analytically monitored by SAXS. Additionally, we used as food components oil, starch, skimmed milk powder and mixture thereof to provide a preferably realistic environment. Large aggregates of up to 56 nm were formed in the absence of food additives. In contrast, the presence of oil and starch limit the radii of aggregates to about 10 nm. Milk powder shows strong protective properties resulting in only small aggregates of 6 nm radii. Our results indicate that silver can indeed pass the digestion process in a nanoscale form depending on the nanoparticle coating and additional ingredients. These results have an impact on future toxicological considerations regarding silver nanoparticle-containing consumer products. T2 - 5th Nano Today Conference CY - Waikoloa Village, HI, USA DA - 06.12.2017 KW - SAXS KW - Artificial digestion KW - Silver nanoparticles KW - Food additives PY - 2017 AN - OPUS4-43499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulla, Hannes T1 - In situ PXRD monitoring of a mechanochemical cocrystal formation in milling jars of different material N2 - We present an in situ PXRD investigation of the mechanochemical cocrystal formation of pyrazinamide with pimelic acid in two milling jar materials. In the steel jar a polymorph transformation presenting an exception of Ostwald’s rule of stages is observed. T2 - BESSY User Meeting 2017 CY - Bessy II (HZB), Berlin, Germany DA - 14.12.2017 KW - In situ KW - XRD KW - Polymorph KW - Cocrystal KW - Milling PY - 2017 AN - OPUS4-43502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Fischer, Daniel T1 - Charakterisierung von dotierten Zinnoxidschichten für die Detektion von Gasen durch ellipsometrische Messung der Oberflächenplasmonenresonanz N2 - In der vorliegenden Dissertation wird die Verbesserung von Gassensoren durch Beschichtung mit dotierten Zinnoxidschichten untersucht, wobei zur Messung der Gase die Methode der oberflächenplasmonenresonanzverstärkten Ellipsometrie (SPREE) angewendet wurde. Die vorgestellten Ergebnisse unterteilen sich dabei in drei Schritte: Herstellung der Schichtsysteme, Analyse der chemischen, strukturellen und optischen Eigenschaften, sowie die Anwendung in der SPREE Gasmessung. Die dotierten Zinnoxidschichten wurden erfolgreich mittels Hochfrequenz-Magnetronsputtern hergestellt, indem das Zinnoxidtarget mit dem metallischen Dotierungsmaterial (Eisen bzw. Nickel) modifiziert wurde. Die chemische Analyse der Schichten wurde mit energiedispersiver Röntgenspektroskopie (EDX), Flugzeit-Sekundärionenmassenspektrometrie (TOF-SIMS) und Röntgenfluoreszenz unter streifendem Einfall (GI-XRF) durchgeführt. Die EDX Untersuchungen zeigten qualitativ, dass das Dotierungsmaterial in die Schicht eingebaut wurde. Mithilfe der TOF-SIMS Experimente konnte nachgewiesen werden, dass die Dotierungskonzentration innerhalb der Schicht heterogen verteilt ist und mithilfe der GI-XRF Messung konnte der Dotierungsgrad quantitativ mit ca. 10% bestimmt werden. Für die strukturelle Untersuchung wurden die Methoden der Rasterkraftmikroskopie (AFM) und Transmissionselektronenmikroskopie (TEM) ausgewählt. Die AFM Messungen zeigten, dass die Schichten eine mittlere quadratische Rauheit kleiner als 1 nm aufweisen und die Rauheit damit nicht als Faktor in der Gasmessung berücksichtigt werden muss. In den TEM Messungen wurde der Schichtaufbau bestätigt und gezeigt, dass in den dotierten Schichten nanokristalline Strukturen vorliegen. Die optische Charakterisierung der Schichten wurde mit spektraler Ellipsometrie (SE) durchgeführt, um die dielektrische Funktion in Abhängigkeit der Dotierung zu untersuchen. Dafür wurden Modelle für die dielektrische Funktion auf der Basis von mehreren Gauss-Funktionen entwickelt. Es zeigte sich, dass die undotierten Schichten sich wie typische Dielektrika mit Bandkanten >4 eV verhält und mit drei Gauss-Funktionen simuliert werden kann. Für die dotierten Schichten verschiebt sich die Bandkante, in Abhängigkeit vom Grad der Dotierung und dem Oxidationsgrad, zu bis zu 2.1 eV. Außerdem muss das Modell um eine zusätzliche Gauss-Funktion im nahen Infrarot erweitert werden, die auf die Anwesenheit von metallischen Nanopartikeln zurückzuführen ist. Weiterhin zeigte sich, dass die dielektrischen Eigenschaften von der Dicke der Schicht abhängen. Die Benutzung der Zusatzschichten in der SPREE Gasmessung zeigte, dass diese Schichten die Sensoroberfläche effektiv vor Degradation schützt. Weiterhin wurde nachgewiesen, dass die Sensitivität der jeweiligen Sensorschicht für bestimmte Gase von der Dotierung der Schicht abhängt. Es wurde gezeigt, dass eine Eisendotierung zu einer erhöhten Sensitivität für Kohlenmonoxid führt, während undotierte Schichten vor allem unpolare Alkane bevorzugen. Die Nickel-dotierten Schichten zeigten im Vergleich zur Eisendotierung deutlich schlechtere Ergebnisse für alle Gase. Diese Effekte wurden auf die unterschiedliche Bindungsstärke der Gase an die metallischen Nanopartikel und das Vorhandensein einer unterschiedlichen Zahl an Adsorptionsplätzen zurückgeführt. Für Wasserstoff wurden für alle Proben vergleichbare Ergebnisse gefunden, was darauf zurückzuführen ist, dass diese Moleküle aufgrund der geringen Größe und Masse in die Schicht diffundieren. Zusätzlich wurde das SPREE Verfahren signifikant verbessert, indem die Druckabhängigkeit Sensoren erstmals erfasst wurde. Weiterhin wurde die Auswertung weiterentwickelt, indem nur einzelne Parameter des Stokes-Vektors für die Gasmessung benutzt wurden. KW - Oberflächenplasmonen KW - Ellipsometrie KW - Transparente Halbleiter KW - Dotiertes Zinnoxid KW - Gasmessung PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435039 DO - https://doi.org/10.14279/depositonce-5969 SP - 1 EP - 154 PB - Technische Universität CY - Berlin AN - OPUS4-43503 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique A1 - Chapartegui, Ander T1 - Alcoholism clinical biomarkers and mass spectrometry N2 - Heavy alcohol induces several chronic diseases, including cirrhosis. Consequently, cirrhotic patients need liver transplantation. However, alcoholic patients are not suitable for this. How can be physicians sure of non-alcohol consumption of a potential organ receptor? Monitoring of biomarkers by mass spectrometric techniques is today the most suitable option. This subject was discussed at the Graduate School of Analytical Science Adlershof (SALSA) in Berlin, as a part of a lecture series in analytical science. T2 - Analytical Challenges - School of Analytical Sciences Adlershof CY - Berlin, Germany DA - 12.12.2017 KW - Alcoholism KW - Biomarkers KW - Mass spectrometry KW - Transferrin PY - 2017 AN - OPUS4-43535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kormunda, M. T1 - Study of magnetron sputtering deposited ultrathin FeSnOx films for Surface Plasmon Resonance sensors towards gas sensing applications N2 - In this study, series of coatings with the goal of sensitising gold SPR sensors towards CO, NH4, etc. were prepared. To better understand the mechanism behind the sensitizing effect and to enable the targeted production of optimized layers, the wide range of coatings was studied by multiple methods from spectroscopic ellipsometry for their dielectric function, by XPS for chemical composition and SEM, TEM to determine their microscopic structure. The coatings were deposited at inert Ar gas and reactive Ar/O2 gas mixture by RF magnetron sputtering or DC pulsed magnetron sputtering with settable RF bias on the substrates. The plasma processes were monitors by mass spectrometry. The metal oxide coatings in SPR sensors have to be prepared reproducible with thickness about 5 nm therefore lower deposition rate conditions were advantages. T2 - THE 14th INTERNATIONAL SYMPOSIUM ON SPUTTERING & PLASMA PROCESSES,ISSP 2017 CY - Kanazawa, Japan DA - 05.07.2017 KW - Surface Plasmon Resonance KW - Magnetron sputtering KW - FeSnOx PY - 2017 AN - OPUS4-43536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - New approaches in isotope analysis - molecular absorption spectrometry N2 - Variations in the isotope amount composition of some elements like lithium, boron, magnesium, calcium and copper have been used as proof of provenance of a sample and to describe geological processes. Routinely, isotope compositions are determinate by mass spectrometry; the working horse of the isotope analysis. However, mass spectrometric methods are expensive, time consuming and they require a high qualified analysist. Here an alternative faster and low cost optical method for isotope ratio determination is proposed: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Stable isotope amount composition of X= Li, B, Mg, Ca, Cu and Sr have been determined by monitoring the absorption spectrum of their monohydride (XH) in graphite furnace HR-CS-MAS. T2 - Seminar at Princeton University CY - Princeton, NJ, USA DA - 16.10.2017 KW - Isotope KW - High-Resolution Continuum Source Molecular Absorption Spectrometry KW - HR-CS-MAS KW - Isotopic shift KW - Graphite furnace KW - Isotope ratio PY - 2017 AN - OPUS4-43538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kormunda, M. T1 - Study of magnetron sputtering deposited ultrathin FeSnOx films for Surface Plasmon Resonance sensors towards gas sensing applications N2 - In this study, series of coatings with the goal of sensitising gold SPR sensors towards CO, NH4, etc. were prepared. To better understand the mechanism behind the sensitizing effect and to enable the targeted production of optimized layers, the wide range of coatings was studied by multiple methods from spectroscopic ellipsometry for their dielectric function, by XPS for chemical composition and SEM, TEM to determine their microscopic structure. The coatings were deposited at inert Ar gas and reactive Ar/O2 gas mixture by RF magnetron sputtering or DC pulsed magnetron sputtering with settable RF bias on the substrates. The plasma processes were monitors by mass spectrometry. The metal oxide coatings in SPR sensors have to be prepared reproducible with thickness about 5 nm therefore lower deposition rate conditions were advantages. T2 - THE 14th INTERNATIONAL SYMPOSIUM ON SPUTTERING & PLASMA PROCESSES,ISSP 2017 CY - Kanazawa, Japan DA - 05.07.2017 KW - Surface Plasmon Resonance KW - Magnetron sputtering KW - FeSnOx PY - 2017 AN - OPUS4-43539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Rauscher, H. A1 - Mech, A. A1 - Gaillard, C. A1 - Stintz, M. A1 - Wohlleben, W. A1 - Weigel, St. A1 - Ghanem, A. A1 - Hodoroaba, Vasile-Dan A1 - Babick, F. A1 - Mielke, Johannes T1 - Recommendations on a revision of the EC definition of nanomaterial based on analytical possibilities; updated N2 - In October 2011 the European Commission (EC) published a "Recommendation on the definition of na-nomaterial" (2011/696/EU), to promote consistency in the interpretation of the term "nanomaterial" for legislative and policy purposes in the EU. The EC NM Definition includes a commitment to its review in the light of experience and of scientific and technological developments. This review is ongoing in 2017 and as a contribution to the review the Joint Research Centre of the European Commission (JRC) has already developed a series of three scientific-technical reports with the title: “Towards a review of the EC Recommendation for a definition of the term nanomaterial” which provides to the EC policy services sci-ence-based options on how the definition could be revised or supported with additional guidance. The overarching nature and wide scope of the EC NM Definition, as it does not exclude a priori any particulate material regardless the state, form and size, creates many analytical challenges in its imple-mentation for all stakeholders, including enterprises and regulators. The NanoDefine project has as core objective to support the implementation of the EC NM Definition. In an earlier report1 key aspects of the EC NM Definition were addressed, with the goal to improve the implementability of the EC NM Definition. Based on further developments and results obtained in NanoDefine project that first report was updated and is presented here. The key aspects are discussed based on the results of four years of research performed within the framework of the project. As a result this report assesses how well the requirements of the EC NM Definition can be fulfilled with currently available analytical possibilities. It presents recommendations and options on a revision of the EC NM Definition to improve the implementability of the definition based on currently available analytical possi-bilities, according to the state of the art in 2017. Of the technical issues considered in this report, the following seem to deserve the most attention in terms of clarification of the definition and/or provision of additional implementation guidance: 'external dimension', ‘number based particle size distribution‘, ‘polydispersity‘ and ‘upper size limit‘, the term ‘particle’, the ‘means to prove that a material is not a nanomaterial‘ and ‘the role of the volume specific sur-face area (VSSA)‘, and "particulate materials'. KW - EU definition of a nanomaterial KW - Nanoparticles KW - Revision KW - Update 2017 PY - 2017 UR - http://www.nanodefine.eu/index.php/nanodefine-publications/nanodefine-technical-reports SP - D7.10, 1 EP - D7.10, 71 PB - The NanoDefine Consortium CY - Wageningen, The Netherlands AN - OPUS4-43540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Maiwald, Michael ED - Maiwald, Michael T1 - Validation report on NMR N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug and play integration, even though they may appear to be more complex at first sight. Smart sensors enable concepts like self-diagnostics, self-calibration, and self-configuration/ parameterization whenever our current automation landscape allows it. Here we summarize the currently discussed general requirements for process sensors 4.0 and introduce a smart online NMR sensor module as example, which was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (www.consensspire.eu). KW - Process Monitoring KW - Online NMR Spectroscopy KW - Indirect Hard Modeling KW - Process Control KW - Process Analytical Technology KW - CONSENS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435521 SP - 1 EP - 31 AN - OPUS4-43552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Licht ins Dunkle - In situ Untersuchungen mechanochemischer Reaktionen N2 - Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals. The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms. We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In this contribution, I will discuss our recent results investigating the formation of (polymorphic) cocrystals and metal phosphonates. First investigations of a mechanochemical synthesis under controlled temperature which allow determining the activation barrier are presented. Furthermore, in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat.5 Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds. T2 - PRORA Fachtagung Prozessnahe Röntgenanalytik CY - Berlin, Germany DA - 30.11.2017 KW - Mechanochemie KW - XRD KW - In situ PY - 2017 AN - OPUS4-43562 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical reactions - new insights in formation pathways N2 - Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals. The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms. We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases because of the reaction heat. Based on the data, temperature rises as postulated in the magma plasma and hot spot theory can be excluded for soft matter milling syntheses. Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds. T2 - Wissenschaftsforum Chemie CY - Berlin, Germany DA - 10.09.17 KW - Mechanochemistry KW - In situ PY - 2017 AN - OPUS4-43563 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Russina, M. A1 - Günther, G. A1 - Grzimek, V. A1 - Gainov, R. A1 - Drescher, L. A1 - Kaulich, T. A1 - Graf, W. A1 - Urban, B. A1 - Daske, A. A1 - Grotjahn, K. A1 - Hellhammer, R. A1 - Buchert, G. A1 - Kutz, H. A1 - Rossa, L. A1 - Sauer, O.-P. A1 - Fromme, M. A1 - Wallacher, D. A1 - Kiefer, K. A1 - Klemke, B. A1 - Grimm, N. A1 - Gerischer, S. A1 - Tsapatsaris, N. A1 - Rolfs, K. T1 - Upgrade project NEAT02016 at Helmholtz Zentrum Berlin – What can be done on the medium power neutron source N2 - The neutron time-of-flight spectrometer NEAT has a long history of successful applications and is best suited to probe dynamic phenomena directly in the large time domain 10(-14) - 10(-10) s and on the length scale ranging from 0.05 to up to about 5 nm. To address user community needs for more powerful instrumental capabilities, a concept of the full upgrade of NEAT has been proposed. The upgrade started in 2010 after a rigorous internal and external selection process and resulted in 300-fold neutron count rate increase compared to NEAT01995. Combined with new instrumental and sample environmental capabilities the upgrade allows NEAT to maintain itself at the best world class level and provide an outstanding experimental tool for a broad range of scientific applications. The advanced features of the new instrument include an integrated guide-chopper system that delivers neutrons with flexible beam properties: either highly homogeneous beam with low divergence suitable for single crystals studies or "hot-spot" neutron distribution serving best small samples. Substantial increase of the detector angle coverage is achieved by using 416 He-3 position sensitive detectors. Placed at 3m from the sample, the detectors cover 20m(2) area and are equipped with modern electronics and DAQ using event recording techniques. The installation of hardware has been completed in June 2016 and on January 23, 2017 NEAT has welcomed its first regular users who took advantage of the high counting rate, broad available range of incoming neutron wavelengths and high flexibility of NEAT. Here we present details of NEAT upgrade, measured instrument characteristics and show first experimental results. KW - Neutron scattering KW - Neutron spectroscopy KW - Instrumentation KW - Time-of-flight neutron spectroscopy KW - Nanoscale dynamics PY - 2017 DO - https://doi.org/10.1016/j.physb.2017.12.026 SN - 0921-4526 VL - 551 SP - 506 EP - 511 PB - Elsevier B.V. AN - OPUS4-43514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana T1 - Online NMR Spectroscopy for Process Monitoring in Intensified Continuous Production Plants N2 - Process analytical techniques are extremely useful tools for chemical production and manufacture and are of particular interest to the pharmaceutical, food and (petro-) chemical industries. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and relatively inexpensive analysers, which feature advantages like low cost, low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, sufficient robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. A major advantage of NMR spectroscopy is that the method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical comparison method which is independent of the matrix. This is an important prerequisite for robust data evaluation strategies within a control concept and reduces the need for extensive maintenance of the evaluation model over the time of operation. Additionally, NMR spectroscopy provides orthogonal, but complimentary physical information to conventional, e.g., optical spectroscopy. It increases the accessible information for technical processes, where aromatic-to-aliphatic conversions or isomerizations occur and conventional methods fail due to only minor changes in functional groups. As a technically relevant example, the catalytic hydrogenation of 2-butyne-1,4-diol and further pharmaceutical reactions were studied using an online NMR sensor based on a commercially available low-field NMR spectrometer within the framework of the EU project CONSENS (Integrated Control and Sensing). T2 - EuroPACT 2017 CY - Potsdam, Germany DA - 10.05.2017 KW - Process Monitoring KW - Online NMR Spectroscopy KW - Process analytical technology KW - Hydrogenation KW - Indirect Hard Modeling KW - CONSENS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435507 AN - OPUS4-43550 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Process monitoring of intensified continuous production units with compact NMR spectroscopy N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and inexpensive analysers, which feature advantages like low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. Otherwise there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Union’s Research Project CONSENS (www.consens-spire.eu) by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. The presented NMR module is provided in an explosion proof housing with a module size of 57 x 57 x 85 cm and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling (IHM) was selected for data analysis of the low-field NMR spectra. A set-up for monitoring continuous reactions in a thermostated 1/8” tubular reactor using automated syringe pumps was used to validate the IHM models by using high-field NMR spectroscopy as analytical reference method. T2 - Seminar, Institute of Technical Biocatalysis, Hamburg University of Technology CY - Hamburg, Germany DA - 13.01.2017 KW - Process monitoring KW - Online NMR spectroscopy KW - Indirect hard modeling KW - Process control KW - Process analytical technology KW - CONSENS PY - 2017 AN - OPUS4-43551 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Immunoanalytical Methods for Environmental, Food and Clinical Analysis N2 - The Short Course “Immunoanalytical Methods for Environmental, Food and Clinical Analysis” offers training in antibody-based analytical techniques. The course is suitable also for beginners. The Short Course comprises Lecture Units teaching the concepts, equipment, reagents and explains the protocols to be used in the practical part. Simple “Hands On” units are offered employing portable instrumentation. – The Short Course spans from antigen production, generation of antibodies, assay development and optimization, data evaluation to the different formats that have been developed. Examples are provided from the areas of environmental analysis (pharmaceuticals, hormones and anthropogenic markers in water and wastewater), food analysis (caffeine in beverages, mycotoxins) and clinical diagnostics (infarction biomarkers). The attendants will be enabled to select an appropriate method and to judge its applicability for their given analytical problem. T2 - Pittcon 2017 CY - Chicago, IL, USA DA - 07.03.2017 KW - FPIA KW - ELISA KW - LFIA KW - Immunoassays PY - 2017 AN - OPUS4-43521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beyer, Sebastian T1 - Colloidal metalorganic frameworks as novel biofunctional nanoparticles for immunoassay applications N2 - Metal-organic framework (MOF) colloids have unique features that render them ideal signalling agents for realizing advanced immunoassay-based detection systems. MOFs are porous coordination polymers of metal nodes and organic linkers. The pore size of MOFs can be engineered and tailored to allow specific host (MOF) and guest (analyte) interactions. The particle sizes of the colloidal MOF can be tailored by employing methods from colloidal chemistry in wet synthesis. The adaption of established Layer-by-Layer polyelectrolyte coating protocols [1] allows equipping colloidal MOF particles with a nanometer thin polyelectrolyte membrane. This polyelectrolyte membrane serves as an interface for antibody binding. These biofunctional MOF nanoparticles have shown a strong immuno-binding that is sufficient for solid state immunoassays. Our current research addresses the design of luminescence encoded colloidal particle libraries by adjusting the ratios of e.g. Terbium (green) and Europium (red) metal nodes in mixed lanthanide based MOF-76. These mixed lanthanide MOF-76 particles are envisioned to allow multiplexed immuno-detection of endocrine disruptors such as bisphenol A. In addition we investigate the detection of analytes that do not allow the production of antibodies due to their inherent properties. Such “difficult analytes” have a strong hydrophobicity or are very small or highly toxic molecules. One example is the common plasticizer dioctylphthalate that is also a potent endocrine disruptor. MOF colloids can address this issue by specific host (MOF) : guest (analyte) interactions that result in analyte-specific colour change or exciplex-based fluorescence emission. Our overall aim is to develop methodologies that allow parallel sensing of two endocrine disruptors (e.g. bisphenol A & phthalates) by simultaneous immuno-detection and MOF:analyte specific interactions. T2 - BioSensor 2017 - 1st European and 10th German BioSensor Symposium CY - Potsdam, Germany DA - 20.03.2017 KW - MOFs KW - Immunoassay KW - Nanoparticles PY - 2017 AN - OPUS4-43522 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Fluorescence polarization immunoassays - Comparison of platforms N2 - Immunoassays are in the majority of formats heterogeneous assays with one of the commodities – antibody or antigen – immobilized on a solid substrate or sometimes to nanoparticles or beads. All these formats require a washing step in order to separate bound from non-bound species before generating the measurement signal. Measuring fluorescence polarization is a method to distinguish between a fluorescent macromolecule and a low-molecular weight fluorophore. After irradiation of the sample with polarized light, a macromolecule like e.g. an antibody, will emit still highly polarized light (high polarization, resp. small difference in degree of polarization to the background). In a fluorescence polarization immunoassay, the fluorescence of an analyte surrogate (a fluorescence “tracer”) is followed. Depolarization is high and so the measured polarization is low. When antibody is added, the tracer is bound, depolarization decreases and the in polarization is high. Increasing amounts of analyte more and more impede the tracer being bound by the tracer and thus the decreases, the typical sigmoidal relationship is obtained (Fig. 1). We dispose of 5 polarization platforms reading in plate mode, strip mode and cuvette mode. One is able to register polarization changes with time and so allows for kinetic measurements another one is hand-held. We have been comparing FPIA formats before [1-4] and now a comprehensive view on sensitivities, the importance of fast vs. slow binding kinetics as well as the choice of format can be presented. T2 - BioSensor 2017 - 1st European and 10th German BioSensor Symposium CY - Potsdam, Germany DA - 20.03.2017 KW - FPIA KW - Immunoassay KW - Fluoreszenz PY - 2017 AN - OPUS4-43523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Strategien für das Screening und Monitoring nach anthropogenen Markern (anstatt nach prioritären Substanzen) N2 - Der Vortrag schildert Strategien für das Screening und Monitoring nach anthropogenen Markern in der Oberflächengewässeranalytik, anstatt nach prioritären Substanzen, wie sie beispielsweise die Beobachtungsliste zur Wasserrahmenrichtlinie auflistet, zu screenen. T2 - Anakon 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Anthropogene Marker KW - Immunoassay KW - ELISA KW - Koffein KW - Carbamazepin KW - Screeningverfahren KW - Monitoring PY - 2017 AN - OPUS4-43524 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aldrabee, A. A1 - Wriekat, A. A1 - Abu Saleem, K. A1 - Radtke, Martin T1 - Non-destructive SR-XRF analysis of ancient Mamluk-Ayyubid glazed pottery fragments from Karak Castle, Jordan N2 - Sixteen Ayyubid-Mamluk glazed pottery sherds were analyzed in order to identify and characterize the elemental composition to determine their provenance. The tested sherds were collected from the historical site of Karak Castle, southern Jordan. Chemical analysis for the sixteen samples has been carried out using Synchrotron Radiation X-ray Fluorescence Spectrometry (SR-XRF) Technique. Furthermore, the semiquantitative analysis of the elements Fe – Cu – Zn – Br – Rb – Sr – Y – Zr – Nb – Mo – Pd – Ag – Cd and Pb has been performed for the samples based on Principal Component Analysis (PCA) and hierarchical Cluster Analysis with Bray-Curtis in order to define grouping of different glazed pottery by obtaining information on their similarity and clustering. The results of chemical analysis provided persuasive evidence that the Karak Castle pottery sherds have at least three different sources of provenance. KW - BAMline KW - Karak Castle KW - Synchrotron KW - XRF PY - 2015 VL - 8 IS - 3 SP - 157 EP - 163 AN - OPUS4-43489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter T1 - Immunoanalytical Methods for Environmental, Food and Clinical Analysis: Immunomicroarrays N2 - This short course offers an introduction in immunomicroarrays and its application in environmental, food and clinical analysis. Basic principles of microarray fabrication, including spotting techniques and immobilization chemistry are presented, as well as different immunoassay formats and data treatment strategies. Furthermore, principles of bead-based suspension arrays are introduced, including principles of ligand and receptor immobilization, encoding and read-out strategies. T2 - Pittcon CY - Chicago, IL, USA DA - 05.03.2017 KW - Bead-based assay KW - Suspension arrays KW - Microarrays KW - Immunoanalytical methods KW - Multiplexing PY - 2017 AN - OPUS4-43490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Tobias T1 - Application of two calibration-free LIBS techniques N2 - Two calibration-free (CF) LIBS approaches are used for the quantitative analysis of cement samples: the CF-LIBS based on the Boltzmann plot method and the Monte Carlo (MC) LIBS based on the iterative spectrum fitting. In CF-LIBS, the inverse problem is solved, i.e. the elemental concentrations are determined by the reconstruction of plasma parameters from spectra. The MC-LIBS technique solves the direct problem by finding the highest correlation between the model-generated and experimental spectrum. The accuracy of both calibration-free LIBS methods suffers from factors such as inaccurately determined instrumental function, the deviation of experimental plasma from the mathematical model used, not taking into account the collection geometry, and from the uncertainty of spectroscopic data. The both calibration-free LIBS approaches are first applied to synthetic spectra which perfectly suit the mathematical model of the method, i.e. the model of the uniform, isothermal, and stationary plasma. This test yields the accuracy of both the approaches for the ideal case. In addition, the accuracy of both the methods is investigated for non-uniform and non-isothermal plasma, because real laser-induced plasma often has high gradients in temperature and particle number densities. Finally, both calibration-free LIBS approaches are applied to experimental spectra obtained from cement samples. The figures of merits of two approaches are compared when working with both synthetic and experimental spectra. T2 - LIBS 2018 at SciX 2018 CY - Atlanta, GA DA - 21.10.2018 KW - Plasma diagnostics KW - Laser induced plasma KW - LIBS KW - Plasma modeling PY - 2018 AN - OPUS4-46931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler T1 - In-situ und Ex-situ Röntgencomputertomographie: Messung des Verhaltens von Beton im Verlauf von mechanischen, thermischen und hydraulischen Prozessen N2 - Um das grundlegende Verhalten des Betons zu verstehen, wird eine zerstörungsfreie Messmethode benötigt, die in der Lage ist, nicht nur Änderungen des Materials wie Feuchtigkeitsumverteilung, Korrosion und Dehnung zu messen, sondern auch die innere Struktur des Materials im Dreidimensionalen aufzulösen, so dass Versagensmechanismen und Transportphänomene direkt auf bestimmte Eigenschaften der heterogenen Materialstruktur bezogen werden können. Die Röntgencomputertomographie (CT) hat sich als ideal für solche Zwecke erwiesen. Diese Präsentation demonstriert die Fähigkeiten der CT zur Identifizierung quantitativer Materialeigenschaften wie Faserorientierung, Rissoberfläche, Korrosionsverteilung und Änderungen des volumetrischen Feuchtigkeitsanteils. Durch die Beschreibung der Ergebnisse einer Reihe von Ex-situ und In-situ Testprogrammen für Bedingungen wie mechanische Belastung, Wassertransport und thermische Exposition, sind auch die Nutzungsmöglichkeiten von diesem Verfahren dargestellt. T2 - DGZfP Arbeitskreis Berlin (403. Sitzung) CY - Berlin, Germany DA - 04.12.2018 KW - Röntgencomputertomographie (CT) KW - In-situ Prüfung KW - Faserverstärkter Beton (FRC) KW - Digitale Volumenkorrelation (DVC) KW - Feuchtigkeitsmessung PY - 2018 AN - OPUS4-46932 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arlt, T. A1 - Kardjilov, N. A1 - Kupsch, Andreas A1 - Manke, I. A1 - Salvemini, F. A1 - Grazzi, F. T1 - Neutronen-Laminografie am Beispiel eines historischen Artefakts T1 - Neutron computed laminography on an ancient metal artifact N2 - Die Computer-gestützte Laminografie (CL) wurde als komplementäre Methode zur Computertomografie für die dreidimensionale Bildgebung von lateral ausgedehnten Objekten entwickelt. Ursprünglich für medizinische Zwecke verwendet, wurde diese Methode kürzlich als zerstörungsfreie nicht-invasive Methode nicht nur in der Materialforschung, sondern auch mit steigendem Interesse für kunsthandwerkliche und historische Objekte eingesetzt. Hier wird die Computer-gestützten Laminografie mit polychromatischer Neutronenstrahlung an einer historischen Tsuba eingesetzt, einem Stichblatt eines japanischen Schwerts. Eine Analyse der Lötstellen gibt Rückschlüsse auf das Herstellungsverfahren. Zudem wurden unterschiedliche Materialsysteme gefunden, vermutlich um dem Tsuba lokal eine höhere Stabilität zu verleihen. Die Messungen wurden an der Imaging-Beamline CONRAD-2 an der Neutronenquelle BER 2 des Helmholtz-Zentrums Berlins (HZB) durchgeführt. KW - Neutronenlaminographie KW - Computertomographie PY - 2018 DO - https://doi.org/10.3139/120.111261 SN - 0025-5300 VL - 60 IS - 12 SP - 1209 EP - 1214 PB - Carl Hanser Verlag CY - München AN - OPUS4-46936 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - How can we use psychology to optimize the NDT inspection process and prevent human error N2 - The aim of this presentation is to highlight how psychology can be used to prevent human error. It starts with examples of accidents, incidents and events that have happened due to too little attention being dedicated to human factors. It continues arguing that human factors are one of the main factors influencing the reliability of non-destructive testing and gives definitions of the main terms. Furthermore, it presents a method used to identify risks in mechanized NDT to be used for the purposes of the final disposal of spent nuclear fuel and presents a study, in which human-centred design and eye tracking have been used to optimism the inspection procedure. The conclusion is that human factors methods can be used to identify problems during the inspection process and generate mitigation strategies that can be used to decrease human error and enhance safety. T2 - The Nordic Symposium on Nuclear Power CY - Stockholm, Sweden DA - 26.11.2018 KW - Zerstörungsfreie Prüfung KW - Human factors KW - Human error KW - Risk management PY - 2018 AN - OPUS4-46938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Bestimmung des Ligningehalts mittels NIR Spektroskopie N2 - Im DFG-Schwerpunktprogramm 1374, Teilprojekt FunWood IV, erfolgt in Kooperation mit dem Institut für Bioanalytik an Hochschule für angewandte Wissenschaften, Coburg und dem Helmholtz-Zentrum für Umweltforschung (UFZ), Leipzig die Untersuchung des Ligningehalts von natürlich gealterten Hölzern. Zu diesem Zweck soll an der BAM eine NIR spektroskopische Methode entwickelt werden, die auch zur Untersuchung großer Stückzahlen geeignet ist. Insgesamt liegen exponierte Proben von 13 verschiedenen Hölzern vor, die sukzessive durch die Kooperationspartner kryovermahlen und getrocknet werden. Für jede der 13 Arten wurden jeweils 300 Holzstücken ausgebracht, exponiert und im Sommer 2018 wieder eingesammelt. Die Ergebnisse sollen als Grundlage für die Bewertung eines Langzeitversuchs zum Einfluss von Waldbewirtschaftungsintensität und Baumartenidentität über mehrere geographische Dimensionen dienen. T2 - Projekttreffen DFG-Schwerpunktprogramm 1374, Teilprojekt FunWood IV CY - Institut für Bioanalytik, Hochschule für angewandte Wissenschaften, Coburg, Germany DA - 15.11.2018 KW - Lignin KW - NIR Spektroskopie KW - Chemometrie PY - 2018 AN - OPUS4-46981 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Carvalho, Ana Margarida A1 - Véliz Montes, Cinthya A1 - Schneider, Rudolf A1 - Madder, A. T1 - An anti-caffeine antibody−oligonucleotide conjugate for DNA-directed immobilization in environmental immunoarrays N2 - The development of fast and cheap highthroughput platforms for the detection of environmental contaminants is of particular importance to understand the human-related impact on the environment. The application of DNA-directed immobilization (DDI) of IgG molecules is currently limited to the clinical diagnostics scenario, possibly because of the high costs of production of such addressable platforms. We here describe the efficient and specific hybridization of an antibody−oligonucleotide conjugate to a short 12-mer capture probe. The specific antibody used is a monoclonal antibody against caffeine, a stimulant and important anthropogenic marker. With this work, we hope to contribute to broadening the application potential of DDI to environmental markers in order to develop cheaper and more stable high-throughput screening platforms for standard Routine analysis of pollutants in a variety of complex matrices. KW - Oligo KW - Antikörperkonjugate KW - Antikörper KW - Biokonjugation KW - Koffein KW - Array PY - 2018 DO - https://doi.org/10.1021/acs.langmuir.8b01347 SN - 0743-7463 VL - 34 IS - 49 SP - 14834 EP - 14841 PB - American Chemical Society CY - Hoboken, New Jersey, USA AN - OPUS4-46982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schwaar, Timm A1 - Remmler, Dario A1 - Börner, Hans G. T1 - Spec2Seq N2 - Spe2Seq automatically translates mass spectrometry fragment spectra of precision polymers into their corresponding sequence. This software is especially useful for combinatorial approaches. KW - Java GUI KW - Polymers KW - Mass spectroscopy (MS) PY - 2018 SP - 1 EP - 8 PB - Humboldt-Universität CY - Berlin AN - OPUS4-46987 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In-situ investigations of mechanochemical reactions N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic[1], metal-organic[2], and inorganic[3] compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms remain often unclear. In the last years, have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy.[4] Here, we present an in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time.[5] Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. T2 - ACS Conference Boston CY - Boston, USA DA - 19.08.2018 KW - Mechanochemistry KW - In situ KW - Kinetic PY - 2018 AN - OPUS4-46989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - New insights in mechanochemical processes using real-time in situ investigations N2 - Mechanochemistry is increasingly used for synthesizing various materials including metal organic compounds and cocrystals. Although this synthesis approach offers a fast and pure synthesis in high yields, there is a lack in understanding the mechanisms of milling reactions. The necessary data can only be obtained in in situ experiments, which were only recently established for milling reactions. Herein, we present a novel setup enabling a combined in situ investigation of mechanochemical reactions using synchrotron XRD and Raman spectroscopy. T2 - ECM31 CY - Oviedo, Spain DA - 18.08.2018 KW - Mechanochemistry KW - In situ PY - 2018 AN - OPUS4-46990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical reactions N2 - Presentation of the recent results in the context of in situ investigations of reactions using X-ray diffraction. T2 - Germany Brazil Workshop: New light on mechanisms of chemical reactions CY - Kiel, Germany DA - 31.07.2018 KW - In situ KW - XRD PY - 2018 AN - OPUS4-46991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Hydrogen assisted cracking phenomena in duplex stainless steels elucidated by in- and ex-situ ToF-SIMS experiments N2 - In the presented research, the high potential and abilities of secondary ion mass spectrometry (ToF-SIMS) to detect and locally map the hydrogen distribution in two types of duplex stainless steels are shown. The research validates certain proposed mechanisms by combining ToF-SIMS with high-resolution scanning electron microscopy and electron-backscattered diffraction. The combination of data from several techniques on the same region was conducted in this field for the first time by applying data treatment of the ToF-SIMS raw data and data fusion approach. This powerful combination of methods allows reviewing of the occurring processes related to hydrogen assisted cracking. The step beyond the state of the art in this field was gained here by developing permeation and mechanical loading experiments within the ToF-SIMS during chemometric imaging of the hydrogen distribution in the microstructure. The research presents the necessary correlation between the hydrogen distribution and the resulted structural changes, the diffusion behavior in a duplex microstructure and stress induced diffusion of hydrogen by applying external load at the microscale. T2 - 6th WMRIF Early Career Scientist Summit CY - NPL Teddington UK DA - 18.06.2018 KW - ToF-SIMS KW - Duplex stainless steel KW - LDX KW - EBSD KW - Data-fusion PY - 2018 AN - OPUS4-46865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino T1 - Gas Source Localisation from the Next Dimension N2 - Leaking methane (CH4) from infrastructures, like pipelines, industrial complexes and landfills, or accidental hazardous goods transports is critical for the environment, but can also pose a risk to human life. To enable a fast detection and localisation of these kind of leaks, we developed a novel robotic platform for aerial remote gas sensing. The platform combines an unmanned micro aircraft (UAV), a 3-axis aerial stabilisation gimbal and an open-path gas detector based on the tunable diode laser absorption spectroscopy (TDLAS). T2 - PhD Poster Session an der Universität Örebro CY - Örebro, Sweden DA - 27.11.2018 KW - Gas Source Localisation KW - Mobile Robot Olfaction KW - UAV KW - TDLAS KW - Gas Spectroscopy PY - 2018 AN - OPUS4-46869 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino T1 - Aerial-based Gas Source Localisation using an Open-Path Gas Detector N2 - Presentation of the aerial robotic platform to localise gas sources with an open-path gas detector based on the tunable diode laser absorption spectroscopy (TDLAS) and project overview. T2 - Seminarserie an der Universität Örebro CY - Örebro, Sweden DA - 28.11.2018 KW - Gas Source Localisation KW - Gas Spectroscopy KW - UAV KW - TDLAS PY - 2018 AN - OPUS4-46870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vranic, Marija T1 - Expression, purification and characterization of the recombinant cysteine-rich biomarker Hepcidin-25 N2 - Hepcidin regulates iron homeostasis in response to inflammation, erythropoietic demand, and iron stores. The native state of hepcidin-25 is an attractive target for the development of a reliable analytical tool that can quantify the hepcidin concentration in biological samples and reveal iron metabolic disorders. Therefore, a selective immunoassay would have to discriminate between different types of hepcidin and quantify only hepcidin-25’s concentration. The peptide contains a well-defined β-sheets and a β-hairpin loop stabilized by four disulfide bonds. Recently, it was shown that hepcidin-25 contains an ATCUN motif at its N-terminus. This motif is known to have high affinity towards Cu2+ and Ni2+. One of the aims of this study is to determine the three-dimensional (3D) structure of metal-bound hepcidin-25. Here, we present an optimized procedure for preparing natively folded hepcidin 25 (~2.80 kDa) and structural analysis of metal binding to hepcidin-25. Hepcidin was expressed as a His6-SUMO-hepcidin-25 fusion protein (~16.20 kDa) in Escherichia coli, Origami B strains, and purified as a soluble recombinant protein in three steps. After purification based on the nickel affinity chromatography, the purified His6-SUMO-hepcidin 25 fusion protein was cleaved by the SUMO-specific ULP1 protease. The liberated hepcidin 25 was further purified on a Superdex 30 16/600 column and folded in the last step of purification in the presence of glutathione. Freshly expressed hepcidin was kept in its reduced form to prevent misfolding and allow for efficient removal of the SUMO tag. The presence of natively folded hepcidin 25 after RP-HPLC was confirmed by ESI-MS and NMR spectroscopy. Based on published chemical shifts, we achieved a nearly complete assignment of the labeled and unlabeled hepcidin-25 at pH=3. Comparison of 1H chemical shifts and TOCSY spectra at pH=7 in the presence and absence of Ni2+ demonstrates that the metal binds at the N-terminus of hepcidin 25. Chemical shift changes due to metal complexation decrease further away from the metal binding site. T2 - 28th International Conference on Magnetic Resonance in Biological Systems, ICMRBS CY - Dublin, Irland DA - 19.08.2018 KW - Peptides KW - Metalloproteins KW - Copper KW - ATCUN KW - Nickel KW - NMR KW - SUMO KW - Fusion protein KW - Iron disorders KW - ESI-MS KW - RP-HPLC PY - 2018 AN - OPUS4-46944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vranic, Marija T1 - Metal-binding properties of the cystein-rich biomarker Hepcidin-25 N2 - Hepcidin-25 regulates iron homeostasis in response to inflammation, erythropoietic demand and iron stores. The liver synthesizes three types of hepcidin, only hepcidin-25 indirectly regulates and coordinates use and storage of iron. Hepcidin-25 contains a well defined β-sheet and β-hairpin loop stabilized by four disulfide bonds. The N-terminus which plays a crucial role in the biological activity of hepcidin-25 was found to be disordered. The ATCUN motif sequence is present at the N-terminus (Asp-Thr-His). The ATCUN motif (H2N-X-X-His) binds Cu2+ and Ni2+ with high affinity and always contains histidine in its sequence. NMR provides an ideal tool to determine hepcidin-25’s threedimensional(3D) structure taking into account the Cu2+ and Ni2+ binding capacity of hepcidin’s ATCUN motif. T2 - 3rd International Conference Proteins and Peptides, Structure, Function and Biotechnology CY - Geneva, Switzerland DA - 23.07.2018 KW - Peptides KW - Metalloproteins KW - Chromatography KW - ATCUN KW - Nickel KW - Copper KW - SUMO KW - Fusion protein KW - Iron disorders KW - ESI-MS KW - RP-HPLC PY - 2018 AN - OPUS4-46945 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vranic, Marija T1 - Metal-binding properties of the cysteine-rich biomarker Hepcidin-25 N2 - Comparison of 1H chemical shifts and TOCSY data in the presence and absence of Ni2+ demonstrates that the metal binds at the N-terminus of the hepcidin-25. Chemical shift changes due to metal complexation decrease further away from the metal binding site, with the smallest effect at phenylalanine [Phe-4], proline [Pro-5] and isoleucine [Ile-6]. T2 - 8th Peptide Engineering Meeting CY - Berlin, Germany DA - 08.11.2018 KW - Peptides KW - Metalloproteins KW - Copper KW - ATCUN PY - 2018 AN - OPUS4-46946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Gottlieb, Cassian A1 - Günther, Tobias A1 - Millar, Steven ED - Forde, Mike T1 - Application of laser induced breakdown spectroscopy N2 - A big part of the infrastructure is made of concrete, which is a multiphase system made of cement, aggregates, water and pores. Concrete is often used in combination with steel as reinforced concrete. Environmental influences, especially the ingress of harmful ions in combination with the ingress of water, trigger different damage processes which reduce the designed lifetime of a structure. The ingress of chlorides from de-icing salt or sea water leads to corrosion of the reinforcement. In addition, the carbonation of the concrete may trigger the corrosion of the reinforcement. The ingress of alkalis from deicing salts may cause the expansion of the amorphous silica aggregates (alkali-silica reaction) through formation of a swelling gel of calcium silicate hydrate if water is present. The ingress of sulphates may cause spalling of the concrete surface due to ettringite formation. For the standard procedure in civil engineering cores are taken, cut in slices, grinded and the obtained homogenized powder is solved in acid and investigated by standard procedures. BAM has developed the LIBS technique for the 2D evaluation of the chemical composition of concrete. The technique is established for automated laboratory use with high numbers of samples to investigate transport processes of harmful species (Cl-, CO2 , SO4 2-and alkalis) in concrete. Information about ingress depth and the quantitative values are important to estimate the remaining lifetime of the infrastructure. LIBS is a surface technique. To get information about the ingress depth, a drill core has to be taken and cut in the middle. The measurements are carried out at the cross section. The main advantages of LIBS are the direct measurement on the surface of the concrete, fast analysis (sample rate 100 Hz) with a spatial resolution of up to 100 µm, the consideration of the heterogeneity of the concrete and the possibility of automated measurements which save a lot of manpower and time. As an example the investigation of ingress profiles for standard diffusion and migration tests in civil engineering takes hours in comparison to just a few minutes using LIBS. At the same time a 2D-evaluation provides information about hot spots of elemental concentration which may not be found by standard methods. The state of the art of LIBS technique for applications in civil engineering will be presented, including typical results of 2D investigation of concrete in laboratory. The performance is also demonstrated by examples for onsite applications using a mobile LIBS system. The road map to standardization is presented as well. T2 - Structural Faults + Repair-2018 CY - Edinburgh, UK DA - 15.05.2018 KW - Sulphate KW - Chloride KW - Concrete KW - LIBS PY - 2018 SN - 0-947644-86-5 DO - https://doi.org/10.25084/sfr.2018.0030 SP - 1 EP - 7 PB - University of Edinburgh CY - Edinburgh AN - OPUS4-46947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Application of LIBS for the chemical investigation of concrete infrastructure N2 - Overview about LIBS applications in civil engineering T2 - Structural Faults + Repair-2018 CY - Edinburgh, UK DA - 15.05.2018 KW - On-site measurements KW - LIBS KW - Concrete KW - Chloride KW - Sulfates PY - 2018 AN - OPUS4-46948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Günther, Tobias T1 - Boosting of chlorine emission by electric discharge reheating in laser-induced plasma N2 - For the determination of the remaining life-time and the degree of damage of reinforced concrete structures such as marine construction, bridges or parking decks, a highly precise measurement of harmful species is also required for trace elements. One of the most interesting elements is chlorine, because above a certain threshold corrosion is triggered. To increase the intensity of the chlorine line, helium is usually used, which is costly. To overcome this problem, low electrical discharge reheating is used which operates in air atmosphere. A comparison between results obtained by measuring with helium and reheating by electrical discharge is presented. The performance is compared by the resulting calibration curves and the calculated limit of detection obtained by 15 reference samples based on cement with NaCl. Concentrations of reference samples range from 0.05 to 2.5 wt% chlorine. T2 - Xth international conference on Laser-Induced Breakdown Spectroscopy CY - Atlanta, GA, USA DA - 21.10.2018 KW - LIBS KW - Electric discharge KW - Plasma reheating PY - 2018 AN - OPUS4-46792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Temporal evaluation and imaging of laser-induced plasmas on cement-based materials N2 - In civil engineering, the laser-induced breakdown spectroscopy has been applied as a fast and reliable method for a quantitative evaluation of concrete cores. Due to a two-dimensional scanning, the heterogeneity of concrete can be evaluated and elements like Cl, Na, and S are related to the cement matrix only. This study deals with the temporal evaluation and imaging of laser-induced plasmas on cement-based materials, in order to investigate the impact of aggregates with diffrent grain size on the spectral response in LIBS. T2 - Xth international conference on Laser-Induced Breakdown Spectroscopy CY - Atlanta, GA, USA DA - 21.10.2018 KW - LIBS KW - Concrete KW - Grain size PY - 2018 AN - OPUS4-46794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram T1 - Maths challenges in purity determination N2 - Purity determination requires specific analytical and assessment approaches since the values to be determined are close to physical limits. The paper deals with some techniques that may tackle the issue. T2 - International Seminar on Mathematics, statistics and computation to support measurement quality CY - Sankt Petersburg, Russsia DA - 29.05.2018 KW - Assessment KW - Analytics KW - Purity PY - 2018 AN - OPUS4-46795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram T1 - ISO 17034 und ISO Guide 33: Use of CRM in the calibration laboratory N2 - RM certified according to the rules of international standards may be used as the basis of traceability also in the calibration laboratory. The paper describes approaches and gives examples. T2 - Akkreditierungskonferenz AKKKO2018 CY - Berlin, Germany DA - 11.06.2018 KW - Calibration laboratory KW - CRM KW - Uses PY - 2018 AN - OPUS4-46796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Günther, Tobias T1 - Plasma reheating in LIBS with electric discharge to detect halogens in low concentrations N2 - The Laser-induced Breakdown Spectroscopy (LIBS) is an useful analytical technique for the chlorine detection in building materials, specifically in the reinforcement concrete. If chlorine exceeds a specific concentration threshold, the result can be pitting corrosion of the reinforcement, which affects the stability and lifetime of building structures like marine constructions, bridges or parking decks. The critical chlorine content based to cement is 0.4 wt.-% based to the cement for reinforced concrete. The ingress of chlorides from sea water or de-icing salt leads to corrosion of the reinforcement. The chlorine spectral line Cl I at 837.59 nm shows a good performance in helium atmosphere. For measurements without helium we used a electric discharge setup to reheat the Laser-induced plasma with a voltage below 100 V. In this case the reheating shows an increasing chlorine emission in air atmosphere. This work shows chlorine calibration curves with LIBS in a helium flow and LIBS with electric discharge reheating in air atmosphere. The determination of the limit of detection (LOD) for both setups and the measurement results of a drill core sample with a quantitative chlorine ingress profile will be presented. T2 - Xth international conference on Laser-Induced Breakdown Spectroscopy CY - Atlanta, GA, USA DA - 21.10.2018 KW - LIBS KW - Laser induced plasma KW - Plasma reheating KW - Electric discharge PY - 2018 AN - OPUS4-46797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Grzimek, V. A1 - Günther, G. A1 - Svetogorov, R. A1 - Veziri, C. M. A1 - Kapsi, M. A1 - Karanikolos, G. N. A1 - Prokhnenko, O. A1 - Bewley, R. A1 - Russina, M. T1 - Explaining water adsorption in one-dimensional channels in AlPO4-5 on molecular scale N2 - The adsorption of water in one-dimensional channels in porous aluminophosphate material AlPO4-5 has been studied by a combination of gravimetric Analysis techniques, neutron and X-ray diffraction and Neutron spectroscopy. Molecular structure of AlPO4-5 consists of 12-membered rings of alternating, corner-sharing AlO4 and PO4 tetrahedra connected by oxygen bridges into sheets in the (a, b) plane. The sheets are connected by oxygen bridges along the c crystal axis and form onedimensional channels of which the largest, formed by the 12-membered rings, have a van der Waals Diameter of about 8.3 Å. Gradually increasing the amount of adsorbed water we could follow the evolution of the confined water mobility in a systematic way and identify the molecular mechanism of water adsorption. We focused particularly on the range of low and medium relative pressures up to p/p0=0.32, where a Change from a hydrophobic behavior to a steep, capillary condensation like water intake has been observed. At the Initial adsorption stages water occupies positions close to the pore walls causing the contraction of channels in the (a, b) plane and the prolongation of the channels along c axis in AlPO4-5. With the progressing intake water molecules form chains along the main channels. The cooperative interactions between water molecules lead to the onset of phonon-like cooperative modes and, surprisingly, to the increase of diffusive-like motion, which slow down only in the final adsorption stages when AlPO4-5 channels are completely filled. KW - AlPO4-5 KW - Water adsorption KW - Confined water KW - 1-dimensional, KW - Diffusion PY - 2018 DO - https://doi.org/10.1016/j.micromeso.2018.11.025 SN - 1387-1811 VL - 304 SP - 109201 PB - Elsevier Inc. AN - OPUS4-46798 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raysyan, Anna T1 - Development of dipstick immunoassays for environmental and diagnostic applications missions from plastic materials N2 - Development of dipstick immunoassays for environmental analysis and integration the technology for diagnostic applications missions. T2 - Arbeitskreistreffen Immunoassays CY - Hennigsdorf, Germany DA - 26.11.2018 KW - Environmental analysis KW - LFIA KW - BPA KW - DCF PY - 2018 AN - OPUS4-46801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram T1 - Forthcoming endeavours of ISO/REMCO N2 - Recent activities of ISO/REMCO are documented, and forthcoming endeavours discussed. T2 - III International Conference on reference materials in measurement and technology CY - Ekaterinburg, Russia DA - 11.09.2018 KW - Normative guidelines KW - Standardisation KW - REMCO PY - 2018 AN - OPUS4-46802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram T1 - Validation of methods for the determination of qualitative properties N2 - Validation of analytical methods is well described for quantitative approaches. Qualitative methods meet certain problems in fulfilling all requirements of a method validation. The paper discusses requirements and points which may possibly left out. T2 - III International Conference on reference materials in measurement and technology CY - Ekaterinburg, Russia DA - 11.09.2018 KW - validation, qualitative methods PY - 2018 AN - OPUS4-46804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Non-metals in inorganic reference materials N2 - The analysis of non-metals normally is carried out using elemental analysers which require reference material for calibration. In the lecture the CRM-program of BAM suitable for non-metal-analysis is presented. There are CRMs available with non-metal contents in the low ppm up to the high percent region. T2 - CETAMA 2018 CY - Paris, France DA - 27.11.2018 KW - CRM KW - Non-metals KW - Carbon KW - Sulfur KW - Oxygen KW - Nitrogen KW - Hydrogen KW - Reference material PY - 2018 AN - OPUS4-46968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Scharf, Holger A1 - Lkhagvasuren, B. A1 - Oyuntungalag, U. A1 - Rausch, J. T1 - Certified reference material for determination of total cyanide in soil [BAM-U116/CGL306] N2 - CRM (Certified Reference Material) BAM-U116/CGL306 “Cyanide in soil” was produced within a framework of cooperation between CGL (Central Geological Laboratory) of Mongolia and Federal Institute for Materials Research and Testing (BAM) of Germany in 2013-2017. The CRM BAM-U116/CGL306 represents a mixture of a sandy soil collected from a contaminated former gasworks area in the Berlin region (Germany) and an unpolluted sandy soil from Nalaikh region (Mongolia). The bulk candidate material for this reference material was prepared at CGL CRM Laboratory exclusively destined to the preparation of reference materials and equipped with modern technical equipment. Homogeneity, stability and shelf life were studied in full compliance with ISO Guide 35. The CRM was evaluated as sufficiently homogeneous. Statistical evaluation of certification analysis was software packages SoftCRM and ProLab Plus. Certified value of total cyanide of the CRM is 12.0 mg/kg and expanded uncertainty was assigned as 0.8 mg/kg. The intended purpose of this material is the verification of analytical results obtained for the mass fraction of total cyanide in soils and soil-like materials applying the standardized procedure ISO 11262:2011. As any reference material, it can also be used for routine performance checks (quality control charts) or validation studies. KW - CRM KW - Cyanide in soil KW - Total cyanide PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-469694 DO - https://doi.org/10.17265/2162-5263/2018.04.004 SP - 149 EP - 161 PB - David Publishing AN - OPUS4-46969 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin T1 - Accelerating Chemical Process Development and Manufacturing – Design and Validation of an Integrated NMR Micro Mixer N2 - The future competitiveness of the process industry and their providers depends on its ability to deliver high quality and high value products at competitive prices in a sus-tainable fashion, and to adapt quickly to changing customer needs. The transition of process industry due to the mounting digitalization of technical devices and their pro-vided data used in chemical plants proceeds. Though, the detailed characteristics and consequences for the whole chemical and pharmaceutical industry are still unfore-seeable, new potentials arise as well as questions regarding the implementation. As the digitalization gains pace fundamental subjects like the standardization of device interfaces or organization of automation systems must be answered. Still, process in-dustry lack of sufficient system and development concepts with commercial advantage from this trend. Compared to traditional batch processes, intensified continuous production allows new and difficult to produce compounds with better product uniformity and reduced consumption of raw materials and energy. Flexible (modular) chemical plants can pro-duce various products using the same equipment with short down-times between campaigns, and quick introduction of new products to the market. Full automation is a prerequisite to realize such benefits of intensified continuous plants. In continuous flow processes, continuous, automated measurements and closed-loop control of the product quality are required. Consequently, the demand for smart sensors, which can monitor key variables like component concentrations in real-time, is increasing. Low-Field NMR spectroscopy presents itself as such an upcoming smart sensor1,2 (as addressed, e.g., in the CONSENS project3). Systems utilizing such an online NMR analyzer benefits through short development and set-up times when applied to modular production plants starting from a desired chemical reaction3. As an example for such a modular process unit, we present the design and validation of an integrated NMR micro mixer based on computational mod-elling suited for a desired chemical reaction. This method includes a proper design of a continuous reactor, which is optimized through computational fluid dynamics (CFD) for the demands of the NMR sensor as well as for the given reaction conditions. The system was validated with a chemical reaction process. References: [1] M. V. Gomez et al., Beilstein J. Org. Chem. 2017, 13, 285-300 [2] K. Meyer et al., Trends Anal. Chem. 2016, 83, 39-52 [3] S. Kern et al., Anal Bioanal Chem. 2018, 410, 3349-3360 T2 - Kolloquium Arbeitskreis Prozessanalytik CY - Hannover, Germany DA - 03.12.2018 KW - NMR KW - Reaction Monitoring KW - Digital Twin KW - Flow Chemistry KW - Process Analytical Technology PY - 2018 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-46972 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Validation of artificial defects for Non-destructive testing measurements on a reference structure N2 - Non-destructive testing was established over the last decades as an important tool for assessing damages, material characterization and quality assurance in civil engineering. For example, Ground Penetrating Radar (GPR) can be used to scan large areas of concrete structures to determine the spatial position of the reinforcement. With the ultrasonic echo method, the thickness of concrete structures can be easily determined even if a high density of reinforcement is given. Various methods and processes have been developed for the validation of NDT procedures aiming at ensuring the quality of measurements in practical use. The Probability of Detection (POD) for example, is an available method to compare different technical devices with each other quantitatively regarding their performance. With this method, the best suited testing device for a specific inspection task under defined boundary conditions can be selected. By using the Guide to the Expression of Uncertainty in Measurement (GUM), it is possible to quantify the measurement uncertainty of an inspection procedure for a specific task. Another important aspect to improve the acceptance of non-destructive testing methods is the development of reference specimens. Reference specimens serve for the calibration and further development of NDT methods under realistic conditions in different laboratories under the same conditions. This is an essential prerequisite for round robin tests. A particular challenge here is the most realistic representation of a damage that can occur at building sites. Possible damages include for example horizontal and vertical cracks or honeycombs in concrete. Such a reference structure was built for the development of a new design of power plant constructions. Comparative studies on the manufacturing of realistic honeycombs and delaminations were carried out in advance on a test specimen. The results of this study are presented here. T2 - ICCRRR 2018 - Concrete Repair, Rehabilitation and Retrofitting CY - Cape Town, South Africa DA - 19.11.2018 KW - Zerstörungsfreie Prüfung KW - Nondestructive testing KW - Ultraschall KW - Kiesnest KW - Honeycomb KW - Ultrasonic Echo PY - 2018 AN - OPUS4-46974 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ studies of mechanochemistry: a force of synthesis N2 - Recent results in the field of mechanisms and kinetics of mechanochemical reactions. T2 - Seminar GFZ Potsdam CY - Postdam, Germany DA - 28.03.2018 KW - In situ KW - XRD KW - Rietveld PY - 2018 AN - OPUS4-46992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Synchrotron X-ray Investigations N2 - Summary of the techniques available at the BAMline and µspot BEamline. T2 - Workshop Humboldt University and Hebrew University of Jerusalem CY - Berlin, Germany DA - 09.10.2018 KW - In situ KW - XRD PY - 2018 AN - OPUS4-46993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - New insights in mechanochemical processes using real-time In situ investigations N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic[1], metal-organic[2], and inorganic[3] compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms remain often unclear. In the last years, have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy.[4] Here, we present an in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time.[5] Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. T2 - 5th International Conference "Fundamental Bases of Mechanochemical Technologies" CY - Novosibirsk, Russia DA - 25.06.2018 KW - Mechanochemistry KW - XRD KW - Kinetic KW - Coordination polymers PY - 2018 AN - OPUS4-46994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ characterization of nucleation, growth, crystallization and dissolution of nanoscaled iron oxides N2 - Nucleation and growths of iorn oxide nanoparticles studied in situ using XRD, XRF, SAXS and XANES. T2 - International CRC meeting CY - Berlin, Germany DA - 10.10.2018 KW - XRD KW - XANES PY - 2018 AN - OPUS4-46995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina T1 - Mechanochemical synthesis of metal phosphonates N2 - The exploration of metal phosphonates chemistry has gained great interest during the last decades, because of their structural diversity. Transition metal phosphonates are promising candidates for an application as electrocatalysts in oxygen evolution reactions (OER). Here, we present the in situ investigation of mechanochemical syntheses of different manganese phosphonates by synchrotron X-ray diffraction. Nitrilotri(methylenephosphonic acid) and N,N-Bis(phosphonomethyl)glycine were chosen as ligands. The liquid-assisted milling process can be divided into three steps, including an amorphous stage. One of the products has not been obtained by classical solution chemistry before. These metal phosphonates and/or their derivatives are considered to be active in electrochemical energy conversion. The verification of their applicability is one of the topics of our resent research. T2 - Fundamental Bases of Mechanochemical Technologies CY - Novosibirsk, Russia DA - 25.06.2018 KW - Metal phosphonates KW - Mechanochemistry KW - PXRD KW - Thermography PY - 2018 AN - OPUS4-46996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - In situ investigation of mechanochemical Knoevenagel condensations of benzaldehyde derivates N2 - Mechanochemistry is known for short reaction times, nearly quantitative conversions, and decreasing amount of solvents. Among organic syntheses, the Knoevenagel condensation is an important C-C bond forming reaction. We investigated the reaction of benzaldehyde derivates (nitro- and fluoro-derivates) with malononitrile syntheses by a combination of different in situ investigation techniques. T2 - BESSY II User Meeting CY - Berlin, Germany DA - 05.12.2018 KW - Mechanochemistry KW - In situ PY - 2018 AN - OPUS4-46997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina T1 - In situ investigation of milling reactions and structure determination of the products using X-ray diffraction N2 - Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. By milling the reactants, various organic, inorganic, and metal-organic compounds can be obtained in high yields. Although mechanochemistry is widely used, the underlying mechanisms are not fully understood making mechanochemical reactions difficult to predict. Metal phosphonates are metal-organic compounds accessible by grinding. Because of their structural diversity, the exploration of the chemistry of metal phosphonates has gained considerable interest during the last decades. Transition metal phosphonates are promising candidates for an application as electrocatalysts in oxygen evolution reaction (OER). Here, we present the in situ investigation of the mechanochemical synthesis of a manganese(II)-phosphonate by synchrotron X-ray diffraction and thermography. The product has not been obtained by classical solution chemistry before and its crystal structure was determined from PXRD data. The milling process can be divided into different steps, with the product crystallization corresponding with the highest temperature rise. The activity of this metal phosphonate towards OER was measured and is presented here. T2 - International School of Crystallography - 52nd Course: Quantum Crystallography CY - Erice, Italy DA - 1.06.2018 KW - Metal phosphonates KW - Mechanochemistry KW - PXRD KW - OER KW - Thermography PY - 2018 AN - OPUS4-46998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina T1 - In situ investigation of mechanochemical syntheses of manganese phosphonates with N-containing ligands N2 - Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. The exploration of the chemistry of metal phosphonates has gained considerable interest during the last decades due to their structural diversity. We synthesized manganese phosphonates in milling reactions. The mechanochemical reactions were investigated in situ to reveal the underlying mechanisms. T2 - Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 05.12.2018 KW - Metal phosphonates KW - Mechanochemistry KW - PXRD KW - In situ KW - Thermography PY - 2018 AN - OPUS4-46999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Helmerich, Rosemarie ED - Hu, Chang Bin T1 - Engineering Education in Europe N2 - The book chapter first analyses the history of higher education in Europe. Second step describes the current Bologna process. Finally, the rule of the Bundesanstalt für Materialforschung und -Prüfung (BAM) in supporting PhD-students during their research and preparation of theire theses in cooperation with Universities is described KW - History of education KW - Bologna process KW - BAM PY - 2018 SN - 978-7-114-14938-2 SP - 61 EP - 71 PB - China Communication Press Co., Ltd. CY - Fuzhou, China ET - 1. AN - OPUS4-46871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breitfeld, Steffen T1 - BaF-Coordination polymers: Mechanochemical syntheses of new coordination polymers with a direct Ba-F bond N2 - Metal organic frameworks (MOFs) and coordination polymers (CPs) Play an important role in different fields of applications like e.g. catalysis, separations, gas storages, sensors or optoelectronics. Moreover, particularly fluorinated metal-organic frameworks (FMOFs) are in the focus of interest during the last years. Due to the strong electronegativity of fluorine the FMOFs show beside an enhanced thermal stability excellent optical and electrical properties compared to non-fluorinated frameworks. In most cases fluorine is implemented using perfluorinated organic linkers at the synthesis, usually performed by solvothermal synthesis. However, only few examples are known so far where fluorine is coordinated directly to the metal cation. Recently we reported about successful mechanochemical syntheses and characterization of fluorine-containing coordination polymers of alkaline earth metals by milling M(OH)2 (M: Ca, Sr, Ba) with fluorinated benzene dicarboxylic acids. In the present study, it was shown that it is possible to connect fluorine directly to Barium using a mechanochemical synthesis route. A new phase pure barium coordination polymer, BaF-benzene-dicarboxylate (BaF(p-BDC)0.5), was synthesized by milling starting either from barium hydroxide or from barium acetate as sources for barium cations. In both cases the second reactant was 1,4-benzenedicarboxylic acid (H2(p-BDC)). Ammonium fluoride was used as fluorinating agent directly at milling. Although single crystals are not accessible so far and the structure was not solved yet, both the 19F MAS NMR spectrum and the FT IR spectrum give strong evidence that fluorine as well as 1,4-benzenedicarboxylate are connected to barium. This is the first mechanochemical synthesis of coordination polymers where fluorine is directly coordinated to the metal cation. The new compound BaF(p-BDC)0.5 was characterized by X-ray powder diffraction, FT IR- and 19F, 1H-13C CP MAS NMR spectroscopies, DTA-TG and elemental analysis. T2 - Konferenz CY - Oberjoch, Germany DA - 22.07.20108 KW - Mechanochemical syntheses KW - Coordination polymers KW - Direct fluorine-metal bond KW - Alkaline earth metal PY - 2018 AN - OPUS4-46897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breitfeld, Steffen T1 - High energy ball milling of a new representative of coordination polymers without organofluorine linkers N2 - Metal organic frameworks and coordination polymers play an important role in different fields of applications. Moreover, particularly fluorinated metal-organic frameworks (FMOFs) are in the focus of interest during the last years. In most cases, fluorine is implemented using perfluorinated organic linkers at the synthesis, usually performed by solvothermal synthesis. However, only few examples are known so far where fluorine is coordinated directly to the metal cation. Recently, we reported about mechanochemical syntheses and characterization of fluorine-containing coordination polymers of alkaline earth metals by milling M(OH) (M: Ca, Sr, Ba) with fluorinated benzene dicarboxylic acids 2 and we reported about mechanochemical syntheses of alkaline earth metal fluorides with ammonium fluoride. Now we are reporting about a combination of both synthesis routes. That is the first mechanochemical synthesis of coordination polymers where fluorine is coordinated directly to the metal cation. T2 - Konferenz CY - Berlin, Germany DA - 30.11.2017 KW - Metal organic frameworks KW - Coordination polymer KW - Mechanochemical syntheses KW - Direct fluorine-metal bond KW - Alkaline earth metal PY - 2017 AN - OPUS4-46898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Im Wohnzimmer haben wir es zuerst – Wie Innovationen für den Massenmarkt die Digitalisierung der Prozessindustrie vorantreiben N2 - Automatisierungstechnik, sowie die Informations- und Kommunikationstechnik (IKT) verschmelzen zunehmend. In der Prozessindustrie tut man sich aber schwer, die heu-te schon möglichen daten- oder modellbasierten Steuerungen auf Basis smarter Sen-soren und Aktoren einzusetzen oder allein Anforderungen daran vorzugeben. Viele aktuelle Entwicklungen der Zulieferer werden verwehrt und man wartet lieber ab. Es bilden sich schon jetzt rasant schnell neue digitale Geschäftsmodelle in der Pro-zessindustrie, wie es schon mit der zunehmenden Verbreitung des Internets beobach-tet werden konnte. Wenn die Automatisierer und Anlagenspezialisten jetzt nicht ge-stalten, tun es andere. Früher war es umgekehrt: Informations- und Kommunikationstechnik für Profis konn-ten sich nur die Großkonzerne leisten. Die Technologie vom Personalcomputer bis zum Smart-Gerät und ihre Peripherie wurden und werden ausschließlich durch den Massenmarkt vorangetrieben. Also müssen wir umdenken und Wege finden, die rasch voranschreitende Informations- und Kommunikationstechnik geschickt für die Digitalisierung umbiegen. Der Beitrag erörtert aktuelle Diskussionen über netzartige Verbindungen der Feldge-räte (Sensoren und Aktoren) untereinander und zur Cloud sowie über virtuelle Server-verbünde und Applikationen, die auf Cloud-Diensten basieren. Mit einem solchen System ist die Einrichtung beliebiger Dienstleistungen und Funktionen auf der Basis der jeweils gängigen Methoden und Technologie des Internets möglich. Beispiele für Dienstleistungen sind beispielsweise auf prozessanalytische oder Sensordaten auf-bauende Instandhaltungsdienste oder Energiedienste für Anlagen. T2 - 14. Kolloquium Prozessanalytik CY - Hannover, Germany DA - 03.12.2018 KW - Digitalisierung KW - Prozessindustrie KW - Prozessanalytik KW - Automatisierung KW - Innovationen KW - Informations- und Kommunikationstechnik PY - 2018 AN - OPUS4-46899 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Buttler, Sabine A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 23. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik: Polyzyklische aromatische Kohlenwasserstoffe (PAK) in Boden, Mineralölkohlenwasserstoffe (MKW) in Boden, Elemente in Sediment und Gesamtcyanid in Boden. KW - Gesamtcyanid KW - Boden KW - Eignungsprüfung KW - MKW KW - PAK KW - Schwermetalle PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473403 SP - 1 EP - 261 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-47340 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Buttler, Sabine A1 - Becker, Roland T1 - Bericht zum 24. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik: Polychlorierte Biphenyle (PCB) in Boden, Mineralölkohlenwasserstoffe (MKW) in Boden, Elemente in Boden und Gesamtcyanid in Boden. KW - Spurenelemente KW - Boden KW - Gesamtcyanid KW - Eignungsprüfung KW - MKW KW - PCB PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473418 SP - 1 EP - 183 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-47341 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Xu, W. A1 - Zscherpel, Uwe A1 - Peng, J. A1 - Luo, L. A1 - Gao, X. A1 - Li, J. T1 - Investigation on Wall Thickness Ranges Using Digital Radiography for Tangential Projection Technique N2 - X-ray testing is based on the attenuation of X-rays when passing through matter. Image detectors acquire the X-ray information which is defined by the local penetrated wall thickness of the tested sample. By X-ray absorption in the detector and following read-out and digitization steps a digital image is generated. As detectors a radiographic film and film digitization, a storage phosphor imaging plate and a special Laser scanner (Computer Radiography - CR) or a digital detector array (DDA) can be used. The digital image in the computer can then be further analyzed using many types of image processing. In the presented work the automated evaluation of wall thickness profiles are investigated using a test steel pipe with 9 different wall thicknesses and various X-ray voltages and different filter materials at the tube port and intermediate between object and detector. In this way the influence of different radiation qualities on the accuracy of the automated wall thickness evaluation depending on the penetrated wall thickness of the steel pipe was investigated. T2 - 10th International Conference on Information Optics and Photonics CY - Beijing, China DA - 08.07.2018 KW - Image evaluation KW - Computed radiography (CR) KW - Digital Detector Array (DDA) KW - Tangential radiography KW - Wall thickness measurement PY - 2018 SN - 978-1-51062580-8 DO - https://doi.org/10.1117/12.2506324 SN - 0277-786X VL - 10964 SP - Article Number: UNSP 109645B PB - SPIE CY - Bellingham, WA AN - OPUS4-47346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Image Quality in Industrial Radiology N2 - Overview on Concepts and Methodology used for quality ensurance in industrial radiology. The past, present and future. T2 - General Assembly of Academia NDT International CY - Brescia, Italy DA - 12.10.2018 KW - Image quality KW - Computed radiography (CR) KW - Digital Detector Array (DDA) KW - Film radiography PY - 2018 AN - OPUS4-47347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Chemical and electrochemical interaction mechanisms of metal-reducing bacteria with gold surfaces N2 - Bacterial biofilms are considered one of the salient contributing factors to the deterioration of metals and their alloys, occurring in virtually all environments and across various industrial systems. Considering the sheer magnitude of detrimental effects, it is of pertinent interest to elucidate the interaction mechanisms of sessile bacteria with metal and metal oxide surfaces to facilitate the development of efficient antifouling strategies. A common constituent of microbial communities within aquatic and sedimentary settings, the Shewanella genus consists of facultatively aerobic, Gram-negative bacterium which exhibit exceptional plasticity in respiratory capacities. During aerobic conditions, Shewanella utilizes oxygen as a terminal electron acceptor; conversely, under anaerobic conditions, it is able to undertake respiration by reducing alternative terminal electron acceptors such as oxidized metals via extracellular electron transfer mechanisms not yet thoroughly discerned. The aim of this work is to explicate the mechanisms governing the initial bacterial adhesion and subsequent biofilm formation on metallic surfaces. To investigate this dynamic interplay, a combined approach has been followed which couples surface enhanced Raman spectroscopy (SERS) with electrochemical techniques using Shewanella sp. model biofilms. Gold nano-islands deposited on thin glass slides have been chosen as inert model substrates with good uniformity and high surface enhancement factor. Furthermore, the utilization of gold as substrate material not only allowed the differentiation of the sole effect of substrate polarization on bacterial attachment but also enabled a precise adjustment of the surface chemistry and surface energy by means of surface functionalization with organothiol self-assembled monolayers. The results present the correlation of the primary settlement rate of bacteria on metallic substrates with the environmental parameters such as electrolyte composition and pH as well as surface-related properties like hydrophobicity/hydrophilicity and polarization. With the overall strategic goal of transferring this methodology to technical systems the results provide the fundamental basis for the bottom-up design of anti-fouling surfaces. T2 - Electrochemistry 2016 CY - Göslar, Germany DA - 26.09.2016 KW - Bacterial biofilms KW - Electrochemistry KW - Microbiology KW - Surface enhanced Raman spectroscopy KW - Raman spectroscopy KW - Microbiologically induced corrosion KW - Anti-fouling KW - Shewanella KW - Biocorrosion PY - 2016 AN - OPUS4-47243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Chemical and electrochemical interaction mechanisms of metal-reducing bacteria with gold surfaces N2 - Bacterial biofilms are considered one of the salient contributing factors to the deterioration of metals and their alloys, occurring in virtually all environments and across various industrial systems. Considering the sheer magnitude of detrimental effects, it is of pertinent interest to elucidate the interaction mechanisms of sessile bacteria with metal and metal oxide surfaces to facilitate the development of efficient antifouling strategies. A common constituent of microbial communities within aquatic and sedimentary settings, the Shewanella genus consists of facultatively aerobic, Gram-negative bacterium which exhibit exceptional plasticity in respiratory capacities. During aerobic conditions, Shewanella utilizes oxygen as a terminal electron acceptor; conversely, under anaerobic conditions, it is able to undertake respiration by reducing alternative terminal electron acceptors such as oxidized metals via extracellular electron transfer mechanisms not yet thoroughly discerned. The aim of this work is to explicate the mechanisms governing the initial bacterial adhesion and subsequent biofilm formation on metallic surfaces. To investigate this dynamic interplay, a combined approach has been followed which couples surface enhanced Raman spectroscopy (SERS) with electrochemical techniques using Shewanella sp. model biofilms. Gold nano-islands deposited on thin glass slides have been chosen as inert model substrates with good uniformity and high surface enhancement factor. Furthermore, the utilization of gold as substrate material not only allowed the differentiation of the sole effect of substrate polarization on bacterial attachment but also enabled a precise adjustment of the surface chemistry and surface energy by means of surface functionalization with organothiol self-assembled monolayers. The results present the correlation of the primary settlement rate of bacteria on metallic substrates with the environmental parameters such as electrolyte composition and pH as well as surface-related properties like hydrophobicity/hydrophilicity and polarization. With the overall strategic goal of transferring this methodology to technical systems the results provide the fundamental basis for the bottom-up design of anti-fouling surfaces. T2 - Electrochemistry 2016 CY - Göslar, Germany DA - 26.09.2016 KW - Biofilms KW - Electrochemistry KW - Biocorrosion KW - Surface enhanced Raman Spectroscopy KW - Bacteria KW - Microbiological induced corrosion KW - Microbiology PY - 2016 AN - OPUS4-47246 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kastanias, Elaine T1 - Chemical interaction mechanisms of metal reducing bacteria on gold surfaces N2 - Bacterial biofilms represent a ubiquitous form of microbial life on Earth. Due to an evolved armory of protean biological responses to external stimuli, bacteria are able to adhere to, colonize and thrive on virtually all surfaces, whether natural or synthetic, even in challenging environmental conditions. In addition to significant health risks, biofilms are among the salient contributors to the deterioration of metals and their alloys, thereby causing safety risks for technical equipment. Hence, understanding the interaction mechanisms of electroactive sessile bacteria with metal surfaces is vital for facilitating the development of efficient control strategies and novel anti-fouling surfaces in various industries and technologies. The present study focusses on a combined spectroelectrochemical approach, melding methods of surface enhanced Raman spectroscopy (SERS) and electrochemical techniques, to investigate the chemical characteristics and redox activities of electroactive bacteria during the initial stages of biofilm formation. Gold has been selected as a model substrate due to its inert character, considerably high surface enhancement factor, as well as its capability to allow surface chemistry modifications and substrate polarization in order to precisely control the surface charge. Square wave voltammetry (SWV) and cyclic voltammetry (CV) studies have been performed for quantitative determination of flavin concentration and electrochemical impedance spectroscopy (EIS) has been utilized to study the changes in electrochemical processes within biofilms during different stages of growth. Shewanella sp. have been chosen as microorganisms within this work due to their versatile exoelectrogenic respiratory behavior and their distinct ability to reduce metals via extracellular electron transfer mechanisms involving self-secreted electron shuttle redox molecules such as flavins. To further explicate the process of diffusion of flavins within biofilms, a model system has been developed to simulate the structural features of the bacterial extracellular polymeric substances typically found in biofilms. This has been achieved by creating hydrogel films comprised of calcium-cross-linked alginate. The results demonstrate an interplay of factors contributing to the initial phases of bacterial settlement and biofilm formation as a function of environmental parameters. Furthermore, the results allow insight into the diffusion of flavins, much like they would in a natural biofilm, and how their redox behavior affects the biofilm development. T2 - 232nd ECS Meeting CY - National Harbor, MD, USA DA - 01.10.2017 KW - Biofilms KW - Electrochemistry KW - Microbiology KW - Bacterial Extracellular Electron Transfer Mechanisms KW - Surface Enhanced Raman Spectroscopy KW - Spectroelectrochemical Techniques KW - Biocorrosion PY - 2017 AN - OPUS4-47248 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kastanias, Elaine A1 - Özcan Sandikcioglu, Özlem T1 - Chemical and electrochemical interaction mechanisms of metal-reducing bacteria with gold surfaces N2 - Bacterial biofilms are considered one of the salient contributing factors to the deterioration of metals and their alloys, occurring in virtually all environments and across various industrial systems. Considering the sheer magnitude of detrimental effects, it is of pertinent interest to elucidate the interaction mechanisms of sessile bacteria with metal and metal oxide surfaces to facilitate the development of efficient antifouling strategies. A common constituent of microbial communities within aquatic and sedimentary settings, the Shewanella genus consists of facultatively aerobic, Gram-negative bacterium which exhibit exceptional plasticity in respiratory capacities. During aerobic conditions, Shewanella utilizes oxygen as a terminal electron acceptor; conversely, under anaerobic conditions, it is able to undertake respiration by reducing alternative terminal electron acceptors such as oxidized metals via extracellular electron transfer mechanisms not yet thoroughly discerned. The aim of this work is to explicate the mechanisms governing the initial bacterial adhesion and subsequent biofilm formation on metallic surfaces. To investigate this dynamic interplay, a combined approach has been followed which couples surface enhanced Raman spectroscopy (SERS) with electrochemical techniques using Shewanella sp. model biofilms. Gold nano-islands deposited on thin glass slides have been chosen as inert model substrates with good uniformity and high surface enhancement factor. Furthermore, the utilization of gold as substrate material not only allowed the differentiation of the sole effect of substrate polarization on bacterial attachment but also enabled a precise adjustment of the surface chemistry and surface energy by means of surface functionalization with organothiol self-assembled monolayers. The results present the correlation of the primary settlement rate of bacteria on metallic substrates with the environmental parameters such as electrolyte composition and pH as well as surface-related properties like hydrophobicity/hydrophilicity and polarization. With the overall strategic goal of transferring this methodology to technical systems the results provide the fundamental basis for the bottom-up design of anti-fouling surfaces. T2 - Electrochemistry 2016 CY - Goslar, Germany DA - 26.09.2016 KW - Biofilms KW - Electrochemistry KW - Microbiology KW - Bacterial Extracellular Electron Transfer Mechanisms KW - Surface Enhanced Raman Spectroscopy KW - Spectroelectrochemical Techniques KW - Biocorrosion PY - 2016 AN - OPUS4-47249 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moldovan, R.-P. A1 - Wenzel, B. A1 - Teodoro, R. A1 - Neumann, W. A1 - Dukic-Stefanovic, S. A1 - Kraus, Werner A1 - Rong, P. A1 - Deuther-Conrad, W. A1 - Hey-Hawkins, E. A1 - Krügel, U. A1 - Brust, P. T1 - Studies towards the development of a PET radiotracer for imaging of the P2Y1 receptors in the brain: synthesis, 18F-labeling and preliminary biological evaluation N2 - Purine nucleotides such as ATP and ADP are important extracellular signaling molecules in almost all tissues activating various subtypes of purinoreceptors. In the brain, the P2Y1 receptor (P2Y1R) subtype mediates trophic functions like differentiation and proliferation, and modulates fast synaptic transmission, both suggested to be affected in diseases of the central nervous system. Research on P2Y1R is limited because suitable brain-penetrating P2Y1R-selective tracers are not yet available. Here, we describe the first efforts to develop an 18F-labeled PET tracer based on the structure of the highly affine and selective, non-nucleotidic P2Y1R allosteric modulator 1-(2-[2-(tert-butyl)phenoxy]pyridin-3-yl)-3- [4-(trifluoromethoxy)phenyl]urea (7). A small series of fluorinated compounds was developed by systematic modification of the p-(trifluoromethoxy)phenyl, the urea and the 2-pyridyl subunits of the lead compound 7. Additionally, the p-(trifluoromethoxy)phenyl subunit was substituted by carborane, a boron-rich cluster with potential applicability in boron neutron capture therapy (BNCT). By functional assays, the new fluorinated derivative 1-{2-[2-(tert-butyl)phenoxy]pyridin-3-yl}-3-[4-(2-fluoroethyl) phenyl]urea (18) was identified with a high P2Y1R antagonistic potency (IC50 ¼10 nM). Compound [18F] 18 was radiosynthesized by using tetra-n-butyl ammonium [18F]fluoride with high radiochemical purity, radiochemical yield and molar activities. Investigation of brain homogenates using hydrophilic interaction chromatography (HILIC) revealed [18F]fluoride as major radiometabolite. Although [18F]18 showed fast in vivo metabolization, the high potency and unique allosteric binding mode makes this class of compounds interesting for further optimizations and investigation of the theranostic potential as PET tracer and BNCT agent. KW - Purine P2Y1 receptors KW - Positron emission tomography KW - Brain PET tracers KW - Radiometabolites KW - Micellar chromatography KW - Hydrophilic interaction chromatography PY - 2019 DO - https://doi.org/10.1016/j.ejmech.2019.01.006 SN - 0223-5234 VL - 165 SP - 142 EP - 159 PB - Elsevier CY - Amsterdam AN - OPUS4-47253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - The future of analytical sciences: Trends and challenges N2 - What is the future of Analytical Sciences? The talk starts with a definition, comparing the current view with that from 1968. How do wie set trends? How do we get Analytics inside? Some examples of "Big Science" are given and discussed in relation to a definition of AS. How does AS face the current Grand Challenges? As exaples for something significant, several exaples are presented, such as Climate Change of Hydrogen Storage. Another important trand are eScience and automation concepts for AS, which are highlighted. But (Analytical) Science has to be politcal in our times to face Fake News and to breake barriers! T2 - Sonderkolloquium Abteilung 1 "Analytische Chemie; Referenzmaterialien" CY - Berlin, Germany DA - 05.10.2018 KW - Analytical science KW - Grand challenges KW - Big science KW - Fake news KW - Climate change PY - 2018 AN - OPUS4-47285 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schoenhals, Andreas T1 - Structure property relationships of thin polymer films N2 - Polymers at interfaces play a major role in a broad variety of applications ranging from engineering purposes (for instance polymer based nanocomposites) to high tech implications (for instance light emitting diodes). Here, thin films with thicknesses down to few nanometers are prepared on different substrates as model systems for polymer composites. The thin films are investigated by a combination of surface analytical and volume sensitive methods. As surface analytical methods atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and contact angle measurements (CAM) are employed. As volume sensitive broadband dielectric spectroscopy (BDS), specific heat spectroscopy (SHS), and ellipsometry are used. Especially attention is paid to understand the glass transition behavior of thin films because the glass transition is the key phenomenon determines the application of polymers also in thin films. To understand the glass transition behavior of thin films, which is controversially discussed in literature, a three layer model is discussed. Firstly, a mobile surface layer is assumed at polymer air interface of the film due to missing of segment/segment interactions. Secondly, in the middle of the film a bulk-like layer should be expected. Thirdly, for polymers having non-repulsive interactions with the substrate an irreversibly adsorbed layer is expected to be formed. Due the adsorption the molecular mobility of the segments in this layer is slowed down. What is measured for the glass transition of thin films is a complicated average of all of these effects. The different layers are hardly to address separately. Therefore, in the presentation especially model systems are selected and investigated to verify the layer model. T2 - Seminarvortrag Universität Dortmund CY - Dortmund, Germany DA - 29.01.2019 KW - Thin polymer films PY - 2019 AN - OPUS4-47289 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winkelmann, A. A1 - Nolze, Gert A1 - Cios, G. A1 - Tokarski, T. T1 - Mapping of local lattice parameter ratios by projective Kikuchi pattern matching N2 - We describe a lattice-based crystallographic approximation for the analysis of distorted crystal structures via Electron Backscatter Diffraction (EBSD) in the scanning electron microscope. EBSD patterns are closely linked to local lattice parameter ratios via Kikuchi bands that indicate geometrical lattice plane projections. Based on the transformation properties of points and lines in the real projective plane, we can obtain continuous estimations of the local lattice distortion based on projectively transformed Kikuchi diffraction simulations for a reference structure. By quantitative image matching to a projective transformation model of the lattice distortion in the full solid angle of possible scattering directions, we enforce a crystallographically consistent approximation in the fitting procedure of distorted simulations to the experimentally observed diffraction patterns. As an application example, we map the locally varying tetragonality in martensite grains of steel. KW - EBSD KW - Scanning electron microscopy KW - Orientation refinement PY - 2018 DO - https://doi.org/10.1103/PhysRevMaterials.2.123803 SN - 2475-9953 VL - 2 IS - 12 SP - 123803, 1 EP - 15 PB - American Physical Society CY - College Park, MD AN - OPUS4-47296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhua, L A1 - Ewert, Uwe A1 - Xianga, X. A1 - Pengc, Y. A1 - Wanga, X. T1 - Synchrotron phase-contrast CT to segment the structure boundaries of a TRISO-coated particle N2 - Tri-structural Isotropic (TRISO)-coated particle is the fission energy source and the first safety barrier in high temperature gas-cooled reactors (HTGRs). The integrity of TRISO particle should be carefully tested before operation because the shape may affect the failure possibility of the particles, leading to increased risk of fission product release. Due to the large difference in density between the kernel and the coating layers in TRISO particles, traditional X-ray radiography cannot achieve a good image quality in terms of identifying coating layers reliably, while phase-contrast CThas the advantageof being sensitive to boundaries. This paperpresents a non-destructive test and evaluation (NDT&E) method to facilitate 3-dimensional (3D) measurement of a TRISO particle's structure, using a synchrotron phase-contrast CT. After reconstructed, the TRISO particle was rendered in a 3D space and the thickness and asphericity of the TRISO particle's layers were measured. It was found that the thickness of coating layers of the tested particle obeys Gaussian distribution. The deviation of thicknesses of the kernel and the other four layers is −2.42%, −16.32%, 26.51%, 0.98% and 7.49% compared with the design parameters. The deviation of asphericity of the kernel, IPyC and OPyC layers is −11.51%, −0.41% and 3.39%, respectively. The effect of the deviations on the temperature distribution and failure probability calculation of the particle will be investigated in the future. KW - TRISO KW - 3D visualization KW - 3D particle analysis KW - Three-dimensional measurement PY - 2019 DO - https://doi.org/10.1016/j.ndteint.2019.01.003 VL - 103 SP - 12 EP - 18 PB - Elsevier Ltd. AN - OPUS4-47303 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - May the Force be with you - Mechanochemical syntheses studied in situ N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic, metal-organic, and inorganic compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms remain often unclear. In the last years, have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy. Here, we present an in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time. Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. T2 - Seminar Universität Montpellier CY - Montpellier, France DA - 24.01.2019 KW - Mechanochemistry KW - In situ PY - 2019 AN - OPUS4-47261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - New insights in mechanochemical processes using real-time in situ investigations N2 - Use of synchrotron radiation for special sample conditions. Recent work of the group at BESSY II. T2 - DESY Usermeeting Satelite Workshop CY - Hamburg, Germany DA - 22.01.2019 KW - XRD KW - In situ KW - Rietveld KW - Synchrotron PY - 2019 AN - OPUS4-47262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - High temperature oxidation/sulfidation meets X-ray absorption near edge structure spectroscopy (XANES) N2 - Ferritic-martensitic alloys with 12-16 % Cr in weight are subject to devices for various energy systems, such as coal power plants and waste incineration plants. These materials are exposed to a highly corrosive environment which lead to a degradation of the material. Especially the simultaneous oxidation and sulfidation is thereby of special interest. Proper spatially resolved measurements that determine not only chemical compositions but phases are rare. However, precise phase identification and quantification of corrosion products within the multi-phase corrosion scales is a key aspect to understand diffusion paths of metal ions and gas ions/molecules. This study investigated Fe-Cr model alloys with Cr contents from 0 to 13 % in weight in 0.5 % SO2 and 99.5 % Ar atmosphere to aim in a fundamental and systematic analysis. Samples were aged at 650 °C for time scales from 12 h to 250 h. The results presented here correspond to depth dependent phase identification of oxide and sulphide phases in the corrosion scales by using X-ray absorption near edge spectroscopy (XANES). Per sample a series of ca. 20 spots (1-5 µm spot size) from scale-gas to scale-metal interface were measured. XANES spectroscopy was performed at the Fe-K edge (7.11 keV) on polished cross sections. The collected spectra were fitted to a combination of reference materials to quantify the present phases at different positions within the scale.The phase distribution differs with Cr content and the Cr diffusion through pure Fe-oxide and mixed Fe-Cr-oxide phases is discussed. T2 - EFC Workshop "High Temperature Corrosion" CY - Frankfurt am Main, Germany DA - 26.09.2018 KW - High temperature corrosion KW - XANES PY - 2018 AN - OPUS4-47277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - Early stages of high temperature oxidation/sulfidation studied by synchrotron x-ray diffraction and spectroscopy N2 - Ferritic high temperature alloys are widely used as boiler tube and heat exchanger materials in coal, biomass and co-fired power plants. All technologies have in common that the applied materials are exposed to different temperatures, process pressures and reactive atmospheres that lead to a change of the material properties and a further degradation of the material. Material changes caused by aging in highly corrosive and toxic gases such as SO2 are mainly studied ex situ after the reaction is finished. The solid material is deposited in the atmosphere for a certain period of time, and material changes are then examined by various microscopic techniques such as optical microscopy (OM), electron microprobe analysis (EMPA), scanning electron microscopy (SEM and TEM) and X-ray diffraction (XRD). Nevertheless, extensive efforts were made to study material changes of high temperature alloys under oxidizing and reducing atmospheres by environmental scanning electron microscopy or in situ TEM techniques However, the possibilities of microscopic in situ techniques are very limited for the use of highly corrosive and toxic gases such as SO2. Since Sulfur induced corrosion at temperatures relevant for coal and biomass fired power plants, which is causing breakaway oxidation and sulfide precipitation at grain boundaries, is still of scientific interest, the current work focuses on the effect of SO2 in an initial stage of corrosion of ferritic alloys. For the analysis of early stages of combined oxidation and sulphidation processes of Fe-Cr model alloys the usage of a light furnace to conduct a rapid reactive annealing experiment is feasible. Previous studies presented distinct results of the influence of chromium on early high temperature corrosion by SO2 by this technique and subsequent classical metallographic analyses. However, it is still not possible to trace the corrosion mechanism in real time by conducting single aging experiments. The current work introduces two different approaches to study the initial stages of high temperature oxidation processes by applying above state of the art X-ray diffraction and spectroscopy methods. One part focuses on the real time observation of the formation of corrosion products such as oxides and sulfides by energy dispersive X-ray diffraction (EDXRD). The potential of this technique to study crystallization and growth processes of thin films in a reactive environment in real time was previously shown for different compound semiconductors. This approach was now applied to follow oxidation and sulphidation processes of ferritic model alloys in SO2 and SO2/H2O environments. The diffraction signals of the X-rays were detected during the corrosion process and the peak area and positions were analyzed as a function of time. This procedure enables monitoring external oxide growth and material loss in real time in an early stage of corrosion. The other part of the current work presents the possibilities of X-ray absorption near edge structure spectroscopy (XANES) to characterize oxide scales and their growth mechanisms. Precise phase identification and quantification of corrosion products in a multi-phase oxide/sulfide scale is a pre-requisite to understand diffusion paths of metal ions and gas components. It is a challenging task to distinguish structurally similar reaction products such as Fe3O4 and FeCr2O4 especially in thin films with texture effects by diffraction. To illustrate for example Cr-out diffusion of an alloy throughout an inner and external oxide scale the differentiation of Fe3O4 and FeCr2O4 is indispensable. XANES uses the photoionization effect at the metal absorption edge in an aging product and accesses by this structural and chemical information. The current work uses XANES at the Fe-K and Cr-K absorption edge to identify various aging products grown as thin layers on alloys after short time aging experiments. A reaction chamber for combining high temperature oxidation experiments with surface sensitive X-ray absorption near edge structure spectroscopy will be introduced and first results of XANES on scales at high temperatures will be presented. T2 - ISHOC 2018 CY - Matsue, Japan DA - 22.10.2018 KW - Corrosion KW - Sulfidation KW - In situ KW - Diffraction KW - XANES PY - 2018 AN - OPUS4-47278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dreyer, Christian T1 - Composite mit strukturintegrierter Sensorik N2 - Der Vortrag gibt einen Überblick über aktuelle Möglichkeiten zur Integration von sensorischen Funktionen in Leichtbauwerkstoffe, mit Fokus auf Faserverbundkunststoffe (FVK). Neben den unterschiedlichen Arten der eingesetzten Sensoren werden auch deren Arbeitsweisen, Anwendungsbereiche und Anwendungsbreiten erläutert. Es erfolgt eine Diskussion der Auswirkungen der Integration von Sensoren in die Bauteilstruktur und daraus abgeleitet eine Betrachtung der Vor- und Nachteile der einzelnen Methoden. Das lernen die Teilnehmer im Vortrag: Integration von Sensoren in Faserverbundstrukturen Anwendungen von Sensorik Auswirkungen der Funktionsintegration auf die Composite T2 - 3. Anwendertreff Leichtbau CY - Würzburg, Germany DA - 04.12.2018 KW - Zerstörungsfreie Prüfung KW - Ultraschallprüfung KW - Faserverbundwerkstoffe PY - 2018 AN - OPUS4-47313 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - van de Kreeke, Johannes T1 - Databases for proficiency testing schemes and certified reference materials - EPTIS and COMAR N2 - Databases for proficiency testing schemes and certified reference materials - EPTIS and COMAR are introduced against the background of market developments. T2 - IUPAC/CITAC Workshop on Quality of Test Results for Conformity Assessment of a Chemical Composition, Isranalytica 2019 CY - Tel Aviv, Israel DA - 21.01.2019 KW - COMAR KW - Reference materials (RM) KW - EPTIS KW - Proficiency testing (PT) PY - 2019 AN - OPUS4-47314 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Hard X-ray spectroscopy and imaging at the BAMline and MySpot beamlines at BESSY II (Berlin, Germany) N2 - Overview of the X-ray based analytical methods conducted at the BAMline and µSpot Beamline for structure analysis. T2 - Pccr2 + AfLS conference CY - Accra, Ghana DA - 29.01.2019 KW - X-ray spectroscopy KW - Synchrotron KW - Beamline KW - Material characterization PY - 2019 AN - OPUS4-47319 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kittner, Maria T1 - Thermoanalytical methods for the optimisation of microplastic analysis in freshwater sediment samples N2 - Results of various thermoanalytical techniques are presented for the analysis of microplastics in sediment samples. The homogeneity and the representativness of samples war controlled, as well as steps of separation and microplastic detection by these techniques. T2 - MICRO CY - Lanzarote, Spain DA - 19.11.2018 KW - Water KW - Microplastics KW - Sampling KW - Sampling techniques PY - 2018 AN - OPUS4-47322 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Quantitative biocide profile measurements by calibrated XPS N2 - This presentation provides an update on recent results from quantitative XPS-measurements of real and artificial biofilms. NAP-XPS, lab-based XPS and synchrotron-based XPS was used to obtain a vertical concentration profile of iodine in agarose-films with information depth ranging from 1 to 18 nm. T2 - Project meeting MetVBadBugs CY - Turin, Italy DA - 05.02.2019 KW - Biofilms KW - NAP-XPS KW - XPS KW - Iodine KW - Agarose PY - 2019 AN - OPUS4-47332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - EMPIR project ALCOREF - certified forensic alcohol reference materials N2 - The talk presents a short summary of the EMPIR Project ALCOREF "Certified forensic alcohol reference materials". An interlaboratory comparison of analytical methods for the quantification of ethanol in water and a comparison of certified ethanol in water reference materials are proposed. T2 - EURAMET SCOA Meeting CY - Brno, Czech Republic DA - 05.02.2019 KW - Breath alcohol analyser KW - Certified reference material KW - Interlaboratory comparison PY - 2019 AN - OPUS4-47333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ewert, Uwe A1 - Zscherpel, Uwe A1 - Vogel, Justus A1 - Zhang, F. A1 - Long, N.X. A1 - Nguyen, T.P. T1 - Visibility of Image Quality Indicators (IQI) by Human Observers in Digital Radiography in Dependence on Measured MTFs and Noise Power Spectra N2 - Digital radiographic images were analysed to predict the visibility of image quality indicators (IQI), based on normalized noise power spectra (NNPP) and modulation transfer function (MTF) measurements. The fixed pattern noise of some digital detectors result in different noise spectra, which influence the visibility of different IQIs, depending on the hole diameter. Studies, based on measurement of basic spatial resolution and contrast to noise ratio were performed together with presampled MTF measurements and the NNPS in dependence on the spatial frequency. Plate hole IQIs, step hole IQIs, and equivalent penetrameter sensitivity (EPS) IQIs based on ASTM E 746 were measured to verify the influence of the different parameters. Modelling of digital images was used to verify the applied numeric tools. A study has been performed for imaging plates and digital detector arrays to analyse differences. Formulas for the prediction of the visibility functions for hole type IQIs are derived. In consequence the standards for characterization and classification of computed radiography (ASTM E 2446) and radiography with DDAs (ASTM E 2597) need to be revised. T2 - 12th ECNDT 2018 CY - Gothenburg, Sweden DA - 11.06.2018 KW - Image evaluation KW - Computed radiography (CR) KW - Digital Detector Array (DDA) KW - Detail detection PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473486 UR - www.ndt.net/?id=22967 SN - 1435-4934 VL - 23 IS - 8 SP - 1 EP - 7 PB - NDT.net CY - Kirchwald AN - OPUS4-47348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ewert, Uwe A1 - Zscherpel, Uwe A1 - Zhang, F. A1 - Long, N.X. A1 - Phong, N. T1 - Essentielle Parameter zur numerischen Abschätzung der Sichtbarkeit von Bildgüteprüfkörpern in der digitalen Radiographie N2 - Die Voraussetzungen für die Vorhersage der Sichtbarkeit von Bildgüteprüfkörpern (BPK) wurden seit Beginn der kommerziellen Anwendung der technischen Radiographie diskutiert und in diversen nationalen und internationalen Standards festgeschrieben. Diese Fragen werden nach Einführung der digitalen Radiographie und der CT wieder neu diskutiert. Draht BPKs wurden in Deutschland seit 1935 (DIN 1915: 1935) und später in den meisten europäischen Ländern benutzt. In den USA und Frankreich wurden vorzugsweise BPKs mit Löchern verwendet (ASTM E 1025 seit 1984 oder E 1742 seit 1992 bzw. die Vorgängernorm MIL STD-543 seit 1962). Jetzt werden auch die Umrechnungsnormen zur Erkennbarkeit von Draht zu Loch-BPKs in Frage gestellt. ISO 19232-3, der französische RCCM-Kode einerseits und ASTM E 747 und ASME BPVC Section V Tab. T-276 andererseits unterscheiden sich erheblich bei den Anforderungen im Bereich hoher Wandstärken (Hochenergieradiographie). Untersuchungen dazu werden vorgestellt. Mit Einführung der digitalen Detektoren ändern sich auch die Rauschspektren. Durch die Herstellung werden insbesondere bei Speicherfolien "Rauschmuster" eingeprägt, die bei hohen Belichtungsdosen sichtbar werden. Diese veränderten Rauschspektren ergeben auch veränderte Erkennungsparameter für menschliche Bildauswerter. Hierzu wurden an ausgewählten Detektoren MTFs (presampled) und normierte Rauschspektren gemessen. Erweiterte Erkennbarkeits-Formeln zur Vorhersage der Sichtbarkeit von BPKs für Bildauswerter und erste Ergebnisse werden vorgestellt. T2 - DGZfP-Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Image quality KW - Computed radiography (CR) KW - Digital Detector Array (DDA), KW - Sichtbarkeit von Anzeigen PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473496 UR - www.ndt.net/?id=23069 VL - 2018 SP - 1 EP - 14 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung e.V. (DGZfP) AN - OPUS4-47349 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brückner, B. A1 - Zscherpel, Uwe T1 - Spektroskopie gepulster Röntgenquellen N2 - Spektren von gepulsten Röntgenquellen wie Blitzröhren, Linearbeschleuniger (LINACs) oder Betatrons lassen sich in der Literatur nicht finden. Eine gängige Lehrmeinung ist, dass sich solche Spektren nicht messen lassen. Deshalb wurden in Zusammenarbeit mit der Goethe-Universität Frankfurt und neuester Messtechnik diese Problematik untersucht. Es wurde ein CeBr3-Szintillator-Kristall mit einem klassischen Photoelektronenvervielfacher (PMT) und einer analogen Übertragungskette verwendet, der über Stunden Integrationszeit nur einen sehr geringen Untergrund detektiert. Als kritischter Punkt stellte sich die geeignete Kollimierung von Quelle und Detektor bei möglichst großem Abstand heraus. Zu diesem Zweck wurde das verwendete 7 MeV-Betatron in einen 3t-Bleibunker betrieben, der ein Austrittsloch von 1 mm für die erzeugte Röntgenstrahlung besaß. Der Detektor wurde mit einem Densimet-Zylinder abgeschirmt. Damit konnte die Bedingung für die Spektroskopie gepulster Quellen erreicht werden: pro Puls darf nur 1 Photon den Detektorkristall erreichen, damit ohne Pile-up seine Energie vermessen werden kann. Trotz schnellster Elektronik war es nicht möglich, mehere Photonen pro Röntgenpuls (beim Betatron ca. 1 Mikrosekunde) spektral richtig aufzulösen. Die gemessenen Spektren zeigen die erwartete Form, wie sie z.B. mit aRTist simuliert werden können. T2 - DGZfP-Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Spektroskopie KW - Betatron KW - Röntgenblitzröhre PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-473505 SP - 1 EP - 2 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung e.V. (DGZfP) AN - OPUS4-47350 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Optimum Magnification Factor in Digital Radiography - Selection Criteria and Formulas N2 - The transition from X-ray film to digital detectors in radiography is accompanied by an increase of unsharpness due to the larger inherent digital detector unsharpness in comparison to film. The basic spatial resolution of digital detectors (see EN ISO 17636-2) is used today to describe this unsharpness. The geometrical unsharpness of the radiographic projection of object structures onto the detector plane is determined by the focal spot size of the X-ray tube and the magnification. The focal spot size is measured today (see ASTM E 1165) from pin hole camera exposures or edge unsharpness (see ASTM E 2903). The final image unsharpness is a result of a convolution of the geometrical and inherent detector unsharpness function, divided by the magnification factor of the object onto the detector plane. Different approximations of this convolution result in ASTM E 1000 and ISO 17636-2 in different optimum values for the magnification factor for a given focal spot size of a X—ray tube and the basic spatial resolution of the detector. The higher contrast sensitivity, an advantage of digital radiography, compared to film radiography is furthermore improved when using higher X-ray voltages as used with film and smaller focal spots of the X-ray tubes. This allows a higher distance between object and detector resulting in reduced object scatter in the image. The interactions between all these parameters will be discussed and simple rules for practitioners will be derived in this contribution. T2 - 12th ECNDT 2018 CY - Gothenburg, Sweden DA - 11.06.2018 KW - Digital Radiology KW - Image unsharpness KW - Optimum magnification PY - 2018 AN - OPUS4-47351 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - DIN EN 12681:2017 für die radiographhische Gußteilprüfung mit Film oder digitalen Detektoren N2 - Vorstellung der Konzepte and Anwendungsbereiche der neuen Norm DIN EN 12681 in 2 Teilen: Film und digitale Prüfung T2 - Röntgentechnologietage 2018 CY - Stockelsdorf bei Lübeck, Germany DA - 20.02.2018 KW - Gussteilprüfung KW - DIN EN 12681:2017 KW - Filmbasierend KW - Digitale Röntgendetektoren PY - 2018 AN - OPUS4-47352 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - DIN EN ISO 17636:2013 für die radiographische Schweißnahtprüfung mit Film oder digitalen Detektoren N2 - Die aktuelle Normentwicklung für radiographische Schweißnahtprüfung wird diskutiert und die Konsequenzen für die praktische Anwendung anhand von Beispielen erläutert. T2 - Röntgentechnologietage 2018 CY - Stockelsdorf bei Lübeck, Germany DA - 20.02.2018 KW - Digitale Radiographie KW - Schweißnahtprüfung KW - DIN EN ISO 17636 PY - 2018 AN - OPUS4-47353 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Aktuelle Normungsaktivitäten in der industriellen Durchstrahlungsprüfung N2 - Neue Normen bei DIN, CEN ISO ASTM und IIW für die industrielle Durchstrahlungsprüfung mit Film und digitalen Detektoren. Stand der Technik und neue Entwicklungen T2 - Radiographie-Forum von Baker Hughes CY - Ahrensburg, Germany DA - 20.06.2018 KW - Wall thickness measurement KW - Aktuelle Normentwicklung KW - Schweißnahtprüfung KW - Digital radiography KW - Computed radiography (CR) KW - Digital Detector Array (DDA) KW - Tangential radiography KW - Image evaluation PY - 2018 AN - OPUS4-47354 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Annual Report of Sub-Commission V-A "Radiography-based weld inspection" N2 - A Summary pf the activities of the IIW sub-commission V-A in 2018 for radiographic weld inspection. T2 - Annual Assembly of IIW CY - Bali, Indonesia DA - 15.07.2018 KW - Radiograpgy KW - Weld Inspection KW - International Institute of Welding PY - 2018 AN - OPUS4-47355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Update on Revision of ISO 24497 - NDT - MMM - Technique N2 - Presentation of the final compromise reached in 2018 for revision of ISO 24497, final draft for voting at ISO can be prepared now. T2 - IIW Annual Assembly 2018 CY - Bali, Indonesia DA - 15.07.2018 KW - NDT - Metal Magnetic Memory KW - Revision of ISO 24497 KW - New ISO draft PY - 2018 AN - OPUS4-47356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Computer Tomography used for inspection of critical Zones in AM parts N2 - Overview on CT for AM, starting from the CT principle, the added value of CT in Additive Manufacturing (AM), examples of CT results on AM workpieces and conclusions. T2 - IIW Annual Assembly 2018, joint seminar on AM CY - Bali, Indonesia DA - 15.07.2018 KW - Computed Tomographie KW - Additive Manufacturing KW - Added Value PY - 2018 AN - OPUS4-47357 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope ratio measurements and certification of iRMs at BAM N2 - This presentation gives a short overview of isotope ratio measurements being carried out in the past few years at BAM in different fields such as plant metabolism, food web structures and archaeology. The corresponding isotope reference materials which have been certified at BAM in parallel are presented as well. Additionally an outlook is being provided on future iRM projects. T2 - Meeting of the Isotope Ratio Working Groupt of CCQM CY - Ottawa, Canada DA - 04.10.2018 KW - Isotope reference material KW - Delta value KW - Isotope amount ratio KW - Traceability KW - Uncertainty PY - 2018 AN - OPUS4-47159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xiao, J. A1 - Vogl, Jochen A1 - Rosner, M. A1 - Deng, L. A1 - Jin, Z. T1 - A validated analytical procedure for boron isotope analysis in plants by MC-ICP-MS N2 - Boron (B) is an essential micronutrient for plant growth. Lack of valid methods for pretreatment and measurement of δ11B in plant restrict applications of it in the biosphere. Dry ashing, one step cation exchange and micro-sublimation were combined to separate and purify boron (B) in plant tissues. The low procedure blank, high B recovery and the accurate δ11B values of the plant reference materials demonstrate that this method is suitable and valid for B pretreatment and δ11B measurement in plant samples by MC-ICP-MS. Based on this method, the δ11B in different plants (Brassica napus, Chenopodium album L, moss, lichen, and Nostoc commune) was analyzed. For Brassica napus, δ11B increased gradually from root to leaf, and then decreased to rapeseed. For the same parts, the δ11B increased from the lower parts to the higher parts. This variation may be due to the B(OH)3 transporter of NIP6;1 and the incorporation of B into the cell. The reason for lower δ11B values in shell and rapeseed compared to those in leaves presumably is to the preferred Transport of borate in the phloem. The largest δ11B fractionation between leaf and root in Brassica napus and Chenopodium album L was +24.2‰ and +26.6‰, respectively. The large variation and fractionation of δ11B within plants indicates that δ11B is a good tracer to study the B translocation mechanisms and metabolism within plants. The δ11B in Nostoc commune, lichen, and moss showed variations of -4.1‰ to +21.5‰, −9.4‰ to +7.3‰, and −18.3‰ to +11. 9‰, respectively. In the same site, δ11B in different plants ranked Nostoc commune>moss>lichen and δ11B in mosses growing in different environment ranked soil>tree>rock. Rain and soil available B are the main B sources for these plants. The δ11B in Nostoc commune, lichen, and moss may be a useful tracer to study the atmospheric B input. In the future, plants culture experiments under certain environments and studies from molecular level are necessary to decipher the variation of δ11B and fractionation mechanisms within plants. KW - Boron isotope KW - Isotopic fractionation KW - Micro-sublimation KW - Plant tissue KW - MC-ICP-MS PY - 2019 DO - https://doi.org/10.1016/j.talanta.2018.12.087 SN - 0039-9140 SN - 1873-3573 VL - 196 SP - 389 EP - 394 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-47160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gaillard, C. A1 - Mech, A. A1 - Wohlleben, W. A1 - Babick, F. A1 - Hodoroaba, Vasile-Dan A1 - Ghanem, A. A1 - Weigel, S. A1 - Rauscher, H. T1 - A technique-driven materials categorisation scheme to support regulatory identification of nanomaterials N2 - Worldwide there is a variety of regulatory provisions addressing nanomaterials. The identification as nanomaterial in a regulatory context often has the consequence that specific legal rules apply. In identifying nanomaterials, and to find out whether nanomaterial-specific provisions apply, the external size of particles is globally used as a criterion. For legal certainty, its assessment for regulatory purposes should be based on measurements and methods that are robust, fit for the purpose and ready to be accepted by different stakeholders and authorities. This should help to assure the safety of nanomaterials and at the same time facilitate their international trading. Therefore, we propose a categorisation scheme which is driven by the capabilities of common characterisation techniques for particle size measurement. Categorising materials according to this scheme takes into account the particle properties that are most important for a determination of their size. The categorisation is exemplified for the specific particle number based size metric of the European Commission's recommendation on the definition of nanomaterial, but it is applicable to other metrics as well. Matching the performance profiles of the measurement techniques with the material property profiles (i) allows selecting the most appropriate size determination technique for every type of material considered, (ii) enables proper identification of nanomaterials, and (iii) has the potential to be accepted by regulators, industry and consumers alike. Having such a scheme in place would facilitate the regulatory assessment of nanomaterials in regional legislation as well as in international relations between different regulatory regions assuring the safe trade of nanomaterials. KW - Nanomaterial KW - Nanoparticles KW - Categorisation scheme KW - EC definition of a nanomaterial KW - Regulatory identification of nanomaterials PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471623 DO - https://doi.org/10.1039/C8NA00175H SN - 2516-0230 SP - 1 EP - 11 PB - The Royal Society of Chemistry AN - OPUS4-47162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohamed, Zainelabdeen H. A1 - Arenz, C. A1 - Soukka, T. T1 - Five-, four- and three-dentate Europium chelates for anion sensing and their applicability to enzymatic dephosphorylation reactions N2 - The design of anion-sensitive probes with sufficient sensitivity and selectivity is a demanding task in analytical sciences and chemical sensor technology. The reversible binding of Anions to lanthanide centers is a possible approach for the development of molecular anion sensors, as reversibility is a prerequisite for continuous sensing and monitoring of enzymatic reactions. Some anion species lead to a strong increase of luminescence intensities and lifetimes by the replacement of luminescence quenching water molecules, though the selectivity of the luminescence response is still a major problem. We synthesized a series of positively charged pyridyl-based multidentate europium complexes (five-, four- and three dentate) including sensitizing chromophores and studied their luminescence intensity and lifetime responses to different polyphosphates, pyrophosphate, phosphate anions, and carboxyanions. The results revealed that the number and symmetry of the binding sites have a significant impact on the response. The five-dentate complex was used for the real-time monitoring of the activity of the ATP hydrolyzing enzyme apyrase. KW - Europium KW - Luminescence KW - Anions KW - Apyrase PY - 2018 UR - https://onlinelibrary.wiley.com/doi/10.1002/slct.201803287 DO - https://doi.org/10.1002/slct.201803287 SN - 2365-6549 VL - 3 IS - 44 SP - 12430 EP - 12439 PB - Wiley-VCH CY - Weinheim AN - OPUS4-47163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El-Khatib, A. H. A1 - Radbruch, H. A1 - Trog, S. A1 - Neumann, B. A1 - Paul, F. A1 - Koch, A. A1 - Linscheid, M. W. A1 - Jakubowski, Norbert A1 - Schellenberger, E. T1 - Gadolinium in human brain sections and colocalization with other elements N2 - Recent recommendations by the Food and Drug Administration1 and the European Medicines Agency2 are to limit the clinical use of linear gadolinium-based contrast agents (GBCAs) due to convincing evidence of deposition in tissues. Macrocyclic GBCA continued to be considered safe, provided that patients have normal renal function. To date, given the low sensitivity of conventional MRI, there has been a debate about the signal increase following the injections of a macrocyclic GBCA. KW - Gadolinium PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471309 DO - https://doi.org/10.1212/NXI.0000000000000515 SN - 2332-7812 VL - 6 IS - 1 SP - e515, 1 EP - 3 PB - American Academy of Neurology AN - OPUS4-47130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - qNMR an der BAM - Aktuelle Aktivitäten und Strategie N2 - Der Vortrag gibt eine Übersicht über aktuelle qNMR-Aktivitäten im Fachbereich 1.4. Dies umfasst beispielsweise die Online-Anwendung zur Prozessüberwachung, aber auch die Reinheitsuntersuchung von Reinstoffkomponenten für die Herstellung von Referenzgasgemischen. Zusätzlich wird ein Ausblick in die aktuelle Strategie hinsichtlich der Rückführung von qNMR-Ergebnissen mittels primärer Referenzmaterialien gegeben. T2 - 10. Sitzung der Next-NMR-Arbeitsgruppe CY - Karlsruhe, Germany DA - 11.12.2018 KW - qNMR KW - NMR-Spektroskopie PY - 2018 AN - OPUS4-47131 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Daum, Werner A1 - Czichos, Horst ED - Grote, Karl-Heinrich ED - Bender, Beate ED - Göhlich, Dietmar T1 - Messtechnik und Sensorik N2 - Für den allgemeinen Maschinenbau wichtige Messtechnik und Sensorik werden grundlegend und anwendungsbezogen beschrieben. KW - Messtechnik KW - Sensorik KW - Maschinenbau PY - 2018 SN - 978-3-662-54804-2 DO - https://doi.org/10.1007/978-3-662-54805-9 SP - W 2 EP - W 44 PB - Springer Vieweg CY - Berlin ET - 25 AN - OPUS4-47132 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Heideklang, René T1 - Data fusion for multi-sensor nondestructive detection of surface cracks in ferromagnetic materials N2 - Fatigue cracking is a dangerous and cost-intensive phenomenon that requires early detection. But at high test sensitivity, the abundance of false indications limits the reliability of conventional materials testing. This thesis exploits the diversity of physical principles that different nondestructive surface inspection methods offer, by applying data fusion techniques to increase the reliability of defect detection. The first main contribution are novel approaches for the fusion of NDT images. These surface scans are obtained from state-of-the-art inspection procedures in Eddy Current Testing, Thermal Testing and Magnetic Flux Leakage Testing. The implemented image fusion strategy demonstrates that simple algebraic fusion rules are sufficient for high performance, given adequate signal normalization. Data fusion reduces the rate of false positives is reduced by a factor of six over the best individual sensor at a 10 μm deep groove. Moreover, the utility of state-of-the-art image representations, like the Shearlet domain, are explored. However, the theoretical advantages of such directional transforms are not attained in practice with the given data. Nevertheless, the benefit of fusion over single-sensor inspection is confirmed a second time. Furthermore, this work proposes novel techniques for fusion at a high level of signal abstraction. A kernel-based approach is introduced to integrate spatially scattered detection hypotheses. This method explicitly deals with registration errors that are unavoidable in practice. Surface discontinuities as shallow as 30 μm are reliably found by fusion, whereas the best individual sensor requires depths of 40–50 μm for successful detection. The experiment is replicated on a similar second test specimen. Practical guidelines are given at the end of the thesis, and the need for a data sharing initiative is stressed to promote future research on this topic. KW - Data fusion KW - Non destructive testing KW - Multi-sensor KW - Surface cracks PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471339 DO - https://doi.org/10.18452/19586 SP - 1 EP - 157 CY - Berlin AN - OPUS4-47133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moldenhauer, Laura A1 - Helmerich, Rosemarie A1 - Köppe, E. A1 - Wittmann, H.-J. T1 - Experimental modeling approach for determining the moisture damping exponent of a bluetooth low energy signal in moist building material N2 - The presented development of a damping model is a research component of an experimental feasibility study about moisture in building materials measured with Bluetooth® Low Energy (BLE) signals. This study may be part of a structural health- and long-term monitoring aiming at early damage detection in the built infrastructure and is increasingly focusing on wireless sensor network technology. It is investigated, how the Received Signal Strength Indicator (RSSI) of a BLE signal, transmitted from the BLE-module embedded in building materials with changing moisture content is damped. The aim of the modelling is the derivation of a damping equation for the formal model to determine the moisture damping exponent to finding a correlation. T2 - 34th Danubia Adria Symposium on Advances in Experimental Mechanics CY - Trieste, Italy DA - 19.09.2017 KW - BLE Bluetooth low energy KW - Sensor network KW - RSSI Received Signal Strength Indicator KW - Structural Health Monitoring KW - Moisture measurements PY - 2018 DO - https://doi.org/10.1016/j.matpr.2018.08.124 SN - 2214-7853 VL - 5 IS - Issue 13, Part 2 SP - 26469 EP - 26792 PB - Elsevier Ltd. CY - Radarweg 29, 1043 NX Amsterdam, The Netherlands AN - OPUS4-47171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumacher, David A1 - Zscherpel, Uwe A1 - Ewert, Uwe T1 - Recent developments of photon counting and energy discriminating detectors for radiographic imaging N2 - The direct detection of X-ray photons into electrical signals is enabled by usage of highly absorbing photo conducting materials (e.g. CdTe) as detection layer of an underlying CMOS semiconductor X-ray image detector. If the read-out speed is high enough (ca. 50 - 100 ns dead time) single X-ray photons can be counted and their energy measured. Read-out noise and dark image correction can be diminished. By setting energy thresholds, selected energy ranges of the X-ray spectrum can be detected or suppressed. This allows material discrimination or reduction of scattered radiation, which results in an enhanced contrast sensitivity. T2 - Far East NDT New Technology & Application Forum (FENDT) CY - Xi'an, China DA - 22.06.2017 KW - Industrial X-ray imaging KW - Photon counting KW - Energy discrimination KW - Dual energy imaging KW - Direct detection PY - 2018 UR - https://ieeexplore.ieee.org/document/8584559 SN - 978-1-5386-1615-4 DO - https://doi.org/10.1109/FENDT.2017.8584559 VL - 2017 SP - 281 EP - 285 PB - IEEE Xplore AN - OPUS4-47175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D. L. A1 - Sander, L. C. A1 - Wise, S. A. A1 - Philipp, Rosemarie A1 - Hein, Sebastian A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Chan, P. A1 - Lee, H. A1 - Tang, H. A1 - Tang, P. A1 - Yip, Y. A1 - Lu, T. A1 - Cheow, P. S. A1 - Teo, T. L. A1 - Sega, M. A1 - Rolle, F. A1 - Baek, S. A1 - Kim, B. A1 - Lee, S. A1 - Cabillic, J. A1 - Fallot, C. A1 - Hua, T. A1 - Dazhou, C. A1 - Changjun, Y. A1 - Chunxin, L. A1 - Hongmei, L. A1 - Lippa, K. A1 - Itoh, N. A1 - Quinn, L. A1 - Prevoo-Franzsen, D. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. A1 - Gündüz, S. A1 - Krylov, A. A1 - Mikheeva, A. A1 - Baldan, A. A1 - van der Hout, J. W. A1 - van der Veen, A. M. H. T1 - CCQM-K131 Low-polarity analytes in a multicomponent organic solution: Polycyclic aromatic hydrocarbons (PAHs) in acetonitrile N2 - Solutions of organic analytes of known mass fraction are typically used to calibrate the measurement processes used to determine these compounds in matrix samples. Appropriate value assignments and uncertainty calculations for calibration solutions are critical for accurate measurements. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2015 the Organic Analysis Working Group (OAWG) sponsored CCQM-K131 "Low-Polarity Analytes in a Multicomponent Organic Solution: Polycyclic Aromatic Hydrocarbons (PAHs) in Acetonitrile". Polycyclic aromatic hydrocarbons (PAHs) result from combustion sources and are ubiquitous in environmental samples. The PAH congeners, benz[a]anthracene (BaA), benzo[a]pyrene (BaP), and naphthalene (Nap) were selected as the target analytes for CCQM-K131. These targets span the volatility range of PAHs found in environmental samples and include potentially problematic chromatographic separations. Nineteen NMIs participated in CCQM-K131. The consensus summary mass fractions for the three PAHs are in the range of (5 to 25) μg/g with relative standard deviations of (2.5 to 3.5) %. Successful participation in CCQM-K131 demonstrates the following measurement capabilities in determining mass fraction of organic compounds of moderate to insignificant volatility, molar mass of 100 g/mol up to 500 g/mol, and polarity pKow < −2 in a multicomponent organic solution ranging in mass fraction from 100 ng/g to 100 μg/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, and (3) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Naphthalene (Nap) KW - Organic calibration solution KW - Polycyclic aromatic hydrocarbon (PAH) PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471442 DO - https://doi.org/10.1088/0026-1394/56/1A/08003 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1A SP - 08003, 1 EP - 102 PB - IOP Science AN - OPUS4-47144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Diepeveen, L. E. A1 - Laarakkers, C. M. M. A1 - Martos, G. A1 - Pawlak, M. E. A1 - Uguz, F. F. A1 - Verbene, K. E. S. A. A1 - van Swelm, R. P. L. A1 - Klaver, S. A1 - de Haan, A. F. J. A1 - Pitts, K. R. A1 - Bansal, S. S. A1 - Abbas, Ioana M. A1 - Fillet, M. A1 - Lefebvre, T. A1 - Geurts-Moespot, A. J. A1 - Girelli, D. A1 - Castagna, A. A1 - Herkert, M. A1 - Itkonen, O. A1 - Olbina, G. A1 - Tomosugi, N. A1 - Westerman, M. E. A1 - Delatour, V. A1 - Weykamp, C. W. A1 - Swinkels, D. W. T1 - Provisional standardization of hepcidin assays: creating a traceability chain with a primary reference material, candidate reference method and a commutable secondary reference material N2 - Hepcidin-25 concentrations measured by various methods differ considerably, complicating interpretation. Here, a previously identified plasma-based candidate secondary reference material (csRM) was modified into a serum-based two-leveled sRM. We validated its functionality to increase the equivalence between methods for international standardization. We applied technical procedures developed by the International Consortium for Harmonization of Clinical Laboratory Results. The sRM, consisting of lyophilized serum with cryolyoprotectant, appeared commutable among nine different measurement procedures using 16 native human serum samples in a first round robin (RR1). Harmonization potential of the sRM was simulated in RR1 and evaluated in practice in RR2 among 11 measurement procedures using three native human plasma samples. Comprehensive purity analysis of a candidate primary RM (cpRM) was performed by state-of-the-art procedures. The sRM was value assigned with an isotope dilution mass spectrometry-based candidate reference method calibrated using the certified pRM. The inter-assay CV without harmonization was 42.1% and 52.8% in RR1 and RR2, respectively. In RR1, simulation of harmonization with sRM resulted in an inter-assay CV of 11.0%, whereas in RR2 calibration with the material resulted in an inter-assay CV of 19.1%. Both the sRM and pRM passed international homogeneity criteria and showed long-term stability. We assigned values to the low (0.95 ± 0.11 nmol/L) and middle concentration (3.75 ± 0.17 nmol/L) calibrators of the sRM. Standardization of hepcidin is possible with our sRM, which value is assigned by a pRM. We propose the implementation of this material as an international calibrator for hepcidin-25. KW - Reference material KW - Peptide KW - Biomarker KW - Bioanalysis KW - Mass spectrometry KW - LC-MS/MS KW - Iron deficiency KW - MALDI-TOF MS KW - UHPLC-MS/MS KW - ELISA KW - Immunoassay PY - 2018 DO - https://doi.org/10.1515/cclm-2018-0783 SN - 1437-4331 SN - 1434-6621 VL - 57 IS - 6 SP - 864 EP - 872 PB - De Gruyter CY - Berlin AN - OPUS4-47153 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tleuova, A. A1 - Schenderlein, Matthias A1 - Mutaliyeva, B. A1 - Aidarova, S. A1 - Sharipova, A. A1 - Bekturganova, N. A1 - Miller, R. A1 - Grigoriev, D. T1 - Selection and study of alkoxysilanes as loading in submicrocapsules for self-lubricating coatings N2 - The possibility and conditions for the formation of nano- or submicrocapsules loaded with hydrophobic active ingredients (alkoxysilanes) into the matrix of coatings with self-lubricating effect are considered. The optimal composition of the alkoxysilane submicrocapsules, and their physicochemical properties were determined. The longer the radical chain length is, the lower is the rate of hydrolysis, and, accordingly, the more stable is the formed emulsion. The methods of laser correlation spectroscopy in measuring the size and zeta potentials of the submicrocapsules with different loads of the active agent allowed to determine the optimal ratios of the active ingredients. The optimal concentration of the active agent is between 4 and 9%. Based on contact angle studies, octadecyltrimethoxysilane was selected as optimum compound. The introduction of 4 wt% of octadecyltrimethoxysilane reduces the friction coefficient of coatings by 20–30% under vibrating motion and by 15–20% under continuous motion. The data obtained can also be useful for the encapsulation of other hydrophobic active agents and for various other purposes, for example, for the introduction of biocidal agents. KW - Microencapsulation KW - Spontaneous emulsification KW - Self-lubricating coating KW - Antifriction coefficient KW - Alkoxysilanes PY - 2019 DO - https://doi.org/10.1016/j.colsurfa.2018.12.018 SN - 0927-7757 SN - 1873-4359 IS - 563 SP - 359 EP - 369 PB - Elsevier AN - OPUS4-47233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Denkler, Tilman T1 - Comparison of the operation of accreditation bodies in Europe N2 - This study was designed to examine and compare the operation of accreditation bodies in Europe. A management tool, the Process Maturity Benchmarking Tool (PMBT), was elaborated and validated by applying it to various accreditation bodies. By applying the tool, the values of indicators were determined, thus enabling a comparison of the accreditation bodies despite different operational processes and organizational forms. The management tool PMBT is based on the analysis of selected processes with high relevance for the operation of accreditation bodies. The processes are derived from a process map designed for accreditation bodies in a universally applicable way. The indicators used to characterize the processes come from two sources: The first source relates to data already available from internal databases, reports, financial audits etc. The second source is derived from a self-evaluation of process maturity performed by the accreditation bodies. The criteria for evaluating process maturity were designed by applying the criteria of the EFQM excellence model 2013 of the European Foundation for Quality Management (EFQM) to the processes identified in the process map. The project Comparison of the Operation of Accreditation Bodies in Europe comprised three stages. In the first stage, the processes of accreditation bodies were systematically analyzed. A process map was developed and processes of special relevance for the performance of accreditation bodies were identified and underpinned by indicators as described above. In the second stage, the processes of the German accreditation body DAkkS were assigned to the tool. This stage was used to check and modify the indicators when necessary. In the third stage, the transferability of the model was analyzed by extension to seven other accreditation bodies operating in Europe. The third stage of the project ended with a workshop attended by the eight accreditation bodies, which was used to present and discuss the results of the comparison and to identify best practices. KW - Accreditation KW - Benchmarking PY - 2019 SP - 1 EP - 83 AN - OPUS4-47235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst A1 - Wiggenhauser, Herbert T1 - The LAUS: First Applications of a New System for Ultrasonic Imaging of Very Concrete Structures N2 - The LAUS (Large Aperture Ultrasonic System) has been developed to image very thick concrete structures, which are not accessible for commercial systems. The device and the corresponding software is the result of joint Research of BAM, an ultrasonic instrument manufacturer and University of Kassel, Germany. It consists of 12 separate Arrays of 32 point-contact shear wave transducers each, which can be deployed in flexible configurations. Each array is combined with battery and transmitter, receiver and wireless communication electronics. Three case histories are presented. First the system was deployed on a 5-m thick heavily reinforced foundation slab. The reflection of the slab’s bottom was imaged clearly. In addition, a multiple reflection was registered, thus giving hope that even thicker elements might be imaged by the instrument. Second, the LAUS was used to investigate a massive bridge girder where a heavy rainstorm during concreting had led to imperfections that were visible after removing the formwork was removed. The LAUS could image tendon ducts in 1.8m depth and the backwall closely behind them. Some limited areas showed blurred reflections and were checked by drill holes; these areas were affected by diffuse damage which could be repaired by injections. Third, a large retaining wall was checked for thickness. Meanwhile, the LAUS has been used in underground waste deposits (nuclear and other) for quality assurance of sealing plugs. A confirmed penetration depth of about 7 m has been reached. T2 - SMT and NDT-CE 2018 CY - New Brunswick, NJ, USA DA - 27.08.2018 KW - LAUS (Large Apertur Ultrasonic System) KW - Ultrasonic echo KW - Deep penetration KW - Concrete PY - 2019 UR - https://asnt.org/smt18papers SN - 978-1-57117-456-7 VL - 11/19 SP - 208 EP - 213 PB - The American Society for Nondestructive Testing, Inc. CY - Columbus, OH, USA AN - OPUS4-47238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulow, Anicó A1 - Witte, S. A1 - Beyer, S. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, H. A1 - Streli, C. T1 - A new experimental setup for time- and laterally-resolved X-ray absorption fine structure spectroscopy in a 'single shot' N2 - In this work, a new setup for dispersive XAFS measurements is presented. This reproducible and scanningfree setup yields both time- and laterally-resolved XAFS experiments in a ‘single-shot’. It allows a straightforward adjustment for probing different elements covering many relevant applications in materials science. An incoming energetic broadband beam is diffracted by a Si (111) crystal after passing through the sample and collected by an area sensitive detector. Depending on the energy range of the incoming beam, XANES and/or EXAFS spectra can be recorded with a time resolution down to 1 s. The feasibility of this setup was demonstrated at the BAMline at BESSY II (Berlin, Germany) with reference Fe and Cu foils and the results are hereby presented and discussed. Additionally, an application where time resolution on the second scale is required is briefly evaluated. The presented example concerns studying early stages of zinc(II)2-methylimidazolate (ZIF-8) crystallization. This is particularly important for biomedical applications. KW - X-ray spectroscopy KW - X-ray absorption fine structure KW - Time-resolved KW - Laterally-resolved KW - Experimental setup PY - 2019 DO - https://doi.org/10.1039/c8ja00313k SN - 0267-9477 SN - 1364-5544 VL - 34 IS - 1 SP - 239 EP - 246 PB - Royal Society of Chemistry CY - London AN - OPUS4-47207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thiel, Erik A1 - Ziegler, Mathias A1 - Studemund, Taarna T1 - Localization of subsurface defects in uncoated aluminum with structured heating using high-power VCSEL laser arrays N2 - We report on photothermal detection of subsurface defects by coherent superposition of thermal wave fields. This is made possible by structured heating using high-power VCSEL laser arrays whose individual emitter groups can be arbitrarily controlled. In order to locate the defects, we have developed a scanning method based on the continuous wavelet transformation with complex Morlet wavelet using the destructive interference effect of thermal waves. This approach can also be used for thermally very fast and highly reflective materials such as uncoated aluminum. We show that subsurface defects at an aspect ratio of defect width to defect depth down to 1/3 are still detectable in this material. KW - Thermography KW - Heat diffusion KW - Laser thermography KW - Structured heating KW - NDT KW - Subsurface defects KW - Thermal wave KW - VCSEL KW - Wavelet transformation PY - 2019 DO - https://doi.org/10.1007/s10765-018-2478-9 SN - 1572-9567 SN - 0195-928X VL - 40 IS - 2 SP - 17, 1 EP - 13 PB - Springer Science+Business Media, LLC, part of Springer Nature 2019 AN - OPUS4-47208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas A1 - Perez Alonso, M. T1 - Is there a need for a new standard for determination of steel cleanliness using high frequency ultrasonic testing? N2 - Increased use of high performance steel (HPS) for demanding applications calls for non-destructive ultrasonic testing methods which is covered by standards like SEP 1927 (1) and ASTM E588 (2). Here, an adaption of standards like increasing sensitivity and resolution of ultrasonic testing may be needed in order to improve determination of steel cleanliness. Modern requirements on standardization in that field have been evaluated during the INCAFAT project “A novel approach for rating fatigue-initiating inclusions in highly demanding steel” which was funded by the European Commission. Main results of this research show that an adapted standard should be open to different type of specimen due to the diversity in application. This includes a wide range from bars, rings and plates as well as different inspection sensitivities. An adapted standard should be open to the definition of the volume to be investigated and open to be selected by the user. Furthermore, for enhanced resolution the frequency range should be extended to higher frequencies. The use of focal beam probes shall be mandatory and probes should be selected according to the geometry of the specimen. Therefore, calibration procedures have to be improved significantly to allow proper sizing of indications. Indication height shall be directly transferred into an equivalent disc shaped reflector taking distance amplitude curves as well as signal amplitude distribution and signal travel time into account. A new standard draft proposal taking all these requirements into account has been filed in the frame of the INCAFAT project and is now on discussion. T2 - ECNDT - European Conference on Non-Destructive Testing 2018 CY - Gothenburg, Sweden DA - 11.06.2018 KW - Cleaniliness purity grade ultrasound non-destructive volumetric measurement standard PY - 2018 AN - OPUS4-47210 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Is phased array the future in modern ultrasonic rail inspection? N2 - Compared to standard ultrasonic testing methods the application of phased arrays offers advantages and flexibility by the electronic steering possibilities to control the transmitted and received sound fields as well as the image based evaluation of the recorded scans. For more than one decade phased array systems have been introduced and used in the railway sector for the inspection of wheelsets in the workshops. Up to the present field applications of phased array systems in rail inspection are rather rare. On the other hand a lot of scientific work on rail testing using phased arrays has been carried out in the recent past. Mechanized ultrasonic rail inspection poses strong challenges e.g. due to the harsh environment, complex flaw types and high inspection speeds. Different tasks have to be carried out by non-destructive testing ranging from manufacturing inspection of thermite welds to in-service inspection for operational induced flaws in the rail head, rail web and rail foot as well as rolling contact fatigue. This work will give an overview and categorization of different present approaches for rail testing using phased array. Phased array systems typically offer digital image based inspection results. This make these systems become the perfect candidates to feed inspection data into a modern big data based workflow, using e.g. cloud computing, signal processing and data fusion for recording, positioning and tracking of flaws and artefacts in rails and to gain additional benefit. Evaluation of promising innovative approaches and solutions for phased array based ultrasonic rail inspection in the frame of “Industry 4.0” will be discussed. T2 - QNDE - Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Burlington, VT, USA DA - 15.07.2018 KW - Rail Inspection Phased Array Ultrasound PY - 2018 AN - OPUS4-47211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Microplastics: Degradation properties of polymers in the environment N2 - The accumulation of plastics leaked into the environment achieve a high perception in the last years. It is uncontroversial that often an uncontrolled, high consumption of plastic products and a poor waste management resulted in plastic findings all over in the environment. However, less is known about the relevant pathways and fate of plastic in the environment. Especially plastic fragments smaller 5 mmm, so called microplastics, achieve a high attention, because their amount and risks arising from these fragments are still unknown. The basic mechanisms of plastic or more precise, of different polymer degradation processes are often not considered, resulting in unrealistic statements. For generation of fundamental understanding of this problem we developed in the last years a fast thermoanalytical method for identification and mass quantification of microplastics in complex samples. The presentation will also give a short introduction about polymer degradation. T2 - Environmental Geosciences Seminar CY - Vienna, Austria DA - 19.11.2018 KW - Microplastic KW - Analysis KW - Standardisation PY - 2018 AN - OPUS4-47182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Kunststoffe in der Umwelt: Elastomere, Thermoplaste und Duroplaste – worüber sprechen wir eigentlich und was sind die analytischen Herausforderungen? N2 - Übersichtsvortrag zur Thematik Kunststoffe in der Umwelt. Es werden Aspekte zu Definitionen, Eigenschaften und Analytischen Möglichkeiten und Herrausforderungen angesprochen. T2 - Arbeitsgespräch der Ressortforschungseinrichtungen CY - Berlin, Germany DA - 26.11.2018 KW - Mikroplastik KW - Umwelt KW - Polymere Eigenschaften PY - 2018 AN - OPUS4-47183 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Turning up the heat: a thermoanalytical approach for the detection of microplastics N2 - The presentation deals with the analysis of plastics in environmental samples using the TED-GC-MS method. The method and its working principles are presented, method characteristics and application examples are given. Advantages and disadvantages compared to other methods are highlighted. T2 - Linnaeus Eco-Tech 2018 CY - Kalmar, Sweden DA - 19.11.2018 KW - Microplastics KW - Tire wear KW - Thermoanalysis KW - TED-GC-MS PY - 2018 AN - OPUS4-47185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Comparison of the performance of ultrasonic non-destructive testing methods on inspection of fibre reinforced plastics N2 - In the last twenty years, components made of fibre-reinforced plastic became a prominently used material in safety-relevant structures. Periodic in-service inspection of these structures using reliable non-destructive testing methods became a relevant issue in the field. The goal of the EMRP-funded project VITCEA (Validated Inspection Techniques for Composites in Energy Applications) aims on the evaluation of the performance of various non-destructive testing methods on the inspection of fibre-reinforced plastics. In this talk the results of the comparison of different ultrasonic testing methods will be discussed. There are two challenges for the ultrasonic inspection of fibre-reinforced plastics. Firstly, different material properties of the fibre and the resin cause anisotropic acoustical behaviour of the material. Secondly, the physical layout of fibre layers leads to complex structures of fibre-reinforced plastic parts, and thus to a complex acoustical response. Both result in a reduction of the signal to noise ratio and make interpretation of measurement results rather extensive. During the VITCEA project, the acoustical behaviour of fibre-reinforced plate materials has been simulated. Specimens with artificial flaws for the evaluation of the detection thresholds have been designed and manufactured. Various mechanized ultrasonic testing methods including phased-array sensors, air-coupled transducers, immersion tank testing and contact technique have been evaluated on the specially designed specimen. Laboratory scale tests and a round robin test have been carried out. The probability of detection and the detection thresholds for each method have been estimated. T2 - ECNDT - European Conference on Non-Destructive Testing 2018 CY - Gothenburg, Sweden DA - 11.06.2018 KW - Comparison ndt methods FRP fibre reinforced plastics ultrasound PY - 2018 AN - OPUS4-47213 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Ist die Ultraschall-Phased-Array-Technik die Zukunft der mechanisierten Schienenprüfung im Zeitalter von Bahn 4.0? N2 - Die Ultraschall Phased-Array Technik bietet durch die variable elektronische Steuerung des Schallfeldes gegenüber konventioneller Prüftechnik Vorteile bei vielen Prüfaufgaben, sowohl bei der Datenaufnahme als auch der bildhaften Bewertung. Die mechanisierte Schienenprüfung stellt sehr hohe Anforderungen an die Prüftechnik insbesondere durch die hohen Prüfgeschwindigkeiten von bis zu 20 m/s. Im Rahmen dieses Vortrags wird evaluiert, welche Lösungsansätze auf Basis der Ultraschall Phased-Array Technik vielversprechend erscheinen für einen Einsatz im Umfeld von Bahn 4.0. T2 - 10. Fachtagung ZfP im Eisenbahnwesen CY - Wittenberge, Germany DA - 13.03.2018 KW - Eisenbahn KW - Phased Array KW - Ultraschall KW - Mechanisierte Schienenprüfung PY - 2018 AN - OPUS4-47214 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas A1 - Casperson, Ralf A1 - Rühe, Sven A1 - Mook, Gerhard T1 - Signal processing for non-destructive testing of railway tracks N2 - Increased speed, heavier loads, altered material and modern drive systems result in an increasing number of rail flaws. The appearance of these flaws also changes continually due to the rapid change in damage mechanisms of modern rolling stock. Hence, interpretation has become difficult when evaluating non-destructive rail testing results. Due to the changed interplay between detection methods and flaws, the recorded signals may result in unclassified types of rail flaws. Methods for automatic rail inspection (according to defect detection and classification) undergo continual development. Signal processing is a key technology to master the challenge of classification and maintain resolution and detection quality, independent of operation speed. The basic ideas of signal processing, based on the Glassy-Rail-Diagram for classification purposes, are presented herein. Examples for the detection of damages caused by rolling contact fatigue also are given, and synergetic effects of combined evaluation of diverse inspection methods are shown. T2 - QNDE - Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Provo, UT, USA DA - 16.07.2017 KW - Rail KW - Inspection KW - Train KW - Ultrasound KW - Signal KW - Processing PY - 2018 DO - https://doi.org/10.1063/1.5031528 VL - 1949 SP - 030005-1 EP - 030005-7 AN - OPUS4-47217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg A1 - Spranger, Holger A1 - Ewert, Uwe T1 - THz Applications for Non-Destructive Testing N2 - Up to now THz-TDS-systems aren’t considered to be nondestructive testing facilities for large scale industrial applications, despite it was proven that they provide a comprehensive set of quality parameters. A practical approach to bring THz-TDS in addition to already existing testing systems into the industrial mainstream is systematic development of future test procedures and test facilities for dielectrics. For this purpose polyeth-ylene test specimen with introduced artefacts were designed, to evaluate the detection sensitivity of Time of Flight measurements based on dielectrics. SAFT reconstructed tomograms are presented which visualize the sizes and location of artificially introduced flaws. T2 - 2017 Far East NDT New Technology & Application Forum (FENDT) CY - XI'an, China DA - 22.06.2017 KW - THz radiation KW - Dielectric materials KW - Image reconstruction KW - Terahertz synthetic aperture PY - 2018 DO - https://doi.org/10.1109/FENDT.2017.8584511 VL - 12 SP - 272 EP - 276 PB - IEEE Conference Publication CY - USA AN - OPUS4-47220 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Determination of chromatographic parameters of a miniaturized AF4 channel and its comparison with a conventioanl AF4 channel N2 - The performance of a miniaturized channel for the separation of polymer and metal nanoparticles (NP) using Asymmetrical Flow Field-Flow Fractionation (AF4) was investigated and compared with a conventional AF4 system. To develop standard separation methods, experimental parameters like cross flow, gradient profile and injection time were varied and optimized. Corresponding chromatographic parameters were calculated and compared. Our results indicate that the chromatographic resolution in the miniaturized channel is lower, whereas significantly shorter analyses time and less solvent consumption were obtained. Moreover, the limit of detection (LOD) and limit of quantification (LOQ) obtained from hyphenation with a UV-detector are obviously lower than in a conventional channel, which makes the miniaturized channel interesting for trace analysis. T2 - BAM Seminar CY - Berlin, Germany DA - 31.08.2016 KW - Nanoparticles separation asymetrical flow field flow fractionation PY - 2016 AN - OPUS4-47190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Zengchao A1 - Meier, Florian A1 - Weidner, Steffen ED - Weidner, Steffen T1 - Comparison of miniaturized and conventional asymmetrical flow field flow fractionation (AF4) channels for nanoparticle separation N2 - The performance of a miniaturized channel for the separation of polymer and metal nanoparticles (NP) using Asymmetrical Flow Field-Flow Fractionation (AF4) was investigated and compared with a conventional AF4 system. To develop standard separation methods, experimental parameters like cross flow, gradient profile and injection time were varied and optimized. Corresponding chromatographic parameters were calculated and compared. Our results indicate that the chromatographic resolution in the miniaturized channel is lower, whereas significantly shorter analyses time and less solvent consumption were obtained. Moreover, the limit of detection (LOD) and limit of quantification (LOQ) obtained from hyphenation with a UV-detector are obviously lower than in a conventional channel, which makes the miniaturized channel interesting for trace analysis. KW - Nanoparticles separation asymetrical flow field flow fractionation PY - 2017 DO - https://doi.org/10.3390/separations4010008 SN - 2297-8739 VL - 4 IS - 1 SP - 8, 1 EP - 11 AN - OPUS4-47196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wasmer, Paul A1 - Prager, Jens T1 - Eindimensionaler phononischer Kristall zur Schallisolierung in Stäben T1 - One-dimensional phononic crystal for sound insulation in rods N2 - Die Untersuchung von Schallausbreitung in periodischen Strukturen ist aktuell von großem Interesse für eine zielgerichtete Beeinflussung von Schallwellen in einem großen Frequenzbereich. Hierbei liegt der Fokus insbesondere auf den phononische Kristalle (PnK’s), einer periodischen Anordnung von Streuzentren in einer Matrix. PnK’s können neben anderen Anwendungen, wie der Sensoranwendung oder der Nutzung als effektiver Wellenleiter, als Schallisolator dienen. In dieser Arbeit wird ein neuartiger PnK aus einer periodischen Anordnung von Zylindern untersucht, welcher zur Schallisolation verwendet werden kann. Zunächst wird die Struktur simuliert, dabei wird ein achsensymmetrisches Modell mit einem 3D-Modell verglichen. Im Anschluss wird die simulierte Geometrie gefertigt und vermessen. N2 - The analysis of acoustic wave behavior in periodic structures is of great interest for the targeted manipulation of acoustic waves in a wide frequency range. In the focus are phononic crystals (PnC's), a periodic arrangement of scatterers in a host matrix. They can be used for various aspects, for example for sensor applications or as effectiv waveguides, but also for sound insulation. In this work, a new PnC consisting of a periodic arrangement of cylinders, which can be used for sound insulation, is investigated. To begin with, the geometry is simulated and an axisymmetric and a 3D-model are compared. The simulated geometry is fabricated and transmission behavior is measured. KW - Phononischer Kristall KW - Ultraschallmessung KW - Akustischer Isolator KW - Stabstruktur KW - Rod structure KW - Acoustic insulation KW - Phononic crystal KW - Ultrasonic measurement PY - 2019 DO - https://doi.org/10.1515/teme-2018-0065 SN - 0171-8096 VL - 86 IS - 2 SP - 66 EP - 72 PB - De Gruyter CY - Oldenbourg AN - OPUS4-47478 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - 16RPT02 ALCOREF - Certified forensic alcohol reference materials N2 - The presentation summarises main achievements obtained in the first half of the EMPIR project ALCOREF. T2 - EMPIR Mid-term Review Conference 2019 CY - Berlin, Germany DA - 28.02.2019 KW - Certified reference material KW - Breath alcohol analyser KW - EMPIR PY - 2019 AN - OPUS4-47482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ickert, Stefanie A1 - Schwaar, Timm A1 - Springer, A. A1 - Grabarics, M. A1 - Riedel, Jens A1 - Beck, S. A1 - Pagel, K. A1 - Linscheid, M. W. T1 - Comparison of the fragmentation behavior of DNA and LNA single strands and duplexes N2 - DNA and locked nucleic acid (LNA) were characterized as single strands, as well as double stranded DNA-DNA duplexes and DNA-LNA hybrids using tandem mass spectrometry with collision-induced dissociation. Additionally, ion mobility spectrometry was carried out on selected species. Oligonucleotide duplexes of different sequences – bearing mismatch positions and abasic sites of complementary DNA 15-mers – were investigated to unravel general trends in their stability in the gas phase. Single stranded LNA oligonucleotides were also investigated with respect to their gas phase behavior and fragmentation upon collision-induced dissociation. In contrast to the collision-induced dissociation of DNA, almost no base loss was observed for LNAs. Here, backbone cleavages were the dominant dissociation pathways. This finding was further underlined by the need for higher activation energies. Base losses from the LNA strand were also absent in fragmentation experiments of the investigated DNA-LNA hybrid duplexes. While DNA-DNA duplexes dissociated easily into single stranded fragments, the high stability of DNA-LNA hybrids resulted in predominant fragmentation of the DNA part rather than the LNA, while base losses were only observed from the DNA single strand of the hybrid. KW - Oligonucleotide fragmentation KW - Locked nucleic acids KW - Collision induced dissociation (CID) KW - Double strands KW - Ion mobility spectrometry PY - 2019 DO - https://doi.org/10.1002/jms.4344 VL - 54 IS - 5 SP - 402 EP - 411 PB - Wiley AN - OPUS4-47485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - About Standardization and Analytics of Microplastics N2 - Presentation about national and international standardization of microplastic analysis, as well as the project RUSEKU T2 - Industrievereinigung Chemiefaser e.V. CY - Frankfurt, Germany DA - 26.02.2019 KW - Standardisation KW - Microplastic KW - Analysis PY - 2019 AN - OPUS4-47577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Mikroplastik in der Umwelt und im Trinkwasser: Einordnung der Relevanz und der Methodik N2 - Überblick zur Thematik Mikroplastik mit speziellem Fokus auf Trinkwasser T2 - 20. Jahrestagung Trinkwasserringversuche Nordrhein-Westfalen – Niedersachsen CY - Osnabrück, Germany DA - 06.03.2019 KW - Trinkwasser KW - Umwelt KW - Mikroplastik PY - 2019 AN - OPUS4-47578 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Plastik im Boden, Aktueller Forschungsstand N2 - Der Vortrag gibt einen Überblick über ein laufendes Vorhaben zum Thema Mikroplastik in Böden. T2 - NUA-Veranstaltung "Plastik in Natur und Umwelt" CY - Münster, Germany DA - 08.03.2019 KW - Mikroplastik KW - Böden KW - Analytik PY - 2019 AN - OPUS4-47579 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Harmonisierung von Untersuchungsverfahren für (Mikro-)Plastik in der Umwelt N2 - Im Rahmen der Thematik "Recycling von Kunststoffen" wird die Thematik "Mikroplastik" vorgestellt T2 - Berliner Recycling- und Rohstoffkonferenz CY - Berlin, Germany DA - 11.03.2019 KW - Mikroplastik KW - Standarisierung KW - Analytik PY - 2019 AN - OPUS4-47582 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Analytik von Mikroplastik mittels Thermoextraktion Desorption Gas Chromatographie Massen Spektrometrie (TED-GC-MS): Nun auch die Luft? N2 - Der Vortrag gibt eine Überblick über die Messung von Mikroplastik mittels TED-GC-MS mit speziellem Fokus auf Luftgetragene Partikel T2 - Odour and Emissions of Plastic Materials CY - Kassel, Germany DA - 19.03.2019 KW - Mikroplastik KW - Standarisierung KW - Analytik PY - 2019 AN - OPUS4-47583 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - CAT-Technologie zur Bestimmung der Haftfestigkeit Dünner Schichten N2 - Der Vortrag widmet sich der „CAT-TECHNOLOGIE ZUR BESTIMMUNG DER HAFTFESTIGKEIT DÜNNER SCHICHTEN“ und beschreibt die Punkte „Motivation –CAT-Technologie“ (CAT: Centrifugal Adhesion Testing) und die „Haftfestigkeit von Schichten“, (Ag-Schichten auf N-BK7 Glas, Cr- und Al-Schichten auf Borofloat 33 Glas, Au-Schichten auf N-BK7 Glas und SiO2-Schichten auf CR39 Polymer) im Einzelnen. T2 - EFDS, Workshop: Haft- und Antihaftschichten CY - Dresden, Germany DA - 31.01.2019 KW - CAT-Technologie KW - Centrifugal Adhesion Testing KW - Dünne Schichten KW - Haftfestigkeit PY - 2019 AN - OPUS4-47489 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Thermography using High-Power Laser Arrays N2 - Due to their high irradiance and wide modulation bandwidth, high-power lasers open up a wide field of application. For example, the classical methods of pulse and lock-in thermography can be realized in high quality. In addition, structured heating is also possible by using arrays of such lasers. This makes it possible to implement new thermographic methods, such as interference-based detection of cracks or super resolution. T2 - Fifth NDTonAIR Training Event: Thermography Workshop CY - Linz, Austria DA - 13.02.2019 KW - Thermography KW - Laser Thermography KW - Super Resolution KW - Thermal Waves KW - NDT PY - 2019 AN - OPUS4-47491 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kruschwitz, Sabine A1 - Zhang, Z. A1 - Weller, A. A1 - Nordsiek, S. T1 - Effect of evaporative drying on complex conductivity spectra of sandstones N2 - Dehydration is a common process occurring in natural environments, rocks, and building materials. Suitable methods for monitoring the changing moisture content should be identified. We have investigated the impact of dehydration of sandstones on complex conductivity spectra. Spectral induced polarization measurements were performed on five sandstone samples during evaporative drying. The complex conductivity spectra indicate considerable changes with decreasing saturation. The relationship between conductivity and saturation can be described by a power law known as the second empirical Archie equation. Separate saturation exponents have been determined for the real and imaginary parts of conductivity. The imaginary part of conductivity indicates higher saturation exponents for the investigated sandstones compared to the real part. Obviously, the saturation exponents depend on the method used for changing water saturation. Evaporative drying, which is used in our experiments, causes an increase of pore-water salinity and results in lower saturation exponents for the real part of conductivity but higher exponents for the imaginary part in comparison with the classical imbibition/Drainage technique. We evaluate a theoretical approach that considers the influence of pore water salinity on the saturation exponents of the real and imaginary parts of conductivity. The complex conductivity spectra are processed by a Debye decomposition procedure. The resulting integrating parameters such as direct current resistivity, total chargeability, normalized chargeability, and mean relaxation time indicate a power law dependence on saturation. Our experiments indicate that the imaginary part of conductivity and normalized chargeability have a high sensitivity related to the drying process of rocks and might be suitable indicators to Monitor the changes of moisture content in sandstones. KW - Saturation KW - Spectral induced polarization KW - Sandstones KW - Evaporative drying PY - 2019 DO - https://doi.org/10.1190/GEO2018-0054.1 SN - 0016-8033 VL - 84 IS - 1 SP - MR61 EP - MR72 PB - SEG - Society of Exploration Geophysicists CY - Tulsa, Okla. AN - OPUS4-47499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gramse, G. A1 - Schönhals, Andreas A1 - Kienberger, F. T1 - Nanoscale dipole dynamics of protein membranes studied by broadband dielectric microscopy N2 - We investigate the nearfield dipole mobility of protein membranes in a wide frequency range from 3 kHz to 10 GHz. The results of our nanoscale dielectric images and spectra of bacteriorhodopsin (bR) reveal Debye relaxations with time constants of τ ∼ 2 ns and τ ∼ 100 ns being characteristic of the Dipole moments of the bR retinal and α-helices, respectively. However, the dipole mobility and therefore the protein biophysical function depend critically on the amount of surface water surrounding the protein, and the characteristic mobility in the secondary structure is only observed for humidity levels <30%. Our results have been achieved by adding the frequency as a second fundamental dimension to quantitative dielectric microscopy. The key elements for the success of this advanced technique are the employed heterodyne detection scheme, the broadband electrical signal source, a high frequency optimized cabling, development of calibration procedures and precise finite element modelling. Our study demonstrates the exciting possibilities of broadband dielectric microscopy for the investigation of dynamic processes in cell bioelectricity at the individual molecular level. Furthermore, the technique may shed light on local dynamic processes in related materials science applications like semiconductor Research or nano-electronics. KW - Broadband dielectric microscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475230 DO - https://doi.org/10.1039/c8nr05880f SN - 2040-3372 VL - 11 IS - 10 SP - 4303 EP - 4309 PB - RSC AN - OPUS4-47523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim T1 - Zerstörungsfreie Lokalisierung von Flüssigwasser in Schichtaufbauten N2 - Die Idee des Dissertationsprojekts ist der parallele Einsatz des Radarverfahrens und der Neutronensonde zur Lokalisierung von Feuchteschäden in Fußbodenaufbauten. Hierbei soll die integrale Messweise der Neutronensonde durch die vertikale Information des Radarsignals ergänzt werden, um zukünftig auf zerstörende Sondierungsbohrungen verzichten zu können. Primäres Ziel ist eine automatisierte und zerstörungsfreie Klassifizierung und Quantifizierung verschiedener Schadensfälle im Fußboden, welche zur Abschätzung und Auswahl des Sanierungsaufwands dienen soll. In systematischen Laborstudien an modular aufgebauten Referenzprobekörpern werden die Nachweisgrenzen der beiden Verfahren für unterschiedliche, häufig anzutreffende Fußbodenaufbauten untersucht. Hierfür wurde ein Satz verschiedenster Estrichprobekörper gefertigt und deren Hydratisierungsprozess gravimetrisch und mit den benannten Feuchtemessverfahren beobachtet. In der laufenden Auswertung konnten bereits signifikante Signalmerkmale der Radarmessungen extrahiert, sowie dessen Korrelation zum Feuchteverlauf der Proben gezeigt werden. Der modulare Aufbau der Fußbodenschichten zur Simulation von gängigen Feuchteschäden folgt im Anschluss. Über Datenfusion und Signalverarbeitung sollen so innovative Auswertungsansätze entwickelt und deren Validität an realen Schadensfällen geprüft werden. T2 - Doktorandenseminar BAM Abt. 8 CY - Berlin, Germany DA - 25.02.2019 KW - Radar KW - Feuchte KW - Fußboden KW - Signalmerkmale KW - Datenfusion KW - Maschinelles Lernen PY - 2019 AN - OPUS4-47526 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nöller, Renate T1 - Scientific analysis of the Humboldt fragments N2 - The presented Humboldt Codices are from the early colonial period of Mexico and originate from different localities 1. typical indigen colors and mixtures: cochineal (red), indigo (blue and green), carbon (black), mangle, zacatlaxcalli, organic (brown, yellow)- critical! 2. colonial influence: iron gall ink for writing 3. single fragments belong together: are cut (fragments IX-XII), from Mizquahuala distributed (VII, XIII, XIV, [XV]) (VII, XIII in Mexico, XIV in Paris) T2 - Workshop: Manuscripta Americana: Aufarbeitung einer Sammlung; Staatsbibliothek zu Berlin - PK CY - Berlin, Germany DA - 14. Februar 2019 KW - Humboldt Codices KW - XRF-, VIS- FTIR-spectroscopy KW - Dyes PY - 2019 AN - OPUS4-47589 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hübert, Thomas A1 - Majewski, J. A1 - Banach, Ulrich A1 - Detjens, Marc A1 - Tiebe, Carlo T1 - Response Time Measurement of Hydrogen Sensors N2 - The efficiency of gas sensor application for facilitating the safe use of hydrogen depends considerably on the sensor response to a change in hydrogen concentration. Therefore, the response time has been measured for five different-type commercially available hydrogen sensors. Experiments showed that all these sensors surpass the ISO 26142 standard; for the response times t90 values of 2 s to 16 s were estimated. Results can be fitted with an exponential or sigmoidal function. It can be demonstrated that the results on transient behaviour depend on both the operating parameters of sensors and Investigation methods, as well as on the experimental conditions: gas change rate and concentration jump. T2 - 7th International Conference on Hydrogen Safety (ICHS 2017) CY - Hamburg, Germany DA - 11.09.2017 KW - Response time KW - Hydrogen sensor KW - Test facility KW - t90 value PY - 2017 SN - 978-88-902391 SP - 1251 EP - 1261 AN - OPUS4-47592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Plasma induced generation of acoustic waves N2 - Due to the multi-physical appearance of gas discharges the possibilities of interaction with their surrounding environment are very wide. Some of the most common applications are surface or material modification, light sources and electric propulsion. Since atmosphere pressure plasma generate a huge amount of thermal energy caused by collisions in the sheath, this temperature alternation is also able to produce acoustic waves in the ambient gas volume (as lightning and thunder). The plasma-chemical interaction provides the most significant Impact to the generated heat and electro-hydrodynamic force, detectable by acoustic sensors. This contribution gives an overview of experimental acoustic analysis of diffuse coplanar surface dielectric barrier discharges and provides a basic physical straight-forward model. In addition to the characterization, possible applications (e.g. plasma acoustic loudspeaker or transducer for air-coupled ultrasonic testing) concerning these discharge types are presented. T2 - DPG Frühjahrstagung (SMuK) CY - Munich, Germany DA - 17.03.2019 KW - Gas discharges KW - Atmospheric pressure plasma KW - Diffuse dielectric barrier discharges PY - 2019 AN - OPUS4-47595 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bente, Klaas T1 - Quantitative, zeiteffiziente, winkel- und frequenzaufgelöste Analyse von Elektretwandlern im Hör- und Ultraschallbereich N2 - Elektretwandler sind sensitive und immer verschleißresistentere Schallwandler, wodurch sie verbreitet Einsatz im Hör- und Ultraschallbereich finden. Geladene, zelluläre Polypropylen-Folien eignen sich besonders gut als Wandlermaterial aufgrund ihrer, verglichen mit Piezokompositen, hundertfach niedrigeren akustischen Impedanz bei gleichem piezoelektrischem Koeffizienten. Doch das winkel- und frequenzabhängige Verhalten der Wandler ist kaum untersucht und wenig quantifiziert. In dieser Arbeit wird gezeigt, dass diese Folien eine schichtdickenabhängige Sensitivität zwischen 0.1 mV/Pa und 10 mV/Pa aufwiesen. Ein Maximum in der Sensitivität fand sich nahe ihrer mechanischen Resonanzfrequenz im Ultraschallbereich, aber auch im niederfrequenten Hörschallbereich. Darüber hinaus konnte die Winkelabhängigkeit der Sensitivität charakterisiert werden. Die Analyse konnte dabei zeiteffizient mit einem breitbandig emittierenden, thermoakustischen Wandler umgesetzt werden, sodass pro Winkel eine Messung für die Berechnung der Übertragungsfunktion des Wandlers genügte. Quantifiziert wurden die Ergebnisse durch das einmalige Vermessen des Schallfeldes des Emitters mittels Laser-Doppler-Vibrometrie. Mit den erzielten Ergebnissen wurde zum einen das komplexe Sensitivitätsverhalten der Wandler untersucht, aber auch eine grundlegende Methodik aufgezeigt, wie Wandler quantitativ, multivariat charakterisiert werden können. Winkel- und frequenzaufgelöste Sensitivitäten erlauben zum einen die Analyse der Anwendbarkeit der Wandler für sämtliche Einsatzgebiete, zum anderen stehen so Rückschlüsse über die mechanische Dynamik von Elektretfolien in Aussicht, da deren Sensitivität direkt mit ihrem Elastizitätsmodul skaliert. T2 - DAGA 2019 CY - Rostock, Germany DA - 18.03.2019 KW - Luftultraschall KW - Ultraschall KW - Elektretwandler KW - Thermoakustik KW - Wandlercharakterisierung PY - 2019 AN - OPUS4-47597 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hofmann, Michael A1 - Moufid, M. A1 - El Bari, N. A1 - Tiebe, Carlo A1 - Bouchikhi, B. T1 - Testing of a developed multigas sensor system for outdoor odour nuisance monitoring N2 - This work presents the testing of a developed elec¬tronic nose for outdoor odour nuisance monitoring. The sensor system consists of a sampling system, a measuring cell equipped with commercially available low-cost gas sensor elements and a data acquisition system. The sensor testing showed that the developed prototype is able to distinguish, identify and partially quantify individual odorous substances like ethanol, ammonia and hydrogen sulphide. Ethanol and ammonia could even be detected below or near their odour threshold. T2 - ALLSENSORS 2019, The Fourth International Conference on Advances in Sensors, Actuators, Metering and Sensing CY - Athens, Greece DA - 24.02.2019 KW - Electronic nose KW - Outdoor odour KW - Machined olfaction KW - Sensor testing PY - 2019 UR - https://www.thinkmind.org/index.php?view=article&articleid=allsensors_2019_2_40_70065 SN - 978-1-61208-691-0 SN - 2519-836X SP - 27 EP - 28 PB - The ThinkMind Digital Library AN - OPUS4-47505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hofmann, Michael T1 - Testing of a Developed Multigas Sensor System for Outdoor Odour Nuisance Monitoring N2 - This work presents the testing of a developed electronic nose for outdoor odour nuisance monitoring. The sensor system consists of a sampling system, a measuring cell equipped with commercially available low-cost gas sensor elements and a data acquisition system. The sensor testing showed that the developed prototype is able to distinguish, identify and partially quantify individual odorous substances like ethanol, ammonia and hydrogen sulphide. Ethanol and ammonia could even be detected below or near their odour threshold. T2 - ALLSENSORS 2019, The Fourth International Conference on Advances in Sensors, Actuators, Metering and Sensing CY - Athens, Greece DA - 24.02.2019 KW - Electronic nose KW - Outdoor odour KW - Machined olfaction KW - Sensor testing PY - 2019 AN - OPUS4-47506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Surface characterisation of bacteria and biofilms by NAP-XPS N2 - INTRODUCTION: X-ray photoelectron spectroscopy (XPS) provides elemental and chemical information from the outermost ~10 nm of the sample surface. This is in the same order of magnitude as the thickness of the outer bacterial membrane of gram-negative bacteria, as well as outer membrane molecules as exopolysaccharides and lipopolysaccharides, commonly attached to the cell surface. With the development of near-ambient pressure (NAP)-XPS, bacteria can be analysed with minimal sample preparation. This is in contrast to ultra-high vacuum XPS, where complex sample preparation including freeze-drying or fast-freezing is required, a treatment that may introduce artefacts or degrade the biological constituents. METHODS: EnviroESCA is a laboratory based NAP-XPS instrument, equipped with a monochromated Al Kα radiation source and a differentially pumped energy analyser connected to an exchangeable sample environment, a basic build-up is displayed in Figure 1c. It allows for measurements in various gas-atmospheres, including water vapor, which makes it possible to characterise bacteria and other biological samples close to their natural, hydrated state. Artificial model-biofilms of exopolysaccharides, planktonic Pseudomonas Fluorescens and biofilms of Escherichia Coli have been characterised in hydrated and dried state. RESULTS: High-resolution XPS-spectra from carbon, oxygen, nitrogen and phosphorous can be assigned to carbohydrates, lipids and proteins in general agreement with litterature2,3. Especially the carbon 1s peak is of interest (see Figure 1a and b), which reveal components originating from aliphatic carbon, single bounded carbon and double bounded/acetal carbon. A series of measurements of an E. coli biofilm from 11 mbar in humid environment to 1 mbar air reveal changes in the C1s peak, which suggests that the bacterial surface undergo substantial change. DISCUSSION & CONCLUSIONS: Bacterial samples can be analysed under near-ambient pressure conditions in various states of hydration with minimal sample preparation. Such investigations of bacterial cell wall surfaces are essential for studying biological interfaces at work. T2 - Biointerfaces International Conference CY - Zurich, Switzerland DA - 14.08.2018 KW - Bacteria KW - E. coli KW - NAP-XPS KW - Biofilms KW - Alginate PY - 2018 AN - OPUS4-45717 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik T1 - Two-dimensional interference of photothermally generated moving thermal waves N2 - Structured illumination using high-power diode lasers generates a two-dimensional interference of thermal waves. In addition, the sources and the sample are moving relative to each other. Using different configurations, we investigate the validity of the temporal and spatial superposition principle of the heat diffusion equation for these cases both experimentally and by numerical-analytical modelling. Furthermore, we investigate the potential of this approach for non-destructive testing. T2 - 14th Quantitative Infrared Thermography Conference CY - Berlin, Germany DA - 24.05.2018 KW - Thermography KW - Thermal Wave KW - VCSEL KW - Laser KW - Thermal diffusion PY - 2018 AN - OPUS4-45621 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Schönhals, Andreas A1 - Frick, B. A1 - Zorn, R. ED - Kremer, Friedrich ED - Loidl, Alois T1 - The scaling of the molecular dynamics of liquid crystals as revealed by broadband dielectric, specific heat, and neutron spectroscopy N2 - A combination of different complementary methods is employed to investigate scaling of the molecular dynamics of two different liquid crystals. Each method is sensitive to different kind of fluctuations and provides therefore a different window to look at the molecular dynamics. In detail, broadband dielectric spectroscopy is combined with specific heat spectroscopy and neutron scattering. As systems the nematic liquid crystal E7 and a discotic liquid crystalline pyrene are considered. First of all it was proven that both systems show all peculiarities which are characteristic for glassy dynamics and the glassy state. Especially for the nematic liquid crystal E7 it could be unambiguously shown by a combination of dielectric and specific heat spectroscopy that the tumbling mode is the underlying motional process responsible for glassy dynamics. Dielectric investigations on the discotic liquid crystalline pyrene reveal that at the phase transition from the plastic crystalline to the hexagonal columnar liquid crystalline phase the molecular dynamics changes from a more strong to fragile temperature dependence of the relaxation rates. Moreover a combination of results obtained by specific heat spectroscopy with structural methods allows an estimation of the length scale relevant for the glass transition. KW - Broadband dielectric spectroscopy KW - Specific heat spectroscopy KW - Rod-like liquid crystals KW - Discotic liquid crystals PY - 2018 UR - https://link.springer.com/content/pdf/10.1007%2F978-3-319-72706-6.pdf SN - 978-3-319-72705-9 SN - 978-3-319-72706-6 DO - https://doi.org/10.1007/978-3-319-72706-6_9 SN - 2190-930X SN - 2190-9318 SP - 279 EP - 306 PB - Springer International publishing AG CY - Cham, Switzerland ET - 1. AN - OPUS4-45624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Rosner, M. A1 - Curbera, J. A1 - Peltz, U. A1 - Peplinski, Burkhard T1 - Lead isotope analysis in magic artefacts from the Berlin museums N2 - A set of 59 ancient magical artefacts, mainly made of lead, was selected from the collections of the Staatliche Museen zu Berlin in order to unravel their origins. All the selected artefacts have been studied for their Pb isotope compositions, which covered the whole range of the Mediterranean ore deposits. However, the majority (≈86%) were made of lead matching the small compositional range of the Laurion ore deposits. Only eight out of the 59 artefacts were made of recycled lead or lead from other ore deposits. Additionally, all but two were approximately dated based on their inscriptions. The lead isotopic composition together with information obtained from the inscriptions, the resulting dating, the context of the find and the known history of each item allowed us to gain more detailed information about the origins of these magical artefacts. The Attic provenance of 36 curse tablets was confirmed, whereas for 11 curse tablets previously classified as non-Attic, the provenance was either confirmed and specified (six artefacts) or changed to Attic (five artefacts). Surprisingly, the majority (six out of eight) of the analysed curse tablets from the Egyptian collection showed a lead isotopic composition closely matching that of Laurion. A Laurion-like lead isotopic composition was also observed for three of the four analysed oracular tablets from Dodona. Together with the dating information, this points to Laurion as the major and dominant lead source in the Aegean, at least during the fourth–third century B.C. The few curse tablets from earlier than the fourth–third century B.C. point to the use of multiple and thus isotopically more variable lead sources compared with the Roman times. KW - Lead isotopes KW - Pb isotopes KW - Greek curse tablets KW - Antikensammlung Berlin KW - Ägyptisches Museum Berlin PY - 2018 DO - https://doi.org/10.1007/s12520-016-0445-6 SN - 1866-9557 SN - 1866-9565 VL - 10 IS - 5 SP - 1111 EP - 1127 PB - Springer Verlag CY - Berlin AN - OPUS4-45628 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ickert, Stefanie T1 - Vacuum ultraviolet light as a new Tandem MS method N2 - Tandem MS techniques are widely used for both, structure and sequence elucidation of biopolymers. Thereby, fragmentation activation is realized by various methods, for example with lasers or collisions with neutral gases. In this study, we present a new Tandem MS System using a commercially available vacuum ultraviolet lamp. On the one hand, this approach provides efficient fragmentation in both ionization modes, positive as well as negative. On the other hand, it enables an additional previously not achieved post ionization of the fragments. While the first results in atypical fragment patterns and, thus provides orthogonal information, the second is crucial especially to identify low abundant ions. T2 - EMSC 2018 CY - Saarbruecken, Germany DA - 4.3.2018 KW - Tandem MS PY - 2018 AN - OPUS4-45671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Akhemtova, Irina A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Mechanochemical synthesis of cerium(IV)-phosphonates N2 - The syntheses and crystal structures of two cerium(IV) phosphonates are presented. Cerium(IV) bis(phenylphosphonate) Ce(O3PC6H5)2 1 can be formed from precipitation and mechanochemical reaction, whereas cerium(IV) bis(carboxymethylphosphonate) monohydrate Ce(O3PCH2COOH)2 H2O 2 is only accessible via ball milling. All reactions proceed very fast and are completed within a short time span. In situ measurements for the syntheses of 1 show that the product occurs within seconds or a few minutes, respectively. The structures were solved from powder X-ray diffraction data. KW - In situ studies KW - Mechanochemistry KW - XRD PY - 2018 DO - https://doi.org/10.1007/s10853-018-2507-x SN - 0022-2461 SN - 1573-4803 VL - 53 IS - 19 SP - 13733 EP - 13741 PB - Springer Science + Business Media B.V. AN - OPUS4-45672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Akhmetova, Irina A1 - Schuzjajew, K. A1 - Wilke, M. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Rademann, K. A1 - Roth, C. A1 - Emmerling, Franziska T1 - Synthesis, characterization and in situ monitoring of the mechanochemical reaction process of two manganese(II)-phosphonates with N-containing ligands N2 - Two divalent manganese aminophosphonates, manganese mono (nitrilotrimethylphosphonate) (MnNP3) and manganese bis N-(carboxymethyl)iminodi(methylphosphonate)) (Mn(NP2AH)2), have been prepared by mechanochemical synthesis and characterized by powder X-ray diffraction (PXRD). The structure of the novel compound Mn(NP2AH)2 was determined from PXRD data. MnNP3 as well as Mn(NP2AH)2 exhibits a chain-like structure. In both cases, the manganese atom is coordinated by six oxygen atoms in a distorted octahedron. The local coordination around Mn was further characterized by extended X-ray absorption fine structure. The synthesis process was followed in situ by synchrotron X-ray diffraction revealing a three-step reaction mechanism. The asprepared manganese(II) phosphonates were calcined on air. All samples were successfully tested for their suitability as catalyst material in the oxygen evolution reaction. KW - Mechanochemistry KW - In situ KW - XRD PY - 2018 DO - https://doi.org/10.1007/s10853-018-2608-6 SN - 0022-2461 SN - 1573-4803 VL - 53 IS - 19 SP - 13390 EP - 13399 PB - Springer Science + Business Media B.V. AN - OPUS4-45673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bastuck, M. A1 - Baur, T. A1 - Richter, Matthias A1 - Mull, B. A1 - Schütze, A. A1 - Sauerwald, T. T1 - Comparison of ppb-level gas measurements with a metal-oxide semiconductor gas sensor in two independent laboratories N2 - In this work, we use a gas sensor system consisting of a commercially available gas sensor in temperature cycled operation. It is trained with an extensive gas profile for detection and quantification of hazardous volatile organic compounds (VOC) in the ppb range independent of a varying background of other, less harmful VOCs and inorganic interfering gases like humidity or hydrogen. This training was then validated using a different gas mixture generation apparatus at an independent lab providing analytical methods as reference. While the varying background impedes selective detection of benzene and naphthalene at the low concentrations supplied, both formaldehyde and total VOC can well be quantified, after calibration transfer, by models trained with data from one system and evaluated with data from the other system. The lowest achievable root mean squared errors of prediction were 49 ppb for formaldehyde (in a concentration range of 20–200 ppb) and 150 μg/m³ (in a concentration range of 25–450 μg/m³) for total VOC. The latter uncertainty improves to 13 μg/m³ with a more confined model range of 220–320 μg/m³. The data from the second lab indicate an interfering gas which cannot be detected analytically but strongly influences the sensor signal. This demonstrates the need to take into account all sensor relevant gases, like, e.g., hydrogen and carbon monoxide, in analytical reference measurements. KW - Indoor air quality KW - Volatile organic compounds KW - Calibration transfer KW - Selective quantification KW - Inter-lab comparison PY - 2018 DO - https://doi.org/10.1016/j.snb.2018.06.097 SN - 0925-4005 VL - 273 SP - 1037 EP - 1046 PB - Elsevier B.V. AN - OPUS4-45609 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ermawati, F. U. A1 - Supardi, Z. A. I. A1 - Suasmoro, S. A1 - Hübert, Thomas T1 - Contribution of Relaxation Effect to the Permittivity of Mg1-xZnxTiO3 Ceramics N2 - This work reported the investigation on the effect of relaxation to the permittivity (epsilon' r ) characteristic of Mg1-x Zn x TiO3 ceramics for x = 0 – 0.5 (MZT0 – MZT0.5) measured from 1 Hz to 330 MHz. Within that frequency range, the relaxation effect that consists of the space charge (SC) and the dipolar (D) polarization mechanisms were identified. The contribution of the D relaxation in MZT0 – MZT0.2 systems extents overall from about 100 Hz to 330 MHz, while that in MZT0.3 – MZT0.5 systems is from 50 kHz to 330 MHz. The remaining frequencies, i.e. from 1 to 90 Hz for MZT0 – MZT0.2 and from 1 Hz to 50 kHz for MZT0.3 – MZT0.5, are attributed to the SC relaxation. The D polarization mechanism provides constant epsilon' r values which vary from (15.4 – 17.0) ± 0.3 throughout the samples. Contribution of the SC polarization mechanism to the characteristic is supported by the simultaneous presence of different content and level of resistivity of the secondary phase of (Mg1-αZnα)2TiO4 in MZT0 – MZT0.2 systems and of (Zn1-αMgα)2TiO4 in MZT0.3 – MZT0.5, along with the presence of the main Mg1-x Zn x TiO3 phase, as a result of the variation of zinc content in the systems. T2 - The 5th International Conference on Advanced Materials Sciences and Technology (ICAMST 2017) CY - Makassar, Indonesia DA - 19.09.2017 KW - Dielectric ceramic KW - dipolar polarization KW - Mg1-xZnxTiO3 KW - permittivity KW - space charge polarization PY - 2018 DO - https://doi.org/10.1088/1757-899X/367/1/012003 SN - 1757-8981 VL - 367 SP - 1 EP - 6 PB - IOP Publishing Ltd AN - OPUS4-45618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rauscher, H. A1 - Hodoroaba, Vasile-Dan T1 - The NanoDefine Decision Framework and NanoDefiner e-Tool: a practical guide to the identification of nanomaterials N2 - The European Commission's recommendation on the definition of nanomaterial [2011/696/EU] is broadly applicable across different regulatory sectors and requires the quantitative size determination of constituent particles in samples down to 1 nm. A material is a nanomaterial if 50 % or more of the particles are in the size range 1-100 nm. The implementation of the definition in a regulatory context challenges measurement methods to reliably identify nanomaterials and ideally also non-nanomaterials as substance or product ingredient as well as in various matrices. The EU FP7 NanoDefine project [www.nanodefine.eu] addressed these challenges by developing a robust, readily implementable and cost-effective measurement strategy to decide for the widest possible range of materials whether it is a nanomaterial or not. It is based on existing and emerging particle measurement techniques evaluated against harmonized, material-dependent performance criteria and by intra- and inter-lab comparisons. Procedures were established to reliably measure the size of particles within 1-100 nm, and beyond, taking into account different shapes, coatings and chemical compositions in industrial materials and consumer products. Case studies prove their applicability for various sectors, including food, pigments and cosmetics. A main outcome is the establishment of an integrated tiered approach including rapid screening (tier 1) and confirmatory methods (tier 2), a decision support flow scheme and a user manual to guide end-users, such as manufacturers, in selecting appropriate methods. Another main product is the “NanoDefiner” e-Tool which implements the flow scheme in a user-friendly software and guides the user in a semi-automated way through the entire decision procedure. It allows a cost-effective selection of appropriate methods for material classification according to the EC's nanomaterial definition and provides a comprehensive report with extensive explanation of all decision steps to arrive at a transparent identification of nanomaterials as well as non-nanomaterials for regulatory purposes. The project has received funding from the European Union’s Seventh Programme for research, technological development and demonstration under grant agreement No 604347. T2 - BAM-PTB Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - Definition of nanomaterial KW - Regulation PY - 2018 AN - OPUS4-45633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maurino, V. A1 - Hodoroaba, Vasile-Dan T1 - Synthesis of Shape controlled TiO2 N2 - Titanium dioxide is one of the most studied metal oxides due to its chemical, surface, electronic and (photo)catalytic properties, providing this material of multisectorial applications ranging from healthcare, photocatalysis, smart materials with self cleaning and self sterilizing properties and solar energy harvesting. However it is difficult to correlate the functional properties of TiO2 nanomaterials to the properties at single nanoparticle level due to the high polydispersity in shape, size and surface features of the currently available TiO2 nanoparticles (NPs). Although intensive experimental and theoretical studies have been conducted on the reactivity of different surfaces of metal oxides such as TiO2 much less attention is paid on the dependence of functional properties, like photocatalytic activity, dye adsorption, open circuit potential and fill factor in dye sensitized solar cells, on crystal facets in different orientations. One of the goal of SETNanoMetro project was the development of design rules to tune crystal facets of TiO2 NPs in order to optimize and control functional properties. In the present work we have developed a series of design rules in order to obtain sets of anatase TiO2 NPs with low polydispersity and to tune their shape and size by hydrothermal processing of Ti(IV)-Triethanolamine complex in presence of different shape controllers. Through a careful experimental design, a predictive soft model was developed. The model is able to predict the synthesis outcome allowing to tune the shape factor from 5 (prisms) to 1.5 (bipyramids) to 0.2 (platelets). This allows to control the main crystal facets exposed ranging from (100) to (001). Due to the dependence of functional properties of nanomaterials on shape distribution and not only size, the availability of NPs sets with uniform and well defined and tunable shapes can be of paramount relevance in order to produce reference nanomaterials for shape measurement. T2 - NanoWorkshop 2018 (Workshop on reference nanomaterials, current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2018 KW - Anatase KW - Shape control KW - Hydrothermal synthesis KW - Nanoparticles PY - 2018 AN - OPUS4-45634 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona T1 - The Role of Conformity Assessment in the Digital Transformation: Focusing on Cybersecurity N2 - Digital transformation and especially the dramatic rise of products and services connected to the Internet of Things raise the questions on how to deal with the increasing risks related to Privacy and Cybersecurity. Presumably, these risks seem to be insufficiently reflected in the European Union’s current regulative system – by being neither part of the traditional definition of a safe product nor part of product-specific vertical or horizontal directives. Certification based on standards as underlying requirements has been identified by policymakers as an instrument to address this issue. The latest European draft regulation aims at increasing security and trust in ICT products and services, and reducing current European market fragmentation with a new Cybersecurity Certification Framework. Based on the results of a qualitative analysis of stakeholder statements on the current proposal on the Cybersecurity Act, this paper discusses elements of the proposed Cybersecurity Certification Framework. As a theoretical background, this paper provides definitions of the terms Safety, IT-security, and Cybersecurity, presents selected Cybersecurity-related standards and provides an outlook on future challenges to Conformity Assessment in the digital transformation. T2 - 23rd EURAS Annual Standardisation Conference "Standards for a Smarter Future" CY - Dublin, Irland DA - 13.06.2018 KW - Cybersecurity KW - Certification KW - Conformity Assessment KW - IT-Security PY - 2018 AN - OPUS4-45687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosemann, Paul A1 - Kauss, N. T1 - Visualisierung werkstoffbedingter Lochkorrosionsanfälligkeit durch die KorroPad-Prüfung N2 - Mit der KorroPad-Prüfung können lochkorrosionsanfällige Oberflächen einfach, schnell und kostengünstig nachgewiesen werden. Das KorroPad ist damit für Hersteller, Verarbeiter, Anwender und Forscher eine interessante Alternative zu zeitintensiven Auslagerungsversuchen und elektrochemischen Untersuchungsmethoden, die normalerweise bei der Charakterisierung nichtrostender Stähle zur Anwendung kommen. Mit der KorroPad-Prüfung können aber auch werkstoff und gefügebedingte Einflussfaktoren sichtbar gemacht werden, die Lochkorrosionsanfälligkeit verursachen. Um dies zu veranschaulichen, wird die Nachweisgrenze des KorroPads an Referenzlegierungen mit abgestuftem Chromgehalt aufgezeigt. Darauf aufbauend wird dargestellt, wie die Sensibilisierung nichtrostender Stähle durch Chromverarmung mit einer gezielten Verschärfung der KorroPad-Prüfung nachgewiesen werden kann. KW - Korrosion KW - Nichtrostender Stahl KW - KorroPad KW - Passivschicht KW - Lochkorrosion KW - EPR KW - Korrosionsschnelltest KW - Qualitätssicherung PY - 2018 UR - https://www.wotech-technical-media.de/womag/autoren/Rosemann_Paul.php DO - https://doi.org/10.7395/2018/Rosemann1 IS - 7-8 SP - 1 EP - 5 PB - WOMAG AN - OPUS4-45688 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosemann, Paul A1 - Kauss, N. T1 - Visualisierung werkstoffbedingter Lochkorrosionsanfälligkeit durch die KorroPad-Prüfung N2 - Mit der KorroPad-Prüfung können lochkorrosionsanfällige Oberflächen einfach, schnell und kostengünstig nachgewiesen werden. Das KorroPad ist damit für Hersteller, Verarbeiter, Anwender und Forscher eine interessante Alternative zu zeitintensiven Auslagerungsversuchen und elektrochemischen Untersuchungsmethoden, die normalerweise bei der Charakterisierung nichtrostender Stähle zur Anwendung kommen. Mit der KorroPad-Prüfung können aber auch werkstoff- und gefügebedingte Einflussfaktoren sichtbar gemacht werden, die Lochkorrosionsanfälligkeit verursachen. Um dies zu veranschaulichen, wird die Nachweisgrenze des Korro-Pads an Referenzlegierungen mit abgestuftem Chromgehalt aufgezeigt. Darauf aufbauend wird dargestellt, wie die Sensibilisierung nichtrostender Stähle durch Chromverarmung mit einer gezielten Verschärfung der KorroPad-Prüfung nachgewiesen werden kann. KW - Korrosion KW - Nichtrostender Stahl KW - KorroPad KW - Korrosionsschnelltest KW - Passivschicht KW - EPR KW - Qualitätssicherung PY - 2018 SN - 2195-5905 IS - 7-8 SP - 18 EP - 20 PB - WOMAG CY - Waldshut-Tiengen AN - OPUS4-45689 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Datenfusion –Informationsgewinn aus Multisensordaten N2 - Angetrieben durch Digitalisierung und die sogenannte Industrie 4.0 steigt die Erwartungshaltung gegenüber der Nutzung von Sensorik. Die Unsicherheit, Widersprüchlichkeit und Redundanz separat verarbeiteter einzelner Quellen soll durch die synergetische Zusammenführung heterogener Datensätze überwunden werden. Dabei steht der zunehmenden Aufgabenkomplexität eine ebenso zunehmende Verfügbarkeit an Sensoren, Daten und Rechenleistung gegenüber. Der Begriff Datenfusion fasst Ansätze zusammen, die Daten zu abstrakteren, aber besser verständlichen Informationen verarbeiten. Die Fusion ist Kernbestandteil effektiver Assistenzsysteme und beweist in vielzähligen Aufgaben - von militärischen Anwendungen über Flug- und Fahrassistenzsysteme, bis in den Heimbereich – ihr großes Potenzial. Durch die wachsende Automatisierung bei der Messdatenerfassung wird Datenfusion auch in der industriellen Qualitätsprüfung und –sicherung zunehmend attraktiver. Der Vortrag gibt einen Überblick über den breiten Themenkomplex und widmet sich dabei im Theorieteil speziell der Fragen, welche Informationen in multivariaten Datensätzen stecken und wie sie extrahiert werden können. Anschließend wird ein Beispiel für die erfolgreiche Anwendung zur zerstörungsfreien Prüfung von Betonbauteilen vorgestellt. Der dargestellte Datensatz ist klein, heterogen, hochdimensional und unausgeglichen. Anhand von Algorithmen mit unterschiedlicher Leistungsfähigkeiten hinsichtlich Anpassungsfähigkeit und Invarianz gegenüber Höherdimensionalität wird erläutert welche Prozesse zur Verbesserung der Informationsqualität nötig sind. T2 - Vortragsreihe des Kompetenzzentrums Datenanalyse CY - BAM UE, Berlin, Germany DA - 25.07.2018 KW - Maschinelles Lernen KW - Datenfusion KW - ZfP KW - Beton KW - Korrosion PY - 2018 AN - OPUS4-45602 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lauer, Franziska A1 - Diehn, Sabrina A1 - Seifert, Stephan A1 - Kneipp, Janina A1 - Sauerland, V. A1 - Barahona, C. A1 - Weidner, Steffen T1 - Multivariate analysis of MALDI imaging mass spectrometry data of mixtures of single pollen grains N2 - Mixtures of pollen grains of three different species (Corylus avellana, Alnus cordata, and Pinus sylvestris) were investigated by matrixassisted laser desorption/ionization time-of-flight imaging mass spectrometry (MALDI-TOF imaging MS). The amount of pollen grains was reduced stepwise from > 10 to single pollen grains. For sample pretreatment, we modified a previously applied approach, where any additional extraction steps were omitted. Our results show that characteristic pollen MALDI mass spectra can be obtained from a single pollen grain, which is the prerequisite for a reliable pollen classification in practical applications. MALDI imaging of laterally resolved pollen grains provides additional information by reducing the complexity of the MS spectra of mixtures, where frequently peak discrimination is observed. Combined with multivariate statistical analyses, such as principal component analysis (PCA), our approach offers the chance for a fast and reliable identification of individual pollen grains by mass spectrometry. KW - MALDI Imaging MS KW - Pollen grains KW - Multivariate Statistics KW - Hierarchical cluster analysis KW - Principal component analysis PY - 2018 DO - https://doi.org/10.1007/s13361-018-2036-5 SN - 1044-0305 SN - 1879-1123 VL - 29 IS - 11 SP - 2237 EP - 2247 PB - Springer AN - OPUS4-45607 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Mechanochemical Syntheses of Metal Phosphonates N2 - Mechanochemistry is a suitable method for synthesizing a variety of metal phosphonates. By varying the ratio of the reactants, it is possible to control the reaction pathway. With this approach targeted synthesis of a certain composition is possible. Several new metal phosphonate structures were solved from the powder X-ray diffraction data including molecular metal phosphonates. The results demonstrate a new fast, facile, and environmental friendly alternative for the preparation of metal phosphonates. In situ investigations of the milling processes provided insights into the formation process of metal phosphonates. A multi-step diffusion mechanism was identified for most systems. Crystalline phases were obtained intermediately, suggesting that the synthesis is following Ostwald’s rules of stages. T2 - 1st European Workshop on Metalphophantes CY - Swanse, UK DA - 18.09.2018 KW - Mechanochemistry PY - 2018 AN - OPUS4-46382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Determination of the Microscopic Dose-Damage Relation for Radiation of different Linear Energy Transfer N2 - The determination of the microscopic dose-damage relationship for DNA in an aqueous environment is of a fundamental interest for dosimetry and applications in radiation therapy and protection. We combine geant4 particle-scattering simulations in water with calculations concerning the movement of biomolecules to obtain the energy deposit in the biologically relevant nanoscopic volume.[1] We juxtaposition these results to the experimentally determined damage to obtain the microscopic dose-damage relationship at a molecular level. This approach is tested for an experimentally challenging system concerning the direct irradiation of plasmid DNA (pUC19) in water with electrons as primary particles.[2] Here a microscopic target model for the plasmid DNA based on the relation of lineal energy and radiation quality is used to calculate the effective target volume. It was found that on average fewer than two ionizations within a 7.5-nm radius around the sugar-phosphate backbone are sufficient to cause a single strand break, with a corresponding median lethal energy deposit being E1/2=6±4 eV.[1] The presented method is applicable for ionizing radiation (e.g., γ rays, x rays, and electrons) and a variety of targets, such as DNA, proteins, or cells. [1] Hahn, M. B., Meyer, S., Kunte, H.-J., Solomun, T. & Sturm, H. Measurements and simulations of microscopic damage to DNA in water by 30 keV electrons: A general approach applicable to other radiation sources and biological targets. Phys. Rev. E 95, 052419 (2017). [2] Hahn, M. B. et al. Direct electron irradiation of DNA in a fully aqueous environment. Damage determination in combination with Monte Carlo simulations. Phys. Chem. Chem. Phys. 19, 1798–1805 (2017). T2 - DYSON 2018 CY - Potsdam, Germany DA - 08.10.2018 KW - DNA KW - Dosimetry KW - Electron irradiation KW - Geant4 KW - Hydroxyl radical KW - LET KW - Linear energy transfer KW - Low energy electrons KW - MCS KW - Microdosimetry KW - Monte-Carlo simulations KW - Radiation damage KW - Radiation therapy KW - SEM KW - Electron Microscope KW - LEE KW - Protein PY - 2018 AN - OPUS4-46383 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Characterisation of magnetron sputtered SnZnOx by means of spectroscopic ellipsometry - how can we analyse TCO materials optically? N2 - Transparent conductive oxide (TCO) films are a vital part of a large part of modern technology. The production of TCO materials has sparked much development in plasma coating technology. Quality control measurements of these layers are therefore important in many fields of optics and electronics such as high efficiency thin film photovoltaics. In this presentation, we report on optical measurements of ZnSnOx layers generated by DC/RF magnetron plasma co-sputtering. By changing the respective power on two different targets, the overall power, the gas composition and post-treatment, the properties of this type of layers can be varied in a number of parameters. The optical, electrical, and chemical properties of TCO layers are the technically most important properties together with the layer thickness. The dielectric function of layers is accessible by means of spectroscopic ellipsometry, which also yields the very important value for the layer thickness at the same time. It would be a significant step forward in quality control to use this non-destructive method also as a fast test for electrical properties. Therefore, we report on the optical properties connected to the production parameters, and also on our preliminary results connecting the optical dielectric function (in the visible and near infrared) to the electrical conductivity of the layers. We discuss the effect of deposition parameters on the optical properties of the layers and present an approach for correlating optical and electrical properties. Further, we discuss the question of accuracy of optical properties gained from model-fit-based optical methods and the use of different parameterised models for the dielectric function to achieve this. T2 - PSE 2018 - 16th Conference on Plasma Surface Engineering CY - Garmisch-Partenkirchen, Germany DA - 17.09.2018 KW - Mixed Oxides KW - TCO KW - Quality Control KW - Ellipsometry KW - Optical Constants PY - 2018 AN - OPUS4-46388 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Borghetti, P. A1 - Ortel, Erik A1 - Wirth, Thomas A1 - Blanco, M. A1 - Gómez, E. A1 - Martinez, A. A1 - Jupille, J. A1 - Martra, G. A1 - Hodoroaba, Vasile-Dan T1 - Control of functionalization of supports for subsequent assembly of titania nanoparticle films N2 - For self‐assembling of TiO2 nanoparticles in multiple layers by layer‐by‐layer deposition to be applied to TiO2 thin films with defined and homogeneous thickness for large‐scale applications, the proper functionalization of substrate surface is a prerequisite to guarantee sufficient adhesion. The substrates selected and tested in the present paper were conductive, fluorine‐doped tin oxide (FTO) glass, nonconductive silica glass, and titanium alloy. The current study focusses on the analytical control of the stepwise functionalization of the substrates with 3‐aminopropyltriethoxysilane and glutaraldehyde (GA) for both the FTO glass and silica glass and with 3‐aminepropyl phosphonic acid and GA for Ti alloy. The analyses have been conducted by means of surface sensitive methods, X‐ray photoelectron spectroscopy, Auger electron spectroscopy, and time‐of‐flight secondary ions mass spectrometry. Chemical composition of surface of functionalized substrates shows differences in the degree and type of modification in dependence on substrate. It could be demonstrated that the best functionalized substrates were the conductive FTO glasses. The analysis of the functionalized Ti substrates has revealed that the surface coverage with 3‐aminepropyl phosphonic acid and GA molecules is an inhomogeneous one, and further optimization of the two‐step functionalization on the Ti alloy substrate is necessary. KW - Nanoparticles KW - Surface functionalization KW - TiO2 KW - SEM/EDX KW - Auger Electron Spectroscopy KW - ToF-SIMS KW - Thin films PY - 2018 DO - https://doi.org/10.1002/sia.6398 SN - 0142-2421 SN - 1096-9918 VL - 50 IS - 11 SP - 1200 EP - 1206 PB - John Wiley & Sons, Ltd. AN - OPUS4-46406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Workshop: Basic Statistics for NMR N2 - qNMR provides the most universally applicable form of direct concentration or purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. The workshop presents basic terms of statistics and uncertainty analysis, which are the basis for qNMR spectroscopy and data analysis such as, e.g., standard deviations, linear regression, significance tests, etc. and gives typical examples of applications in qNMR spectroscopy. T2 - qNMR-Summit 2018 CY - Würzburg, Germany DA - 10.10.2018 KW - Quantitative NMR Spectroscopy KW - Statistics KW - Quality Assurance KW - NMR validation KW - qNMR PY - 2018 AN - OPUS4-46368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Tragbare RFA an Gläsern: Ergebnisse und Grenzen N2 - Vorstellung der Ergebnisse der Messungen an Gläsern von Goethes Prismen. T2 - 3. Goethe/Ritter-Workshop CY - Berlin, Germany DA - 25.05.2018 KW - Goethe KW - Farbenlehre KW - Prisma KW - Handheld KW - XRF PY - 2018 AN - OPUS4-46369 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kneipp, Janina A1 - Zhang, Zhiyang T1 - Mapping the Inhomogeneity in Plasmonic Catalysis on Supported Gold Nanoparticles Using Surface-Enhanced Raman Scattering Microspectroscopy N2 - The characterization of a catalyst often occurs by averaging over large areas of the catalyst material. On the other hand, optical probing is easily achieved at a resolution at the micrometer scale, specifically in microspectroscopy. Here, using surface-enhanced Raman scattering (SERS) mapping of larger areas with micrometer-sized spots that contain tens to hundreds of supported gold nanoparticles each, the photoinduced dimerization of p-aminothiophenol (PATP) to 4,4′-dimercaptoazobenzene (DMAB) was monitored. The mapping data reveal an inhomogeneous distribution of catalytic activity in the plasmon-catalyzed reaction in spite of a very homogeneous plasmonic enhancement of the optical signals in SERS. The results lead to the conclusion that only a fraction of the nanostructures may be responsible for a high catalytic activity. The high spot-to-spot variation in catalytic activity is also demonstrated for DMAB formation by the plasmon-catalyzed reduction from p-nitrothiophenol (PNTP) and confirms that an improvement of the accuracy and reproducibility in the characterization of catalytic reactions can be achieved by microspectroscopic probing of many positions. Using SERS micromapping during the incubation of PATP, we demonstrate that the reaction occurs during the incubation process and is influenced by different parameters, leading to the conclusion of dimerization in a gold-catalyzed, nonphotochemical reaction as an alternative to the plasmon-catalyzed process. The results have implications for the future characterization of new catalyst materials as well as for optical sensing using plasmonic materials. KW - P-aminothiophenol KW - Silver nanoparticles KW - Chemical transformation KW - Metal nanoparticles KW - Coupling reactions KW - AU nanoparticle KW - AG nanoparticle KW - Spectroscopy KW - Sers KW - Molecule PY - 2018 DO - https://doi.org/10.1021/acs.analchem.8b01701 VL - 90 IS - 15 SP - 9199 EP - 9205 PB - American Chemical Society AN - OPUS4-46372 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - Airborne Laser-Induced Plasma as an Ambient Desorption/Ionization Source for Mass Spectrometry and its Characterization N2 - Laser-induced plasma (LIP) has drawn significant amount of attentions in the past decades, particular in elemental analyses for solid or liquid samples. Through proper focusing of the highly energetic laser beam, the plasma can also be ignited in the ambient air, where airborne analytes can be ionized. Such an effect enabled the use of airborne LIP as an ambient ionization source for mass spectrometric analyses. In contrast to other ambient desorption/ionization sources, airborne LIP does not require a specific discharge medium or expensive gas stream. Meanwhile, the airborne LIP produces reagent ion species for both proton-transfer and charge-transfer reactions in addition to the vacuum ultraviolent photons that are capable of promoting single photon ionization, which can be utilized to ionize polar and non-polar analytes. In order to gauge the analytical performance of airborne LIP, it is critical to understand the undergoing chemistry and physics during and after the plasma formation. Due to the ambient nature of airborne LIP, the variations of air composition and flow strongly affect the plasma behaviors. Preliminary result suggested the addition of a laminar flow of nitrogen gas favored the formation of protonated species (MH+) against the molecular ones (M+). Although the gas addition approach cannot fully tune the ionization process towards the specific production of pseudo-molecular species versus molecular ones, the alternation of molecular ion formation can be used for analyte recognitions through post processing of the ion patterns. The pulsed character of the used lasers makes the reagent ion equilibrium both transient- and highly fluid-dynamically controlled. The acoustic shock-waves induced by the airborne LIP get affected by an applied gas streams towards the plasma center, influencing the molecular-ion and ion-ion interactions in the near proximity of the plasma. To understand the airborne LIP formation, the temporally and spatially resolved optical emission spectra were recorded. The results will be correlated to time-resolved mass-spectrometric investigations of the ion profile during different stages of the plasma formation. As one example, the formation of pyrylium ion originating from aromatic compounds will be highlighted. T2 - SciX 2018 CY - Atlanta, GA, USA DA - 21.10.2018 KW - Laser-Induced Plasma KW - Ambient Desorption/Ionization KW - Mass Spectrometry KW - Characterization PY - 2018 AN - OPUS4-46376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Advances of Model-Based Data Evaluation Concepts for Quantitative Online NMR Spectroscopy N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module used for process characterisation and optimisation. Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). Based on concentration measurements of reagents and products by online NMR spectroscopy a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR module was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (“Integrated CONtrol and SENsing”, www.consens-spire.eu). T2 - SciX 2018 CY - Atlanta, GA, USA DA - 22.10.2018 KW - Online NMR Spectroscopy PY - 2018 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-46377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Witte, Steffen T1 - XAFS@BAMline N2 - X-ray Absorption fine structure spectroscopy (XAFS) is a frequently employed technique in order to investigate structural composition and Change of chemical compounds such as catalytic species or corrosion processes. These structural properties are essential (i) to understand underlying reaction mechanism and (ii) to further improve the design of materials. While XAFS measurements are usually performed with ionization Chambers or simple fluorescence detectors, we at BAMline specialize in measurements with innovative set-ups that meet Specialrequirements such as time resolution, (3D-) spatial Resolution or demanding sample environments. This contribution presents various available XAFS configurations with their corresponding applications. In particular, these comprise single -shot XAFS for time- resolved measurements, grazing-exit XAFS with energy and a spatially resolved detector for the characterization of thin films and an in situ grazing incidence Setup for the characterization of corrosion layers. Additionally,the possibility of analyzing Minute samples in total-reflection geometry is demonstrated. T2 - EXRS 2018 CY - Ljubljana, Slovenia DA - 24.06.2018 KW - XANES KW - XAFS KW - BAMline KW - Synchrotron KW - TXRF PY - 2018 AN - OPUS4-46361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Witte, Steffen T1 - S2XAFS@work: Customization for the Characterization of VOx based Catalysts N2 - X-ray absorption fine structure spectroscopy (XAFS) is a frequently employed technique in order to investigate structural composition and change of chemical compounds such as catalytic species. These structural properties are essential (i) to understand underlying reaction mechanism and (ii) to further improve the design of efficient catalysts. This investigation is based on a newly developed XAFS setup comprising both time- and lateral-resolved XAFS information simultaneously in a single-shot (S2XAFS). The primary broadband beam is generated by a filter/X-ray-mirror combination (bandpass). The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by an area sensitive detector with a theta to 2 theta geometry. This facile, stable and scanningless setup was tested at the BAMline @ BESSY-II (Berlin, Germany). This contribution focuses on further experimental optimizations allowing the characterization of supported vanadium oxide (VOx) based catalysts at the lower hard X-ray regime (5 to 6 keV). First S2XAFS measurements of these catalysts are presented herein. Supported VOx catalysts show promising results in the oxidation of methane to formaldehyde. S2XAFS allows determining the structural composition of the metal (i.e. vanadium) based on a fast and smart setup. It is therefore an ideal tool to identify crucial roles of chemical compounds in catalytic reactions. T2 - XAFS 2018 CY - Cracow, Poland DA - 22.07.2018 KW - XANES KW - XAFS KW - BAMline KW - Synchrotron PY - 2018 AN - OPUS4-46362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Witte, Steffen T1 - TXRF-XANES: a unique experimental setup for chemical speciation of traces down to pg range N2 - Description of the set-up and first results for TXRF-XANES at BAMline T2 - XAFS 2018 CY - Cracow, Poland DA - 22.07.2018 KW - TXRF KW - XANES KW - Synchrotron KW - BAMline PY - 2018 AN - OPUS4-46363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - The colour X-ray camera – Basics and applications of a 2D X-ray detector N2 - The Color X-ray Camera CXC or SLcam® is an energy-resolving X-ray camera capable of energy- and space-resolved measurements. It consists of a high-speed CCD detector coupled to a polycapil-lary optic that conducts the X-ray photons from the probe to distinct pixels onto the detector. The camera is capable of fast acquisition of spatially and energy resolved fluorescence images. A dedicated software enables the acquisition and the online processing of the spectral data for all 69696 pixels, leading to a real-time visualization of the elements distribution in a sample. It was developed in a joint project with BAM, IFG Berlin and PN Sensors. In this contribution we will mainly discuss the use of the CXC at our beamline, the BAMline at BESSY II and imaging applications of the CXC from different areas, like biology and archaeometry. Additionally new developments for the use of the detector without optics, like wavelength dispersive detection or 1shot-XANES, will be presented. T2 - Seminar Strahlenphysikalische Anwendungen in Technik und Medizin CY - ATi Wien, Austria DA - 24.01.2018 KW - XRF KW - Synchrotron KW - BAMline PY - 2018 AN - OPUS4-46365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kowarik, Stefan A1 - Pithan, L. A1 - Nabok, D. A1 - Cocchi, C. A1 - Beyer, P. A1 - Duva, G. A1 - Simbrunner, J. A1 - Rawle, J. A1 - Nicklin, C. A1 - Schäfer, P. A1 - Draxl, C. A1 - Schreiber, F. T1 - Molecular structure of the substrate-induced thin-film phase of tetracene N2 - We present a combined experimental and theoretical study to solve the unit-cell and molecular arrangement of the tetracene thin film (TF) phase. TF phases, also known as substrate induced phases (SIP), are polymorphs that exist at interfaces and decisively impact the functionality of organic thin films, e.g., in a transistor channel, but also change the optical spectra due to the different molecular packing. As SIPs only exist in textured ultrathin films, their structure determination remains challenging compared to bulk materials. Here, we use grazing incidence Xray diffraction and atomistic simulations to extract the TF unit-cell parameters of tetracene together with the atomic positions within the unit-cell. KW - X-ray DIFFRACTION KW - Tetracene KW - Semiconductor KW - Optoelectronics KW - Molecule PY - 2018 DO - https://doi.org/10.1063/1.5043379 VL - 149 IS - 14 SP - 144701-1 EP - 144701-5 PB - AIP Publishing AN - OPUS4-46399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duva, G. A1 - Pithan, L. A1 - Zeiser, C. A1 - Reisz, B. A1 - Dieterle, J. A1 - Hofferberth, B. A1 - Beyer, P. A1 - Bogula, L. A1 - Opitz, A. A1 - Kowarik, Stefan A1 - Hinderhofer, A. A1 - Gerlach, A. A1 - Schreiber, F. T1 - Thin-Film Texture and Optical Properties of Donor/Acceptor Complexes. Diindenoperylene/F6TCNNQ vs Alpha-Sexithiophene/ F6TCNNQ N2 - In this work, two novel donor/acceptor (D/A) complexes, namely, diindenoperylene (DIP)/1,3,4,5,7,8-hexafluoro-tetracyanonaphthoquinodimethane (F6TCNNQ) and alpha-sexithiophene (6T)/F6TCNNQ, are studied. The D/A complexes segregate in form of π−π stacked D/A cocrystals and can be observed by X-ray scattering. The different conformational degrees of freedom of the donor molecules, respectively, seem to affect the thin-film crystalline texture and composition of the D/A mixtures significantly. In equimolar mixtures, for DIP/F6TCNNQ, the crystallites are mostly uniaxially oriented and homogeneous, whereas for 6T/F6TCNNQ, a mostly 3D (isotropic) orientation of the crystallites and coexistence of domains of pristine compounds and D/A complex, respectively, are observed. Using optical absorption spectroscopy, we observe for each of the two mixed systems a set of new, strong transitions located in the near-IR range below the gap of the pristine compounds: such transitions are related to charge-transfer (CT) interactions between donor and acceptor. The optical anisotropy of domains of the D/A complexes with associated new electronic states is studied by ellipsometry. We infer that the CT-related transition dipole moment is perpendicular to the respective π-conjugated planes in the D/A complex. KW - Optical properties KW - Molecular semiconductor KW - X-ray diffraction PY - 2018 DO - https://doi.org/10.1021/acs.jpcc.8b03744 SP - 18705 EP - 18714 PB - ACS AN - OPUS4-46400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bertovic, Marija T1 - Assessing and Treating Risks in Mechanised NDT: A Human Factors Study N2 - Reliability of NDT is affected by human factors, which have thus far received the least amount of attention in the reliability assessments. With increased use of automation, in terms of mechanised testing (automation-assisted inspection and the corresponding evaluation of data), higher reliability standards are believed to have been achieved. However, human inspectors, and thus human factors, still play an important role throughout this process and the risks involved in this application are unknown. The aim of this study was to explore for the first time the risks associated with mechanised NDT and find ways of mitigating their effects on the inspection performance. Hence, the objectives were to identify and Analyse potential risks in mechanised NDT and devise measures against them. To address those objectives, a risk assessment in form of a Failure Modes and Effects Analysis (FMEA) was conducted. This analysis revealed potential for failure during both the acquisition and evaluation of NDT data that could be assigned to human, technology, and organisation. Since the existing preventive measures were judged to be insufficient to defend the system from identified failures, new preventive measures were suggested. KW - NDT KW - Human factors KW - Risk assessment KW - FMEA KW - Reliability KW - Human error PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-463325 SN - 1616-069X IS - 161 SP - 52 EP - 62 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-46332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - State-of-the-Art in Multiple-Sample Evaluation of Adhesive and Bonding Strength N2 - The paper addresses the “State-of-the-Art in Multiple-Sample Evaluation of Adhesive and Bonding Strength” and the following points are discussed in more detail: 1. Motivation (coatings, varnishes, tapes, laminates, CFRP, adhesive-bonded joints) 2. Conventional single-sample testing (evaluation of adhesive and bonding strength; failure pattern) 3. Multiple-sample handling (MSH), bonding (MSB), and testing: centrifugal adhesion testing (CAT) (multiple-sample approach, tensile test within a centrifuge) 4. Application examples of CAT-Technology™ (laminates, optical coatings, CFRP joints) Finally, a summary is given regarding status quo and benefits of CAT-technology under tensile stress conditions whereas examples of testing in a centrifuge under compressive stress conditions are mentioned in the outlook. T2 - The 5th International Conference Competitive Materials and Technology Processes CY - Miskolc-Lillafüred, Hungary DA - 08.10.2018 KW - Centrifugal Adhesion Testing KW - CAT KW - Multiple-sample handling (MSH) KW - Multiple-sample bonding (MSB) KW - Tensile strength of laminates KW - Tensile strength of coatings KW - Adhesive strength KW - Bonding strength PY - 2018 AN - OPUS4-46336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kormunda, M. T1 - Optical and Electrical Properties of reactive/nonreactive Magnetron Deposited SnZnOxCoatings Annealed at Various Temperatures N2 - ZnSnOx coatings were deposited from two 2in magnetron targets made of ZnO and SnO2 connected to DC pulsed and RF power supplies, respectively. The pure Ar and reactive gas mixture Ar/O2 were used. DC pulsed power applied on ZnO target was kept constant 50W 50kHz, 20% d.c. and the RF power applied on SnO2 target was set to values from 0W (pure ZnO deposited) up to 150W (up to 8 at.% of Sn in films). The deposited films were investigated by multiple techniques as deposited at RT as well as after annealing at temperatures 200o C and 450o C. The lower annealing temperature is still compatible with many of common polymeric substrates. The amount of Sn in the films is proportional to applied RF power on SnO2 target. But there is also significant influence of the post Deposition annealing on the film compositions. The ratio Zn/Sn is reduced by the annealing process. Therefore the annealing is promoting the migration of Sn toward the surface and Zn to inside. Moreover the films deposited in oxygen rich reactive gas mixture does not reduces the resistivity with added Sn in contrary to films deposited in Ar where the resistivity was reduced by 5 orders of magnitudes. The plasma parameters were investigated and mean energies of dominant species were in DC pulsed only about 3eV and DC + RF powered plasma up to 15eV. The expected higher energetic particles in the RF influenced plasma deliver an additional energy to the growing film. Therefore, we observed systematic differences between refractive indexes in the films deposited with low RF powered SnO2 magnetron at RT and post-annealed at 200 ° and practically no difference between RT and post-annealed film at higher RF power above 50 W. The XRD results proved the transitions from an amorphous to more crystalline structure by post-annealing of the films. T2 - PSE 2018 - 16th Conference on Plasma Surface Engineering CY - Garmisch-Partenkirchen, Germany DA - 17.09.2018 KW - Reactive sputtering KW - Plasma diagnostics KW - Optical films KW - TCO PY - 2018 AN - OPUS4-46347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - SAXS in Analysis of Ultra-small Size-adjustable Zinc Oxide Nanoparticles for Controlled Band Gap Engineering N2 - Zinc oxide (ZnO) as a wide-bandgap II-VI semiconductor finds application in areas like optoelectronics, photocatalysis as well as in detection systems. While band-gap engineering in macroscopic ZnO can be performed by alloying, the band-gap of ZnO nanoparticles is also dependent on their size. Since small-angle X-ray scattering (SAXS) provides a much higher resolution in terms of ultra-small nanoparticle size analysis compared to other techniques, it allows for a careful examination of the correlation between particle size and band-gap. We report on the microwave-assisted synthesis of oleate-capped, photoluminescent zinc oxide nanoparticles with adjustable size as dispersions in organic solvents. The spherical particles were obtained by hydrolysis of the metal precursor in presence of a strong base at temperatures above the solvent’s boiling point. Hence, the reaction is dramatically accelerated and within seconds – instead of hours at lower temperatures –, narrowly dispersed particle systems are yielded. The particles’ sizes as derived from SAXS strongly depend on the reaction temperature and time. Choosing the right reaction conditions, the particle size and thus their band gap can be finely tuned. A size increase can be achieved both by increasing the reaction temperature and the reaction time. See Figure 1 for an exemplary comparison of five-minute syntheses at different temperatures. Here, the yielded particles display diameters between 5.0 and 7.6 nm and corresponding band-gaps of 3.32 up to 3.41 eV. The size increase is accompanied by a red-shift of the UV/Vis absorption edges and fluorescence emission. Furthermore, these particles can be transferred into water by coating with polysorbates. T2 - SAS2018 XVII International Small Angle Scattering Conference CY - Traverse City, Michigan, USA DA - 07.10.2018 KW - SAXS KW - Zinc oxide nanoparticles KW - Microwave synthesis PY - 2018 AN - OPUS4-46348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abbas, Ioana M. A1 - Vranic, M. A1 - Hoffmann, Holger A1 - El-Khatib, Ahmed H. A1 - Montes-Bayón, M. A1 - Möller, H. M. A1 - Weller, Michael G. T1 - Investigations of the copper peptide hepcidin-25 by LC-MS/MS and NMR (+) N2 - Hepcidin-25 was identified as the main iron regulator in the human body, and it by binds to the sole iron-exporter ferroportin. Studies showed that the N-terminus of hepcidin is responsible for this interaction, the same N-terminus that encompasses a small copper(II)-binding site known as the ATCUN (amino-terminal Cu(II)- and Ni(II)-binding) motif. Interestingly, this copper-binding property is largely ignored in most papers dealing with hepcidin-25. In this context, detailed investigations of the complex formed between hepcidin-25 and copper could reveal insight into its biological role. The present work focuses on metal-bound hepcidin-25 that can be considered the biologically active form. The first part is devoted to the reversed-phase chromatographic separation of copper-bound and copper-free hepcidin-25 achieved by applying basic mobile phases containing 0.1% ammonia. Further, mass spectrometry (tandem mass spectrometry (MS/MS), high-resolution mass spectrometry HRMS)) and nuclear magnetic resonance (NMR) spectroscopy were employed to characterize the copper-peptide. Lastly, a three-dimensional (3D)model of hepcidin-25with bound copper(II) is presented. The identification of metal complexes and potential isoforms and isomers, from which the latter usually are left undetected by mass spectrometry, led to the conclusion that complementary analytical methods are needed to characterize a peptide calibrant or reference material comprehensively. Quantitative nuclear magnetic resonance (qNMR), inductively-coupled plasma mass spectrometry (ICP-MS), ion-mobility spectrometry (IMS) and chiral amino acid analysis (AAA) should be considered among others. KW - Metalloprotein KW - Peptide KW - Chromatography KW - High pH KW - Mobile phase KW - Metrology KW - Purity KW - Reference material KW - ATCUN KW - Copper KW - Nickel PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-457796 UR - http://www.mdpi.com/1422-0067/19/8/2271 DO - https://doi.org/10.3390/ijms19082271 SN - 1422-0067 VL - 19 IS - 8 SP - 2271, 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-45779 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Abbas, Ioana M. T1 - Development of LC-MS/MS methods for the quantitative determination of hepcidin-25, a key regulator of iron metabolism N2 - Isotope-dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) is emerging in the field of clinical chemistry and laboratory medicine as an alternative to immunoassays and is acknowledged as the MS “gold standard” for small biomolecule quantification. Hepcidin-25, a key iron-regulatory peptide hormone discovered in 2000, has revolutionized the understanding of iron disorders and its quantitative determination in biological samples should advance the management of iron-related pathology (diagnosis, prognosis and treatment). This study applied LC-MS/MS, using the triple quadrupole (QqQ) mass spectrometer, in a rapid and robust analytical strategy for the quantification of hepcidin-25 in human serum, to be implemented in routine laboratories. For this purpose, two sample preparation strategies and two complementary chromatographic separation conditions were investigated, where the use of acidic mobile phases (0.1% trifluoroacetic acid) was compared with a novel approach involving solvents at high pH (containing 0.1% ammonia). The application of these LC-MS/MS methods to human samples in an intra-laboratory comparison, using the same hepcidin-25 calibrators, yielded a very good correlation of the results. The LC-MS/MS employing trifluoroacetic acid-based mobile phases was selected as a highly sensitive (limit of quantification LOQ of 0.5 μg/L) and precise (coefficient of variation CV<15%) method and was recommended as a reference method candidate for hepcidin-25 quantification in real samples (in the dynamic range of 0.5-40 μg/L). One of the novel aspects of the methodology was the use of amino- and fluoro-silanized autosampler vials to reduce the interaction of the 25-residue peptide to laboratory glassware surfaces. Moreover, this LC-MS/MS method was used for an international round robin study, applying a secondary reference material as a calibrator. By determining the degree of equivalence between the results of the ten participating methodologies, the performance of the method developed in this study was found to be in the optimal range as defined by the International Consortium for Harmonization of Clinical Laboratory Results (ICHCLR). In this work, the formation of hepcidin-25 complexes with copper(II) was investigated. The first reversed-phase chromatographic separation of hepcidin-25/Cu2+ and hepcidin-25 (copper “free”) was achieved by applying mobile phases containing 0.1% of ammonia (pH 11). LC-MS/MS and high-resolution mass spectrometry (Fourier-transform ion cyclotron resonance (FTICR) MS) were applied for the mass spectrometric characterization of the formed hepcidin-25-Cu(II) species at pH values of 11 and 7.4 respectively. A new species corresponding to hepcidin-25 complexed with two copper ions was identified at high pH. KW - Copper KW - LC-MS/MS KW - Chromatography KW - Mass spectrometry KW - Metal complex KW - Metalloprotein KW - Peptide KW - Metrology KW - Reference material PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:11-110-18452/20119-6 UR - https://edoc.hu-berlin.de/handle/18452/20119?show=full DO - https://doi.org/10.18452/19358 SP - 1 EP - 156 CY - Berlin AN - OPUS4-45780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Santos de Freitas, M. A1 - Araghi, R. R. A1 - Brandenburg, E. A1 - Leiterer, Jork A1 - Emmerling, Franziska A1 - Folmert, K. A1 - Gerling-Driessen, U. I. M. A1 - Bardiaux, B. A1 - Böttcher, C. A1 - Pagel, K. A1 - Diehl, A. A1 - v. Berlepsch, H. A1 - Oschkinat, H. A1 - Koksch, B. T1 - The protofilament architecture of a de novo designed coiled coil-based amyloidogenic peptide N2 - Amyloid fibrils are polymers formed by proteins under specific conditions and in many cases they are related to pathogenesis, such as Parkinson’s and Alzheimer’s diseases. Their hallmark is the presence of a β-sheet structure. High resolution structural data on these systems as well as information gathered from multiple complementary analytical techniques is needed, from both a fundamental and a pharmaceutical perspective. Here, a previously reported de novo designed, pH-switchable coiled coil-based peptide that undergoes structural transitions resulting in fibril formation under physiological conditions has been exhaustively characterized by transmission electron microscopy (TEM), cryo-TEM, atomic force microscopy (AFM), wide-angle X-ray scattering (WAXS) and solid-state NMR (ssNMR). Overall, a unique 2-dimensional carpet-like assembly composed of large coexisiting ribbon-like, tubular and funnel-like structures with a clearly resolved protofilament substructure is observed. Whereas electron microscopy and scattering data point somewhat more to a hairpin model of β-fibrils, ssNMR data obtained from samples with selectively labelled peptides are in agreement with both, hairpin structures and linear arrangements. KW - Amyloid KW - Elektronenmikroskopie PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-458713 UR - https://www.sciencedirect.com/science/article/pii/S1047847718301333 DO - https://doi.org/10.1016/j.jsb.2018.05.009 SN - 1047-8477 VL - 203 IS - 3 SP - 263 EP - 272 PB - Elsevier AN - OPUS4-45871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana A1 - Maiwald, Michael T1 - Produzieren Sie schon oder kalibrieren Sie noch? – Online-NMR-Spektrometer als Smarte Feldgeräte N2 - Der Übergang von der aktuellen Automatisierungslandschaft zur nächsten Generation von Automatisierungskonzepten für die Prozessindustrie hat bereits begonnen. Intelligente Funktionen der Sensoren vereinfachen ihre Anwendung und ermöglichen eine Plug-and-Play-Integration, auch wenn sie auf den ersten Blick komplexer erscheinen mögen. Dies ist die Basis für die Digitalisierung der Prozessindustrie und hilft uns, komplexere Prozesse schneller umzusetzen. Der Vortrag fasst die derzeit diskutierten allgemeinen Anforderungen an „Smarte Feldgeräte“ zusammen und diskutiert dieses am Beispiel eines smarten Online-NMR-Sensors. NMR-Spektroskopie bietet sich durch den Vorteil der direkten Vergleichsmethode (ohne Kalibrierung) für die Prozess-Steuerung an und verringert somit die Rüstzeiten. Zudem basiert der Sensor auf physikalisch motivierten Modellen (Indirect Hard Modeling, IHM), die sich modular kombinieren lassen. Die Methoden wurden anhand eines vorgegebenen pharmazeutischen Reaktionsschrittes im Rahmen des „Horizon 2020“-Projekts CONSENS der Europäischen Union demonstriert und validiert. Zuletzt werden Anforderungen an die Weiterentwicklung der Datenauswertemethoden diskutiert, um letztlich die semantische Information aus den Messdaten herauszulesen oder das in der Industrie 4.0 geforderte „durchgehende Engineering“ für die Automatisierungskomponenten zu ermöglichen. T2 - ProcessNet-Jahrestagung und 33. DECHEMA-Jahrestagung der Biotechnologen CY - Aachen, Germany DA - 10.09.2018 KW - Prozessindustrie KW - Prozessanalytik KW - Online-NMR-Spektroskopie KW - Datenkonzepte KW - Datenanalyse KW - CONSENS PY - 2018 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-45934 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope dilution mass spectrometry applied as primary method of measurement with examples from the ENVCRM project N2 - The presentation describes the application of isotope dilution mass spectrometry as a primary method of measurement with all Advantages and disadvantges. This is exempflified for the candidate reference materials within the EnvCRM Project. T2 - Workshop Matrix Reference Materials for Environmental Analysis CY - Gebze, Turkey DA - 16.05.2018 KW - Reference material KW - Soil KW - Heavy metals PY - 2018 AN - OPUS4-45896 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tatzel, Michael T1 - How to measure the three-isotope composition of metal(oid) elements by MC-ICP-MS N2 - In chemical elements with three or more stable isotopes, mass-dependent stable isotope fractionation yields correlated isotope ratios, m2/m1 and m3/m1. In three-isotope space, i.e. in a δ’m2/δ’m1 vs. δ’m3/δ’m1 plot, data align along a slope θ, the so called ‘triple isotope fractionation exponent’ that scales the two isotope ratios. Theoretical calculations predict small differences in θ for kinetic- and equilibrium isotope fractionation (Young et al. 2002) and thus the precise measurement of θ allows constraining the reaction mechanism. However, due to an apparent lack of precision of stable isotope analysis by MC-ICP-MS, θ is merely used as analytical quality control, i.e. for demonstration that samples and standards plot within their analytical precision in the range of theoretical θ-values originating in δ-zero. We show how θ can be determined precisely enough by MC-ICP-MS to distinguish kinetic- and equilibrium isotope fractionation, even when isotopic differences between samples are low. For low magnitudes of isotope fractionation, we exploit new, isotopically fractionated isotope standard materials (Vogl et al. 2016). We determine quality norms regarding interferences and measurement conditions to warrant trueness and to maximize precision. We exemplary explore the measurement of the three-isotope composition of Mg stable isotopes, budget the uncertainty of θ-values, and report the first θ-values of carbonate-water pairs and bioapatite. Our measurement approach adds a new dimension to isotope data beyond the δ-scale that has a high potential to reveal different modes of (bio)mineral precipitation in the sedimentary and biological record and thus to contribute solving conundrums in the Earth and Life Sciences. T2 - 13. Symposium Massenspektrometrische Verfahren der Elementspurenanalyse CY - Berlin, Germany DA - 03.09.2018 KW - Isotope fractionation KW - Delta values KW - Magnesium PY - 2018 AN - OPUS4-45898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana A1 - Kern, Simon A1 - Meyer, Klas A1 - Wander, Lukas A1 - Bornemann-Pfeiffer, Martin A1 - Maiwald, Michael T1 - Produzieren Sie schon oder kalibrieren Sie noch? – Online-NMR-Spektrometer als Smarte Feldgeräte N2 - Der Vortrag zeigt allgemeine Anforderungen an "smarte Feldgeräte" und deren Entwicklung in den vergangenen Jahren. Am Beispiel eines smarten Online-NMR-Sensors, der in einem EU-Projekt von der BAM entwickelt wurde, wird die Umsetzung der Anforderung aufgezeigt. Schließlich werden weitere Technologieanforderungen und Lösungsansätze vorgestellt. T2 - ProcessNet-Jahrestagung und 33. DECHEMA-Jahrestagung der Biotechnologen CY - Aachen, Germany DA - 10.09.2018 KW - Prozessanalytik KW - Prozessindustrie KW - Online-NMR-Spektroskopie KW - Datenkonzepte KW - Datenanalyse KW - CONSENS PY - 2018 UR - https://onlinelibrary.wiley.com/doi/abs/10.1002/cite.201855229 DO - https://doi.org/10.1002/cite.201855229 SN - 0009-286X N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. VL - 90 IS - 9 SP - 1236 EP - 1236 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-45901 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottu Mukkula, A. R. A1 - Engell, S. A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Maiwald, Michael T1 - PAT-basierte iterative Optimierung der Fahrweise eines kontinuierlichen organischen Syntheseprozesses N2 - Im Zuge der Digitalisierung der Prozessindustrie werden zunehmend modellbasiere Echtzeitoptimierungsverfahren eingesetzt, sog. „Advanced Process Control“. Mithilfe der sogenannten Modifier-Adaptation ist eine iterative Betriebspunktoptimierung auch mit ungenauen Modellen möglich, sofern zuverlässige Prozessdaten zur Verfügung stehen. Am Beispiel eines smarten Online-NMR-Sensors, der in einem EU-Projekt von der BAM entwickelt wurde, konnte das Konzept in einer modularen Produktionsanlage zur Herstellung eines pharmazeutischen Wirkstoffs erfolgreich getestet werden. T2 - ProcessNet-Jahrestagung und 33. DECHEMA-Jahrestagung der Biotechnologen CY - Aachen, Germany DA - 10.09.2018 KW - Prozessanalytik KW - Echtzeitoptimierungsverfahren KW - Modifier-Adaptation KW - Prozess-Steuerung KW - Betriebspunktoptimierung KW - CONSENS PY - 2018 UR - https://onlinelibrary.wiley.com/doi/abs/10.1002/cite.201855233 DO - https://doi.org/10.1002/cite.201855233 SN - 0009-286X VL - 90 SP - 1237 EP - 1237 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-45902 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Loehr, Konrad T1 - Towards single cell arraying for LA-ICP-MS N2 - Analysis of single cells via LA-ICP-MS is a technique with great potential, however manual targeting of single cells is laborious and therefore microarraying of cells looks promising. In this work, we investigate the potential of a commercial non-contact piezo dispenser arraying system (S3, Scienion AG, Berlin), equipped with a novel technology for single-cell isolation called CellenONE™ (Cellenion, Lyon). Usually if one aims to create a microarray of single cells via spotting a suitably diluted cell suspension, one will observe a Poisson-distributed cell number per spot. CellenONE™ overcomes this problem by controlling the number of cells optically in the piezo dispense capillary (PDC) via image recognition to obtain true single cell arrays. The figures of merit of the customized and optimized setup will be presented. In a proof of concept experiment we investigated the trace elemental fingerprint of THP-1 cells by LA-ICP-TOF-MS (Analyte G2, Teledyne Cetac; icpTOF, TOFWERK) and quantified two metal cell dyes, mDOTA-Ho (CheMatech, Dijon), and Ir-DNA intercalator (Fluidigm, San Francisco). For that, matrix matched calibration standards after Wang et al. were successfully prepared using the same arraying system. We believe that this novel approach opens new ways for automated quantitative single cell LA-ICP-MS. T2 - DIAGNOSTICS 8.0 CY - Berlin, Germany DA - 06.09.2018 KW - High throughput KW - Single cell KW - Laser ablation KW - ICP-MS KW - CellenONE PY - 2018 AN - OPUS4-45904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Delta values & isotope ratios - potential CCQM comparisons N2 - The talk presents several potential CCQM comparisons for delta values and isotope ratios with a focus on metals and semi-metals. T2 - CCQM IRWG Meeting CY - Paris, France DA - 18.04.2018 KW - Isotope amount ratio KW - Traceability KW - Uncertainty PY - 2018 AN - OPUS4-45895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosemann, Paul A1 - Kauss, N. T1 - Visualization of material-related susceptibility to pitting corrosion with the “KorroPad” indicator test N2 - The KorroPad indicator test was invented at the Federal Institute for Materials Research and Testing to detect stainless-steel surfaces susceptible to pitting corrosion. The KorroPad indicator test is thus an interesting alternative for manufacturers, processors, users and researchers to time consuming exposition experiments and complex electrochemical investigations, which are normally used to reveal surface-related processing errors resulting in reduced pitting corrosion resistance. Furthermore, the KorroPad indicator test can be used to visualize alloy- and microstructure-related factors causing susceptibility to pitting corrosion. The detection limit of the KorroPad indicator test was characterized in this work using reference alloys with different chromium content (5 % to 18 %). The alloy-specific detection limit was shifted successfully to higher chromium content by increasing the concentrations of NaCl and K3[Fe(CN)6]. The modified KorroPads can now be used to establish an alloy-specific quality control regarding the pitting corrosion resistance of different stainless steel grades. T2 - EUROCORR CY - Krakow, Poland DA - 09.09.2018 KW - Corrosion KW - KorroPad KW - Stainless steel KW - Corrosion resistance KW - Corrosion testing KW - Pitting corrosion PY - 2018 AN - OPUS4-45953 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Detjens, Marc A1 - Hübert, Thomas A1 - Tiebe, Carlo A1 - Banach, Ulrich T1 - Coulometric trace humidity measurement in technical gases N2 - Trace humidity was measured by using miniaturized planar coulometric sensors in technical gases such as hydrogen, nitrogen, helium, nitrous oxide, and synthetic air. Frost point temperatures tf in the gases ranged from −60 °C to −30 °C, which is equivalent to a vapour mole fraction xv from 10 μmol mol−1 to 376 μmol mol−1. In addition, the generated humidity was determined by using a precision dew point hygrometer as reference. Nonlinear calibration functions were calculated that correlated electric current (sensor signal) and reference humidity. Parameters of functions were tested with one-way analysis of variances (ANOVA) to prove if all used sensors had a similar behavior in the same gas during experiments. Results of ANOVA confirmed that averaged functions can be applied for trace humidity measurement in nitrogen, helium, nitrous oxide, and synthetic air. The calculated functions were negligibly different for nitrogen, helium, and synthetic air. In humidified nitrous oxide, a minor change of parameters was observed due to lower electrical currents. In total contrast to that, the measured sensor signals were significantly higher in humidified hydrogen and each sensor required its own calibration function. The reason was a recombination effect that favoured multiple measurements of water molecules. Nevertheless, it was possible to measure continuously trace humidity in all tested gases by using coulometric sensors with an expanded uncertainty below 2 K (k = 2). KW - ANOVA KW - Trace humdity measurement KW - Coulometric sensors KW - Chemical sensors KW - Measurement uncertainty PY - 2018 DO - https://doi.org/10.1063/1.5008463 SN - 0034-6748 SN - 1089-7623 VL - 89 IS - 8 SP - 085004, 1 EP - 8 PB - American Institute of Physics (AIP) CY - Maryland (USA) AN - OPUS4-45956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tiebe, Carlo A1 - Detjens, Marc A1 - Banach, Ulrich A1 - Hübert, Thomas T1 - Measurement uncertainty of coulometric trace humidity sensors N2 - Especially trace amounts of water vapour in gases can be reliably determined by coulometric trace humidity sensors. The principle of these sensors is based on water vapour absorption in a hygroscopic layer and its subsequent electrolytic decomposition. The calibration of sensors was performed in the humidity range, expressed as frost point temperature, from −30°C to −80°C . This range is equivalent to volume fractions smaller than 376 µL·L−1. Generated humidity was measured with coulometric sensors and a chilled dew point hygrometer that was used as reference. An empirical non-linear function was found between sensor signal and measured reference humidity. This function consists of two parameters with a measurement uncertainty. Both calibration parameters were checked by means of one-way analysis of variance. It showed that gas specific function can be used for humidity measurement in nitrogen, hydrogen, dinitrogen monoxide, compressed and synthetic air. It is possible to determine trace humidity in all tested gases with an expanded uncertainty less than 2.1 K (coverage factor k=2 ) regarding frost point temperature. KW - Trace humidity KW - Coulometric sensor KW - Measurement uncertainty KW - ANOVA PY - 2018 DO - https://doi.org/10.1515/teme-2018-0031 SN - 0171-8096 VL - 85 IS - 12 SP - 746 EP - 753 PB - De Gruyter CY - Oldenbourg AN - OPUS4-45959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Development of a device for staged determination of water activity and moisture content N2 - Moisture content and water activity are important parameters of product characterization; thus, an exact determination is necessarily required in a wide range of industrial applications. Moisture content of materials is the content of non-chemically bound water in a solid or liquid. Water activity (aW) is a characteristic/parameter of the non-chemically bound ("free") water in materials and is measured as humidity over a solid/liquid surface at constant temperature (equilibrium moisture content). It is an important parameter to characterize the quality of pharmaceutical and food products. In our contribution, we present a developed device for staged determination of water activity and moisture content of liquid and solid materials. T2 - Eurosensors 2018 CY - Graz, Austria DA - 09.09.2018 KW - Water activity KW - Moisture content KW - Measuring cell KW - Sorption isotherm PY - 2018 AN - OPUS4-45943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donėlienė, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. A1 - Hodoroaba, Vasile-Dan T1 - Electron Microscopy and X-Ray Diffraction Analysis of Titanium Oxide Nanoparticles Synthesized by Pulsed Laser Ablation in Liquid N2 - A femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD(two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. KW - Laser ablation in liquid KW - Nanoparticles KW - Titanium oxide KW - Particle morphology PY - 2018 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/electron-microscopy-and-xray-diffraction-analysis-of-titanium-oxide-nanoparticles-synthesized-by-pulsed-laser-ablation-in-liquid/AE368446FAC70E08C514F9AEABFD131B DO - https://doi.org/10.1017/S1431927618009030 VL - 24 IS - S1 (August) SP - 1710 EP - 1711 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-45949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Kim, K. J. T1 - Measurement of Elemental Composition of FeNi and SiGe Thin Films by Electron Probe Microanalysis with Stratagem Software N2 - The present study repeats electron probe microanalysis (EPMA) measurements with the thin film analysis software Stratagem on an Fe-Ni thin films on silicon and reports - for the first-time – results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide substrate. If the very good EPMA/Stratagem results for the FeNi system were expected due to previous studies [2], the data obtained for the SiGe films are particularly valuable, because of the challenging insulator substrate of Al2O3. The conductivity of the Si1-xGex surface necessary for charging-free analysis was ensured by applying conductive copper tape onto film surface down to sample stage. Four accelerating voltages, 15, 20, 25 and 30 kV, have been applied, so that the Ge Kα X-ray line at 9.87 keV could be excited. KW - thin film analysis KW - X-ray spectroscopy KW - Fe-Ni KW - Si-Ge KW - Stratagem KW - Electron probe microanalysis (EPMA) PY - 2018 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/measurement-of-elemental-composition-of-feni-and-sige-thin-films-by-electron-probe-microanalysis-with-stratagem-software/D4CF5D45B11FCF0DEC8155A89EDACF25 DO - https://doi.org/10.1017/S1431927618004282 VL - 24 IS - S1 (August) SP - 758 EP - 759 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-45950 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Hertwig, Andreas A1 - Kraehnert, R. A1 - Hodoroaba, Vasile-Dan T1 - Analysis of mesoporous iridium oxide thin films by the combined methodical approach SEM/EDS/STRATAGem N2 - For the determination of porosity of Ir oxide thin films, electron probe microanalysis (EPMA) can be used as part of a combined SEM/EDS/STRATAGem analysis. The mass deposition (in μg cm-2) of films was calculated with the analysis software STRATAGem via k-values measured with EDS. The average density of coated films was obtained from the mass deposition and the film thickness as measured by the cross-section SEM. The porosity was calculated by dividing the average film density by the bulk (theoretical) density of the film material. Film porosities were counterchecked by spectroscopic ellipsometry (SE) using the Bruggeman effective medium approximation (BEMA). The results obtained by both analytical approaches/methods used, SEM/EDS/STRATAGem and SE were in good agreement. KW - Porous thin films KW - Iridium oxide KW - Electron probe microanalysis (EPMA) KW - Spectroscopic ellipsometry PY - 2018 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/analysis-of-mesoporous-iridium-oxide-thin-films-by-the-combined-methodical-approach-semedsstratagem/7607018338B542D8B8C4D944392781EF DO - https://doi.org/10.1017/S1431927618004300 SN - 1431-9276 SN - 1435-8115 VL - 24 IS - S1 (August) SP - 762 EP - 763 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-45951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Jürgens, Maria A1 - Olbricht, Jürgen A1 - Winkelmann, Aimo T1 - Improving the precision of orientation measurements from technical materials via EBSD pattern matching N2 - We use pattern matching of experimental and dynamically simulated backscattered Kikuchi diffraction (BKD) patterns to increase the orientation precision of electron backscatter diffraction (EBSD) measurements. In order to quantify the improvement in orientation precision, we analyze the experimental distribution of the kernel average misorientation (KAM) angles. We find that for the same raw data, i.e. the same EBSD data acquisition time budget, the pattern matching approach improves the KAM resolution by an order of magnitude compared to orientation data delivered from the conventional Hough-transform based data analysis. This quantitative improvement enables us to interpret small orientation changes in plastically deformed materials which are hidden in noisy orientation data delivered from the reference EBSD system. As an application example, we analyze a ferritic-martensitic steel (P92) sample before and after low-cycle fatigue (LCF) loading (±0.3% strain) at 620 °C. Whereas the low precision of the EBSD orientation data from the manufacturer software does not allow a reliable discrimination of the gradually changing microstructure, we find very clear systematic differences of the local microstructure after the pattern matching orientation refinement of the initial, raw pattern data. For the investigated P92 sample, the KAM-angle histograms are well described by two log-normal distributions indicating the already tempered and the remaining and mostly untempered martensite. KW - Misorientation KW - Thermo-mechanical loading KW - Martensite KW - Log-normal distribution KW - Bimodal distribution PY - 2018 DO - https://doi.org/10.1016/j.actamat.2018.08.028 VL - 159 SP - 408 EP - 415 PB - Elsevier Ltd. AN - OPUS4-46454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Han, M. A1 - Chen, C. A1 - Zhao, G. A1 - Li, L. A1 - Yo, B. A1 - Huang, X. A1 - Zhu, Y. T1 - Blind lattice-parameter determination of cubic and tetragonal phases with high accuracy using a single EBSD pattern N2 - The Bravais lattices and their lattice parameters are blindly determined using electron backscatter diffraction (EBSD) patterns of materials with cubic or tetragonal crystal structures. Since the geometric relationships in a single EBSD pattern are overdetermined, the relative errors of determining the lattice parameters as well as the axial ratios are confined to about 0.7 ± 0.4% and 0.07 ± 0.03%, respectively, for ideal simulated EBSD patterns. The accuracy of the crystal orientation determination reaches about 0.06 ± 0.03°. With careful manual band detection, the accuracy of determining lattice parameters from experimental patterns can be as good as from simulated patterns, although the results from simulated patterns are often better than expermental patterns, which are lower quality and contain uncertain systematic errors. The reasonably high accuracy is obtained primarily because the detection of the diffracting-plane traces and zone axes is relatively accurate. The results here demonstrate that the developed procedure based on the EBSD technique presents a reliable tool for crystallographic characterization of the Bravais lattices of unknown phases. KW - EBSD KW - Bravais lattice KW - Lattice parameters KW - Kikuchi pattern PY - 2018 DO - https://doi.org/10.1107/S2053273318010963 SN - 2053-2733 VL - 74 IS - 6 SP - 630 EP - 639 PB - International Union of Crystallography AN - OPUS4-46455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Principles for the development of standards for investigation procedures of plastics in environmental media and materials N2 - An overview about the current status of microplastic analysis is given with scope on hamonisation and standarisation. T2 - Annual ISO/TC 61 Meeting CY - Saitama, Japan DA - 24.09.2018 KW - Standardisation KW - Microplastic KW - Analysis PY - 2018 AN - OPUS4-46457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Entwicklung einer schnellen und robusten Methode für die Analytik von Mikroplastik in Wasser N2 - Vortrag im Rahmen der Preisverleihung zum Mülheimer Wasser Award 2018, Vorstellung der TED-GC-MS als Methode für Mikroplastik Analyse T2 - 3. Wasseranalytisches Seminar (MWAS 2018) CY - Mülheim a.d. Ruhr, Germany DA - 12.09.2018 KW - Mikroplastik KW - Analytik PY - 2018 AN - OPUS4-46459 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eisentraut, Paul A1 - Dümichen, Erik A1 - Ruhl, A. A1 - Jekel, M. A1 - Albrecht, M. A1 - Gehde, M. A1 - Braun, Ulrike T1 - Two Birds with One Stone-Fast and Simultaneous Analysis of Microplastics: Microparticles Derived from Thermoplastics and Tire Wear N2 - Analysis of microplastic particles (MP) in environmental samples needs sophisticated techniques and is time intensive due to sample preparation and detection. An alternative to the most common (micro ) spectroscopic techniques, FTIR or Raman spectroscopy, are the thermoanalytical methods, where specific decomposition products can be analyzed as marker compounds for different kind of plastics types and mass contents. Thermal extraction desorption gas chromatography mass spectrometry (TED-GC-MS) allows the fast identification and quantification of MP in environmental samples without sample preparation. Whereas up to now only the analysis of thermoplastic polymers was realized, this is the first time that even the analysis of tire wear (TW) content in environmental samples is possible. Various marker compounds for TW were identified. They include characteristic decomposition products of elastomers, antioxidants and vulcanization agents. Advantages and drawbacks of these marker substances were evaluated. Environmental samples from street run off were exemplarily investigated and presented. KW - TED-GC-MS KW - Microplastic KW - Tire wear PY - 2018 DO - https://doi.org/10.1021/acs.estlett.8b00446 VL - 5 IS - 10 SP - 608 EP - 613 PB - American Chemical Society AN - OPUS4-46460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Park, J. A1 - Kim, G. B. A1 - Lippitz, Andreas A1 - Kim, Y. M. A1 - Jung, D. A1 - Unger, Wolfgang A1 - Kim, Y.-P. A1 - Lee, T. G. T1 - Plasma-polymerized antifouling biochips for label-free measurement of protease activity in cell culture media N2 - We report polyethylene glycol (PEG)-grafting antifouling surfaces using a plasma copolymerized (PcP) technique to monitor protease activity in complex media. By varying the mixing ratio of the PEG and ethylenediamine (EDA) precursors, the PcP-PEG-EDA (PcP-PE) film was able to easily control surface amine density with good preservation of the internal PEG structure. We found that nonspecific protein adsorption was dramatically reduced in serum-containing media on the PcP-PE films, as opposed to that on plasma polymerized-EDA (PP-E) films without PEG. When SPR sensor chips coated with PcP-PE film were employed to detect protease activity, biotinylated luciferase probes (luciferase-peptide-biotin) on streptavidin-conjugated SPR chips enabled real-time and label-free measurement of matrix metalloproteinase activity in cell culture media. Owing to its excellent antifouling ability, this newly developed method boasts minimal nonspecific binding and can serve as a biochip platform to promote a wide range of applications in the biological field. KW - Polyethylene glycol (PEG)-grafting antifouling surface KW - Biochip KW - ATR-FTIR spectroscopy KW - XPS KW - NEXAFS KW - Plasma PY - 2019 DO - https://doi.org/10.1016/j.snb.2018.10.123 SN - 0925-4005 VL - 281 SP - 527 EP - 534 PB - Elsevier B.V. AN - OPUS4-46463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bente, Klaas T1 - The thermoacoustic effect and its application in air-coupled testing of composite structures N2 - Airborne ultrasonic testing of lightweight, structured composite materials enables fast and contact-free non-destructive testing in aerospace and avoids material degradation due to contact with a coupling liquid. Established resonant air-coupled transducers consist of piezocomposite materials and several matching layers or more advanced materials like charged cellular polypropylene. The relaxation time and the specific frequency of such mechanical ultrasound emitters limit the spectrum of applications for each device. A short pulse length is key for reliable defect detection and each component at test can be best characterized at material- and geometry-specific frequencies. Here we show that focused thermoacoustic transducers are suited for testing lightweight, structured composite plates. Since the ultrasound is generated in air, these transducers show no resonance behavior and emit a broadband acoustic spectrum between 1.2 kHz and 1 MHz. Composite specimens of 3 mm to 9 mm thickness made of polylactide with a honeycomb structure were tested. Flat bottom holes were introduced to quantify the spatial resolution of the imaging method inside the strongly anisotropic specimen. As no broadband receivers are available yet, cellular polypropylene transducers were used as receivers, which limits the bandwidth of the method towards the bandwidth of the receiver. Nevertheless, we demonstrate the competitiveness of the thermoacoustic transducer compared to mechanical emitters at their respective resonance frequencies. Because a thermoacoustic transmitter features a nearly ideal pulse width, a single transmitter can be coupled with receivers with different resonance frequencies. With the development of broadband ultrasound receivers, air-coupled ultrasound spectroscopy will likely be possible in the near future. The analyzed transducer holds the potential to speed up testing during production and maintenance in aerospace and automotives. Its combination with a broadband receiver could also expand the application field of air-coupled ultrasonic testing from a qualitative error detection towards a quantitative, spatially resolved analysis of mechanical material properties. T2 - 10th International Symposium on NDT in Aerospace CY - Dresden, Germany DA - 24.10.2018 KW - Thermoacoustics KW - Ultrasonic Testing KW - Broadband KW - Ultrasound Emission PY - 2018 AN - OPUS4-46466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bente, Klaas T1 - The thermoacoustic effect and its application in air-coupled testing of composite structures N2 - Airborne ultrasonic testing of lightweight, structured composite materials enables fast and contact-free non-destructive testing in aerospace and avoids material degradation due to contact with a coupling liquid. Established resonant air-coupled transducers consist of piezocomposite materials and several matching layers or more advanced materials like charged cellular polypropylene. The relaxation time and the specific frequency of such mechanical ultrasound emitters limit the spectrum of applications for each device. A short pulse length is key for reliable defect detection and each component at test can be best characterized at material- and geometry-specific frequencies. Here we show that focused thermoacoustic transducers are suited for testing lightweight, structured composite plates. Since the ultrasound is generated in air, these transducers show no resonance behavior and emit a broadband acoustic spectrum between 1.2 kHz and 1 MHz. Composite specimens of 3 mm to 9 mm thickness made of polylactide with a honeycomb structure were tested. Flat bottom holes were introduced to quantify the spatial resolution of the imaging method inside the strongly anisotropic specimen. As no broadband receivers are available yet, cellular polypropylene transducers were used as receivers, which limits the bandwidth of the method towards the bandwidth of the receiver. Nevertheless, we demonstrate the competitiveness of the thermoacoustic transducer compared to mechanical emitters at their respective resonance frequencies. Because a thermoacoustic transmitter features a nearly ideal pulse width, a single transmitter can be coupled with receivers with different resonance frequencies. With the development of broadband ultrasound receivers, air-coupled ultrasound spectroscopy will likely be possible in the near future. The analysed transducer holds the potential to speed up testing during production and maintenance in aerospace and automotives. Its combination with a broadband receiver could also expand the application field of air-coupled ultrasonic testing from a qualitative error detection towards a quantitative, spatially resolved analysis of mechanical material properties. T2 - 10th International Symposium on NDT in Aerospace CY - Dresden, Germany DA - 24.10.2018 KW - Thermoacoustics KW - Ultrasonic Testing KW - Broadband KW - Ultrasound Emission PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-464677 SN - 978-3-940283-96-2 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-46467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Chemical modification of graphene and carbon nano tubes as viewed by xps and nexafs spectroscopies with dft spectra simulation N2 - Graphene is a two-dimensional carbon network with unique properties. However, its low solubility, poor reactivity and the limited accessibility of a well-defined basal plane are major challenges for applications. An ideal method to overcome these problems is the covalent attachment of functional molecules to its surface which enable further reactive modifications for specific applications. There are several technologies for surface functionalization of graphene and related CNT materials. To get control on the functionalization process and to optimize the performance of the modified surfaces analytical tools for surface chemical characterization are required. X-ray absorption (NEXAFS) and photoelectron spectroscopy (XPS) have been identified to be rather powerful here [1-3]. Specifically, NEXAFS spectroscopy underpinned by quantum chemical spectrum simulations [4] is unique in a way to address changes of aromaticity and defect formation at the graphene surface during functionalization. For relevant surface modification technologies, we present examples on how NEXAFS and XPS can do a good job. All presented modifications aim on the production of platforms for defined functional 2D nanomaterials, as for example multifunctional hybrid architectures. In detail, we investigated: • A wet chemical method for covalent functionalization of graphene sheets by a one-pot nitrene [2+1] cycloaddition reaction under mild conditions. Here a reaction between 2,4,6-trichloro-1,3,5-triazine and sodium azide with thermally reduced graphene oxide (TRGO) results in defined dichlorotriazine-functionalized graphene sheets. • Graphene and carbon nanotube functionalized by Vacuum-Ultraviolet (VUV) induced photochemical or r.f. cw low pressure plasma processes to introduce amino, hydroxy or brominated functionalities. To underpin finger-print information delivered by C K-edge NEXAFS we studied the effects of selected point and line defects as well as chemical modifications for a single graphene layer model by density functional theory based spectrum simulations. References [1] P.-L. Girard-Lauriault et al., Appl. Surf. Sci., 258 2012 8448-8454, DOI: 10.1016/j.apsusc.2012.03.012 [2] A. Lippitz et al., Surf. Sci., 611 2013 L1-L7, DOI: 10.1016/j.susc.2013.01.020 [3] A. Faghani et al., Angew. Chemie (International ed.), 56 2017 2675-2679, DOI:10.1002/anie.201612422 [4] C. Ehlert, et al., Phys.Chem.Chem.Phys., 16 2014 14083-14095, DOI: 10.1039/c4cp01106f T2 - AVS 65th INTERNATIONAL SYMPOSIUM CY - Long Beach, CA, USA DA - 21.10.2018 KW - Graphene KW - Plasma KW - Nitrene [2+1] cycloaddition KW - XPS KW - NEXAFS PY - 2018 AN - OPUS4-46468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Acquiring and Documenting Reproducible Spectra, Depth Profiles and Images: XPS, AES and SIMS N2 - In this talk sample prep/handling, instrument calibration and data acquisition methods with examples from XPS, Auger and SIMS will be addressed in terms of their contributions to the reproducibility of data delivered by the methods. Active parties in the field are VAMAS TWA 2 “Surface chemical analysis” (http://www.vamas.org/twa2/index.html), ISO/TC 201 “Surface chemical analysis” (https://www.iso.org/committee/54618.html) and the Surface Analysis Working Group (SAWG) at the International Meter Convention (https://www.bipm.org/en/ committees/cc/wg/sawg.html). The tools to improve the reproducibility of spectra, depth profiles and images at these international platforms are inter-laboratory comparisons, validated SOPs, standards and certified reference materials (CRM) as well as uncertainty budgets and establishment of traceability chains. The last point is of specific importance because all the methods, XPS, Auger and SIMS, are not primary methods. To address quantitative XPS, AES and SIMS results of relevant inter-laboratory comparisons organized by SAWG considering measurands as alloy surface composition and thickness of thin films will be introduced. These comparisons delivered results which are viewed to be benchmarking, some of them resulted in ISO/TC 201 standards. For quantitative XPS and AES the principal outline of an uncertainty budget will be discussed together with the audience. Another issue of quantitative XPS which definitely needs consideration are valid methods for a determination of the transmission function of the instruments and even for the emission angle in the respective experiments. Concerning the field of depth profiling it has to be investigated together with the audience whether the ISO (or ASTM) standards we have are sufficient to guarantee comparable results. Having in mind the number of different sputter ion species available today and range of samples of interest (metals, semiconductors, organic films) this might be questionable. And, how do depth profiling by AR-XPS and variable excitation energy XPS compete here? For imaging surface chemical analysis, the characterization of the imaging system is an issue to be investigated. Here the determination of lateral resolution is a relevant topic. Finally, the future needs to develop metrology for new applications e.g., ambient-pressure XPS, bio samples, and core-shell nanoparticles, will be issues raised for a discussion with the audience. T2 - 17th Topical Conference on Quantitative Surface Analysis (QSA 17) CY - Long Beach, CA, USA DA - 21.10.2018 KW - Depth Profiles and Images KW - X-ray Photoelectron Spectroscopy (XPS) KW - Auger Electron Spectroscopy (AES) KW - SIMS KW - Reproducible Spectra PY - 2018 AN - OPUS4-46470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Electron Microscopy and X-Ray Diffraction Analysis of Titanium Oxide Nanoparticles Synthesized by Pulsed Laser Ablation in Liquid N2 - A femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated by XRD and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. T2 - Microscopy & Microanalysis 2018 CY - Baltimore, MD, USA DA - 05.08.2018 KW - Nanoparticles KW - Titanium oxide KW - Laser ablation in liquid KW - Electron microscopy KW - XRD PY - 2018 AN - OPUS4-46502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement of Elemental Composition of FeNi and SiGe Thin Films by Electron Probe Microanalysis with Stratagem Software N2 - The present study repeats electron probe microanalysis (EPMA) measurements with the thin film analysis software Stratagem on an Fe-Ni thin films on silicon and reports - for the first-time – results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide substrate. If the very good EPMA/Stratagem results for the FeNi system were expected due to previous studies, the data obtained for the SiGe films are particularly valuable, because of the challenging insulator substrate of Al2O3. The conductivity of the Si1-xGex surface necessary for charging-free analysis was ensured by applying conductive copper tape onto film surface down to sample stage. Four accelerating voltages, 15, 20, 25 and 30 kV, have been applied, so that the Ge Kα X-ray line at 9.87 keV could be excited. T2 - Microscopy & Microanalysis 2018 CY - Baltimore, MD, USA DA - 05.08.2018 KW - Electron probe microanalysis (EPMA) KW - Fe-Ni KW - Si-Ge KW - Stratagem KW - X-ray spectroscopy KW - thin film analysis PY - 2018 AN - OPUS4-46506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Z. A1 - Kruschwitz, Sabine A1 - Weller, A. A1 - Halisch, M. T1 - Enhanced pore space analysis by use of µ-CT, MIP, NMR, and SIP N2 - We investigate the pore space of rock samples with respect to different petrophysical parameters using various methods, which provide data on pore size distributions, including micro computed tomography (µ-CT), mercury Intrusion porosimetry (MIP), nuclear magnetic resonance (NMR), and spectral-induced polarization (SIP). The resulting cumulative distributions of pore volume as a function of pore size are compared. Considering that the methods differ with regard to their limits of resolution, a multiple-length-scale characterization of the pore space is proposed, that is based on a combination of the results from all of these methods. The approach is demonstrated using samples of Bentheimer and Röttbacher sandstone. Additionally, we compare the potential of SIP to provide a pore size distribution with other commonly used methods (MIP, NMR). The limits of Resolution of SIP depend on the usable frequency range (between 0.002 and 100 Hz). The methods with similar Resolution show a similar behavior of the cumulative pore volume distribution in the verlapping pore size range. We assume that µ-CT and NMR provide the pore body size while MIP and SIP characterize the pore throat size. Our study Shows that a good agreement between the pore radius distributions can only be achieved if the curves are adjusted considering the resolution and pore volume in the relevant range of pore radii. The MIP curve with the widest range in Resolution should be used as reference. KW - Pore space KW - Induced polarization KW - Mercury intrusion porosimetry KW - µ-CT KW - NMR PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-465071 DO - https://doi.org/10.5194/se-9-1225-2018 SN - 1869-9510 SN - 1869-9529 VL - 9 IS - 6 SP - 1225 EP - 1238 PB - Copernicus Publications CY - Göttingen AN - OPUS4-46507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Von Ägypten bis Hiddensee – Analyse von Gold mit Synchrotronstrahlung - Update 2018 N2 - Gold ist eines der sieben schon im Altertum bekannten Metalle und wurde wg. seines Glanzes und seiner Seltenheit von alters her als Tauschmittel und zur Herstellung von Schmuck benutzt. Außerdem ist es einfach bearbeitbar und weitestgehend gegen chemische Einflüsse resistent. Die Untersuchungen von Gold mit synchrotronstrahlungsangeregter Röntgenfluoreszenzanalyse sind zerstörungsfrei und geben Auskunft über die in der untersuchten Probe vorhandenen chemischen Elemente. Bei den hier vorgestellten Untersuchungen an der BAMline stehen Fragestellungen wie Herkunft, Herstellungsverfahren und Zusammengehörigkeit von Goldfunden im Vordergrund. Die verschiedenen Fragestellungen werden an einer Reihe von Beispielen erläutert die vom Wikingerschatz aus Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten langen. Zusätzlich werden die modernen Messmethoden vorgestellt, die am Synchrotron heutzutage zur Verfügung stehen. T2 - Vorlesung FU Berlin Einführung in die Archäometrie CY - Berlin, Germany DA - 01.11.2018 KW - Gold KW - Synchrotron KW - XRF KW - BAMline PY - 2018 AN - OPUS4-46451 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis T1 - Ein Überblick über die Scaled Boundary Finite Element Method für akustische Wellenausbreitung in Festköpern N2 - In diesen Vortrag sind Ergebnissen der letzten Jahre zu der SBFEM an der BAM zu finden. Dabei wurde besonders auf die Stärken der Methode eingegangen. T2 - Doktorandenseminar – Ultraschallmesstechnik CY - Gohrisch, Germany DA - 28.10.2018 KW - SBFEM KW - Kontaktbedingungen PY - 2018 AN - OPUS4-46452 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Snow, T. T1 - Modular SAXS data corrections N2 - A standardized methodology for the correction of scattering patterns, the calculation of uncertainties, the subtraction of backgrounds and solvents, optionally followed by the azimuthal averaging/reduction step, is presented. T2 - XVII International Small Angle Scattering Conference - SAS2018 CY - Traverse City, Michigan, USA DA - 07.10.2018 KW - Small-angle scattering KW - Software KW - Sata corrections KW - Quality PY - 2018 AN - OPUS4-46520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jemian, P. T1 - NXcanSAS: standard to store reduced SAS data of any dimension N2 - A SAS-specific extension of the NeXus file standard has been put together for the community to interchangably store measurement data, accompanied by all possible metadata. T2 - XVII International Small Angle Scattering Conference - SAS2018 CY - Traverse City, Michigan, USA DA - 07.10.2018 KW - Small-angle scattering KW - Data standard KW - NeXus KW - Archival format KW - Quality PY - 2018 AN - OPUS4-46521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fortini Moustafa Osman, Renata T1 - Development of a method for measuring the rigidity of nanofibers N2 - Over the past decades, the growing industry working for lightweight constructions has demanded materials exhibiting improved properties such as higher mechanical modulus and strength, better chemical resistance and lower costs of production. It is known that especially nanofibers tend to enhance the mechanical, thermal and electrical properties of polymers. Therefore, some types of nanofibers are already being used embedded in polymeric matrix of sports equipment, aircraft parts and automobile components. However, nanofibers are a relatively new material category, the consequences of which for mankind are not yet fully known. Nanofibers detached from polymeric materials can be released into the environment during, e.g., processing and aging. The risks in dealing with such nanofibers are generally unknown, even if further studies of health aspects are being carried out. Problems always arise when the fibers can penetrate the cells, thus the mechanical rigidity of nanofibers is a key factor in assessing the risks. Common methods describe the geometry of nanofibers. These methods are necessary, but not sufficient to describe the mechanical properties, as for during manufacture and aging these properties may change; the modulus and strength values may differ from those of the original fibers. Different experimental techniques for nanomechanical testing have been studied using the atomic force microscope, the scanning electron microscope and transmission electron microscope, showing promising results. This project aims to evaluate the bending stiffness of CNTs with an experimental setup within the Dynamic Scanning Electron Microscope. Based on the Euller-Bernoulli beam theory, the Young’s modulus of CNTs can be obtained using the resonance frequency of mechanically excited nanofibers, its dimensions and density. The resonance frequency is acquired by extracting the signals of the secondary electrons when the nanofibers show significant vibration movement, also possible to be seen on the microscope images. The electronic signals of the secondary electrons are filtered and treated by a lock-in amplifier, so the corresponding amplitude and phase values can be evaluated. This method could be applied to any nanofiber that has the shape similar to a symmetric beam. T2 - Workshop on Reference Nanomaterials Current situation and needs: development, measurement, standarization CY - Berlin, Germany DA - 14.05.2018 KW - Nanofiber KW - Rigidity KW - Resonance KW - DySEM PY - 2018 AN - OPUS4-46527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Diehn, Sabrina A1 - Zimmermann, B. A1 - Bagcioglu, M. A1 - Seifert, Stephan A1 - Kohler, A. A1 - Ohlson, M. A1 - Fjellheim, S. A1 - Weidner, Steffen A1 - Kneipp, Janina T1 - Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) shows adaption of grass pollen composition N2 - MALDI time-of-flight mass spectrometry (MALDI-TOF MS) has become a widely used tool for the classification of biological samples. The complex chemical composition of pollen grains leads to highly specific, fingerprint-like mass spectra, with respect to the pollen species. Beyond the species-specific composition, the variances in pollen chemistry can be hierarchically structured, including the level of different populations, of environmental conditions or different genotypes. We demonstrate here the sensitivity of MALDI-TOF MS regarding the adaption of the chemical composition of three Poaceae (grass) pollen for different populations of parent plants by analyzing the mass spectra with partial least squares discriminant analysis (PLS-DA) and principal component analysis (PCA). Thereby, variances in species, population and specific growth conditions of the plants were observed simultaneously. In particular, the chemical pattern revealed by the MALDI spectra enabled discrimination of the different populations of one species. Specifically, the role of environmental changes and their effect on the pollen chemistry of three different grass species is discussed. Analysis of the Group formation within the respective populations showed a varying influence of plant genotype on the classification, depending on the species, and permits conclusions regarding the respective rigidity or plasticity towards environmental changes. KW - Pollen KW - MALDI-TOF MS KW - Classification KW - Partial least square discriminant analysis (PLS-DA) KW - Principal component analysis (PCA) PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-465294 DO - https://doi.org/10.1038/s41598-018-34800-1 SN - 2045-2322 VL - 8 IS - 1 SP - 16591, 1 EP - 11 PB - Nature AN - OPUS4-46529 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Analysis of Mesoporous Iridium Oxide Thin Films by the Combined Methodical Approach SEM/EDS/STRATAGem N2 - For the determination of porosity of Ir oxide thin films, electron probe microanalysis (EPMA) can be used as part of a combined SEM/EDS/STRATAGem analysis. The mass deposition (in μg cm-2) of films was calculated with the analysis software STRATAGem via k-values measured with EDS. The average density of coated films was obtained from the mass deposition and the film thickness as measured by the cross-section SEM. The porosity was calculated by dividing the average film density by the bulk (theoretical) density of the film material. Film porosities were counterchecked by spectroscopic ellipsometry (SE) using the Bruggeman effective medium approximation (BEMA). The results obtained by both analytical approaches/methods used, SEM/EDS/STRATAGem and SE were in good agreement. T2 - Microscopy & Microanalysis 2018 CY - Baltimore, MD, USA DA - 05.08.2018 KW - Electron probe microanalysis (EPMA) KW - Iridium oxide KW - Porous thin films KW - Spectroscopic ellipsometry PY - 2018 AN - OPUS4-46509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - McSAS for SAS analysis: Usage, Benefits and Potential Pitfalls N2 - An introductory lecture for users at the Diamond Light Source, on how to use the McSAS software to analyze their data. T2 - Small Angle Scattering Training School CY - Diamond Light Source, Didcot, United Kingdom DA - 04.06.2018 KW - Small-angle scattering KW - Software KW - Analysis PY - 2018 AN - OPUS4-46517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - How good is SAXS? Results from a large Round Robin on an easy sample N2 - 22 laboratories returned 45 small-angle scattering datasets on a suspension of silver nanoparticles. The variance of the results has been analyzed in order to estimate the expected accuracy and precision of the small-angle scattering technique. T2 - XVII International Small Angle Scattering Conference - SAS2018 CY - Traverse City, Michigan, USA DA - 07.10.2018 KW - Small-angle scattering KW - Round Robin KW - Silver nanoparticles KW - Quality KW - McSAS PY - 2018 AN - OPUS4-46518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias T1 - Wind Vector Estimation on Multirotor Aircraft N2 - Small unmanned aircraft (UA) are used increasingly as flying sensor platforms. Amongst other things they are used for environmental monitoring, for example gas distribution mapping. Sometimes, these applications require knowledge of the ambient wind field, which can be measured by additional devices like anemometers. In general, it would be interesting to avoid such additional apparatuses. One way to achieve this is to estimate the wind vector, that is both the wind direction and speed, from the state variables of the UA. T2 - IEEE Sensors 2018 CY - New Delhi, India DA - 28.10.2018 KW - UAV KW - Wind vector KW - Estimation KW - Multirotor aircraft PY - 2018 AN - OPUS4-46479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias T1 - Comparison of the Temperature Behavior of Oil and Gas Damped Piezoresistive Accelerometers N2 - This study presents the characterization of a piezoresistive accelerometer damped with silicon oil for the application in drop tests carried out at BAM. Experiments were performed with the Hopkinson Bar method in close correlation to the real-world application conditions. The results point out certain limitations regarding the temperature influence and the frequency response. Additional experiments were performed with a gas damped type of piezoresistive accelerometer, which has superior specifications, particularly for low temperatures. The results allow for a comparison. T2 - IEEE SENSORS 2018 CY - Neu Delhi, Indien DA - 28.10.2018 KW - Accelerometer KW - Temperature behavior KW - Frequency response KW - Hopkinson Bar KW - Drop test PY - 2018 AN - OPUS4-46484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lörchner, Dominique A1 - Kroh, L.W. A1 - Köppen, Robert T1 - First insights into electrochemical transformations of two triazine-based brominated flame retardants in model systems N2 - In this work, a study of electrochemical conversion was performed to elucidate different degradation pathways of the heterocyclic brominated flame retardants 1,3,5-Tris-(2,3-dibromopropyl)-1,3,5-triazine-2,4,6-trione (TDBP-TAZTO) and 2,4,6-Tris-(2,4,6-tribromo-phenoxy)-1,3,5-triazine (TTBP-TAZ). EC/MS was used to simulate the (bio)-transformation processes and to identify possible transformation products (TPs) which have never been reported before. For TDBP-TAZTO, six new TPs were observed after the electrochemical oxidation (applied potential of 0 to 1,800 mV vs. Pd/H2). In case of TTBP-TAZ, seven debromination products were generated with an applied potential of 0 to 2,200 mV vs. Pd/H2. The main degradation pathways confirmed by high resolution mass spectrometry for both compounds were hydroxylation, debromination as well as dehydrobromination. KW - Emerging/novel brominated flame retardant KW - Transformation products KW - Electrochemistry mass spectrometry PY - 2018 DO - https://doi.org/10.1039/c8ay01968a SN - 1759-9660 SN - 1759-9679 VL - 10 IS - 43 SP - 5164 EP - 5170 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-46488 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Spectroscopic characterization of semiconductor and lanthanide-based nanocrystals with vis and NIR emission N2 - Common approaches to improve the optical properties of semiconductor quantum dots and lanthanide doped nanophosphors present core/shell structures as radiationless deactivation at the particle surface is usually the main energy loss mechanism. This has led to increasingly sophisticated particle architectures using multishell systems with shells of different chemical composition and thickness and initiated an increasing number of quantitative spectroscopic studies focusing on the key performance parameter photoluminescence quantum yield to identify optimum particle structures. This is particularly challenging in the long wavelength region > 1000 nm and for nonlinear emitters like upconversion nanocrystals. Here, we present suitable absolute methods to quantify the photoluminescence of these different emitters in the vis/NIR/IR and as function of excitation power density and underline the impact of such measurements on a profound mechanistic understanding of the nonradiative deactivation pathways in semiconductor and upconversion nanocrystals of different size and particle architecture in different environments. T2 - NANO 2018 CY - Hong Kong, People's Republic of China DA - 24.06.2018 KW - Upconversion KW - Semiconductor KW - Quantum dot KW - Nanoparticle KW - Absolute fluorometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Fluorescence KW - Surface chemistry KW - Deactivation pathways KW - Modeling KW - Size PY - 2018 AN - OPUS4-45797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Yamamoto, K. A1 - Grulke, E. A. T1 - Size and shape distribution of bipyramidal TiO2 nanoparticles by transmission electron microscopy – an inter-laboratory comparison N2 - Extraction of true, 3D shape (and size) of non-spherical nanoparticles (NPs) is associated with errors by conventional 2D electron microscopy using projection images. Significant efforts within the ISO technical committee TC 229 ‘Nanotechnologies’ are aimed at establishing accurate TEM and SEM measurement of NP size and shape as robust, standard procedures. Study groups have been organizing inter-laboratory comparisons on well-selected NP systems according to the market needs, such as aggregated titania nano-powder for which size and shape distribution of primary crystallites of irregular shape must be measured accurately. To be noticed is e. g. the fact that the measurement procedure allows only manual selection of the particles clearly distinguishable for analysis as well as manual definition of the contour of the imaged NPs. An inter-laboratory exercise on titania NPs (pure anatase, grown by hydrothermal synthesis) of well-defined non-spherical shape, i.e. bipyramidal has been recently started within ISO/TC 229 under similar conditions as for the irregular shaped titania. Overlapped particles were allowed to be considered, as long as they are clearly distinguishable. One decisive NP selection criterion was to analyze only those NPs with a roundness value below 0.7, i.e. the NPs laying on the support foil and, hence, with projection areas clearly deviating from perfect circles (R=1). The overall evaluation (for 15 labs) of the size descriptors (area, Feret, minFeret, perimeter) and shape descriptors (aspect ratio, roundness, compactness, extent) by analysis of variance is just to be finished and included in ISO/WD 21363 Nanotechnologies -- Protocol for particle size distribution by transmission electron microscopy. KW - Nanoparticles KW - Electron microscopy KW - Titanium oxide KW - Particle size distribution PY - 2018 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/size-and-shape-distribution-of-bipyramidal-tich-nanoparticles-by-transmission-electron-microscopy-an-interlaboratory-comparison/9E2FA0C716DB5F881E3032D014DFD52B DO - https://doi.org/10.1017/S1431927618009017 SN - 1431-9276 SN - 1435-8115 VL - 24 IS - S1 (August 2018) SP - 1706 EP - 1707 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-46005 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Procop, Mathias T1 - Check of the performance of EDS systems attached to the SEM with the test material EDS-TM001/2 and evaluation software package EDS spectrometer test - Application, experiences and updates N2 - The test material EDS-TM001 together with an accompanying software package, “EDX spectrometer check”, have been made available in 2009 by BAM to be employed by EDS (energy dispersive spectrometer) users to check the performance of an EDS attached to the SEM. Particularly for test laboratories operating under accreditation schemes like ISO/IEC 17025, a periodical control of the critical instrumental parameters in end-user laboratories is required. With EDS-TM001 or EDS-TM002 (second generation) test material, this periodical check is simplified to the acquisition of only one 10 kV spectrum. The software “EDX spectrometer check” is destined to evaluate automatically this spectrum and determine the performance of the EDS in terms of energy resolution and calibration as well as possible alteration of low-energy efficiency due to detector contamination. Energy resolution can be compared with the specified values according to the international ISO standard ISO 15632:2012. EDS-TM is a synthetic material consisting of a thick layer of C, Al, Mn, Cu and Zr in a well-defined composition, deposited on a steel (in case of EDS-TM001) or silicon (in case of EDS-TM002) substrate. Meanwhile, more than one hundred laboratories use the EDS-TM001 or EDS-TM002 test material for the periodical check of their EDS. A detailed description of the test material and software together with examples of application was published recently. New results and gained experiences will be presented as well. When the FWHM of lines appearing in the EDS-TM spectrum are determined, the spectrum background must be subtracted accurately. The applied physical background subtraction procedure is robust and takes into account the transmission of the detector window. While the previous version considers only Moxtek AP windows, the new version includes selection of silicon nitride window and the case of windowless detector. Moreover, the new version allows importing of spectra in Bruker spx format and EMSA/MSA files from EDAX TEAM software. KW - EDS KW - Performance check KW - SEM KW - Test material KW - X-ray spectrometer PY - 2018 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/check-of-the-performance-of-eds-systems-attached-to-the-sem-with-the-test-material-edstm0012-and-evaluation-software-package-eds-spectrometer-test-application-experiences-and-updates/3D01FDC765C3ECD734CB8DEC7081DAE2 DO - https://doi.org/10.1017/S1431927618004142 SN - 1431-9276 SN - 1435-8115 VL - 24 IS - S1 (August) SP - 730 EP - 731 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-46006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - NIR-Ringversuch II: Jetzt geht es los ! N2 - Ziele und Durchführung eines geplanten Ringversuchs zur Untersuchung eines Dreikomponentensystems mittels NIR werden vorgestellt. Der Vortrag enthält einen kurzen Rückblick auf einen 2014 durchgeführten Ringversuch, wobei ein flüssiges Zweikomponentensystem untersucht wurde. Im Anschluss erfolgt die Erläuterung der verwendeten Komponenten, es werden Teilnahmebedingungen und mögliche Zeiträume bekannt gegeben. T2 - 14. PAT ERFA CY - Leverkusen, Germany DA - 18.09.2018 KW - NIR KW - Chemometrie KW - Ringversuch PY - 2018 AN - OPUS4-46008 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dzierliński, M. T1 - Towards UAV-based Detection of Leaking Gas Pipelines N2 - Leaking methane (CH4) from infrastructures, such as pipelines and landfills, is critical for the environment but can also pose a safety risk. Nowadays, after a period of failure-free exploitation, a significant increase in fires and explosions due to pipeline leakages, can be observed. Particularly problematic are the gas pipelines in Poland that were built several decades ago. At that time, the technical standards and building regulations were more lenient than those currently being in force. The integrity of the gas pipelines is difficult to inspect as they are not piston-optimized (they were not built for this purpose). To overcome this challenge, the UDT is looking for methods that enable a fast and reliable detection and localization of leaking pipelines over long distances. The BAM has developed a robotic platform for aerial remote gas sensing that meets the expectations of UDT. Spectroscopic measurement methods for remote sensing of selected gases lend themselves for use on mini-copters, which offer several advantages for inspection and surveillance over traditional methods. No direct contact with the target gas is needed and thus the influence of the aerial platform on the measured gas plume can be kept to a minimum. This allows to overcome one of the major issues with gas-sensitive mini-copters. On the other hand, remote gas sensors, most prominently Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensors have been too bulky given the payload and energy restrictions of minicopters. Here, we present the Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), which combines a novel lightweight TDLAS sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile octocopter. It enables tomographic reconstruction of gas plumes and a localization of gas sources. Currently, UDT and BAM are cooperating to develop and validate an effective leakage detection method based on the UAV-REGAS platform. We present first results showing its performance under realistic conditions. Depending on the results, UDT may use this platform in their inspection practice in the near future. T2 - 1st EARSeL Workshop UAS “UAS for mapping and monitoring” CY - Warsaw, Poland DA - 05.09.2018 KW - UAV KW - Localization of gas sources KW - In-situ and remote gas sensing KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - Wind estimation PY - 2018 AN - OPUS4-45991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rietz, U. T1 - Determination of coating properties by using analytical centrifugation N2 - The majority of all products have coated surfaces designed to fulfil different requirements. Building constructions are exposed to external influences like a wide temperature and humidity range, rain and UV radiation to name a few. The extension of machine life for metal cutting tools, like drills or milling cutters is another field of application for coated surfaces. The surfaces have to be modified in a way to maintain their specific functionality. Although adhesion testing of coatings is of great interest, it is still a challenge to obtain reliable quantitative results and to meet economic requirements. In this talk we deal with the curing behaviour of different 2-component epoxy paint systems for corrosion protection of metal constructions. After preparation of specimens the strength was determined in specified time intervals during curing. It could be shown that epoxy paints differ significantly on curing time as well as final strength. The second experimental study deals with coating systems on glass fibre reinforced plastics which are used for wind power turbines to reduce abrasive wear and ice adhesion for aerodynamic and safety reasons. All measurements have been carried out by CAT-TechnologyTM (Centrifugal Adhesion Testing), which uses the radially directed centrifugal force as test-load. The multi-sample test instrument analyses up to eight test specimen under identical testing conditions. By varying the rotational speed (100 rpm up to 13,000 rpm), forces from 0.1 N to 6.5 kN are applied. Upon reaching the critical rupture force, the stamp separates from the substrate and a sample related IR-signal is sent from the spinning rotor. For each test specimen breaking force is calculated and displayed in real-time. The innovative measurement principle meets the requirements of DIN EN 15870 and ISO 4624. T2 - EURADH 2018 CY - Lisbon, Portugal DA - 05.07.2018 KW - Adhesive strength determination KW - CAT-technology KW - Centrifugal adhesion testing KW - Metal coatings KW - Decorative coatings on polymer substrates PY - 2018 AN - OPUS4-46001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Choi, Youungeun A1 - Kotthoff, Lisa A1 - Olejko, L. A1 - Resch-Genger, Ute A1 - Bald, Ilko T1 - DNA origami-based Förster resonance energy-transfer nanoarrays and their application as ratiometric sensors N2 - DNA origami nanostructures provide a platform where dye molecules can be arranged with nanoscale accuracy allowing to assemble multiple fluorophores without dye–dye aggregation. Aiming to develop a bright and sensitive ratiometric sensor system, we systematically studied the optical properties of nanoarrays of dyes built on DNA origami platforms using a DNA template that provides a high versatility of label choice at minimum cost. The dyes are arranged at distances, at which they efficiently interact by Förster resonance energy transfer (FRET). To optimize array brightness, the FRET efficiencies between the donor fluorescein (FAM) and the acceptor cyanine 3 were determined for different sizes of the array and for different arrangements of the dye molecules within the array. By utilizing nanoarrays providing optimum FRET efficiency and brightness, we subsequently designed a ratiometric pH nanosensor using coumarin 343 as a pH-inert FRET donor and FAM as a pH-responsive acceptor. Our results indicate that the sensitivity of a ratiometric sensor can be improved simply by arranging the dyes into a well-defined array. The dyes used here can be easily replaced by other analyte-responsive dyes, demonstrating the huge potential of DNA nanotechnology for light harvesting, signal enhancement, and sensing schemes in life sciences. KW - DNA origami KW - FRET KW - Sensing KW - Ratiometric sensing KW - Fluorescence PY - 2018 DO - https://doi.org/10.1021/acsami.8b03585 SN - 1944-8244 SN - 1944-8252 VL - 10 IS - 27 SP - 23295 EP - 23302 PB - ACS AN - OPUS4-46002 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Weiterentwicklung der VSSA-Screening-Methode zur Identifizierung von NanoPulvern N2 - Der Vortrag zeigt zwei Möglichkeiten zur Verbesserung der VSSA-Screening-Methode zur Identifizierung von Nanopulvern auf. Bisher ist das Verfahren nur für monodisperse Partikel mit idealer Kugelform valide. Die Verteilungsbreite der Partikelgröße soll durch die Nutzung des Modells einer logarithmischen Normalverteilung implementiert werden. Die Abweichung der gemessenen Partikel von einer idealen Kugel in Sphärizität, Rundheit und Rauigkeit sind über einen Morphologiefaktor MF zu berücksichtigen. An einem konkreten Beispiel werden Auswirkungen der Implementierungen rechnerisch dargestellt und mit dem bisherigen Verfahren verglichen. T2 - NanoDefine Follow-up Meeting CY - Frankfurt/ Main, Germany DA - 25.09.2018 KW - VSSA KW - Nano particle KW - Particle size KW - Nano screening PY - 2018 AN - OPUS4-46070 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cohen, Zina T1 - X-Ray Fluorescence Analysis of black Medieval Inks: Characterization and Interpretation. Case Study of an 11th century Egyptian Corpus N2 - This study focuses on the analysis of a corpus of manuscripts found in Fustat (medieval Cairo, Egypt) in the biggest medieval “archive” found until now: the Cairo Geniza. The giant collection of mostly Jewish documents has been attracting scholars’ attention a lot but so far, the material aspects of these documents seem to have been mainly neglected. Application of scientific methods of analysis, especially X-Ray fluorescence characterization, contributes to our understanding of the materials used for production of manuscripts during the Middle ages. Our corpus of the 11th century manuscripts comprises manuscripts written by scribes belonging to three Jewish communities that co-existed in Cairo during this period: the Karaites, the so-called Jerusalemites (or Palestinian) and the so-called Babylonians (or Iraqi), three different communities with different traditions and different leaders. The differences manifest themselves also in the paleographical properties of the manuscripts produced within each community. Can we extend the differences detected by the paleographical analysis to differences in composition of the writing materials and especially the composition of the inks? Or can we relate the differences in the composition to the manuscript type (legal, private...), or to another criterion. In this presentation, we offer answers to some of the questions using statistical analysis of the measurements results. T2 - Konferenz Natural Sciences and Technology in Manuscript Analysis CY - Hamburg, Germany DA - 13.06.2018 KW - Ink KW - Manuscript KW - XRF analysis PY - 2018 AN - OPUS4-46044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cohen, Zina T1 - Approche archéométrique de fragments de la Génizah du Caire conservés à la Bibliothèque Universitaire de Cambridge N2 - Quelles informations sur les matériaux d'écriture peut on obtenir grâce à des analyses archéométriques ? T2 - Konferenz Journée FSP-PATRIMA / EPHE CY - Paris, France DA - 24.01.2017 KW - Ink KW - Manuscript KW - XRF analysis PY - 2017 AN - OPUS4-46048 LA - fra AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Plasma Activation and Plasma-assisted ALD Surface Modification of Polymers for Improved Bonding and Adhesive Strength N2 - Bonding strength is crucial on polymers of low surface energy, for clean surfaces limited to 0.5, 1, and 2 MPa for PTFE, PP, and PE. Plasma treatment may improve bonding strength by a factor of 2 (PTFE) or 5 (PP and PE). The efficiency of treatment is usually 10% as both low pressure and atmospheric pressure processes show low topographic conformity. Besides, lifetime of activation/modification is rather short. Hence, bonding has to be carried out immediately after plasma treatment. The concept of plasma-assisted ALD (atomic layer deposition) interlayers was introduced in the project HARFE of SENTECH (modification/deposition/in-situ monitoring) and BAM (bonding, characterization, testing). ALD deposition has a high surface conformity and for dielectric films of Al2O3 also a good long-term stability given that the films are dense enough. Based on TMA and O2/O3 precursors, ALD layer stacks from 60 to 375 monolayers were prepared under different conditions. For a transfer time of 24 hours from deposition to measurement, bonding strength could be increased up to 5 MPa (PTFE) respectively 10 MPa (PP, PE). The huge potential of ALD layers as adhesive interlayers was demonstrated for Al2O3 on stainless steel with bonding strength beyond 15 MPa, i.e. interface strength within the ALD stack is also in this range. This is a prerequisite for subsequent PVD/CVD-deposition in hybrid systems. By means of the SI ALD LL system of SENTECH thermal and plasma-supported ALD processes can be alternatively realized. Ellipsometric in-situ monitoring provides monolayer sensitivity and reveals that the efficient bonding of the lower ALD layers on the polymer has to be further improved. Testing of bonding strength was realized by CAT (centrifugal adhesion testing) technology. It was shown that ALD modification correlates with the increase of surface energy and bonding strength. T2 - PSE 2018 - 16th Conference on Plasma Surface Engineering CY - Garmisch-Partenkirchen, Germany DA - 17.09.2018 KW - Plasma activation KW - Plasma-assisted ALD modification KW - Adhesive ALD interlayer KW - Bonding strength KW - Adhesive strength PY - 2018 AN - OPUS4-46015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Engell, S. T1 - PAT‐basierte iterative Optimierung der Fahrweise eines kontinuierlichen organischen Syntheseprozesses N2 - Generell ist es Ziel der Prozessführung, Reaktions- und Trennprozesse wirtschaftlich optimal zu betreiben. Hierzu werden in großen Anlagen modellbasiere Echtzeitoptimierungsverfahren (Real-time Optimization, RTO) eingesetzt. Die Qualität der Ergebnisse der Optimierung hängt dabei entscheidend von der Güte des verwendeten Modells ab. Die Entwicklung hochgenauer Modelle ist allerdings aufwändig, was für kleine Produktionsvolumina ein wesentliches Hindernis zur Nutzung solcher Methoden darstellt. Mit Hilfe der sogenannten Modifier-Adaptation ist eine iterative Betriebspunktoptimierung auch mit ungenauen Modellen möglich, wenn Messungen der für die Bewertung relevanten Größen (beispielsweise Produktkonzentrationen im Ausgangsstrom) verfügbar sein. Für eine Lithiierungsreaktion in einem bei INVITE kontinuierlich betriebenen Reaktor wurde im Rahmen des EU-Projekts CONSENS eine solche iterative Optimierung auf der Grundlage einer Messung der Zusammensetzung des Ausgangsstroms des Reaktors mit einem Online-NMR-Spektrometer realisiert. Das Spektrometer wurde an den Betrieb in einer explosionsgefährdeten Umgebung angepasst. Es konnte gezeigt werden, dass die Messdaten genau genug sind, um darauf eine Optimierung der Produktausbeute aufzubauen. Die iterative Optimierung führt den Prozess ausgehend vom mit dem Modell berechneten Betriebspunkt schrittweise zum wirtschaftlichen Optimum für die reale Anlage. Dabei reagiert die Optimierung auch auf unbekannte Abweichungen im Prozess (wie die Zusammensetzung des Feeds) und fährt iterativ den jeweils optimalen Betriebspunkt an. Die Arbeiten wurden im Rahmen des EU-SPIRE-Projekts CONSENS, Förderkennzeichen 636942, durchgeführt. T2 - ProcessNet-Jahrestagung und 33. DECHEMA-Jahrestagung der Biotechnologen CY - Aachen, Germany DA - 10.09.2018 KW - Prozessindustrie KW - Prozessanalytik KW - Betriebspunktoptimierung KW - Quadratic approximation (MAWQA) KW - Modellbasierte Optimierung KW - CONSENS PY - 2018 AN - OPUS4-46020 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - Certified reference materials for breath alcohol control – the ALCOREF project N2 - ALCOREF is a project within the European Metrology Programme for Innovation and Research (EMPIR. It is part of the 2016 EMPIR Research Potential Call dedicated to build up metrological and research capacity in less developed National Metrology Institutes (NMIs). The project will develop long term expertise for the production and certification of ethanol/water reference materials in the participating NMIs. Materials to be developed will be suitable for the calibration and approval of evidential breath alcohol analysers as defined by recommendation R 126 of the International Organization of Legal Metrology (OIML). Certification includes the characterisation of the materials, assessment of homogeneity, stability and uncertainty. Target certified values and volumes will address end-users’ needs regarding regional legal limits for alcohol in traffic and the instrumentation for breath analyser calibration available in different countries. Thus, the project supports the law enforcement of national drink-driving legislation. The consortium comprises of 11 institutions from 10 European countries. Project participants will establish reliable analytical methods for the purity assessment of ethanol, such as Karl-Fischer titration, to achieve traceability of their certified values. Chromatographic or density methods for the quantification of ethanol in water will also be established, validated and applied for homogeneity and stability assessment. An interlaboratory comparison will be conducted within the European Association of National Metrology Institutes’ (EURAMET) Technical Committee Metrology in Chemistry to test the equivalence of the new certified reference materials and the analytical methods implemented. The poster will present the outline and first results of the ALCOREF project. T2 - BERM-15 International Symposium on Biological and Environmental Reference Materials CY - Berlin, Germany DA - 24.09.2018 KW - Certified Reference Material KW - Breath alcohol control KW - ALCOREF PY - 2018 AN - OPUS4-46061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas T1 - GPR Testing of concrete structures N2 - The basics of ground penetrating radar and its NDT application in civil engineering were shown. T2 - NDT&E Advanced Training Workshop CY - Berlin, Germany DA - 27.06.2018 KW - GPR KW - Concret KW - NDT PY - 2018 AN - OPUS4-46297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Investigation of core-shell nanoparticles using a combination of scanning Auger microscopy (SAM) and scanning electron microscopy (SEM) N2 - Products containing engineered nanoparticles already encounter us in most areas of our daily life including cosmetics, clothing, detergents, paints, batteries and displays. In most cases the particles exhibit a core-shell morphology either voluntarily or involuntarily. The properties of the nanoparticle shell determine the interaction with their environment and, thus, reliable control over these properties means reliable control over the particles performance and their toxicity. Therefore, sophisticated techniques to measure thickness and elemental composition of the nanoparticle shell are urgently required. Scanning Auger microscopy (SAM) is a powerful technique with a lateral resolution below 10 nm and a chemical contrast based on the characteristic kinetic energy of Auger electrons related to specific atomic levels and, thus, to a specific element. This work explores the potential of SAM for characterizing the core-shell structure of nanoparticles. A sample system of upconversion NaYF4:Yb,Er cores coated with SiO2 is investigated. Auger spectra, line scans and elemental maps of single nanoparticles will be presented. Challenges encountered will be highlighted, such as damage to the sample by electron beam irradiation. Scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) are performed on the same samples, in order to verify the SAM results. T2 - BAM PhD Retreat CY - Warnemünde, Germany DA - 28.09.2018 KW - Core-shell nanoparticles KW - SAM KW - SEM KW - Surface analysis PY - 2018 AN - OPUS4-46270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vlajića, M. A1 - Unger, Wolfgang A1 - Bruns, J. A1 - Rueck-Braun, K. T1 - Photoswitching of fulgimides in different environments on silicon surfaces N2 - Reversible light-modulation of fulgimide based monolayers on Si(1 1 1) and Si(1 0 0) was investigated using ATR-FTIR spectroscopy. Fulgimide monolayers were prepared from neat COOH-terminated SAMs on Si(1 1 1) obtained from methyl undec-10-enoate, (1:1)-diluted COOH-terminated monolayers on Si(1 1 1), and GPTMS monolayers on Si(1 0 0). The epoxy-terminated monolayer on oxidized Si(1 0 0) was characterized with ellipsometry, XPS, as well as contact angle measurements, and ATR-FTIR spectroscopy revealed a strong influence of toluene water content on reproducible high-quality monolayer formation. The results of this study show that environmental polarity has a strong influence on fulgimide imide IR band locations and read-out options for the two photostationary states PSS(365 nm), containing E/Z- and C-isomers, and PSS(545 nm), with solely the E/Zisomers. Neat COOH-terminated monolayers on flat Si(1 1 1) have the Advantage of high functional Group concentration, orientation and stability, and an upright arrangement of fulgimide head groups. KW - Surface functionalization KW - Photoswitchable monolayers KW - ATR-FTIR spectroscopy KW - XPS PY - 2019 DO - https://doi.org/10.1016/j.apsusc.2018.09.159 SN - 0169-4332 SN - 1873-5584 VL - 465 SP - 686 EP - 692 PB - Elsevier B.V. AN - OPUS4-46276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Benefits & peculiarities of using highpower lasers for lock-in thermography N2 - Optical lock-in thermography is a completely contactless and very sensitive NDE technique. As an optical source of energy, incandescent (i.e. halogen) lamps are most commonly used because they are relatively inexpensive, do not need any work safety measures and offer high irradiances at the test site. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration. Altogether using lasers considerably increases the application range of lock-in thermography, since especially for metals with a high reflectance and high thermal diffusivity a high irradiance is vitally important to allow for lock-in testing [1, 2]. We report on the mentioned benefits of using such high-power lasers and analyze the range of materials to be tested using lock-in thermography in dependence on the laser irradiance, the modulation frequency, the infrared camera as well as the optical and thermal material parameters. In this context, we also address a number of systematic errors caused by the use of ideal and non-ideal heat sources. For example, the measured phase angle in lock-in thermography depends on the irradiance and the modulation bandwidth of the source. This in turn has a decisive influence on the uncertainty in the quantification of, e.g. layer thicknesses. T2 - INTERNATIONAL SCHOOL OF QUANTUM ELECTRONICS, 62nd Course, Progress in Photoacoustic & Photothermal Phenomena CY - Erice, Italy DA - 06.09.2018 KW - Thermography KW - Laser thermography KW - Lock-in thermography KW - NDT PY - 2018 AN - OPUS4-46282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Detjens, Marc A1 - Fechner, A. A1 - Sielemann, S. A1 - Lorek, A. A1 - Wernecke, R. A1 - Stoltenberg, H. T1 - Development of a device for staged determination of water activity and moisture content N2 - Moisture content and water activity are important parameters for quality characterization of products like bulk materials, powders, granules. Thus, an exact determination is necessarily required in a wide range of industrial applications. Moisture of materials is the content of non-chemically bound water in a solid or liquid. Water activity (aW) is a characteristic/parameter of the non-chemically bound ("free") water in materials and is measured as humidity over a solid/liquid surface at constant temperature (equilibrium moisture content). It is an important parameter to characterize the quality of e. g. pharmaceutical and food products. In our contribution, we present the developed MOISHUM device for staged determination of water activity and moisture content of liquid and solid materials. T2 - Eurosensors 2018 CY - Graz, Austria DA - 09.09.2018 KW - Water activity KW - Moisture KW - Coulometric humidity sensor KW - MOISHUM PY - 2018 SN - 2504-3900 SP - 7253, 1 EP - 4 PB - MDPI AN - OPUS4-46210 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang A1 - Kjaervik, Marit T1 - New work item proposal for a technical report for ISO/TC 201 WG 4 “Surface characterization of biomaterials”: Surface chemical analysis – Surface chemical analysis of cells and biofilms N2 - The proposed ISO Technical Report provides a description of a variety of physical methods of analytical chemistry by which bacteria and biofilms can be analysed. The state of the art, sample requirements and strengths associated with each method are identified. T2 - 27th Plenary Meeting of ISO/TC 201 CY - Cancun, Mexico DA - 2018-09-20 KW - Surface chemical analysis of biofilms KW - XPS KW - Fourier-Transform Infrared Spectroscopy KW - 3D nano SIMS KW - Raman-spectroscopy PY - 2018 AN - OPUS4-46214 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cant, D. T1 - Surface chemical analysis – Electron spectroscopies – Measurement of the thickness and nature of nanoparticle coatings N2 - Recent years have seen increasing development of nanoparticles for applications in a wide range of fields, including but not limited to areas of great impact such as catalysis, medicine, energy, optoelectronics, cosmetics, and many others. In particular, nanoparticles bearing some form of coating layer, whether by design or due to incidental processes such as contamination or oxidation, are among the most commonly studied and utilised. In the characterisation of nanoparticles, the surface properties are of great importance, because a large proportion of the particle forms a part of the surface or interface. In the case of coated nanoparticles, the thickness of the coating is significant in determining the properties of the nanoparticle, and defines its interactions with its environment. Measurement of surface chemistry and coating thickness of nanoparticles is a challenge to which electron spectroscopies are well suited, due to high surface sensitivity, well-understood physical principles and accessibility. T2 - Annual Meeting of ISO/TC 201/SC7 CY - Cancun, Mexico DA - 21.09.2018 KW - Nanoparticle characterization KW - X-ray Photoelectron Spectroscopy (XPS) KW - Auger Electron Spectroscopy (AES) KW - Core-shell nanoparticles PY - 2018 AN - OPUS4-46259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Vortragsreihe des Kompetenzzentrums Datenanalyse Datenfusion –Informationsgewinn aus Multisensordaten N2 - Angetrieben durch Digitalisierung und die sogenannte Industrie 4.0 steigt die Erwartungshaltung gegenüber der Nutzung von Sensorik. Die Unsicherheit, Widersprüchlichkeit und Redundanz separat verarbeiteter einzelner Quellen soll durch die synergetische Zusammenführung heterogener Datensätze überwunden werden. Dabei steht der zunehmenden Aufgabenkomplexität eine ebenso zunehmende Verfügbarkeit an Sensoren, Daten und Rechenleistung gegenüber. Der Begriff Datenfusion fasst Ansätze zusammen, die Daten zu abstrakteren, aber besser verständlichen Informationen verarbeiten. Die Fusion ist Kernbestandteil effektiver Assistenzsysteme und beweist in vielzähligen Aufgaben - von militärischen Anwendungen über Flug- und Fahrassistenzsysteme, bis in den Heimbereich – ihr großes Potenzial. Durch die wachsende Automatisierung bei der Messdatenerfassung wird Datenfusion auch in der industriellen Qualitätsprüfung und –sicherung zunehmend attraktiver. Der Vortrag gibt einen Überblick über den breiten Themenkomplex und widmet sich dabei speziell der Fragen, welche Informationen in multivariaten Datensätzen stecken und wie sie extrahiert werden können. Abschließend wird ein Beispiel für die erfolgreiche Anwendung zur zerstörungsfreien Prüfung von Betonbauteilen vorgestellt. Der systematische Vergleich von Algorithmen, die Charakteristika des Labordatensatzes in unterschiedlicher Weise adressieren erlaubt überraschende Schlussfolgerungen. T2 - Vortrag CY - BAM Berlin, Germany DA - 25.07.2018 KW - Datenanalyse PY - 2018 AN - OPUS4-46260 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breßler, Ingo T1 - SASfit, McSAS and beyond: Prospect of complementary tools for SAS data analysis N2 - Data analysis of SAS measurements has been dominated by the classical curve fitting approach. This method finds optimal parameters of a scattering model composed of analytical expressions. SASfit represents such a classical curve fitting toolbox: it is one of the mature programs for small-angle scattering data analysis and has been available and used for many years. The latest developments [1] will be extended by improving the interoperability of the extensive data base of models with third-party analysis software. An updated format of model definitions is also presented, which allows model function plug-ins to be used with the Python language. To complement the classical curve fitting method, the user-friendly opensource Monte Carlo regression package McSAS was developed. Most importantly, the form-free Monte Carlo approach of McSAS means that it is not necessary to provide any further mathematical restrictions to the Parameter distribution. Future developments include separating the core optimization from the GUI (allowing 'headless' integration), as well as parallel computing which reduces the computing time proportional to the number of available computing cores. The headless mode is presented by an example of Operation within interactive programming environments such as a Jupyter notebook. The promising results of Monte Carlo based data analysis for determining form-free Parameter distributions motivated the evaluation of the method with dynamic light scattering (DLS) data. For this purpose, the method was adapted for analyzing correlation curves such as those from multi-angle dynamic light scattering (DLS) data. The development of McDLS intends to overcome limitations of existing methods at reliably determining the modality of size distributions. An example of Monte Carlo based data analysis of multimodal DLS measurements will be presented. T2 - XVII International Small Angle Scattering Conference - SAS2018 CY - Traverse City, MI, USA DA - 07.10.2018 KW - Data analysis KW - Small angle scattering KW - Dynamic light scattering PY - 2018 AN - OPUS4-46308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - Mechanochemie N2 - In 3 Minuten sollte das Thema der Dissertation ohne zusätzliche Materialien vorgestellt werden. T2 - FameLab Germany 2018 CY - Potsdam, Germany DA - 15.03.2018 KW - Mechanochemie PY - 2018 AN - OPUS4-46319 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - Mechanochemical Knoevenagel condensations of benzaldehyde derivates investigated in situ N2 - Mechanochemistry is widely applicable for the synthesis of inorganic, metal-organic, and organic compounds. It is known for short reaction times, nearly quantitative conversions, and decreasing amount of solvents, which opens the field to more environmentally friendly syntheses routes. Among organic syntheses, the Knoevenagel condensation is an important C-C bond forming reaction leading to α,β-unsaturated compounds. To gain more information on the underlying processes, we investigated the syntheses by a combination of different in situ investigation techniques, including synchrotron X-ray diffraction, Raman spectroscopy and thermography. This combination provides information on the structural changes and temperature influences during milling. Benzaldehyde derivates (nitro- and fluoro-derivates) reacted with malononitrile to the respective benzylidenemalononitriles. The in situ investigations show direct and quantitative conversions. In the case of the fluorinated benzaldehyde derivates we showed the possibility of using liquid substrates in mechanochemical organic synthesis. Surprisingly, after crystallization from a viscous state, the material was suitable for single-crystal X-ray analysis. T2 - Powder Diffraction School 2018 CY - Villigen, Switzerland DA - 24.09.2018 KW - C-C coupling KW - Mechanochemistry KW - In situ KW - Knoevenagel PY - 2018 AN - OPUS4-46320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias A1 - Maierhofer, Christiane A1 - Krankenhagen, Rainer A1 - Röllig, Mathias T1 - Characterization of defects in fibre reinforced composites (FRC) using passive and active thermography N2 - Impact damages and delaminations in fibre-reinforced composites (FRC) might not be visible at the surface, but could have an influence on the resistance and on the long-term behaviour of the component. Therefore, and especially for safety relevant structures, non-destructive methods are required for the assessment of such damages. Active thermography methods are suitable to characterize damages after loading using different kind of excitation techniques and various configurations of infrared (IR) camera and heating sources. Here, flash lamps, impulse excitation with infrared radiator and lock-in technique with halogen lamps or widened laser beams are suited. In addition, non-optical sources like sonotrodes (requiring direct contact to the structure) or induction generators (only suited for carbon fibre reinforced polymer (CFRP) structures) could be applied as well. For the investigation of the evolution of the damage during the impact, passive thermography can be applied in-situ. Elastic and plastic deformations alter the temperature of the structure and thus the temperature on the surface. In this contribution, at first the general principles of quantitative defect characterisation in FRC using active thermography with flash, impulse and lock-in excitation are described. Optical and thermal properties of the FRC material and its anisotropy are considered. Results of phase differences obtained at flat bottom holes with flash and lock-in thermography are compared for qualifying both methods for quantitative defect characterization. Secondly, the damage evolution of CFRP and GFRP structures under impact load and static tensile loading is described. The spatial and temporal evolution of the surface temperature enables us to distinguish matrix cracks or fibre-matrix separation from delaminations between the layers. Afterwards, all results for loading defects, obtained by passive and active thermography, are compared with each other. Fig. 1 and 2 show the difference of passive and flash thermography obtained at impact and tensile loaded CFRP plates, respectively. As one purpose of these investigations is the development of standards within national (DIN) and European (CEN) standardisation bodies, new draft and final standards are presented and further needs are discussed at the end of the presentation. T2 - INTERNATIONAL SCHOOL OF QUANTUM ELECTRONICS, 62nd Course, Progress in Photoacoustic & Photothermal Phenomena CY - Erice, Italy DA - 06.09.2018 KW - Thermography KW - Flash thermography KW - Lock-in thermography KW - CFRP KW - GFRP PY - 2018 AN - OPUS4-46283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sharma, Govind T1 - Distinction of tendon ducts and rebars by GPR reflection signal patterns N2 - We investigated the possibility of surrounding waves along with perimeter of large diameter tendon ducts during ground penetrating radar (GPR) testing of concrete structures. The surrounding waves influence the primary reflection from tendon duct and alter the phase as well as amplitude of signal depending on the diameter of the tendon duct. This phenomenon was studied in detail by conducting several simulations using a commercial software Reflexw®. Finite Difference Time Domain method was adopted to analyze reflection patterns from objects of various diameters located at different depths in concrete media. The proposed methodology will be useful in qualitative assessment of size of metallic objects greater than a diameter of 6 cm. In general, the identification of large diameter tendon ducts in a civil structure is carried out by prior knowledge of the civil plan and its diagonal appearance to smaller diameter object mesh. The proposed methodology will enhance the confidence in identification of the larger diameter tendon ducts even if the civil plan is not known accurately. T2 - 17th International Conference on Ground Penetrating Radar CY - Rapperswil, Switzerland DA - 18.06.2018 KW - Ground penetrating radar KW - Rebar KW - Concrete PY - 2018 AN - OPUS4-46246 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sharma, Govind A1 - Kind, Thomas T1 - Distinction of tendon ducts and rebars by GPR reflection signal patterns N2 - We investigated the possibility of surrounding waves along with perimeter of large diameter tendon ducts during ground penetrating radar (GPR) testing of concrete structures. The surrounding waves influence the primary reflection from tendon duct and alter the phase as well as amplitude of signal depending on the diameter of the tendon duct. This phenomenon was studied in detail by conducting several simulations using a commercial software Reflexw®. Finite Difference Time Domain method was adopted to analyze reflection patterns from objects of various diameters located at different depths in concrete media. The proposed methodology will be useful in qualitative assessment of size of metallic objects greater than a diameter of 6 cm. In general, the identification of large diameter tendon ducts in a civil structure is carried out by prior knowledge of the civil plan and its diagonal appearance to smaller diameter object mesh. The proposed methodology will enhance the confidence in identification of the larger diameter tendon ducts even if the civil plan is not known accurately. T2 - 17th International Conference on Ground Penetrating Radar CY - Rapperswil, Switzerland DA - 18.06.2018 KW - Ground penetrating radar KW - Rebar KW - Concrete PY - 2018 SN - 978-1-5386-5776-8 SP - 232 EP - 235 AN - OPUS4-46247 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - Chemical characterisation of (core-shell) nanoparticles using PCA assisted ToF-SIMS and XPS N2 - The analysis of nanomaterials is currently an important task - especially in case of risk assessment – as the properties of these material class are not well understood. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surface’s chemical composition must be investigated to get a better understanding and prediction of the nanomaterials’ behavior. ToF-SIMS and XPS have proven to be powerful tools to determine the general chemical composition. The superior surface sensitivity of ToF-SIMS furthermore allows us to study mainly the utmost atomic layers and thus gives us an idea of the interactions involved. Here, we present initial data on the analysis of Hyflon®-polystyrene core-shell nanoparticles which can be used as a model system due to the known preparation and a rather good chemical as well as physical separation of core and shell. Furthermore, results on Au nanoparticles with and without an antibody shell are presented. Principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - 3rd NanoSafety Forum for Young Scientists CY - Valetta, Malta DA - 08.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS PY - 2018 AN - OPUS4-46248 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - Chemical characterisation and classification of (Core-Shell) nanoparticles using PCA assisted ToF-SIMS N2 - The analysis of nanomaterials is currently an important task - especially in case of risk assessment – as the properties of these material class are not well understood and their growing use in everyday life. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surface’s chemical composition must be investigated to get a better understanding and prediction of the nanomaterials’ behaviour. ToF-SIMS and XPS have proven to be powerful tools to determine the general chemical composition. The superior surface sensitivity of ToF-SIMS furthermore allows us to study mainly the utmost atomic layers and thus gives us an idea of possible interactions involved. Supported by multivariate data analysis such as principal component analysis (PCA), the method can also be used for sub-classification of different materials using slight differences in surface chemistry. Here, we present data of the analysis of Hyflon®-polystyrene core-shell nanoparticles which can be used as a model system due to the known preparation and a rather good chemical as well as physical separation of core and shell. Principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. This is achieved by measurement of a statistically relevant set of samples for every particle sample. We acquired surface spectra under static SIMS conditions with Bi32+ and analysed the resulting spectra by PCA. The carefully selected and refined peaks allow a reasonable categorization and further a reliable allocation of blank feeds. In detail, the fluorine containing, organic fragments are an indication for a heterogeneous shell that has errors. Furthermore, results on Au nanoparticles with and without an antibody shell are presented. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - SIMS-Europe CY - Münster, Germany DA - 16.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS KW - PCA KW - Titania KW - Core-Shell PY - 2018 AN - OPUS4-46249 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas A1 - Schneider, Markus A1 - Schäpe, Kaija T1 - Classification of engineered Titania nanomaterials via surface analysis using principal component analysis (PCA) assisted Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) N2 - Due to the growing number of engineered nanomaterials (NM) the need for a reliable risk assessment for these materials is today bigger than ever before. Especially the nanomaterial’s surface or shell directly interacts with its environment and therefore is a crucial factor for NM’ toxicity or functionality. Especially, titania is one of the NM with the greatest technological importance. It is used for a large number of applications and can be found in food, cosmetics, glasses, mirrors, paints to mention only a few. In 2012, experts estimate[d] the annual European nano-titania production or utilization at an amount of more than 10,000 t. Great progress has been achieved in the area of NM investigation and characterization during the past decade. A variety of publications provide information about technological innovation as well as hazard potential, which means the potential risk on human health and ecosystems. However, enhanced data harmonization and well-defined standards for nanomaterial analysis, could significantly improve the reliability of such studies which often suffers from varying methods, parameters and sample preparations. To develop a suitable approach for the NM’s risk assessment, the ACEnano project aims at establishing a toolbox of verified methods. The size of this well-structured European project allows to handle even those big challenges like data harmonization and standardization. Due to its powerful combination of superior surface sensitivity and lateral resolution down to the Nano regime, ToF-SIMS could become one of these toolbox methods. Supported by multivariate data analysis such as principal component analysis (PCA), the method can be used for sub-classification of nanomaterial families using slight differences in surface chemistry. Here, we show a PCA supported classification of titania nanoparticles from various sources (NIST, JRC, BAM) with ToF-SIMS. Parameters like size, shell, pre-preparation and crystal system cause variance in the data and allow us to distinguish the species from each other. Moreover, this variance in the data also occurs and can be used for investigation when we compare our measurements of particle ensembles with those of grown titania films. The carefully selected and refined peaks allow a reasonable particle categorization and further a reliable allocation of blank feeds, which introduces a promising approach for NM characterization in the context of NM risk assessment. T2 - SIMS-Europe CY - Münster, Germany DA - 16.09.2018 KW - Nanoparticles KW - ToF-SIMS KW - XPS KW - PCA KW - Titania PY - 2018 AN - OPUS4-46250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Overview on the most advanced and suitable NanoDefine measurement methods N2 - The EC Recommendation on the definition of nanomaterial, based solely on size of the constituent particles, foresees development of harmonised measurement methods ensuring ‘consistent results across materials and over time’. The EU/FP7 research project NanoDefine has been exclusively dedicated to support the implementation of this EC Recommendation for the European Union’s legislation. For the first time, measurement techniques able to determine the size of nanoparticles have been evaluated systematically on a well-defined set of quality control materials (spherical, monodisperse) as well as industrial materials of complex shapes and considerable polydispersity. Particularly based on the analytical performance of the measurement techniques as tested on the challenging real-world particulate materials, it was possible to formulate recommendations for use of a new tiered approach consisting of screening and confirmatory techniques. Thus, a consistent framework of guidance for nanomaterial identification according to the EC Definition has been issued in form of the NanoDefiner e-tool, with a transparent decision flow scheme and an extensive user manual. Selected examples of analysis and classification as nano-/non-nanomaterials will be given, highlighting the limits of applicability of the available measurement techniques in dependence on sample properties. On some recent relevant developments in sample preparation – as a crucial part for an accurate analysis - will be also reported. T2 - VCI-NanoDefine Follow-up Meeting CY - VCI, Frankfurt am Main, Germany DA - 25.09.2018 KW - Nanoparticles KW - Nanomaterial KW - EC definition of nanomaterial KW - Nanoparticle size distribution PY - 2018 AN - OPUS4-46251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - improved traceability chain of nanoparticle size measurements - Is a liaison to CEN/TC 352 nanotechnologies useful? N2 - The main objectives of the new EMPIR project nPSize are to establish EU capability of traceable measurement of NP size and shape, lower uncertainties of NP size measurement by developement of new nano-CRMs, new models (physical and machine learning), 3D method combination, and also by new ISO and CEN standards on accurate NP size measurement and guidance and knowledge transfer. The envisaged outcomes of the project will be presented and their suitability will be discussed to be taken over as pertinent contributions to normative projects within CEN/TC 352 Nanotechnologies. T2 - Joint Working Groups and 24th CEN/TC 352 Nanotechnologies Meetings CY - DIN, Berlin, Germany DA - 09.10.2018 KW - Nanoparticles KW - Size KW - Particle size distribution KW - Particle shape KW - Traceability KW - Standardisation KW - CEN/TC 352 Nanotechnologies PY - 2018 AN - OPUS4-46252 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Check of the energy-dispersive X-ray spectrometers (EDS) performance with the BAM test material EDS-TM001/2 and BAM software EDS spectrometer test N2 - The test material EDS-TM001 together with an accompanying software package, “EDX spectrometer check”, have been made available in 2009 by BAM to be employed by EDS (energy dispersive spectrometer) users to check the performance of an EDS attached to the SEM. Particularly for test laboratories operating under accreditation schemes like ISO/IEC 17025, a periodical control of the critical instrumental parameters in end-user laboratories is required. With EDS-TM001 or EDS-TM002 (second generation) test material, this periodical check is reduced to the acquisition of only one 10 kV spectrum. The software “EDX spectrometer check” is destined to evaluate automatically this spectrum and determine the performance of the EDS in terms of energy resolution and calibration as well as possible alteration of low-energy efficiency due to detector contamination. Energy resolution can be compared with the specified values according to the international ISO standard ISO 15632:2012. EDS-TM is a synthetic material consisting of a thick layer of C, Al, Mn, Cu and Zr in a well-defined composition, deposited on a steel (in case of EDS-TM001) or silicon (in case of EDS-TM002) substrate. Meanwhile, more than one hundred laboratories (most of them located in Germany) use the EDS-TM001 or EDS-TM002 test material for the periodical check of their EDS. A detailed description of the test material and software together with examples of application was published recently. New results and gained experiences will be presented as well. T2 - BERM-15: International Symposium on Biological and Environmental Reference Materials CY - Berlin, Germany DA - 24.09.2018 KW - EDS KW - SEM/EDX KW - Test material KW - EDS-TM001 KW - EDS-TM002 KW - EDS Spectrometer Test KW - X-rays PY - 2018 AN - OPUS4-46253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram T1 - The new ISO Guide 35:2017: New airflow, new approaches, and more freedom for RMP N2 - An overlook over the new ISO Guide 35:2017 is given, with focus on the new, sometimes challenging opprotunities and approaches of this Guide. T2 - DAkkS Informationsveranstaltung zur Akkreditierung von RMP CY - Berlin, Germany DA - 15.02.2018 KW - reference materials, requirements, guidance PY - 2018 AN - OPUS4-46772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Tobias T1 - Application of two calibration-free LIBS techniques for synthetic spectra of cement samples N2 - Two calibration-free LIBS techniques are used for the quantitative analysis of synthetic cement samples: the CF-LIBS based on the Boltzmann plot method and the Monte Carlo (MC) LIBS based on the iterative spectrum fitting. In CF-LIBS, the inverse problem is solved, i.e. the elemental concentrations are determined by the reconstruction of plasma parameters from spectra. The MC-LIBS technique solves the direct problem by finding the highest correlation between the model-generated and experimental spectrum. The accuracy of both calibration-free LIBS methods suffers from factors such as inaccurately determined instrumental function, the deviation of experimental plasma from the mathematical model used, not taking into account the collection geometry and from the uncertainty of spectroscopic data. Therefore, the both calibration-free LIBS approaches are applied to synthetic spectra which perfectly suit the mathematical model of the method. This test yields the accuracy of both the approaches for the ideal case. In addition, the accuracy of both methods is investigated for non-isothermal plasma, because real laser-induced plasma often has high gradients in temperature. Both methods assume an isothermal plasma. T2 - Xth international conference on Laser-Induced Breakdown Spectroscopy CY - Atlanta, GA, USA DA - 21.10.2018 KW - Cement KW - MC-LIBS KW - LIBS KW - CF-LIBS PY - 2018 AN - OPUS4-46774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, W T1 - Peculiarities of qualitative RM and accreditation of their producers N2 - Similarities and differences between accreditation strategies for producers of quantirative and qualitative reference materials are discussed, and possible approaches for the differeing parts in the process developed. T2 - DAkkS Informationsveranstaltung zur Akkreditierung von RMP CY - Berlin, Germany DA - 15.02.2018 KW - Qualitative analysis KW - Reference materials PY - 2018 AN - OPUS4-46777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Schnelle quantitative Untersuchung der Elementverteilungen im Beton mittels LIBS N2 - Die Laserinduzierte Plasmaspektroskopie (engl.: Laser-induced Breakdown Spectroscopy, kurz: LIBS) ist eine Kombination aus Laserablation mittels eines energiereichen Laser-Pulses, der Erzeugung eines Plasmas auf der zu untersuchenden Oberfläche und dem quantitativen Nachweis der Elementzusammensetzung durch spektroskopische Untersuchung der vom Plasma emittierten Strahlung. Ein LIBS-Gerät liefert dem sachkundigen Planer Daten für die Bewertung des Ist-Zustandes von Bauwerken unserer Infrastruktur durch die zweidimensionale Erfassung von Elementverteilungen. Typische Anwendungen sind die Erfassung von Chlor, Schwefel, Kohlenstoff, Natrium, Kalium und Lithium in Beton oder als – Qualitätssicherung – der Nachweis der mit einem Marker versehenen Tiefenhydrophobierung. In Zusammenarbeit zwischen Industriepartnern und der BAM wurden ein Labor und ein mobiles LIBS-System für die Vor-Ort-Messungen entwickelt. Die Analyse erfolgt vollautomatisch. Die Ortsauflösung beträgt bis zu 0,1 mm x 0,1 mm. Es können Messflächen von 140 mm x 170 mm gescannt werden. Die Erstellung von 2D-Elementverteilungen im Beispiel unten benötigt weniger als 10 Minuten. T2 - ibausil - 20. Internationale Baustofftagung CY - Weimar, Germany DA - 12.09.2018 KW - LIPS KW - Chlorid KW - LIBS KW - Beton PY - 2018 AN - OPUS4-46778 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heck, C. A1 - Michaeli, Y. A1 - Bald, Ilko A1 - Ebenstein, Y. T1 - Analytical epigenetics: single-molecule optical detection of DNA and histone modifications N2 - The field of epigenetics describes the relationship between genotype and phenotype, by regulating gene expression without changing the canonical base sequence of DNA. It deals with molecular genomic information that is encoded by a rich repertoire of chemical modifications and molecular interactions. This regulation involves DNA, RNA and proteins that are enzymatically tagged with small molecular groups that alter their physical and chemical properties. It is now clear that epigenetic alterations are involved in development and disease, and thus, are the focus of intensive research. The ability to record epigenetic changes and quantify them in rare medical samples is critical for next generation diagnostics. Optical detection offers the ultimate single-molecule sensitivity and the potential for spectral multiplexing. Here we review recent progress in ultrasensitive optical detection of DNA and histone modifications. KW - Epigenetics KW - Fluorescence KW - SERS PY - 2019 UR - https://www.sciencedirect.com/science/article/pii/S095816691830082X DO - https://doi.org/10.1016/j.copbio.2018.09.006 SN - 0958-1669 VL - 55 SP - 151 EP - 158 PB - Elsevier AN - OPUS4-46680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Thin polymer films as model systems for polymer nanocomposites N2 - Polymers at interfaces play a major role in a broad variety of applications ranging from engineering purposes (for instance polymer based nanocomposites) to high tech implications (for instance light emitting diodes). Here, thin films with thicknesses down to few nanometers are prepared on different substrates as model systems for polymer composites. The thin films are investigated by a combination of surface analytical and volume sensitive methods. As surface analytical methods atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and contact angle measurements (CAM) are employed. As volume sensitive broadband dielectric spectroscopy (BDS), specific heat spectroscopy (SHS), and ellipsometry are used. Especially attention is paid to understand the glass transition behavior of thin films because the glass transition is the key phenomenon determines the application of polymers also in thin films. To understand the glass transition behavior of thin films, which is controversially discussed in literature, a three layer model is discussed. Firstly, a mobile surface layer is assumed at polymer air interface of the film due to missing of segment/segment interactions. Secondly, in the middle of the film a bulk-like layer should be expected. Thirdly, for polymers having non-repulsive interactions with the substrate an irreversibly adsorbed layer is expected to be formed. Due the adsorption the molecular mobility of the segments in this layer is slowed down. What is measured for the glass transition of thin films is a complicated average of all of these effects. The different layers are hardly to address separately. Therefore, in the presentation especially model systems are selected and investigated to verify the layer model. T2 - Kolloquiumsvortrag and der Universität des Saarlandes CY - Saarbrücken, Gemany DA - 20.11.2018 KW - Thin polymer films PY - 2018 AN - OPUS4-46692 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schönhals, Andreas A1 - Zorn, R. T1 - Quasi-elastic scattering of high free volume polymers by neutron time-of-flight spectroscopy N2 - Experimental report to proposal 13562 Quasi-elastic scattering of the polymer with intrinsic microporoasity PIM-1 is measured by neutron time-of-flight spectroscopy and discussed. KW - Neutron scattering KW - PIM-1 PY - 2018 SP - 1 EP - 2 CY - Garching AN - OPUS4-46693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Airborne testing of molded polymer compounds N2 - Modern and energy-efficient materials are essential for innovative designs for aerospace and automotive industries. Current technologies for rapid manufacturing such as additive manufacturing and liquid composite moulding by polymer Extrusion allow innovative ways of creating robust and lightweight constructions. Commercially available printing devices often use polylactide (PLA) or acrylonitrile butadiene styrene (ABS) as raw material. Therefore, parameters like the infill ratio, influencing the ability to resist mechanical stress, may have a beneficial impact on the lifetime of components. These manufacturing technologies require a good knowledge about materials and even adapted non-destructive testing technologies and methods. Airborne ultrasonic testing has beneficial advantages for testing those lightweight constructions. It is a contact-free testing method, which does not require a liquid couplant. Therefore, it allows fast test cycles without any unwanted alternations of the material properties due to interactions with any coupling liquid. This contribution deals with the characterisation of printed specimens based on PLA by using airborne ultrasound and presents the current edge of non-destructive testing and evaluation using airborne ultrasonic transducers. The specimens, manufactured by polymer extrusion, are printed as thin plates. The infill ratio, as well as the material thickness, were varied to model density imperfections with different geometric shapes and properties. For better understanding of the limits of airborne ultrasonic testing in transmission, we compared own-developed transducers based on different physical principles: on ferroelectrets, on the thermoacoustic effect, as well as a new type of transducers based on gas discharges. T2 - 10th International Symposium on NDT in Aerospace CY - Dresden, Germany DA - 26.10.2018 KW - Airborne ultrasonic testing KW - Transducers KW - Ferroelectret KW - Thermoacoustic KW - Plasma KW - Polymer testing PY - 2018 AN - OPUS4-46655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Air-coupled ultrasonic ferroelectret transducers with additional bias voltage for testing of composite structures N2 - Common air-coupled transducers for non-destructive testing consist of a piezocomposite material and several matching layers. Better acoustical matching to air is achieved by transducers based on charged cellular polypropylene (PP). This material has about hundred times lower acoustic impedance than any piezocomposite, having about the same piezoelectric coefficient. The piezoelectric properties of cellular PP are caused by the polarization of air cells. Alternatively, a ferroelectret receiver can be understood as a capacitive microphone with internal polarization creating permanent internal voltage. The sensitivity of the receiver can be increased by applying additional bias voltage. We present an ultrasonic receiver based on cellular PP including a high-voltage module providing bias voltage up to 2 kV. The application of bias voltage increased the signal by 12 to 15 dB with only 1 dB increase of the noise. This receiver was combined with a cellular PP transmitter in through transmission to inspect several test specimens consisting of glass-fiber-reinforced polymer face sheets and a porous closed-cell PVC core. These test specimens were inspected before and after load. Fatigue cracks in the porous PVC core and some fatigue damage in the face sheets were detected. These test specimens were originally developed to emulate a rotor blade segment of a wind power plant. Similar composite materials are used in lightweight aircrafts for the general aviation. The other inspected test specimen was a composite consisted of glass-fiber-reinforced polymer face sheets and a wooden core. The structure of the wooden core could be detected only with cellular PP transducers, while commercial air-coupled transducers lacked the necessary sensitivity. Measured on a 4-mm thick carbon-fiber-reinforced polymer plate, cellular PP transducers with additional bias voltage achieved a 32 dB higher signal-to-noise ratio than commercial air-coupled transducers. T2 - 10th International Symposium on NDT in Aerospace CY - Dresden, Germany DA - 26.10.2018 KW - Airborne ultrasonic testing KW - Air-coupled ultrasonic testing KW - Ferroelectret KW - Composites KW - Rotor blade PY - 2018 AN - OPUS4-46656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Schadow, Florian A1 - Nielow, Dustin A1 - Trappe, Volker T1 - Air-coupled ultrasonic ferroelectret transducers with additional bias voltage for testing of composite structures N2 - Common air-coupled transducers for non-destructive testing consist of a piezocomposite material and several matching layers. Better acoustical matching to air is achieved by transducers based on charged cellular polypropylene (PP). This material has about hundred times lower acoustic impedance than any piezocomposite, having about the same piezoelectric coefficient. The piezoelectric properties of cellular PP are caused by the polarization of air cells. Alternatively, a ferroelectret receiver can be understood as a capacitive microphone with internal polarization creating permanent internal voltage. The sensitivity of the receiver can be increased by applying additional bias voltage. We present an ultrasonic receiver based on cellular PP including a high-voltage module providing bias voltage up to 2 kV. The application of bias voltage increased the signal by 12 to 15 dB with only 1 dB increase of the noise. This receiver was combined with a cellular PP transmitter in through transmission to inspect several test specimens consisting of glass-fiber-reinforced polymer face sheets and a porous closed-cell PVC core. These test specimens were inspected before and after load. Fatigue cracks in the porous PVC core and some fatigue damage in the face sheets were detected. These test specimens were originally developed to emulate a rotor blade segment of a wind power plant. Similar composite materials are used in lightweight aircrafts for the general aviation. The other inspected test specimen was a composite consisted of glass-fiber-reinforced polymer face sheets and a wooden core. The structure of the wooden core could be detected only with cellular PP transducers, while commercial air-coupled transducers lacked the necessary sensitivity. Measured on a 4-mm thick carbon-fiber-reinforced polymer plate, cellular PP transducers with additional bias voltage achieved a 32 dB higher signal-to-noise ratio than commercial air-coupled transducers. T2 - 10th International Symposium on NDT in Aerospace CY - Dresden, Germany DA - 26.10.2018 KW - Airborne ultrasonic testing KW - Air-coupled ultrasonic testing KW - Ferroelectret KW - Composites KW - Transducers PY - 2018 SP - 1 EP - 6 AN - OPUS4-46657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Voll integrierte und vernetzte Systeme und Prozesse - Perspektive: Smarte Sensorik, Aktorik und Kommunikation T1 - Fully integrated distributed systems and processes – Perspective: Smart sensors, actuators, and communication N2 - Unternehmen der chemischen Industrie müssen neuen Pfade beschreiten, um in einem veränderten Umfeld erfolgreich bestehen zu können. Dazu gehört insbesondere, das Potenzial digitaler Technologien zu nutzen. Die volle Integration und intelligente Vernetzung von Systemen und Prozessen kommt allerdings nur zögerlich voran. Dieser Beitrag ist ein Loblied auf die Feldebene. Er möchte dazu ermutigen, die Digitalisierung der Prozessindustrie auf Basis smarter Sensorik, Aktorik und Kommunikation ganzheitlicher zu denken und informiert über aktuelle technische Perspektiven, wie das Ein-Netzwerk-Paradigma, Ad-hoc-Vernetzungen, Edge-Computing, FPGAs, virtuelle Maschinen oder Blockchain. Diese geben smarter Sensorik, Aktorik und Kommunikation eine völlig neue Perspektive. N2 - Chemical companies must find new paths to success in a changing environment. In particular, this will involve exploiting the potential of digital technologies. However, the full integration and intelligent interconnection of systems and processes is only making slow progress. This contribution aims to encourage the more comprehensive use of digitization in the process industry based on smart sensors, actuators, and communications, and informs about current technical possibilities such as the “one-network paradigm”, ad-hoc connections, edge computing, FPGAs, virtual machines and blockchain. These offer a new scope for smart sensors, actuators, and communications. KW - Smarte Sensoren KW - Smarte Aktoren KW - Digitalisierung der Prozessindustrie KW - Prouess-Sensoren 4.0 KW - Smart sensors KW - Smart actuators KW - Digitization of process industry KW - Process sensors 4.0 PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-466642 DO - https://doi.org/10.17560/atp.v60i10.2376 SN - 2364-3137 VL - 60 IS - 10 SP - 70 EP - 85 PB - Vulkan Verlag CY - Essen AN - OPUS4-46664 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Delbeck, S. A1 - Vahlsing, Thorsten A1 - Leonhardt, S. A1 - Steiner, G. A1 - Heise, H.M. T1 - Non-invasive monitoring of blood glucose using optical methods for skin spectroscopy - opportunities and recent advances N2 - Diabetes mellitus is a widespread disease with greatly rising patient numbers expected in the future, not only for industrialized countries but also for regions in the developing world. There is a need for efficient therapy, which can be via self-monitoring of blood glucose levels to provide tight glycemic control for reducing the risks of severe health complications. Advancements in diabetes technology can nowadays offer different sensor approaches, even for continuous blood glucose monitoring. Non-invasive blood glucose assays have been promised for many years and various vibrational spectroscopy-based methods of the skin are candidates for achieving this goal. Due to the small spectral signatures of the glucose hidden among a largely variable background, the largest signal-to-noise ratios and multivariate calibration are essential to provide the method applicability for self-monitoring of blood glucose. Besides multiparameter approaches, recently presented devices based on photoplethysmography with wavelengths in the visible and near-infrared range are evaluated for their potential of providing reliable blood glucose concentration predictions. KW - Non-invasive glucose sensing KW - Vibrational spectroscopy KW - Photoplethysmography KW - Multivariate calibration KW - Validation studies PY - 2019 DO - https://doi.org/10.1007/s00216-018-1395-x SN - 1618-2650 SN - 1618-2642 VL - 411 IS - 1 SP - 63 EP - 77 PB - Springer-Verlag GmbH Germany, part of Springer Nature AN - OPUS4-46714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vahlsing, Thorsten A1 - Delbeck, S. A1 - Leonhardt, S. A1 - Heise, H.M. T1 - Noninvasive monitoring of blood glucose using color-coded photoplethysmographic images of the illuminated fingertip within the visible and near-infrared range: Opportunities and questions N2 - Noninvasive blood glucose assays have been promised for many years and various molecular spectroscopy-based methods of skin are candidates for achieving this goal. Due to the small spectral signatures of the glucose used for direct physical detection, moreover hidden among a largely variable background, broad spectral intervals are usually required to provide the mandatory analytical selectivity, but no such device has so far reached the accuracy that is required for self-monitoring of blood glucose (SMBG). A recently presented device as described in this journal, based on photoplethysmographic fingertip images for measuring glucose in a nonspecific indirect manner, is especially evaluated for providing reliable blood glucose concentration predictions. KW - Color sensing KW - Noninvasive glucose sensing KW - Plethysmographic skin imaging KW - Skin tissue spectroscopy KW - Visible/near-infrared spectroscopy PY - 2018 DO - https://doi.org/10.1177/1932296818798347 SN - 1932-2968 VL - 12 IS - 6 SP - 1169 EP - 1177 PB - Sage Publishing AN - OPUS4-46715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - A new set of zinc based calibration samples for GD-OES N2 - The analysis of Zinc layers on Iron sheets is one of the most essential application of Glow Discharge - Optical Emission Spectrometry (GD-OES). Since the year 2000 for this application calibration of GD-OES instruments mostly included the set of the six calibration samples CZ 2009-CZ 2014 from CKD. These CRMs are no longer available. Furthermore, in this application the analysis of Al and Mg became essential. To overcome this lack of calibration materials, the working group VDEh FA II.47 decided to organize the production and characterization of a new set of certified reference materials. T2 - BERM CY - Berlin, Germany DA - 23.09.2018 KW - GD-OES KW - CRM KW - Zinc PY - 2018 AN - OPUS4-46718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - A new set of zinc based calibration samples for GD-OES N2 - The analysis of Zinc layers on Iron sheets is one of the most essential application of Glow Discharge - Optical Emission Spectrometry (GD-OES). Since the year 2000 for this application calibration of GD-OES instruments mostly included the set of the six calibration samples CZ 2009-CZ 2014 from CKD. These CRMs are no longer available. Furthermore, in this application the analysis of Al and Mg became essential. To overcome this lack of calibration materials, the working group VDEh FA II.47 decided to organize the production and characterization of a new set of certified reference materials. T2 - 4th International Glow Discharge Spectroscopy Symposium CY - Berlin, Germany DA - 15.04.2018 KW - GD-OES KW - CRM KW - Zinc PY - 2018 AN - OPUS4-46719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Beck, M. A1 - Becker, S. A1 - Beckmann, Jörg A1 - Cojocari, O. A1 - Feige, V. A1 - Fischer, B. A1 - Friederich, F. A1 - Globisch, B. A1 - Haupt, H. A1 - Hechtfischer, G. A1 - Hens, K. A1 - Hübers, H.-W. A1 - Jelonnek, J. A1 - Jonuscheit, J. A1 - Keil, A. A1 - Kleine-Ostmann, T. A1 - Nickel, H.-U. A1 - Peichl, M. A1 - Peters, O. A1 - Sprenger, T. A1 - Steiger, A. A1 - van Frank, S. A1 - Vieweg, N. A1 - Werner, M. A1 - Wilk, R. T1 - Terahertzsysteme - Anwendungsfelder und Systeme N2 - Die nicht ionisierende elektromagnetische Strahlung im Bereich von Terahertz-Frequenzen ermöglicht berührungslose und zerstörungsfreie Mess- und Prüftechnik in zahlreichen Bereichen. Nach ersten Anwendungen in der Astronomie und der Atmosphärenforschung wurden in letzter Zeit Anwendungsfelder in der Sicherheitstechnik, der Medizintechnik, der Nachrichtentechnik und der zerstörungsfreien Prozess- und Qualitätskontrolle erschlossen. Dielektrische Materialien wie Kunststoffe und Keramiken können von Terahertz-Wellen durchdrungen werden. Das ermöglicht Untersuchungen des Objektinneren ohne spezielle Schutzmaßnahmen, wie sie z.B. beim Röntgen notwendig sind. Die Richtlinie erleichtert die Verständigung zwischen Nutzern, Herstellern und dem Vertrieb von Terahertz-Systemen. In der Richtlinie werden bekannte Einsatzgebiete sowie die eingesetzten Verfahren und Funktionsprinzipien aufgeführt, um den Leser bei der Auswahlentscheidung zu unterstützen. Nach einer kurzen Einführung in die physikalischen Grundlagen und Hinweisen zur elektromagnetischen Verträglichkeit, zum Strahlenschutz und zur regulierten Frequenzvergabe werden die verschiedenen Geräteklassen von Terahertz-Systemen ausführlich vorgestellt. Die Richtlinie gibt Hinweise zur messtechnischen Charakterisierung von Terahertz-Wellen. Einsatzgebiete von Terahertz-Systemen, wie die zerstörungsfreie Prüfung, die Dicken- und Abstandsmessung, die Tomografie und die chemische Analytik, werden mit ihren spezifischen Eigenschaften im Detail beschrieben. Umfangreiche Literaturverweise vereinfachen eine vertiefte Beschäftigung mit den Themen der Richtlinie. Eine tabellarische Übersicht mit einer Zusammenfassung, welche Terahertz-Systeme für welche Anwendungsfelder eingesetzt werden können, vervollständigt die Richtlinie. KW - Terahertzsysteme KW - THz-Wellen PY - 2018 UR - https://www.vdi.de/5590 VL - VDI/VDE 5590 Blatt 2 SP - 1 EP - 27 PB - VDI-Verlag CY - Düsseldorf ET - Entwurf - November 2018 AN - OPUS4-46727 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kunz, Valentin T1 - How to meet new challenges in advanced nanoparticle analytics N2 - Three current research projects performed at BAM’s Division for Surface Analysis and Interfacial Chemistry are presented that tackle important challenges with regard to the characterization of nanomaterials: 1) The characterization at ambient pressure, 2) the investigation of core-shell nanoparticles, and 3) the characterization of non-spherical particles by electron microscopy. 1) Surface analytical techniques such as Photoelectron Spectroscopy (XPS) or Secondary Ion Mass Spectrometry (SIMS) typically require measurements in ultra-high vacuum. However, for many applications (e.g. catalysis and nanotoxicology) it is important to know the surface chemical properties of nanomaterials at ambient conditions. Therefore, near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS) was used to investigate nanoparticles in suspension. The used instrumental set-up allows to directly insert nanoparticle suspensions into the analysis chamber and to measure without prior sample preparation. Compared to dry reference samples measured under high-vacuum, a shift towards higher binding energies was observed for silver nanoparticles in water, indicating a change of surface potential at the water-nanoparticle interface. 2) To determine the dimensions of core-shell nanoparticles (shell thickness, core and total diameter), scanning transmission X-ray microscopy (STXM) was used. The analyzed model system consists of a polytetrafluorethylene (PTFE) core surrounded by a polystyrene (PS) shell, providing a strong X-ray absorption contrast at the C K-edge and a well-defined interface. The introduced STXM‐based methodology yields particle dimensions in agreement with scanning electron microscopy (SEM) results and provides additional information such as the position of the particle core, which cannot be extracted from a SEM micrograph. 3) The accurate measurement of size distributions of non-spherically shaped nanoparticles (representing most of the industrial nanoparticulate materials) is a challenging analytical task. High-resolution electron microscopy (TEM and SEM) is best suited to access the shape of individual nanoparticles. To fill the gap between ideal, monodisperse particles of spherical shape and complex real-world samples, BAM has started the work to develop reference nanoparticles of controlled shape, such as TiO2 platelets, bipyramids, and elongated particles. Results of a recent ISO inter-laboratory comparison will be shown with emphasis on the measurement parameters, descriptors and data analysis. T2 - NanoSafe Conference 2018 CY - Grenoble, France DA - 5.11.2018 KW - Nanoparticles PY - 2018 AN - OPUS4-46730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Multi-method analysis of pore-controlled mesoporous oxide materials N2 - Determining the porosity of catalytic layers is crucial for quality assurance. We present results of a multi-method study to determine thickness, porosity, dielectric function and other properties of pure and mixed iridium and titanium oxide layers used in electrocatalytic water splitting. T2 - European Optical Society Biennial Meeting (EOSAM) 2018 CY - Delft, The Netherlands DA - 08.10.2018 KW - Multi-method analysis KW - Mesoporous oxide materials KW - Electro catalytic water splitting KW - Electron probe X-ray microanalysis (EPMA) KW - Spectroscopic ellipsometry (SE) KW - Optical porosimetry PY - 2018 AN - OPUS4-46740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abdoul-Carime, H. A1 - Bald, Ilko A1 - Illenberger, E. A1 - Kopyra, J. T1 - Selective synthesis of ethylene and acetylene from dimethyl sulfide cold films controlled by slow electrons N2 - One of the major challenges in chemical synthesis is to trigger and control a specific reaction route leading to a specific final product, while side products are avoided. Methodologies based on resonant processes at the molecular level, for example, photochemistry, offer the possibility of inducing selective reactions. Electrons at energies below the molecular ionization potential (<10 eV) are known to dissociate molecules via resonant processes with higher cross sections and specificity than photons. Here we show that even subexcitation electrons with energies as low as 1 eV produce ethylene and acetylene from dimethyl sulfide in competing reactions. However, the production of ethylene can specifically be targeted by controlling the energy of electrons (∼3 to 4 eV). Finally, pure ethylene is selectively desorbed by heating the substrate from 90 to 105 K. Beyond the synthesis of these versatile hydrocarbons for various industrial applications from a biogenic sulfur compound, our findings demonstrate the feasibility of electron-induced selective chemistry applicable on the nanoscale. KW - Low-energy electrons KW - Dissociative electron attachment KW - Green chemistry PY - 2018 DO - https://doi.org/10.1021/acs.jpcc.8b07377 SN - 1932-7447 VL - 122 IS - 42 SP - 24137 EP - 24142 PB - ACS AN - OPUS4-46679 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raysyan, Anna T1 - A fast dipstick immunoassay for the determination of DCF in the breast milk N2 - Diclofenac (DCF) is a non-steroidal anti-inflammatory drug (NSAID) with analgetic, anti-inflammatory, and antipyretic properties. The mechanism of action of diclofenac, like that of other NSAIDs, involves inhibition of cyclooxygenase (COX-1 and COX-2). Another pharmacological effect is preventing of prostaglandin synthesis in vitro. Prostaglandins are mediators of inflammation, because diclofenac is an inhibitor of prostaglandin synthesis. A method has been developed to analyse for diclofenac (DCF) in the milk. T2 - BIONNALE Speed Lecture Award 2018 CY - Berlin, Germany DA - 20.06.2018 KW - Milk KW - DCF KW - Immunoassay PY - 2018 AN - OPUS4-46753 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Raysyan, Anna T1 - Breaking the wall of complicated laboratory methods N2 - How intricate lab methods make it to the lay(wo)men’s hand. T2 - Falling Walls Lab Adlershof CY - Berlin, Germany DA - 28.09.2018 KW - Easy-use device PY - 2018 AN - OPUS4-46755 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Mechanistic investigations of mechanosyntheses N2 - Mechanochemistry is a fast and efficient method applicable for the synthesis of new organic, metal-organic, and inorganic compounds. The direct monitoring of milling reactions is still challenging. The underlying reaction mechanisms often remain unclear. In the last years, we have established a tandem in situ approach for investigating mechanochemical reactions using time-resolved in situ XRD coupled with Raman spectroscopy. A further development is the in situ coupling of synchrotron XRD, Raman spectroscopy, and thermography allowing the observation of mechanochemical reactions in real time. [5] Information on the crystalline, molecular, and temperature state of the materials during grinding could be collected. The chemical composition of the reaction mixture was found to be directly correlated with changes in the temperature profile of the reaction. Furthermore, the presented setup allows the detection of crystalline, amorphous, eutectic as well as liquid intermediates. Based on these data, metastable polymorphs of cocrystals and coordination polymorphs could be isolated and struc-turally characterized. A multi-step diffusion mechanism was identified for most systems. Crystalline phases were obtained intermediately, suggesting that the synthesis is following Ostwald’s rules of stages. The resulting deeper kinetic and thermodynamic understanding of milling processes is the key for future optimization of mechanochemical syntheses. T2 - Beilstein Symposium MECHANOCHEMISTRY: MICROSCOPIC AND MACROSCOPIC ASPECTS CY - Rüdesheim, Germany DA - 13.11.2018 KW - Mechanochemistry KW - Phosphonates KW - In situ PY - 2018 AN - OPUS4-46758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - BAM and Division 6.1 N2 - This is a short overview of BAM and Division 6.1. We have insight into BAM's roles and responsibilities and the work we are doing in Division 6.1. T2 - Visit at CSEM Landquart CY - Landquart, Switzerland DA - 13.08.2018 KW - ToF-SIMS KW - AES KW - XPS KW - SEM PY - 2018 AN - OPUS4-46765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sunderkötter, Jan T1 - Qualitätssicherung im Labor auf Grundlage der ISO/IEC 17025 N2 - Die Begriffe Qualität und Kompetenz im Labor werden beleuchtet und der Inhalt der ISO/IEC 17025 dargestellt und erläutert. T2 - Herbstschule 2018 Qualitätssicherung in der Analytischen Chemie CY - Berlin, Germany DA - 29.10.2018 KW - Qualitätssicherung KW - Akkreditierung KW - Konformitätsbewertung KW - ISO/IEC 17025 PY - 2018 AN - OPUS4-46849 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Vogl, Jochen T1 - Roadmap for the purity determination of pure metallic elements – Basic rinciples and helpful advice N2 - High purity materials can serve as a realisation of the Système International d’Unitès (SI) unit amount of substance for the specific element. Solutions prepared from such high purity materials using gravimetric preparation and the concept of molar mass are used as calibration solutions in many fields of analytical chemistry. Calibration solutions prepared this way provide the traceability to the SI and are the metrological basis in elemental analysis. The preparation and characterization of such primary pure substances, representing the realisation of the SI unit amount of substance, is undertaken only by a small number of National Metrology Institutes (NMI) and Designated Institutes (DI). Many other NMIs and DIs, however, prepare elemental calibration solutions as calibrants for their measurement services, such as the certification of matrix Reference Materials or the provision of reference values for Proficiency Testing schemes. The elemental calibration solutions used for this purpose are not a direct service to customers, such as preparing secondary calibration solutions, but provide the source of traceability for the other services. Hence, it is necessary for the NMI or DI to obtain data on the purity of the pure metals or other materials used to prepare the solutions with measurement uncertainties meeting the needs of the above described services. This is commonly undertaken as a “fit for purpose” assessment, appropriate for the uncertainty requirement of the service provided to customers. As a consequence, total purity measurements are a long-term strategy of CCQM-IAWG. Several studies were conducted (CCQM-P107, CCQM-K72 and CCQM-P149) on the measurement of the purity of zinc. From these studies, several conclusions can be drawn for the purity assessment of a pure (metallic) element. These conclusions will be put together in this document in order to assist all NMIs/DIs in performing a purity assessment, whenever needed. KW - Purity assessment KW - Metal assay approach KW - Impurity assessment approach KW - Traceability PY - 2018 UR - https://www.bipm.org/wg/CCQM/IAWG/Allowed/April_2017/CCQM-IAWG17-28.pdf.pdf SP - 1 EP - 9 CY - Sevre AN - OPUS4-46834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kadlag, Y. A1 - Tatzel, Michael A1 - Frick, D. A. A1 - Becker, H. T1 - Silicon isotope constraints on the formation of silicates and metal in EH chondrites N2 - Bulk enstatite chondrites (EC) and their achondritic counterpart, the aubrites, have the lightest measured Si isotope composition of all rocks in the solar system. Some authors proposed that the enrichment of 28Si in EC metal by equilibrium or kinetic isotope fractionation processes in the solar nebula may have led to the negative δ30/28Si of bulk EC. Because EC are also depleted in refractory elements, loss of a heavy Si component with refractory elements might be an alternative explanation. To further constrain their genesis, we analysed for the first time in situ Si-isotope ratios simultaneously with major- and trace element abundances in silicate and metal phases of Sahara 97072 (EH3) and Indarch (EH4). T2 - 81st Annual Meeting of The Meteoritical Society 2018 CY - Moscow, Russia DA - 22.07.2018 KW - Si isotopes PY - 2018 SN - 1945-5100 VL - 53 SP - 6154 EP - 6154 PB - Wiley AN - OPUS4-46835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hofmann, Michael A1 - Tiebe, Carlo T1 - VDI/VDE 3518 - Technische Richtlinie für Multigassensoren N2 - Der Beitrag präsentiert die erarbeiteten technischen Richtlinien zur Anwendung und Prüfung von Multigassensoren innerhalb der Richtlinienreihe VDI/VDE 3518 sowie in diesem Zusammenhang die Möglichkeiten der Sensorprüfung im akkreditierten Prüflabor des Fachbereichs 8.1 der BAM. Im Speziellen wird das in Kürze veröffentlichte Blatt 3 der Richtlinienreihe vorgestellt, das Bezug auf Multigassensoren für geruchsbezogene Messungen mit elektronischen Nasen nimmt. T2 - 5. Fachsymposium "Intelligente Sensorik/Analytik und sichere Sensornetze: Innovative Technologien und neue Anwendungsfelder" CY - Eggenstein -Leopoldshafen, Germany DA - 14.11.2018 KW - Multigassensoren KW - Richtlinie KW - Prüfung KW - Elektronische Nase PY - 2018 UR - http://hybridsensornet.org/symposien.html SP - 61 EP - 62 AN - OPUS4-46839 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hofmann, Michael T1 - VDI/VDE 3518 Technische Richtlinie für Multigassensoren N2 - Der Beitrag präsentiert die erarbeiteten technischen Richtlinien zur Anwendung und Prüfung von Multigassensoren innerhalb der Richtlinienreihe VDI/VDE 3518 sowie in diesem Zusammenhang die Möglichkeiten der Sensorprüfung im akkreditierten Prüflabor des Fachbereichs 8.1 der BAM. Im Speziellen wird das in Kürze veröffentlichte Blatt 3 der Richtlinienreihe vorgestellt, das Bezug auf Multigassensoren für geruchsbezogene Messungen mit elektronischen Nasen nimmt. T2 - 5. Fachsymposium "Intelligente Sensorik/Analytik und sichere Sensornetze: Innovative Technologien und neue Anwendungsfelder" CY - Eggenstein-Leopoldshafen, Germany DA - 14.11.2018 KW - Multigassensoren KW - Richtlinie KW - Prüfung KW - Elektronische Nase PY - 2018 AN - OPUS4-46840 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Concepts from seismic interferometry transferred to sonic and ultrasonic concrete inspection and monitoring N2 - Seismic interferometry (SI) deals either with the sensible detection of changes in the subsurface or with the reconstruction of virtual signals between two receivers by crosscorrelation of signals from diffuse sources. These concepts can be applied in NDT in civil engineering for various purposes, e. g. to detect changes in bridges. Here it is demonstrated using data from a reference structure on our test site. Practical applications can be expected in the very near future. T2 - European Conference on Non-Destructive Testing (ECNDT) CY - Gothenburg, Sweden DA - 11.6.2018 KW - Ultrasound KW - Monitoring KW - Concrete KW - Interferometry KW - Coda PY - 2018 AN - OPUS4-46844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Chapartegui, Ander T1 - MOFs as optical sensor elements against endocrine disrupting phthalates N2 - The development of optical sensing technologies for Endocrine Disrupting Chemicals (EDCs) was urgently needed to facilitate currently unmet demands on comprehensive monitoring of These substances, thus ensuring consumer safety. T2 - SALSA CY - Berlin, Germany DA - 01.05.2018 KW - MOF KW - Short chained phthalates PY - 2018 AN - OPUS4-46889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Chapartegui, Ander T1 - Metal-Organic Frameworks as turn on fluorescent optical sensors against endocrine disrupting phthalate plasticizers N2 - The development of quick and simple optical sensing technologies for Endocrine Disrupting Chemicals (EDCs) is needed to facilitate monitoring of these substances to ensure consumer safety. Optical sensing was achieved against phthalates acting as EDC that have host guest interaction with an intercalated Metal-organic framework (MOF), resulting in a fluorescence emission upon excitation. The fluorescent turn-on signal was generated by using a fluorophore with a structural component that has little fluorescence unless excimers are formed. Strategies to engineer functional MOF structures suitable for sensing EDC phthalates were developed, and the characterization of the MOFs with and without present phthalates was done by single crystal XRD, PXRD, RAMAN and Thermogravimetry. Extensive photo-physical characterization of host-guest complexes of different phthalates and the MOF as well as the resulting exciplex fluorescence was performed. Photo physical characterization revealed an analyte specific fluorescence fingerprint that allows discerning even minute changes in chemical structures of the analyte and therefore paving the way for sensing tools in real world analytical applications. The presented capability of MOFs to sense EDCs is envisioned to complement established methods from analytical chemistry such as mass spectrometry based methods which can’t be used on site and are often associated with infrastructural capacity constraints T2 - EURoptrode CY - Naples, Italy DA - 25.03.2018 KW - MOF KW - Short chained Phthalates PY - 2018 AN - OPUS4-46890 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Fast quantitave chemical analysis of concrete using LIBS N2 - Overview about LIBS applications for investigation of building materials. T2 - NDT&E Advanced Training Workshop CY - Berlin, Germany DA - 27.06.2018 KW - LIBS KW - Concrete KW - Damage processes KW - Chlorid KW - Sulfate KW - Alkalies PY - 2018 AN - OPUS4-46821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg ED - Jaunich, Matthias ED - Wolf, Dietmar ED - Schade, U. ED - Kerstin, von der Ehe T1 - THz-and mid IR Fourier Transform Spectroscopy on Physical Aged Polyethylene N2 - THz and mid IR spectroscopy of high-molecular PE (HMW) and ultra high-molecular PE (UHMW) reveals modifications of the molecular structure. Characteristic absorption bands are changed if the two materials are exposed by γ-Co60 radiation up to 600 kGy and subsequently stored at an annealing temperature of 398 K until for 729 days. T2 - 43rd International Conference on Infrared, Millimeter and Terahertz Waves (IRMMW-THZ), 2018 CY - Nagoya, Japan DA - 09.09.2018 KW - THz Spectroscopy PY - 2018 SN - 978-1-5386-3809-5 SN - 2162-2027 SP - 1 EP - 1 PB - IEEE Xplore Digital Library AN - OPUS4-46824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Application of LIBS for the chemical investigation of concrete infrastructure N2 - Concrete is often used in combination with steel as reinforced concrete. Environmental influences, especially the ingress of harmful ions in combination with the ingress of water, trigger different damage processes which reduce the designed lifetime of a structure. The ingress of chlorides from de-icing salt or sea water leads to corrosion of the reinforcement. Also the carbonation of the concrete may trigger the corrosion of the reinforcement. The ingress of alkalis from de-icing salts may cause the expansion of the amorphous silica aggregates (alkali-silica reaction) through formation of a swelling gel of calcium silicate hydrate if water is present. The ingress of sulfates may cause spalling of the concrete surface due to ettringite formation. BAM has developed the LIBS technique for automated laboratory use with high numbers of samples to investigate transport processes of harmful species (Cl-, CO2, SO42- and alkalis) in concrete. Information about ingress depth and the quantitative values are important to estimate the remaining lifetime of the infrastructure. To get information about the ingress depth, a core has to be taken and cut in the middle. The measurements are carried out at the cross section. The main advantages of LIBS are the direct measurement on the surface of the concrete, fast analysis (sample rate 100 Hz) with a spatial resolution of up to 100 µm, the consideration of the heterogeneity of the concrete. The possibility of automated measurements saves a lot of manpower and time. At the same time a 2D-evaluation provides information about hot spots of elemental concentration which may not be found by standard methods. Typical results of 2D investigation of concrete in laboratory will be presented. The performance is also demonstrated by examples for onsite applications using a mobile LIBS system. The road map to standardization is presented as well. T2 - 12th ECNDT CY - Gothenburg, Sweden DA - 11.06.2018 KW - LIBS KW - Concrete KW - Chloride KW - Sulfates KW - Heterogeneity PY - 2018 AN - OPUS4-46828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Gottlieb, Cassian A1 - Günther, Tobias A1 - Völker, Tobias ED - Ludwig, H.-M. T1 - Schnelle quantitative Untersuchung von Elementverteilungen in Beton mittels LIBS N2 - Die Laserinduzierte Plasmaspektroskopie (engl.: Laser-induced Breakdown Spectroscopy, kurz: LIBS) ist eine Kombination aus Laserablation mittels eines energiereichen Laser-Pulses, der Erzeugung eines Plasmas auf der zu untersuchenden Oberfläche und dem quantitativen Nachweis der Elementzusammensetzung durch spektroskopische Untersuchung der vom Plasma emittierten Strahlung. Ein LIBS-Gerät liefert dem sachkundigen Planer Daten für die Bewertung des Ist-Zustandes von Bauwerken unserer Infrastruktur durch die zweidimensionale Erfassung von Elementverteilungen. Typische Anwendungen sind die Erfassung von Chlor, Schwefel, Kohlenstoff, Natrium, Kalium und Lithium in Beton oder als – Qualitätssicherung – der Nachweis der mit einem Marker versehenen Tiefenhydrophobierung. In Zusammenarbeit zwischen Industriepartnern und der BAM wurden ein Labor und ein mobiles LIBS-System für die Vor-Ort-Messungen entwickelt. Die Analyse erfolgt vollautomatisch. Die Ortsauflösung beträgt bis zu 0,1 mm x 0,1 mm. Es können Messflächen von 140 mm x 170 mm gescannt werden. Die Erstellung von 2D-Elementverteilungen im Beispiel unten benötigt weniger als 10 Minuten. T2 - ibausil - 20. Internationale Baustofftagung CY - Weimar, Germany DA - 12.09.2018 KW - LIPS KW - LIBS KW - Beton KW - Chlorid PY - 2018 SN - 978-3-00-059950-7 VL - 2 SP - 2380 EP - 2387 PB - F.A. Finger-Institut für Baustoffkunde, CY - Weimar AN - OPUS4-46779 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Application of LIBS for the chemical investigation of concrete infrastructure N2 - The majority of the built infrastructure is made of concrete, which is a multiphase system made of cement, aggregates, water and pores. Concrete is often used in combination with steel as reinforced concrete. Environmental influences, especially the ingress of harmful ions in combination with the ingress of water, trigger different damage processes which reduce the designed lifetime of a structure. The ingress of chlorides from de-icing salt or sea water leads to corrosion of the reinforcement. Also the carbonation of the concrete may trigger the corrosion of the reinforcement. The ingress of alkalis from de-icing salts may cause the expansion of the amorphous silica aggregates (alkali-silica reaction) through formation of a swelling gel of calcium silicate hydrate if water is present. The ingress of sulfates may cause spalling of the concrete surface due to ettringite formation. For the standard procedure in civil engineering cores are taken, cut in slices, grinded and the obtained homogenized powder is solved in acid and investigated by standard procedures. BAM has developed the LIBS technique for the 2D evaluation of the chemical composition of concrete [1-11]. The technique is established for automated laboratory use with high numbers of samples to investigate transport processes of harmful species (Cl-, CO2, SO42- and alkalis) in concrete. Information about ingress depth and the quantitative values are important to estimate the remaining lifetime of the infrastructure. LIBS is a surface technique. To get information about the ingress depth, a core has to be taken and cut in the middle. The measurements are carried out at the cross section. The main advantages of LIBS are the direct measurement on the surface of the concrete, fast analysis (sample rate 100 Hz) with a spatial resolution of up to 100 µm, the consideration of the heterogeneity of the concrete and the possibility of automated measurements which save a lot of manpower and time. As an example the investigation of ingress profiles for standard diffusion and migration tests in civil engineering takes hours in comparison to just a few minutes using LIBS. At the same time a 2D-evaluation provides information about hot spots of elemental concentration which may not be found by standard methods. Ingress of chlorides due to a crack in a repair mortar. Left: Photo of the cross section of a concrete core and the surface investigated by LIBS (area 70 mm x 70 mm). Right: Color coded chlorine intensity on the cross section of a concrete core, dark red represents high chlorine content. The state of the art of LIBS technique for applications in civil engineering will be presented, including typical results of 2D investigation of concrete in laboratory. The performance is also demonstrated by examples for onsite applications using a mobile LIBS system. The road map to standardization is presented as well. T2 - ICCRRR2018, 5th international conference on Concrete Repair, Rehabilitation and Retrofitting CY - Cape Town, South Africa DA - 19.11.2018 KW - LIBS KW - Chlorid KW - Alkalies KW - Concrete KW - Damage PY - 2018 AN - OPUS4-46781 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - Detection of ion ingress by LIBS for Evaluation of the remaining lifetime of a concrete structure N2 - The majority of the built infrastructure is made of concrete, which is a multiphase system made of cement, aggregates, water and pores. Concrete is often used in combination with steel as reinforced concrete. Environmental influences, especially the ingress of harmful ions in combination with the ingress of water, trigger different damage processes which reduce the designed lifetime of a structure. The ingress of chlorides from de-icing salt or sea water leads to corrosion of the reinforcement. Also the carbonation of the concrete may trigger the corrosion of the reinforcement. The ingress of alkalis from de-icing salts may cause the expansion of the amorphous silica aggregates (alkali-silica reaction) through formation of a swelling gel of calcium silicate hydrate if water is present. The ingress of sulfates may cause spalling of the concrete surface due to ettringite formation. For the standard procedure in civil engineering cores are taken, cut in slices, grinded and the obtained homogenized powder is solved in acid and investigated by standard procedures. BAM has developed the LIBS technique for the 2D evaluation of the chemical composition of concrete [1-11]. The technique is established for automated laboratory use with high numbers of samples to investigate transport processes of harmful species (Cl-, CO2, SO42- and alkalis) in concrete. Information about ingress depth and the quantitative values are important to estimate the remaining lifetime of the infrastructure. LIBS is a surface technique. To get information about the ingress depth, a core has to be taken and cut in the middle. The measurements are carried out at the cross section. The main advantages of LIBS are the direct measurement on the surface of the concrete, fast analysis (sample rate 100 Hz) with a spatial resolution of up to 100 µm, the consideration of the heterogeneity of the concrete and the possibility of automated measurements which save a lot of manpower and time. As an example the investigation of ingress profiles for standard diffusion and migration tests in civil engineering takes hours in comparison to just a few minutes using LIBS. At the same time a 2D-evaluation provides information about hot spots of elemental concentration which may not be found by standard methods. Ingress of chlorides due to a crack in a repair mortar. Left: Photo of the cross section of a concrete core and the surface investigated by LIBS (area 70 mm x 70 mm). Right: Color coded chlorine intensity on the cross section of a concrete core, dark red represents high chlorine content. The state of the art of LIBS technique for applications in civil engineering will be presented, including typical results of 2D investigation of concrete in laboratory. The performance is also demonstrated by examples for onsite applications using a mobile LIBS system. The road map to standardization is presented as well. T2 - ASNT SMT/NDT-CE 2018 CY - New Brunswick, NJ, USA DA - 27.08.2018 KW - Damage processes KW - LIBS KW - Concrete KW - Chloride PY - 2018 AN - OPUS4-46782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Tobias T1 - Quantitative on-site analysis of harmful elements in building structures with a mobile LIBS-System N2 - Environmental influences and damage processes drastically reduce the durability of concrete and reinforced concrete structures. Much of this damage can be traced back to the penetration of harmful elements into the concrete. These elements cause damage processes such as the chlorine-induced corrosion, the alkali-silica reaction or the carbonization. For the maintenance the knowledge of the element concentration and the penetration depth of these harmful elements is essential. Based on this data, a maintenance concept can be developed and an estimation of the remaining service life-time can be carried out. Typically, chemical analyzes are used to determine harmful elements in concrete, which are costly and time consuming. As an alternative method LIBS is used. On-site measurements were carried out with a mobile LIBS-System to determine harmful elements in a parking garage. A scanner is used to obtain a two-dimensional element mapping. For the quantitative analysis, a calibration of the system is carried out with 15 reference samples based on cement with NaCl with a concentration range of chlorine of 0.05 to 2.5 wt.%. To determine the penetration profile of the harmful element chlorine, concrete cores were drilled, split and analyzed directly on-site. T2 - Xth international conference on Laser-Induced Breakdown Spectroscopy CY - Atlanta, GA, USA DA - 21.10.2018 KW - LIBS KW - Mobile-LIBS KW - On-site analysis KW - Concrete PY - 2018 AN - OPUS4-46790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Günther, Tobias T1 - Spatially resolved determination of chloride content on rough surfaces using LIBS N2 - The durability and the lifetime of reinforced concrete structures can be drastically reduced by the influence of damage processes. One of the most common causes is chloride-induced corrosion, which is triggered by increased chloride content near the reinforcement. In a study, the chloride content should be determined directly at corrosion areas. The LIBS system used consists of a micro-chip laser (3 mJ, 100 Hz, 1.5ins) and two compact spectrometers covering the wavelength range of 177-355 nm (UV) and 750-940 nm (NIR). The analysis of the chloride content was carried out via the atomic chlorine spectral line 837.59 nm, using helium for signal amplification. Calibrations were carried out for quantitative chlorine measurements with 15 reference samples in the working range of 0.05 to 6.00 wt% chlorine. The calibration of the LIBS system was done according to DIN 32 645 and was tested for linearity. The determination of the quantitative chlorine contents was carried out on samples which were broken and thus have a high surface roughness. This requires real time correction of the focus point to compensate for the roughness of the samples. The poster shows spatially resolved element distributions and determined quantitative chloride concentrations near the corrosion Areas. T2 - Xth international conference on Laser-Induced Breakdown Spectroscopy CY - Atlanta, GA, USA DA - 21.10.2018 KW - LIBS KW - Rough surface KW - Chloride PY - 2018 AN - OPUS4-46791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilsch, Gerd A1 - Bohling, C. A1 - Molkenthin, A. T1 - Mobiles LIBS-Gerät (Laser Induced Breakdown Spectroscopy) N2 - Schädigungen durch Korrosion der Bewehrung von Stahlbetonbauwerken unserer Infrastruktur sind u. a. mit dem Eindringen von Chloriden aus Tausalzen oder Meereswasser verbunden. In den Regelwerken sind daher Grenzwerte für den maximal zulässigen Chlorid-Gehalt deiniert. Die Einhaltung dieser Grenzwerte wird in der Praxis über die Entnahme von Bohrmehl oder die Entnahme von Bohrkernen überwacht. Die Bohrkerne werden in Zylindersegmente von meist zwei cm Höhe geschnitten, dann gemahlen und mit Säure aufgeschlossen. Das Bohrmehl aus verschiedenen Tiefenabschnitten kann direkt mit Säure aufgeschlossen werden. Der Chlorid-Gehalt im Aufschluss wird dann meist mittels Potentiometrischer Titration bestimmt. Dieses Vorgehen ist mit einem hohen Zeit- und Personalaufwand verbunden. Die Information über die Heterogenität des Betons geht dabei aufgrund der Homogenisierung bei der Probenvorbereitung oder bei der Entnahme von Bohrmehl verloren. Der Chlorid-Gehalt wird in der homogenisierten Betonprobe (Zement, Wasser und Gesteinskörnung) analysiert und die Werte bezogen auf den Beton angegeben. Demgegenüber sind die Grenzwerte des maximal zulässigen Chlorid-Gehaltes auf den Zement bezogen. Da die Rezeptur des Betons fast nie verfügbar ist, wird die Umrechnung vom Gehalt bezogen auf den Beton zum Gehalt bezogen auf den Zement über eine zusätzliche Analyse oder durch Abschätzung durchgeführt. Als Ergänzung zum Standardverfahren wurde in der Bundesanstalt für Materialforschung und –prüfung das LIBS- Verfahren (Laser Induced Breakdown Spectroscopy) für die Untersuchung der chemischen Zusammensetzung von Baustofen im Labor seit einigen Jahren erfolgreich eingesetzt. In einem vom Bundeswirtschatsministerium geförderten Projekt sollten die sich ergänzenden Kompetenzen eines Forschungspartners (BAM), eines Geräteherstellers (SECOPTA analytics GmbH) und eines potentiellen Anwenders (Ingenieurbüro Specht, Kalleja und Partner) in die Entwicklung eines mobilen LIBS Gerätes (BauLIBS) eingehen. Dieser Artikel stellt das Messprinzip und seine wesentlichen Vorteile vor, gibt einen Überblick über das entwickelte mobile LIBS-Gerät und seine Leistungsparameter. Anschließend werden einige erfolgreiche Anwendungsbeispiele zur Untersuchung von Schädigungsprozessen direkt an der Beton-Infrastruktur vorgestellt und ein Ausblick auf zuküntige Entwicklungen gegeben. Das BauLIBS-Gerät liefert dem sachkundigen Planer Daten für die Bewertung des Istzustandes von Bauwerken unserer Infrastruktur durch die zweidimensionale Erfassung von Elementverteilungen. Typische Anwendungen sind die Erfassung von Chlor, Schwefel, Kohlenstof, Natrium, Kalium und Lithium in Beton oder als Qualitätssicherung der Nachweis der mit einem Marker versehenen Tiefenhydrophobierung. KW - Mobiles LIBS KW - Beton KW - Chloride KW - Sulfate KW - Schädigung PY - 2018 VL - 160 IS - Juni 2018 SP - 46 EP - 50 PB - DGZfP CY - Berlin AN - OPUS4-46806 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - LIBS - Ein Tool zur Untersuchung der chemischen Zusammensetzung von Beton N2 - Die „Laser Induced Breakdown Spectroscopy“ (LIBS) bietet die Möglichkeit, direkt auf der optisch zugänglichen Oberfläche von Baustoffen 2-dimensional die Elementverteilung zu erfassen. Durch das zugrundeliegende Prinzip sind alle Elemente des Periodensystems detektierbar, auch leichte Elemente wie Wasserstoff oder Lithium. Einerseits können alle für die Zusammensetzung des Zementes und der Gesteinskörnung relevanten Elemente erfasst werden, andererseits auch die für Schädigungsprozesse in Beton wichtigen Elemente Chlor, Schwefel, Natrium, Kalium, Kohlenstoff und Stickstoff. Der Nachweis kann simultan erfolgen. Der Vorteil des Verfahrens liegt in der einfachen Probenvorbereitung, der direkten Messung auf der Oberfläche des Festkörpers und der Schnelligkeit der Messung. Die Heterogenität von Beton wird im Ergebnis berücksichtigt. Die Konzentrationen von schädigenden Ionen lassen sich bezogen auf den Bindemittelgehalt angeben. LIBS liefert standardmäßig qualitative Werte. Durch Kalibrierung anhand von Referenzproben ist eine Quantifizierung der Ergebnisse möglich. Das Potenzial des Verfahrens wird am Beispiel der Bestimmung der Chlorid-Verteilung in der Bindemittelmatrix vorgestellt. Andere Anwendungen sind die Bestimmung der Karbonatisierungstiefe, die Bestimmung des Eintrages von Alkalien oder die Bestimmung der Verteilung von Schwefel. Das Verfahren kann im Labor zur Untersuchung einer großen Anzahl von Proben oder vor-Ort zur schnellen Entscheidungsfindung eingesetzt werden. Kommerzielle Geräte sind seit kurzem verfügbar. Die örtliche Auflösung der Messung beträgt bis zu 0,1 mm × 0,1 mm. Ein Messpunkt hat einen Durchmesser von ca. 100 μm. Die Messfrequenz liegt bei 100 Hz. Als Ergebnis entstehen für jedes Element eine 2D-Darstellungen der Konzentration über der Messfläche. Der Scan eines Bohrkerns von 50 mm x 70 mm dauert bei einer Auflösung von 0,5 mm lateral und 1 mm vertikal ca. 7 min. Es können auch raue oder gebrochene Oberflächen durch Nachführung der z-Achse untersucht werden. Die Nachweisgrenze für die Bestimmung des Chlorgehaltes bezogen auf den Bindemittelgehalt liegt bei 0,03 M-%. Der Unterausschuss LIBS im Bauwesen im FA ZfP im Bauwesen der DGZfP arbeitet an der Erstellung von Merkblättern und Regelwerken zur Anwendung des Verfahrens. T2 - Bauwerksdiagnose 2018 CY - Berlin, Germany DA - 15.02.2018 KW - Alkalien KW - LIBS KW - Beton KW - Schädigung KW - Chlorid KW - Sulfat PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-468076 UR - https://www.ndt.net/search/docs.php3?id=22621 AN - OPUS4-46807 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd T1 - LIBS - Ein Tool zur Untersuchung der chemischen Zusammensetzung von Beton N2 - Dargestellt werden die Möglichkeiten von LIBS zur Untersuchung von Baustoffen und aktuelle Anwendungsbeispiele. T2 - LIBS Seminar - Immer wissen was drin ist CY - Telow, Germany DA - 28.06.2018 KW - Alkalien KW - LIBS KW - Beton KW - Schädigung KW - Chloride KW - Sulfate PY - 2018 AN - OPUS4-46820 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Development of immuno-assays and metal-staining techniques for bioimaging of cells and tissues using LA-ICP-MS N2 - We are using LA-ICP-MS to quantify metals in biological cells and thin cuts of tissues from varies organs. Different applications will be presented to demonstrate the state of the art of bioimaging to visualize the elemental distribution pattern in soft bio-materials (tissue, single cells) of metals, metal containing stains and metal-tagged antibodies. For this purpose, different strategies for metal tagging will be presented and will be compared in terms of analytical figures of merit. First applications for detection of biomarkers in animal and human tissue samples will be presented. In a first example, we have applied LA-ICP-MS to visualize the local distribution of proteins, which are used as bio-markers for neurodegenerative diseases. For this purpose, brain tissues from mice experiments have been stained by metal-tagged antibodies. House-keeping proteins have been investigated as internal cellular standards. Additionally, ink-jet printing of metal doped inks onto the surface of tissue samples has been applied for drift corrections and quantification. Validation of our results are achieved in comparison to immune-histochemical staining and optical microscopy. In a second example, we used specific metal-tagged antibodies for detection of biomarker specific for prostate cancer. For this purpose, micro tissue arrays are incubated with metal-tagged antibodies for bioimaging of samples from many patients using simultaneous detection of all relevant biomarkers and their tags. For improvement of sensitivity in the next example application nanoparticle tagged antibodies for detection of metallothionines in eye lens tissue samples will be discussed. Recently we have used our tagging and staining strategies to determine the cell cycle of single cells, which is of future interest for toxicological studies. Finally, future trends in elemental microscopy and mass cytometry imaging will be discussed. T2 - Workshop on Laser Bioimaging Mass Spectrometry CY - Münster, Germany DA - 24.05.2018 KW - Single cell analysis KW - LA-ICP-MS KW - Immuno-Assays PY - 2018 AN - OPUS4-45160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Glass transition of thin polymeric films as revealed by calorimetric and dielectric techniques N2 - The structure and dynamics of thin polymeric films is reviewed and discussed in the frame work of novel theoretical approaches T2 - Lähnwitzseminar on Calorimetry CY - Rostock-Warnemünde, Germany DA - 03.06.2018 KW - Thin polymeric films KW - Dielectric spectroscopy KW - Thermal süectroscopy PY - 2018 AN - OPUS4-45164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Standardization of ellipsometry N2 - The talk addresses the STANDARDIZATION OF ELLIPSOMETRY and the following points are discussed in more detail: historical background of ellipsometry, history of International Conferences on Ellipsometry, Workshops Ellipsometry in Germany and Europe, information on German/European Working Group Ellipsometry, technical/industrial importance of ellipsometry, applications on non-ideal material systems and standardization activities on ellipsometry. T2 - DIN NA Dünne Schichten für die Optik, Mainz CY - Mainz, Germany DA - 06.06.2018 KW - Standardization KW - Ellipsometry KW - Modelling KW - Accreditation PY - 2018 AN - OPUS4-45167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik A1 - Kreutzbruck, M. A1 - Studemund, T. A1 - Ziegler, Mathias T1 - Thermal wave interference with high-power VCSEL arrays for locating vertically oriented subsurface defects N2 - Among the photothermal methods, full-field thermal imaging is used to characterize materials, to determine thicknesses of layers, or to find inhomogeneities such as voids or cracks. The use of classical light sources such as flash lamps (impulse heating) or halogen lamps (modulated heating) led to a variety of nondestructive testing methods, in particular, lock-in and flash-thermography. In vertical-cavity surface-emitting lasers (VCSELs), laser light is emitted perpendicularly to the surface with a symmetrical beam profile. Due to the vertical structure, they can be arranged in large arrays of many thousands of individual lasers, which allows power scaling into the kilowatt range. Recently, a high-power yet very compact version of such a VCSEL-array became available that offers both the fast timing behavior of a laser as well as the large illumination area of a lamp. Moreover, it allows a spatial and temporal control of the heating because individual parts of the array can be controlled arbitrarily in frequency, amplitude, and phase. In conjunction with a fast infrared camera, such structured heating opens up a field of novel thermal imaging and testing methods. As a first demonstration of this approach, we chose a testing problem very challenging to conventional thermal infrared testing: The detection of very thin subsurface defects perpendicularly oriented to the surface of metallic samples. First, we generate destructively interfering thermal wave fields, which are then affected by the presence of defects within their reach. It turned out that this technique allows highly sensitive detection of subsurface defects down to depths in excess of the usual thermographic rule of thumb, with no need for a reference or surface preparation. T2 - 44TH ANNUAL REVIEW OF PROGRESS IN QUANTITATIVE NONDESTRUCTIVE EVALUATION CY - Provo, Utah DA - 16.07.2017 KW - Laser applications KW - Thermography KW - VCSEL KW - Subsurface defects PY - 2018 SN - 978-0-7354-1644-4 DO - https://doi.org/10.1063/1.5031547 SN - 0094-243X VL - 1949 SP - UNSP 060001, 1 EP - 8 AN - OPUS4-45171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul T1 - Entwicklung eines Ultraschallsenors zur Flüssigkeitsanalyse in Rohrleitungen N2 - Zur Messung von Konzentrationen in Flüssigkeiten können akustische Sensoren genutzt werden. Ziel der vorliegend Arbeit ist es einen Sensor zu entwerfen der sehr hohe Messgenauigkeiten erzielen kann. Der Sensor besteht aus einem rechteckigen Rohr, welches auf einem Halbraum angebracht ist. Die Konzentrationsbestimmung erfolgt anhand des Resonanzverhaltens der Struktur, wodurch eine hohe Messgenauigkeit erreicht werden kann. Um den Sensors zu verwirklichen, muss eine Optimierung der Geometrie mit vielen Iterationsschritten durchlaufen werden. Da keine analytische Beschreibung des akustischen Verhaltens vorliegt, wird eine effiziente Simulationsmethode benötigt. Die Scaled Boundary Finite Element Method (SBFEM) für prismatische Strukturen erscheint für die Simulation geeignet, da Teile der Geometrie ohne neue Vernetzung geändert werden können. Für die Berechnung des Sensors wird ein Modell der akustischen Fluid-Struktur Interaktion benötigt, das bisher nicht vorhanden ist. Die Präsentation behandelt die Implementierung des Fluidmodells in die SBFEM und deren Validierung. Für die Validierung werden die Ergebnisse mit analytischen Beispielen ohne Fluid-Struktur Kopplung und mit Comsol-Ergebnissen der Dispersionskurven mit Wasser gefüllter Rohre verglichen. Schließlich wird das neuartige Verfahren für die Modellierung der Sensorgeometrie angewendet. An einer einfachen Geometrie wird das Sensorprinzip zur Bestimmung der Salzkonzentration demonstriert. T2 - DAGA 2018 - 44. Jahrestagung für Akustik CY - Munich, Germany DA - 19.03.2018 KW - Scaled Boundary Finite Element Method KW - Penalty Parameter KW - Fluid-Structure Interaction PY - 2018 AN - OPUS4-45259 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul T1 - A fluid model for the simulation of fluid-structure interaction in the scaled Boundary finite element method for prismatic Structures N2 - The Scaled Boundary Finite Element Method (SBFEM) for prismatic structures is an efficient method for the simulation of acoustic behavior. Hence a further development of the method is of great interest. The wave propagation can be calculated for isotropic and anisotropic materials in solids. As for many applications the acoustic behavior in fluids and the behavior in case of fluid-structure interaction (FSI) is subject of research, the implementation of a fluid model in SBFEM for prismatic structures is needed. In case of FSI the coupling between fluid and solid domains can be performed without additional effort when describing both domains in the same variables. Hence a displacement-based fluid description is used. As the discretized formulation leads to spurious modes, a penalty method to suppress the unphysical behavior is chosen. To validate the derived model a comparison with analytical solutions of purely fluid domains is made. As to verify that in case of FSI the model shows the right behavior, dispersion curves of water-filled pipes are calculated and compared to results obtained with Comsol. T2 - 89th GAMM Annual Meeting CY - Munich, Germany DA - 19.03.2018 KW - Scaled Boundary Finite Element Method KW - Fluid-Structure Interaction KW - Penalty Parameter PY - 2018 AN - OPUS4-45260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul T1 - Ultraschallausbreitung in periodischen Strukturen - Simulation und Experiment N2 - Die Untersuchung von Ultraschallausbreitung in periodischen Strukturen ist aktuell von großem Interesse für eine zielgerichtete Beeinflussung der Schallausbreitung. Die bekanntesten Vertreter periodischer Strukturen sind die sogenannten phononischen Kristalle. Als phononischen Kristall bezeichnet man eine periodische Struktur bestehend aus einer Matrix, in die Störungen aus einem zweiten Material eingebracht worden ist. Dabei unterscheiden sich Matrixmaterial und das eingebrachte Material sehr stark in ihren akustischen Eigenschaften. Ein phononischer Kristall erzeugt Bandlücken, in denen die Schalltransmission durch den Kristall vollständig unterbunden ist. Außerhalb der Bandlücken hingegen findet eine ungehinderte Schallausbreitung statt. Diese speziellen Eigenschaften können beispielsweise dazu genutzt werden, frequenzselektive Wellenleiter zu konzipieren oder Schallfelder zu fokussieren. Die Kristallstrukturen können anhand der Anzahl der Dimensionen, in welchen eine Schallausbreitung unterbunden wird, unterteilt werden. So verhindert ein eindimensionaler Kristall nur die Schallausbreitung in eine Raumrichtung, wohingegen ein zwei- oder dreidimensionaler Kristall die Schallausbreitung in mehreren Raumrichtungen unterbindet. Für technische Anwendungen sind aufgrund ihrer einfachen Fertigung insbesondere ein- und zweidimensionale Strukturen von Interesse. In den vorgestellten Arbeiten werden ein- und zweidimensionale Kristalle theoretisch und experimentell untersucht. Für den eindimensionalen Fall wurde eine entartete Form des phonischen Kristalls gewählt, wobei ein Vollzylinder mit periodischer Querschnittsänderung betrachtet wurde. Ziel ist es dabei, die Schallausbreitung in axialer Richtung zu verhindern. Inspiriert wurde diese Anordnung durch die in [1] vorgestellte Tubular-Bell-Geometrie und dient als Vorarbeit für die Entwicklung eines Sensorsystems. Im Falle des zweidimensionalen Kristalls wird die Schallausbreitung in einer Platte mit regelmäßigen Bohrungen untersucht. Hier soll keine Schallausbreitung in der Ebene stattfinden. Als Voruntersuchungen werden zunächst Berechnungen mit Hilfe der Finiten Elementen Methode (FEM) und der Scaled Boundary Finite Element Method (SBFEM) durchgeführt. Für die Berechnung der Dispersionskurven der Strukturen wurde COMSOL Multiphysics genutzt. Die hierbei gewonnenen Erkenntnisse liefern eine Vorhersage der Übertragungseigenschaften der Strukturen. Zur Simulation der Schallausbreitung in der eindimensionalen Struktur wird ein effizienter, achsensymmetrischer Ansatz der SBFEM verwendet. Hierbei entsteht ein numerisches Modell mit einer sehr geringen Anzahl an Freiheitsgraden. Diese effiziente Beschreibung ermöglicht eine zielgerichtete Optimierung der Geometrie der Struktur in Hinblick auf die geforderten akustischen Eigenschaften. Anhand der Simulationsergebnisse werden Testkörper für beide Strukturen gefertigt und deren Übertragungsverhalten im Vergleich mit den numerischen Ergebnissen experimentell überprüft. [1] – Lucklum R., Zubtsov M., Pennec Y. – Tubular Bell – Ein neuartiger Ultraschall-Rohrsensor, 3. Workshop des Fachausschusses der DEGA e.V., Messtechnische Anwendung von Ultraschall 20.06-22.06.2016, Kloster Drübeck T2 - 4. Workshop des Fachausschusses Ultraschall CY - Drübeck - Ilsenburg, Germany DA - 18.06.2018 KW - Phononisch Kristall KW - Sensorentwicklung PY - 2018 AN - OPUS4-45261 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul A1 - Krome, Fabian A1 - Bulling, Jannis A1 - Prager, Jens T1 - Entwicklung eines Ultraschallsensors zur Flüssigkeitsanalyse in Rohrleitungen N2 - Zur Messung von Konzentrationen in Flüssigkeiten können akustische Sensoren genutzt werden. Ziel der vorliegend Arbeit ist es einen Sensor zu entwerfen der sehr hohe Messgenauigkeiten erzielen kann. Der Sensor besteht aus einem rechteckigen Rohr, welches auf einem Halbraum angebracht ist. Die Konzentrationsbestimmung erfolgt anhand des Resonanzverhaltens der Struktur, wodurch eine hohe Messgenauigkeit erreicht werden kann. Um den Sensors zu verwirklichen, muss eine Optimierung der Geometrie mit vielen Iterationsschritten durchlaufen werden. Da keine analytische Beschreibung des akustischen Verhaltens vorliegt, wird eine effiziente Simulationsmethode benötigt. Die Scaled Boundary Finite Element Method (SBFEM) für prismatische Strukturen erscheint für die Simulation geeignet, da Teile der Geometrie ohne neue Vernetzung geändert werden können. Für die Berechnung des Sensors wird ein Modell der akustischen Fluid-Struktur Interaktion benötigt, das bisher nicht vorhanden ist. Die Präsentation behandelt die Implementierung des Fluidmodells in die SBFEM und deren Validierung. Für die Validierung werden die Ergebnisse mit analytischen Beispielen ohne Fluid-Struktur Kopplung und mit Comsol-Ergebnissen der Dispersionskurven mit Wasser gefüllter Rohre verglichen. Schließlich wird das neuartige Verfahren für die Modellierung der Sensorgeometrie angewendet. An einer einfachen Geometrie wird das Sensorprinzip zur Bestimmung der Salzkonzentration demonstriert. T2 - DAGA 2018 - 44. Jahrestagung für Akustik CY - Munich, Germany DA - 19.03.2018 KW - Scaled Boundary Finite Element Method KW - Penalty Parameter KW - Sensorentwicklung PY - 2018 SN - 978-3-939296-13-3 VL - 2018 SP - 1023 EP - 1026 AN - OPUS4-45262 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hofmann, Michael T1 - Multigas Sensor System for Outdoor Odour Nuisance Monitoring N2 - The presentation gives a brief overview of the main goals, the used methods and the first results of the PMARS OdourSense project. In cooperation with the Moulay Ismaïl University in Meknès (Morocco), a multi-gas sensor system for odour nuisance monitoring in outdoor air and a method for testing/calibration of such devices are being developed in this project. T2 - German-Moroccan Workshop on PMARS III CY - Bonn, Germany DA - 20.06.2018 KW - Air-pollution monitoring KW - Multi-gas sensor system KW - Odour KW - Electronic nose KW - Outdoor odour control PY - 2018 AN - OPUS4-45266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scala-Benuzzi, M. L. A1 - Takara, E. A. A1 - Alderete, M. A1 - Soler-Illia, G. J. A. A. A1 - Schneider, Rudolf A1 - Raba, J. A1 - Messina, G. A. T1 - Ethinylestradiol quantification in drinking water sources using a fluorescent paper based immunosensor N2 - In this work we report a novel paper-based analytical device read-out via LED-induced fluorescence detection (FPAD) for the quantification of the emerging pollutant ethinylestradiol (EE2) in river water samples. The PAD was used as a reaction platform for a competitive enzyme immunoassay. For the PAD development, microzones of filter paper, printed by a wax printing method, were modified with amino-functionalized SBA-15 and subsequently, anti-EE2 specific antibodies were covalently immobilized. The determination of EE2 in water was carried out by adding a fixed concentration of EE2 conjugated with the enzyme horseradish peroxidase (HRP) to samples and standards. Then, the FPAD were added and incubated for 10 min. Finally, the detection was performed by the reaction of 10-acetyl-3,7-dihydroxyphenoxazine (ADHP) whose oxidation is catalyzed by HRP in the presence of H2O2, obtaining the highly fluorescent resorufin (R). Resorufin was detected by LED excitation at 550 nm, observing emission at 585 nm. The EE2 concentration in the samples was inversely proportional to the relative fluorescence obtained from the enzymatic reaction products. The FPAD assay showed a detection Limit (LOD) of 0.05 ng L−1 and coefficients of variation (CV) below 4.5% within-assay and below 6.5% between-assay, respectively. The results obtained show the potential suitability of our FPAD for the selective and sensitive quantification of EE2 in river water samples. In addition, it has the PADs advantages of being disposable, easy to apply and inexpensive. KW - Immunoassay KW - Arzneimittel KW - Antikörper KW - LED-induzierte Fluoreszenz KW - Paper based devices KW - Mesoporöses Silica KW - Partikel PY - 2018 DO - https://doi.org/10.1016/j.microc.2018.05.038 SN - 0026-265X VL - 141 SP - 287 EP - 293 PB - Elsevier B.V. CY - Amsterdam, NL AN - OPUS4-45269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - HR-MS non-target analysis for transformation products of emerging organic contaminants in waste water fractions pre-screened by ELISA N2 - The talk introduces the technique of LC-ELISA: fractionating pre-concentrated water samples, analyzing them for containing compounds that bind to hapten-selective antibodies followed by high-Resolution mass spectrometry non-target analysis of "positive" fractions for Transformation products of emerging organic contaminants. T2 - SETAC 2018 CY - Rom, Italy DA - 13.05.2018 KW - Umweltschadstoffe KW - LC-ELISA KW - Hochauflösende Massenspektrometrie KW - LC-MS/MS PY - 2018 AN - OPUS4-45270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yuan, Huan A1 - Gornushkin, Igor B. A1 - Gojani, Ardian A1 - Wang, X. H. A1 - Rong, Ming Zhe T1 - Laser-induced plasma imaging for low-pressure detection N2 - A novel technique based on laser induced plasma imaging is proposed to measure residual pressure in sealed containers with transparent walls, e.g. high voltage vacuum interrupter in this paper. The images of plasma plumes induced on a copper target at pressure of ambient air between 10−2Pa and 105Pa were acquired at delay times of 200ns, 400ns, 600ns and 800ns. All the plasma images at specific pressures and delay times showed a good repeatability. It was found that ambient gas pressure significantly affects plasma shape, plasma integral intensities and expansion dynamics. A subsection characteristic method was proposed to extract pressure values from plasma images. The method employed three metrics for identification of high, intermediate and low pressures: the distance between the target and plume center, the integral intensity of the plume, and the lateral size of the plume, correspondingly. The accuracy of the method was estimated to be within 15% of nominal values in the entire pressure range between 10−2Pa and 105Pa. The pressure values can be easily extracted from plasma images in the whole pressure range, thus making laser induced plasma imaging a promising technique for gauge-free pressure detection. KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2018 DO - https://doi.org/10.1364/OE.26.015962 SN - 1094-4087 VL - 26 IS - 12 SP - 15962 EP - 15971 PB - Optical Society of America under the terms of the OSA Open Access Publishing Agreement AN - OPUS4-45219 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hakim, I. A1 - Schumacher, David A1 - Sundar, V. A1 - Donaldson, S. A1 - Creuz, A. A1 - Schneider, R. A1 - Keller, J. A1 - Browning, C. A1 - May, D. A1 - Abo Ras, M. A1 - Meyendorf, N. ED - Chimenti, D. E. ED - Bond, L. J. T1 - Volume imaging NDE and serial sectioning of carbon fiber composites N2 - A composite material is a combination of two or more materials with very different mechanical, thermal and electrical properties. The various forms of composite materials, due to their high material properties, are widely used as structural materials in the aviation, space, marine, automobile, and sports industries. However, some defects like voids, delamination, or inhomogeneous fiber distribution that form during the fabricating processes of composites can seriously affect the mechanical properties of the composite material. In this study, several imaging NDE techniques such as: thermography, high frequency eddy current, ultrasonic, x-ray radiography, x-ray laminography, and high resolution x-ray CT were conducted to characterize the microstructure of carbon fiber composites. Then, a 3D analysis was implemented by the destructive technique of serial sectioning for the same sample tested by the NDE methods. To better analyze the results of this work and extract a clear volume image for all features and defects contained in the composite material, an intensive comparison was conducted among hundreds of 3D-NDE and multi serial sections’ scan images showing the microstructure variation. T2 - 44TH ANNUAL REVIEW OF PROGRESS IN QUANTITATIVE NONDESTRUCTIVE EVALUATION CY - Provo, Utah, USA DA - 16.07.2017 KW - Carbon fiber reinforced polymers KW - Non-destructive testing KW - Thermography KW - Eddy current KW - Ultrasound KW - X-ray radiography KW - X-ray laminography KW - X-ray computed tomography KW - Serial sectioning PY - 2018 DO - https://doi.org/10.1063/1.5031590 VL - 1949 SP - 120003-1 EP - 120003-10 PB - AIP Publishing AN - OPUS4-45173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Boehm, Rainer A1 - Heckel, Thomas ED - Bond, Leonard T1 - Simulation of Sparse Matrix Array Designs N2 - Matrix phased array probes are becoming more prominently used in industrial applications. The main drawbacks, using probes incorporating a very large number of transducer elements, are needed for an appropriate cabling and an ultrasonic device offering many parallel channels. Matrix arrays designed for extended functionality feature at least 64 or more elements. Typical arrangements are square matrices, e.g., 8 by 8 or 11 by 11 or rectangular matrixes, e.g., 8 by 16 or 10 by 12 to fit a 128-channel phased array system. In some phased array systems, the number of simultaneous active elements is limited to a certain number, e.g., 32 or 64. Those setups do not allow running the probe with all elements active, which may cause a significant change in the directivity pattern of the resulting sound beam. When only a subset of elements can be used during a single acquisition, different strategies may be applied to collect enough data for rebuilding the missing information from the echo signal. Omission of certain elements may be one approach, overlay of subsequent shots with different active areas may be another one. This paper presents the influence of a decreased number of active elements on the sound field and their distribution on the array. Solutions using subsets with different element activity patterns on matrix arrays and their advantages and disadvantages concerning the sound field are evaluated using semi-analytical simulation tools. Sound field criteria are discussed, which are significant for non-destructive testing results and for the system setup. T2 - QNDE 2017 CY - Utah, USA DA - 16.07.2017 KW - Imaging KW - Phased Array KW - Sparse Array KW - Matrix Array PY - 2018 DO - https://doi.org/10.1063/1.5031560 SP - 1949 EP - 1958 PB - AiP CY - Melville, NY 11747 - 4300, USA AN - OPUS4-45175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya T1 - Multimodal cleavable reporters for the optical quantification of functional groups on nano- and microparticles N2 - Polymer nanoparticles (NPs) are of increasing importance for a wide range of applications in the material and life sciences. This includes their application as carriers for e.g., analyte-responsive ligands for DNA sequencing platforms, drugs as well as dye molecules for use as multichromophoric reporters for signal enhancement in optical assays or the fabrication of nanosensors and targeted probes in bioimaging studies. All these applications require surface functionalization of the particles with e.g., ligands, sensor dyes, or analyte recognition moieties like biomolecules, and subsequently, the knowledge of the chemical nature and total number of surface groups as well as the number of groups accessible for coupling reactions. Particularly attractive for the latter are optically active reporters together with sensitive and fast optical assays, which can be read out with simple, inexpensive instrumentation. We assessed a variety of conventional and newly developed colorimetric and fluorometric labels for optical surface group analysis, utilizing e.g., changes in intensity and/or color for signal generation. Moreover, novel cleavable and multimodal reporters were developed which consist of a reactive group, a cleavable linker, and an optically active moiety, chosen to contain also heteroatoms for straightforward method validation by elemental analysis, ICP-OES, ICP-MS or NMR. In contrast to conventional labels measured bound at the particle surface, which can favor signal distortions by scattering and encoding dyes, cleavable reporters can be detected colorimetrically or fluorometrically both attached at the particle surface and after quantitative cleavage of the linker in the transparent supernatant after particle removal e.g., by centrifugation. Here, we present first results obtained for the optical quantification of carboxylic and amino groups on a series of self-made polystyrene NPs with different types of labels and compare their potential and drawbacks for surface group analysis. T2 - NanoWorkshop 2018 CY - Berlin, Germany DA - 14.05.2018 KW - Optical assays KW - Cleavable probes KW - Conventional dyes KW - Nanoparticles PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-45177 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Simple and Validated Methods for Quantifying Functional Groups, Ligands, and Biomolecules on Nanomaterials N2 - Many applications of nanomaterials in the life sciences require the controlled functionalization of these materials with ligands like polyethylene glycol (PEG) and/or biomolecules such as peptides, proteins, and DNA. This enables to tune their hydrophilicity and biocompatibility, minimize unspecific interactions, improve biofunctionalization efficiencies, and enhance blood circulation times. Moreover, it is the ultimate prerequisite for their use as reporters in assays or the design of targeted optial probes for bioimaging. At the core of these functionalization strategies are reliable and validated methods for surface group and ligand quantification that can be preferably performed with routine laboratory instrumentation, require only small amounts of substances, and are suitable for many different types of nanomaterials. We present here versatile and simple concepts for the quantification of common functional groups, ligands, and biomolecules on different types of organic and inorganic nano-materials, using different types of optical reporters and method validation with the aid of multimodal reporters, method comparisons, and mass balances. T2 - NanoWorkshop 2018 CY - Berlin, Germany DA - 14.05.2018 KW - Surface functionalization KW - Nanoparticles KW - Surface chemistry KW - Multimodal reporters PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-45179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement of nanoparticle size and shape distribution – Current situation and outlook N2 - The EC Recommendation on the definition of nanomaterial, based solely on size of the constituent particles, foresees development of harmonised measurement methods ensuring ‘consistent results across materials and over time’. The EU/FP7 research project NanoDefine has been exclusively dedicated to support the implementation of this EC Recommendation for the European Union’s legislation. For the first time, measurement techniques able to determine the size of nanoparticles have been evaluated systematically on a well-defined set of quality control materials (spherical, monodisperse) as well as industrial materials of complex shapes and considerable polydispersity. Particularly based on the analytical performance of the measurement techniques as tested on the challenging real-world particulate materials, it was possible to formulate recommendations for use of a new tiered approach consisting of screening and confirmatory techniques. Thus, a consistent framework of guidance for nanomaterial identification according to the EC Definition has been issued in form of the NanoDefiner e-tool, with a transparent decision flow scheme and an extensive user manual. Selected examples of analysis and classification as nano-/non-nanomaterials will be given, highlighting the limits of applicability of the available measurement techniques in dependence on sample properties. On some recent relevant developments in sample preparation – as a crucial part for an accurate analysis - will be also reported. Further, ISO/TC 229 ‘Nanotechnologies’ activities aiming at establishing accurate TEM and SEM measurement of NP size and shape as robust, traceable, standard procedures are highlighted. With participation of BAM, study groups have been organizing inter-laboratory comparisons on well-selected NP systems according to the market needs, such as aggregated or shape-controlled titania nano-powder for which size and shape distribution of primary particles must be measured accurately. T2 - Symposium Preparation, Characterization and Processing of Nano and Submicron Powders CY - Berlin, Germany DA - 14.06.2018 KW - Nanoparticles KW - Nanomaterial KW - EC definition KW - Nanoparticle size distribution PY - 2018 AN - OPUS4-45191 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Wandel der Prozessanalytik vom Exot zur Informationsquelle der digitalisierten Automation N2 - Die ehemals wegen komplexer Technik und vergleichsweise hohen Wartungskosten beim Anwender ungeliebte Prozessanalysentechnik (PAT) erfährt sich mittlerweile immer mehr als etablierender Bereich mit einem großen Zuwachs und Dynamik. Die Prozesskontrolle und -steuerung über physikalische Kenngrößen wie Druck und Temperatur lässt eine weitere Optimierung der Anlagen kaum mehr zu. Nur mittels stoffspezifischer Analysen lassen sich Rohstoffschwankungen, Ausbeuten und Energieeinsatz konsequent optimieren. Der systematische Einsatz der Prozessanalysentechnik verändert Prozesse und Produktionsumgebungen und hat damit die Chance, Kernstück dezentral automatisierter Produktionseinheiten zu werden. Ein neuer Arbeitskreis der NAMUR AK 3.7 „Smarte Sensorik, Aktorik und Kommunikation“ wird diesem verstärkt Rechnung tragen. Es werden reale Anwendungsbeispiele aufgezeigt, die eine schnelle Amortisation von PAT im Prozess untermauern. T2 - ACHEMA 2018 - AUTOMATION IM DIALOG CY - Frankfurt a. M., Germany DA - 11.06.2018 KW - Prozessanalytik KW - Automation KW - Industrie 4.0 KW - Prozessanalysentechnik KW - NAMUR KW - ZVEI PY - 2018 AN - OPUS4-45193 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lauer, Franziska T1 - Multivariate analysis of MALDI imaging mass spectrometry data of mixtures of single pollen grains N2 - Here, we present an advanced approach to identify pollen grains in mixtures based on: - a simplified sample preparation procedure - MALDI imaging mass spectrometry - chemometric tools Our goals are to: - explore the biomolecular variations in pollen - determine species-specific peak patterns - discriminate and identify single pollen grains in mixtures using MSI T2 - 66th Conference on Mass Spectrometry and Allied Topics CY - San Diego, CA, USA DA - 03.06.2018 KW - Pollen PY - 2018 AN - OPUS4-45196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas T1 - Process monitoring with online NMR spectroscopy – An enabler for “Industrie 4.0” in process industry N2 - Improvement in deep process understanding is a mandatory prerequisite for the application of modern concepts like Industrial Internet of Things (IIoT) or “Industrie 4.0”. This is particularly relevant in new process concepts such as intensified production in modularized plants. The direct hyphenation with online methods of process analytical technology (PAT) allows profound insights into the actual reactions within chemical and pharmaceutical production steps and provides necessary information for associated control strategies. While the industrial application of online Raman spectroscopy has already been successfully demonstrated, low-field NMR spectroscopy is not yet adequately developed as an online method for use in process industry. The high information content combined with the low calibration effort makes NMR spectroscopy a highly promising method for modern process automation with a high flexibility due to short set-up times and low requirements regarding validation. This is a major advantage especially within multi-purpose production plants, as well as for processes suffering from fluctuating quality of raw materials. NMR spectroscopy has a high potential for direct quantitative information, while cutting the calibration and validation needs to a minimum and thus exhibiting short set-up times. Within the EU project CONSENS, an NMR analyzer for direct implementation in an industrial process environment was developed based on a commercially available laboratory instrument. The challenge was not only the hyphenation to the production plant itself, but also to fulfill all requirements of chemical industry, e.g., explosion safety regulations (ATEX), robust automation and modern, as well as classical communication interfaces. The presented NMR module involves a compact spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction), and evaluation. The module transforms the acquired online spectra of various technically relevant reactions to either conventional 4‒20 mA signals as well as WiFi based OPC-UA communication protocols. The concept was evaluated on two processes of pharmaceutical and chemical industry. As the first example the continuous synthesis of 2-nitrodiphenylamine starting from aniline and o-fluoronitrobenzene, activated by an organometallic lithium reagent, was studied. This application is highly demanding for a reliable automated evaluation of the obtained NMR spectra, which was realized by developing a physically motivated model-based approach. In the second example, a stage of the synthesis of the industrially important solvent tetrahydrofurane consisting of the catalytic hydrogenation of 2-butine-1,4-diol was monitored. This reaction is proceeding via an intermediate product and suffers from competitive reaction paths. In this application different spectroscopic methods were combined with the data obtained from classical process sensors, e.g., pressure, temperature and flow transducers for the development of innovative control concepts. T2 - ACHEMA CY - Frankfurt/M., Germany DA - 11.06.2018 KW - Nuclear magnetic resonance KW - Process monitoring KW - Process industry KW - Low field nmr KW - Industrie 4.0 PY - 2018 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-45197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Isleyen, A. T1 - A joint research project for the sustainable production of certified matrix reference materials for environmental analysis N2 - This project aims to develop capacity to produce certified reference materials (CRMs) for environmental analysis by transferring know-how between the partners and combining their skills to focus on environmental CRM production. The production process includes good manufacturing practices for processing materials, method development, the validation and application of homogeneity, stability and characterisation tests, the calculation of individual uncertainties (between-unit inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. An inter laboratory comparison registered as a EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills. T2 - BERM-14 CY - National Harbor, Maryland, USA DA - 11.10.2015 KW - Reference material KW - Priority pollutants KW - Toxic metals KW - PFOS KW - PFOA PY - 2015 AN - OPUS4-45251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Isleyen, A. T1 - Matrix reference materials for environmental analysis N2 - This project aims to develop capacity to produce certified reference materials (CRMs) for environmental analysis by transferring know-how between the partners and combining their skills to focus on environmental CRM production. The production process includes good manufacturing practices for processing materials, method development, the validation and application of homogeneity, stability and characterisation tests, the calculation of individual uncertainties (between-unit inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. An inter laboratory comparison registered as a EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills. T2 - 9th International Conference on Instrumental Methods of Analysis: Modern Trends and Applications CY - Kalamata, Greece DA - 20.09.2015 KW - Priority substances KW - Toxic metals KW - PFOS KW - PFA PY - 2015 AN - OPUS4-45252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Isleyen, A. T1 - Three candidate certified reference materials for environmental analysis N2 - This project aims to develop capacity to produce certified reference materials (CRMs) for environmental analysis by transferring know-how between the partners and combining their skills to focus on environmental CRM production. The production process includes good manufacturing practices for processing materials, method development, the validation and application of homogeneity, stability and characterisation tests, the calculation of individual uncertainties (between-unit inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. An inter laboratory comparison registered as a EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills. T2 - 10th International Conference on Instrumental Methods of Analysis CY - Heraklion, Greece DA - 17.09.2017 KW - Certified reference materials KW - Toxic metals KW - PFOS KW - PFOA PY - 2017 AN - OPUS4-45253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Näykki, Teemu T1 - A joint research project for the sustainable production of certified matrix reference materials for environmental analysis N2 - This project aims to develop capacity to produce certified reference materials (CRMs) for environmental analysis by transferring know-how between the partners and combining their skills to focus on environmental CRM production. The production process includes good manufacturing practices for processing materials, method development, the validation and application of homogeneity, stability and characterisation tests, the calculation of individual uncertainties (between-unit inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. An inter laboratory comparison registered as a EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills. T2 - EcoBalt 2016 CY - Tartu, Estonia DA - 09.10.2016 KW - Certified reference material KW - Toxic metals KW - PFOS KW - PFOA PY - 2016 AN - OPUS4-45254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Isleyen, A. T1 - Joint research project for the production of certified matrix reference materials for environmental analysis N2 - Reliable analysis of chemical indicators in water, sediment and soil samples for the purpose of environmental pollution assessment poses one of the greatest analytical challenges, having in mind the complexity of sample matrix and low concentrations of pollutants. Organics (pesticides, PAHs, PFOS, etc.) and heavy metals (Hg, Cd, Ni, Pb and As) represent target parameters. Laboratories performing sampling and tests in this field regulated by respective EU directives, need strong support in order to establish a quality system. It is necessary to provide appropriate calibrators i.e. matrix CRMs relates to the unique sample matrices representing typical samples in the geomorphological and anthropological sense. In addition to that, bearing in mind the complexity and instability of environmental samples, it is very difficult to obtain appropriate referents materials with no local providers. Our project is aiming to develop capacity to produce CRMs for environmental analysis by transferring the theoretical and practical know-how between the partners and combining their skills to focus on environmental CRM production in accordance with ISO Guide 34. Our project will have an impact on environmental monitoring in the partnering countries and on the scientific community, who will use the newly developed reference materials. Furthermore, partners will develop strategies for producing new CRMs either on their own or in cooperation. This will lead to regional CRM producers serving scientific and official laboratories. T2 - 2nd International Congress of Chemists and Chemical Engineers of B&H CY - Sarajevo, Bosnia and Herzegovina DA - 21.10.2016 KW - CRM KW - Environmental analysis KW - CRM producer KW - Quality system PY - 2016 AN - OPUS4-45257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Kotschate, Daniel T1 - New technologies for air-coupled ultrasonic transducers N2 - Air-coupled ultrasonic testing (ACUT) has experienced rapid growth within the last years. It is especially well suited to inspection of lightweight structures consisting of composite materials and adhesive joints. Uniform coupling and easy maintenance are its advantages compared to contact technique. However, the impedance mismatch between the transducer and air poses a major challenge to the development of ACUT transducers. Commercially available air-coupled transducers consist of a piezocomposite material and matching layers. Their fabrication is difficult in handling and their signal-to-noise ratio sometimes not sufficient for various testing requirements. However, there are several innovative approaches using other materials and other physical principles to transmit and receive an ultrasonic pulse. We present a review of the latest advances in research on air-coupled transducers for non-destructive testing, including previously unpublished results. We recognize two major directions as most promising: ferroelectrets and thermoacoustic transducers. Ferroelectrets are charged cellular polymers exhibiting piezoelectric properties. Their small acoustic impedance is matched to air better than matching layers applied in conventional air-coupled transducers. Applying bias voltage to a ferroelectret receiver is the latest development in this field, which increased the received signal by 12 to 15 dB. Thermoacoustic transducers use heat to initiate an ultrasonic wave, acting as transmitters. The working principle is known from nature as thunder and lightning: thermal energy of an electrically heated material, which can also be air, is converted into acoustic energy. Some thermoacoustic transmitters consist of a conductive layer with a thickness in the nanometer range deposited on a solid substrate. Another possibility is to use an electric spark. For the first time, measurements of the sound field of an electric spark up to 500 kHz were performed. Thermoacoustic transducers enable excitation of extremely broadband pulses while producing high pressure levels, which opens new possibilities for advanced signal processing. T2 - 12th European conference on Non-Destructive Testing CY - Gothenburg, Sweden DA - 11.06.2018 KW - Air-coupled ultrasonic testing KW - Atmospheric pressure plasma KW - Cellular polypropylene KW - Ferroelectret KW - Transducer PY - 2018 SP - ECNDT-0608-2018, 1 EP - 9 AN - OPUS4-45209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grager, J.-C. A1 - Kotschate, Daniel A1 - Gamper, J. A1 - Gaal, Mate A1 - Pinkert, K. A1 - Mooshofer, H. A1 - Goldammer, M. A1 - Grosse, C. U. T1 - Advances in air-coupled ultrasonic testing combining an optical microphone with novel transmitter concepts N2 - Air-coupled ultrasound (ACU) is increasingly used for automated and contactless inspection of large-scale composite structures as well as for non-destructive testing (NDT) of water-sensitive or porous materials. The major challenge to overcome using ACU in NDT is the enormous loss of ultrasonic energy at each solid-air interface caused by the high acoustic impedance mismatch. Resonant low-frequency piezoceramic transducers are specially designed to achieve high sound pressure levels. For an expanded use of this technique, however, the spatial resolution needs to be increased. Recent studies of our collaborative research group demonstrated the successful application of a resonance-free, highly sensitive receiver that uses a Fabry-Pérot etalon instead of piezoceramic materials or membranes. However, to reach the full potential of this broadband small-aperture optical microphone, novel transmitter concepts have to be developed and evaluated for advanced NDT applications. Different types of transmitter were tested in combination with the optical microphone acting as receiver and they were compared to conventional piezoceramic transducers in through-transmission mode. Monolithic carbon fiber-reinforced plastics (CFRP) and CFRP sandwich structures containing different defect types were inspected. Presented results are processed as C-scan images and further evaluated for spatial resolution, signal-to-noise ratio and sensitivity of each measurement setup. Novel transmitter concepts, such as ferroelectret and thermoacoustic emitters, show promising findings with a considerably improved time and spatial resolution for ACU-NDT. T2 - 12th European conference on Non-Destructive Testing CY - Gothenburg, Sweden DA - 11.06.2018 KW - Air-coupled ultrasonic testing KW - Optical microphone KW - Thermoacoustic KW - Cellular polypropylene KW - Ferroelectret KW - Transducer PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-452114 SP - ECNDT-0166-2018, 1 EP - 10 AN - OPUS4-45211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nöller, Renate T1 - Cinnabar reviewed: characterization of the red pigment and its reactions N2 - In the majority of cases, the red color of cinnabar on objects of cultural heritage is well preserved, though turning black is often claimed and has been the subject of investigations. To evaluate conditions for the stability of the pigment and understand the reactions, in this paper the problem is approached from various viewpoints. First of all the natural form cinnabarite is compared with the artificially prepared pigment vermilion. This establishes a differentiation of types in terms of quality, depending on structural impurities. With regard to the pigment’s reactions influencing the discoloration, the most commonly mentioned environmental factors, such as radiation or halogens, are evaluated. In relation to various usages, the pigment’s structural stability is then viewed in connection with adjacent pigments, glues, and the substrate, which may lead to a brown or black coloration or even the release of mercury, whereas the color is preserved in most cases when used on lime or in ink and lacquer. Due to the materials’ properties, attention is drawn to the fact that discoloration to a brownish-black is not necessarily a sign of damage and harmful reaction products, but may indicate good preservation of the painted material, provided that the mercury can be bound in the substrate. KW - Preservation KW - Cinnabar KW - Vermilion KW - Differentiation of cinnabar KW - Impurities KW - Color change KW - Photosensitivity KW - Halogens PY - 2014 DO - https://doi.org/10.1179/2047058413Y.0000000089 VL - 60 IS - 2 SP - 79 EP - 87 PB - Taylor & Francis CY - UK AN - OPUS4-44786 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - Chemical Analysis of Core-Shell Nanoparticles using ToF-SIMS and XPS N2 - The analysis of nanomaterials is current an important task - especially in case of risk assessment, as the properties of these material class are not well understood currently. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surfaces chemical composition has to be investigated to get a better understanding and prediction of the nanomaterials' behavior. ToF-SIMS has proven as a powerful tool to determine said chemical composition. Its superior surface sensitivity allows us to study mainly the utmost atomic layer and therefore gives us an idea of the interactions involved. Here, we show first result from the validation of the method for the analysis of polystyrene and gold nanoparticles. ToF-SIMS will be compared to other methods like XPS, T-SEM or REM. Furthermore, principle component analysis (PCA) will be used to detect the influence of different sample preparation performed by an innovative microfluidic device. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - DPG-Frühjahrstagung der Sektion Kondensierte Materie gemeinsam mit der EPS CY - Berlin, Germany DA - 11.03.2018 KW - XPS KW - ToF-SIMS KW - Nanoparticles PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-44790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Investigation of core-shell nanoparticles using scanning transmission x-ray microscopy (STXM) N2 - A scanning transmission x-ray microscopy (STXM) based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core-shell nanoparticles which exhibit a strong x-ray absorption contrast and a well-defined interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less x-ray beam induced damage of the sample is achieved by recording STXM images only at two predetermined energies of maximum absorption contrast, instead of recording a stack of images across the whole absorption edge. A model core-shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, is used for demonstration. Near edge x-ray absorption fine structure (NEXAFS) spectroscopy confirms the significant difference in x-ray absorption behavior between PTFE and PS. Additionally, due to the insolubility of styrene in PTFE a well-defined interface between particle core and shell is expected. In order to validate the STXM results, both the naked PTFE cores as well as the complete core-shell nanoparticles are examined by scanning electron microscopy (SEM). The introduced STXM based methodology yields particle dimensions in good agreement with the SEM results (deviation equal or less than 10%) and provides additional information such as the position of the particle core which cannot be extracted from a SEM micrograph. T2 - DPG-Frühjahrstagung der Sektion Kondensierte Materie gemeinsam mit der EPS CY - Berlin, Germany DA - 11.03.2018 KW - STXM KW - SEM KW - PS KW - PTFE KW - Core-shell nanoparticles PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-44654 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Codawelleninterferometrie zur Detektion von Spannungszuständen in Betonbauteilen N2 - Informationen zu in Betonbauteilen stattfindenden Umlagerungsprozessen sowie Druckspannungsverteilungen können mit konventioneller Messtechnik bislang nicht zweifelsfrei beantwortet werden. Ultraschallmessungen mit eingebetteten Sensoren könnten hier eine sinnvolle Ergänzung zur konventionellen Messtechnik sein. Durch Einsatz der Codawelleninterferometrie (CWI) sind hiermit schon sehr kleine Änderungen im Material detektierbar. Um diese neue Methodik zu evaluieren, wurde das Forschungsprojekt „Querkrafttragfähigkeit von Spannbetonbrücken – Erfassung von Spannungszuständen in den Spannbetonversuchsträgern mit Ultraschallsensoren“ durch die Bundesanstalt für Straßenwesen (BASt) initiiert. In diesem Projekt wurden durch die Bundesanstalt für Materialforschung und –prüfung (BAM) Ultraschall-Transducer in mehrere Spannbetonträger des Instituts für Massivbau der RWTH Aachen eingebettet, die anschließend bis zum Bruch belastet wurden. Der Belastungsversuch an einem der Spannbetondurchlaufträger zeigte das große Potential dieser Methodik. Die im Netzwerk erfassten Änderungen der Ultraschallwellengeschwindigkeit geben die Spannungsverhältnisse im Längsschnitt des Trägers schon bei sehr niedrigen Belastungen qualitativ richtig wieder und zeigen bei hohen Belastungen eine gute Korrelation zum Rissbild. Dabei weisen räumliche Anomalien und Änderungen in der Charakteristik der Geschwindigkeitsänderungen oft schon auf Rissbildung hin, wenn diese noch nicht an der Oberfläche sichtbar ist. Dies zeigt das Potential im Hinblick auf eine Frühwarnung. Hierfür und ebenso in Bezug auf eine Quantifizierung der Effekte ist aber noch Entwicklungsarbeit notwendig. Ein Vorteil der Methodik ist, dass die Transducer nicht direkt am Ort der Änderung platziert werden müssen und einen relativ großen Bereich um die Transducer herum erfassen. T2 - DGZfP Jahrestagung CY - Leipzig, Germany DA - 07.05.2018 KW - Ultraschall KW - Monitoring KW - Codawelleninterferometrie KW - Brückenträger PY - 2018 AN - OPUS4-44863 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya T1 - Multimodal cleavable reporters for the optical quantification of functional groups on nano- and microparticles N2 - Nano- and microparticles are of increasing importance for a wide range of applications in the material and life sciences. Examples are their use as carriers for dye molecules and drugs, multichromophoric reporters for signal enhancement strategies in optical assays, targeted probes for bioimaging, and biosensors. All these applications require surface functionalization of the particles with e.g., ligands (to tune the dispersibility and prevent unspecific interactions), crosslinkers, sensor dyes, or analyte recognition moieties like biomolecules, and subsequently, the knowledge of the chemical nature and total number of surface groups as well as the number of groups accessible for coupling reactions. Particularly attractive for the latter are sensitive and fast photometric or fluorometric assays, which can be read out with simple, inexpensive instrumentation. Here, we present a novel family of cleavable photometric and multimodal reporters for the quantification of conjugatable amino and carboxyl surface groups on nano- and microparticles. These probes allow for the determination of particle-bound labels, unbound reporters in the supernatant, and reporters cleaved off from the particle surface as well as the remaining thiol groups on the particles by photometry and inductively coupled optical emission spectrometry (32S ICP-OES).3 Comparison of the performance of these cleavable reporters with conventional labels, utilizing changes in intensity and/or colour of absorption and/or emission, underlines the analytical potential of this versatile concept which elegantly circumvents signal distortions by light scattering and encoding dyes, and enables straightforward validation by method comparison. T2 - INNANOPART Open day CY - London, UK DA - 24.04.2018 KW - Nanoparticle KW - Surface groups KW - Cleavable reporter PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-44828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moser, Marko A1 - Nirmalananthan-Budau, Nithiya A1 - Behnke, Thomas A1 - Geißler, Daniel A1 - Resch-Genger, Ute T1 - Multimodal cleavable reporters versus conventional labels for optical quantification of accessible amino and carboxy groups on nano- and microparticles N2 - Many applications of nanometer- and micrometer-sized particles include their surface functionalization with linkers, sensor molecules, and analyte recognition moieties like (bio)ligands. This requires knowledge of the chemical nature and number of surface groups accessible for subsequent coupling reactions. Particularly attractive for the quantification of these groups are spectrophotometric and fluorometric assays, which can be read out with simple instrumentation. In this respect, we present here a novel Family of cleavable spectrophotometric and multimodal reporters for conjugatable amino and carboxyl surface groups on nano- and microparticles. This allows determination of particle-bound labels, unbound reporters in the supernatant, and reporters cleaved off from the particle surface, as well as the remaining thiol groups on particle, by spectrophotometry and inductively coupled optical emission spectrometry (32S ICP-OES). Comparison of the performance of these cleavable reporters with conductometry and conventional labels, utilizing changes in intensity or Color of absorption or emission, underlines the analytical potential of this versatile concept which elegantly circumvents Signal distortions by scattering and Encoding dyes and enables straightforward validation by method comparison. KW - Polymer particles KW - Cleavable reporter KW - Optical quantification KW - Validation PY - 2018 DO - https://doi.org/10.1021/acs.analchem.8b00666 SN - 1520-6882 SN - 0003-2700 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. VL - 90 IS - 9 SP - 5887 EP - 5895 PB - ACS Publ. CY - Washington, DC AN - OPUS4-44830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen T1 - Cyclic polylactides via ring-expansion polymerization N2 - We will report on a new kind of ring-expansion polymerization (REP) of cyclic esters based of three classes of catalysts. In contrast to REP described previously these new polymerizations are characterized by a self-extrusion of the catalysts resulting in cyclic homopolyesters as the only reaction product. These REP of L-lactide were performed in bulk at temperatures between 100 and 180°C without racemization. A simplified scheme of a REP catalyzed by BuCa or SnBi is presented below. With meso-lactide temperatures down to 60°C were realized. Depending on catalyst, time and temperature with equal quantities of even and odd-numbered cycles a strong predominance of either even or odd-numbered cycles was found. T2 - 255th ACS National Meeting CY - New Orleans, LA, USA DA - 18.03.2018 KW - MALDI-TOF MS KW - Poly(lactide) KW - Polymerisation KW - Catalysts PY - 2018 AN - OPUS4-44833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geißler, Daniel T1 - Synthesis of polymeric nanobeads with different surface group densities and their charaterization using multimodal cleavable reporters and lanthanide tags N2 - Polymeric nanoparticles (NP) are of increasing importance for a wide range of applications in the material and life sciences, including their use as drug carriers, fluorescent sensors and multimodal reporters in a large variety of bioassays and bioimaging studies. Application-relevant properties of NP include their size (and size distribution), shape, optical properties, and ease of subsequent functionalization, e.g. with linkers, sensor molecules, and bioligands. In this respect, knowledge of the chemical nature, the total number of surface groups and the number of groups accessible for subsequent coupling reactions is mandatory.1 Commercially available polystyrene NP often contain different additives like stabilizers, radical starters and crosslinkers, which can influence the quantification of surface functionalities. Moreover, they often have unknown surface group densities that may vary from batch to batch, which complicates or even hampers their reliable use in many (bio)applications. To circumvent these issues, we synthesized amino- and carboxy-functionalized, monodisperse 100 nm polystyrene NP with three different, well-defined surface group densities. Using a recently developed approach for the quantification of functional groups on nano- and microparticles with cleavable reporters,2 we quantified the assessible functional groups on the self-synthesised PS particles via optical spectroscopy (photometry) and inductively coupled optical emission spectrometry (32S ICP-OES). In addition, we developed a fluorimetric approach for the quantification of surface functional groups on nanoparticles based on the labelling with luminescent lanthanide complexes (LLC). In contrast to common organic dyes, LLC are not prone to photo¬luminescence quenching arising from reabsorption or dye aggregation, and thus, enable a reliable fluorometric quantification of the assessible functional groups on NP surfaces. Moreover, lanthanide tags can be detected with high specificity and sensitivity with analytical techniques such as XPS and ICP-MS, which allow for the multimodal validation of the fluorometric quantification approach. T2 - RSC-NPL Symposium "Nanoparticle concentration – critical needs and state-of-the-art measurement" and EMPIR 14IND12 Innanopart Open Day CY - London, UK DA - 24.05.2018 KW - Nanoparticle KW - Functional group KW - Quantification PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-44836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jin, Z. A1 - Geißler, Daniel A1 - Qiu, X. A1 - Wegner, Karl David A1 - Hildebrandt, N. T1 - A rapid, amplification-free, and sensitive diagnostic assay for single-step multiplexed fluorescence detection of microRNA N2 - The importance of microRNA (miRNA) dysregulation for the development and progression of diseases and the discovery of stable miRNAs in peripheral blood have made these short-sequence nucleic acids next-generation biomarkers. Here we present a fully homogeneous multiplexed miRNA FRET assay that combines careful biophotonic design with various RNA hybridization and ligation steps. The single-step, single-temperature, and amplification-free assay provides a unique combination of performance parameters compared to state-of-the-art miRNA detection technologies. Precise multiplexed quantification of miRNA-20a, -20b, and -21 at concentrations between 0.05 and 0.5 nm in a single 150 mL sample and detection limits between 0.2 and 0.9 nm in 7.5 mL serum samples demonstrate the feasibility of both highthroughput and point-of-care clinical diagnostics. KW - Clinical diagnostics KW - FRET KW - MicroRNA KW - Multiplexing KW - Time-gated fluorescence detection PY - 2015 DO - https://doi.org/10.1002/anie.201504887 SN - 1433-7851 SN - 1521-3773 VL - 54 IS - 34 SP - 10024 EP - 10029 PB - Wiley-VCH CY - Weinheim AN - OPUS4-44837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Franz, Philipp T1 - Zerstörungsfreie Charakterisierung und Qualitätssicherung der Materialeigenschaften und Beständigkeit additiv gefertigter Kunststoffteile N2 - Mit additiven Fertigungsverfahren hergestellte Bauteile und Produkte aus Kunststoffen werden zunehmend nicht mehr nur als Prototypen, sondern als voll funktionsfähige Bauteile und Produkte gefertigt. Bedingt durch die Fertigungsprozesse und den schichtweisen Aufbau resultieren physikalische Materialeigenschaften, die stark von den Fertigungsparametern abhängen und zudem anisotrop sind. Von den Fertigungsparametern werden auch die Oberflächeneigenschaften beeinflusst, sodass zu erwarten ist, dass sich die Beständigkeit gegenüber äußeren Umwelteinflüssen bei additiv gefertigten Bauteilen von der konventionell gefertigter unterscheiden kann. Nachfolgend wird daher die Entwicklung eines Qualitätssicherungskonzeptes basierend auf spektroskopischen und zerstörungsfreien Prüfverfahren vorgestellt, in dem der Alterungsprozess von mittels Fused Deposition Modelling (FDM) und mittels Lasersintering (LS) hergestellten Probekörpern untersucht wird. T2 - DGZfP-Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Additive Fertigung KW - Kunststoffe KW - Zerstörungsfreie Prüfung PY - 2018 AN - OPUS4-44896 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Franz, Philipp A1 - Metz, Christain A1 - Brackrock, Daniel A1 - Fischer, C. A1 - Wachtendorf, Volker A1 - Maierhofer, Christiane T1 - Zerstörungsfreie Charakterisierung und Qualitätssicherung der Materialeigenschaften und Beständigkeit additiv gefertigter Kunststoffteile N2 - Mit additiven Fertigungsverfahren hergestellte Bauteile und Produkte aus Kunststoffen werden zunehmend nicht mehr nur als Prototypen, sondern als voll funktionsfähige Bauteile und Produkte gefertigt. Bedingt durch die Fertigungsprozesse und den schichtweisen Aufbau resultieren physikalische Materialeigenschaften, die stark von den Fertigungsparametern abhängen und zudem anisotrop sind. Von den Fertigungsparametern werden auch die Oberflächeneigenschaften beeinflusst, sodass zu erwarten ist, dass sich die Beständigkeit gegenüber äußeren Umwelteinflüssen bei additiv gefertigten Bauteilen von der konventionell gefertigter unterscheiden kann. Nachfolgend wird daher die Entwicklung eines Qualitätssicherungskonzeptes basierend auf spektroskopischen und zerstörungsfreien Prüfverfahren vorgestellt, in dem der Alterungsprozess von mittels Fused Deposition Modelling (FDM) und mittels Lasersintering (LS) hergestellten Probekörpern untersucht wird. T2 - DGZfP-Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Additive Fertigung KW - Kunststoffe KW - Zerstörungsfreie Prüfung PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-449016 SN - 978-3-940283-92-4 VL - DGZfP BB 166 SP - Mo.2.A.1, 1 EP - 9 AN - OPUS4-44901 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saloga, Patrick E. J. T1 - Microwave-assisted high-speed silver nanoparticle synthesis N2 - Ever since increasing a reaction’s yield while shortening the reaction time is the main objective in synthesis optimization. Microwave reactors meet these demands. In literature however their usage is under discussion due to claims of the existence of non-thermal effects resulting from the microwave radiation. Especially for nano-reference-material syntheses it is of crucial importance to be aware of influences on the reaction pathway. Therefore, we compare ultra-small silver nanoparticles with mean radii of 3 nm, synthesized via conventional and microwave heating. We employed a versatile one-pot polyol synthesis of poly(acrylic acid) (PAA) stabilized silver nanoparticles, which display superior catalytic properties. No microwave specific effects in terms of particle size distribution characteristics, as derived by small-angle X-ray scattering (SAXS) and dynamic light scattering (DLS), are revealed. Due to the microwave reactor’s characteristics of a closed system, syntheses can be carried out at temperatures beyond the solvent’s boiling point. Particle formation was accelerated by a factor of 30 by increasing the reaction temperature from 200 °C to 250 °C. The particle growth process follows a cluster coalescence mechanism. A post-synthetic incubation step at 250 °C induces a further growth of the particles while the size distribution broadens. Thus, utilization of microwave reactors enables an enormous decrease of the reaction time as well as the opportunity of tuning the particles’ size. Possibly, decomposition of the stabilizing ligand at elevated temperatures results in reduced yields. A temperature of 250 °C and a corresponding reaction time of 30 s represent a compromise between short reaction times and high yields. T2 - NanoWorkshop 2018 (Workshop on Reference Nanomaterials. Current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2016 KW - SAXS KW - Microwave synthesis KW - Silver nanoparticles PY - 2018 AN - OPUS4-44904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Determining the shell thickness of core-shell nanoparticles using scanning transmission X-ray microscopy (STXM) N2 - A scanning transmission x-ray microscopy (STXM) based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core-shell nanoparticles which exhibit a strong x-ray absorption contrast and a well-defined interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less x-ray beam induced damage of the sample is achieved by recording STXM images only at two predetermined energies of maximum absorption contrast, instead of recording a stack of images across the whole absorption edge. A model core-shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, is used for demonstration. Near edge x-ray absorption fine structure (NEXAFS) spectroscopy confirms the significant difference in x-ray absorption behavior between PTFE and PS. Additionally, due to the insolubility of styrene in PTFE a well-defined interface between particle core and shell is expected. In order to validate the STXM results, both the naked PTFE cores as well as the complete core-shell nanoparticles are examined by scanning electron microscopy (SEM). The introduced STXM based methodology yields particle dimensions in agreement with the SEM results and provides additional information such as the position of the particle core which cannot be extracted from a SEM micrograph. T2 - Innanopart open day CY - London, UK DA - 25.04.2018 KW - STXM KW - SEM KW - PTFE KW - PS KW - Polymer KW - Core-shell nanoparticles PY - 2018 AN - OPUS4-44841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kern, Simon A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gräßer, Patrick A1 - Paul, Andrea A1 - King, R. A1 - Maiwald, Michael T1 - Online low-field NMR spectroscopy for process control of an industrial lithiation reaction—automated data analysis N2 - Monitoring specific chemical properties is the key to chemical process control. Today, mainly optical online methods are applied, which require time- and cost-intensive calibration effort. NMR spectroscopy, with its advantage being a direct comparison method without need for calibration, has a high potential for closed-loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and rough environments for process monitoring and advanced process control strategies. We present a fully automated data analysis approach which is completely based on physically motivated spectral models as first principles information (Indirect Hard Modelling – IHM) and applied it to a given pharmaceutical lithiation reaction in the framework of the European Union’s Horizon 2020 project CONSENS. Online low-field NMR (LF NMR) data was analysed by IHM with low calibration effort, compared to a multivariate PLS-R (Partial Least Squares Regression) approach, and both validated using online high-field NMR (HF NMR) spectroscopy. KW - Online NMR spectroscopy KW - Process analytical technology KW - Partial Least Squares Regression KW - Indirect Hard Modeling KW - Benchtop NMR Spectroscopy KW - Smart Sensors KW - CONSENS PY - 2018 UR - https://link.springer.com/article/10.1007/s00216-018-1020-z DO - https://doi.org/10.1007/s00216-018-1020-z SN - 1618-2642 SN - 1618-2650 VL - 410 IS - 14 SP - 3349 EP - 3360 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-44847 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin A1 - Solomun, Tihomir A1 - Sturm, Heinz T1 - Standard procedure for the irradiation of biomolecules with radiation of different linear energy transfer N2 - The damage caused by ionizing radiation to DNA and proteins is the reason to treat cancer by radiation therapy. A better understanding of the molecular processes and quantification of the different damaging mechanisms is the prerequisite to develop more efficient therapies. Hereby the understanding of the processes involved in the damage to DNA are of key interest due to its central role in reproduction and mutation. For radiation with low linear energy transfer (LET), most of the damage is caused by the secondary particles produced by scattering of the ionizing radiation with water. Thereby a multitude of species are produced, whereby especially kinetic low energy electrons, prehydrated electrons, OH-radicals and ions are of importance. With higher LET the relative amount of the direct damaging effects increases. This is especially important considering the increased usage of high LET nucleons in radiation therapy. Therefore, the quantification of the contribution to DNA damage of direct and indirect effects and the different secondary species is of high interest due to the increase of radio biological efficiency when applying high LET radiation. Here we present an approach to investigate the relative contributions to DNA strand break yield for radiation of different LET within a single electron microscope in combination with electron scattering simulations. T2 - XI International Radiation Protection Association Conference 2018 America CY - Havanna, Cuba DA - 16.04.2018 KW - Dosimetry KW - Linear energy transfer KW - Radiation damage KW - LET KW - Electron irradiation KW - Low energy electrons KW - Hydroxyl radicals KW - DEA KW - DET KW - Microdosimetry KW - Geant4 KW - Electron irradiation of DNA KW - DNA PY - 2018 VL - 2018 SP - 1 EP - 5 AN - OPUS4-44848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Coelho Lima, Isabela A1 - Niederleithinger, Ernst T1 - Alternative imaging conditions for reverse time migration N2 - Ultrasound echo is a widely used NDT technique for determining the internal geometry of structures. Reverse-time migration (RTM) has been recently introduced to NDT applications, as an imaging method for ultrasound data, to overcome some of the limitations (e.g. imaging steeply dipping reflector) experienced by the Synthetic Aperture Focusing Technique (SAFT), the most commonly used imaging algorithm for these measurements. The standard implementation of RTM also experiences some drawbacks caused by its imaging condition, which is based on the zero-lag of the cross-correlation between source and receiver wavefields and generates high-amplitude low-frequency artifacts. Three alternative imaging conditions, developed for seismic data applications, were tested for their ability to provide better images than the standard cross-correlation: illumination compensation, deconvolution and wavefield decomposition. A polyamide specimen was chosen for the simulation of a synthetic experiment and for real data acquisition. The migrations of both synthetic and real data were performed with the software Madagascar. The illumination imaging condition was able to reduce the low-frequency noise and had a good performance in terms of computing time. The deconvolution improved the resolution in the synthetic tests, but did not showed such benefit for the real experiments. Finally, as for the wavefield decomposition, although it presented some advantages in terms of attenuating the low-frequency noise and some unwanted reflections, it was not able to image the internal structure of the polyamide as well as the cross-correlation did. Suggestions on how to improve the cost-effectiveness of the implementation of the deconvolution and wavefield decomposition were presented, as well as possible investigations that could be carried out in the future, in order to obtain better results with those two imaging conditions. T2 - DGZfP Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Ultrasound KW - Reverse time migration KW - Imaging condition KW - Concrete PY - 2018 AN - OPUS4-44873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane A1 - Röllig, Mathias A1 - Heckel, Thomas A1 - Brackrock, Daniel A1 - Gaal, Mate T1 - Charakterisierung von Impactschäden während und nach der Belastung mit thermografischen Verfahren und mit Ultraschall N2 - Der Umfang der durch Impacts in Faserverbundmaterialien erzeugten Schäden ist abhängig von der Energie des Impacts, von der Zusammensetzung und dem Aufbau der Faserverbundwerkstoffe und von der Geometrie der Bauteile und hier im Wesentlichen von der Dicke des Bauteils. Der zerstörungsfreie Nachweis dieser Schädigungen kann sowohl mit Ultraschallverfahren als auch mit Verfahren der aktiven Thermografie erfolgen. Ein Vergleich der Nachweisempfindlichkeiten dieser Verfahren für die unterschiedlichen Schädigungen wird in diesem Beitrag in Abhängigkeit vom verwendeten Faserverbundwerkstoff (CFK und GFK), der Dicke des Materials und von der Impactenergie durchgeführt. Ergänzt werden die im Anschluss an die Schädigung eingesetzten ZfP-Verfahren mit zeitlich hochaufgelösten Thermografiemessungen, die bereits während des Impacts aufgenommen wurden. T2 - DGZfP Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Thermografie KW - Ultraschall KW - Faserverbundwerkstoffe KW - Impactschäden PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-448773 SN - 978-3-940283-92-4 VL - 166 SP - 1 EP - 8 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-44877 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane T1 - Charakterisierung von Impactschäden während und nach dem Impact mit thermografischen Verfahren und mit Ultraschall N2 - Der Umfang der durch Impacts in Faserverbundmaterialien erzeugten Schäden ist abhängig von der Energie des Impacts, von der Zusammensetzung und dem Aufbau der Faserverbundwerkstoffe und von der Geometrie der Bauteile und hier im Wesentlichen von der Dicke des Bauteils. Der zerstörungsfreie Nachweis dieser Schädigungen kann sowohl mit Ultraschallverfahren als auch mit Verfahren der aktiven Thermografie erfolgen. Ein Vergleich der Nachweisempfindlichkeiten dieser Verfahren für die unterschiedlichen Schädigungen wird in diesem Beitrag in Abhängigkeit vom verwendeten Faserverbundwerkstoff (CFK und GFK), der Dicke des Materials und von der Impactenergie durchgeführt. Ergänzt werden die im Anschluss an die Schädigung eingesetzten ZfP-Verfahren mit zeitlich hochaufgelösten Thermografiemessungen, die bereits während des Impacts aufgenommen wurden. T2 - DGZfP Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Thermografie KW - Ultraschall KW - Faserverbundwerkstoffe KW - Impactschäden PY - 2018 AN - OPUS4-44878 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Hydrogen trapping in T24 steel weld joints – Microstructure influence vs. experimental design effect on activation energy for diffusion N2 - A common approach to describe hydrogen traps is by their activation energy that is necessary to release hydrogen from the trap. In the present study, Cr-Mo-V steel T24 (7CrMoVTiB10-10) base material and TIG weld metal were investigated. Electrochemically hydrogen charged specimens were analyzed by thermal desorption analysis (TDA) with different linear heating rates. The results show two different effects. At first, the microstructure effect on trapping is evident in terms of higher hydrogen concentrations in the weld metal and increased activation energy for hydrogen release. Secondly, it is necessary to monitor the real specimen temperature. A comparison between the adjusted heating rate and the real specimen temperature shows that the calculated activation energy varies by factor two. Thus, the trap character in case of the base material changes to irreversible at decreased temperature. Hence, the effect of the experimental procedure must be considered as well if evaluating TDA results. T2 - Forschungsseminar Fügetechnik des IWF, Otto-von-Guericke-Universität CY - Magdeburg, Germany DA - 25.04.2018 KW - Creep-resisting materials KW - Diffusion KW - Weld metal KW - Hydrogen embrittlement PY - 2018 AN - OPUS4-44879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, Gudrun A1 - Emmerling, Franziska A1 - Kemnitz, Erhard T1 - Barium coordination polymers based on fluorinated and fluorine-free benzene-dicarboxylates: Mechanochemical synthesis and spectroscopic characterization N2 - A series of new Ba-based coordination polymers (CPs) were mechanochemically synthesized by milling Ba-hydroxide samples with perfluorinated and fluorine-free benzene-dicarboxylic acids, including tetrafluoroisophthalic acid (H2mBDC-F4), tetrafluorophthalic acid (H2oBDC-F4), isophthalic acid (H2mBDC) and phthalic acid (H2oBDC). The new fluorinated CPs: [Ba(mBDC-F4)$0.5H2O] (1) and [Ba(oBDC-F4)·1.5H2O] (2) are compared to their nonfluorinated counterparts: [Ba(mBDC)·2.5H2O] (3), and [Ba(oBDC)·1H2O] (4). These materials are thoroughly characterized using powder X-ray diffraction. The products obtained by milling are all hydrated but vary in their water contents. Compositions and local structures are investigated by elemental analysis, thermal analysis, MAS NMR and attenuated total reflectioninfrared spectroscopy. These materials exhibit high thermal stabilities but small surface areas that remain unchanged even after thermal treatments. KW - Mechanochemical synthesis KW - Barium KW - Fluorine KW - Coordination polymers KW - PXRD KW - MAS NMR spectroscopy PY - 2018 UR - https://www.sciencedirect.com/science/article/pii/S1293255817310798 DO - https://doi.org/10.1016/j.solidstatesciences.2018.03.013 SN - 1293-2558 SN - 1873-3085 VL - 79 SP - 99 EP - 108 PB - Elsevier AN - OPUS4-44880 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Sporkert, F. A1 - Lô, I. A1 - Baumgartner, M. T1 - The determination of ethyl glucuronide in hair: Experiences from nine consecutive interlaboratory comparison rounds N2 - The increasing request for hair ethyl glucuronide (HEtG) in alcohol consumption monitoring according to cut-off levels set by the Society of Hair Testing (SoHT) has triggered a proficiency testing program based on interlaboratory comparisons (ILC). Here, the outcome of nine consecutive ILC rounds organised by the SoHT on the determination of HEtG between 2011 and 2017 is summarised regarding interlaboratory reproducibility and the influence of procedural variants. Test samples prepared from cut hair (1 mm) with authentic (in-vivo incorporated) and soaked (in-vitro incorporated) HEtG concentrations up to 80 pg/mg were provided for 27–35 participating laboratories. Laboratory results were evaluated according to ISO 5725-5 and provided robust averages and relative reproducibility standard deviations typically between 20 and 35% in reasonable accordance with the prediction of the Horwitz model. Evaluation of results regarding the analytical techniques revealed no significant differences between gas and liquid chromatographic methods In contrast, a detailed evaluation of different sample preparations revealed significantly higher average values in case when pulverised hair is tested compared to cut hair. This observation was reinforced over the different ILC rounds and can be attributed to the increased acceptance and routine of hair pulverisation among laboratories. Further, the reproducibility standard deviations among laboratories performing pulverisation were on average in very good agreement with the prediction of the Horwitz model. Use of sonication showed no effect on the HEtG extraction yield. KW - Ethyl glucuronide KW - Interlaboratory comparison KW - Proficiency testing KW - Society of hair testing KW - Reproducibility KW - Pulverization PY - 2018 DO - https://doi.org/10.1016/j.forsciint.2018.04.025 SN - 0379-0738 SN - 1872-6283 VL - 288 SP - 67 EP - 71 PB - Elsevier AN - OPUS4-44881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard A1 - Kunisch, E. A1 - Kinne, R. W. T1 - μCT begleitete in-situ Druckversuche an spongiösem Knochen - Vergleich(ende Bestimmung) des experimentellen und simulierten Verschiebungsfeldes mit der simulierten internen Spannung N2 - Untersuchungen haben gezeigt, dass sich ältere Schafe gut als Modell für die mi-nimalinvasive Behandlung von Osteoporose eignen [1]. Um einen Behandlungs-effekt nachzuweisen, wird dabei unter anderem die Belastungsfähigkeit des Kno-chens durch Druckversuche an kleinen Zylindern aus den behandelten und unbe-handelten Knochen bestimmt. Diese hatten hier einen Durchmesser von 10 mm und eine Höhe von 13 mm. Für den in-situ Druckversuch wurde eine Deben CT5000 verwendet. In einer Serie von Druckerhöhungen wurden die Proben je-weils tomographiert. Dabei ergab sich zunächst, dass mit der µCT innerhalb der Knochen im oberen und unteren Bereich schon Brüche nachgewiesen werden können, obwohl die gemessene Kraftaufnahmekurve keine Unstetigkeit zeigt. Deswegen wurden die starren Probenaufnehmer der Deben Anordnung durch bewegliche Aufnehmer ergänzt, die eine leichte Verkippung der belasteten Ober-flächen ausgleichen können. Ein Vergleich der gemessenen und der aus den µCT-Daten berechneten Verschiebungsfelder ergab trotz der komplexen Struktur der Knochen gute Übereinstimmungen. Diese Verschiebungen wurden dann mit den aus den µCT Daten simulierten mechanischen Druckversuchen, Von-Mise-Spannungen und daraus berechneten Verschiebungen verglichen. (VGStudioMax Simulation). T2 - DGZfP-Jahrestagung CY - Leipzig, Germany DA - 07.05.2018 KW - Computer Tomographie KW - In-situ Druckversuch KW - Simulation PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-448827 UR - https://www.ndt.net/?id=23080 SN - 978-3-940283-92-4 VL - DGZfP BB 166 SP - 1 EP - 7 PB - DGZfP CY - Berlin AN - OPUS4-44882 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stajanca, Pavol A1 - Topolniak, Ievgeniia A1 - Pötschke, Samuel A1 - Krebber, Katerina ED - Kalli, K. ED - Mendez, A. ED - Bunge, C.-A. T1 - Solution doping of commercial plastic optical fibers N2 - Solution doping of off-the-shelf plastic optical fibers (POFs) represents rather simple and cheap way for preparing custom cladding-doped POFs (CD-POFs) with short to medium lengths. CD-POFs are especially attractive for environmental sensing applications, but might be of interest for illumination task as well. In this work, the proposed doping technique is tested with three different commercial low-cost polymethyl methacrylate (PMMA) POFs; Eska CK-40 and Eska GK-40 from Mitsubishi Rayon and Raytela PGU-FB1000 from Toray. The aim of the work is to aid the selection of the most suitable fiber yielding highest optical quality of prepared CD-POFs. Firstly, the optimal doping times are determined for the individual fiber types using short fiber samples. Secondly, longer 10 m CD-POFs are prepared from all tested fibersusing the optimized doping procedure. Finally, attenuation of pristine POFs and prepared CD-POFs is measured using optical time domain reflectometry in order to characterize the impacts of the doping on fiber optical properties. In addition, the importance of post-doping drying procedure for CD-POF optical performance is investigated as well. The results suggest that, although doping of all tested fibers is generally feasible, Eska CK-40 is the most suitable candidate with regard to the Doping efficiency and fiber post-doping performance. T2 - SPIE Photonics Europe 2018 CY - Strasbourg, France DA - 22.04.2018 KW - Plastic optical fibers KW - Solution doping KW - Polzmethyl methacrylate KW - PMMA KW - Rhodamine B KW - Fluorescent optical fibers KW - Cladding-doped fibers PY - 2018 DO - https://doi.org/10.1117/12.2315619 SN - 0277-786X VL - 10681 SP - 106810O-1 EP - 106810O-7 AN - OPUS4-44907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stajanca, Pavol T1 - Solution doping of commercial plastic optical fibers N2 - Solution doping of off-the-shelf plastic optical fibers (POFs) represents rather simple and cheap way for preparing custom cladding-doped POFs (CD-POFs) with short to medium lengths. CD-POFs are especially attractive for environmental sensing applications, but might be of interest for illumination task as well. In this work, the proposed doping technique is tested with three different commercial low-cost polymethyl methacrylate (PMMA) POFs; Eska CK-40 and Eska GK-40 from Mitsubishi Rayon and Raytela PGU-FB1000 from Toray. The aim of the work is to aid the selection of the most suitable fiber yielding highest optical quality of prepared CD-POFs. Firstly, the optimal doping times are determined for the individual fiber types using short fiber samples. Secondly, longer 10 m CD-POFs are prepared from all tested fibers using the optimized doping procedure. Finally, attenuation of pristine POFs and prepared CD-POFs is measured using optical time domain reflectometry in order to characterize the impacts of the doping on fiber optical properties. In addition, the importance of post-doping drying procedure for CD-POF optical performance is investigated as well. The results suggest that, although doping of all tested fibers is generally feasible, Eska CK-40 is the most suitable candidate with regard to the doping efficiency and fiber post-doping performance. T2 - SPIE Photonics Europe 2018 CY - Strasbourg, France DA - 22.04.2018 KW - Plastic optical fibers KW - Solution doping KW - Polymethyl methacrylate KW - PMMA KW - Rhodamine B KW - Fluorescent optical fibers KW - Cladding-doped fibers PY - 2018 AN - OPUS4-44908 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Simple and Versatile Methods for Quantifying Functional Groups, Ligands, and Biomolecules on Nanomaterials N2 - Many applications of nanomaterials in the life sciences require the controlled functionalization of these materials with ligands like polyethylene glycol (PEG) and/or biomolecules such as peptides, proteins, and DNA. This enables to tune their hydrophilicity and biocompatibility, minimize unspecific interactions, improve biofunctionalization efficiencies, and enhance blood circulation times. Moreover, it is the ultimate prerequisite for their use as reporters in assays or the design of targeted optial probes for bioimaging. At the core of these functionalization strategies are reliable and validated methods for surface group and ligand quantification that can be preferably performed with routine laboratory instrumentation, require only small amounts of substances, and are suitable for many different types of nanomaterials. We present here versatile and simple concepts for the quantification of common functional groups, ligands, and biomolecules on different types of organic and inorganic nano-materials, using different types of optical reporters and method validation with the aid of multimodal reporters, method comparisons, and mass balances. T2 - INNANOPART open day CY - London, UK DA - 24.04.2018 KW - Surface functionalization KW - Nanoparticles KW - Surface chemistry KW - Multimodal reporters PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-44849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya T1 - Multimodal cleavable reporters vs conventional labels for optical quantification of amino and carboxy groups on nanomaterials and microparticles N2 - Carboxy, amino, and thiol groups play a critical role in a variety of physiological and biological processes and are frequently used for bioconjugation reactions. Moreover, they enable size control and tuning of the surface during the synthesis of particle systems. Especially, thiols have a high binding affinity to noble metals and semiconductors (SC). Thus, simple, inexpensive, robust, and fast methods for the quantification of surface groups and the monitoring of reactions involving ligands are of considerable importance for the characterization of modified or stabilized nanomaterials including polymers. We studied the potential of the Ellman’s assay, recently used for the quantification of thiol ligands on SC nanocrystals by us1 and the 4-aldrithiol assay for the determination of thiol groups in molecular systems and on polymeric, noble and SC nanomaterials. The results were validated with ICP-OES and reaction mechanisms of both methods were studied photometrically and with ESI-TOF-MS. The investigation of the reaction mechanisms of both methods revealed the influence of different thiols on the stoichiometry of the reactions2, yielding different mixed disulfides and the thiol-specific products spectroscopically detected. The used methods can quantify freely accessible surface groups on nanoparticles, e.g., modified polystyrene nanoparticles. For thiol ligands coordinatively bound to surface atoms of, e.g., noble or SC nanomaterials, depending on the strength of the thiol-surface bonds, particle dissolution prior to assay performance can be necessary. We could demonstrate the reliability of the Ellman’s and aldrithiol assay for the quantification of surface groups on nanomaterials by ICP-OES and derived assay-specific requirements and limitations. Generally, it is strongly recommended to carefully control assay performance for new samples, components, and sample ingredients to timely identify possible interferences distorting quantification. T2 - BAM-BfR Seminar 2018 CY - Berlin, Germany DA - 15.02.2018 KW - Surface functionalization KW - Nanoparticles KW - Surface chemistry KW - Multimodal reporters PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-44850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schumacher, David A1 - Sharma, R. A1 - Grager, J.-C. A1 - Schrapp, M. T1 - Scatter and beam hardening reduction in industrial computed tomography using photon counting detectors N2 - Photon counting detectors (PCD) offer new possibilities for x-ray micro computed tomography (CT) in the field of non-destructive testing. For large and/or dense objects with high atomic numbers the problem of scattered radiation and beam hardening severely influences the image quality. This work shows that using an energy discriminating PCD based on CdTe allows to address these problems by intrinsically reducing both the influence of scattering and beam hardening. Based on 2D-radiographic measurements it is shown that by energy thresholding the influence of scattered radiation can be reduced by up to in case of a PCD compared to a conventional energy-integrating detector (EID). To demonstrate the capabilities of a PCD in reducing beam hardening, cupping artefacts are analyzed quantitatively. The PCD results show that the higher the energy threshold is set, the lower the cupping effect emerges. But since numerous beam hardening correction algorithms exist, the results of the PCD are compared to EID results corrected by common techniques. Nevertheless, the highest energy thresholds yield lower cupping artefacts than any of the applied correction algorithms. As an example of a potential industrial CT application, a turbine blade is investigated by CT. The inner structure of the turbine blade allows for comparing the image quality between PCD and EID in terms of absolute contrast, as well as normalized signal-to-noise and contrast-to-noise ratio. Where the absolute contrast can be improved by raising the energy thresholds of the PCD, it is found that due to lower statistics the normalized contrast-to-noise-ratio could not be improved compared to the EID. These results might change to the contrary when discarding pre-filtering of the x-ray spectra and thus allowing more low-energy photons to reach the detectors. Despite still being in the early phase in technological progress, PCDs already allow to improve CT image quality compared to conventional detectors in terms of scatter and beam hardening reduction. KW - X-ray computed tomography KW - Photon counting detector KW - CdTe sensor KW - Non-destructive testing KW - Beam hardening KW - Scattered radiation PY - 2018 UR - http://iopscience.iop.org/article/10.1088/1361-6501/aabef7/meta DO - https://doi.org/10.1088/1361-6501/aabef7 SN - 1361-6501 VL - 29 IS - 7 SP - 075101, 1 EP - 12 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-44959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Völker, Tobias A1 - Kazakov, Alexander Ya. T1 - Extension and investigation by numerical simulations of algorithm for calibration-free laser induced breakdown spectroscopy N2 - Accuracy of calibration-free (CF) methods in laser-induced breakdown spectroscopy (LIBS) depends on experimental conditions and instrumental parameters that must match a CF LIBS model. Here, the numerical study is performed to investigate effects of various factors, such as the optical density, plasma uniformity, line overlap, noise, spectral resolution, electron density and path length on the results of CF-LIBS analyses. The effects are examined one-by-one using synthetic spectra of steel slag samples that fully comply with the mathematical model of the method. Also, the algorithm includes several new features in comparison with previously proposed CF algorithms. In particular, it removes limits on the optical thickness of spectral lines that are used for the construction of the Saha-Boltzmann plot; it retrieves the absorption path length (Plasma diameter) directly from spectral lines; it uses the more realistic Voigt line profile function instead of the Lorentzian function; and it employs the pre-calculated and tabulated thin-to-thick line ratios instead of approximating functions for selfabsorption correction. KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics KW - Calibration free LIBS PY - 2018 DO - https://doi.org/10.1016/j.sab.2018.06.011 SN - 0584-8547 VL - 147 SP - 149 EP - 163 PB - Elsevier B.V. AN - OPUS4-45340 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Improved algorithm for calibration-free laser induced breakdown spectroscopy N2 - An improved algorithm for calibration-free laser induced breakdown spectroscopy (CF LIBS) is presented which includes several novel features in comparison with previously proposed similar algorithms. In particular, it allows using spectral lines with arbitrary optical thickness for the construction of Saha-Boltzmann plots, retrieves the absorption path length (plasma diameter) directly from a spectrum, replaces the Lorentzian line profile function by the Voigt function, and allows for self-absorption correction using pre-calculated and tabulated data rather than approximating functions. The tabulated data embody the solutions of the radiative transfer equation for numerous combinations of optical thicknesses and line widths. The algorithm is thoroughly verified with synthetic spectra. T2 - 14TH European Workshop on Laser Ablation 2018 (EWLA2018) CY - Pau, France DA - June 26 - 29, 2018 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics KW - Calibration free LIBS PY - 2018 AN - OPUS4-45343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Laser induced plasma: Modeling, diagnostics, and applications N2 - Laser-induced plasmas are widely used in many areas of science and technology; examples include spectrochemical analysis, thin film deposition, material processing, and even jet propulsion. Several topics will be addressed. First, general phenomenology of laser-induced plasmas will be discussed. Then, a chemical model will be presented based on a coupled solution of Navier-Stokes, state, radiative transfer, material transport, and chemical (Guldberg-Waage) equations. Results of computer simulations for several chemical systems will be shown and compared to experimental observations obtained by optical imaging, spectroscopy, and tomography. The latter diagnostic tools will also be briefly discussed. Finally, a prospective application of laser-induced plasma and plasma modeling will be illustrated on the example of calibration-free MC LIBS (Monte Carlo Laser Induced Breakdown Spectroscopy), in which concentrations of elements in materials are found by fitting model-generated and experimental spectra. T2 - Invited talk at Yeshiva University, New York, USA CY - Yeshiva University, New York, USA DA - 4.24.2018 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2018 AN - OPUS4-45344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Jens A1 - Larsson, H. A1 - Temps, F. A1 - Hartke, B. T1 - Resonance dynamics of DCO (<(X over tilde>(2)A') simulated with the dynamically pruned discrete variable representation (DP-DVR) N2 - Selected resonance states of the deuterated formyl radical in the electronic ground state X^2A´ are computed using our recently introduced dynamically pruned discrete variable representation [H. R. Larsson, B. Hartke, and D. J. Tannor, J. Chem. Phys. 145, 204108 (2016)]. Their decay and asymptotic distributions are analyzed and, for selected resonances, compared to experimental results obtained by a combination of stimulated emission pumping and velocity-map Imaging of the product D atoms. The theoretical results show good agreement with the experimental kinetic energy distributions. The intramolecular vibrational energy redistribution is analyzed and compared with previous results from an effective polyad Hamiltonian. Specifically, we analyzed the part of the wavefunction that remains in the interaction region during the decay. The results from the polyad Hamiltonian could mainly be confirmed. The C=O stretch quantum number is typically conserved, while the D-C=O bend quantum number decreases. Differences are due to strong anharmonic coupling such that all resonances have major contributions from several zero-order states. For some of the resonances, the coupling is so strong that no further zero-order states appear during the dynamics in the interaction region, even after propagating for 300 ps. KW - Reaction dynamics KW - Spectroscopy KW - Quantum state PY - 2018 DO - https://doi.org/10.1063/1.5026459 SN - 0021-9606 VL - 148 IS - 20 SP - 204309-1 EP - 204309-15 PB - AIP publishing CY - New York AN - OPUS4-45345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dai, X. A1 - Zhang, W. A1 - Li, H. A1 - Huang, T. A1 - Li, M. A1 - Quan, C. A1 - Zhang, Q. A1 - Davies, S. R. A1 - Warren, J. A1 - Lo, M.-F. A1 - Kakoulides, E. A1 - Gören, A. C. A1 - Marbumrung, S. A1 - Pfeifer, Dietmar A1 - Ün, I. A1 - Gündüz, S. A1 - Yilmaz, H. A1 - Kankaew, P. A1 - Sudsiri, N. A1 - Shearman, K. A1 - Pookrod, P. A1 - Polzer, J. A1 - Radeck, W. T1 - CCQM-K104 key comparison (avermectin B(1)a) on the characterization of organic substances for chemical purity N2 - Under the Comité Consultatif pour la Quantité de Matière (CCQM), a key comparison, CCQM-K104, was coordinated by the National Institute of Metrology (NIM). The comparison was designed to demonstrate a laboratory's performance in determining the mass fraction of the main component in a complex high purity organic material. Nine NMIs or DIs participated in the comparison. Eight participants reported their results. An additional impurity was resolved from the avermectin B1a peak and was tentatively identified as an unknown impurity by NMIA (National Measurement Institute (Australia)). It was subsequently identified by NIM as a diastereoisomer of avermectin B1a at the C-26 position. Final reference value (KCRV) = 924.63 mg/g, with uncertainty (k=1) = 3.89 mg/g, and expanded uncertainty = 8.97 mg/g. The degrees of equivalence with the avermectin B1a KCRV for each participant were reported. The measurement results and degrees of equivalence should be indicative of the performance of a laboratory's measurement capability for the purity assignment of organic compounds of high structural complexity (relative molecular mass range of 500 Da -1000 Da and low polarity (-log KOW ≤ -2). KW - NMR KW - Key comparision KW - CCQM PY - 2017 DO - https://doi.org/10.1088/0026-1394/54/1A/08019 SN - 0026-1394 VL - 54 SP - 2 EP - 32 AN - OPUS4-45381 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yildirim, Arda T1 - Liquid Crystals Forming a Columnar Mesophase: Structure, Dynamics and Electric Conductivity N2 - The molecular dynamics and ionic conductivity of ionic liquid crystals (ILCs) forming a columnar mesophase, two linear-shaped tetramethylated guanidinium triflates ILCs having different lengths of alkyl chains, were investigated by a combination of Broadband Dielectric Spectroscopy (BDS) and Specific Heat Spectroscopy (SHS). Three processes were detected by BDS; at low temperature γ-process, at higher temperatures α-process and at even higher temperatures conductivity. The γ-process indicates localized fluctuations, and the α-process designates cooperative fluctuations. Slightly different restrictions were found for conductivity processes of LC536 and LC537 due to the slightly different lengths of alky chains. The conductivity mechanisms in the plastic crystalline and the columnar mesophase have been revealed by BDS and different charge carriers were assigned for the different phases. Furthermore, the cooperative dynamics were also probed by SHS. The cooperative dynamics probed by the different techniques (BDS and SHS) compared, and assigned to the different restrictions on the cooperativity due to the difference in the sensitivity of the techniques. T2 - Seminar Vortrag Technische Universität Berlin CY - Berlin, Germany DA - 28.06.2018 KW - Columnar Liquid Crystals KW - Ionic Liquid Crystals PY - 2018 AN - OPUS4-45383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian T1 - Active thermography for quality assurance of 3D-printed polymer structures N2 - Active thermography with flash and halogen light excitation is used as a method for non-destructive testing of 3D-printed polymer components. Test specimens with artificial defects have been generated, using laser sintering and fused layer modeling. These test specimens have been investigated in different measurement configurations with both excitation methods. Afterwards, the different measurement conditions were compared regarding their capability to detect the defects. Furthermore, advanced analysis methods are used, to fully exploit the capabilities of these techniques. T2 - 14th Quantitative InfraRed Thermography Conference CY - Berlin, Germany DA - 25.06.2018 KW - Additive manufacturing KW - Active thermography KW - Artificial weathering PY - 2018 AN - OPUS4-45387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Manolov, Manol T1 - Bestimmung der Maschinennachgiebigkeit beim Einsatz sphärischer Indenter in der Instrumentierten Eindringprüfung N2 - Der Einfluss der Maschinennachgiebigkeit einschließlich der elastischen Verformung des Indenters ist bei der Bestimmung der entsprechenden Werkstoffcharakteristiken insbesondere beim Einsatz von sphärischen Indentern unter höheren Prüfkräften von Bedeutung. Mit zunehmender Prüfkraft wird die Maschinennachgiebigkeit kraftabhängig und kann im idealen Fall als Funktion von Prüfkraft und gemessener Eindringtiefe für vorgegebene Indenterradien dargestellt werden. Angegeben ist ein vereinfachtes Verfahren zur Bestimmung der Maschinennachgiebigkeit. T2 - Sensoren und Messsysteme CY - Nürnberg, Germany DA - 26.06.2018 KW - Maschinennachgiebigkeit KW - Instrumentierte Eindringprüfung KW - Sphärische Indenter KW - Vereinfachtes Verfahren KW - Kraftabhängige Funktion KW - Härtevergleichsplatten KW - Eindringmodul PY - 2018 AN - OPUS4-45390 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian A1 - Franz, Philipp A1 - Fischer, C. A1 - Wachtendorf, Volker A1 - Maierhofer, Christiane T1 - Active thermography for quality assurance of 3D-printed polymer structures N2 - Additively manufactured test specimens made of polyamide 12 (PA 12) by Laser Sintering (LS) as well as of acrylnitril-butadien-styrol (ABS) by Fused Layer Modeling (FLM), were tested with active thermography. For this, two different excitation methods (flash and impulse excitation) were used and compared, regarding the suitability for the detection of constructed and imprinted defects. To increase the quality of the thermograms, data processing methods like thermal signal reconstruction (TSR) and Fourier-Transformation were applied. Furthermore, the long-term stability of the probes towards environmental stress, like UV-radiation, heat, water contact and frost is being investigated in the presented project with artificial weathering tests. T2 - 14th Quantitative InfraRed Thermography Conference CY - Berlin, Germany DA - 25.06.2018 KW - Additive manufacturing KW - Active thermography KW - Artificial weathering PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453919 SP - Tu.3.A.2, 1 EP - 9 AN - OPUS4-45391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Manolov, Manol A1 - Subaric-Leitis, Andreas A1 - Bartholmai, Matthias T1 - Bestimmung der Maschinennachgiebigkeit beim Einsatz sphärischer Indenter in der Instrumentierten Eindringprüfung N2 - Es wird ein vereinfachtes Verfahren für die Bestimmung und Implementierung der Maschinennachgiebigkeit bei der Verwendung eines sphärischen Indenters dargestellt. Die Maschinennachgiebigkeit wird bei deutlicher Kraftabhängigkeit als Funktion der Kraft in die Auswertung implementiert. Als sensitiver Kennwert dient der aus der instrumentierten Eindringprüfung an Härtevergleichsplatten ermittelte Eindringmodul. T2 - Sensoren und Messsysteme CY - Nürnberg, Germany DA - 26.06.2018 KW - Maschinennachgiebigkeit KW - Instrumentierte Eindringprüfung KW - Sphärische Indenter KW - Vereinfachtes Verfahren KW - Kraftabhängige Funktion KW - Härtevergleichsplatten KW - Eindringmodul PY - 2018 SN - 978-3-8007-4683-5 SN - 0932-6022 VL - 19. ITG/GMA-Fachtagung SP - 565 EP - 569 PB - VDE Verlag GmbH CY - Berlin AN - OPUS4-45394 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard A1 - Kunisch, E. A1 - Kinne, R. W. T1 - Serial in situ compression of spongiosa cylinder observed by μCT, compared to simulated stress, strain, and movement N2 - Minimally invasive injection of calcium phosphate cement into bone defects in aged sheep vertebrae has been used as a model for the treatment of osteoporotic vertebral fractures. One of the therapeutic criteria is a compression test of non-treated or treated vertebral bodies. In the present study, an in situ compression test with a stepwise load increase was performed with small spongiosa cylinders from the vertebrae under continuous monitoring by μCT. This allows localization of bone cracks and the visualization of correct placement and form of the bone cylinder. In addition, the effects of an uneven load distribution on the sample due to an irregular shape and a subsequent underperformance of the test sample can be excluded by controlling its shape under increasing load. There was a good agreement between the measured data and those obtained by simulated load-dependent transformation on the basis of a digital volume correlation between consecutive compression tests on the bone surface under the assumption of homogeneous bone material. Mechanic simulation was executed by directly using structural voxel data, resulting in maps of Von Mise stresses and predicted displacements. T2 - 12th ECNDT CY - Gothenburg, Sweden DA - 11.6.2018 KW - Computed tomography KW - In-situ compression KW - Simulation PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453317 SN - 978-91-639-6217-2 SP - 0162, 1 EP - 7 AN - OPUS4-45331 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nutsch, A. T1 - A Methodology to Obtain Traceability and Validation of Calibration Samples for Thin Metal Alloy Layers for X-Ray Fluorescence Tools N2 - Statistic process control as well as process capability demand for calibrated determination of layer thicknesses in various industries, e.g. automotive, aerospace, microelectronics manufacturing. Calibration requires well know and well characterized samples. A calibration laboratory accredited according to DIN EN ISO 17025 has the objective to distribute standards traceable to SI units to industrial laboratories for quality control of manufacturing of various products. Especially, the thickness determination of thin metallic coatings e.g. from galvanic processes or layer deposition using X-Ray Fluorescence can be significantly improved by customized calibration samples. This is essential as the measurement uncertainty directly correlates to the capability performing reliable control of processes with high yield. For calibration laboratories, the validation of results using round robins and the direct comparison to national metrology institutes is a prerequisite to demonstrate the competence to perform calibration services. In this paper a strategy to obtain traceability and validation for thin alloy layers as well as first results are presented. The combined use of the accredited method for determination of mass per area from measurement of mass and area combined with standard free X-Ray Fluorescence as well as chemical analysis of dissolved samples with thin layers is deployed for material systems as NixZn1-x as well as NixP1-x. The obtained results are compared to reference free X-Ray Fluorescence at the BESSY II laboratories of Physikalisch-Technische Bundesanstalt. An excellent agreement of the obtained measured values as mass per unit area and alloy concentrations from the different applied methods within the measurement uncertainty was observed for NixP1-x showing the successful performed traceability of the calibration samples to SI units in combination with a validation of results by national metrology institutes and the round robin approach. T2 - European Conference on X-Ray Spectrometry CY - Ljubljana, Slowenia DA - 24.06.2018 KW - Traceability KW - Thin metal alloy layers KW - X-ray fluorescence PY - 2018 AN - OPUS4-45317 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc T1 - Ionische Flüssigkeiten als neuartige Sensorbeschichtung für coulometrische Spurenfeuchtesensoren N2 - Die Arbeit präsentiert erste Messungen mit coulometrischen Sensoren, die mit einer ionischen Flüssigkeit beschichtet sind. Diese Sensoren werden in der Industrie verwendet, um die Spurenfeuchte in unterschiedlichen Gasen zu messen. Normalerweise erfolgt eine Beschichtung der Sensoren mit Phosphorpentoxid und dessen Hydrolyseprodukte. In dieser Arbeit wurde stattdessen eine hygroskopische ionische Flüssigkeit benutzt. Die generierte Gasfeuchte für die Untersuchungen betrug bezogen auf die Frostpunkttemperatur -80 °C bis -30 °C, was gleichbedeutend mit einem Wasserdampf-Stoffmengenanteil von 0,5 μmol·mol-1 bis 376 μmol·mol-1 ist. Zusätzlich zu der Messung mit coulometrischen Sensoren erfolgte eine Referenzmessung der Gasfeuchte mittels eines Taupunkthygrometers. Erste Ergebnisse haben gezeigt, dass es möglich ist mit dieser Art der Beschichtung unterschiedliche Gasfeuchten zu messen. Aber es ergaben sich trotz gleicher Feuchte unterschiedliche Signalintensitäten bei den benutzen Sensoren und es zeigte sich eine Drift des Sensorsignales. T2 - Sensoren und Messsysteme CY - Nuremberg, Germany DA - 26.06.2018 KW - Spurenfeuchtemessung KW - Elektrolyseverfahren KW - Ionische Flüssigkeiten KW - Sensorbeschichtung PY - 2018 AN - OPUS4-45318 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc A1 - Tiebe, Carlo A1 - Banach, Ulrich A1 - Ritter, U. T1 - Ionische Flüssigkeiten als neuartige Sensorbeschichtung für coulometrische Spurenfeuchtesensoren N2 - Die Arbeit präsentiert erste Messungen mit coulometrischen Sensoren, die mit einer ionischen Flüssigkeit beschichtet sind. Diese Sensoren werden in der Industrie verwendet, um die Spurenfeuchte in unterschiedlichen Gasen zu messen. Normalerweise erfolgt eine Beschichtung der Sensoren mit Phosphorpentoxid und dessen Hydrolyseprodukte. In dieser Arbeit wurde stattdessen eine hygroskopische ionische Flüssigkeit benutzt. Die generierte Gasfeuchte für die Untersuchungen betrug bezogen auf die Frostpunkttemperatur -80 °C bis -30 °C, was gleichbedeutend mit einem Wasserdampf-Stoffmengenanteil von 0,5 μmol·mol-1 bis 376 μmol·mol-1 ist. Zusätzlich zu der Messung mit coulometrischen Sensoren erfolgte eine Referenzmessung der Gasfeuchte mittels eines Taupunkthygrometers. Erste Ergebnisse haben gezeigt, dass es möglich ist mit dieser Art der Beschichtung unterschiedliche Gasfeuchten zu messen. Aber es ergaben sich trotz gleicher Feuchte unterschiedliche Signalintensitäten bei den benutzen Sensoren und es zeigte sich eine Drift des Sensorsignales. T2 - Sensoren und Messsysteme CY - Nuremberg, Germany DA - 26.06.2018 KW - Spurenfeuchtemessung KW - Sensorbeschichtung KW - Elektrolyseverfahren KW - Ionische Flüssigkeiten PY - 2018 SN - 978-3-8007-4683-5 SN - 0932-6022 SP - 520 EP - 523 PB - VDE VERLAG GMBH CY - Berlin, Offenbach AN - OPUS4-45319 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kakoulides, E. T1 - Development of Certified Reference Materials for the calibration of breath analyzers N2 - IAPR participates in the EMPIR 16SRT02, entitled ‘Certified forensic alcohol reference materials - ALCOREF’ funded by EURAMET as an external funded partner. The Research in this project will address the needs for better enforcement of drink-driving legislation in several European countries, by building up long-term capacities for the production and certification of forensic alcohol reference materials, suitable for the calibration of evidential breath alcohol analyzers. The certification procedure includes characterization of the materials, assessment of homogeneity, stability, and uncertainty estimation. An interlaboratory comparison will be conducted to test the materials and capabilities developed. EMPIR 16SRT02-ALCOREF project is coordinated by BAM (DE). T2 - 7th National Metrology Congress CY - Athens, Greece DA - 11.05.2018 KW - Certified reference materials KW - Metrology institute KW - Calibration KW - Uncertainty PY - 2018 N1 - Sprache der Posterpräsentation: Griechisch AN - OPUS4-45321 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias T1 - Temperature characteristics of a piezoresistive accelerometer for high impact shock application N2 - This study presents the characterization of a piezoresistive accelerometer damped with silicon oil for the application in drop tests carried out at BAM. Experiments were performed with the Hopkinson Bar method in close correlation to the real-world application conditions. The results point out certain limitations regarding the temperature influence and the frequency response. Additional experiments were performed with a gas damped type of piezoresistive accelerometer, which has superior specifications, particularly for low temperatures. The results allow for a comparison. T2 - Sensoren und Messsysteme CY - Nürnberg, Germany DA - 26.06.2018 KW - Piezoresistive accelerometer KW - Hopkinson bar KW - High impact shock application KW - Temperature characteristics KW - Drop test PY - 2018 AN - OPUS4-45322 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias ED - Werner, Klaus-Dieter T1 - Temperature characteristics of a piezoresistive accelerometer for high impact shock application N2 - This study presents the characterization of a piezoresistive accelerometer damped with silicon oil for the application in drop tests carried out at BAM. Experiments were performed with the Hopkinson Bar method in close correlation to the real-world application conditions. The results point out certain limitations regarding the temperature influence and the frequency response. Additional experiments were performed with a gas damped type of piezoresistive accelerometer, which has superior specifications, particularly for low temperatures. The results allow for a comparison. T2 - Sensoren und Messsysteme CY - Nürnberg, Germany DA - 26.06.2018 KW - Piezoresistive accelerometer KW - High impact shock application KW - Drop test KW - Temperature characteristics KW - Hopkinson bar PY - 2018 SN - 978-3-8007-4683-5 SN - 0932-6022 SP - 465 EP - 467 PB - VDE Verlag GmbH CY - Berlin AN - OPUS4-45323 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - Conventional and HF Eddy Current Testing of Composite Pressure Vessels N2 - Composite pressure vessels consist of an internal liner (Steel, aluminum, or plastic) which stores the liquid or gas and CFRP (carbon fiber reinforced plastics) which serves as pressure resistance. These vessels comprise some advantages compared with conventional vessels made of steel or aluminum and their application grew strongly over the last decade. The reason for this trend is the tremendous weight saving. However, the long-time behavior for filling and discharging cycles and the creep strength of composite vessels is not fully understood. Therefore, BAM started an internal project to investigate degradation of these material systems. Normally, high-frequency eddy current testing (HF-ET, f > 10 MHz) is deployed for CFRP due to the low conductivity of the fibers, which is in the order of 0.01 MS/s, and the capacitive coupling between them. Nevertheless, in some cases conventional ET can be applied. Some first results using conventional ET for detecting leakages in the internal liners are already presented. This contribution gives an update of our investigation using both conventional and high-frequency ET. Therefore, we developed an ET equipment based on a vector network analyzer using frequencies between 300 kHz and 2 GHz. The focus concerns the study of the aging effects. T2 - 12th European conference on Non-Destructive Testing (ECNDT) CY - Gothenburg, Sweden DA - 11.06.2018 KW - Eddy current testing KW - Composite KW - Pressure vessel PY - 2018 AN - OPUS4-45302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - New technologies for air-coupled ultrasonic transducers N2 - Air-coupled ultrasonic testing (ACUT) has experienced rapid growth within the last years. It is especially well suited to inspection of lightweight structures consisting of composite materials and adhesive joints. Uniform coupling and easy maintenance are its advantages compared to contact technique. However, the impedance mismatch between the transducer and air poses a major challenge to the development of ACUT transducers. Commercially available air-coupled transducers consist of a piezocomposite material and matching layers. Their fabrication is difficult in handling and their signal-to-noise ratio sometimes not sufficient for various testing requirements. However, there are several innovative approaches using other materials and other physical principles to transmit and receive an ultrasonic pulse. We present a review of the latest advances in research on air-coupled transducers for non-destructive testing, including previously unpublished results. We recognize two major directions as most promising: ferroelectrets and thermoacoustic transducers. Ferroelectrets are charged cellular polymers exhibiting piezoelectric properties. Their small acoustic impedance is matched to air better than matching layers applied in conventional air-coupled transducers. Applying bias voltage to a ferroelectret receiver is the latest development in this field, which increased the received signal by 12 to 15 dB. Thermoacoustic transducers use heat to initiate an ultrasonic wave, acting as transmitters. The working principle is known from nature as thunder and lightning: thermal energy of an electrically heated material, which can also be air, is converted into acoustic energy. Some thermoacoustic transmitters consist of a conductive layer with a thickness in the nanometer range deposited on a solid substrate. Another possibility is to use an electric spark. For the first time, measurements of the sound field of an electric spark up to 500 kHz were performed. Thermoacoustic transducers enable excitation of extremely broadband pulses while producing high pressure levels, which opens new possibilities for advanced signal processing. T2 - 12th European conference on Non-Destructive Testing CY - Gothenburg, Sweden DA - 11.06.2018 KW - Transducer KW - Air-coupled ultrasonic testing KW - Atmospheric pressure plasma KW - Cellular polypropylene KW - Ferroelectret PY - 2018 AN - OPUS4-45304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Akustische Emission von Plasma bei dielektrischer Oberflächenentladung und Mikrohohlkathoden-Entladung N2 - Die physikalische Komplexität der Gasentladungen führt zu vielen Möglichkeiten für die Interaktion der Entladung mit ihrer Umgebung. Zu den typischen Anwendungen zählen Modifikationen der Materialoberflächen und Erzeugung von Ionen für Massenspektroskopie. Atmosphärendruckplasma generiert eine große Menge thermischer Energie wegen der Kollisionen in der Plasmarandschicht. Eine rasche Temperaturänderung kann in dem umgebenden Gas eine akustische Welle erzeugen, wie beim Blitz und Donner, was als thermoakustischer Effekt bekannt ist. Außerdem kann auch die Bewegung der Ladungsträger im elektrischen Feld, bekannt als ionischer Wind, eine akustische Welle erzeugen. In diesem Beitrag werden Versuche mit akustischer Emission von Plasma bei dielektrischer Oberflächenentladung und bei Mikrohohlkathoden dargestellt. Es werden auch mögliche Anwendungen für Plasmadiagnostik, sowie für den Bau von Schallwandlern für den Hör- und Ultraschallbereich präsentiert. Verglichen mit anderen Methoden der Schallerzeugung, hat die thermoakustische Anregung den Vorteil, dass sie auch ohne eine schwingende Masse auskommt, womit eine große Bandbreite erreicht wird, sowie den Vorteil einer guten Anpassung der akustischen Impedanz. T2 - 4. Workshop des Fachausschusses Ultraschall der DEGA e.V. CY - Kloster Drübeck, Germany DA - 18.06.2018 KW - Plasmadiagnostik KW - Plasma KW - Atmosphärendruckplasma KW - Akustik KW - Ultraschall KW - Luftultraschall PY - 2018 AN - OPUS4-45305 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Schadow, Florian A1 - Nielow, Dustin A1 - Trappe, Volker T1 - Prüfung von Rotorblattschalen mit Luftultraschall N2 - Um den sicheren Betrieb von Windkraftanlagen zu gewährleisten, werden Rotorblätter nach der Fertigung und nach Reparatur mit verschiedenen zerstörungsfreien Verfahren auf Schaden untersucht. Bei der Fertigung von Blattschalen, die in einer Sandwich-Schalenbauweise gefertigt werden, entstehen Imperfektionen, die unter Belastung zu großen Rissen führen können. Zur Prüfung von Blattschalen wird unter anderem Ultraschallprüfung in Kontakttechnik eingesetzt. Um den Wartungsaufwand von Ultraschallanlagen zu reduzieren und um manche Kompositstrukturen vor Koppelmittel zu schützen, wird die Anwendung von Luftultraschall erforscht. Insbesondere große Fortschritte gibt es im Bereich der Entwicklung neuer Wandler. In diesem Beitrag berichten wir über die Luftultraschallprüfung von Schalen für Rotorblätter. Es wurden typische Sandwichschalenstrukturen hergestellt und mit einem eigenentwickelten Schalenprüfstand unter simulierter Betriebsbeanspruchung belastet. Die in den Schalenprüfkörpern entstandenen Schäden wurden außerhalb des Prüfstandes mit Luftultraschall in Durchschallung untersucht. Es wurden fokussierende Wandler auf Basis von Ferroelektreten entwickelt und für diese Prüfungen eingesetzt. Mit zusätzlicher elektrischer Vorspannung konnte die Empfindlichkeit der Empfänger deutlich erhöht werden. Die nach dem Lastwechsel entstandenen Schäden in den Rotorblattschalen waren eindeutig zu detektieren. T2 - DGZfP-Jahrestagung CY - Leipzig, Germany DA - 07.05.2018 KW - Wandler KW - Rotorblattschalen KW - Luftultraschall KW - Ferroelektret PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453066 SP - 7 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung e.V. (DGZfP) AN - OPUS4-45306 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Prüfung von Rotorblattschalen mit Luftultraschall N2 - Um den sicheren Betrieb von Windkraftanlagen zu gewährleisten, werden Rotorblätter nach der Fertigung und nach Reparatur mit verschiedenen zerstörungsfreien Verfahren auf Schaden untersucht. Bei der Fertigung von Blattschalen, die in einer Sandwich-Schalenbauweise gefertigt werden, entstehen Imperfektionen, die unter Belastung zu großen Rissen führen können. Zur Prüfung von Blattschalen wird unter anderem Ultraschallprüfung in Kontakttechnik eingesetzt. Um den Wartungsaufwand von Ultraschallanlagen zu reduzieren und um manche Kompositstrukturen vor Koppelmittel zu schützen, wird die Anwendung von Luftultraschall erforscht. Insbesondere große Fortschritte gibt es im Bereich der Entwicklung neuer Wandler. In diesem Beitrag berichten wir über die Luftultraschallprüfung von Schalen für Rotorblätter. Es wurden typische Sandwichschalenstrukturen hergestellt und mit einem eigenentwickelten Schalenprüfstand unter simulierter Betriebsbeanspruchung belastet. Die in den Schalenprüfkörpern entstandenen Schäden wurden außerhalb des Prüfstandes mit Luftultraschall in Durchschallung untersucht. Es wurden fokussierende Wandler auf Basis von Ferroelektreten entwickelt und für diese Prüfungen eingesetzt. Mit zusätzlicher elektrischer Vorspannung konnte die Empfindlichkeit der Empfänger deutlich erhöht werden. Die nach dem Lastwechsel entstandenen Schäden in den Rotorblattschalen waren eindeutig zu detektieren. T2 - DGZfP-Jahrestagung CY - Leipzig, Germany DA - 07.05.2018 KW - Wandler KW - Rotorblattschalen KW - Luftultraschall KW - Ferroelektret PY - 2018 AN - OPUS4-45307 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane A1 - Heckel, Thomas A1 - Brackrock, Daniel A1 - Gower, M. A1 - Lodeiro, M. A1 - Baker, G. T1 - Quantitative comparison of different non-destructive techniques for the detection of artificial defects in GFRP N2 - In order to test their suitability different non-destructive methods were performed to inspect a GFRP plate with artificial defects. These defects were manufactured by means of thin PTFE sheets inserted between two plies in three different depth. The inspection methods were microwave reflection, flash thermography and phased array ultrasonics, all applied to the same specimen. Selected results are shown for all methods demonstrating opportunities and limits of the particular inspection methods. The achieved detection limits and further application aspects are compared directly to provide a useful information for the planning of inspection tasks. T2 - ECNDT CY - Gothenburg, Sweden DA - 11.06.2018 KW - Fiber resisted polymers KW - Non-destructive testing KW - Thermographic testing KW - Ultrasonic testing PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453728 SP - ECNDT-0247-2018 AN - OPUS4-45372 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Ziegler, Mathias A1 - Maierhofer, Christiane ED - Maldague, X. T1 - Systematic errors in the evaluation of uncorrected data from thermographic lock-in measurements N2 - Lock-in thermography (LT) is based on the correct evaluation of phase differences between the temperature oscillations at different surface regions of the object under test during periodic heating. Since the usual heating procedures contain a DC component, the actual heating pattern achieved is not harmonic. This causes systematic deviations when phase differences are determined by means of harmonic analysis, e.g. with FFT analysis. The resulting errors depend clearly on the ratio between DC and AC amplitude, which is demonstrated at simulated and experimentally recorded temperature transients. Further experimental LT data obtained by different oscillating energy inputs showed a variety of possible shapes of transients with different DC components. T2 - 14th QIRT Conference CY - Berlin, Germany DA - 26.06.2018 KW - NDT KW - Lock-in Thermography KW - FFT PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453768 SP - 539 EP - 547 PB - QIRT Council AN - OPUS4-45376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer T1 - Systematic errors in the evaluation of uncorrected data from thermographic lock-in measurements N2 - Lock-in thermography (LT) is based on the correct evaluation of phase differences between the temperature oscillations at different surface regions of the object under test during periodic heating. Since the usual heating procedures contain a DC component, the actual heating pattern achieved is not harmonic. This causes systematic deviations when phase differences are determined by means of harmonic analysis, e.g. with FFT analysis. The resulting errors depend clearly on the ratio between DC and AC amplitude, which is demonstrated at simulated and experimentally recorded temperature transients. Further experimental LT data obtained by different oscillating energy inputs showed a variety of possible shapes of transients with different DC components. T2 - 14th QIRT Conference CY - Berlin, Germany DA - 26.6.2018 KW - Lock-in thermography KW - Non-destructive testing KW - FFT PY - 2018 AN - OPUS4-45377 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Fischer, S. A1 - Grauel, Bettina A1 - Alivisatos, A. P. A1 - Resch-Genger, Ute T1 - Quantum Yields, Surface Quenching, and Passivation Efficiency for Ultrasmall Core/Shell Upconverting Nanoparticles N2 - We synthesized and characterized a set of ultrasmall hexagonal-phase NaGdF4: 20% Yb3+, 2% Er3+ upconversion nanoparticles with core diameters of 3.7 ± 0.5 nm. In order to assess passivation effects and the influence of possible core−shell intermixing and to identify optimum particle structures for combined imaging in the visible and near-infrared (vis−NIR: 410−850 nm) and short-wave infrared (SWIR: 1520 nm), NaYF4 shells of varying thicknesses (monolayer to 10 nm) were introduced and the influence of this parameter on the upconversion and downshifting photoluminescence of these particles was studied at different excitation power densities. This included excitation power-dependent emission spectra, slope factors, quantum yields, and excited state decay kinetics. These measurements revealed enhancement factors of the upconversion quantum yield of >10 000 in the low power region and an excitation power density-independent quantum yield of the downshifted emission at 1520 nm between 0.1 and 14%. The optimized shell thickness for combined vis and SWIR imaging was identified as 5 nm. Moreover, lifetimes and quantum yields can be continuously tuned by shell thickness which can be exploited for lifetime multiplexing and encoding. The fact that we did not observe a saturation of the upconversion quantum yield or the excited state decay kinetics with increasing shell thickness is ascribed to a strong intermixing of the active core with the inert shell during the shelling procedure. This indicates the potential of spectroscopic tools to detect cation intermixing. KW - Nanoparticle KW - Upconversion KW - Quenching PY - 2018 DO - https://doi.org/10.1021/jacs.8b01458 IS - 140 SP - 4922 EP - 4928 PB - American Chemical Society AN - OPUS4-45378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst A1 - Ertel, J.-P. T1 - Foundations N2 - Overview on NDT methods for foundations as a preparation for the practical training T2 - NDT&E Advanced Training Workshop CY - Berlin, Germany DA - 27.06.2018 KW - Nondestructive testing KW - Foundations KW - Pile KW - Integrity PY - 2018 AN - OPUS4-45362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard A1 - Kunisch, E. A1 - Kinne, R. W. T1 - Micro-CT begleitete in-situ Druckversuche an spongiösem Knochen - Vergleich(ende Bestimmung) des experimentellen und simulierten Verschiebungsfeldes mit der simulierten internen Spannung N2 - Untersuchungen haben gezeigt, dass sich ältere Schafe gut als Modell für die mi-nimalinvasive Behandlung von Osteoporose eignen [1]. Um einen Behandlungs-effekt nachzuweisen, wird dabei unter anderem die Belastungsfähigkeit des Kno-chens durch Druckversuche an kleinen Zylindern aus den behandelten und unbe-handelten Knochen bestimmt. Diese hatten hier einen Durchmesser von 10 mm und eine Höhe von 13 mm. Für den in-situ Druckversuch wurde eine Deben CT5000 verwendet. In einer Serie von Druckerhöhungen wurden die Proben je-weils tomographiert. Dabei ergab sich zunächst, dass mit der µCT innerhalb der Knochen im oberen und unteren Bereich schon Brüche nachgewiesen werden können, obwohl die gemessene Kraftaufnahmekurve keine Unstetigkeit zeigt. Deswegen wurden die starren Probenaufnehmer der Deben Anordnung durch bewegliche Aufnehmer ergänzt, die eine leichte Verkippung der belasteten Ober-flächen ausgleichen können. Ein Vergleich der gemessenen und der aus den µCT-Daten berechneten Verschiebungsfelder ergab trotz der komplexen Struktur der Knochen gute Übereinstimmungen. Diese Verschiebungen wurden dann mit den aus den µCT Daten simulierten mechanischen Druckversuchen, Von-Mise-Spannungen und daraus berechneten Verschiebungen verglichen. (VGStudioMax Simulation). T2 - DGZfP-Jahrestagung CY - Leipzig, Germany DA - 07.05.2018 KW - Computer Tomographie KW - In-situ Druckversuch KW - Simulation PY - 2018 AN - OPUS4-44883 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard A1 - Joschko, M. A1 - Walla, M. A1 - Barkusky, D. A1 - Gerlach, F. T1 - Wunderwelt der Mikro-Computertomografie: Die Wurzeln des Raps N2 - Mit Hilfe der Computertomographie können zerstörungsfrei Bilder des Bodengefüges gewonnen werden. Sowohl die verschiedene Dichte des Bodens als auch Hohlräume und Poren sowie Wurzeln und anderes organisches Material können dargestellt werden. Die Wurzeln werden dabei lagerichtig wiedergegeben. Begrenzt wird dieses durch die Ortsauflösung des jeweiligen Tomogramms. Ist die Methode für eine Fragestellung aus der landwirtschaftlichen Praxis – Einfluss der Bodenbearbeitung auf das Wurzelbild von Raps – geeignet? T2 - BraLa 2018 CY - Paaren, Germany DA - 10.05.2018 KW - Computertomographie KW - Bodenstruktur PY - 2018 AN - OPUS4-44884 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Already producing or still calibrating? – Online NMR spectroscopy as smart field device N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. Industry 4.0, IIoT, or Lab 4.0 will enable us to handle more complex processes in shorter time. Intensified production concepts require for adaptive analytical instruments and control technology to realize short set-up times, modular control strategies. They are based on a digitized Laboratory 4.0. T2 - GA-Conference CY - BASF, Ludwigshafen, Germany DA - 16.05.2018 KW - Process Monitoring KW - Online NMR Spectroscopy KW - Industrie 4.0 KW - Indirect Hard Modeling KW - Laboratory 4.0 KW - CONSENS PY - 2018 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-44895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Dai, X. A1 - Zhang, W. A1 - Li, H. A1 - Huang, T. A1 - Li, M. A1 - Quan, C. A1 - Zhang, Q. A1 - Davies, S. R A1 - Warren, J. A1 - Lo, M.-F. A1 - Kakoulides, E. A1 - Ceyhan Gören, A. A1 - Marbumrung, S. A1 - Pfeifer, Dietmar A1 - Ün, I. A1 - Gündüz, S. A1 - Yilmaz, H. A1 - Kankaew, P. A1 - Sudsiri, N. A1 - Shearman, K. A1 - Pookrod, P. A1 - Polzer, J. A1 - Radeck, W. T1 - CCQM-K104 Key Comparison on the characterization of organic substances for chemical purity - Avermectin B1a N2 - Anwendungen von qNMR KW - qNMR PY - 2017 SP - 1 EP - 32 AN - OPUS4-45035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - van Schaik, S. A1 - Helman-Wazny, A. A1 - Nöller, Renate T1 - Writing, painting and sketching at Dunhuang: assessing the materiality and function of early Tibetan manuscripts and ritual items N2 - The paintings and manuscripts discovered in the sealed ‘library cave’ in Dunhuang, Western China, contain the earliest surviving examples of Tibetan artistic and scribal practice (9the10th centuries AD). Despite their importance, their material characteristics have not previously been studied. The present paper discusses the results of the analysis of paper and pigments in a selection of items across a variety of forms and functions: (i) Buddhist manuscripts, (ii) official letters, (iii) hung paintings, (iv) ritual items, (v) banners, and (vi) stencils and preliminary sketches. The material analysis of these items is presented in historical context, to address three research questions. First, whether there is a correspondence between the materials used in the creation of these objects and their geographical origin. Second, in terms of the choices made in the available materials and techniques, whether there is a detectable correlation between materials chosen and the intended function of the objects. Third, whether the characteristics of the objects analysed here be considered to be part of a broader Central Asian artistic and scribal culture. The authors conclude that a local culture of paper and pigment production can be detected in these results, though further research is needed especially on the geographical origin of raw materials for pigments. The results show that artists and scribes made technological choices in paper and pigments depending on the function of the objects they were creating. Finally, understanding of the broader Central Asian context of these results will depend on future analysis of material from other archaeological sites, and comparison with the results of this study. KW - Tibetan Dunhuang manuscripts KW - VIS KW - XRF KW - Fibre analysis PY - 2014 DO - https://doi.org/10.1016/j.jas.2014.09.018 VL - 53 SP - 110 EP - 132 PB - Elsevier Ltd. AN - OPUS4-44766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beyer, Sebastian A1 - Schürmann, Robin A1 - Feldmann, Ines A1 - Blocki, A. A1 - Bald, Ilko A1 - Schneider, Rudolf A1 - Emmerling, Franziska T1 - Maintaining Stable Zeolitic Imidazolate Framework (ZIF) Templates during Polyelectrolyte Multilayer Coating N2 - Equipping ZIF particles with a polyelectrolyte membrane provides functional groups at their interface, enabling further conjugations necessary for applications such as targeted drug delivery. Previous approaches to coat ZIF particles with polyelectrolytes led to surface corrosion of the template material. This work overcomes previous limitations by performing a Layer-by-Layer (LbL) polyelectrolyte coating onto ZIF-8 and ZIF-67 particles in nonaqueous environment. Using the 2-methylimidazolium salt of polystyrensulfonic acid instead of the acid itself and polyethyleneimine in methanol led to intact ZIF particles after polyelectrolyte coating. This was verified by electron microscopy. Further, zetapotential and atomic force microscopy measurements confirmed a continuous polyelectrolyte multilayer built up. The here reported adaption to the well-studied (LbL) polyelectrolyte selfassembly process provides a facile method to equip ZIF particles with a nanometer thin polyelectrolyte multilayer membrane. KW - Zeolithe KW - Molecular Organic Frameworks KW - MOF KW - ZIF KW - Layer-by-Layer KW - Beschichtung KW - Polyelektrolyt PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-447729 DO - https://doi.org/10.1016/j.colcom.2017.11.004 SN - 2215-0382 VL - 22 SP - 14 EP - 17 PB - Elsevier B.V. CY - Amsterdam, NL AN - OPUS4-44772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumacher, David A1 - Meyendorf, N. A1 - Hakim, I. A1 - Ewert, Uwe ED - Chimenti, D. E. ED - Bond, L. J. T1 - Defect recognition in CFRP components using various NDT methods within a smart manufacturing process N2 - The manufacturing process of carbon fiber reinforced polymer (CFRP) components is gaining a more and more significant role when looking at the increasing amount of CFRPs used in industries today. The monitoring of the manufacturing process and hence the reliability of the manufactured products, is one of the major challenges we need to face in the near future. Common defects which arise during manufacturing process are e.g. porosity and voids which may lead to delaminations during operation and under load. To find irregularities and classify them as possible defects in an early stage of the manufacturing process is of high importance for the safety and reliability of the finished products, as well as of significant impact from an economical point of view. In this study we compare various NDT methods which were applied to similar CFRP laminate samples in order to detect and characterize regions of defective volume. Besides ultrasound, thermography and eddy current, different X-ray methods like radiography, laminography and computed tomography are used to investigate the samples. These methods are compared with the intention to evaluate their capability to reliably detect and characterize defective volume. Beyond the detection and evaluation of defects, we also investigate possibilities to combine various NDT methods within a smart manufacturing process in which the decision which method shall be applied is inherent within the process. Is it possible to design an in-line or at-line testing process which can recognize defects reliably and reduce testing time and costs? This study aims to show up opportunities of designing a smart NDT process synchronized to the production based on the concepts of smart production (Industry 4.0). A set of defective CFRP laminate samples and different NDT methods were used to demonstrate how effective defects are recognized and how communication between interconnected NDT sensors and the manufacturing process could be organized. T2 - 44TH ANNUAL REVIEW OF PROGRESS IN QUANTITATIVE NONDESTRUCTIVE EVALUATION CY - Provo, Utah, USA DA - 16.07.2017 KW - Carbon fiber reinforced polymers KW - Non-destructive testing KW - Smart industry (4.0) KW - Ultrasound KW - Laminography KW - Serial sectioning KW - Computed tompgraphy PY - 2018 SN - 978-0-7354-1644-4 DO - https://doi.org/10.1063/1.5031521 SN - 0094-243X VL - 1949 SP - UNSP 020024, 1 EP - 11 PB - AIP Publishing AN - OPUS4-44773 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Nützmann, Kathrin A1 - Kranzmann, Axel A1 - Klaus, M. A1 - Genzel, C. T1 - Real time observation of high temperature oxidation and sulfidation of Fe-Cr model alloys N2 - Insights into early damage mechanisms during high-temperature gas corrosion provide important aspects for the prediction of the long-term stability of hightemperature materials exposed to a hot and corrosive environment. The current work presents a real time study concerning the combined oxidation and sulfidation of ferritic model alloys in a hot SO2 containing atmosphere using energy dispersive X-ray diffraction. The applied high temperature reactor allows the transmittance of high energetic X-rays in order to collect X-ray diffraction pattern of the sample surface in situ during the reaction with the reactive environment. The results revealed that the first phases crystallizing on iron with 2 wt% chromium and with 9 wt% chromium are oxides. The aging experiments at T = 650° C with 0.5% SO2 and 99.5% Ar were followed in situ and caused an external mixed oxide-sulfide layer on top of iron with 2 wt% chromium. On the higher alloyed material the external scale consists of iron oxides and the inner scale of mixed (Fe,Cr)-oxides and chromium-sulfides. The oxide content continuously increases parallel to an increase of the sulfide amount. Thus, the initially formed (Fe,Cr)-oxides do not have a protective character and support the transport of sulfur through the growing oxide scale. KW - High temperature corrosion KW - In situ diffraction KW - Sulfidation PY - 2018 DO - https://doi.org/10.1002/maco.201709892 SN - 0947-5117 VL - 69 IS - 6 SP - 678 EP - 689 PB - Wiley VCH Verlag AN - OPUS4-44776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias A1 - Stegemann, Robert A1 - Sonntag, Nadja A1 - Pohl, Rainer A1 - Kreutzbruck, Marc T1 - Benefits of GMR sensors for high spatial resolution NDT applications N2 - Magneto resistance sensors like GMR (giant magneto resistance) or TMR (tunnel magneto resistance) are widely used in industrial applications, examples are position measurement and read heads of hard disk drives. However, in case of non-destructive testing (NDT) applications these sensors, although their properties are outstanding like high spatial resolution, high field sensitivity, low cost and low energy consumption, never reached a technical transfer to an application beyond sci-entific scope. This paper deals with benefits of GMR/TMR sensors in terms of high spatial resolution testing for different NDT applica-tions. The first example demonstrates the preeminent advantages of MR-elements compared with conventional coils used in eddy current testing (ET). The probe comprises one-wire excitation with an array of MR elements. This led to a better spatial resolution in terms of neighboring defects. The second section concentrates on MFL-testing (magnetic flux leakage) with active field excitation during and before test-ing. The latter illustrated the capability of highly resolved crack detection of a crossed notch. This example is best suited to show the ability of tiny magnetic field sensors for magnetic material characterization of a sample surface. Another example is based on characterization of samples after tensile test. Here, no external field is applied. The magnetization is only changed due to external load and magnetostriction leading to a field signature which GMR sensors can resolve. This gives access to internal changes of the magnetization state of the sample under test. T2 - QNDE 2017 CY - Provo, Utah, USA DA - 16.07.2017 KW - GMR KW - Non-destructive testing KW - Sensor arrays KW - Spatial resolution PY - 2018 SN - 978-0-7354-1644-4 DO - https://doi.org/10.1063/1.5031535 SN - 0094-243X VL - 1949 SP - UNSP 040001, 1 EP - 10 AN - OPUS4-45050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf A1 - Pohl, Rainer A1 - Munzke, Dorit A1 - Becker, Ben A1 - Pelkner, Matthias T1 - Eddy current testing of composite pressure vessels N2 - The use of composite pressure vessels instead of conventional vessels made of steel or aluminum grew strongly over the last decade. The reason for this trend is the tremendous weight saving in case of composite vessels. However, the long-time behavior is not fully understood for filling and discharging cycles and creep strength and their influence on the CFRP coating (carbon fiber reinforced plastics) and the internal liner (steel, aluminum, or plastics). The CFRP ensures the pressure resistance while the inner liner is used as container for liquid or gas. To overcome the missing knowledge of ageing BAM started an internal project to investigate degradation of these material systems. Therefore, applicable testing methods like eddy current testing are needed. Normally, high-frequency eddy current testing (HF-ET, f > 10 MHz) is deployed for CFRP due to its low conductivity of the fiber, which is in the order of 0.01 MS/s, and the capacitive coupling between the fibers. Nevertheless, in some cases conventional ET can be applied. We show a concise summary of studies on the application of conventional ET of composite pressure vessels. T2 - QNDE 2017 CY - Provo, Utah, USA DA - 16.07.2017 KW - Eddy current KW - Composite KW - Pressure vessel PY - 2018 SN - 978-0-7354-1644-4 DO - https://doi.org/10.1063/1.5031622 SN - 0094-243X VL - 1949 SP - UNSP 160004, 1 EP - 8 AN - OPUS4-45051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abbas, Ioana M. A1 - Hoffmann, Holger A1 - Montes-Bayón, M. A1 - Weller, Michael G. T1 - Improved LC-MS/MS method for the quantification of hepcidin-25 in clinical samples N2 - Mass spectrometry-based methods play a crucial role in the quantification of the main iron metabolism regulator hepcidin by singling out the bioactive 25-residue peptide from the other naturally occurring N-truncated isoforms (hepcidin-20, -22, -24), which seem to be inactive in iron homeostasis. However, several difficulties arise in the MS analysis of hepcidin due to the sticky character of the peptide and the lack of suitable standards. Here, we propose the use of amino- and fluoro-silanized autosampler vials to reduce hepcidin interaction to laboratory glassware surfaces after testing several types of vials for the preparation of stock solutions and serum samples for isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS). Furthermore, we have investigated two sample preparation strategies and two chromatographic separation conditions with the aim of developing an LC-MS/MS method for the sensitive and reliable quantification of hepcidin-25 in serum samples. A chromatographic separation based on usual acidic mobile phases was compared with a novel approach involving the separation of hepcidin-25 with solvents at high pH containing 0.1% of ammonia. Both methods were applied to clinical samples in an intra-laboratory comparison of two LC-MS/MS methods using the same hepcidin-25 calibrators with good correlation of the results. Finally, we recommend an LC-MS/MS-based quantification method with a dynamic range of 0.5–40 μg/L for the assessment of hepcidin-25 in human serum that uses TFA-based mobile phases and silanized glass vials. KW - HPLC KW - Liquid chromatography KW - Mass spectrometry KW - Silanization KW - Mobile phase KW - Adsorption KW - Peptide losses KW - Recovery KW - Validation KW - Quality control KW - QC KW - Iron disorders KW - Chronic kidney disease KW - Metrology KW - Round robin exercise KW - Basic solvent KW - Peptide analysis PY - 2018 DO - https://doi.org/10.1007/s00216-018-1056-0 SN - 1618-2642 SN - 1618-2650 VL - 410 IS - 16 SP - 3835 EP - 3846 PB - Springer Nature CY - Heidelberg AN - OPUS4-45053 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Juds, Carmen T1 - Finding peptide binders for polypropylene using phage display and next generation sequencing N2 - Phage display is used to find specific target binding peptides for polypropylene (PP) surfaces. PP is one of the most commonly used plastics in the world. Millions of tons are produced every year. PP binders are of particular interest because so far gluing or printing on PP is challenging due to its low surface energy. A phage display protocol for PP was developed followed by Next Generation DNA Sequencing of the whole phage library. Data analysis of millions of sequences yields promising peptide candidates which were synthesized as PEG conjugates. Fluorescence-based adsorption-elution-experiments show high adsorption on PP for several sequences. T2 - BAM PhD Day CY - Berlin-Adlershof, Germany DA - 31.05.2018 KW - Polymer KW - Glue KW - Amplification KW - Illumina KW - PEG KW - Sanger sequencing KW - SALSA KW - Data analysis KW - Fluorescence PY - 2018 AN - OPUS4-45055 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Swaraj, S. A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Shell thickness determination for PTFE‐PS core‐shell nanoparticles using scanning transmission X‐ray microscopy (STXM) N2 - A scanning transmission X‐ray microscopy (STXM)‐based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core‐shell nanoparticles, which exhibit a strong X‐ray absorption contrast and a well‐defined interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less X‐ray beam‐induced damage of the sample is achieved by recording STXM images only at 2 predetermined energies of maximum Absorption contrast, instead of recording a stack of images across the whole absorption edge. A model core‐shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, is used for demonstration. Near‐edge X‐ray absorption fine structure spectroscopy confirms the significant difference in X‐ray absorption behavior between PTFE and PS. Additionally, because of the insolubility of styrene in PTFE a well‐defined interface between particle core and shell is expected. To validate the STXM results, both the naked PTFE cores as well as the complete core‐shell nanoparticles are examined by scanning electron microscopy (SEM). The introduced STXM‐based methodology yields particle dimensions in agreement with the SEM results and provides additional information such as the position of the particle core, which cannot be extracted from a SEM micrograph. T2 - European conference on applications of surface and interface analysis (ECASIA'17) CY - Montpellier, France DA - 24.09.2017 KW - Core-shell nanoparticles KW - Polymers KW - PS KW - PTFE KW - SEM KW - STXM PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-449700 DO - https://doi.org/10.1002/sia.6464 SN - 1096-9918 SN - 0142-2421 VL - 50 IS - 11 SP - 1077 EP - 1082 PB - John Wiley & Sons CY - Hoboken, New Jersey, USA AN - OPUS4-44970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Particles in PVD-coatings: Imperfection or functional add-on feature? N2 - The application of PVD-coatings ranges from mechanical engineering, i.e. thicker tribological coatings, to precision optics, i.e. thinner optical coatings. For physical vapor deposition (PVD) technologies such as evaporation, sputtering, ion beam assisted/driven deposition, vacuum is a prerequisite for two reasons: at first process-related ones (evaporation source, plasma discharge, and mean free path) and at second coating-related ones (pure, perfect, and dense films). Usually, the goal is a homogenous coating of defined stoichiometry and micro-structure without any imperfection. However, the implementation of micro- or nano-particles may occur accidentally or delibe-rately. Independent of the particle origin, there are two fundamental rules regarding coating functionality: at first, the larger the particle diameter to coating thickness ratio the more affected the functionality of the coating, and at second, the larger the material contrast in terms of the functional feature of interest the more affected the coating performance. Hence, embedded particles have to be avoided for the majority of thin films by all means. The unintended implementation of particles usually results in a malfunction of the coating from the beginning or is at least considered as a weak point of the coating creating a time-dependent defect under service conditions. The intended implementation of particles on surfaces and in coatings may create add-on features, topographic ones and functional ones, however, the facts mentioned hold true. Examples of particle-initiated coating defects are demonstrated in dependence on the origin and the field of application. Strategies for deliberate attachment/embedding of particles on surfaces/in coatings are discussed regarding process compatibility and coating integrity. For industrial applications, both the validation of process compatibility of particle injection and the plasma resistance of particles under vacuum and plasma conditions have to be confirmed. Further points of interest are the homogeneity of particle distribution and the avoidance of particle agglomeration which is still a crucial point for dry dispersed particles. So far, technical applications are limited to PVD hybrid coatings, plasma dispersion coatings are still a challenge except for applications where homogeneity is not required as in case of product authentication. T2 - ICMCTF 2018, International Conference on Metallurgical Coatings and Thin Films CY - San Diego, CA, USA DA - 23.04.2018 KW - PVD-coatings KW - PVD-processes KW - Unintended particle generation KW - Particles as imperfections KW - Deliberate particle implementation KW - Particles as add-on features PY - 2018 AN - OPUS4-44973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zauer, M. A1 - Prinz, Carsten A1 - Adolphs, J. A1 - Emmerling, Franziska A1 - Wagenführ, A. T1 - Sorption surfaces and energies of untreated and thermally modified wood evaluated by means of excess surface work (ESW) N2 - Water vapor sorption surface areas and sorption energies of untreated and thermally modified Norway spruce [Picea abies (L.) Karst.], sycamore maple (Acer pseudoplatanus L.) and European ash (Fraxinus excelcior L.) were investigated by means of dynamic vapor sorption (DVS) measurements and excess surface work (ESW) evaluation method, respectively. Adsorption and desorption experiments in the hygroscopic range and desorption tests from water saturation were conducted. Thermodynamically, ESW is the sum of the surface free energy and the isothermal isobaric work of sorption. From the amount adsorbed in the first Minimum a specific surface area similar to the BET surface area can be obtained. The results show that untreated spruce has a significantly higher specific water vapor Sorption surface and sorption energy compared to both hardwoods maple and ash. Thermal modification of the woods leads to a significant reduction of water vapor Sorption surface and sorption energy. The determined surface area and energy are higher in desorption direction than in adsorption direction, whereby the highest values in Desorption direction from water saturation, especially for maple and ash, were obtained. The surface areas calculated by means of the ESW method are similar to the surface areas calculated by means of the BET method, particularly in adsorption direction. KW - Excess surface work KW - Dynamic vapor sorption KW - Wood KW - BET PY - 2018 DO - https://doi.org/10.1007/s00226-018-1021-2 SN - 1432-5225 SN - 0043-7719 VL - 52 IS - 4 SP - 957 EP - 969 PB - Springer CY - Berlin Heidelberg AN - OPUS4-44975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Multi-functional coatings for optical sensor applications: Surface plasmon resonance & magneto-optical coupling N2 - Multi-functional coatings are a key requirement for surface engineering. General demands are adhesion and long-term stability under service conditions. The modification of surfaces by means of PVD-, ECD- or hybrid processes allows an add-on functionalization of surfaces by a huge diversity of materials with both lateral and vertical micro-/nano-designs. This fact is a prerequisite for micro- and sensor-systems in lab-on-chip and sensor-on-chip technology. Two layer-based sensor principles are presented, i.e. surface plasmon resonance enhanced spectroscopic ellipsometry (SPREE) for detection of hazardous gases and magneto-optical sensors on smart-coated fiber Bragg gratings (FBG) for structural health monitoring (SHM). The interdependence of substrate features, coating properties, and layer design is discussed firstly for gas sensitivity and selectivity of SPREE-sensors and secondly for sensitivity and selectivity of magneto-strictive coatings to mechanical strain or external magnetic fields resulting in an optical displacement of the Bragg wavelength of FBG-sensors. Moreover, generic features such long-term stability, crucial process-related fabrication conditions, and effects of operational and environmental parameters are discussed with respect to the sensor performance. It has been shown that appropriate layer design and adapted selection of layer materials (SnOx/Au, Fe/Ni:SnOx/Au; Ni/NiFe-Cu-Cr) result in improved sensor parameters and may enable new sensor applications. T2 - SVC TechCon 2018 CY - Orlando, FL, USA DA - 05.05.2018 KW - Multi-functional coatings for sensors KW - Surface plasmon resonance enhanced ellipsometry (SPREE) KW - Gas monitoring KW - Magneto-optical coupling (MOC) KW - Structural health monitoring (SHM) PY - 2018 AN - OPUS4-44976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zhang, Zeyu A1 - Weller, Andreas T1 - Beobachtung der Trocknung von Gesteinen mit Spektraler Induzierter Polarisation N2 - Bei der Trocknung von Gesteinen vermindert sich der Anteil des Wasservolumens im Porenraum, der als Sättigung bezeichnet wird. Mit abnehmender Sättigung sinkt die elektrische Leitfähigkeit des Gesteins. Die Abhängigkeit der elektrischen Leitfähigkeit von der Sättigung wird durch ein Potenzgesetz entsprechend der 2. Archie-Gleichung beschrieben: log(#CHR:sigma_LOWER#)=n log(Sw), wobei n der Sättigungsexponent ist. Bei der Trocknung von Gesteinen muss beachtet werden, dass die Wasserleitfähigkeit mit abnehmender Sättigung zunimmt, da die Konzentration der im Wasser gelösten Salze ansteigt. Das hat zur Folge, dass die bei Trocknungsexperimenten bestimmten Sättigungsexponenten deutlich kleiner sind als bei Verdrängungsexperimenten (z.B. Wasser durch Öl) mit gleichbleibender Wasserleitfähigkeit. Bei der Spektral(en) Induzierten Polarisation wird die komplexe elektrische Leitfähigkeit des Gesteins als Funktion der Frequenz betrachtet. Für den Real- und Imaginärteil der elektrischen Leitfähigkeit werden unterschiedliche Sättigungsexponenten bestimmt. Wir haben an zwei Sandsteinproben (Langenauer und Gravenhorster Sandstein) und einem Baumberger Kalksandstein Trocknungsexperimente durchgeführt. Die Sättigung wurde schrittweise von 100 % bis auf 10 % reduziert. In jeder Sättigungsstufe wurden an den Proben die Spektren der komplexen elektrischen Leitfähigkeit aufgezeichnet. Unsere Experimente zeigen, dass die Sättigungsexponenten für den Imaginärteil der komplexen elektrischen Leitfähigkeit mit 1,23 bis 1,59 deutlich größer sind als die des Realteils mit Werten zwischen 0,41 und 0,90. Dieser Unterschied resultiert aus der Tatsache, dass der Imaginärteil der Leitfähigkeit weniger stark mit zunehmender Wasserleitfähigkeit ansteigt als der Realteil. Für den Realteil der elektrischen Leitfähigkeit wird nach der 1. Archie-Gleichung ein linearer Zusammenhang zwischen Wasserleitfähigkeit und Gesteinsleitfähigkeit erwartet. Der Anstieg des Imaginärteils mit der Wasserleitfähigkeit kann mit einem Potenzgesetz mit einem Exponenten zwischen 0.1 und 0.62 beschrieben werden. Unsere Experimente zeigen, dass der Imaginärteil der elektrischen Leitfähigkeit wesentlich deutlicher auf die Austrocknung von Gesteinen reagiert und damit ein wirksamer Indikator zur Überwachung von Sättigungsänderungen sein kann. T2 - Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Leoben, Austria DA - 12.2.2018 KW - Spektral induzierte Polarisation KW - Sandsteine KW - Trocknung PY - 2018 AN - OPUS4-45000 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - NMR spectroscopy for online monitoring and process control N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example. Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). Based on concentration measurements of reagents and products by the NMR analyzer a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (“Integrated CONtrol and SENsing”, www.consens-spire.eu). T2 - REsearch and Development Seminar, Syngenta Crop Protection AG CY - Münchwilen, Switzerland DA - 22.05.2018 KW - Process monitoring KW - Online NMR spectroscopy KW - Indirect hard modeling KW - Benchtop NMR spectroscopy PY - 2018 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-45003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - NMR spectroscopy for online monitoring and process control N2 - Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example.Based on concentration measurements of reagents and products by the NMR analyzer a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme. T2 - Global Expert Meeting Analytical Quantification, Syngenta Crop Protection AG CY - Stein, Switzerland DA - 22.05.2018 KW - Process monitoring KW - Online NMR spectroscopy KW - Indirect hard modeling KW - Benchtop NMR spectroscopy PY - 2018 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-45004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Already producing or still calibrating? – Online NMR spectroscopy as smart field device N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example. Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). Based on concentration measurements of reagents and products by the NMR analyzer a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (“Integrated CONtrol and SENsing”, www.consens-spire.eu). T2 - Analytical Chemists Meeting, Syngenta Crop Protection Monthey SA CY - Monthey, Switzerland DA - 23.05.2018 KW - Process monitoring KW - Online NMR spectroscopy KW - Indirect hard modeling KW - Benchtop NMR spectroscopy KW - Direct loop control PY - 2018 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-45006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Büchele, Dominique T1 - Comparison between uni- and multivariate data analysis for the determination of nutrients in soils using XRF N2 - Aim of the Federal Institute for Materials Research and Testing (BAM) in the frame of I4S - “Intelligence for Soil” is the characterization of an X-ray fluorescence (XRF) based sensor for robust online-application of arable land.Fast soil mapping for agricultural purpose allows the site-specific optimized introduction of plant essential nutrients like S, K, Ca, and Fe. This is important given that the distribution of minor and trace elements varies widely. The non-destructive and contactless XRF is suitable for rapid in-situ analysis on the field due to minimal sample preparation and simultaneous multi-element analysis. Soils are already considered as a complex matrix due to their wide range of elements in different contents, especially light elements with low atomic numbers (Z<19). Problems by measuring soil samples also arise from heterogeneity of the sample and matrix effects. Large grain size distribution causes strong inhomogeneity and matrix effects occur through physical properties related to high concentration of main components. Matrix-specific calibration strategies for determination of total major and minor plant essential nutrients are particularly important regarding these difficulties. For accurate calibration, data treatment and evaluation must also be considered. Empirical univariate and multivariate data analysis were compared regarding their analytical figures of merit. Using principal component analysis (PCA) it was possible to classify German soils in different groups as sand, clay and silt. A calibration curve was obtained by partial least squares regression (PLSR) and the elemental content of German soils was predicted. Elemental distribution maps for different German arable lands were created and the results compared to reference measurements. The correlation between predicted values and reference values were in good agreement for most major and minor nutrients. T2 - BonaRes Conference CY - Berlin, Germany DA - 26.02.2018 KW - PLSR KW - XRF KW - Soil KW - PCA PY - 2018 AN - OPUS4-45007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Determination of plant essential nutrients in soils using DP-LIBS N2 - In respect of an efficient cultivation of agricultural cropland, a site-specific fertility management is necessary. Therefore, affordable and extensive mapping methods are needed. The research projects I4S (intelligence for soil) has the goal to develop a system for this purpose. I4S is one of ten interdisciplinary research project associations of the innovation programme called BonaRes, which is funded by the German Federal Ministry of Education and Research (BMBF). The system includes a sensor platform, which contains different sensors, like XRF, VIS-NIR, Gamma and LIBS. The main task of LIBS measurements in this project is the real-time determination of the elemental contents of major and minor nutrients in soils, like calcium, magnesium, potassium. LIBS (laser-induced breakdown spectroscopy) is known as a fast and simultaneous multi-element analysis with little or no sample preparation. The main task of LIBS measurements in this project is the real-time determination of the elemental contents of nutrients in soils, like calcium, magnesium, potassium. For this purpose, a special setup has been designed. The sample uptake operates with the help of a rotatable sample plate which circulates with different velocities to simulate the application on the field. To provide a higher intensity and a better reproducibility of the obtained signal, a double-pulse Nd:YAG laser (1064 nm)was used. In order to minimize dust formation from the soil during the operation of the laser, a dust removal by suction has been integrated. When using relative methods such as LIBS, a suitable calibration curve is needed for absolute quantification. The complex matrix of soils, as well as the influence of moisture and grain size in soils makes the absolute quantification by LIBS challenging. To overcome these influences, chemometric methods were used. With the principal component analysis (PCA) a classification of soils into different soil types was performed and a calibration curve based on partial least squares regression (PLSR) was generated. With this calibration model’s elemental distribution maps for different German agricultural fields were created. T2 - ESAS CANSAS CY - Berlin, Germany DA - 20.03.2018 KW - LIBS KW - Soil KW - PCA KW - PLSR PY - 2018 AN - OPUS4-45008 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - XPS at BAM - Some insights into our activities N2 - Some examples will be given showing the application of XPS in different fields, like polymers, nanoparticles, solar cells and inorganic thin films. T2 - Besuch beim GFZ Potsdam CY - Potsdam, Germany DA - 18.05.2018 KW - XPS KW - Surface analytics KW - Nanoparticles KW - Polymers KW - Solar cells PY - 2018 AN - OPUS4-44981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Simple and versatile methods for quantifying functional groups, ligands, and biomolecules on nanomaterials N2 - Many applications of nanomaterials in the life sciences require the controlled functionalization of these materials with ligands like polyethylene glycol (PEG) and/or biomolecules such as peptides, proteins, and DNA. This enables to tune their hydrophilicity and biocompatibility, minimize unspecific interactions, improve biofunction-nalization efficiencies, and enhance blood circulation times and is the ultimate prerequisite for their use as reporters in assays or the design of targeted optial probes for bioimaging. At the core of these functionalization strategies are reliable and validated methods for surface group and ligand quantification that can be preferably performed with routine laboratory instrumentation, require only small amounts of substances, and are suitable for many different types of nanomaterials. We present here versatile and simple concepts for the quantification of common functional groups, ligands, and biomolecules on different types of organic and inorganic nano-materials, using different types of optical reporters and method validation with the aid of multimodal reporters and mass balances. T2 - RSC Symposium on Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - PEG ligands KW - Surface group analysis KW - Upconverting nanoparticles KW - Integrating sphere spectroscopy KW - Absolute fluorescence quantum yield KW - Fluorescence decay kinetics PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-44986 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Controlled electrospray deposition of nanoparticles for improved analysis by electron microscopy N2 - Of many experimental techniques for measuring particle sizes and size distributions, electron microscopy (EM) is considered as the gold standard, especially in the nano range (1–100 nm). Furthermore, high-resolution X-ray spectroscopy (EDX) in conjunction with EM can be applied to individual NPs. Preparation of an EM sample for generic particulate materials is a difficult task. Usually, the particles in a suspension are deposited on a support. However, this procedure includes the drying of larger solvent amounts on the substrate itself, and this can affect the spatial distribution of the deposited particles. One possibility to overcome this is the use of an electrospray system, where the suspension of particles is sprayed onto the substrate in charged droplets that are so small that they either dry off on the substrate immediately without affecting the position of particles, or even already during their flight time to the substrate. Additionally, the charging of particles minimizes agglomeration and aggregation, maximizing the collection of the EM grids. The prototype of an electrospray deposition system from RAMEM under its trademark IONER (www.ioner.eu) was tested. Electrospray is theoretically described since a long time, but no dedicated commercial instruments are available for the preparation of TEM grids yet, apart from electrostatic deposition of aerosols. Several materials have been sprayed onto TEM grids and the resulting particle distributions were evaluated. Operation parameters such as the sample flow-rate, capillary – substrate distance, electric field strength and sampling period length have been optimized. It was found that the particles deposited by electrospray generally show a much more homogeneous spatial distribution on the substrate and a substantial increase of the number of single particles (suited to automatic analysis). The project has received funding from the European Union’s Seventh Programme for research, technological development and demonstration under grant agreement No 604347. T2 - NanoWorkshop 2018 (Workshop on reference nanomaterials, current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2018 KW - Nanoparticles KW - Electrospray KW - Electron microscopy PY - 2018 AN - OPUS4-44994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Improved traceability chain of nanoparticle size measurements – the new EMPIR project nPSize N2 - Coming as response to the needs expressed by The European Commission mandating CEN, CENELEC and ETSI to develop European standards for methods that can characterize reliably manufactured nanomaterials, a new European metrology research project ‘nPSize - Improved traceability chain of nanoparticle size measurements’ has received funding for the next three years. The project will develop methods, reference materials and modelling to improve the traceability chain, comparability and compatibility for nanoparticle size measurements to support standardization. nPSize has selected only those nanoparticle sizing techniques which are able to provide traceable results: electron microscopy (SEM, TSEM and TEM), AFM and SAXS. Metrologists from national metrological or designated institutes (PTB, LNE, LGC, VSL, SMD and BAM) will work together with scientists with know-how in development of new nano reference nanoparticles (CEA, University of Turin, LGC, BAM) and with experts in advanced data processing, e.g. by machine learning (POLLEN). With the support of DIN, the project outcomes will be channelized to standardization bodies such as ISO/TC 229 ‘Nanotechnologies’/JWG 2 ‘Nanoparticle Measurement and Characterization’ (SEM, TSEM and TEM), CEN/TC 352 ‘Nanotechnologies’ (SEM, TSEM and TEM), ISO/TC 201/SC 9 (AFM), ISO/TC 24/SC 4 (SAXS). Three technical work packages will ensure input for impact to standardization community, nanoparticle manufacturers, instrument manufacturers, and (accredited) service laboratories: - WP1 Performance and traceability of characterization methods - WP2 Reference materials - Preparation and Characterization - WP3 Modelling and development of measurement procedures Well-defined non-spherical nanoparticles shapes such as cubes, platelets, bipyramids, rods/acicular will be developed, with mono- and polydisperse size distribution, as well as with accurate particle number concentration (by SAXS and isotopically enrichment for ICP-MS). Physical modelling of the signal for TSEM, SEM, 3D-AFM and SAXS will be used to feed machine learning modeling from a-priori measurement data. Further, data fusion will be developed for hybrid sizing techniques: SEM with TSEM/TEM, SEM/TSEM with AFM, SEM/TSEM with SAXS with the final aim of improving the true shape and size of non-spherical nanoparticles by a better estimation of the measurement uncertainties. In the second half-time of the project dedicated workshops (focused on method improvement and reference materials development) will be organized to disseminate the gained knowledge to end-users. Further, a data library with relevant tagged measurement data is planned to be organized and made publicly available. Inter-laboratory comparisons based on the newly developed multi-modal nano reference materials will be organized preferably within VAMAS/TWA 34 ‘Nanoparticle populations’. T2 - NanoWorkshop 2018 (Workshop on reference nanomaterials, current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2018 KW - Nanoparticles KW - Size KW - Shape KW - Traceable size PY - 2018 AN - OPUS4-44995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Shape controlled TiO2 nanoparticles as candidates for nano-CRM’s – an ISO case study N2 - Extraction of true, 3D shape (and size) of non-spherical nanoparticles (NPs) is associated with errors by conventional 2D electron microscopy using projection images. Significant efforts within the ISO technical committee TC 229 ‘Nanotechnologies’ are aimed at establishing accurate TEM and SEM measurement of NP size and shape as robust, standard procedures. Study groups have been organizing inter-laboratory comparisons on well-selected NP systems according to the market needs, such as aggregated titania nano-powder for which size and shape distribution of primary crystallites of irregular shape must be measured accurately. To be noticed is e. g. the fact that the measurement procedure allows only manual selection of the particles clearly distinguishable for analysis as well as manual definition of the contour of the imaged NPs. An inter-laboratory exercise on titania NPs (pure anatase, grown by hydrothermal synthesis) of well-defined non-spherical shape, i.e. bipyramidal has been recently started within ISO/TC 229 under similar conditions as for the irregular shaped titania. Overlapped particles were allowed to be considered, as long as they are clearly distinguishable. One decisive NP selection criterion was to analyze only those NPs with a roundness value below 0.7, i.e. the NPs laying on the support foil and, hence, with projection areas clearly deviating from perfect circles (R=1). The overall evaluation (for 15 labs) of the size descriptors (area, Feret, minFeret, perimeter) and shape descriptors (aspect ratio, roundness, compactness, extent) by analysis of variance is just to be finished and included in ISO/WD 21363 Nanotechnologies -- Protocol for particle size distribution by transmission electron microscopy. T2 - NanoWorkshop 2018 (Workshop on reference nanomaterials, current situation and needs: development, measurement, standardization) CY - Berlin, Germany DA - 14.05.2018 KW - Titanium oxide KW - Nanoparticles KW - Shape-controlled KW - Electron microscopy KW - Reference material PY - 2018 AN - OPUS4-44996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Metrology for spatially resolved chemical analysis at the micro and nanometre scales Surface Analysis Working Group (SAWG) - Report for 16th Meeting (2017/18) N2 - Following the 2017 meeting, progress with the Key Comparison CCQM-K153 related to the BET specific surface lead by UNIIM and the Pilot Study P-190 “Thickness Measurement of nm HfO2 Films” lead by KRISS will be discussed. The 16th meeting of SAWG will focus on •survey on CMC claims submitted with reference to K-129 and K-136. •the overall and SAWG specific aspects of the CCQM Strategy process, •a consideration of comparisons on convention methods as recommended by the CCQM Plenary Meeting 2017, •the 2019 CCQM Workshop and paper(s) for Metrologia’s Special Issue, •discussion of future comparisons. T2 - 24th meeting of the CCQM 2018 CY - Paris, France DA - 19.04.2018 KW - Surface chemical analysis KW - Metrology KW - Inter-laboratory comparisons PY - 2018 AN - OPUS4-44998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Büchele, Dominique T1 - Comparison between uni- and multivariate data Analysis for the determination of nutrients in soils using XRF N2 - As part of the BonaRes research initiative funded by the German Federal Ministry of Education and Research (BMBF), strategies are being developed to use soil as a sustainable resource in the bioeconomy. The interdisciplinary subproject I4S - “Intelligence for soil” - is responsible for the development of an integrated system for site-specific management of soil fertility. For this purpose, a platform is constructed and various sensors are installed. Real-time data will be summarized in models and decision-making algorithms will be used to control fertilization and accordingly improve soil functions. This would allow investigations in close meshed dynamic grid and fast analysis of large areas to generate higher yields. This is important given that the distribution of minor and trace elements varies widely. Aim of the Federal Institute for Materials Research and Testing (BAM) in the frame of I4S is the characterization of an X-ray fluorescence (XRF) based sensor for robust online-analysis of arable land. The non-destructive and contactless XRF is suitable for rapid in-situ analysis on the field due to minimal sample preparation and simultaneous multi-element analysis. Soils are already considered as a complex matrix due to their wide range of elements in different contents, especially light elements with low atomic numbers (Z<19). Problems by measuring soil samples also arise from heterogeneity of the sample and matrix effects. Large grain size distribution causes strong inhomogeneity and matrix effects occur through physical properties related to high concentration of main components. Matrix-specific calibration strategies for determination of total major and minor plant essential nutrients are particularly important regarding these difficulties. For accurate calibration, data treatment and evaluation must also be considered. Univariate and multivariate data analysis were compared regarding their analytical figures of merit. Using principal component analysis (PCA) it was possible to classify German soils in different groups as sand, clay and silt. Calibration models were obtained by partial least squares regression (PLSR) and the content of macro- and micronutrients in German soils was predicted. Elemental distribution maps for different German arable lands were created and the results compared to reference measurements. The correlation between predicted values and reference values were in good agreement for most major and minor nutrients. T2 - ESAS/CANAS CY - Berlin, Germany DA - 20.03.2018 KW - Soil KW - XRF KW - PCA KW - PLSR PY - 2018 AN - OPUS4-45010 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Determination of plant essential nutrients in soils using DP-LIBS N2 - In respect of an efficient cultivation of agricultural cropland, a site-specific fertility management is necessary. Therefore, affordable and extensive mapping methods are needed. For this purpose, the research project I4S (intelligence for soil) has the goal to develop an integrated system. This system includes a sensor platform, which contains different sensors, like XRF, VIS-NIR, Gamma and LIBS. LIBS (laser-induced breakdown spectroscopy) is known as a fast and simultaneous multi-element analysis with little or no sample preparation. The main task of LIBS measurements in this project is the real time determination of the elemental contents of nutrients in soils, like calcium, magnesium, potassium. For this purpose, a special setup has been designed. The sample uptake operates with the help of a rotatable sample plate which circulates with different velocities to simulate the application on the field. To provide a higher intensity and a better reproducibility of the obtained signal, a double-pulse Nd:YAG laser (1064 nm) was used. In order to minimize dust formation from the soil during the operation of the laser, a dust removal by suction has been integrated.[1] When using relative methods such as LIBS, a suitable calibration curve is needed for absolute quantification. The complex matrix of soils, as well as the influence of moisture and grain size in soils makes the absolute quantification by LIBS challenging. To overcome these influences, chemometric methods were used. With the principal component analysis (PCA) a classification of soils into different soil types was performed and a calibration curve based on partial least squares regression (PLSR) was generated. With this calibration model’s elemental distribution maps for different German agricultural fields were created. T2 - Bonares Conference CY - Berlin, Germany DA - 26.02.2018 KW - LIBS KW - Soil KW - PCA KW - PLSR PY - 2018 AN - OPUS4-45011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Bestimmung von Makro- und Mikronährstoffen in Böden mittels laserinduzierter Plasmaspektroskopie N2 - In respect of an efficient cultivation of agricultural cropland, a site-specific fertility management is necessary. Therefore, affordable and extensive mapping methods are needed. The research projects I4S (intelligence for soil) has the goal to develop a system for this purpose. I4S is one of ten interdisciplinary research project associations of the innovation programme called BonaRes, which is funded by the German Federal Ministry of Education and Research (BMBF). The system includes a sensor platform, which contains different sensors, like XRF, VIS-NIR, Gamma and LIBS. The main task of LIBS measurements in this project is the real-time determination of the elemental contents of major and minor nutrients in soils, like calcium, magnesium, potassium. LIBS (laser-induced breakdown spectroscopy) is known as a fast and simultaneous multi-element analysis with little or no sample preparation. The main task of LIBS measurements in this project is the real-time determination of the elemental contents of nutrients in soils, like calcium, magnesium, potassium. For this purpose, a special setup has been designed. The sample uptake operates with the help of a rotatable sample plate which circulates with different velocities to simulate the application on the field. To provide a higher intensity and a better reproducibility of the obtained signal, a double-pulse Nd:YAG laser (1064 nm) was used. In order to minimize dust formation from the soil during the operation of the laser, a dust removal by suction has been integrated. When using relative methods such as LIBS, a suitable calibration curve is needed for absolute quantification. The complex matrix of soils, as well as the influence of moisture and grain size in soils makes the absolute quantification by LIBS challenging. To overcome these influences, chemometric methods were used. With the principal component analysis (PCA) a classification of soils into different soil types was performed and a calibration curve based on partial least squares regression (PLSR) was generated. With this calibration model’s elemental distribution maps for different German agricultural fields were created. T2 - Doktorandenseminar AK Prozessanalytik GDCh CY - Berlin, Germany DA - 25.02.2018 KW - LIBS KW - Boden KW - Nährstoffe KW - Univariat KW - Multivariat PY - 2018 AN - OPUS4-45012 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Le, Quynh Hoa T1 - Rezension: Röntgenfluoreszenzanalyse in der Laborpraxis N2 - Dieses Buch ist definitiv eine Empfehlung an alle, die mit RFA arbeiten müssen. Außerdem bietet es nützliche und praktische Informationen für Forscher, die an einem bestimmten Thema arbeiten, das im Antragsteil erwähnt wird. Dies wird ihnen während ihrer Forschung helfen, Proben vorzubereiten sowie Fehler in der RFA-Analyse zu erkennen und somit zu vermeiden. Die Stärken des Buches liegen im verständlichen Text und darin, dass alle notwendigen Schritte der Analysenverfahren Punkt für Punkt aufgeführt sind. Obwohl die Autoren eine unglaubliche Arbeit geleistet haben, um den Leser auf den neuesten Stand zu bringen, sind einige Teile ziemlich kurz gehalten. Die Auflistung von weiterführender Literatur, einschließlich wichtiger Normen und Gesetze, verringert dieses Manko etwas und verweist die interessierten Leser auf ergänzende Quellen. KW - Fluoreszenz KW - Oberflächenanalytik KW - Elementanalyse PY - 2018 DO - https://doi.org/10.1002maco.201870055 SN - 1521-4176 VL - 69 IS - 5 SP - 3 PB - WILEY-VCH Verlag GmbH & Co. KgaA CY - Weinheim AN - OPUS4-44930 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Haferkamp, Sebastian A1 - Akhmetova, Irina A1 - Röllig, Mathias A1 - Maierhofer, Christiane A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical one-pot syntheses N2 - We present an in situ triple coupling of synchrotron X-ray diffraction with Raman spectroscopy, and thermography to study milling reactions in real time. This combination of methods allows a correlation of the structural evolution with temperature information. The temperature information is crucial for understanding both the thermodynamics and reaction kinetics. The reaction mechanisms of three prototypical mechanochemical syntheses, a cocrystal formation, a C@C bond formation (Knoevenagel condensation), and the formation of a manganese-phosphonate, were elucidated. Trends in the temperature development during milling are identified. The heat of reaction and latent heat of crystallization of the product contribute to the overall temperature increase. A decrease in temperature occurs via release of, for example, water as a byproduct. Solid and liquid intermediates are detected. The influence of the mechanical impact could be separated from temperature effects caused by the reaction. KW - In situ studies KW - Mechanochemistry KW - Raman spectroscopy KW - Thermography KW - X-ray diffraction PY - 2018 DO - https://doi.org/10.1002/anie.201800147 SN - 1433-7851 SN - 1521-3773 VL - 57 IS - 20 SP - 5930 EP - 5933 PB - Wiley-VCH CY - Weinheim AN - OPUS4-44946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Plasma Germany, Fachausschuss Normung, Berichtszeitraum Herbst 2017 – Frühjahr 2018 N2 - Der Vortrag gibt den aktuellen Stand der Normung im Bereich der Oberflächen-technik insbesondere der Oberflächenanalytik und der Oberflächenmess- und -prüftechnik wider. Vorgestellt wird der Status technischer Berichte, Normenentwürfe und Normen u.a. zur Charakterisierung von funktionellen Glasoberflächen für bioanalytische Anwendungen, zur Messung der Schichtdicke von Nanomaterialien mittels Ellipsometrie, zur Kalibrierung von Interferometern und Interferenzmikroskopen für die Formmessung, zur Rockwelleindringprüfung zur Bewertung der Schicht-haftung, zu den Grundlagen der Ellipsometrie, zur Messung der Schichtdicke mittels Wirbelstromverfahren, zur Schichtpotentialmessung von Mehrfach-Nickelschichten, zu Filtern und Augenschutzgeräten gegen Laserstrahlung sowie zur Bestimmung der Schichthaftung mittels Zugversuch. T2 - Plasma Germany, Fachausschuss Normung, Frühjahrssitzung CY - Kiel, Germany DA - 17.04.2018 KW - Stand der Normung KW - Oberflächentechnik KW - Oberflächenanalytik KW - Oberflächenmesstechnik KW - Oberflächenprüftechnik PY - 2018 AN - OPUS4-44729 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Usmani, Shirin A1 - Stephan, Ina A1 - Huebert, Thomas A1 - Kemnitz, E. T1 - Nano metal fluorides for wood protection against fungi N2 - Wood treated with nano metal fluorides is found to resist fungal decay. Sol−gel synthesis was used to synthesize MgF2 and CaF2 nanoparticles. Electron microscopy images confirmed the localization of MgF2 and CaF2 nanoparticles in wood. Efficacy of nano metal fluoride-treated wood was tested against brown-rot fungi Coniophora puteana and Rhodonia placenta. Untreated wood specimens had higher mass losses (∼30%) compared to treated specimens, which had average mass loss of 2% against C. puteana and 14% against R. placenta, respectively. Nano metal fluorides provide a viable alternative to current wood preservatives. KW - Brown-rot fungi KW - Coniophora puteana KW - Fluoride nanoparticles KW - Fluorolytic sol−gel KW - Rhodonia placenta KW - SEM wood characterization KW - Wood protection PY - 2018 DO - https://doi.org/10.1021/acsanm.8b00144 SN - 2574-0970 VL - 2018 SP - 1 EP - 6 PB - American Chemical Society (ACS) CY - Washington DC, US AN - OPUS4-44730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Almeida, Â. A1 - Freitas, R. A1 - Calisto, V. A1 - Esteves, V. I. A1 - Schneider, Rudolf A1 - Soares, A. M. V. M. A1 - Figueira, E. A1 - Campos, B. A1 - Barata, C. T1 - Effects of carbamazepine and cetirizine under an ocean acidification scenario on the biochemical and transcriptome responses of the clam Ruditapes philippinarum N2 - Several works evaluated the toxicity of pharmaceutical drugs and climate related changes in invertebrates but few explored the combined effects of both stressors, namely considering their mode of action (MoA). Carbamazepine (CBZ) and cetirizine (CTZ) are pharmaceutical drugs detected in the environment and the toxicity derived from the combined effects of these drugs with ocean acidification (OA) is poorly explored. Thus, the present study investigated the biochemical parameters related to an oxidative stress response and the transcription of genes related to the MoA of CBZ (1.0 mg/L) and CTZ (0.6 mg/L) in the clam Ruditapes philippinarum chronically exposed (28 days) to control (7.8) and low (7.5) pH conditions. The results obtained showed that despite the clams accumulated both drugs, at low pH the clams exposed to CTZ decreased drug concentration and BCF values (CTZ uptake: 2.0 ± 0.5 ng/g fresh weight; BCF: 3.8 ± 0.9) in comparison with clams exposed to control pH (CTZ uptake: 2.9 ± 0.3 ng/g fresh weight; BCF: 5.5 ± 0.6). No oxidative stress was induced by the exposure to CBZ or CTZ at each pH level, but the transcription of several genes related with the MoA (neurotransmission, immunity and biomineralization) was altered by low pH, drug exposure and the combination of both stressors. At both pH conditions, CBZ increased the transcription of GABA receptor gene (neurotransmission) and CTZ led to a decrease of Perlucin gene (biomineralization) transcription. The transcription of MyD88 gene (immunity) decreased at low pH (7.5) combined with drug exposure (CBZ or CTZ). Thus, it was highlighted that the interaction of drug exposure and low pH conditions can change bivalves’ sensitivity to drugs or alter drugs toxicity. KW - Carbamazepine KW - Biomarker KW - ELISA KW - Biochemische Parameter PY - 2018 DO - https://doi.org/10.1016/j.envpol.2017.12.121 SN - 0269-7491 VL - 235 SP - 857 EP - 868 PB - Elsevier Ltd. CY - Amsterdam, NL AN - OPUS4-44739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterization of co (polyamide)s N2 - Charactrization of Co(polyamide)s Molar mass distribution; Functionalization; supression of end group effects in favor of sequence distribution analysis; Evidence of of randomization with increasing reaction time T2 - Polyamide Meeting, DSM CY - Sittard, The Netherlands DA - 20.04.2018 KW - Liquid chromatography KW - Mass spectrometry of polymers PY - 2018 AN - OPUS4-44747 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dhamo, Lorena T1 - Synthesis and optical characterization of ternary Quantum Dots: AgInS /ZnS N2 - Ternary semiconductors quantum dots (t-QD) are Cd-free nanocrystals made from I-III-VI group elements like silver or copper, indium and sulfide yielding CIS (CuInS2) or AIS (AgInS2) QDs. They are interesting alternatives to Cd-based QDs for applications as solar concentrators or optically active material for solar cells, light emitting diodes (LED) or reporters for diagnostic assays. To avoid ligand exchange procedures for high quality QDs, commonly synthesized in high boiling apolar solvents with apolar surface ligands, AIS QDs are synthesized in aqueous solution, required for bioanalytical application, by a microwave-assisted procedure. The surface of these QDs is passivated by a ZnS shell to enhance photoluminescence quantum yield (PL QY) and prevent material decomposition and oxidation. The resulting AIS/ZnS QDs exhibit broad PL spectra in the visible and near infrared, tunable by size and chemical composition. I will show the simple synthetic procedure and a spectroscopic study of different AIS QDs evaluating their PL properties and stability, PL QY, and PL decay kinetics. The analyzed sample showed long lifetimes, relatively high QY (50%) and good stability. Ligand conjugation is also performed to allow the embedding in polymer matrix, which requires apolar cappng. The simple aqueous synthesis together with the tunable emission color, the high PL QY, the high absorption coefficients and the long luminescence lifetimes make these t-QDs promising Cd-free materials for many different applications in the material and life sciences. T2 - NanoWorkshop CY - Berlin, Germany DA - 14.05.2018 KW - Synthesis KW - Quantum dots KW - Optical spectroscopy PY - 2018 AN - OPUS4-45115 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zavoiura, Oleksandr A1 - Resch-Genger, Ute A1 - Seitz, Oliver T1 - Quantum dot-PNA conjugates for target-catalyzed RNA detection N2 - Detection of pathogenic nucleic acids remains one of the most reliable approaches for the diagnosis of a broad range of diseases. Current PCR-based methods require experienced personnel and cannot be easily used for point-of care diagnostics, making alternative strategies for the sensitive, reliable, and cost-efficient detection of pathogenic nucleic acids highly desirable. Here, we report an enzyme-free method for the fluorometric detection of RNA that relies on a target-induced fluorophore transfer onto a semiconductor quantum dot (QD), uses PNA probes as selective recognition elements and can be read out with simple and inexpensive equipment. For QD-PNA conjugates with optimized PNA content, limits of detection of dengue RNA in the range of 10 pM to 100 nM can be realized within 5 h in the presence of a high excess of noncomplementary RNA. KW - FRET KW - Fluorescence KW - DNA KW - Assay KW - Quantum dot KW - Nano KW - Particle KW - Synthesis KW - Ligation Assay PY - 2018 DO - https://doi.org/10.1021/acs.bioconjchem.8b00157 SN - 1043-1802 VL - 29 IS - 5 SP - 1690 EP - 1702 PB - ACS Publications AN - OPUS4-45120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Aktivitäten der BAM im EU-Projekt NanoDefine N2 - Die Präsentation gibt einen Überblick über die Aktivitäten der BAM im EU-Projekt 'NanoDefine'. Verknüpfungen zur Entwicklung von nano-Referenzmaterialien, ISO- und VAMAS-Aktivitäten und anderen nano-Projekten werden vorausschauend diskutiert. T2 - Expertenaustausch zum Thema ‘Nanosicherheit’ zwischen BMU, BMWi und BAM CY - Berlin, Germany DA - 01.06.2018 KW - Nanomaterial KW - ISO KW - NanoDefine KW - EU-Definition KW - Nanopartikel PY - 2018 AN - OPUS4-45078 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc T1 - Elektrolyseverfahren zur Bestimmung der Spurenfeuchte N2 - Die Spurenfeuchte ist eine wichtige Messgröße bei der Qualitätsbeurteilung von technischen und medizinischen Gasen und muss daher zuverlässig gemessen werden. Der Spurenbereich ist definiert durch einen Wasserdampf-Stoffmengenanteil kleiner als 2600 µmol/mol bzw. einer Frostpunkttemperatur kleiner -10 °C. Eine geeignete Methode für die kontinuierliche Spurenfeuchtemessung stellt das Elektrolyseverfahren bzw. coulometrische Messprinzip dar. Bei diesem Prinzip strömt ein feuchtes Gas über eine hygroskopische Phosphorpentoxid-Schicht, welche kontinuierlich Wasserdampf absorbiert. Durch das Anlegen einer Zersetzungsspannung wird das absorbierte Wasser elektrolysiert und der resultierende Elektrolysestrom korreliert zum Feuchtegehalt im Gas. Neben dem Einfluss von unterschiedlichen Gasen auf das Messverfahren, wurde der Einfluss der Druckfeuchte im Druckbereich von 2 bis 15 bar untersucht. Des Weiteren wurde eine neuartige Sensorbeschichtung basierend auf einer ionischen Flüssigkeit getestet und es wurde ein Prototyp für die abgestufte Bestimmung der Wasseraktivität und der Materialfeuchte aufgebaut. T2 - Seminar am Institut für Chemie und Biotechnik CY - Technische Universität Ilmenau, Ilmenau, Germany DA - 06.06.2018 KW - Elektrolyseverfahren KW - Spurenfeuchte in Gasen KW - Druckfeuchte KW - Materialfeuchte KW - Ionische Flüssigkeit PY - 2018 AN - OPUS4-45122 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred A1 - Feldmann, Ines A1 - Günther, Tobias A1 - Wilsch, Gerd ED - Glaser, L. T1 - Analytische Untersuchungen an Glasmalfarben mittels EDX und LIBS N2 - Nach 1850 wurde zur weiteren Herabsetzung der Einbrenntemperatur von Glasmalfarben Borax (Na2B4O7 · 10 H2O) zugesetzt. Das Verhältnis war nun 1 Teil SiO2, 3 Teile PbO und 0,5 Teile Borax. Der analytische Nachweis von Bor in eingebrannten Malschichten war bisher jedoch nicht möglich.Daher wurden in Laborversuchen Glasmalfarben mit unterschiedlichem Gehalt an Borax auf Modellgläser aufgetragen, eingebrannt und anschließend unter simulierten Umweltbedingungen zeitraffend im Klimaschrank bewittert. Mit Hilfe von elektronenmikroskopischen Untersuchungen können Malschichten charakterisiert werden und somit Hinweise auf mögliche Schadensursachen liefern. Erste Versuche zum Nachweis von Bor erfolgten mit Hilfe von LIBS-Messungen (Laser Induced Breakdown Spectroscopy) an im Labor hergestellten Glasmalfarben mit unterschiedlichem Boraxgehalt. T2 - Archäometrie und Denkmalpflege 2018 CY - Hamburg, Germany DA - 20.03.2018 KW - Glasmalfarben KW - Umweltsimulation KW - Analytik PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-450664 SN - 978-3-945931-16-5 DO - https://doi.org/10.3204/DESY-PROC-2018-01 SN - 1435-8077 SP - 283 EP - 285 PB - Deutsches Elektronen -Synchrotron CY - Hamburg AN - OPUS4-45066 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saleh, Maysoon I. T1 - Synthesis and systematic characterization of core-muti-shell NaYF4:Er3+, Yb3+@SiO2@Au nanoparticles for the enhancement of fluorescence emission N2 - The aim of this work is to investigate the Synthesis of core-shell upconverting nanoparticles (UCNP). The UCNP are coated with a Gold Shell to plasmonically enhance the fluorescence emision. The distance between the UCNP core and the plasmonic structure is tuned by the aid of a silica at different Shell thicknesses. T2 - Work shop on Refer ence Nanomaterials jointly organized by BAM and PTB CY - Berlin, Germany DA - 14.05.2018 KW - Upconversion nanoparticles KW - Silica coating KW - Plasmonic enhancement PY - 2018 AN - OPUS4-45067 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Joschko, M. T1 - Relationship between soil structure and carbon dynamics in agricultural soils : potential for a farmer`s tool ? N2 - Soil structure, the spatial arrangement of soil elements, integrates a variety of drivers in agricultural soil (parent material, tillage, crop rotation, organic fertilizer, below ground biodiversity). It is related to almost all soil functions. Relationships between soil structure and the carbon sequestration potential of soil are known from the comparison of different land use systems (grassland vs. tilled soils ) and are expected to be a general phenomenon. Therefore , we expect soil structure assessed by modern non - destructive methods to be a valuable tool for the optimization of soil organic matter management in agricultural soils T2 - Soil organic matter management in agriculture – International Symposium CY - Brunswick, Germany DA - 29.05.2018 KW - Computed tomography KW - Carbon dynamics KW - Soil PY - 2018 AN - OPUS4-45068 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred T1 - Analytische Untersuchungen an Glasmalfarben mittels EDX und LIBS N2 - Nach 1850 wurde zur weiteren Herabsetzung der Einbrenntemperatur von Glasmalfarben Borax (Na2B4O7 · 10 H2O) zugesetzt. Das Verhältnis war nun 1 Teil SiO2, 3 Teile PbO und 0,5 Teile Borax. Der analytische Nachweis von Bor in eingebrannten Malschichten war bisher jedoch nicht möglich. In Laborversuchen wurden Glasmalfarben mit unterschiedlichem Gehalt an Borax auf Modellgläser aufgetragen, eingebrannt und anschließend unter simulierten Umweltbedingungen zeitraffend im Klimaschrank bewittert. Mit Hilfe von elektronenmikroskopischen Untersuchungen können Malschichten charakterisiert werden und somit Hinweise auf mögliche Schadensursachen liefern. Der Nachweis von Bor erfolgte mit Hilfe von LIBS-Messungen (Laser Induced Breakdown Spectroscopy) an im Labor hergestellten Glasmalfarben mit unterschiedlichem Boraxgehalt. T2 - Archäometrie und Denkmalpflege 2018 CY - Hamburg, Germany DA - 20.04.2018 KW - Glasmalfarben KW - Umweltsimulation KW - Analytik PY - 2018 AN - OPUS4-45069 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Spectroscopic ellipsometry for the determination of thickness and porosity of mesoporous metal oxide films N2 - Thin mesoporous metal oxide films are versatile and attractive candidates for several energy applications like photovoltaics, electrolysis or batteries. Due to their high surface area and ordered pore structure, mesoporous metal oxides demonstrate higher activities. The performance of the porous films is affected by properties like size and shape of the mesopores as well as the crystallinity of the framework. The exact determination and metrological evaluation of the complex morphology of thin mesoporous films requires a new analytical approach employing to combined data of different analytical methods. In this contribution we present a novel evaluation procedure for spectroscopic ellipsometry (SE) to analyse thin mesoporous iridium oxide films. Mesoporous iridium oxide films were prepared via dip-coating of a solution containing a triblock-copolymer as structure directing agent and an iridium precursor in ethanol. Deposited films were calcined in air at temperatures between 300 and 600 °C. Their morphology was studied with SEM and an electron probe microanalysis (EPMA) and correlated via SE with a Bruggeman effective medium approximation (BEMA). The developed SE model described the film thickness as well as the porosity. ... The contribution will assess in detail the novel approach to analyse the morphology and porosity of thin metal oxide films with spectroscopic ellipsometry. Moreover, the advantages of the new developed approach will be discussed as well as combination of datasets from multiple measurements to development new methods for innovative energy technologies. T2 - 30. Deutsche Zeolith-Tagung gemeinsam mit dem Jahrestreffen der ProcessNet-Fachgruppe Adsorption CY - Christian-Albrechts-Universität zu Kiel, Germany DA - 28.02.2018 KW - Mesoporous materials KW - Iridium oxide films KW - Electro catalyst KW - Spectroscopic ellipsometry KW - Thin film metrology KW - Multi-sample analysis PY - 2018 AN - OPUS4-45134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Spectroscopic ellipsometry for the determination of thickness and porosity of mesoporous metal oxide films N2 - Thin mesoporous metal oxide films are versatile and attractive candidates for several energy applications like photovoltaics, electrolysis or batteries. Due to their high surface area and ordered pore structure, mesoporous metal oxides demonstrate higher activities. The performance of the porous films is affected by properties like size and shape of the mesopores as well as the crystallinity of the framework. The exact determination and metrological evaluation of the complex morphology of thin mesoporous films requires a new analytical approach employing to combined data of different analytical methods. In this contribution we present a novel evaluation procedure for spectroscopic ellipsometry (SE) to analyse thin mesoporous iridium oxide films. Mesoporous iridium oxide films were prepared via dip-coating of a solution containing a triblock-copolymer as structure directing agent and an Iridium precursor in ethanol. Deposited films were calcined in air at temperatures between 300 and 600 °C. Their morphology was studied with SEM and an electron probe microanalysis (EPMA) and correlated via SE with a Bruggeman effective medium approximation (BEMA). The developed SE model described the film thickness as well as the porosity. ... The contribution will assess in detail the novel approach to analyse the morphology and porosity of thin metal oxide films with spectroscopic ellipsometry. Moreover, the advantages of the new developed approach will be discussed as well as combination of datasets from multiple measurements to development new methods for innovative energy technologies. T2 - 10th Workshop Ellipsometry 2018 CY - Chemnitz University of Technology, Germany DA - 19.03.2018 KW - Mesoporous materials KW - Iridium oxide films KW - Electro catalyst KW - Spectroscopic ellipsometry KW - Thin film metrology KW - Multi-sample analysis PY - 2018 AN - OPUS4-45143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hiebl, B. A1 - Ascher, Lena A1 - Luetzow, K. A1 - Kratz, K. A1 - Gruber, C. A1 - Mrowietz, C. A1 - Nehring, M. E. A1 - Lendlein, A. A1 - Franke, R.- P. A1 - Jung, F. T1 - Albumin solder covalently bound to a polymer membrane: New approach to improve binding strength in laser tissue soldering in-vitro N2 - Laser tissue soldering (LTS) based on indocyanine green (ICG)-mediated heat- denaturation of proteins might be a promising alternative technique for micro-suturing, but up to now the Problem of too weak shear strength of the solder welds in comparison to sutures is not solved. Earlier reports gave promising results showing that solder supported by carrier materials can enhance the cohesive strength of the liquid solder. In these studies, the solder was applied to the carriers by dip coating. Higher reliability of the connection between the solder and the carrier material is expected when the solder is bound covalently to the carrier material. In the present study a poly(ether imide) (PEI) membrane served as carrier material and ICG- supplemented albumin as solder substrate. The latter was covalently coupled to the carrier membrane under physiological conditions to prevent structural protein changes. As laser source a diode continuous-wave laser emitting at 808 nm with intensities between 250mW and 1500mW was utilized. The Albumin functionalized carrier membrane was placed onto the tunica media of explanted pig thoracic aortae forming an overlapping area of approximately 0.5×0.5 cm2. All tests were performed in a dry state to prevent laser light absorption by water. Infrared spectroscopy, spectro-photometrical determination of the secondary and Primary amine groups after acid orange II staining, contact angle measurements, and atomic force microscopy proved the successful functionalization of the PEI membrane with albumin. A laser power of 450mW LTS could generate a membrane-blood vessel connection which was characterized by a shear strength of 0.08±0.002MPa, corresponding to 15% of the tensile strength of the native blood vessel. Theoretically, an overlapping zone of 4.1mmaround the entire circumference of the blood vessel could have provided shear strength of the PEI membrane-blood vessel compound identical to the tensile strength of the native blood vessel. These in-vitro results confirmed the beneficial effects of solder reinforcement by carrier membranes, and suggest LTS with covalently bound solders on PEI substrates for further studies in animal models. KW - Tissue soldering KW - Albumin KW - Polymer membrane KW - Laser PY - 2018 DO - https://doi.org/10.3233/CH-189108 SN - 1386-0291 SN - 1875-8622 VL - 69 IS - 1-2 SP - 317 EP - 326 PB - IOS Press AN - OPUS4-45149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Busch, I. A1 - Unger, Wolfgang T1 - Analytical and topographical Reference Material for the Nanoscale N2 - Reliable standards are required to support research and development as well as end-user in application. Appropriate standards have to fulfill three requirements: small uncertainty, easy to use and low overall costs of application. For calibration of microscopes at nanoscale and/or element analysis special requirements for standards are given, which are challenging in manufacture. T2 - Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - XPS KW - Imaging KW - Reference material KW - NoStep Standards PY - 2018 AN - OPUS4-45156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Bestimmung der Partikelgrößenverteilung mittels Zentrifugen-Sedimentationsverfahren nach ISO 13318-2 (Küvette) N2 - Im Vortrag werden das Messprinzip des Zentrifugen-Sedimentationsverfahrens erläutert und die Anforderungen der zugrundeliegenden Normen diskutiert. Es schließen sich umfangreiche Ausführungen zur praktischen Durchführung der Messung, insbesondere auch zu den vorbereitenden Arbeiten, sowie zur Auswertung der Rohdaten an. Nach einem Vergleich der Ergebnisse mit anderen Messverfahren, wird das Verfahren in einer Zusammenfassung bewertet. T2 - Rheologie und Stabilität von dispersen Systemen CY - Potsdam, Germany DA - 14.04.2018 KW - Partikelgrößenverteilung KW - Analytische Zentrifuge PY - 2018 AN - OPUS4-45098 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Spectroscopic ellipsometry for the determination of thickness and porosity of mesoporous metal oxide films N2 - Thin mesoporous metal oxide films are versatile and attractive candidates for several energy applications like photovoltaics, electrolysis or batteries. Due to their high surface area and ordered pore structure, mesoporous metal oxides demonstrate higher activities. The performance of the porous films is affected by properties like size and shape of the mesopores as well as the crystallinity of the framework. The exact determination and metrological evaluation of the complex morphology of thin mesoporous films requires a new analytical approach employing to combined data of different analytical methods. In this contribution we present a novel evaluation procedure for spectroscopic ellipsometry (SE) to analyse thin mesoporous iridium oxide films. Mesoporous iridium oxide films were prepared via dip-coating of a solution containing a triblock-copolymer as structure directing agent and an iridium precursor in ethanol. Deposited films were calcined in air at temperatures between 300 and 600 °C. Their morphology was studied with SEM and an electron probe microanalysis (EPMA)and correlated via SE with a Bruggeman effective medium approximation (BEMA). The developed SE model described the film thickness as well as the porosity. Figure 1a shows a top-view SEM image of mesoporous IrO2 film calcined at 375 °C. The image reveals that the films exhibit a well-ordered mesopore structure with an average pore diameter of 16 nm and a periodic distance between pore centres of 24 nm (FFT inset). Figure 1b is a parity plot of film thicknesses determined by cross-section SEM versus SE of IrO2 film samples prepared at different calcination temperatures. The porosity from the SE model is in good agreement to the porosity values obtained by EPMA. The contribution will assess in detail the novel approach to analyse the morphology and porosity of thin metal oxide films with spectroscopic ellipsometry. Moreover, the advantages of the new developed approach will be discussed as well as combination of datasets from multiple measurements to development new methods for innovative energy technologies. T2 - 30. Deutsche Zeolith-Tagung und Jahrestreffen der ProcessNet-Fachgruppe Adsorption CY - Kiel, Germany DA - 28.02.2018 KW - Mesoporous materials KW - Iridium oxide films KW - Electro catalyst KW - Spectroscopic ellipsometry KW - Thin film metrology KW - Multi-sample analysis PY - 2018 AN - OPUS4-45101 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Irradiation of biomolecules in liquid with electrons of different linear energy transfer N2 - The damage caused by ionizing radiation to DNA and proteins is the reason to treat cancer by radiation therapy. A better understanding of the molecular processes and quantification of the different damaging mechanisms is the prerequisite to develop more efficient therapies. Hereby the understanding of the processes involved in the damage to DNA are of key interest due to its central role in reproduction and mutation. For radiation with low linear energy transfer (LET), most of the damage is caused by the secondary particles produced by scattering of the ionizing radiation with water. Thereby a multitude of species are produced, whereby especially kinetic low energy electrons, prehydrated electrons, OH-radicals and ions are of importance. With higher LET the relative amount of the direct damaging effects increases. This is especially important considering the increased usage of high LET particles in radiation therapy. Therefore, the quantification of the contribution to DNA damage of direct and indirect effects and the different secondary species is of high interest due to the increase of radio biological efficiency when applying high LET radiation. Here we present an approach to investigate the relative contributions to DNA strand break yield for radiation of different LET within a single electron microscope in combination with electron scattering simulations. T2 - International workshop on radiation damage to DNA CY - Aussois, France DA - 27.05.2018 KW - Radiation damage KW - LET KW - Geant4 KW - DNA KW - Radiation therapy KW - Hydroxyl radical KW - Low energy electrons KW - Dosimetry KW - Microdosimetry KW - Electron irradiation KW - Sem KW - Linear energy transfer KW - MCS KW - Monte-Carlo simulations PY - 2018 AN - OPUS4-45103 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Ectoine protects biomolecules from ionizing radiation: Molecular mechanisms N2 - The compatible solute and osmolyte ectoine is an effective protectant of biomolecules and whole cells against heating, freezing and high salinity. The protection of cells (human Keratinocytes) by ectoine against ultraviolet radiation was also reported by various authors, although the underlying mechanism is not yet understood. We present results on the irradiation of biomolecules (DNA) with ionizing radiation (high energy electrons) in fully aqueous environment in the presence of ectoine and high salt concentrations. The results demonstrate an effective radiation protection of DNA by ectoine against the induction of single strand breaks by ionizing radiation. The effect is explained by an increased in low-energy electron scattering at the enhanced free-vibrational density of states of water due to ectoine, as well as the action of ectoine as an OH-radical scavenger. This was demonstrated by Raman spectroscopy, electron paramagnetic resonance (EPR) and Monte-Carlo simulations (Geant4). T2 - DPG-Frühjahrstagung der Sektion Kondensierte Materie gemeinsam mit der EPS CY - Berlin, Germany DA - 11.03.2018 KW - Ionizing radiation KW - Ectoine KW - Radiation damage KW - Radiation protection KW - Dosimetry KW - Ectoin KW - Ectoine radiation protection KW - Compatible solute KW - Osmolyte KW - Aqueous solution KW - OH-radical KW - Radical scavenger KW - Hydroxyl radical KW - Hydroxyectoine KW - Ectoine radical scavenger KW - Low energy electrons KW - Geant4 PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-446202 N1 - Poster basiert auf: https://nbn-resolving.org/urn:nbn:de:kobv:b43-419332 AN - OPUS4-44620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Salge, T. A1 - Wäsche, Rolf A1 - Hodoroaba, Vasile-Dan T1 - Advanced light element and low energy X-ray analysis of a TiB2 – TiC – SiC ceramic material using EDS spectrum imaging N2 - The accurate EDS microanalysis of light elements such as boron and carbon by spectrum imaging will be demonstrated using a sintered hard ceramic material composed of the three major phases titanium boride (TiB2), titanium carbide (TiC), silicon carbide (SiC) and minor phases, sub-μm in size. The combination of these three materials leads to improved mechanical and tribological properties. Silicon carbide is a material used for mechanical seals. It has the disadvantage of reduced failsafe running functions, causing increased wear when running dry. The added titanium components (TiC and TiB2) improve the failsafe running functions. This technology has already been transferred to industrial applications. KW - EDS KW - Spectrum imaging KW - Ceramic KW - Phase analysis KW - Light elements PY - 2018 UR - https://www.bruker.com/fileadmin/user_upload/8-PDF-Docs/X-rayDiffraction_ElementalAnalysis/Microanalysis_EBSD/LabReports/App_eds_10_LE_keramik_Rev1_1_lores.pdf SP - 1 EP - 5 CY - Berlin AN - OPUS4-44622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Zhiyang A1 - Gernert, U. A1 - Gerhardt, R. F. A1 - Höhn, E.-M. A1 - Belder, D. A1 - Kneipp, Janina T1 - Catalysis by Metal Nanoparticles in a Plug-In Optofluidic Platform: Redox Reactions of p-Nitrobenzenethiol and p-Aminothiophenol N2 - The spectroscopic characterization by surface-enhanced Raman scattering (SERS) has shown great potential in studies of heterogeneous catalysis. We describe a plug-in multifunctional optofluidic platform that can be tailored to serve both as a variable catalyst material and for sensitive optical characterization of the respective reactions using SERS in microfluidic systems. The platform enables the characterization of reactions under a controlled gas atmosphere and does not present with limitations due to nanoparticle adsorption or memory effects. Spectra of the gold-catalyzed reduction of p-nitrothiophenol by sodium borohydride using the plug-in probe provide evidence that the borohydride is the direct source of hydrogen on the gold surface, and that a radical anion is formed as an intermediate. The in situ monitoring of the photoinduced dimerization of p-aminothiophenol indicates that the activation of oxygen is essential for the plasmon-catalyzed oxidation on gold nanoparticles and strongly supports the central role of metal oxide species. KW - Gaseous reactants KW - Heterogeneous catalysis KW - Microfluidics KW - Optofluidics KW - Radicals KW - Reusable KW - Surface-enhanced Raman scattering (SERS) PY - 2018 UR - https://pubs.acs.org/doi/10.1021/acscatal.8b00101 DO - https://doi.org/10.1021/acscatal.8b00101 VL - 8 IS - 3 SP - 2443 EP - 2449 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-44628 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas T1 - Determination of the glass transition region of thin PVME films by means of spectroscopic ellipsometry N2 - In this presentation, we report on the Determination of the glass transition temperature of thin layers of Polyvinylmethylether (PVME) depending on the thickness of the polymer layer. The glass Transition of thin polymer layers is currently under much investigation due to the nano-confinement effects proposed to appear in dependence on the layer thicknesses in the nm range. The properties of the polymer, the temperature range, as well as the thicknesses range of the polymer layers pose a serious challenge to the investigation by means of spectroscopic ellipsometry. By careful choice of experimental parameters, we were able to investigate the thickness change by temperature of PVME layers in the range between 2 and 300 nm and in the temperature range between 200 K and 340 K. By optimizing the analysis process, we were able to determine Tg values within this parameter range with sufficient accuracy to investigate the Tg change due to confinement effects. Alongside the change of position of the glass transition with thickness, we discuss the details of the ellipsometric analysis and its implications for the resulting thermal properties of the thin polymer layers as well as the accuracy of the Tg value with respect to the method used in the analysis process. T2 - Workshop Ellipsometry 2018 CY - Chemnitz, Germany DA - 19.03.2018 KW - Polymers KW - PVME KW - Temperature dependent ellipsometry KW - Glass transition PY - 2018 AN - OPUS4-44672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas T1 - Calibration samples and the GUM-compliant determination of uncertainties in ellipsometry N2 - Ellipsometry is well known as a highly sensitive and reproducible surface analysis technique. However, in a context of metrological applications, the most important property of a measurement process is accuracy, relying on statistical precision, (reproducibility) and trueness (in an absolute sense versus a given standard). The latter is much more difficult to achieve. In this presentation, we discuss the possibility of establishing ellipsometry in a diverse metrological landscape by means of defining standard procedures and best practice methodologies for the measurement and for calibration purposes. The most important task of this approach is to determine the model-inherent uncertainty, originating from parameter coupling. We achieve this by means of sensitivity analysis of the parameters resulting from the fit process. We discuss the definition of reference materials by which accuracy can be made available for ellipsometry, passed along between ellipsometry laboratories and for other measurement techniques. The determination of uncertainty is presented in this work for a number of examples involving difficult analysis models employed for samples from different production environments. We present a standardization initiative with the goal to disseminate this work into an international standard alongside an inter-laboratory study comparing the results for complex samples gained by laboratories with different instrumentation. We also present the results gained within EURAMET projects focused on the metrology of materials with strong non-idealities used in photovoltaics and other energy technology. T2 - Workshop Ellipsometry 2018 CY - Chemnitz, Germany DA - 19.03.2018 KW - Ellipsometric metrology KW - Reference samples KW - Reference procedures KW - Standardization PY - 2018 AN - OPUS4-44674 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hansen, B. A1 - Hodoroaba, Vasile-Dan T1 - Analysis of a certified copper alloy with Micro-XRF on SEM N2 - Copper alloys have found widespread application in various fields. The elemental composition determines the properties of the alloys and consequently their application. Therefore, knowing the composition of a copper alloy is very important. Metrological institutes like the BAM (German Federal Institute for Materials Research and Testing) offer reference materials that can be used to prove the accuracy of the applied analysis method. The aim of this application note is to demonstrate how Micro-X-ray fluorescence spectroscopy (Micro-XRF) expediently supplements the analysis of copper alloys by using Bruker’s micro-focus X-ray source XTrace attached to a scanning electron microscope (SEM) and operating with an energy dispersive spectrometer. KW - XRF KW - µ-XRF KW - SEM/EDX KW - Copper alloy PY - 2018 UR - https://www.bruker.com/fileadmin/user_upload/8-PDF-Docs/X-rayDiffraction_ElementalAnalysis/Microanalysis_EBSD/LabReports/App_mxrf_sem_03_analysis_Cu_alloy_lores.pdf SP - 1 EP - 4 PB - Bruker Nano GmbH CY - Berlin AN - OPUS4-44677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donėlienė, J. A1 - Rudzikas, M. A1 - Rades, Steffi A1 - Dörfel, Ilona A1 - Peplinski, Burkhard A1 - Sahre, Mario A1 - Pellegrino, F. A1 - Maurino, V. A1 - Ulbikas, J. A1 - Galdikas, A. A1 - Hodoroaba, Vasile-Dan T1 - Morphology and structure of TixOy nanoparticles generated by femtosecond laser ablation in water N2 - In this work femto-second pulsed laser ablation in liquid (PLAL) procedure for the generation of titanium oxide nanoparticles (NP) is reported with the purpose of understanding morphology and structure of the newly generated NPs. Ablation duration was varied for optimization of NP generation processes between 10 and 90 min. Surface morphology of NPs as well as their size and shape (distribution) were analysed by various complementary electron microscopy techniques, i.e. SEM, TSEM and TEM. The crystalline structure of titanium oxide particles was investigated byXRD(two instruments operated in different geometries) and HR-TEM. Concentration of generated titanium oxide NPs in liquid was analysed by ICP-MS. A mix of crystalline (mainly anatase), partly crystalline and amorphous spherical titanium oxide NPs can be reported having a mean size between 10 and 20 nm, which is rather independent of the laser ablation (LA) duration. A second component consisting of irregularly shaped, but crystalline titanium oxide nanostructures is co-generated in the LA water, with more pronounced occurrence at longer LA times. The provenance of this component is assigned to those spherical particles generated in suspension and passing through the converging laser beam, being hence subject to secondary irradiation effects, e. g. fragmentation. KW - Titanium oxide KW - Nanoparticles KW - Laser ablation in liquid KW - Particle morphology KW - Nanoparticle structure PY - 2018 DO - https://doi.org/10.1088/2053-1591/aaba56 SN - 2053-1591 VL - 5 IS - 4 SP - 045015-1 EP - 045015-12 PB - IOP Publishing CY - London, UK AN - OPUS4-44678 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Cyber-physical Testlabs: Anforderungen an modulare Labore im Zeitalter der Digitalisierung N2 - Von der zunehmenden Digitalisierung sind alle Bereiche von Wirtschaft, Industrie und Gesellschaft betroffen. Die Digitalisierung führt zu einer verstärkten virtuellen Nutzung von Ressourcen und zu einer hochdynamischen Entwicklung der zugehörigen Forschungs- und Technologiefelder. Neue Technologien sind die Basis für die erfolgreiche Weiterentwicklung des Wirtschaftsstandortes Deutschland und für eine Wertschöpfung in globalen Märkten. Die nachhaltige Sicherheit neuer Technologien schafft das Vertrauen der Bürger in den Wandel und sichert unsere Zukunft. Im Vortrag werden Anforderungen und Lösungsvorschläge für das Labor der Zukunft diskutiert. Industrie 4.0 bzw. das Labor 4.0 hilft uns, komplexere Prozesse schneller umzusetzen. Entwicklung von Anlagen und Prozessen beginnt im Labor 4.0. Dazu werden offene, nicht proprietäre Schnittstellen und Standards bei Laborgeräten und Feldgeräten dringend benötigt. Der Standard OPC-UA wird derzeit als gesetzt gesehen. Als nächstes ist die Festlegung der Semantik (Companion Specification) erfordert. Als Bitte an die Zulieferer und Geräterhersteller wird gerichtet, möglichst keine Alleingänge hinsichtlich Schnittstellen, Standards oder GUI zu unternehmen, sondern diese mit den Anwendern abzustimmen. Auf diese Weise ergibt sich das in Industrie 4.0 geforderte "durchgehende Engineering“. Die Sicherung der Wettbewerbsfähigkeit des Standorts Deutschland/Europa ergibt sich dann gleich in doppelter Hinsicht: Sichere, verfügbare und effiziente Herstellung international wettbewerbsfähiger Produkte für die Anwender sowie weltweiter Export von Mess- und Regeltechnik für die Messtechnikbranche. T2 - Analytica Expertenpanel: IoT im Labor 4.0 - Laborgeräte auf dem Weg zu Smart Devices CY - München, Germany DA - 11.04.2018 KW - Smarte Feldgeräte KW - Cyber-physical Test Labs KW - Industrie 4.0 KW - Cyberphysisches Labor PY - 2018 AN - OPUS4-44679 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Already Analyzing or Still Calibrating? - Demonstration of an online NMR analyzer in pilot scale N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example. Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). Based on concentration measurements of reagents and products by the NMR analyzer a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (“Integrated CONtrol and SENsing”, www.consens-spire.eu). T2 - analytica conference 2018 CY - München, Germany DA - 10.04.2018 KW - Online NMR spectroscopy PY - 2018 AN - OPUS4-44680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana T1 - Process monitoring with online NMR spectroscopy – an enabler for Industrial Internet of Things (IIoT) N2 - Improvement in deep process understanding is a mandatory prerequisite for the application of modern concepts like Industrial Internet of Things (IIoT) or “Industrie 4.0”. This is particularly relevant in new process concepts such as intensified production in modularized plants. The direct hyphenation with online methods of process analytical technology (PAT) allows profound insights into the actual reactions within chemical and pharmaceutical production steps and provides necessary information for associated advanced control strategies. While the industrial application of online Raman spectroscopy has already been successfully demonstrated, low-field NMR spectroscopy is not yet adequately developed as an online method for use in process industry. The high Information content combined with the low calibration effort makes NMR spectroscopy a highly promising method for modern process automation with a high flexibility due to short set-up times and novel calibration concepts. This is a Major advantage especially within multi-purpose production plants, as well as for processes suffering from fluctuating quality of raw materials. The concept was evaluated on several example processes of pharmaceutical and chemical industry. The one presented here represents a stage of the synthesis of the industrially important solvent tetrahydrofuran consisting of the catalytic hydrogenation of 2-butine-1,4-diol was monitored. This reaction is proceeding via an intermediate product and suffers from competitive reaction paths. In this application, different spectroscopic methods were combined with the data obtained from classical process sensors, e.g., pressure, temperature, and flow transducers for the development of innovative control concepts. Such an analyzer for direct implementation in an industrial process environment based on a commercially available laboratory benchtop NMR instrument was recently developed within the EU project CONSENS (www.consens-spire.eu), challenging hyphenation to the production plant as well as compliance to all requirements of chemical industry such as explosion safety regulations (ATEX), robust automation, and modern, as well as classical communication interfaces such as OPC-UA or 4–20 mA communication. T2 - 12. Interdisziplinäres Doktorandenseminar CY - Berlin, Germany DA - 25.03.2018 KW - Hydration KW - Online NMR spectroscopy KW - Process analytical technology KW - Process monitoring KW - Process control PY - 2018 AN - OPUS4-44684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Terborg, R. A1 - Hodoroaba, Vasile-Dan T1 - Analysis of the elemental composition and thickness of a Fe-Ni film on Si using Bruker ESPRIT and SAMx STRATAGem N2 - Quantitative analysis of a bulk sample requires that the composition of the sample is homogeneous over the analyzed volume. For inhomogenous samples the calculation of the matrix effects is not correct and this can lead to wrong results in the element concentrations. For samples containing a layer structure a different quantitative evaluation has to be applied. This can be provided with the standard-based analysis in ESPRIT in combination with the STRATAGem software. KW - Thin film analysis KW - SEM/EDX KW - EPMA KW - k-values PY - 2018 UR - https://www.bruker.com/products/x-ray-diffraction-and-elemental-analysis/eds-wds-ebsd-sem-micro-xrf-and-sem-micro-ct/quantax-eds-for-sem/applications/layer-analysis.html SP - 1 EP - 4 CY - Berlin AN - OPUS4-44594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Günther, Tobias A1 - Wilsch, Gerd T1 - Impact of grain sizes on the quantitative concrete analysis using laser-induced breakdown spectroscopy N2 - In civil engineering concrete is the most used building material for making infrastructures like bridges and parking decks worldwide. It is as a porous and multiphase material made of aggregates with a defined grain size distribution, cement and water as well as different additives and admixtures depending on the application. Different grain sizes are important to ensure the needed density and compressive strength. The resulting porous cement matrix contains a mixture of flour grains (aggregates with a grain size below 125 lm) and cement particles (particle size≈50lm). Harmful species like chlorides may penetrate together with water through the capillary pore space and may trigger different damage processes. The damage assessment of concrete structures in Germany is estimated due to the quantification of harmful elements regarding to the cement content only. In the evaluation of concrete using LIBS a two-dimensional scanning is necessary to consider the heterogeneity caused by the aggregates. Therefore, a LIBS system operating with a low energy NdCr:YAG laser, a pulse energy of 3 mJ, a wavelength of 1064 nm, a pulse width of 1.5 ns and a Repetition rate of 100 Hz has been used. Different Czerny-Turner spectrometers with CCD detectors in the UV and NIR range have been used for the detection. Large aggregates (macro-heterogeneity) can be excluded from the evaluation, whereas small aggregates in the range of the laser spot size (flour grains) cannot be spatially resolved. In this work the micro heterogeneity caused by flour grains and their impact on the quantification with LIBS will be discussed. To analyze the effect of changing grain sizes and ratios, the ablation behavior has been determined and compared. Samples with defined grain sizes were made and analyzed using LIBS. The grain size distributions were analyzed with laser diffraction (LDA). KW - LIBS KW - Concrete KW - Micro heterogeneity KW - Grain sizes PY - 2018 DO - https://doi.org/10.1016/j.sab.2018.02.004 SN - 0584-8547 SN - 0038-6987 VL - 142 SP - 74 EP - 84 PB - Elsevier AN - OPUS4-44595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Faser-basierter magneto-optischer Schicht-Sensor zum Monitoring von Bauteilen N2 - In Glasfasern eingeschriebene Bragg-Gitter (FBG: fibre-based Bragg gratings) sind über die Verschiebung der Bragg-Wellenlänge in der Lage, Stauchungen und Dehnungen von Glasfasern hochgenau zu erfassen. In Kompositwerkstoffe eingebettete faseroptische Sensoren können Bauteile bezüglich ihrer mechanischen Integrität überwachen und früh-zeitig Informationen über Materialveränderungen gewinnen. Um die Zuverlässigkeit eines solchen Sensors zu gewährleisten, ist es wichtig, die korrekte Funktion des Sensors im Verbund mit der Werkstoff-Matrix on-line und in-situ sicherzu-stellen. Im Rahmen des DFG-Projekts FAMOS² (FAser-basierter Magneto-Optischer SchichtSensor) wurde ein selbstdiagnosefähiger Schichtsensor entwickelt, der mit Hilfe von magnetostriktiven Aktorschichten aus Nickel bzw. Eisen-Nickel validiert werden kann. Der FAMOS²-Schichtsensor wird durch ein PVD (physical vapour deposition)/ECD (electro-chemical deposition) Hybridschichtsystem realisiert, das auf dem Fasermantel im Bereich des FBG haftfest, homogen und langzeitfunktional abzuscheiden ist. Dabei wird in einem ersten Schritt ein etwa 100 Nanometer dünnes PVD-Schichtsystem aus Chrom und Kupfer als Haftvermittler auf der Glasfaser bzw. als leitfähige Startschicht für den nachfolgenden ECD-Prozess abgeschieden. Um eine rotationssymmetrische Schich-tabscheidung zu gewährleisten, erfolgt während der PVD-Beschichtung eine Rotation der Glasfasern. In einem zweiten Schritt wird dann unter Verwendung eines klassischen Watts-Elektrolyten in einer speziell entwickelten ebenfalls rotationssymmetrisch aufgebau-ten ECD-Durchströmungszelle dann die etwa 30 Mikrometer dicke, magnetostriktive Ak-torschicht auf dem PVD-Schichtsystem abgeschieden, im Vergleich sowohl reine Nickel-Schichten als auch Nickel-Eisen-Schichten. Ein äußeres Magnetfeld dehnt die magnetostriktive Aktorschicht und damit auch die Faser reversibel. Diese Dehnung führt zu einer Verschiebung der Bragg-Wellenlänge, welche direkt mit der Stärke eines zu messenden oder zu Validierungszwecken vorgegebenen Magnetfeldes korreliert. Die Anpassung der Beschichtungsverfahren an die Fasergeome-trie und die mechanischen Eigenschaften der Hybridschichten werden hinsichtlich der me-chanischen Integrität des faseroptischen Sensors diskutiert und der Nachweis der Selbst-diagnosefähigkeit erbracht. T2 - 13. ThGOT Thementage Grenz- und Oberflächentechnik und 11. Thüringer Biomaterial-Kolloquium CY - Zeulenroda, Germany DA - 13.03.2018 KW - Magneto-optischer Sensor KW - Faser-Bragg Gitter KW - Magnetostriktive Beschichtung KW - Selbstkalibrierung KW - Bauteilmonitoring PY - 2018 AN - OPUS4-44598 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Mitzkus, Anja A1 - Sahre, Mario A1 - Weise, Matthias A1 - Köppe, Enrico A1 - Bartholmai, Matthias A1 - Basedau, Frank A1 - Hofmann, Detlef A1 - Schukar, Vivien T1 - Faser-basierter magneto-optischer Schicht-Sensor zum Monitoring von Bauteilen N2 - In Glasfasern eingeschriebene Bragg-Gitter (FBG: fibre-based Bragg gratings) sind über die Verschiebung der Bragg-Wellenlänge in der Lage, Stauchungen und Dehnungen von Glasfasern hochgenau zu erfassen. In Kompositwerkstoffe eingebettete faseroptische Sensoren können Bauteile bezüglich ihrer mechanischen Integrität überwachen und früh-zeitig Informationen über Materialveränderungen gewinnen. Um die Zuverlässigkeit eines solchen Sensors zu gewährleisten, ist es wichtig, die korrekte Funktion des Sensors im Verbund mit der Werkstoff-Matrix on-line und in-situ sicherzu-stellen. Im Rahmen des DFG-Projekts FAMOS² (FAser-basierter Magneto-Optischer SchichtSensor) wurde ein selbstdiagnosefähiger Schichtsensor entwickelt, der mit Hilfe von magnetostriktiven Aktorschichten aus Nickel bzw. Eisen-Nickel validiert werden kann. Der FAMOS²-Schichtsensor wird durch ein PVD (physical vapour deposition)/ECD (electro-chemical deposition) Hybridschichtsystem realisiert, das auf dem Fasermantel im Bereich des FBG haftfest, homogen und langzeitfunktional abzuscheiden ist. Dabei wird in einem ersten Schritt ein etwa 100 Nanometer dünnes PVD-Schichtsystem aus Chrom und Kupfer als Haftvermittler auf der Glasfaser bzw. als leitfähige Startschicht für den nachfolgenden ECD-Prozess abgeschieden. Um eine rotationssymmetrische Schich-tabscheidung zu gewährleisten, erfolgt während der PVD-Beschichtung eine Rotation der Glasfasern. In einem zweiten Schritt wird dann unter Verwendung eines klassischen Watts-Elektrolyten in einer speziell entwickelten ebenfalls rotationssymmetrisch aufgebau-ten ECD-Durchströmungszelle dann die etwa 30 Mikrometer dicke, magnetostriktive Ak-torschicht auf dem PVD-Schichtsystem abgeschieden, im Vergleich sowohl reine Nickel-Schichten als auch Nickel-Eisen-Schichten. Ein äußeres Magnetfeld dehnt die magnetostriktive Aktorschicht und damit auch die Faser reversibel. Diese Dehnung führt zu einer Verschiebung der Bragg-Wellenlänge, welche direkt mit der Stärke eines zu messenden oder zu Validierungszwecken vorgegebenen Magnetfeldes korreliert. Die Anpassung der Beschichtungsverfahren an die Fasergeome-trie und die mechanischen Eigenschaften der Hybridschichten werden hinsichtlich der me-chanischen Integrität des faseroptischen Sensors diskutiert und der Nachweis der Selbst-diagnosefähigkeit erbracht. T2 - 13. ThGOT Thementage Grenz- und Oberflächentechnik und 11. Thüringer Biomaterial-Kolloquium CY - Zeulenroda, Germany DA - 13.03.2018 KW - Magneto-optischer Sensor KW - Faser-Bragg Gitter KW - Magnetostriktive Beschichtung KW - Selbstkalibrierung KW - Bauteilmonitoring PY - 2018 SN - 978-3-00-058187-8 SP - 1 EP - 5 CY - Jena AN - OPUS4-44599 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinen, S. A1 - Rackow, S. A1 - Cuellar-Camacho, J. L. A1 - Donskyi, Ievgen A1 - Unger, Wolfgang A1 - Weinhart, M. T1 - Transfer of functional thermoresponsive poly(glycidyl ether) coatings for cell sheet fabrication from gold to glass surfaces N2 - Thermoresponsive polymer coatings can facilitate cell sheet fabrication under mild conditions by promoting cell adhesion and proliferation at 37 1C. At lower temperatures the detachment of confluent cell sheets is triggered without enzymatic treatment. Thus, confluent cell sheets with intact extracellular matrix for regenerative medicine or tissue engineering applications become available. Herein, we applied the previously identified structural design parameters of functional, thermoresponsive poly(glycidyl ether) brushes on gold to the more application-relevant substrate glass via the self-assembly of a corresponding block copolymer (PGE-AA) with a short surface-reactive, amine-presenting anchor block. Both, physical and covalent immobilization on glass via either multivalent ionic interactions of the anchor block with bare glass or the coupling of the anchor block to a polydopamine (PDA) adhesion layer on glass resulted in stable coatings. Atomic force microscopy revealed a high degree of roughness of covalently attached coatings on the PDA adhesion layer, while physically attached coatings on bare glass were smooth and in the brush-like regime. Cell sheets of primary human dermal fibroblasts detached reliably (86%) and within 20 ± 10 min from physically tethered PGE-AA coatings on glass when prepared under cloud point grafting conditions. The presence of the laterally inhomogeneous PDA adhesion layer, however, hindered the spontaneous temperature-triggered cell detachment from covalently grafted PGE-AA, decreasing both detachment rate and reliability. Despite being only physically attached, self-assembled monolayer brushes of PGE-AA block copolymers on glass are functional and stable thermoresponsive coatings for application in cell sheet fabrication of human fibroblasts as determined by X-ray photoelectron spectroscopy. KW - X-ray photoelectron spectroscopy KW - Thermoresponsive poly(glycidyl ether) coatings KW - Cell sheet fabrication KW - Nm film thickness PY - 2018 DO - https://doi.org/10.1039/c7tb03263c SN - 2050-750X SN - 2050-7518 VL - 6 IS - 10 SP - 1489 EP - 1500 PB - The Royal Society of Chemistry AN - OPUS4-44600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc T1 - Ionic Liquid Based Coulometric Trace Humidity Sensors N2 - This work presents a first attempt to use ionic liquids as a new coating for planar coulometric sensors. These sensors are used for the measurement of trace humidity in various gases. Usually, the coating of the sensors is tetraphosphorus decaoxide and its hydrolysis products. Instead, a hygroscopic ionic liquid was used as sensor coating in this work. Generated frost point temperatures tf in the gas ranged from -80 °C to -30 °C, which is equivalent to vapour mole fractions xv from 0.5 μmol·mol-1 to 376 μmol·mol-1. In addition to the coulometric sensors, the generated humidity is determined by a precision dew point hygrometer as reference. First results show that it is possible to measure humidity withionic liquid based coulometric sensors. T2 - ALLSENSOR 2018 CY - Rom, Italy DA - 25.03.2018 KW - Ionic liquids KW - Coulometric sensors KW - Sensor coating KW - Trace humidity measurement PY - 2018 AN - OPUS4-44601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Controlled deposition of nanoparticles by electrospray for improved analysis by imaging techniques N2 - Of many experimental techniques for measuring particle sizes and size distributions, electron microscopy (EM) is still considered as the gold standard, especially in the nano range (1–100 nm). Furthermore, high-resolution X-ray spectroscopy (EDX) in conjunction with EM can be applied to individual NPs. Preparation of an EM sample for generic particulate materials is a difficult task. Usually the particles in a suspension are deposited on a support. However, this procedure includes the drying of larger solvent amounts on the substrate itself, and this can affect the spatial distribution of the deposited particles. One possibility to overcome this is the use of an electrospray system, where the suspension of particles is sprayed onto the substrate in charged droplets that are so small that they either dry off on the substrate immediately without affecting the position of particles, or even already during their flight time to the substrate. Additionally, the charging of particles minimizes agglomeration and aggregation, maximizing the collection of the EM grids. The prototype of an electrospray deposition system from RAMEM under its trademark IONER (www.ioner.eu) was tested. Electrospray is theoretically described since a long time, but no dedicated commercial instruments are available for the preparation of TEM grids yet, apart from electrostatic deposition of aerosols.2 Several materials have been sprayed onto TEM grids and the resulting particle distributions were evaluated. Operation parameters such as the sample flow-rate, capillary – substrate distance, electric field strength and sampling period length have been optimized. It was found that the particles deposited by electrospray generally show a much more homogeneous spatial distribution on the substrate and a substantial increase of the number of single particles (suited to automatic analysis). T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - Electrospray deposition KW - Nanoparticles KW - Electron microscopy PY - 2018 AN - OPUS4-44802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Lessons on measurement of nanoparticle size and shape learnt from NanoDefine N2 - The EC Recommendation on the definition of nanomaterial1, based solely on size of the constituent particles, foresees development of harmonised measurement methods ensuring ‘consistent results across materials and over time’. The EU/FP7 large research project NanoDefine (http://www.nanodefine.eu) has been exclusively dedicated to support the implementation of this EC Recommendation for the European Union’s legislation. For the first time, measurement techniques able to determine the size of nanoparticles have been evaluated systematically on a well-defined set of quality control materials (spherical, monodisperse) as well as industrial materials of complex shapes and considerable polydispersity. Particularly based on the analytical performance of the measurement techniques as tested on the challenging real-world particulate materials, it was possible to formulate recommendations for use of a new tiered approach consisting of screening and confirmatory techniques. Thus, a consistent framework of guidance for nanomaterial identification according to the EC Definition has been issued in form of the NanoDefiner e-tool (https://labs.inf.fh-dortmund.de/NanoDefiner), with a transparent decision flow scheme and an extensive user manual. Selected examples of analysis and classification as nano-/non-nanomaterials will be given, highlighting the limits of applicability of the available measurement techniques in dependence on sample properties. On some recent relevant developments in sample preparation – as a crucial part for an accurate analysis - will be also reported. T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - Nanoparticles KW - Nanomaterial KW - Particle size distribution KW - EU definition of nanomaterial PY - 2018 AN - OPUS4-44804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel A1 - Gaal, Mate A1 - Kersten, H. T1 - Untersuchung der akustischen Eigenschaften von Plasmalautsprechern auf Basis einer dielektrischen gehemmten Oberflächenentladung (SDBD) N2 - Analog zu Blitz und Donner können elektrische Entladungen innerhalb eines Gasvolumens als akustische Quellen agieren und haben daher eine starke Verbreitung als diagnostische Methode (bspw. in der Raumakustik und bei der Ortung von Teilentladungen). Diese auf dem Prinzip der Thermoakustik beruhende Möglichkeit der Schallerzeugung und die damit verbundenen physikalischen Wechselwirkungen machen die Notwendigkeit einer mechanisch ausgelenkten Membran überflüssig. Dabei wird dem hochfrequenten Träger das Nutzsignal aufgeprägt, welches eine Volumenänderung des umliegenden Gases um seinen Ruhezustand verursacht. Durch die somit hervorgerufene zyklische thermische Wechselwirkung mit dem umliegenden Gasgemisch bedarf es daher ebenfalls keiner akustischen Anpassung. In den vorgestellten Ergebnissen wurde das Übertragungsverhalten eines Oberflächenplasmas (SDBD, surface dielectric barrier discharge) untersucht. Als Maß für den Wirkungsgrad und das Übertragungsverhalten des Aktuators wurden Klirrfaktor- und THD- Messungen und unter Variation der Eingangsleistungen durchgeführt. Durch die positiven akustischen Eigenschaften eröffnen sich neue Applikationen für den Einsatz von Plasmahochtönern wie bspw. zerstörungsfreie Werkstoffprüfung von Verbundsystemen und Klebeverbindungen im Automobilsektor oder im Bauwesen. T2 - 44. Jahrestagung für Akustik (DAGA 2018) CY - Munich, Germany DA - 19.03.2018 KW - Gas discharges KW - Atmospheric pressure plasma KW - Surface dielectric barrier discharge KW - Plasma speaker PY - 2018 SN - 978-3-939296-13-3 SP - 555 EP - 558 AN - OPUS4-44812 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maierhofer, Christiane A1 - Röllig, Mathias A1 - Gower, M. A1 - Lodeiro, M. A1 - Baker, G. A1 - Monte, C. A1 - Adibekyan, A. A1 - Gutschwager, B. A1 - Knazowicka, L. A1 - Blahut, A. T1 - Evaluation of different techniques of active thermography for quantification of artificial defects in fiber-reinforced composites using thermal and phase contrast data analysis N2 - For assuring the safety and reliability of components and constructions in energy applications made of fiber-reinforced polymers (e.g., blades of wind turbines and tidal power plants, engine chassis, flexible oil and gas pipelines) innovative non-destructive testing methods are required. Within the European Project VITCEA complementary methods (shearography, microwave, ultrasonics and thermography) have been further developed and validated. Together with partners from the industry, test specimens have been constructed and selected on-site containing different artificial and natural defect artefacts. As base materials, carbon and glass fibers in different orientations and layering embedded in different matrix materials (epoxy, polyamide) have been considered. In this contribution, the validation of flash and lock-in thermography to these testing problems is presented. Data analysis is based on thermal contrasts and phase evaluation techniques. Experimental data are compared to analytical and numerical models. Among others, the influence of two different types of artificial defects (flat bottom holes and delaminations) with varying diameters and depths and of two different materials (CFRP and GFRP) with unidirectional and quasi-isotropic fiber alignment is discussed. KW - Active thermography KW - CFRP KW - GFRP KW - Delaminations KW - Flash excitation KW - Lock-in excitation PY - 2018 DO - https://doi.org/10.1007/s10765-018-2378-z SN - 0195-928X SN - 1572-9567 VL - 39 IS - 5 SP - Article 61, 1 EP - 37 PB - Springer AN - OPUS4-44687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dieck, S. A1 - Ecke, M. A1 - Rosemann, Paul A1 - Halle, T. T1 - Reversed austenite for enhancing ductility of martensitic stainless steel N2 - Quenching and partitioning (Q&P) heat Treatment increases the deformability of high-strength martensitic steels. Therefore, it is necessary to have some metastable austenite in the microstructure, which transforms in martensite during plastic deformation (TRIP effect). The austenitic-martensitic microstructure is gained by an increased austenitization temperature, water quenching and additional partitioning. The partitioning enables local carbon diffusion, which stabilizes retained austenite and leads to partial reversion of martensite to austenite. The influence of partitioning time was studied for the martensitic stainless steel AISI 420 (X46Cr13, 1.4034). In line with these efforts, metallographic, XRD and EBSD measurements were performed to characterize the microstructural evolution. The mechanical properties were tested using tension and compression loading. Additional corrosion investigations showed the benefits of Q&P heat treatment compared to conventional tempering. The reversion of austenite by the partitioning treatment was verified with EBSD and XRD. Furthermore, the results of the mechanical and corrosion testing showed improved properties due to the Q&P heat treatment. T2 - International Conference on Martensitic Transformations CY - Chicago, IL, USA DA - 09.07.2017 KW - Heat treatment KW - High ductility KW - Martensitic stainless steels KW - Quenching and partitioning KW - Transformation induced plasticity KW - KorroPad KW - EBSD KW - Mechanical testing PY - 2018 SN - 978-3-319-76968-4 DO - https://doi.org/10.1007/978-3-319-76968-4_19 SP - 123 EP - 128 PB - Springer AN - OPUS4-44689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scala-Benuzzi, M. L. A1 - Raba, J. A1 - Soler-Illia, G. J. A. A. A1 - Schneider, Rudolf A1 - Messina, G. A. T1 - Novel electrochemical paper-based immunocapture assay for the quantitative determination of ethinylestradiol in water samples N2 - We report a novel and innovative electrochemical paper-based immunocapture assay (EPIA) to address the need for ultrasensitive detection of emerging pollutants without regulatory status and whose effects on environment and human health are not completely yet understood. In particular, we present the application of this system toward highly sensitive detection of the emerging pollutant ethinyl estradiol (EE2). The EPIA approach is based on the use of paper microzones modified with silica nanoparticles (SNs) and anti-EE2 specific antibodies for capture and preconcentration of EE2 from river water samples. After the preconcentration procedure, the paper microzones are placed onto a screen-printed carbon electrode modified with electrochemically reduced graphene (RG). The bound EE2 is subsequently desorbed adding a diluted solution of sulfuric acid on the paper microzones. Finally, recovered EE2 is electrochemically detected by OSWV. The proposed novel methodology showed an appropriate LOD and linear range for the quantification of EE2 for water samples with different origins. The nonsophisticated equipment required, the adequate recovery values obtained (from 97% to 104%, with a RSD less than 4.9%), and the appropriate LOD and linear range value (0.1 ng L−1 and 0.5−120 ng L−1, respectively) achieved by our immunocapture sensor present significant analytical figures of merit, particularly when the routine quantification of EE2 is considered. In addition, our System was based on electrochemical paper-based technology, which allows obtainment of portable, easy-to-use, inexpensive, and disposable devices. The EPIA can also serve as a general-purpose immunoassay platform applicable to quantitation of other drugs and emerging pollutants in environmental samples. KW - Immunoassay KW - EE2 KW - Estrogens KW - Screen-printed electrode KW - Square-wave voltammetry PY - 2018 DO - https://doi.org/10.1021/acs.analchem.8b00028 SN - 0003-2700 SN - 1520-6882 VL - 90 IS - 6 SP - 4104 EP - 4111 PB - American Chemical Society CY - Washington, D.C., USA AN - OPUS4-44690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Immunoanalytical methods for screening and monitoring in environmental analysis N2 - A vast number of emerging pollutants has been detected in the environment over the last decades. Analytical methods suitable for trace analysis are needed that are desirably also fast, inexpensive and, if possible, robust and portable. Immunoanalytical methods which are available in a broad range of formats, can be profitably used here to analyze for the distribution and the trends of concentration levels of contaminants in the environment. Some of these formats are single-analyte but high-throughput methods. In order to use them wisely, indicator substances, sometimes called anthropogenic markers, should be selected and used in screening approaches. Other methods are suitable to be performed on portable instrumentation in the field (on-site) or in facilities such as wastewater treatment plants for on-line monitoring. Furthermore, there are the socalled array technologies that allow for parallel analysis of several analytes of interest (multiplexing). The microtiter-plate based ELISA (Enzyme-linked Immunosorbent Assay) is the method of choice for the analysis of a large number of samples [1]. ELISA screening data for anthropogenic markers such as the antiepileptic carbamazepine, the analgesic diclofenac, the anti-histaminic cetirizine, the steroid hormone estrone, the antimicrobial sulfamethoxazole, the stimulants caffeine and cocaine, the priority pollutant bisphenol A, and the bile acid isolithocholic acid [2] are presented. For on-site screening and monitoring, simpler formats, like mix-and-read assays, e.g. the Fluorescence Polarization Immunoassay (FPIA) or Lateral-flow Immunoassays (LFIA) are more suitable tools. Electrochemical formats run on portable devices provide additional advantages as no light source is required. Some examples are presented and discussed. The suitability of multi-analyte formats such as immunomicroarrays depends on the choice of a signal-producing system that provides small uncertainties and good reproducibility of the measurements. Biochip (“flat”) arrays read out on slide scanners and bead-based (“suspension”) arrays read out in flow cytometers are two options and show their distinct pros and cons. Altogether these approaches show the great potential immunoanalytical methods provide for the screening for environmental contaminants in the aquatic environment. T2 - analítica 2018 CY - Porto, Portugal DA - 26.03.2018 KW - Carbamazepine KW - Caffeine KW - Diclofenac KW - LC-ELISA KW - Fluorescence PY - 2018 AN - OPUS4-44691 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Evaluation of particle sizing techniques for the implementation of the EC definition of a nanomaterial N2 - Many techniques are available for measuring particle size distribution. For ideal materials (spherical particles, well dispersed) it is possible to evaluate the Performance of These methods. The performance of the analytical instrumentation for the purpose of classifying materials according to EC Definition is unknown. In this work the performance of commercially available particle sizing techniques on representative NanoDefine set of real-world testing materials (RTM) and quality control materials (QCM) for the implementation of the Definition is evaluated. T2 - 4. Sitzung des wissenschaftlichen Beirats zum Themefeld Umwelt der BAM CY - BAM, Berlin, Germany DA - 13.04.2018 KW - Nanoparticles KW - Nanomaterial KW - Characterization methods KW - EU definition KW - Nanodefine PY - 2018 AN - OPUS4-44693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - nPSize - Improved traceability chain of nanoparticle size measurements N2 - The overall objective of project Improved traceability chain of nanoparticle size measurements is to improve the traceability chain for nanoparticle size measurements. The main impact will be achieved by manifold contributions to standard documents for CEN/TC 352 “Nanotechnologies”, which directly addresses the research needs of CEN, CENELEC and ETSI mandated by EC to develop standards for methods and reference materials to accurately measure the size and size distribution of nanoparticles. This will take place in collaboration with ISO/TC229 ‘Nanotechnologies’, ISO/TC24/SC4 ‘Particle characterization’ and ISO/TC201 ‘Surface analysis’/ SC9 ‘Scanning probe microscopy’. T2 - 4. Sitzung des wissenschaftlichen Beirats zum Themefeld Umwelt der BAM CY - BAM, Berlin, Germany DA - 13.04.2018 KW - Nanoparticles KW - Nanoparticle size KW - Traceability KW - Standardization PY - 2018 AN - OPUS4-44695 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, Gudrun A1 - Emmerling, Franziska A1 - Kemnitz, Erhard T1 - Ca-Tetrafluorophthalate and Sr-isophthalate: mechanochemical synthesis and characterization in comparison with other Ca-and Sr-coordination polymers N2 - New Ca- and Sr-based coordination polymers (CPs) were mechanochemically synthesized by milling metal hydroxide samples (M = Ca, Sr) with tetrafluorophthalic acid (H2oBDC-F4) and isophthalic acid (H2mBDC). [Ca(oBDC-F4)(H2O)2] (1) exhibits a small surface area which is slightly increased after removing the crystal water. On the other hand, the hydrated sample of the nonfluorinated [Sr(mBDC)(H2O)3.4] (2) reveals a small BET surface area which remains unchanged even after the release of crystal water via thermal treatment. The new compounds 1 and 2 are similar to their Sr- and Ca-analogs, respectively. These findings are confirmed by thermal analysis, MAS NMR, and ATR-IR measurements, in addition to the Le Bail refinements for the measured powder X-ray data of 1 and 2. Ca- and Sr-CPs based on perfluorinated dicarboxylic systems and their nonfluorinated analogs diverse in structural and chemical properties depending on the geometries of the organic linkers and the presence of fluorine atoms. The fluorinations of organic ligands lead to the formation of fluorinated CPs with higher dimensionalities compared to their nonfluorinated counterparts. Conversely, the thermal stabilities of the latter are higher than those of the fluorinated CPs. KW - Mechanochemistry PY - 2018 DO - https://doi.org/10.1039/c8dt00695d SN - 1477-9226 SN - 1477-9234 VL - 47 IS - 16 SP - 5743 EP - 5754 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-44696 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Aktuelle Herausforderungen für die Prozessanalytik – von der Online-NMR-Spektroskopie im Feld bis zum Plasmaspektrometer auf dem Acker N2 - Der Vortrag stellt einige aktuelle Herausforderungen für die Prozessanalytik und mögliche Antworten vor. Gepulste Raman-Spektrometer akkumulieren das Raman-Signal mit Hilfe schneller optischer Schalter im Picosekunden-Bereich, bevor langlebigere Fluoreszenzanregung entsteht. Damit lassen sich stark fluoreszierende Materialien untersuchen, die bislang nicht zugänglich sind. Eine weitere interessante Entwicklung ist etwa die Shifted excitation Raman difference spectroscopy (SERDS) die besonders für biologische Anwendungen interessant ist. Flexible, modulare Produktionsanlagen stellen einen vielversprechenden Ansatz für die kontinuierliche Produktion von Fein- und Spezialchemikalien dar. In einem EU-Projekt wurde die Feldintegration eines Online-NMR-Sensormoduls als smartes Modul für die Prozesskontrolle vorangebracht. Dieses Modul basiert auf einem kommerziell erhältlichen Niederfeld-NMR-Spektrometer, welche zurzeit für die Anwendung im Laborbereich erhältlich ist. Für die Feldintegration wurde ein ATEX-zertifiziertes, explosionsgeschütztes Gehäuse entwickelt sowie Automationsschemen für den unbeaufsichtigten Betrieb und für die kalibrierfreie spektrale Datenauswertung erstellt. Eine sehr gut anwendbare analytische Messtechnik zur Kontrolle der elementaren Zusammensetzung von verschiedensten Materialien ist die laserinduzierte Plasmaspektroskopie (LIPS, engl. LIBS - Laser-induced Breakdown Spectroscopy). Bei der LIBS wird ein kurz gepulster Laser auf eine Probe fokussiert, um ein Leuchtplasma zu erzeugen. Das dabei erzeugte Atomemissionsspektrum ermöglicht eine qualitative und quantitative Analyse der Zusammensetzung der Probe bezüglich praktisch aller Elemente des Periodensystems. In einem aktuellen Projekt wird diese Methode neben anderen zur Online-Analyse von Ackerböden für die ortsspezifischer Bewirtschaftung (Precision Agriculture) weiterentwickelt und bewertet. T2 - Seminar der Institute Analytische Chemie CY - Universität Duisburg-Essen, Essen, Germany DA - 23.04.2018 KW - Prozessanalytik KW - Time-gated Raman-Spektroskpie KW - Online-NMR-Spektroskopie KW - Laser-induced Breakdown Spectroscopy KW - Online-RFA-Spektroskopie PY - 2018 AN - OPUS4-44754 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Leonhard, H. T1 - Schnell und einfach: Test auf Korrosionsgefahr N2 - Bei Unvollständigkeit oder Beschädigung der schützenden Passivschicht auf nichtrostenden Stahloberflächen ist es nicht weit bis zur Korrosion an Rohrsystemen oder Behältern. Schadensereignisse und Produktionsausfälle sind unausweichlich. KW - Nichtrostender Stahl KW - Korrosionsschnelltest KW - KorroPad KW - Passivschicht PY - 2018 SN - 1860-1901 IS - 1 SP - 20 EP - 21 PB - Verlag moderne Industrie GmbH CY - Landsberg AN - OPUS4-44755 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Leonhard, H. T1 - Tatort Stahl: Fehlstellen auf der Spur N2 - Rohrleitungssysteme und Behälter aus nichtrostendem Stahl sind mit einer Passivschicht vor Korrosion geschützt. Kritisch wird es, wenn diese Schicht unvollständig oder beschädigt ist. Ein Schnelltest soll Fehlstellen innerhalb von nur 15 Minuten überführen - auch ohne Spezialwissen. KW - Nichtrostender Stahl KW - Korrosionsschnelltest KW - KorroPad KW - Passivschicht PY - 2018 SN - 1614-7200 VL - 2018 IS - 4 SP - 66 EP - 68 PB - Publish Industry Verlag CY - München AN - OPUS4-44756 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Würth, Christian T1 - Systematic characterization of Upconversion nanoparticles: Effect of size, microenvironment, Energy transfer, shells N2 - Solid state multi-band emitters like lanthanide doped up-conversion nanoparticles (UCNPs) are promising materials for energy and biotechnologies. These materials are excitable in the near infrared (NIR) and show emission bands from UV to SWIR with excellent photostability, and long luminescence lifetimes in the µs range. The efficiency of these materials, i.e. the multiphoton absorption processes, the excitation power dependent population, and deactivation dynamics are strongly influenced by the particle size, structure, doping concentration, surface chemistry, and microenvironment. For applications UCNPs have to be optimized to meet the application relevant optical properties like the upconversion quantum yield (UC) and downshifting quantum yield (PL), luminescence lifetime and emission spectra. We investigated ß-NaYF4 NPs co-doped with Yb3+ and Er3+ in aqueous and organic media and as powder. For the later, bulk and nanomaterial is compared. For dispersed particles the influence of surface chemistry (ligands), microenvironment (solvent) and size (10 to 43 nm) was studied. Especially for bioapplications the Förster-Resonance-Energy-Transfer (FRET) efficiency from UCNPs to organic dye molecules (rose bengal and sulforhodamine B) was optimized with respect to the UCNP size. T2 - UpCon 2018 CY - Valencia, Spanien DA - 02.04.2018 KW - Nanoparticle KW - Upconversion KW - Quenching PY - 2018 AN - OPUS4-44762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Remmler, Dario T1 - Two-dimensional screening of large peptide libraries to identify solubilizers with tailored release capabilities N2 - Small organic molecule drugs are one of the key classes, taking increasingly important roles in modern drug development strategies. With the focus on small molecule drugs, difficulties originate frequently from a pronounced lipophilic character, resulting in poor water solubility, low bioavailability and unfavored pharmacokinetics. Recently, peptide-poly(ethylene glycol) conjugates (peptide-PEG conjugates) were described as precisely tunable platforms to solubilize a broad scope of fluorescent or non-fluorescent small organic molecules [1-2]. Selection of drug hosting peptides was achieved by combinatorial means, which can further be extended by implementation of a drug release screening step. One-bead-one-compound peptide libraries are powerful tools to select high affinity binders. However, the selection of positive hits from the peptide libraries remains tedious as it occurs by handpicking, strongly limiting the pool of investigated beads. Here we report our recent results on improving the analytical platform, using automated fluorescence scanning and MALDI-ToF-ToF MS/MS imaging to screen larger sets of beads, broadening the statistical base and unraveling more precisely suitable peptides. The screening puts special emphasis on loading capacities and drug-release of transporters by performing additional washing steps in different media (cf. Fig. 1). Peptides representing strong, medium, weak releaser were chosen for further analysis and synthesized as peptide-polymer transporters. Release was analyzed by fluorescence anisotropy and fluorescence correlation spectroscopy, due to the fluorescent characteristics of the drug. Solubilization studies confirmed sufficient loading capacities for a potential anti-Alzheimer disease drug of three transporter molecules representing strong/weak drug releaser, reaching solubilization of up to 1:3.4 (µmol drug/µmol conjugate). Fluorescence anisotropy and fluorescence correlation spectroscopy of the drug-loaded transporter showed significant differences in drug releasing properties, confirming the screening process. T2 - 15th European Symposium on Controlled Drug Delivery CY - Egmond aan Zee, The Netherlands DA - 11.04.2018 KW - Combinatorial library KW - Bioconjugates KW - Screening KW - Pharmaceuticals KW - Biotechnology KW - Drugs PY - 2018 AN - OPUS4-44713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian A1 - Franz, Philipp A1 - Wachtendorf, Volker A1 - Maierhofer, Christiane A1 - Fischer, C. ED - Ziegahn, K.-F. T1 - Additiv gefertigte Polymerbauteile: Untersuchung der Beständigkeit durch künstliche Bewitterung und zerstörungsfreie Charakterisierung N2 - Es wird ein Verfahren zur Charakterisierung der Beständigkeit und Langzeitstabilität von additiv gefertigten Kunststoff-Bauteilen vorgestellt. Dabei sollen die Prüfkörper über 2000 Stunden künstlich bewittert und währenddessen die Änderungen der Eigenschaften der Bauteile zerstörungsfrei untersucht werden. T2 - 47. Jahrestagung der Gesellschaft für Umweltsimulation e.V. CY - Stutensee, Germany DA - 21.03.2018 KW - Additive Fertigung KW - Künstliche Bewitterung KW - Thermografie KW - Additive manufacturing PY - 2018 VL - 47. SP - 99 EP - 105 PB - Gesellschaft für Umweltsimulatin e.V. AN - OPUS4-44638 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosner, Martin T1 - Intercomparison of delta26Mg Values in Mg Isotope RMs and Standards N2 - Accurate measurements of stable isotope abundance ratio variations are often reported using artifact based delta-scales, which rely on suitable isotopic reference materials (iRM) for their realization. For example, variations in the 26Mg/24Mg isotope abundance ratio in natural systems are typically reported as delta26Mg values that represents the relative difference between the 26Mg/24Mg ratio measured in a sample relative to its measurement preferably in an iRM. In the past, such delta26Mg measurements were referenced to NIST SRM 980, the initial zero of the delta26Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. It was then replaced by a Mg solution (DSM3), the new zero of the delta26Mg scale. A potential replacement iRM for DSM3 has been developed, ERM-AE143. This iRM has also been measured for its absolute isotope amount ratios1,2 making it traceable to the SI. The results of an delta26Mg intercomparison experiment include the Mg iRMs SRM 980, IRMM-009, ERM-AE143, AE144, AE145 standards DSM3 and Cambridge-1. The intercomparison involved 5 expert laboratories, consisting of 3 national metrological institutes (BAM, NIST, PTB) and 2 scientific research laboratories (GFZ Potsdam, UBremen). The iRMs were measured relative to AE143 and cover a range of ≈5 ‰ in delta26Mg. IRMM-009 has the lowest delta26Mg value while DSM3 has the highest, spanning a range in values that covers natural Mg isotope variations. The 2SD reproducibilities of the individual values from the different laboratories range from 0.02 to 0.26 ‰. The mean delta26Mg values, calculated from the laboratory means however show 2SD reproducibilities varing between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for delta26Mg determinations. T2 - Goldschmidt 2017 CY - Paris, France DA - 13.08.2017 KW - Magnesium delta value KW - Isotope reference material KW - Intercalibration KW - Magnesium isotope ratio PY - 2017 AN - OPUS4-44639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tatzel, Michael T1 - Exploring variations in the three-isotope space: A new approach and application to magnesium isotope fractionation in the mammal food web N2 - In chemical elements with three or more stable isotopes, mass-dependent stable isotope fractionation is expressed by co-varying isotope ratios. In the three-isotope space ((δ’m2/δ’m1)/(( δ’m3/δ’m1)) these plot along a line with a slope (β), the so called ‘terrestrial fractionation line’. This partitioning of stable isotopes results from both kinetic and equilibrium reactions that are characterized by specific β-values. For the natural range of isotope ratios of ‘novel’ stable isotope systems such as Si, Mg, Fe, Zn, Cu this information cannot be accessed because samples fall close to the delta-zero standard where the current measurement precision is too low to resolve small differences in β. We present a new approach to resolve deviations from a reference slope β by standard-sample bracketing against material offset from the natural range. We use this approach to explore the isotope fractionation mechanism in the mammalian food web. We have analyzed Mg stable isotope ratios in bone bioapatite of herbivore, omnivore and carnivore mammals. Positive shifts in δ26/24Mg along the trophic chain (from herbivore to carnivore) together with β= 0.513 suggest the presence of two isotope fractionation mechanisms operating during biomineralization. While positive shifts in δ26/24Mg are in favor of equilibrium isotope fractionation process, the proximity of β to the theoretically calculated β(kinetic) of typically 0.511 suggests the presence of a second component that fractionates stable isotopes kinetically. The herein presented approach is applicable to any element with 3+ stable isotopes analyzed by multi-collector inductively coupled plasma mass spectrometry. T2 - ESAS & CANAS 2018 CY - Berlin, Germany DA - 20.03.2018 KW - Magnesium delta values KW - Equilibrium isotope fractionation KW - Kinetic isotope fractionation KW - Measurement uncertainty KW - Mammals KW - Food web PY - 2018 AN - OPUS4-44643 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Absolute Isotope Ratios N2 - Measurement results and scientific models leading to important decisions in forensics, food fraud or climatology are based on isotope ratio data. Molar masses of multi-isotopic elements are as well based on isotope ratio data. Thus, in the case of Si, isotope ratios directly impact the redefinition of the SI base units kilogram and mole. Therefore, new strategies are required leading to new primary isotope reference materials, whose isotope ratios are traceable to the SI. This in turn will ensure the comparability of isotope ratio data and will render the traceability exception requested by the CCQM superfluous. Such new procedures will be developed for the key elements S, Si, Ca, Sr and Nd at relative uncertainty levels of ≤ 0.01 %. T2 - EURAMET TC-MC Meeting CY - Vienna, Austria DA - 05.02.2018 KW - Metrology in chemistry KW - Isotope amount ratio KW - SI traceability KW - Atomic weight KW - Molar mass KW - Synthetic isotope mixtures PY - 2018 AN - OPUS4-44644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - Switchable Rotaxanes operating in multilayers on solid supports N2 - Interfaces provide the structural basis for function as, for example, encountered in nature in the membrane-embedded photosystem or in technology in solar cells. Synthetic functional multilayers of molecules cooperating in a coupled manner can be fabricated on surfaces through layer-by-layer self-assembly. Ordered arrays of stimuli-responsive rotaxanes undergoing well-controlled axle shuttling are excellent candidates for coupled mechanical motion. Such stimuli-responsive surfaces may help integrating synthetic molecular machines in larger systems exhibiting even macroscopic effects or generating mechanical work from chemical energy through cooperative action. The present work demonstrates the successful deposition of ordered mono- and multilayers of chemically and photochemically switchable rotaxanes on gold surfaces. Two substrates are investigated – silicon and gold. Of these materials, only gold showed to be suitable for the development of highly preferential oriented rotaxane layers. XPS indicates for both substrates that our layer-by-layer approach worked and a layer growth with every deposition step is present. NEXAFS showed that both stimuli cause an increase of the multilayer's preferential orientation and that the switching is reversible. However, these effects are only observed for the multilayers on gold surfaces. T2 - DPG-Frühjahrstagung der Sektion Kondensierte Materie gemeinsam mit der EPS CY - Berlin, Germany DA - 11.03.2018 KW - XPS KW - NEXAFS KW - Rotaxanes KW - Multilayers PY - 2018 AN - OPUS4-44794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - Chemical Analysis of Core-Shell Nanoparticles using ToF-SIMS and XPS N2 - The analysis of nanomaterials is currently an important task - especially in case of risk assessment – as the properties of these material class are not well understood. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surface’s chemical composition must be investigated to get a better understanding and prediction of the nanomaterials’ behavior. ToF-SIMS and XPS have proven to be powerful tools to determine the general chemical composition. The superior surface sensitivity of ToF-SIMS furthermore allows us to study mainly the utmost atomic layer and thus gives us an idea of the interactions involved. Here, we present initial data on the analysis of Hyflon®-polystyrene core-shell nanoparticles which can be used as a model system due to the known preparation and a rather good chemical as well as physical separation of core and shell. Furthermore, principle component analysis (PCA) will be used to detect the influence of sample preparation and for a better separation of different samples. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - XPS KW - ToF-SIMS KW - Nanoparticles PY - 2018 AN - OPUS4-44795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nöller, Renate T1 - Mit Zinnoberrot markiert-Pigmentanalyse zur Zuordnung von Manuskripten der Seidenstraße N2 - Zinnober (HgS) ist neben Eisenoxiden (Fe2O3 oder FeOOH) das am häufigsten verwendete mineralische Rotpigment. Die relativ seltenen Vorkommen in der Natur wurden schon in der Vorgeschichte abgebaut und in Gräbern und auf Felsmalerei als rote Farbe verwendet. In Asien spielt Zinnoberrot als Schreibtusche eine wichtige Rolle. Besonders zur Zeit des Buddhismus findet sich das Rot verstärkt auch auf Wandmalerei und Statuen. Schon früh beherrschte man die synthetische Herstellung und Optimierung des Pigments mit Zusatzstoffen, so dass von einer regional unterschiedlichen Verarbeitung auszugehen ist. Auf Grund seiner physikalisch-chemischen Eigenschaften (gute Eindringtiefe, konservierende Wirkung) wurde das leuchtend rote Farbpigment auch als Handelsware genutzt. Die Pigmentanalyse gibt Auskunft über - kulturelle Vorkommen, die Nutzung von Zinnober als Rotpigment in einem bestimmten Kontext. - natürliche Vorkommen, die Herkunft des Minerals entsprechend der regionalen Bildungsbedingungen. - Werkstätten, die Herstellung als Farbpigment mit unterschiedlichen Techniken. Vorgestellt werden rote Tinten und Tuschen auf Schriftstücken der Seidenstraßenkulturen mit Zinnober als charakteristisch für eine bestimmte Tradition in der Verwendung und möglicher Indikator für kulturellen Austausch. Die in unterschiedlichen Schriften und Sprachen erhaltenen Manuskriptfragmente gelangten Anfang des letzten Jahrhunderts von der Oasenstadt Turfan nach Berlin, wo sie entziffert und kulturhistorisch erforscht werden. Die chemische Zusammensetzung ihrer Rottöne wird differenziert und in Rückkopplung mit der historischen Klassifikation der untersuchten Objekte verglichen. Eine solche Identifizierung von Farbtypen kann zur Einordnung von Kulturobjekten fragwürdiger Herkunft herangezogen werden. T2 - Konservierungswissenschaft im Dialog 2016, Öffentliche Vortragsreihe des Rathgen-Forschungslabors CY - Staatliche Museen zu Berlin, Germany DA - 2016 KW - Zinnoberrot KW - Pigmentanalyse KW - Manuskripte KW - Seidenstraßenkultur PY - 2016 AN - OPUS4-44796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nöller, Renate T1 - Characteristic features of lapis lazuli from different provenances revised by μXRF and ESEM N2 - The objective of this study is to find out how far geochemical characteristics of the blue mineral pigment can be confirmed in respect to its provenance. In dependence of the quantity of samples analysed from a special geological region and the methods applied, a range of variation is taken into consideration. To provide clues, a multi-technique analytical approach with µXRF and ESEM is applied to samples from the most famous deposits. Special elements determined as fingerprint are related to the textural features corresponding directly to the geological conditions of forming. The results and the statistical output allow a differentiation that enables an optimized local classification of the blue stone. To be aware of the limits of analysis is an absolute requirement for each geo-tracing implemented on blue coloured cultural objects of unknown provenance. For testing the possible sources of lapis lazuli, the blue pigment used as paint on murals and as ink on manuscripts from the Silk Road is analysed in an exemplary way. T2 - International Symposium of Archaeometry ISA CY - Kalamaka, Greece DA - 15.05.2016 KW - Lapis Lazuli KW - Provenance studies KW - µXRF KW - ESEM PY - 2016 AN - OPUS4-44797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Volume specific surface area (VSSA) by BET as a reliable metric for (nano)particle size analysis for powders N2 - We discuss the role of the volume specific surface area (VSSA) as determined from the specific surface area measured by the (extended) Brunauer-Emmett-Teller (BET) technique, in the identification process of powdered nano- and non-nanomaterials in line with the EU definition of nanomaterial. Results obtained in the NanoDefine project demonstrate that under appropriate conditions, VSSA can be used as proxy to the number-based particle size distribution. The extent of agreement between nano/non-nano classification by electron microscopy (EM) and classification by VSSA is investigated systematically on a large set of diverse particulate substances, representing most of the cases expected in regulatory practice. Thus, parameters such as particle shape, size polydispersity/multi-modality, and particle (inner or coating) porosity are evaluated. Based on these results, we derive a tiered screening strategy for powders, involving the use of VSSA for the purpose of implementing the definition of nanomaterial, and recommend it for inclusion in a technical guidance for the implementation of the definition. T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - Nanoparticles KW - Nanomaterial KW - Particle size distribution KW - BET KW - VSSA PY - 2018 AN - OPUS4-44801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schäferling, Michael T1 - Effects of solvent and excitation power on ratiometric upconversion luminescence based temperature sensing using NaYF4:Yb3+,Er3+ N2 - Thermal sensing using the luminescence intensity ratio of the green Er3+ emissions is affected by the solvent and requires steady-state conditions during the excitation. It is important to keep the excitation power at a moderate level or short exposure times to avoid local heating of aqueous samples. The solvent also determines whether the red emission of Er3+ is excited via a two- or three-photon process. T2 - 2nd conference on properties, design and applications of upconversion nanomaterials CY - Valencia, Spain DA - 04.04.2018 KW - Upconversion luminescence KW - Temperature sensing KW - Excitation path PY - 2018 AN - OPUS4-44819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - A standard procedure for the irradiation of biomolecules with radiation of varying linear energy transfer N2 - The damage caused by ionizing radiation to DNA and proteins is the reason to treat cancer by radiation therapy. A better understanding of the molecular processes and quantification of the different damaging mechanisms is the prerequisite to develop more efficient therapies. Hereby the understanding of the processes involved in the damage to DNA are of key interest due to its central role in reproduction and mutation. For radiation with low linear energy transfer (LET), most of the damage is caused by the secondary particles produced by scattering of the ionizing radiation with water. Thereby a multitude of species are produced, whereby especially kinetic low energy electrons, prehydrated electrons, OH-radicals and ions are of importance. With higher LET the relative amount of the direct damaging effects increases. This is especially important considering the increased usage of high LET nucleons in radiation therapy. Therefore, the quantification of the contribution to DNA damage of direct and indirect effects and the different secondary species is of high interest due to the increase of radio biological efficiency when applying high LET radiation. Here we present an approach to investigate the relative contributions to DNA strand break yield for radiation of different LET within a single electron microscope in combination with electron scattering simulations. T2 - IRPA 2018 CY - Havanna, Cuba DA - 16.04.2018 KW - Dosimetry KW - Microdosimetry KW - LET KW - SEM KW - DNA KW - Radiation damage KW - OH radicals KW - LEE KW - Ionizing radiation KW - Geant4 PY - 2018 AN - OPUS4-44820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Development of a standard procedure for the irradiation of biomolecules N2 - The damage caused by ionizing radiation to DNA and proteins is the reason to treat cancer by radiation therapy. A better understanding of the molecular processes and quantification of the different damaging mechanisms is the prerequisite to develop more efficient therapies. Hereby the understanding of the processes involved in the damage to DNA are of key interest due to its central role in reproduction and mutation. For radiation with low linear energy transfer (LET), most of the damage is caused by the secondary particles produced by scattering of the ionizing radiation with water. Thereby a multitude of species are produced, whereby especially kinetic low energy electrons, prehydrated electrons, OH-radicals and ions are of importance. With higher LET the relative amount of the direct damaging effects increases. This is especially important considering the increased usage of high LET nucleons in radiation therapy. Therefore, the quantification of the contribution to DNA damage of direct and indirect effects and the different secondary species is of high interest due to the increase of radio biological efficiency when applying high LET radiation. Here we present an approach to investigate the relative contributions to DNA strand break yield for radiation of different LET within a single electron microscope in combination with electron scattering simulations. T2 - IRPA 2018 CY - Havanna, Cuba DA - 16.04.2018 KW - DNA KW - Radiation damage KW - Ionizing radiation KW - Linear energy transfer KW - IRPA KW - LET KW - Electrons KW - SEM KW - Cancer therapy KW - OH radicals KW - LEE KW - Geant4 PY - 2018 AN - OPUS4-44821 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Andresen, Elina T1 - Functionalisation studies of UCNPs for pH-sensing N2 - Functionalisation of UCNPs with analyte-responsive dyes as resonance energy transfer (RET)acceptors, which is in the focus of our work, will yield chemoresponsive nanoprobes with unique features: they can be excited in the NIR range (which minimizes the photo-damage of biological samples, as well as the autofluoresence background) and one of their several sharp UC emission bands can be used as donor for RET sensing applications in combination with analyte-sensitive dyes which serve as indicators, whereas the other UC band(s) can act as internal reference. The first step upon preparation of such nanosensors is the functionalisation of the UCNPs with different surface chemistries for indicator conjugation. Desirable are systems with short distance between the UCNP(donor) and the indicator (acceptor) as a prerequisite for efficient RET. Additionally, dyes with a large spectral overlap between their absorption and one of the UC emission bands are required. Several classes of pH-responsive fluorescent dyes like xanthenes are eligible. Here, we present first studies to optimize the surface functionalization to achieve high RET efficiencies, which would improve the performance of such nanosensors for ratiometric fluorescence measurements of pH in biological matrices. T2 - 2nd Conference on Properties, Design and Applications of Upconversion Nanomaterials CY - Valencia, Spain DA - 04.04.2018 KW - PH-sensing KW - Upconverting nanoparticles KW - Rhodamine PY - 2018 AN - OPUS4-44823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eisenreich, F. A1 - Kathan, M. A1 - Dallmann, A. A1 - Ihrig, S. P. A1 - Schwaar, Timm A1 - Schmidt, B. M. A1 - Hecht, S. T1 - A photoswitchable catalyst system for remote-controlled (co)polymerization in situ N2 - The fundamental properties of a polymeric material are ultimately governed by its structure, which mainly relies on monomercomposition and connection, topology, chain length, and polydispersity. Thus far, these structural characteristics are typicallyset ex situ by the specific polymerization procedure, eventually limiting the future design space for the creation of moresophisticated polymers. Herein, we report on a single photoswitchable catalyst system, which enables in situ remote controlover the ring-opening polymerization of l-lactide and further allows regulation of the incorporation of trimethylene carbonateand δ -valerolactone monomers in copolymerizations. By implementing a phenol moiety into a diarylethene-type structure,we exploit light-induced keto–enol tautomerism to switch the hydrogen-bonding-mediated monomer activation reversiblyON and OFF. This general and versatile principle allows for exquisite external modulation of ground-state catalysis of a livingpolymerization process in a closed system by ultraviolet and visible light and should thereby facilitate the generation of newpolymer structures. KW - Polymers PY - 2018 DO - https://doi.org/10.1038/s41929-018-0091-8 SN - 2520-1158 VL - 1 IS - 7 SP - 516 EP - 522 PB - Nature CY - London AN - OPUS4-45407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altenburg, Simon T1 - Continuous and Laplace transformable approximation for the temporal pulse shape of Xe-flash lamps for flash thermography N2 - In flash thermography, the temperature transient is strongly influenced by the temporal shape of the heating pulse for samples with high thermal diffusivity or very thin samples. Here, we present a closed phenomenological approximation of the temporal shape of pulses of Xe-flash lamps. It is a non-stitched solution, has a simple Laplace transform and is suitable for different lamps and energy settings. It is demonstrated that simulated temperature transients, based on this approximation, are well consistent with experimental data. T2 - 14th Quantitative InfraRed Thermography Conference CY - Berlin, Germany DA - 25.06.2018 KW - Finite pulse length KW - Flash thermography KW - Laplace transform KW - NDT KW - Pulse shape KW - Thickness determination PY - 2018 AN - OPUS4-45411 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Batzorig, L. T1 - Certified reference material of total cyanide in soil/BAM-U 116/CGL 306 N2 - Due to their toxicity and widespread application for mining and industrial purposes, cyanides are ranking among the most important inorganic pollutants which should be tested and monitored not only in the aquatic environment, but also in soils and soil-like materials. Reference materials of soils with relevant contents of cyanide to ensure reliable test results of laboratories are rare today. New certified reference material (CRM) BAM-U116/CGL306 “Cyanide in soil” was produced within a framework of cooperation between Central Geological Laboratory (CGL) of Mongolia and Federal Institute for Materials Research and Testing (BAM) of Germany in 2013-2017. The CRM BAM-U116/CGL306 represents a mixture of a sandy soil collected from a contaminated former gasworks area in the Berlin region (Germany) and an unpolluted sandy soil from Nalaikh region (Mongolia). The bulk candidate material for this reference material was prepared at CGL CRM Laboratory exclusively destined to the preparation of reference materials and equipped with modern technical equipment. Homogeneity, stability and shelf life were studied in full compliance with ISO Guide 35. The CRM was evaluated as sufficiently homogeneous. Statistical evaluation of certification analysis was performed using software packages SoftCRM and ProLab Plus. Certified value of total cyanide of the CRM is 12.0 mg/kg and expanded uncertainty was assigned as 0.8 mg/kg. The intended purpose of this material is the verification of analytical results obtained for the mass fraction of total cyanide in soils and soil-like materials applying the standardized procedure ISO 11262:2011. As any reference material, it can also be used for routine performance checks (quality control charts) or validation studies. T2 - Geoanalysis 2018 CY - Sydney, Australia DA - 08.07.2018 KW - Certified reference material KW - Cyanide in soil KW - Total cyanide PY - 2018 AN - OPUS4-45417 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meiling, T. T. A1 - Schürmann, Robin A1 - Vogel, Stefanie A1 - Ebel, Kenny A1 - Nicolas, C. A1 - Milosavljević, A. R. A1 - Bald, Ilko T1 - Photophysics and chemistry of nitrogen-doped carbon nanodots with high photoluminescence quantum yield N2 - Fluorescent carbon nanodots (CNDs) are very promising nanomaterials for a broad range of applications because of their high photostability, presumed selective luminescence, and low cost at which they can be produced. In this respect, CNDs are superior to well-established semiconductor quantum dots and organic dyes. However, reported synthesis protocols for CNDs typically lead to low photoluminescence quantum yield (PLQY) and low reproducibility, resulting in a poor understanding of the CND chemistry and photophysics. Here, we report a one-step synthesis of nitrogen-doped carbon nanodots (N-CNDs) from various carboxylic acids, Tris, and ethylenediaminetetraacetic acid resulting in high PLQY of up to 90%. The reaction conditions in terms of starting materials, temperature, and reaction time are carefully optimized and their influence on the photophysical properties is characterized. We find that citric acid-derived N-CNDs can result in a very high PLQY of 90%, but they do not Show selective luminescence. By contrast, acetic acid-derived N-CNDs show selective luminescence but a PLQY of 50%. The chemical composition of the surface and core of these two selected N-CND types is characterized among others by high-Resolution synchrotron X-ray photoelectron spectroscopy using single isolated N-CND clusters. The results indicate that photoexcitation occurs in the N-CND core, whereas the emission properties are determined by the N-CND surface groups. KW - Carbon nanodots KW - Fluorescence KW - Synchrotron XPS PY - 2018 DO - https://doi.org/10.1021/acs.jpcc.8b00748 SN - 1932-7447 VL - 122 IS - 18 SP - 10217 EP - 10230 PB - American Chemical Society CY - Washington, DC AN - OPUS4-45426 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - López-Serrano Oliver, Ana A1 - Baumgart, S. A1 - Bremser, Wolfram A1 - Flemig, Sabine A1 - Wittke, D. A1 - Grützkau, A. A1 - Luch, A. A1 - Haase, A. A1 - Jakubowski, Norbert T1 - Quantification of silver nanoparticles taken up by single cells using inductively coupled plasma mass spectrometry in the single cell measurement mode N2 - The impact of nanoparticles, NPs, at the single cell level has become a major field of toxicological research and different analytical methodologies are being investigated to obtain biological and toxicological information to better understand the mechanisms of cell–NP interactions. Here, inductively coupled plasma mass spectrometry in the single cell measurement mode (SC-ICP-MS) is proposed to study the uptake of silver NPs, AgNPs, with a diameter of 50 nm by human THP-1 monocytes in a proof-ofprinciple experiment. The main operating parameters of SC-ICP-MS have been optimized and applied for subsequent quantitative analysis of AgNPs to determine the number of particles in individual cells using AgNP suspensions for calibration. THP-1 cells were incubated with AgNP suspensions with concentrations of 0.1 and 1 µg/mL for 4 and 24 hours. The results reveal that the AgNP uptake by THP-1 monocytes is minimal at the lower dose of 0.1 µg/mL (roughly 1 AgNP per cell was determined), whereas a large cell-to-cell variance dependent on the exposure time is observed for a 10 times higher concentration (roughly 7 AgNPs per cell). The method was further applied to monitor the AgNP uptake by THP-1 cells differentiated macrophages incubated at the same AgNP concentration levels and exposure times demonstrating a much higher AgNP uptake (roughly from 9 to 45 AgNPs per cell) that was dependent on exposure concentration and remained constant over time. The results have been compared and validated by sample digestion followed by ICP-MS analysis as well as with other alternative promising techniques providing single cell analysis. KW - Silbernanopartikel KW - ICP-MS KW - Einzelzellanalyse PY - 2018 DO - https://doi.org/10.1039/C7JA00395A SN - 0267-9477 VL - 33 IS - 7 SP - 1256 EP - 1263 PB - Royal Society of Chemistry CY - London AN - OPUS4-45473 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Almeida, Â. T1 - Pharmaceutical drugs under an ocean acidification scenario: the biochemical and transcriptomic effects on the clam Ruditapes philippinarum N2 - Carbamazepine (CBZ) and cetirizine (CTZ) are pharmaceutical drugs detected in the aquatic environment. However, the effects to marine invertebrates derived from the combination of these drugs with decreased pH conditions due to ocean acidification are poorly explored. This study investigated the biochemical parameters related to metabolic capacity and oxidative stress response and the transcription of genes related to the mode of action (MoA) of CBZ (1.0 μg/L) and CTZ (0.6 μg/L) in the clam Ruditapes philippinarum chronically exposed (28 days) to control (7.8) and low (7.5) pH conditions. The biochemical parameters applied were: the activity of electron transport system (indicator of organisms’ metabolic capacity); lipid peroxidation content (indicator of cell damage); total glutathione peroxidase activity (indicator of antioxidant defense). The transcription of genes related with drug neurotransmission and metabolism, cell defense and immunity and biomineralization was studied. No metabolic changes and oxidative stress was induced by the exposure to CBZ or CTZ at each pH level, but the transcription of several genes related with the MoA (neurotransmission, immunity and biomineralization) was altered by low pH, drug exposure and the combination of both stressors. In conclusion, it was shown that the interaction of drug exposure and low pH conditions can change bivalves’ sensitivity to drugs or alter drugs toxicity. T2 - 31st Congress of the New European Society for Comparative Physiology and Biochemistry ESCPB CY - Porto, Portugal DA - 09.09.2018 KW - Pharmaceutical Drugs KW - Climate Changes KW - Bivalves KW - Biomarkers KW - Transcriptomic PY - 2018 AN - OPUS4-45474 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Stephan T1 - New immunoassay for quantification of diclofenac in water samples N2 - Diclofenac (DCF) is a widely used drug against fever, inflammation, pain, and rheumatic diseases. An average of 70 % of the ingested diclofenac is excreted in the urine. Thus, 63 tons per year are introduced into the water cycle in Germany. Due to insufficient removal of diclofenac in wastewater treatment plants, residues of diclofenac can be found in surface water and sometimes in drinking water. In order to establish an immunoassay, an anti-DCF antibody was required. Some antibody developments have been reported, based on an immunogen resulting from direct coupling of diclofenac to proteins via the carboxylic function. Finally, we used a monoclonal antibody, clone F01G21. T2 - Tag der Biotechnologie der TU Berlin CY - Berlin, Germany DA - 13.07.2018 KW - Wasserproben KW - Arzneimittel KW - Antikörper KW - ELISA PY - 2018 AN - OPUS4-45475 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baldofski, Stefanie T1 - Hapten Design for the Production of Antibodies against Small Molecules N2 - Highly selective and sensitive antibodies are only available for a limited number of small molecules. Hence the development of new antibodies is important to exploit the full potential of immunoanalytics. Small molecules do not elicit an immune response in mammals unless conjugated to carrier molecules. The choice of the structures to be conjugated, called haptens, is critical for the antibody production. Here we present our Approach to produce antibodies for the plasticizer diisononyl 1,2-cyclehexane-dicarboxylic acid (DINCH) and di-2-ethylhexyl terephthalate (DEHT) as well as the bile acid isolithocholic acid (ILA). T2 - Tag der Biotechnologie der TU Berlin CY - Berlin, Germany DA - 13.07.2018 KW - Antikörper KW - ELISAS KW - Immunoassay KW - Phthalate KW - Weichmacher KW - DINCH KW - DEHT KW - Isolithocholsäure KW - Isolithocholic Acid PY - 2018 AN - OPUS4-45476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziegler, Mathias A1 - Thiel, Erik A1 - Studemund, T. T1 - Thermography using a 1D laser array – From planar to structured heating N2 - In the field of optically excited thermography, flash lamps (impulse shaped planar heating) and halogen lamps (modulated planar heating) have become established for the specific regimes of impulse and lock-in thermography. Flying-spot laser thermography is implemented by means of a rasterized focused laser, e. g. for crack detection (continuous wave operation) and photothermal material characterization (high-frequency modulated). The availability of novel technologies, i. e. fast and high-resolution IR cameras, brilliant innovative light sources and high-performance data acquisition and processing technology will enable a paradigm shift from stand-alone photothermal and thermographic techniques to uniform quantitative measurement and testing technology that is faster and more precise. Similar to an LED array, but with irradiance two orders of magnitude higher, a new type of brilliant laser source, i. e. the VCSEL array (vertical-cavity surface-emitting laser), is now available. This novel optical energy source eliminates the strong limitation to the temporal dynamics of established light sources and at the same time is spectrally clearly separated from the detection wavelength. It combines the fast temporal behavior of a diode laser with the high optical irradiance and the wide illumination area of flash lamps. In addition, heating can also be carried out in a structured manner, because individual areas of the VCSEL array can be controlled independently of each other. This new degree of freedom enables the development of completely new thermographic NDT methods. KW - Thermography KW - Laser thermography KW - Laser KW - Lock-in KW - VCSEL KW - Thermal wave KW - Photothermal PY - 2018 UR - https://www.hanser-elibrary.com/doi/abs/10.3139/120.111209 DO - https://doi.org/10.3139/120.111209 SN - 0025-5300 VL - 60 IS - 7-8 SP - 749 EP - 757 PB - Carl Hanser Verlag CY - München AN - OPUS4-45482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Remmler, Dario A1 - Schwaar, Timm A1 - Pickhardt, M. A1 - Donth, C. A1 - Mandelkow, E. A1 - Weller, Michael G. A1 - Börner, H. T1 - On the way to precision formulation additives: 2D-screening to select solubilizers with tailored host and release capabilities N2 - A 2-dimensional high-throughput screening method is presented to select peptide sequences from large peptide libraries for precision formulation additives, having a high capacity to specifically host a drug of interest and provide tailored drug release properties. The identified sequences are conjugated with poly(ethylene glycol) (PEG) to obtain peptide-PEG conjugates that proved to be valuable as solubilizers for small organic molecule drugs to overcome limitations of poor water-solubility and low bio-availability. The 2D-screening method selects peptide sequences on both (i) high loading capacities and (ii) preferred drug-release capabilities as demonstrated on an experimental Tau-protein aggregation inhibitor/Tau- deaggregator with potentials for an anti-Alzheimer disease drug (BB17). To enable 2D-screening, a one-bead one-compound (OBOC) peptide library was immobilized on a glass slide, allocating individual beads to permanent positions. While the first screening step involved incubation of the supported OBOC library with BB17 to identify beads with high drug binding capacities by fluorescence scanner readouts, the second step reveals release properties of the high capacity binders by incubation with blood plasma protein model solutions. Efficiently peptides with high BB17 capacities and either keeper or medium or fast releaser properties can be identified by direct sequence readouts from the glass slide supported resin beads via matrix-assisted laser desorption/ionization time-of-flight tandem mass spectrometry. Four peptides are synthesized as peptide-PEG solubilizers representing strong, medium, weak releasers and non-binders. Loading capacities reached up to 1:3.4 (mol drug per mol carrier) and release kinetics (fast/medium/slow) are in agreement with the selection process as investigated by fluorescence anisotropy and fluorescence correlation spectroscopy. The ability of BB17/conjugate complexes to inhibit the aggregation of Tau4RDΔK (four repeat Tau ((M)Q244-E372 with deletion of K280), 129 residues) in N2a cells is studied by a Tau-pelleting assay showing the modulation of cellular Tau aggregation. Promising effects such as the reduction of 55% of total Tau load are observed for the strong releaser additive. Studies of in vitro Thioflavin S Tau-aggregation assays show half-maximal inhibitory activities (IC50 values) of BB17/conjugates in the low micro-molar range. KW - Block copolymer KW - Drug transporters KW - Peptide library screening KW - Formulation additives PY - 2018 DO - https://doi.org/10.1016/j.jconrel.2018.06.032 SN - 0168-3659 SN - 1873-4995 VL - 285 SP - 96 EP - 105 PB - Elsevier CY - Amsterdam AN - OPUS4-45483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schade, U. A1 - Ritter, E. A1 - Aziz, E. F. A1 - Puskar, L. A1 - Beckmann, Jörg T1 - Spectroscopic ellipsometry on liquids in the far infrared N2 - The far infrared refractive indices and the extinction coefficients of liquids can be obtained by means of spectroscopic ellipsometry in attenuated total reflection configuration. Such optical constants will contribute to a spectroscopic data base in the far infrared and terahertz spectral regions. The experimental implementation and the calibration procedure of the method are described in detail. The temperature dependency of the optical constants for water over a broad spectral range is exemplarily presented. T2 - 42nd International Conference on Infrared, Millimeter and THz Waves CY - Cancun, Mexico DA - 27.08.2017 KW - Ellipsometry KW - Far Infrared KW - ATR KW - Attenuated total reflection KW - Calibration KW - Extinction coefficients KW - Refractive index measurement KW - Spectroscopic ellipsometry KW - Far infrared refractive index KW - Terahertz spectral region KW - Optical constant KW - Attenuated total reflection configuration KW - Liquid extinction coefficient KW - Optical refraction KW - Optical variables control KW - Optical reflection KW - Liquids KW - Optical films KW - Optical polarization KW - Optical variables measurement PY - 2017 UR - http://ieeexplore.ieee.org/stamp/stamp.jsp?tp=&arnumber=8066931&isnumber=8066832 DO - https://doi.org/10.1109/IRMMW-THz.2017.8066931 SN - 2162-2035 SP - MD.1.5-1 EP - MD.1.5-2 PB - IEEE CY - Danvers AN - OPUS4-42028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg A1 - Spranger, Holger T1 - THz-TDS-SAFT for the detection of inherent discontinuities in dielectric materials N2 - Today X-ray tomography and Ultrasound Synthetic Aperture Focusing Techniques are representative examples for defect imaging in the field of nondestructive testing. THz time domain spectroscopy (TDS) operates with short electromagnetic pulses. The sensitivity of the pulses to optical material property changes makes THz-TDS attractive for the detection of flaws in dielectric materials. Unfortunately, the X-ray computed tomography (CT) model holds only for THz-TDS reconstruction if minor refraction index differences between the inhomogeneities and the surrounding material matrix exist. A Time Domain SAFT algorithm has been developed to overcome the restrictions. THz time domain measurement on representative sample sets with inherent artefacts were performed to use them for the Image reconstructions. The results will be presented and compared with optical surface images of the used test objects to evaluate the SAFT algorithm in relation to the econstruction quality. T2 - 42nd International Conference on Infrared, Millimeter and Terahertz Waves CY - Cancun, Mexico DA - 27.08.2017 KW - THz-TDS-Saft KW - Tomography KW - Dielectric materials KW - Image reconstruction KW - Terahertz spectroscopy KW - Terahertz wave imaging KW - Time-domain analysis KW - X-ray tomography KW - Ultrasound synthetic aperture focusing techniques KW - Terahertz time domain spectroscopy KW - Time domain SAFT algorithm KW - Image reconstructions KW - Optical surface images KW - Computed tomography KW - Dielectrics KW - Time measurement KW - Reflection PY - 2017 UR - http://ieeexplore.ieee.org/stamp/stamp.jsp?tp=&arnumber=8067159&isnumber=8066832 SN - 978-1-5090-6048-1 DO - https://doi.org/10.1109/IRMMW-THz.2017.8067159 SP - TD.19-1 EP - TD.19-2 PB - IEEE CY - Danvers, USA AN - OPUS4-42030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg T1 - THz-TDS-SAFT for the detection of inherent discontinuities in dielectric materials N2 - X-ray computed tomography (CT) model holds only for THz-TDS reconstruction if minor refraction index differences between the inhomogeneities and the surrounding material matrix exist. A Time Domain SAFT algorithm has been developed to overcome the restrictions. THz time domain measurement on representative sample sets with inherent artefacts were performed to use them for the Image reconstructions. The results will be presented and compared with optical surface images of the used test objects to evaluate the SAFT algorithm in relation to the reconstruction quality. T2 - 42nd International Conference on Infrared, Millimeter and THz waves CY - Cancun, Mexico DA - 27.08.2017 KW - THz-time-domain spectroscopy KW - SAFT KW - Tomography PY - 2017 AN - OPUS4-42034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Comparison of Raman spectroscopic approaches for the quantitative characterization of Escherichia coli cultivation samples N2 - The growing need to implement sensors such as NIR or Raman spectroscopy for the in-situ monitoring of bioprocesses which follows the standards of Quality by Design is either restricted by the impact of the huge water signal or by a disturbing fluorescence background originating from compounds in the culture media. Furthermore, the characterization of the bioprocess samples is challenging due to changing conditions in course of cultivation. Here we evaluate two different process-suitable Raman spectroscopic approaches, namely time-gated Raman which bears the potential to extract the Raman signal from the fluorescence background, and cw- Raman with NIR excitation in combination with Surface Enhanced Raman Spectroscopy- (SERS) to investigate cell-free supernatants of Escherichia coli sampled over the course of a cultivation. A confocal Raman microscope was used as a reference for the process devices. The concentration of the analytes, glucose, acetate as well as metabolites such as cAMP, AMP and amino-acids were determined by offline by High-Performance Liquid Chromatography (HPLC) to serve as reference for the calibration of the Raman and SERS spectral data. Multivariate evaluation of the Raman and SERS spectra by Partial Least Squares Regression (PLSR) yielded for most of the analytes robust correlations at each sampling point. Repeated investigation of the off-line samples over a larger experimental period suggested not only a high reliability of the Raman data in general but also a high repeatability of the SERS experiments. Similar spectral features in different quality and signal/noise ratios were measured with all three set-ups. Major results of the comparison of the different Raman spectroscopic approaches and their combination with SERS are summarized and conclusions are drawn on which approach provides the most accurate concentration data among the target analytes. Acknowledgement The authors kindly thank Mario Birkholz (IHP, Frankfurt (Oder), Germany) for the opportunity to use a confocal Raman microscope, Alex Bunker and Tapani Viitala (Division of Pharmaceutical Biosciences, Centre for Drug Research, University of Helsinki, Finland). T2 - PAT ERFA Workshop 2017 CY - Basel, Switzerland DA - 19.09.2017 KW - TimeGated KW - Raman KW - SERS KW - Bioprocess PY - 2017 AN - OPUS4-42118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Werner, Klaus-Dieter A1 - Johann, Sergej A1 - Daum, Werner ED - Cosmi, F. T1 - Characterization of the temperature behavior of a piezoresistive accelerometer N2 - Piezoresistive accelerometers use a strain-sensing element, generally made of semiconductor material, e.g., silicon to convert the mechanical motion into an electrical signal. This element is usually designed in form of a cantilever beam loaded with a mass. Acceleration causes bending of the beam, which produces a change of electrical resistance proportional to the applied acceleration. Main advantages of piezoresistive accelerometers in comparison to other types, e.g., piezoelectric and capacitive, is their robust and highly dynamic behavior, which qualifies them for application in high impact shock applications. Mechanical damping is typically implemented with silicon oil in a way that the output signal is undistorted over a wide frequency range. These characteristics principally qualify them for the application in drop tests carried out at BAM, for which they are calibrated over the frequency range from 1 to 4 kHz. However, using silicon oil for damping, has the drawback of temperature dependent change of its viscosity, leading to temperature dependent deviation of the accelerometer’s sensitivity. This study presents experimental results of the temperature behavior of a piezoresistive accelerometer with a dynamic range up to ±5000 g. This type of accelerometer is applied for drop tests which are partially performed at temperatures of -40 or +100 °C. T2 - 34th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Trieste, Italy DA - 19.09.2017 KW - Accelerometer KW - Temperature behavior KW - Drop test PY - 2017 UR - https://www.openstarts.units.it/handle/10077/14921 SN - 978-88-8303-863-1 SP - 93 EP - 95 CY - Trieste AN - OPUS4-42109 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, Norman A1 - Jadhav, A. A1 - Shreykar, M. A1 - Behnke, Thomas A1 - Nirmalananthan-Budau, Nithiya A1 - Resch-Genger, Ute A1 - Sekar, N. T1 - Coumarin-rhodamine hybrids-novel probes for the optical measurements of viscosity and polarity N2 - A comprehensive systematic study of Absorption and fluorescence properties in solvents of varying viscosity and polarity of three novel and red-emitting coumarin-rhodamine hybrid derivatives with differences in the rigidity of their substituents is presented. This includes ethanol-polyethylene glycol, toluene-polyethylene glycol, and tolueneparaffin mixtures. Moreover, protonation-induced effects on the spectroscopic properties are studied. A viscosity-induced emission enhancement was observed for all coumarin-rhodamine hybrid derivatives. MCR2 bearing a julolidine donor showed the expected low sensitivity to viscosity whereas MCR3 with its freely rotatable diphenylamino Substituent revealed a particularly pronounced sensitivity to this parameter. Moreover, MCR2 shows an enhancement in Emission in the open, i.e., protonated form in conjunction with a largely Stokes shift fluorescence in the deep red spectral region. This enables the application of these dyes as viscosity sensors and as far red emitting pH-sensitive probes. KW - Fluorescence KW - Dye KW - Quantum yield KW - Viscosity KW - Polarity KW - Environment KW - Probe KW - Coumarin KW - Rhodamine KW - Synthesis PY - 2017 DO - https://doi.org/10.1007/s10895-017-2165-4 SN - 1573-4994 SN - 1053-0509 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. VL - 27 IS - 6 SP - 1949 EP - 1956 PB - CrossMark AN - OPUS4-42584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Evaluation of particle sizing techniques for implementation of the EC Definition of a nanomaterial N2 - Many techniques are available for measuring particle size distribution. For ideal materials (spherical particles, well dispersed) it is possible to evaluate the Performance of these methods. The performance of the analytical instrumentation for the purpose of classifying materials according to EC Definition is unknown. In this work the performance of commercially available particle sizing techniques on representative NanoDefine set of real-world testing materials (RTM) and quality control materials (QCM) for the implementation of the Definition is evaluated. T2 - Final NanoDefine Outreach Event Classification of nanomaterials according to the EU definition CY - Brüssel, Belgium DA - 19.09.2017 KW - Nanomaterial classification KW - Particle sizing techniques KW - Nanoparticles KW - EC definition of a nanomaterial PY - 2017 UR - http://www.nanodefine.eu/index.php/nanodefine-meetings/125-final-outreach-event-2017 AN - OPUS4-42507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Electrospray as a sample preparation tool for electron microscopy: Toward quantitative evaluation of nanoparticles N2 - Electrospray ionization constitutes a promising deposition technique for high-resolution imaging. Particle distribution on TEM grids takes place homogeneously and no losses occur. Suspension must be appropriate (stabilizer may induce artefacts). ESI parameters need to be optimized for each material. T2 - Final NanoDefine Outreach Event: Classification of nanomaterials according to the EU definition CY - Brüssel, Belgium DA - 19.09.2017 KW - Electrospray deposition KW - Electron microscopy KW - Nanoparticles PY - 2017 UR - http://www.nanodefine.eu/index.php/nanodefine-meetings/125-final-outreach-event-2017 AN - OPUS4-42508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Volume specific surface area (VSSA) by BET: concept and demonstration on industrial materials N2 - Volume specific surface area (VSSA) as measured by BET constituites a simple and reliable solution to (most) powders. Porous, coated, polydisperse/multimodal materials are to be treated with care, i.e. doubled by analysis with electron microscopy or more advanced BET analysis (e.g. t-plot)for each material in part. T2 - Final NanoDefine Outreach Event: Classification of nanomaterials according to the EU definition CY - Brüssel, Belgium DA - 19.09.2017 KW - VSSA KW - BET KW - Nanoparticles KW - Powder KW - Nanomaterial classfication PY - 2017 UR - http://www.nanodefine.eu/index.php/nanodefine-meetings/125-final-outreach-event-2017 AN - OPUS4-42509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Boehm, Rainer T1 - Cone type Phased Array Design for High Speed Hollow Axle Inspection N2 - To increase inspection speed and inspection reliability the use of phased array system is a superior solution. Especially for shaft inspection phased array setups are commonly used. For hollow axle inspection typically a number conventional probes rotating through the axles drilling are applied, without demounting the axes and without dismantling the wheels and the brake discs. A new approach using a cone type array operated in immersion technique will allows to increase inspection speed and reduce the mechanical effort of the inspection system by rotating the sound field for the circumferential scan electronically. Only a linear movement of the probe is necessary to move the phased array cone forward and backwards inside the drilling. By applying additional focal laws the beam can be inclined exactly and be focused in the plane vertical to the specimen axis to concentrate the sound in the zones close to the external surface of the railway axle. The cone type phased array probe has been optimized to detect transversal flaws in and close to the outer surface of the hollow axle, whose surface lies in the radial-radial plane. The prototype probe system and its performance will be presented. T2 - ESIS TC24 Workshop: Integrity of Railway Structures CY - Wittenberge, Germany DA - 25.09.2017 KW - Hollow Axle Inspection KW - Ultrasound KW - UT KW - Phased Array KW - Cone Type Array PY - 2017 AN - OPUS4-42523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moufid, M. T1 - An electronic nose for the detection and discrimination of environmental pollutant gases in the aglomeration of the city of meknes N2 - The ambient air quality around residential areas is influenced by industrial objects, including industrial sewage, livestock farming and landfill sites. These sites are generating malodours or toxic gases involving degradation of ambient air quality, which may constitute a risk in human health if maximum emission limits are exceeded. Therefore, appropriate tools allowing detection of harmful or bad odorous, subsequently contributing to a reduction of odour nuisance are greatly needed. The aim of this study was to demonstrate the capability of an electronic nose E-nose to discriminate various gas samples collected from six different sites from the agglomeration of Meknès city corresponding to municipal landfill, in the city at 2 km of landfill, industrial estate wastewater, traffic road, and sheep breeding. The investigations were carried out with an E-nose system based on an array of six-commercial MQ sensors. Further, a pattern recognition technique known as Principal Component Analysis (PCA), Linear Discriminent Analysis (LDA), and Support Vector Machines (SVMs) was implemented to study the discrimination capability of the sensor array. PCA results demonstrate excellent discriminating ability of the dataset with a score of 99.47 %. Additionally, another measurement database containing 12 air atmospheric samples was projected on the previously built PCA model to check the stability of the E-nose. The LDA was applied to the same dataset and showed a good discrimination between the ambient air samples of the six sites. Furthermore, SVMs technique was also used to build a classifier and reached a score of 100 % success rate in the recognition of the analysed samples. The obtained results of six areas demonstrate the increasing interests and the applicability of E-noses for ambient air quality classification of six areas caused by emitted decomposed organic matters. T2 - Eighth International Workshop on Biosensors for Food Safety and Environmental Monitoring CY - Rabat, Morocco DA - 12.10.2017 KW - Pattern recognition methods KW - Electronic nose KW - Gas sensor KW - Malodour detection KW - Environmental analysis PY - 2017 AN - OPUS4-42525 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haferkamp, Sebastian A1 - Fischer, Franziska A1 - Kraus, Werner A1 - Emmerling, Franziska T1 - Mechanochemical Knoevenagel condensation investigated in situ N2 - The mechanochemical Knoevenagel condensation of malononitrile with p-nitrobenzaldehyde was studied in situ using a tandem approach. X-ray diffraction and Raman spectroscopy were combined to yield time-resolved information on the milling process. Under solvent-free conditions, the reaction leads to a quantitative conversion to p-nitrobenzylidenemalononitrile within 50 minutes. The in situ data indicate that the process is fast and proceeds under a direct conversion. After stopping the milling process, the reaction continues until complete conversion. The continuous and the stopped milling process both result in crystalline products suitable for single crystal X-ray diffraction. KW - Mechanochemistry KW - Ball milling KW - C–C coupling KW - In situ KW - Knoevenagel condensation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-425388 DO - https://doi.org/10.3762/bjoc.13.197 VL - 13 SP - 2010 EP - 2014 PB - Beilstein-Institut AN - OPUS4-42538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thünemann, Andreas T1 - SAXS for the determination of the size distribution of nanoparticles: Application in catalysis N2 - The open source software packages SASfit1 and McSAS2 are widely used to determine the size distribution of nanoparticles. SASfit is based on classical curve fitting. The type of size distribution needs to be provided as constraint for analysis. Very often the lognormal size distribution is useful as shown for the characterization of single- and multimodal magnetic iron oxide particles. The use of SASfit is part of efforts to standardize analyzing methods for magnetic nanoparticles within the EU project NanoMag (www.nanomag-project.eu). In contrast to SASfit, it is not necessary to provide the type of size distribution when using the program McSAS. Both programs provide tools that allow the user to estimate uncertainties of the derived size distributions. Such is helpful in the development of nanoscale reference materials for environmental, health and safety measurements. As an example, a detailed study on using SAXS in the characterization of ultra-small-silver nanoparticles is presented. These particles are useful in the catalytic reduction of 4-nitrophenol and display an adjustable activity (see Figure). Figure. Core-shell silver nanoparticles catalyze the reduction of 4-nitrophenol and display an increasing catalytic activity when stabilized with different ligands in the line bovine serum albumin (BSA), glutathione (GSH) and polyacrylic acid (PAA).5 T2 - International SAXS Symposium CY - Graz, Austria DA - 26.09.2017 KW - SAXS KW - Small-angle X-ray scattering KW - Silver nanoparticles PY - 2017 AN - OPUS4-42251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Gebhard, R. T1 - Synchrotron radiation–induced X-ray fluorescence (SRXRF) analyses of the Bernstorf Gold N2 - The gold finds from Bernstorf, in the Freising district of Bavaria, were discovered in 1998, in the area of a Bronze Age settlement. First analyses with X-ray fluorescence (XRF) revealed gold of an unusually high purity grade, which was explained by the use of cementation techniques. A newer analysis with laser ablation inductively coupled plasma mass spectrometry (LA–ICP–MS) indicated an even higher purity. The analytical results were the starting point of an ongoing discussion. In this study, we re-analysed 11 gold samples with Synchrotron radiation–induced X-ray fluorescence at the BAMline at BESSY. In a thorough analysis, different excitation and detection conditions were applied to confirm or disprove the previous results. It was shown that the purity of the gold from the specimen is higher than 99.9%. The main impurities are silver in a range between 20 and 200 μg/g and copper between 1 and 10 μg/g. The results are in very good agreement with the LA–ICP–MS measurements and provide basic information for discussions about provenance, processing techniques or considerations of authenticity. KW - Gold KW - Synchrotron KW - XRF KW - BESSY KW - Archeometry PY - 2017 DO - https://doi.org/10.1111/arcm.12294 SN - 0003-813X SN - 1475-4754 VL - 59 IS - 5 SP - 891 EP - 899 PB - Wiley AN - OPUS4-42540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Usmani, Shirin M. T1 - Wood protection with MgF2 and CaF2 nanoparticles N2 - Sol-gel synthesis was used to prepare nanoparticles of MgF2 and CaF2. These nanoparticles were tested for their application in wood protection. In comparison to control samples, wood specimens treated with MgF2 and CaF2 showed lower mass loss under exposure to termites and fungi. Samples treated with MgF2 performed better at protecting wood from cellulose degradation when exposed to termites. Conversely, in the presence of fungi, mass loss in treated samples was similar irrespective of the chemical composition (MgF2 and CaF2) of the treatment. A possible explanation for this difference in results between termites and fungi could be their different mechanism of cellulose hydrolysis. Thus, future wood preservatives would need to be customized according to their specific application. T2 - 19th International Sol-Gel Conference CY - Liege, Belgium DA - 03.09.2017 KW - Nanoparticles KW - Wood protection KW - Fungi KW - Termites PY - 2017 AN - OPUS4-42541 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hertwig, Andreas A1 - Hinrichs, K. A1 - Beck, Uwe A1 - Esser, N. T1 - Editorial to the proceedings of the 7th conference on spectroscopic N2 - The 7th International Conference on Spectroscopic Ellipsometry (ICSE-7) was held in Berlin in June 2016, jointly organised by ICSE and BAM. The publication of the proceedings special issue in Applied Surface Science follows this event. In the special issue, about 100 articles on current topics of optics and surface science related to ellipsometry, polarimetry, and similar techniques are presented, underpinning the high significance of these techniques for many fields of materials science. T2 - 7th International Conference on Spectroscopic Ellipsometry, ICSE-7 CY - Berlin, Germany DA - 06.06.2016 KW - Spectroscopic ellipsomety PY - 2017 DO - https://doi.org/10.1016/j.apsusc.2017.04.081 SN - 0169-4332 VL - 2017 IS - 421 SP - 269 EP - 270 PB - Elsevier B.V. AN - OPUS4-42554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Léonard, Fabien A1 - Stein, J. A1 - Soutis, C. A1 - Withers, P. J. T1 - The quantification of impact damage distribution in composite laminates by analysis of X-ray computed tomograms N2 - One of the great strengths of X-ray computed tomography over conventional inspection methods (ultrasound, thermography, radiography) is that it can image damage in 3D. However for curved ordeformed composite panels it can be difficult to automatically ascribe the damage to specific plies or inter-ply interfaces. An X-ray computed tomography (CT) data processing methodology is developed to extract the through-thickness distribution of damage in curved or deformed composite panels. The method is applied to [(0°/90°)2]s carbon fibre reinforced polymer (CFRP) panels subjected low velocity impact damage (5 J up to 20 J) providing 3D ply-by-ply damage visualisation and analysis. Our distance transform approach allows slices to be taken that approximately follow the composite curvature allowing the impact damage to be separated, visualised and quantified in 3D on a ply-by-ply basis. In this way the interply delaminations have been mapped, showing characteristic peanut shaped delaminations with the major axis oriented with the fibres in the ply below the interface. This registry to the profile of the panel constitutes a significant improvement in our ability to characterise impact damage in composite laminates and extract relevant measurements from X-ray CT datasets. KW - Delamination KW - Impact behaviour KW - Non-destructive testing KW - X-ray computed tomography KW - Distance transform PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0266353817307157?via%3Dihub DO - https://doi.org/10.1016/j.compscitech.2017.08.034 SN - 0266-3538 SN - 1879-1050 VL - 152 SP - 139 EP - 148 PB - Elsevier Ltd. AN - OPUS4-42556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosu, Dana-Maria A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Kraehnert, R. A1 - Hertwig, Andreas ED - Hertwig, Andreas ED - Hinrichs, K. ED - Beck, Uwe ED - Esser, N. T1 - Ellipsometric porosimetry on pore-controlled TiO2 layers N2 - The practical performance of surface coatings in applications like catalysis, water splitting or batteries depends critically on the coating materials’ porosity. Determining the porosity in a fast and nondestructive way is still an unsolved problem for industrial thin-films technology. As a contribution to calibrated, non-destructive, optical layer characterisation, we present a multi-method comparison study on porous TiO2 films deposited by sol-gel synthesis on Si wafers. The ellipsometric data were collected on a range of samples with different TiO2 layer thickness and different porosity values. These samples were produced by templated sol-gel synthesis resulting in layers with a well-defined pore size and pore density. The ellipsometry measurement data were analysed by means of a Bruggeman effective medium approximation (BEMA), with the aim to determine the mixture ratio of void and matrix material by a multi-sample analysis strategy. This analysis yielded porosities and layer thicknesses for all samples as well as the dielectric function for the matrix material. Following the idea of multi-method techniques in metrology, the data was referenced to imaging by electron microscopy (SEM) and to a new EPMA (electron probe microanalysis) porosity approach for thin film analysis. This work might lead to a better metrological understanding of optical porosimetry and also to better-qualified characterisation methods for nano-porous layer systems. 1. IntroductionPorous materials, especially porous thin films play an importantrole in chemical and physical technology in every case where thecontact area between two media has to be maximised. From cataly-sis to photochemistry and photovoltaics, the applications of porouslayer materials are diverse and numerous [1–6].The accurate and non-destructive characterisation of porousfilms for layered systems poses a challenge. This applies especiallyfor the key parameter of porous films, their porosity, i.e. the mix-ing ratio between the Matrix of the film (host material) and thepore volume which is empty or filled with a fluid medium (inclu-sions). This parameter influences most of the physical and chemicalproperties of a porous thin film and is therefore essential for theunderstanding as well as the optimisation of this class of materials. T2 - International Conference on Spectroscopic Ellipsometry (ICSE-7) CY - Berlin, Germany DA - 06.06.2016 KW - Spectroscopic ellipsometry KW - Porous materials KW - Porosimetry KW - Multi-sample analysis KW - Thin film metrology PY - 2017 DO - https://doi.org/10.1016/j.apsusc.2016.11.055 SN - 0169-4332 SN - 1873-5584 VL - 421 IS - Part B SP - 487 EP - 493 PB - Elsevier B.V. AN - OPUS4-42517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - Airborne laser spark ionization N2 - A novel ionization scheme for ambient mass spectrometry is presented and discussed. Desorption and ionization are achieved by a quasi-continuous laser induced plasma (LIP) ignited in front of the atmospheric pressure interface of a time-of-flight mass spectrometer. This setup comprises the advantages of i) an ambient probe, ii) electro neutrality, iii) low power consumption, iv) a sufficient duty cycle, v) a ubiquitous plasma medium (air) and vi) high sensitivity caused by the high electron number densities. The plasma properties and operating conditions are investigated to understand the processes that lead to the formation of molecular ions. Comprehensive studies include optical emission spectroscopy, shadowgraphic shockwave visualization and time-of-flight mass spectrometry investigations. The observed MS signal (including reagent-ion signal, as well as analyte spectra) closely resembles the ionization behavior of other electrically-driven plasma-based ionization sources, such as DBD, LTP or DART. Conversely that means that although LIPs are commonly known to have temperatures way above 10.000 K and thus efficiently atomize and ionize molecules, MS spectra were obtained that showed the formation of intact molecular ions. For an insight into the LIP properties the optical emission of the LIP is examined and exhibits a pronounced degree of dissociation into atomic and ionic species, which reflects the higher temperature and electron density inside a LIP. Accordingly, rather elemental (ICP-type) than molecular spectra should be expected. However due to the absence of such ions, we conclude that the analyte does not enter the hot center of the plasma itself. Moreover, the initial, highly-excited plasma species react cascade-like to lower energetic species via reactive collision with the surrounding atmosphere, which can then subsequently ionize molecules of interest. The concept potentially involves charge transfer, proton transfer, electron impact and photoionization. These assumptions are confirmed via the shadowgraphs of the expanding shockwave around the LIP. An effective spatial separation between the two regions is maintained by concentrically expanding pressure waves resulting in a strongly unidirectional diffusion. Additionally, the strictly outbound matter transport suggests a rarefaction inside the plasma region for each plasma event. T2 - SCIX 2017 CY - Reno, Nevada, USA DA - 08.10.2017 KW - Ambient ionization KW - Mass spectrometry KW - Laser KW - Plasma PY - 2017 UR - https://www.scixconference.org/program/final-program?symposium=17ACS01&p=8810/#session AN - OPUS4-42609 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - Airborne laser spark ionization N2 - A novel ionization scheme for ambient mass spectrometry is presented and discussed. Desorption and ionization are achieved by a quasi-continuous laser induced plasma (LIP) ignited in front of the atmospheric pressure interface of a time-of-flight mass spectrometer. This setup comprises the advantages of i) an ambient probe, ii) electro neutrality, iii) low power consumption, iv) a sufficient duty cycle, v) a ubiquitous plasma medium (air) and vi) high sensitivity caused by the high electron number densities. The plasma properties and operating conditions are investigated to understand the processes that lead to the formation of molecular ions. Comprehensive studies include optical emission spectroscopy, shadowgraphic shockwave visualization and time-of-flight mass spectrometry investigations. The observed MS signal (including reagent-ion signal, as well as analyte spectra) closely resembles the ionization behavior of other electrically-driven plasma-based ionization sources, such as DBD, LTP or DART. Conversely that means that although LIPs are commonly known to have temperatures way above 10.000 K and thus efficiently atomize and ionize molecules, MS spectra were obtained that showed the formation of intact molecular ions. For an insight into the LIP properties the optical emission of the LIP is examined and exhibits a pronounced degree of dissociation into atomic and ionic species, which reflects the higher temperature and electron density inside a LIP. Accordingly, rather elemental (ICP-type) than molecular spectra should be expected. However due to the absence of such ions, we conclude that the analyte does not enter the hot center of the plasma itself. Moreover, the initial, highlyexcited plasma species react cascade-like to lower energetic species via reactive collision with the surrounding atmosphere, which can then subsequently ionize molecules of interest. The concept potentially involves charge transfer, proton transfer, electron impact and photoionization. These assumptions are confirmed via the shadowgraphs of the expanding shockwave around the LIP. An effective spatial separation between the two regions is maintained by concentrically expanding pressure waves resulting in a strongly unidirectional diffusion. Additionally, the strictly outbound matter transport suggests a rarefaction inside the plasma region for each plasma event. T2 - IPOIMS CY - Menorca, Spain DA - 16.10.2017 KW - Laser KW - Ambient ionization KW - Plasma KW - Mass spectrometry PY - 2017 UR - http://ipoims.com/downloads/Abstracts_IPOIMS_10102017.pdf AN - OPUS4-42610 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Myrach, Philipp T1 - Laser Thermography – Evolution from a highly specialized into a versatile tool for NDE N2 - Laser thermography has its roots in the late-1960s when Kubiak first used a focused light source to raster-scan a specimen containing surface breaking cracks and employed an infrared detector to monitor the blocking effect of the cracks on the heat flow. Nowadays, this technique has evolved into the flying-spot laser thermography. In the mid-1970s, when Rosencwaig and Gersho worked out the theory for the photoacoustic effect, they laid the foundation for the development of the photothermal testing methodology. The decisive difference to the flying-spot technique is that in the photothermal methodology, a high-frequency modulated laser beam is used, which explicitly uses the concept of the thermal wave. Starting in the 1980s, infrared cameras came into play and enabled full-field thermal imaging, but this time, slow thermal light sources were used. Today, flash lamps (pulsed planar heating) and halogen lamps (modulated planar heating) have been established as the standard light sources for the specific regimes of pulsed and lock-in thermography. Only recently, the availability of novel technologies – fast and high-resolution infrared cameras, innovative brilliant laser sources and high-performance data acquisition and processing technology – has enabled a paradigm shift from the separated photothermal and thermographic methodologies to a versatile tool for NDE that combines both approaches. In addition, the heating can also be spatially structured using laser arrays. This new degree of freedom allows the development of completely new thermography NDE methods. In the talk, we present current activities with kilowatt-class high-power laser sources for advanced flying-spot, pulsed, lock-in and laser-projected thermography. T2 - NDE 2017 CY - Chennai, India DA - 14.12.2017 KW - Thermografie KW - Laser KW - Zerstörungsfreie Prüfung KW - Lock-in KW - VCSEL KW - photothermisch PY - 2017 AN - OPUS4-43425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Already Producing or Still Calibrating? – Online NMR Spectroscopy as Smart Field Device. N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example, which was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. T2 - Tackling the Future of Plant Operation - Jointly towards a Digital Process Industry CY - Barcelona, Spain DA - 13.12.2017 KW - Process Monitoring KW - Smart Sensors KW - Online NMR Spectroscopy KW - Indirect Hard Modeling KW - Process Analytical Technology KW - CONSENS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-434330 AN - OPUS4-43433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas T1 - Standardised and referenced surface analysis with ellipsometry - Is ellipsometry a metrological tool? N2 - Ellipsometry is a valuable surface analysis tool with an unmatched sensitivity towards surface layer properties. In this presentation, an initiative is discussed to make ellipsometry also a metrological tool. This is usually seen as very difficult due to the model-based nature of the analysis process. By establishing standardisation and reference materials, ellipsometry can be made traceable and can also become a valuable part of the traceable thin film metrology landscape. This is important because this technique has much potential to determine complex material parameters much needed in the production of high-tech products. T2 - University (UNL), Engineering Department CY - Lincoln, Nebraska, USA DA - 06.11.2017 KW - Metrology KW - Spectroscopic Ellipsometry KW - Reference Materials KW - Traceability KW - Measurement Uncertainty PY - 2017 AN - OPUS4-43412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rietz, U. A1 - Lerche, D. A1 - Hielscher, Stefan A1 - Grunwald, Daniel A1 - Beck, Uwe ED - Frenz, H. ED - Langer, J. B. T1 - CAT-Technologie als neues Multiprobenverfahren N2 - Das Fügeverfahren Kleben bietet viele Vorteile, wie das Verbinden verschiedener Materialklassen und eine Lastverteilung über den gesamten Fügebereich, und erfordert schnelle Prüfverfahren zur Ermittlung von Verbundeigenschaften. Das Messprinzip CAT-Technologie® (Centrifugal Adhesion Testing) verwendet die radial gerichtete Zentrifugalkraft als Belastungsgröße, die durch programmierbare Variation der Drehzahl statisch oder dynamisch vorgegeben wird. Bei Erreichen der kritischen Beanspruchung trennt sich der Prüfstempel vom Substrat, zeitgleich wird ein positionsbezogenes Signal aus dem drehenden Rotor gesendet und zusammen mit der Drehzahl an die PC-Software übertragen. Für jede Probe wird die Bruchkraft berechnet und in Echtzeit angezeigt. Der Adhesion Analyser LUMiFrac® untersucht simultan bis zu acht Prüfkörper unter identischen Bedingungen. Das neue Messprinzip erfüllt die Anforderungen von DIN EN 15870, DIN EN 14869-2 und ISO 4624. Neben der Festigkeitsbestimmung von Klebverbindungen ist die Haftung von Schichtsystemen ein weiterer wichtiger Anwendungsbereich. Ergebnisse für Zug- und Scherbeanspruchung, realisiert mit unterschiedlichen Prüfkörper-Layouts, werden vorgestellt und Festigkeit beeinflussende Faktoren, wie Prüfgeschwindigkeit oder Substratverformung bei Beanspruchung, werden aufgezeigt. Die Charakterisierung von Klebebandeigenschaften über die Möglichkeiten der Schälprüfung hinaus wird gezeigt. Des Weiteren werden experimentelle Ergebnisse durch zyklische Belastung (Ermüdung) im Vergleich zu Stan-dard-Tests diskutiert. T2 - Tagung „Werkstoffprüfung" 2017 CY - Berlin, Germany DA - 30.11.2017 KW - Adhäsion KW - Festigkeit KW - Scherbelastung KW - Zugbelastung KW - analytische Zentrifuge PY - 2017 SN - 978-3-9814516-7-2 SN - 1861-8154 SP - 277 EP - 282 PB - DVM Deutscher Verband für Materialforschung und -prüfung CY - Berlin AN - OPUS4-43414 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krome, Fabian A1 - Gravenkamp, H. A1 - Birk, C. T1 - Prismatic semi-analytical elements for the simulation of linear elastic N2 - This work addresses the computation of stiffness matrices for general prismatic structures with an arbitrary cross section. The presented approach is based on the scaled boundary finite element method (SBFEM), a semi-analytical method, which can be used to model structures by only discretizing the boundary of a domain. For prismatic structures, the process is further simplified, as only the cross section of the structure has to be discretized. Thus, a particular semi-analytical finite element is constructed for bounded and unbounded domains. The proposed approach leads to a frequency-dependent stiffness matrix. This stiffness matrix can easily be coupled to other prismatic SBFEM domains or general SBFEM domains. Necessary modifications to include forces along the scaling direction, such as body loads, are addressed. The results of the proposed approach are compared to those of traditional FEM models obtained using commercially available software. KW - Scaled boundary finite element method KW - Elasticity KW - Prismatic structures KW - Body-loads PY - 2017 DO - https://doi.org/10.1016/j.compstruc.2017.06.015 VL - 192 SP - 83 EP - 95 PB - Elsevier Ltd. AN - OPUS4-43415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krome, Fabian A1 - Gravenkamp, Hauke T1 - 3-D Waveguide modeling and simulation using SBFEM N2 - The modeling of waveguides by means of the Scaled Boundary Finite Element Method (SBFEM) has recently been addressed and is considered an effective procedure for the simulation of ultrasonic guided waves in plates and uniform structures, as well as their interaction with defects. This work presents the extension of the known applications like uniform concrete foundation cylinders to structures with more complex shapes and defects. The main focus is the required modeling of 3-D structures in SBFEM to solve these efficiently. Furthermore the coupling of different models is discussed. This involves models like a mainly uniform foundation cylinder with varying material behavior or geometry in certain areas which has to be modeled in 3-D SBFEM. With the presentation of numerical examples the accuracy and performance of the modeling is discussed and the advantages in improving numerical stability are shown. T2 - ICSV22 CY - Florence, Italy DA - 12.07.2015 KW - Scaled boundary finite element method PY - 2015 SP - 2805 EP - 2810 AN - OPUS4-43416 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Daum, Werner T1 - VDI/VDE Standardization Activities of DIC Measurement Techniques N2 - With more than 180.000 engineers and scientists VDI Association of German Engineers and VDE Association for Electrical, Electronic & Information Technologies are belonging to the major technical and scientific associations in Europe. Both organizations promote the advancement of technology and among other things by developing recognized technical regulations as national and international standards. Since 2011 Technical Committee 2.15 Optical Measuring Methods for Structure Analysis and Monitoring as a common committee of both organizations is working among other things on the development of standards for optical measuring and testing methods. The committee consists of 27 members representing industrial users, system manufacturers, research institutes and universities. Currently the committee is drafting the new standard VDI/VDE 2626 Part 1 - Optical measuring procedures – Image correlation methods – Basics and equipment, which will be introduced in this presentation. Draft VDI/VDE 2626 Part 1 describes practical acceptance and reverification procedures for the evaluation of the accuracy of optical measuring systems based on digital image correlation (DIC) methods. The document applies to DIC measurement systems used a) for full-field determination of two- or three-dimensional displacement of surfaces, and b) for full-field determination of the elongation or strain of surfaces. The standard describes quality parameters as well as methods and reference objects for their determination. The quality parameters serve to specify DIC systems, and to compare different systems. They are equally suitable a) for acceptance tests as well as b) for reverification of DIC systems within the framework of a quality management system. The acceptance test is used to determine whether the DIC system complies with the quality parameter limits specified by the manufacturer, or with contractually agreed limits by the manufacturer and user, respectively. For this test the quality parameters zero-displacement error, zero-strain error, and displacement error are defined and used. Zero-displacement error and zero-strain error describe minimum measurement uncertainties of the DIC system a user has to reckon with. They are influenced by different uncertainty contributions. The quality parameter displacement error is used to check the ability of the DIC system to determine absolute displacements within the measurement volume and to confirm the traceability of this measurement to the SI system. Reverification of DIC systems serves to ensure long-term compliance with specified limits for the quality parameters. By comparing the results of successive reverification measurements of the quality parameters used for the acceptance test, it is possible to analyze trends with respect to changes in DIC system characteristics. T2 - Annual International DIC Society Conference 2017 CY - Barcelona, Spain DA - 06.11.2017 KW - Digital image correlation KW - Standardization PY - 2017 AN - OPUS4-43373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Streeck, C. T1 - Quantitative XRF analysis of industrial thin film samples by calibration using thin film RMs N2 - X-ray fluorescence (XRF) analysis is a well suited methodology for thin film analysis. With XRF the mass deposition of elements can be non-destructively determined. By knowledge of the density of the thin film as well the thickness can be given. In the field of industrial thin film manufacturing various material systems and layer structures are used. the analysis relies on well-known calibration samples or even reference materials to determine absolute analytical results from the measurement values recorded. Within this concept of chemical traceability the calibration sample has to be as similar as possible to the industrial thin film sample with respect to the spatial distribution of elemental composition in order to minimize matrix effects or analysis related uncertainties. The procurement of such certified similar calibration samples or reference materials including their required traceability is a challenge due to limited number of available calibration samples or reference materials, in particular at the nanoscale. There are only few providers of calibration standards for layer or coating thicknesses which are suitable for XRF analysis. The limited number of available certified reference materials (CRMs) for XRF thin film analysis and in parallel the growing market of novel thin film materials induces a growing gap of required calibration samples for XRF analysis. The exploitation of process-near samples benefits from a leverage effect: on one hand reference materials are needed for calibration and alignment procedures for X-ray fluorescence devices. They are customized for the special need of the end-user, e.g. a company producing thin film solar cells. On the other hand the market for EDXRF devices develops positively by providing novel thin film calibration samples for industry and end user-related production processes or application. Two aspects are hereby being addressed; the improvement of product quality which in certain sectors like aerospace and automotive industry directly translates to product safety as well as the expansion of the sales potential of EDXRF measuring devices. T2 - Annual Meeting ISO TC 201 SC10 CY - Brescia, Italy DA - 17.09.2017 KW - XRF KW - Calibration KW - Traceability PY - 2017 AN - OPUS4-43375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Byambadulam, E. T1 - Certified reference material for determination of total cyanide in soil N2 - Due to their toxicity and widespread application for mining and industrial purposes, cyanides are ranking among the most important inorganic pollutants which should be tested and monitored not only in the aquatic environment, but also in soils and soil-like materials. Reference materials of soils with relevant contents of cyanide to ensure reliable test results of laboratories are rare today. New certified reference material (CRM) BAM-U116/CGL306 “Cyanide in soil” was produced within a framework of cooperation between Central Geological Laboratory (CGL) of Mongolia and Federal Institute for Materials Research and Testing (BAM) of Germany in 2013-2017. The CRM BAM-U116/CGL306 represents a mixture of a sandy soil collected from a contaminated former gasworks area in the Berlin region (Germany) and an unpolluted sandy soil from Nalaikh region (Mongolia). The bulk candidate material for this reference material was prepared at CGL CRM Laboratory exclusively destined to the preparation of reference materials and equipped with modern technical equipment. Homogeneity, stability and shelf life were studied in full compliance with ISO Guide 35. The CRM was evaluated as sufficiently homogeneous. Stability study proved that the quality of the material can be ensured for at least two years upon receipt when stored at a temperature below 25 °C in its original tightly closed bottle. Statistical evaluation of certification analysis was performed using software packages SoftCRM and ProLab Plus. Certified value of total cyanide of the CRM is 12.0 mg/kg and expanded uncertainty was assigned as 0.8 mg/kg. The intended purpose of this material is the verification of analytical results obtained for the mass fraction of total cyanide in soils and soil-like materials applying the standardized procedure ISO 11262:2011. As any reference material, it can also be used for routine performance checks (quality control charts) or validation studies. T2 - Conference on Mineral Resources and Analytical Techniquesconference on Mineral Resources and Analytical Techniques CY - Ulaanbaatar, Mongolia DA - 23.11.2017 KW - Certified reference material KW - Cyanide in soil KW - Total cyanide PY - 2017 AN - OPUS4-43382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hönig, Gerald A1 - Schlichting, S. T1 - QCSE tuning in polar GaN/AlN heterostructures N2 - We show both theoretically and experimentally how the encapsulation of the active region by additional guard layers can be used to achieve a significant reduction of the built-in electric fields in polar nitride heterostructures. This reduction of the QCSE results in a strongly enhanced emission intensity and faster recombination dynamics in the active region. In particular we are able to shift the emission energy of 4-nm-thick GaN nano-discs up to 3.32 eV, which is just 150 meV below the bulk GaN bandgap as compared to a red-shift of about 1 eV in a conventional heterostructure with the same thickness. T2 - SPIE. PHOTONICS WEST OPTO CY - San Francisco, CA, USA DA - 29.01.2018 KW - QCSE KW - Piezopolarization KW - Spontaneous Polarization KW - IFGARD KW - Nanoheterostructures KW - Nonpolar PY - 2018 AN - OPUS4-43383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Jonietz, Florian T1 - 3D-Scannen mit integrierter thermografischer Qualitätsprüfung N2 - Sowohl die 3D-Formbestimmung als auch die Thermografie sind Verfahren der Qualitätssicherung. Im vorgestellten Projekt wird versucht, die beiden Methoden zusammenzuführen. Das Prinzip des für die Formbestimmung verwendeten 3D-Scanners beruht auf dem bereits bekannten Verfahren der Streifenlichtprojektion. Die Neuartigkeit des hier verwendeten 3D-Scanners besteht darin, dass nicht im sichtbaren, sondern im infraroten Spektralbereich gearbeitet wird. Dadurch wird es möglich, nicht die Reflexion, sondern die Wärmestrahlung des Prüfobjektes nach Absorption der eingebrachten Strahlung auszuwerten. Dies ermöglicht erstmals, transparente und stark absorbierende Oberflächen zu erfassen. Die Anregung mit Wärmestrahlung stellt das Bindeglied zum Verfahren der aktiven Thermografie für die Detektion verdeckter Schäden dar. Bei letzterem Verfahren wird der Wärmestau über Defekten beim Eindringen der Wärme in die Tiefe des Materials gemessen. Dabei stellen Defekte eine Störung des 3D-Scan-Verfahrens dar, während umgekehrt unregelmäßig geformte Oberflächen das thermografische Verfahren erschweren, d.h. der Messeffekt eines der Verfahren ist ein Störeffekt für das jeweils andere Verfahren. Es wird zum einen der Frage nachgegangen, inwieweit das 3D-Scan-Verfahren durch verdeckte Defekte beeinträchtigt wird, und zum anderen die Möglichkeit untersucht, den vorhandenen 3D-Scanner auch für die aktive Thermografie einzusetzen. Vor allem wurden CFK-Proben mit künstlich eingebrachten Defekten untersucht. Es werden die Möglichkeiten und Grenzen der vorhandenen Messapparatur für die Defekterkennung aufgezeigt. T2 - 3D-NordOst 2017 CY - Berlin, Germany DA - 7.12.2017 KW - Streifenprojektion KW - Zerstörungsrfreie Prüfung KW - Thermographic testing KW - 3D-Scanner PY - 2017 AN - OPUS4-43358 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Antibodies on Beads - Nanokonjugate für die Analytik N2 - The presentation deals with the progess, the use of beads brings with it when developing and using immunoanalytical methods. While with conventional assays (e.g. ELISA) fill/empty/wash steps have to be performed within the same microplate well, antibodies on beads bring the possibility of incubating the sample with the capture antibodies in one compartment and then transport it, e.g. in microfluidic channels, to the site of detection. Especially magnetic nanoparticles, that can be captured and released easily, have a wide field of application. T2 - Wissenschaft trifft Wirtschaft - Analytik im Nanobereich CY - Berlin, Germany DA - 07.12.2017 KW - Nanoteilchen KW - Nanogold KW - Sensor KW - Mikrofluidik PY - 2017 AN - OPUS4-43359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Copolymer structure elucidation by multidimensional techniques with focus on UPLC x ESI-TOF-MS N2 - Structure elucidation of complex synthetic copolymers still represents a challenge. An one-dimensional separation technique cannot give the answer to the question: What are the molar mass distribution (MMD), the functionality distribution (FTD), the chemical composition distribution (CCD), the monomer sequence distribution (MSD), the topology differences within a single broad distributed polymer sample? Since the first LC/ ESI-MS experiment of the Nobel prize winner John B. Fenn in 1984, the coupling of liquid chromatographic to mass spectrometric techniques gained a continuous rapid development. Often the deficiencies of stand-alone methods can be bridged. LC, blind to structural information needs mass spectrometry as one of the most powerful detectors able to give detailed information on e.g. the repeat units, functionalization or copolymer composition of the chromatographic separated constituents. A separation prior to MS reduces radical the dispersity which is one of the reasons for failing of MS. Also problems with different ionization probabilities in complex mixtures can partly be overcame. Different LC separation techniques as size exclusion chromatography (SEC), liquid adsorption chromatography (LAC), liquid chromatography at critical conditions (LCCC) and gradient elution liquid chromatography (GELC) combined with Matrix assisted Laser Desorption Ionization (MALDI) respectively Electrospray Ionization (ESI) Time of Flight (TOF) mass spectrometry are able to give information which otherwise are completely inaccessible. In some cases CID tandem mass spectrometry is applied. Fragmentation of suitable precursor ions resulted in typical fragment ion patterns. This technique enables an additional information on e.g. sequences, structural defects and topology of complex polymer mixtures. Herein a new approach is demonstrated to provide evidence of different functionalities and short block sequences in statistical EO-PO copolymers. Furthermore silsesquioxane mixtures and Polyglycerols are investigated concerning occurring topology effects. T2 - 253rd ACS National Meeting CY - San Francisco, CA, USA DA - 02.04.2017 KW - Copolymer KW - Microstructure KW - Liquid chromatography KW - Mass spectrometry PY - 2017 AN - OPUS4-43372 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Risinggård, H. K. A1 - Cooil, S. A1 - Mazzola, F. A1 - Hu, D. A1 - Kjaervik, Marit A1 - Østli, E. R. A1 - Patil, N. A1 - Preobrajenski, A. A1 - Ewans, A. D. A1 - Breiby, D. W. A1 - Trinh, T. T. A1 - Wells, J. W. T1 - Degradation of the chemotherapy drug 5-fluorouracil on medical-grade silver surfaces N2 - The degradation of the chemotherapy drug 5-fluorouracil by a non-pristine metal surfaces is studied.Using density functional theory, X-ray photoelectron spectroscopy and X-ray absorption spectroscopy we show that the drug is entirely degraded by medical-grade silver surfaces, already at body temperature,and that all of the fluorine has left the molecule, presumably as HF. Remarkably, this degradation is even more severe than that reported previously for 5-fluorouracil on a pristine monocrystalline silver surface(in which case 80% of the drug reacted at body temperature) [1]. We conclude that the observed reaction is due to a reaction pathway, driven by H to F attraction between molecules on the surface, which results in the direct formation of HF; a pathway which is favoured when competing pathways involving reactive Ag surface sites are made unavailable by environmental contamination. Our measurements indicate that realistically cleaned, non-pristine silver alloys, which are typically used in medical applications, can result in severe degradation of 5-fluorouracil, with the release of HF – a finding which may have important implications for the handling of chemotherapy drugs. KW - Surface science KW - Chemotherapy KW - DFT KW - Photoemission KW - Fluorouracil KW - Silver PY - 2018 DO - https://doi.org/10.1016/j.apsusc.2017.11.221 SN - 0169-4332 VL - 435 SP - 1213 EP - 1219 PB - Elsevier CY - Amsterdam, The Netherlands AN - OPUS4-43450 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René T1 - Identifizierung verschiedener Defekttypen in Ti-6Al-4V mittels Röntgen-Refraktion N2 - Das selektive Laserschmelzen (SLM) ist eine pulverbasierte, additive Fertigungsmethode, welche die Herstellung von komplex und individuell geformten Bauteilen ermöglicht. Im Laufe der vergangenen Jahre haben verschiedene Branchen, unter anderem die Luft- und Raumfahrt Industrie, begonnen diese Technologie intensiv zu erforschen. Insbesondere die Titanlegierung Ti-6Al-V4, welche aufgrund ihrer Kombination von mechanischen Eigenschaften, geringer Dichte und Korrosionsbeständigkeit häufig in der Luft- und Raumfahrt eingesetzt wird, eignet sich für die Herstellung mittels SLM. Allerdings können durch nicht optimal gewählte Prozessparameter, welche für gewöhnlich in einer Energiedichte zusammengefasst werden, Defekte in den Bauteilen entstehen. In dieser Studie wurde untersucht, in wie weit Röntgen-Refraktionsradiographie geeignet ist diese Defekte zu detektieren und zu charakterisieren. Bei der Röntgen- Refraktionsradiographie wird die Röntgenstrahlung, nachdem sie die Probe transmittiert hat, über einen Analysatorkristall gemäß der Bragg-Bedingung in den 2D-Detektor reflektiert und dabei nach ihrer Ausbreitungsrichtung gefiltert. Dadurch wird neben der Schwächung auch die Ablenkung der Röntgenstrahlung durch Refraktion im inneren der Probe zur Bildgebung ausgenutzt. Aus den aufgenommen Refraktionsradiogrammen kann der Refraktionswert berechnet werden. Dieser ist ein Maß für die Menge an inneren Oberflächen in der Probe. Zum einen konnte gezeigt werden, dass die Röntgen-Refraktionsradiographie Defekte detektieren kann, die kleiner sind als die Ortsauflösung des verwendeten 2DDetektors. Zum anderen können zwei verschiedene Typen von Defekten unterschieden werden. Bei dem ersten Typ handelt es sich um runde Poren mit geringer innerer Oberfläche. Diese, sogenannten „keyhole pores“ sind charakteristisch für eine zu hohe Energiedichte während des SLM Prozesses. Bei dem zweiten Typ handelt es sich um nicht komplett aufgeschmolzenes Pulver. Diese Defekte zeichnen sich durch eine hohe innere Oberfläche aus und sind charakteristisch für eine zu geringe Energiedichte. Vergleichende Messungen mit hochauflösender Synchrotron CT und optischer Mikroskopie bestätigen die charakteristischen Formen der verschiedenen Defekte. T2 - Symposium zerstörungsfreie Materialcharakterisierung - Charakterisierung additiv gefertigter Komponenten CY - Berlin, Germany DA - 28.11.2017 KW - Additive Fertigung KW - Röntgen-Refraktion KW - Porosität PY - 2017 AN - OPUS4-43403 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jensen, S. A. A1 - Rosu, Dana Maria A1 - Hertwig, Andreas A1 - Hansen, P.-E. T1 - Use of Rayleigh-Rice Theory for Analysis of Ellipsometry Data on Rough CIGS Films N2 - Ellipsometry is a useful tool for studying the optical properties of thin films such as photovoltaic devices. We employ Müller matrix ellipsometry to study the thin film photovoltaic material copper indium gallium selenide Cu(In,Ga) Se2 (CIGS), a commercially relevant material with high energy conversion efficiency. Confocal microscopy reveals an rms roughness of 68 nm, which greatly affects the ellipsometry data. Rayleigh-Rice theory is employed to account for the optical properties of the surface roughness in the ellipsometry experiment, and a library search method is used to compare Müller parameters calculated for various CIGS compositions, to the measured data. The Müller parameters calculated with the Rayleigh-Rice model are found to correspond well with the measured data, and a surface roughness of 37nm and a correlation length of 125nm are extracted. KW - Photovoltaics KW - Thin Films KW - Ellipsometry KW - Scattering Theory KW - Optical Wavefield KW - Simulation KW - Müller Polarimetry KW - Multidimensional Spectroscopy PY - 2017 DO - https://doi.org/10.1002/pssc.201700217 SN - 1862-6351 VL - 14 IS - 12 SP - 1700217, 1 EP - 5 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-43390 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Instrumented Indentation Testing (IIT) - A critical journey from the very first steps to the modern state of the art N2 - Nowadays the Instrumented Indentation Testing (IIT), in the nano range often named as nano indention, is one of the most commonly used methods to determine the mechanical properties of materials in the micro and nano range. This method is already extensive standardized in DIN EN ISO 14577 part 1-4. In the past, the application of this standard in testing praxis shows that the established values have an excellent precision. On the other side, the trueness as comparability of obtained results with reference values is not so good. To improve accuracy of IIT the use of a variable ε and the consideration of the lateral displacement during indentation became normative requirements during the last revision of ISO 14577. Starting with the beginning of instrumented indentation testing in 1898 the historical background and the main assumption of the Oliver and Pharr method will be explained and critical discussed. It will be shown how to apply the use of a variable ε and the consideration of the lateral displacement during indentation in the daily testing work to improve accuracy of IIT. Finally, ongoing standardization projects in the field of IIT will be briefly presented. T2 - Advanced nano-mechanical techniques for academic and industrial research. MML Conference and Workshop CY - Warwick, UK DA - 13.12.2017 KW - ISO 14577 KW - Instrumented Indentation Testing KW - Nanoindentation KW - IIT KW - Mechanical properties KW - Variable epsilon KW - Lateral displacement PY - 2017 AN - OPUS4-43466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Dynamic instrumented indentation test application and standardisation N2 - The draft of part 5 of ISO 14577 specifies verification and calibration of testing machines for carrying out the measurement of the dynamic material response when an oscillatory force or displacement, with amplitudes small in comparison to the prescribed target values, is imparted to the indenter while the indenter is continuously loaded to a prescribed target load or target depth or while the load or displacement is held constant at a prescribed target value. In case of a material showing plastic-elastic behavior, the measured dynamic response is used for continuous evaluation of the dynamic stiffness of the contact as a function of depth and frequency. Using the dynamic stiffness of the contact a reduced dynamic modulus will be calculated. In case of a material showing visco-elastic behavior from the measured dynamic response also the dynamic contact damping coefficient as function of depth and frequency is evaluated continuously. Using dynamic contact stiffness and dynamic contact damping coefficient reduced lost and storage modulus for visco-elastic materials will be calculated. The main normative requirements of the draft are discussed and their applications are illustrated by examples from daily experimental praxis. T2 - 13th Conference on Local Mechanical Properties CY - Košice, Slovak Republic DA - 06.11.2017 KW - ISO 14577 KW - Instrumented indentation testing KW - Nanoindentation KW - IIT KW - Mechanical properties KW - Dynamic testing KW - Visco-elastic KW - Loss modul KW - Storage modul PY - 2017 AN - OPUS4-43468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas T1 - Reading Between the Lines – Automated Data Analysis for Low-Field NMR Spectra N2 - For reaction monitoring using NMR instruments, in particular, after acquisition of the FID the data needs to be corrected in real-time for common effects using automated methods. When it comes to NMR data evaluation under industrial process conditions, the shape of signals can change drastically due to nonlinear effects. However, the structural and quantitative information is still present but needs to be extracted by applying predictive models. Acquired raw spectra were processed with the following tools: · Phase correction using the Entropy minimization method · Baseline correction using a low-order Polynomial fit · Alignment (icoshift) Pure component models based on Pseudo-Voigt functions can be derived via peak fitting of measured pure components or by the use of spin calculations. T2 - Tackling the Future of Plant Operation - Jointly towards a Digital Process Industry CY - Barcelona, Spain DA - 13.12.2017 KW - Process Monitoring KW - Online NMR Spectroscopy KW - Indirect Hard Modeling KW - Spectral Modeling KW - Process Analytical Technology KW - CONSENS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-434346 AN - OPUS4-43434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana T1 - Design and Validation of a Compact Online NMR Module N2 - The recent developments of inovative compact NMR spectrometers are therefore remarkable due to their possible application in process analytical technology (PAT) in an industrial environment without high maintenance requirements. spectroscopic methods, NMR spectroscopy offers some unique features for online reaction monitoring. However, those benefits have not been exploited for PAT applications so far. Within the CONSENS Project, the challenge to adapt a commercially available benchtop NMR spectrometer to the full requirements of an automated chemical production environment was tackled successfully. was provided in an explosion proof housing and involves a compact NMR spectrometer together with an automated data acquisition and evaluation unit, flow control, as well as data communication. T2 - Tackling the Future of Plant Operation - Jointly towards a Digital Process Industry CY - Barcelona, Spain DA - 13.12.2017 KW - Process Monitoring KW - Online NMR Spectroscopy KW - Indirect Hard Modeling KW - Explosion Safety KW - Field Integration KW - CONSENS KW - Process Analytical Technology KW - OPC UA PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-434351 AN - OPUS4-43435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael ED - Pinnow, C. J. ED - Schäfer, S. T1 - "Prozess‐Sensoren 4.0" – Chancen für neue Automatisierungskonzepte und neue Geschäftsmodelle in der Prozessindustrie N2 - Prozess-Sensoren 4.0 vereinfachen ihre Einbindung über Plug and Play, obwohl sie komplexer werden. Sie bieten Selbstdiagnose, Selbstkalibrierung und erleichterte Parametrierung. Über die Konnektivität ermöglichen die Prozess-Sensoren den Austausch ihrer Informationen als Cyber-physische Systeme mit anderen Prozess-Sensoren und im Netzwerk. Der Aufbruch von der aktuellen Automation zum smarten Sensor hat bereits begonnen. Automatisierungstechnik und Informations- und Kommunikationstechnik (IKT) verschmelzen zunehmend. Wenn die Prozessindustrie dieses nicht definiert, tun es andere. Für die weitere Entwicklung von der Ist‐Situation zu einer Industrie-4.0-Welt in der Prozessindustrie werden mehrere Szenarien diskutiert. Diese reichen vom erleichterten Abruf sensorbezogener Daten über zusätzliche Kommunikationskanäle zwischen Sensor und mobilen Endgeräten über vollständig bidirektionale Kommunikation bis hin zur Einbindung der Cloud und des Internets in virtualisierte Umgebungen. Um zu einer störungsfreien Kommunikation aller Sensoren untereinander zu kommen, muss mindestens ein einheitliches Protokoll her, das alle Sensoren sprechen und verstehen. Der derzeit greifbarste offengelegte Standard, der moderne Kommunikationsanforderungen erfüllt, ist OPC Unified Architecture (OPC-UA). Viele halten das Sortieren der Kommunikationsstandards für eines der wesentlichen Errungenschaften von Industrie 4.0. Eine Topologie für smarte Sensoren, das Zusammenwirken mit daten- und modellbasierte Steuerungen bis hin zur Softsensorik sowie weitere Anforderungen an Sensoren sind jedoch heute noch nicht angemessen beschrieben. Wir müssen jetzt schnell die Weichen für eine smarte und sichere Kommunikationsarchitektur stellen, um zu einer störungsfreien Kommunikation aller Sensoren auf Basis eines einheitlichen Protokolls zu kommen, welches alle Sensoren ausgeben und verstehen. Aktuelle und zukünftige öffentliche Förderung von Industrie 4.0-Projekten sind eine gute Investition. Wegen der hohen Komplexität und Interdisziplinarität gelingt die Umsetzung nur gemeinsam zwischen Anwendern aus der Prozessindustrie, Software- und Geräteherstellern und Forschungsgruppen. Anwender sind gefragt, diese neue Technologie durch eine beschleunigte Validierung und Akzeptanz umzusetzen. Sie erhalten die einzigartige Chance, ihre Prozesse und Anlagen wettbewerbsfähig zu halten. Kooperativ betriebenen F&E-Zentren und gemeinsam anerkannten Applikationslaboren kommt dafür eine hohe Bedeutung zu. T2 - Tagung Industrie 4.0 - "Safety und Security - Mit Sicherheit gut vernetzt", Hochschule für Technik und Wirtschaft CY - Berlin, Germany DA - 28.04.2017 KW - Prozessanalytik KW - Online-NMR-Spektroscopie KW - Industrie 4.0 KW - Automatisierung KW - Prozessindustrie KW - Smarte Sensoren KW - Sensoren PY - 2017 SN - 978-3-410-26406-4 SP - 135 EP - 150 PB - Beuth CY - Berlin AN - OPUS4-43436 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Anomalous surface composition in thin films of a poly(vinyl methyl ether) / polystyrene blend N2 - Highly surface-sensitive X-ray photoelectron spectroscopy at HE-SGM beamline revealed in the outermost region (< 2nm) of thin films (15 -65 nm) of PVME/PS blends a relative high amount of PS, whereas in slightly deeper regions PVME was enriched. Such enrichment of PVME in the whole near-surface region was proposed in former investigations based on conventional XPS studies. T2 - Bessy User Meeting 2017 CY - Berlin, Germany DA - 13.12.2017 KW - Energy resolved XPS KW - Depth profiling KW - Thin films KW - Polymer blends PY - 2017 AN - OPUS4-43443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Donsky, I. S. T1 - 2D nanomaterials with switchable pathogen binding N2 - Graphene derivatives have shown great promise in the field of pathogen binding and sensing. Due to their diverse applications, they show a variety of activities that range from bacterial adhesion to bacterial resistance. Therefore, domination of the graphene-pathogen interactions is highly relevant for producing 2D platforms with the desired applications. In order to gain control over the interactions between graphene and biosystems, mechanisms should be fully understood. The surface functionality of graphene is one of the most important factors that dominates its interactions with biosystems and pathogens. Covalent functionalization is a robust method through which functionality, chemical structure, and subsequently physicochemical properties of graphene are abundantly manipulated. A critical issue for preparing graphene-based 2D materials with a defined surface structure, however, is controlling the functionalization in terms of number, position, and type of functional groups. T2 - 9th Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Graphene KW - Functionalization KW - XPS KW - C Kedge NEXAFS PY - 2017 AN - OPUS4-43456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Quantitative chemical depth-profiling by synchrotron-radiation-XPS: Investigation of SrF2-CaF2 core-shell nanoparticles N2 - SrF2 nanoparticles can be doped with trivalent earth metal ions such as Eu3+ and Tb3+ to generate materials exhibiting an intensive red or green fluorescence. A CaF2 shell increases intensity, fluorescence lifetie and quantum yield. The chemical composition of the nanoparticle core-shell region is investigated by XPS at different excitation energies corresponding to different information depths. T2 - Ninth Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Core-shell nanoparticles KW - Synchrotron-XPS KW - Depth-profiling PY - 2017 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-43464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hüllmann, Dino T1 - A low-cost cable-suspended parallel manipulator for testing 3D olfaction algorithms N2 - Cable-suspended parallel manipulators have been a topic of research for multiple decades and called special attention in the fields of simulations. However, they are also well-suited for the simple evaluation of aerial-based mobile robot olfaction (MRO) algorithms, such as gas source localization and gas distribution mapping. Based on an open source framework for 3D printers, we designed a low-cost underconstrained, cable-suspended parallel manipulator. Computations are carried out purely on an Atmel ATmega2560 microcontroller. T2 - 33rd Danubia- Adria Symposium on Advances in Experimental Mechanics CY - Trieste, Italy DA - 19.09.2017 KW - Cable-suspended parallel manipulator KW - 3D KW - Mobile robot olfaction PY - 2017 AN - OPUS4-42317 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ickert, Stefanie T1 - Collision Specific Fragmentation of Oligonucleotides in Tandem Mass Spectrometry N2 - Tandem MS experiments allow the fast acquisition of spectral datasets with enormous size and unprecedented content of information. The most commonly used method is undoubtedly collision induced dissociation (CID). The relatively young technical adaptation of CID to modern day Orbitrap experiments needs a higher confinement voltage and has accordingly been named higher-energy collisional dissociation HCD. Despite the name the absolute value of transferred energy per collision in HCD is lower than in CID. Since for many proteins CID and HCD result in comparable fragmentation patterns the two techniques are often treated as interchangeable. This approach is, however, not without pitfalls as other classes of biomolecules often exhibit strongly pronounced fragmentation specificity. As an example, MS/MS experiments on several 4-mer oligonucleotides were conducted employing both collision methods and the results were thoroughly compared. It is apparent that not only the total fragment yield but also the identity of the observed fragments differ significantly between the two methods. T2 - Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie DGMS CY - Kiel, Germany DA - 05.03.2017 KW - Tandem MS KW - DNA KW - Mass Spectrometry PY - 2017 AN - OPUS4-42328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ickert, Stefanie T1 - Collision Induced Dissociation of DNA Oligonucleotides Studied by Tandem Mass Spectrometry and Ion Mobility N2 - Multiply negatively charged DNA oligonucleotides of small sizes (n=15-40) have been subjected to a comprehensive tandem mass spectrometric study (MS/MS). Collision induced dissociation (CID) mass spectrometry (MS) was applied as a tool to break down isolated DNA oligonucleotides with a defined number of charges. Various lenghts and sequences were analyzed and all of them showed a comparable direct correlation regarding the threshold collision energy for fragmentation and dependence on number of charges on the precursor ions. It was also revealed that the increase in charges and thus Coulomb repulsion results in the transition from a folded, compact form to an elongated structure of the precursor ions. T2 - Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie DGMS CY - Hamburg, Germany DA - 28.02.2016 KW - Ion Mobility KW - DNA KW - Mass Spectrometry PY - 2016 AN - OPUS4-42329 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ickert, Stefanie T1 - DNA Oligonucleotide Fragmentation in Tandem Mass Spectrometry Experiments N2 - Multiply negatively charged DNA oligonucleotides of small sizes (n=15-40 bases) have been subjected to a comprehensive tandem mass spectrometric study (MS/MS). Collision induced dissociation (CID) mass spectrometry (MS) was applied as a tool to break down isolated DNA oligonucleotides with a defined number of charges. Various lenghts and sequences were analyzed unravelling a comparable direct correlation between the threshold collision energy for fragmentation and the charge-per-base density in the precusor ion. It was also revealed that the increase in charges and thus Coulomb repulsion results in the transition from a folded, compact form to an elongated structure of the precusor ions. T2 - International Mass Spectrometry Conference IMSC CY - Toronto, Canada DA - 20.08.2016 KW - Mass Spectrometry KW - DNA KW - Tandem MS PY - 2016 AN - OPUS4-42330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Low pressure plasma, UV photo and wet chemical modification of graphite, graphene and carbon nano tubes N2 - Graphene is a two-dimensional carbon network with unique properties, including high mechanical stiffness, strength, and elasticity, outstanding electrical and thermal conductivity, and many others. Despite these advantages, its low solubility, poor reactivity and the limited accessibility of a well-defined basal plane are major challenges for applications. An ideal method to overcome these problems is the covalent attachment of functional molecules to its surface which enables further reactive modifications for specific applications. There is a number of different technologies for surface functionalization of graphene and related CNT materials. However, to get control on the functionalization process and to optimize the performance of the modified surfaces analytical tools for surface chemical characterization are required. X-ray absorption (NEXAFS) and photoelectron spectroscopy (XPS) have been identified to be rather powerful here. Specifically NEXAFS spectroscopy underpinned by quantum chemical spectrum simulations is unique in a way to address changes of aromaticity and defect formation at the graphene surface during functionalization. For relevant surface modification technologies, we present examples on how NEXAFS and XPS can perform well. All presented modifications aim on the production of platforms for defined functional 2D nanomaterials, as for example multifunctional hybrid architectures. In detail, we investigated: • Graphene and carbon nanotube functionalized by a Vacuum-Ultraviolet (VUV) induced photochemical process in NH3 or O2 atmospheres in order to introduce amino or hydroxy functionalities, respectively. • Br bonding on r.f. cw low pressure plasma brominated graphite surfaces by using Br2 and bromoform as plasma gases. • A wet chemical method for covalent functionalization of graphene sheets by a one-pot nitrene [2+1] cycloaddition reaction under mild conditions. Here a reaction between 2,4,6-trichloro-1,3,5-triazine and sodium azide with thermally reduced graphene oxide (TRGO) results in defined dichlorotriazine-functionalized graphene sheets. T2 - The 17th European Conference on Applications of Surface and Interface Analysis CY - Montpellier, France DA - 24.09.2017 KW - Graphene KW - XPS KW - NEXAFS PY - 2017 AN - OPUS4-42787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Lange, Nele T1 - Selektive chemische Modifikation von Siliziumnitrid-Oberflächen für neuartige biosensorische Applikationen N2 - Biosensoren gewinnen in den letzten Jahren zunehmend an Bedeutung. So erfolgt die Identifizierung des Analyten mit Biosensoren deutlich schneller und unkomplizierter als mit herkömmlichen analytischen Methoden. Aufgrund des Schlüssel-Schloss-Prinzips ist zudem die Detektion von Biosensoren äußerst selektiv. Die Herstellung dieser Sensoren erfolgt häufig trotz der Unzuverlässigkeit der Silanchemie über die Silanisierung der Si-H- bzw. Si-OH-Bindungen an der Silizium-Oberfläche. Die Abhängigkeit von Temperatur- und pH-Wert, sowie die Veränderung der Filmdicke bei nur kleinen Schwankungen des Wassergehalts während der Umsetzung werden oft vernachlässigt. Seltener wird die Si-NHx-Bindung genutzt, um dünne organische Filme zu erzeugen. Im Rahmen dieser Arbeit wurde eine neue Funktionalisierungsstrategie entwickelt, die die Silanchemie vermeidet. Die Idee basiert auf der Herstellung einer Azid-terminierten Oberfläche erzeugt aus Oberflächenaminen des materialintrinsischen Stickstoffs von Siliziumnitrid (Si3N4). Diese Azidgruppen bildeten die Grundlage für die Click-Chemie mit geeigneten Alkin-terminierten (Bio)molekülen und die anschließende Immobilisierung von ausgewählten Analyten. Die Funktionalisierungsstrategie umfasst die Erzeugung von NHx-terminierten Si3N4-Oberflächen durch Flusssäureätzung gefolgt von deren Umwandlung in Azidgruppen durch verschiedene Methoden. Im Anschluss wurden Alkine durch die Kupfer-katalysierte Azid-Alkin-Cycloaddition (CuAAC, Click-Chemie) an die Azid-terminierte Oberfläche immobilisiert. Der Erfolg der einzelnen Reaktionsschritte wurde durch oberflächenanalytische Methoden, durch XPS, NEXAFS und ToF-SIMS, überprüft. Die Charakterisierung der gebildeten Triazolringe erfolgte anhand des N 1s-XP-Spektrums sowie der NEXAFS C K-Kante. Die CF3-Gruppe wurde anhand der C 1s und F 1s-XP-Spektren, sowie der NEXAFS F K-Kante identifiziert. ToF-SIMS Untersuchungen bestätigten ebenfalls die Bindung des Alkins an die Si3N4-Oberfläche. Im weiteren Verlauf der Arbeit wurde die direkte Anbindung eines Biomoleküls an die Si3N4 Oberfläche getestet. Hierfür wurde das Biotin/Streptavidin-System durch eine Click-Reaktion an der Oberfläche verankert. Die erfolgreiche Biotin/Streptavidin-Interaktion wurde ebenfalls mit XPS, NEXAFS und ToF-SIMS nachgewiesen. Der Erfolg der Click-Reaktionen war sowohl bei der Methodenentwicklung als auch bei der Immobilisierung des Modellfilms vom genutzten Lösungsmittel abhängig. Neben der direkten Immobilisierung von (Bio)molekülen an die Si3N4-Oberfläche durch die Click-Chemie gelang es auch einen Kupfer(II)trifluormethoxyphenanthrolin-Komplex als künstliche Nuklease über Amid-Kopplung an die Si-NHx-Oberfläche zu binden. Hierbei diente ein OCF3-Substituent des Kupfer(II)trifluormethoxyphenanthrolin-Komplexes als XPS-Sonde. Die Identifizierung des Komplexes erfolgte anhand der OCF3-Komponente im C 1s- und F 1s-XP-Spektrum und der NEXAFS F K-Kante, sowie des Cu 2p-XP-Spektrums. Die ToF-SIMS-Massenspektren bestätigten ebenfalls die Bindung des Komplexes. Die Kupfermenge wurde mit der Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS) zu 0.08 µg/cm2 bestimmt, was 87 x 1012 Kupferatome pro cm2 entspricht. Nach der Verifizierung des immobilisierten Komplexes erfolgte die Untersuchung der Spaltaktivität der auf der Si3N4-Oberfläche gebundenen künstlichen Nuklease gegenüber Plasmid-DNA. Hierbei wurde eine Zunahme der Spaltaktivität mit zunehmender DNA-Inkubationszeit festgestellt. Weiterhin ist bemerkenswert, dass der verwendete Kupfer(II)trifluormethoxyphenanthrolin-Komplex erst auf der Oberfläche seine Spaltaktivität entfaltet. Kontrollproben in Lösung zeigten im Gegensatz zu dem immobilisierten Komplex keine Spaltaktivität. KW - Surface Chemistry KW - Silicon Nitride KW - Click Chemistry KW - DNA Cleavage KW - XPS KW - NEXAFS KW - ToF-SIMS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:188-fudissthesis000000105216-6 SP - 1 EP - 240 PB - Freie Universität CY - Berlin AN - OPUS4-42790 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Harald A1 - Unger, Wolfgang A1 - Schulte, Petra T1 - Nanotechnologie Aktivitäten der BAM N2 - Die Präsentation gibt einen Überblick über die verschiedenen Aktivitäten der BAM im Bereich der Nanotechnologie mit den Schwerpunkten Nanopartikel und Nanosicherheit. Es wird sowohl die Transportsicherheit, als auch die Sicherheit von Batterien mit Nanopartikeln angesprochen. Verschiedene BAM-Projekte zum Thema Nano werden vorgestellt, beginnend mit relevanten REFOPlanprojekten über die Erstellung der OECD nanoTG110 bis hin zu EU-Projekten zur Standardisierung von Messungen an Nanomaterialien, hier insbesondere AEROMET, NanoDefine, NanoValid und EC4SafeNano. T2 - Nano-Behördenklausur der Bundesoberbehörden CY - Berlin, Germany DA - 02.11.2017 KW - Nano KW - Nanotechnologie KW - Nanopartikel KW - Nanosicherheit KW - Nanoanalytik PY - 2017 AN - OPUS4-42793 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Herbstsitzung Plasma Germany 2017, Frohnhausen N2 - Der Vortrag widmet sich den Normenentwicklungen auf den Gebieten der • Chemische Oberflächenanalyse und Rastersondenmikroskopie • Elektronenmikroskopie und Mikrobereichsanalyse • Prüfverfahren (zu Nanotechnologien) • Hardness Testing • Oberflächenmesstechnik im Mikro- und Nanobereich • Kohlenstoff- und keramische Hartstoffschichten • Mess- und Prüfverfahren für Schichten und Schichtsysteme • Dünne Schichten für die Optik • Coating Qualification Tests T2 - FA_NORMUNG_PLASMA_GERMANY CY - Frohnhausen, Germany DA - 08.11.2017 KW - Normen KW - Oberflächentechnik KW - Oberflächenanalytik KW - Oberflächenmesstechnik PY - 2017 AN - OPUS4-42821 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesterle, Diana T1 - Hinterglasmalerei als Technik der Klassischen Moderne 1905-1955. Ein Forschungsprojekt N2 - Im Rahmen des Förderprogramms „Forschung in Museen“ hat die VolkswagenStiftung dem Museum Penzberg - Sammlung Campendonk ein dreijähriges Forschungsvorhaben über die „Hinterglasmalerei als Technik der Klassischen Moderne 19051955“ bewilligt. Projektpartner sind die BAM Bundesanstalt für Materialforschung und -prüfung, Berlin und das Doerner Institut, München. Das interdisziplinäre Forschungsteam von Kunsthistorikern, Restauratoren und Chemikern untersucht die Hinterglasmalerei als eigenständige und kunsthistorisch relevante Werkgruppe und gibt Aufschluss über die Maltechnik und die verwendeten Materialien. Obwohl die Klassische Moderne gut erforscht ist, hat sich die Kunstgeschichte bisher nicht eingehend mit Hinterglasbildern des 20. Jahrhunderts beschäftigt. Dennoch sind von der Hinterglastechnik wichtige Impulse für die Malerei der Moderne ausgegangen. Zwar wurde dieses Thema vereinzelt in Publikationen erwähnt, doch eine umfassende Darstellung steht bis heute aus. Daher ist es das Ziel, die Hinterglasmalerei innerhalb der Klassischen Moderne zu verorten und die Verbreitungswege vom „Blauen Reiter“ zum Rheinischen Expressionismus, über die Galerie „Der Sturm“ bis zum Bauhaus zu ergründen. In dem Projekt geht es um die Erfassung der Künstler und des Umfangs ihres Hinterglasbild-Œuvres. Daneben steht die Untersuchung ausgewählter Bilder durch das Forschungsteam im Vordergrund. Durch die Zusammenführung der kunsttechnologischen Untersuchungen mit den Ergebnissen der Materialanalyse ist ein tieferes Verständnis der künstlerischen Besonderheiten der modernen Hinterglaskunst zu erwarten. Der Schwerpunkt der analytischen Untersuchungen ist eine Kombination von non-invasiven, mobilen Techniken zur Farbmittelidentifizierung und Bindemittelklassifizierung, die in situ durchgeführt wird. An einer begrenzten Anzahl von Hinterglasarbeiten werden Mikroproben genommen um die genaue Zusammensetzung der Malschicht zu bestimmen und um die Ergebnisse der mobilen Messungen zu validieren. An ausgewählten Werken der Moderne sollen die bisherigen Ergebnisse exemplarisch erläutert werden. T2 - 10. Tagung zur Hinterglaskunst CY - Bernried, Germany DA - 13.10.2017 KW - Hinterglasmalerei KW - Spektroskopie KW - Moderne Kunst PY - 2017 AN - OPUS4-42826 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lavric, V. A1 - Isopescu, R. A1 - Maurino, V. A1 - Pellegrino, F. A1 - Pellutiè, L. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan T1 - A new model for nano-TiO2 crystal birth and growth in hydrothermal treatment using an oriented attachment approach N2 - The synthesis of TiO2 was studied in an original hydrothermal process that uses triethanolamine titanium complex Ti(TeoaH)2 as a Ti precursor and triethanolamine (TeoaH3) as a shape controller to obtain bipyramidal anatase nanoparticles. Backed-up by experimental evidence, i.e., time profiles for Ti(IV) species concentrations together with crystal shape and particle size distributions measured by dynamic light scattering and electron microscopy, a mathematical model was built. The model includes chemical reactions responsible for TiO2 generation in solution and the subsequent anatase nucleation and crystal growth. The oriented attachment mechanism was adopted to explain the build-up of crystals with equilibrium anatase structure (Wulff structure) and time-varying shape factor. This complex mathematical model was solved writing and validating an in-house software using the Matlab (Natick, MA, USA) environment. The process was simulated for a batch time of 50 h, and the results, in terms of main species concentration and crystal size distributions, are in rather good agreement with the experimental measurements. KW - Nanoparticles KW - TiO2 KW - SEM/EDX KW - Modelling KW - Crystal growth PY - 2017 UR - http://pubs.acs.org/doi/pdf/10.1021/acs.cgd.7b00302 DO - https://doi.org/10.1021/acs.cgd.7b00302 SN - 1528-7483 SN - 1528-7505 VL - 17 IS - 11 SP - 5640 EP - 5651 PB - ACS Publications AN - OPUS4-42724 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lauer, Franziska T1 - Quantitative profiling of pollen grain mixtures by multivariate MALDI-TOF MSI N2 - Anemophilous plants produce pollen grains, which have to be monitored to provide a national information network for persons suffering from an allergy. The current conventional characterization and identification of pollen is performed by time-consuming microscopic examinations based on the genus-specific pollen shape and size. These examinations need proficient researchers, are not statistically validated, and additionally rely on relatively inaccurate observations of the pollination process. A variety of spectroscopic and spectrometric approaches have been proposed to develop a fast and reliable pollen identification using specific molecular information. Amongst them, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) was recently applied for the rapid investigation of such complex biological samples. The combination of obtained peak patterns from pollen mass spectra and multivariate statistic provide a powerful tool for identifying taxonomic relationships. A novel application based on the use of conductive carbon tape as MALDI target simplified the sample preparation and yielded enhanced the quality of the mass spectra. This led to a sufficient statistical analysis of the MS pattern, which is important when identify pollen grains in natural species mixtures. Based on this approach, promising results could be obtained by MALDI-TOF MS imaging (MSI) of artificial pollen mixtures followed by multivariate analysis. Of special interest is here the determination of the detection limit (number of pollen grains). Therefore, different pollen grain compositions were investigated for quantitative profiling of each individual pollen species within these complex mixtures. Our results can be used to improve the taxonomic differentiation and identification of pollen species and might be useful for the development of a routine method to identify pollen based on imaging mass spectrometry. T2 - Euroanalysis 2017 CY - Stockholm, Sweden DA - 28.08.2017 KW - MALDI-TOF MS KW - Imaging KW - Conductive carbon tape KW - Pollen KW - PCA PY - 2017 AN - OPUS4-42749 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lauer, Franziska T1 - Identification of pollen grains in mixtures using hyperspectral MALDI-TOF MS imaging N2 - Anemophilous plants produce pollen grains, which promote allergies. Therefore, pollen are monitored to provide a national information network. Their conventional identification and differentiation is performed by time-consuming microscopic examinations based on the genus-specific pollen morphology. A variety of spectroscopic and spectrometric approaches have been proposed to develop a fast and reliable pollen identification using specific molecular information. Amongst them, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) showed a high potential for the successful investigation of such complex biological samples. Specifically, it was illustrated that MALDI-MS imaging provides a powerful tool to identify pollen grains in pollen mixtures on the basis of ion intensity plots. More recently, the evaluation of the obtained peak patterns from pollen mass spectra with multivariate statistics enables a consistent and rapid identification of the taxonomic relationships. A novel application using conductive tape on the MALDI target simplifies sample preparation and enhanced the quality of the mass spectra. This led to a comprehensive analysis of the MS patterns, which is important when identifying pollen grains from different plant species in mixtures. Here, we present further developments in MALDI-MS imaging of mixtures of pollen from different plant species. By combining conductive tape sample preparation with MALDI MSI and chemometric analysis, first promising results were obtained. In addition, we discuss the ability of partial least square regression (PLS-R) to identify pollen species based on independent reference spectra and present first results obtained with artificial pollen mixtures. These methods will be used in future online identification of pollen species in natural pollen mixtures. T2 - Workshop “FT‐IR Spectroscopy in Microbiological and Medical Diagnostics” CY - Robert Koch‐Institute, Berlin, Germany DA - 19.10.2017 KW - MALDI-TOF MS KW - Imaging KW - Pollen KW - MVA PY - 2017 AN - OPUS4-42750 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lauer, Franziska T1 - Multivariate MALDI-TOF MS imaging of artificial pollen grain mixtures N2 - About one in seven German citizens is suffering from respiratory allergies, which are mainly caused by anemophilous plant pollen. These pollen grains are monitored to provide a national information network. Their conventional identification is performed by time-consuming microscopic examinations based on the genus-specific pollen morphology. A variety of spectroscopic and spectrometric approaches have been proposed to develop a fast and reliable pollen identification using specific molecular information. Amongst them, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) showed a high potential for the successful investigation of such complex biological samples. The evaluation of the obtained peak patterns from pollen mass spectra with multivariate statistics enables a consistent and rapid identification of the taxonomic relationships. T2 - OurCon V CY - Doorn, The Netherlands DA - 25.09.2017 KW - MALDI-TOF MS KW - Imaging KW - Pollen KW - MVA PY - 2017 AN - OPUS4-42752 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Prozess-Spektroskopie in Mikroemulsionen für das Online-Monitoring einer homogenen Hydroformylierungsanlage N2 - Homogen katalysierte Reaktionsschritte sind ein wichtiges Werkzeug in der chemischen Industrie. Durch die milden Reaktionsbedingungen hinsichtlich Temperatur und Druck bei gleichzeitig hoher Selektivität bieten diese die Möglichkeit energieeffizienter und ressourcenschonender Produktionsschritte. Eine der wichtigsten industriellen Anwendungen bildet die Hydroformylierung. Hier besteht das Katalysatorsystem meist aus Übergangsmetallkomplexen, vorwiegend Kobalt und Rhodium, die zur Steuerung der Selektivität und Löslichkeit mit mehrzähnigen Liganden koordiniert sind. Diese Komplexe liegen für eine effiziente Katalysator-rückführung in wässriger Lösung vor, was jedoch die Anwendbarkeit auf kurzkettige Edukte mit hinreichender Wasserlöslichkeit beschränkt. Ein möglicher Lösungsansatz für die Verwendung langkettiger Alkene ist die Umsetzung der Reaktion in einer Mikroemulsion. Durch die gesteigerte Phasen-grenzfläche besteht ein effektiver Kontakt von Katalysator und Reaktanden bei gleichzeitiger Möglichkeit der Produktseparation durch Phasentrennung, während der Katalysator dem Reaktionsschritt zurückgeführt wird und das Verfahren damit wirtschaftlich macht. Am Beispiel der Reaktion von 1-Dodecen zu Tridecanal wird der Einsatz von Online-NMR- und -Raman-Spektroskopie für die Prozessanalytik (sowie Applikation von komplexen Regelungskonzepten) innerhalb eines mizellaren Systems demonstriert. Ein speziell konzipierter Laboraufbau ermöglicht die Durchführung von Experimenten unter Prozessbedingungen für die in Mikroemulsionen äußerst anspruchsvolle Entwicklung und Kalibrierung von multivariaten Modellen für die Raman-Spektroskopie. Diese konnten anschließend im Rahmen einer mehrtägigen Betriebs-studie einer Miniplant am realen technischen System erprobt werden. T2 - Bruker Optics Anwendertreffen 2017 CY - Ettlingen, Germany DA - 07.11.2017 KW - Prozessanalytik KW - Reaktionsmonitoring KW - Industrie 4.0 KW - Online-Raman-Spektroskopie KW - Online-NMR-Spektroskopie KW - Hydroformylierung KW - Mikroemulsionen PY - 2017 AN - OPUS4-42753 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc T1 - Temperature influence on coulometric trace humidity measurement N2 - Coulometric sensors were tested in humidified synthetic air at various gas temperatures. Generated frost point temperature in the gas ranged from -30 °C to -60 °C and were measured by coulometric sensors and in addition by a calibrated dew point hygrometer. The gas temperatures, which were measured by a calibrated Pt100 sensor, were set to -20 °C, 0 °C, 23 °C, 40 °C, 50 °C, and 60 °C during the experiments. Empiric nonlinear functions were calculated between the humidity and the sensor signal. In comparison to the measured signals at 23 °C, the sensor signals were lower at the other gas temperatures. Measurements at 60 °C showed indistinct results due to a great signal noise. The response behavior of the sensors was similar at 23 °C, 40 °C and 50 °C. In contrast to that, the sensors reacted slowly at a gas temperature of -20 °C and 0 °C. In summary, with coulometric sensors it was possible to measure continuously trace humidity with an expanded uncertainty below 2 K. T2 - IEEE Sensors 2017 CY - Glasgow, Scotland, UK DA - 30.10.2017 KW - Coulometric sensors KW - Trace humidity measurement KW - Temperature influence KW - Chemical reaction KW - Response behavior PY - 2017 AN - OPUS4-42756 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - Coupled molecular switching processes in ordered mono- and multilayers of stimuli-responsive rotaxanes on gold surfaces N2 - Interfaces provide the structural basis for function as, for example, encountered in nature in the membrane-embedded photosystem or in technology in solar cells. Synthetic functional multilayers of molecules cooperating in a coupled manner can be fabricated on surfaces through layer-by-layer self-assembly. Ordered arrays of stimuli-responsive rotaxanes undergoing well-controlled axle shuttling are excellent candidates for coupled mechanical motion. Such stimuli-responsive surfaces may help integrating synthetic molecular machines in larger systems exhibiting even macroscopic effects or generating mechanical work from chemical energy through cooperative action. The present work demonstrates the successful deposition of ordered mono- and multilayers of chemically switchable rotaxanes on gold surfaces. For the first time, rotaxane mono- and multilayers are shown to reversibly switch in a coupled manner between two ordered states as revealed by linear dichroism effects in angle-resolved NEXAFS spectra. Such a concerted switching process is observed only when the surfaces are well packed, while less densely packed surfaces lacking lateral order do not exhibit such effects. T2 - SupraChem 2015 CY - Berlin, Germany DA - 22.02.2015 KW - NEXAFS KW - Rotaxanes KW - Molecular machines KW - XPS KW - ToF-SIMS KW - AFM PY - 2015 AN - OPUS4-42800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Rui A1 - Russo, Patrícia A. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Jeon, Taeyeol A1 - Pinna, Nicola T1 - Hybrid organic–inorganic transition-metal phosphonates as precursors for water oxidation electrocatalysts N2 - Efficient water oxidation catalysts are required for the development of water splitting technologies. Herein, the synthesis of layered hybrid NiFephenylphosphonate compounds from metal acetylacetonate precursors and phenylphosphonic acid in benzyl alcohol, and their Oxygen evolution reaction performance in alkaline medium, are reported. The hybrid particles are formed by inorganic layers of NiO6 and FeO6 distorted octahedra separated by bilayers of the organic group, and template the Formation in situ of NiFe hydroxide nanosheets of sizes between 5 and 25 nm and thicknesses between 3 and 10 nm. X-ray absorption spectroscopy measurements suggest that the hybrid also acts as a template for the local structure of the metal sites in the active catalyst, which remain distorted after the transformation. Optimum electrocatalytic activity is achieved with the hybrid compound with a Fe content of 16%. The combination of the synergistic effect between Ni and Fe with the structural properties of the hybrid results in an efficient catalyst that generates a current density of 10 mA cm−2 at an overpotential of 240 mV, and also in a stable catalyst that operates continuously at low overpotentials for 160 h. KW - Water oxydation catalysis KW - EXAFS PY - 2017 DO - https://doi.org/10.1002/adfm.201703158 SN - 1616-301X SN - 1616-3028 VL - 27 IS - 40 SP - Article 1703158, 1 EP - 11 PB - WILEY-VCH Verlag CY - Weinheim AN - OPUS4-42783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Leonhard, H. T1 - Oberflächendetektive im Praxiseinsatz - Schnelltest auf Korrosionsgefahr an nichtrostenden Stählen N2 - Die Passivschicht von Behältern und Rohrsystemen aus nichtrostendem Stahl ist nicht nur durch den rauen Industriealltag gefährdet. Schon im Neuzustand können Schäden entstehen, etwa durch Schleifvorgänge oder ungenügende Entfernung von Anlauffarben. TÜV SÜD Chemie Service beteiligte sich an der Prüfung eines von der BAM entwickelten Schnelltests. Das Korropad-Verfahren liefert in nur 15 Minuten eine verlässliche Aussage zum Zustand der Passivschicht. KW - Nichtrostender Stahl KW - Korrosionsschnelltest KW - KorroPad KW - Passivschicht PY - 2017 SN - ISSN 0009-2800 VL - 50. Jahrgang IS - 10-2017 SP - 34 EP - 35 PB - Konradin-Verlag Robert Kohlhammer GmbH CY - Leinfelden-Echterdingen AN - OPUS4-42735 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Harald T1 - Projekt Nano-TG110 N2 - Die OECD-TG110 mit dem Titel "Particle Size Distribution Fibre Length and Diameter Distribution" wurde 1981 erstellt und seither nicht überarbeitet. Nanomaterialien, wie Nanopartikel oder Nanofasern werden nicht adressiert, genausowenig wie moderne Messverfahren. Das hier vorgestellte Projekt hat zur Aufgabe, die Größenmessung von Nanopartikeln und Nanofasern in einer neuen Technical Guideline der OECD zu standardisieren. Es wird die Projekthistorie dargestellt, die Anforderungen, der aktuelle Projekt-Bearbeitungsstand wird beleuchtet und die weiteren Arbeiten werden kurz skizziert. T2 - Nano-Behördenklausur der Bundesoberbehörden CY - Berlin, Germany DA - 02.11.2017 KW - Nano KW - Nanopartikel KW - Nanoparticle KW - OECD KW - Guideline PY - 2017 AN - OPUS4-42737 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rosner, M. T1 - Intercomparison of d26Mg Values in Mg Isotope RMs and Standards N2 - Accurate measurements of stable isotope abundance ratio variations are often reported using artifact based delta-scales, which rely on suitable isotopic reference materials (iRM) for their realization. For example, variations in the 26Mg/24Mg isotope abundance ratio in natural systems are typically reported as delta26Mg values that represents the relative difference between the 26Mg/24Mg ratio measured in a sample relative to its measurement preferably in an iRM. In the past, such delta26Mg measurements were referenced to NIST SRM 980, the initial zero of the delta26Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. It was then replaced by a Mg solution (DSM3), the new zero of the delta26Mg scale. A potential replacement iRM for DSM3 has been developed, ERM-AE143. This iRM has also been measured for its absolute isotope amount ratios1,2 making it traceable to the SI. The results of a delta26Mg intercomparison experiment include the Mg iRMs SRM 980, IRMM-009, ERM-AE143, AE144, AE145 standards DSM3 and Cambridge-1. The intercomparison involved 5 expert laboratories, consisting of 3 national metrological institutes (BAM, NIST, PTB) and 2 scientific research laboratories (GFZ Potsdam, UBremen). The iRMs were measured relative to AE143 and cover a range of ≈5 ‰ in delta26Mg. IRMM-009 has the lowest delta26Mg value while DSM3 has the highest, spanning a range in values that covers natural Mg isotope variations. The 2SD reproducibilities of the individual values from the different laboratories range from 0.02 to 0.26 ‰. The mean delta26Mg values, calculated from the laboratory means however show 2SD reproducibilities varing between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for delta26Mg determinations. 1 JAAS, 2015, 31,179; 2JAAS, 2016, 31, 1440 T2 - Goldschmidt Conference 2017 CY - Paris, France DA - 13.08.2017 KW - Iisotope reference materials KW - Delta values KW - Magnesium isotope PY - 2017 AN - OPUS4-42742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Delta values, Delta zero reference materials and uncertainties N2 - Discussion of Delta values, Delta scales, delta Zero reference materials and measurement uncertainties for delta-values under metrological aspects. T2 - CCQM Isotope Ratio Task Group CY - Delft, Netherlands DA - 27.10.2017 KW - Traceability KW - Measurement uncertainty KW - Delta scale KW - Reference material PY - 2017 AN - OPUS4-42743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kaur, I. A1 - Ellis, L.-J. A1 - Romer, I. A1 - Tantra, R. A1 - Carriere, M. A1 - Allard, S. A1 - Mayne-L'Hermite, M. A1 - Minelli, C. A1 - Unger, Wolfgang A1 - Potthoff, A. A1 - Rades, Steffi A1 - Valsami-Jones, E. T1 - Dispersion of nanomaterials in aqueous media: Towards protocol optimization N2 - The sonication process is commonly used for de-agglomerating and dispersing nanomaterials in aqueous based media, necessary to improve homogeneity and stability of the suspension. In this study, a systematic step-wise approach is carried out to identify optimal sonication conditions in order to achieve a stable dispersion. This approach has been adopted and shown to be suitable for several nanomaterials (cerium oxide, zinc oxide, and carbon nanotubes) dispersed in deionized (DI) water. However, with any change in either the nanomaterial type or dispersing medium, there needs to be optimization of the basic protocol by adjusting various factors such as sonication time, power, and sonicator type as well as temperature rise during the process. The approach records the dispersion process in detail. This is necessary to identify the time Points as well as other above-mentioned conditions during the sonication process in which there may be undesirable changes, such as damage to the particle surface thus affecting surface properties. Our goal is to offer a harmonized approach that can control the Quality of the final, produced dispersion. Such a guideline is instrumental in ensuring dispersion quality repeatability in the nanoscience community, particularly in the field of nanotoxicology. KW - Dispersion of nanomaterials KW - Aqueous media KW - Protocol development PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435886 UR - https://www.jove.com/video/56074 DO - https://doi.org/10.3791/56074 SN - 1940-087X IS - 130 SP - e560741, 1 EP - e560741, 23 PB - MyJove Corp. CY - Cambridge, MA, USA AN - OPUS4-43588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaraj, S. A1 - Dietrich, Paul A1 - Unger, Wolfgang T1 - Simultaneous surface and bulk sensitive XAS measurements of magnetic particle clusters N2 - Magnetic iron oxide nanoparticle clusters (mnpc) coated with organic stabilizers were investigated using scanning transmission x-ray microscopy (STXM). Simultaneous surface and bulk sensitive Fe L3 edge absorption spectra, obtained using a photomultiplier tube and a channeltron, were used to detect subtle changes in the oxidation state in the surface and bulk of Iron Oxide mnpc. The effectiveness of this mode of STXM operation is demonstrated for These nanoparticle clusters. T2 - X-Ray Microscopy Conference 2016 (XRM 2016) CY - Oxford, UK DA - 15.08.2016 KW - Scanning transmission x-ray microscopy (STXM) KW - Magnetic nanoparticles KW - Fe L3 edge absorption spectra PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435907 UR - http://iopscience.iop.org/article/10.1088/1742-6596/849/1/012014/meta DO - https://doi.org/10.1088/1742-6596/849/1/012014 VL - 849 SP - 012014, 1 EP - 012014, 4 PB - IOP Publishing AN - OPUS4-43590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wunderle, B. A1 - Onken, T. A1 - Heilmann, J. A1 - Silbernagl, Dorothee A1 - Arnold, J. A1 - Bieniek, T. A1 - Pufall, R. T1 - Reliability of sputtered thin aluminium films under accelerated stress testing by vibration loading and modeling N2 - Aluminium is still one of the most important contact metallisations for power electronic chips like MOSFETs or IGBTs. With a large difference in thermal expansion coefficients (CTEs) between aluminium and silicon and the temperatures generated in hot-spots during high power transients, these layers are prone to failure due to thermo-mechanical fatigue. Usually lifetime assessment is done by subjecting dedicated test specimens to standardised stress tests as e.g. active or passive thermal cycling. This paper proposes a novel method for accelerated stress testing and lifetime modelling of thin aluminium films in the high-cycle fatigue regime by isothermal mechanical loading. The proposed novel test method is suggested to complement or replace resource-demanding thermal cycling tests and allow simple in-situ monitoring of failure. T2 - 6th Electronic System-Integration Technology Conference (ESTC) CY - Grenoble, France DA - 13.09.2016 KW - Semiconductor device reliability KW - Thermal expansion KW - AFM KW - Vibrations KW - Nanoroughness KW - Accelerated stress testing KW - Active thermal cycling KW - Power electronic chips KW - Sputtered thin aluminium film KW - Thermomechanical fatigue PY - 2016 DO - https://doi.org/10.1109/ESTC.2016.7764458 SP - 1 EP - 14 PB - IEEE AN - OPUS4-43595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Adão, Filipe Jorge Santos Ferreira A1 - Rosemarie, Helmerich A1 - Gerrit, Voigt A1 - Laura, Moldenhauer A1 - Neumann, Patrick P. ED - Motavalli, M. ED - Ilki, A. T1 - Humidity monitoring in concrete using Bluetooth Low Energy sensors N2 - The vulnerability of low quality concrete to changing weather conditions is well known. The constant exposure to temperature changes, biological activity, and humidity ends up in damage to buildings and structures which contain this material. It is therefore necessary to take preventive measures to control the extent of the damage done by weathering and possible penetration of adverse chemicals into structures which need public safety. The Federal Institute for Materials Research and Testing (BAM), in cooperation with the small enterprise LinTech GmbH, is working on a project to monitor humidity changes in concrete by analyzing the changes in signal strength (RSSI) from Bluetooth Low Energy sensors. In this paper, we show results which demonstrate the influence of changing water content in concrete on the received RSSI. We observed that as water content in concrete decreases, the received RSSI improves. However, the damping effect is not linearly proportional to water content, rather exponentially proportional. This suggests that changes in the received signal strength are more easily observed when water content in concrete is higher. Finally, we reconstructed a RSSI distribution map using computed tomography. T2 - SMAR 2017 CY - Zurich, Switzerland DA - 13.09.2017 KW - Bluetooth Low Energy Computed Tomography KW - RSSI KW - Concrete KW - Water KW - Monitoring KW - Computed Tomography PY - 2017 UR - http://www.smar-conferences.org/smar/SMAR_2017_Proceedings/papers/153.pdf VL - 2017 SP - 1 EP - 8 CY - Zurich, Switzerland AN - OPUS4-43597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moraleja, I. A1 - Mena, M. L. A1 - Lázaro, A. A1 - Neumann, B. A1 - Tejedor, A. A1 - Jakubowski, Norbert A1 - Gómez-Gómez, M. M. A1 - Esteban-Fernández, D. T1 - An approach for quantification of platinum distribution in tissues by LA-ICP-MS imaging using isotope dilution analysis N2 - Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been revealed as a convenient technique for trace elemental imaging in tissue sections, providing elemental 2D distribution at a quantitative level. For quantification purposes, in the last years several approaches have been proposed in the literature such as the use of CRMs or matrix matched standards. The use of Isotope Dilution (ID) for quantification by LA-ICP-MS has been also described, being mainly useful for bulk analysis but not feasible for spatial measurements so far. In this work, a quantification method based on ID analysis was developed by printing isotope-enriched inks onto kidney slices from rats treated with antitumoral Pt-based drugs using a commercial ink-jet device, in order to perform an elemental quantification in different areas from bio-images. For the ID experiments ¹⁹⁴Pt enriched platinum was used. The methodology was validated by deposition of natural Pt standard droplets with a known amount of Pt onto the surface of a control tissue, where could be quantified even 50 pg of Pt, with recoveries higher than 90%. The amount of Pt present in the whole kidney slices was quantified for cisplatin, carboplatin and oxaliplatin-treated rats. The results obtained were in accordance with those previously reported. The amount of Pt distributed between the medullar and cortical areas was also quantified, observing different behavior for the three drugs. KW - Isotopic dilution KW - LA-ICP-MS KW - Quantification KW - Imaging KW - Kidney KW - Pt-based drugs PY - 2018 DO - https://doi.org/10.1016/j.talanta.2017.09.031 SN - 0039-9140 VL - 178 SP - 166 EP - 171 PB - Elsevier AN - OPUS4-43627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grötzsch, D. A1 - Streeck, C. A1 - Nietzold, Carolin A1 - Malzer, W. A1 - Mantouvalou, I. A1 - Nutsch, A. A1 - Dietrich, Paul A1 - Unger, Wolfgang A1 - Beckhoff, B. A1 - Kanngießer, B. T1 - A sealable ultrathin window sample cell for the study of liquids by means of soft X-ray spectroscopy N2 - A new sample cell concept for the analysis of liquids or solid-liquid interfaces using soft X-ray spectroscopy is presented, which enables the complete sealing of the cell as well as the Transport into vacuum via, for example, a load-lock system. The cell uses pressure monitoring and active as well as passive pressure regulation systems, thereby facilitating the full control over the pressure during filling, sealing, evacuation, and measurement. The cell design and sample preparation as well as the crucial sealing procedure are explained in detail. As a first proof-of-principle experiment, successful nitrogen K-edge fluorescence yield near-edge X-ray absorption fine structure experiments of a biomolecular solution are presented. For this purpose, it is shown that the careful evaluation of all involved parameters, such as window type or photon flux, is desirable for optimizing the experimental result. KW - X-ray spectroscopy KW - Analysis of liquids KW - Wet cell KW - Concanavalin A KW - NEXAFS PY - 2017 DO - https://doi.org/10.1063/1.5006122 SN - 0034-6748 SN - 1089-7623 VL - 88 IS - 12 SP - 123112-1 EP - 123112-7 PB - American Institute of Physics AN - OPUS4-43611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas T1 - NEXAFS and XPS investigations of a dual switchable rotaxane multilayer N2 - A multilayer consisting of two different rotaxanes was investigated with different analytical methods. The rotaxanes can be switched with two different stimuli - chemical and photochemical. XPS indicates that our layer-by-layer approach worked and a layer growth with every deposition step is present. NEXAFS showed that both stimuli cause an increase of the multilayer's preferential orientation. T2 - BESSY User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - NEXAFS KW - XPS KW - Rotaxanes PY - 2017 AN - OPUS4-43616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hofmann, D. A1 - Rahammer, M. A1 - Liewald, M. A1 - Heckel, Thomas A1 - Huppmann, M. T1 - Vergleich von zerstörungsfreien und zerstörenden Prüfungen dünner Strukturklebungen in der Umformtechnik T1 - Comparison of non destructive and destructive tests of thin structural bonds in the forming technology N2 - Der vorliegende Fachartikel stellt die wichtigsten zerstörungsfreien Prüfmethoden zur Qualitätssicherung von dünnen Strukturklebungen vor. Auf diese Weise wird ersichtlich, welche Methoden neben der zerstörenden Prüfung von dünnen Strukturklebungen eingesetzt werden können, um einen Haftfestigkeitsverlust zu detektieren. Steigende Leichtbau- und Dämpfungsanforderungen an großflächige Blechbauteile sorgen trotz erhöhter Kosten für einen zunehmenden Einsatz von modernen hybriden Schichtverbundwerkstoffen in zahlreichen Konstruktionsanwendungen. In der Luft- und Raumfahrtindustrie gehören solche Werkstoffe seit geraumer Zeit zum aktuellen Stand der Technik, wohingegen diese Werkstoffkonzepte in der mobilen Großserie derzeit nur selten zum Einsatz kommen. Neben dem Materialversagen der einzelnen Schichten von Schichtverbundwerkstoffen spielt das interlaminare Versagen der Schichten untereinander eine entscheidende Rolle. In der Umformtechnik ist es möglich, dass die polymere Zwischenschicht und das Deckblech nach der Umformung noch in Kontakt stehen, obwohl die Scherfestigkeit bereits überschritten wurde. Dieser Kraftschluss der beiden Fügepartner resultiert aus den schwachen Van-der-Waals-Kräften, die eine eindeutige Detektion mit Hilfe von zerstörungsfreier Prüfung erschweren. Die vorliegende Publikation soll die Eignung diverser zerstörungsfreier Prüfverfahren auf die Detektion von sogenannten „kissing bonds“ (schwaches Anhaften der Schichten nach Versagen der Verbindung) überprüfen. KW - Zerstörungsfreie Prüfung KW - Zerstörende Prüfung KW - Klebeverbindungen KW - Umformtechnik PY - 2016 DO - https://doi.org/10.3139/120.110949 SN - 0025-5300 VL - 58 IS - 11-12 SP - 975 EP - 981 PB - Carl Hanser Verlag GmbH & Co. KG CY - München AN - OPUS4-43620 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Boehm, Rainer A1 - Heckel, Thomas A1 - Spruch, W. A1 - Beggerow, T. T1 - Ultrasonic Phased Array Design Study for High Speed Axle Inspection using an Electronically Rotating Beam N2 - For in-service inspections on wheelset axles with a hollow drilling, mechanized ultrasound inspection systems with single element probes are typically used. The ultrasonic testing in the zones close to the external surface of the railway axles can be realized from the inside of the bore hole, without demounting the wheelset and without dismantling the wheels and the brake discs. The testing system must be able to find flaws in the external surface of the hollow shafts, whose surface lies in the radial-radial plane, these are called transversal flaw. Presently testing systems are used, where scanning is realized in the circumferential direction by mechanical rotation of the probe system in the actual drilling. The phased array probe system, which is presented here, can carry out the rotation scan electronically. The scan can be carried out by simply moving the system forward and backwards through the drilling without mechanical rotation. Manipulation becomes simpler and the inspection time can be shortened considerably. The ultrasonic beam can be inclined exactly and be focused in the plane vertical to the specimen axis. The probe is designed with help of indispensable simulations using especially designed software developed by BAM. The feasibility and the alignment between the simulated and experimental results were shown in earlier projects reported by Boehm et al. (2006) and Völz et al. (2012). The main task here is to optimize a probe for bore holes with a diameter of 65 mm with an increase in sensitivity and a high spatial resolution. This development will be carried out by use of extensive simulations and result in certain changes of the relevant probe parameters. KW - Phased Array KW - Ultrasound KW - Axle inspection PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-436230 DO - https://doi.org/10.1016/j.prostr.2017.07.001 VL - 2017 IS - 4 SP - 71 EP - 78 PB - Elsevier B.V. AN - OPUS4-43623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kowarik, Stefan T1 - Fiber Optic sensing @BAM N2 - I will discuss fiber optic sensing principles at BAM. Overlapping areas of interes between our group and the Institut für Angewandte Photonik will be discussed. T2 - Eingeladener Vortrag am Institut für Angewandte Photonik Adlershof CY - Adlershof, Berlin, Germany DA - 19.11.2017 KW - Faseroptische Sensorik KW - Fiber optic sensing KW - X-ray optics PY - 2017 AN - OPUS4-43587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - New insights in formation pathways: in situ investigations of mechanochemical reactions N2 - Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals.1 The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms.2,3 We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In this contribution, I will discuss our recent results investigating the formation of (polymorphic) cocrystals and metal phosphonates.4 First investigations of a mechanochemical synthesis under controlled temperature which allow determining the activation barrier are presented. Furthermore, in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat.5 Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds. T2 - International Conference on Mechanochemistry and Mechanical Alloying, INCOME 2017 CY - Kosice, Slovakia DA - 03.09.2017 KW - Mechanochemistry KW - In situ PY - 2017 AN - OPUS4-43564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical reactions N2 - Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals.1,2 The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms.3,4 We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy (Fig.1a) The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In this talk I will discuss our recent results investigating the formation of (polymorphic) cocrystals.6-7 First investigations of a mechanochemical synthesis under controlled temperature (Fig 2a) which allow determining the activation barrier are presented.8 Furthermore, in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat. T2 - Kolloquium Anorganische und Analytische Chemie Universität Freiburg CY - Freiburg, Germany DA - 20.12.2017 KW - In situ KW - Mechanochemistry KW - Rietveld PY - 2017 AN - OPUS4-43566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical syntheses: New insights in formation pathways N2 - Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals.1,2 The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms.3,4 We recently introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy (Fig.1a) The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. In this talk I will discuss our recent results investigating the formation of (polymorphic) cocrystals. T2 - CF@Bo2017 Crystal Forms Bologna 2017 CY - Bologna, Italy DA - 04.06.2017 KW - Mechanochemistry PY - 2017 AN - OPUS4-43567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Adão, Filipe Jorge Santos Ferreira T1 - Humidity monitoring in concrete using Bluetooth Low Energy sensors N2 - The vulnerability of low quality concrete to changing weather conditions is well known. The constant exposure to temperature changes, biological activity, and humidity ends up in damage to buildings and structures which contain this material. It is therefore necessary to take preventive measures to control the extent of the damage done by weathering and possible penetration of adverse chemicals into structures which need public safety. The Federal Institute for Materials Research and Testing (BAM), in cooperation with the small enterprise LinTech GmbH, is working on a project to monitor humidity changes in concrete by analyzing the changes in signal strength (RSSI) from Bluetooth Low Energy sensors. In this paper, we show results which demonstrate the influence of changing water content in concrete on the received RSSI. We observed that as water content in concrete decreases, the received RSSI improves. However, the damping effect is not linearly proportional to water content, rather exponentially proportional. This suggests that changes in the received signal strength are more easily observed when water content in concrete is higher. Finally, we reconstructed a RSSI distribution map using computed tomography T2 - SMAR 2017 CY - Zurich, Switzerland DA - 13.09.2017 KW - RSSI KW - Concrete KW - Water KW - Monitoring KW - Computed Tomography PY - 2017 AN - OPUS4-43599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guerra, M. F. A1 - Fischer, M. A1 - Radtke, Martin A1 - Reinholz, Uwe T1 - Inca figurines from the Ethnologisches Museum in Berlin: an analytical study of some typical and atypical productions N2 - Fourteen hollow and one cast anthropomorphic and zoomorphic figurines produced in Incan times for ritual offerings from the Ethnologisches Museum in Berlin were selected to investigate the technologies and alloys used for their fabrication with portable optical microscopy and non-destructive XRF elemental analysis. This group of gold and silver figurines includes typical specimens of the Inca production, such as the four silver figurines from the Island Coati in Lake Titicaca and the two gold figurines from Pachacamac, as well as specimens that are seldom present in collections, which makes them atypical. In addition to the tall figurines with atypical hair or standing pose, one bicolour figurine half silver, half gold) and another with coloured inlays were included in this study for comparison. The large majority of the silver specimens are made from very high quality alloys and the gold figurines are made from alloys containing low copper contents and silver ranging from 30wt% to 52wt%. KW - Gold KW - pXRF KW - Inca PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-436015 DO - https://doi.org/10.4000/bifea.8232 SN - 0303-7495 VL - 46 IS - 1 SP - 221 EP - 251 PB - Institut Français d'Études Andines AN - OPUS4-43601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Zerstörungsfreie Prüfung von Komposit-Druckbehältern und ferromagnetischen Kunststoffen unter Verwendung von Wirbelstromprüfgeräten N2 - Metallische Druckgefäße werden aus Gründen der Gewichtseinsparung zunehmend durch Composite-Druckgefäße ersetzt. Während der Alterungsprozess bei metallischen Druckgefäßen durch Wöhlerkurven hinreichend beschrieben wird, ist der Alterungsmechanismus bei Composite-Druckgefäßen noch nicht vollständig geklärt. Im Rahmen des BAM-interne Themenfeldprojekts COD-AGE werden mit diversen Verfahren alterungsbegleitende, zerstörungsfreie Prüfungen an Composite-Druckgefäßen durchgeführt. Im ersten Teil dieses Vortrages werden Ergebnisse der konventionellen und hochfrequenten Wirbelstromprüfung vorgestellt. Der zweite Teil des Vortrages beschäftigt sich mit der Prüfbarkeit von Kunststoffen aus Kunstharz und 3D-Druck mit dem Wirbelstromverfahren durch Zugabe ferromagnetischer Nanopartikel bzw. Verwendung von ferromagnetischem Filament. T2 - DGZfP Arbeitskreis Berlin CY - Berlin, Germany DA - 03.01.2018 KW - Wirbelstromprüfung KW - Druckbehälter KW - CFK KW - Ferromagnetischer Kunststoff KW - COD-AGE PY - 2018 AN - OPUS4-43700 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saloga, Patrick E. J. A1 - Kästner, Claudia A1 - Thünemann, Andreas T1 - High-speed but not magic: Microwave-assisted synthesis of ultra-small silver nanoparticles N2 - Reaction procedures have been improved to achieve higher yields and shorter reaction times: one possibility is the usage of microwave reactors. In the literature, this is under discussion, for example, nonthermal effects resulting from the microwave radiation are claimed. Especially for the synthesis of nanomaterials, it is of crucial importance to be aware of influences on the reaction pathway. Therefore, we compare the syntheses of ultra-small silver nanoparticles via conventional and microwave heating. We employed a versatile one-pot polyol synthesis of poly(acrylic acid)-stabilized silver nanoparticles, which display superior catalytic properties. No microwave-specific effects in terms of particle size distribution characteristics, as derived by small-angle X-ray scattering and dynamic light scattering, are revealed. Because of the characteristics of a closed system, microwave reactors give access to elevated temperatures and pressures. Therefore, the speed of particle formation can be increased by a factor of 30 when the reaction temperature is increased from 200 to 250 °C. The particle growth process follows a cluster coalescence mechanism. A postsynthetic incubation step at 250 °C induces a further growth of the particles while the size distribution broadens. Thus, utilization of microwave reactors enables an enormous decrease of the reaction time as well as the opportunity of tuning the particle size. Possibly, decomposition of the stabilizing ligand at elevated temperatures results in reduced yields. A compromise between short reaction times and high yields can be found at a temperature of 250 °C and a corresponding reaction time of 30 s. KW - Silver nanoparticles KW - SAXS KW - Small-angle X-ray scattering KW - Microwave synthesis PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-437028 DO - https://doi.org/10.1021/acs.langmuir.7b01541 SN - 0743-7463 SN - 1520-5827 VL - 34 IS - 1 SP - 147 EP - 153 PB - American Chemical Society CY - Washington, D.C. AN - OPUS4-43702 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Elektronenstrahl-Mikroanalyse (ESMA) an heterogenen Proben N2 - Grundkenntnisse zum besseren Verständnis der Funktionsweise der Elektronenstrahl-Mikroanalyse (ESMA) werden präsentiert und anhand Beispielen diskutiert. Das physikalische Messprinzip von ESMA am REM, das Wechselwirkungs- und Informationsvolum und die Anregung der charakteristischen Röntgenlinien werden erklärt. Verschiedene potentielle Artefakte, wie z.B. Heterogenität der Probenzusammensetzung, Oberflächenbeschaffenheit der Probe und Linienüberlagerung werden eingeführt. Die physikalischen Grenzen der analytischen Methode werden spezifiziert. T2 - Industrietreffen im Forschungs- und Innovationszentrum (FIZ) der BMW Group CY - Munich, Germany DA - 09.01.2018 KW - ESMA KW - REM KW - Elementzusammensetzung KW - REM/EDX PY - 2018 AN - OPUS4-43708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Seuthe, T. A1 - Grehn, M. A1 - Eberstein, M. A1 - Rosenfeld, A. A1 - Mermillod-Blondin, A. T1 - Time-resolved microscopy of fs-laser-induced heat flows in glasses N2 - Time-resolved phase-contrast microscopy is employed to visualize spatio-temporal thermal transients induced by tight focusing of a single Ti:sapphire fs-laser pulse into a solid dielectric sample. This method relies on the coupling of the refractive index change and the sample temperature through the thermo-optic coefficient dn/dT. The thermal transients are studied on a timescale ranging from 10 ns up to 0.1 ms after laser excitation. Beyond providing direct insights into the laser–matter interaction, analyzing the results obtained also enables quantifying the local thermal diffusivity of the sample on a micrometer scale. Studies conducted in different solid dielectrics, namely amorphous fused silica (a-SiO2), a commercial borosilicate glass (BO33, Schott), and a custom alkaline earth silicate glass (NaSi66), illustrate the applicability of this approach to the investigation of various glassy materials. KW - Femtosecond laser KW - Phase-contrast microscopy KW - Heat diffusion KW - Glasses PY - 2018 DO - https://doi.org/10.1007/s00339-017-1465-5 SN - 0947-8396 SN - 1432-0630 VL - 124 IS - 1 SP - 60, 1 EP - 6 PB - Springer-Verlag AN - OPUS4-43739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Khosravi, Z. A1 - Kotula, S. A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Klages, C.-P. T1 - IR- and NEXAFS-spectroscopic characterization of plasma-nitrogenated polyolefin surfaces N2 - Modification of polyethylene and polypropylene surfaces by atmospheric-pressure plasmas using mixtures of nitrogen and hydrogen was studied using Fouriertransform infrared spectroscopy in the attenuated total reflection mode (FTIR-ATR) and by near-edge x-ray absorption fine structure spectroscopy (NEXAFS) in order to shed some light on the chemical nature of nitrogen-containing functional Groups on the polymer surface. Using FTIR-ATR spectroscopy combined with hydrogendeuterium isotope exchange of active hydrogen atoms, it was shown that the direct treatment of PE foils by dielectric barrier discharges (DBDs) in N2/H2 mixtures and a subsequent exposure of the samples to the ambient air results in the formation of –NH2 moieties of primary amides on the polymer surface. Corresponding in situ experiments with streaming N2/H2 DBD post-discharges virtually free of H2O and O2, on the other hand, showing the absence of –NH2, proving that no primary amines or amides are formed by this treatment although substantial amounts of nitrogen are incorporated. Moreover, directly N2/H2-plasma-treated polymer surfaces, similar to afterglow-treated low-density polyethylene (LDPE), show amphiphilic character as to be seen by chemical derivatization with nucleophilic reagents 4-(trifluoromethyl) phenylhydrazine and 4-(trifluoromethyl)benzylamine, in addition to electrophilic aromatic aldehydes normally used to derivatize such surfaces. The presence of imines or other functional groups with CN moieties which may be invoked to explain the dual (amphiphilic) reactivity is proven by NEXAFS studies on ultrathin plasma-treated PE films, confirming significant amounts of nitrogen in CN bonds and carbon in CC bonds. KW - X-ray spectroscopy KW - IR spectroscopy KW - Plasma-nitrogenated polyolefin surfaces KW - Unsaturated CN bonds KW - NEXAFS PY - 2017 DO - https://doi.org/10.1002/ppap.201700066 SN - 1612-8869 SN - 1612-8850 VL - 15 IS - 1 SP - e1700066, 1 EP - 15 PB - WILEY-VCH Verlag GmbH & Co. KGaA, CY - Weinheim AN - OPUS4-43786 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koegler, M. A1 - Paul, Andrea A1 - Anane, E. A1 - Birkholz, M. A1 - Bunker, A. A1 - Viitala, T. A1 - Maiwald, Michael A1 - Junne, S. A1 - Neubauer, P. T1 - Comparison of time-gated surface-enhanced Raman spectroscopy (TG-SERS) and classical SERS based monitoring of Escherichia coli cultivation samples N2 - The application of Raman spectroscopy as a monitoring technique for bioprocesses is severely limited by a large background signal originating from fluorescing compounds in the culture media. Here, we compare time-gated Raman (TG-Raman)-, continuous wave NIRprocess Raman (NIR-Raman), and continuous wave micro-Raman (micro-Raman) approaches in combination with surface enhanced Raman spectroscopy (SERS) for their potential to overcome this limit. For that purpose, we monitored metabolite concentrations of Escherichia coli bioreactor cultivations in cell-free supernatant samples. We investigated concentration transients of glucose, acetate, AMP, and cAMP at alternating substrate availability, from deficiency to excess. Raman and SERS signals were compared to off-line metabolite analysis of carbohydrates, carboxylic acids, and nucleotides. Results demonstrate that SERS, in almost all cases, led to a higher number of identifiable signals and better resolved spectra. Spectra derived from the TG-Raman were comparable to those of micro-Raman resulting in well-discernable Raman peaks, which allowed for the identification of a higher number of compounds. In contrast, NIR-Raman provided a superior performance for the quantitative evaluation of analytes, both with and without SERS nanoparticles when using multivariate data analysis. KW - Time-gated Raman (TG-Raman) KW - Surface-enhanced Raman spectroscopy (SERS) KW - Multivariate data analysis KW - Metabolite quantification KW - Escherichia coli PY - 2018 DO - https://doi.org/10.1002/btpr.2665 SN - 1520-6033 SN - 8756-7938 VL - 34 IS - 6 SP - 1533 EP - 1542 PB - Wiley AN - OPUS4-45831 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Growth kinetics and molecular mobility of irreversibly adsorbed layers in thin polymer films N2 - In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is expected to from. These adsorbed layers have shown greate potential for technological applications. However, their growth kinetics and molecular dynamics are still not fully understood. This is partly due to the hard accessibility of these layers in thin films. Here, the irreversibly adsorbed layers of homopolymer thin films are revealed by solvent-leaching experiments. First, the growth kinetics of these layers is investigated as a function of annealing time, annealing temperature, leaching time and the original filme thickness. The film thickness, topography and the quality of the adsorbed layer is controlled by Atomic Force Microscopy (AFM). Secondly, the molecular mobility of the adsorbed layer is investigated by Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor arrangement is employed to measure the layer with a free surface. The results are quantitatively compared and discussed with respect to recently published work. T2 - 10th Conference on Broadband Dielectric Spectroscopy and its Applications CY - Brussles, Belgium DA - 26.08.2018 KW - Thin polymer films PY - 2018 AN - OPUS4-45837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Tiebe, Carlo T1 - Two tasks in environmental monitoring - calibration and characterization of gas sensors and remote gas sensing with multicopter platforms - Part 1 N2 - Leaking methane from infrastructures, such as pipelines and landfills, is critical for the environment but can also pose a safety risk. To enable a fast detection and localization of these kind of leaks, BAM developed a novel robotic platform for aerial remote gas sensing. Spectroscopic measurement methods for remote sensing of selected gases lend themselves for use on mini-copters, which offer a number of advantages for inspection and surveillance over traditional methods. No direct contact with the target gas is needed and thus the influence of the copter downwash on the measured gas plume can be kept to a minimum. This allows to overcome one of the major issues with gas-sensitive mini-copters. On the other hand, remote gas sensors, most prominently Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensors have been too bulky given the payload and energy restrictions of mini-copters. Here, we present the Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), which combines a novel lightweight TDLAS sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile multicopter. The proposed system can be deployed in scenarios that cannot be addressed by currently available systems and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO). It enables tomographic reconstruction of gas plumes and a localization of gas sources. We also present first results showing its performance under realistic conditions. T2 - Aarhus University, Department of Environmental Science, External seminar with Matthias Bartholmai and Carlo Tiebe CY - Roskilde, Denmark DA - 29.08.2018 KW - Environmental monitoring KW - Remote gas sensing KW - Flying platforms KW - Mobile robot olfaction KW - UAS PY - 2018 AN - OPUS4-45838 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - van Wasen, Sebastian T1 - Airborne laser-spark ion source for direct microfluidic coupling N2 - The development and improvement of new ionization techniques for mass spectrometry often requires dedicated, specific sampling approaches. Recently, a novel ionization scheme for ambient MS has been introduced based on a quasi-continuous laser-induced plasma, which was ignited directly before the MS inlet. This setup combines the general advantages of ambient ionization, provides electro neutrality, sufficient duty cycle and a ubiquitous plasma medium. A high repetition rate DPSS laser (Conqueror 3-LAMBDA, Nd:YVO4, 1 - 500 kHz, average output power: 12 W at 50 kHz, Compact Laser Solutions GmbH, Germany) and the corresponding optomechanical system were installed on an optical breadboard above the inlet of a LCQ DecaXP ion trap mass spectrometer. The quasi-continuous airborne plasma was ignited inside the sprayed sample in front of the inlet via focused laser irradiation. The introduction of liquid samples into laser-induced plasmas requires higher plasma power during solvent evaporation as compared to gaseous samples. This increased demand was approached via a two-fold strategy: Firstly, an alternative, more powerful, laser plasma driven by the fundamental instead of the second harmonic wavelength was implemented, which provided a 10-fold increase of signal intensity, while maintaining the same reagent ion pattern as the previous plasma. Protonated water clusters [(H2O]nH]+, NH4+ as well as charge transfer promoting ion O2+, dominated the reagent ion mass spectrum. Secondly, a miniaturized nebulizer was used to minimize the size of the plasma quenching solvent droplets. The result of these improvements was a new and very stable ion source for direct microfluidic coupling. A variety of samples demonstrated the performance of the ion source. A laser-driven plasma was shown to be a powerful ion source for gaseous and solid samples. For the first time, liquid samples were examined using the novel source. In addition to demonstrating an improved strategy for igniting the laser plasma, this contribution also covers the miniaturization of the spray source for enhanced ionization, while minimizing sample consumption via a microfluidic spray systems. T2 - International Mass Spectrometry Conference 2018 CY - Florence, Italy DA - 26.08.2018 KW - Airborne KW - Laser-spark KW - Laser-induced plasma KW - Microfluidic KW - Mass Spectrometry PY - 2018 AN - OPUS4-45839 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Breitfeld, Steffen A1 - Scholz, G. A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - BaF-benzenedicarboxylate: the first mechanochemical N2 - Anewbariumcoordination polymer, BaF-benzenedicarboxylate (BaF(p-BDC)0.5), with fluorine directly coordinated to the metal cation, was prepared by mechanochemical synthesis routes. Phase-pure BaF-benzenedicarboxylate was synthesized by milling starting either from barium hydroxide or from Barium acetate as sources for barium cations. In both cases, the second reactant was 1,4-benzenedicarboxylic acid (H2(p-BDC)). Ammonium fluoride was used as fluorinating agent directly at milling. This is the first mechanochemical synthesis of coordination polymers where fluorine is directly coordinated to the metal cation. Following the second possibility, barium acetate fluoride (Ba(OAc)F) is formed as ntermediate product after milling, and the new coordination polymer is accessible only after washing with water and dimethyl sulfoxide. The new compound BaF(p-BDC)0.5 was characterized by X-ray powder diffraction, FTIR-, and 19F, 1H-13C CP MAS NMR spectroscopies, DTA-TG, and elemental Analysis. KW - Milling KW - MOF PY - 2018 DO - https://doi.org/10.1007/s10853-018-2331-3 SN - 0022-2461 VL - 53 IS - 19 SP - 13682 EP - 13689 PB - Springer AN - OPUS4-45677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Haferkamp, Sebastian A1 - Kraus, Werner T1 - Studies on the mechanochemical Knoevenagel condensation of fluorinated benzaldehyde derivates N2 - The mechanochemical Knoevenagel condensation of three fluorinated benzaldehyde derivates and malononitrile was investigated. The reactions were performed under solvent- and catalyst-free conditions and resulted in highly crystalline products after crystallization from a viscous phase in the milling jar. The quality of the obtained crystals was sufficient for single-crystal X-ray diffraction circumventing a recrystallization step. To gain more information on the reaction, progress was investigated in situ using time-resolved Raman spectroscopy. The results show a direct conversion of the reactants. KW - C-C coupling KW - Knoevenagel condensation KW - In situ KW - Mechanochemistry PY - 2018 DO - https://doi.org/10.1007/s10853-018-2492-0 SN - 0022-2461 VL - 53 IS - 19 SP - 13713 EP - 13718 PB - Springer Link AN - OPUS4-45682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fernández, L. A1 - Lin, Z. A1 - Schneider, Rudolf A1 - Esteves, V. I. A1 - Cunha, Â. A1 - Tomé, J. P. C. T1 - Antimicrobial Photodynamic Activity of Cationic Nanoparticles Decorated with Glycosylated Photosensitizers for Water Disinfection N2 - The antimicrobial photodynamic approach has been demonstrated as an efficient and sustainable process for the eradication of microbial pathogens. In this work, silica-coated Magnetite nanoparticles (NPs) were used as carriers of glycosylated porphyrins and phthalocyanines. Their subsequent cationization resulted in the production of stable antimicrobial photosensitizing materials, effective against E. coli. Suspensions of the photocatalysts in water present bimodal size distributions formed by big clusters and small NPs with hydrodynamic diameters between 8 and 38 nm. The presence of small NPs in the suspensions is related to an effective photodynamic inactivation (PDI) of E. coli cells. Glycosylation of the PS showed a positive effect on the PDI performance, which could be related to a higher accumulation of the photocatalyst over the bacterial cell membrane. In addition, these biocidal agents proved to be photostable and their photoactive performance decreased only between 23% and 28% upon 5 PDI cycles, mostly because of the loss of material between cycles, which makes them promising materials for water disinfection purposes. KW - Photodynamische Inaktivierung KW - E. coli KW - Photokatalyse KW - Bakterien KW - Nanopartikel KW - Photosensibilisator KW - Porphyrin KW - Phthalocyanin PY - 2018 DO - https://doi.org/10.1002/cptc.201700169 SN - 2367-0932 VL - 2 IS - 7 SP - 596 EP - 605 PB - Wiley VHC CY - Weinheim AN - OPUS4-45684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona ED - Jakobs, K. ED - O'Connor, R.V. T1 - The Role of Conformity Assessment in the Digital Transformation: Focusing on Cybersecurity N2 - Digital transformation and especially the dramatic rise of products and services connected to the Internet of Things raise the questions on how to deal with the increasing risks related to Privacy and Cybersecurity. Presumably, these risks seem to be insufficiently reflected in the European Union’s current regulative system – by being neither part of the traditional definition of a safe product nor part of product-specific vertical or horizontal directives. Certification based on standards as underlying requirements has been identified by policymakers as an instrument to address this issue. The latest European draft regulation aims at increasing security and trust in ICT products and services, and reducing current European market fragmentation with a new Cybersecurity Certification Framework. Based on the results of a qualitative analysis of stakeholder statements on the current proposal on the Cybersecurity Act, this paper discusses elements of the proposed Cybersecurity Certification Framework. As a theoretical background, this paper provides definitions of the terms Safety, IT-security, and Cybersecurity, presents selected Cybersecurity-related standards and provides an outlook on future challenges to Conformity Assessment in the digital transformation. T2 - 23rd EURAS Annual Standardisation Conference "Standards for a Smarter Future" CY - Dublin, Irland DA - 13.06.2018 KW - Conformity Assessment KW - Cybersecurity KW - Certification KW - IT-Security PY - 2018 SN - 978-3-95886-229-6 VL - 2018 SP - 183 EP - 202 PB - Verlagshaus Mainz GmbH Aachen CY - Aachen AN - OPUS4-45686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Timofeev, Juri T1 - Gesteuerte Risserzeugung in Stahlbeton zur Qualifizierung von ZfPBau-Anwendungen N2 - Die Zerstörungsfreie Prüfung im Bauwesen (ZfPBau) liefert ergänzende Informationen für die Planung von Ertüchtigungsmaßnahmen an Bauwerken. Die ZfPBau bzw. die Prüflösungen müssen zur Validierung an bestimmten Vergleichskörpern untereinander verglichen werden. Risse in Stahlbeton sind nicht notwendigerweise ein Schaden, in DIN EN 1992-1-1 werden etwa nur Risse mit einer Rissbreite größer 0,2 mm erfasst. Risse können aber ein Hinweis auf statische Probleme sein oder einen Schadensprozess fördern, etwa die Depassivierung der Bewehrung durch die beschleunigte Diffusion von Kohlendioxid. Deshalb ist die Bestimmung der Risstiefe und des Rissverlaufs für die Dauerhaftigkeitsabschätzung eines Bauwerks von Interesse. Die Vergleichbarkeit von ZfPBau-Verfahren zur Charakterisierung von Rissen in Stahlbeton hängt wesentlich davon ab, dass die untersuchten Risse ein vergleichbares Prüfproblem darstellen. Risse in Stahlbeton werden charakterisiert durch die Rissbreite, die Risstiefe, den Rissverlauf und die Lage bzw. Orientierung zur Oberfläche. Es muss wegen der Vielzahl von Schadensbildern eine Prioritätensetzung und Fokussierung auf besonders praxisrelevante Fälle vorgenommen werden. Dazu zählen z.B. bewehrungskreuzende und oberflächenoffene Risse, die für die Tragfähigkeit einer Konstruktion relevant sein können. Eine ausgewählte Prüfaufgabe ist dann die Detektion von Rissen senkrecht zur Oberfläche und die Bestimmung der Risstiefe. Der Sprengmörtel „Betonamit“, dessen Wirkung auf seiner extremen Expansionsfähigkeit beruht, wird zur Risserzeugung in gezielt angeordnete Bohrlöcher gefüllt. Wichtig bei der Erzeugung von Rissen ist die Bohrlochparametervariation zur gezielten Risssteuerung. Es werden der Durchmesser, die Tiefe, die Füllhöhe und die Anordnung der Fülllöcher variiert. Die Risse entstehen im Wesentlichen in Abhängigkeit vom Volumen des eingefüllten Sprengmittels. Der Nachweis der Risstiefen erfolgte zerstörend, d.h. durch Sägen des Vergleichskörpers und Ausmessen der Risse. Das Poster stellt die Arbeitsschritte, die erzeugten Risse und die statistische Auswertung dar. Ein Vergleichsversuch mit internationaler Beteiligung hat begonnen mit der Zielsetzung die Risserzeugung in unterschiedlichen Umgebungen zu vergleichen. T2 - Bauwerksdiagnose 2018 CY - Berlin, Germany DA - 15.02.2018 KW - Zerstörungsfreie Prüfung von Stahlbeton KW - Risse KW - Vergleichskörper PY - 2018 UR - https://www.bauwerksdiagnose2018.de/Portals/bauwerksdiagnose2018/P/p8.pdf AN - OPUS4-45738 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schürmann, Robin A1 - Vogel, Stefanie A1 - Ebel, Kenny A1 - Bald, Ilko T1 - The physico-chemical basis of DNA radiosensitization: Implications for cancer radiation therapy N2 - High-energy radiation is used in combination with radiosensitizing therapeutics to treat cancer. The most common radiosensitizers are halogenatednucleo-sides and cisplatin derivatives, and recently also metal nanoparticles have been suggested as potentialradiosensitizing agents. The radiosensitizingaction of these compounds can at least partly be ascribed to an enhancedreactivity towards secondary low-energy electrons generated along the radiation track of the high-energyprimary radiation, or to an additional emission of secondary reactive electrons close to the tumor tissue. This is referred to as physico-chem ical radiosensitization. In this Conceptarticle we presentcurrent experimental methodsused to study fundamentalprocesses of physico-chemical radiosensitization and discuss the most relevant classes of radiosensitizers. Open questions in the current discussions are identified and future directions outlined, which can lead to optimized treatment protocols or even novel therapeuticconcepts. KW - DNA KW - Radiosensitization KW - Radiation damage KW - Low energy electrons PY - 2018 DO - https://doi.org/10.1002/chem.201800804 SN - 1521-3765 SN - 0947-6539 VL - 24 IS - 41 SP - 10271 EP - 10279 PB - WILEY AN - OPUS4-45742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heck, Christian A1 - Kanehira, Y. A1 - Kneipp, Janina A1 - Bald, Ilko T1 - Placement of single proteins within the SERS hot spots of self-assembled silver nanolenses N2 - This study demonstrates the bottom-up synthesis of silver nanolenses.Arobust coating protocol enabled the functionalization of differently sized silver nanoparticles with DNAsingle strands of orthogonal sequence.Coated particles 10 nm, 20 nm, and 60 nm in diameter were self-assembled by DNAorigami scaffolds to form silver nanolenses.Single molecules of the protein streptavidin were selectively placed in the gap of highest electric field enhancement. Streptavidin labelled with alkyne groups served as model analyte in surface- enhanced Raman scattering (SERS) experiments.Bycorre- lated Raman mapping and atomic force microscopy, SERS signals of the alkyne labels of asingle streptavidin molecule, from asingle silver nanolens,were detected. The discrete,self- similar aggregates of solid silver nanoparticles are promising for plasmonic applications. KW - DNA origami KW - Surface enhanced Raman scattering KW - Protein KW - Single molecule KW - Nanotechnology PY - 2018 DO - https://doi.org/10.1002/anie.201801748 SN - 1433-7851 VL - 57 IS - 25 SP - 7444 EP - 7447 PB - WILEY AN - OPUS4-45743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heck, Christian A1 - Kanehira, Yuya A1 - Kneipp, Janina A1 - Bald, Ilko T1 - Platzierung einzelner Proteine in den SERS-Hot-Spots selbstorganisierte Silbernanolinsen N2 - Diese Studie demonstriert die Bottom-up-Synthese von Silbernanolinsen. Ein robustes Beschichtungsprotokoll ermçglichte die Funktionalisierung unterschiedlich großer Silbernanopartikel mit einzelstr-ngiger DNAunterschiedlicher Sequenz. Derartig beschichtete Partikel mit Durchmessern von 10 nm, 20 nm und 60 nm wurden mithilfe von DNA-Origami- Gergsten zu Silbernanolinsen angeordnet. Ein einzelnes Mo- lekgldes Proteins Streptavidin ist in demjenigen Spalt zwi- schenden Partikeln immobilisiert worden, der die hçchste Feldverst-rkung zur Verfggung stellt. Streptavidin war dabei mit Alkin-Gruppen modifiziert und fungierte als Modellanalyt in Experimenten zur oberfl-chenverst-rkten Raman-Streuung (SERS). Korrelierte Raman- und Rasterkraftmikroskopie- Messungen ermçglichten die Aufnahme von SERS-Signalen der Alkingruppen eines einzelnen Streptavidins,von einer einzelnen Silbernanolinse.Diese diskreten, selbst-hnlichen Silbernanopartikelaggregate versprechen vielf-ltige Anwen- dungen im Feld der Plasmonik KW - DNA Origami KW - Oberflächen verstärkte Raman Streuung KW - Proteine KW - Einzelmolekülspektroskopie KW - Nanotechnologie PY - 2018 DO - https://doi.org/10.1002/ange.201801748 SN - 1521-3757 SN - 0044-8249 VL - 130 IS - 25 SP - 7566 EP - 7569 PB - WILEY AN - OPUS4-45744 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Size and shape distribution of bipyramidal TiO2 nanoparticles by TEM - An inter-laboratory comparison N2 - Extraction of true, 3D shape (and size) of non-spherical nanoparticles (NPs) is associated with errors by conventional 2D electron microscopy using projection images. Significant efforts within the ISO technical committee TC 229 ‘Nanotechnologies’ are aimed at establishing accurate TEM and SEM measurement of NP size and shape as robust, standard procedures. Study groups have been organizing inter-laboratory comparisons on well-selected NP systems according to the market needs, such as aggregated titania nano-powder for which size and shape distribution of primary crystallites of irregular shape must be measured accurately. To be noticed is e. g. the fact that the measurement procedure allows only manual selection of the particles clearly distinguishable for analysis as well as manual definition of the contour of the imaged NPs. An inter-laboratory exercise on titania NPs (pure anatase, grown by hydrothermal synthesis) of well-defined non-spherical shape, i.e. bipyramidal has been recently started within ISO/TC 229 under similar conditions as for the irregular shaped titania. Overlapped particles were allowed to be considered, as long as they are clearly distinguishable. One decisive NP selection criterion was to analyze only those NPs with a roundness value below 0.7, i.e. the NPs laying on the support foil and, hence, with projection areas clearly deviating from perfect circles (R=1). The overall evaluation (for 15 labs) of the size descriptors (area, Feret, minFeret, perimeter) and shape descriptors (aspect ratio, roundness, compactness, extent) by analysis of variance is just to be finished and included in ISO/WD 21363 Nanotechnologies -- Protocol for particle size distribution by transmission electron microscopy. T2 - Microscopy & Microanalysis 2018 CY - Baltimore, MD, USA DA - 05.08.2018 KW - Nanoparticles KW - Electron microscopy KW - ISO KW - Nanotechnology PY - 2018 AN - OPUS4-45750 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Check of the performance of EDS systems attached to the SEM with the test material EDS-TM001/2 and evaluation software package EDS spectrometer test -application, experiences and updates N2 - The test material EDS-TM001 together with an accompanying software package, “EDX spectrometer check”, have been made available in 2009 by BAM to be employed by EDS (energy dispersive spectrometer) users to check the performance of an EDS attached to the SEM. Particularly for test laboratories operating under accreditation schemes like ISO/IEC 17025, a periodical control of the critical instrumental parameters in end-user laboratories is required. With EDS-TM001 or EDS-TM002 (second generation) test material, this periodical check is simplified to the acquisition of only one 10 kV spectrum. The software “EDX spectrometer check” is destined to evaluate automatically this spectrum and determine the performance of the EDS in terms of energy resolution and calibration as well as possible alteration of low-energy efficiency due to detector contamination. Energy resolution can be compared with the specified values according to the international ISO standard ISO 15632:2012. EDS-TM is a synthetic material consisting of a thick layer of C, Al, Mn, Cu and Zr in a well-defined composition, deposited on a steel (in case of EDS-TM001) or silicon (in case of EDS-TM002) substrate. Meanwhile, more than one hundred laboratories use the EDS-TM001 or EDS-TM002 test material for the periodical check of their EDS. A detailed description of the test material and software together with examples of application was published recently. New results and gained experiences will be presented as well. When the FWHM of lines appearing in the EDS-TM spectrum are determined, the spectrum background must be subtracted accurately. The applied physical background subtraction procedure is robust and takes into account the transmission of the detector window. While the previous version considers only Moxtek AP windows, the new version includes selection of silicon nitride window and the case of windowless detector. Moreover, the new version allows importing of spectra in Bruker spx format and EMSA/MSA files from EDAX TEAM software. T2 - Microscopy & Microanalysis 2018 CY - Baltimore, MD, USA DA - 05.08.2018 KW - X-ray spectrometer KW - EDS KW - SEM KW - Performance check KW - Test material PY - 2018 AN - OPUS4-45751 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schaepe, Kaija A1 - R. Bhandari, D. A1 - Werner, J. A1 - Henss, A. A1 - Pirkl, A. A1 - Kleine-Boymann, M. A1 - Rohnke, M. A1 - Wenisch, S. A1 - Neumann, E. A1 - Janek, J. A1 - Spengler, B. T1 - Imaging of lipids in native human bone sections using TOF-secondary ion mass spectrometry, atmospheric pressure scanning microprobe matrix-assisted laser desorption/ionization orbitrap mass spectrometry, and orbitrap-secondary ion mass spectrometry N2 - A method is described for high-resolution label-free molecular imaging of human bone tissue. To preserve the lipid content and the heterogeneous structure of osseous tissue, 4 μm thick human bone sections were prepared via cryoembedding and tape-assisted cryosectioning, circumventing the application of organic solvents and a decalcification step. A protocol for comparative mass spectrometry imaging (MSI) on the same section was established for initial analysis with time-of-flight secondary ion mass spectrometry (TOF-SIMS) at a lateral resolution of 10 μm to <500 nm, followed by atmospheric pressure scanning microprobe matrix-assisted laser desorption/ionization (AP-SMALDI) Orbitrap MSI at a lateral resolution of 10 μm. This procedure ultimately enabled MSI of lipids, providing the lateral localization of major lipid classes such as glycero-, glycerophospho-, and sphingolipids. Additionally, the applicability of the recently emerged Orbitrap-TOF-SIMS hybrid system was exemplarily examined and compared to the before-mentioned MSI methods. KW - ToF-SIMS KW - MALDI KW - Mass spectrometry imaging KW - Lipids KW - Osteoporosis KW - Bone KW - Surface analysis PY - 2018 UR - https://pubs.acs.org/doi/10.1021/acs.analchem.8b00892 DO - https://doi.org/10.1021/acs.analchem.8b00892 SN - 0003-2700 SN - 1520-6882 VL - 90 IS - 15 SP - 8856 EP - 8864 PB - ACS Publ. CY - Washington, DC AN - OPUS4-45730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiggenhauser, Herbert A1 - Köpp, Christian A1 - Timofeev, Juri A1 - Azari, H. T1 - Controlled creating of cracks in concrete for non-destructive testing N2 - The non-destructive assessment of cracks in concrete is a common task for which non-destructive evaluation solutions have been published. Primarily, these tests have been carried out on artificial cracks that have been created by using notches instead of natural cracks. This study evaluates a procedure designed to create reproducible and controlled cracks in concrete. The procedure is based on using expanding mortar in a series of blind holes. This is done in combination with carefully aligned reinforcement to guide the direction of the crack development. The depth of the crack is also controlled by reinforcement. Crack depth varies statistically in the range of the Maximum aggregate size (16 mm) used for concrete. KW - Non-destructive testing of concrete KW - Cracks KW - Reference specimen PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-457367 UR - https://rdcu.be/4IPN DO - https://doi.org/10.1007/s10921-018-0517-x SN - 0195-9298 SN - 1573-4862 VL - 37 IS - 3 SP - 67, 1 EP - 9 PB - Springer CY - New York AN - OPUS4-45736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Liehr, Sascha ED - Peng, G.D. T1 - Polymer fiber sensors for structural and civil engineering applications N2 - This chapter gives an overview about polymer optical fiber (POF) sensors with the focus on structural and civil engineering applications. POF properties such as the high-strain range, the low Young’s modulus, and specific scattering effects open new fields for fiber-optic sensing applications. POF properties, sensitivities, and cross-sensitivities that are relevant for sensing are introduced. Advantages and limitations are discussed. State-of-the-art POF sensors and application examples are presented in subsections with regard to their underlying measurement principles. KW - Optical fiber sensors KW - Polymer optical fibers (POF) KW - Structural health monitoring KW - Distributed sensor PY - 2018 UR - https://link.springer.com/referenceworkentry/10.1007%2F978-981-10-1477-2_3-1 SN - 978-981-10-1477-2 DO - https://doi.org/10.1007/978-981-10-1477-2_3-1 SP - 1 EP - 36 PB - Springer Nature CY - Singapore AN - OPUS4-45754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - The LAUS: First applications of a new system for ultrasonic imaging of very concrete structures N2 - The LAUS (Large Aperture Ultrasonic System) has been developed to image very thick concrete structures, which are not accessible for commercial systems. The device and the corresponding software is the result of joint research of BAM, an ultrasonic instrument manufacturer and University of Kassel, Germany. It consists of 12 separate arrays of 32 point-contact shear wave transducers each, which can be deployed in flexible configurations. Each array is combined with battery and transmitter, receiver and wireless communication electronics. Three case histories are presented. First the system was deployed on a 5-m thick heavily reinforced foundation slab. The reflection of the slab’s bottom was imaged clearly. In addition, a multiple reflection was registered, thus giving hope that even thicker elements might be imaged by the instrument. Second, the LAUS was used to investigate a massive bridge girder where a heavy rainstorm during concreting had led to imperfections that were visible after removing the formwork was removed. The LAUS could image tendon ducts in 1.8m depth and the backwall closely behind them. Some limited areas showed blurred reflections and were checked by drill holes; these areas were affected by diffuse damage which could be repaired by injections. Third, a large retaining wall was checked for thickness. Meanwhile, the LAUS has been used in underground waste deposits (nuclear and other) for quality assurance of sealing plugs. A confirmed penetration depth of about 7 m has been reached. T2 - ASNT SMT/NDT-CE 2018 CY - New Brunswick, NJ, USA DA - 27.8.2018 KW - LAUS KW - Ultrasound KW - Imaging KW - Concrete PY - 2018 AN - OPUS4-45828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Unger, Wolfgang T1 - Summary of ISO/TC 201 technical report: ISO/TR 19693 surface chemical analysis—characterization of functional glass substrates for biosensing applications N2 - ISO/TR 19693:2018—Surface chemical analysis—Characterization of functional glass substrates for biosensing applications gives an overview of methods, strategies, and guidance to identify possible sources of problems related to substrates, device production steps (cleaning, activation, and chemical modification), and shelf life (storage conditions and aging). It is particularly relevant for surface chemical analysts characterizing glass‐based biosensors, and developers or quality managers in the biosensing device production community. Based on quantitative and qualitative surface chemical analysis, strategies for identifying the cause of poor Performance during device manufacturing can be developed and implemented. A review of measurement capabilities of surface analytical methods is given to assist readers from the biosensing community. KW - Bio sensing device KW - Surface chemical analysis KW - XPS KW - SIMS KW - Standardization PY - 2018 DO - https://doi.org/10.1002/sia.6481 SN - 0142-2421 SN - 1096-9918 VL - 50 IS - 8 SP - 835 EP - 838 PB - John Wiley & Sons, Ltd. AN - OPUS4-45829 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baer, D. R. A1 - Karakoti, A. S. A1 - Clifford, C. A. A1 - Minelli, C. A1 - Unger, Wolfgang T1 - Importance of sample preparation on reliable surface characterisation of nano‐objects: ISO standard 20579‐4 N2 - The international ISO Standard 20579‐4, dealing with the history and preparation of nano‐objects for surface analysis, has been developed to help address some of the replication and reproducibility issues caused by the fundamental nature of nanoobjects. Although all types of samples requiring surface analysis need thoughtful preparation, nano‐objects, for which many properties are controlled by their surfaces, present additional challenges in order to avoid variations and artefacts due to the handling and preparation of materials prior to analysis. This international standard is part of a series of standards related to preparation of samples for surface chemical analysis. Parts 1 and 2 of ISO Standard series 20579 address general issues that apply to many samples. Part 3, which is still in development, will focus on biomaterials. Part 4 specifically considers issues that arise due to the inherent nature of nano‐objects. Because of sensitivity to their environment, the standard indicates the minimum Information that needs to be reported about the handling and preparation of nano‐objects prior to surface analysis. This information should become part of sample provenance information that helps assure the reliability and usefulness of data obtained from surface‐analysis in the context of the synthesis, processing, and analysis history of a batch of material. Application of this standard can help address reproducibility and traceability issues associated with synthesis, processing, and characterization of nano‐objects in research and commercial applications. KW - Nano‐object characterization KW - Nanoparticle characterization KW - Provenance information KW - Sample preparation KW - Surface analysis PY - 2018 DO - https://doi.org/10.1002/sia.6490 SN - 0142-2421 SN - 1096-9918 VL - 50 IS - 9 SP - 902 EP - 906 PB - John Wiley & Sons, Ltd. AN - OPUS4-45830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Towards the standardization of dynamic instrumented indentation testing N2 - Nowadays the Instrumented Indentation Testing (IIT) is one of the most commonly used methods to determine the mechanical properties of materials in the nano range. This method is already extensive standardized in EN ISO 14577 part 1-4. Because of the great interest of researchers and industries in investigations of time depending material behavior mostly all suppliers of IIT equipment are offering the possibility of dynamic testing. Realizing this development ISO/TC 164/SC3 Hardness Testing has proposed to start the new standardization project “Linear elastic dynamic instrumented indentation testing DIIT”. The development of this standard is accompanied by the first international intercomparing exercise comparing results of dynamic instrumented indentation testing from testing machines using different hardware solutions and different models for data evaluation. The draft of part 5 of ISO 14577 “Linear elastic dynamic instrumented indentation testing DIIT” specifies verification and calibration of testing machines for carrying out the measurement of the dynamic material response when an oscillatory force or displacement, with amplitudes small in comparison to the prescribed target values, is imparted to the indenter while the indenter is continuously loaded to a prescribed target load or target depth or while the load or displacement is held constant at a prescribed target value. In case of a material showing plastic-elastic behavior, the measured dynamic response is used for continuous evaluation of the dynamic stiffness of the contact as a function of depth and frequency. Using the dynamic stiffness of the contact a reduced dynamic modulus will be calculated. In case of a material showing visco-elastic behavior from the measured dynamic response also the dynamic contact damping coefficient as function of depth and frequency is evaluated continuously. Using dynamic contact stiffness and dynamic contact damping coefficient reduced lost and storage modulus for visco-elastic materials will be calculated. The main normative requirements of the draft will be presented and discussed in the light of the first results of the intercomparing excise. T2 - IIW6, International Indentation Workshop 6 CY - Sapporo, Japan DA - 02.07.2018 KW - ISO 14577 KW - Instrumented indentation testing KW - Nanoindentation KW - IIT KW - Mechanical properties KW - Dynamic testing KW - Visco-elastic KW - Loss module KW - Storage module PY - 2018 AN - OPUS4-45850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik T1 - Structured heating in active thermography by using laser arrays N2 - Lock-in- and flash thermography are standard methods in active thermography. They are widely used in industrial inspection tasks e.g. for the detection of delaminations, cracks or pores. The requirements for the light sources of these two methods are substantially different. While lock-in thermography requires sources that can be easily and above all fast modulated, the use of flash thermography requires sources that release a very high optical energy in the very short time. By introducing high-power vertical cavity surface emitting lasers (VCSELs) arrays to the field of thermography a source is now available that covers these two areas. VCSEL arrays combine the fast temporal behavior of a diode laser with the high optical irradiance and the wide illumination range of flash lamps or LEDs and can thus potentially replace all conventional light sources of thermography. However, the main advantage of this laser technology lies in the independent control of individual array areas. It is therefore possible to heat not only in terms of time, but also in terms of space. This new degree of freedom allows the development of new NDT methods. We demonstrate this approach using a test problem that can only be solved to a limited extent in active thermography, namely the detection of very thin, hidden defects in metallic materials that are aligned vertically to the surface. For this purpose, we generate destructively interfering thermal wave fields, which make it possible to detect defects within the range of the thermal wave field high sensitivity. This is done without pre-treatment of the surface and without using a reference area to depths beyond the usual thermographic rule of thumb. T2 - ConaEnd&Iev 2018 CY - Sao Paulo, Brazil DA - 27.08.2018 KW - VCSEL KW - Active thermography KW - Laser KW - Structured heating KW - Subsurface defects PY - 2018 AN - OPUS4-45851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stegemann, Robert A1 - Cabeza, Sandra A1 - Pelkner, Matthias A1 - Lyamkin, Viktor A1 - Pittner, Andreas A1 - Werner, Daniel A1 - Wimpory, R. A1 - Boin, M. A1 - Kreutzbruck, Marc A1 - Bruno, Giovanni T1 - Influence of the microstructure on magnetic stray fields of low-carbon steel welds N2 - This study examines the relationship between the magnetic mesostructure with the microstructure of low carbon steel tungsten inert gas welds. Optical microscopy revealed variation in the microstructure of the parent material, in the heat affected and fusion zones, correlating with distinctive changes in the local magnetic stray fields measured with high spatial resolution giant magneto resistance sensors. In the vicinity of the heat affected zone high residual stresses were found using neutron diffraction. Notably, the gradients of von Mises stress and triaxial magnetic stray field modulus follow the same tendency transverse to the weld. In contrast, micro-X-ray fluorescence characterization indicated that local changes in element composition had no independent effect on magnetic stray fields. KW - TIG-welding KW - GMR sensors KW - Magnetic stray field KW - Neutron diffraction KW - Residual stress KW - Microstructure KW - Low carbon steel PY - 2018 DO - https://doi.org/10.1007/s10921-018-0522-0 SN - 0195-9298 SN - 1573-4862 VL - 37 IS - 3 SP - 66,1 EP - 18 PB - Springer US CY - New York AN - OPUS4-45855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bosc-Bierne, Gaby T1 - A generic, cost-efficient HPLC-HRMS method for quality control of peptide pools N2 - Synthetic peptide pools are used in antigen-specific T-cell assays, which are an important part in vaccine and immunotherapeutic clinical trials. As the analytical characterization is challenging due to the similarity of the single peptides or is expensive due to isotope labeled standards, usually only a pre-characterization of the single peptides is performed. However, a regular quality control of the peptide mix would be highly desirable. Therefore, a cost-efficient high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) method for quality control of a model peptide pool is developed. Peptides were synthesized using peptides&elephants proprietary libraries of individual peptides (LIPS) technology and purified by reversed-phase chromatography to > 90% each. The lyophilized single peptides were combined to a model peptide pool and analyzed by reversed-phase high-performance capillary liquid chromatography coupled to an orbitrap mass spectrometer. Separation was performed on a capillary reversed phase column (2 μm, ID x L 300 μm x 150 mm) with a linear gradient of acetonitrile + 0,05% trifluoroacetic acid. After optimizing the injection mode, the gradient elution, the temperature and the additives a model peptide pool was separated. The extracted ion chromatogram (XIC) was studied to confirm the exact masses. By combination of capillary HPLC and HRMS a new cost-efficient quality control method could be developed for the separation and identification of complex synthetic peptide pools. T2 - 5th European Congress of Immunology CY - Amsterdam, The Netherlands DA - 02.09.2018 KW - Peptide pools KW - Quality control KW - LC-MS PY - 2018 AN - OPUS4-45858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael A1 - Klaer, R.-H. A1 - Wagner, A. T1 - 100 % Digital in der Prozessindustrie - Tutzing-Symposion Teil 3: Intelligente Nutzung von Daten und Bausteinen der Digitalisierung N2 - Digitalisierung und Industrie 4.0 verändern komplette Geschäftsmodelle, heben neue Effizienzpotenziale und stärken die Wettbewerbsfähigkeit. Auf dem 57. Tutzing-Symposion vom 15.–18.04.2018 wurde mit Vorträgen und Kreativworkshops erkundet, welche speziellen Anforderungen die Prozessindustrie hat, welche digitalen Innovationen bereits umgesetzt wurden und wo noch Handlungsbedarf besteht. Ein Workshop befasste sich mit den Themenfeldern Datenkonzepte, Datenanalyse, Big Data und künstliche Intelligenz. Es geht nicht um die Digitalisierung von heute. Im Angesicht der wachsenden Digitalisierung unserer Prozesse stellt sich die Frage, ob wir den Prozess wirklich gut kennen. Ob alle Verfahrensschritte detailliert hinterlegt wurden. Nur mit einem heuristischen Ansatz kann das vorhandene Wissen nicht digitalisiert werden. Sehr schnell werden die Mechanismen eines Massenmarktes mit denen einer Nische verwechselt. Nicht jeder Mechanismus, den wir von großen Suchmaschinen oder Einkaufsportalen kennen, gibt uns einen Hinweis auf Nutzen und Verfügbarkeit für die Prozess- oder pharmazeutische Industrie. Eine gute Analyse der Anforderungen in der Zukunft mit einem Abgleich der derzeitigen technischen Möglichkeiten ist Voraussetzung für eine Verbesserung der derzeitigen digitalen Umsetzung. Dabei ist es sinnvoll unkonventionelle Methoden einzusetzen. KW - Digitalisierung KW - Prozessindustrie KW - Tutzing-Symposion KW - Datenkonzepte KW - Datenanalyse KW - Big Data KW - Künstlicher Intelligenz PY - 2018 UR - https://www.chemanager-online.com/themen/produktion/100-digital-der-prozessindustrie SN - 1436-2597 VL - 21 IS - 9 SP - 6 EP - 9 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-45861 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica T1 - Nanocrystals as labeling reagents for bioimaging by LA-ICP-MS N2 - Imaging of elemental distributions in single cell assays as well as tissue sections can be performed by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). This powerful technique offers precise spatially resolved measurements at trace and ultratrace levels and has been established as an excellent tool to answer analytical, biological and biomedical questions. To date, mass cytometry is already able to simultaneously detect up to 40 cellular targets due to conjugation of isotopically pure lanthanides to affinity binders, e.g. antibodies. To further enhance the ability of multiparametric analysis to more than 100 analytes at once, we investigated lanthanide nanocrystals as new, highly sensitive metal tags for identification of targets in clinical cell assays and tissue samples. Multiparametric analysis will be possible by encoding the lanthanide composition of nanocrystals associated to the affinity binders. Nanocrystals showed remarkable potential for sensitive detection in MS due to high stability and signal amplification compared to e.g. polymer tags, carrying fewer metal atoms. Furthermore, the nanocrystals allow multimodal imaging due fluorescence of Eu3+ as well as contrast enhancing properties of Gd3+ in magnetic resonance imaging. Synthesis of functionalized lanthanide nanocrystals for further bioconjugation was performed with high reproducibility and monodisperse size distribution. For proof of principle, the uptake and distribution of these nanocrystals within the monolayered cell line A549 were investigated by mapping the intensities at subcellular resolution using LA-ICP-MS. It could be shown, that the cells were efficiently labeled with the nanocrystals. Additionally, the bioconjugation of the nanocrystals to antibodies and particularly the preservation of the antibody specificity was investigated using Dot Blot experiments. All in all, the results imply high sensitivity and the possibility of multiparametric analysis by doting various lanthanides into the nanocrystals. T2 - ICPMS Anwendertreffen 2018 CY - Berlin, Germany DA - 03.09.2018 KW - Bioimaging KW - Nanoparticle KW - Immuno-assay KW - Lanthanide PY - 2018 AN - OPUS4-45865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica T1 - Nanocrystals as labeling reagents for imaging mass cytometry N2 - Imaging of elemental distributions in single cell assays as well as tissue sections can be performed by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). This powerful technique offers precise spatially resolved measurements at trace and ultratrace levels and has been established as an excellent tool to answer analytical, biological and biomedical questions. To date, mass cytometry is already able to simultaneously detect up to 40 cellular targets due to conjugation of isotopically pure lanthanides to affinity binders, e.g. antibodies. To further enhance the ability of multiparametric analysis to more than 100 analytes at once, we investigated lanthanide nanocrystals as new, highly sensitive metal tags for identification of targets in clinical cell assays and tissue samples. Multiparametric analysis will be possible by encoding the lanthanide composition of nanocrystals associated to the affinity binders. Nanocrystals showed remarkable potential for sensitive detection in MS due to high stability and signal amplification compared to e.g. polymer tags, carrying fewer metal atoms. Furthermore, the nanocrystals allow multimodal imaging due fluorescence of Eu3+ as well as contrast enhancing properties of Gd3+ in magnetic resonance imaging. Synthesis of functionalized lanthanide nanocrystals for further bioconjugation was performed with high reproducibility and monodisperse size distribution. For proof of principle, the uptake and distribution of these nanocrystals within the monolayered cell line A549 were investigated by mapping the intensities at subcellular resolution using LA-ICP-MS. It could be shown, that the cells were efficiently labeled with the nanocrystals. Additionally, the bioconjugation of the nanocrystals to antibodies and particularly the preservation of the antibody specificity was investigated using Dot Blot experiments. All in all, the results imply high sensitivity and the possibility of multiparametric analysis by doting various lanthanides into the nanocrystals. T2 - Bioimaging Workshop BI(MS)2 CY - Münster, Germany DA - 24.05.2018 KW - Bioimaging KW - Nanoparticle KW - LA-ICP-MS KW - Lanthanide PY - 2018 AN - OPUS4-45867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Puthiyaveettil, N. T1 - Numerical study of laser line thermography for crack detection at high temperature N2 - The detection of cracks before the failure is highly significant when it comes to safety-relevant structures. Crack detection in metallic samples at high surface temperature is one of the challenging situation in manufacturing industries. Laser thermography has already proved its detection capability of surface cracks in metallic samples at room temperature. In this work a continuous wave (CW) laser use to generate a laser, which is using to scan the metal surface with notch. The corresponding heat distribution on the surface monitored using infrared thermal (IR) camera. A simplified 3D model for laser thermography is developed and validated with experimental results. A dedicated image processing algorithm developed to improve the detectability of the cracks. To understand the dependency of surface temperature, laser power, laser scanning speed etc. in defect detection, we carried out parametric studies with our validated model. Here we report the capability of laser thermography in crack detection at elevated temperature. T2 - Conference QIRT 2018 CY - Berlin, Germany DA - 25.06.2018 KW - Thermography KW - Laser Thermography KW - Cracks PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-454441 DO - https://doi.org/10.21611/qirt.2018.076 AN - OPUS4-45444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Lock-in Thermography using High-Power Laser Sources N2 - Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test specimen. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration. We present current activities with kilowatt-class high-power laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages. T2 - 12th European Conference on Non-destructive Testing CY - Gothenburg, Sweden DA - 11.06.2018 KW - Thermography KW - Laser Thermography KW - Lock-in Thermography PY - 2018 AN - OPUS4-45445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Lock-in Thermography using High-Power Laser Sources N2 - Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent (i.e. halogen) lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test site. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz, see Fig.1. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration. Using the one-dimensional solution to the thermal heat diffusion equation together with the absorptance of the material which is illuminated with a harmonically modulated light source, we can calculate the temperature oscillation at the surface of a solid. As a second step, we calculate the corresponding oscillation of the total thermal emission using Stefan-Boltzmann law as a first order approximation and taking into account the emissivity of the material. Within this framework we can calculate the minimal irradiance of a light source necessary to provoke a measurable signal within a thermographic camera at a noise equivalent temperature difference (NETD) of 30 mK. In Fig. 2 this relationship is displayed for a wide spectrum of modulation frequencies and for a number of different light sources scaled to the same electrical input power and illumination area. Using this figure, it is now easily possible to analyze the range of materials to be tested using lock-in thermography, since only the materials (dotted lines) below the irradiance-vs-frequency curves (solid lines) are heated in excess of the camera’s NETD. This figure clearly shows that laser sources considerably increase the application range of lock-in thermography, since especially for metals with a high reflectance and high thermal diffusivity a high irradiance is vitally important to allow for lock-in texting. We present current activities with kilowatt-class high-power laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages. T2 - Conference QIRT 2018 CY - Berlin, Germany DA - 25.06.2018 KW - Thermography KW - Laser Thermography KW - Lock-in Thermography PY - 2018 AN - OPUS4-45447 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Lock-in Thermography using High-Power Laser Sources N2 - Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent (i.e. halogen) lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test site. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz, see Fig.1. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration. Using the one-dimensional solution to the thermal heat diffusion equation together with the absorptance of the material which is illuminated with a harmonically modulated light source, we can calculate the temperature oscillation at the surface of a solid. As a second step, we calculate the corresponding oscillation of the total thermal emission using Stefan-Boltzmann law as a first order approximation and taking into account the emissivity of the material. Within this framework we can calculate the minimal irradiance of a light source necessary to provoke a measurable signal within a thermographic camera at a noise equivalent temperature difference (NETD) of 30 mK. In Fig. 2 this relationship is displayed for a wide spectrum of modulation frequencies and for a number of different light sources scaled to the same electrical input power and illumination area. Using this figure, it is now easily possible to analyze the range of materials to be tested using lock-in thermography, since only the materials (dotted lines) below the irradiance-vs-frequency curves (solid lines) are heated in excess of the camera’s NETD. This figure clearly shows that laser sources considerably increase the application range of lock-in thermography, since especially for metals with a high reflectance and high thermal diffusivity a high irradiance is vitally important to allow for lock-in texting. We present current activities with kilowatt-class high-power laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages. T2 - Conference QIRT 2018 CY - Berlin, Germany DA - 25.06.2018 KW - Thermography KW - Laser Thermography KW - Lock-in Thermography PY - 2018 AN - OPUS4-45449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Burgholzer, P. A1 - Berer, T. A1 - Ziegler, Mathias A1 - Thiel, Erik A1 - Ahmadi, Samim A1 - Gruber, J. A1 - Mayr, G. A1 - Hendorfer, G. T1 - Blind structured illumination as excitation for super-resolution photothermal radiometry N2 - Using an infrared camera for radiometric imaging allows the contactless temperature measurement of multiple surface pixels simultaneously. From the measured surface data, a sub-surface structure, embedded inside a sample or tissue, can be reconstructed and imaged when heated by an excitation light pulse. The main drawback in radiometric imaging is the degradation of the spatial resolution with increasing depth, which results in blurred images for deeper lying structures. We circumvent this degradation with blind structured illumination, combined with a non-linear joint sparsity reconstruction algorithm. The ground-breaking concept of super-resolution can be transferred from optics to thermographic imaging. T2 - Conference QIRT 2018 CY - Berlin, Germany DA - 25.06.2018 KW - Thermography KW - Laser thermography KW - Super resolution PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-454506 SN - 978-3-940283-94-8 DO - https://doi.org/10.1080/17686733.2019.1655247 SP - We.3.A.2, 1 EP - 7 AN - OPUS4-45450 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kage, Daniel A1 - Fischer, Linn A1 - Hoffmann, Katrin A1 - Thiele, T. A1 - Schedler, U. A1 - Resch-Genger, Ute T1 - Close spectroscopic look at dye-stained polymer microbeads N2 - Dye-stained micrometer-sized polymer beads are important tools in the life sciences with applications in biomedical, biochemical, and clinical research. Here, bead-based assays are increasingly used, for example, in DNA sequencing and the detection of autoimmune diseases or pathogenic microorganisms. Moreover, stained beads are employed as calibration tools for fluorescence microscopy and flow cytometry methods with increasing complexity. To address the requirements concerning the relevant fluorescence features, the spectroscopic properties of representative polymer beads with diameters ranging from about 1 to 10 μm stained with varying concentrations of rhodamine 6G were systematically assessed. The observed dependence of the spectral properties, fluorescence decay kinetics, and fluorescence quantum yields on bead size and dye loading concentration is attributed to different fluorescence characteristics of fluorophores located in the particle core and near-surface dye molecules. Supported by the fluorescence anisotropy measurements, the origin of the observed alteration of fluorescence features is ascribed to a combination of excitation energy transfer and polarity-related effects that are especially pronounced at the interface of the bead and the surrounding medium. The results of our studies underline the need to carefully control and optimize all Parameters that can affect the fluorescence properties of the dye-stained beads. KW - Fluorophore KW - Polymer particles KW - Photophysics KW - Life sciences KW - Standards PY - 2018 DO - https://doi.org/10.1021/acs.jpcc.8b02546 SN - 1932-7447 VL - 122 IS - 24 SP - 12782 EP - 12791 PB - ACS Publications CY - Washington, DC AN - OPUS4-45453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane T1 - Quantification of impact damages in CFRP and GFRP structures with thermography and ultrasonics N2 - For the quantification of impact damage in CFRP and GFRP structures, first passive thermography measurements have been performed at the front and rear side of the test specimens during low velocity impact load. After loading, the damaged structures have been investigated non-destructively with active thermography with flash excitation and with step heating and with two different ultrasonic methods (phased array and air coupled ultrasonics). The damage sizes quantified with all methods are evaluated and compared. In addition, the depth of the greatest damage inside the different test specimens is analysed. T2 - QIRT Conference 2018 CY - Berlin, Germany DA - 25.06.2018 KW - Thermography KW - Ultrasonics KW - CFRP KW - GFRP KW - Impact PY - 2018 AN - OPUS4-45458 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc T1 - Influence of Gas Pressure on Coulometric Trace Humidity Measurement N2 - Planar coulometric sensors were investigated in humidified synthetic air at various absolute gas pressures, i. e. 2 bar, 5, bar, 10 bar, and 15 bar. Humidified gas flow at adjusted gas pressure was split into two flows, one passed a coulometric sensor and the other one passed a reference hygrometer after decompression. Both signals were recorded and then compared after calculation of resulting frost point temperature. Calculation is based on a calibration function obtained at ambient pressure. Comparison showed that an increasing pressure resulted in a higher derivation between sensor signal (calculated frost point temperature) and reference frost point temperature. At an absolute pressure of 2 bar the differences were minor in consideration of the uncertainty, however at 15 bar the differences were 6.77 K. Nevertheless, it was possible to measure the gas humidity at higher pressure with coulometric trace humidity sensors. T2 - 17th International Meeting of Chemical Sensors, IMCS 2018 CY - Vienna, Austria DA - 15.07.2018 KW - Gas pressure influence KW - Coulometric sensors KW - Trace humidity measurement PY - 2018 AN - OPUS4-45535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc A1 - Tiebe, Carlo A1 - Banach, Ulrich T1 - Influence of Gas Pressure on Coulometric Trace Humidity Measurement N2 - Planar coulometric sensors were investigated in humidified synthetic air at various absolute gas pressures, i. e. 2 bar, 5, bar, 10 bar, and 15 bar. Humidified gas flow at adjusted gas pressure was split into two flows, one passed a coulometric sensor and the other one passed a reference hygrometer after decompression. Both signals were recorded and then compared after calculation of resulting frost point temperature. Calculation is based on a calibration function obtained at ambient pressure. Comparison showed that an increasing pressure resulted in a higher derivation between sensor signal (calculated frost point temperature) and reference frost point temperature. At an absolute pressure of 2 bar the differences were minor in consideration of the uncertainty, however at 15 bar the differences were 6.77 K. Nevertheless, it was possible to measure the gas humidity at higher pressure with coulometric trace humidity sensors. T2 - 17th International Meeting of Chemical Sensors, IMCS 2018 CY - Vienna, Austria DA - 15.07.2018 KW - Gas pressure influence KW - Coulometric sensors KW - Trace humidity measurement PY - 2018 SN - 978-3-9816876-9-9 DO - https://doi.org/10.5162/IMCS2018/P2EC.7 SP - 715 EP - 716 PB - AMA Service GmbH CY - Wunstorf / Germany AN - OPUS4-45539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piedade, M. F. M. T1 - Crystal Engineering through Solvent Mediated Control of Molecular Conformation: The Case of 5-Hydroxynicotinic Acid N2 - The importance of molecular conformation for polymorphism and its repercussions in terms of tight control over the industrial production of crystalline organic materials with highly reproducible physicochemical properties has long been recognized. Efforts to understand how a crystallization solvent can direct the formation of a polymorph containing a specific molecular conformation are, however, relatively scarce. Nicotinic acid (NA) and its hydroxyl derivatives (2-, 4-, 5-, and 6-hydroxynicotinic acids) are very good models for such studies. Indeed, regardless of the solvent, NA always crystallizes as a single polymorph with the molecule in the same neutral conformation. In contrast, the hydroxyl derivatives are prone to polymorphism and solvate formation and, depending on the crystallization conditions, the molecules in the crystal lattice can exhibit hydroxyl, oxo, or zwitterionic conformations. The present study focused on 5-hydroxynicotinicacid (5HNA) shows that by judicious selection of the solvent it is possible to obtain 1:1 solvates, where solvation memory is not completely lost and the tautomer preferred in solution persists in the crystalline state: zwitterionic in 5HNA·H2O and neutral in 5HNA·DMSO. Nevertheless, upon thermal desolvation the obtained materials evolve to the same unsolvated form where the molecule is in a zwitterionic conformation. The structures of 5HNA·H2O and 5HNA·DMSO obtained from single crystal-ray diffraction are discussed and compared with that of 5HNA solved from powder data. The energetics of the dehydration/desolvation process was also fully characterized by thermogravimetry (TG), differential scanning calorimetry (DSC) and Calvet microcalorimetry. T2 - BACG 2018 CY - Limerick, Ireland DA - 20.06.2018 KW - Crystal Engineering KW - 5-hydroxynicotinic acid KW - Molecular Conformation PY - 2018 AN - OPUS4-45519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN T1 - Improvement of effectiveness of in-service inspection in nuclear power plants (IAEA-TECDOC-1853) N2 - This publication represents a consensus among experts drawn from the IAEA and global practitioners to compile a set of common or good individual practices for use at nuclear power plants to improve ISI effectiveness. It sets forth a number of strategies and practices for improving the effectiveness of ISI and investigates the role of ISI in maintaining or improving safety at plants and the relationship of ISI improvement to cost. Strategies for improving ISI effectiveness are discussed, with consideration given to the entire framework of ISI, including effective selection of the proper inspection scope, inspection interval and NDE efficiency. This publication is an update of the publication IAEA-TECDOC-1400, Improvement of In-service Inspection in Nuclear Power Plants, which was published in 2004. It takes into account new techniques and technologies for qualification processes for methodologies, equipment, procedures and personnel as well human factors in NDE inspections. KW - NDT KW - Nuclear power KW - Human factors KW - In-service inspection KW - ISI effectiveness KW - Non-destructive testing PY - 2018 UR - https://www-pub.iaea.org/MTCD/Publications/PDF/TE-1853web.pdf SN - 978-92-0-106618-3 SN - 1011-4289 VL - 1853 SP - 1 EP - 85 PB - International Atomic Energy Agency CY - Vienna AN - OPUS4-46163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wanner, C. A1 - Poethig, R. A1 - Carrero, S. A1 - Fernandez-Martinez, A. A1 - Jäger, Christian A1 - Furrer, G. T1 - Natural occurrence of nanocrystalline Al-hydroxysulfates: Insights on formation, Al solubility control and As retention N2 - Nanocrystalline basaluminite [Al4OH10(SO4)(H2O)3–5] and Aggregation of the e-Keggin polyoxocation [Al12(AlO4)(OH)24(H2O)12]7+, referred to as Al13, have both been described to form in acid mine Drainage environments. Although the chemical composition is quite similar, their crystalline varieties significantly differ, demonstrating that various types of Al-hydroxysulfates can form under similar conditions and that their respective formation is not fully understood yet. Here, we report the occurrence of nanocrystalline precipitates that form naturally in a small alpine catchment in Switzerland where an acidic mountainous stream (pH 4) is neutralized successively after mixing with several neutral tributaries. The stepwise neutralization in conjunction with the large amount of precipitates provide an ideal setting for obtaining new insights into (i) the structure of naturally forming Al-hydroxysulfates, (ii) their formation mechanism, (iii) their role in controlling the solubility of Al, and (iv) their ability to lower the mobility of As. Synchrotron-based high-energy X-ray diffraction and subsequent pair distribution function analyses demonstrate that these precipitates are structurally identical to basaluminite samples obtained from acid mine drainage sites. In contrast, only minor amounts of tetrahedrally coordinated Al, as present in Al13, were identified by nuclear magnetic resonance spectroscopy. The precipitates are further characterized by elevated As concentrations up to 600 lg/g, whereas other heavy metals are at background concentrations only. Given the low As concentrations in the stream from which precipitation occurs (<0.03 mg/L), high As concentrations confirm that basaluminite serves as a highly efficient As sink, which is attributed to its high anion-exchange capacity. Chemical analysis of streamwater samples in combination with geochemical modeling show that precipitation occurs instantaneously upon mixing with neutral streams. Moreover, our data reveal that the precipitation of basaluminite exerts a strong solubility control on dissolved Al concentrations as manifested by the quasi-constant basaluminite ion activity product observed during neutralization from pH 5 to pH 5.9. We hypothesize that in our field system, high fluoride and sulfate concentrations on the order of 100 and 1–2 mg/L, KW - Basaluminite KW - Al13 KW - Acid rock drainage KW - Arsenic retention KW - Aluminum KW - Anion exchange PY - 2018 DO - https://doi.org/10.1016/j.gca.2018.06.031 SN - 0016-7037 SN - 1872-9533 VL - 238 SP - 252 EP - 269 PB - Elsevier Ltd. AN - OPUS4-46164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - van de Kreeke, Johannes T1 - COMAR, where do you go? N2 - Currently BAM is undertaking efforts to recode the COMAR database and redefine its profile. These efforts are explained and placed into the broader perspective of the international RM market. T2 - REFERENCE MATERIALS IN MEASUREMENT AND TECHNOLOGY CY - Yekaterinburg, Russian Federation DA - 11.09.2018 KW - Reference materials KW - Proficiency testing KW - COMAR KW - EPTIS KW - RM and PT PY - 2018 AN - OPUS4-46175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - van de Kreeke, Johannes T1 - COMAR database: current efforts N2 - Currently BAM is making efforts to recode COMAR, the database for CRMs and reshape its profile as a database intended for qualitatively top-of-the-market CRMs. These efforts are highlighted and placed into the broad perspective of the international RM markets. A link to EPTIS, the database for PT schemes as a blueprint for the recoding is provided. T2 - BERM-15: International Symposium on Biological and Environmental Reference Materials CY - Berlin, Germany DA - 24.09.2018 KW - Reference materials KW - Proficiency testing KW - COMAR KW - EPTIS KW - RM and PT PY - 2018 AN - OPUS4-46179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim T1 - Thermographic super resolution using structured 1D laser illumination and joint sparsity N2 - Thermographic NDE is based on the interaction of thermal waves with inhomogeneities. These inhomogeneities are related to sample geometry or material composition. Although thermography is suitable for a wide range of inhomogeneities and materials, the fundamental limitation is the diffusive nature of thermal waves and the need to measure their effect radiometrically at the sample surface only. The propagation of the thermal waves from the heat source to the inhomogeneity and to the detection surface results in a degradation in the spatial resolution of the technique. A new concerted ansatz based on a spatially structured heating and a joint sparsity of the signal ensemble allows an improved reconstruction of inhomogeneities. As a first step to establish an improved thermographic NDE method, an experimental setup was built based on structured 1D illumination using a flash lamp behind a mechanical aperture. As a follow-up to this approach, we now use direct structured illumination using a 1D laser array. The individual emitter cells are driven by a random binary pattern and additionally shifted by fractions of the cell period. The repeated measurement of these different configurations with simultaneously constant inhomogeneity allows for a reconstruction that makes use of joint sparsity. With analytical-numerical modelling or numerical FEM simulations, we study the influence of the parameters on the result of non-linear reconstruction. For example, the influence of the illumination pattern as a variable heat flux density and Neumann boundary condition for convolution with the constant Green's function can be studied. These studies can be used to derive optimal conditions for a measurement technique. T2 - 62. International School of Quantum Electronics die Tagung “Progress in Photoacoustic & Photothermal Phenomena" CY - Erice, Italy DA - 06.09.2018 KW - Super resolution KW - Virtual wave KW - Laser thermography KW - 1d laser KW - Joint sparsity KW - Laser array KW - VCSEL array KW - High-power laser PY - 2018 AN - OPUS4-46180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska T1 - Acoustic Emission T1 - Überwachung und Charakterisierung von Werkstoffen mittels Schallemissionsanalyse N2 - Das Phänomen Schallemission (eng. Acoustic Emission, AE) ist eine Begleiterscheinung bei aktiven Mechanismen und Prozessen wie sie in Werkstoffen auftreten, die einer Belastung durch Krafteinwirkung oder durch Änderung der Umgebungsbedingungen ausgesetzt sind. Plastische Verformung, Risswachstum, Korrosion oder der Übergang zu einer anderen Phase generieren u.a. transiente elastische Wellen, die sich im Werkstoff und an der Materialoberfläche ausbreiten. Auftretende Auslenkungen von wenigen hundert Pikometern sind mit piezo-elektrischen AE Sensoren detektierbar. Aufzeichnungsraten von bis zu 40 MHz ermöglichen dabei zeitliche Auflösungen von einigen Nano- bis Mikrosekunden. Die Dechiffrierung der detektierten Informationen ist für die Material- und Versagenscharakterisierung sowie für Anwendungen in der Struktur- oder Prozessüberwachung ein zentraler Forschungsschwerpunkt. Nach einem kurzen Überblick zu den Grundlagen werden ausgewählte Ansätze der AE Methode vorgestellt und diskutiert: 1) AE Monitoring von Pipelines als Referenzmessung für die Entwicklung eines akustischen faseroptischen Monitorings (AGIFAMOR) 2) Schwellwertfreie AE Messung im 4-Punkt-Rohrbiegeprüfstand BAM_9.1 (AGIFAMOR) 3) Kombination von AE mit Röntgen-Mikrotomografie und die Anwendung der frequenzbasierten Mustererkennung ermöglichen eine Zuordnung von AE und Mechanismen (Ergebnisse aus dem SNSF Projekt Nr. 127'134, Baensch 2014, Diss. ETH No. 22372) T2 - Abteilungsseminar BAM-8.1 CY - BAM UE, Berlin, Germany DA - 08.10.2018 KW - Acoustic Emission (AE) KW - Monitoring KW - Non-threshold measurement KW - Unsupervised pattern recognition PY - 2018 AN - OPUS4-46202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yuan, Huan A1 - Gojani, Ardian A1 - Gornushkin, Igor B. A1 - Wang, X. T1 - Investigation of laser-induced plasma at varying pressure and laser focusing N2 - Expansion dynamics of laser-induced plasma is studied for different focal positions of the ablation laser in the pressure range 10-2 - 105 Pa of the ambient air. The experimental results indicate that both the parameters significantly affect the plasma size, shape, intensity, reproducibility, and distance from the target surface. At pressures above 10 Pa, the plasma plume is confined by the ambient gas; the plumes are more compact and travel shorter distances from the target as compared to the analogous plume characteristics at pressures below 10 Pa. The pulse-to-pulse reproducibility of the integral emission intensity of the plasma is also different for different focal positions and pressures. It is found that the focal positions -1 cm and -2 cm below the target surface yield the most reproducible and intense emission signals as measured at the 600 ns delay time with the 100 ns gate. The information obtained can be of importance for pulsed laser deposition, laser welding, and analytical spectroscopy at reduced pressures. In general, a correct choice of the focal position and pressure of an ambient gas is very important for obtaining the strongest plasma emission, good reproducibility, and desired plasma plume shape. KW - Laser-induced plasma KW - Plasma expansion KW - Imaging PY - 2018 DO - https://doi.org/10.1016/j.sab.2018.10.005 SN - 0584-8547 VL - 150 SP - 33 EP - 37 PB - Elsevier AN - OPUS4-46207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Software- and instrument development for characterization of nano-(C)RMs N2 - This poster deals with improvements and characteriztion of small-angle scattering limitations, by looking at the trifecta of Data collection and uncertainty propagation, data analysis methodologies, and real-world tests. It is found that - with appropriate care and instrumentation - accuracies of 1% on mean nanomaterial sizes, and 10% on the size distribution width as well as the volume fraction can be achieved. T2 - BAM-PTB Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - Small-angle scattering KW - Instrumentation KW - Methodology KW - MAUS KW - Data analysis KW - Data correction PY - 2018 AN - OPUS4-46107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Plasma fundamentals and diagnostics N2 - This course will provide an introduction to plasma diagnostic techniques. The major focus of the course will be on the discussions of the practical procedures as well as the underlying physical principles for the measurements of plasma fundamental characteristics (e.g., temperatures, thermodynamic properties, and electron number density). Particular emphasis will be placed on inductively coupled plasma–atomic emission spectrometry, but other analytical plasmas will also be used as examples when appropriate. Selected examples on how one can manipulate the operating conditions of the plasma source, based on the results of plasma diagnostic measurements, to improve its performance used for spectrochemical analysis will also be covered. Topics to be covered include thermal equilibrium, line profiles, temperatures, electron densities, excitation processes, microreactions, pump and probe diagnostics, tomography, temporal and spatial resolution. Basics of plasma computer modeling will be presented. T2 - 03.-06. September 2018, 13 Symposium "Massenspektrometrische Verfahren der Elementspurenanalyze", BAM, Berlin, Adlershof CY - BAM, Berlin, Adlershof, Germany DA - 03.09.2018 KW - Thermal equilibrium KW - Plasma processes KW - Electron number density KW - Temperatures KW - Emission line profiles KW - Spatial information KW - Plasma modeling PY - 2018 AN - OPUS4-46108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Dynamical chemical model of laser induced plasma N2 - Laser induced plasma (LIP) is a highly dynamic, short living event which presents significant difficulty for both diagnostics and modeling. The former requires precise spatially- and time-resolved measurements on a micron-nanosecond scale while the latter needs numerous descriptive parameters; many of them can only be obtained from experiment. Diagnostics and modeling should always complement each other for obtaining a truthful picture of LIP. In this presentation, a newly developed collisional-dominated model will be presented. The model is based on the coupled Navier-Stokes, state, radiative transfer, material transport, and chemical equations. The model incorporates plasma chemistry through the equilibrium approach that relies on atomic and molecular partition functions. Several chemical systems are modeled including Si-C-Cl-N and B-H-Cl systems. The model is used to study the equilibrium states of the systems as functions of the concentrations of plasma species and plasma temperature. The model also predicts the evolution of number densities of atomic and molecular species in the expanding plasma plume. T2 - 18.09.2018, 9th International Conference on PLASMA PHYSICS AND PLASMA TECHNOLOGY (PPPT‐9) CY - Minsk, Belorussia DA - 17.09.2018 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2018 AN - OPUS4-46111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Shabanov, Sergej V. T1 - Chemistry in laser‑induced plasmas at local thermodynamic equilibrium N2 - The equation of state for plasmas containing negative and positive ions of elements and molecules formed by these elements is modeled under the assumption that all ionization processes and chemical reactions are at local thermal equilibrium and the Coulomb interaction in the plasma is described by the Debye–Hückel theory. The hierarchy problem for constants of molecular reactions is resolved by using three different algorithms for high, medium, and low temperatures: the contraction principle, the Newton–Raphson method, and a scaled Newton–Raphson method, respectively. These algorithms are shown to have overlapping temperature ranges in which they are stable. The latter allows one to use the developed method for calculating the equation of state in combination with numerical solvers of Navier–Stokes equations to simulate laser-induced Plasmas initiated in an atmosphere and to study formation of molecules and their ions in such plasmas. The method is applicable to a general chemical network. It is illustrated with examples of Ca–Cl and C–Si–N laser-induced plasmas. KW - Plasma KW - LIBS KW - Plasma modeling PY - 2018 DO - https://doi.org/10.1007/s00339-018-2129-9 SN - 1432-0630 SN - 0947-8396 VL - 124 IS - 10 SP - 716, 1 EP - 21 PB - Springer AN - OPUS4-46112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino A1 - Neumann, Patrick P. T1 - Control of a spherical parallel manipulator with three degrees of freedom N2 - In robotic applications, it is often necessary to orient a sensor quickly. Spherical parallel manipulators (SPM) are well suited for this purpose since they offer superior dynamics and structural stiffness as compared to serial manipulators. To control them, however, the kinematic equations have to be known. In this paper, a SPM with three degrees of freedom and the kinematic equations describing its mechanical properties are presented. T2 - 35th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Sinaia, Romania DA - 25.09.2018 KW - Spherical parallel manipulator KW - Control PY - 2018 AN - OPUS4-46142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias T1 - Concept of a gas-sensitive nano aerial robot swarm for indoor air quality monitoring N2 - In industrial environments, airborne by-products such as dust and (toxic) gases, constitute a major risk for the worker’s health. Major changes in automated processes in the industry lead to an increasing demand for solutions in air quality management. Thus, occupational health experts are highly interested in precise dust and gas distribution models for working environments. For practical and economic reasons, high-quality, costly measurements are often available for short time-intervals only. Therefore, current monitoring procedures are carried out sparsely, both in time and space, i.e., measurement data are collected in single day campaigns at selected locations only. Real-time knowledge of contaminant distributions inside the working environment would also provide means for better and more economic control of air impurities. For example, the possibility to regulate the workspace’s ventilation exhaust locations can reduce the concentration of airborne contaminants by 50%. To improve the occupational health and safety of (industrial) workplaces, this work aims for developing a swarm of gas-sensitive aerial nano robots for monitoring indoor air quality and for localizing potential emission sources. T2 - Tag der offenen Tür auf dem Testgelände der BAM (BAM TTS) CY - Baruth/Mark - OT Horstwalde, Germany DA - 29.09.2018 KW - Mobile Robot Olfaction KW - Swarm KW - Nano aerial robot KW - Gas sensing PY - 2018 AN - OPUS4-46147 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hüllmann, Dino A1 - Bartholmai, Matthias ED - Pastramă, D. Ş ED - Constantinescu, D. M. T1 - Concept of a gas-sensitive nano aerial robot swarm for indoor air quality monitoring N2 - In industrial environments, airborne by-products such as dust and (toxic) gases, constitute a major risk for the worker’s health. Major changes in automated processes in the industry lead to an increasing demand for solutions in air quality management. Thus, occupational health experts are highly interested in precise dust and gas distribution models for working environments. For practical and economic reasons, high-quality, costly measurements are often available for short time-intervals only. Therefore, current monitoring procedures are carried out sparsely, both in time and space, i.e., measurement data are collected in single day campaigns at selected locations only. Real-time knowledge of contaminant distributions inside the working environment would also provide means for better and more economic control of air impurities. For example, the possibility to regulate the workspace’s ventilation exhaust locations can reduce the concentration of airborne contaminants by 50%. To improve the occupational health and safety of (industrial) workplaces, this work aims for developing a swarm of gas-sensitive aerial nano robots for monitoring indoor air quality and for localizing potential emission sources. T2 - 35th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Sinaia, Romania DA - 25.09.2018 KW - Mobile Robot Olfaction KW - Swarm KW - Nano aerial robot KW - Gas sensing PY - 2018 SN - 978-606-23-0874-2 SP - 139 EP - 140 PB - PRINTECH CY - Bukarest AN - OPUS4-46137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Concept of a gas-sensitive nano aerial robot swarm for indoor air quality monitoring N2 - In industrial environments, airborne by-products such as dust and (toxic) gases, constitute a major risk for the worker’s health. Major changes in automated processes in the industry lead to an increasing demand for solutions in air quality management. Thus, occupational health experts are highly interested in precise dust and gas distribution models for working environments. For practical and economic reasons, high-quality, costly measurements are often available for short time-intervals only. Therefore, current monitoring procedures are carried out sparsely, both in time and space, i.e., measurement data are collected in single day campaigns at selected locations only. Real-time knowledge of contaminant distributions inside the working environment would also provide means for better and more economic control of air impurities. For example, the possibility to regulate the workspace’s ventilation exhaust locations can reduce the concentration of airborne contaminants by 50%. To improve the occupational health and safety of (industrial) workplaces, this work aims for developing a swarm of gas-sensitive aerial nano robots for monitoring indoor air quality and for localizing potential emission sources. T2 - 35th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Sinaia, Romania DA - 25.09.2018 KW - Mobile Robot Olfaction KW - Swarm KW - Nano aerial robot KW - Gas sensing PY - 2018 AN - OPUS4-46140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino A1 - Kohlhoff, Harald A1 - Erdmann, Jessica A1 - Neumann, Patrick P. ED - Pastramă, D. Ş. ED - Constantinescu, D. M. T1 - Control of a spherical parallel manipulator with three degrees of freedom N2 - In robotic applications, it is often necessary to orient a sensor quickly. Spherical parallel manipulators (SPM) are well suited for this purpose since they offer superior dynamics and structural stiffness as compared to serial manipulators. To control them, however, the kinematic equations have to be known. In this paper, a SPM with three degrees of freedom and the kinematic equations describing its mechanical properties are presented. T2 - 35th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Sinaia, Romania DA - 25.09.2018 KW - Spherical parallel manipulator KW - Control KW - 3 DoF PY - 2018 SN - 978-606-23-0874-2 SP - 159 EP - 160 PB - PRINTECH CY - Bukarest AN - OPUS4-46141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahmadi, Samim T1 - Thermal wave field engineering using structured 1D laser illumination N2 - Thermal waves are solutions of the heat diffusion equation for periodic boundary conditions and can be seen analogously to strongly damped waves. Although the underlying differential equation differs from the wave equation, the essential property for analogy between both equations is linearity such that superposition applies. This linearity is maintained even after a linear transformation, such as the Fourier transform from time to frequency domain. It follows that the temporal superposition principle is already used in active thermography, e.g. in pulsed thermography, as a superposition of many individual frequencies. However, the systematic spatial superposition has not yet been fully exploited, mainly due to a lack of suitable energy sources. As a first step, we are investigating how thermal wave fields of arbitrary space-time structures can be engineered using structured laser illumination. The proof of principle was shown using a laser coupled projector. Unfortunately, the available optical output power was limited due to the thermal stress limit of the device. That is why we are working towards a more sophisticated moving 1D array of high-power diode lasers. We characterized the novel light source and believe that apart from the benefit of spatial and temporal illumination it can combine the temporal regimes of impulse and lock-in thermography. In a second step, we investigate moving and oscillating line sources with different line shapes. We use a Green’s Function ansatz to analytically model the thermal wave propagation of structured 1D laser illumination in isotropic materials. Furthermore, we show some methods how they can be implemented. With this technique, we were able to accelerate our detection method firstly presented in for vertical narrow defects by factor three. Generally, we believe that this technique opens up similar opportunities than in other NDE methods. High-resolution ultrasound, for example, is also based on the superposition of single emitters and a recent concept suggests an option to deal with the diffusion wave character of the thermal waves. T2 - 62. International School of Quantum Electronics die Tagung “Progress in Photoacoustic & Photothermal Phenomena” CY - Erice, Italy DA - 06.09.2018 KW - Thermal wave KW - Thermal wave field KW - Thermal engineering KW - Structured laser illumination KW - 1d laser KW - Laser array KW - Laser thermography PY - 2018 AN - OPUS4-46193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hollamby, M. J. T1 - Formation and magnetic alignment of a photoconductive organogel formed by an alkyl-C60 hydrophobic amphiphile N2 - The formation and alignment of gel fibres in alkanes (solvents) was investigated. The gel fibres consist of small amphiphilic molecules containing a C60 molecule and a small ligand chain. Under the right conditions, these self-assemble in core-shell micelles, which themselves pack into micron-sized fibre-like structures. These can be aligned using a strong magnetic field, as investigated using SANS with a 17T superconducting magnet at a range of field strengths. T2 - 7th EuCheMS Chemistry Congress CY - Liverpool, UK DA - 26.08.2018 KW - Small-angle scattering KW - Alignment KW - SANS KW - SAXS PY - 2018 AN - OPUS4-46101 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bernegger, Raphael T1 - Quantitative determination of the geometry of defects by pulse thermography N2 - Pulsed thermography is a well-known non-destructive testing technique and has proven to be a valuable tool for examination of material defects. Material defects are often simulated by flat-bottom holes (FBH) or grooves. Typically, analytical 1D models are used to determine the defect depth of FBHs, grooves or delaminations. However, these models cannot take into account lateral heat flows, or only to a limited extent (semi-empirical model). They are therefore limited by the FBHs aspect ratio (diameter to remaining wall thickness), to ensure that the heat flow above the defect can still be described one-dimensionally. Here, we present an approach for quantitative determination of the geometry of FBH or grooves. For this purpose, the results of a numerical 2D model are fitted to experimental data, e.g., to determine simultaneously the defect depth of a FBHs or groove and its diameter or width, respectively. The model takes lateral heat flows into account as well as thermal losses. Figure 1 shows the temperature increase of a pulsed thermography measurement at three different locations on the sample. The numerical model is fitted to the experimental data (red lines) to quantify the groove. The numerical simulation matches the experimental data well. T2 - Progress in Photoacoustic & Photothermal Phenomena CY - Erice, Italy DA - 06.09.2018 KW - Pulse thermography KW - Numerical modelling KW - 2D model KW - Data reconstruction KW - Flat bottom holes KW - Notches KW - Opaque materials PY - 2018 AN - OPUS4-46103 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lemke, Nora T1 - Protein quantification of an Alzheimer’s biomarker via isotope dilution inductively coupled plasma mass spectrometry N2 - Neurodegenerative diseases are one of the major problems for our ageing society. Alzheimer’s disease (AD) as the most common neurodegenerative disorder affects over 46.8 million people worldwide and the number will increase as the population ages. The diagnosis of AD is challenging and only half of the patients are identified yet and often only in late stages. One reason is that existing assays for identification and quantification of AD biomarkers lack accuracy and are poorly comparable. This study is part of the EU project “ReMiND” aiming to develop accurate, reliable and traceable methods for the detection and quantification of known and suspected AD biomarkers. Our target is the tau protein, as brain load and distribution of tau is highly correlated with the clinical progression of AD. We intend to develop a measurement method for the accurate quantification of tau by means of inductively coupled plasma mass spectrometry (ICP-MS). ICP-MS is a powerful method for the matrix independent quantitative analysis of target elements. Developed for the use in inorganic trace analysis, ICP-MS is nowadays emerging as a valuable tool for bioanalytical questions. Especially the use of ICP-MS for quantitative proteomics by measuring heteroatoms is highly promising, considering that established quantification methods like organic mass spectrometry depend on the existence of matched protein and peptide standards or labelling of the target protein. In this work, we applied isotope dilution analysis (IDA) using ICP-MS to quantify proteins of known stoichiometry via their sulphur content. Sulphur is present in two amino acids, cysteine and methionine, and hence is omnipresent in nearly all proteins. A NIST standard bovine serum albumin (BSA) was quantified using sulfur IDA to optimize sample preparation and method parameters. Our goal is to employ the developed method in a proof of concept study for the quantification of the AD biomarker tau extracted from brains of a mouse model for AD. T2 - 26. ICPMS-Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - ICP-MS KW - Isotope dilution KW - Protein analysis PY - 2018 AN - OPUS4-46585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Anforderungen der Prozessindustrie an Gerätekommunikation N2 - Der Vortrag gibt einen Überblick über die aktuellen Diskussionen zu Feldgerätekommunikation in der Prozessindustrie. Diese verfolgt seitens der Anwender in der NAMUR das NOA-Konzept (NOA = NAMUR Open Architecture). In gemeinsamen Aktivitäten mit dem ZVEI werden mit Zielstellung Mitte/Ende 2019 folgende Konzepte vorangebracht: NOA Informationsmodell in OPC UA, Informationssicherheit und das Konzept des „Verification of Request“. Gemeinsam mit Geräte- und Softwareherstellern sollen auch M+O-Sensoren (Maintenance und Optimization) konzipiert werden. Aus dem NAMUR AK 3.7 heraus wurde im Oktober ein Erweiterter Arbeitskreis „Smarte Sensoren, Aktoren und Kommunikation“ kontituiert, dem auch Geräte- und Softwarehersteller und das BSI angehören. Hier werden konkrete Anwendungsfälle für smarte Feldgeräte und Anforderungen an M+O-Sensoren erarbeitet, um die Bereitstellung und den Einsatz smarter Automatisierungskomponenten zu beschleunigen. Zukünftig werden das „Smarte Labor“ und die „Smarte Produktion“ stärker zusammenwachsen. T2 - 5. Sitzung Projektgruppe „Vernetzte Laborgeräte“ SPECTARIS e.V., Berlin CY - Berlin, Germany DA - 14.11.2018 KW - Prozessindustrie KW - Digitalisierung KW - Industrie 4.0 KW - NAMUR Open Architecture (NOA) KW - M+O-Sensoren KW - Spectaris PY - 2018 AN - OPUS4-46586 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Unger, Wolfgang T1 - New work item proposal for a technical report for ISO/TC 201 WG4 “Surface characterization of biomaterials”: Surface chemical analysis – Surface chemical analysis of cells and biofilms N2 - The proposed ISO Technical Report provides a description of a variety of physical methods of analytical chemistry by which bacteria and biofilms can be analysed. The state of the art, sample requirements and strengths associated with each method are identified. Presented at the DIN-meeting for NA 062-08-16 AA „Chemische Oberflächenanalyse und Rastersondenmikroskopie“ T2 - 18. Sitzung des DIN-meeting NA 062-08-16 AA "Chemische Oberflächenanalyse und Rastersondenmikroskopie“ CY - Berlin, Germany DA - 08.11.2018 KW - 3D nano SIMS KW - Fourier transform infrared spectroscopy KW - Raman-spectroscopy KW - Biofilms KW - XPS PY - 2018 AN - OPUS4-46548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Measurement of the thickness and nature of nanoparticle coatings - ISO/PWI TR 23173 N2 - This presentation explains the outline and scientific content of the ISO technical report 23173 "Measurement of the thickness and nature of nanoparticle coatings using electron spectroscopies". This technical report deals with those electron spectroscopy methods that are able to determine the coating thickness of nanoparticles. This specifically includes X-ray photoelectron spectroscopy (XPS), energy-resolved X-Ray photoelectron spectroscopy (ERXPS) using synchrotron radiation, near abient pressure photoelectron spectroscopy (NAPXPS) and Auger electron spectroscopy (AES). T2 - 18. Sitzung des DIN-Normenausschusses 062-08-16 AA CY - Berlin, Germany DA - 08.11.2018 KW - Core-shell nanoparticles KW - Electron spectroscopy KW - XPS KW - Synchrotron radiation KW - AES PY - 2018 AN - OPUS4-46550 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg T1 - Optischer Ansatz zur Bestimmung von Materialeigenschaften und Schichtstrukturen N2 - THz-TDS Systeme können zeitaufgelöst die Amplitude der elektrischen Feldstärke E(t) detektieren. Der Vorteil des verwendeten Messprinzips besteht in dem gleichzeitigen Nachweis von Amplitude und Phase des zwischen der Antenne und dem Detektor sich ausbreitenden elektrischen Feldes eines Impulses. Befindet sich im Strahlengang dielektrisches Material, dann ändern sich die Laufzeit (Time of Flight) und Amplitude des Impulses im Vergleich zum freien Strahlengang. Planare Fehlstellen, wie Risse oder delaminierte Schichten in Kompositen sowie mehrschichtig aufgebaute Dielektrika können als optische Mehrschichtsysteme aufgefasst werden, mit denen sich die beobachteten Transmissions- und Reflektionseigenschaften im THz-Bereich erklären lassen. Bei Entwicklung eines optischen Schichtenmodells für das jeweilig ausgewählte Schichtensystem lassen sich zeitliche Impulsverläufe in Abhängigkeit von der Schichtenfolge- und deren –dicke berechnen. Durch den Fit der experimentell gewonnener Daten mit den aus dem Schichtenmodell berechneten Impulssequenzen lassen sich unter Verwendung der Methode der kleinsten Quadrate Schichtdicken oder die Brechungsindizes der einzelnen Schichten im jeweiligen Testobjekt bestimmen. Anhand eines repräsentativen Beispiels wird die Entwicklung des Schichtenmodells erklärt und die erreichten Genauigkeiten zur Bestimmung der Schichtdicken und Brechungsindizes anhand selbst entwickelter Testkörper diskutiert. T2 - Workshop „Wertschöpfungspotential der neuen Mikrowellen- und Terahertz-Sensorik in der Kunststoffindustrie" CY - Würzburg, Germany DA - 07.11.2018 KW - Dickenmessung, KW - Zeitaufgelöste THz-Spektroskopie PY - 2018 AN - OPUS4-46629 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziegler, Mathias A1 - Thiel, Erik T1 - Wenn die Wärme Wellen schlägt N2 - Mit Laserlicht kann man eine Materialoberfläche berührungslos und schnell moduliert aufheizen. Dabei entsteht eine stark gedämpfte Wärmewelle, die tief ins Material eindringen kann. Erzeugt und überlagert man solche thermischen Wellen auf kohärente Weise, dann kann man damit versteckte Materialfehler zerstörungsfrei und sehr präzise aufspüren. Sogar eine bildgebende Tomografie ist denkbar. KW - Thermography KW - Laser thermography KW - Lock-in thermography KW - NDT KW - Thermal waves PY - 2018 DO - https://doi.org/10.1002/piuz.201801512 SN - 0031-9252 VL - 49 IS - 6 SP - 296 EP - 303 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-46630 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg T1 - Hat die Nutzung der Terahertz-Strahlung eine Zukunft in der Zerstörungsfreien Prüfung? N2 - Die zeitaufgelöste THz-Spektroskopie (THz-TDS) ist eine relativ junge Technologie, die im Bereich der Zerstörungsfreien Werkstoffprüfung (ZfP) seit einiger Zeit genutzt wird. Es werden die neusten Entwicklungen in Verbindung mit deren Perspektiven in der ZfP vorgestellt und diskutiert. T2 - DGZfP Arbeitskreis Zwickau-Chemnitz CY - Ackerbürgersaal am Kornmarkt 5, Zwickau, Germany DA - 16.10.2018 KW - Zeitaufgelöste THz Spektroskopie KW - ZfP 4.0 PY - 2018 AN - OPUS4-46637 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - Distance maps and Avizo workflows for impact damage characterisation in composite panels N2 - During their life cycle, composite structures used in aircraft structures can be subjected to high- and low-velocity impact loading. High velocity impact damage is usually easy to detect as it creates visible external damage. Low-velocity impacts are more complex to assess because, although significant damage can be generated internally, there can be little indication of external damage on the impacted surface, leading to the term BVID. Impact damage, especially barely visible impact damage, is therefore of primary concern for design and maintenance of modern aircraft composite structures. As a result there is a concerted research effort to improve the damage resistance and tolerance of these materials. One of the great strengths of X-ray computed tomography over conventional inspection methods (ultrasound, thermography, radiography) is that it can image damage in 3D. or inter-ply interfaces. An X-ray computed tomography (CT) data processing methodology is developed to extract the through-thickness distribution of damage in curved or deformed composite panels. The method is applied to [(0°/90°)2]s carbon fibre reinforced polymer (CFRP) panels subjected to low velocity impact damage (5 J up to 20 J) providing 3D ply-by-ply damage visualisation and analysis. Our distance transform approach allows slices to be taken that approximately follow the composite curvature allowing the impact damage to be separated, visualised and quantified in 3D on a ply-by-ply basis. In this way the interply delaminations have been mapped, showing characteristic peanut shaped delaminations with the major axis oriented with the fibres in the ply below the interface. This registry to the profile of the panel constitutes a significant improvement in our ability to characterise impact damage in composite laminates and extract relevant measurements from X-ray CT datasets. T2 - Avizo/Amira User group meeting CY - Berlin, Germany DA - 14.11.2018 KW - Impact damage KW - Damage histogram KW - Damage correlation map KW - Composite panel KW - X-ray computed tomography PY - 2018 AN - OPUS4-46598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Millar, Steven A1 - Gottlieb, Cassian A1 - Sankat, Nina A1 - Wilsch, Gerd A1 - Kruschwitz, Sabine T1 - Chlorine determination in cement-bound materials with Laser-induced Breakdown Spectroscopy (LIBS) – A review and validation N2 - The determination of chloride is still one of the main tasks for the evaluation of reinforced concrete structures. The corrosion of the reinforcement induced by the penetrating chlorides is the dominant damage process affecting the lifetime of concrete structures. In the recent years different research groups demonstrated that LIBS can be a fast and reliable method to quantify chlorine in cement-bound materials. Because chlorine in concrete can only occur as solved ions in the pore solution or bound in salts or hydrated cement phases, the detected emission of chlorine can be correlated with the chloride concentration determined e.g. with potentiometric titration. This work inter alia describes the production of reference samples and possible side effects during the production process. Due to transport processes in the porous matrix of the cement a misinterpretation of the concentrations is possible. It is shown how to overcome these effects and higher precisions of the single measurements can be realised. Using the calibration method, blank sample method and noise method, three different ways of calculating the limit of detection (LOD) and limit of quantification (LOQ) are compared. Due to the preparation of the reference samples a precision of the whole calibration model of sx0 = 0.023 wt% is determined. The validation of the model is based on different test sets, which are varying in their composition (different Cl-salts, water-to-cement ratios and additives). The determined mean error of the validation is 0.595 ± 0.063 wt%, which is comparable to standardised methods like potentiometric titration, direct potentiometry or photometry (0.40 ± 0.06 wt%) [1]. KW - LIBS KW - Chlorine KW - Cement KW - Calibration KW - Validation PY - 2018 DO - https://doi.org/10.1016/j.sab.2018.05.015 SN - 0584-8547 VL - 147 IS - September SP - 1 EP - 8 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-46558 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Smarte Feldgeräte – Nur "Smartisiert" oder Echte Chance für die Zukünftige Automatisierung? N2 - Um in einem veränderten Umfeld erfolgreich bestehen zu können, müssen Chemieunternehmen neue Pfade beschreiten. Dazu gehört insbesondere das Potential digitaler Technologien. Die volle Integration und intelligente Vernetzung von Systemen und Prozessen kommt zögerlich voran. Dieser Vortrag ist ein Loblied auf die Feldebene. Er möchte dazu ermutigen, die Digitalisierung der Prozessindustrie auf Basis smarter Sensorik, Aktorik und Kommunikation ganzheitlicher zu denken und informiert über aktuelle technische Perspektiven, wie das „Ein-Netzwerk-Paradigma“, Ad-hoc-Vernetzungen, Edge-Computing, FPGAs, virtuelle Maschinen oder Blockchain. Diese geben smarter Sensorik, Aktorik und Kommunikation eine völlig neue Perspektive. N2 - To successfully survive in a changing environment, chemical companies must find new paths. The potential of digital technologies belongs to these. A full integration and intelligent interconnection of systems and processes progresses only hesitantly. This talk is a hymn on the field level. It should encourage to think digitization of process industry based on smart sensors, actuators, and communication more comprehensively and informs about current technical perspectives such as the “one-network paradigm”, ad-hoc connections, edge computing, FPGAs, virtual machines and blockchain. These give smart sensors, actuators, and communication a new perspective. T2 - Smart Field Devices – Just „smartified“ or a Real Chance for Future Automation? T2 - NAMUR Hauptsitzung 2018 CY - Bad Neuenahr, Germany DA - 08.11.2018 KW - Smarte Feldgeräte KW - Sensorik KW - Digitalisierung KW - Edge Computing KW - Dezentrale Netzwerke KW - NAMUR PY - 2018 AN - OPUS4-46559 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel A1 - Wendland, Saskia A1 - Gaal, Mate T1 - Airborne testing of molded polymer compounds N2 - Modern and energy-efficient materials are essential for innovative designs for aerospace and automotive industries. Current technologies for rapid manufacturing such as additive manufacturing and liquid composite moulding by polymer Extrusion allow innovative ways of creating robust and lightweight constructions. Commercially available printing devices often use polylactide (PLA) or acrylonitrile butadiene styrene (ABS) as raw material. Therefore, parameters like the infill ratio, influencing the ability to resist mechanical stress, may have a beneficial impact on the lifetime of components. These manufacturing technologies require a good knowledge about materials and even adapted non-destructive testing technologies and methods. Airborne ultrasonic testing has beneficial advantages for testing those lightweight constructions. It is a contact-free testing method, which does not require a liquid couplant. Therefore, it allows fast test cycles without any unwanted alternations of the material properties due to interactions with any coupling liquid. This contribution deals with the characterisation of printed specimens based on PLA by using airborne ultrasound and presents the current edge of non-destructive testing and evaluation using airborne ultrasonic transducers. The specimens, manufactured by polymer extrusion, are printed as thin plates. The infill ratio, as well as the material thickness, were varied to model density imperfections with different geometric shapes and properties. For better understanding of the limits of airborne ultrasonic testing in transmission, we compared own-developed transducers based on different physical principles: on ferroelectrets, on the thermoacoustic effect, as well as a new type of transducers based on gas discharges. T2 - 10th International Symposium on NDT in Aerospace CY - Dresden, Germany DA - 24.10.2018 KW - Air-coupled ultrasonic testing KW - Polymer KW - Plasma acoustics KW - Gas discharges KW - Atmospheric pressure plasma PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-465609 VL - 168 SP - Th.6.C.1, 1 EP - 7 AN - OPUS4-46560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Atmospheric pressure gas discharges and their acoustic emissions N2 - Overview about modelling, simulations and measurement of acoustic interactions caused by surface dielectric barrier discharges, micro hollow cathode discharges and plasma jets. T2 - Workgroup seminar on plasma physics and technology CY - Kiel, Germany DA - 25.10.2018 KW - Atmospheric pressure plasma KW - Gas discharges KW - Plasma acoustics KW - Plasma jet KW - Dielectric barrier discharge KW - Micro hollow cathode discharge PY - 2018 AN - OPUS4-46561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Nanoanalytik-Aktivitäten @ BAM N2 - In dieser Präsentation werden Aktivitäten im Bereich der 'nano'-Charakterisierung bei der BAM vorgestellt. Beispiele von F&E-Projekten und -Kooperationen im nano-Analytik-Bereich bei der BAM werden genannt. Thematische Kooperations-Möglichkeiten zwischen BAM und dem Netzwerk NanoAnalytik und -Messtechnik in der Produktion werden diskutiert. T2 - Treffen des Netzwerkes NanoAnalytik und -Messtechnik CY - Berlin, Germany DA - 06.11.2018 KW - Nanoanalytik KW - Nano-Projekte KW - Nano-Kompetenzzentrum KW - Nano-Charakterisierung PY - 2018 UR - https://www.nanoinitiative-bayern.de/nanoanalytik/ AN - OPUS4-46563 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin T1 - Accelerating chemical process development and manufacturing – Design and validation of an integrated NMR micro mixer N2 - The future competitiveness of the process industry and their providers depends on its ability to deliver high quality and high value products at competitive prices in a sustainable fashion, and to adapt quickly to changing customer needs. The transition of process industry due to the mounting digitalization of technical devices and their provided data used in chemical plants proceeds. Though, the detailed characteristics and consequences for the whole chemical and pharmaceutical industry are still unforeseeable, new potentials arise as well as questions regarding the implementation. As the digitalization gains pace fundamental subjects like the standardization of device interfaces or organization of automation systems must be answered. Still, process industry lack of sufficient system and development concepts with commercial advantage from this trend. Intensified continuous processes are in focus of current research. Compared to traditional batch processes, intensified continuous production allows new and difficult to produce compounds with better product uniformity and reduced consumption of raw materials and energy. Flexible (modular) chemical plants can produce various products using the same equipment with short down-times between campaigns, and quick introduction of new products to the market. Full automation is a prerequisite to realize such benefits of intensified continuous plants. In continuous flow processes, continuous, automated measurements and closed-loop control of the product quality are required. Consequently, the demand for smart sensors, which can monitor key variables like component concentrations in real-time, is increasing. Low-Field NMR spectroscopy presents itself as such an upcoming smart sensor (as addressed, e.g., in the CONSENS project – http://www.consens-spire.eu/). Systems utilizing such an online NMR analyzer benefits through short development and set-up times when applied to modular production plants starting from a desired chemical reaction. As an example for such a modular process unit, we present the design and validation of an integrated NMR micro mixer based on computational modelling suited for a desired chemical reaction. This method includes a proper design of a continuous reactor, which is optimized through computational fluid dynamics (CFD) for the demands of the NMR sensor as well as for the given reaction conditions. The system was validated with a chemical reaction process. T2 - ProcessNet PAAT Jahrestreffen CY - Cologne, Germany DA - 12.11.2018 KW - NMR KW - Reaction monitoring KW - Digital twin KW - Flow chemistry KW - Process analytical technology PY - 2018 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-46579 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Analysis of the operation of accreditation bodies in Europe N2 - The presentation gives an overview of the PMBT-Management tool and ist first application with eight European accreditation bodies. T2 - EUROLAB TCQA Meeting 2018 CY - Berlin, Germany DA - 15.11.2018 KW - Accreditation KW - EFQM Excellence Model KW - Benchmarking PY - 2018 AN - OPUS4-46613 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Pérez Alonso, M. A1 - Albarrán Sanz, J. A1 - Dinkel, M. A1 - Heckel, Thomas A1 - Kotschate, Daniel A1 - Cabeza, Sandra A1 - Senaneuch, J. A1 - Heikkila, I. A1 - Toscanelli, O. T1 - A novel approach for rating fatigue-initiating inclusions in highly demanding steel (INCAFAT) N2 - INCAFAT project aimed to improve existing fatigue damage models by establishing the most suitable combination of measurement techniques to characterise harmful inclusion populations in highly demanding steels. The different inclusion assessments carried out confirm that, chemical composition, secondary metallurgy and manufacturing route affect content, nature, size and shape of inclusions. According to the FEM model, inclusions produce an alteration of the stress field in their surrounding region, which can promote a fatigue failure. Experimental work on fatigue testing has demonstrated that depending on the stressed direction fatigue failures in highly demanding steels could be produced by different types of inclusions. Fractography analyses confirmed that meso-inclusions harmful in fatigue cannot be rated by standard methods, nor 10 MHz ultrasonic testing (macro) or micro-cleanness assessments. The necessity of rating these meso-inclusions has led to critical evaluation of Extreme Value Analysis according to ASTM E2283-08 and the development of high frequency immersion ultrasonic testing. EVA methodology based on inclusion width can be applied reliably when principal stress is parallel to the rolling direction. On the contrary, if inclusions are testing in the elongated directions its fails. On the other hand, the guidelines and recommendations for high frequency ultrasonic testing have been compiled in a new European standard draft. This method based on focal beam probes and high-resolution devices is able to provide information on meso-inclusion distribution. KW - Material characterisation KW - Non-destructive testing KW - Ultrasonic testing KW - Cleanliness PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479219 UR - https://publications.europa.eu/en/publication-detail/-/publication/6bd25206-316a-11e8-b5fe-01aa75ed71a1/language-en/format-PDF/source-68610160 SN - 978-92-79-76985-6 DO - https://doi.org/10.2777/473350 SN - 1831-9424 SN - 1018-5593 SP - 1 EP - 154 AN - OPUS4-47921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sargent, M A1 - Goenaga-Infante, H A1 - Inagaki, K A1 - Ma, L A1 - Meija, J A1 - Pramann, A A1 - Rienitz, O A1 - Sturgeon, R A1 - Vogl, Jochen A1 - Wang, J A1 - Yang, L T1 - The role of ICP-MS in inorganic chemical metrology N2 - ICP-MS has played a key role in inorganic chemical metrology for 25 years, from the 1993 CIPM feasibility study which led to establishment of the CCQM. Since that time, the Inorganic Analysis Working Group of the CCQM has organised 56 international comparisons involving measurements by ICP-MS and, in a recent comparison, 16 different national institutes submitted their results using the technique. Metrological applications of ICP-MS currently address an enormous range of measurements using a wide variety of instrumentation, calibration strategies and methodologies. This review provides an overview of the ICP-MS field with an emphasis on developments which are of particular relevance to chemical metrology. Examples from CCQM comparisons and the services available from the participants are used to illustrate how the capability and scope of ICP-MS methods have expanded far beyond the expectations of 1993. This is due in part to the research and development Programmes of the national institutes which participate in the CCQM. They have played a key role in advancing new instrumentation and applications for elemental analysis, isotope dilution mass spectrometry, determination of isotopic ratio or composition, and speciation of organometallic compounds. These developments are continuing today, as demonstrated by work in new fields such as heteroatom quantitation of proteins, characterisation and counting of nanoparticles using spICP-MS, and LA-ICP-MS analysis of solid materials. KW - CCQM KW - Metrology KW - Interlaboratory comparison KW - ICP-MS KW - Mass spectrometry KW - Hyphenated KW - Isotope ratio PY - 2019 DO - https://doi.org/10.1088/1681-7575/ab0eac VL - 56 IS - 3 SP - 034005 PB - IOP Publishing AN - OPUS4-47929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Realization of SI traceability for Mg isotope amount ratios & delta values N2 - In isotope ratio applications metrological principles such as measurement uncertainty and SI traceability often are not considered or realized. This is also well-documented by the traceability exception related to delta scale isotope ratio measurements CCQM requested from the CIPM. Generally, delta scale isotope ratio measurements can be performed on a precision level that is significantly lower than the uncertainty level of isotope amount ratio measurements. In the case of magnesium, we demonstrated for the first time that isotope amount ratios can be measured with uncertainties close to the typical precision of magnesium delta values, δ26/24Mg, which are at the 0.1 ‰ level. In the past, δ26/24Mg measurements were referenced to NIST SRM 980, the initial zero of the δ26/24Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of NIST SRM 980 became apparent and NIST SRM 980 was replaced by an intermediate artefact, DSM3. To solve this problem a suite of magnesium isotope reference materials, ERM-AE143, -AE144, and -AE145, has been certified in a first study by applying an ab initio calibration for absolute Mg isotope ratios without any a priori assumptions, a procedure which fulfils all requirements of a primary method of measurement. Thus, these materials qualified to establish SI-traceability for magnesium delta measurements. In a second study five expert laboratories participated to cross-calibrate all available magnesium isotope standards, which are NIST SRM 980, IRMM-009, ERM-AE143, ERM-AE144, ERM-AE145 and the standards DSM3 and Cambridge-1. The mean δ26/24Mg values for the individual iRMs, calculated from the laboratory means show 2 SD reproducibilities varying between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1 ‰ for δ26/24Mg determinations. Thus, SI traceability for magnesium isotope amount ratios and delta values is demonstrated to be established. T2 - CCQM Workshop on "Advances in Metrology in Chemistry and Biology" CY - Sèvres, France DA - 09.04.2019 KW - Delta values KW - SI traceability KW - Isotope amount ratio KW - Magnesium PY - 2019 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. AN - OPUS4-47930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt (RUSEKU) N2 - Im Rahmen des Statuskonferenz der BMBF Fördermassnahme wurde über den Projektfortschritt berichtet. T2 - Statusfonferenz der BMBF Fördermassnahme "Plastik in der Umwelt" CY - Berlin, Germany DA - 09.04.2019 KW - Sedimenttaionskasten KW - Probenahme KW - Mikroplastik KW - TED-GC-MS PY - 2019 AN - OPUS4-47796 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Mikroplastik Analytik: Probennahme, Probenaufbereitung, Detektionsverfahren N2 - Das Diskussionspapier zur Mikroplastik Analytik wurde vorgestellt. Es entstand im Rahmen des Querschnitthemas 1 des BMBF Forschungsschwerpunktes Plastik in der Umwelt. T2 - Statuskonferenz der BMBF Fördermassnahme "Plastik in der Umwelt" CY - Berlin, Germany DA - 09.04.2019 KW - Harmonisierung KW - Mikroplastik KW - Probenahme KW - Detektion KW - Aufbereitung PY - 2019 AN - OPUS4-47797 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hüllmann, Dino A1 - Bartholmai, Matthias A1 - Tiebe, Carlo T1 - Concept of a gas-sensitive nano aerial robot swarm for indoor air quality monitoring N2 - In industrial environments, airborne by-products such as dust and (toxic) gases, constitute a major risk for the worker’s health. Major changes in automated processes in the industry lead to an increasing demand for solutions in air quality management. Thus, occupational health experts are highly interested in precise dust and gas distribution models for working environments. For practical and economic reasons, high-quality, costly measurements are often available for short time-intervals only. Therefore, current monitoring procedures are carried out sparsely, both in time and space, i.e., measurement data are collected in single day campaigns at selected locations only. Real-time knowledge of contaminant distributions inside the working environment would also provide means for better and more economic control of air impurities. For example, the possibility to regulate the workspace’s ventilation exhaust locations can reduce the concentration of airborne contaminants by 50%. To improve the occupational health and safety of (industrial) workplaces, this work aims for developing a swarm of gas-sensitive aerial nano robots for monitoring indoor air quality and for localizing potential emission sources. T2 - NetMon International training course - Low-cost Environmental Monitoring CY - BAM, Berlin, Germany DA - 09.04.2019 KW - Gas sensing KW - Mobile Robot Olfaction KW - Nano aerial robot KW - Swarm PY - 2019 AN - OPUS4-47799 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Bosse, H. ED - Buhr, E. ED - Dziomba, T. ED - Hodoroaba, Vasile-Dan ED - Klein, T. ED - Krumrey, M. T1 - NanoWorkshop 2018: Workshop on Reference Nanomaterials N2 - The Scope of the Workshop was to provide a forum for discussion on progress in development, characterisation and application of reference nanomaterials. Results of recently finsihed national and international research projects have been presented. Moreover, the need for future developments have been addressed. Attendees of teh Workshop were expected to be experts from academia, research institutes, regulatory bodies and industry working or interested in the area of reference nanomaterials. The following structure of Workshop was planned: the main focus of the first day was on reference material needs and development, while teh second day was focussed on reference materials characterisation and standardisation. Over 111 participants frm 13 countries and teh European Joint Research Centre have regsitered for the Workshop with 16 platform presentations and 42 poster contributions grouped in 2 sessions and 10 topical areas. A summary of the observations, analysis and conclusions of the Workshop is made including an overview table of links to information on existing reference nanomaterials. KW - Reference Nanomaterials KW - Nanometrology KW - Standardization KW - Nanoparticle Characterization KW - Comparability of Measurement Results KW - Nanomaterial Properties PY - 2019 SN - 78-3-95606-440-1 DO - https://doi.org/10.7795/110.20190412 SN - 0179-0609 VL - 2018 SP - 1 EP - 315 PB - Physikalisch-Technische Bundesanstalt CY - Braunschweig AN - OPUS4-47861 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hampel, Marco A1 - Schenderlein, Matthias A1 - Schary, Christian A1 - Dimper, Matthias A1 - Özcan Sandikcioglu, Özlem T1 - Efficient detection of localized corrosion processes on stainless steel by means of scanning electrochemical microscopy (SECM) using a multi-electrode approach N2 - High resolution analysis of corrosion processes on stainless steels is a challenging task. The application of local electrochemical techniques such as scanning electrochemical microscopy (SECM) has opened new possibilities for the detection of corrosion products and activity on metallic surfaces. However, due to its stochastic nature, the analysis of pitting corrosion requires being at the right place at the right time. Scanning over large areas at a high resolution not only leads to long scan durations but also leaves many short-lived processes undetected. In this paper we present the combined automated operation of SECM and wire multi-electrodes connected to a multi-electrode analyzer (MMA). The inter-electrode currents between 25 wire electrodes connected via zero resistance ammeters (ZRA) are measured by the MMA at open circuit potential (OCP) and the electrodes reporting anodic currents are detected automatically to be analyzed by means of SECM. The results demonstrate the successful application of this methodology for the detection of unstable and stable pitting processes on 304 stainless steel in a corrosive aqueous environment. KW - Scanning electrochemical microscope (SECM) KW - Localised corrosion KW - Corrosion monitoring PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-478646 DO - https://doi.org/10.1016/j.elecom.2019.02.019 VL - 101 SP - 52 EP - 55 PB - Elsevier B.V. AN - OPUS4-47864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schwaar, Timm A1 - Lettow, Maike A1 - Remmler, Dario A1 - Börner, H. G. A1 - Weller, Michael G. T1 - Efficient Screening of Combinatorial Peptide Libraries by Spatially Ordered Beads Immobilized on Conventional Glass Slides N2 - Screening of one-bead-one-compound (OBOC) libraries is a proven procedure for the identification of protein-binding ligands. The demand for binders with high affinity and specificity towards various targets has surged in the biomedical and pharmaceutical field in recent years. The traditional peptide screening involves tedious steps such as affinity selection, bead picking, sequencing, and characterization. Herein, we present a high-throughput “all-on-one chip” system to avoid slow and technically complex bead picking steps. On a traditional glass slide provided with an electrically conductive tape, beads of a combinatorial peptide library are aligned and immobilized by application of a precision sieve. Subsequently, the chip is incubated with a fluorophore-labeled target protein. In a fluorescence scan followed by matrix-assisted laser desorption/ionization (MALDI)-time of flight (TOF) mass spectrometry, high-affinity binders are directly and unambiguously sequenced with high accuracy without picking of the positive beads. The use of an optimized ladder sequencing approach improved the accuracy of the de-novo sequencing step to nearly 100%. The new technique was validated by employing a FLAG-based model system, identifying new peptide binders for the monoclonal M2 anti-FLAG antibody, and was finally utilized to search for IgG-binding peptides. In the present format, more than 30,000 beads can be screened on one slide. KW - Peptide library KW - HTS KW - Target KW - MALDI KW - Mass spectrometry KW - Biochip KW - Lab-on-a-Chip KW - Array KW - Screening KW - Ladder sequencing KW - Binder KW - Pharmaceutical PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-478973 UR - https://www.mdpi.com/2571-5135/8/2/11 DO - https://doi.org/10.3390/ht8020011 VL - 8 IS - 2 SP - 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-47897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stroh, Julia A1 - Ali, Naveed Zafar A1 - Maierhofer, Christiane A1 - Emmerling, Franziska T1 - Ettringite via Mechanochemistry: A Green and Rapid Approach for Industrial Application N2 - Here, we report on a first mechanochemical synthesis of ettringite, an important cement hydrate phase. The mineral compound ettringite ([Ca3Al(OH)6]2·(SO4)3·26H2O) occurs rarely in nature, but is common for cement-based materials. Ettringite has wide technical application in the ceramic and paper industry. However, its typical wet-chemical synthesis is cumbersome and produces waste water and CO2 emissions. Here, we investigate the first mechanochemical synthesis of ettringite for developing an easy and sustainable alternative for industrial application. The mechanosynthesis was monitored in situ by coupled synchrotron X-ray diffraction (XRD) and infrared thermography (IRT). The consumption of the reactants and the formation of the reaction product were monitored with time-resolved XRD. IRT showed the temperature increase based on the exothermic reaction. The reaction conversion was significantly improved changing the strategy of the mechanosynthesis from a one- to a two-step process. The latter included neat pregrinding of solid reactants followed by a delayed addition of the stoichiometric amount of water. Thus, an increase of reaction conversion from 34 to 94% of ettringite could be achieved. KW - XRD KW - Mechanochemistry KW - Ettringite KW - In situ PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479016 DO - https://doi.org/10.1021/acsomega.9b00560 SN - 2470-1343 VL - 4 IS - 4 SP - 7734 EP - 7737 PB - ACS Publications CY - Washington, DC AN - OPUS4-47901 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Surov, Artem O. A1 - Vasilev, Nikita A. A1 - Churakov, Andrei V. A1 - Stroh, Julia A1 - Emmerling, Franziska A1 - Perlovich, German L. T1 - Solid Forms of Ciprofloxacin Salicylate: Polymorphism, Formation Pathways, and Thermodynamic Stability N2 - The crystallization of ciprofloxacin - an antibacterial fluoroquinolone compound - with salicylic acid resulted in the isolation of five distinct solid forms of the drug, namely, an anhydrous salt, two polymorphic forms of the salt monohydrate, methanol and acetonitrile solvates, and the salt-cocrystal hydrate. The salicylate salts were investigated by different analytical techniques ranging from powder and single crystal X-ray diffractometry, differential scanning calorimetry, thermogravimetric analysis, variable temperature powder X-ray diffraction, dynamic vapor sorption analysis, dissolution, and solubility investigations. Real-time in situ Raman spectroscopy was used to investigate the mechanochemical formation pathways of the different solid polymorphs of ciprofloxacin salicylate. The mechanism of the phase transformation between the crystalline forms was evaluated under mechanochemical conditions. It was found that the formation pathway and kinetics of the grinding process depend on the form of the starting material and reaction conditions. The analysis of the solid-state thermal evolution of the hydrated salts revealed the two-step mechanism of dehydration process, which proceeds through a formation of the distinct intermediate crystalline products. KW - Cocrystal KW - Polymorphism KW - Ciprofloxacin KW - XRD KW - DSC PY - 2019 DO - https://doi.org/10.1021/acs.cgd.9b00185 SN - 1528-7483 VL - 19 IS - 5 SP - 2979 EP - 2990 PB - American Chemical Society AN - OPUS4-47903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina T1 - New transition metal phosphonates obtained by mechanochemistry N2 - Metal phosphonates are metal-organic compounds consisting of a metal core and a phosphonate ligand. Depending on the nature of the ligand, metal phosphonates appear in different structures covering the range from molecular compounds to three-dimensional networks. Due to their structural diversity, the chemistry of metal phosphonates has gained great interest during the last decades. Metal phosphonates can be used for various applications as gas storage and separation, magnetism, and energy conversion. Especially transition metal phosphonates are promising candidates as electrocatalysts. Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. By milling the reactants, various organic, inorganic, and metal-organic compounds can be obtained in high yields. Here, we present the synthesis of different new metal phosphonates obtained by grinding of metal acetates with respective phosphonic acids. By varying the ratio of the reactants, we are able to determine the composition of the final products. The addition of small amounts of liquid to the grinding process tends to increase the product’s crystallinity. The crystal structures of the new compounds were determined from powder X-ray data. T2 - 27th Annual Meeting of the German Crystallographic Society CY - Leipzig, Germany DA - 25.03.2019 KW - Metal phosphonates KW - Mechanochemistry KW - PXRD KW - Structure solution PY - 2019 AN - OPUS4-47837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Neumann, Patrick P. A1 - Hüllmann, Dino A1 - Bartholmai, Matthias T1 - VDI/VDE 3518 Technische Richtlinie für Multigassensoren N2 - Der Beitrag präsentiert die erarbeiteten technischen Richtlinien zur Anwendung und Prüfung von Multigassensoren innerhalb der Richtlinienreihe VDI/VDE 3518 sowie in diesem Zusammenhang die Möglichkeiten der Sensorprüfung im akkreditierten Prüflabor des Fachbereichs 8.1 der BAM. Im Speziellen wird das in Kürze veröffentlichte Blatt 3 der Richtlinienreihe vorgestellt, das Bezug auf Multigassensoren für geruchsbezogene Messungen mit elektronischen Nasen nimmt. T2 - NetMon International training course - Low-cost Environmental Monitoring CY - BAM, Berlin, Germany DA - 09.04.2019 KW - Multigassensoren KW - Prüfung KW - Richtlinie PY - 2018 AN - OPUS4-47885 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraffert, K. A1 - Karg, M. A1 - Schmack, R. A1 - Clavel, G. A1 - Boissiere, C. A1 - Wirth,, Thomas A1 - Pinna, N. A1 - Kraehnert, R. T1 - Stabilization of Mesoporous Iron Oxide Films against Sintering and Phase Transformations via Atomic Layer Deposition of Alumina and Silica N2 - The stabilization of crystal phases and nanostructured morphologies is an essential topic in application-driven design of mesoporous materials. Many applications, e.g. catalysis, require high temperature and humidity. Typical metal oxides transform under such conditions from a metastable, low crystal-line material into a thermodynamically more favorable form, i.e. from ferrihy-drite into hematite in the case of iron oxide. The harsh conditions induce also a growth of the crystallites constituting pore walls, which results in sintering and finally collapse of the porous network. Herein, a new method to stabi-lize mesoporous templated metal oxides against sintering and pore collapse is reported. The method employs atomic layer deposition (ALD) to coat the internal mesopore surface with thin layers of either alumina or silica. The authors demonstrate that silica exerts a very strong influence: It shifts hematite formation from 400 to 600 °C and sintering of hematite from 600 to 900 °C. Differences between the stabilization via alumina and silica are rationalized by a different interaction strength between the ALD material and the ferrihydrite film. The presented approach allows to stabilize mesoporous thin films that require a high crystallization temperature, with submonolayer quantity of an ALD material, and to apply mesoporous materials for high temperature applications. KW - Mesoporous oxides KW - Atomic layer deposition KW - Stabilization PY - 2018 DO - https://doi.org/10.1002/admi.201800360 VL - 5 IS - 14 SP - 1800360-1 EP - 1800360-9 PB - Wiley-VCH AN - OPUS4-47869 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Schütze, A. T1 - Gas sensor characterization and calibration N2 - The lecture about gas sensor characterization and calibration contains the content of 3S: Sensitivity, selectivity and stability, sensor drift, aging and poisoning as well as gas mixing systems for laboratory and field calibration, measurement uncertainty for sensor calibration and traceable calibration of gas sensor systems. T2 - International training course - Low-cost Environmental Monitoring – from sensor principles to novel services CY - Berlin, Germany DA - 09.04.2019 KW - Measurement uncertainty KW - Gas mixing system KW - Sensor drift KW - Sensor aging and poisoning PY - 2019 AN - OPUS4-47850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Le, Quynh Hoa A1 - Bäßler, Ralph A1 - Bettge, Dirk A1 - Kratzig, Andreas A1 - Knauer, S. T1 - Factors Influencing Droplet Corrosion in Dense Phase CO2 N2 - Recent studies have shown that even at a very low concentration of impurities (less than 100 ppmv of SO2, NO2, O2 and H2O) the droplet formation and condensation of sulfuric and nitric acids in dense phase CO2 are possible and observable. To reveal the mechanism of droplet corrosion in dense phase CO2 at high pressure and low temperature, further studies on factors that affect wettability and resulting corrosion behaviors of transport pipeline steels are needed. In this study, effects of surface morphology were investigated by varying surface roughness of carbon steel coupons exposed to CO2 stream containing impurities to measure the wettability by contact angle and to observe the condensation as well as possible droplet corrosion that followed. Other considered factors were: pH of the droplet, temperature, droplet volume, and exposure time. T2 - NACE International Corrosion Conference 2019 CY - Nashville, TN, USA DA - 24.03.2019 KW - CCUS KW - Dense phase KW - CO2 KW - Droplet KW - Corrosion KW - Condensation KW - Carbon steel PY - 2019 SP - 13017-1 EP - 13017-13 PB - NACE International CY - Houston AN - OPUS4-47915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Shabanov, Sergej V. A1 - Sennikov, P. G. T1 - Equilibrium Chemistry in BCl3–H2–Ar Plasma N2 - The approach, which was developed earlier for modeling chemical reactions in laser induced plasmas, is applied to radio-frequency discharge plasmas. The model is based on the assumption that all ionization processes and chemical reactions are at local thermodynamic equilibrium. A chemical composition of an argon-hydrogen plasma with an Addition of boron trichloride is studied as a function of plasma temperature and mole ratio H2∕BCl3. It is established that more than twenty simple and composite molecules and ions can be formed in the course of chemical reactions. The results are compared with those obtained earlier by means of another equilibrium model that uses ab-initio quantum chemical computations of thermochemical and kinetic data and a 0D thermochemical quilibrium solver. KW - Modeling chemical reactions KW - Plasma physics KW - Plasma enhanced chemical vapor deposition PY - 2019 DO - https://doi.org/10.1007/s11090-019-09985-6 VL - 39 IS - 4 SP - 1087 EP - 1102 PB - Springer AN - OPUS4-47817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Geant4: A universal Monte-Carlo toolkit for Particle scattering simulations N2 - Particle scattering simulations are an useful tool to plan experiments, design detectors, estimate doses in irradiated materials and medical treatment planning. Geant4 is a Monte-Carlo toolkit for the simulation of of particles scattering in matter. Photons, electrons, ions etc can be simulated with energies in the eV to GeV range. Their interactions with matter in arbitrary scattering geometries be studied. Scattering models, cross sections and material parameters can be set to cover interactions in gas, liquid and solid state. The import of geometries from computer aided design files or the protein data base is possible. It is currently being applied in high energy and nuclear physics, accelerator and detector design, space application, dosimetry and medical sciences. In this first part of the talk a brief overview over the structure, functionality and possible applications of Geant4 will be given. In the second part an example application will be presented: The determination of the microscopic dose-damage relations in aqueous environment for electron irradiated plasmid DNA will be explained. Therefore, we combine electron scattering simulations in water with calculations concerning the movement of biomolecules to obtain the energy deposit in the biologically relevant nanoscopic volume. We present, how to combine these simulational results and experimental data via a generalized damage model to determine the microscopic dose-damage relation at a molecular level. T2 - Department 6 Seminar CY - Berlin, Germany DA - 04.04.2019 KW - Geant4 KW - Dosimetry KW - Microdosimetry KW - Radiation damage KW - Electron irradiation KW - Monte-Carlo Simulation KW - Monte-Carlo Simulations KW - DNA KW - Computer simulation KW - Geant4-DNA PY - 2019 AN - OPUS4-47819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - Distance transforms and correlation maps: advanced impact damage characterisation in composite panels N2 - One of the great strengths of X-ray computed tomography over conventional inspection methods (ultrasound, thermography, radiography) is that it can image damage in 3D. However for curved or deformed composite panels, it can be difficult to automatically ascribe the damage to specific plies or inter-ply interfaces. An X-ray computed tomography (CT) data processing methodology is developed to extract the through-thickness distribution of damage in curved or deformed composite panels. The method is applied to [(0°/90°)2]s carbon fibre reinforced polymer (CFRP) panels subjected low velocity impact damage (5 J up to 20 J) providing 3D ply-by-ply damage visualisation and analysis. Our distance transform approach allows slices to be taken that approximately follow the composite curvature allowing the impact damage to be separated, visualised and quantified in 3D on a ply-by-ply basis. In this way the interply delaminations have been mapped, showing characteristic peanut shaped delaminations with the major axis oriented with the fibres in the ply below the interface. This registry to the profile of the panel constitutes a significant improvement in our ability to characterise impact damage in composite laminates and extract relevant measurements from X-ray CT datasets. T2 - Dagstuhl Seminar 19151 Quantitative data visualisation challenge CY - Dagstuhl, Germany DA - 11.04.2019 KW - Computed tomography KW - X-ray computed tomography KW - Data processing PY - 2019 AN - OPUS4-47830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - Good practice guide on the correct choice of characterisation technique based on level of accuracy and type of measurement N2 - The characterisation of AM structures is an important aspect of the AM process, required in order to: 1. optimise the AM printing process 2. assess the quality of produced parts A wide range of characterisation techniques are available, and the selection can be complex, based on multiple factors. One output from the MetAMMi project is a good practice guide on the correct choice of characterisation technique. T2 - Workshop on additive manufacturing CY - Berlin, Germany DA - 13.05.2019 KW - X-ray computed tomography KW - Mechanical properties KW - Microstructural analysis KW - Defect detection PY - 2019 AN - OPUS4-48262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - XCT simulation: Effects of error sources on dimensional measurements for medical and standard objects N2 - The quantification of experimental and data analysis errors is most of the times jeopardised by the presence of surface roughness, waviness, as well as by typical measurement artefacts of the XCT technique (for instance refraction at sharp edges). One way to at least estimate the influence of those factors on dimensional measurements and on tolerances is to simulate them using Monte-Carlo method. An alternative strategy is to use independent knowledge (e.g. CMM data) to smoothen/calibrate/correct XCT data. T2 - Workshop on additive manufacturing CY - Berlin, Germany DA - 13.05.2019 KW - aRTist KW - Part geometry KW - Part material KW - Beam hardening KW - Partial volume effect PY - 2019 AN - OPUS4-48263 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - Digital image analysis procedures for dimension, dimensional error, and 3D bulk defect assessment N2 - XCT is a powerful technique for dimensional measurements of AM parts. AM parts pose new challenges to the metrologists and CT specialists. Robust digital image analysis have been proposed for dimensional measurements and defect detections based on experience within the MetAMMI project. T2 - Workshop on additive manufacturing CY - Berlin, Germany DA - 13.05.2019 KW - X-ray computed tomography KW - Metrology KW - Implant PY - 2019 AN - OPUS4-48264 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Paz, B. A1 - Völling, E. T1 - On the ore provenance of the Trojan silver artefacts N2 - Lead isotopes are a well-established tool to trace the geographic origin of samples and artefacts in archaeology and geochemistry. In archaeology, lead isotopes are often applied to gain information on the provenance of the used ores especially in lead and silver artefacts. The assignment of a specific and unambiguous provenance in most cases is not possible or at least hindered due to several limitations such as ore deposits overlapping in their lead isotopic composition, a large spread within one ore deposit or a missing overlap with known mining sites. Such difficult cases can only be solved by using information from sources being independent of the isotope data. This information can be of chemical nature such as concentrations of key elements or they can be of archaeological nature such as cultural or trade route information.Within this study, we combined lead isotope data of ores and artefacts with silver mass fractions in the ore deposits, Au/Ag-ratios in ores and artefacts and finally archaeological Information on the cultural context in the Mediterranean and Anatolian Region. This approach enabled us to significantly reduce the potential number of mining regions. Finally, the potential sources could be narrowed down to the three remaining locations the Central Taurus, Arap Dağ and the Eastern Troad. Beneath these three locations, the Central Taurus shows the highest probability for the geographic origin of the galena which has been used to create the Trojan silver artefacts. KW - Trojan silver artefacts KW - Priam's treasure KW - Lead isotope composition KW - Central Taurus KW - Ore provenance KW - Elemental composition PY - 2019 DO - https://doi.org/10.1007/s12520-018-0756-x SN - 1866-9557 SN - 1866-9565 VL - 11 IS - 7 SP - 3267 EP - 3277 PB - Springer Verlag AN - OPUS4-48272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roloff, Alexander A1 - Nirmalananthan-Budau, Nithiya A1 - Rühle, Bastian A1 - Borcherding, H. A1 - Thiele, T. A1 - Schedler, U. A1 - Resch-Genger, Ute T1 - Quantification of Aldehydes on Polymeric Microbead Surfaces via Catch and Release of Reporter Chromophores N2 - Aldehyde moieties on 2D-supports or microand nanoparticles can function as anchor groups for the attachment of biomolecules or as reversible binding sites for proteins on cell surfaces. The use of aldehyde-based materials in bioanalytical and medical settings calls for reliable methods to detect and quantify this functionality. We report here on a versatile concept to quantify the accessible aldehyde moieties on particle surfaces through the specific binding and subsequent release of small reporter molecules such as fluorescent dyes and nonfluorescent chromophores utilizing acylhydrazone formation as a reversible covalent labeling strategy. This is representatively demonstrated for a set of polymer microparticles with different aldehyde labeling densities. Excess reporter molecules can be easily removed by washing, eliminating inaccuracies caused by unspecific adsorption to hydrophobic surfaces. Cleavage of hydrazones at acidic pH assisted by a carbonyl trap releases the fluorescent reporters rapidly and quasi-quantitatively and allows for their fluorometric detection at low concentration. Importantly, this strategy separates the signal-generating molecules from the bead surface. This circumvents common issues associated with light scattering and signal distortions that are caused by binding-induced changes in reporter fluorescence as well as quenching dye− dye interactions on crowded particle surfaces. In addition, we demonstrate that the release of a nonfluorescent chromophore via disulfide cleavage and subsequent quantification by absorption spectroscopy gives comparable results, verifying that both assays are capable of rapid and sensitive quantification of aldehydes on microbead surfaces. These strategies enable a quantitative comparison of bead batches with different functionalization densities, and a qualitative prediction of their coupling efficiencies in bioconjugations, as demonstrated in reductive amination reactions with Streptavidin. KW - Fluorescent label KW - Surface group quantification KW - Polymer particle KW - Cleavable linker KW - Catch and release assay PY - 2019 DO - https://doi.org/10.1021/acs.analchem.8b05515 SN - 0003-2700 SN - 1520-6882 VL - 91 IS - 14 SP - 8827 EP - 8834 PB - ACS Publications AN - OPUS4-48284 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Laser induced Plasma: Modeling and diagnostics N2 - Laser-induced plasmas are widely used in many areas of science and technology; examples include spectrochemical analysis, thin film deposition, material processing, and even jet propulsion. Several topics will be addressed. First, general phenomenology of laser-induced plasmas will be discussed. Then, a chemical model will be presented based on a coupled solution of Navier-Stokes, state, radiative transfer, material transport, and chemical (Guldberg-Waage) equations. Results of computer simulations for several chemical systems will be shown and compared to experimental observations obtained by optical imaging, spectroscopy, and tomography. The latter diagnostic tools will also be briefly discussed. T2 - Lecture at the Dept of Chemistry of Czeged University (Hungary) on 31.05.2019 CY - Czeged, Hungary DA - 31.05.2019 KW - Plasma KW - LIBS KW - Plasma modeling PY - 2019 AN - OPUS4-48188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Several approaches to calibration-free LIBS: Advantages and pitfalls N2 - An overview of calibration-free laser induced breakdown spectroscopy (CF LIBS) methods is presented. Advantages and pitfalls of these methods are critically discussed. T2 - Workshop of the Spectrochemical Working Committee (SWC) of the Hungarian Academy of Sciences CY - Budapest, Hungary DA - 05.06.2019 KW - Calibration-free LIBS KW - CF LIBS algorithms PY - 2019 AN - OPUS4-48189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kowarik, Stefan A1 - Bogula, A1 - Boitano, A1 - Carla, A1 - Pithan, A1 - Schafer, A1 - Wilming, A1 - Zykov, A1 - Pithan, T1 - A novel 3D printed radial collimator for x-ray diffraction N2 - We demonstrate the use of a 3D printed radial collimator in X-ray powder diffraction and surface sensitive grazing incidence X-ray diffraction. We find a significant improvement in the overall Signal to background ratio of up to 100 and a suppression of more than a factor 3⋅10⁵ for undesirable Bragg reflections generated by the X-ray “transparent” windows of the sample environment. The background reduction and the removal of the high intensity signals from the windows, which limit the detector’s dynamic range, enable significantly higher sensitivity in experiments within sample environments such as vacuum chambers and gas- or liquid-cells. Details of the additively manufactured steel collimator geometry, alignment strategies using X-ray fluorescence, and data analysis are also briefly discussed. The flexibility and affordability of 3D prints enable designs optimized for specific detectors and sample environments, without compromising the degrees of freedom of the diffractometer. KW - 3D printing PY - 2019 DO - https://doi.org/10.1063/1.5063520 SN - 0034-6748 VL - 90 IS - 3 SP - 035102, 1 EP - 8 PB - AIP AN - OPUS4-48171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bäßler, Ralph T1 - Book review: Impedance spectroscopy - Theory, experiment and applications N2 - This textbook fulfills its dedication of being the “essential reference for the field, featuring protocols, analysis,fundamentals and the latest advances” of impedance spectroscopy to its readers. It really provides an insight in all facets of this powerful technique. It should not be missed in the bookshelf of electrochemists and all other interested researchers and engineers who want to be on the current state of this technique. KW - Impedance spectroscopy KW - Surface PY - 2019 DO - https://doi.org/10.1002/maco.201970064 SN - 1521-4176 SN - 0947-5117 VL - 70 IS - 6 SP - 1133 PB - WILEY ‐ VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-48210 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geilert, Sonja A1 - Vogl, Jochen A1 - Rosner, M. A1 - Eichert, T. T1 - Boron isotope variability related to boron speciation (change during uptake and transport) in bell pepper plants and SI traceable n(11B)/n(10B) ratios for plant reference materials N2 - Rationale: Boron (B) is an essential micronutrient in plants and its isotope variations are used to gain insights into plant metabolism, which is important for crop plant cultivation. B isotope variations were used to trace intra‐plant fractionation mechanisms in response to the B concentration in the irrigation water spanning the range from B depletion to toxic levels. Methods: A fully validated analytical procedure based on multi‐collector inductively coupled plasma mass spectrometry (MC‐ICP‐MS), sample decomposition and B Matrix separation was applied to study B isotope fractionation. The Validation was accomplished by establishing a complete uncertainty budget and by applying reference materials, yielding expanded measurement uncertainties of 0.8‰ for pure boric acid solutions and ≤1.5‰ for processed samples. With this validated procedure SI traceable B isotope amount ratios were determined in plant reference materials for the first time. Results: The B isotope compositions of Irrigation water and bell pepper samples suggest passive diffusion of the heavy 11B isotope into the roots during low to high B concentrations while uptake of the light 10B isotope was promoted during B depletion, probably by active processes. A systematic enrichment of the heavy 11B isotope in higher located plant parts was observed (average Δ11Bleaf‐roots = 20.3 ± 2.8‰ (1 SD)), possibly by a facilitated transport of the heavy 11B isotope to growing Meristems by B transporters. Conclusions: The B isotopes can be used to identify plant metabolism in Response to the B concentration in the irrigation water and during intra‐plant B transfer. The large B isotope fractionation within the plants demonstrates the importance of biological B cycling for the global B cycle. KW - isotope fractionation KW - boron KW - delta value KW - metabolism KW - bell pepper KW - SI traceability KW - measurement uncertainty PY - 2019 DO - https://doi.org/10.1002/rcm.8455 SN - 1097-0231 SN - 0951-4198 VL - 33 IS - 13 SP - 1137 EP - 1147 PB - John Wiley & Sons Ltd. AN - OPUS4-48213 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Investigations of HKUST-1 exposed to argon, pyridine, methanol and water vapor by near-ambient pressure XPS N2 - Metal-organic frameworks (MOFs) are suitable materials for gas storage of small molecules due to their nanoporous, crystalline structure. The extensively studied MOF HKUST-1 consist of Cu(II)-dimers in a paddlewheel structure, with 1,3,5-benzenetricarboxylic acid (BTC) as organic linker. Instability to humidity remains an issue for many types of MOFs, and for HKUST-1, it has been found that exposure to water vapor creates a surface barrier which reduces the gas uptake rate. Near-ambient pressure XPS (NAP-XPS) is a promising method for investigations of the stability and interaction of HKUST-1 with various gas molecules. The oxidation state of copper can be monitored before, during and after exposure to various gases. This does not only provide information on the stability of the MOFs, but also on the interaction with the gas molecules and the reversibility of the processes. NAP-XPS measurements of HKUST-1 exposed to methanol, pyridine and water vapor were performed with EnviroESCA, a laboratory NAP-XPS instrument developed by SPECS. Cu 2p, O 1s and C 1s core level spectra were acquired in pressure ranging from 10-5 to 8 mbar to assess the oxidation state of copper and the stability of the organic linker. HKUST-1 does not show interaction with pyridine, but there are indications of copper-reduction upon exposure to methanol and water vapor. Radiation induced damage is considered and two different approaches for determining the ratio of Cu(I) to Cu(II) will be discussed. T2 - Bunsentagung 2019 - 118th General Assembly of the German Bunsen Society for Physical Chemistry CY - Jena, Germany DA - 30.05.2019 KW - XPS KW - MOF KW - HKUST-1 KW - NAP-XPS KW - Metal organic frameworks PY - 2019 AN - OPUS4-48195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wahl, S. A1 - El-Refaei, S. M. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Amsalem, P. A1 - Lee, K.-S. A1 - Koch, N. A1 - Doublet, M.-L. A1 - Pinna, N. T1 - Zn0.35Co0.65O – A Stable and highly active oxygen evolution catalyst formed by zinc leaching and tetrahedral coordinated cobalt in wurtzite structure N2 - To arrive to sustainable hydrogen-based energy solutions, the understanding of water-splitting catalysts plays the most crucial role. Herein, state-of-the-art hypotheses are combined on electrocatalytic active metal sites toward the oxygen evolution reaction (OER) to develop a highly efficient catalyst based on Earth-abundant cobalt and zinc oxides. The precursor catalyst Zn0.35Co0.65O is synthesized via a fast microwaveassisted approach at low temperatures. Subsequently, it transforms in situ from the wurtzite structure to the layered γ-Co(O)OH, while most of its zinc leaches out. This material shows outstanding catalytic Performance and stability toward the OER in 1 m KOH (overpotential at 10 mA cm−2 ηinitial = 306 mV, η98 h = 318 mV). By comparing the electrochemical results and ex situ analyses to today’s literature, clear structureactivity correlations are able to be identified. The findings suggest that coordinately unsaturated cobalt octahedra on the surface are indeed the active centers for the OER. KW - Oxygen Evolution Catalyst KW - XAFS KW - Oxygen evolution reaction (OER) KW - Cobalt and zinc oxides PY - 2019 DO - https://doi.org/10.1002/aenm.201900328 SN - 1614-6832 SN - 1614-6840 VL - 9 IS - 20 SP - 1900328,1 EP - 10 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-48200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szymoniak, Paulina A1 - Li, Z. A1 - Wang, D.-Y. A1 - Schoenhals, Andreas T1 - Dielectric and flash DSC investigations on an epoxy based nanocomposite system with MgAl layered double hydroxide as nanofiller N2 - Nanocomposites based on MgAL layered double hydroxides (LDH) and an epoxy resin were prepared and investigated by a combination of complementary methods. As epoxy resin Bisphenol A diglycidyl ether (DGEBA) was used with Diethylenetriamine as curing agent. The LDH was modified with taurine, which acts as an additional crosslinking agent due to its amine groups. The epoxy resin was cured in a presence of the nanofiller, which was added to the system in various concentrations. X-ray scattering, by combination of SAXS and WAXS was used to characterize the morphology of the obtained nanocomposites. These investigations show that the filler is distributed in the matrix as small stacks of ca. 10 layers. The molecular dynamics of the system, as probe for structure, was investigated by broadband dielectric spectroscopy. In addition to the - and -relaxation (dynamic glass transition), characteristic for the unfilled materials, a further process was found which was assigned to localized fluctuations of segments physically adsorbed or chemically bonded to the nanoparticles. The dielectric -relaxation is shifted to higher temperatures for the nanocomposites in comparison to the pure material but depends weakly on the content of nanoparticles. Further, for the first time Flash DSC was employed to a thermosetting system to investigate the glass transition behavior of the nanocomposites. The heating rates were converted in to relaxation rates. For low concentrations of the nanofiller the thermal data overlap more or less with that of the pure epoxy. For higher concentrations the thermal data are shifted significantly to higher temperatures. This is discussed in terms the cooperativity approach to the glass transition. KW - Nanocomposites KW - Broadband dielectric spectroscopy KW - Flash DSC PY - 2019 DO - https://doi.org/10.1016/j.tca.2019.01.010 SN - 0040-6031 VL - 677 SP - 151 EP - 161 PB - Elsevier AN - OPUS4-48218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Shedding Light into Polymer Microstructure N2 - It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. Nowadays a wide range of different analytical separation techniques and multi-detection possibilities are available. The challenge consists in a clever combination of these techniques coordinated with the heterogeneity to be investigated. A number of applications will be presented from e.g. topology elucidation of branched EO-PO “academic” copolymers to copolymer composition of partially broadly distributed progressively tailored “industrial relevant” copolymers consisting of e.g. polyamides, polycarbonates and polysiloxanes. Multidimensional separation techniques will be demonstrated with focus on mass spectrometric detection techniques (ESI-/MALDI-TOF-MS) coupled online or semi-online to prior separation. T2 - FAST 2019, COAST Community of Innovation CY - Veldhoven, The Netherlands DA - 21.05.2019 KW - LCCC KW - Mass spectrometry of polymers KW - SEC KW - LC x MALDI/ESI-TOF-MS coupling PY - 2019 AN - OPUS4-48222 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Coupling of chromatographic and spectrometric techniques for polymer characterization N2 - Presentation of coupling of polymer chromatography and polymer mass spectrometry based on different examples. T2 - Kolloquium CY - Universität für Bodenkultur, Wien, Austria DA - 14.06.2019 KW - LCCC KW - Mass spectrometry of polymers KW - LC x MALDI/ESI-TOF-MS KW - Liquid chromatography of polymers PY - 2019 AN - OPUS4-48223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino T1 - Wind Vector Estimation on Multirotor Aircraft N2 - Small unmanned aircraft are used increasingly as flying sensor platforms to perform tasks such as gas distribution mapping or environmental monitoring. Sometimes, these applications require knowledge of the ambient wind field. In general, it would be interesting to avoid any additional hardware, both on ground and on the aircraft. Here, we present an approach to estimate the wind vector just by exploiting the state variables of the aircraft. T2 - 18th International Symposium on Olfaction and Electronic Nose (ISOEN) CY - Fukuoka, Japan DA - 26.05.2019 KW - Wind vector KW - UAV KW - Multirotor aircraft PY - 2019 AN - OPUS4-48242 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino T1 - A Realistic Remote Gas Sensor Model for Three-Dimensional Olfaction Simulations N2 - Remote gas sensors like those based on the Tunable Diode Laser Absorption Spectroscopy (TDLAS) enable mobile robots to scan huge areas for gas concentrations in reasonable time and are therefore well suited for tasks such as gas emission surveillance and environmental monitoring. A further advantage of remote sensors is that the gas distribution is not disturbed by the sensing platform itself if the measurements are carried out from a sufficient distance, which is particularly interesting when a rotary-wing platform is used. Since there is no possibility to obtain ground truth measurements of gas distributions, simulations are used to develop and evaluate suitable olfaction algorithms. For this purpose several models of in-situ gas sensors have been developed, but models of remote gas sensors are missing. In this paper we present two novel 3D ray-tracer-based TDLAS sensor models. While the first model simplifies the laser beam as a line, the second model takes the conical shape of the beam into account. Using a simulated gas plume, we compare the line model with the cone model in terms of accuracy and computational cost and show that the results generated by the cone model can differ significantly from those of the line model. T2 - 18th International Symposium on Olfaction and Electronic Nose (ISOEN) CY - Fukuoka, Japan DA - 26.05.2019 KW - Gas simulation KW - Remote gas sensor KW - TDLAS KW - Sensor model PY - 2019 AN - OPUS4-48245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hillger, W. T1 - Charakterisierung von Luftultraschallprüfköpfen mit thermoakustischen Wandlern N2 - Nicht nur die Qualitätssicherung von Bauteilen wird immer wichtiger und muss immer höheren Anforderungen entsprechen, sondern auch die dafür verwendete Prüfeinrichtung und die Sensorik. Für die Qualitätssicherung von Ultraschall-Prüfköpfen mit Luftankopplung bestand die bisherige Lösung darin, baugleiche Wandler als Aktuatoren (Referenzsender) einzusetzen. Für eine Weiterentwicklung der Wandler ist eine akustische Quelle wünschenswert, die eine weit größere Bandbreite mit flachem Frequenzgang aufweist, als die zu untersuchenden Prüfköpfe. Hier bieten sich thermoakustische Wandler an, die keine ausgeprägten Resonanzen haben und über eine hohe Bandbreite verfügen (min. 10 kHz bis 1 MHz). Diese wurden von der BAM in Berlin entwickelt und decken den Frequenzbereich von typischen Luftultraschall-Prüfköpfen vollständig ab. Der Vortag beschreibt die Besonderheiten der Ansteuerung dieser Wandler, die einen Innenwiderstand von ca. 7 Ohm besitzen und eine Pulsleistung von etwa 10 kW benötigen. Ferner werden erste Ergebnisse der Charakterisierung von unterschiedlichen piezokeramischen Prüfköpfen im Frequenzbereich von 50 kHz bis 500 kHz präsentiert. Beispielhaft zeigte ein Prüfkopf mit mehreren Anpassschichten lokale Frequenzunterschiede im Schallfeld. T2 - DACH-Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Ultrasound KW - Air coupled ultrasound KW - Thermoacoustics PY - 2019 UR - https://jahrestagung.dgzfp.de/Portals/jt2019/Dokumente/Kufa_GESAMT_klein_.pdf AN - OPUS4-48255 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred T1 - Determination of boron in 19th and 20th century paint layers using LIBS N2 - 19th and 20th centuries glass paint layers consist of a colour body and a colourless lead silicate flux, in which borax or boric acid was added as further component to improve the paint ability and to reduce the firing temperature for multiple layers of paint. Model glasses were used in laboratory tests to investigate the stability of glass paints with additions of boron oxide. To determine boron in paint layers, a LIBS-system with pulsed NdYAG-laser was used. T2 - Technart 2019 CY - Brugge, Belgien DA - 07.05.2019 KW - Stained glass windows KW - Glass paints KW - LIBS PY - 2019 AN - OPUS4-48229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Caetano, D. M. A1 - Rabuske, T. A1 - Fernandes, J. A1 - Pelkner, Matthias A1 - Fermon, C. A1 - Cardoso, S. A1 - Ribes, B. A1 - Franco, F. A1 - Paul, J. A1 - Piedade, M. A1 - Freitas, P. P. T1 - High-Resolution Nondestructive Test Probes Based on Magnetoresistive N2 - This paper discloses two high-sensitivity probes for Eddy Current Nondestructive Test (NDT) of buried and surface defects. These probes incorporate eight and 32 magnetoresistive sensors, respectively, which are optimized for high sensitivity and spatial resolution. The signal processing and interfacing are carried out by a full-custom application-specific integrated circuit (ASIC). The ASIC signal chain performs with a thermal input-referred noise of 30 nV/√Hz at 1 kHz, with 66 mW of power consumption, in a die with 3.7 × 3.4 mm 2 . NDT results are presented, showing that there is an increase in spatial resolution of surface defects when contrasted to prior art, enabling the probes to resolve defects with diameters of 0.44 mm, pitches of 0.6 mm, and minimum edge distance as low as 0.16 mm. The results also show that the probe for buried defects is a good all-round tool for detection of defects under cladding and multiple-plate flat junctions. KW - ASIC KW - Magnetoresistive sensor KW - Nondestructive testing KW - Eddy current testing KW - High resolution PY - 2019 DO - https://doi.org/10.1109/TIE.2018.2879306 VL - 66 IS - 9 SP - 7326 EP - 7337 PB - IEEE AN - OPUS4-48239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Structure analytics with Hard X-rays at the BAMline and µSpot beamlines N2 - An overview of the research areas at the structure analysis division is given. Specifically the in situ characterization of dynamic processes with hard X-ray diffraction and absorption spectroscopy at the BAMline and µSpot beamlines (BESSY-II). T2 - BAM-IFW Workshop CY - Dresden, Germany DA - 28.03.2019 KW - Structure analysis KW - X-ray Spectroscopy KW - Synchrotron KW - Beamline KW - Material characterization PY - 2019 AN - OPUS4-47695 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Plasma-akustische Wechselwirkungen von Mikrohohlkathodenentladungen N2 - Während des Entladungsprozesses interagieren Mikrohohlkathodenentladungen (engl. micro hollow cathode discharges) durch verschiedenste physikalische Phänomene mit ihrer Umgebung. Analog zu Funken- und Koronaentladung treten neben den optischen Erscheinungen auch akustische Wechselwirkungen bis in den Ultraschallbereich auf. Diese Wechselwirkungen sind bisher jedoch nur selten Gegenstand der Forschung gewesen. Durch elektro-chemischen Prozesse und die Stromdichteverteilung während des Zündvorgangs erfährt das angrenzende Fluid eine, durch den thermoakustischen Effekt hervorgerufene, rapide Dichteänderung und erzeugt somit eine akustische Emission. Dieser Beitrag gibt einen Überblick über den letzten Stand der akustischen Beschreibung der Mikrohohlkathode. Weiterhin wird anhand von Anwendungsbeispielen, wie der Charakterisierung von akustischen Sensoren, sowie der Nutzung innerhalb der zerstörungsfreien Werkstoffprüfung, die Nutzung dieser Entladungsart präsentiert. Darüber hinaus erlaubt die Kenntnis hinsichtlich der akustischen Eigenschaften der Entladung wichtige Rückschlüsse im Rahmen der Plasmadiagnostik. T2 - DAGA - Jahrestagung für Akustik CY - Rostock, Germany DA - 18.03.2019 KW - Micro hollow cathode discharge KW - Atmospheric pressure plasma KW - Acoustic emitter PY - 2019 AN - OPUS4-47601 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Plasma-akustische Wechselwirkungen von Mikrohohlkathodenentladungen N2 - Während des Entladungsprozesses interagieren Mikrohohlkathodenentladungen (engl. micro hollow cathode discharges) durch verschiedenste physikalische Phänomene mit ihrer Umgebung. Analog zu Funken- und Koronaentladung treten neben den optischen Erscheinungen auch akustische Wechselwirkungen bis in den Ultraschallbereich auf. Diese Wechselwirkungen sind bisher jedoch nur selten Gegenstand der Forschung gewesen. Durch elektro-chemischen Prozesse und die Stromdichteverteilung während des Zündvorgangs erfährt das angrenzende Fluid eine, durch den thermoakustischen Effekt hervorgerufene, rapide Dichteänderung und erzeugt somit eine akustische Emission. Dieser Beitrag gibt einen Überblick über den letzten Stand der akustischen Beschreibung der Mikrohohlkathode. Weiterhin wird anhand von Anwendungsbeispielen, wie der Charakterisierung von akustischen Sensoren, sowie der Nutzung innerhalb der zerstörungsfreien Werkstoffprüfung, die Nutzung dieser Entladungsart präsentiert. Darüber hinaus erlaubt die Kenntnis hinsichtlich der akustischen Eigenschaften der Entladung wichtige Rückschlüsse im Rahmen der Plasmadiagnostik. T2 - DAGA - Jahrestagung für Akustik CY - Rostock, Germany DA - 18.03.2019 KW - Micro hollow cathode discharge KW - Atmospheric pressure plasma PY - 2019 AN - OPUS4-47602 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Silbernagl, Dorothee A1 - Szymoniak, Paulina A1 - Hodoroaba, Vasile-Dan A1 - Sturm, Heinz T1 - The effect of boehmite nanoparticles (gamma‐AlOOH) on nanomechanical and thermomechanical properties correlated to crosslinking density of epoxy N2 - We show that complex physical and chemical interactions between boehmite nanoparticles and epoxy drastically affect matrix properties, which in the future will provide tuning of material properties for further optimization in applications from automotive to aerospace. We utilize intermodulation atomic force microscopy (ImAFM) for probing local stiffness of both particles and polymer matrix. Stiff particles are expected to increase total stiffness of nanocomposites and the stiffness of polymer should remain unchanged. However, ImAFM revealed that stiffness of matrix in epoxy/boehmite nanocomposite is significantly higher than unfilled epoxy. The stiffening effect of the boehmite on epoxy also depends on the particle concentration. To understand the mechanism behind property alteration induced by boehmite nanoparticles, network architecture is investigated using dynamic mechanical thermal analysis (DMTA). It was revealed that although with 15 wt% boehmite nanoparticles the modulus at glassy state increases, crosslinking density of epoxy for this composition is drastically low. KW - Crosslinking density KW - Epoxy KW - Intermodulation KW - Atomic force microscopy KW - Nanomechanical properties KW - Boehmite nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476050 DO - https://doi.org/10.1016/j.polymer.2018.12.054 SN - 0032-3861 SN - 1873-2291 VL - 164 SP - 174 EP - 182 PB - Elsevier AN - OPUS4-47605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul T1 - Entwicklung eines Ultraschallrohrsensors auf Basis phononischer Kristalle N2 - Die Messung von Flüssigkeitskonzentrationen in Rohrsystemen ist von großem Interesse für viele unterschiedliche Anwendungen. Die meisten Messsysteme sind jedoch nicht in der Lage, die Flüssigkeit direkt im Rohr zu untersuchen und es muss eine zusätzliche Vorrichtung, wie z.B. einem Bypass, angebracht werden, welche den Kontakt zwischen Flüssigkeit und Sensor ermöglicht. Um den Einbauaufwand gering zu halten und die Strömungseigenschaften des Rohres nicht zu beeinflussen, wird ein neuartiges Messsystem entwickelt, welches als Teil der Rohrwand ausgeführt werden kann. Dieses neuartige System ist angelehnt an die Idee der phononischen Kristallen (PnK). PnK’s bestehen im Allgemeinen aus einem Matrixmaterial, in welchem Streuzentren periodisch angeordnet sind. Dies führt beim Eintreffen einer akustischen Welle in definierten Frequenz-bereichen, sogenannter Bandlücken, zu zunehmender destruktiven Interferenz. Wird innerhalb einer solchen Bandlücke durch Einbringen einer flüssigkeitsgefüllten Kavität ein Resonanzverhalten erzeugt, kann dies genutzt werden, um die Flüssigkeit zu analysieren. Im Rahmen von Voruntersuchung wird zunächst das akustische Verhalten des PnK’s, welcher für die Sensorentwicklung genutzt werden soll, unter Vernachlässigung der Flüssigkeit ausführlich untersucht. Hierbei werden zunächst die Bandlücken ermittelt und das Übertragungsverhalten betrachtet. Dieses wird im Anschluss experimentell überprüft. Hierzu werden neben herkömmlichen Fertigungsverfahren auch additive Verfahren zur Herstellung der Proben genutzt. T2 - DAGA 2019 CY - Rostock, Germany DA - 18.03.2019 KW - Ultraschallsensor KW - Phononische Kristalle PY - 2019 AN - OPUS4-47608 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gea, M. A1 - Bonetta, S. A1 - Iannarelli, L. A1 - Giovannozzi, A. M. A1 - Maurino, V. A1 - Bonetta, S. A1 - Hodoroaba, Vasile-Dan A1 - Armato, C. A1 - Rossi, A. M. A1 - Schilirò, T. T1 - Shape-engineered titanium dioxide nanoparticles (TiO2-NPs): cytotoxicity and genotoxicity in bronchial epithelial cells N2 - The aim of this study was to evaluate cytotoxicity (WST-1 assay), LDH release (LDH assay) and genotoxicity (Comet assay) of three engineered TiO2-NPs with different shapes (bipyramids, rods, platelets) in comparison with two commercial TiO2-NPs (P25, food grade). After NPs characterization (SEM/T-SEM and DLS), biological effects of NPs were assessed on BEAS-2B cells in presence/absence of light. The cellular uptake of NPs was analyzed using Raman spectroscopy. The cytotoxic effects were mostly slight. After light exposure, the largest cytotoxicity (WST-1 assay) was observed for rods; P25, bipyramids and platelets showed a similar effect; no effect was induced by food grade. No LDH release was detected, confirming the low effect on plasma membrane. Food grade and platelets induced direct genotoxicity while P25, food grade and platelets caused oxidative DNA damage. No genotoxic or oxidative damage was induced by bipyramids and rods. Biological effects were overall lower in darkness than after light exposure. Considering that only food grade, P25 and platelets (more agglomerated) were internalized by cells, the uptake resulted correlated with genotoxicity. In conclusion, cytotoxicity of NPs was low and affected by shape and light exposure, while genotoxicity was influenced by cellular-uptake and aggregation tendency. KW - Nanoparticles KW - Shape-engineered KW - Raman spectroscopy KW - Genotoxic and oxidative damage KW - Cytotoxicity PY - 2019 UR - https://www.sciencedirect.com/science/article/pii/S0278691519301036?via%3Dihub DO - https://doi.org/10.1016/j.fct.2019.02.043 SN - 0278-6915 SN - 1873-6351 VL - 127 SP - 89 EP - 100 PB - Elsevier AN - OPUS4-47532 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Equilibrium chemistry of boron halides in plasma chemical reactors N2 - High purity halides of III-VI group elements, especially chloride and fluorides, are used in gas phase technologies for obtaining high purity materials and coatings. The reduction of halides in hydrogen-halide mixtures can be achieved in various discharge plasmas, e.g. inductively coupled, ark, and even laser-induced plasmas. Existing models of such plasmas are not sufficiently accurate to predict a yield of the targeted compounds and to describe the plasma processes involved in formation of these compounds. Besides, a construction of costly plasma-chemical reactors can be alleviated by the prior modeling of plasma processes that may occur in such reactors. A goal of this work is to extend the model, which was initially developed for laser induced Plasmas, to plasmas used in chemical reactors, in particular, the inductively-coupled-RF discharge Plasma. The model predicts equilibrium chemical compositions of reaction mixtures as functions of plasma temperature and stoichiometry of reactants. The mixtures investigated are BCl3/H2/Ar and BF3/H2/Ar where Ar serves as the plasma-forming gas and H2 as a binding agent which binds the active species Cl and F and Cl- and F-containing intermediates to produce gaseous B and its condensate. An additional goal is to obtain information about intermediate reaction products for different ratios of BCl3/H2 and BF3/H2 and at different temperatures and different Ar flow rates. It is found that the desired components B and B2 appear at appreciable concentrations of >0.1% and ~0.01% respectively only at temperatures above 3000 K. It is also established that the effect of charged species on the reaction products is miniscule for temperatures below 5000 K. The expected yield of boron as a function of the original mole fraction H2/BCl3 and H2/BF3 is calculated. The mole fractions are varied in the range 0.1-1000 and the temperature in the range 1000-10000 K. It is shown that the yield of boron increases with increasing the molar ratio H2/BCl3 and H2/BF3 up to ~100 in the temperature range 2000-5000 K. At higher temperatures, T>5000 K, the boron concentration reaches its maximum and does not depend on the concentration of hydrogen; all molecules dissociate and chemical reactions proceed only between charged particles (mostly elemental ions) and electrons. The calculated plasma parameters and composition are compared with experimental data obtained by optical emission spectroscopy. The calculated plasma temperature and electron density are shown to be in good agreement with the measured ones. T2 - European Winter Conference on Plasma Spectrochemistry (EWSPS-2019) CY - Pau, France DA - 03.02.2019 KW - Chemical reactors KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2019 AN - OPUS4-47541 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stroh, Julia T1 - In situ full phase analysis of the early cement hydration N2 - Fresh cement paste is a suspension consisting of a hydraulic binder (cement), water, and numerous minor components – admixtures. Addition of admixtures aims at specific modification of properties of the fresh cement paste or hardened cementitious building material. Specific admixtures, so-called superplasticizers (SP), are used to improve the flowability of the fresh cement paste with reduced water content. The latter is the starting material for the high-strength concrete. Thus, SPs are essential for the ambitious construction projects. However, uncontrollable retardation of the setting time in presence of SPs is occasionally observed. Obviously, SPs influence early products of the cement hydration leading to changes in the microstructure development. The hardening is thus delayed, and the quality of the resulting building material suffers. The mechanisms of the admixture action during the hydration process are still intensively investigated [1-7]. A detailed understanding of the admixture effects during the early hydration stage is the key to control and individual adjustment of the cement-based construction materials. We use the unique combination of the wall-free sample holder and the time-resolved X-ray scattering analysis to achieve the full information about the hydrate phases formed under the influence of admixtures. We use ultrasonic levitator to start the cement hydration in levitated cement pellets [8, 9]. The sample levitation allows collection of the unimpaired information about cement hydrate phases. The most beneficial is the avoiding of the contributions of the sample holder material to the data signal. We induce the cement hydration by adding water to unhydrated Portland cement during the data acquisition. The full phase composition of the hydrating cementitious system can be gathered in situ using wide angle X-ray scattering (WAXS). During the hydration of cement both crystalline and amorphous hydrate phases are formed. WAXS data contain the information about crystalline phases behind the Bragg reflections, whereas the amorphous hydrates influence the appearance of the background. Application of the data analysis specific for crystalline or amorphous phases is needed. The data quantification by the Rietveld method allows to conclude about the changes of the phase amounts due to the presence of admixture. The calculation of the pair distribution functions allows analysis of the amorphous hydrates. Based on this information, the SP effects and the extent of their involvement into the ongoing reactions can be concluded. A detailed understanding of the complex cement hydration process is envisioned. T2 - Anakon 2019 CY - Münster, Germany DA - 25.03.2019 KW - Cement KW - Admixtures KW - Pair Distribution Functions KW - X-ray diffraction KW - Total scattering analysis PY - 2019 AN - OPUS4-47664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Griepentrog, Michael A1 - Hertwig, Andreas A1 - Hielscher, Stefan A1 - Weise, Matthias T1 - Auf dem Weg zu Industrie 4.0: Bestimmung von Messunsicherheitsbudgets in der Oberflächentechnik N2 - Vorgestellt wurde die Bestimmung von Messunsicherheitsbudgets für sehr unterschiedliche physikalische Größen, die in der Oberflächentechnik von hoher Relevanz sind: Stufenhöhe h, Schichtdicke d, Eindringhärte HIT und Haftfestigkeit. Die Unterschiede betreffen die Art der Prüfmethodik (optisch zerstörungsfrei vs. mechanisch invasiv/zerstörend), die laterale Größe des Integrationsgebietes der Messung (lokal: nano bis sub-mikro vs. global: mikro bis makro) und die Art der Bestimmung von Messunsicherheitsbudgets (physikalische Größen: direkt rückführbar; Werkstoffkenngröße: genormt; Systemkenngröße: genormt). Im Rahmen von Industrie 4.0 werden ausgehend der geforderten Spezifikation des beschichteten Produkts (Mittelwert mit Vertrauensbereich oder Mindestwert) durchgehende Toleranzbänder zur Oberflächenmodifizierung/Beschichtung des Substrats, einhergehend mit Prozessfenstern, die diese Toleranzbänder garantieren, erforderlich, die zuverlässig erfasst werden müssen. Die Frage der anzuwendenden Mess- und Prüftechnik und die damit notwendige Betrachtung von Messunsicherheitsbudgets ist für die Digitalisierung von Konditionierungs-, Zustands-, Regel- und Steuergrößen unverzichtbar. Mit Blick auf die Einhaltung von Prozessfenstern und die dafür notwendige Prozessführung wird technologisches Kern-Know-how digitalisiert, das es unbedingt zu schützen gilt. Nur lokale Netze können diese Sicherheit garantieren, in globalen Netzen ist die Datensicherheit bestenfalls maximierbar T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik und 6. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Oberflächentechnik KW - Messunsicherheit KW - Messtechnik KW - Prüftechnik KW - Haftfestigkeit PY - 2019 SN - 978-3-00-058187-8 VL - 2019 SP - 1 EP - 10 AN - OPUS4-47670 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hertwig, Andreas T1 - Multi-methods surface analysis involving spectroscopic ellipsometry: New measurements for optical and energy applications N2 - Surface analysis is still gaining importance, as most modern technology is in essence surface and thin film technology. In microelectronics and optics but also in many fields of energy storage and conversion, thin surface layers or structured surfaces are key components. Optical surface measurements are useful because of their reliability, robustness, and scalability – properties, which are especially desirable in a production environment. However, many of these methods take require considerable effort in data analysis. Spectroscopic ellipsometry (SE) is maybe the prime example of this class of methods. To combine the advantages of SE with metrological trueness and traceability, we combine it in a group of other methods, such as electron microscopy, instrumental surface analysis, X-ray diffraction. This presentation will give an overview on the principles of SE, its available quantities and the general properties of this measurement technique. Several examples from current and past projects of BAM-6.7 will show how a measurement community involving ellipsometry can benefit many fields of interest, from polymer science to energy applications. In the context of creating a “measurement landscape”, standardisation and standard compliance play an important role. The efforts of BAM in standardisation and accrediting of ellipsometry will be shown demonstrating the possible impact on quality assurance in different fields of technology. T2 - Abteilungskolloquium 2018, BAM CY - BAM, Berlin, Germany DA - 12.12.2018 KW - Spectroscopic ellipsometry KW - Surface analysis KW - Thin film technology KW - Reference materials PY - 2018 AN - OPUS4-47671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian A1 - Emmerling, Franziska T1 - In situ investigations of mechanochemical reactions N2 - Mechanochemistry paves the way to simple, fast, and green syntheses. Despite considerable effort, there remains a lack in understanding of the underlying mechanisms. In situ investigations help to understand these mechanisms, which occur during a mechanochemical reaction. Here we present a universal strategy for simultaneous real-time in situ analysis, combining X-ray diffraction, Raman spectroscopy, and thermography. The potential of our approach is shown for different model reactions. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - In situ KW - Mechanochemistry KW - Milling PY - 2019 AN - OPUS4-47701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Goenaga-Infante, H. A1 - Malinovskiy, D. A1 - Vocke, R. D. A1 - Murphy, K. A1 - Nonose, N. A1 - Rienitz, O. A1 - Noordmann, J. A1 - Näykki, T. A1 - Sara-Aho, T. A1 - Ari, B. A1 - Cankur, O. T1 - CCQM-P134 Pb isotope amount ratios and delta-values in bronze N2 - Isotope amount ratios (hereafter referred to as simply isotope ratios) are proving useful in an ever increasing array of applications that range from studies unravelling transport processes, to pinpointing the provenance of specific samples as well as trace element quantification by using isotope dilution mass spectrometry (IDMS). These expanding applications encompass fields as diverse as archaeology, food chemistry, forensic science, geochemistry, medicine and metrology. However, to be effective tools, the isotope ratio data must be reliable and traceable to enable the comparability of measurement. The importance of traceability and comparability in isotope ratio analysis has already been recognized by the Inorganic Analysis Working Group (IAWG) within the CCQM. Three pilot studies have focused on the quality of isotope ratio determinations (P48 “U isotope ratios in urine”, P75 “stable isotopes in Methionine”, P105 “87Sr/86Sr in wine”). Moreover, isotope ratio measurements are fundamental to IDMS amount of substance determinations. For example, when Pb quantification using IDMS is undertaken, this requires the measurements of Pb isotope ratios. While the requirements for isotope ratio accuracy and precision in the case of of IDMS are generally quite modest, “absolute” Pb isotope ratio measurements for geochemical age dating and source rock characterization as well as forensic provenance and fingerprinting studies require Pb isotope ratio measurements of the highest quality. To support present and future CMCs on isotope ratio determinations, a Key Comparison was urgently needed. Therefore, it was decided at the IAWG meeting in Paris in April 2011 that a Key Comparison on the determination of Pb isotope ratios in a pure Pb solution and in a bronze sample should be organized and accompanied by a pilot study. Measuring Pb isotope amount ratios in a pure Pb solution, while seemingly straight forward, rigorously tests the ability of analyst to correct for any instrumental effects (such as mass discrimination and blank correction) on the measured ratios. Pb, present in trace amounts in a metal matrix sample (e.g. Pb in bronze), provides a real world test of the whole chemical and instrumental procedure, from chemical separation and sample purification to analysis and subsequent correction of appropriate instrumental effects on the separated samples. A suitable bronze material with a Pb mass fraction between 10 and 100 mg·kg-1 was available at BAM. A high purity solution of Pb with a mass fraction of approximately 100 mg·kg-1 was also available. By comparing the Pb isotope ratio results obtained for the bronze sample with the Pb isotope ratio results from the Pb solution, potential biases arising from the processing of the bronze sample could be effectively identified and separated from the instrumental effects arising from the measurement and data processing protocol. KW - Isotope ratio KW - Delta value KW - Molar mass KW - Measurement uncertainty KW - Traceability PY - 2017 UR - https://www.bipm.org/wg/CCQM/IAWG/Allowed/IAWG_Pilot_Studies/CCQM-P134.pdf SP - 1 EP - 42 PB - BIPM (Bureau International des Poids et Mesures) CY - Paris AN - OPUS4-47709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Calibration of Mg isotope amount ratios and delta values N2 - In the past, δ26/24Mg measurements were referenced to NIST SRM 980, the initial zero of the δ26/24Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. To solve this problem a suite of magnesium isotope reference materials, ERM-AE143, -AE144 and -AE145, has been certified in a first study by applying an ab initio calibration for absolute Mg isotope ratios without any a priori assumptions, a procedure which fulfils all requirements of a primary method of measurement. We could achieve for the first time measurement uncertainties for isotope amount ratios close to the typical precision of magnesium delta values, δ26/24Mg, which are at the 0.1 ‰ level (2SD). In addition, it was demonstrated that commonly used fractionation laws are invalid for correcting Mg isotope ratios in multi-collector ICPMS as they result in a bias which is not covered by its associated uncertainty. Depending on their type, fractionation laws create a bias up to several per mil, with the exponential law showing the smallest bias between 0.1 ‰ to 0.7 ‰. With these isotope reference materials, it is possible to establish SI-traceability for magnesium delta measurements. To realize this, we organized a second study within which five expert laboratories participated to cross-calibrate all available magnesium isotope standards, which are NIST SRM 980, IRMM-009, ERM-AE143, ERM-AE144, ERM-AE145 and the standards DSM3 and Cambridge-1. The mean δ26/24Mg values for the individual iRMs, calculated from the laboratory means show 2 SD reproducibilities varying between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for δ26/24Mg determinations (2SD). Thus, SI traceability for magnesium isotope amount ratios and delta values is demonstrated to be established. T2 - European Winter Conference on Plasma Spectrochemistry CY - Pau, France DA - 03.02.2019 KW - Delta value KW - SI-traceability KW - Absolute isotope ratio PY - 2019 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. AN - OPUS4-47710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gojani, Ardian T1 - Quantitative and qualitative analysis of liquid samples N2 - Spatial heterodyne spectroscopy (SHS) is an optical setup that combines both dispersive and interference based methods to obtain spectroscopic information. It has the high light throughput characteristic for interference based methods, but at the same time it has the high resolution typical of grated spectrometers. The basic SHS optical setup is similar to that of the Michelson interferometer, with the mirrors replaced by diffraction gratings positioned at fixed, equal distances from the beamsplitter and are slightly tilted. The resulting interference pattern is recorded by a digital camera and the spectrum is recovered by using Fourier Transformation. Although initially SHS was developed for astronomical and satellite-based atmospheric measurements, where spectroscopy of faint but large light sources are investigated, but in recent years the application of SHS spectroscopy is gaining popularity. Our research group is active both in Raman-SHS and LIBS-SHS, due to the fact that there are many overlapping challenges for the two spectroscopies in terms of optical and optoelectronic optimization. In the present study, we investigated the possibility of using SH detection for the qualitative and quantitative Raman spectroscopy of liquid samples. We constructed our own compact spatial heterodyne spectrometer using 300 mm-1 gratings (Newport), a 50:50 cube beamsplitter (Thorlabs), dischroic mirrors, bandpass and notch filters (Semrock), a Tamron telelens and a Retiga R1 CCD camera. A DPSS laser (532 nm, 20 ns) with variable energy and repetition rate (up to 100 µJ and 80 kHz) was used for excitation, with its beam driven through a 10x microscope objective (Thorlabs) to focus the laser light inside the liquid samples. The evaluation of the recorded interference patterns was carried out by self-developed software written in Octave. In the qualitative experiments, we investigated several oils and additives and employed principal component analysis (PCA) for their classification. It was found that the recorded spectra could be separated well in the subspace of just two principal components. The quantitative experiments were conducted with two sets of binary solvent mixtures (isopropanol-cyclohexane, glycerol-water). The simple univariate method based on the net intensity of one spectral peak did not give good results, but principal component regression (PCR) gave rise to fairly good and robust calibrations. Our results therefore show that a relatively simple and robust SHS setup can be advantageously used for both quantitative and qualitative Raman spectroscopy. T2 - European Winter Conference on Plasma Spectrochemistry (EWSPS-2019) CY - Pau, France DA - 03.02.2019 KW - SHS KW - Raman spectroscopy KW - Spatial Heterodyne Spectrometer PY - 2019 AN - OPUS4-47542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling chemistry in laser-induced and other types of plasmas N2 - A goal of this work is to extend the model, which was initially developed for laser induced plasmas, to plasmas used in chemical reactors, in particular, the inductively-coupled-RF discharge plasma. The model predicts equilibrium chemical compositions of reaction mixtures as functions of plasma temperature and stoichiometry of reactants. The mixtures investigated are BCl3/H2/Ar and BF3/H2/Ar where Ar serves as the plasma-forming gas and H2 as a binding agent which binds the active species Cl and F and Cl- and F-containing intermediates to produce gaseous B and its condensate. An additional goal is to obtain information about intermediate reaction products for different ratios of BCl3/H2 and BF3/H2 and at different temperatures and different Ar flow rates. It is found that the desired components B and B2 appear at appreciable concentrations of >0.1% and ~0.01% respectively only at temperatures above 3000 K. It is also established that the effect of charged species on the reaction products is miniscule for temperatures below 5000 K. The expected yield of boron as a function of the original mole fraction H2/BCl3 and H2/BF3 is calculated. The mole fractions are varied in the range 0.1-1000 and the temperature in the range 1000-10000 K. It is shown that the yield of boron increases with increasing the molar ratio H2/BCl3 and H2/BF3 up to ~100 in the temperature range 2000-5000 K. At higher temperatures, T>5000 K, the boron concentration reaches its maximum and does not depend on the concentration of hydrogen; all molecules dissociate and chemical reactions proceed only between charged particles (mostly elemental ions) and electrons. The calculated plasma parameters and composition are compared with experimental data obtained by optical emission spectroscopy. The calculated plasma temperature and electron density are shown to be in good agreement with the measured ones. T2 - Workshop on Laser and Plasmas Applications CY - Bari, Italy DA - 04.03.2019 KW - Plasma KW - LIBS KW - Plasma modeling PY - 2019 AN - OPUS4-47545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - van Wasen, Sebastian T1 - High resolution mass spectrometry of acoustically-levitated droplets N2 - Acoustic levitators generate acoustic standing waves between a transducer and a concave reflector. These acoustic waves are separated by multiple integer numbers of half wavelengths. Thus, acoustic levitation is the effect that a small volume (5 nL-10 μL) of sample can be levitated in a contact-free manner. Until now, levitation in analytical chemistry has primarily been associated with optical techniques such as Raman, X-Ray or UV/Vis spectroscopy. Less common applications are combinations of acoustic levitation with mass spectrometry. One reason for this being that the acoustic field surrounding the droplet effectively shields the sample, thus making it inaccessible to most ambient ionization techniques. Any effective investigation of acoustically-levitated droplets therefore requires the physical removal of some of the sample from the confine region of the acoustic trap before analysis. T2 - DGMS 2019 CY - Rostock, Germany DA - 10.03.2019 KW - Acoustical Levitation KW - Mass Spectrometry KW - Ambient Ionization KW - Laser PY - 2019 AN - OPUS4-47552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter T1 - Multiplexed immunoassays on polystyrene core/silica shell microparticles: Applications in environmental and food analysis, and biotechnology N2 - Clinical, environmental, and food analysis, require efficient and accurate quantitative analysis. Immunoassays take advantage of highly selective and affine binding of an antibody towards an antigen, being easy-to-use and allowing for high sample throughput. However, common immunoassays, e. g. ELISA are not capable of multiplexed analysis, thus limiting possible applications. On the other hand, multi-analyte methods, e.g. liquid chromatographytandem mass spectrometry requires expensive equipment, trained analysts and the time of analysis usually limits sample throughput. This bottleneck can be overcome combining the suspension array technology, where particles are encoded to allow multiplexed detection, with fluorescence immunoassays to create suspension array fluorescence immunoassays (SAFIA). Polystyrene core/silica shell microparticles serve as platform for SAFIA. While an encoding dye is introduced in the polystyrene core, the silica shell is used for immobilization: For competitive hapten immunoassays small molecules are immobilized on the surface, serving as a competitive binding site for selective antibodies. For quantification of proteins, antibodies can be immobilized on the surface and the sandwich immunoassay format can be employed. All mentioned immunoassays can be executed wash-free and highly parallelized, allowing up to 500 determinations within three hours. In contrast to ELISA, short incubation times, a wash-free mix-and-read procedure and automated flow-cytometric read-out makes SAFIA applicable for even non-trained personal. SAFIA showed excellent performance in studies on the origin and fate of drug residues in waste water, which is important to assess clearance rates of wastewater treatment plants. Furthermore, SAFIA can be employed in environmental screenings, detecting pollution of natural river waters by tracking anthropogenic marker substances. It was successfully employed in clinical and food analysis applications, e.g. the quantification of the anti-inflammatory drug diclofenac in breast milk or the quantification of caffeine in beverages. Due to multiplexing capacities, SAFIA can significantly improve biotechnological processes, as in the screening of hybridoma cells for selective and efficient antibody production. For small molecule analytes, limits of detection down to 4 ng/L and for proteins below 25 ng/mL (IgG) were observed, which makes SAFIA applicable to all addressed analytical issues. Moreover, in the analysis of real-world samples, SAFIA shows higher accuracy in contrast to ELISA, indicating higher matrix stability and thus higher robustness in analysis. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Bead-based-assay KW - SAFIA KW - Immunoassay KW - Flow cytometry KW - Diclofenac PY - 2019 AN - OPUS4-47638 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter T1 - Spheriplex multiplexed immunoassays: A practical tool for environmental, food and bioanalysis N2 - Clinical, environmental, and food analysis, require efficient and accurate quantitative analysis. Immunoassays take advantage of highly selective and affine binding of an antibody towards an antigen, being easy-to-use and allowing for high sample throughput. However, common immunoassays, e. g. ELISA are not capable of multiplexed analysis, thus limiting possible applications. On the other hand, multi-analyte methods, e.g. liquid chromatographytandem mass spectrometry requires expensive equipment, trained analysts and the time of analysis usually limits sample throughput. This bottleneck can be overcome combining the suspension array technology, where particles are encoded to allow multiplexed detection, with fluorescence immunoassays to create suspension array fluorescence immunoassays (SAFIA). Polystyrene core/silica shell microparticles serve as platform for SAFIA. While an encoding dye is introduced in the polystyrene core, the silica shell is used for immobilization: For competitive hapten immunoassays small molecules are immobilized on the surface, serving as a competitive binding site for selective antibodies. For quantification of proteins, antibodies can be immobilized on the surface and the sandwich immunoassay format can be employed. All mentioned immunoassays can be executed wash-free and highly parallelized, allowing up to 500 determinations within three hours. In contrast to ELISA, short incubation times, a wash-free mix-and-read procedure and automated flow-cytometric read-out makes SAFIA applicable for even non-trained personal. SAFIA showed excellent performance in studies on the origin and fate of drug residues in waste water, which is important to assess clearance rates of wastewater treatment plants. Furthermore, SAFIA can be employed in environmental screenings, detecting pollution of natural river waters by tracking anthropogenic marker substances. It was successfully employed in clinical and food analysis applications, e.g. the quantification of the anti-inflammatory drug diclofenac in breast milk or the quantification of caffeine in beverages. Due to multiplexing capacities, SAFIA can significantly improve biotechnological processes, as in the screening of hybridoma cells for selective and efficient antibody production. For small molecule analytes, limits of detection down to 4 ng/L and for proteins below 25 ng/mL (IgG) were observed, which makes SAFIA applicable to all addressed analytical issues. Moreover, in the analysis of real-world samples, SAFIA shows higher accuracy in contrast to ELISA, indicating higher matrix stability and thus higher robustness in analysis. T2 - Industry on Campus 2019 CY - Berlin, Germany DA - 27.03.2019 KW - Bead-based-assay KW - SAFIA KW - Immunoassay KW - Flow cytometry KW - Diclofenac PY - 2019 AN - OPUS4-47639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Choi, Youngeun A1 - Schmidt, Carsten A1 - Tinnefeld, Philip A1 - Bald, Ilko A1 - Roedinger, Stefan T1 - A new reporter design based on DNA origami nanostructures for quantification of short oligonucleotides using microbeads N2 - The DNA origami technique has great potential for the development of brighter and more sensitive reporters for fluorescence based detection schemes such as a microbead-based assay in diagnostic applications. The nanostructures can be programmed to include multiple dye molecules to enhance the measured signal as well as multiple probe strands to increase the binding strength of the target oligonucleotide to these nanostructures. Here we present a proof-of-concept study to quantify short oligonucleotides by developing a novel DNA origami based reporter system, combined with planar microbead assays. Analysis of the assays using the VideoScan digital imaging platform showed DNA origami to be a more suitable reporter candidate for quantification of the target oligonucleotides at lower concentrations than a conventional reporter that consists of one dye molecule attached to a single stranded DNA. Efforts have been made to conduct multiplexed analysis of different targets as well as to enhance fluorescence signals obtained from the reporters. We therefore believe that the quantification of short oligonucleotides that exist in low copy numbers is achieved in a better way with the DNA origami nanostructures as reporters. KW - Origami KW - Nanostructures KW - Microbeads KW - DNA origami KW - Oligonucleotides PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476443 DO - https://doi.org/10.1038/s41598-019-41136-x SN - 2045-2322 VL - 9 SP - 4769, 1 EP - 8 PB - Nature AN - OPUS4-47644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Daniel T1 - Visualisierung von mikro- und nanoskalierten Oberflächenstrukturen mittels abbildender Ellipsometry N2 - In den letzten Jahren hat die Einbindung der abbildenden Ellipsometrie in die Gruppe der optischen Verfahren zur Oberflächencharakterisierung ein enormes Potential bei der Analyse von topologischen Strukturänderungen gezeigt. Der dabei abgebildete Kon-trast wurde typischerweise auf Änderungen im Brechungsindex, Absorptionseffekte oder Schichtdickenänderungen zurückgeführt. In späteren Studien wurde festgestellt, dass auch andere Faktoren, wie etwa die Krümmung der Oberfläche oder Kanten von Struktu-ren einen signifikanten Einfluss auf die Messung der ellipsometrischen Paramater haben. Um diese Effekte aus der ellipsometrischen Messung extrahieren zu können, wird auf die Analyse der Müller-Matrix zurückgegriffen. In dem hier vorliegenden Beitrag wird gezeigt, wie die Müller-Matrix-Imaging Ellipsomet-rie (MM-IE) zur Charakterisierung von Oberflächenstrukturen verwendet werden kann. Dazu werden mikro- und nanoskaliert gekrümmte Oberflächen zunächst mit verschiede-nen Referenzmethoden, wie Rasterelektronenmikroskopie (SEM), Lichtmikroskopie (OM), Weißlichtinterferenzmikroskopie (WLIM) und Rasterkraftmikroskopie (AFM) vali-diert erfasst. Der anschließende Vergleich mit den Ergebnissen der Müller-Matrix-Ima-ging-Ellipsometrie ermöglicht eine Korrelation der zugrunde liegenden Strukturphäno-mene mit den ellipsometrischen Daten. In diesem Artikel wird das Prinzip an drei industriell relevanten Strukturgruppen demonstriert: Sub-Mikropartikel, Mikropartikel und sub-mikroskalierte Vertiefungen. T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Ellipsometrie KW - Nanoskaliert KW - Mikroskaliert KW - Oberflächengeometrie KW - Brechungsindex KW - Müller-Matrix-Ellipsometrie PY - 2019 AN - OPUS4-47645 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Daniel A1 - Beck, Uwe T1 - Visualisierung von mikro- und nanoskalierten Oberflächenstrukturen mittels abbildender Ellipsometrie N2 - In den letzten Jahren hat die Einbindung der abbildenden Ellipsometrie in die Gruppe der optischen Verfahren zur Oberflächencharakterisierung ein enormes Potential bei der Analyse von topologischen Strukturänderungen gezeigt. Der dabei abgebildete Kon-trast wurde typischerweise auf Änderungen im Brechungsindex, Absorptionseffekte oder Schichtdickenänderungen zurückgeführt. In späteren Studien wurde festgestellt, dass auch andere Faktoren, wie etwa die Krümmung der Oberfläche oder Kanten von Struktu-ren einen signifikanten Einfluss auf die Messung der ellipsometrischen Paramater haben. Um diese Effekte aus der ellipsometrischen Messung extrahieren zu können, wird auf die Analyse der Müller-Matrix zurückgegriffen. In dem hier vorliegenden Beitrag wird gezeigt, wie die Müller-Matrix-Imaging Ellipsomet-rie (MM-IE) zur Charakterisierung von Oberflächenstrukturen verwendet werden kann. Dazu werden mikro- und nanoskaliert gekrümmte Oberflächen zunächst mit verschiede-nen Referenzmethoden, wie Rasterelektronenmikroskopie (SEM), Lichtmikroskopie (OM), Weißlichtinterferenzmikroskopie (WLIM) und Rasterkraftmikroskopie (AFM) vali-diert erfasst. Der anschließende Vergleich mit den Ergebnissen der Müller-Matrix-Ima-ging-Ellipsometrie ermöglicht eine Korrelation der zugrunde liegenden Strukturphäno-mene mit den ellipsometrischen Daten. In diesem Artikel wird das Prinzip an drei industriell relevanten Strukturgruppen demonstriert: Sub-Mikropartikel, Mikropartikel und sub-mikroskalierte Vertiefungen. T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik und 6. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Ellipsometrie KW - Nanoskaliert KW - Mikroskaliert KW - Oberflächengeometrie KW - Brechungsindex KW - Müller-Matrix-Ellipsometrie PY - 2019 SN - 978-3-00-062102-4 SP - 1 EP - 5 AN - OPUS4-47646 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ou, D. A1 - Schumacher, David A1 - Zscherpel, Uwe A1 - Xiao, Y. T1 - Dual-energy materials characterization methods for laminography image enhancement based on photon counting detector N2 - Laminography is a widely used NDT technique for large flat object which cannot be investigated by traditional computed tomography. However, due to the limited scanning angle of laminography, the reconstructed image has more artifact interference, which seriously affects the reconstructed image quality. Reducing artifacts of the laminography image and enhancing the images have become important research effort. In this paper, we present dual-energy materials characterization methods based on photon counting detectors to reduce artifacts and enhance image for laminography. The photon counting detector used in this study allows the setting of two independent energy thresholds in order to acquire dual-energy images for laminography from a single scan. The dual energy imaging methods of basis material decomposition (BMD) and weighted logarithmic subtraction (WLS) were studied in the paper with respect to laminography image enhancement. A fast decomposition algorithm on laminographic projection domain with approximating the inverse dual-energy equations to calculate the thickness of basic materials was used in the BMD dual-energy imaging methods. The experimental results show that the BMD method can characterize materials and enhance features of the basic material within the laminographic dataset. In the WLS method, a linear operation was applied on dual-energy images reconstruction directly, which can eliminate the attenuation of one specific material in the resultant image by setting an appropriate weighting factor. In our experiments. WLS method was used successfully to eliminate the strong artifacts generated by the special material and enhance the images. Dual-energy materials characterization methods based on photon counting detectors show potential applications in laminography. KW - Photon Counting Detectors KW - Dual Energy Imaging KW - Data Processing KW - X-ray PY - 2019 DO - https://doi.org/10.1088/1748-0221/14/02/P02018 SN - 1748-0221 VL - 14 SP - P02018, 1 EP - 13 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-47573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Thorid T1 - Nanoskalige Haftvermittler zur Erhöhung der Haft- bzw. Klebfestigkeit unter Verwendung von ALD-Hybridprozessen N2 - Ziel des Projektes HARFE (Haftfestigkeit Reproduzierbarkeit Festigkeit) war es, eine Er-höhung der Haft- bzw. Klebfestigkeit auf Niedrigenergie-Polymeren (PE, PP, PTFE) zu erreichen. SENTECH realisierte dazu plasmachemische Oberflächenaktivierungen mit O2 und die Abscheidung von Aluminiumoxidschichten (Al2O3) mittels Atomic Layer Deposition (ALD), wobei die Ellipsometrie zum in-situ Monitoring der ALD-Prozesse diente. Die BAM charakterisierte die modifizierten Oberflächen bezüglich der Oberflächenenergie (OFE) und bestimmte die Verbund- bzw. Klebfestigkeit mittels der Zentrifugentechnologie T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik und 6. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Haftvermittler KW - ALD-Hybridprozesse KW - Klebfestigkeit KW - Atomic Layer Deposition KW - Al2O3-Schichten KW - Oberflächenenergie PY - 2019 AN - OPUS4-47653 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Thorid A1 - Hidde, Gundula A1 - Beck, Uwe A1 - Naumann, F. A1 - Kärkkänen, I. A1 - Gargouri, H. T1 - Nanoskalige Haftvermittler zur Erhöhung der Haft- bzw. Klebfestigkeit unter Verwendung von ALD-Hybridprozessen N2 - Ziel des Projektes HARFE (Haftfestigkeit Reproduzierbarkeit Festigkeit) war es, eine Er-höhung der Haft- bzw. Klebfestigkeit auf Niedrigenergie-Polymeren (PE, PP, PTFE) zu erreichen. SENTECH realisierte dazu plasmachemische Oberflächenaktivierungen mit O2 und die Abscheidung von Aluminiumoxidschichten (Al2O3) mittels Atomic Layer Deposition (ALD), wobei die Ellipsometrie zum in-situ Monitoring der ALD-Prozesse diente. Die BAM charakterisierte die modifizierten Oberflächen bezüglich der Oberflächenenergie (OFE) und bestimmte die Verbund- bzw. Klebfestigkeit mittels der Zentrifugentechnologie T2 - 14. ThGOT Thementage Grenz- und Oberflächentechnik und 6. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 12.03.2019 KW - Haftvermittler KW - ALD-Hybridprozesse KW - Klebfestigkeit KW - Atomic Layer Deposition KW - Al2O3-Schichten KW - Oberflächenenergie PY - 2019 SN - 978-3-00-062102-4 SP - 1 EP - 2 CY - Zeulenroda, Germany AN - OPUS4-47656 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - Time- and lateral-resolved X-ray absorption fine structure spectroscopy N2 - X-ray absorption fine structure (XAFS) spectroscopy is a powerful and widely used tool for material characterization. It is non-destructive, element-sensitive and requires no long-range order of the sample, making it suitable for the investigation of amorphous phases. XAFS includes the X-ray absorption near edge structure (XANES) and the extended X-ray absorption fine structure (EXAFS), providing information about the electronical state of the absorbing atom and the spatial order of the neighboring atoms respectively. Our new approach presented here is derived from the classical dispersive XAFS setup. The aim is to have a scanningless, stable and reproducible setup for applications, in which dynamic processes occur in the second time scale. A broad polychromatic beam passes through the sample and is dispersed afterwards by a convexly bent Si (111) crystal. All energies are reflected under different angles and thus spatially separated, allowing a position sensitive detector to record a spectrum over the energy range of the incoming beam in a single shot. Tests of this setup were performed at the BAMline @ BESSY-II (Berlin, Germany) with different metal foils. First in situ measurements comprised the investigation of the early stages of the zinc(II)2-methylimidazolate (ZIF-8) crystallization. This topic of metal-organic-frameworks (MOF) research is of interest for medical applications. Structural changes with a time resolution of 1 s could be followed. The second dimension of the broad beam can be used for a lateral resolution. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - X-ray absorption fine structure KW - Synchrotron based methods KW - X-ray spectroscopy PY - 2019 AN - OPUS4-47660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lemke, Nora T1 - Optimization of protein quantification via isotope dilution ICP-MS of a standard reference protein N2 - Quantitative proteomics are nowadays one of the key tasks in life sciences. A multitude of methods for protein quantification are established and more techniques are developed each year, but there still is a lack of well characterized and quantified protein standards. We aim to develop an ICP-MS based method to quantify pure proteins reliably and traceable to SI. Here, we employ isotope Dilution analysis for the quantification of proteins of known stoichiometry via their sulfur content. T2 - European Winter Conference on Plasma Spectrochemistry 2019 CY - Pau, France DA - 03.02.2019 KW - ICP-MS KW - Isotope dilution KW - Proteins PY - 2019 AN - OPUS4-47933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weber, Kathrin A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Stephan-Scherb, Christiane T1 - A µ‐XANES study of the combined oxidation/sulfidation of Fe–Cr model alloys N2 - The precise analysis of cation diffusion profiles through corrosion scales is an important aspect to evaluate corrosion phenomena under multicomponent chemical load, as during high‐temperature corrosion under deposits and salts. The present study shows a comprehensive analysis of cation diffusion profiles by electron microprobe analysis and microbeam X‐ray absorption near edge structure (µ‐XANES) spectroscopy in mixed oxide/sulfide scales grown on Fe–Cr model alloys after exposing them to 0.5% SO2. The results presented here correspond to depth‐dependent phase identification of oxides and sulfides in the corrosion scales by µ‐XANES and the description of oxidation‐state‐dependent diffusion profiles. Scales grown on low‐ and high‐alloyed materials show both a well‐pronounced diffusion profile with a high concentration of Fe3+ at the gas and a high concentration of Fe2+ at the alloy interface. The distribution of the cations within a close‐packed oxide lattice is strongly influencing the lattice diffusion phenomena due to their different oxidation states and therefore different crystal‐field preference energies. This issue is discussed based on the results obtained by µ‐XANES analysis. KW - X-ray absorption spectroscopy KW - Oxidation KW - Sulfidation PY - 2019 DO - https://doi.org/10.1002/maco.201810644 VL - 70 IS - 8 SP - 1360 EP - 1370 PB - Wiley VCH-Verlag AN - OPUS4-47934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bierstedt, Andreas A1 - You, Yi A1 - van Wasen, Sebastian A1 - Bosc-Bierne, Gaby A1 - Weller, Michael G. A1 - Riedel, Jens T1 - Laser-Induced Microplasma as an Ambient Ionization Approach for the Mass-Spectrometric Analysis of Liquid Samples N2 - An airborne high repetition rate laser-induced plasma was applied as a versatile ambient ionization source for mass-spectrometric determinations of polar and nonpolar analytes in solution. The laser plasma was sustained between a home-built pneumatic nebulizer and the inlet capillary of an Orbitrap mass spectrometer. To maintain stable conditions in the droplet-rich spray environment, the plasma was directly fed by the fundamental output (λ = 1064 nm) of a current state-of-the-art diode-pumped solid-state laser. Ionization by the laser-driven plasma resulted in signals of intact analyte ions of several chemical categories. The analyte ions were found to be fully desolvated since no further increase in ion signal was observed upon heating of the inlet capillary. Due to the electroneutrality of the plasma, both positive and negative analyte ions could be formed simultaneously without altering the operational parameters of the ion source. While, typically, polar analytes with pronounced gas phase basicities worked best, nonpolar and amphoteric compounds were also detected. The latter were detected with lower ion signals and were prone to a certain degree of fragmentation induced during the ionization process. All the described attests the laser-induced microplasma by a good performance in terms of stability, robustness, sensitivity, and general applicability as a self-contained ion source for the liquid sample introduction. KW - Laser KW - Laser-induced plasma KW - Ambient ionization KW - Mass Spectrometry PY - 2019 DO - https://doi.org/10.1021/acs.analchem.9b00329 SN - 0003-2700 VL - 91 IS - 9 SP - 5922 EP - 5928 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-47939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - X-ray imaging with coded apertures N2 - Coded aperture imaging systems are in use in astrophysics since the 1960's. We want to adapt this technique for full field x-ray fluorescence imaging in combination with a color-x-ray-camera. T2 - Seminar des Atominstituts der TU Wien CY - Vienna, Austria DA - 14.05.2019 KW - Reconstruction KW - X-ray spectroscopy KW - X-ray fluorescence KW - Spectroscopy KW - Imaging KW - Coded apertures PY - 2019 AN - OPUS4-47997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ferreira da Silva, F. A1 - do N. Varella, M. T. A1 - Jones, N. C. A1 - Vrönning Hoffmann, S. A1 - Denifl, S. A1 - Bald, Ilko A1 - Kopyra, J. T1 - Electron-Induced Reactions in 3-Bromopyruvic Acid N2 - 3-Bromopyruvic acid (3BP) is a potential anticancer drug, the action of which on cellular metabolism is not yet entirely clear. The presence of a bromine atom suggests that it is also reactive towards low-energy electrons, which are produced in large quantities during tumour Radiation therapy. Detailed knowledge of the interaction of 3BP with secondary electrons is a prerequisite to gain a complete picture of the effects of 3BP in different forms of Cancer therapy. Herein, dissociative electron attachment (DEA) to 3BP in the gas phase has been studied both experimentally by using a crossed-beam setup and theoretically through scattering and quantum chemical calculations. These results are complemented by a vacuum ultraviolet absorption spectrum. The main fragmentation channel is the formation of Br@ close to 0 eV and within several resonant features at 1.9 and 3–8 eV. At low electron energies, Br@ formation proceeds through s* and p* shape resonances, and at higher energies through core-excited resonances. It is found that the electron-capture cross-section is clearly increased compared with that of non-brominated pyruvic acid, but, at the same time, fragmentation reactions through DEA are significantly altered as well. The 3BP transient negative ion is subject to a lower number of fragmentation reactions than those of pyruvic acid, which indicates that 3BP could indeed act by modifying the electron-transport chains within oxidative phosphorylation. It could also act as a radio-sensitiser. KW - Density functional calculations KW - Dissociative electron attachment KW - Drug discovery KW - Gas-phase reactions KW - Sensitizers PY - 2019 DO - https://doi.org/10.1002/chem.201806132 SN - 0947-6539 VL - 25 IS - 21 SP - 5498 EP - 5506 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-48003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Noeller, Renate A1 - Feldmann, Ines A1 - Kasztovszky, Z. A1 - Szőkefalvi-Nagy, Z. A1 - Kovács, I. T1 - Characteristic Features of Lapis Lazuli from Different Provenances, Revised by µXRF, ESEM, PGAA and PIXE N2 - The objective of this study is to find out, to what extent the geochemical characteristics of lapis lazuli can be utilized in respect to its provenance. A wide range of variables is taken into consideration depending on the quantity of samples analysed from a specific geological region and the methods applied. In order to provide evidence, a multi-technique analytical approach using µXRF, ESEM, PGAA and PIXE is applied to samples from the most famous deposits of lapis lazuli. Special elements determined as fingerprints are compared in relation to the forming conditions obvious in textural features. The results and statistical output allow a differentiation that enables an optimized local classification of the blue stone. An absolute requirement for all geo-tracing performed on blue colored cultural objects of unknown provenance is awareness of the limits of analysis. The possible sources of lapis lazuli are tested by analysing the blue pigment used as paint on murals and ink on manuscripts from the Silk Road. KW - Provenance studies KW - Micro-XRF KW - Lapis lazuli KW - ESEM KW - PGAA KW - PIXE KW - Pigment analyses PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480048 DO - https://doi.org/10.17265/2328-2193/2019.02.003 VL - 7 IS - 2 SP - 57 EP - 69 PB - David Publishing AN - OPUS4-48004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Trimpin, S. A1 - Inutan, E. A1 - Karki, S. A1 - Elia, E. A1 - Zhang, W. A1 - Weidner, Steffen A1 - Marshall, D. A1 - Hoang, K. A1 - Lee, C. A1 - Davis, E. A1 - Smith, V. A1 - Meher, A. A1 - Cornejo, M. A1 - Auner, G. A1 - McEwen, C. T1 - Fundamental studies of new ionization technologies and insights from IMS-MS N2 - Exceptional ion mobility spectrometry mass spectrometry (IMS-MS) developments by von Helden, Jarrold, and Clemmer provided technology that gives a view of chemical/biological compositions previously not achievable. The ionization method of choice used with IMS-MS has been electrospray ionization (ESI). In this Special issue contribution, we focus on fundamentals of heretofore unprecedented means for transferring volatile and nonvolatile compounds into gas-phase ions singly and multiply charged. These newer ionization processes frequently lead to different selectivity relative to ESI and, together with IMS-MS, may provide a more comprehensive view of chemical compositions directly from their original Environment such as surfaces, e.g., tissue. Similarities of results using solvent- and matrix-assisted ionization are highlighted, as are differences between ESI and the inlet ionization methods, especially with mixtures such as bacterial extracts. Selectivity using different matrices is discussed, as are results which add to our fundamental knowledge of inlet ionization as well as pose additional avenues for inquiry. IMS-MS provides an opportunity for comparison studies relative to ESI and will prove valuable using the new ionization technologies for direct analyses. Our hypothesis is that some ESI-IMS-MS applications will be replaced by the new ionization processes and by understanding mechanistic aspects to aid enhanced source and method developments this will be hastened. KW - Inlet ionization KW - Vacuum ionization KW - Matrices KW - Fundamentals KW - Ion mobility PY - 2019 DO - https://doi.org/10.1007/s13361-019-02194-7 SN - 1044-0305 SN - 1879-1123 VL - 30 IS - 6 SP - 1133 EP - 1147 PB - Springer AN - OPUS4-48011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pötzsch, Sina T1 - Book review: Practical testing and evaluation of plastics N2 - One can conclude, this first edition of “Practical Testing and Evaluation of Plastics” provides a comprehensive and compact reference. It can be recommended as clear overview as well as introducing manual for everyone working with characterization and testing of plastics. KW - Plastic KW - Testing PY - 2019 DO - https://doi.org/10.1002/maco.201970054 SN - 0947-5117 SN - 1521-4176 VL - 70 IS - 5 SP - 931 EP - 932 PB - Wiley-VCH CY - Weinheim AN - OPUS4-48013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Thomas A1 - Darlatt, Erik A1 - Lippitz, Andreas A1 - Müller, S. A1 - Schalley, C. A1 - Unger, Wolfgang T1 - Systematic XP and NEXAFS spectroscopy studies of (ter-)pyridineterminated self-assembled monolayers and their addressability for functional molecules N2 - The chemical composition of surfaces functionalized with self-assembled monolayers (SAMs) is an important parameter that determines their performance in a broad range of applications, from immobilizing molecular machines to initiation and growth control of MOFs (Metal-Organic Frameworks). In this article, a critical Survey of XPS (X-ray photoelectron spectroscopy) and NEXAFS (near edge X-ray absorption fine structure) spectroscopy data for pyridine-functionalized monolayers on gold surfaces is presented to compile correlations that have been indiscernible before. Monolayers with aromatic backbones are compared to monolayers with aliphatic backbones. Monolayers with pyridine end-groups are compared to mixed monolayers formed terpyridine-functionalized by molecules end-groups and non-functionalized molecules. Thiol-oxidation during ageing of the SAMs in air is addressed. And finally, the addressability of the SAMs for the deposition of metal-ions and organic molecules is investigated and compared. This work consequently delivers a comprehensive set of spectroscopic data of (ter-)pyridine-terminated SAMs and their performance as template for the preparation of functional multilayers of macrocycles exhibiting a preferential orientation. KW - (ter-)pyridineterminated self-assembled monolayer KW - X-ray Photoelectron Spectroscopy (XPS) KW - NEXAFS PY - 2019 DO - https://doi.org/10.1016/j.elspec.2019.03.011 VL - 233 SP - 28 EP - 37 PB - Elsevier B.V. AN - OPUS4-48018 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Holzweber, Markus A1 - Lippitz, Andreas A1 - Hesse, R. A1 - Denecke, R. A1 - Werner, W. A1 - Unger, Wolfgang T1 - The use of ionic liquids for the determination of the spectrometer transmission function in X-ray photoelectron spectroscopy (XPS) N2 - The uncertainty of measurement in quantitative XPS analysis can be reduced by using a calibrated spectrometer transmission function T (E), which is usually determined by taking spectra from Au, Ag, Cu and Ge elemental reference materials. However, this approach is quite time-consuming due to required sample preparation steps like sputter cleaning etc., and the relatively big number of samples to be measured. This contribution proposes the use of the ionic liquids [C2C1im][NTf2] and [C3C1im][NTf2] as reference materials for a determination of T(E). These multi-elemental samples deliver five intensive photoemission peaks, F 1s, O 1s, N 1s, C 1s and S 2p, in an energy window from 160 eV to 700 eV which is of specific interest for applications of quantitative XPS for surface chemical analysis of soft matter, one of the major applications of XPS. KW - Quantitative XPS KW - Ionic liquid KW - Transmission function PY - 2019 DO - https://doi.org/10.1016/j.elspec.2019.03.008 VL - 233 SP - 51 EP - 56 PB - Elsevier B.V. AN - OPUS4-48019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Metrology for spatially resolved chemical analysis at the micro and nanometre scales Surface Analysis Working Group (SAWG) - Report for 17th Meeting (2018/19) N2 - The SAWG was established as an ad-hoc working group in 2003 before being established as a permanent working group. The first comparison was in 2007. Dr Unger recalled the terms of reference for the group, which paralleled those of the CCQM itself, with a focus on spatially resolved chemical surface analysis at the micro- and nano-scale. The group also had a remit to act as a forum for exchange of information on research and development of surface analysis, establish contact with relevant stakeholders and promote the development of SI traceable chemical surface measurements. The group currently had participants from 18 institutes, although five had not sent participants to recent meetings. Reporting progress on studies, Dr Unger said that P-190CCQM-K-157 (measurement of HfO2 in thin film) had been completed, and the subsequent K-157 approved is ongoing and that for CCQM-K153 (Measurement of Specific Adsorption of N2 and Kr on nonporous SiO2 at liquid nitrogen temperature by BET) was at the draft B was completed stageand distributed to CCQM WG chairpersons for approval. Dr Unger reported that CCQM-K-153 had covered measurement of specific absorption of nitrogen or krypton on nonporous silica at liquid nitrogen [ambient] temperature. This included an application of the BET method, a standard method for determination of surface area. This fitted into the ‘nonporous’ region of the SAWG measurement space, which included microporous, mesoporous and microporous regions. Of these regions, CCQM-K136 and CCQM-K153 demonstrated capability in meso- and microporous media respectively. CCQM-K153 involved two measurands; amount of absorbed gas at liquid nitrogen temperature, expressed as specific absorption, and the BET surface area. Specific absorption could in principle be traceable to the SI; BET was operationally defined. Five institutes participated. A detailed uncertainty budget was available for both measurands. Results had been excellent, with all laboratories agreeing well within their uncertainties and all in agreement with the reference value. Reporting on CCQM P190, Dr Unger described the study objective measurand (amount of substance of HfO2 in a thin film), samples and methods. After showing transmission electron microscope images obtained in the study, he briefly reviewed the conclusions. The study identified a need to handle carbon contamination, harmonise the XPS measurement protocol, determine emission angle and identify a consensus value for attenuation length. These conclusions had informed the design of the proposed ongoing K157 study approved at the 24th Meeting of te CCQM. The group planned a number of comparisons for the next three years: 2019: A pilot study on the amount of substance in a thin organic layer (previously approved). 2020: CCQMK-157, Measurement of the amount of substance of HfO2; A Key comparison on specific gas adsorption on microporous samples and a Pilot study on Homogeneous surface composition of an ionic liquid. 2021: A key comparison measuring the amount of substance in a thin organic layer. Dr Unger additionally described a recently proposed pilot study to examine chemical composition in a deep nanoscale layer. This was important for the electronics industry. Four participants had expressed interest. The measurand will be the amount of Ir(ppy)2(acac) in a thin organic layer within an organic layer stack on a silicon substrate. He also reported that SAWG had started work on characterisation of graphene material grown by chemical vapour decomposition (CVD). The work would examine coverage on the substrate, number of layers, level of disorder, uncertainty budgets associated with the measurement, and data analysis. A link to VAMAS Technical Work Area 41 “Graphene and Related 2D Materials“ would also be established. Looking forward, Dr Unger said the group had established a task group on application of Raman spectroscopy. This had important applications but was currently seen as qualitative. He presented the terms of reference for the task group for approval by the CCQM. Dr Unger reviewed the SAWG activities that have progressed the state of the art in measurement science. He listed the past and ongoing comparisons that had addressed new and challenging measurement problems, and drew attention to a number of key publications in surface analysis. He additionally described stakeholder engagement activities, including collaboration with VAMAS, input to ISO TC 201, contributions to Euramet projects, and contributions to two recent stakeholder workshops. T2 - 25th meeting of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM) CY - Paris, France DA - 11.04.2019 KW - Surface chemical analysis KW - Metrology KW - International Meter Convention PY - 2019 AN - OPUS4-48020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hüllmann, Dino A1 - Kohlhoff, Harald A1 - Erdmann, Jessica A1 - Neumann, Patrick P. ED - Pastramă, Ş. D. ED - Constantinescu, D. M. T1 - Control of a spherical parallel manipulator N2 - In mobile robot applications, some sensors such as open-path gas detectors or laser rangefinders need to be aimed at specific targets in order to get the desired measurements. To do this in a fast and elegant manner, we present a spherical parallel manipulator with three degrees of freedom. Compared to typical serial manipulators, it offers superior dynamics and structural stiffness, which are important parameters for this type of task. We present the mechanical design and derive kinematic equations both to compute set-points for the desired orientation and to estimate the current state of the system. A PID controller is used to generate control signals. T2 - 35th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Sinaia, Romania DA - 25.09.2018 KW - Spherical parallel manipulator KW - Sensor orientation KW - Sensor alignment KW - Sensor aiming PY - 2019 DO - https://doi.org/10.1016/j.matpr.2019.03.145 SN - 2214-7853 VL - 12 IS - 2 SP - 423 EP - 430 PB - Elsevier CY - Amsterdam, Netherlands AN - OPUS4-48044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Optimization and detailed spectroscopic characterization of an improved SH-LIBS setup N2 - The spatial heterodyne detection principle has a great potential in spectroscopy. It has an optical setup similar to that of a Michelson interferometer, with the mirrors replaced by diffraction gratings positioned at fixed, equal distances from the beamsplitter and are slightly tilted. The resulting interference pattern is recorded by a digital camera and the spectrum is recovered by using Fourier transformation. Although SHS was initially developed for astronomical and satellite-based atmospheric measurements, but in recent years it has been started to be applied in other branches of spectroscopy too. Recently the area of laser-induced breakdown spectroscopy (LIBS) has also discovered the potential of SHS. The main appeal of SHS detection in LIBS includes the compactness and robustness of the setup (in view of field applications) and the flexibility to optimize the setup for either high sensitivity or for high resolution, which can be benficially exploited in applications like stand-off measurements, quantitative analysis with isotope resolution, etc. In the present work, we have improved and further optimized our initial LIBS-SHS setup described in a previous conference. By using optical simulations, we have modelled the light transmission efficiency, instrumental function and imaging properties of the system. We significantly improved and automated the spectral and image data processing sequence. The optimizations carried out resulted in an improved spectral resolution and repeatability, a lower spectral background and the elimination of the central line artifact originating from the Fourier transformation procedure. A detailed characterization of the LIBS spectroscopy performance (e.g. resolution, spectral coverage, tuning range, linearity, etc.), including a comparison with that of a LIBS setup based on a conventional dispersion CCD spectrometer was also performed. T2 - European Winter Conference on Plasma Spectrochemistry (EWSPS-2019) CY - Pau, France DA - 03.02.2019 KW - SHS KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Spatial heterodyne spectrometer PY - 2019 AN - OPUS4-48047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schroeder, Barbara A1 - Le Xuan, Hoa A1 - Völzke, Jule L. A1 - Weller, Michael G. T1 - Preactivation Crosslinking - An Efficient Method for the Oriented Immobilization of Antibodies N2 - Crosslinking of proteins for their irreversible immobilization on surfaces is a proven and popular method. However, many protocols lead to random orientation and the formation of undefined or even inactive by-products. Most concepts to obtain a more targeted conjugation or immobilization requires the recombinant modification of at least one binding partner, which is often impractical or prohibitively expensive. Here a novel method is presented, which is based on the chemical preactivation of Protein A or G with selected conventional crosslinkers. In a second step, the antibody is added, which is subsequently crosslinked in the Fc part. This leads to an oriented and covalent immobilization of the immunoglobulin with a very high yield. Protocols for Protein A and Protein G with murine and human IgG are presented. This method may be useful for the preparation of columns for affinity chromatography, immunoprecipitation, antibodies conjugated to magnetic particles, permanent and oriented immobilization of antibodies in biosensor systems, microarrays, microtitration plates or any other system, where the loss of antibodies needs to be avoided, and maximum binding capacity is desired. This method is directly applicable even to antibodies in crude cell culture supernatants, raw sera or protein-stabilized antibody preparations without any purification nor enrichment of the IgG. This new method delivered much higher signals as a traditional method and, hence, seems to be preferable in many applications. KW - Antibody coating KW - Proximity-enhanced reaction KW - Immunoglobulins KW - IgG KW - Protein A KW - Protein G KW - Immunoprecipitation KW - Immunocapture KW - Regeneration KW - Biosensor KW - Immunosensor KW - Affinity chromatography KW - Immunoaffinity extraction KW - Oriented immobilization KW - Immunoassay KW - Bioconjugation PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479786 DO - https://doi.org/10.3390/mps2020035 SN - 2409-9279 VL - 2 IS - 2 SP - 1 EP - 14 PB - MDPI CY - Basel, Switzerland AN - OPUS4-47978 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - EMPIR Project ALCOREF - Proposal for EURAMET SCOA intercomparisons N2 - The talk presents a short summary of the EMPIR Project ALCOREF "Certified forensic alcohol reference materials". An interlaboratory comparison of analytical methods for the quantification of ethanol in water and a comparison of certified ethanol in water reference materials are proposed. T2 - CCQM Organic Analysis Working Group Meeting CY - Paris, France DA - 08.04.2019 KW - Certified reference material KW - EMPIR KW - EURAMET PY - 2019 AN - OPUS4-47988 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona T1 - Vorstellung BAM Initiative: QI-FoKuS N2 - Mit QI-FoKuS / Forschung für Konformitätsbewertung und Sicherheit streben wir auf Basis einer wiederkehrenden Befragung von Unternehmen und Konformitätsbewertungsstellen in Deutschland die Schaffung einer besseren Datengrundlage für die Forschung an. Diese soll es erleichtern, wichtige Zusammenhänge evidenzbasiert zu analysieren, um das systemische Zusammenwirken der Elemente der Qualitätsinfrastruktur besser zu verstehen. Dabei sollen zunächst die Elemente Konformitätsbewertung und Akkreditierung besonders im Vordergrund stehen. T2 - Erfahrungsaustausch des VAZ e.V. CY - Berlin, Germany DA - 07.05.2019 KW - Managementsysteme KW - Unternehmensbefragung KW - QI-FoKuS KW - Konformitätsbewertung KW - Zertifizierung PY - 2019 AN - OPUS4-47971 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Andresen, Elina A1 - Schäferling, M. T1 - Surface modifications for photon-upconversion-based energy-transfer nanoprobes N2 - An emerging class of inorganic optical reporters are nearinfrared (NIR) excitable lanthanide-based upconversion nanoparticles (UCNPs) with multicolor emission and long luminescence lifetimes in the range of several hundred microseconds. For the design of chemical sensors and optical probes that reveal analyte-specific changes in their spectroscopic properties, these nanomaterials must be combined with sensitive indicator dyes that change their absorption and/or fluorescence properties selectively upon interaction with their target analyte, utilizing either resonance energy transfer (RET) processes or reabsorption-related inner filter effects. The rational development of UCNP-based nanoprobes for chemical sensing and imaging in a biological environment requires reliable methods for the Surface functionalization of UCNPs, the analysis and quantification of Surface groups, a high colloidal stability of UCNPs in aqueous media as well as the chemically stable attachment of the indicator molecules, and suitable instrumentation for the spectroscopic characterization of the energy-transfer systems and the derived nanosensors. These topics are highlighted in the following feature article, and examples of functionalized core−shell nanoprobes for the sensing of different biologically relevant analytes in aqueous environments will be presented. Special emphasis is placed on the intracellular sensing of pH. KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - FRET KW - Surface chemistry PY - 2019 DO - https://doi.org/10.1021/acs.langmuir.9b00238 SN - 0743-7463 VL - 35 IS - 15 SP - 5093 EP - 5113 PB - ACS AN - OPUS4-47975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Hüllmann, Dino A1 - Bartholmai, Matthias ED - Pastramă, Ş. D. ED - Constantinescu, D. M. T1 - Concept of a gas-sensitive nano aerial robot swarm for indoor air quality monitoring N2 - In this paper, we introduce a nano aerial robot swarm for indoor air quality monitoring applications such as occupational health and safety of (industrial) workplaces. The concept combines a robotic swarm composing of nano Unmanned Aerial Vehicles (nano UAVs), based on the Crazyflie 2.0 quadrocopter, and small lightweight metal oxide gas sensors for measuring the Total Volatile Organic Compound (TVOC) in ppb and estimating the eCO2 (equivalent calculated carbon-dioxide) concentration in ppm. TVOC is a measure for the indoor air quality. An indoor localization and positioning system will be used to estimate the absolute 3D position of the swarm like GPS. Based on this novel indoor air quality monitoring concept, the development and validation of new algorithms in the field of Mobile Robot Olfaction (MRO) are planned, namely gas source localization and gas distribution mapping. A test scenario will be built up to validate and optimize the gas-sensitive nano aerial robot swarm for the intended applications. T2 - 35th Danubia Adria Symposium on Advances in Experimental Mechanics CY - Sinaia, Romania DA - 25.09.2018 KW - Nano aerial robot KW - UAV KW - Swarm KW - Indoor air quality KW - Monitoring KW - Concept PY - 2019 DO - https://doi.org/10.1016/j.matpr.2019.03.151 SN - 2214-7853 VL - 12 IS - 2 SP - 470 EP - 473 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-48055 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kowalke, J. A1 - Arnold, C. A1 - Ponomarev, I. A1 - Jäger, Christian A1 - Kroll, P. A1 - Brendler, E. A1 - Kroke, E. T1 - Structural Insight into Layered Silicon Hydrogen Phosphates Containing [SiO6] Octahedra Prepared by Different Reaction Routes N2 - The layered silicophosphate Si(HPO4)(2) was prepared via a novel synthesis approach using silicon nanopowder and ortho-phosphoric acid at 150 degrees C providing a polycrystalline product. Silicophosphate compounds with sixfold coordinated silicon atoms obtained from pyrophosphoric acid H4P2O7 and tetraalkoxysilanes via a sol-gel route exhibit the same short-range order. The solid products were analyzed with XRD, elemental analysis (ICP-AES), and detailed NMR spectroscopic studies, including H-1, C-13, Si-29, and P-31 MAS-, P-31-Si-29-REDOR, HETCOR, and CP-RFDR experiments. DFT calculations support the structure of Si(HPO4)(2) consisting of layers of [SiO6] octahedra linked by [O3P(OH)] tetrahedra. The OH groups point to the neighboring layers and may be substituted by ethoxy or other groups. KW - Silicon KW - Phosphorus KW - Sol-gel processes KW - NMR spectroscopy KW - Computational chemistry PY - 2019 DO - https://doi.org/10.1002/ejic.201801321 IS - 6 SP - 828 EP - 836 PB - ChemPubSoc AN - OPUS4-48058 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - Engell, S. A1 - Paul, Andrea A1 - King, R. A1 - Maiwald, Michael T1 - Raw data of pilot plant runs for CONSENS project (Case study 1) N2 - In case study one of the CONSENS project, two aromatic substances were coupled by a lithiation reaction, which is a prominent example in pharmaceutical industry. The two aromatic reactants (Aniline and o-FNB) were mixed with Lithium-base (LiHMDS) in a continuous modular plant to produce the desired product (Li-NDPA) and a salt (LiF). The salt precipitates which leads to the formation of particles. The feed streams were subject to variation to drive the plant to its optimum. The uploaded data comprises the results from four days during continuous plant operation time. Each day is denoted from day 1-4 and represents the dates 2017-09-26, 2017-09-28, 2017-10-10, 2017-10-17. In the following the contents of the files are explained. KW - Process Analytical Technology KW - Multivariate Data Analysis KW - Nuclear Magnetic Resonance KW - Near Infrared Spectroscopy KW - Continuous Manufacturing KW - CONSENS PY - 2018 DO - https://doi.org/10.5281/zenodo.1438233 PB - Zenodo CY - Geneva AN - OPUS4-48063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Prager, Jens T1 - Bestimmung der Rissgeometrie bei der zerstörungsfreien Ultraschallprüfung mit geführten Wellen N2 - In der zerstörungsfreien Prüfung werden in zunehmendem Maße geführte Ultraschallwellen zur Lokalisation von Fehlstellen genutzt. Geführte Ultraschallwellen zeichnen sich dadurch aus, dass sie große Distanzen innerhalb des zu prüfenden Bauteiles zurücklegen können. Das Ultraschallwellenfeld setzt sich dabei aus verschieden Moden zusammen. Etablierte Prüfverfahren mit geführten Wellen ermitteln häufig nur die Position der Fehlstelle, wobei die Laufzeiten der reflektierten Signale ausgewertet wird. Modenumwandlung bleibt dabei zumeist unberücksichtigt. Die Charakterisierung der Fehlstelle, zum Beispiel hinsichtlich der Länge eines Risses, ist dagegen herausfordernd. Aussagekräftige Zusammenhänge zwischen der Dimension oder Geometrie der Fehlstelle und ihrer Interaktion mit der Ultraschallwelle zu finden, ist Teil aktueller Forschung. Insbesondere eine Betrachtung der Moden höherer Ordnung und deren Amplitudenverhältnisse kann beim Aufspüren dieser Zusammenhänge hilfreich sein. Im Beitrag werden zunächst die Zusammenhänge zwischen den beiden fundamentalen Moden in einer isotropen Platte und der Länge eines Risses untersucht. Aus den Ergebnissen wird ein inverses Verfahren motiviert. Ein Algorithmus wird vorgestellt, der die Risslänge im Modell solange variiert, bis er die modalen Zusammenhänge einer Vorgabe oder einer Messung rekonstruiert. Die eingesetzte Scaled Boundary Finite Element Method ermöglicht dabei eine sehr kurze Rechenzeit in jeden Optimierungsschritt. Zusätzlich ermöglicht die Methode eine Auswertung der modalen Zusammenhänge ohne Postprocessing, was die Rechenzeiten weiter verkürzt. T2 - DAGA 2019 CY - Rostock, Germany DA - 18.03.2019 KW - Geführte Wellen KW - Scaled Boundary Finite Element Method KW - Amplitudenverhältnisse PY - 2019 AN - OPUS4-47730 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Martin T1 - Development of a biosensor for the online detection of explosives N2 - An affinity column, which removed up to 99 % of high affinity Anti-TNT antibody at high antibody concentrations, was manufactured based on a monolithic glass core and a trinitroaniline-BSA conjugate. To detect the label Dy654 in the nM range an epi-fluorescence microscope setup with a CMOS camera was established to serve as online fluorescence detector with multiplexing capabilities. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Online fluorescence KW - Trinitro KW - Affinty KW - Antibody PY - 2019 AN - OPUS4-47745 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Marquardt, J. A1 - Gurieva, G. A1 - Stephan-Scherb, Christiane A1 - Schorr, S. T1 - The Effect of Copper Vacancies on the Anion Position of Chalcopyrite Type CuGaS2 N2 - The prediction of structural parameters and optoelectronic properties of compound semiconductors is very important. However, calculations often neglect chemical variability and structural defects. In chalcopyrite type semiconductors one of the major defects are copper vacancies (V Cu). The four cation neighbors of the anion determine its position in the chalcopyrite type structure expressed by the Wyckoff position 8d (x, 1/4, 1/8). Intrinsic point defects like V Cu and anti-sites may cause variations of the Anion position in the middle of the cation tetrahedron, especially in the Anion position Parameter x. For stoichiometric chalcopyrite type compounds a formalism according to the principle of conservation of tetrahedral bonds (CTB) can be applied to calculate the anion position parameter, but it fails in the case of off-stoichiometric chalcopyrites. This case study of chalcopyrite type CuGaS 2 and Mn-substituted GuGaS 2 shows that the experimentally determined anion position Parameter x deviate from values calculated by CTB approach. The systematic investigation of off-stoichiometric CuGaS 2 and Mn-substituted GuGaS 2 demonstrates the effect of copper vacancies on the average radii of the cation sites (Wyckoff positions 4a and 4b) as well as on the anion position Parameter x. By applying an elaborated CTB Approach implementing copper vacancies an agreement between experimental and calculated anion position Parameter x can be obtained. KW - Chalcogenides KW - Neutron diffraction KW - Copper vacancies PY - 2019 DO - https://doi.org/10.1002/pssa.201800882 VL - 216 IS - 15 SP - 1800882 PB - Wiley AN - OPUS4-47748 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Michael A1 - Buzanich, Günter A1 - Jähn, Katharina A1 - Reinholz, Uwe A1 - Radtke, Martin T1 - Analysis of cobalt deposition in periprosthetic bone specimens by high-resolution synchroton XRF in undecalcified histological thin sections N2 - Increasing numbers of implant revisions are a current clinical issue. Interactions of the endoprosthesis biomaterial with the body affect implantation time by wear processes, i.e. corrosion and abrasion. Previously, cobalt-chrome implants were shown to cause high levels of cobalt ions being deposited in the bone matrix. To determine a poten- tial functional role of these ions on bone homeostasis, we have developed a non-destructive dual analysis of highly sensitive elemental analysis by synchrotron XRF directly in undecalcified histological bone thin sections (4 μm). In this study, samples from 28 bone samples from hip endoprosthesis carriers (Surface Replacement Arthroplasty, metal-on-metal bearing) with an implant lifetime of 17–1750 days were used. Results were compared to age- matched control specimens. The histological analysis identified areas of bone cell activity and assigned them for XRF measurements. Co-Cr wear particles were identified in the bone marrow. In addition, Co ions were highly enriched in the mineralized bone matrix. The cobalt deposits were not homogeneously distributed, and areas of high signal intensity were identified. Co was distinctly deposited in the newly formed osteoid layer, but also within deeper layers of the bone matrix, whereby the Co concentration increased with higher degrees of bone matrix mineralization. In the current study, we determined cobalt accumulations in the bone matrix and showed for the first time via synchrotron XRF with a high spatial resolution direct on histological slides, that cobalt deposits in the mineralized bone matrix in a mineral-specific way that is dependent upon the implant lifetime. KW - Implant material KW - Cobalt deposition KW - Bone matrix KW - High-resolution synchrotron XRF KW - Histology PY - 2019 DO - https://doi.org/10.1016/j.mtla.2019.100290 SN - 2589-1529 VL - 6 SP - 100290, 1 EP - 8 PB - Elsevier Inc. CY - Amsterdam, Niederlande AN - OPUS4-47620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis T1 - Comparison of different models for stress singularities in higher order finite element methods for elastic waves N2 - The Spectral Element Method (SEM) has been proven to be an efficient numerical method for solving the wave equation in linear elastic bodies. This efficiency is reduced if a stress singularity is present in the body. For example, re-entrant corners, material interfaces, fixed boundaries, and especially crack tips can cause stress singularities. To preserve the efficiency of the SEM, special solution strategies are required. There are many approaches which consider stress singularities, but comparisons are rare for dynamic problems. Finding an efficient model is an important step for many applications. In particular, applications for structural health monitoring and non-destructive evaluation rely on accurate and efficient crack models. In this contribution, we present several models to capture singularities in combination with the SEM. The theory behind the models are shortly summarized and we show results for different benchmark problems in two dimensions. The first model deploys a new class of singular elements. For these singular elements, the crack tip approximation is computed based on the static Scaled Boundary Finite Element Method (SBFEM). The second model uses the continued‐fraction‐based SBFEM, while the third model uses an hp-refinement near the singularity. The models are compared among each other and evaluated in terms of their respective efficiency and accuracy. T2 - GAMM 2019 CY - Vienna, Austria DA - 18.02.2019 KW - SBFEM KW - Stress singularities KW - Higher order FEM PY - 2019 AN - OPUS4-47753 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg T1 - Synthetische Aperturfokussierung für die Terahertzspektroskopie N2 - Die zeitaufgelöste THz-Spektroskopie (THz-TDS) operiert mit elektromagnetischen Impulsen, die ein Amplitudenspektrum im unteren THz-Bereich aufweisen. Die THz-TDS ist in der Lage, dielektrische Volumina zerstörungs- und kontaktfreie zu durchstrahlen. Um eine 3D-THz Bildung zu ermöglichen, wurde für die THz-TDS ein rechnergestütztes Mess- und Rekonstruktionsverfahren (THz-TD-SAFT) entwickelt, mit dem es gelingt, unter Verwendung der im Zeitbereich registrierten THz-TDS-Daten das Volumeninnere in Form eines dreidimensionalen Tomogramms zu rekonstruieren. Die THz-TD-SAFT basiert auf die für die Ultraschalltechnik entwickelte Synthetische Apertur Fokussierung (SAFT) bzw. des heuristisch begründeten Algorithmus des Synthetischen Apertur Radars (SAR). Anhand von Beispielen wird die Möglichkeiten der THz-TD-SAFT demonstriert und nachgewiesen, dass mit dem Rekonstruktionsansatz die künstlich eingebauten Fehlstellen bezüglich der Position und Größe geometrisch richtig im Tomogramm abgebildet werden können. T2 - 4. Fachseminar, Mikrowellen- und Terahertz-Prüftechnik in der Praxis CY - Fürth, Germany DA - 02.04.2019 KW - Zeitaufgelöste THz-Spektroskopie KW - THz-TD-SAFT KW - THz-Tommographie PY - 2019 AN - OPUS4-47756 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Neumann, Patrick P. A1 - Hüllmann, Dino A1 - Tiebe, Carlo T1 - KonSens (Kommunizierende Sensorsysteme für die Bauteil- und Umweltüberwachung) - Projektergebnisse N2 - Im Projekt KonSens werden für die Anwendungsbeispiele bauteilintegrierte Sensorik für Betonkomponenten und mobile Multigassensorik Sensorsysteme in Form von Funktionsmustern entwickelt, validiert und angewendet. Schwerpunkte liegen einerseits in der Detektion und Bewertung von Korrosionsprozessen in Beton und andererseits in der Detektion und Quantifizierung sehr geringer Konzentrationen toxischer Gase in der Luft. Dabei ist die Adaption der sensorischen Methoden aus dem Labor in reale Messumgebungen inklusive geeigneter Kommunikationstechnik ein wichtiger Aspekt. T2 - NetMon International training course - Low-cost Environmental Monitoring CY - BAM, Berlin, Germany DA - 09.04.2019 KW - Umweltmonitoring KW - Bauwerksüberwachung KW - RFID-Sensorsysteme KW - pH-Sensor KW - Fluoreszenzsensoren PY - 2019 AN - OPUS4-47763 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nikitin, D. A1 - Madkour, Sherif A1 - Pleskunov, P A1 - Tafiichuk, R A1 - Shelemin, A A1 - Hanus, J A1 - Gordeev, I A1 - Sysolyatina, E A1 - Ermolaeva, S A1 - Titov, V A1 - Schönhals, Andreas A1 - Choukourov, A T1 - Cu nanoparticles constrain segmental dynamics of crosslinked polyethers: a trade -off between non-fouling and antibacterial properties N2 - Copper has a strong bactericidal effect against multi-drug resistant pathogens and polyethers are known for their resistance to biofilm formation. Herein, we combined Cu nanoparticles (NPs) and a polyether Plasma polymer in the form of nanocomposite thin films and studied whether both effects can be coupled. Cu NPs were produced by magnetron sputtering via the aggregation in a cool buffer gas whereasolyether layers were synthesized by Plasma-Assisted Vapor Phase Deposition with poly(ethylene oxide) (PEO) used as a precursor. In situ specific heat spectroscopy and XPS analysis revealed the formation of a modified polymer layer around the NPs which propagates on the scale of a few nanometers from the Cu NP/polymer interface and then transforms into a bulk polymer phase. The chemical composition of the modified layer is found to be ether-deficient due to the catalytic influence of copper whereas the bulk polymer Phase exhibits the chemical composition close to the original PEO. Two cooperative glass transition phenomena are revealed that belong to the modified polymer layer and the bulk phase. The former is characterized by constrained mobility of polymer segments which manifests itself via a 30 K increase of dynamic glass transition temperature. Furthermore, the modified layer is characterized by the heterogeneous structure which results in higher fragility of this layer as compared to the bulk phase. The Cu NPs/polyether thin films exhibit reduced Protein adsorption; however, the constrained segmental dynamics leads to the Deterioration of the non-fouling properties for ultra-thin polyether coatings. The films are found to have a bactericidal effect against multi-drug resistant Gram-positive Methicillin-Resistant Staphylococcus aureus and Gram-negative Pseudomonas aeruginosa. KW - Nanocomposites KW - Specific heat spectroscopy PY - 2019 DO - https://doi.org/10.1039/c8sm02413h VL - 15 IS - 13 SP - 2884 EP - 2896 PB - RSC AN - OPUS4-47765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geilert, S. T1 - Si isotope fractionation during BIF formation – inferences from a modern Archean ocean analogue N2 - Silica-rich sedimentary rocks like cherts and BIFS, typical for the Archean, have been used to reconstruct temperatures and other properties of the early oceans through the study of their Si isotope variations. Precambrian cherts and BIFS span a δ30Si range of ~7‰, with BIFs being about 2‰ lower in δ30Si than cherts. These lower δ30Si signatures have been attributed to represent contributions from different input sources such as hydrothermal fluids, variable continental weathering regimes or sorption onto Fe oxides/hydroxides [e.g. 2 and references therein]. In this study, fluids and BIF-like sediments have been investigated for their Si isotope compositions in Paulina Lake (PL), a hydrothermally-influenced crater lake in the Newberry Caldera, Oregon, USA. PL lake sediments are rich in silica (~65wt% SiO2) and are composed of up to 22.5wt% Fe2O3, which is comparable to Archean BIFs and thus serve as a modern Archean ocean analogue. We compared our analyses with East Lake (EL), the twin Newberry crater lake without hydrothermal input. Dissolved Si in EL has an average δ30Si signature of +1.55±0.16‰ (1sd) and sediments an average δ30Si signature of +0.18±0.28‰ (1sd). Dissolved Si in PL has an average δ30Si signature of +2.02±0.15‰ (1sd), whereas the sediments show a large range in δ30Si values between +0.59‰ and -1.24‰. PL sediments show a trend towards more negative δ30Si with increasing Fe2O3 contents. The magnitude of Si isotope fractionation thus appears to depend on the presence of Fe. This fractionation induced by interaction with Fe precipitation is defined here as the offset in δ30Si between PL and EL sediments at comparable depths (Δ30SiPL-EL). The resulting Δ30SiPL-EL values range between +0.69 and -1.42‰ and increase with increasing Fe2O3 content in the sediments. Our results are the first to quantify the magnitude of Fe-induced δ30Si fractionation observed in a natural analogue of the Archean ocean and can explain the lighter δ30Si signatures found in BIFs. T2 - Fourth General Meeting of the SPP 1833 “Building a Habitable Earth” CY - Cologne, Germany DA - 27.03.2019 KW - Archean ocean KW - Si isotope fractionation KW - Delta values PY - 2019 AN - OPUS4-47711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bente, Klaas A1 - Oeff, Julius A1 - Gaal, Mate T1 - Quantitative, zeiteffiziente, winkel- und frequenzaufgelöste Analyse von Elektretwandlern im Hör- und Ultraschallbereich N2 - Die Bildgebung oder Analyse von Materialien mittels luftgekoppelten Ultraschalls profitiert von einer hohen Geschwindigkeit, Flexibilität und Materialschonung des assoziierten Verfahrens. Die Luftankopplung hat jedoch den wesentlichen Nachteil, dass die auftretenden Impedanzsprünge an Grenzflächen zu enormen Verlusten in den Signalamplituden führen. Ultraschallwandler, die laut genug senden und sensitiv genug empfangen, um die geringen Signalamplituden noch auswerten zu können, sind somit zentraler Gegenstand der aktuellen Forschung und Entwicklung. Vielversprechende Wandlertypen sind piezokeramische Wandler, Elektretwandler, aber auch passive, breitbandige Ultraschallempfänger, wie optische Mikrophone. Die quantitative Charakterisierung der Sensitivitäten solcher Wandler wird oft vernachlässigt, da kein simples, universelles Verfahren zur Verfügung steht. In diesem Beitrag geht es um die Methodik der Charakterisierung von Luftultraschallwandlern mittels thermoakustischer Ultraschallsender. Thermoakustische Wandler erzeugen Ultraschall durch das schnelle heizen eines finiten Volumens an Luft vor dem Wandler. Die erhöhte interne Energie führt zu einer Druckänderung, welche sich als akustische Welle fortpflanzen kann. Da keine mechanische Volumenarbeit vom Wandler erbracht wird, funktioniert das Verfahren resonanzfrei. Die Charakterisierung wird am Beispiel von Elektretwandlern durchgeführt. Elektretwandler sind sensitive und immer verschleißresistentere Schallwandler, wodurch sie verbreitet Einsatz im Hör- und Ultraschallbereich finden. Geladene, zelluläre Polypropylen-Folien eignen sich besonders gut als Wandlermaterial aufgrund ihrer, verglichen mit Piezokompositen, hundertfach niedrigeren akustischen Impedanz bei gleichem piezoelektrischem Koeffizienten. Doch das winkel- und frequenzabhängige Verhalten der Wandler ist kaum untersucht und wenig quantifiziert. Es wird gezeigt, dass diese Folien eine schichtdickenabhängige Sensitivität in Größenordnungen zwischen 0.1 mV/Pa und 10 mV/Pa aufwiesen. Ein Maximum in der Sensitivität fand sich nahe ihrer mechanischen Resonanzfrequenz im Ultraschallbereich, aber auch im niederfrequenten Hörschallbereich. Darüber hinaus konnte die Winkelabhängigkeit der Sensitivität charakterisiert werden. Die Analyse konnte dabei zeiteffizient gestaltet werden, da pro Winkel eine Messung für die Berechnung der Übertragungsfunktion des Wandlers genügte. Quantifiziert wurden die Ergebnisse durch das einmalige Vermessen des Emitters mittels Laser-Doppler-Vibrometrie (LDV). Mit den erzielten Ergebnissen wurde zum einen das komplexe Sensitivitätsverhalten der Wandler untersucht, aber auch eine grundlegende Methodik aufgezeigt, wie Wandler quantitativ, multivariat charakterisiert werden können. Winkel- und frequenzaufgelöste Sensitivitäten erlauben zum einen die Analyse der Anwendbarkeit der Wandler für sämtliche Einsatzgebiete, zum anderen stehen so Rückschlüsse über die mechanische Dynamik von Elektretfolien in Aussicht, da deren Sensitivität direkt mit ihrem Elastizitätsmodul skaliert. T2 - DAGA 2019 CY - Rostock, Germany DA - 18.03.2019 KW - Luftultraschall KW - Ultraschall KW - Elektretwandler KW - Thermoakustik KW - Wandlercharakterisierung PY - 2019 SP - 748 AN - OPUS4-47712 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoevelmann, J. A1 - Stawski, T. M. A1 - Besselink, R. A1 - Freeman, H. M. A1 - Dietmann, K. M. A1 - Mayanna, S. A1 - Pauw, Brian Richard A1 - Benning, L. G. T1 - A template-free and low temperature method for the synthesis of mesoporous magnesium phosphate with uniform pore structure and high surface area N2 - Mesoporous phosphates are a group of nanostructured materials with promising applications, particularly in biomedicine and catalysis. However, their controlled synthesis via conventional template-based routes presents a number of challenges and limitations. Here, we show how to synthesize a mesoporous Magnesium phosphate with a high surface area and a well-defined pore structure through thermal decomposition of a crystalline struvite (MgNH4PO4·6H2O) precursor. In a first step, struvite crystals with various morphologies and sizes, ranging from a few micrometers to several millimeters, had been synthesized from supersaturated aqueous solutions (saturation index (SI) between 0.5 and 4) at ambient pressure and temperature conditions. Afterwards, the crystals were thermally treated at 70–250 °C leading to the release of structurally bound water (H2O) and ammonia (NH3). By combining thermogravimetric analyses (TGA), scanning and transmission electron microscopy (SEM, TEM), N2 sorption analyses and small- and wide-angle X-ray scattering (SAXS/WAXS) we show that this decomposition process results in a pseudomorphic transformation of the original struvite into an amorphous Mg-phosphate. Of particular importance is the fact that the final material is characterized by a very uniform mesoporous structure with 2–5 nm wide pore channels, a large specific surface area of up to 300 m2 g−1 and a total pore volume of up to 0.28 cm3 g−1. Our struvite decomposition method is well controllable and reproducible and can be easily extended to the synthesis of other mesoporous phosphates. In addition, the so produced mesoporous material is a prime candidate for use in biomedical applications considering that Magnesium phosphate is a widely used, non-toxic substance that has already shown excellent biocompatibility and biodegradability. KW - Struvite KW - SAXS KW - Scattering KW - Nanoporous KW - Geology PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477130 DO - https://doi.org/10.1039/c8nr09205b VL - 11 IS - 14 SP - 6939 EP - 6951 PB - Royal Society of Chemistry AN - OPUS4-47713 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - King, R. A1 - Engell, S. A1 - Paul, Andrea A1 - Pereira Remelhe, M. A1 - Maiwald, Michael T1 - Flexible Automation with compact NMR instruments N2 - Modular plants using intensified continuous processes represent an appealing concept to produce pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes, and it enables plug-and-produce reconfiguration for fast product changes. To facilitate this flexibility by real-time quality control, we developed a solution that can be adapted quickly to new processes and includes a compact Nuclear Magnetic Resonance (NMR) spectrometer for online quality monitoring as well as a new model-based control approach. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including ro-bust evaluation of sensor data. Here, we present alternatives for the quantitative determination of the analytes using modular, physically motivated models. These models can be adapted to new substances solely by the use of their corresponding pure component spectra, which can either be derived from experimental spectra as well as from quantum mechanical models or NMR predictors. Modular means that spec-tral models can simply be exchanged together with alternate reagents and products. Beyond that, we comprehensively calibrated an NIR spectrometer based on online NMR process data for the first time within an industrial plant. The integrated solution was developed for a metal organic reac-tion running on a commercial-scale modular pilot plant and it was tested under industrial conditions. T2 - 7th Annual PANIC Conference CY - Hilton Head Island, South Carolina, USA DA - 03.03.2019 KW - Online NMR Spectroscopy PY - 2019 AN - OPUS4-47715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias A1 - Tiebe, Carlo T1 - Wind Vector Estimation on Multirotor Aircraft N2 - An equation for wind vector estimation using a multirotor aircraft as a flying anemometer is shown. To compute the wind vector an estimate of the thrust of the aircraft is required, which is related to the rotational speed of the rotors. Hence, a sensing system for the rotational speed using phototransistors is presented. T2 - NetMon International training course - Low-cost Environmental Monitoring CY - BAM, Berlin, Germany DA - 09.04.2019 KW - Anemometer KW - Phototransistor KW - Thrust KW - Wind PY - 2019 AN - OPUS4-47801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Mobile robot olfaction with flying platforms N2 - This presentation gives an introduction to the gas-sensitive aerial robots developed at BAM, including various application examples in the field of mobile robot olfaction: gas source localization and gas distribution mapping. T2 - NetMon International training course - Low-cost Environmental Monitoring CY - BAM, Berlin, Germany DA - 09.04.2019 KW - Localization of gas sources KW - Mobile Robot Olfaction KW - Tomographic reconstruction of gas plumes KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - UAV-REGAS KW - Nano UAV Swarm PY - 2019 AN - OPUS4-47802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Measurement and Simulation of the Microscopic Energy Deposit: A general approach applicable to Ionizing Radiation Sources of varying Linear Energy Transfer N2 - The determination of microscopic dose-damage relations in aqueous environment is of fundamental interest for dosimetry and its application in radiation-therapy and protection. We present a combined experimental and simulational approach to quantify the microscopic energy deposit at biomolecules in liquid environment which is applicable to a wide range of primary radiation sources, e.g. photons, electrons or ions, and targets, such as DNA, proteins or cells.Therefore, we combine Geant4 particle-scattering simulations in water with calculations concerning the movement of biomolecules to obtain the energy deposit in the biologically relevant nanoscopic volume. We present, how to combine these simulational results and experimental data via a generalised damage model to determine the microscopic dose-damage relation at a molecular level. To show the viability of this approach, we apply this method to an experimentally challenging system, the direct irradiation of plasmid DNA (pUC19) in water with electrons as primary particles. Here we combine electron-scattering simulations with calculations concerning the diffusion and convection induced movement of the DNA, within a coarse-grained model of the irradiated liquid. Additionally a microscopic target model for DNA molecules based on the relation of lineal energy and radiation quality is used to calculate their effective target volume. It was found that on average fewer than two ionisations within a 7.5\,nm radius around the sugar-phosphate backbone are sufficient to cause a single strand break, with a corresponding median lethal energy deposit being E\textsubscript{1/2}=6+-4\,eV. The presented method is applicable for all types of ionising radiation and a broad variety of biological targets. T2 - CCQM Workshop CY - Paris, France DA - 09.04.2019 KW - Dosimetry KW - Microdosimetry KW - Geant4 KW - Geant4-DNA KW - DNA KW - Electron irradiation KW - Monte-Carlo Simulation PY - 2019 UR - https://www.bipm.org/utils/en/pdf/Workshop-CCQM2019-EP1.pdf AN - OPUS4-47810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von Törne, Wipert Jannik T1 - Identifizierung und Charakterisierung technischer Transformationsprodukte von Warfarin N2 - Das Therapeutikum Warfarin ist bis heute der bekannteste Vertreter der antikoagulanten Rodentizide. In dieser Arbeit wurden Phase I Metabolite mittels einer elektrochemischen Durchflusszelle simuliert und analysiert. Weitere Transformations- und Abbauprozesse wurde durch UV-Bestrahlung und Ozonung generiert, gaschromatographisch getrennt und miteinander verglichen. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Warfarin PY - 2019 AN - OPUS4-47733 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ali, Naveed A1 - Komal, N. A1 - Malik, Z. A1 - Chaudhary, A.J. T1 - Synthesis, characterization and properties of hierarchically assembled antimony oxyhalides nanonetworks N2 - The novel synthesis route has been developed for hierarchically structured; nanorods and nanosheets of Sb4O5Cl2 from a single precursor, with dimension range between 57–90 nm. X-ray powder diffraction analysis confirmed the monoclinic crystal symmetry in P21/c(14)with structure type Sb4O5Cl2 for both forms; the nanorods and nanosheets. Rietveld refinements and crystallite size investigations of the powder patterns revealed significant enhancement in intensity with subtle variation in the lattice parameters and crystallite size decrease in case of nanosheets in comparison to the nanorods assembly. Through scanning electron microscopy, a composition commensurate to Sb4O5Cl2 at% with averaged dimensions; dia.∼90 nm, l ∼ 2 μm for nanorods and dia.∼50–150 nm for nanosheets got corroborated. Owing to the quantum confinement a band gap widening was observed while moving from bulk to nano regime, i.e. 3.25, 3.31 and 3.34 eV, for bulk, nanosheets, and nanorods, respectively. In the case of nanosheets, the highest value of dielectric constant was observed, i.e. 87, as compared to nanorods and the bulk, i.e. 40 and 35.5, respectively. The nanosheets also showed the highest value of dielectric and tangent loss with an increase in frequency due to the least crystallite size of these nanonetworks. Nanosheets depicted the higher AC conductivity at low frequency due to the alignment of the charges but its value decreases at the higher frequency due to lack of time for charge reorientation. The hopping phenomenon was observed in all three cases with the most prominent one in bulk case at higher frequencies. KW - Nanorods KW - Nanosheets KW - Antimony oxychloride ( Sb4O5Cl2) KW - Optical properties KW - Dielectric properties PY - 2019 DO - https://doi.org/10.1088/2053-1591/ab0da9 SN - 2053-1591 VL - 6 IS - 6 SP - 065035 PB - IOP AN - OPUS4-47734 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler T1 - Application of ultrasonic techniques for quality assurance of salt concrete engineered barriers: Shape, cracks and delamination N2 - The closure of underground nuclear waste disposal facilities requires reliable gas- and water-tight engineered barriers. In Germany, barriers made from salt concrete have been evaluated in full scale. While the barriers seem to fulfill the requirements regarding permeability, some unexpected cracks have been detected at the surface and at depth. In cooperation between the Federal Company for Radioactive Waste Disposal (BGE) and the Federal Institute for Materials Research and Testing (BAM), several experiments have been carried out to evaluate the applicability for ultrasonic measurements in crack detection and general quality assurance. Both commercial instruments and specially developed devices have been tested on site. Using commercial ultrasonic echo devices designed for concrete inspection it was possible to detect cracks and objects in salt concrete up to a depth of 2 m. The check for delamination in shotcrete is another field of application. A unique device available at BAM, the wide aperture, deep penetration instrument LAUS, was able to locate cracks and objects up to a depth of 8 m so far, which is thought to be a record for ultrasonic echo measurements in concrete. Adapted imaging procedures, partly adopted from geophysics, helped to reveal 3D structure at depth. In addition, we have developed ultrasonic probes to be deployed in boreholes, currently at up to 20 m depth. They can collect information on cracks and other features in a radius of about 1.5 m around the borehole in the current version and might be used in echo or transmission mode. Evaluation experiments have been performed at an experimental barrier at the ERAM site in Morsleben, Germany. The results showed several empty and injected cracks as well as built-in instrumentation. The results have been verified using borehole endoscopy as well as core examination and will be used to set up a reliable quality assurance system for engineered barriers. All instruments are based on ultrasonic shear wave transducers with a frequency range between 25 kHz and 100 kHz. Current research focuses on the improvement of the hardware (e. g. optimization of array characteristics) and imaging techniques such as Reverse Time Migration, both aiming at the improvement of depth of penetration, resolution and probability of detection. T2 - 2nd International Conference on Monitoring in Geological Disposal of Radioactive Waste CY - Paris, France DA - 09.04.2019 KW - Morsleben Repository (ERAM) KW - Engineered Barrier System (EBS) KW - Large Aperture Ultrasonic System (LAUS) KW - Ultrasonic-Echo Borehole Probe KW - Reverse Time Migration (RTM) PY - 2019 AN - OPUS4-47781 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis A1 - Prager, Jens T1 - Bestimmung der Rissgeometrie bei der zerstörungsfreien Ultraschallprüfung mit geführten Wellen N2 - In der zerstörungsfreien Prüfung werden in zunehmendem Maße geführte Ultraschallwellen zur Lokalisation von Fehlstellen genutzt. Geführte Ultraschallwellen zeichnen sich dadurch aus, dass sie große Distanzen innerhalb des zu prüfenden Bauteiles zurücklegen können. Das Ultraschallwellenfeld setzt sich dabei aus verschieden Moden zusammen. Etablierte Prüfverfahren mit geführten Wellen ermitteln häufig nur die Position der Fehlstelle, wobei die Laufzeiten der reflektierten Signale ausgewertet wird. Modenumwandlung bleibt dabei zumeist unberücksichtigt. Die Charakterisierung der Fehlstelle, zum Beispiel hinsichtlich der Länge eines Risses, ist dagegen herausfordernd. Aussagekräftige Zusammenhänge zwischen der Dimension oder Geometrie der Fehlstelle und ihrer Interaktion mit der Ultraschallwelle zu finden, ist Teil aktueller Forschung. Insbesondere eine Betrachtung der Moden höherer Ordnung und deren Amplitudenverhältnisse kann beim Aufspüren dieser Zusammenhänge hilfreich sein. Im Beitrag werden zunächst die Zusammenhänge zwischen den beiden fundamentalen Moden in einer isotropen Platte und der Länge eines Risses untersucht. Aus den Ergebnissen wird ein inverses Verfahren motiviert. Ein Algorithmus wird vorgestellt, der die Risslänge im Modell solange variiert, bis er die modalen Zusammenhänge einer Vorgabe oder einer Messung rekonstruiert. Die eingesetzte Scaled Boundary Finite Element Method ermöglicht dabei eine sehr kurze Rechenzeit in jeden Optimierungsschritt. Zusätzlich ermöglicht die Methode eine Auswertung der modalen Zusammenhänge ohne Postprocessing, was die Rechenzeiten weiter verkürzt. T2 - DAGA 2019 - 45. Jahrestagung für Akustik CY - Rostock, Germany DA - 18.03.2019 KW - Geführte Ultraschallwellen KW - Zerstörungsfreien Prüfung KW - Scaled Boundary Finite Element Method PY - 2019 VL - 45 SP - 1063 PB - Deutsche Gesellschaft für Akustik e.V. AN - OPUS4-47783 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel A1 - Gaal, Mate T1 - Plasma-akustische Wechselwirkungen von Mikrohohlkathodenentladungen N2 - Während des Entladungsprozesses interagieren Mikrohohlkathodenentladungen (engl. micro hollow cathode discharges) durch verschiedenste physikalische Phänomene mit ihrer Umgebung. Analog zu Funken- und Koronaentladung treten neben den optischen Erscheinungen auch akustische Wechselwirkungen bis in den Ultraschallbereich auf. Diese Wechselwirkungen sind bisher jedoch nur selten Gegenstand der Forschung gewesen. Durch elektro-chemischen Prozesse und die Stromdichteverteilung während des Zündvorgangs erfährt das angrenzende Fluid eine, durch den thermoakustischen Effekt hervorgerufene, rapide Dichteänderung und erzeugt somit eine akustische Emission. Dieser Beitrag gibt einen Überblick über den letzten Stand der akustischen Beschreibung der Mikrohohlkathode. Weiterhin wird anhand von Anwendungsbeispielen, wie der Charakterisierung von akustischen Sensoren, sowie der Nutzung innerhalb der zerstörungsfreien Werkstoffprüfung, die Nutzung dieser Entladungsart präsentiert. Darüber hinaus erlaubt die Kenntnis hinsichtlich der akustischen Eigenschaften der Entladung wichtige Rückschlüsse im Rahmen der Plasmadiagnostik. T2 - 45. Jahrestagung für Akustik (DAGA 2019) CY - Rostock, Germany DA - 18.03.2019 KW - Micro hollow cathode discharge KW - Atmospheric pressure plasma PY - 2019 SP - 1049 EP - 1051 AN - OPUS4-47790 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona T1 - Cybersicherheit als eine Voraussetzung für sichere Produkte, Dienstleistungen und Prozesse: Der neue europäische Rechtsakt zur Cybersicherheit N2 - Bedeutung von Cybersicherheit für die Konformitätsbewertung Vorstellung Rechtsakt zur Cybersicherheit [COM(2017)477] vom 13.9.2017 bzw. letzter Entwurf vom 12.3.2019 Ergebnisse einer Analyse der Reaktionen von interessierten Kreisen Kurzvorstellung ausgewählter Normen im Bereich Cybersicherheit T2 - EUROLAB-D Kolloquium CY - BAM, Berlin, Germany DA - 09.04.2019 KW - Cybersicherheit KW - Zertifizierung KW - Cybersecurity Act KW - Cybersecurity PY - 2019 AN - OPUS4-47771 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wasmer, Paul A1 - Bulling, Jannis A1 - Prager, Jens T1 - Entwicklung eines Ultraschallrohrsensors auf Basis phononischer Kristalle N2 - Die Messung von Flüssigkeitskonzentrationen in Rohrsystemen ist von großem Interesse für viele unterschiedliche Anwendungen. Die meisten Messsysteme sind jedoch nicht in der Lage, die Flüssigkeit direkt im Rohr zu untersuchen und es muss eine zusätzliche Vorrichtung, wie z.B. einem Bypass, angebracht werden, welche den Kontakt zwischen Flüssigkeit und Sensor ermöglicht. Um den Einbauaufwand gering zu halten und die Strömungseigenschaften des Rohres nicht zu beeinflussen, wird ein neuartiges Messsystem entwickelt, welches als Teil der Rohrwand ausgeführt werden kann. Dieses neuartige System ist angelehnt an die Idee der phononischen Kristallen (PnK). PnK’s bestehen im Allgemeinen aus einem Matrixmaterial, in welchem Streuzentren periodisch angeordnet sind. Dies führt beim Eintreffen einer akustischen Welle in definierten Frequenz-bereichen, sogenannter Bandlücken, zu zunehmender destruktiven Interferenz. Wird innerhalb einer solchen Bandlücke durch Einbringen einer flüssigkeitsgefüllten Kavität ein Resonanzverhalten erzeugt, kann dies genutzt werden, um die Flüssigkeit zu analysieren. Im Rahmen von Voruntersuchung wird zunächst das akustische Verhalten des PnK’s, welcher für die Sensorentwicklung genutzt werden soll, unter Vernachlässigung der Flüssigkeit ausführlich untersucht. Hierbei werden zunächst die Bandlücken ermittelt und das Übertragungsverhalten betrachtet. Dieses wird im Anschluss experimentell überprüft. T2 - DAGA 2019 - 45. Jahrestagung für Akustik CY - Rostock, Germany DA - 18.03.2019 KW - Phononischer Kristall KW - Ultraschall KW - Flüssigkeitssensor KW - Scaled Boundary Finite Element Method PY - 2019 SP - 1030 EP - 1033 AN - OPUS4-47780 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel A1 - Gohlke, Dirk T1 - Herausforderungen bei der Prüfung von Schmiedeteilen durch Vorsatzkeile für Longitudinalwellenprüfköpfe N2 - Trotz moderner Sensortechnologien und Rekonstruktionsmethoden, findet die manuelle und automatisierte Ultraschallprüfung durch konventionelle Senkrecht- und Winkelprüfköpfe vielfach industriellen Einsatz. Um einen flexiblen Prüfeinsatz und die Prüfbarkeit von einfachen sowie komplexen Geometrien zu gewährleisten, werden dort oftmals Vorlaufkeile für die Winkelprüfung mit Longitudinalwellen angewendet um eine Anzeigenschräglage und deren Reflektivität auszugleichen bzw. zu verbessern. Durch den unterschiedlichen Aufbau, im Vergleich zu integrierten Scherwellen-Winkelprüfköpfen, können jedoch während der Prüfung Fehlanzeigen generiert werden. Diese fehlerhaften Anzeigen beruhen auf Mehrfachreflexionen und Wellenumwandlungen innerhalb des Vorlaufkeils, aufgrund der Geometrie, und können im Feld nur bedingt von realen Anzeigen unterschieden werden. Dieser Beitrag zeigt die geometrische Betrachtung bei der Verwendung von Vorlaufkeilen und wurde experimentell durch die Bestimmung der Richtcharakteristik und dem Einsatz von elektrodynamischen Sonden validiert. Des Weiteren ermöglichen die so gewonnenen Abhängigkeiten einen vom Keilwinkel abhängigen Verstärkungsausgleich und somit eine korrekte Größenbestimmung durch einen geeigneten Vergleichsfehler. T2 - DACH Tagung der DGZfP CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Kotakttechnik KW - Wellenausbreitung KW - Richtcharakteristik PY - 2019 AN - OPUS4-48094 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - How to write your thesis N2 - Useful tips & tricks to overcome procrastination and get you PhD thesis written. T2 - 13. Interdisziplinäres Doktorandenseminar CY - Berlin, Germany DA - 19.03.2019 KW - Outreach KW - Pomodore KW - Deep work PY - 2019 AN - OPUS4-48097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkler, Nicolas P. T1 - Remote gas sensing with multicopter platforms N2 - This presentation gives an introduction to the gas-sensitive aerial robots developed at BAM, including various application examples in the field of mobile robot olfaction: gas source localization and gas distribution mapping. T2 - Zweites Innovationsforum "Autonome, mobile Dienste; Services für Mobilität" CY - Berlin, Germany DA - 04.06.2019 KW - Localization of gas sources KW - Mobile Robot Olfaction KW - Nano UAV Swarm KW - Tomographic reconstruction of gas plumes KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - UAV-REGAS PY - 2019 AN - OPUS4-48167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf A1 - Pohl, Rainer A1 - Lohde, Sebastian A1 - Aydoğdu, M. T1 - Zerstörungsfreie Prüfung von Composite-Druckgefäßen mit konventioneller und hochfrequenter Wirbelstromtechnik N2 - Composite-Druckgefäße für den Gefahrguttransport sowie für Wasserstoff- und Erdgasfahrzeuge bestehen aus einem lasttragenden Composite und einer gasdichten, metallischen oder polymeren Barriereschicht (Liner). Zur Untersuchung des Alterungsverhaltens solcher Composite-Druckgefäße wurde in der BAM das interdisziplinäre Themenfeldprojekt COD-AGE durchgeführt. Ziel des Projektes war die Entwicklung von Methoden und Modellen zur Beschreibung und Bestimmung des Alterungsverhaltens von Carbonfaser-Compositen am Beispiel von Druckgefäßen, um eine bessere Vorhersage der Alterung und der sicheren Gebrauchsdauer zu ermöglichen. Ein Schwerpunkt in diesem Projekt war die Bereitstellung geeigneter ZfP-Methoden. Dabei ging es sowohl um versuchsbegleitende Prüfungen, als auch um die mögliche Entwicklung von Prüfeinrichtungen für den späteren praktischen Gebrauch. In dem Vortrag werden Prüfergebnisse der alterungsbegleitenden Wirbelstromprüfung an Composite-Druckgefäßen vorgestellt. In Alterungsversuchen wurden Druckgefäße aus einem ca. 4 mm dicken Aluminiumliner und ca. 8 mm dicker CFK-Ummantelung untersucht. Typisches Einsatzgebiet solcher Druckgefäße sind Atemschutzgeräte der Feuerwehr. Die Druckgefäße wurden sowohl mit konventioneller Wirbelstromtechnik von außen und von innen als auch mit hochfrequenter Wirbelstromtechnik von außen geprüft. Es konnten sowohl Beschädigungen des metallischen Liners, als auch Strukturen des CFK-Geflechts nachgewiesen werden. Eine besondere mechanische Herausforderung bestand in der Prüfung der Innenseite der Liner, da hier eine zylindrische Fläche mit einem Innendurchmesser von 150 mm durch einen Zugang von nur 15 mm Durchmesser geprüft werden muss. T2 - DACH-Jahrestagung CY - Friedrichshafen, Germany DA - 26.05.2019 KW - Wirbelstromprüfung KW - COD-AGE KW - Composite-Druckgefäß KW - CFK PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481243 SN - 978-3-947971-02-2 VL - 171 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-48124 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - New insights in cocrystal formations: in situ investigations of mechanochemical syntheses N2 - Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals. The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms. We introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. We discuss our recent results investigating the formation of (polymorphic) cocrystals. First investigations of a mechanochemical synthesis under controlled temperature which allow determining the activation barrier are presented.6 Furthermore, X-ray diffraction and in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat. Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds. T2 - CSEC Seminar University of Edinburgh CY - Edinburgh, Scotland DA - 16.05.2019 KW - Mechanochemistry KW - Acoustic levitation KW - In situ PY - 2019 AN - OPUS4-48098 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel A1 - Gohlke, Dirk A1 - Dobrovolskij, P. A1 - Vrana, J. A1 - Heckel, Thomas T1 - Herausforderungen bei der Prüfung von Schmiedeteilen durch Vorsatzkeile für Longitudinalwellenprüfköpfe N2 - Trotz moderner Sensortechnologien und Rekonstruktionsmethoden, findet die manuelle und automatisierte Ultraschallprüfung durch konventionelle Senkrecht- und Winkelprüfköpfe vielfach industriellen Einsatz. Um einen flexiblen Prüfeinsatz und die Prüfbarkeit von einfachen sowie komplexen Geometrien zu gewährleisten, werden dort oftmals Vorlaufkeile für die Winkelprüfung mit Longitudinalwellen angewendet um eine Anzeigenschräglage und deren Reflektivität auszugleichen bzw. zu verbessern. Durch den unterschiedlichen Aufbau, im Vergleich zu integrierten Scherwellen-Winkelprüfköpfen, können jedoch während der Prüfung Fehlanzeigen generiert werden. Diese fehlerhaften Anzeigen beruhen auf Mehrfachreflexionen und Wellenumwandlungen innerhalb des Vorlaufkeils, aufgrund der Geometrie und können im Feld nur bedingt von realen Anzeigen unterschieden werden. Dieser Beitrag zeigt die geometrische Betrachtung bei der Verwendung von Vorlaufkeilen und wurde experimentell durch die Bestimmung der Richtcharakteristik und dem Einsatz von elektrodynamischen Sonden validiert. Des Weiteren ermöglichen die so gewonnenen Abhängigkeiten einen vom Keilwinkel abhängigen Verstärkungsausgleich und somit eine korrekte Größenbestimmung durch einen geeigneten Vergleichsfehler. T2 - DACH-Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Richtcharakteristik KW - Vorlaufkeile KW - Mehrfachreflexion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480999 VL - 2019 SP - 1 EP - 7 PB - DGZfP Deutsche Gesellschaft für Zerstörungsfreie Prüfung AN - OPUS4-48099 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Procop, Mathias T1 - Check of Energy-Dispersive X-ray Spectrometers (EDS) Performance with the BAM Test Material EDSTM001/2 and BAM Software EDS Spectrometer Test N2 - The test material EDS-TM001 together with an accompanying software package, “EDX spectrometer check”, have been made available in 2009 by BAM to be employed by EDS (energy-dispersive X-ray spectrometer) users to check the performance of an EDS attached to the SEM. Particularly for test laboratories operating under accreditation schemes like ISO/IEC 17025, a periodical control of the critical instrumental parameters in end-user laboratories is required. With EDS-TM001 or EDS-TM002 (second generation) test material, this periodical check is simplified to the acquisition of only one 10 kV spectrum. The software “EDX spectrometer check” is destined to evaluate automatically this spectrum and determine the performance of the EDS in terms of energy resolution and calibration, as well as possible alteration of low-energy Efficiency due to detector contamination. Energy resolution can be compared with the specified values according to the international ISO standard ISO 15632:2012. EDS-TM is a synthetic material consisting of a 6 μm thick layer of C, Al, Mn, Cu and Zr deposited on a steel (in case of EDS-TM001) or silicon (in case of EDS-TM002) substrate. The chemical composition of EDS-TM was chosen such as to give nearly equal intensities of the low energy lines in a 10 kV spectrum, thus, making it very sensitive against spectrometer efficiency changes. Meanwhile, about 150 laboratories use the EDS-TM001 or EDS-TM002 test material for the periodical check of their EDS. A detailed description of the test material and software together with examples of application was published recently. New results and gained experiences will be presented as well. When the FWHM of the X-ray lines in the EDS-TM spectrum are determined, the spectrum background must be subtracted accurately. The applied physical background subtraction procedure is robust and takes into account the transmission of the detector window. While the previous version considers only Moxtek AP windows, the new version includes selection of silicon Nitride window and the case of windowless detector. Moreover, the new version allows importing of spectra in Bruker spx-format and EMSA/MSA files from EDAX TEAM software. Windowless detectors have been also tested demonstrating long-term stability after repeated heating and cooling cycles. In this case, the appropriate Background subtraction is decisive for accurate detector characterization. Detailed results will be presented. T2 - EMAS 2019 - 16th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS CY - Trondheim, Norway DA - 19.05.2019 KW - EDS KW - Test material KW - Software KW - Spectrometer check KW - X-ray spectroscopy PY - 2019 AN - OPUS4-48103 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. T1 - Measurement of Elemental Composition of FeNi and SiGe Alloy Thin Films by EMPA and µ-XRF N2 - It was demonstrated in the past that the electron probe microanalysis (EPMA) can be applied to determine accurately both elemental composition and thickness of thin films by using the dedicated software package for thin film analysis Stratagem. A relatively small number of film materials such as pure metallic films of platinum and nickel, binary alloys of Fe-Ni, and Pt-Ni-Co ternary alloy films has been reported in literature as working successfully. Further, the software can be applied ‘inversely’, i.e., by feeding it with the thickness of the film and using the determined mass coating, one can easily calculate the film density, which for porous layers leads us to the true film porosity. The present study repeats measurements on an already tested system of Fe-Ni thin films on silicon and reports for the first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide substrate. Standard-based and standardless EPMA (with EDS) results were used in combination with Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Compared to EPMA, XRF has a larger information depth and a higher elemental sensitivity because of a generally lower background. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. The atomic fractions of all the samples including the references have been certified by RBS (Rutherford backscattering spectrometry) and ICP-AES (inductively coupled plasma atomic emission spectroscopy). T2 - EMAS 2019 - 16th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS CY - Trondheim, Norway DA - 19.05.2019 KW - Thin film analysis KW - SEM/EDS KW - EPMA KW - Fe-Ni KW - Si-Ge PY - 2019 AN - OPUS4-48104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Analysis of elemental composition and porosity of mesoporous IrOx-TiOx thin films by SEM/EDS N2 - Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material, as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge even for modern analytical techniques and requires new approaches employing the combination/complementation of data of different analytical methods. In this contribution, we characterise thin mesoporous iridium-titanium mixed oxide film properties by electron probe microanalysis (EPMA) with energy-dispersive X-ray spectroscopy (EDS) at an SEM. Mesoporous iridium oxide - titanium oxide (IrOx-TiOx) films were prepared via dip-coating of a solution containing a triblock-copolymer as structure-directing agent, an iridium precursor as well as a titanium precursor in ethanol. IrOx-TiOx films were synthesized with different amounts of iridium and calcined in air. The SEM micrographs reveal for all films the achievement of a well-ordered mesoporous structure and homogeneous films with thicknesses between 67 nm and 152 nm. For the determination of film elemental composition and porosity, EPMA can be used as part of a combined SEM/EDS/STRATAGem analysis. Elemental compositions and mass depositions (in μg cm-2) of IrOx-TiOx films were calculated with the thin film analysis Software STRATAGem via k-values measured with SEM/EDS. Pure bulk Ir, TiO2 and Si were measured as references. The average density of the films was obtained from the mass Deposition and the film thickness as measured by cross-section SEM. The porosity was then extracted from the measured average film density divided by a theoretical bulk density. The latter is calculated from the weight fractions of IrOx and TiOx as determined with STRATAGem and the bulk mass densities of IrO2 and TiO2 (rutil) from literature. The fitting results of the k-values from the STRATAGem software, which are in fair agreement with the measured k-values. The application of the SEM/EDS/STRATAGem approach for accurate porosity determination on pure mesoporous TiOx films and pure porous IrOx films has been recently demonstrated. The porosities of pure IrOx, TiOx and mixed IrOx-TiOx films in this study have been determined. The contribution will assess in detail the advantages and limitations of the combined SEM/EDS/STRATAGem analysis for the morphology and porosity of thin metal oxide films. Moreover, the comparison with other measurement techniques and the combination of datasets from multiple measurements will be discussed. T2 - EMAS 2019 - 16th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS CY - Trondheim, Norway DA - 19.05.2019 KW - Thin films KW - Porous layers KW - Electron probe microanalysis (EPMA) KW - Porosity PY - 2019 AN - OPUS4-48107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - High-Quality Data in Microbeam Analysis – Possible Joint Exercises N2 - Microbeam analysis data are of continuously improving quality, this owing mainly to developments in instrumentation (hardware and software) and computer performance. The knowledge and skills of the operators must be also kept correspondingly updated. To be deemed as technically competent, the laboratories must be accredited according to an accreditation scheme, mostly following ISO/IEC 17025. International standards are able to provide requirements, specifications, guidelines or characteristics of methods, instruments or samples with the final goal that these can be used consistently in accredited laboratories. In the field of electron microscopy and microbeam Analysis standardisation and metrology are terms that are encountered rather seldom at major conferences and scientific publications. Several ISO standards already published and used successfully by a large part of the electron microscopy and microbeam analysis community. For example, file formats such as EMSA/MSA for spectral-data exchange or tagged image file format (TIFF) for SEM images; procedures for the specification of X-ray spectrometers, the specification of certified reference materials (CRMs), and for measurement of average grain size by electron backscatter diffraction (EBSD); and guidelines for calibrating image magnification in SEM or TEM. A main task of ISO technical committee TC 202 ‘Microbeam Analysis’ is to identify feasible projects/proposals needed to be developed into new international standards, particularly in respect to recent technology, such the silicon drift detector (SDD). As far as the metrological aspects are regarded, The International Bureau of Weights and Measures (BIPM) through the Consultative Committee for the Amount of Substance (CCQM) is concerned with the metrological aspect in Chemistry and Biology. In particular, the Surface Analysis Working Group (SAWG) assists in identifying and establishing inter-laboratory work to test the consistency as well as to improve the traceability of spatially resolved chemical surface analysis at the micro and nanoscale. Examples of recent projects on quantitative microbeam analysis at low energies, such as the quantification of light elements such as carbon and nitrogen will be presented. The significant sources of measurement uncertainty will be emphasized. These are: quality of the unknown and the reference materials used, the quantification model, instrumental parameters like take-off-angle, spectrometer efficiency, and particularly the beam current. The crucial importance of working with uniform and well-defined measurement and data evaluation protocols will be discussed in compliance with the ISO document “Guide to the expression of uncertainty in measurement (GUM)”. Another international platform where pre-standardisation work can be organised is VAMAS (Versailles Project on Advanced Materials and Standards). International collaborative Projects aim at providing the technical basis for harmonised measurements, testing, specifications, and standards to be further developed at ISO level. One key point of VAMAS activities is constituted by inter-laboratory comparisons for high-quality data. In the field of microbeam analysis, the technical working area (TWA) 37 Quantitative Microstructural Analysis deals with corresponding projects. Good ideas, e.g., on analysis at low energies, are particularly encouraged by directly contacting the author. Support and guidance will be supplied. T2 - EMAS 2019 - 16th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS CY - Trondheim, Norway DA - 19.05.2019 KW - Data KW - Inter-laboratory comparison KW - Electron probe microanalysis (EPMA) KW - EBSD KW - VAMAS KW - Electron microscopy PY - 2019 AN - OPUS4-48108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lörchner, Dominique A1 - Kraus, Werner A1 - Köppen, Robert T1 - Photodegradation of the novel brominated flame retardant 2,4,6-Tris-(2,4,6-tribromophenoxy)-1,3,5-triazine in solvent system: Kinetics, photolysis products and pathway. N2 - In this study the direct and indirect photolysis of the novel brominated flame retardant 2,4,6-Tris-(2,4,6-tribromophenoxy)-1,3,5-triazine (TTBP-TAZ) in an organic solvent mixture (60:30:10, ACN:MeOH:THF) under UV-(C) and simulated sunlight irradiation was investigated, and the formed photo-transformation products were identified for the first time. TTBP-TAZ was almost completely degraded within 10 min under UV-(C) irradiation. Due to the fast degradation no specific kinetic order could be observed. In comparison, the reaction under simulated sunlight irradiation was much slower and thus, the kinetic first-order could be determined. The observed photolysis rate constant k as well as the half-life time t1/2 were estimated to be k = (0.0163 ± 0.0002) h-1 and t1/2 = 42.3 h, respectively. The addition of 2-propanol and hydrogen peroxide to investigate the influence of indirect photolysis under UV-(C) irradiation causes no influence on the degradation of TTBP-TAZ. Nevertheless, the removal of TTBP-TAZ under UV-(C) and simulated sunlight without additional chemicals (except solvent) indicates that the direct photolysis plays a significant role in the degradation mechanism of TTBP-TAZ. In both irradiation experiments, TTBP-TAZ was quantitatively degraded that involve the formation of previously unknown PTPs. Overall, two main PTPs were determined when irradiated with UV-(C) and eight sequential debromination products were observed when irradiated by simulated sunlight. These were determined by HPLC-DAD and - MS/(MS), respectively. Based on the chosen experimental conditions the consecutive debromination as well as photo-Fries rearrangement was confirmed as the main degradation pathway by high resolution mass spectrometry and X-ray diffraction. KW - XRD KW - Direct/indirect photolysis KW - HRMS KW - Photo-transformation products KW - TTBP-TAZ PY - 2019 DO - https://doi.org/10.1016/j.chemosphere.2019.04.184 SN - 0045-6535 SN - 1879-1298 VL - 229 SP - 77 EP - 85 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-48066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Fachbereich 8.4 - Akustische Verfahren N2 - Die akustischen Verfahren der zerstörungsfreien Prüfung werden vorgestellt, die im Fachbereich 8.4 der BAM entwickelt werden. T2 - DGZfP Sitzung des Fachausschusses Luftfahrt CY - Berlin, Germany DA - 18.04.2019 KW - Ultraschall KW - Luftultraschall KW - Tauchtechnik KW - Geführte Wellen PY - 2019 AN - OPUS4-48069 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Brinker, U. A1 - Meinel, Dietmar A1 - Teßmann, B. A1 - Lübke, H. ED - Lewerentz, Annette T1 - Die menschlichen Skelettreste der zur anthropologischen Rudolf-Virchow-Sammlung gehörenden Kollektion des Fundplatzes Rinnukalnsim Norden Lettlands – Resultat eines Forschungsstreites des 19. Jahrhunderts im damaligen Livland N2 - In der anthropologischen Rudolf-Virchow-Sammlung der Berliner Gesellschaft für Anthropologie, Ethnologie und Urgeschichte (BGAEU) befindet sich eine größere Anzahl menschlicher Schädel aus dem Gebiet des heutigen Lettlands, die Mehrzahl dabei von der im Norden Lettlands am Burtnieksee gelegenen Fundstelle Riņņukalns. Der nachfolgende Aufsatz beschreibt die Gründe, warum diese Stücke in den 1870er Jahren in die Sammlung gelangt sind, und präsentiert eine anthropologische Dokumentation und Analyse der Schädelfunde vom Riņņukalns aus der Sammlung. KW - Mikro-CT KW - Anthropologie KW - Schädelfunde PY - 2018 SN - 978-3-86757-994-0 SN - 0178-7896 VL - 39 SP - 35 EP - 54 PB - Berliner Gesellschaft für Anthropologie, Ethnologie und Urgeschichte CY - Berlin AN - OPUS4-48071 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Hofmann, Michael T1 - Monitoring der Ameisensäurekonzentration in Bienenstock-Luft N2 - Die Varroose gilt weltweit als eine der bedeutendsten Erkrankungen der westlichen Honigbiene, Apis mellifera. Verursacht wird sie durch den Ektoparasiten Varroa destructor, der durch Saugen der Hämolymphe und Virenübertragung sowohl die Bienenbrut als auch die adulten Individuen schädigt. Ohne imkerliche Unterstützung gehen betroffene Bienenvölker in der Regel innerhalb von drei Jahren ein. Als bewährte, häufige Behandlung wird flächendeckend 60%ige Ameisensäure (AS) -im Bienenstock appliziert über verschiedene Verdampfungssysteme- eingesetzt. Sie wirkt als einziger zugelassener Wirkstoff gegen die Varroamilbe auch in die verdeckelte Brut hinein und birgt kein Risiko der Resistenzentwicklung. Allerdings ist das therapeutische Fenster, der Bereich zwischen Milbenabtötung und Bienenschädigung, relativ schmal und die tatsächliche AS-Konzentration im Bienenstock stark abhängig von äußeren Einflussfaktoren, wie Temperatur oder Applikationsart. Eine Bestimmung der exakten AS-Konzentration im Bienenstock ist also notwendig, um einerseits das Wirkungsoptimum zu bestimmen und andererseits bei Übersteigen der Maximalkonzentrationen mit Folge-Schädigung der Bienen, ein rechtzeitiges Eingreifen der Imker zu ermöglichen. Die Entwicklung eines Detektors zur Bestimmung der tatsächlichen AS-Konzentration in der Bienenstockluft würde einen großen Fortschritt in den Bereichen der Bienenforschung, der Varroa-Behandlung in der Imkerei, sowie einer gesundheitlich bedenklichen AS-Exposition für den Imker bedeuten. Langfristiges Ziel dieses Projekts ist es, ein mobiles, einfach handhabbares Gerät zur Detektion der AS-Konzentration in der Bienenstock-Luft während einer AS-Behandlung zu entwickeln. Grundlage hierfür bietet ein kommerziell verfügbares Multigassensorsystem (PEN3, AIRSENSE Analytics GmbH, Schwerin). Ziel der beschriebenen Vorversuche ist die generelle Eignungsprüfung des Multigassensorsystems PEN3 zur Detektion der hohen AS-Konzentration in Gasgemischen unter Bedingungen wie sie im Bienenstock während einer AS-Behandlung herrschen. Als Messplatz zur Detektion von AS in Luft wurden zwei Systeme vorbereitet: A) Eine Plexiglasbox mit einem Volumen von ca.1,9 l diente als Prüfkammer, wurde von einem Gasstrom befeuchteter synthetischer Luft durchströmt (50 mL min-1, 100 mL min-1 oder 300 mL min-1) und zur Temperierung auf 25 °C auf einer Heizmatte bzw. auf 35 °C in einem Ofen platziert. AS-Wasser-Gemische verschiedener Volumenverhältnisse (0-100%) wurden in einer Glasschale (Oberfläche Flüssigphase 9,6 cm2) in der Prüfkammer vorgelegt. B) In einer durch eine Heizmatte auf 25 °C temperierten, zwei-zargigen Segeberger Beute wurden vier Messpunkte angebracht (davon drei in der oberen und einer in der unteren Etage) und 60%ige AS über einen Nassenheider-Verdampfer vertikal vorgelegt. Zur Detektion des AS-Luft-Gemischs wurde das PEN3 Multigassensorsystem genutzt. Das zu untersuchende Gasgemisch wurde über die internen zehn Metalloxid-Halbleiterdetektoren (1-10) der PEN3 geleitet. Das so generierte Messsignal beschreibt ein Widerstandsverhältnis zwischen dem Widerstandwert zum Zeitpunkt der Messung (R) und dem elektrischen Widerstand bei der Nullluft-Messung (R0), wobei hier befeuchtete synthetische Luft mit einer reltativen Feuchte von 49 % ± 4 % oder Raumluft genutzt wurde. Gase unterschiedlicher Zusammensetzung können anhand der dargestellten Signalmuster verschiedener Sensoren voneinander unterschieden werden. In beiden Messsystemen wiesen die Sensorelemente 1, 6, 7, 8 und 9 gesteigerte Sensitivitäten beim Vorliegen von Ameisensäure im Gasgemisch auf. Die größten Widerstandsverhältnisse zeigten dabei die Sensorelemente 6, 8 und 9, sodass hier von der höchsten Empfindlichkeit für AS auszugehen ist. Basierend auf den erhobenen Messdatensätzen wurden Hauptkomponenten- (PCA) und lineare Diskriminanzanalysen (LDA) zur Dimensionsreduktion durchgeführt, um charakteristische Muster aus den Messsignalen zu extrahieren. Die PCA- und LDA-Plots für die jeweils bedeutsamsten Komponenten PC 1 und PC 2 bzw. LD 1 und LD 2 eines Versuchslaufs in der Plexiglasbox (A) bei einer Temperatur von 35°C, einem Volumenstrom von 300 mL min-1 und variablen Ameisensäure-Wasser-Volumenverhältnissen von 0 % bis 100 %. Deutlich erkennbar sind die Abhängigkeiten der Komponenten PC 1 und LD 1 (Abszissen) vom vorgelegten AS-Wasser-Volumenverhältnis. Unsere Ergebnisse zeigen, dass das Multigassensorsystem zur Bestimmung von AS in Luft unter ähnlichen Bedingungen wie bei einer AS-Behandlung im Bienenstock angewandt werden kann. Die Versuche zeigen, dass die im PEN3 eingesetzten Metalloxid-Sensoren bzw. Metalloxidsensor-Arrays zur Detektion von AS in Luft auch bei höheren Konzentrationen als beispielsweise der MAK-Wert von 5 µmol/mol zur Überwachung des AS-Gehaltes in Bienenstöcken angewandt werden können. Aufgrund der Möglichkeit der quasi Echtzeit-Messdatengenerierung, der geringen Kosten kommerziell verfügbarer Sensorelemente, der Portabilität und der Möglichkeit zur Miniaturisierung zeichnen sich solche Messsysteme zukünftig durch eine besondere Praxisnähe aus. Diese Erkenntnisse sind Grundlage für eine Verbesserung des Detektionsverfahrens und zur Vorhersage über die Effizienz und Effektivität der Varroha-Milbenbehandlung. T2 - Tierbiochemisches Seminar CY - Freie Universität Berlin, Germany DA - 24.05.2019 KW - Ameisensäure KW - Methansäure KW - Multigassensor KW - Sensorik KW - Biene KW - Imker PY - 2019 AN - OPUS4-48076 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hirschberger, Paul A1 - Baurzhan, Zhandos A1 - Tiebe, Carlo A1 - Hofmann, Michael A1 - Hüllmann, Dino A1 - Bartholmai, Matthias T1 - Indoor air quality monitoring using flying nanobots: Design and experimental study N2 - In this paper, we introduce a nano aerial robot swarm for Indoor Air Quality (IAQ) monitoring applications such as occupational health and safety of (industrial) workplaces. The robotic swarm is composed of nano Unmanned Aerial Vehicles (UAVs), based on the Crazyflie 2.0 quadrocopter, and small lightweight Metal Oxide (MOX) gas sensors for measuring the Total Volatile Organic Compound (TVOC), which is a measure for IAQ. An indoor localization and positioning system is used to estimate the absolute 3D position of the swarm similar to GPS. A test scenario was built up to validate and optimize the swarm for the intended applications. Besides calibration of the IAQ sensors, we performed experiments to investigate the influence of the rotor downwash on the gas measurements at different altitudes and compared them with stationary measurements. Moreover, we did a first evaluation of the gas distribution mapping performance. Based on this novel IAQ monitoring concept, new algorithms in the field of Mobile Robot Olfaction (MRO) are planned to be developed exploiting the abilities of an aerial robotic swarm. T2 - 18th International Symposium on Olfaction and Electronic Nose CY - Fukuoka, Japan DA - 26.05.2019 KW - Nano aerial robot KW - Swarm KW - Indoor air quality KW - Monitoring PY - 2019 SN - 978-1-5386-3641-1 SP - 1 EP - 3 PB - IEEE CY - USA AN - OPUS4-48148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Indoor air quality monitoring using flying nanobots: Design and experimental study N2 - In this paper, we introduce a nano aerial robot swarm for Indoor Air Quality (IAQ) monitoring applications such as occupational health and safety of (industrial) workplaces. The robotic swarm is composed of nano Unmanned Aerial Vehicles (UAVs), based on the Crazyflie 2.0 quadrocopter, and small lightweight Metal Oxide (MOX) gas sensors for measuring the Total Volatile Organic Compound (TVOC), which is a measure for IAQ. An indoor localization and positioning system is used to estimate the absolute 3D position of the swarm similar to GPS. A test scenario was built up to validate and optimize the swarm for the intended applications. Besides calibration of the IAQ sensors, we performed experiments to investigate the influence of the rotor downwash on the gas measurements at different altitudes and compared them with stationary measurements. Moreover, we did a first evaluation of the gas distribution mapping performance. Based on this novel IAQ monitoring concept, new algorithms in the field of Mobile Robot Olfaction (MRO) are planned to be developed exploiting the abilities of an aerial robotic swarm. T2 - 18th International Symposium on Olfaction and Electronic Nose CY - Fukuoka, Japan DA - 26.05.2019 KW - Nano aerial robot KW - Swarm KW - Indoor air quality KW - Monitoring PY - 2019 AN - OPUS4-48149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Aerial- and ground-based gas tomography for increasing environmental safety in chemical industry (AGATO) N2 - In AGATO, we combine ground and aerial robots into a heterogeneous robot swarm, equip robots with gas sensors (in-situ/open-path) and/or reflectors as payload, reconstruct potential gas plumes/clouds in 3D, and identify potential gas leaks based on reconstructed tomographic images. T2 - 18th International Symposium on Olfaction and Electronic Nose CY - Fukuoka, Japan DA - 26.05.2019 KW - Mobile Robot Olfaction KW - Tomographic reconstruction of gas plumes KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - UAV-REGAS PY - 2019 AN - OPUS4-48150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Estimation of measurement uncertainty of instrumented indentation testing N2 - Some critical discussion of the state of the art of uncertainty evaluationin Instrumented Indentation Testing IIT Nowadays the Instrumented Indentation Testing (IIT), in the nano range often named as nano indention, is one of the most commonly used methods to determine the mechanical properties of materials in the micro and nano range. This method is already extensive standardized in ISO 14577 part 1-4. In the past, the application of this standard in testing praxis shows that the established values have an excellent precision.If an uncertainty is calculated, the range of values within which the true value is asserted to lie with some level of confidencewill be known. In part 1 of ISO 14577 [1] two methods for evaluation of the uncertainty in IIT are mentioned: Method 1 for determining uncertainty considers only those uncertainties associated with the overall measurement performance of the testing machine with respect to the reference blocks. Method 2calculates a combined uncertainty from individual contributions. These may be grouped into random and systematic uncertainties. Both methods will be described in detail using examples from the dailyexperimental praxis. The comparabilityof both methods will be critically discussed. Finally, it will be showedhow the calculated uncertaintiescan be used for performancetests and product specifications. Acknowledgement This work was performed under the support of the EMPIR project 17NRM05Advancing measurement uncertainty̶ comprehensiveexamples for key international standards References [1] ISO 14577 part 1 (2017) T2 - KLA Nanomechanical Testers User Workshop CY - Langen, Germany DA - 02.05.2019 KW - Instrumented Indentation Testing KW - IIT KW - nanoindentation KW - mechanical properties KW - uncertainty KW - performance test KW - product specification PY - 2019 AN - OPUS4-48141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement of elemental composition of Fe1-xNix and Si1-xGex alloy thin films by EMPA and µ-XRF N2 - It was demonstrated in the past that the electron probe microanalysis (EPMA) can be applied to determine accurately both elemental composition and thickness of thin films by using the dedicated software package for thin film analysis Stratagem. A relatively small number of film materials such as pure metallic films of platinum and nickel, binary alloys of Fe-Ni, and Pt-Ni-Co ternary alloy films has been reported in literature as working successfully. Further, the software can be applied ‘inversely’, i.e., by feeding it with the thickness of the film and using the determined mass coating, one can easily calculate the film density, which for porous layers leads us to the true film porosity. The present study repeats measurements on an already tested system of Fe-Ni thin films on silicon and reports for the first-time results of analysis on Si-Ge thin films deposited on a non-conductive aluminium oxide substrate. Standard-based and standardless EPMA (with EDS) results were used in combination with Stratagem for the quantification. Further, X-ray fluorescence analysis (XRF) can be used for the determination of elemental composition and thickness of such films as well. In this case, XRF with a μ-focus X-ray source (μ-XRF) attached to a SEM was applied. For quantification, a fundamental parameter (FP) approach has been used to calculate standard-based and standardless results. Compared to EPMA, XRF has a larger information depth and a higher elemental sensitivity because of a generally lower background. Both thin film systems have been chosen as samples of an international round robin test (RRT) organised in the frame of standardisation technical committee ISO/TC 201 ‘Surface chemical analysis’, under the lead of KRISS. The main objective of the RRT is to compare the results of atomic fractions of Fe1-xNix and Si1-xGex alloy films obtained by different surface Analysis techniques, such as X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), and secondary ion mass spectrometry (SIMS) applied in the depth-profiling operation mode. Five samples of different atomic fractions of each thin film system, i.e., Fe1-xNix and Si1-xGex, have been grown by ion beam sputter deposition on silicon and Al2O3 wafers, respectively. Reference FeNi and SiGe films with well-known elemental composition and thickness have been also supplied for standard-based analysis. The atomic fractions of all the samples including the references have been certified by RBS (Rutherford backscattering spectrometry) and ICP-AES (inductively coupled plasma atomic emission spectroscopy). T2 - EMAS 2019 - 16th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS CY - Trondheim, Norway DA - 19.05.2019 KW - EPMA KW - FeNi KW - SiGe KW - Thin film analysis KW - µ-XRF PY - 2019 AN - OPUS4-48113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Detection of microplastics using thermoanalytical methods  N2 - The presentation summarized the use of thermal analytic methods for the detection of microplastics. T2 - Workshop State of teh art of anylatical methodes for reliable detection of micro- and nanoplastics CY - Ispra, Italy DA - 13.05.2019 KW - microplastics, sampling, sampling techniques, water PY - 2019 AN - OPUS4-48119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tukhmetova, Dariya A1 - Langhammer, Nicole A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Online Isotope Analysis of Sulfur in Proteins via Capillary Electrophoresis Coupled With Multicollector ICP‐MS (CE/MC‐ICP‐MS): A Proof of Concept Study N2 - Isotope ratio analysis of sulfur in biological samples using inductively coupled plasma-mass spectrometry (ICP-MS) has gained significant interest for applications in quantitative proteomics. Advancements like coupling separation techniques with multicollector ICP-MS (MC-ICP-MS) enhance the throughput of species-specific sulfur isotope ratio measurements, fostering new avenues for studying sulfur metabolism in complex biological matrices. This proof-of-concept study investigates the feasibility of online CE/MC-ICP-MS for directly analyzing sulfur isotope ratios in proteins (albumin). Leveraging our previous work on the applicability of CE/ICP-MS for quantifying sulfur-containing biological molecules, we explore its potential for sulfur isotope analysis. Our results demonstrate that direct analysis of sulfur isotopes in albumin protein using online capillary electrophoresis MC-ICP-MS (CE/MC-ICP-MS) eliminates the need for laborious pretreatment steps, while yielding isotope ratios comparable to the reference values. Although initial precision can be improved through further system optimization and protein injection techniques, this approach paves the way for future analysis of mixtures of various biological compounds in, for example, clinical diagnosis studies. KW - Isotope analysis KW - Sulfur KW - CE/MC-ICP-MS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612439 DO - https://doi.org/10.1002/elps.202400128 SN - 0173-0835 SP - 1 EP - 6 PB - Wiley-Blackwell CY - Weinheim AN - OPUS4-61243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Machine learning - Examples from BAM Line N2 - This talk explores applications of artificial intelligence in the field of spectroscopy, with a special focus on research conducted at BAMline. We begin with an overview of synchrotron radiation and its unique capabilities in material analysis. The first part of the talk will cover the integration of AI algorithms in quantifying X-ray fluorescence measurements, providing enhanced precision and efficiency in data analysis. Following this, we will examine the role of language models in spectroscopic research, showcasing how these tools can facilitate the control of complex experimental set-ups T2 - Analytical Academy CY - Berlin, Germany DA - 12.11.2024 KW - ChatGPT KW - Neural networks KW - XRF KW - Synchrotron KW - BAMline PY - 2024 AN - OPUS4-61698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan T1 - Enhancing the Efficiency and Accessibility of Grazing Exit X-ray Absorption Spectroscopy for Corrosion and Layered Materials Analysis N2 - In the field of materials science, there is a critical need for efficient and effective characterization techniques, especially in the investigation of corrosion processes of compositionally complex alloys (CCAs) or the analysis of layered structures. This talk presents an advanced approach that combines grazing-exit X-ray absorption near-edge structure spectroscopy (GE-XANES) with Bayesian optimization (BO) to significantly improve the efficiency of data acquisition while retaining the depth-resolved, element-specific analysis capabilities that are critical for studying these materials under ambient conditions. Using a non-destructive, scan-free GE-XANES setup coupled with a pnCCD detector and grazing exit X-ray fluorescence spectroscopy (GE-XRF) geometry, our method enables precise analysis at sub-micrometer depths without the need for high vacuum environments or extensive sample preparation. The integration of BO reduces experimental time by a factor of 50, overcoming the practical limitations of conventional GE-XANES and increasing its applicability in the study of surface catalysis and corrosion processes. We validate this optimized approach through comparative studies on a CrCoNi alloy and a reference layered sample, demonstrating its potential to revolutionize materials analysis by increasing both efficiency and accessibility. T2 - Gesellschaft Deutscher Chemiker (GDCh) CY - Clausthal-Zellerfeld, Germany DA - 20.06.2024 KW - GEXRF KW - GEXANE KW - ML PY - 2024 AN - OPUS4-61788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duddi, M. A1 - Kocherla, Amarteja A1 - Subramaniam, K. V. L. T1 - Evaluation of boundary and material influences on the dynamic electromechanical impedance response of the embedded PZT sensor in concrete N2 - The article explores the material and structural size effects on the electrical impedance response of the embedded PZT sensors which are used as an sensors/actuator in the smart sensing concrete. An embedded sensor for use in concrete monitoring is developed using Lead Zirconate Titanate (PZT). The electrical impedance (EI) response of the sensor placed inside concrete cubes of varying sizes are recorded for an applied electrical input of varying frequency. The dynamic response of the embedded PZT sensor to the applied electrical input is determined by the mechanical impedance offered by the surrounding medium. In specimens of finite size, the mechanical impedance to the motion of the PZT is influenced by the combination of dynamic material resistance and structural stiffness (size of the structure). The current study examined the effects of material resistance and size of structure on the EI response of the PZT sensor embedded in concrete medium. The influence of the size of the medium from small-sized specimens is seen in the form of secondary peaks, identified as structural peaks, on the resonance spectrum of the embedded PZT sensor. The structural peaks on the EI response are very dominant in the concrete cube of small sizes. Magnitude and intensity of these structural peaks attenuate with an increase in the size of the concrete cube. Also, the EI response from the smaller-sized specimens registered a significant leftward shift in the spectrum. The observations from the numerical simulations also showed the mechanical impedance of the surrounding concrete medium to the motion of the PZT also increases and converges at 150 mm. At sizes below 150 mm, the structural effects that are influenced by the specimen boundary must be separated to access the material properties of the concrete medium from the measured EI response of an embedded PZT sensor. At sizes, larger than 150 mm, the dynamic motion of the PZT patch and the measured EI response of the PZT patch depend only on the dynamic material properties of the concrete medium around the sensor. The zone of influence and its importance in standardization of PZT sensor for SHM of concrete structures is discussed. KW - PZT KW - Concrete sensor KW - Embedded KW - Electrical impedance KW - Mechanical impedance KW - Zone of influence PY - 2023 DO - https://doi.org/10.1016/j.sna.2023.114575 SN - 0924-4247 SN - 1873-3069 VL - 361 SP - 1 EP - 12 PB - Elsevier CY - Amsterdam AN - OPUS4-61791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dhull, N. A1 - Kaur, Gurpreet A1 - Jindal, K. A1 - Verma, M. A1 - Tomar, M. T1 - Microfluidics integrated NiO based electrolyte-gated FETs for the detection of cortisol N2 - A microfluidics integrated EGFET has been devised using NiO for the detection of cortisol. A low detection limit of 0.5 fg mL−1 has been achieved and human salivary cortisol has been successfully assessed. KW - Microfluidic system KW - Field effect transistor (FET) KW - Electrolyte gating PY - 2022 DO - https://doi.org/10.1039/d2tb01652d SN - 2050-7518 VL - 10 IS - 44 SP - 9226 EP - 9234 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-61772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - From Egypt to Hiddensee – Analysis of Gold with Synchrotron Radiation V N2 - Gold is one of the seven metals already known in antiquity and was used from time immemorial as a medium of exchange and for the production of jewelry because of its luster and rarity. In addition, it is easy to work and largely resistant to chemical influences. Investigations of gold using synchrotron radiation excited X-ray fluorescence analysis are non-destructive and provide information about the chemical elements present in the sample under investigation. The investigations presented here at BAMline focus on questions such as the origin, manufacturing process, and association of gold findings. The different questions are explained by a number of examples ranging from the Viking treasure from Hiddensee to the Nebra Sky Disk and finds from Egypt. The find from Bernstorf is discussed in detail. A Bayesian treatment of the authenticity is shown. T2 - Ringvorlesung Einführung in die Archäometrie CY - Berlin, Germany DA - 01.11.2024 KW - Gold KW - Synchrotron KW - XRF KW - BAMline KW - Bayes PY - 2024 AN - OPUS4-61699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - ChatGPT and EPICS: LLM-Enhanced Control Systems for Synchrotron Beamlines N2 - The BAMlineat BESSY II represents a hard X-ray spectroscopy facility enabling non-destructive analysis across diverse research areas like materials science, chemistry, biology, and cultural heritage studies. As a multipurpose beamline serving users from various disciplines, it underscores the necessity of adaptable and efficient control systems to maximize beamline utilization and scientific output. In this contribution, we detail the innovative integration of ChatGPT, OpenAI’s state-of-the-art Large Language Model (LLM), with the Experimental Physics and Industrial Control System (EPICS) which underpins the operational framework of the BAMline. This integration leverages the advanced natural language processing (NLP) capabilities of ChatGPT, presenting a revolutionary approach to beamline control that markedly simplifies user interaction. Through this, we facilitate a user-friendly pathway to executing complex experimental setups, eliminating the barrier imposed by conventional scripting languages and the often-challenging graphical user interfaces. This innovation promises to significantly streamline experimental workflows, thereby enhancing the efficiency of scientific research conducted at the beamline. Further enhancing this user-centric approach, we introduce an advanced graphical user interface (GUI) application. This novel application seamlessly melds the LLM’s NLP capabilities with EPICS, thereby enabling researchers to articulate experimental requirements through simple textual or voice commands. This interface interprets these commands to manipulate various beamline components, including but not limited to the Double Crystal Monochromator (DCM), Double Multilayer Monochromator (DMM), as well as various filters and slits. By parsing user input, extracting pertinent parameters, and generating a structured JSON object that reflects the desired device positions and experimental settings, the GUI application bridges the gap between complex control commands and intuitive user interactions. This advancement not only lowers the entry threshold for new users but also streamlines the operational workflow for experienced researchers. Looking ahead, we aim to extend the system to cover the entire experimental cycle, from setup to data analysis. Using LLMs, one could translate plain-language experiment descriptions into precise operational commands, revolutionizing the research process and making advanced scientific exploration more accessible to a wider community. T2 - International Conference on Synchrotron Radiation Instrumentation (SRI) CY - Hamburg, Germany DA - 26.08.2024 KW - Chatgpt KW - EPICS KW - BAMline KW - Synchrotron PY - 2024 AN - OPUS4-61700 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Decoding the Elemental Fingerprints of Ancient Gold: A Synchrotron-based Approach N2 - This contribution focuses on the application of synchrotron radiation X-ray fluorescence (SR XRF) for the analysis of ancient gold objects at the BAMline, showcasing several noteworthy examples. One prominent artifact is the Sky Disc of Nebra, which presented a relatively straightforward question to be addressed: Do the gold inlays belong together, and can we glean insights about their origin? In contrast, the analysis of the Bernstorf gold, an alleged Bronze Age treasure composed of exceptionally pure gold, posed a more intricate challenge. The debate surrounding its authenticity prompted an in-depth investigation utilizing SR XRF with different experimental conditions. This approach, involving the analysis of trace elements, played a pivotal role in elucidating the nature and age of the gold, offering valuable insights into its production Platinum emerges as a crucial trace element for gold analysis, given its typically low concentration in gold artifacts, often in the range of a few parts per million (ppm). Accurately measuring Platinum in the presence of overlapping emission lines from gold is arduous. To overcome this challenge, BAMline developed a wavelength dispersive set-up known as D2XRF, employing a pixelated energy-dispersive X-ray detector (pnCCD). This innovative approach enables the resolution of overlapping emission lines, leading to a remarkable detection limit of 1 ppm for Platinum in gold samples. Furthermore, the application of the pnCCD for imaging element distributions on a Phoenician ivory artifact will be showcased. This technique allows for the visualization and mapping of various elements, which opens the possibility to reconstruct the original appearance. The comprehensive analysis of ancient gold artifacts at BAMline has provided valuable insights into the craftsmanship, trade, and technological advancements of ancient civilizations. By unraveling the complex stories these artifacts carry, our studies contributed significantly to the fields of archaeology, history, and materials science. It underscores the importance of interdisciplinary approaches in piecing together the puzzle of human history, revealing the interconnectedness of cultures through the lens of non-destructive analysis. T2 - Denver X-ray Conference 2024 CY - Denver, CO, USA DA - 04.08.2024 KW - Gold KW - Synchrotron KW - XRF KW - BAMline PY - 2024 AN - OPUS4-61701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - ChatGPT and EPICS: LLM-Enhanced Control Systems for Synchrotron Beamlines N2 - The BAMline at BESSY II represents a hard X-ray spectroscopy facility enabling non-destructive analysis across diverse research areas like materials science, chemistry, biology, and cultural heritage studies. As a multipurpose beamline serving users from various disciplines, it underscores the necessity of adaptable and efficient control systems to maximize beamline utilization and scientific output. In this contribution, we detail the innovative integration of ChatGPT , OpenAI’s state-of-the-art Large Language Model (LLM), with the Experimental Physics and Industrial Control System (EPICS) which underpins the operational framework of the BAMline. This integration leverages the advanced natural language processing (NLP) capabilities of ChatGPT, presenting a revolutionary approach to beamline control that markedly simplifies user interaction. Through this, we facilitate a user-friendly pathway to executing complex experimental setups, eliminating the barrier imposed by conventional scripting languages and the often-challenging graphical user interfaces. This innovation promises to significantly streamline experimental workflows, thereby enhancing the efficiency of scientific research conducted at the beamline. Further enhancing this user-centric approach, we introduce an advanced graphical user interface (GUI) application. This novel application seamlessly melds the LLM’s NLP capabilities with EPICS, thereby enabling researchers to articulate experimental requirements through simple textual or voice commands. This interface interprets these commands to manipulate various beamline components, including but not limited to the Double Crystal Monochromator (DCM), Double Multilayer Monochromator (DMM), as well as various filters and slits. By parsing user input, extracting pertinent parameters, and generating a structured JSON object that reflects the desired device positions and experimental settings, the GUI application bridges the gap between complex control commands and intuitive user interactions. This advancement not only lowers the entry threshold for new users but also streamlines the operational workflow for experienced researchers. Looking ahead, we aim to extend the system to cover the entire experimental cycle, from setup to data analysis. Using LLMs, one could translate plain-language experiment descriptions into precise operational commands, revolutionizing the research process and making advanced scientific exploration more accessible to a wider community. T2 - European X-ray Spectrometry Conference CY - Athens, Greece DA - 24.06.2024 KW - EPICS KW - ChatGPT KW - BAMline KW - Synchrotron PY - 2024 AN - OPUS4-61702 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Getting more efficient – The use of Bayesian optimization and Gaussian processes at the BAMline N2 - The BAMline, a beamline for material science research at BESSY II, has been operated by the Bundesanstalt für Materialforschung und -prüfung for over two decades. In the last few years, Bayesian optimization (BO) with Gaussian processes (GP) has been introduced as a transformative method in this setting. This contribution highlights the integration and impact of BO and GP in refining BAMline operations. We will explore the impact of integrating Bayesian methods, especially when combined with Gaussian processes, on the operational efficiency of the BAMline. Our discussion commences with an overview of the fundamental concepts of active learning and optimization. This is followed by an in-depth analysis of specific case studies, drawing on our direct experience with these innovative methods. For this our focus is on three key applications: Alignment of Optical Elements (DCM and DMM): The implementation of Bayesian optimization using Gaussian processes has revolutionized the alignment process for the Double Crystal Monochromator (DCM) and the Double Multilayer Monochromator (DMM). This approach greatly reduced manual effort and enhanced the efficiency and effectiveness of the alignment procedure. Optimal Spot Selection for Spatial Mapping in XRF Studies: In X-ray fluorescence (XRF) experiments, determining the most informative sampling spots is crucial. The introduction of BO, informed by GP, has significantly improved the selection process, especially in large or heterogeneous samples. This methodology ensures maximum information gain, optimizing the balance between comprehensive mapping and resource management. Selection of Optimal Energies for XANES Measurements in GEXANES Geometry: In the specific context of X-ray Absorption Near Edge Structure (XANES) studies using Grazing Exit (GEXANES) geometry, the Bayesian approach with Gaussian processes is now utilized to identify the most effective energy settings. This results in detailed spectral data acquired in a much shorter time. We also address challenges and limitations encountered during implementation. Additionally, the versatility of this approach in addressing a range of different research questions will be demonstrated. T2 - Machine Learning Conference for X-Ray and Neutron-Based Experiments CY - Garching bei München, Germany DA - 08.04.2024 KW - BAMline KW - Synchrotron KW - XRF KW - Bayes PY - 2024 AN - OPUS4-61703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Vergangenheit verifiziert: Datierung und Authentizität mittels Bayes’scher Methoden N2 - In der Archäologie ist die präzise Datierung von Funden und die Verifikation ihrer Authentizität von entscheidender Bedeutung, um Erkenntnisse über vergangene Zivilisationen zu gewinnen. Während traditionelle Methoden wie die Radiokarbon-Datierung bereits seit Jahrzehnten etabliert sind, hat die Anwendung der Bayes’schen Statistik in den letzten Jahren an Bedeutung gewonnen. Dieser Ansatz erlaubt es, vorhandene Unsicherheiten in archäologischen Daten systematisch zu berücksichtigen und bietet somit eine leistungsfähige Ergänzung zu herkömmlichen Methoden. Die Bayes’sche Theorie basiert auf der Aktualisierung von Wahrscheinlichkeiten anhand neuer Daten. Dies ist besonders nützlich in der Archäologie, wo neue Funde oft bestehende Theorien und Annahmen in Frage stellen. Durch die Kombination von Prior-Wissen mit neuen Daten ermöglicht die Bayes'sche Methode eine adaptive und flexible Datierung und Verifizierung. Ein Beispiel für die Anwendung dieser Methode ist die Radiokarbon-Datierung. Während die traditionelle Radiokarbon-Datierung einen geschätzten Zeitraum bietet, kann die Bayes'sche Analyse dazu verwendet werden, die Unsicherheit dieses Zeitraums zu quantifizieren und zu verfeinern. Dies ist besonders wertvoll bei der Datierung von Artefakten aus Zeiträumen, in denen mehrere historische Ereignisse stattfanden. Zudem ist die Bayes'sche Methode auch bei der Überprüfung der Authentizität von Funden nützlich. Durch die Kombination verschiedener Datenquellen, wie z.B. Inschriften, Materialanalysen und Kontextinformationen, können Archäologen die Wahrscheinlichkeit der Echtheit eines Artefakts bestimmen. Trotz ihrer Stärken ist die Anwendung der Bayes’schen Statistik in der Archäologie nicht ohne Herausforderungen. Die Wahl der Prior-Wahrscheinlichkeit kann subjektiv sein und die Methode erfordert eine sorgfältige Überlegung und Expertise. Die Bayes’sche Methode in der Archäologie ein leistungsfähiges Werkzeug, um Datierungen zu verfeinern und die Authentizität von Funden zu überprüfen. Während traditionelle Methoden weiterhin eine zentrale Rolle spielen, ermöglicht der Bayes’sche Ansatz eine nuanciertere und adaptivere Analyse, die das Potential hat, unser Verständnis der Vergangenheit zu vertiefen. T2 - NAHM workshop CY - Bonn, Germany DA - 18.10.2023 KW - Bayes KW - Bernstorf KW - Gold KW - Datierung KW - Herkunft KW - Suchtheorie PY - 2024 AN - OPUS4-61705 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - BAMline@BESSY2 - Advanced Techniques and Applications N2 - Synchrotron radiation sources offer a wide range of possibilities in materials research due to their unique properties in terms of intensity, polarization and adjustability. A basic introduction about the creation and special properties of synchrotron radiation will be given. Examples of current work at BAMline, the high-energy measuring facility of the Federal Institute for Materials Research and Testing at the synchrotron BESSY, are used to illustrate the possibilities and limitations of existing measuring methods.” T2 - GDCH Kolloquium CY - Clausthal-Zellerfeld, Germany DA - 17.11.2022 KW - Synchrotron KW - BAMline KW - XRF KW - XANES PY - 2022 AN - OPUS4-61706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Seena Prem, Pranav T1 - Investigation of Instrumental Isotope Fractionation in ICPMS N2 - Instrumental Isotopic Fractionation (IIF) is the fractionation of isotopes within the mass spectrometer, resulting in a deviation of the measured isotope ratio from the true isotope ratio in a sample. The foremost challenge in obtaining highly precise and accurate absolute isotope ratio measurements lies in implementing adequate corrections for IIF. The causes of IIF are not yet completely understood and differ according to the type of instrument. We are using certified isotope reference materials to investigate the IIF behavior in in different types of ICPMS instruments with different mass separation devices including double focusing sector field (single and multicollector), quadrupole filter and time-of-flight ICPMS. T2 - DAAS PhD Seminar CY - Berlin, Germany DA - 16.11.2023 KW - Isotope ratios KW - Instrumental Isotope Fractionation KW - MCICPMS PY - 2023 AN - OPUS4-61722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Yue A1 - Colnaghi, Timoteo A1 - Gong, Yilun A1 - Zhang, Huaide A1 - Yu, Yuan A1 - Wei, Ye A1 - Gan, Bin A1 - Song, Min A1 - Marek, Andreas A1 - Rampp, Markus A1 - Zhang, Siyuan A1 - Pei, Zongrui A1 - Wuttig, Matthias A1 - Ghosh, Sheuly A1 - Körmann, Fritz A1 - Neugebauer, Jörg A1 - Wang, Zhangwei A1 - Gault, Baptiste T1 - Machine learning‐enabled tomographic imaging of chemical short‐range atomic ordering N2 - In solids, chemical short‐range order (CSRO) refers to the self‐organization of atoms of certain species occupying specific crystal sites. CSRO is increasingly being envisaged as a lever to tailor the mechanical and functional properties of materials. Yet quantitative relationships between properties and the morphology, number density, and atomic configurations of CSRO domains remain elusive. Herein, it is showcased how machine learning‐enhanced atom probe tomography (APT) can mine the near‐atomically resolved APT data and jointly exploit the technique's high elemental sensitivity to provide a 3D quantitative analysis of CSRO in a CoCrNi medium‐entropy alloy. Multiple CSRO configurations are revealed, with their formation supported by state‐of‐the‐art Monte‐Carlo simulations. Quantitative analysis of these CSROs allows establishing relationships between processing parameters and physical properties. The unambiguous characterization of CSRO will help refine strategies for designing advanced materials by manipulating atomic‐scale architectures. KW - Chemical short-range order (CSRO) KW - Atom probe tomography (APT) KW - Machine learning PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623777 DO - https://doi.org/10.1002/adma.202407564 SN - 1521-4095 VL - 36 IS - 44 SP - 1 EP - 9 PB - Wiley-VCH CY - Weinheim AN - OPUS4-62377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arıkan, Muzaffer A1 - Demir, Tuğçe Kahraman A1 - Yıldız, Zeynep A1 - Nalbantoğlu, Özkan Ufuk A1 - Korkmaz, Nur Damla A1 - Yılmaz, Nesrin H. A1 - Şen, Aysu A1 - Özcan, Mutlu A1 - Muth, Thilo A1 - Hanoğlu, Lütfü A1 - Yıldırım, Süleyman T1 - Metaproteogenomic analysis of saliva samples from Parkinson's disease patients with cognitive impairment N2 - Cognitive impairment (CI) is very common in patients with Parkinson’s Disease (PD) and progressively develops on a spectrum from mild cognitive impairment (PD-MCI) to full dementia (PDD). Identification of PD patients at risk of developing cognitive decline, therefore, is unmet need in the clinic to manage the disease. Previous studies reported that oral microbiota of PD patients was altered even at early stages and poor oral hygiene is associated with dementia. However, data from single modalities are often unable to explain complex chronic diseases in the brain and cannot reliably predict the risk of disease progression. Here, we performed integrative metaproteogenomic characterization of salivary microbiota and tested the hypothesis that biological molecules of saliva and saliva microbiota dynamically shift in association with the progression of cognitive decline and harbor discriminatory key signatures across the spectrum of CI in PD. We recruited a cohort of 115 participants in a multi-center study and employed multi-omics factor analysis (MOFA) to integrate amplicon sequencing and metaproteomic analysis to identify signature taxa and proteins in saliva. Our baseline analyses revealed contrasting interplay between the genus Neisseria and Lactobacillus and Ligilactobacillus genera across the spectrum of CI. The group specific signature profiles enabled us to identify bacterial genera and protein groups associated with CI stages in PD. Our study describes compositional dynamics of saliva across the spectrum of CI in PD and paves the way for developing non-invasive biomarker strategies to predict the risk of CI progression in PD. KW - Cognitive impairment (CI) KW - Parkinson’s disease (PD) KW - Metaproteogenomic analysis KW - Saliva sample PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624228 DO - https://doi.org/10.1038/s41522-023-00452-x SN - 2055-5008 VL - 9 IS - 1 SP - 1 EP - 10 PB - Nature Publ. Group CY - London AN - OPUS4-62422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Narayanan, A. A1 - Duddi, M. A1 - Kocherla, Amarteja A1 - Subramaniam, K. V. L. T1 - Continuous monitoring of the early-age strength development of cement paste using embeddable piezoelectric-based ultrasonic transducers N2 - A piezoelectric-based ultrasonic transducer that can be embedded at the time of casting is developed for the purpose of continuously monitoring the early-age strength development of cement paste. The transducers that have been developed are equipped with various levels of protection in order to enhance their resilience in an alkaline environment and mitigate the risk of short-circuits. The transducers are operated in actuator-receiver mode. The obtained ultrasonic signal is analyzed in frequency domain. The initial and final setting time estimated from calorimetry measurements demonstrated a strong agreement with the proposed frequency domain approach. The observed behavior of concrete in wave transmission measurements exhibits similarities to that of an electronic filter. Initially, concrete behaves similar to a low-pass filter, but as time elapses, it transitions into a high-pass filter. T2 - 9th Civil Structural Health Monitoring Workshop (CSHM-9) CY - Kuwait City, Kuwait DA - 12.02.2024 KW - Hydration KW - Embedded sensor KW - Early-age KW - Cementitious KW - PZT KW - Ultrasonic PY - 2024 SN - 978-3-031-62252-6 SN - 978-3-031-62255-7 SN - 978-3-031-62253-3 DO - https://doi.org/10.1007/978-3-031-62253-3_4 SN - 2366-2557 N1 - Serientitel: Lecture notes in civil engineering – Series title: Lecture notes in civil engineering VL - 516 SP - 44 EP - 51 PB - Springer Nature Switzerland CY - Cham AN - OPUS4-62593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Maierhofer, Christiane A1 - Röllig, Mathias A1 - Krankenhagen, Rainer A1 - Myrach, Philipp T1 - Comparison of quantitative defect characterization using pulse-phase and lock-in thermography: Erratum N2 - Based on the results of a study on systematic errors in thermographic lock-in measurements [14th Quantitative Infrared Thermography Conference (2018)], the results and conclusions of the earlier publication [Appl. Opt. 55, D76 (2016)] were reconsidered. It turned out that the reported uncertainties for phase values from lock-in measurements were set too low according to the current state of knowledge. One of the conclusions drawn at the time can no longer be upheld, as the experimental values are too imprecise. PY - 2024 DO - https://doi.org/10.1364/AO.545147 SN - 1559-128X SN - 0003-6935 SN - 1539-4522 VL - 63 IS - 31 SP - 8295 EP - 8296 PB - Optical Society of America (OSA) CY - Washington, DC AN - OPUS4-62549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Danischewski, Julia L. A1 - You, Yi A1 - Bauer, Lauren A1 - Riedel, Jens A1 - Shelley, Jacob T. T1 - Use of Resonant Acoustic Fields as Atmospheric-Pressure Ion Gates N2 - Ion optics are crucial for spectrometric methods such as mass spectrometry (MS) and ion mobility spectrometry (IMS). Among the wide selection of ion optics, temporal ion gates are of particular importance for time-of-flight MS (TOF-MS) and drift-tube IMS. Commonly implemented as electrostatic ion gates, these optics offer a rapid, efficient means to block ion beams and form discrete ion packets for subsequent analysis. Unfortunately, these devices rely on pulsed high voltage sources and are not fully transparent, even in their open state, which can lead to ion losses and contamination. Here, a novel atmospheric-pressure ion gate based on a resonant acoustic field structure is described. This effect was accomplished through the formation of a resonant, standing acoustic wave of alternating nodes and antinodes. Alignment of an atmospheric-pressure gaseous ion beam with an antinode, i.e. a region of transient pressure, of the acoustic structure acted as a gate and blocked ions from impinging on ion-selective detectors, such as a mass spectrometer and a Faraday plate. The velocity of the ion stream and acoustic power were found to be critical parameters for gating efficiency. In the presence of an acoustic field (i.e., a closed gate), ion signals decreased by as much as 99.8% with a response time faster than the readout of the ion-measurement devices used here (ca. 75 ms). This work demonstrates the basis for a low-cost, acoustic ion gate, which is optically transparent and easily constructed with low-power, off-the-shelf components, that could potentially be used with MS and IMS instrumentation. KW - Acoustic Ion Manipulation PY - 2025 DO - https://doi.org/10.1021/acs.analchem.4c05493 SN - 1520-6882 VL - 97 IS - 5 SP - 2890 EP - 2898 PB - American Chemical Society AN - OPUS4-62648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bosc-Bierne, Gaby A1 - Weller, Michael G. T1 - Investigation of impurities in peptide pools T1 - Untersuchung von Verunreinigungen in Peptidpools N2 - Peptide pools are important research tools in different biomedical fields. They consist of a complex mixture of defined peptides, which places high demands on the production and quality control of these products. Previously it has been shown that the combination of UHPLC with high-resolution mass-spectrometry (HRMS) is a fast and powerful method to confirm the relative concentration and the structural identity of all peptides expected to be in the pool. In this work, the additional information contained in the UV chromatograms and mass spectra is used to search for impurities due to synthesis by-products and degradation during storage and transportation and to identify possible analytical artifacts. It was shown that most impurities are only present in trace amounts and can be considered uncritical for most applications. The most frequent and perhaps unexpected impurities were homo- and heterodimers caused by the free cysteines contained in these peptide pools. Furthermore, pyroglutamate and aspartimide formation, deamidation, methionine oxidation, and amino acid deletions could be found. This list is not intended to be comprehensive, but rather a brief guide to quickly identify impurities and, in the long term, to suggest possible changes in the composition of the peptide pools to avoid such impurities by design or by special precautions. N2 - Peptidpools sind wichtige Forschungsinstrumente in verschiedenen biomedizinischen Bereichen. Sie bestehen aus einer komplexen Mischung definierter Peptide, was hohe Anforderungen an die Herstellung und Qualitätskontrolle dieser Produkte stellt. In der Vergangenheit wurde gezeigt, dass die Kombination von UHPLC mit hochauflösender Massenspektrometrie (HRMS) eine schnelle und leistungsfähige Methode zur Bestätigung der relativen Konzentration und der strukturellen Identität aller Peptide ist, die in dem Pool erwartet werden. In dieser Arbeit werden die zusätzlichen Informationen, die in den UV-Chromatogrammen und Massenspektren enthalten sind, genutzt, um nach Verunreinigungen zu suchen, die auf Nebenprodukte der Synthese und den Abbau während der Lagerung und des Transports zurückzuführen sind, und um mögliche analytische Artefakte zu identifizieren. Es hat sich gezeigt, dass die meisten Verunreinigungen nur in Spuren vorhanden sind und für die meisten Anwendungen als unkritisch angesehen werden können. Die häufigsten und vielleicht unerwartetsten Verunreinigungen waren Homo- und Heterodimere, die durch die in diesen Peptidpools enthaltenen freien Cysteine verursacht werden. Außerdem wurden Pyroglutamat- und Aspartimidbildung, Deamidierung, Methioninoxidation und Aminosäuredeletionen festgestellt. Diese Liste erhebt keinen Anspruch auf Vollständigkeit, sondern ist eher ein kurzer Leitfaden, um Verunreinigungen schnell zu identifizieren und langfristig mögliche Änderungen in der Zusammensetzung der Peptidpools vorzuschlagen, um solche Verunreinigungen durch Design oder besondere Vorsichtsmaßnahmen zu vermeiden. KW - Synthetic peptides KW - Degradation KW - Synthetic artifacts KW - Peptide losses KW - Stability of peptides KW - Disulfide dimers KW - Cysteine dimers KW - Isomers KW - Cysteine alkylation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626987 DO - https://doi.org/10.3390/separations12020036 SN - 2297-8739 VL - 12 IS - 2 SP - 1 EP - 18 PB - MDPI AG CY - Basel AN - OPUS4-62698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hauschildt, Charlotte T1 - New Approaches to PFAS Quali- and Quantification using GC-MS N2 - Known as “forever chemicals”, per- and polyfluoroalkyl substances (PFAS) are a class of synthetically produced chemicals that includes an estimated 10.000 compounds. Due to the persistence, toxicity and ubiquitous occurrence, research has focused on the qualification and quantification of the most important compounds as well as on the investigation of toxicity and possible routes of entry over the last 10 years. Liquid chromatography - mass spectrometry (LC-MS) is the analytical standard to test for PFAS, as the spectrum of detectable compounds is significantly more comprehensive than it is currently the case with gas chromatography - mass spectrometry (GC-MS). However, to be able to test for PFAS contamination in a more process-independent manner and to make the analysis more widely accessible, methods based on GC-MS are currently being developed. Since GC-MS methods only cover a fraction of the compounds belonging to the PFAS group so far, further development of the corresponding measurement methods is inevitable [1, 2]. The here described work is part of the EU project 23IND13 ScreenFood [3]. The aim is to develop sensitive analytical GC-MS methods that contribute to an improved identification and quantification of various PFAS (both currently regulated and emerging PFAS) in selected food and food packaging matrices. Of particular interest as a food contact material are native and recycled polymers such as PET. Besides, various techniques, including solvent-free variants such as thermal desorption GC-MS, will be tested for a quick and easy analysis. Multiple derivatization approaches, which cover different PFAS subgroups, will also be tested and evaluated. This poster will present the overall project objectives and first results. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Per- and Polyfluoroalkyl Substances (PFAS) KW - Gas chromatography - mass spectrometry (GC-MS) KW - EU Project KW - Derivatization methods PY - 2025 AN - OPUS4-62709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Vogel, Christian A1 - Slee, D. ED - Naidu, R. T1 - Chapter 5 Analytical techniques for Per- and Polyfluoroalkyl substances (PFAS) N2 - Per- and polyfluoroalkyl substances (PFAS) are a group of various anthropogenic organic products, in which the hydrogen atoms on the carbon skeleton of at least one carbon atom have been completely replaced by fluorine atoms. Because this group contains more than 7 million compounds, they can have very different properties. PFAS analysis in environmental samples is currently mainly utilized by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and related techniques as well as gas chromatography-mass spectrometry (GC-MS) to conduct target analysis. However, to get a better overview of the amount of “total” amount of PFAS, sum parameter methods like total oxidizable precursor assay (TOPA), absorbable organic fluorine (AOF), and extractable organic fluorine (EOF) are in development. Additionally, for research purposes, several spectroscopical methods like X-ray photoelectron spectroscopy (XPS), fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy, particular induced gamma-ray emission (PIGE) spectroscopy as well as19 F nuclear magnetic resonance (NMR), infrared, and Raman spectroscopy are available. Therefore, an overview is given on currently available analytical techniques for PFAS in environmental samples and their application possibilities discussed for different kinds of PFAS subgroups. KW - Per- and polyfluoroalkyl substances (PFAS) KW - Analytics KW - Liquid chromatography - mass spectrometry (GC-MS) KW - Sum parameter PY - 2025 DO - https://doi.org/10.1515/9783110796797-005 SP - 143 EP - 168 PB - De Gruyter AN - OPUS4-62662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Duddi, M. A1 - Kocherla, Amarteja A1 - Subramaniam, K. V. L. T1 - Real-time monitoring of concrete properties using an embedded smart piezoelectric sensor with active and passive sensing abilities N2 - Concrete undergoes physical and chemical changes from the time of casting. These changes in early stage of hydration of concrete, highly influence the final properties and overall performance of concrete structures. Comprehensive health monitoring sensors can help to improve the quality and performance of concrete structures by providing detailed and accurate real-time information about the properties and condition of concrete at different stages of its life cycle. In this study, an embedded smart PZT (Lead Zirconate and Titanium) sensor is developed and its potential for comprehensive health monitoring of concrete structures is explored. To protect the PZT sensor from short-circuiting and alkaline environment, a robust and sensitive protection scheme is developed. The developed embedded smart PZT sensor was placed in the concrete during casting to infer the in-situ properties of concrete through active and passive sensing techniques. Through active sensing techniques Electrical Impedance (EI) and wave propagation (WP), the hydration and damage are monitored, respectively; through passive sensing techniques vibration, and acoustic emission (AE), the development of Young’s modulus and cracking in concrete are monitored. The methodology to infer the changes inworkability, complete set behavior, property development, and crack opening in concrete structures is developed. The reproducibility of all these techniques using the developed embedded smart PZT sensor is established. Since the developed sensor is capable of both active and passive sensing, it allows for a more comprehensive and flexible approach to health monitoring. This contributes to increased data accuracy, reliability, and a more holistic understanding of the concrete structure’s condition. T2 - 1st Interdisciplinary Symposium on Smart & Sustainable Infrastructure (ISSSI 2023) CY - Vancouver, BC, Canada DA - 04.09.2023 KW - Embedded smart PZT sensor KW - Electrical impedance (EI) KW - Wave propagation (WP) KW - Acoustic emission (AE) KW - Vibration monitoring KW - Hydration KW - Damage PY - 2024 SN - 978-3-031-53388-4 SN - 978-3-031-53389-1 SN - 978-3-031-53391-4 DO - https://doi.org/10.1007/978-3-031-53389-1_96 SN - 2211-0844 N1 - Serientitel: RILEM bookseries – Series title: RILEM bookseries VL - 48 SP - 1089 EP - 1100 PB - Springer Nature CY - Cham AN - OPUS4-62681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Mensing, Friedrich A1 - Kruschwitz, Sabine T1 - Estimation of cement content in concrete by spatially resolved laser induced breakdown spectroscopy N2 - The cement content in concrete significantly influences critical properties such as durability, permeability, strength, and workability. Traditional methods for estimating the cement content face limitations. These include the need for comprehensive chemical and solubility knowledge, extensive sample preparation, and their time-consuming and destructive nature. This study investigates the application of laser-induced breakdown spectroscopy (LIBS) as an alternative method. It involves probing concrete samples with high spatial resolution and analyzing the resultant spectra. The methodology is first tested on mesoscale concrete models to assess limitations and inherent errors. Subsequently, the methodology is applied to actual concrete samples with varying cement content and aggregate size distributions. The results demonstrate a promising accuracy, with an average relative error of approximately 8%. This paper offers a comprehensive evaluation of the method's advantages, limitations, and factors influencing its practical applicability in field conditions. KW - LIBS KW - Spectroscopy KW - Cement content KW - Elemental mapping PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-620112 DO - https://doi.org/10.1016/j.cemconres.2024.107714 SN - 1873-3948 VL - 189 SP - 1 EP - 10 PB - Elsevier Ltd. AN - OPUS4-62011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blume, Simon T1 - Isotopic analysis of lithium via acousto-optically gated high-repetition laser-induced breakdown spectroscopy and spatial heterodyne spectroscopy N2 - Acousto-optically gating the emission signal from a laser-induced breakdown spectroscopy (LIBS) plasma negates some of the line-broadening effects, therefore, improving the signal line shape. However, the remaining influences disallow the differentiation of the contributions of the individual lithium isotopes, even when utilizing a high-resolution spatial heterodyne spectrometer (SHS). Nevertheless, isotopic analysis of lithium with LIBS is still feasible, because lithium exhibits a strong self-absorption dip in the emission signal, which is likewise characterized by the isotopic shift and even benefits from the broad emission lines typically observed in LIBS. The isotopic ration can be resolved from the absorption dip via high-resolution SHS. T2 - SciX 2024 CY - Raleigh, NC, USA DA - 20.10.2024 KW - LIBS KW - SHS KW - Isotopic analysis KW - Lithium PY - 2024 AN - OPUS4-62012 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - ChatGPT and EPICS: LLM-Enhanced Control Systems for Synchrotron Beamlines N2 - The document highlights ChatGPT-EPICS integration for synchrotron beamline automation, employing tools like motor records, PV naming systems, and LLM inference. It evaluates efficiency and challenges in implementing automated motor optimization and handling EPICS controls. T2 - BESSY science seminar CY - Online meeting DA - 22.11.2024 KW - Chatgpt KW - EPICS KW - BAMline PY - 2024 AN - OPUS4-61896 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zöllner, Moritz T1 - Thermal decomposition of dolomite: Raman spectroscopy as a thermometric tool for the analysis of carbonates in mortar binders. N2 - The reconstruction of the thermal history of minerals is an on-going challenge in the study of anthropogenic materials, e.g., ceramics and mortar binders. For millennia carbonate rocks have been used as the starting material, though the exact manufacturing procedures are often unknown. Preparatory parameters such as firing temperature, heating and cooling rates, soaking time, and kiln atmosphere greatly influence the chemical and structural properties of the resulting products. Analysis of replicas produced under well-defined laboratory conditions help identify indicators for such process parameters and therefore provide valuable insights into historical production workflows. Raman micro-spectroscopy is a valuable method here because of its high sensitivity for crystal-chemical alterations coupled with a high spatial resolution. Previous studies on pyrogenic anhydrite were able to distinguish between gypsum materials that were heated at different temperatures between 400 – 900 °C [1, 2]. The results of thermal experiments with natural dolomite powder between 500 – 900 °C are presented, evaluating the thermal decomposition of dolomite and the consequent formation of calcium carbonate. Raman measurements were performed at room temperature on calcinated samples, as well as subsequently hydrated and re-carbonated samples. A peak-fitting routine using python scripts was employed to extract the peak positions and the full width at half maximum (FWHM) values of the ν1-, ν4- and L-bands of the carbonates. The results reveal the formation of Mg-calcite from dolomite at 700 – 750 °C and the formation of Mg-free calcite after calcination above 750 °C and subsequent hydration and re-carbonation. The findings from the thermal experiments are compared with Raman-microscopy mappings on medieval and reenacted mortars containing dolomite. Mg-calcite with comparable peak position and FWHM values have been successfully identified, proving Raman spectroscopy to be a suitable tool for elucidating the manufacturing procedures of anthropogenic materials. T2 - European Mineralogical Conference 2024 CY - Dublin, Ireland DA - 18.08.2024 KW - Raman spectroscopy KW - Dolomite KW - Mineral thermometry PY - 2024 AN - OPUS4-61975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zöllner, Moritz T1 - Thermal decomposition of dolomite: Raman spectroscopy as a thermometric tool for the analysis of carbonates in mortar binders. N2 - High-spectral resolution Raman spectroscopy is a powerful tool for the chemical and structural analysis in material sciences. Beyond its usage for the qualitative identification of minerals, Raman spectroscopy has been applied for the quantitative characterisation of chemical phases. The precise measurement of Raman peak position and band width values allows for an empirical differentiation of chemically similar phases and thus provides valuable insights to the structural properties of a material. In the field of archaeometry, the crystal structure of minerals can be used to elucidate the preparatory parameters of historical samples, such as the firing temperature. Comparison of historical materials with replicas produced under well-defined laboratory conditions help identify indicators for such process parameters. Previous Raman studies on pyrogenic anhydrite were able to distinguish between gypsum materials that were heated at different temperatures between 400–900 °C [1–3]. The results of thermal experiments with natural dolomite powder between 500–900 °C are presented, evaluating the thermal decomposition of dolomite and the consequent formation of calcium carbonate. Raman measurements were performed with excitation at 532 nm and 1800 mm-1 grating at room temperature on calcinated samples, as well as subsequently hydrated and re-carbonated samples. These high-resolution conditions are necessary to resolve the individual spectral contributions of different calcium/magnesium carbonate species. However, this sensitivity does not come without potential pitfalls. While the usage of micro-Raman spectroscopy with high spectral resolution shows great promise for evaluating minor shifts in peak positions and band widths, several technical aspects must be considered. For example, great care must be taken to exclude the thermal impact of the highly focused Raman laser on the sample. Similarly, exact standard operating procedures have to be followed to circumvent mechanical hysteresis in the alignment of the spectrographs’ grating. The influence of these two effects is presented and effective countermeasures are introduced to avoid resulting systematic errors. Statistical reliability and chemical imaging both rely on the individual analysis of thousands of Raman spectra. Thus, besides the spectral acquisition, also highly automated data analysis must be applied. Therefore, a peak-fitting routine using python scripts was employed to extract the peak positions and the full width at half maximum (FWHM) values of the ν1-, ν4- and L-bands of the carbonates. The results reveal the formation of Mg-calcite from dolomite at 700–750 °C and the formation of Mg-free calcite after calcination above 750 °C and subsequent hydration and re-carbonation (Fig. 1a). The findings from the thermal experiments are compared with Raman-microscopy mappings on medieval and reenacted mortars containing dolomite. Mg-calcite with comparable peak position and FWHM values have been successfully identified (Fig. 1b), proving Raman spectroscopy to be a suitable tool for elucidating the manufacturing procedures of anthropogenic materials. T2 - 16th GeoRAMAN Conference CY - Rhodes, Greece DA - 24.09.2024 KW - Raman spectroscopy KW - Dolomite KW - Mineral thermometry PY - 2024 AN - OPUS4-61977 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zöllner, Moritz T1 - Thermal decomposition of dolomite: Raman spectroscopy as a thermometric tool for the analysis of carbonates in mortar binders N2 - The reconstruction of the thermal history of minerals is an on-going challenge in the study of anthropogenic materials, e.g., ceramics and mortar binders. For millennia carbonate rocks have been used as the starting material, though the exact manufacturing procedures are often unknown. Preparatory parameters such as firing temperature, heating and cooling rates, soaking time, and kiln atmosphere greatly influence the chemical and structural properties of the resulting products. Analysis of replicas produced under well-defined laboratory conditions help identify indicators for such process parameters and therefore provide valuable insights into historical production workflows. Raman micro-spectroscopy is a valuable method here because of its high sensitivity for crystal-chemical alterations coupled with a high spatial resolution. Previous studies on pyrogenic anhydrite were able to distinguish between gypsum materials that were heated at different temperatures between 400–900 °C [1-3]. The results of thermal experiments with natural dolomite powder between 500–900 °C are presented, evaluating the thermal decomposition of dolomite and the consequent formation of calcium carbonate. Raman measurements were performed at room temperature on calcinated samples, as well as subsequently hydrated and re-carbonated samples. Raman band positions and the full width at half maximum (FWHM) values of the ν1-, ν4- and L-bands of the carbonates are extracted and reveal the formation of Mg-calcite from dolomite at 700–750 °C and the formation of Mg-free calcite after calcination above 750 °C and subsequent hydration and re-carbonation. The findings from the thermal experiments are compared with Raman-microscopy mappings on medieval and reenacted mortars containing dolomite. Mg-calcite with comparable peak position and FWHM values have been successfully identified, proving Raman spectroscopy to be a suitable tool for elucidating the manufacturing procedures of anthropogenic materials. T2 - SciX 2024 CY - Raleigh, NC, USA DA - 20.10.2024 KW - Raman spectroscopy KW - Dolomite KW - Mineral thermometry PY - 2024 AN - OPUS4-61978 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufgard, Josefin T1 - Use Your Time (Domain) Wisely: Streamlined Analysis of Complex Mixtures with Pulsed-Laser Techniques N2 - This study aims to streamline complex mixture analysis through the parallel ionization of all analytes without extensive preprocessing. Here, pulsed laser ablation of single droplets is used with modified cross-correlation, a phase-sensitive algorithm. This combined method allows contactless chemical investigation with minimal sample pretreatment, as well as the separation of analytes in mixtures and reconstruction of analyte-specific mass spectra. T2 - SciX 2024 CY - Raleigh, NC, USA DA - 20.10.2024 KW - MS KW - Data analysis KW - Laser ablation PY - 2024 AN - OPUS4-62120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufgard, Josefin T1 - Use Your Time (Domain) Wisely: Streamlined Analysis of Complex Mixtures with Pulsed-Laser Techniques N2 - This study aims to streamline complex mixture analysis through the parallel ionization of all analytes without extensive preprocessing. Here, pulsed laser ablation of single droplets is used with modified cross-correlation, a phase-sensitive algorithm. This combined method allows contactless chemical investigation with minimal sample pretreatment, as well as the separation of analytes in mixtures and reconstruction of analyte-specific mass spectra. T2 - Future WINS: Corss-sections and interfaces in science, careers, and communication CY - Berlin, Germany DA - 21.11.2024 KW - MS KW - Data analysis KW - Laser ablation PY - 2024 AN - OPUS4-62124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weller, Michael G. T1 - Challenges of protein analysis N2 - Selected Projects BAM Division 1.5 Test for sensitive SARS-CoV-2 detection Corundum as a novel affinity support Troponin biosensor based on chemiluminescence Plant virus purification (CCMV) Protein Quantification by 1H-NMR Ultra-miniaturized Biosensors N2 - Ausgewählte Projekte BAM-Abteilung 1.5 Test für empfindlichen SARS-CoV-2-Nachweis Korund als neuartige Affinitätscarriermaterialien Troponin-Biosensor auf Basis von Chemilumineszenz Reinigung von Pflanzenviren (CCMV) Proteinquantifizierung durch 1H-NMR Ultra-miniaturisierte Biosensoren T2 - Klausurtagung der MPI Abteilung „Multiphasenchemie“ CY - Mainz, Germany DA - 19.11.2024 KW - Corona test KW - Corundum KW - Affinity separation KW - Affinity chromatography KW - Troponin biosensor KW - Peptide aptamer KW - Cowpea chlorotic mottle virus KW - Nanoparticle KW - Nanocarrier KW - Nuclear magnetic resonance NMR KW - Protein quantification KW - HyPhox KW - Ring resonator PY - 2024 AN - OPUS4-62126 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Bosc-Bierne, Gaby A1 - Weller, Michael G. T1 - Investigation of Impurities in Peptide Pools N2 - Peptide pools are important research tools in different biomedical fields. They consist of a complex mixture of defined peptides, which places high demands on the production and quality control of these products. Previously it was shown that the combination of UHPLC with high-resolution mass-spectrometry (HRMS) is a fast and powerful method to confirm the relative concentration and the structural identity of all peptides expected to be in the pool. In this work, the additional information contained in the UV chromatograms and mass spectra is used to search for impurities due to synthesis by-products, degradation during storage and transportation and to identify possible analytical artifacts. It was shown that most impurities are only present in trace amounts and can be considered uncritical for most applications. The most frequent and perhaps unexpected impurities were homo- and heterodimers caused by the free cysteines contained in these peptide pools. Furthermore, pyroglutamate and aspartimide formation, deamidation, methionine oxidation, and amino acid deletions could be found. This list is not intended to be comprehensive, but rather a brief guide to quickly identify impurities and, in the long term, to suggest possible changes in the composition of the peptide pools to avoid such impurities by design or by special precautions. N2 - Peptidpools sind wichtige Forschungswerkzeuge in verschiedenen biomedizinischen Bereichen. Sie bestehen aus einer komplexen Mischung definierter Peptide, was hohe Anforderungen an die Produktion und Qualitätskontrolle dieser Produkte stellt. Zuvor wurde gezeigt, dass die Kombination von UHPLC mit hochauflösender Massenspektrometrie (HRMS) eine schnelle und leistungsstarke Methode ist, um die relative Konzentration und die strukturelle Identität aller Peptide zu bestätigen, die im Pool erwartet werden. In dieser Arbeit werden die zusätzlichen Informationen in den UV-Chromatogrammen und Massenspektren genutzt, um nach Verunreinigungen durch Synthesenebenprodukte, Abbau während der Lagerung und des Transports zu suchen und mögliche analytische Artefakte zu identifizieren. Es wurde gezeigt, dass die meisten Verunreinigungen nur in Spuren vorhanden sind und für die meisten Anwendungen als unkritisch angesehen werden können. Die häufigsten und vielleicht unerwartetsten Verunreinigungen waren Homo- und Heterodimere, die durch die in diesen Peptidpools enthaltenen freien Cysteine verursacht wurden. Außerdem konnten Pyroglutamat- und Aspartimidbildung, Deamidierung, Methioninoxidation und Aminosäurendeletion festgestellt werden. Diese Liste erhebt keinen Anspruch auf Vollständigkeit, sondern soll vielmehr eine kurze Anleitung zur schnellen Identifizierung von Verunreinigungen und langfristig zur Anregung möglicher Änderungen in der Zusammensetzung der Peptidpools sein, um solche Verunreinigungen durch Design oder besondere Vorsichtsmaßnahmen zu vermeiden. KW - Peptides KW - Mixtures KW - Degradation KW - Rearrangement KW - Cystein-Dimers KW - Immunology KW - MHC PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621270 DO - https://doi.org/10.20944/preprints202412.0832.v1 SP - 1 EP - 16 PB - MDPI CY - Basle, Switzerland AN - OPUS4-62127 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Fischer, Janina A1 - Kaufmann, Jan Ole A1 - Weller, Michael G. T1 - Simple Determination of Affinity Constants of Antibodies by Competitive Immunoassays N2 - The affinity constant, also known as the equilibrium constant, binding constant, equilibrium association constant, or the reciprocal value, the equilibrium dissociation constant (Kd), can be considered as one of the most important characteristics for any antibody-antigen pair. Many methods based on different technologies have been proposed and used to determine this value. However, since a very large number of publications and commercial datasheets do not include this nformation, significant obstacles in performing such measurements seem to exist. In other cases where such data are reported, the results have often proved to be unreliable. This situation may indicate that most of the technologies available today require a high level of expertise that does not seem to be available in many laboratories. In this paper, we present a simple approach based on standard immunoassay technology that is easy and quick to perform. It relies on the effect that the molar IC50 approaches the Kd value in the case of infinitely small concentrations of the reagent concentrations. A two-dimensional dilution of the reagents leads to an asymptotic convergence to Kd. The approach has some similarity to the well-known checkerboard titration used for the optimization of immunoassays. A well-known antibody against the FLAG peptide, clone M2, was used as a model system and the results were compared with other methods. This approach could be used in any case where a competitive assay is available or can be developed. The determination of an affinity constant should belong to the crucial parameters in any quality control of antibody-related products and assays and should be mandatory in papers using immunochemical protocols. N2 - Die Affinitätskonstante, auch bekannt als Gleichgewichtskonstante, Bindungskonstante, Gleichgewichtsassoziationskonstante oder der Kehrwert, die Gleichgewichtsdissoziationskonstante (Kd), kann als eine der wichtigsten Eigenschaften für jedes Antikörper-Antigen-Paar angesehen werden. Es wurden viele Methoden auf der Grundlage verschiedener Technologien vorgeschlagen und verwendet, um diesen Wert zu bestimmen. Da jedoch eine sehr große Anzahl von Veröffentlichungen und kommerziellen Datenblättern diese Informationen nicht enthalten, scheint es erhebliche Hindernisse bei der Durchführung solcher Messungen zu geben. In anderen Fällen, in denen solche Daten angegeben werden, haben sich die Ergebnisse oft als unzuverlässig erwiesen. Diese Situation könnte darauf hindeuten, dass die meisten der heute verfügbaren Technologien ein hohes Maß an Fachwissen erfordern, das in vielen Laboren nicht vorhanden zu sein scheint. In diesem Artikel stellen wir einen einfachen Ansatz vor, der auf der Standard-Immunoassay-Technologie basiert und einfach und schnell durchzuführen ist. Er beruht auf dem Effekt, dass sich der molare IC50-Wert dem Kd-Wert im Fall unendlich kleiner Konzentrationen der Reagenzienkonzentrationen nähert. Eine zweidimensionale Verdünnung der Reagenzien führt zu einer asymptotischen Konvergenz zu Kd. Der Ansatz weist eine gewisse Ähnlichkeit mit der bekannten Schachbrett-Titration auf, die zur Optimierung von Immunoassays verwendet wird. Ein bekannter Antikörper gegen das FLAG-Peptid, Klon M2, wurde als Modellsystem verwendet und die Ergebnisse wurden mit anderen Methoden verglichen. Dieser Ansatz kann in allen Fällen verwendet werden, in denen ein kompetitiver Test verfügbar ist oder entwickelt werden kann. Die Bestimmung einer Affinitätskonstante sollte zu den entscheidenden Parametern in jeder Qualitätskontrolle von Antikörper-bezogenen Produkten und Tests gehören und in Veröffentlichungen, die immunchemische Protokolle verwenden, obligatorisch sein. KW - ELISA KW - Microplate KW - Microtiter plate KW - IC50 KW - Test midpoint KW - Competitive immunoassay KW - Law of mass action KW - Thermodynamics KW - Equilibrium constant KW - SPR KW - Surface plasmon resonance KW - Clones KW - Interaction KW - kd value KW - ITC KW - MST PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621298 DO - https://doi.org/10.20944/preprints202404.0996.v1 SP - 1 EP - 11 PB - MDPI CY - Basle, Switzerland AN - OPUS4-62129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Bosc-Bierne, Gaby A1 - Ewald, Shireen A1 - Kreuzer, Oliver J. A1 - Weller, Michael G. T1 - Efficient Quality Control of Peptide Pools N2 - Peptide pools composed of short amino acid sequences have proven to be versatile tools in various research areas and clinical applications. They are powerful tools for epitope mapping, immunotherapy, and vaccine development. Their importance lies in their ability to map complex protein structures, enabling a comprehensive understanding of immune responses and facilitating the identification of potential therapeutic agents. The application of peptide pools also extends to the field of personalized medicine, offering tailored solutions for diseases such as cancer and infectious diseases. Peptide pools are complex mixtures of immunostimulatory antigens primarily intended for T-cell stimulation. They are commercially available in many different compositions and variants. However, unlike other reagents that consist of only one or a few compounds, peptide pools are highly complex products with limited stability. This makes their quality control a major challenge. Quantitative peptide analysis usually requires sophisticated methods, in most cases isotope-labeled standards and reference materials. None of these are routinely available for these products. Synthesis and purification of all labeled peptides might be required. Usually, this approach would be prohibitively laborious and expensive. Therefore, an approach is needed to provide a practical and feasible method for quality control of peptide pools. With insufficient quality control, the use of such products could lead to incorrect experimental results, which would worsen the well-known reproducibility crisis in the biomedical sciences. Here we propose the use of ultra-high performance liquid chromatography (UHPLC) with two detectors, a standard UV detector (at 214 nm) for quantitative analysis and a high-resolution mass spectrometer (HRMS) for identity confirmation. To be cost-efficient and fast, quantification and identification are performed in one chromatographic run. An optimized protocol is shown, and different peak integration methods are compared and discussed. This work was performed using a peptide pool known as CEF, which consists of 32 peptides derived from cytomegalovirus (CMV), Epstein-Barr virus (EBV) and influenza virus, ranging from 8 to 12 amino acids in length. N2 - Peptidpools, die aus kurzen Aminosäuresequenzen bestehen, haben sich in verschiedenen Forschungsbereichen und klinischen Anwendungen als vielseitige Werkzeuge erwiesen. Sie sind leistungsstarke Werkzeuge für die Epitopkartierung, die Immuntherapie und die Impfstoffentwicklung. Ihre Bedeutung liegt in ihrer Fähigkeit, komplexe Proteinstrukturen zu kartieren, was ein umfassendes Verständnis der Immunantworten ermöglicht und die Identifizierung potenzieller Therapeutika erleichtert. Die Anwendung von Peptidpools erstreckt sich auch auf den Bereich der personalisierten Medizin und bietet maßgeschneiderte Lösungen für Krankheiten wie Krebs und Infektionskrankheiten. Peptidpools sind komplexe Mischungen immunstimulierender Antigene, die hauptsächlich zur T-Zell-Stimulation bestimmt sind. Sie sind in vielen verschiedenen Zusammensetzungen und Varianten im Handel erhältlich. Im Gegensatz zu anderen Reagenzien, die nur aus einer oder wenigen Verbindungen bestehen, sind Peptidpools jedoch hochkomplexe Produkte mit begrenzter Stabilität. Dies macht ihre Qualitätskontrolle zu einer großen Herausforderung. Die quantitative Peptidanalyse erfordert in der Regel ausgefeilte Methoden, in den meisten Fällen isotopenmarkierte Standards und Referenzmaterialien. Keines dieser Verfahren ist für diese Produkte routinemäßig verfügbar. Möglicherweise ist die Synthese und Reinigung aller markierten Peptide erforderlich. In der Regel wäre dieser Ansatz unerschwinglich aufwendig und teuer. Daher ist ein Ansatz erforderlich, der eine praktische und praktikable Methode für die Qualitätskontrolle von Peptidpools bietet. Bei unzureichender Qualitätskontrolle könnte die Verwendung solcher Produkte zu falschen Versuchsergebnissen führen, was die bekannte Reproduzierbarkeitskrise in den biomedizinischen Wissenschaften verschlimmern würde. Hier schlagen wir die Verwendung der Ultrahochleistungsflüssigkeitschromatographie (UHPLC) mit zwei Detektoren vor, einem Standard-UV-Detektor (bei 214 nm) für die quantitative Analyse und einem hochauflösenden Massenspektrometer (HRMS) für die Identitätsbestätigung. Um kosteneffizient und schnell zu sein, werden Quantifizierung und Identifizierung in einem chromatographischen Durchlauf durchgeführt. Es wird ein optimiertes Protokoll vorgestellt und verschiedene Peak-Integrationsmethoden werden verglichen und diskutiert. Diese Arbeit wurde mit einem Peptidpool namens CEF durchgeführt, der aus 32 Peptiden besteht, die vom Cytomegalovirus (CMV), Epstein-Barr-Virus (EBV) und Influenzavirus stammen und zwischen 8 und 12 Aminosäuren lang sind. KW - Quality control KW - UHPLC-UV-HRMS KW - Relative peptide quantification KW - Compound confirmation KW - Structure confirmation KW - Cost efficiency KW - Infectious diseases KW - Orbitrap PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621307 DO - https://doi.org/10.20944/preprints202404.0992.v1 SP - 1 EP - 18 PB - MDPI CY - Basle, Switzerland AN - OPUS4-62130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Yi T1 - Advanced Repetition-Rate Modulation and Computational Strategies for Background-Free LIBS Using Non-Gated Spectrometers N2 - Laser-induced breakdown spectroscopy (LIBS) is recognized for its rapid, direct elemental analysis capabilities. However, its general adoption is constrained by the reliance on expensive, high-power consumption, gated cameras such as intensified charge-coupled devices (CCDs). These devices, while sensitive, are expensive and possess low frame rates, limiting their efficacy in dynamic or challenging environments. Our study proposes an innovative approach that leverages non-gated spectrometers in conjunction with the framework of correlation spectroscopy to isolate analyte signals responsive to a specific repetition-rate modulation pattern, thereby yielding spectra with zero background. We utilized a diode-pumped solid-state laser, with repetition rates ranging from 10 Hz to 30 kHz, to induce plasma in aqueous solutions containing various alkaline and earth-alkaline metals. With a non-gated single-grating linear CCD spectrometer, we found that the continuum signal plateaued at approximately 7 kHz. In contrast, atomic emissions from the dissolved analytes showed continued increases. Notably, atomic emissions from the solvent (water) were observable only above 8.5 kHz, at a significant high rate of increase. Through computational synthesis of a modulation pattern, we determined an optimized scheme that effectively discriminates continuum and analyte signals; this pattern was optimized with a genetic algorithm. The spectral matrix correlating signal intensity with laser repetition rate and wavelength was used as the input of the model. Meanwhile, the fitness function that extracts the background-free spectra was built in-house and inspired by the Gardner transform, which exploits the power of Fourier transform, allowing for flagging and splitting analyte signal from other undesired features. This approach bypasses the limitations associated with gated cameras, while providing a cost-effective alternative for robust LIBS applications. This advancement is particularly relevant in field, portable and remote applications, aligning with the ongoing demand for accessible, high-performance analytical tools in diverse scientific fields. T2 - SCIX 2024 Conference CY - Raleigh, NC, USA DA - 20.10.2024 KW - LIBS KW - Data Processing KW - High Repetition Rate KW - Repetition Rate Modulation KW - Data-Oriented Experimental Design PY - 2024 AN - OPUS4-62137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Li, Xunyu T1 - Atomic Isotope Analysis of Lithium with Spatial Heterodyne Spectrometry and Lineshape Recovery through Deconvolution N2 - A spatial heterodyne spectrometer (SHS) was combined with a reduced-pressure glow discharge to demonstrate the analytical utilization of high resolving-power spectral analysis for atomic isotopes. In the experimental illustrations, we will demonstrate the spectra for the lithium isotope ratio through the D-lines featuring 6Li and 7Li. The SHS utilized in our setup boasts single-digit picometer resolution, enabling the precise discrimination of three separate spectral bands in real-time. To further enhance the spectral quality and improve quantification accuracy, we established an innovative approach to recover the natural lineshape, avoiding interferences from the instrumental function that broadens fine features. By understanding the inherent characteristics of an SHS interferogram and leveraging computational capabilities, we will demonstrate the direct extraction of the numerical presentation of the instrumental function from an SHS interferogram; this instrumental function was used for spectral data processing that enables significant improvements in spectral resolution through deconvolution algorithms. The resulting high-quality spectra enabled precise quantitative determination of lithium concentrations and isotope ratios. We aim to showcase the procedures involved in fine-tuning an SHS platform, along with software design strategy to track real-time spectral variations. Meanwhile, the concept of the lineshape recovery through deconvolution will also be discussed. Furthermore, atomic lithium spectra featuring various isotope compositions will be presented to highlight the potential of SHS in real-life applications. T2 - SCIX 2024 Conference CY - Raleigh, NC, USA DA - 20.10.2024 KW - Spatial Heterodyne Spectrometry KW - High-Resolution Spectrometry KW - Isotopic Analysis KW - Line Shape Recovery KW - Instrumental Function PY - 2024 AN - OPUS4-62138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saeidfirozeh, H. A1 - Kubelík, P. A1 - Laitl, V. A1 - Krivkova, A. A1 - Vrabel, J. A1 - Rammelkamp, K. A1 - Schroder, S. A1 - Gornushkin, Igor B. A1 - Kepes, E. A1 - Zabka, J. A1 - Ferus, M. A1 - Porízka, P. A1 - Kaiser, J. T1 - Laser-induced breakdown spectroscopy in space applications: Review and prospects N2 - This review describes the principles and summarizes the challenges of analytical methods based on optical emission spectroscopy (OES) in space applications, with a particular focus on Laser-Induced Breakdown Spectroscopy (LIBS). Over the past decade, LIBS has emerged as a powerful analytical technique for space exploration and In-Situ Resource Utilization (ISRU) of celestial bodies. Its implementation has been suggested for various segments of the Space Resources Value Chain, including prospecting, mining, and beneficiation. Current missions to Mars, including the ChemCam instrument on the Curiosity rover, the SuperCam on the Perseverance rover, and the MarSCoDe on the Zhurong rover, are considered flagship applications of LIBS. Despite neither the Pragyan rover nor the Vikram lander waking from the lunar night, the success of the Chandrayaan-3 mission marks another milestone in the development of LIBS instruments, with further missions, including commercial ones, anticipated. This paper reviews the deployment of LIBS payloads on Mars rovers, upcoming missions prospecting the Moon and asteroids, and LIBS analysis of meteorites. Additionally, it highlights the importance of data processing specific to space applications, emphasizing recent trends in transfer learning. Furthermore, LIBS combined with other spectroscopic techniques (e.g., Raman Spectroscopy, Mass Spectrometry, and Fourier-Transform Infrared Spectroscopy) represents an intriguing platform with comprehensive analytical capabilities. The review concludes by emphasizing the significance of LIBS-based contributions in advancing our understanding of celestial bodies and paving the way for future space exploration endeavors KW - Laser-induced breakdown spectroscopy KW - Mars KW - Moon KW - Asteroids KW - Meteorites KW - Machine learning KW - Transfer learning KW - Raman spectroscopy KW - Mass spectrometry KW - Fourier-transform infrared spectroscopy PY - 2024 DO - https://doi.org/10.1016/j.trac.2024.117991 VL - 181 SP - 1 EP - 22 PB - Elsevier B.V. AN - OPUS4-62142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kalbe, Ute A1 - Schröder, Simon Alexander A1 - Richter, Matthias A1 - Horn, Wolfgang A1 - Stephan, Ina A1 - Hohmann, Gloria A1 - Ziegert, Christof T1 - Identifikation und Einordnung von historischen Lehmbauteilen für die Wiederverwendung hinsichtlich Anreicherung von Schadstoffen und bauschädlichen Salzen T1 - Identification and classification of historical earth construction elements for recycling in respect of accumulation of pollutants and structurally damaging salts N2 - Lehmbaustoffe, einschließlich Lehm aus dem historischen Baubestand, bieten ein hohes Potenzial für ihre Wiederverwendbarkeit und die Schonung natürlicher Ressourcen. Zur Bewertung des Wiederverwendungspotenzials gibt es nur wenige Studien hinsichtlich der Schadstoffbelastung und der Anreicherung von Salzen in Gebäuden aus dem historischen Bestand. Tonminerale, die in Lehmbaustoffen als Bindemittel fungieren, können Schadstoffe binden. Die Region Mitteldeutschland ist geprägt durch jahrzehntelange Einwirkung erheblicher Schadstoffemissionen aus der Chemie- und Braunkohleindustrie. Der Eintrag von Schadstoffen in Lehmbaustoffe ist außerdem aus geogenen Hintergrundbelastungen denkbar, z. B. in Auenböden beeinflusst durch Einträge aus dem Erzbergbau. Salzbildende Anionen wie Chloride oder Nitrate können aufgrund ihrer hohen Löslichkeit mittels kapillarer Kräfte durch die Porenstruktur transportiert werden. In Lehmwänden können sie vor allem in oberflächennahen Lagen, in denen höhere Verdunstungsraten vorherrschen, durch Bindung mit in Lösung vorliegenden oder baustoffeigenen Kationen auskristallisieren und bauschädliche Salze ausbilden. Auch durch spezifische Nutzungen akkumulierte Schadstoffe, z. B. durch die Einwirkung von Tabakrauch, könnten theoretisch einer Wiederverwendung von Lehm entgegenstehen. In Anbetracht der Herausforderungen hinsichtlich der klimatischen und gesellschaftlichen Veränderungen, sind wissenschaftliche Erkenntnisse im Lehmbau erforderlich, die eine Integration in eine nachhaltige Kreislaufwirtschaft ermöglichen. Bei bisherigen Gesetzgebungsverfahren zu rezyklierten Baustoffen wurden Lehmbaustoffe noch nicht berücksichtigt. Ziel einer Vorstudie im Rahmen der WIR!-Initiative GOLEHM ist die Überprüfung der Wiederverwendbarkeit Wiederverwendbarkeit von Lehmbaustoffen aus historischen Bauten an Stichproben hinsichtlich der Umwelt- und Nutzerverträglichkeit. Für den Raum Mitteldeutschland können damit Anhaltspunkte darüber gegeben werden, welche Schadstoffe und bauschädlichen Salze in welchem Maße in Lehmbaustoffen aus dem Gebäudebestand erwartet werden können. Daraus können Hinweise zum Umgang mit Lehmbaustoffen aus historischen Gebäuden abgeleitet werden. Darüber hinaus wurden exemplarisch an zwei Gebäuden mikrobiologische Untersuchungen zur Ermittlung einer möglichen Belastung mit Schimmelpilzen vorgenommen. N2 - Earth construction materials, including earth from historical building stock, offer high potential in terms of their recyclability and sparing use of natural resources. Yet, only a few studies have been conducted on the levels of pollutants and the accumulation of salts in buildings from the historical building stock to enable an assessment of the potential for recycling. The aim of a preliminary study as part of the GOLEHM Initiative from WIR! is to use spot checks to review the recyclability of earth construction materials from historical buildings in terms of environmental impact and tolerance by users. This could provide indicators for the Central Germany region on which pollutants and structurally damaging salts can be expected in earth construction materials from the building stock and to what extent, allowing conclusions to be drawn on how to manage earth construction materials from historical buildings. Additionally, microbiological inspections of two sample buildings were performed to assess a potential contamination with mould. T2 - Lehm 2024 Fachtagung CY - Weimar, Germany DA - 27.09.2024 KW - Lehm KW - Wiederverwendung KW - Kreislaufwirtschaft KW - Schadstoffe KW - Bauschädliche Salze PY - 2024 SP - 1 EP - 8 CY - Weimar AN - OPUS4-61883 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Völker, Tobias A1 - Mensing, Friedrich A1 - Kruschwitz, Sabine T1 - Estimation of cement content in concrete by spatially resolved laser induced breakdown spectroscopy – Dataset N2 - This dataset includes both simulated and raw measurement data as detailed in the journal paper [1]. File names follow the format SampleNo_Type, where SampleNo corresponds to the sample identifier listed in Table 1, and Type specifies the data type: either syn (synthetic) or exp (experimental). For experimental data, a slice index is appended to the file name in the format SampleNo_Type_Slice, identifying the specific subsample. [1] https://doi.org/10.1016/j.cemconres.2024.107714 KW - LIBS KW - Spectroscopy KW - Cement content KW - Elemental mapping PY - 2024 DO - https://doi.org/10.5281/zenodo.14246581 PB - Zenodo CY - Geneva AN - OPUS4-62394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, Steven A1 - Lippa, Katrice A1 - Shimuzu, Yoshitaka A1 - Lalerle, Beatrice A1 - Saito, Takeshi A1 - Duewer, David A1 - Dai, Xinhua A1 - Davies, Stephen A1 - Ricci, Marina A1 - Baldan, Annarita A1 - Lang, Brian A1 - Sarge, Stefan A1 - Wang, Haifeng A1 - Pratt, Ken A1 - Josephs, Ralf A1 - Mariassy, Mikael A1 - Pfeifer, Dietmar A1 - Warren, John A1 - Bremser, Wolfram A1 - Ellison, Stephen A1 - Toman, Blaza A1 - Nelson, Michael A1 - Huang, Ting A1 - Fajgelj, Ales A1 - Gören, Ahmet A1 - Mackay, Lindsey A1 - Wielgosz, Robert T1 - Methods for the SI-traceable value assignment of the purity of organic compounds (IUPAC Technical Report) N2 - The “purity” of an organic compound typically refers, in practice, to an assignment of the mass fraction content of the primary organic component present in the material. The “purity” value of an organic primary calibrator material is the ultimate source of metrological traceability of any quantitative measurement of the content of that compound in a given matrix. The primary calibrator may consist of a Certified Reference Material (CRM) whose purity has been assigned by the CRM producer or a laboratory may choose to value-assign a material to the extent necessary for their intended application by using appropriately valid methods. This report provides an overview of the approach, performance and applicability of the principal methods used to determine organic purity including mass balance, quantitative NMR, thermal methods and direct-assay techniques. A statistical section reviews best practice for combination of data, value assignment as the upper limit values corresponding to 100 % purity are approached and how to report and propagate the standard uncertainty associated with the assigned values. KW - Calibration hierarchy KW - Certified reference materials KW - Mass balance KW - Measurement uncertainty KW - Organic purity KW - Primary calibrators KW - Primary reference materials KW - qNMR KW - Related-structure impurities KW - Thermal analysis KW - Titrimetry KW - Traceability KW - Uncertainty propagation KW - Volatile organic compounds KW - Water content PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627932 DO - https://doi.org/10.1515/pac-2020-0804 SN - 0033-4545 SN - 1365-3075 VL - 95 IS - 1 SP - 1 EP - 77 PB - de Gruyter CY - Berlin AN - OPUS4-62793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zöllner, Moritz T1 - Raman spectroscopy as a thermometric tool for the analysis of mortar binders N2 - The reconstruction of the thermal history of anthropogenic materials is crucial for understanding historical manufacturing techniques. Preparatory parameters such as firing temperature, heating and cooling rates, soaking time, and kiln atmosphere significantly affect the chemical and structural properties of the final product. Comparing historical materials with replicas produced under well-defined laboratory conditions helps identify indicators for these parameters. This comparative approach is greatly enhanced by spectroscopic analyses. Raman spectroscopy has proven to be a powerful tool in this field due to its high sensitivity to crystal-chemical alterations and high spatial resolution. The results of thermal experiments with gypsum and carbonate raw materials at burning temperatures up to 1000 °C are presented. Precise measurements of Raman peak positions and Raman band widths enable the differentiation of chemically similar phases. Changes in the Raman band parameters are evident even after the subsequent hydration-hardening process of the fired samples, allowing the spectral discrimination of samples treated at different temperatures steps. These findings from the thermal experiments are further applied to Raman micro-spectroscopic mappings of medieval and reenacted mortars. The extracted Raman band parameters show comparable values between the experimental and real-life samples, proving Raman spectroscopy as a suitable tool for estimating the burning temperature and thus elucidating the manufacturing procedures of anthropogenic materials. T2 - Jahrestagung Archäometrie und Denkmalpflege 2025 CY - Dresden, Germany DA - 18.03.2025 KW - Raman spectroscopy KW - Mineral thermometry PY - 2025 AN - OPUS4-62778 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufgard, Josefin T1 - Use Your Time (Domain) Wisely: Streamlined Analysis of Complex Mixtures with Pulsed-Laser Techniques N2 - Analyzing complex mixtures with mass spectrometry (MS) usually requires extensive sample preprocessing and separation techniques such as high-pressure iquid chromatography (HPLC). This approach allows for subsequent detection of one analyte at a time but at a cost of throughput. Recently, increasing attention has been put on thesimultaneous ionization of all analytes in complex mixtures without extensive preprocessing, aiming to streamline the analysis process while accepting a compromise in identification. Such methods are commonly referred to as direct mass-spectrometric analysis. Among those, pulsed laser-based ablation, allows for contactless chemical investigation and reaction monitoring in situ, with minimal sample pretreatments. Specifically, the mid-infrared lasers encompass the fundamental vibrational resonances of typical biological matrices and solvents; their use results in efficient material removal from the bulk phase. Interestingly, the resulting analyte chronograms during the ablation process showed that the analytes were not detected concomitantly. Instead, chronograms offered time-domain information by being detected at different timestamps. It is certain that chemical information is encoded in the time domain. However, the analyte-specific chronograms could be difficult to interpret with conventional workflows as they mostly overlap. In this study, we aim exploiting the commonly discarded information in the time domain as an orthogonal dimension to the m/z domain, achieving ategorization and grouping mass-spectral peaks according to their chemical origins. Here, we applied a pulsed diode-pumped solid-state (DPSS) laser at 3-μm wavelength to 10 μL hanging droplets of analyte. A secondary electrospray ionization (SESI) source was built in-house to ionize ablated analytes. With a model sample, i.e. a mixture of two antibiotics, remarkable differences in their chronograms were observed. In fact, the time-domain information reflects the chemical signature of the analytes and can provide an additional data dimension for accurate interpretation. With a phase-sensitive algorithm, the modified cross-correlation (mXcorr), the similarity between chronograms can be gauged. Consequently, mass-spectral peaks that shared the same chronogram features were grouped together, yielding analyte-specific mass spectra that can aid analyte identification. Lastly, the applicability for biological samples, such as peptides, will be discussed. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Mass specrometry KW - Laser Ablation KW - secondary ionization PY - 2024 AN - OPUS4-62733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Holstein, Tanja A1 - Muth, Thilo ED - Salerno, C. T1 - Bioinformatic workflows for metaproteomics N2 - The strong influence of microbiomes on areas such as ecology and human health has become widely recognized in the past years. Accordingly, various techniques for the investigation of the composition and function of microbial community samples have been developed. Metaproteomics, the comprehensive analysis of the proteins from microbial communities, allows for the investigation of not only the taxonomy but also the functional and quantitative composition of microbiome samples. Due to the complexity of the investigated communities, methods developed for single organism proteomics cannot be readily applied to metaproteomic samples. For this purpose, methods specifically tailored to metaproteomics are required. In this work, a detailed overview of current bioinformatic solutions and protocols in metaproteomics is given. After an introduction to the proteomic database search, the metaproteomic post-processing steps are explained in detail. Ten specific bioinformatic software solutions are focused on, covering various steps including database-driven identification and quantification as well as taxonomic and functional assignment. KW - Metaproteomics KW - Microbiomes KW - Proteomics KW - Bioinformatic workflow KW - Taxonomic assignment KW - Functional assignment KW - Protein quantification PY - 2024 SN - 978-1-0716-3909-2 SN - 978-1-0716-3910-8 SN - 978-1-0716-3912-2 DO - https://doi.org/10.1007/978-1-0716-3910-8_16 SN - 1064-3745 SN - 1940-6029 N1 - Serientitel: Methods in molecular biology – Series title: Methods in molecular biology VL - 2820 SP - 187 EP - 213 PB - Springer CY - New York, NY AN - OPUS4-62741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - NMR Spectroscopy as a PAT tool: Field integration of a laboratory instrument N2 - Companies of chemical industry find themselves more often in a rapidly changing environment, e.g., due to variability of raw material quality or energy costs and efficiency. Process optimization and new process concepts become more and more important. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds like exothermic reactions with high heat dissipation. Highly automated chemical process monitoring along with real-time quality control are prerequisites to such concepts and, thus, should be based on chemical information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. Field studies in modular and conventional production plant setups show promising results gaining process knowledge for further optimization. NMR spectroscopy appeared as preeminent online analytical method and allows using a modular data analysis approach, which can even serve as reliable reference method for further calibration-dependent PAT applications (e.g., NIR or Raman spectroscopy). Based on experiences from earlier field studies an improved field enclosure setup was developed and built, including the option of a secondary analytical method (e.g., optical spectroscopy). Integrated control systems allow for a flexible implementation based on the available automation infrastructure at the chemical plant or pilot plant setup. In the future, modular interconnecting “smart” PAT systems and process equipment have the potential speed up the setup of production equipment for chemicals and pharmaceuticals and therefore help to reduce the time-to-market. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - NMR Spectroscopy KW - Process Analytical Technology KW - Field Integration KW - Benchtop-NMR PY - 2025 AN - OPUS4-62744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Tobias T1 - Laser-Induced Breakdown Spectroscopy for Concrete Analysis: Applications and Practical Benefits N2 - Reinforced concrete structures are exposed not only to mechanical loads but also to chemical degradation, which can significantly impact their longevity and performance. Effective assessment and maintenance require a detailed understanding of the ingress of harmful species, such as chlorides or sulfates. Traditional analysis methods, like wet chemical analysis of drill dust or ground core samples, often require homogenization leading to the loss of crucial spatial information in sub-millimeter regions such as localized high concentrations of elements, e.g. in cracks. Laser-induced breakdown spectroscopy (LIBS) offers a cutting-edge solution, providing rapid, multi-element analysis with high spatial resolution from micrometer to millimeter scales. LIBS is capable of detecting both light and heavy elements, making it a powerful tool for detailed concrete analysis. Despite its clear advantages, LIBS is not commonly used in civil engineering. This presentation will showcase practical examples demonstrating the effectiveness and advantages of LIBS in concrete analysis, highlighting real-world applications provided by members of the “LIBS” subcommittee of the technical committee “Civil-Engineering” of the German Society for Non-Destructive Testing (DGZfP). Key examples will be discussed, including measurements from car parks or bridges, alongside an introduction to the newly released DGZfP leaflet B14 providing guidelines for the quantitative determination of chlorine content in concrete by LIBS. Furthermore, prospective applications of LIBS including material identification and classification for concrete recycling, and other emerging uses in civil engineering, will also be presented, showcasing the versatility and future potential of this technology. T2 - Conference on durability of building materials and systems in the transportation infrastructure CY - Mendrisio, Switzerland DA - 22.03.2025 KW - LIBS KW - Spectroscopy KW - Concrete KW - Structural Diagnostics PY - 2025 AN - OPUS4-62822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sparber‐Sauer, Monika A1 - Ferrari, Andrea A1 - Kosztyla, Daniel A1 - Ladenstein, Ruth A1 - Cecchetto, Giovanni A1 - Kazanowska, Bernarda A1 - Scarzello, Giovanni A1 - Ljungman, Gustaf A1 - Milano, Giuseppe Maria A1 - Niggli, Felix A1 - Alaggio, Rita A1 - Vokuhl, Christian A1 - Casanova, Michela A1 - Klingebiel, Thomas A1 - Zin, Angelica A1 - Koscielniak, Ewa A1 - Bisogno, Gianni T1 - Long‐term results from the multicentric European randomized phase 3 trial CWS/RMS‐96 for localized high‐risk soft tissue sarcoma in children, adolescents, and young adults N2 - Background: CWS/RMS‐96 was an international multicenter trial with randomization between two therapy arms of the standard four‐drug therapy (vincristine, ifosfamide, adriamycin, dactinomycin [VAIA]) versus an intensified six‐drug regimen (carboplatin, epirubicin, vincristine, dactinomycin, ifosfamide, and etoposide [CEVAIE]) for high‐risk rhabdomyosarcoma (RMS), extraskeletal Ewing sarcoma (EES), and undifferentiated sarcoma (UDS) in children, adolescents, and young adults aiming to improve their survival. Intensified chemotherapy with CEVAIE did not improve outcome. Methods: Patients younger than 21 years with a previously untreated localized HR‐RMS, EES, and UDS were enrolled from Cooperative Weichteilsarkom Studiengruppe (CWS) centers in Germany, Austria, Poland, Switzerland, and from Italian Soft Tissue Sarcoma Committee (STSC) centers. Randomization (1:1) to receive either 9 × 21 days cycles of VAIA or CEVAIE was performed separately in CWS and STSC. Hyperfractionated accelerated radiotherapy (32–44.8 Gy) was added at week 9–12 according to histology and response to chemotherapy. A secondary microscopically complete nonmutilating resection was performed if possible. Primary endpoints were response to chemotherapy, event‐free (EFS) and overall survival (OS). Results: Five hundred fifty‐seven patients (HR‐RMS:n = 416, EES and UDS:n = 141) underwent randomization: VAIA (n = 273) or CEVAIE (n = 284). Radiotherapy was given to 70% of patients in both groups. A secondary resection was performed in 47% and 48% patients, respectively. The 5‐year EFS and OS for the VAIA and CEVAIE treatment arms were 59.8% and 60.8% (p = .89), and 74.2% and 68.3% (p = .16), respectively. No differences in response, toxicity, or second malignancies emerged in the two groups. Conclusion: The use of an intensified regimen failed to show a significant improvement in tumor response and outcome of patients with localized HR‐RMS, EES, and UDS. KW - CEVAIE KW - CWS-96 KW - High-risk soft tissue sarcoma KW - Randomization KW - Rhabdomyosarcoma KW - RMS-96 KW - VAIA PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629373 DO - https://doi.org/10.1002/pbc.29691 SN - 1545-5017 VL - 69 IS - 9 SP - 1 EP - 11 PB - Wiley CY - New York, NY AN - OPUS4-62937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Capozzi, Staci L. A1 - Xia, Chunjie A1 - Shuwal, Matthew A1 - Zaharias Miller, Gillian A1 - Gearhart, Jeff A1 - Bloom, Erica A1 - Gehrenkemper, Lennart A1 - Venier, Marta T1 - From watersheds to dinner plates: Evaluating PFAS exposure through fish consumption in Southeast Michigan N2 - Muscle tissue and organ samples of six different fish species were collected from ten locations in Southeast Michigan’s Huron and Rouge watersheds. Per- and polyfluoroalkyl substances (PFAS) were analyzed in 36 samples comprising filets, liver, gut, and eggs using targeted analysis and the direct total oxidizable precursor (dTOP) assay on a subset of six samples. The median concentrations of the ΣPFAS in filets from the Huron and Rouge watersheds were 13 and 6.3 ng/g wet weight (w.w.), respectively. Perfluorooctane sulfonate (PFOS) was the most detected and abundant compound in fish organs, with the liver having the largest overall burden of PFAS. The highest percent increase in targeted PFAS after the dTOP assay was observed in the Catfish filet (552%) while the smallest increase was in the Catfish liver (32%) accounting for 1.3 and 8.1 nMole F/g dry weight (d.w.), respectively. The positive matrix factorization (PMF) analysis revealed three distinct PFAS sources, of which the one attributed to PFOS explained 73% of the data. Results from this work have important implications for fish consumption in Michigan waterways. Among the filet samples analyzed, the calculated daily consumption limit of total PFOS was exceeded in approximately 82% and 91% of samples for adults and children over the age of seven years old, respectively. KW - Direct total oxidizable precursor (dTOP) assay KW - Huron river watershed KW - Positive matrix factorization (PMF) KW - Rouge river watershed KW - Consumption limit PY - 2023 DO - https://doi.org/10.1016/j.chemosphere.2023.140454 SN - 1879-1298 VL - 345 SP - 1 EP - 9 PB - Elsevier CY - Amsterdam AN - OPUS4-62423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hauschildt, Charlotte T1 - New Approaches to PFAS Quali- and Quantification using GC-MS N2 - Known as “forever chemicals”, per- and polyfluoroalkyl substances (PFAS) are a class of synthetically produced chemicals that includes an estimated 10.000 compounds. Due to the persistence, toxicity and ubiquitous occurrence, research has focused on the qualification and quantification of the most important compounds as well as on the investigation of toxicity and possible routes of entry over the last 10 years. Liquid chromatography - mass spectrometry (LC-MS) is the analytical standard to test for PFAS, as the spectrum of detectable compounds is significantly more comprehensive than it is currently the case with gas chromatography - mass spectrometry (GC-MS). However, to be able to test for PFAS contamination in a more process-independent manner and to make the analysis more widely accessible, methods based on GC-MS are currently being developed. Since GC-MS methods only cover a fraction of the compounds belonging to the PFAS group so far, further development of the corresponding measurement methods is inevitable [1, 2]. The here described work is part of the EU project 23IND13 ScreenFood [3]. The aim is to develop sensitive analytical GC-MS methods that contribute to an improved identification and quantification of various PFAS (both currently regulated and emerging PFAS) in selected food and food packaging matrices. Of particular interest as a food contact material are native and recycled polymers such as PET. Besides, various techniques, including solvent-free variants such as thermal desorption GC-MS, will be tested for a quick and easy analysis. Multiple derivatization approaches, which cover different PFAS subgroups, will also be tested and evaluated. This poster will present the overall project objectives and first results. Acknowledgment: The project (23IND13, ScreenFood) has received funding from the European Partnership on Metrology, co-financed from the European Union’s Horizon Europe Research and Innovation Programme and by the Participating States. T2 - PFAS - Vermeidbar, Ersetzbar, Unverzichtbar?! (FU Berlin) CY - Berlin, Germany DA - 07.04.2025 KW - Per- and Polyfluoroalkyl Substances (PFAS) KW - Gas Chromatography - Mass Spectrometry (GC-MS) KW - EU Project KW - Derivatization Methods KW - Food Contact Material (FCM) PY - 2025 AN - OPUS4-62970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, Hans R. A1 - Weidner, Steffen M. T1 - H2O-Initiated Polymerization of L-Lactide N2 - Water-initiated ring-opening polymerizations (ROPs) of L-lactide (LA) were performed in bulk at 140 °C, whereupon 11 different salts or complexes of low-toxic metal ions such as tin (II), Zn(II), Zr(IV), and Bi(III) were used as catalysts. Only four catalysts gave satisfactory results despite a long reaction time (24 h). The influence of the temperature was studied with tin (II) 2-ethylhexanoate (SnOct2), dibutyltin oxide (Bu2SnO), and zinc bis-acetylacetonate (Zn(acac)2) and zirconium acetylacetonate (Zr(acac)4). With SnOct2, Bu2SnO and Zr(acac)4 the time was varied at 140 °C to compare their reactivity. Furthermore, two series of ROPs were carried out with variation of the LA/H2O ratio to verify the control of the molecular weight by the monomer-initiator ratio. Bi- or tri-modal molecular weight distributions (MWD) were found for most of the ROPs and bimodal melting endotherms in the differential scanning calorimetry (DSC) heating traces. The thickness and dependence of the 3D packing of the crystallites were monitored by small-angle X-ray scattering (SAXS) measurements. KW - MALDI-TOF MS KW - Polylactide KW - Polymerization KW - Crystallization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-628761 DO - https://doi.org/10.1007/s10924-025-03565-w SN - 1572-8919 SP - 1 EP - 15 PB - Springer Science and Business Media LLC AN - OPUS4-62876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tannenberg, Robert T1 - Multichannel real-time detection of biomarkers with highly miniaturized photonic microchips N2 - The development of novel photonic microchips is a promising approach to advance the detection of biomarkers through multichannel real-time analysis. This study reports the successful development of a backside released CMOS chip designed for the multichannel real-time detection of biomarkers. Operating at a wavelength of 1550 nm, the microchip features three detection channels in addition to a reference channel, enabling simultaneous analysis of multiple biomarkers. The microchip incorporates micro-ring resonators that are directly functionalized with specific bioreceptors, which significantly improves the affinity towards target biomarkers. The employed surface functionalization strategy enables versatile immobilization of receptor molecules and serves as a starting point for various analytical applications. A tunable laser is utilized as the excitation source, providing precise wavelength tuning and stable optical output, essential for achieving optimal resonance conditions within the micro-ring resonators. Our chips use integrated multi-mode interferometers as beam-splitter, grating coupler and Ge-photodiodes, resulting in an ultra-small footprint. The complete chip including metal pads has an area of 1 mm2. The results indicate that the developed multichannel photonic microchip system enables online detection of multiple biomarkers. The compact and highly miniaturized design of this microchip positions them as promising candidates for point-of-care diagnostics and personalized medicine applications. With further advancements, this technology opens a path to transform biomarker detection across various medical fields, offering rapid, reliable, and cost-effective diagnostic solutions. In conclusion, the presented multichannel photonic microchips signify a substantial leap forward in real-time biomarker detection, providing a robust platform for future research and clinical applications. T2 - SPIE Optics + Optoelectronics 2025 CY - Prague, Czech Republic DA - 07.04.2025 KW - Biosensor KW - Optics KW - Silicon semiconductor KW - Proteins KW - Clinical chemistry PY - 2025 AN - OPUS4-62954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zöllner, Moritz T. A1 - Dariz, Petra A1 - Riedel, Jens A1 - Schmid, Thomas T1 - Dolomite and Mg Calcite as Mineral Thermometers in Mortar Binders. A High Resolution Raman Spectroscopic Study N2 - This paper suggests the use of high‐resolution Raman scattering bands of MgCa carbonates as posteriori thermometer minerals in archaeometric studies. Therefore, the thermal behavior of two dolomite samples and the hydration and carbonation reaction in air of the decomposition products were investigated by Raman microspectroscopy. The increase in the calcination temperature resulted in the formation of – Raman silent MgO and – inert Mg calcite at 700°C–750°C. In contrast, the decarbonation, hydration, and recarbonation of sample material exposed to 750°C–900°C in a muffle furnace led to the appearance of Mg‐free calcite. High spectral resolution Raman spectroscopy enabled a spectral distinction between these two groups due to differences in the band parameters (peak position, bandwidth) of the vibrational (v1, v4, L) modes of calcite. In combination with Raman microspectroscopic mapping, this spectral information represents a new approach for the estimation of burning temperatures of medieval high‐fired gypsum mortars via natural dolomite impurities. Thus, the results of this work highlight the importance and potential of Raman microspectroscopy as a thermometric tool for elucidating the thermal history of anthropogenic fired materials, with potential applications for archaeometry and art technology, as well as for quality controls in the frame of the production of mineral mortar binders and ceramics or bricks, respectively. KW - Mineral thermometry KW - Raman spectroscopy KW - Dolomite KW - High-fired gypsum mortar PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630270 DO - https://doi.org/10.1002/jrs.6810 SN - 1097-4555 SP - 1 EP - 13 PB - Wiley AN - OPUS4-63027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aree, T. A1 - Saenger, W. A1 - Leibnitz, Peter A1 - Hoier, H. T1 - Crystal structure of heptakis(2,6-di-O-methyl)-β-cyclodextrin dihydrate: A water molecule in an apolar cavity N2 - Heptakis(2,6-di-O-methyl)-β-cyclodextrin crystallized from water at 18 °C as dihydrate (DIMEB·2 H₂O) in the monoclinic space group P2₁ with unit cell dimensions a=15.2415(5), b=10.6391(4), c=23.3239 (8) Å, β=101.798(1)°. X-ray analysis reveals a torus-like macrocycle stabilized by systematic hydrogen bonds O-3–H··O-2’ and C-6–H··O-5’ between adjacent glucose residues. The O-6–CH₃ methoxy groups of three glucose units are directed toward but do not close the cavity. Both ends of the cavity are closed by adjacent molecules which are related by the characteristics of ‘cage type’ crystal packing. One water molecule is included in the apolar cavity of the torus and has very high anisotropic thermal displacement factor due to lack of hydrogen bonding interactions to DIMEB, while the other one is located in an intermolecular void and forms hydrogen bonds to O-3 and O-6 oxygen atoms. KW - β-Cyclodextrin KW - Dimethylated β-cyclodextrin KW - Inclusion complexes KW - Hydrogen bonding PY - 1999 DO - https://doi.org/10.1016/S0008-6215(99)00033-6 SN - 0008-6215 N1 - Zu dieser Veröffentlichung existiert ein Corrigendum, das in der Zeitschrift "Carbohydrate research" veröffentlicht wurde, Jg. 318 (1999), H. 1-4, S. 201, DOI: 10.1016/S0008-6215(99)00145-7. Dieses Corrigendum ist in der hiesigen PDF-Datei enthalten. - There is a corrigendum for this publication that was published in the journal "Carbohydrate research", vol. 318 (1999), iss. 1-4, p. 201, doi: 10.1016/S0008-6215(99)00145-7. This corrigendum is included in the present pdf file. VL - 315 IS - 3-4 SP - 199 EP - 205 PB - Elsevier CY - Amsterdam AN - OPUS4-63052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rösler, Alexander A1 - Weidner, Steffen M A1 - Klamroth, Tillmann A1 - Müller, Axel HE A1 - Schlaad, Helmut T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents N2 - The kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations. KW - MALDI-TOF MS KW - Anionic polymerization KW - β‐myrcene KW - Kinetics PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630900 DO - https://doi.org/10.1002/pi.6772 SP - 1 EP - 8 PB - John Wiley & Sons Ltd AN - OPUS4-63090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalichow, Dirk A1 - Wilsch, Gerd A1 - Völker, Tobias T1 - Laser Induced Breakdown Spectroscopy for the Chemical Investigation of Concrete—Status of Practical Application N2 - The assessment and maintenance of reinforced concrete structures depends largely on knowledge of the chloride content and chloride ingress. Common methods are the wet chemical analysis of drill dust or powder from ground drill core segments. However, due to the homogenization process, this approach often fails to detect locally elevated chloride levels. A state-of-the-art alternative method is laser-induced breakdown spectroscopy (LIBS), which offers rapid analysis and the possibility of detecting several chemical elements simultaneously. This method is particularly characterized by its ability to measure light elements such as hydrogen, carbon or sodium. The spatial resolution of LIBS is usually 0.25 mm but can be increased to 0.1 mm or less if required. BARG, is the first commercial building materials laboratory in Germany to use LIBS in practice. The current LIBS setup enables rapid, spatial quantification of the chlorine content and at the same time the creation of element maps that visually represent the distribution of essential elements in the concrete. This method can be used to localize areas of elevated chlorine content, particularly in cracks or near reinforcing bars. With the ability to analyze several elements simultaneously, LIBS can determine measurement points associated with the cement phase and, taking into account the water content, relate the measured contents directly to the cement mass. The detailed ingress profiles determined by LIBS provide essential data for the estimation of accurate chlorine diffusion coefficients, which are crucial for probabilistic lifetime predictions. The estimation of the carbon distribution enables the localization of carbonated regions and their effect on the chloride distribution. The possibility of quantitatively determining the sulfur distribution also indicates areas that are affected by a possible sulfate attack. The presentation uses practical examples to demonstrate the possibilities and advantages of the LIBS method. In addition, the newly published leaflet B14 of the German Society for Non-Destructive Testing (DGZfP) will be presented, which describes the use of LIBS for the quantitative determination of chloride content in concrete. T2 - ICCRRR 2024 CY - Cape Town, South Africa DA - 04.11.2024 KW - Concrete KW - Chloride KW - Corrosion KW - Repair KW - Maintenance PY - 2024 DO - https://doi.org/10.1007/978-3-031-75507-1_40 VL - 59 SP - 411 EP - 420 AN - OPUS4-62480 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dalichow, Dirk T1 - Laser Induced Breakdown Spectroscopy (LIBS) for the chemical investigation of concrete- Status of practical application and regulations in Germany N2 - The assessment and maintenance of reinforced concrete structures depends largely on knowledge of the chloride content and chloride ingress. Common methods are the wet chemical analysis of drill dust or powder from ground drill core segments. However, due to the homogenization process, this approach often fails to detect locally elevated chloride levels. A state-of-the-art alternative method is laser-induced breakdown spectroscopy (LIBS), which offers rapid analysis and the possibility of detecting several chemical elements simultaneously. This method is particularly characterized by its ability to measure light elements such as hydrogen, carbon or sodium. The spatial resolution of LIBS is usually 0.25 mm but can be increased to 0.1 mm or less if required. BARG, is the first commercial building materials laboratory in Germany to use LIBS in practice. The current LIBS setup enables rapid, spatial quantification of the chlorine content and at the same time the creation of element maps that visually represent the distribution of essential elements in the concrete. This method can be used to localize areas of elevated chlorine content, particularly in cracks or near reinforcing bars. With the ability to analyze several elements simultaneously, LIBS can determine measurement points associated with the cement phase and, taking into account the water content, relate the measured contents directly to the cement mass. The detailed ingress profiles determined by LIBS provide essential data for the estimation of accurate chlorine diffusion coefficients, which are crucial for probabilistic lifetime predictions. The estimation of the carbon distribution enables the localization of carbonated regions and their effect on the chloride distribution. The possibility of quantitatively determining the sulfur distribution also indicates areas that are affected by a possible sulfate attack. The presentation uses practical examples to demonstrate the possibilities and advantages of the LIBS method. In addition, the newly published leaflet B14 of the German Society for Non-Destructive Testing (DGZfP) will be presented, which describes the use of LIBS for the quantitative determination of chloride content in concrete. T2 - ICCRRR 2024 CY - Cape Town, South Africa DA - 04.11.2024 KW - Concrete KW - Chloride KW - Corrosion KW - Repair KW - Maintenance PY - 2024 AN - OPUS4-62481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmitt, Johannes T1 - Data Acquisition System for Single Particle Inductively Coupled Plasma Mass Spectrometry (spICP-MS) with Nanosecond Time Resolution N2 - This study presents our data acquisition system prototype for spICP-MS with nanosecond time resolution (nanoDAQ) and a matching data processing approach for nanosecond resolved single particle spICP-MS data. The system continuously samples the secondary electron multiplier (SEM) detector signal with a dwell time of approximately 2 ns and enables the detection of gold nanoparticles (AuNP) as small as 7.5 nm[1] with a commercial single quadrupole ICP-MS instrument. The acquired transient data is processed based on the temporal distance between detector events and the event density. It was shown that the inverse logarithm of the distance between detector events is proportional to the particle size and that the number of detector events corresponding to a particle signal distribution can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion.[1] The high data acquisition frequency of the systems allows recording of a statistically significant number of data points in 60 s or less, which leads to the main time limitation for analyses being merely the sample uptake time and rinsing step between analyte solutions. T2 - 55th Annual Conference of the German Society for Mass Spectrometry CY - Freising, Germany DA - 10.03.2024 KW - Nanoparticles KW - Mass Spectrometry KW - Instrumentation KW - spICP-MS PY - 2024 AN - OPUS4-62315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinelt, Manuel T1 - Capabilities of Surface-Assisted Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (SA-FAPA-MS) for Direct Analysis of Polycyclic Aromatic Hydrocarbons (PAHs) N2 - Ambient desorption/ionization mass spectrometry (ADI-MS) is a growing area in the analytical chemistry of organic molecules. It requires only minimal sample preparation and can reduce analysis time compared to traditional methods.[1] One evolving method is the plasma-based pin-to-capillary Flowing Atmospheric-Pressure Afterglow (FAPA) source. Which is an improved version of the original pin-to-plate FAPA, resulting in significantly lower background signals and less oxidation of the analytes.[2] In our case, samples are probed directly from thin-layer chromatography (TLC) plates, which have shown promising results in improving signal response and performance in mass spectral imaging in previous studies. Especially, cyano (CN)-HPTLC and reversed-phase (RP2)-TLC plates were suited best for the analysis of different organic molecules.[3] In this work, FAPA is investigated as a method to determine polycyclic aromatic hydrocarbons (PAHs). Furthermore, its suitability for rapid screening of real samples was investigated. 30 pure PAH standard samples were analyzed on different TLC surfaces. Cyano (CN)-HPTLC and reversed-phase (RP2)-TLC plates proved to be the most suitable substrate for the analysis of PAH compounds. Linear ranges of up to four orders of magnitude could be achieved. Limits of detection (LOD) of anthracene, chrysene, and fluorene were in the µg/L range. However, these pure analytes differ from PAH samples collected in the environment, which may contain hundreds of different PAHs among other constituents. Therefore, PAH containing real samples were used to test the method and its screening capability on more complex samples. A standard reference material (diesel particulate extract, NIST SRM 1975) was analyzed for method validation. For sample preparation, 1 µL of the extract was spotted directly onto the TLC surface. It was possible to perform a triple determination in approx. 20 min. Therefore, SA-FAPA-MS has a huge potential to be established as a method for rapid qualitative screening of PAHs in real samples. T2 - 55th Annual Conference of the German Society for Mass Spectrometry (Deutsche Gesellschaft für Massenspektrometrie, DGMS). CY - Freising, Germany DA - 10.03.2024 KW - Mass Spectrometry KW - Massenspektrometrie KW - Instrumental Analytical Chemistry KW - Instrumentelle Analytische Chemie KW - Polycyclic Aromatic Hydrocarbons PY - 2024 AN - OPUS4-62316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klewe, Tim A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine T1 - Review of moisture measurements in civil engineering with ground penetrating radar – Applied methods and signal features N2 - When applying Ground Penetrating Radar (GPR) to assess the moisture content of building materials, different medium properties, dimensions, interfaces and other unknown influences may require specific strategies to achieve useful results. Hence, we present an overview of the various approaches to carry out moisture measurements with GPR in civil engineering (CE). We especially focus on the applied Signal features such as time, amplitude and frequency features and discuss their limitations. Since the majority of publications rely on one single feature when applying moisture measurements, we also hope to encourage the consideration of approaches that combine different signal features for further developments. KW - Ground Penetrating Radar KW - Moisture KW - Civil engineering KW - Signal features PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520684 DO - https://doi.org/10.1016/j.conbuildmat.2021.122250 VL - 278 SP - 122250 PB - Elsevier Ltd. AN - OPUS4-52068 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim T1 - Feuchtemessung an Fußböden mit Radar und Neutronensonde – Ein Vergleich von Labor und Praxis N2 - Nach Auftreten eines Feuchteschadens in Fußbodenaufbauten sind sowohl die zeitnahe Feststellung als auch Eingrenzung betroffener Bereiche von besonderer Bedeutung. So können erforderliche Renovierungsmaßnahmen effizient geplant und mögliche Folgeschäden vermieden werden. Zur messtechnischen Beantwortung dieser Fragestellungen werden bereits seit vielen Jahren Neutronensonden eingesetzt, welche allerdings keine Tiefenzuordnung des schadensträchtigen Flüssigwassers zulassen. Hierzu müssen mit hohem zeitlichem und finanziellem Aufwand zerstörende Sondierungsbohrungen vorgenommen werden, welche zukünftig durch den parallelen Einsatz des Radarverfahrens vermieden werden könnten. In systematischen Laborstudien wurden gängige Feuchteschäden an häufig anzutreffenden Fußbodenaufbauten simuliert und deren Einfluss auf das Messsignal untersucht. Hierbei kamen Zementund Anhydritestriche, sowie die Dämmmaterialen Styropor, Styrodur, Glaswolle und Perlite-Schüttung mit variierenden Schichtdicken zum Einsatz, um die vielfältigen Konfigurationen der Praxis abzubilden. Für den gewonnenen Datensatz konnten geeignete Signalmerkmale extrahiert werden, welche mithilfe multivariater Datenauswertung eine Klassifizierung des vorliegenden Schadenfalls zulassen. Zum Ende des Forschungsvorhabens steht besonders die Anwendbarkeit der entwickelten Methoden für die Praxis im Fokus. Hierzu wurden Messungen an realen Schadensfällen durchgeführt und deren Ergebnisse mit den Laboruntersuchungen verglichen. Hierbei stellten sich variierende Schichtdicken, sowie vorkommende Fußbodenheizungen und Armierungsgitter als mögliche Fehlerquellen für eine vollständig automatisierte Auswertung heraus. T2 - 81. Jahrestagung der Deutschen Geophysikalischen Gesellschaft (DGG) CY - Online meeting DA - 01.03.2021 KW - Radar KW - Feuchte KW - Fußboden KW - Neutronensonde PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522227 DO - https://doi.org/10.23689/fidgeo-3955 AN - OPUS4-52222 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Klewe, Tim T1 - Comparison of the Calcium Carbide Method and Darr Drying to Quantify the Amount of Chemically Bound Water in Early Age Concrete N2 - Hydration is the exothermic reaction between anhydrous cement and water, which forms the solid cement matrix of concrete. Being able to evaluate the hydration is of high interest for the use of both conventional and more climate-friendly building materials. The experimental monitoring is based on temperature or moisture measurements. The first needs adiabatic conditions, which can only be achieved in laboratory. The latter is often measured comparing the weight of the material sample before and after oven drying, which is time-consuming. This study investigates the moisture content of two cement-based and two calcium sulphate based mixtures for the first 90 days by using the calcium carbide method and oven drying at 40 °C and 105 °C (Darr method). Thereby, the amount of chemically bound water is determined to derive the degree of hydration. The calcium carbide measurements highly coincide with oven drying at 40 °C. The calcium carbide method is therefore evaluated as a suitable alternative to the time-consuming Darr drying. The prompt results are seen as a remarkable advantage and can be obtained easily in laboratory as well as in the field. KW - Concrete KW - Hydration KW - Material moisture KW - Calcium carbide method KW - Bound water KW - Darr method KW - Oven drying KW - Chemisorption KW - Physisorption PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564519 DO - https://doi.org/10.3390/ma15238422 VL - 15 IS - 23 SP - 1 EP - 16 PB - MDPI AN - OPUS4-56451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Stolpe, Heiko A1 - Wiehle, Philipp T1 - Moisture diffusion affected by the Knudsen effect in temporal changing pore networks N2 - Almost all building materials in civil engineering have an open porosity and interact with or are affected by the environmental conditions. Structures might suffer from effects such as moisture adsorption, carbonation, corrosion, penetration of salt ions and chemical substances, etc. In the hygroscopic range, these processes are mostly driven by diffusion. Due to the confinement of small pores (< 1 µm), the Knudsen effect reduces the molecular diffusion. This reduction can become more significant in case of temporal changing pore systems because of physisorption of water vapor, carbonation, or chemisorption. In this study, unstabilised earth blocks and earth masonry are investigated. In a first step, the pore size distribution of the blocks is measured and sorption isotherms are recorded in experiments. Besides the ordinary physisorption, the involved clay minerals undergo swelling or shrinking due to chemisorption. The following two effects must be considered: first, the reduction of the available pore space by the adsorbed water layer. For this, the Hillerborg sorption theory is used, which is a combination of the well-known Brunauer-Emmett-Teller sorption theory and the Kelvin equation. This allows the computation of adsorbed water layers even in curved pore geometries. Second, the variation of the initial pore size distribution due to chemisorption needs to be modelled. Based on these two models, the effective diffusion coefficient can be predicted. For validation, arrays of relative humidity sensors were embedded into a free-standing earth masonry wall. This monitoring was carried out over more than a year to have a broad variety of environmental conditions and was located in Berlin, Germany. The prediction of the effective diffusion coefficient can also be transferred to other processes and allows the investigation of materials having temporarily changing pore systems. Examples are the carbonation of cementitious materials, alkali silica reaction, calcium leaching of long-lasting structures, etc. This effect becomes most prominent in the meso-pore range and might alter the effective diffusion coefficient by more than 100 %. T2 - 4th International Congress on Materials & Structural Stability CY - Rabat, Morocco DA - 08.03.2023 KW - Earth masonry KW - Material moisture KW - Molecular diffusion KW - Chemisoprtion KW - Knudsen effect KW - Physisorption PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571391 SP - 1 EP - 8 PB - RILEM CY - Champs-sur-Marne AN - OPUS4-57139 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Stolpe, Heiko A1 - Kruschwitz, Sabine ED - Schumann, R. T1 - Correlation between the electric impedance and the water layer thickness in partially saturated screed samples N2 - The moisture content of screed samples is monitored by means of embedded sensors. Relative humidity sensors and multi-ring-electrodes are used to measure the spatial moisture distribution during desorption. Based on the humidity data and the pore volume distribution, the moisture and the water layer thickness within the pore space are predicted. Slit shape as well as cylindrical pores are evaluated. Finally, the measured real part of the electrical impedance and the calculated water layer thickness are correlated. Based on the available data, a significant trend change of the impedance is documented at a water layer thickness of approximately 3 nm. This water layer thickness corresponds to a relative humidity of 88.3%. T2 - 10. CMM Tagung CY - Ettlingen, Germany DA - 10.10.2019 KW - Material moisture KW - Screed KW - Embedded sensors KW - Electric impedance KW - Water layer thickness PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494636 VL - 10 SP - 79 EP - 102 PB - CMM, Karlsruher Institut für Technologie CY - Karlsruhe AN - OPUS4-49463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej A1 - Strangfeld, Christoph A1 - Zimmek, David A1 - Bartholmai, Matthias ED - Helmerich, Rosemarie ED - Ilki, A. ED - Motavalli, M. T1 - Smart electronic helper for long-term monitoring of bridges and building structures N2 - Increasing traffic volume on the one hand and ageing infrastructure on the other hand have created many new challenges for maintenance and structural health monitoring of roads and bridges. In the past, many bridges and road structures have been neglected, often resulting in traffic congestion, road closure, and increased repair costs. This research is concerned with the development of a system to improve the challenge of maintenance and early detection of damage, particularly moisture penetration and corrosion of steel reinforced concrete components. The objective is to develop a method that will also work after 30 years and longer. Many new IoT solutions are equipped with internal energy storage elements (accumulators or batteries) which are inappropriate here, since most relevant signs of concrete degradation occur after decades, where the functioning of such elements are more than questionable. The presented technology approach uses radio-frequency identification (RFID) and enables connectivity to sensors. It offers the advantage of an passive, completely independent energy supply without any energy storage components. Since the system should be permanently embedded in concrete, it is crucial to develop a long-term stable device which is adapted to the environmental influences of the structure, e.g., long-term resistance in very alkaline environment of pH 13. In numerous experiments, the robustness of the system was tested and evaluated. Various tests with encapsulations to protect the electronics were performed, and for long-term validation different concrete specimens were instrumented with RFID-sensor-systems. Their operating time is now around two years and investigations for signs of fatigue and damage to the encapsulation and the electronics are ongoing. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures (SMAR 2019) CY - Potsdam, Germany DA - 27.08.2019 KW - Long term monitoring KW - Passive RFID KW - SHM KW - Sensors KW - Smart structures PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-489890 SP - 1 EP - 6 PB - German Society for Non-Destructive Testing (DGZfP e.V.) AN - OPUS4-48989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Johann, Sergej A1 - Strangfeld, Christoph A1 - Zimmek, David A1 - Bartholmai, Matthias T1 - Smart electronic helper for long-term monitoring of bridges and building structures N2 - Increasing traffic volume on the one hand and ageing infrastructure on the other hand have created many new challenges for maintenance and structural health monitoring of roads and bridges. In the past, many bridges and road structures have been neglected, often resulting in traffic congestion, road closure, and increased repair costs. This research is concerned with the development of a system to improve the challenge of maintenance and early detection of damage, particularly moisture penetration and corrosion of steel reinforced concrete components. The objective is to develop a method that will also work after 30 years and longer. Many new IoT solutions are equipped with internal energy storage elements (accumulators or batteries) which are inappropriate here, since most relevant signs of concrete degradation occur after decades, where the functioning of such elements are more than questionable. The presented technology approach uses radio-frequency identification (RFID) and enables connectivity to sensors. It offers the advantage of an passive, completely independent energy supply without any energy storage components. Since the system should be permanently embedded in concrete, it is crucial to develop a long-term stable device which is adapted to the environmental influences of the structure, e.g., long-term resistance in very alkaline environment of pH 13. In numerous experiments, the robustness of the system was tested and evaluated. Various tests with encapsulations to protect the electronics were performed, and for long-term validation different concrete specimens were instrumented with RFID-sensor-systems. Their operating time is now around two years and investigations for signs of fatigue and damage to the encapsulation and the electronics are ongoing. T2 - SMAR 2019 CY - Potsdam, Germany DA - 27.08.2019 KW - Sensors KW - Passive RFID KW - Smart structures KW - SHT KW - Long term monitoring PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-501931 UR - https://www.ndt.net/?id=25011 SN - 1435-4934 VL - 25 IS - 1 SP - 1 EP - 6 PB - NDT.net CY - Kirchwald AN - OPUS4-50193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim T1 - Signalmerkmale des Radarverfahrens zur Klassifizierung von Feuchteschäden in Fußbodenaufbauten N2 - Zur Eingrenzung und Klassifizierung auftretender Feuchteschäden in geschichteten Fußbodenaufbauten wird bereits seit vielen Jahren das Neutronensondenverfahren eingesetzt. Während eine Eingrenzung des Schadens bereits durch die zerstörungsfrei aufgenommenen Messdaten möglich ist, erfordert die Klassifizierung zeit- und kostenintensive Sondierungsbohrungen. Die somit gewonnenen Tiefeninformationen zur Lage des Flüssigwassers tragen maßgeblich zur Planung der erforderlichen Reparaturarbeiten bei, was die Frage nach einer zerstörungsfreien Alternative zur vertikalen Lokalisierung von Feuchte in Fußböden stellt. Das Radarverfahren ist mit seiner hohen Sensitivität für Wasser besonders geeignet und soll künftig zur automatisierten Klassifizierung typischer Schadensfälle beitragen. In einem laufenden Forschungsvorhaben werden in systematischen Laborstudien gängige Schadensfälle an häufig anzutreffenden Fußbodenaufbauten simuliert und deren Einfluss auf die genannten Verfahren untersucht. Hierbei kommen Zement- und Anhydritestriche, sowie unterschiedliche Dämmmaterialen mit variierenden Schichtdicken zum Einsatz. Wesentlicher Bestandteil der Auswertung ist die Extraktion signifikanter Signalmerkmale des Radarverfahrens, welche Rückschlüsse auf den Schadensfall und ggf. die Wassermenge zulassen. Die Robustheit gegenüber unterschiedlichsten Aufbauten mit wechselnden Schichtdicken und Materialien steht hierbei besonders im Fokus. Erste Ergebnisse empfehlen die Betrachtung der örtlichen Verteilung bestimmter Signalmerkmale im Radargramm (B-Scan), um eine Klassifizierung der Schadensfälle vornehmen zu können. T2 - Fachtagung Bauwerksdiagnose 2020 CY - Berlin, Germany DA - 13.02.2020 KW - Radar KW - Feuchte KW - Signalmerkmale KW - Klassifikation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504143 AN - OPUS4-50414 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Stolpe, Heiko A1 - Wiehle, Philipp T1 - Moisture diffusion affected by the Knudsen effect in temporal changing pore networks N2 - Almost all building materials in civil engineering have an open porosity and interact with or are affected by the environmental conditions. Structures might suffer from effects such as moisture adsorption, carbonation, corrosion, penetration of salt ions and chemical substances, etc. In the hygroscopic range, these processes are mostly driven by diffusion. Due to the confinement of small pores (less than1 µm), the Knudsen effect reduces the molecular diffusion. This reduction can become more significant in case of temporal changing pore systems because of physisorption of water vapor, carbonation, or chemisorption. In this study, unstabilised earth blocks and earth masonry are investigated. In a first step, the pore size distribution of the blocks is measured and sorption isotherms are recorded in experiments. Besides the ordinary physisorption, the involved clay minerals undergo swelling or shrinking due to chemisorption. The following two effects must be considered: first, the reduction of the available pore space by the adsorbed water layer. For this, the Hillerborg sorption theory is used, which is a combination of the well-known Brunauer-Emmett-Teller sorption theory and the Kelvin equation. This allows the computation of adsorbed water layers even in curved pore geometries. Second, the variation of the initial pore size distribution due to chemisorption needs to be modelled. Based on these two models, the effective diffusion coefficient can be predicted. For validation, arrays of relative humidity sensors were embedded into a free-standing earth masonry wall. This monitoring was carried out over more than a year to have a broad variety of environmental conditions and was located in Berlin, Germany. The prediction of the effective diffusion coefficient can also be transferred to other processes and allows the investigation of materials having temporarily changing pore systems. Examples are the carbonation of cementitious materials, alkali silica reaction, calcium leaching of long-lasting structures, etc. These effects are prominent in the meso-pore range and might significantly alter the effective diffusion coefficient. KW - Earth material KW - Material moisture KW - Physisoprtion KW - Chemisorption PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583811 DO - https://doi.org/10.1016/j.matpr.2023.09.034 SN - 2214-7853 SP - 1 EP - 8 PB - Elsevier Ltd. CY - Amsterdam, Niederlande AN - OPUS4-58381 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Küttenbaum, Stefan T1 - Zur Visualisierung von Schäden in Betonschwellen durch zerstörungsfreie Ultraschallprüfung N2 - Die bildgebende Ultraschalltechnik liefert Hinweise auf verdeckte Schäden in Spannbetonschwellen. Dieses zerstörungsfreie Prüfverfahren schafft eine objektive und vergleichbare Basis für die Zustandsbestimmung der Schwellen und ermöglicht die Optimierung von baulichen Erhaltungsstrategien. KW - Spannbetonschwellen KW - Zustandsbewertung KW - Verkehrsinfrastruktur PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-592914 UR - https://www.eurailpress.de/magazine.html SN - 0013-2845 IS - 12/23 SP - 26 EP - 31 PB - DVV Media Group CY - Hamburg AN - OPUS4-59291 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Küttenbaum, Stefan T1 - Zur Visualisierung von Schäden in Betonschwellen durch zerstörungsfreie Ultraschallprüfung N2 - Die bildgebende Ultraschalltechnik liefert Hinweise auf verdeckte Schäden in Spannbetonschwellen. Dieses zerstörungsfreie Prüfverfahren schafft eine objektive und vergleichbare Basis für die Zustandsbestimmung der Schwellen und ermöglicht die Optimierung von baulichen Erhaltungsstrategien. KW - Betonschwellen KW - Ultraschall KW - Schieneninfrastruktur KW - Gleisoberbau KW - Spannbetonschwelle PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591889 UR - https://www.eurailpress.de/etr SN - 0013-2845 IS - 12 SP - 26 EP - 31 PB - DVV Media Group, Eurailpress CY - Hamburg AN - OPUS4-59188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Klewe, Tim T1 - Non-destructive classification of moisture deterioration in layered building floors using ground penetrating radar N2 - In the event of moisture deterioration, rapid detection and localization is particularly important to prevent further deterioration and costs. For building floors, the layered structure poses a challenging obstacle for most moisture measurement methods. But especially here, layer-specific information on the depth of the water is crucial for efficient and effective repairs. Ground Penetrating Radar (GPR) shows the potential to generate such depth information. Therefore, the present work investigates the suitability of GPR in combination with machine learning methods for the automated classification of the typical deterioration cases (i) dry, (ii) wet insulation, and (iii) wet screed. First, a literature review was conducted to identify the most common methods for detecting moisture in building materials using GPR. Here, it especially became clear that all publications only investigated individual time-, amplitude- or frequency features separately, without combining them. This was seen as a potential aspect for innovation, as the multivariate application of several signal features can help to overcome individual weaknesses and limitations. Preliminary investigations carried out on drying screed samples confirmed the profitable use of multivariate evaluations. In addition to the general suitability and dependencies of various features, first limitations due to possible interference between the direct wave and the reflection wave could be identified. This is particularly evident with thin or dry materials, for which the two-way travel times of the reflected radar signals become shorter. An extensive laboratory experiment was carried out, for which a modular test specimen was designed to enable the variation of the material type and thickness of screed and insulation, as well as the simulation of moisture deteriorations. The data collected revealed clear differences between dry and deteriored structures within measured B-scans. These deviations were to be detected with the newly introduced B-scan features, which evaluate the statistical deviation of A-scan features within a survey line. In this way, deteriorations to unknown floor structures are recognized, regardless of the material parameters present. In a subsequent training and cross-validation process of different classifiers, accuracies of over 88 \% of the 504 recorded measurements (252 different experimental setups) were achieved. For that, the combination of amplitude and frequency features, which covered all relevant reflections of the radar signals, was particularly beneficial. Furthermore, the data set showed only small differences between dry floors and deteriored screeds for the B-scan features, which could be attributed to a homogeneous distribution of the added water in the screeds. The successfully separation of these similar feature distributions raised the suspicion of overfitting, which was examined in more detail by means of a validation with on-site data. For this purpose, investigations were carried out at five different locations in Germany, using the identical measurement method like in the laboratory. By extracting drilling cores, it was possible to determine the deterioration case for each measurement point and thus generate a corresponding reference. However, numerous data had to be sorted out before classification, since disturbances due to underfloor heating, screed reinforcements, steel beams or missing insulation prevented comparability with the laboratory experiments. Validation of the remaining data (72 B-scans) achieved only low accuracy with 53 \% correctly classified deterioration cases. Here, the previously suspected overfitting of the small decision boundary between dry setups and deteriored screeds within the laboratory proved to be a problem. The generally larger deviations within (also dry) on-site B-scans were thus frequently misclassified as screed deterioration. In addition, there were sometimes strongly varying layer thicknesses or changing cases of deterioration within a survey line, which caused additional errors due to the local limitation of the drilling core reference. Nevertheless, individual on-site examples also showed the promising potential of the applied signal features and the GPR method in general, which partly allowed a profound interpretation of the measurements. However, this interpretation still requires the experience of trained personnel and could not be automated using machine learning with the available database. Nevertheless, such experience and knowledge can be enriched by the findings of this work, which provide the basis for further research. Future work should aim at building an open GPR data base of on-site moisture measurements on floors to provide a meaningful basis for applying machine learning. Here, referencing is a crucial point, whose limitations with respect to the moisture present and its distribution can easily reduce the potential of such efforts. The combination of several reference methods might help to overcome such limitations. Similarly, a focus on monitoring approaches can also help to reduce numerous unknown variables in moisture measurements and increase confidence in the detection of different deterioration cases. KW - NDT KW - Moisture measurement KW - Ground penetrating radar KW - Building floor PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591044 DO - https://doi.org/10.14279/depositonce-19306 SP - 1 EP - 146 PB - Technische Universität Berlin CY - Berlin AN - OPUS4-59104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Küttenbaum, Stefan A1 - Braml, T. A1 - Taffe, A. A1 - Keßler, S. A1 - Maack, Stefan T1 - Reliability assessment of existing structures using results of nondestructive testing N2 - Making optimal decisions about the reliability of existing structures requires that the information used in assessment adequately represents the properties and the condition of the structures. The knowledge gap regarding a structure to be assessed can be successively filled by individually purposeful observations on site. This paper gives an overview of an approach for utilizing nondestructively gathered measurement results in reliability assessment of existing structures. An essential part of measurement-based stochastic modeling of basic variables is the calculation of measurement uncertainties, which serves to establish confidence in measurement, to ensure the comparability of unambiguously expressed measurement results, and to quantify the quality of the measured information. Regarding the current discourse on how to treat information collected on-site in the context of assessment, the authors recommend that measurement uncertainty becomes an uncertainty component mandatorily to be represented in measurement-based stochastic models. The main steps of the proposed concept are presented, and the advantages of its application are emphasized by means of a prestressed concrete bridge as case study. The bridge is assessed regarding the serviceability limit state decompression using ultrasonic and radar data measured at the structure. KW - Bridge KW - Measurement uncertainty KW - Prestressed concrete KW - Stochastic modeling KW - Probabilistic methods PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529927 DO - https://doi.org/10.1002/suco.202100226 SN - 1751-7648 VL - 22 IS - 5 SP - 2895 EP - 2915 PB - John Wiley & Sons Ltd CY - Oxford AN - OPUS4-52992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moreno Torres, Benjami A1 - Völker, Christoph A1 - Munsch, Sarah Mandy A1 - Hanke, T. A1 - Kruschwitz, Sabine ED - Tosti, F. T1 - An Ontology-Based Approach to Enable Data-Driven Research in the Field of NDT in Civil Engineering N2 - Although measurement data from the civil engineering sector are an important basis for scientific analyses in the field of non-destructive testing (NDT), there is still no uniform representation of these data. An analysis of data sets across different test objects or test types is therefore associated with a high manual effort. Ontologies and the semantic web are technologies already used in numerous intelligent systems such as material cyberinfrastructures or research databases. This contribution demonstrates the application of these technologies to the case of the 1H nuclear magnetic resonance relaxometry, which is commonly used to characterize water content and porosity distri-bution in solids. The methodology implemented for this purpose was developed specifically to be applied to materials science (MS) tests. The aim of this paper is to analyze such a methodology from the perspective of data interoperability using ontologies. Three benefits are expected from this ap-proach to the study of the implementation of interoperability in the NDT domain: First, expanding knowledge of how the intrinsic characteristics of the NDT domain determine the application of semantic technologies. Second, to determine which aspects of such an implementation can be improved and in what ways. Finally, the baselines of future research in the field of data integration for NDT are drawn. KW - Ontology Engineering KW - Interoperability KW - Data-integration KW - NMR relaxometry KW - materials informatics PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529716 DO - https://doi.org/10.3390/rs13122426 SN - 2072-4292 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. VL - 13 IS - 12 SP - 2426 PB - Multidisciplinary Digital Publishing Institute (MDPI) CY - Basel, Switzerland AN - OPUS4-52971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bühling, Benjamin A1 - Maack, Stefan A1 - Schweitzer, T. A1 - Strangfeld, Christoph T1 - Enhancing the spectral signatures of ultrasonic fluidic transducer pulses for improved time-of-flight measurements N2 - Air-coupled ultrasonic (ACU) testing has proven to be a valuable method for increasing the speed in non-destructive ultrasonic testing and the investigation of sensitive specimens. A major obstacle to implementing ACU methods is the significant signal power loss at the air–specimen and transducer–air interfaces. The loss between transducer and air can be eliminated by using recently developed fluidic transducers. These transducers use pressurized air and a natural flow instability to generate high sound power signals. Due to this self-excited flow instability, the individual pulses are dissimilar in length, amplitude, and phase. These amplitude and angle modulated pulses offer the great opportunity to further increase the signal-to-noise ratio with pulse compression methods. In practice, multi-input multi-output (MIMO) setups reduce the time required to scan the specimen surface, but demand high pulse discriminability. By applying envelope removal techniques to the individual pulses, the pulse discriminability is increased allowing only the remaining phase information to be targeted for analysis. Finally, semi-synthetic experiments are presented to verify the applicability of the envelope removal method and highlight the suitability of the fluidic transducer for MIMO setups. KW - Air-coupled ultrasound KW - Fluidics KW - Signal processing KW - Pulse compression KW - MIMO KW - Hilbert transform PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537853 DO - https://doi.org/10.1016/j.ultras.2021.106612 SN - 0041-624X VL - 119 SP - 1 EP - 12 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-53785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bühling, Benjamin A1 - Maack, Stefan A1 - Schönsee, Eric A1 - Schweitzer, Thorge A1 - Strangfeld, Christoph T1 - Acoustic and flow data of fluidic and piezoelectric ultrasonic transducers N2 - This data article presents characteristic acoustic and flow data of a fluidic ultrasonic transducer as well as acoustic data of a commercial piezoelectric ultrasonic transducer used in non-destructive testing for civil engineering. The flow data has been acquired using hot-wire anemometry and a Pitot tube. The three-dimensional acoustic data of both devices has been acquired using a calibrated microphone. The distribution of characteristic acoustic properties of both transducers are extracted and given in addition to the raw data. The data presented in the article will be a valuable source for reference and validation, both for developing fluidic and alternate ultrasound generation technologies. Furthermore, they will give additional insight into the acoustic-flow interaction phenomena of high speed switching devices. This article is accompanying the paper Experimental Analysis of the Acoustic Field of an Ultrasonic Pulse Induced by a Fluidic Switch (Bühling et al., 2021) published in The Journal of the Acoustical Society of America, where the data is interpreted in detail and the rationale for characteristic sound properties of the fluidic transducer are given. KW - Ultrasound KW - Non-destructive testing KW - Air-coupled ultrasound KW - Fluidics KW - Acoustic-flow interaction KW - Piezoelectric transducer PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531308 DO - https://doi.org/10.1016/j.dib.2021.107280 VL - 38 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-53130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Ultraschall-Echoverfahren an Betonbauteilen mit geneigten Rückwänden - Entwicklung von Testkörpern N2 - Mit dem Ultraschall-Echoverfahren können geometrische Abmessungen von Betonbauteilen bestimmt werden. Es hat sich gezeigt, dass die Bauteilrückwand bei der Messung an Massivbrücken häufig nicht planparallel zur Messfläche ausgeführt ist. Es wird erwartet, dass der Einfluss einer Neigung der Rückwand gegenüber der Messfläche auf die Messunsicherheit bei der Dickenbestimmung nicht vernachlässigbar ist. In diesem Beitrag werden die fünf konzipierten Betonprobekörper und ausgewählte Messergebnisse zur Bestimmung dieses Einflusses gezeigt. T2 - DACH-Jahrestagung 2019 - Zerstörungsfreie Materialprüfung CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Messunsicherheit KW - Ultraschall PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504317 AN - OPUS4-50431 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Wiehle, Philipp A1 - Munsch, Sarah Mandy T1 - About the dominance of mesopores in physisorption in amorphous materials N2 - Amorphous, porous materials represent by far the largest proportion of natural and men-made materials. Their pore networks consists of a wide range of pore sizes, including mesoand macropores. Within such a pore network, material moisture plays a crucial role in almost all transport processes. In the hygroscopic range, the pores are partially saturated and liquid water is only located at the pore fringe due to physisorption. Therefore, material parameters such as porosity or median pore diameter are inadequate to predict material moisture and moisture transport. To quantify the spatial distribution of material moisture, Hillerborg’s adsorption Theory is used to predict the water layer thickness for different pore geometries. This is done for all pore sizes, including those in the lower nanometre range. Based on this approach, it is shown that the material moisture is almost completely located in mesopores, although the pore network is highly dominated by macropores. Thus, mesopores are mainly responsible for the moisture storage capacity, while macropores determine the moisture transport capacity, of an amorphous material. Finally, an electrical analogical circuit is used as a model to predict the diffusion coefficient based on the pore-size distribution, including physisorption. KW - Physisorption KW - Mesopores KW - Amorphous materials KW - Macropores KW - Adsorbed water layer thickness KW - Material moisture KW - Moisture distribution PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538525 UR - https://dataverse.harvard.edu/dataset.xhtml?persistentId=doi:10.7910/DVN/NILGW2 DO - https://doi.org/10.3390/molecules26237190 VL - 26 IS - 23 SP - 1 EP - 22 PB - MDPI AN - OPUS4-53852 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bühling, Benjamin A1 - Küttenbaum, Stefan A1 - Maack, Stefan A1 - Strangfeld, Christoph T1 - Development of an Accurate and Robust Air-Coupled Ultrasonic Time-of-Flight Measurement Technique N2 - Ultrasonic time-of-flight (ToF) measurements enable the non-destructive characterization of material parameters as well as the reconstruction of scatterers inside a specimen. The time-consuming and potentially damaging procedure of applying a liquid couplant between specimen and transducer can be avoided by using air-coupled ultrasound. However, to obtain accurate ToF results, the waveform and travel time of the acoustic signal through the air, which are influenced by the ambient conditions, need to be considered. The placement of microphones as signal receivers is restricted to locations where they do not affect the sound field. This study presents a novel method for in-air ranging and ToF determination that is non-invasive and robust to changing ambient conditions or waveform variations. The in-air travel time was determined by utilizing the azimuthal directivity of a laser Doppler vibrometer operated in refracto-vibrometry (RV) mode. The time of entry of the acoustic signal was determined using the autocorrelation of the RV signal. The same signal was further used as a reference for determining the ToF through the specimen in transmission mode via cross-correlation. The derived signal processing procedure was verified in experiments on a polyamide specimen. Here, a ranging accuracy of <0.1 mm and a transmission ToF accuracy of 0.3μs were achieved. Thus, the proposed method enables fast and accurate non-invasive ToF measurements that do not require knowledge about transducer characteristics or ambient conditions. KW - Air-coupled ultrasound KW - Laser Doppler vibrometer KW - Refracto-vibrometry KW - Acousto-optic effect KW - Time-of-flight measurements KW - In-air ranging KW - Non-destructive testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544711 DO - https://doi.org/10.3390/s22062135 VL - 22 IS - 6 SP - 1 EP - 17 PB - MDPI CY - Basel, Switzerland AN - OPUS4-54471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bühling, Benjamin A1 - Maack, Stefan A1 - Strangfeld, Christoph T1 - OsciCheck - A Novel Fluidic Transducer for Air-Coupled Ultrasonic Measurements N2 - Ultrasonic measurement technology has become indispensable in NDT-CE. Air-coupled ultrasonic (ACU) measurement techniques promise to reduce measurement time. However, the signal quality suffers from large specific impedance mismatch at the transducer-air and air-specimen interface. Additionally, large pressure amplitudes are necessary for the penetration depth required in NDT-CE applications. To address the specific requirements of ultrasonic testing in NDT-CE, a robust ACU transducer was developed, that generates ultrasound by quickly switching a pressurized air flow. The simple design of the fluidic transducer makes the device maintenance free and resilient against harsh environmental conditions. Since the signal is generated by aeroacoustics, there is no specific impedance mismatch between the transducer and the surrounding air. The ultrasonic signal exhibits frequencies in the 30-60 kHz range and is therefore well suited to penetrate heterogenous materials such as concrete. This contribution gives an introduction in the working principle and signal characteristics of the fluidic transducer. Its applicability to measurements in concrete is verified. A detailed outlook is given to discuss the future potential of fluidic ultrasonic actuators. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Air-coupled ultrasound KW - Nondestructive testing KW - Fluidics KW - Bistable amplifier KW - Aeroacoustics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555271 UR - https://www.ndt.net/search/docs.php3?id=27319 VL - 2022/09 SP - 1 EP - 9 PB - NDT.net CY - Bad Breisig AN - OPUS4-55527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy T1 - Ermittlung der Oberflächenrelaxivität in Sandsteinen - ein Methodenvergleich N2 - Mit dem zerstörungsfreien Verfahren der nuklear magnetischen Resonanz (NMR) mit Fokus auf 1H-Protonen lässt sich der Feuchtegehalt in porösen Materialien bestimmen und bei einem vollgesättigten Medium eine Porengrößenverteilung ableiten. Für die Ermittlung der Porengrößenverteilung muss die gemessene T2-Relaxationszeitenverteilung mit dem Parameter Oberflächenrelaxivität (OR) umgerechnet werden. Ist dieser Parameter für das zu untersuchende Medium unbekannt, kann dieser mithilfe von Vergleichsverfahren abgeschätzt werden. Dabei kommen z. B. Gassorption, Quecksilberporosimetrie (MIP), Dünnschliff-Mikroskopie oder µ-Computer-Tomographie (µ-CT) zum Einsatz. Da die verschiedenen Verfahren allerdings unterschiedliche Auflösungsgrenzen aufweisen und auf verschiedenen physikalischen Prinzipien beruhen, können die ermittelten ORs für ein Medium stark variieren. Um ein besseres Verständnis für die OR und die Einflüsse der Vergleichsverfahren zu bekommen, wurden 19 verschiedene Sandsteintypen untersucht. Die OR wurde zum einen basierend auf der spezifischen inneren Oberfläche aus der dynamischen Dampfsorption (DVS) und der Gassorption abgeleitet. Zum anderen wurden die Relaxationszeitenverteilungen durch manuelles Anpassen der OR derart in Porengrößenverteilungen umgerechnet, sodass es eine Übereinstimmung mit den Porengrößenverteilungen aus MIP und/oder µ-CT gibt. Die Umrechnung von Relaxationszeitverteilungen in eine Porengrößenverteilung berücksichtigt dabei sowohl fast- als auch slow-diffusion. Insgesamt ergab sich für die Sandsteine ein breites Spektrum an ORs, bei dem die über die innere spezifische Oberfläche ermittelten ORs andere Größenordnungen aufwiesen (< 10 µm/s), als bei dem Vergleich mit MIP oder µ-CT (bis 600 µm/s). Die mit MIP und µ-CT ermittelten Werten lagen dabei um einen Faktor von 1 bis 30 auseinander. Dieser umfangreiche Datensatz, der vier verschiedene Vergleichsverfahren einbezieht, soll neue Erkenntnisse in der Charakterisierung von porösen Materialien (z. B. bezüglich der Oberflächenrauigkeit) und in der Ursache für die starke Variation der OR ermöglichen. Durch das Berücksichtigen von fast- als auch slow-diffusion, können dabei sogar Daten in eine Porengrößenverteilung umgerechnet werden, bei denen das fast-diffusion-Kriterium nach Brownstein und Tarr nicht erfüllt ist. Außerdem ergibt sich aus der Berücksichtigung des slow-diffusion-Regimes ein neues Verständnis für die obere Auflösungsgrenze von NMR. T2 - 82. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Online meeting DA - 07.03.2022 KW - NMR KW - Sandsteine KW - Oberflächenrelaxivität KW - Porengrößenverteilung PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544721 UR - https://e-docs.geo-leo.de/handle/11858/9672 DO - https://doi.org/10.23689/fidgeo-5330 AN - OPUS4-54472 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph T1 - Quantification of the Knudsen Effect on the Effective Gas diffusion Coefficient in Partially Saturated Pore Distributions N2 - The effective gas diffusion coefficient describes the process of gas diffusion in porous materials. Several materials have a significant number of micropores in the lower nanometre range leading to a reduction of gas diffusion (Knudsen effect). In the case of partial pore saturation during adsorption, the available pore space is further reduced, as is the gas diffusion. In this study, the influence of partially saturated pores on the Knudsen effect and on the gas diffusion is quantified. Three different pore geometries are investigated (slit, cylindrical and spherical pores) and three different types of pore size distribution, including a broad equal distribution, three narrow normal distributions and two measured distributions of concrete. Besides the intensive computation of the exact pore saturation, a simplified model with low computational requirements is suggested. This study shows that the influence of the water layer thickness on the effective diffusion becomes significant for pore radii below 50 nm and the assumed pore geometry is important. At the end, the overall effect is quantified for an amorphous material with most pore radii below 30 nm. At a moisture level of 50% relative humidity, the effective diffusion is reduced by 35% due to partial saturation. KW - Effective gas diffusion coefficient KW - Gas transport in porous media KW - Knudsen diffusion KW - Moisture transport KW - Nanopores PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528509 DO - https://doi.org/10.1002/adem.202100106 VL - 23 IS - 10 SP - 2100106 PB - Wiley AN - OPUS4-52850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munsch, Sarah Mandy A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine T1 - Application of 1H proton NMR relaxometry to building materials - A review N2 - Since nuclear magnetic resonance with focus on 1H protons is highly sensitive to pore filling fluids, it is nowadays often applied for the investigation of porous media. Mainly in materials research and especially in the field of non-destructive testing in civil engineering it is increasingly used. Scientific questions about and based on NMR meanwhile cover a broad spectrum. To give an overview, we have reviewed various studies dealing with the determination of moisture contents and parameters such as the pore-size distribution, surface relaxivity, porosity, etc. In some papers, the monitoring of moisture transport in connection with degradation processes or admixtures was the main objective. In other papers, NMR was used for pore space analysis or even applied on site to assess the state of conservation of cultural heritage. Building materials that have been investigated in the presented studies are for example cement, concrete, woods, sandstones etc. In this paper, short descriptions and the significant results of the reviewed articles are summarized and their measurement problems and discrepancies are pointed out. A special feature of this review article is the concise tabular compilation of determined 𝑇1 and 𝑇2 relaxation times, as well as of surface relaxivity values for various materials and components. Finally, relevant aspects are summed up and conclusions about the increasing potential of NMR relaxometry for investigations of porous building materials are drawn, followed by an outlook about future applications and the need for technical development. KW - NMR relaxometry KW - Building materials KW - Natural stones KW - Relaxation times KW - Surface relaxivities KW - Moisture KW - Pore space characterization PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521888 DO - https://doi.org/10.1016/j.jmro.2021.100012 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. VL - 6-7 SP - 100012 PB - Elsevier Inc. CY - Amsterdam AN - OPUS4-52188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Küttenbaum, Stefan A1 - Maack, Stefan A1 - Braml, T. A1 - Taffe, A. A1 - Strübing, T. T1 - Bewertung von Bestandsbauwerken mit gemessenen Daten - Teil 2: Berechnung der Tragwerkszuverlässigkeit unter Einbeziehung der ZfP-Messergebnisse T1 - Reassessment of existing structures based on measured data - Part 2: Structural reliability analyses using NDT results N2 - Durch die Einbeziehung von gemessenen Daten bei der Bewertung von bestehenden Bauwerken können Unsicherheiten bei der Beurteilung des Tragverhaltens reduziert werden, ohne das normative Zuverlässigkeitsniveau einzuschränken. Informationen sind die wesentliche Grundlage für die Analyse der Zuverlässigkeit von Tragwerken. Umso wichtiger ist die Kenntnis über die Präzision und die Richtigkeit der verwendeten Informationen. Aus messtechnischer Sicht kann ein Messwert, dem keine Messunsicherheit beigeordnet wurde, als wertlos erachtet werden. Liegt ein vollständig dokumentiertes Messergebnis vor, so ist die Qualität der gemessenen Information bekannt und deren Vergleichbarkeit gewährleistet. In diesem Beitrag wird am Beispiel einer Spannbetonbrücke und zweier Grenzzustände gezeigt, wie Messergebnisse aus der zerstörungsfreien Prüfung in probabilistische Nachweise von Bestandsbauwerken einfließen können und welche Auswirkungen die Implementierung von gemessenen Daten bei der Bewertung von Bestandsbauwerken haben kann. N2 - Every decision about the reliability of a structure is associated with uncertainties. The reassessment of existing structures remains a major challenge. The decisive difference compared to the design of new structures is the possibility and necessity to collect individual information about the actual condition and properties of the structure. Such knowledge should be appreciated in the reassessment in order to reduce uncertainties and increase the validity of the results. Reliability analyses using measured data require the comparability of measurement results and the evaluation of the quality of the measured information. Both requirements can be met by adequate measurement uncertainty considerations. Besides, the destructive interventions necessary for the measurements should be kept to a minimum. This paper shows how non-destructively gathered measurement results can be incorporated into probabilistic reassessments and which effects the implementation of measured data can have when evaluating existing structures, using a prestressed concrete bridge as a case-study. KW - Nachrechnung KW - Zerstörungsfreie Prüfung KW - Zuverlässigkeitsanalyse KW - Messung KW - Spannbetonbrücke PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519480 DO - https://doi.org/10.1002/best.202000087 SN - 0005-9900 SN - 1437-1006 VL - 116 IS - 3 SP - 183 EP - 199 PB - Ernst & Sohn CY - Berlin AN - OPUS4-51948 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Epple, Niklas A1 - Aligholizadeh, M. T1 - Die Ultraschall-Echomethode – von der Messung zur bautechnischen Kenngröße T1 - Ultrasonic Echo Method - Deriving structural parameters from measured values N2 - Zerstörungsfreie Prüfverfahren liefern wichtige Informationen zur Beurteilung von Bauwerken. Mit ihnen können Materialeigenschaften bestimmt oder die innere Struktur von Bauteilen beschrieben werden. Für letzteres werden in der Regel Volumenverfahren angewandt. Einen besonderen Stellenwert haben in der Praxis die Radar- und die Ultraschall-Echoverfahren. Ihre Anwendung erfordert lediglich eine einseitige Zugänglichkeit zum Bauteil. Zudem lassen sich zahlreiche unterschiedliche Prüfaufgaben lösen. Zum Stand der Technik gehören beispielsweise die Ortung von Bewehrung und Spannkanälen, die Bestimmung der Dicke von Bauteilen oder die Fehlerlokalisierung. In diesem Beitrag wird gezeigt, wie mithilfe von Ultraschall-Echomessungen gesammelte Messwerte in ein quantitatives Messergebnis überführt werden können, das wiederum in ingenieurtechnische Berechnungen einfließen kann. Einleitend werden die Prüfmethode und die Messtechnik erläutert. Anschließend wird das Vorgehen von der Auswertung der Messergebnisse bis zur Bestimmung der bautechnischen Kenngröße – Bauteildicke – gezeigt. Abschließend wird die Methodik an einem Referenzprüfkörper aus Polyamid demonstriert und den Ergebnissen von Messungen an Beton gegenübergestellt. KW - Zerstörungsfreie Prüfung KW - Ultraschall-Echoverfahren KW - Messunsicherheit KW - Bildgebende Darstellung KW - Schallgeschwindigkeit PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521113 DO - https://doi.org/10.1002/best.202000091 VL - 116 IS - 3 SP - 200 EP - 211 PB - Ernst & Sohn AN - OPUS4-52111 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bühling, Benjamin A1 - Strangfeld, Christoph A1 - Maack, Stefan A1 - Schweitzer, T. T1 - Experimental analysis of the acoustic field of an ultrasonic pulse induced by a fluidic switch N2 - Ultrasonic inspection is a common tool for non-destructive testing in civil engineering (NDT-CE). Currently, transducers are coupled directly to the specimen surface, which makes the inspection time-consuming. Air-coupled ultrasound (ACU) transducers are more time-efficient but need a high pressure amplitude as the impedance mismatch between the air and the concrete is high and large penetration depth is needed for the inspection. Current approaches aim at eliminating the impedance mismatch between the transducer and the air to gain amplitude; however, they hardly fulfill the NDT-CE requirements. In this study, an alternative approach for ultrasound generation is presented: the signal is generated by a fluidic switch that rapidly injects a mass flow into the ambience. The acoustic field, the flow field, and their interaction are investigated. It is shown that the signal has dominant frequencies in the range of 35–60 kHz, and the amplitude is comparable to that of a commercial ACU transducer. KW - Air-coupled ultrasound KW - Non-destructive testing KW - Ultrasonic transducer KW - Acoustic-flow interaction PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523862 DO - https://doi.org/10.1121/10.0003937 VL - 149 IS - 4 SP - 2150 EP - 2158 AN - OPUS4-52386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy T1 - Möglichkeiten und Grenzen der zerstörungsfreien Erfassung niedriger Feuchtegehalte in teilgesättigten Sandsteinen mit 1H-NMR N2 - Die zerstörungsfreie Ermittlung der Materialfeuchte in Baustoffen ist für das Bauwesen von großer Bedeutung, denn ein erhöhter Feuchteeintrag kann zu Schimmelbildung, Alkali-Kieselsäure-Reaktionen, Korrosion etc. führen und somit ein hohes Schadenspotential mit sich bringen. Auch wenn zur qualitativen Lokalisierung möglicher Schad- und Risikostellen bereits zahlreiche zerstörungsfreie Verfahren in der Praxis Anwendung finden, besteht ein Mangel an quantitativen Verfahren, die auch bei niedrigen Feuchtegehalten sensitiv sind. Eine Methode zur zerstörungsfreien und quantitativen Bestimmung des Feuchtegehaltes und der effektiven Porosität ist die 1H-Kernspinresonzanzmethode (NMR). Da NMR sensitiv für die molekulare Beweglichkeit von Wasserstoffprotonen ist, lassen sich Informationen über die Bindungsform und -stärke sowie der Umgebung (Porengröße und Mineralzusammensetzung) der Wasserstoffprotonen gewinnen. Obwohl es bereits seit über 20 Jahren mobile NMR-Messeräte gibt, wird NMR heutzutage immer noch weitestgehend im Labor eingesetzt. Dies liegt daran, dass sie aufgrund der verwendeten Permanentmagnete schwer sind und nur äußerst geringe Eindringtiefen ermöglichen. In einer derzeit laufenden Forschungsarbeit wird deshalb ein speziell für Bohrkerne entworfener NMR-Tomograph eingesetzt. Mit seiner minimalen Echozeit von 50 µs lässt sich (abhängig von der Oberflächenrelaxivität) Wasser bis in nanometergroßen Poren erfassen. Um die Sensitivität von NMR bei Teilsättigung zu untersuchen, wurden verschiedene Sandsteinproben in Exsikkatoren mit relativen Luftfeuchten im Bereich von 33 % bis 96 % gelagert. Als Referenzen dienen zum einen das NMR-Signal bei Vollsättigung und zum anderen die Porengrößenverteilung aus Quecksilberporosimetriemessungen (MIP). Um die NMR-Sensitivität zu bewerten, wird die Korrelation der NMR-Amplitude mit den gravimetrisch ermittelten Feuchtegehalten sowie ein Vergleich der Porosität aus NMR und MIP betrachtet. Zu beachten ist in diesem Zusammenhang, dass sowohl die Reduzierung der Wasserfilmdicke als auch die Verkleinerung von Porengrößen zu einer ähnlichen Verkürzung der T2-Relaxationszeit führt. Als Ausblick wird ein Lösungsansatz vorgestellt, bei dem die NMR-Signale mit der Wasserfilmdickenberechnung basierend auf der relativen Luftfeuchte im Material korreliert werden. T2 - 81. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Online meeting DA - 01.03.2021 KW - NMR KW - Sandsteine KW - Porosität KW - Oberflächenrelaxivität KW - Feuchtegehalt PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522271 DO - https://doi.org/10.23689/fidgeo-3957 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-52227 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kanzler, D. A1 - Schmitt, M. A1 - Maack, Stefan A1 - Baensch, F. T1 - Erarbeitung einer Norm für einen standardisierten Prozess zur probabilistischen Bewertung von Prüfverfahren N2 - Im DIN-Normenausschuss Materialprüfung (NMP) wurde das Normungsgremium NA 062-08-28 AA „Qualifizierung von zerstörungsfreien Prüfungen“ reaktiviert. Das Ziel der Reaktivierung ist die Erarbeitung einer Norm für einen standardisierten Prozess zur probabilistischen Bewertung von Prüfverfahren. In der zerstörungsfreien Prüfung (ZfP) führt die Ermittlung von Mess- / Prüfunsicherheiten von Prüfverfahren, in normativer Hinsicht in Deutschland und Europa, noch ein Schattendasein. Die Norm ISO IEC 17025 und auch der VDA-Band 5 wurden weiter in Richtung Messunsicherheit entwickelt, allerdings führt ihre Anwendung in der ZfP zu Problemen. Der Arbeitsausschuss NA 062-08-28 AA soll hier den Brückenschlag zwischen Messunsicherheit, objektiver statistischer Bewertung für ZfP-Verfahren und eine weitere Stärkung der probabilistischen Bruchmechanik erreichen. Geplant ist daher die Erarbeitung einer DIN-Norm, welche die Kriterien für eine korrekte Versuchsplanung, ein praktikables Vorgehen zur Bewertung der Prüfergebnisse und die mathematische Überführung in eine Zuverlässigkeitsaussage enthält. Es soll ein Leitfaden erstellt werden, der für ein möglichst breites Branchenspektrum eingesetzt werden kann, unabhängig von den Besonderheiten verschiedener Industriezweige. Dargestellt werden das relevante Normungsgremium sowie der Hintergrund des zu erstellenden Dokuments. T2 - DGZfP Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Validation KW - Probabilistischen Bewertung KW - Zerstörungsfreie Prüfverfahren KW - POD PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584176 UR - https://www.ndt.net/search/docs.php3?id=28574 SN - 978-3-947971-29-9 SP - 1 EP - 8 PB - NDT.net AN - OPUS4-58417 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Singh, Chandan A1 - Thiele, M. A1 - Dathe, A. A1 - Thamm, S. A1 - Henkel, T. A1 - Sumana, G. A1 - Fritzsche, W. A1 - Czáki, A. T1 - Tri-sodium citrate stabilized gold nanocubes for plasmonic glucose sensing N2 - We report a two-step process for the immobilization of gold nanocubes (Au-NCs) on a glass surface using a combination of extraction and exchange reaction using poly (sodium 4-styrenesulfonate) (PSS) and trisodium citrate (TSC). Cetyltrimethylammonium chloride (CTAC) stabilized gold nanocubes (CTAC/Au-NCs) synthesized by a microfluidic synthesis procedure were successfully deposited on silane-modified glass substrate after extraction of excess CTAC using chloroform followed by exchange of CTAC to TSC on the surface of Au-NCs. Further, TSC/Au-NCs were found to be highly stable and suitable for microfluidic sensing of different glucose concentrations using localized surface plasmon resonance (LSPR) spectroscopy offering an improved sensitivity (126.37 nm/RIU). KW - Gold nanocubes KW - Surfactant KW - Immobilization PY - 2021 DO - https://doi.org/10.1016/j.matlet.2021.130655 SN - 0167-577X SN - 1873-4979 VL - 304 SP - 1 EP - 4 PB - Elsevier CY - New York, NY AN - OPUS4-53216 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Küttenbaum, Stefan A1 - Braml, T. A1 - Heinze, M. A1 - Kainz, C. A1 - Keuser, M. A1 - Kotz, P. A1 - Lechner, T. A1 - Maack, Stefan A1 - Reinke, K.-D. A1 - Schulze, S. A1 - Soukup, A. A1 - Stettner, C. A1 - Taffe, A. A1 - Wöstmann, Jens T1 - Guideline on NDT-supported reliability assessment of existing structures - Current developments in Germany N2 - Information about an existing structure can be collected at certain costs to evaluate the reliability and condition as realistically as necessary. This information can be relevant or irrelevant, true or biased, precise or imprecise. The incorporation of relevant and quality-assessed measured information into reliability reassessment offers the chance to extend remaining lifetimes and support decision making about optimal actions or maintenance strategies. This paper shows recent developments in a national research project that aims to produce a guideline on the NDT-based, structure-specific modification of partial safety factors. The general methodology, results from recalculations according to the Eurocodes and metrologically solvable testing tasks relevant in the recalculation of the concrete bridges are shown and compared with the non-destructive testing methods applicable to concrete bridges. A case study is used to demonstrate that as-built drawings, in this case of the positions of tendons and shear reinforcement, can be verified using the radar method. KW - Non-destructive testing KW - Concrete bridges KW - Partial safety factor modification PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-584862 DO - https://doi.org/10.1002/cepa.2168 SN - 2509-7075 VL - 6 IS - 5 SP - 537 EP - 543 PB - Ernst & Sohn CY - Berlin AN - OPUS4-58486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan A1 - Braml, T. A1 - Taffe, A. A1 - Maack, Stefan ED - Li, J. ED - Spanos, D. ED - Chen, J. B. ED - Peng, Y. B. T1 - Towards NDT-supported decisions on the reliability of existing bridges N2 - A major advantage in the reassessment of existing structures is the possibility of including measured data that describe the actual properties and the current condition of the structure to be reassessed. Currently, the incorporation of such measured information is mostly unregulated. However, the use of measurement results is vitally important, since a measured data-based improvement of the computation models level of approximation can lead at least to more meaningful results, possibly to extended remaining life times of the structure and in the best case to a saving of resources. Conversely, not appreciating well measurable and relevant information can be equated with a waste of resources. In this paper, a concept for the comparable use of non-destructively measured data as basic variables in probabilistic reliability assessments is outlined and examined using a typical prestressed concrete road bridge as a case-study. An essential requirement is the calculation of measurement uncertainties in order to evaluate the quality of the measurement results comparably. In conclusion, the example of ultrasonic and radar measurement data is used to demonstrate the effects that the incorporation of the measured information has on the reliability of the structure. T2 - 13th International Conference on Structural Safety and Reliability (ICOSSAR 2021-2022) CY - Online meeting DA - 13.09.2022 KW - Measurement uncertainty KW - Reliability assessment KW - Existing structures KW - Concrete Bridge KW - Non-Destructive Testing (NDT) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583013 SP - 1 EP - 10 AN - OPUS4-58301 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy A1 - Bintz, Thilo A1 - Heyn, R. A1 - Hirsch, H. A1 - Grunewald, J. A1 - Kruschwitz, Sabine T1 - Detailed investigation of capillary active insulation materials by 1H nuclear magnetic resonance (NMR) and thermogravimetric drying N2 - Capillary active interior insulation materials are an important approach to minimize energy losses of historical buildings. A key factor for their performance is a high liquid conductivity, which enables redistribution of liquid moisture within the material. We set up an experiment to investigate the development of moisture profiles within two different interior insulation materials, calcium-silicate (CaSi) and expanded perlite (EP), under constant boundary conditions. The moisture profiles were determined by two different methods: simple destructive sample slicing with subsequent thermogravimetric drying as well as non-destructive NMR measurements with high spatial resolution. The moisture profiles obtained from both methods show good agreement, when compared at the low spatial resolution of sample slicing, which demonstrates the reliability of this method. Moreover, the measured T2-relaxation-time distributions across the sample depth were measured, which may give further insight into the saturation degree of the different pore sizes. In order to explain differences in the moisture profiles between CaSi and EP, we determined their pore-size distribution with different methods: conversion of the NMR T2 relaxationtime distribution at full saturation, mercury intrusion porosimetry and indirect determination from pressure plate measurements. CaSi shows a unimodal distribution at small pore diameters, while in EP, a bi-modal or wider distribution was found. We assume that the smaller pore diameters of CaSi lead to a higher capillary conductivity, which causes a more distributed moisture profile in comparison with that of EP. T2 - NDT-CE CY - Zurich, Switzerland DA - 16.08.2022 KW - Insulation material KW - Nuclear magnetic resonance KW - Capillary conductivity KW - Pore-size distribution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579172 DO - https://doi.org/10.58286/27205 SN - 1435-4934 VL - 27 IS - 9 SP - 1 EP - 11 AN - OPUS4-57917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan A1 - Taffe, A. A1 - Braml, T. A1 - Maack, Stefan ED - Alexander, M. G. ED - Beushausen, H. ED - Dehn, F. ED - Moyo, P. T1 - Reliability assessment of existing bridge constructions based on results of non-destructive testing N2 - The non-destructive testing methods available for civil engineering (NDT-CE) enable the measurements of quantitative parameters, which realistically describe the characteristics of existing buildings. In the past, methods for quality evaluation and concepts for validation expanded into NDT-CE to improve the objectivity of measured data. Thereby, a metrological foundation was developed to collect statistically sound and structurally relevant information about the inner construction of structures without destructive interventions. More recently, the demand for recalculations of structural safety was identified. This paper summarizes a basic research study on structural analyses of bridges in combination with NDT. The aim is to use measurement data of nondestructive testing methods as stochastic quantities in static calculations. Therefore, a methodical interface between the guide to the expression of uncertainty in measurement and probabilistic approximation procedures (e.g. FORM) has been proven to be suitable. The motivation is to relate the scientific approach of the structural analysis with real information coming from existing structures and not with those found in the literature. A case study about the probabilistic bending proof of a reinforced concrete bridge with statistically verified data from ultrasonic measurements shows that the measuring results fulfil the requirements concerning precision, trueness, objectivity and reliability. T2 - International Conference on Concrete Repair, Rehabilitation and Retrofitting (ICCRRR 2018) CY - Cape Town, South Africa DA - 19.11.2018 KW - NDT KW - Concrete KW - Probabilistic reassessment KW - Bridge PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-467898 DO - https://doi.org/10.1051/matecconf/201819906001 SN - 2261-236X VL - 199 SP - 06001, 1 EP - 9 PB - MATEC Web of Conferences AN - OPUS4-46789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan A1 - Villalobos, S. A1 - Scott, D. T1 - Validation of artificial defects for non-destructive testing measurements on a reference structure N2 - Non-destructive testing was established over the last decades as an important tool for assessing damages, material characterization and quality assurance in civil engineering. For example, Ground Penetrating Radar (GPR) can be used to scan large areas of concrete structures to determine the spatial position of the reinforcement. With the ultrasonic echo method, the thickness of concrete structures can be easily determined even if a high density of reinforcement is given. Various methods and processes have been developed for the validation of NDT procedures aiming at ensuring the quality of measurements in practical use. The Probability of Detection (POD) for example, is an available method to compare different technical devices with each other quantitatively regarding their performance. With this method, the best suited testing device for a specific inspection task under defined boundary conditions can be selected. By using the Guide to the Expression of Uncertainty in Measurement (GUM), it is possible to quantify the measurement uncertainty of an inspection procedure for a specific task. Another important aspect to improve the acceptance of Non-destructive testing methods is the development of reference specimens. Reference specimens serve for the calibration and further development of NDT methods under realistic conditions in different laboratories under the same conditions. A particular challenge here is the most realistic representation of a damage that can occur at building sites. Possible damages include for example horizontal and vertical cracks or honeycombs in concrete. Such a reference structure was built for the development of a new design of power plant constructions. Comparative studies on the manufacturing of realistic honeycombs and delaminations were carried out in advance on a test specimen. The results of this study are presented here. T2 - ICCRRR 2018 - Concrete Repair, Rehabilitation and Retrofitting CY - Cape Town, South Africa DA - 19.11.2018 KW - Zerstörungsfreie Prüfung KW - Nondestructive testing KW - Istzustandserfassung KW - Ultrasonic PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-464497 DO - https://doi.org/10.1051/matecconf/201819906006 SN - 2261-236X VL - 199 SP - 1 EP - 9 PB - EDP Sciences CY - Les Ulis AN - OPUS4-46449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weise, Frank T1 - Analyse des Tausalzeintrages in Fahrbahndeckenbetone im Kontext der Alkali-Kieselsäure-Reaktion N2 - In den letzten Jahren sind im deutschen Bundesautobahnnetz (BAB-Netz) vermehrt AKR-Schäden an Betonfahrbahndecken aufgetreten, die zum Teil zu einer Halbierung ihrer geplanten Nutzungsdauer von 30 Jahren führte. Ursächlich hierfür ist die Verwendung alkaliempfindlicher Gesteinskörnung, die bei gleichzeitiger Anwesenheit von Wasser infolge der Exposition der Fahrbahndecke und dem alkalischen Milieu durch den Einsatz alkalireicher Portlandzemente bei der Betonherstellung zu einer Alkali-Kieselsäure-Reaktion (AKR) führt. Zusätzlich wird der AKR-Schädigungsprozess in Betonfahrbahndecken durch den externen Tausalzeintrag (primär NaCl) im Winter begünstigt. Vor diesem Hintergrund kommt der Ermittlung des Tausalzeintrags in den Fahrbahndeckenbeton eine große Bedeutung zu. Die Analyse des Tausalzeintrags erfolgte bisher ausschließlich nasschemisch an gemahlenen Bohrkernsegmenten. Nachteilig ist hierbei die fehlende differenzierte Betrachtung des Natriumgehaltes im Zementstein und in der Gesteinskörnung. Der alternative Einsatz von LIBS (Laser-induced breakdown spectroscopy) eröffnet in diesem Kontext neue Möglichkeiten. So wird in diesem Beitrag an Hand von Bohrkernen aus einem AKR-geschädigten BAB-Abschnitt exemplarisch die Vorgehensweise bei der LIBS-Analyse zur Ermittlung der Na- und interagierenden Cl-Verteilung an vertikalen Schnittflächen des Bohrkerns aufgezeigt. Da der Tausalzeintrag primär über den Zementstein erfolgt, wurde der verfälschende Na-Grundgehalt der Gesteinskörnung mittels Zementsteinkriteriums (Nutzung unterschiedlichen Ca-Gehalts in Zementstein und Gesteinskörnung) eliminiert. Vergleichend durchgeführte Cl-Mappings mit Mikroröntgenfluoreszenzanalyse (MRFA) belegen die Güte der durchgeführten LIBS-Messungen. Aber auch bei der Verifizierung der Übertragbarkeit der Ergebnisse der zum Ausschluss reaktiver Gesteinskörnung bei Neubau und Erneuerung im BAB-Netz eingesetzten Performanceprüfungen mit externem Alkalieintrag auf Praxisverhältnisse hat sich das LIBSVerfahren bewährt. So wurde festgestellt, dass die mit NaCl-Lösung beaufschlagten Laborprüfkörper aus einem repräsentativen Fahrbahndeckenbeton bei der Klimawechsellagerung (KWL) über ihre gesamte Höhe von 10 cm einen Eintrag von Na und Cl erfahren. Weiterhin konnte im Gegensatz zu bisherigen Annahmen erstmals mit LIBS und Nasschemie gezeigt werden, dass die Frost-Tauwechsel-Phase bei der KWL zu keinem erhöhten Tausalzeintrag führt. T2 - Fachtagung Bauwerksdiagnose 2018 CY - Berlin, Germany DA - 15.02.2018 KW - Baustoffe KW - Betonfahrbahndecken KW - AKR KW - Tausalzeintrag KW - LIBS KW - MRFA KW - Nasschemie KW - Klimawechsellagerung PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-446499 AN - OPUS4-44649 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy T1 - Determining the pore size distribution in synthetic and building materials using 1D NMR N2 - The detection of moisture in building materials has a high priority in civil engineering to locate and prevent possible moisture damages, e.g. mold, corrosion, delamination etc. Furthermore, it is of great significancy to achieve a better understanding of moisture transport and pore space in different materials. To prevent the degeneration of structures and materials, non-destructive testing methods are more and more deployed. As a non-destructive method in this work, nuclear magnetic resonance (NMR) is applied using a strayfield open magnet device that enables one-dimensional measurements in a defined volumen. By using NMR, the water content of the sample can be determined and also the pore size distribution can be deduced from the relaxation time distribution when having a comparison method like mercury intrusion porosimetry. In this study different synthetic homogenous materials with defined and almost unimodal pore size distributions are investigated as well as building materials like screed. For analyzing the pore space, the samples were measured at different saturation levels and the building materials at different hydration states as well. T2 - Magnetic Resonance in Porous Media 14 CY - Gainesville, FL, USA DA - 18.02.2018 KW - Pore size KW - Synthetic and building materials KW - NMR relaxometry KW - Mercury intrusion porosimetry PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-443868 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-44386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oesch, Tyler A1 - Weise, Frank A1 - Meinel, Dietmar A1 - Gollwitzer, Christian T1 - Quantitative in-situ analysis of water transport in concrete completed using X-ray computed tomography N2 - This paper describes a novel methodology for quantitative in-situ moisture measurement without tracking agents using X-ray computed tomography (XCT). The high levels of grey-scale precision required for the measurement of moisture without tracking agents resulted in the need for an additional image calibration procedure to correct for water-related X-ray scattering and for equipment-variability related artefacts arising during in-situ testing. This calibration procedure was developed on the basis of existing principles of XCT image cor-rection. Resulting images of moisture distribution exhibit a high level of agreement with expected material behaviour. This research demonstrated that XCT can be successfully used to measure both moisture-front movement over time and changes in 3D moisture distribution within samples. This approach to moisture measurement lays the groundwork for the planned future investigation of the interaction between cracking induced by varying chemical and mechanical processes and water transport in concrete. KW - X-ray computed tomography (XCT) KW - In-situ testing KW - Water transport KW - Quantitative moisture measurement KW - Concrete PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474395 DO - https://doi.org/10.1007/s11242-018-1197-9 SN - 1573-1634 VL - 127 IS - 2 SP - 371 EP - 389 PB - Springer Netherlands AN - OPUS4-47439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munsch, Sarah Mandy A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine ED - Kärger, J. ED - Heitjans, P. T1 - Determining the pore size distribution in synthetic and building materials using 1D NMR N2 - NMR is gaining increasing interest in civil engineering applications for the use of microstructure characterization as e.g. pore size determination and monitoring of moisture transport in porous materials. In this study, the use of NMR as a tool for pore size characterization was investigated. For our study we used screed and synthetic materials at partial and full saturation. A successful determination could be achieved when having a reference or calibration method, although partly diffusion effects have been registered. Due to these diffusion effects, for the determination of pore size distributions of synthetic materials another NMR device was needed. Finally, the determination of the surface relaxivity of screed (50 μm/s) led to a higher value than first expected from literature. T2 - 14th International Bologna Conference on Magnetic Resonance in Porous Media CY - Gainesville, FL, USA DA - 18.02.2018 KW - NMR relaxometry KW - Pore size distribution KW - Building materials KW - Porous materials KW - Surface relaxivity PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483680 UR - https://diffusion.uni-leipzig.de/pdf/volume31/diff_fund_31(2019)02.pdf SN - 1862-4138 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. VL - 31 IS - 2 SP - 1 EP - 9 PB - University of Leipzig CY - Leipzig AN - OPUS4-48368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bühling, Benjamin A1 - Strangfeld, Christoph A1 - Maack, Stefan T1 - Entwicklung eines luftgekoppelten Ultraschall-Echo-Prüfverfahrens mittels fluidischer Anregung N2 - In vielen technischen Bereichen werden Ultraschallverfahren zur zer-störungsfreien Werkstoffprüfung eingesetzt. Dabei wird ein Schallpuls von einem Prüfkopf in ein Prüfobjekt eingebracht. Der Puls kann unter anderem durch Membra-nen oder Piezoelemente erzeugt werden und wird in der Regel durch direkten Kontakt oder über ein Koppelmittel an das Objekt übertragen. Luftgekoppelter Ultraschall spielt in kommerziellen Anwendungen bisher eine untergeordnete Rolle, da die Dif-ferenz der akustischen Impedanzen von Luft und Festkörpern immense Verluste beim Übergang des Schallsignals hervorruft. In diesem Beitrag soll ein neuartiges Anregungsprinzip vorgestellt werden, mit dem ein Großteil dieser Verluste vermieden wird. Anstelle eines Festkörpers soll mit Hilfe einer fluidischen Düse Druckluft zur Signalerzeugung eingesetzt werden. In die-ser Düse wird eine selbsterhaltende Strömungsinstabilität erzeugt, die einen Schall-puls von bis zu 100 kHz hervorruft, sodass der Impedanzverlust in die Umgebungsluft entfällt. Da die charakteristische Frequenz eines fluidisch generierten Pulses maßgeb-lich von der Bauform der Düse und dem anliegenden Druck abhängt, lässt sich mittels einer geeigneten Strömungsregelung ein breiter Frequenzbereich zur Abtastung nut-zen. Die so emittierten Pulse werden auf das Prüfobjekt gerichtet und die reflektierten Signale mit einem Laservibrometer an der Oberfläche des Objekts im Echo-Verfahren abgetastet. Von drei signalmindernden Materialübergängen bei gewöhnlichem luftge-koppeltem Ultraschall bleibt in dem hier vorgeschlagenen Messystem lediglich die Grenzfläche von Luft zu Prüfkörper, sodass eine höhere Signalausbeute als bisher er-wartet werden kann. T2 - DACH-Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Ultraschall KW - Ultrasound KW - Air-coupled KW - Luftgekoppelt KW - Fluidic oscillator KW - Fluidischer Oszillator KW - Laser-Doppler-Vibrometer KW - Refraktovibrometrie KW - Refracto-vibrometry KW - NDT KW - ZfP PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481207 VL - 2019 SP - 1 EP - 8 PB - DGZfP Deutsche Gesellschaft für Zerstörungsfreie Prüfung AN - OPUS4-48120 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy T1 - Zerstörungsfreie Feuchtebestimmung und Porengrößenabschätzung an Estrichen mittels NMR N2 - Nuklear magnetische Resonanz (NMR) etabliert sich zunehmend im Bauingenieurwesen als eine alternative Methode zur zerstörungsfreien Feuchtebestimmung in Baustoffen. Schäden, die durch einen zu hohen Anteil an Flüssigwasser auftreten können, sind Ablösungen, Korrosion, Frostschäden, Induktion von Salzkristallisationen, etc. Aufgrund der Sensitivität für 1H-Protonen, ist NMR eine geeignete Methode zur Feuchtedetektion. Dabei kann laut Theorie zwischen frei, chemisch oder physikalisch gebundenem Wasser differenziert werden, während in der Praxis abhängig von der Messtechnik und Probengröße größtenteils nur das freie Wasser detektierbar ist. Mithilfe der NMR Relaxometrie lassen sich nicht nur Relaxationsabklingkurven ermitteln, sondern auch Relaxationszeitenverteilungen, sowie bei Vollsättigung ggf. eine Porengrößenverteilung ableiten. Darüber hinaus lassen sich erste Annahmen über die Entwicklung der Porensättigung bei Teilsättigung der Probe treffen. Ziel dieser Arbeit war die Untersuchung der zeitlichen Entwicklung der Porensättigung während des natürlichen Trocknungsprozesses (Teilsättigung) sowie die Ermittlung der Porengrößenverteilung an Beispiel von zementgebundenen Estrichen. Für den Versuch wurden zwei zementgebundene Estrichproben nach abgeschlossener Hydratation wieder aufgesättigt. Während des anschließenden natürlichen Trocknungsprozesses wurden regelmäßig NMR-Messungen durchgeführt sowie die Massenentwicklung observiert. Hauptfokus lag auf der zeitlichen und tiefenabhängigen Entwicklung der Relaxationszeitenverteilungen. Bei fortschreitender Trocknung der Proben konnte eine Verschiebung des Maximums der Relaxationszeitenverteilung zu kleineren Zeiten beobachtet werden. Die Ursache liegt zum einen in dem abnehmenden Anteil an freiem Wasser in größeren Poren und zum anderen in dem verhältnismäßig zunehmenden Signalanteil durch Wasser in kleineren Poren. Durch den Vergleich mit Quecksilberporosimetrie und Gas-Adsorptions-Ergebnissen, konnte aus den NMR-Daten eine unimodale Porengrößenverteilung mit einer dominanten Porengröße von 0,08 bis 0,1 µm und eine effektive Oberflächenrelaxivität von ca. 10 bis 30 µm/s abgeleitet werden. T2 - Bauwerksdiagnose 2018 CY - Berlin, Germany DA - 15.02.2018 KW - Estrich KW - Feuchte KW - NMR KW - Porengrößen KW - Relaxometrie PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-468966 UR - https://www.bauwerksdiagnose2018.de/Portals/bauwerksdiagnose2018/P/p11.pdf N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-46896 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Ermittlung des Flüssigwasseranteils an Kalziumsilikatplatten bei Teilsättigung mittels NMR N2 - Feuchte, insbesondere in Form von Flüssigwasser, stellt in Baustoffen ein hohes Schadenspotential dar. Um mit zerstörungsfreier Prüfung mögliche Risikostellen zu lokalisieren und Präventionsmaßnahmen zu ergreifen, sind Kenntnisse über das Porengefüge und Feuchtetransportmechanismen im Baustoff erforderlich. Eine wesentliche Problematik besteht derzeit in der Erfassung und Quantifizierung von Feuchteverteilungen bei Teilsättigung. Wir verfolgen derzeit einen Ansatz, mittels Nuklear Magnetischer Resonanz (NMR) in Korrelation mit relativen Luftfeuchtmessungen den Flüssigwasseranteil bei Teilsättigung zu ermitteln. Mit Protonen-NMR lassen sich Relaxationszeiten von Wasserstoffprotonen in Abhängigkeit von ihrer Bindungsart und ihrer Umgebung - z. B. Porenstruktur und -größe - erfassen. Allerdings lässt sich bei Materialien mit sehr breiten Porengrößenverteilungen nicht klar differenzieren, ob kurze Relaxationszeiten durch größere teilgesättigte oder kleinere vollgesättigte Poren verursacht werden. Für die Korrelation mit der relativen Luftfeuchte im Baustoff erfolgt zunächst eine künstliche Regulierung im Klimaschrank. Durch einen neuentwickelten Ansatz von Hillerborg lassen sich dann bei jeder Luftfeuchte die adsorbierten Wasserschichtdicken und der Porensättigungsgrad für die vorhandenen Porengrößen berechnen. Mithilfe des berechneten Porensättigungsgrades lässt sich eine genauere Analyse der zeitlichen Entwicklung von Relaxationszeitenverteilungen (insbesondere bei Trocknungs- und Aufsättigungsprozessen) vornehmen. Somit sollen erstmals Aussagen zu kürzeren Relaxationszeiten bei teilgesättigten Porensystemen, die beispielsweise auch eine multimodale Porengrößenverteilung aufweisen, getroffen werden können. In dieser Arbeit wird die Kombination aus NMR und der relativen Luftfeuchte an sehr porösen Dämmplatten aus Kalziumsilikat, die zur Wärmedämmung sowie der Entgegenwirkung von Schimmelbildung eingesetzt werden, angewendet. Untersucht werden 28 Proben à 6 Gruppen, die von unterschiedlichen Herstellern stammen bzw. unterschiedlich hergestellt wurden. T2 - DACH-Jahrestagung CY - Friedrichshafen, Germany DA - 27.05.2019 KW - NMR KW - Kalziumsilikat KW - Flüssigwasser KW - Hygrometrie PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481681 UR - http://www.ndt.net/?id=24594 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-48168 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bühling, Benjamin A1 - Maack, Stefan A1 - Strangfeld, Christoph T1 - Fluidic Ultrasound Generation for Non‐Destructive Testing N2 - AbstractAir‐coupled ultrasonic testing (ACU) is a pioneering technique in non‐destructive testing (NDT). While contact testing and fluid immersion testing are standard methods in many applications, the adoption of ACU is progressing slowly, especially in the low ultrasonic frequency range. A main reason for this development is the difficulty of generating high amplitude ultrasonic bursts with equipment that is robust enough to be applied outside a laboratory environment. This paper presents the fluidic ultrasonic transducer as a solution to this challenge. This novel aeroacoustic source uses the flow instability of a sonic jet in a bistable fluidic switch to generate ultrasonic bursts up to 60 kHz with a mean peak pressure of 320 Pa. The robust design allows operation in adverse environments, independent of the operating fluid. Non‐contact through‐transmission experiments are conducted on four materials and compared with the results of conventional transducers. For the first time, it is shown that the novel fluidic ultrasonic transducer provides a suitable acoustic signal for NDT tasks and has potential of furthering the implementation of ACU in industrial applications.This article is protected by copyright. All rights reserved KW - Aeroacoustics KW - Air-coupled ultrasound KW - Fluidics KW - Harsh environment KW - Laser Doppler vibrometer KW - Non-destructive testing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594273 DO - https://doi.org/10.1002/adma.202311724 SN - 0935-9648 SP - 1 EP - 14 PB - Wiley AN - OPUS4-59427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Johann, Sergej A1 - Strangfeld, Christoph A1 - Müller, Maximilian A1 - Mieller, Björn A1 - Bartholmai, Matthias T1 - RFID sensor systems embedded in concrete – validation experiments for long-term monitoring N2 - Structural Health Monitoring (SHM) is an important part of buildings surveillance and maintenance to detect material failure as early as possible and to contribute in protection of structures and their users. The implementation of Radio Frequency Identification (RFID) sensor systems without cable connection and battery into building components offers innovative possibilities to enable long-term in-situ SHM of addressed structures, bridges. The objectives of the presented study are complete embedding of RFID sensors systems in concrete, full passive communication with the systems, at best for the whole life span of structures. One challenge for this task is the highly alkaline environment in concrete, which requires non-degrading and robust encapsulation. Further Requirements are passive communication and energy supply, appropriate antenna design, placement and fixation in concrete, and the selection and implementation of sensors and connections. The concept is to develop and optimize a simple and robust system, which meets the requirements, as well as comprehensive validation in concrete specimen and real world applications. Two different systems were developed (HF and UHF RFID, respectively). First tasks were the implementation of analog sensors using the superposition principle for the signal adaption. Investigation of suitable materials for robust encapsulation and sensor protection against basic environments. Four materials were investigated in pH 13 solution for 14 days - 3D-Printer-Polymer was completely resolved - PVC has no noticeable decrease in weight - (VitaPro) glass filter for the sensor protector, has weight loss 2.7 % - The epoxy resin has increased by 1.8 % due to moisture expansion Different concrete samples were prepared for the validation of the systems. RFID sensors were embedded in different integration depths. Investigate the energy- and data transfer through concrete, also with varying moisture content. Additionally, signal strength data was used to optimize and validate the antenna characteristics in concrete. Next steps are to guarantee a sufficient energy supply for UHF RFID systems embedded in different concrete mixtures and further embedding the HF and UHF RFID systems in real bridges and buildings to validate the long term monitoring. T2 - DGZfP-Jahrestagung 2017 CY - Koblenz, Germany DA - 22.05.2017 KW - Smart structures KW - RFID sensors KW - Long-term requirements KW - Structural health monitoring KW - Passive RFID KW - Sensor requirements KW - Sensors in concrete PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-403496 UR - https://www.ndt.net/?id=21499 SN - 1435-4934 VL - 22 IS - 9 SP - 1 EP - 7 PB - NDT.net CY - Kirchwald AN - OPUS4-40349 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Johann, Sergej A1 - Strangfeld, Christoph A1 - Müller, Maximilian A1 - Mieller, Björn A1 - Bartholmai, Matthias T1 - RFID sensor systems embedded in concrete – Validation experiments for long-term monitoring T1 - RFID Sensorsysteme eingebettet in Beton – Validierungsexperimente zum Langzeitmonitoring N2 - Structural Health Monitoring (SHM) is an important part of buildings surveillance and maintenance to detect material failure as early as possible and to contribute in protection of structures and their users. The implementation of Radio Frequency Identification (RFID) sensor systems without cable connection and battery into building components offers innovative possibilities to enable long-term in-situ SHM of addressed structures, bridges. The objectives of the presented study are complete embedding of RFID sensors systems in concrete, full passive communication with the systems, at best for the whole life span of structures. One challenge for this task is the highly alkaline environment in concrete, which requires non-degrading and robust encapsulation. Further Requirements are passive communication and energy supply, appropriate antenna design, placement and fixation in concrete, and the selection and implementation of sensors and connections. The concept is to develop and optimize a simple and robust system, which meets the requirements, as well as comprehensive validation in concrete specimen and real world applications. Two different systems were developed (HF and UHF RFID, respectively). First tasks were the implementation of analog sensors using the superposition principle for the signal adaption. Investigation of suitable materials for robust encapsulation and sensor protection against basic environments. Four materials were investigated in pH13 solution for 14 days - 3D-Printer-Polymer was completely resolved - PVC has no noticeable decrease in weight - (VitaPro) glass filter for the sensor protector, has weight loss 2.7% - The epoxy resin has increased by 1.8% due to moisture expansion Different concrete samples were prepared for the validation of the systems. RFID sensors were embedded in different integration depths. Investigate the energy- and data transfer through concrete, also with varying moisture content. Additionally, signal strength data was used to optimize and validate the antenna characteristics in concrete. Next steps are to guarantee a sufficient energy supply for UHF RFID systems embedded in different concrete mixtures and further embedding the HF and UHF RFID systems in real bridges and buildings to validate the long term monitoring. KW - RFID sensors KW - Structural health monitoring KW - Sensors in concrete KW - Smart structures KW - Sensor requirements PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-418331 UR - http://www.ndt.net/?id=21499 SN - 1435-4934 VL - 22 IS - 9 SP - Artikel 8, 1 EP - 7 PB - NDT.net CY - Bad Breisig AN - OPUS4-41833 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine T1 - Monitoring of the absolute water content in porous materials based on embedded humidity sensors N2 - Moisture transport monitoring may indicate the onset of deterioration in porous building materials Prior to damage occurring. Most moisture measurement systems provide only qualitative values, require extensive calibration, or are destructive. Thus, non-destructive and calibration-free monitoring Systems are required. Our approach of moisture monitoring is to embed sensors that measure the relative humidity. In our experiment, screed samples are monitored during the Hydration and evaporation process. Every test sample is equipped with 10 embedded sensors which measure the relative humidity across the sample thickness. Based on Hillerborg’s approach, the relative humidity is converted into the corresponding pore saturation. In our study, the free water is computed without knowledge of the Sorption isotherm. The free water in the pore system is predicted and validated. The predicted weight decrease corresponds conclusively to gravimetrically measured weights. The embedded sensors yield the absolute liquid water content and enable an experimental, non-destructive monitoring of liquid water in porous materials. KW - Moisture measurements KW - Porous materials KW - Embedded sensors KW - Partial pore saturation KW - Sorption isotherm PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453476 DO - https://doi.org/10.1016/j.conbuildmat.2018.05.044 SN - 0950-0618 VL - 177 SP - 511 EP - 521 PB - Elsevier AN - OPUS4-45347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Johann, Sergej A1 - Bartholmai, Matthias T1 - Smart RFID Sensors Embedded in Building Structures for Early Damage Detection and Long-Term Monitoring N2 - In civil engineering, many structures are made of reinforced concrete. Most Degradation processes relevant to this material, e.g., corrosion, are related to an increased level of material moisture. Therefore, moisture monitoring in reinforced concrete is regarded as a crucial method for structural health monitoring. In this study, passive radio frequency identification (RFID)-based sensors are embedded into the concrete. They are well suited for long-term operation over decades and are well protected against harsh environmental conditions. The energy supply and the data transfer of the humidity sensors are provided by RFID. The sensor casing materials are optimised to withstand the high alkaline environment in concrete, having pH values of more than 12. Membrane materials are also investigated to identify materials capable of enabling water vapour transport from the porous cement matrix to the embedded humidity sensor. By measuring the corresponding relative humidity with embedded passive RFID-based sensors, the cement hydration is monitored for 170 days. Moreover, long-term moisture monitoring is performed for more than 1000 days. The Experiments show that embedded passive RFID-based sensors are highly suitable for long-term structural health monitoring in civil engineering. KW - RFID based sensors KW - Embedded sensors KW - Corresponding relative humidity KW - Porous building materials KW - Reinforced concrete KW - Corrosion KW - Civil engineering PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500831 DO - https://doi.org/10.3390/s19245514 VL - 19 IS - 24 SP - 1 EP - 18 PB - MDPI CY - Basel, Swiss AN - OPUS4-50083 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Schönsee, Eric A1 - Jeyifous, Olubunmi Anthony A1 - Mezhov, Alexander A1 - Hüsken, Götz T1 - Introduction of a monitoring system for Bingham fluids in additive manufacturing with concrete N2 - Freeform additive manufacturing of concrete structures is a rising technology in civil engineering with several fascinating advantages. Nonetheless, to ensure reliability and structural integrity, standards and quality control are required in the future to bring this technology into the market. As the concrete is manufactured continuously, continuous quality control of the printing process is also required, i.e. comprehensive process monitoring. At BAM, a test rig will be installed, enabling the printing of concrete structures with a maximum size of 2 m x 1 m x 1 m (l x w x h). Here, process monitoring is the focus of the test rig. In this study, we show the results of the first pump tests, including the measurement of several parameters such as temperature and pressure along the supply system, i.e. from the concrete pump to the printer head. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Additive manufacturing of concrete KW - Process monitoring KW - Non-destructive testing KW - Bingham fluid PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556367 SP - 1 EP - 12 AN - OPUS4-55636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klewe, Tim A1 - Strangfeld, Christoph A1 - Ritzer, Tobias A1 - Kruschwitz, Sabine T1 - Combining Signal Features of Ground-Penetrating Radar to Classify Moisture Damage in Layered Building Floors N2 - To date, the destructive extraction and analysis of drilling cores is the main possibility to obtain depth information about damaging water ingress in building floors. The time- and costintensive procedure constitutes an additional burden for building insurances that already list piped water damage as their largest item. With its high sensitivity for water, a ground-penetrating radar (GPR) could provide important support to approach this problem in a non-destructive way. In this research, we study the influence of moisture damage on GPR signals at different floor constructions. For this purpose, a modular specimen with interchangeable layers is developed to vary the screed and insulation material, as well as the respective layer thickness. The obtained data set is then used to investigate suitable signal features to classify three scenarios: dry, damaged insulation, and damaged screed. It was found that analyzing statistical distributions of A-scan features inside one B-scan allows for accurate classification on unknown floor constructions. Combining the features with multivariate data analysis and machine learning was the key to achieve satisfying results. The developed method provides a basis for upcoming validations on real damage cases. KW - Radar KW - Material Moisture KW - Non-destructive testing KW - Signal Features KW - Civil Engineering KW - Machine Learning PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533606 DO - https://doi.org/10.3390/app11198820 VL - 11 IS - 19 SP - 8820 PB - MDPI AN - OPUS4-53360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lu, Xin A1 - Hicke, Konstantin A1 - Breithaupt, Mathias A1 - Strangfeld, Christoph T1 - Distributed Humidity Sensing in Concrete Based on Polymer Optical Fiber N2 - We present a preliminary investigation on distributed humidity monitoring during the drying process of concrete based on an embedded polymer optical fiber (POF). The water dissipated into the POF changes several properties of the fiber such as refractive index, scattering coefficient and attenuation factor, which eventually alters the Rayleigh backscattered light. The optical time Domain reflectometer (OTDR) technique is performed to acquire the backscattered signal at the wavelengths 650 nm and 500 nm, respectively. Experimental results show that the received signal increases at 650 nm while the fiber attenuation factor clearly increases at 500 nm, as the concrete dries out. In the hygroscopic range, the information retrieved from the signal change at 650 nm agrees well with the measurement result of the electrical humidity sensors also embedded in the concrete sample. KW - Distributed fiber optic sensing KW - Distributed humidity sensing KW - Polymer optical fibers KW - Concrete drying KW - Material moisture KW - Embedded humidity sensors PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537644 DO - https://doi.org/10.3390/polym13213755 SN - 2073-4360 VL - 13 IS - 21 SP - 3755 PB - MDPI CY - Basel, Switzerland AN - OPUS4-53764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Herbst, Tristan T1 - Konzept zur ganzheitlichen Nachhaltigkeitsbewertung des Abbruchs und der Aufbereitung von Mauerwerk N2 - Mit der vorliegenden Arbeit wurde ein methodisches Konzept zur ganzheitlichen Nachhaltigkeitsbewertung des Abbruchs und der Aufbereitung von Mauerwerk bereitgestellt. Das Bewertungskonzept ermöglicht einen ganzheitlichen Vergleich verschiedener Szenarien für den Abbruch und die Aufbereitung von Mauerwerk unter Berücksichtigung der Anwendung von Mauerwerkbruch und aussortierter Fremdstoffe zur Verwertung. Es kombiniert die Kosten-Wirksamkeitsanalyse, die Stoffflussanalyse, die Ökobilanzierung, die Betrachtung sozialer Aspekte und Wirtschaftlichkeitsbetrachtungen bei gleichzeitiger Berücksichtigung der Materialqualitäten. Das Bewertungskonzept basiert im Kern auf der Kosten-Wirksamkeitsanalyse (KWA) mit der Erweiterung um das Gesamtwirksamkeitswert-Kosten-Verhältnis. Hiermit können sowohl monetäre als auch nicht monetäre Effekte beurteilt werden. Ausgangspunkt der KWA ist ein klar definiertes Zielsystem. Im vorliegenden Fall wurden aus der EU-Abfallrahmenrichtlinie, dem Kreislaufwirtschaftsgesetz und der EU-Bauproduktenverordnung die vier Generalziele „Mensch und Umwelt“, „Ressourcenschonung“, „Ausreichende Materialqualität“ sowie „Wirtschaftlichkeit“ abgeleitet. Die Generalziele "Mensch und Umwelt" und "Ressourcenschonung" wurden weiter in Hauptziele, Ziele und Unterziele unterteilt. Die Quantifizierung und Beurteilung dieser beiden Generalziele erfolgt im Rahmen der Wirksamkeitsanalyse. Zur Quantifizierung der abstrakten Ziele wurden konkrete und messbare Zielkriterien ausgewählt, die üblicherweise bei der Ökobilanzierung und sozialorientierten Betrachtungen verwendet werden, z. B. Umweltauswirkungen, Material- und Energieverbrauch. Nach Ermittlung einer Gesamtwirksamkeit und den anfallenden Kosten für jedes Szenario wird das Gesamtwirksamkeit-Kosten-Verhältnis je Szenario errechnet. Dieses Verhältnis bildet die Grundlage für die abschließende Reihung der untersuchten Szenarien entsprechend ihrer nachhaltigkeitsbezogenen Wertigkeit im Sinne der europäischen und deutschen Kreislaufwirtschaft. Mit dem Konzept wird zukünftigen Nutzern eine strukturierte und methodische Bewertungsgrundlage als Planungsinstrument für Abbruchprojekte an die Hand gegeben. Gleichzeitig werden die Nutzer für bestehende Gestaltungsvarianten für den Abbruch und die Aufbereitung von Mauerwerk sowie für die vielfältigen Anwendungsmöglichkeiten von Mauerwerkbruch sensibilisiert. T3 - BAM Dissertationsreihe - 151 KW - Nachhaltigkeit KW - Kosten- und Wirksamkeitsanalyse KW - Mauerwerkbruch KW - Abbruch KW - Aufbereitung PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-384853 SN - 978-3-9817853-8-8 SN - 1613-4249 VL - 151 SP - 1 EP - 146 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38485 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Algernon, A. A1 - Walther, A. A1 - Denzel, W. A1 - Ebsen, B. A1 - Feistkorn, S. A1 - Friese, M. A1 - Grosse, C. A1 - Kathage, S. A1 - Kessler, S. A1 - Köpp, Christian A1 - Krause, M. A1 - Maack, Stefan A1 - Schickert, M. A1 - Taffe, A. A1 - Timofeev, Juri A1 - Wilcke, M. A1 - Wolf, J. T1 - Qualitätssicherung und Validierung der Anwendung zerstörungsfreier Prüfungen von Stahlbetonbauteilen im Bauwesen N2 - Stahlbetontragwerke sind eine wichtige Konstruktionsweise im Bauwesen und ein wachsendes Anwendungsfeld für die Zerstörungsfreie Prüfung (ZfP). Zur Sicherung der Tragsicherheit, strukturellen Integrität, Bestimmung von Geometrien und zur Detektion konstruktiver Elemente wie z.B. Bewehrung, Verankerungen und Spannkanälen besitzen zerstörungsfreie Prüfverfahren in diesem Bereich inzwischen große Relevanz. Durch den bislang erreichten Fortschritt in der Forschung und Entwicklung haben moderne akustische und elektromagnetische Verfahren eine beachtliche Leistungsfähigkeit erreicht. Von Geräteherstellern sind diese in kommerziellen Produktserien umgesetzt worden und finden eine zunehmend breite Anwendung in der Praxis. In einigen anderen Anwendungsgebieten, in denen die ZfP bereits fester Bestandteil von Überwachungen ist, wie z.B. im Maschinenbau und insbesondere in der Kerntechnik und der Luftfahrt, existieren umfangreiche Qualitätssicherungssysteme für die konforme Anwendung und zuverlässige Einbeziehung der ZfP. Dem relativ jungen Entwicklungsstadium moderner ZfP für Stahlbetonbauteile entsprechend müssen solche Konzepte im Bauwesen erst noch entwickelt bzw. implementiert werden. Dementsprechend hat sich der Unterausschuss Qualitätssicherung (UA- S) des Fachausschusses ZfP im Bauwesen (ZfPBau) die Definition und Verbesserung der Qualität von ZfP-Anwendungen sowie insbesondere die verfahrensunabhängige Standardisierung von Prüfprozeduren und statistische Absicherung der Prüfergebnisse zum Ziel gemacht. Die aktuellen Arbeitsfelder beinhalten die Entwicklung praxisgerechter Konzepte für Prüfprozeduren und deren Erprobung in einem Ringversuch sowie die Konzeption von Testkörpern hinsichtlich unterschiedlicher Aspekte wie Parameterstudien, Validierung, Kalibrierung und Simulation. Dabei werden Ansätze anderer Branchen durchaus einbezogen, die Anpassung an die spezifischen Bedürfnisse und Gegebenheiten des Bauwesens wird jedoch als wesentlich angesehen und stellt somit eine wichtige Vorgabe dar. Da die Tätigkeiten nicht auf einzelne Verfahren begrenzt sind, müssen generelle Vorgehensweisen entwickelt werden, die sich auf die jeweiligen Verfahren konkretisieren lassen. Der Vortrag gibt hierzu erste Einblicke in die Arbeit des Ausschusses. T2 - DGZfP-Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Zerstörungsfreie Prüfung KW - Beton KW - Qualitätssicherung KW - Validierung PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472417 SP - 1 EP - 9 AN - OPUS4-47241 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy T1 - Ermittlung der Porosität von Sandsteinen - Vergleich von Quecksilberporosimetrie, Tauchwägung und NMR N2 - Die Porosität sowie die Porengrößenverteilung (PSD) eines Baustoffs sind wichtige petrophysikalische Eigenschaften, die Transportprozesse im Material beeinflussen und im direkten Zusammenhang mit der Schadensanfälligkeit stehen (Frost-Tau-Schäden, Schäden durch Salzeinträge und sauren Regen). Verfahren zur Ermittlung der Porosität stellen die Quecksilberporosimetrie (MIP), das Prinzip der Tauchwägung nach Archimedes (triple weighing method, TWM) und die Nuklear Magnetische Resonanz (NMR) dar. Das Hauptziel dieser Arbeit ist der Vergleich der drei Methoden für die Porositätsbestimmung. Als Untersuchungsmaterial wurde Sandstein gewählt. Als Baustoff wird Sandstein trotz einer teilweise geringen Festigkeit, aber aufgrund seiner Farbvielfalt häufig für Kulturbauten, Gehwegmaterial und Fassaden eingesetzt. Sandsteine weisen zudem meist eine hohe effektive Porosität (bis zu ca. 30 %) und teilweise breite Porengrößenspektren auf, wodurch Feuchte- und Ioneneinträge begünstigt werden und zu z. B. langfristigen Verfärbungen an Sandsteinfassaden führen können. Im Rahmen dieser Arbeit werden die Porositäten von 10 verschiedenen Sandsteinen aus Deutschland und Tschechien bestimmt. Für die Untersuchungen mittels TWM und NMR wurden für jede Sandsteinart zwei zylinderförmige Proben unter Unterdruck mit Leitungswasser aufgesättigt. Beim Vergleich der Verfahren liegt der Fokus insbesondere auf NMR und der verwendeten Gerätetechnik, die mit einer minimalen Echozeit von 50 µs ein Wasserstoffsignal in Sandsteinen aus bis zu ca. 2 nm kleine Poren erfassen kann. Darüber hinaus wird das Auflösungsvermögen von MIP und NMR bezüglich der Poren- bzw. Poreneingangsgrößen diskutiert. Für den Vergleich von NMR und MIP werden an ausgewählten Sandsteinproben ebenfalls die zusätzlich ermittelten PSD in Korrelation zueinander gebracht. Erste Ergebnisse zeigen eine gute Korrelation von NMR- und TWM-Daten, aber teilweise starke Abweichungen zu den mit MIP bestimmten Porositäten. Ergebnisse zu den PSD zeigen teilweise nahezu identische Kurvenverläufe. Jedoch ist die Abschätzung des Umrechnungsfaktors für die NMR-Daten ohne Hinzuziehen von zusätzlichen Referenzverfahren wie Röntgen-Computer-Tomographie oder Spektral Induzierte Polarisation teilweise sehr schwierig. T2 - Bauwerksdiagnose CY - Berlin, Germany DA - 13.02.2020 KW - NMR KW - Porosität KW - Sandsteine KW - Quecksilberporosimetrie KW - Tauchwägung PY - 2020 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-50405 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Embedded passive RFID-based sensors for moisture monitoring in concrete N2 - Moisture measurements based on passive RFID based sensors. These sensors are embedded into stell reinforced concrete to enable long-term monitoring. T2 - IEEE Sensors 2017 CY - Glasgow, Scotland, UK DA - 30.10.2017 KW - Concrete KW - Embedded sensors KW - RFID based sensors KW - Passive sensors KW - Moisture monitoring PY - 2017 AN - OPUS4-42746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Quantification of Perfluorocarboxylic Acids in Water Samples via Static Headspace Gas Chromatography Coupled to Mass Spectrometry N2 - Perfluorocarboxylic acids (PFCAs) are one of the most prominent and studied subgroups of per- and polyfluoroalkyl substances (PFASs), which have attracted great interest in environmental and toxicology research due to their intensive use in combination with their persistence, mobility and potential threat to ecosystems and human health. The standard method to quantify PFCAs in water samples is liquid chromatography or, for additional quantification of ultrashort-chain PFCAs (carbon chain length of two or three carbon atoms) too, hydrophilic interaction liquid chromatography, in each case coupled with mass spectrometry. However, there are a lot of laboratories using MS coupled to headspace gas chromatography systems (HS-GC-MS), usually to quantify a wide range of volatile organic compounds. While PFCAs themselves are difficult to measure with HS-GC-MS in water samples, this challenge can be solved by derivatizing the acids to more volatile compounds, like esters. This approach could enable laboratories using HS-GC-MS to analyse and monitor PFCAs in environmental water samples. By following this idea, we successfully developed a HS-GC-MS method to quantify PFCAs in ultrapure water. Trifluoric acid (TFA), perfluoropropionic acid (PFPrA), perfluorobutanoic acid (PFBA) and perfluorooctanoic acid (PFOS) served as exemplary analytes of PFCAs, which were derivatized with methanol and concentrated sulfuric acid to form methyl esters. The method was optimized by varying different preparation and measurement parameters, leading to limits of detection and quantification in the two-digit ppt-range for all four analytes. The method was than tested on various real water samples, including tap and bottled water, groundwater, landfill leachate, treated wastewater and impinger water from a sewage sludge incineration experiment. Furthermore, snow samples from a ski slope were analysed too. TFA was the most frequently detected PFAA, with concentrations in the ppt and low ppb range. The detection and quantification of the remaining three PFCAs vary with the sample types and sampling location.Our results show that HS-GC-MS is suitable, and enables laboratories with this technique, to quantify PFCAs water samples. T2 - SETAC Europe CY - Vienna, Austria DA - 11.05.2025 KW - Per- and polyfluoroalkyl substances (PFAS) KW - Groundwater KW - GC-MS PY - 2025 AN - OPUS4-63094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Detection, quantification, and treatment of per- and polyfluoroalkyl substances (PFAS) in groundwater (DFEAT-PFAS) N2 - Per- and polyfluoroalkyl substances (PFAS) are a large group of chemicals used in the formulations of thousands of consumer goods. Because of the recent regulations and restrictions on the use of long chain (≥C8) PFAS a significant shift in the industry towards short (C4-C7) and ultrashort (C1-C3) chain alternatives has been recognized the last years. Due to the high polarity and water solubility of ultrashort PFAS, the potential for bioaccumulation is low. However, the high persistence of ultrashort-chain PFAS will result in environmental accumulation, especially in aquatic environments, leading to potential risks for aquatic organisms and increased human external exposure through drinking water. Ultrashort PFAS like trifluoroacetic acid (TFA) are low to moderately toxic to a range of organisms. In the project we are focusing on detecting and removing PFAS, especially ultrashort-chain PFAS from contaminated groundwater. Therefore, we suggest developing and optimizing short- and ultrashort-chain PFAS detection, quantification, and removal. We will design passive sampling devices, which can collect and monitor the temporal profile of PFAS species in groundwater. This will allow us to analyze PFAS contaminations in German and Israeli groundwater using state-of-the-art novel analytical techniques. In addition, contaminated groundwater will be treated via a two-stage process, designed to concentrate the relatively low PFAS concentrations by novel membrane processes including closed-circuit reverse osmosis (CCRO) and mixed matrix composite nanofiltration membranes (MMCM). Afterwards the rejected streams, containing higher concentrations of PFAS will be treated by coagulation and the remaining PFAS adsorbed onto carbonaceous nanomaterials (CNMs). T2 - SETAC Europe CY - Vienna, Austria DA - 11.05.2025 KW - Per- and polyfluoroalkyl substances (PFAS) KW - Groundwater KW - Remediation PY - 2025 AN - OPUS4-63095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Johann, Sergej A1 - Müller, Maximilian A1 - Bartholmai, Matthias T1 - Moisture Measurements with RFID based Sensors in Screed and Concrete N2 - To quantify the moisture in concrete, RFID based humidity sensors are embedded. Passive high frequency, ultra-high frequency RFID tags as well as active Bluetooth sensors are tested. After concreting, all sensors measure the corresponding relative humidity to monitor the concrete moisture. Two case studies are performed, embedding in an existing construction, i.e. the duraBASt test bridge, and embedding in cement based mortar in the laboratory. As basis for robust and long-life sensors in alkaline concrete, different casing materials are tested. Furthermore, signal strength measurements and their sensitivity to different moisture levels are performed. T2 - 8th European Workshop On Structural Health Monitoring CY - Bilbao, Spain DA - 05.07.2016 KW - Humidity sensors KW - Moisture measurements KW - RFID based sensors KW - DuraBASt PY - 2016 SP - 1 EP - 10 AN - OPUS4-36817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Nutzung von ZfP-Daten bei der Nachrechnung von Brücken - Beispiel Regenbrücke Roding N2 - Im Laufe des Lebenszyklus einer Brücke kann es erforderlich sein, diese hinsichtlich der Tragfähigkeit neu zu bewerten. Ursächlich hierfür sind beispielsweise sich ändernde Einwirkungen, wie steigende Verkehrslasten oder auch neuere Erkenntnisse, die beim ursprünglichen Bauwerksentwurf noch nicht berücksichtigt wurden. Die aufgeführten Ursachen treten hierbei meisten nach mehreren Jahrzehnten der Nutzung des Bauwerkes auf. In Deutschland findet eine planmäßige Neubewertung für Brückenbauwerken des Bundes und der Länder auf Basis der im Mai 2011 eingeführten Nachrechnungsrichtline statt. Neben der Neubewertung zur Gewährleistung der Zuverlässigkeit im laufenden Betrieb ist es insbesondere im Rahmen des Abbruches von Bauwerken wichtig Resttragfähigkeiten beurteilen zu können. Die Zuverlässigkeit der Berechnungsergebnisse hängt insbesondere von der Anzahl und von der Qualität der einbezogenen Informationen ab. Durch die Anwendung von zerstörungsfreien Prüfmethoden können quantitative Informationen gesammelt werden, die für die Beurteilung der Tragwerke sowohl relevant als auch ausreichend genau sind. Die gemessenen Daten können explizit in probabilistische Berechnungsmodelle für die Nachrechnung einer Brücke einfließen. Dadurch wird das Modell sukzessive an die Realität angenähert — in anderen Worten: "zugeschärft". Die Zuverlässigkeit der Ergebnisse der Nachrechnung steigt. In diesem Beitrag wird an einem konkreten Beispiel der gegenwärtige Stand von Technik und Forschung für ausgewählte Fragstellungen gezeigt. Im Rahmen der erstellten Abbruchstatik einer vorgespannten Brücke aus Beton wurden Ergebnisse der zerstörungsfreien Prüfung verwendet, um Spanngliedlagen für eine Beprobung zu detektieren. Darüber hinaus wurden die Messergebnisse mit wissenschaftlichen Methoden (Phasenauswertung) ausgewertet, um den Zustand der Verpressung der Spannglieder beurteilen zu können. Weiterhin werden die gewonnenen Messdaten der zerstörungsfreien Prüfung verwendet, um den Nachweis zu erbringen, dass auf deren Grundlage eine zuverlässigere Beurteilung der Tragfähigkeit des Bauwerkes erfolgen kann. Hierfür werden die ersten Ergebnisse der Voruntersuchungen für den Biegenachweis der vorgespannten Brücke präsentiert. T2 - Fachtagung Bauwerksdiagnose 2020 CY - Berlin, Germany DA - 13.02.2020 KW - Zerstörungsfreie Prüfung KW - Brückenbauwerke KW - Nachrechnungsrichtlinie KW - Abbruchstatik PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504471 AN - OPUS4-50447 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lehmann, Jens T1 - Potentialfeldmessung - Korrosionsprüfung von Stahlbetonbauwerken N2 - Durch das alkalische Porenwassermilieu ist Stahl im Beton vor Korrosion geschützt. Unter un-günstigen Umgebungsbedingungen (Karbonatisierung, Chlorideintrag) kann die passive Deck-schicht auf der Stahloberfläche zerstört werden. Im weiteren Verlauf können sich korrosionsbe-dingte Folgeschäden, wie Risse und Abplatzungen am Bauwerk ergeben. Um notwendige Sanie-rungsmaßnahmen sind frühzeitige und weitgehend zerstörungsfrei ermittelte Informationen über das aktuelle Korrosionsverhalten der Stahlbewehrung von großer Bedeutung. Die Potentialfeld-messung ist ein etabliertes und weit verbreitetes Verfahren zur Beurteilung des Korrosionszu-standes der Bewehrung in Stahlbetonbauwerken. Mit Hilfe dieses Verfahrens können Bereiche aktiv korrodierender Bewehrung zerstörungsfrei lokalisiert werden. In der Regel kommt diese Messmethode bei der Detektion chloridinduzierter Korrosion zum Einsatz. T2 - Fachtagung Prüfen von Beton CY - Berlin, Germany DA - 06.10.2016 KW - Stahlbeton KW - Spannbeton KW - Korrosion KW - Zertörungsfreie Prüfung PY - 2016 AN - OPUS4-37711 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brackrock, Daniel A1 - Recknagel, Christoph A1 - Brekow, Gerhard A1 - Kreutzbruck, Marc T1 - Untersuchungen von Glas-Metall Klebverbindungen mit Hilfe von Ultraschall N2 - Klebverbindungen im modernen Hochbau können helfen, innovative ästhetische Bedürfnisse im Fassadenbau umzusetzen, technologische Verbesserungen zu erreichen, aber auch die Wechselwirkung von Gebäuden mit der Umwelt unter energetischen Aspekten zu optimieren. Aufgrund der hohen sicherheitstechnischen Bedeutung gibt es hohe Anforderungen an die Leistungsfähigkeit, Dauerhaftigkeit und die Gütesicherheit. Mit einer zerstörungsfreien praxistauglichen Prüftechnik, die eine sichere Überprüfung der Integrität von Glas-Metall Klebverbindungen im Ingenieurhochbau gewährleistet, kann sowohl ein wichtiger Beitrag zur Qualitätssicherung bei der Herstellung von Fassadenelementen aber auch bei der späteren Bauwerksüberwachung im Verlauf der Nutzungsdauer geleistet werden. Für eine Beurteilung der Qualität der Verbundfuge (z.B. bezgl. Standsicherheit) sind dabei Aussagen zur Homogenität der Verbundfuge, zum adhäsiven und kohäsiven Verbundverhalten gefordert. Hierzu besteht aktuell insbesondere Bedarf an zerstörungsfreien praxisgerechten, hoch ortsauflösenden und möglichst bildgebenden Untersuchungsverfahren. Es wird mit einem Matrixarray und mit konventionellen Winkelprüfköpfen eine Prüftechnik vorgestellt, mit der die Wechselwirkung zwischen Ultraschallwelle und Fehlstelle in der Klebefuge untersucht wird. Hierbei ist das erste Untersuchungsziel, mit einer angepassten Ultraschall-Prüftechnik mögliche Inhomogenitäten oder Schädigungsstellen in der geklebten Glas-Metall Verbindung zu detektieren. Über diese qualitativen Aussagen hinaus werden weiterführende Informationen über die flächenhafte Ausdehnung und den Ort einer mangelnden Klebung ermittelt. Dazu werden die Messwerte zusammen mit den Positionen des Ultraschallprüfkopfs aufgezeichnet. Mit Hilfe einer bildhaften Auswertung der gemessenen Ultraschallechos in Abhängigkeit vom Prüfkopfort werden die Möglichkeiten einer detaillierten Integritätsanalyse der Glas-Metall Klebschicht dargestellt. In diesem Beitrag werden experimentelle Prüfergebnisse vorgestellt, die im Sinne einer Verfahrensvalidierung an einem speziellen Beispielprobekörper zur Nachstellung einer SSG-Verglasung (ermittelt wurden und die Detektion fehlerhafter Klebestellen in einer Glas-Metall-Klebverbindung zum Ziel haben. T2 - DGZfP-Jahrestagung 2014 CY - Potsdam, Germany DA - 26.05.2014 PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-331181 UR - https://www.ndt.net/?id=17428 SN - 978-3-940283-61-0 VL - 148 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-33118 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maack, Stefan A1 - Thunell, B. A1 - Wiggenhauser, Herbert T1 - Study of special challenges for NDT-methods on nuclear structures N2 - The special design of buildings, constructed for nuclear power plants is a particular challenge for the nondestructive testing in the building industry. In particular the major component thicknesses, the degree of reinforcement and surface coating systems make the application of NDT methods difficult. The studies first steps were undertaken to determine to which extent established applications of these techniques are useable in the field of infrastructure buildings. Methods have been evaluated that are already state of the art. So for example the ground penetrating radar was used for locating metallic mounting parts. Furthermore, the low-lying internal structure of the containment was investigated with the ultrasonic method. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - Non-destructive testing KW - Ground penetrating radar KW - Ultrasonic KW - Nuclear structures KW - Pulse echo technique PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-345330 UR - http://www.ndt.net/?id=18422 SN - 1435-4934 VL - 20 IS - 11 SP - 1 EP - 4 PB - NDT.net CY - Kirchwald AN - OPUS4-34533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Beurteilung von Bestandsbauwerken mit zerstörungsfrei gemessenen Daten - Erprobung eines neuen Konzepts an der Regenbrücke Roding N2 - Fortwährend besteht ein wesentlicher Bedarf an Nachrechnungen von bestehenden Brückenbauwerken. Die Zuverlässigkeit der Berechnungsergebnisse hängt insbesondere von der Anzahl und von der Qualität der einbezogenen Informationen ab. Durch die Anwendung von zerstörungsfreien Prüfmethoden können quantitative Informationen gesammelt werden, die für die Beurteilung der Tragwerke sowohl relevant als auch ausreichend genau sind. Die gemessenen Daten können explizit in probabilistische Berechnungsmodelle für die Nachrechnung einer Brücke einfließen. Dadurch wird das Modell sukzessive an die Realität angenähert — in anderen Worten: "zugeschärft". Die Zuverlässigkeit der Ergebnisse der Nachrechnung steigt. In diesem Posterbeitrag wird ein entwickeltes Konzept für die Verwendung von Messergebnissen (anstelle von deterministischen Informationen und Annahmen) im statischen Nachweis zusammengefasst. Am Fallbeispiel einer Spannbetonbrücke werden die Vorteile des dargestellten Ansatzes aufgezeigt. Die Messgrößen (hier die Positionen der Längsspannglieder) und die Messstrategien können anhand von Sensitivitätsanalysen definiert und die Anforderungen an die Messergebnisse aus der statischen Berechnung spezifiziert werden. Die Auswirkungen a) der Messunsicherheit auf die Tragwerkszuverlässigkeit sowie b) von gegenüber den vor den Messungen verfügbaren Informationen abweichenden Messwerten sind am Beispiel der Lokalisierung der Längsspannglieder durch Ultraschall- und Radarmessungen dargestellt. T2 - Fachtagung Bauwerksdiagnose 2020 CY - Berlin, Germany DA - 13.02.2020 KW - Spannbetonbrücke KW - Zerstörungsfreie Prüfung KW - Messung KW - Nachrechnung PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504014 AN - OPUS4-50401 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Küttenbaum, Stefan A1 - Maack, Stefan A1 - Taffe, A. A1 - Braml, T. ED - Sykora, M. ED - Lenner, R. ED - de Koker, N. T1 - On the Treatment of Measurement Uncertainty in Stochastic Modeling of Basic Variables N2 - The acquisition and appropriate processing of relevant information about the considered system remains a major challenge in assessment of existing structures. Both the values and the validity of computed results such as failure probabilities essentially depend on the quantity and quality of the incorporated knowledge. One source of information are onsite measurements of structural or material characteristics to be modeled as basic variables in reliability assessment. The explicit use of (quantitative) measurement results in assessment requires the quantification of the quality of the measured information, i.e., the uncertainty associated with the information acquisition and processing. This uncertainty can be referred to as measurement uncertainty. Another crucial aspect is to ensure the comparability of the measurement results.This contribution attempts to outline the necessity and the advantages of measurement uncertainty calculations in modeling of measurement data-based random variables to be included in reliability assessment. It is shown, how measured data representing time-invariant characteristics, in this case non-destructively measured inner geometrical dimensions, can be transferred into measurement results that are both comparable and quality-evaluated. The calculations are based on the rules provided in the guide to the expression of uncertainty in measurement (GUM). The GUM-framework is internationally accepted in metrology and can serve as starting point for the appropriate processing of measured data to be used in assessment. In conclusion, the effects of incorporating the non-destructively measured data into reliability analysis are presented using a prestressed concrete bridge as case-study. T2 - International Probabilistic Workshop 2022 (IPW2022) CY - Stellenbosch, South Africa DA - 09.09.2022 KW - Reliability KW - Assessment KW - Existing structures KW - Measurement uncertainty PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556580 DO - https://doi.org/10.14311/APP.2022.36.0109 SN - 2336-5382 VL - 36 SP - 109 EP - 118 PB - Czech Technical University CY - Prague AN - OPUS4-55658 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Küttenbaum, Stefan A1 - Maack, Stefan A1 - Taffe, A. T1 - Approach to the development of a model to quantify the quality of tendon localization in concrete using ultrasound N2 - Each engineering decision is based on a number of more or less accurate information. In assessment of existing structures, additional relevant information collected with on-site inspections facilitate better decisions. However, observed data basically represents the physical characteristic of interest with an uncertainty. This uncertainty is a measure of the inspection quality and can be quantified by expressing the measurement uncertainty. The internationally accepted rules for calculating measurement uncertainty are well established and can be applied straightforwardly in many practical cases. Nevertheless, the calculations require the occasionally time-consuming development of an individually suitable measurement model. This contribution attempts to emphasize proposals for modelling the non-destructive depth measurement of tendons in concrete using the ultrasonic echo technique. The proposed model can serve as guideline for the determination of the quality of the measured information in future comparable inspection scenarios. T2 - International Conference on Concrete Repair, Rehabilitation and Retrofitting (ICCRRR 2022) CY - Kapstadt, South Africa DA - 03.10.2022 KW - Reliability KW - Measurement Uncertainty KW - Non-Destructive Testing KW - Existing Concrete Structures PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559927 DO - https://doi.org/10.1051/matecconf/202236403007 SN - 2261-236X VL - 364 SP - 1 EP - 8 PB - EDP Sciences CY - Les Ulis, France AN - OPUS4-55992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gebauer, D. A1 - Gutiérrez, R, A1 - Marx, S. A1 - Butler, M. A1 - Grahl, K. A1 - Thiel, T. A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Pirskawetz, Stephan A1 - Breit, W. A1 - Schickert, M. A1 - Krüger, M. T1 - Interrelated dataset of rebound numbers, ultrasonic pulse velocities and compressive strengths of drilled concrete cores from an existing structure and new fabricated concrete cubes N2 - Two test series were examined using nondestructive measuring methods by six independent laboratories before determining their compressive strength. The nondestructive test methods used were the rebound hammer and ultrasonic pulse velocity measurement. Two types of geometries were investigated: drilled cores and cubes. The measurement procedure for each of these datasets is conditioned to the geometry and is therefore different. The first series consists of 20 drilled cores (approximately diameter/height = 10 cm/20 cm) from the 55-year-old Lahntal Viaduct near Limburg, Germany. After preparation in the first laboratory, the lateral surface of the drilled cores was tested with the rebound hammer using a given pattern. Every laboratory tested every drilled core at different locations. Ultrasonic measurements in transmission were performed repeatedly at predefined points on the flat surfaces of the specimen. The second series consisted of 25 newly manufactured concrete cubes of a mix with a target concrete strength class of C30/37. The edge length was 15 cm. Each laboratory received five specimens of this test series. Thus, contrary to the first series, each specimen was tested by only one laboratory. Two side faces of each cube were tested with the rebound hammer. In addition, ultrasonic measurements were performed by one laboratory. The time of flight was measured between the tested side faces of the rebound hammer at different positions. For both series, rebound hammers were used to determine the R-value as well as the Q-value. The rebound hammer models within the laboratories were always the same, while they differed between the laboratories. The ultrasonic measurements took place with different measurement systems and couplants. Finally, both specimen series were tested destructively for compressive strength. The dataset contains the raw data summarized in tabular form. In addition, relevant calculated data are included in some cases. For the ultrasonic measurements, the time of flight has already been converted into the ultrasonic velocity. Besides, in addition to the raw data of the compressive strength test (force, weight, and geometry values), the calculated compressive strengths and densities are also provided. KW - Nondestructive testing KW - Ultra sound KW - Rebound hammer KW - Existing structure KW - Civil engineering PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-574655 DO - https://doi.org/10.1016/j.dib.2023.109201 SN - 2352-3409 VL - 48 IS - 109201 SP - 1 EP - 13 PB - Elsevier Inc. AN - OPUS4-57465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy T1 - Ermittlung des Flüssigwasseranteils an voll- und teilgesättigten Sandsteinen mittels 1H-NMR und Hygrometrie N2 - Da Feuchte insbesondere in Form von Flüssigwasser ein hohes Schadenspotential für Baustoffe und Konstruktionen darstellt, finden zerstörungsfreie Verfahren wie die Kernspinresonanz (NMR) zunehmend Einsatz im Bauwesen. Auch wenn zur qualitativen Lokalisierung möglicher Schad- und Risikostellen bereits zahlreiche zerstörungsfreie Verfahren in der Praxis Anwendung finden, so besteht beispielweise bei der Porenraumcharakterisierung und dem Verständnis von Feuchtetransportmechanismen weiterhin Forschungsbedarf. Eine besondere Herausforderung stellt in diesem Zusammenhang die (ortsaufgelöste) Erfassung und Quantifizierung von Feuchteverteilungen bei Teilsättigung dar. Mittels 1H-NMR lassen sich der Wassergehalt sowie die Relaxationszeiten der Wasserstoffprotonen in Abhängigkeit von ihrer Bindungsart und der Porenumgebung messen. In vollgesättigten porösen Baustoffen kann somit das NMR-Signal als Porengrößenverteilung interpretiert werden. Da aber in der Praxis nur selten bis nie vollgesättigte Zustände vorliegen, befasst sich eine laufende Forschungsarbeit mit dem Verständnis der NMR-Signale teilgesättigter Porensysteme, die teilweise multimodale Porengrößenverteilungen aufweisen. Im Rahmen dieser Arbeit werden insgesamt 19 Sandsteine aus Deutschland, Tschechien und Italien sowohl im voll- als auch im teilgesättigten Zustand mit NMR untersucht. Definierte teilgesättigte Zustände werden durch Aufsättigen der Proben in Exsikkatoren mit verschiedenen relativen Luftfeuchten (z. B. 33 %, 75 %, 96%) erzeugt. Die Regulierung der Luftfeuchten erfolgt mit Hilfe von gesättigten Salzlösungen. Als Ergebnis wird die Veränderung der Signalamplitude und der T2-Relaxationszeitenverteilungen in Abhängigkeit von dem Feuchtezustand näher betrachtet. Des Weiteren erfolgt die Berechnung des Flüssigwasseranteils bzw. der adsorbierten Wasserfilmdicke einzelner Poren aus der mit Quecksilberporosimetrie bestimmten Porengrößenverteilung und der Annahme einer Porengeometrie (z.B. Schlitz-, Zylinderpore, etc.). Am Ende dieser Arbeit soll der Zusammenhang des NMR-Signals (Amplitude und Relaxationszeiten) mit dem Porensättigungsgrad in einem Porensystem mit multimodaler Porengrößenverteilung bei Teilsättigung aufgezeigt werden. T2 - Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Online meeting DA - 18.05.2020 KW - NMR KW - Sandstein KW - Flüssigwasser KW - Teilsättigung KW - Hygrometrie PY - 2020 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-50861 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - CASPAR - FKZ: 19F2178A "Plattform für die beweissichere und rückführbare Datennutzung im Bauwesen" N2 - Bestandsunterlagen von älteren Bauwerken sind oft nicht in ausreichendem Umfang verfügbar. Soll jedoch der Zustand von z.B. Gebäude oder Brücken bewertet werden, stellen Bestandsunterlagen die Grundlage dafür dar. Ansonsten muss die Bauweise des Bauwerkes kostenintensiv nachvollzogen und mit nachträglichen Untersuchungsverfahren bewertet werden. Heute spielt die digitale Planung im Bauwesen eine immer größere Rolle und Bauvorhaben werden in sogenannten BIM Modellen (Building Information Modelling) geplant. Diese Daten müssen langfristig und manipulationssicher gespeichert werden. In diesem Projekt erarbeiten wir die technologischen Grundlagen, um Daten effizient und sicher zu speichern. Wir erarbeiten eine digitale Schnittstelle, um Daten aus unterschiedlichsten Quellen sicher zusammenzuführen und Informationen semantisch zu verknüpfen. Um den Nachweis für die Nutzbarkeit unserer Technologie zu erbringen, entwickeln wir im Rahmen des beantragten Projekts eine prototypische objektbezogene Datenablage in Form eines Demonstrators, in die digitale Informationen einer realen Brücke überführt werden. T2 - Kick-Off-Meeting Förderprogramm mFUND CY - Online meeting DA - 05.08.2021 KW - Digitalisierung KW - Messdaten KW - Brücken KW - Qualitätssicherung KW - Bauwesen PY - 2021 AN - OPUS4-53220 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Bühling, Benjamin T1 - Low-frequency ultrasound data (pulse-echo technique) with shear horizontal and longitudinal waves on the step-shaped concrete specimen “Pk050” N2 - This dataset contains raw data acquired in ultrasound measurements on a reference specimen made of concrete at Bundesanstalt für Materialforschung und -prüfung (BAM), Berlin (Germany). The internal specimen identifier is “Pk050”. The measurements were conducted using the pulse-echo method. The upper surface of the specimen was defined as measuring area. The aim of the measurements is to determine the geometrical dimensions (thickness) of the specimen “Pk050”. In addition to this, a dataset of a second specimen with identifier “Pk266” has been acquired. Pk266 has the same geometrical dimensions and concrete recipe as Pk050, but contains tendons [Reference: https://doi.org/10.7910/DVN/NUU0WZ]. KW - Ultrasound KW - Pulse echo method KW - Synthetic Aperture Focusing Technique KW - Validation KW - Elastic wave PY - 2023 DO - https://doi.org/10.7910/DVN/9EID5D PB - Harvard College CY - Cambridge, MA, USA AN - OPUS4-57231 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dähne, Siegfried A1 - Yesudas, Kada A1 - Dekhtyar, Marina T1 - The polymethine nature of Vis/NIR chromophores N2 - The polymethine concept is known to rationalize a plethora of spectroscopic issues, thus finding wide applications in modern color theory. This approach was questioned by the arguments in the relevant “dye” literature. Based on the critical analysis of these arguments, the errors are clarified and the superiority of the polymethine concept above other attempts to qualitatively explain color and constitution relationships is exemplified at relevant dye molecules absorbing in the visible and near‐infrared spectral region. The classical chromophore theory, topological approaches, different‐level semiempirical techniques, and DFT/ab initio methods are comparatively analyzed to interpret the optical effects of structural modifications in conjugated compounds regarded as polymethine derivatives. KW - Alternation perturbation effects KW - Color rules KW - Conjugated polymethine chromophore KW - Polymethine concept KW - Red and blue color shifts KW - π-Electron alternation PY - 2023 DO - https://doi.org/10.1002/jccs.202300346 SN - 2192-6549 VL - 71 IS - 1 SP - 99 EP - 117 PB - Wiley CY - Malden, Mass. AN - OPUS4-62842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Capitain, C. A1 - Schüßler, M. A1 - Bugsel, B. A1 - Zweigle, J. A1 - Vogel, Christian A1 - Leube, Peter A1 - Zwiener, C. T1 - Implementation of matrix-matched semiquantification of PFAS in AFFF-contaminated soil N2 - This study presents a novel semiquantification approach for nontarget screening (NTS), combining matrix-matched calibration and ionization class-specific average calibration curves (ACCs) to address the lack of analytical reference standards for most per- and polyfluoroalkyl substances (PFAS). Ionization class-specific ACCs for carboxylic and sulfonic acids, sulfonamides, and cationic PFAS result in high accuracy, with median absolute accuracy quotients below 2.27×. The approach was applied to soil impacted by aqueous film-forming foam (AFFF) contamination. A total of 96 tentatively identified PFAS were semiquantified in addition to 28 quantified compounds based on available standards. Semiquantified concentrations exceeded those of target analytes, demonstrating the critical role of this method in capturing broader PFAS contamination. In this case, validation against extractable organofluorine (EOF) showed a 102% closed mass balance. The innovative approach not only enables comprehensive PFAS contamination assessment in complex matrices but also expands the scope of the NTS for environmental monitoring, remediation, and risk assessment of AFFF-contaminated sites. KW - Per- and polyfluoroalkyl substances (PFAS) KW - Contaminated soil KW - Non-targeted analysis KW - Combustion ion chromatography PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-629445 DO - https://doi.org/10.1021/acs.est.4c14255 SN - 1520-5851 VL - 59 IS - 14 SP - 7338 EP - 7347 PB - American Chemical Society (ACS) CY - Columbus, Ohio AN - OPUS4-62944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rudert, Rainer A1 - Czichocki, G. T1 - Sodium 1,12-dodecylene disulfate hydrate N2 - There are two independent dodecylene disulfate molecules in the crystal of 2Na⁺.C₁₂H₂₄O₈S₂²⁻.2/3H₂O, one with a centrosymmetric conformation, its center lying on a crystallographic center of symmetry, the second with an asymmetric conformation, which is partially disordered. The molecules form a layer structure parallel to the ab plane, the polar parts of neighbouring molecular layers connecting via coordination to the Na⁺ ion. Additionally, there are hydrogen bonds between the water molecule and two sulfate groups. KW - Dodecylene disulfate molecule KW - Crystal structure PY - 1996 DO - https://doi.org/10.1107/S0108270196003071 SN - 0108-2701 SN - 1600-5759 SN - 2053-2296 VL - C52 SP - 1670 EP - 1673 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-62715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mugani, R. A1 - El Khalloufi, F. A1 - Kasada, M. A1 - Redouane, E. M. A1 - Haida, M. A1 - Aba, R. P. A1 - Essadki, Y. A1 - Zerrifi, S. E. A. A1 - Herter, Sven-Oliver A1 - Hejjaj, A. A1 - Aziz, F. A1 - Ouazzani, N. A1 - Azevedo, J. A1 - Campos, A. A1 - Putschew, A. A1 - Grossart, H.-P. A1 - Mandi, L. A1 - Vasconcelos, V. A1 - Oudra, B. T1 - Monitoring of toxic cyanobacterial blooms in Lalla Takerkoust reservoir by satellite imagery and microcystin transfer to surrounding farms N2 - Cyanobacterial harmful algal blooms (CyanoHABs) threaten public health and freshwater ecosystems worldwide. In this study, our main goal was to explore the dynamics of cyanobacterial blooms and how microcystins (MCs) move from the Lalla Takerkoust reservoir to the nearby farms. We used Landsat imagery, molecular analysis, collecting and analyzing physicochemical data, and assessing toxins using HPLC. Our investigation identified two cyanobacterial species responsible for the blooms: Microcystis sp. and Synechococcus sp. Our Microcystis strain produced three MC variants (MC-RR, MC-YR, and MC-LR), with MC-RR exhibiting the highest concentrations in dissolved and intracellular toxins. In contrast, our Synechococcus strain did not produce any detectable toxins. To validate our Normalized Difference Vegetation Index (NDVI) results, we utilized limnological data, including algal cell counts, and quantified MCs in freeze-dried Microcystis bloom samples collected from the reservoir. Our study revealed patterns and trends in cyanobacterial proliferation in the reservoir over 30 years and presented a historical map of the area of cyanobacterial infestation using the NDVI method. The study found that MC-LR accumulates near the water surface due to the buoyancy of Microcystis. The maximum concentration of MC-LR in the reservoir water was 160 μg/L. In contrast, 4 km downstream of the reservoir, the concentration decreased by a factor of 5.39 to 29.63 μg/L, indicating a decrease in MC-LR concentration with increasing distance from the bloom source. Similarly, the MC-YR concentration decreased by a factor of 2.98 for the same distance. Interestingly, the MC distribution varied with depth, with MC-LR dominating at the water surface and MC-YR at the reservoir outlet at a water depth of 10 m. Our findings highlight the impact of nutrient concentrations, environmental factors, and transfer processes on bloom dynamics and MC distribution. We emphasize the need for effective management strategies to minimize toxin transfer and ensure public health and safety. KW - Cyanotoxin KW - HPLC-MS/MS KW - Surface water PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623672 DO - https://doi.org/10.1016/j.hal.2024.102631 SN - 1568-9883 VL - 135 SP - 1 EP - 14 PB - Elsevier CY - Amsterdam AN - OPUS4-62367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Isleyen, Alper A1 - Özcan, Kemal A1 - Tunc, Murat A1 - Boztepe, Aylin A1 - Coşkun, Fatma Gonca A1 - Moshammer, Kai A1 - Shehab, Moaaz A1 - Stratulat, Camelia A1 - Bratu, Adriana A1 - Hafner-Vuk, Katarina A1 - Vogl, Jochen A1 - Strzelec, Michał A1 - Calvo, Mariana Villegas A1 - Frey, Anne Mette A1 - Strauss, Helena T1 - Development of three biofuel CRMs for the quality parameters in biodiesel and wood pellet via a joint research project N2 - Biomass is a key element in biofuels which can be defined as a fuel produced through contemporary biological processes, and its increased use can support the EU’s aims of reducing greenhouse gas emissions. Information on the nature and the quality of the biomass or biofuel is important in order to support the optimization of their combustion with respect to realizing higher efficiencies and lower emissions during energy production. Three reference materials were produced by a collaborative approach among national metrology institutes and designated institutes within the scope of the EMPIR project: BIOFMET. The project was aimed to establish advanced traceable measurement standards for the determination of the calorific value, impurities, and other parameters such as density, kinematic viscosity, moisture, and ash. This paper presents the sampling and processing methodology, homogeneity, stability, characterization campaign, the assignment of property values, and their associated uncertainties in compliance with ISO 17034 for biofuel reference materials: biodiesel, wood pellet powder, and wood pellet. Parameters of interest in biodiesel reference material-UME BIOFMET CRM 01 are gross calorific value (GCV), density, viscosity, and mass fractions of Ca, K, Mg, Na, P, and S elements. Parameters to be certified in wood pellet powder reference material-UME BIOFMET CRM 02 are GCV, moisture, ash, and mass fractions of Al, Cr, K, Mg, Mn, Ni, S, and Zn elements. Parameters to be certified in the wood pellet reference material-UME BIOFMET CRM 03 are GCV and moisture. The homogeneity and stability of the materials were assessed in accordance with ISO 33405. The materials were characterized by interlaboratory comparison studies among competent metrology institute and designated institute laboratories. Assigned values and uncertainties of the certified values were calculated in accordance with ISO 33405, and uncertainties include characterization, homogeneity, and stability components. The developed CRMs are intended to be used for the development and validation of measurement procedures for the determination and quality control/assurance purposes of the quality parameters for biofuels. It should be emphasized that the UME BIOFMET CRM 01-Biodiesel CRM is the first biodiesel reference material certified for calorific value. Among the developed wood CRMs, the pellet form, UME BIOFMET CRM 03, was found to be more stable than the powder one, UME BIOFMET CRM 02, for the moisture parameter. Sixfold lower relative uncertainty value for short-term stability at 45 °C and twofold lower relative uncertainty value for long-term stability at 22 °C were obtained for the moisture parameter of the CRM in pellet form compared to the CRM in powder form. KW - Biofuel KW - Biodiesel KW - Wood pellet KW - Calorific value KW - Moisture KW - Element content PY - 2024 DO - https://doi.org/10.1007/s00216-024-05694-y SP - 1 EP - 13 PB - Springer Science and Business Media LLC AN - OPUS4-62371 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Küttenbaum, Stefan A1 - Feistkorn, S. A1 - Braml, T. A1 - Taffe, A. A1 - Maack, Stefan ED - Rizzo, P. ED - Milazzo, A. T1 - Methods to Quantify the Utility of NDT in Bridge Reassessment N2 - The purpose of this contribution is to introduce and to apply the developed approach of incorporating non-destructively gathered measurement results (instead of deterministic information and assumptions) into a reassessment model of a typical prestressed concrete road bridge and to outline the advantages. An essential part is the quality evaluation of the non-destructively measured information, that deals primarily with two questions. Could the object or parameter to be obtained reliably detected and if, how accurate are the inspection results achieved? Therefore, the importance of the combination of a probability of detection (POD)-approach and measurement uncertainty calculations is emphasized. With regard to the introduced case-study it is shown, for which structure parameters an assumption deviating from the actual (and measurable) situation has a particularly strong (and possibly arithmetically unfavorable) influence on the structural reliability. Measurements on such parameters are particularly beneficial for a reliable and robust reassessment. In conclusion, the individual reassessment results without consideration and with consideration of evaluated non-destructive inspection results are compared. KW - Non-destructive testing (NDT) KW - Structural safety KW - Concrete bridges KW - Measurement uncertainty KW - Probability of detection (POD) PY - 2021 SN - 978-3-030-64593-9 DO - https://doi.org/10.1007/978-3-030-64594-6_40 SN - 2366-2557 VL - 127 SP - 403 EP - 413 PB - Springer Nature Switzerland CY - Cham, Switzerland AN - OPUS4-52009 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Oesch, Tyler A1 - Stelzner, Ludwig A1 - Weise, Frank ED - Herrmann, H. ED - Schnell, J. T1 - Non-destructive evaluation of the contribution of polymer-fibre orientation and distribution characteristics to concrete performance during fire N2 - Although concrete itself is not a combustible material, concrete mixtures with high density, such has high-performance concretes (HPCs), are susceptible to significant damage during fires due to explosive spalling. Past research has shown that the inclusion of polymer fibres in high density concrete can significantly mitigate this fire damage. The exact mechanisms causing this increased spalling resistance are not yet fully under-stood, but it is thought that the fibres facilitate moisture transport during fire exposure, which in turn contributes to relief of internal stresses in the spalling-susceptible region. In this study, X-ray Computed Tomography (CT) was applied to observe the interaction between polymer fibres and cracking during thermal exposure. For this purpose, two concrete samples containing different polymer fibre types were subjected to incremental application of a defined thermal exposure. CT images were acquired before and after each thermal exposure and powerful image processing tools were used to segment the various material components. This enabled a detailed analysis of crack formation and propagation as well as the visualization and quantification of polymer fibre characteristics within the concrete. The results demonstrated that the orientation of both fibres and cracks in polymer-fibre reinforced concrete tend to be anisotropic. The results also indicated that crack geometry characteristics may be correlated with fibre orientation, with cracks tending to run parallel to fibre beds. Clear quantitative relationships were also observed between heating and increasing cracking levels, expressed in terms of both crack surface area and crack volume. KW - X-ray Computed Tomography (CT) KW - Polypropylene Fibres KW - Fire Performance KW - Fibre-Reinforced Concrete (FRC) KW - Fibre Orientation Analysis PY - 2019 SN - 978-3-030-00868-0 DO - https://doi.org/10.1007/978-3-030-00868-0 SP - 51 EP - 73 PB - Springer Nature Switzerland AG AN - OPUS4-47206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Ortsaufgelöste NMR-Relaxometrie an mineralischen Baustoffen N2 - Zahlreiche Schädigungsprozesse in Baustoffen stehen im engen Zusammenhang mit Feuchteeintrag und Feuchtetransport. Als Beispiel sind die schädigende Alkali-Kieselsäurereaktion (AKR) von Beton sowie Frost-Tauwechsel induzierte Gefügeschäden genannt. Zur zerstörungsfreien, ortsaufgelösten Feuchtemessung eignet sich die im Bereich der Geophysik etablierte, aber im Bauingenieurwesen noch wenig verbreitete, Messmethode der Nuklear Magnetischen Resonanz (NMR). Unter Verwendung der NMR-Relaxometrie sind sowohl Aussagen zum Feuchtegehalt und dessen räumliche Verteilung als auch die Charakterisierung der Porengrößen möglich, die das Transportverhalten eines porösen Materials maßgeblich beeinflussen. Zur Erfassung der Mikro- und Mesoporen in Baustoffen ist dabei die Auflösung von kurzen T2 Relaxationszeiten unabdingbar. Bisher ist es mit gängigen NMR-Laborgeräten nur begrenzt möglich, solche kurzen T2-Zeiten schichtselektiv zu erfassen. Vor diesem Hintergrund wurde ein speziell für die Messung an mineralischen Baustoffen optimierter NMR-Tomograph beschafft. Dieser ermöglicht sowohl schichtselektive Messungen von Bohrkernen mit Durchmessern von bis zu 70 mm als auch bildgebende Untersuchungen an Proben mit Durchmessern ≤ 40 mm. Erste Untersuchungsergebnisse an Sandstein, Tuffstein und Beton zeigen die Leistungsfähigkeit des neuen NMR-Tomographen zur Erfassung der porengrößenspezifischen Feuchteverteilung. In diesem Beitrag werden erste Ergebnisse verschiedenartiger Laborversuche exemplarisch dargestellt. Für Sandsteine mit unterschiedlichsten Porengrößenverteilungen wurden mit dem neuen NMR-Tomographen und einem herkömmlichen NMR-System vergleichbare T2 Zeitenverteilungen ermittelt. Am sehr heterogenen Tuffstein konnten unterschiedlich poröse (und feuchte) Bereiche räumlich aufgelöst werden. Im Beton ließ sich der Feuchtetransport im Zementstein porengrößenspezifisch, schichtselektiv und zeitlich aufgelöst verfolgen. Die bisher gewonnenen Ergebnisse zeigen das breite Anwendungsspektrum des neuen NMR Tomographen auf und ermöglichen ein besseres Verständnis des Feuchtetransports und der oft damit einhergehenden Schädigungsprozesse in Baustoffen. T2 - 79. Jahrestagung Deutsche Geophysikalische Gesellschaft CY - Brunswick, Germany DA - 04.03.2019 KW - Concrete KW - NMR KW - Sandstone KW - Capillary suction PY - 2019 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-47501 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Zimmek, David T1 - Experimentelle Validierung eingebetteter Sensorik zur pH-Wert Bestimmung basierend auf Fluoreszenzspektroskopie N2 - Die vorliegende Arbeit beschäftigt sich mit der experimentellen Validierung eingebetteter Sensorik zur pH-Wert Bestimmung basierend auf Fluoreszenspektroskopie. Bisherige Karbonatisierungsmessungen basieren auf zerstörenden Methoden. Durch das Einbetonieren von immer erreichbaren pH-Sonden wird die Überprüfung zerstörungsfrei. Um ein fehlerfreies, reproduzierbares Ergebnis zu gewährleisten, mussten diese pH-Sonden zunächst getestet und eine ausreichend präzise Methode zur Messung entwickelt werden. Durch das Vorgeben unterschiedlicher pH-Milieus und dem Testen verschiedener Messmethoden und Versuchsaufbauten werden Situationen im Beton simuliert. Hierzu werden die pH-Sonden mit unterschiedlich starken basischen und neutralen Lösungen in Kontakt gebracht, wodurch der in den Sonden befindliche Indikator je nach pH-Wert eine blaue oder orange Färbung annimmt. In den Sonden befindliche Quantenpunkte werden durch einen Laser angeregt. Diese Quantenpunkte fluoreszieren aufgrund der Anregung im blauen und orangen Spektrum. Mithilfe der Fluoreszenzspektroskopie wird die durch den Indikator gefilterte Fluoreszenz in Reflexion und Transmission gemessen. Die Ergebnisse werden genutzt, um ein Verhältnis zwischen den zwei Wellenlängen zu berechnen, anhand dessen zu erkennen ist, welche Farbe der Indikator in den Sonden angenommen hat. Die experimentelle Validierung dient der Optimierung der Methodik, des Versuchsaufbaus und der Zusammensetzung der Sonden. Nach eine Reihe unterschiedlicher Versuche, werden Bedingungen geschaffen, welche zu den gewünschten Ergebnissen führen. Das in Reflexion gemessene Licht kann Aussage darüber geben, welche Farbe der Indikator annimmt und das Verhältnis zwischen dem blauen und dem orangen Spektrum gibt die erwarteten Werte zurück. Die Ergebnisse dieser Arbeit sollen in Betonprobekörpern angewandt werden, um die hier erprüfte Methode in Realbedingungen zu testen. KW - pH Wert in Baustoffen KW - Fluoreszenzspektroskopie KW - Eingebettete Sensorik PY - 2018 SP - 1 EP - 68 CY - Berlin AN - OPUS4-46326 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weise, Frank A1 - Kind, Thomas A1 - Stelzner, Ludwig A1 - Wieland, M. T1 - Dunkelfärbung der Betonfahrbahndecke im AKR-Kontext - Ursachenanalyse mit innovativer Prüftechnik T1 - Dark Dyeing of the Concrete Pavement in the AKR Context: Root Cause Analysis with innovative Testing Technology N2 - Die AKR-Schadensevolution von Betonfahrbahndecken ist in der Anfangsphase durch eine Dunkelfärbung der Oberfläche im Fugenbereich gekennzeichnet. Es wird vermutet, dass eine erhöhte Durchfeuchtung der Betonrandzone ursächlich für diese Erscheinung ist. Vor diesem Hintergrund wurde exemplarisch eine Fahrbahnplatte eines repräsentativen Bundesautobahnabschnitts systematisch mit verschiedenartiger zerstörungsfreier Prüftechnik vor Ort untersucht. Die Ergebnisse der zunächst erfolgten großflächigen Durchmusterung mit Radar zeigen, dass in den Bereichen mit einer Dunkelfärbung der Betonfahrbahndecke erhöhte Laufzeiten der Radarimpulse zwischen der Oberfläche und der Rückseite der Betonfahrbahndecke auftreten, was auf eine erhöhte integrale Durchfeuchtung der Betonfahrbahndecke schließen lässt. Vertiefend durchgeführte NMR-Feuchtemessungen in der Betonrandzone zeigen eine gute Korrelation zwischen erhöhtem Feuchtegehalt und der dunkel gefärbten Fahrbahnoberfläche. Die Ergebnisse beider zerstörungsfreien Prüfmethoden lassen den Schluss zu, dass die Betonfahrbahndecke in der Nähe des Fugenkreuzes eine höhere Durchfeuchtung als im Bereich der Querscheinfuge aufweist. Die geringste Durchfeuchtung besitzt die Betonfahrbahndecke in der Plattenmitte. Die mit den zerstörungsfreien Prüfverfahren ermittelten Befunde stimmen prinzipiell gut mit den punktuell mittels Darr-Wäge-Verfahren an Bohrmehlproben gewonnenen Ergebnissen überein. N2 - Darkening of the surface within alkali-silica reaction context - Root cause analysis with non-destructive measurement methods The damage evolution in concrete pavements due to alkali-silica reaction is characterized in the initial phase by a darkening of the surface along joint regions. It is generally assumed that an increased moisture content of the concrete boundary zone is responsible for this visual appearance. Against this background, a concrete pavement slab of a representative German motorway section was systematically investigated in-situ using different non-destructive measurement methods. The results of the high-resolution, planar radar showed an increased time of flight of the radar pulse between the pavement surface and the base of the concrete slab in the darkened areas. This indicated that the overall moisture content is increased near joints in the slab. Additional NMR moisture measurements in the concrete boundary zone confirmed the correlation between increased moisture content and the dark-colored surface of the concrete pavement. The results of both non-destructive measurement methods indicated that the moisture content near the intersection of two joints was higher than the moisture content near the area around the transverse joint. The lowest moisture content was measured in the center of the concrete pavement slab. The results obtained with the two non-destructive testing methods were in overall good agreement with moisture measurements of boring dust analyzed using the gravimetric method. KW - Betonfahrbahndecke KW - Alkali-Kieselsäure-Reaktion KW - Feuchtemessung KW - Radar KW - Nuclear Magnetic Resonance KW - ZfP PY - 2018 DO - https://doi.org/10.1002/best.201800020 SN - 0005-9900 SN - 1437-1006 VL - 113 IS - 9 SP - 647 EP - 655 PB - Wilhelm Ernst & Sohn, Verlag für Architektur und technische Wissenschaften GmbH & Co. KG CY - Berlin AN - OPUS4-46173 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy T1 - NMR zur Beobachtung von Trocknungsprozessen und Hydratationsverhalten an Baustoffen N2 - Im Rahmen der Arbeit soll die Anwendbarkeit des Verfahrens der Nuklear Magnetischen Resonanz (NMR) zur Charakterisierung von Porensystemen und Feuchtetransportmechanismen in Baustoffen untersucht werden. Ein Ziel ist dabei die Bestimmung des Flüssigwasseranteils bei Teilsättigung. Dazu wird die Porensättigung in Abhängigkeit der relativen Luftfeuchte im Porensystem berechnet, um erstmals eine Korrelation zwischen dem NMR-Signal und dem Porensättigungsgrad in einem multimodalen Porengrößensystem bei Teilsättigung vornehmen zu können. Derzeit erfolgen Aufsättigungsversuche an Referenzmaterialien (Sandsteine und Kalziumsilikatplatten). Bereits vorgenommene Untersuchungen bei Vollsättigung an Estrichen haben zunächst eine von der Literatur abweichende Oberflächenrelaxivität ergeben. Dieses Ergebnis legt den Verdacht nahe, dass ein hinreichender Ettringitgehalt, ein Hydratationsprodukt, Einfluss auf die resultierende Oberflächenrelaxivität in Baustoffen haben kann. Somit wird ein weiterer Forschungsschwerpunkt auf den Ettringitgehalt gelegt. Neben ersten Voruntersuchungen mit LIBS und NMR-Spektroskopie, zur Überprüfung der Nachweisbarkeit von Ettringit, sowie ersten Tests zur Steuerung der Ettringitbildung mittels Betonverflüssigern wurde bereits eine Messreihe geplant. Für diese und zukünftige Messungen soll dabei auch erstmals ein neu beschaffter und speziell angefertigter NMR-Tomograph (BAM-Größtgeräteinvestition 2016) Anwendung finden und neue Erkenntnisse ermöglichen. T2 - Doktorandenseminar der 8. Abteilung CY - Berlin, Germany DA - 15.10.2018 KW - NMR KW - Ettringit KW - Relative Luftfeuchte KW - Porenraumanalyse KW - Feuchte PY - 2018 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-46298 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph T1 - Determination of the diffusion coefficient and the hydraulic conductivity of porous media based on embedded humidity sensors N2 - Reinforced concrete and several other building materials deteriorate during their service life. Almost all deterioration processes are related to moisture. For understanding those processes, knowing the exact amount of the moisture content and the moisture transport characteristics is crucial. In fact, the moisture transport in porous materials is a two-phase flow; consisting of the vapour and the liquid phase. The two corresponding parameters are the diffusion coefficient and the hydraulic conductivity. By means of an inverse approach, these two coefficients are experimentally determined. The moisture transport of eight different screed types during hydration and evaporation is monitored based on embedded humidity sensors. The measured humidity profiles are converted into a pore saturation by adapting the approach of Hillerborg to the measured pore volume distribution. The summation of all pore saturations yields the total moisture content including the ink-bottle effect during desorption. The pore volume distribution was determined by mercury intrusion porosimetry as well as by gas adsorption. The measurement of the humidity and the pore saturation in the entire sample enables to invert the mass balance in order to extract the diffusion coefficient and the hydraulic conductivity. The determined diffusion coefficients of the eight investigated screeds are between m2s-1 and m2s-1. KW - Material moisture KW - Moisture transport KW - Embedded sensors KW - Diffusion coefficient KW - Partially saturated pores PY - 2020 DO - https://doi.org/10.1016/j.conbuildmat.2020.120092 VL - 263 SP - 120092 PB - Elsevier Ltd. AN - OPUS4-51029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hicke, Konstantin T1 - KI, Machine Learning und faseroptische Sensorik N2 - Die Verwendung von Methoden des Maschinellen Lernens (ML) und der Künstlichen Intelligenz (KI) im Fachbereich 8.6 Faseroptische Sensorik wird dargestellt. Die vielfältigen Möglichkeiten, Machine Learning auf Basis Künstlicher Neuronaler Netze (ANN) für eine schnelle und effiziente Datenverarbeitung eizusetzen werden demonstriert. Hierfür werden Beispiele für die Anwendungszwecke Messgrößenberechnung, Entrauschen, Interpolation, Bildverarbeitung und Messdatenauswertung aufgezeigt. T2 - Foresight Prozess AM, AP 4, Workshop „In Situ Sensorik“ CY - Online-Meeting DA - 09.11.2020 KW - Verteilte faseroptische Sensorik KW - KI KW - Künstliche Intelligenz KW - Machine Learning KW - Künstliche Neuronale Netze PY - 2020 AN - OPUS4-51545 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - CASPAR - FKZ: 19F2178A "Plattform für die beweissichere und rückführbare Datennutzung im Bauwesen" N2 - Bestandsunterlagen von älteren Bauwerken sind oft nicht in ausreichendem Umfang verfügbar. Soll jedoch der Zustand von z.B. Gebäude oder Brücken bewertet werden, stellen Bestandsunterlagen die Grundlage dafür dar. Ansonsten muss die Bauweise des Bauwerkes kostenintensiv nachvollzogen und mit nachträglichen Untersuchungsverfahren bewertet werden. Heute spielt die digitale Planung im Bauwesen eine immer größere Rolle und Bauvorhaben werden in sogenannten BIM Modellen (Building Information Modelling) geplant. Diese Daten müssen langfristig und manipulationssicher gespeichert werden. In diesem Projekt erarbeiten wir die technologischen Grundlagen, um Daten effizient und sicher zu speichern. Wir erarbeiten eine digitale Schnittstelle, um Daten aus unterschiedlichsten Quellen sicher zusammenzuführen und Informationen semantisch zu verknüpfen. Um den Nachweis für die Nutzbarkeit unserer Technologie zu erbringen, entwickeln wir im Rahmen des beantragten Projekts eine prototypische objektbezogene Datenablage in Form eines Demonstrators, in die digitale Informationen einer realen Brücke überführt werden. T2 - Online-Fachaustausch der mFUND-Begleitforschung Move Mobility | iRights.Lab CY - Online meeting DA - 07.05.2021 KW - Digitalisierung KW - Messdaten KW - Brücken KW - Qualitätssicherung KW - Bauwesen PY - 2021 AN - OPUS4-53221 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gebauer, D. A1 - Beltrán Gutierrez, R. A1 - Marx, S. A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Pirskawetz, Stephan A1 - Breit, W. A1 - Mechtcherine, V. A1 - Grahl, K. A1 - Thiel, T. A1 - Schickert, M. A1 - Krüger, M. T1 - Interrelated Data Set from Nondestructive and Destructive Material Testing of Concrete Compressive Strength Specimens N2 - "This data set contains three different data types obtained from concrete specimens. For each specimen, the rebound numbers, ultrasonic data (ultrasonic velocity, time of flight), and destructive concrete strength are given. Two kind of specimen geometries were tested: cubes and drilled cores. The files are labeled according to the specimen geometry as "cube" or "core" and the type of measurement data as "compressive_strength", "rn_R" and "rn_Q" for rebound numbers as well as "us" for ultrasonic data. The ultrasonic data were generated by six independent laboratories, the rebound numbers by five independent laboratories and the destructive tests by one laboratory. The designation of each specimen establishes the relationship between the different data types." KW - Compressive Concrete Strength KW - Rebound Hammer KW - Ultrasonic Pulse Velocity PY - 2023 DO - https://doi.org/10.7910/DVN/AFCITK PB - Harvard College CY - Cambridge, MA, USA AN - OPUS4-57223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Büyüksahin, Kaan T1 - Weiterentwicklung und Automatisierung einer Ultraschallbohrlochsonde zur zerstörungsfreien Prüfung untertägiger Verschlussbauwerke N2 - Im Jahre 2011 wurde in Deutschland nach 50 Jahren der Ausstieg aus der kommerziellen Kernenergie beschlossen. Fünf Jahre später war Deutschland mit 80.000 GWh immer noch unter den zehn größten Atomstromproduzenten. Im darauffolgenden Jahr wurden weltweit 2.500.000 GWh Atomstrom produziert. Durch die Atomstromproduktion fallen große Mengen an radioaktiven Reststoffen an, die bis zu mehrere tausend Jahre für einen vollständigen Abbau benötigen. Aus dieser Problematik geht die Debatte über den Verbleib der Reststoffe hervor. Die Endlagerung in tiefen Gesteinsschichten ist eine Lösung für das Problem. Voraussetzung ist hierbei allerdings die Gewährleistung eines dauerhaften Schutzes vor ionisierender Strahlung, die durch Verschlüsse der tiefen Gesteinsschichten in Form von Verschlussbauwerken erzielt werden sollen. Es gilt die bauliche Integrität sowie die Dichtwirkung der Verschlussbauwerke dauerhaft zu überwachen und zu prüfen, um eine langfristige Verzögerung der Radionuklidfreisetzung zu gewährleisten. KW - Bohrlochsonde KW - Beton KW - ZfP im Bauwesen KW - Abschlussbauwerke KW - Ultraschall PY - 2022 SP - 1 EP - 77 CY - Berlin AN - OPUS4-54942 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Medina, A. A1 - Ol, M. V. A1 - Greenblatt, D. A1 - Müller-Vahl, H. A1 - Strangfeld, Christoph T1 - High-Amplitude Surge of a Pitching Airfoil: Complementary Wind- and Water-Tunnel Measurements N2 - RECENT interest in gust response, rotorcraft forward flight and wind energy, among other applications, has focused on streamwise oscillations of nominally two-dimensional airfoils in attached and separated flows. The airfoil may be simultaneously held at constant incidence or execute some maneuver, such as pitch. The relative freestream is spatially uniform but temporally unsteady, and this can be accomplished in a ground-test facility in two ways. The first method is to vary the output of the prime mover, such as the rotational speed of the impeller or the blower driving a wind tunnel, or (alternatively) to vary the pressure drop in the tunnel, thereby varying the flow speed in the test section, despite nominally constant primemover revolutions per minute. The second method is used to keep the tunnel’s operating speed constant, as well as to move the test article in the streamwise direction, fore and aft (for example, via an electric linear motor), such that the relative freestream speed felt by the test article varies according to some waveform. Typically, the latter approach is chosen in water tunnels, where there is too much tunnel-circuit inertia to vary the flow speed directly but where the usually low tunnel test section flow speeds enable large excursions in the relative freestream by oscillation of the test article. In fact, outright reverse flow is possible by moving the test article in the laboratory frame at a higher speed than the water-tunnel flow speed. In either case, a sinusoidal relative-speed waveform is the most intuitively realizable, and this can be combined with similar oscillations in the airfoil incidence angle or other kinematics. Although the two methods of realizing streamwise oscillations are mechanically distinct, experimental comparisons between an oscillating test article in a water tunnel and a stationary test article in a wind tunnel with a louvermechanismhave demonstrated agreement in themeasured lift and drag histories. Such experimentswere performed by Granlund et al. for a 10% freestream amplitude oscillation and fixed airfoil incidence, comparing a free-surface water tunnel and a closed-circuit wind tunnel. After buoyancy was subtracted from the wind-tunnel data (resulting from the louver pressure drop) and the model inertia subtracted from the water-tunnel data (resulting from acceleration of the test article), the remaining lift and drag histories matched well at the low freestream oscillation amplitude regime. The work of Granlund et al. was later extended to high-advance-ratio streamwise oscillations of 50% amplitude by Greenblatt et al., where the aerodynamic histories of the water-tunnel and wind-tunnel facilities were compared in combined pitch and freestreamoscillations (governed by relative pitch phase), pure pitch oscillations, and purely freestream oscillations. Agreement between the two facilities’ data for fixed-incidence streamwise oscillations was reasonably good, and in fact, better than agreement in just the static lift and drag, evidently owing to differences in blockage and model-support systems. Additionally, Greenblatt et al. determined there was no strong coupling between simultaneous freestream oscillations and pitch oscillations on resultant lift and moment coefficients. KW - Wind energy KW - Dynamic stall KW - Deep stall KW - Airfoil surging KW - Airfoil pitching PY - 2018 DO - https://doi.org/10.2514/1.J056408 SN - 0001-1452 SN - 1533-385X VL - 56 IS - 4 SP - 1703 EP - 1709 PB - American Institute of Aeronautics and Astronautics AN - OPUS4-43994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bühling, Benjamin T1 - Entwicklung eines luftgekoppelten Ultraschall-Echo-Prüfverfahrens mittels fluidischer Anregung N2 - In vielen technischen Bereichen werden Ultraschallverfahren zur zerstörungsfreien Werkstoffprüfung eingesetzt. Dabei wird ein Schallpuls von einem Prüfkopf in ein Prüfobjekt eingebracht. Der Puls kann unter anderem durch Membranen oder Piezoelemente erzeugt werden und wird in der Regel durch direkten Kontakt oder über ein Koppelmittel an das Objekt übertragen. Luftgekoppelter Ultraschall spielt in kommerziellen Anwendungen bisher eine untergeordnete Rolle, da die Differenz der akustischen Impedanzen von Luft und Festkörpern immense Verluste beim Übergang des Schallsignals hervorruft. In diesem Beitrag soll ein neuartiges Anregungsprinzip vorgestellt werden, mit dem ein Großteil dieser Verluste vermieden wird. Anstelle eines Festkörpers soll mit Hilfe einer fluidischen Düse Druckluft zur Signalerzeugung eingesetzt werden. In dieser Düse wird eine selbsterhaltende Strömungsinstabilität erzeugt, die einen Schallpuls von bis zu 100 kHz hervorruft, sodass der Impedanzverlust in die Umgebungsluft entfällt. Da die charakteristische Frequenz eines fluidisch generierten Pulses maßgeblich von der Bauform der Düse und dem anliegenden Druck abhängt, lässt sich mittels einer geeigneten Strömungsregelung ein breiter Frequenzbereich zur Abtastung nutzen. Die so emittierten Pulse werden auf das Prüfobjekt gerichtet und die reflektierten Signale mit einem Laservibrometer an der Oberfläche des Objekts im Echo-Verfahren abgetastet. Von drei signalmindernden Materialübergängen bei gewöhnlichem luftgekoppeltem Ultraschall bleibt in dem hier vorgeschlagenen Messystem lediglich die Grenzfläche von Luft zu Prüfkörper, sodass eine höhere Signalausbeute als bisher erwartet werden kann. T2 - Akustisches Seminar der TU Berlin CY - Berlin, Germany DA - 24.06.2019 KW - Luftgekoppelter Ultraschall KW - Ultrasound KW - Vibrometer PY - 2019 AN - OPUS4-48303 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Spain - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Spain. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. The study on Spanish CABs is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558465 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-55846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Brazil - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Brazil. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. The study on Brazilian CABs is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556330 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-55633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Ireland - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Ireland. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. The study on Irish CABs is part of a global project that covers various other countries (see www.qi-fokus.de). KW - Quality infrastructure KW - Digitalization KW - Testing KW - Laboratory KW - Certification KW - Conformity assessment KW - Digital transformation KW - TIC KW - Conformity assessment body KW - COVID-19 KW - Calibration PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554877 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-55487 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ladu, Luana A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Peru - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Peru. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. This study is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563417 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-56341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Non-destructive testing at BAM N2 - A brief introduction to non-destructive testing at BAM, Department 8 and its Divisions. T2 - AK Post Docs Symposium CY - BAM Berlin, Germany DA - 02.02.2021 KW - Non-destrucitve testing PY - 2021 AN - OPUS4-52063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Germany - A QI-FoKuS study T1 - Digitalisierung in der Konformitätsbewertung in Deutschland - Eine QI-FoKuS-Studie N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Germany. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. The study on German CABs is part of a global project that covers various other countries (see www.qi-fokus.de). N2 - Dieser Bericht fasst die Ergebnisse der ersten umfassenden Studie zur Digitalisierung der Konformitätsbewertung in Deutschland zusammen. Die Ergebnisse basieren auf Daten einer Umfrage unter Konformitätsbewertungsstellen (KBS), die 2022 durchgeführt wurde. Sie beleuchten den digitalen Reifegrad der Organisationen, die Motive, Vorteile und Hindernisse der digitalen Transformation sowie die aktuellen Technologietrends. Die Studie zu KBS in Deutschland ist Teil eines globalen Projekts, das verschiedene andere Länder umfasst (siehe www.qi-fokus.de). KW - Quality infrastructure KW - Digitalization KW - Testing KW - Conformity assessment KW - Certification KW - Laboratory KW - Digital transformation KW - TIC KW - Conformity assessment body KW - COVID-19 KW - Calibration KW - Corona KW - Digitalisierung KW - Kalibrierung KW - Konformitätsbewertung KW - Konformitätsbewertungsstelle KW - Labor KW - Prüfung KW - Qualitätsinfrastruktur KW - Zertifizierung KW - Digitale Transformation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554885 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-55488 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Non-Destructive Testing: A valuable source of information for reliability assessments N2 - The reassessment of bridges is becoming increasingly important. The basic requirement for analyses of structural safety is reliable knowledge about individual structures. This paper introduces the new approach to evaluate the quality of measured data gained from non-destructive testing (NDT) to provide reliable, objective, and relevant information about existing bridges. The purpose is to relate this validated knowledge to probabilistic analyses. Bridging the gap between NDT and numerical reassessments indicates reduced numerical uncertainties and residual service time extensions. This paper deals with an application of this approach using measurement data collected by ultrasonic technique at a prestressed concrete bridge. T2 - IABSE Symposium 2019 CY - Guimarães, Portugal DA - 27.03.2019 KW - NDT KW - Measurement KW - Structural safety KW - Concrete bridges KW - Eexisting structures PY - 2019 AN - OPUS4-47714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Non-destructive testing application examples using the NMR core-analyzing tomograph N2 - Nuclear magnetic resonance (NMR) with focus on 1H protons is increasingly applied for non-destructive testing applications. Besides mobile NMR, laboratory devices such as the NMR core-analyzing tomograph are used. As their magnetic field is more homogeneous, they enable measurements with higher signal-to-noise ratios (SNR), but with limited sample sizes. The tomograph presented here (8.9 MHz) was constructed for a maximum sample diameter of 70 mm and length of up to 1 m. The resolution, the echo time (min. 50 µs), the SNR and the measurement type can be adjusted by means of exchangable coils. The tomograph enables measurements along the complete sensitive length, slice-selective and even 2- or 3-dimensional measurements. A movable sample lifting system thereby allows a precise positioning of the sample. T2 - Magnetic Resonance in Porous Medie (MRPM) 2022 CY - Online meeting DA - 21.08.2022 KW - Spalling KW - Nuclear magnetic resonance KW - Tomography KW - Moisture transport KW - Frost salt attach PY - 2022 AN - OPUS4-55828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Vries, H. A1 - Jacobs, K. A1 - Egyedi, T. A1 - Eto, M. A1 - Fertig, S. A1 - Kanevskaia, O. A1 - Klintner, L. A1 - Koch, Claudia A1 - Mijatovic, I. A1 - Mirtsch, Mona A1 - Morone, P. A1 - Orviska, M. A1 - Riillo, C. A1 - Scaramuzzino, G. ED - Jacobs, K. T1 - Standardization: Towards an agenda for research N2 - Standardization research is a fairly new and is a still-evolving field of research, with possibly major practical ramifications. This article presents a summary of the authors’ subjective views of the most pressing research topics in the field. These include, among others, standards (e.g. incorporation of ethical issues), the potential impact of standards, the corporate management of standardization and legal issues like Intellectual Property Rights (IPR). In addition, gaps have been identified with a respect to a basic understanding of standardization, suggesting a need for better education in the field. KW - EURAS KW - Impact of standards KW - Intellectual property rights (IPR) KW - Research agenda KW - Standardization research PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-467873 DO - https://doi.org/10.4018/IJSR.2018010104 SN - 2470-8542 VL - 16 IS - 1 SP - 52 EP - 59 PB - IGI Global AN - OPUS4-46787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia A1 - Niederhausen, J. T1 - Vision einer modernen Qualitätsinfrastruktur: digital und vernetzt N2 - „Made in Germany“ steht für Vertrauen in Qualität und Sicherheit, das auch in der digitalen und grünen Transformation gelten soll.  In einer zunehmend digitalisierten Welt muss auch die Qualitätssicherung von Produkten, Prozessen und Dienstleistungen neu gedacht werden. Ziel der Initiative QI-Digital ist es, Lösungen für eine moderne, digitale Qualitätsinfrastruktur (QI) zu schaffen. Im Vortrag wird die Vision einer QI-Digital skizziert, und es werden die nötigen Werkzeuge sowie das Vorgehen der Initiative mithilfe dreier Pilotprojekte dargestellt. T2 - QI-Digital Forum „Made in Germany in der digitalen und grünen Transformation“ CY - Berlin, Germany DA - 11.10.2022 KW - Qualitätsinfrastruktur KW - Digitalisierung KW - Wasserstofftankstelle KW - Additive Fertigung KW - Smart Standard KW - QI-Cloud KW - Zertifikat KW - Prüfung PY - 2022 AN - OPUS4-56185 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Bore hole probe for ultrasound-based quality control of sealing constructions N2 - Several countries, which use or used nuclear power, started to destruct nuclear power plants. Thus, large amounts of radioactive waste have to be stored safely during the next decades. Large underground caverns will be used a nuclear waste disposal. Once the cavern is full, a sealing construction is required. The sealing should avoid the contact to any fluids or substances of the storage barrels and reduce hazardous radiation. T2 - International Symposium Non-Destructive Testing in Civil Engineering CY - Zurich, Switzerland DA - 16.08.2022 KW - Ultrasonic testing KW - Nuclear waste PY - 2022 AN - OPUS4-55530 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mirtsch, Mona A1 - Blind, K. A1 - Koch, Claudia A1 - Dudek, Gabriele T1 - Information security management in ICT and non-ICT sector companies: A preventive innovation perspective N2 - Despite the growing dependence of companies on information technology and the increasingly negative impact of security incidents worldwide, there is little research on the management of information security at the company level. This paper seeks to expand knowledge on the implementation of an information security management system based on the widely used international standard ISO/IEC 27001. We present motives, experienced impacts, and obstacles related to ISO/IEC 27001 implementation using data from a survey of 125 ISO/IEC 27001 certified companies in Germany. Since adoption rates vary between ICT and non-ICT sector companies, we highlight sector-related variations. We classify the adoption of this standard as a preventive organizational innovation and apply Structural Equation Modeling to unearth explanations for the comparatively low adoption of this management system standard among companies outside the ICT sector. We, therefore, derive recommendations for policymakers, standardization, and certification bodies to foster its diffusion. KW - Information Security KW - ISO/IEC 27001 KW - Management system standard KW - Certification KW - Information security management system (ISMS) KW - Preventive Innovation KW - Resource-based-view KW - Institutional theory PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531037 DO - https://doi.org/10.1016/j.cose.2021.102383 SN - 0167-4048 VL - 109 IS - 10 SP - 1 EP - 23 PB - Elsevier Ltd. AN - OPUS4-53103 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Claudia A1 - Blind, K. T1 - Towards Agile Standardization: Testbeds in Support of Standardization for the IIoT N2 - The Industrial Internet of Things (IIoT) poses multiple challenges to traditional standardization, due to the complexity, dynamics, and accelerating speed of technological progress. The need for a timely availability of standards calls for new approaches and tools to enhance standardization processes for smart manufacturing. Industry and standards development organizations worldwide are seeking new solutions. Testbeds have been acknowledged in innovation policy as a powerful tool for knowledge transfer and the further development of emerging technologies. Lately, they have also attracted increasing attention from the standardization perspective as a promising tool for a more agile standards development process. Proponents of such testbeds expect them to support standardization by providing validated solutions and accelerating the processes to meet the growing demands for faster standardization without any detriment to quality. In an explorative, qualitative approach this article is the first to investigate the operation and impact of testbeds in standardization processes based on a multiple case study on testbeds implemented worldwide in the context of the IIoT. KW - Testumgebung KW - Reallabor KW - Normung KW - Standards KW - Standardization KW - Industrie 4.0 KW - Smart manufacturing KW - Industrial internet of things KW - Agility KW - Agile PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513300 DO - https://doi.org/10.1109/TEM.2020.2979697 VL - 68 IS - 1 SP - 59 EP - 74 AN - OPUS4-51330 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Mirtsch, Mona A1 - Koch, Claudia A1 - Dudek, Gabriele A1 - Blind, K. T1 - Die Nutzung und Wirkung genormter Managementsysteme N2 - Das Ziel der Initiative QI-FoKuS ist es, eine Datenbasis für neue wissenschaftliche Erkenntnisse zu Einflussfaktoren und Effekten in der Konformitätsbewertung und Akkreditierung zu schaffen. Ende 2019 wurden in einer ersten Online-Erhebung Unternehmen verschiedener Branchen und Größenklassen in Deutschland zur Nutzung von Managementsystemen und ihren Wirkungen befragt. Diese umfasste weit verbreitete genormte Managementsysteme wie ISO 9001 und ISO 14001 genauso wie bisher wenig untersuchte Systeme wie die ISO 50001 oder ISO/IEC 27001. Es konnten 180 Fragebögen für die vorliegende Studie ausgewertet werden. KW - QI-FoKuS KW - Managementsysteme KW - ISO 9001 KW - ISO/IEC 27001 KW - ISO 50001 KW - ISO 14001 KW - Zertifizierung KW - Konformitätsbewertung KW - Akkreditierung PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510831 SN - 978-3-9818564-3-9 DO - https://doi.org/10.26272/opus4-51083 VL - 1 SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-51083 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Mirtsch, Mona A1 - Koch, Claudia A1 - Dudek, Gabriele A1 - Blind, K. T1 - Die Nutzung und Wirkung der Norm ISO/IEC 27001 für Informationssicherheit in Unternehmen in Deutschland N2 - Das Ziel der Initiative QI-FoKuS ist es, eine Datenbasis für neue wissenschaftliche Erkenntnisse zu Einflussfaktoren und Effekten in der Konformitätsbewertung und Akkreditierung zu schaffen und hierbei insbesondere auch auf aktuelle Trends und Entwicklungen einzugehen. Von Januar bis März 2020 wurden in einer Online-Erhebung Unternehmen verschiedener Branchen und Größenklassen in Deutschland zur Nutzung und den Wirkungen ihres zertifizierten Managementsystems für Informationssicherheit nach ISO/IEC 27001 befragt. Es konnten 125 vollständig ausgefüllte Fragebögen für die vorliegende Studie ausgewertet werden. KW - Managementsysteme KW - ISO/IEC 27001 KW - Informationssicherheit KW - Zertifizierung KW - Konformitätsbewertung KW - Akkreditierung KW - QI-FoKuS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517922 DO - https://doi.org/10.26272/opus4-51792 VL - 2 SP - 1 EP - 28 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-51792 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Mirtsch, Mona A1 - Blind, K. T1 - CORONA-MONITOR - Auswirkungen der Corona-Pandemie auf Konformitätsbewertung und Konformitätsbewertungsstellen in Deutschland N2 - Die Studie fasst Ergebnisse einer Befragung von Konformitätsbewertungsstellen zu deren Lage und den Aussichten während der Corona-Pandemie zusammen. Besondere Schwerpunkte wurden auf die wirtschaftlichen Auswirkungen und die Arbeitsfähigkeit, aber auch auf die Resilienz und die Wirkungen auf die Digitalisierung gelegt. KW - Corona KW - COVID-19 KW - Resilienz KW - Qualitätsinfrastruktur KW - Prüfung KW - Zertifizierung KW - Kalibrierung KW - Inspektion KW - Labor KW - Laboratorium KW - Studie KW - Befragung KW - Digitalisierung PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518276 UR - www.qi-fokus.de DO - https://doi.org/10.26272/opus4-51827 VL - 3 SP - 1 EP - 26 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-51827 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ladu, Luana A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in the Netherlands - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in the Netherlands. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. The study on Dutch CABs is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555852 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-55585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Italy - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Italy. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. The study on Italian CABs is part of a global project that covers various other countries (see www.qi-fokus.de). KW - Quality infrastructure KW - Conformity assessment KW - Conformity assessment body KW - Laboratory KW - Testing KW - Certification KW - Calibration KW - Digitalization KW - Digital transformation KW - COVID-19 KW - TIC PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553708 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-55370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Latvia - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Latvia. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. The study on Latvian CABs is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554987 UR - https://www.qi-fokus.de SP - 1 EP - 45 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-55498 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Mirtsch, Mona A1 - Blind, K. A1 - Castka, P. T1 - Impact of the COVID-19 pandemic on accredited conformity assessment bodies: insights from a multinational study N2 - The COVID-19 pandemic posed new and manifold challenges to organizations and their operations worldwide. Conformity assessment bodies (CABs), such as testing or medical laboratories, certification, and inspection bodies, were also affected by the associated disruptions. Their role in this crisis is highly relevant, as CABs are essential pillars of the quality infrastructure: their activities ensure that products and services meet requirements as defined in standards and regulations, thereby contributing to their safety and reliability. The question arises of how CABs and their operations were affected by the pandemic and how they responded. To this end, we present the results of an international survey of 986 CABs of all types in Germany, the UK, Italy, and New Zealand. Overall, CABs reported, on average, a reduction in demand for their services during the pandemic, facing restrictions in all countries. In addition, the pandemic had an overall negative impact on the CABs’ investment and innovation activities. However, investments in digital infrastructure were increased as a countermeasure, with CABs reporting a higher need for digitalization. The paper highlights and discusses results from in-depth analyses relevant to policymakers and industry alike. KW - Quality Infrastructure KW - Digitalization KW - Testing laboratories KW - Conformity assessment KW - Certification KW - Conformity assessment body KW - Corona KW - Covid-19 KW - Resilience PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556396 DO - https://doi.org/10.1007/s00769-022-01514-x SP - 1 EP - 14 PB - Springer AN - OPUS4-55639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Singapore - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Singapore. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. This study is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561363 UR - https://www.qi-fokus.de SP - 1 EP - 47 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-56136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ladu, Luana A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Mexico - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Mexico. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. This study is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563645 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-56364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ladu, Luana A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in the United Kingdom - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in the United Kingdom. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. This study is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565346 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-56534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ladu, Luana A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Colombia - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Colombia. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. The study on Colombian CABs is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-558484 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-55848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Croatia - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Croatia. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. This study is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565380 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-56538 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ladu, Luana A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in West Africa - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in West Africa. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. This study is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563631 UR - https://www.qi-fokus.de SP - 1 EP - 45 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-56363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in New Zealand - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in New Zealand. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. This study is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity Assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564038 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-56403 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - AI/ML starts with data, …a practical example N2 - A brief introduction to the efforts we have done in our lab towards AI/ML analysis of SAXS data. For this, we need to extend the data with an extensive, structured hierarchy of metadata and associated data. A practical look into the information stored in our files, and the organization of the files in a data catalog is presented. T2 - Benchmarking for AI for Science at the Exascale A2 Workshop for Materials Science CY - Online meeting DA - 23.11.2020 KW - Small angle scattering KW - Machine learning KW - Data organization KW - Data curation KW - Metadata structuring PY - 2020 AN - OPUS4-51660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörenz, Christoph T1 - Improved Sample Preparation for the Analysis of Nanoparticles by Electron Microscopy N2 - In this work, we present various promising sample preparation procedures aiming to avoid drying artifacts and guarantee homogeneously distributed NP samples for imaging techniques like TEM, SEM or AFM. This involves retarded drying in an environment of high relative humidity as well as spin coating or freeze drying of the sample on the substrate. Depending on the type of the NPs, different techniques are successful in obtaining homogenous sample deposition. Simple drying at ambient conditions often results in heavily agglomerated NPs densely packed in coffee ring traces. Retardation of the drying speed in an environment of high relative humidity, however, yields homogeneous NP deposition in the case of bimodal SiO2 and bimodal gold NP’s. In contrast, a sample of bipyramidal TiO2, heavily agglomerated when commonly dried, is successfully dispersed by spin coating the suspension on the substrate. The analysis of the particle size distribution of the bimodal silica and gold samples yielded number ratios resembling the nominal number ratios. The reliable measurement of the NP concentration of polydisperse samples by electron microscopy, even if relative, is new and of special relevance because up to now only the size of the particles, i.e. the abscissa of the PSD, can be measured reliably. T2 - NANOSAFE 2020 CY - Online meeting DA - 16.11.2020 KW - Nanoparticles KW - Particle size distribution KW - Electron microscopy KW - Bimodal KW - SiO2 KW - Gold PY - 2020 AN - OPUS4-51714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörenz, Christoph T1 - Improved Sample Preparation for the Analysis of Nanoparticles by Electron Microscopy N2 - Various promising sample preparation procedures aiming to avoid drying artifacts and guarantee homogeneously distributed NP samples for imaging techniques like TEM, SEM or AFM are presented. This involves retarded drying in an environment of high relative humidity as well as spin coating or freeze drying of the sample on the substrate. Depending on the type of the NPs, different techniques are successful in obtaining homogenous sample deposition. Simple drying at ambient conditions often results in heavily agglomerated NPs densely packed in coffee ring traces. Retardation of the drying speed in an environment of high relative humidity, however, yields homogeneous NP deposition in the case of bimodal SiO2 and bimodal gold NP’s. In contrast, a sample of bipyramidal TiO2, heavily agglomerated when commonly dried, is successfully dispersed by spin coating the suspension on the substrate. The analysis of the particle size distribution of the bimodal silica and gold samples yielded number ratios resembling the nominal number ratios. The reliable measurement of the NP concentration of polydisperse samples by electron microscopy, even if relative, is new and of special relevance because up to now only the size of the particles, i.e. the abscissa of the PSD, can be measured reliably. T2 - EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy" CY - Online meeting DA - 27.10.2020 KW - Nanoparticles KW - Particle size distribution KW - Sample peparation KW - Electron microscopy PY - 2020 AN - OPUS4-51716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement; What nPSize can offer after 2Ys? N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, inter-laboratory comparisons) as pertinent contributions to normative projects within CEN/TC 352 Nanotechnologies are discussed. T2 - 28th Meeting of CEN/TC 352 Nanotechnologies CY - Online meeting DA - 16.10.2020 KW - Nanoparticles KW - CEN/TC 352 Nanotechnologies KW - Particle size distribution KW - Traceability PY - 2020 AN - OPUS4-51437 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marcoulaki, E. T1 - Blueprint for a sustainable new European Centre to support safe innovation for nanotechnology N2 - This paper presents the blueprint for the operation of a sustainable and permanent European Centre of collaborating reference laboratories and research centres, to establish a one-stop shop for a wide variety of nanosafety related services, and to provide a central contact point for questions about nanosafety in Europe. The Centre aims to harmonise service provision, and bring novel risk assessment and management approaches closer to practice. T2 - NANOSAFE 2020 CY - Online meeting DA - 16.11.2020 KW - EC4SafeNano KW - European Centre KW - Nanomaterials KW - Nanosafety KW - Catalogue of Services (CoS) PY - 2020 UR - https://www.nanosafe.org/cea-tech/pns/nanosafe/en AN - OPUS4-51694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, Hans R. A1 - Weidner, Steffen M. A1 - Meyer, A. T1 - About Polycondensation, Disproportionation, and Cyclization of Acetylated Poly(L-Lactide) Esters N2 - L-lactide (LA) is polymerized with ethyl L-lactate or trifluoroethanol as initiators (LA/In = 30/1), and the resulting poly(L-lactide) esters are acetylated with acetic anhydride. The acetylated PLA esters are mixed with SnOct2, dibutyltin bis(4-chlorophenoxide), or dibutyltin bis(pentafluorophenoxide) in solution and crystallized at 120 °C. The doped crystals are annealed at 140 °C or at 160 °C for 7, 14, and 28 days, and the chemical modifications that occurred in the solid state are monitored by matrix-assisted laser desorption/ionization time-of-flight (MALDI TOF) mass spectrometry, gel permeation chromatography (GPC), and differential scanning calorimetry (DSC) measurements. All catalysts promoted polycondensation, while no significant formation of cycles is observed. However, in the presence of SnOct2, disproportionation of chains occurred upon annealing at 120 or 140 °C, and crystallites consisting of extended chains with Mn values ≈3500 – 3600 and low dispersities (Ð < 1.5) are formed. KW - MALDI-TOF MS KW - Polycondensation KW - Polylactides KW - Transesterifcation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630349 DO - https://doi.org/10.1002/macp.202400175 SN - 1521-3935 VL - 225 IS - 19 PB - Wiley VHC-Verlag AN - OPUS4-63034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Operando electrochemical spectroscopic ellipsometry: Material properties of highly active mesoporous IrOx films revealed under realistic OER conditions N2 - Hydrogen production via water electrolysis will be an essential cornerstone in development of sustainable, fossil-free fuel and chemical production on a global scale. The activity and stability of each catalyst is highly dependent on the properties of the coating, i.e., phase composition, crystallinity, accessible surface area, and many other factors. The key to developing improved catalysts is a better understanding of the relationships between their performance, stability, and physicochemical properties. However, these relationships can be complex and are also strongly influenced by the reaction environment. Therefore, operando analysis of the catalyst material during catalysis at realistic potentials and current densities is highly desirable. However, many analytical techniques cannot be applied in liquid environments at realistic potentials and current densities. We propose environmental ellipsometric analysis in a dedicated electrochemical flow cell as a method to evaluate gas evolution reactions operando under realistic working conditions. Figure 1 illustrates schematically the developed technique. Key factors to success are highly active model-type catalysts, a suitable sample environment, and a deep understanding of the appropriate model development, as well as concise cross validation with numerous other analytical techniques. The method was developed and validated by analyzing a calcination series (300 – 600 °C) of mesoporous templated IrOx films ex-situ and operando under oxygen evolution reaction (OER) conditions. The employed environmental electrochemical spectroscopic ellipsometric (ECSE) analysis revealed during OER the change of optical and electronic properties, i.e. the dielectric functions, resistivity and band-to-band transitions (p-d band transitions). Film thickness and porosity were validated by means of scanning electron microscopy (SEM), X-ray reflectometry (XRR) or ellipsometric porosimetry (EP), electrical and electronic properties by means of conductivity measurements, X-ray photoelectron spectroscopy (XPS) or UV-Vis-NIR absorption spectroscopy. The electronic structures of the catalysts from valence electron energy loss spectra (VEELS) derived from ε1 and ε2 from SE measurements reveal a direct correlation with electrochemical activities in OER. In the presentation reversible and irreversible potential-dependent changes of the catalyst properties during operation will be discussed along with the dynamics of gas formation, transport and dissolution at different potentials. T2 - 11th Workshop Ellipsometry (WSE 11) CY - Steyr, Austria DA - 06.09.2021 KW - Ectrocatalysis KW - Mesoporous iridium oxide films KW - Non-destructive operando analysis KW - Oxygen evolution reaction KW - Spectroscopic ellipsometry PY - 2021 AN - OPUS4-53915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tache, O. T1 - Synthesis of SiO2 Nanoparticles as reference materials: Metrological measurements and in-situ kinetics in lab with Small Angle X-Ray Scattering N2 - The unambiguous correlation of possible health and sustainability risks to nanoparticle size must be enabled by reliable measurement of nanoparticle size, to ensure comparability and compatibility between results measured under different methods. The NPSIZE project funded by European Metrology Program (EMPIR) develop methods, reference materials and modelling to improve the traceability chain, comparability and compatibility of nanoparticle size measurements. In this work, we present how spherical silica nanoparticles are synthetized with controlled monomodal or bimodal dispersion to be use as reference materials and international round-robin. Improving the fabrication requires a fine understanding of synthesis (1), coupled with an expertise of in-situ or ex-situ analysis methods. This is a new challenge for the analysis : determining not only average characteristics (size, chemical composition and shape ...) but also the concentration and the distribution over the population studied (2). Small-Angle X-ray Scattering (3) allows very precise measurements of the nanoparticles size and concentration that can be directly link to the metric system (4) (metrological traceability) . We developed a SAXS laboratory instrument dedicated to the in-situ characterization of nanoparticles, which enable fast measurements, and the monitoring of the synthesis parameters. Measurement protocols and software processing chain (5) (i.e. size distribution) are also combined & optimized. T2 - CNANO2021 CY - Toulouse, France DA - 25.11.2021 KW - X-ray scattering KW - Silica particles KW - Synthesis KW - Reference materials PY - 2021 DO - https://doi.org/10.5281/zenodo.5749256 AN - OPUS4-53931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Introduction to Fluorescence Spectroscopy N2 - A brief introduction to fluorescence spectroscopy will be provided, ranging from typically measured fluorescence quantities over instrument-specific contributions to measured fluorescence signals to selected applications. In this context, an overview of the photoluminescence properties of molecular and nanoscale luminescence reporters will be given including a brief insight into their photophysics and fluorescence standards designed by division Biophotonics for the calibration and instrument performance validation of fluorescence measuring devices will be presented. T2 - Analytical Academy BAM CY - Online meeting DA - 17.11.2020 KW - Fluorescence KW - Quality assurance KW - Quantification KW - Linearity KW - Measurement uncertainty KW - Method KW - Nano particle KW - Dye PY - 2020 AN - OPUS4-51619 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hofmann, Detlef T1 - Strukturüberwachung mit lokaler und verteilter faseroptischer Sensorik N2 - Der Vortrag gibt einen Überblick über die Einsatzmöglichkeiten faseroptischer Sensorik (FOS) als ZfP-Verfahren. Dabei werden an Beispielen lokale und verteilte faseroptische Verfahren zur Dehnungs-, Temperatur- und Risserfassung sowie zur akustischen Messung vorgestellt. Weiterhin werden Möglichkeiten zur Selbstdiagnose von FOS aufgezeigt. T2 - InnoTesting2020 "Innovative Ideen - neue Testmethoden" CY - Wildau, Germany DA - 27.02.2020 KW - Faseroptische Sensorik KW - Strukturüberwachung KW - Lichtwellenleiter KW - Zerstörungsfreie Prüfung KW - Selbstdiagnose PY - 2020 AN - OPUS4-51688 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - Comparative study of suitable preparation methods to evaluate irregular shaped, polydisperse nanoparticles by scanning electron microscopy (SEM). N2 - Reliable characterization of materials at the nanoscale regarding their physio-chemical properties is a challenging task, which is important when utilizing and designing nanoscale materials. Nanoscale materials pose a potential toxicological hazard to the environment and the human body. For this reason, the European Commission amended the REACH Regulation in 2018 to govern the classification of nanomaterials, relying on number-based distribution of the particle size. Suitable methods exist for the granulometric characterization of monodisperse and ideally shaped nanoparticles. However, the evaluation of commercially available nanoscale powders is problematic. These powders tend to agglomerate, show a wide particle size distribution and are of irregular particle shape. Zinc oxide, aluminum oxide and cerium oxide with particle sizes less than 100 nm were selected for the studies and different preparation methods were used comparatively. First, the nanoparticles were dispersed in different dispersants and prepared on TEM-supported copper grids. Furthermore, individual powders were deposited on carbon-based self-adhesive pads. In addition, the samples were embedded by hot mounting and then ground and polished. The prepared samples were investigated by scanning electron microscopy (including the transmission mode STEM-in-SEM) and Dynamic Light scattering. The software package ImageJ was used to segment the SEM images and obtain the particle sizes and shapes and finally the number-based particles size distribution with size expressed as various descriptors. T2 - Ceramics 2021 CY - Online meeting DA - 19.04.2021 KW - Nanoparticles KW - Preparation KW - Characterization PY - 2021 AN - OPUS4-53272 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waniek, Tassilo A1 - Zarinwall, A. T1 - Mechanical coupling of matrix and nanoparticles depending on particle surface modification N2 - Boehmite nanoparticles has been successfully functionalized with APTES. After APTES functionalization further modification with tailored molecules e.g. via carboxylic acids is possible. The tailored surface functionalization is strongly enhanced by improved coupling protocols. Arbitrary variation of the functionalization degree is possible. Thereby the temperature stable APTES functionalization enables a wide range of functional groups. By TGA-MS analysis strong evidence for the bonding situation of the APTES on the boehmite surface has been found. Additionally first experiments has been performed to predict the polymer-particle compatibility enhancement via reverse wetting angle measurements with AFM. T2 - Workshop Acting Principles of Nano-Scaled Matrix Additives for Composite Structures CY - BAM, Berlin, Germany DA - 11.10.2019 KW - Surface modification KW - Nanocomposites KW - Boehmite KW - Silane KW - Thermogravimetry KW - Mass spectrometry PY - 2019 AN - OPUS4-49435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - New reference material candidates for traceable size measurement of non-spherical nanoparticles N2 - New model nanoparticles with well-controlled shape were synthesized within the EMPIR project nPSize - Improved traceability chain of nanoparticle size measurements. Their systematic characterization takes place by the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering. Following reference nanoparticle candidates are under investigation with respect to their homogeneity and stability: titania nanoplatelets (10-15 nm x 50-100 nm), titania bipyramides (~60 nm x 40 nm), titania acicular particles (100 nm x 15-20 nm; aspect ratio 5.5/6), gold nanorods (~10 nm x 30 nm), and gold nanocubes (~55 nm x 55 nm x 55 nm). T2 - HyMET Workshop on optical surface analysis methods for nanostructured layers CY - Berlin, Germany DA - 10.10.2019 KW - Nanoparticles KW - Reference materials KW - Traceability KW - Particle size distribution PY - 2019 AN - OPUS4-49285 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - Novel insights into high temperature corrosion phenomena by advanced X-ray methods N2 - A variety of materials of technological interest change their properties through contact with reactive media. Solid-gas reactions lead to a variety of reaction products on the surfaces and internal interfaces. The observation of nucleation and growth processes in the environment where they occur (in situ) from a chemical-structural perspective is especially challenging for aggressive atmospheres. The talk presents innovative approaches to study corrosion mechanisms using advanced X-ray methods. Using energy dispersive X-ray diffraction and X-ray absorption spectroscopy in different tailor made environmental reaction chambers, valuable insights into high temperature oxidation and sulfidation processes were gained. Fe-based alloys were exposed to hot and reactive atmospheres containing gases like SO2, H2O and O2 at 650°C. During the gas exposure the tailor made reaction chambers were connected to a high energy diffraction end station at the synchrotron. The crystallization and growth of oxide and sulfide reaction products at the alloy surfaces were monitored by collecting full diffraction pattern every minute. Careful examination of shape and intensity of phase-specific reflections enabled to a detailed view on growth kinetics. These studies showed, oxides are the first phases occurring immediately after experimental start. As soon as reactive gas media enter the chamber, the conditions change and different reaction products, such as sulfides start to grow. A comparison of different gas environments applied, illustrated the differences in the type of reaction products. The in situ observation of high temperature material degradation by corrosion made it possible to study the contribution of phases, which are not stable at room temperature. For instance, wuestite (Fe1-xO), was frequently observed at high temperatures in humid gases on Fe with 2 wt.% and 9 wt.% chromium, but not at room temperature. The strength of the occurrence of this phase additionally explains why, despite a higher Cr content, ferritic alloys with 9 wt.% Cr in a challenging atmosphere prevent the intrinsic formation of protective layers. The in situ observations were supplemented by careful considerations of thermodynamic boundary conditions and detailed post characterization by classical metallographic analysis. Additionally, the structure and chemistry of the dominant oxide layers were evaluated using X-ray absorption near edge structure spectroscopy. The talk will give an overview about chances and challenges for studying high temperature corrosion phenomena by advanced X-ray methods. T2 - MRS Spring Meeting CT08.02.01 CY - Online Meeting DA - 18.04.2021 KW - XRD KW - Spectroscopy KW - Corrosion KW - High temperature KW - In-situ PY - 2021 AN - OPUS4-52486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bäßler, Ralph T1 - Preliminary Study on Al2O3 Sol-Gel Coating for Corrosion Protection of Martensitic Stainless Steel in Artificial Geothermal Water N2 - Al2O3 coatings are often used as protective layers on steels against electrochemical and high-temperature corrosion because they are chemically inert and stable at elevated temperatures. This study presents preliminary work on the possibilities of using Al2O3 sol-gel coatings for corrosion protection of martensitic stainless steels in geothermal environments. Al2O3 sol-gel coatings were applied on UNS S42000, which is known to be susceptible to uniform and localized corrosion. The coated steel specimens were then tested in two types of artificial geothermal water, which simulate the geothermal fluids found in Sibayak (SBY), Indonesia, and North German Basin (NGB), Germany, respectively. SBY has pH 4 and 1.5 g/L of chloride ions, whereas NGB has a pH of 6 and 166 g/L of chloride ions. All experiments were carried out in autoclaves at 150 °C and 1 MPa under the deaerated condition. Evaluations were performed by investigating the surface profiles of both uncoated and coated steels before and after the corrosion test using a Laser Scanning Microscope (LSM) and Scanning Electron Microscope (SEM). Finally, Electrochemical Impedance Spectroscopy (EIS) was performed to compare the corrosion resistance of Al2O3 coated steels in SBY and NGB solutions. It was observed from the corrosion test that Al2O3 coatings are more suitable for use in the geothermal water with a higher pH. T2 - AMPP Annual International Corrosion Conference 2021 CY - Online Meeting DA - 19.04.2021 KW - Protective coating KW - Sol-gel coating KW - Geothermal KW - Martensitic steel KW - Corrosion PY - 2021 AN - OPUS4-52500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ciornii, Dmitri T1 - Knowledge, Information and Data Readiness Levels (KaRL) approach for Nanorisk Governance N2 - Nanomaterials may have brought many beneficial innovations with them in our daily lives and and have become indispensable for the society. However, one needs to be concerned of the risks which are still unknown and not sufficietly studied and therefore there is a need for a nanorisk governance. At the core of nanorisk governance is gathering, processing and analysing reliable data which will be used for decision making. The challenge is to assure data reliability and transform it into knowledge. To address this challenge, we used analogy to technology readiness level (TRL) approach (developed by NASA), and elaborated knowledge readiness level (KaRL). KaRL is a nine-scale system to categorize data and knowledge (documents) into levels of readiness for particular purposes and to enhance readiness level by using quality and completeness filters, compliance requirements, nanorisk-related tools, stakeholders’ input. By our approach we addressed key issues in nanotechnology such as societal and ethical concerns, circular economy and sustainability, traceability of data, knowledge and decisions. T2 - EC - HORIZON EUROPE NMBP-13 Joint Conference Risk Governance of nanotechnology CY - Online meeting DA - 12.04.2021 KW - Knowledge Readiness Level KW - Nanorisk KW - Nanomaterials KW - Data PY - 2021 AN - OPUS4-52471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement; What nPSize can offer to CEN/TC 352? N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, inter-laboratory comparisons) as pertinent contributions to normative projects within CEN/TC 352 Nanotechnologies are discussed. E.g. the first technical report of nPSize on full algorithm sequences for nanoparticle detection and size measurement as developed on both a physical basis (SEM, TSEM, AFM and SAXS) and by machine learning is put at disposal. T2 - 29th Meeting of CEN/TC 352 Nanotechnologies CY - Online meeting DA - 25.03.2021 KW - Nanoparticles KW - Electron microscopy KW - CEN/TC 352 Nanotechnologies KW - Particle size distribution KW - Modelling KW - Machine learning PY - 2021 AN - OPUS4-52464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Advanced characterization of nanomaterials N2 - The rational synthesis and use of nanomaterials require the characterization of many different properties, ranging from particle size and size distribution over surface chemistry to more applicationrelevant features like optical, electrochemical, and magnetic properties. In the following, several methods for the characterization of functional groups on nanomaterials, like polymer and silica nanoparticles, semiconductor quantum dots, and lanthanide-based upconversion nanocrystals are presented. Additionally, procedures for the measurement of the key spectroscopic performance parameters of nanomaterials with linear and nonlinear photoluminescence, such as the photoluminescence quantum yield, are presented for the UV/vis/NIR/SWIR. T2 - Summerschool CY - Bad Honnef, Germany DA - 22.07.2019 KW - Quantum yield KW - Nanoparticle KW - Fluorescence KW - Quantum dot KW - NIR KW - SWIR KW - Quality assurance KW - Calibration PY - 2019 AN - OPUS4-48630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - Unravelling high temperature oxidation phenomena by in situ x-ray techniques N2 - Unravelling high temperature oxidation phenomena by in situ x-ray techniques. A multi techqnique approach to study high temperature gas corrosion is presented. T2 - Gordon Research Conference on High Temperature Corrosion CY - New London, NH, USA DA - 20.07.2019 KW - Corrosion KW - High temperature KW - Diffraction KW - Spectroscopy PY - 2019 AN - OPUS4-48772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Spectroscopic ellipsometric analysis of elemental composition and porosity of mesoporous iridium-titanium mixed oxide thin films for electrocatalytic splitting of water N2 - Porous materials play an important role in several fields of technology, especially for energy applications like photovoltaics, electrolysis or batteries. The activity of porous films is affected by properties like porosity, film thickness, chemical composition of the material as well as the crystallinity of the framework. The complex morphology of such porous films constitutes a challenge for modern analytical techniques and requires approaches employing the combination/complementation of data of different analytical methods. In this contribution we characterize thin mesoporous iridium-titanium mixed oxide film properties by spectroscopic ellipsometry (SE). Mesoporous iridium oxide - titanium oxide (IrOx-TiOx) films were prepared via dip-coating of a solution containing a triblock-copolymer as structure-directing agent, an iridium precursor as well as a titanium precursor in ethanol. Deposited films with different amounts of iridium (0 wt%Ir to 100 wt%Ir) were synthesized and calcined in air. The thin films were analyzed with SE using the Bruggeman effective medium approximation (BEMA) for modelling. The results were compared with electron probe microanalysis (EPMA) as part of a combined SEM/EDS/STRATAGem Analysis. T2 - 8th International conference on spectroscopic ellipsometry (ICSE-8) CY - Barcelona, Spain DA - 26.05.2019 KW - Mesoporous iridium-titanium mixed oxides KW - Thin films KW - Spectroscopic ellipsometry KW - Oxygen evolution reaction KW - EPMA KW - Ellipsometric porosimetry PY - 2019 AN - OPUS4-48387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - High-Quality Experimental Data in Electron Microscopy and Microanalysis – What can, and should we jointly do? N2 - There are different ways how to prove the quality of the results obtained by electron microscopy and related microanalysis techniques, e.g. use of validated standard operation procedures, participation in proficiency testing exercises, use of certified reference materials, etc. International standards are able to provide requirements, specifications, guidelines or characteristics of methods, instruments or samples with the final goal that these can be used consistently in accredited laboratories. In the field of electron microscopy and microbeam analysis standardization and metrology are terms which are encountered rather seldom at major conferences and scientific publications. Nevertheless, spectra formats like EMSA/MSA for spectral-data exchange or tagged image file format (TIFF) for SEM, guidelines for performing quality assurance procedures or for the specification of X-ray spectrometers as well as of certified reference materials (CRMs) in EPMA, or measurement of average grain size by electron backscatter diffraction (EBSD), or guidelines for calibrating image magnification in SEM or TEM are ISO standards already published and used successfully by a large part of the electron microscopy and microbeam analysis community. A main and continuous task of ISO/TC 202 and its subcommittees is to identify and evaluate feasible projects/proposals needed to be developed into new international standards, particularly in respect to recent but established technology, such the silicon drift detector (SDD) EDS one. Another international platform in the frame of which pre-standardization work can be organized is VAMAS (Versailles Project on Advanced Materials and Standards). International collaborative projects involving aim at providing the technical basis for harmonized measurements, testing, specifications, and standards to be further developed at ISO level. One key point of VAMAS activities is constituted by inter-laboratory comparisons for high-quality data. In the field of microbeam analysis, the technical working area (TWA) 37 Quantitative Microstructural Analysis deals with corresponding projects. Good ideas, e.g. on analysis of low-Z materials/elements and at low energies are particularly encouraged by directly contacting the author. Support and already available guidance will be supplied. T2 - Microscopy & Microanalysis 2019 CY - Portland, OR, USA DA - 03.08.2019 KW - Pre-standardisation KW - Inter-laboratory comparison KW - VAMAS KW - ISO KW - Electron microscopy KW - Microanalysis PY - 2019 AN - OPUS4-48672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Omar, Hassan A1 - Hiid, Gundula A1 - Szymoniak, Paulina A1 - Hertwig, Andreas A1 - Schönhals, Andreas T1 - Growth kinetics of the adsorbed layer of poly(bisphenol A carbonate) and its effect on the glass transition behavior in thin films N2 - The glass transition behavior of thin films of poly(bisphenol A carbonate) (PBAC) was studied employing ellipsometry. The glass transition temperature increases with the reduction of the film thickness. This result is attributed to the formation of an adsorbed layer with a reduced mobility compared to bulk PBAC. Therefore, for the first time, the growth kinetics of the adsorbed layer of PBAC was investigated, prepared by leaching samples from a 200 nm thin film which were annealed for several times at three different temperatures. The thickness of each prepared adsorbed layer was measured by multiple scans using atomic force microscopy (AFM). Additionally, an unannealed sample was measured. Comparison of the measurements of the unannealed and the annealed samples provides proof of a pre-growth regime for all annealing temperatures which was not observed for other polymers. For the lowest annealing temperature after the pre-growth stage only a growth regime with a linear time dependence is observed. For higher annealing temperatures the growth kinetics changes from a linear to a logarithmic growth regime at a critical time. At the longest annealing times the films showed signs of dewetting where segments of the adsorbed film were removed from the substrate (dewetting by desorption). The dependence of the surface roughness of the PBAC surface on annealing time also confirmed that the films annealed at highest temperatures for the longest times desorbed from the substrate. KW - Ultra thin polymer films PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-574531 DO - https://doi.org/10.1039/D3RA02020G SN - 2046-2069 VL - 13 IS - 21 SP - 14473 EP - 14483 PB - RSC Publishing CY - London AN - OPUS4-57453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cakir, Cafer Tufan A1 - Piotrowiak, T. A1 - Reinholz, Uwe A1 - Ludwig, A. A1 - Emmerling, Franziska A1 - Streli, C. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin T1 - Exploring the Depths of Corrosion: A Novel GE-XANES Technique for Investigating Compositionally Complex Alloys N2 - In this study, we propose the use of nondestructive, depth-resolved, element-specific characterization using grazing exit X-ray absorption near-edge structure spectroscopy (GE-XANES) to investigate the corrosion process in compositionally complex alloys (CCAs). By combining grazing exit X-ray fluorescence spectroscopy (GE-XRF) geometry and a pnCCD detector, we provide a scanning-free, nondestructive, depth-resolved analysis in a sub-micrometer depth range, which is especially relevant for layered materials, such as corroded CCAs. Our setup allows for spatial and energy-resolved measurements and directly extracts the desired fluorescence line, free from scattering events and other overlapping lines. We demonstrate the potential of our approach on a compositionally complex CrCoNi alloy and a layered reference sample with known composition and specific layer thickness. Our findings indicate that this new GE-XANES approach has exciting opportunities for studying surface catalysis and corrosion processes in real-world materials. KW - Degradation mechanisms KW - Grazin exit XANES KW - Depth resolved XANES KW - Compositional complex alloys KW - Corrosion PY - 2023 DO - https://doi.org/10.1021/acs.analchem.3c00404 VL - 95 SP - 4810 EP - 4818 PB - ACS Publications AN - OPUS4-57823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fritzsche, Sven A1 - Pauw, Brian Richard A1 - Weimann, Christiane A1 - Sturm, Heinz T1 - First of its kind: A test artifact for direct laser writing N2 - With femtosecond-laser direct writing (fs-LDW) maturing in all aspects as a manufacturing technology, a toolset for quality assurance must be developed. In this work we introduce a first of its kind test artifact. Test artifacts are standardized 3D models with specific geometric features to evaluate the performance of writing parameters. Test artifacts are already common in other 3D additive manufacturing technologies e.g. selective laser melting. The test artifact introduced in this work was developed in particular to accommodate the high geometrical resolution of fs-LDW structures and the limited possibilities to examine the resulting structure. Geometric accuracy, surface adhesion as well as confocal Raman spectroscopy results were considered when evaluating the design of the test artifact. We will explain the individual features and design considerations of our fs-LDW test artifact. The difference between two slicers, Cura and 3DPoli, and the implications on measured feature sizes and the general shape is quantified. The measured geometries are used to derive a general design guide for a specific combination of photoresists, laser power and scanning speed and to analyze the geometric accuracy of a structure produced using these guidelines. The shown test artifact is publicly available as STL file on GitHub (https://github.com/BAMresearch/2PP-TestArtifact) and in the supplement. KW - Laser direct writing KW - Multi photon lithography KW - Reference material KW - Raman spectroscopy KW - Confocal raman imaging KW - Slicers KW - Open data on zenodo PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580951 DO - https://doi.org/10.1088/1361-6501/acc47a VL - 34 IS - 7 SP - 1 EP - 14 PB - IOP Science AN - OPUS4-58095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Yusenko, Kirill A1 - Stawski, Tomasz A1 - Kulow, Anicó A1 - Cakir, Cafer Tufan A1 - Röder, Bettina A1 - Naese, Christoph A1 - Britzke, Ralf A1 - Sintschuk, Michael A1 - Emmerling, Franziska T1 - BAMline - A real-life sample materials research beamline N2 - With increasing demand and environmental concerns, researchers are exploring new materials that can perform as well or better than traditional materials while reducing environmental impact. The BAMline, a real-life sample materials research beamline, provides unique insights into materials’ electronic and chemical structure at different time and length scales. The beamline specializes in x-ray absorption spectroscopy, x-ray fluorescence spectroscopy, and tomography experiments. This enables real-time optimization of material properties and performance for various applications, such as energy transfer, energy storage, catalysis, and corrosion resistance. This paper gives an overview of the analytical methods and sample environments of the BAMline, which cover non-destructive testing experiments in materials science, chemistry, biology, medicine, and cultural heritage. We also present our own synthesis methods, processes, and equipment developed specifically for the BAMline, and we give examples of synthesized materials and their potential applications. Finally, this article discusses the future perspectives of the BAMline and its potential for further advances in sustainable materials research. KW - Extended X-ray absorption fine structure KW - Energy storage KW - Environmental impacts KW - Nondestructive testing techniques KW - X-ray fluorescence spectroscopy KW - Corrosion KW - Near edge X-ray absorption fine structure spectroscopy KW - X-ray absorption spectroscopy PY - 2023 DO - https://doi.org/10.1063/5.0157194 VL - 158 IS - 24 SP - 1 EP - 22 PB - AIP Publishing AN - OPUS4-57824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fiedler, Saskia A1 - Ton-That, C. A1 - Phillips, M. R. T1 - Defect-free ZnO nanorods with high angular distribution for enhanced excitonic emission N2 - AbstractLow-temperature hydrothermal growth has emerged as a popular method for the fabrication of ZnO nanorods (NRs), increasing the functionality and utility of ZnO-based devices. In this work, we study the influence of growth time, temperature and seed layer on the dimensions and angular distribution of ZnO NRs. High-quality NRs with a crisscrossed 60° angular distribution have been grown with a 20–60 nm diameter and 600 nm length. We show that, within the ideal range of growth parameters, the growth time and temperature have no controllable influence on NR diameter and length, while the deposition method and size of the pre-growth deposited ZnO seeds affects diameter and NR angular alignment. We demonstrate advantages of using crisscross-aligned NRs over planar ZnO for the enhancement of ZnO excitonic emission by optical coupling with gold nanoparticles. These results can be readily adapted for applications that involve surface coating-mediated enhancement of both light emission and injection. KW - ZnO nanorod KW - Hydrothermal growth KW - Seed layer KW - Angular distribution KW - Cathodoluminescence KW - Luminescence enhancement PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618176 DO - https://doi.org/10.1557/s43578-023-00941-x SN - 0884-2914 SN - 2044-5326 VL - 38 IS - 8 SP - 2145 EP - 2155 PB - Springer CY - Berlin AN - OPUS4-61817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schardt, Annika A1 - Schmitt, Johannes A1 - Engelhard, Carsten T1 - Single particle inductively coupled plasma mass spectrometry with nanosecond time resolution N2 - In this proof-of-principle study, we present our contribution to single particle inductively coupled plasma mass spectrometry (spICP-MS) developments with a novel in-house built data acquisition system with nanosecond time resolution (nanoDAQ) and a matching data processing approach. The new system can continuously sample the secondary electron multiplier (SEM) detector signal and enables the detection of gold nanoparticles (AuNP) as small as 7.5 nm with the commercial single quadrupole ICP-MS instrument used in this study. Recording of the SEM signal by the nanoDAQ is performed with a dwell time of approximately 4 ns. A tailored method was developed to process this type of transient data, which is based on determining the temporal distance between detector events that is denoted as event gap (EG). We found that the inverse logarithm of EG is proportional to the particle size and that the number of detector events corresponding to a particle signal distribution can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. Due to the high data acquisition frequency, a statistically significant number of data points can be obtained in 60 s or less and the main time limitation for analyses is merely the sample uptake time and rinsing step between analyte solutions. At this stage, the data processing method provides average information on complete data sets only and will be adapted to enable particle-by-particle analysis with future hardware/software revision. KW - ICP-MS KW - Nanoparticles KW - Nanosecond time resolution KW - Single particle detection PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612706 DO - https://doi.org/10.1039/d3ja00373f SN - 1364-5544 SN - 0267-9477 VL - 39 IS - 2 SP - 389 EP - 400 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-61270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. A1 - Weidner, Steffen A1 - Meyer, A. T1 - About alcohol-initiated polymerization of glycolide and separate crystallization of cyclic and linear polyglycolides N2 - Alcohol-initiated polymerizations of glycolide (GL) catalyzed by tin(II) 2-ethylhexanoate (SnOct2) were carried out in bulk with variation of GA/In ratio, temperature and time. Due to a rather strong competition of cyclization polyglycolide (PGA) free of cycles were never obtained. When the cyclic catalysts 2,2-dibutal-2-stanna − 1,3-dithiolane (DSTL) or 2-stanna 1,3-dioxo-4,5,6,7 bibenzepane (SnBiph) were used in combination with 1,4-butanediol the influence of cyclization was even stronger. Furthermore, the degrees of polymerization were higher than the GA/alcohol ratio due to rapid polycondensation in the solid state. At 160 °C or below, the matrixassisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectra indicated separate crystallization of low molar mass cyclic and linear PGAs from the same reaction mixture (also observed for poly(L-lactide)s). KW - MALDI TOF MS KW - Polyglycolide KW - Ring opening polymerization KW - Cyclization KW - Crystallization PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-607282 DO - https://doi.org/10.1016/j.polymer.2024.127440 SN - 0032-3861 VL - 309 SP - 1 EP - 9 PB - Elsevier Ltd. AN - OPUS4-60728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schardt, Annika A1 - Schmitt, Johannes A1 - Engelhard, Carsten T1 - Cover image for the article "Single particle inductively coupled plasma mass spectrometry with nanosecond time resolution" N2 - Image for the front cover of the issue 39(2) of the JAAS (Journal of Analytical Atomic Spectrometry). See Annika Schardt et al., pp. 389–400. Image reproduced by permission of Annika Schardt, Johannes Schmitt and Carsten Engelhard. KW - Analytical chemistry KW - Nanoparticles KW - Single-particle characterization KW - Instrumentation KW - spICP-MS PY - 2024 DO - https://doi.org/10.1039/D4JA90005G SN - 1364-5544 SN - 0267-9477 VL - 39 IS - 2 SP - 295 PB - Royal Society of Chemistry (RSC) CY - Cambridge AN - OPUS4-62156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andreato, E. A1 - Panov, N. A1 - Artiga, A. A1 - Osipova, Viktoriia A1 - Resch-Genger, Ute A1 - Ximendes, E. A1 - Molina, P. A1 - Canton, P. A1 - Marin, R. T1 - Indium-Based Fluoride Nanoparticles Doped with Chromium for Near-Infrared Luminescence N2 - Transition metal (TM) and rare earth (RE) ion-doped nanoparticles (NPs) are photoluminescent materials of technological relevance in bioimaging, sensing, and light conversion. Fluoride NPs are particularly attractive in this context, since they combine low-energy phonons, high chemical stability, optical transparency, size, and architecture tunability. Yet, nearly all reported colloidal fluoride NPs (e.g., NaYF4 and LiYF4) can only be efficiently doped with RE3+ and not with luminescent TM ions. Herein, we contribute to filling this gap in materials science by reporting Na3InF6 NPs doped with Cr3+ as a model luminescent TM ion. We unveil the heat-driven NP formation mechanism, which involves a cubic-to-monoclinic phase conversion, similarly to the cubic-tohexagonal phase conversion in NaYF4. Reaction temperatures above 225 °C and reaction time have a limited impact on the NP morphology, while the amount of fluoride precursor and oleylamine grants control over the NP size. After verifying that Na3InF6 NPs show negligible cytotoxicity toward U-87 cell line, we study the optical properties of these NPs upon Cr3+ doping. Temperature-dependent photoluminescence measurements indicate that Cr3+ ions experience a weak crystal field in the Na3InF6 host lattice, while their photoluminescence lifetime varies linearly in the 20−50 °C range. These results set the ground for further studies of photoluminescent TM-doped fluoride NPs, toward their applications in bioimaging, sensing, and light-converting devices. KW - Quality assurance KW - Fluorescence KW - Traceability KW - Nano KW - Particle KW - Synthesis KW - Quantum yield KW - NIR KW - Mechanism KW - Characterization KW - XRD KW - Phase transition KW - Ligand KW - Surface KW - Doping KW - Lifetime PY - 2025 DO - https://doi.org/10.1021/acs.chemmater.4c03335 SN - 1520-5002 SP - 1 EP - 14 PB - American Chemical Society AN - OPUS4-63073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - Syntheses of cyclic polylactides and the problem of catenane formation N2 - Cyclic poly(L-lactide)s (PLAs) were prepared in bulk either by ring-expansion polymerization (REP) or by ring-opening polymerization (ROP) with simultaneous polycondensation (ROPPOC). In contrast to REP the latter method involves formation of linear chains and thus, may involve formation of polydisperse catenanes that affect crystallization. The reprecipitated PLAs were annealed at 120 °C and compared with regard to melting temperature (Tm) and melting enthalpy (ΔHm). For similar molar masses the PLAs prepared by REP and ROPPOC had almost identical Tm's and crystallinities. Furthermore, the influence of REP and ROPPOC catalysts on the morphology of the virgin reaction products was compared. KW - MALDI-TOF MS KW - Catenane KW - Polylactide PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625061 DO - https://doi.org/10.1039/d4ra08683j VL - 15 IS - 5 SP - 3686 EP - 3692 PB - RSC AN - OPUS4-62506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - Analysis of Lamb wave mode repulsion and its implications to the characterisation of adhesive bonding strength N2 - Lamb waves are widely used for non-destructive evaluation of material parameters as well as for detection of defects. Another application of Lamb waves is quality control of adhesive joints. Researchers are currently investigating shear horizontal and zero-group velocity modes for characterisation of the adhesive bonding strength. In a new approach, Lamb wave mode repulsion is used to obtain the coupling strength between different layers to characterise the adhesive bonding strength. The modes of the individual layers become coupled in the multilayered systems forming particular regions, the so-called mode repulsion regions. This study investigates these modes and their interaction in two-layered plate-like structures with varying coupling strength both numerically, with the Scaled Boundary FEM, and experimentally. T2 - International Congress on Ultrasonics CY - Bruges, Belgium DA - 03.09.2019 KW - Lamb waves KW - Multi-layered system KW - Adhesive joint KW - Mechanical strength KW - Scaled Boundary FEM PY - 2019 AN - OPUS4-48910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian T1 - Untersuchung der Beständigkeit additiv gefertigter Bauteile mit Thermografie nach künstlicher Bewitterung N2 - Additiv gefertigte Prüfkörper aus Polyamid 12 (Laser Sinter Verfahren) und Acrylnitril-Butadien-Styrol (Fused Layer Modeling Verfahren) wurden über 2000 Stunden künstlich bewittert und ihr Alterungsverhalten untersucht. Die Ergebnisse wurden anschließend mit denen von Prüfkörpern verglichen, welche auf dieselbe Weise künstlich bewittert, aber mittels konventionellem Kunststoff-Spritzguss hergestellt wurden. Die Erkenntnisse dienen für die Entwicklung einer Strategie für eine Qualitätskontrolle von additiv gefertigten Kunststoffteilen. T2 - 48. Jahrestagung der Gesellschaft für Umweltsimulation e.V. (GUS) CY - Stutensee-Blankenloch, Germany DA - 27.03.2019 KW - Additive Fertigung KW - Künstliche Bewitterung KW - Thermografie KW - Zerstörungsfreie Prüfung KW - Additive manufacturing KW - Kunststoffe PY - 2019 AN - OPUS4-48328 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Fritzsche, Sven A1 - Weimann, Christiane A1 - Pauw, Brian Richard A1 - Sturm, Heinz T1 - 2PP-TestArtifact N2 - This repository contains a test artifact (TA), also called test structure, designed for two-photon polymerization (also known as Direct Laser Writing (DLW) or Two/Multi-photon lithography (2PA/MPA)). Test artifacts can be used to compare structures, to check options used by the slicer, check the state of the 2PP machine itself or to get a construction guidelines for a certain combination of power, velocity and settings. The associated paper can be found here: https://dx.doi.org/10.1088/1361-6501/acc47a General ideas behind the test artifact: 1. optimized for 2PP-DLW 2. should be fast and easy to analyse with optical microscopy or 3. scanning electron microscopy without tilt. 3. short time to fabricate 4. include a reasonable amount of different features 5. bulk and small structures on the substrate KW - Reference structure KW - Calibration structure KW - Test structure KW - Laser writing KW - Two-photon polymerization KW - 3D printing KW - Additive manufacturing KW - Microprinting KW - Multi-photon light structuring PY - 2023 DO - https://doi.org/10.6084/m9.figshare.22285204.v2 PB - Digital Science CY - Cambridge, MA, USA AN - OPUS4-57165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - View into the depths of copolymer microstructure by a special approach of LC-MS data evaluation N2 - It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. This is and will remain a challenge for analysts. First a very short overview will be given concerning the common liquid separation techniques for polymers (SEC, LAC, LCCC, GELC) coupled to soft ionization mass spectrometric methods like MALDI and ESI-MS with focus on their limitations. For very broadly distributed samples or chemical very similar species the superposition of different separation mechanisms in chromatography is unavoidable or the separation efficiency cannot be optimized. Different ionization probabilities and species of the same nominal mass with completely different structures are just two problems of mass spec of complex polymer mixtures. Subsequently, different examples will be shown how these limitations in some cases could be outsmarted. First example will be the separation of statistical EO-PO copolymers of different chemical compositions by end group functionality and the quantification of end group fractions over the whole CCD. Here an UP-LCCC / ESI-TOF-MS coupling is applied. Further for different kinds of polymers it will be shown how it could be realized to obtain information on small isobaric/isomeric topological heterogeneities by coupling UP-SEC / ESI-TOF-MS. All results are based on the data processing of reconstructed ion chromatograms of single mass traces of complex ESI-MS spectra. T2 - SCM-9 CY - Amsterdam, The Netherlands DA - 29.01.2019 KW - Reconstructed ion chromatograms KW - Copolymer KW - Microstructure KW - LC x ESI-TOF-MS PY - 2019 AN - OPUS4-47836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Surface and Microbeam Analytical Methods @BAM N2 - An overview of the activities in the field of surface and microbeam analysis at BAM-6.1 is given with focus on physico-chemical characterization at the nanoscale. Ideas of potential joint activities are presented: structural and chemical analysis of graphene, deposition techniques for nanoparticles, EBSD on steel for a broader range of methods, instruments and types of steel, soft X-ray Analysis of low-Z materials, analysis of mesoporous thin films, etc. T2 - BAM-IFW Workshop CY - Dresden, Germany DA - 28.03.2019 KW - PC characterisation KW - Nanoscale KW - Nanoparticles PY - 2019 AN - OPUS4-47860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steinhoff, U. A1 - Hodoroaba, Vasile-Dan T1 - EMPIR Erläuterung der Fördermaßnahme und Beispiele aus der Nanotechnologie N2 - Das EMPIR-Förderprogramm wird kurz erläutert und laufende Projekte aus der Nanotechnologie werden vorgestellt. Der Schwerpunkt liegt auf Standardisierungsprojekten, die gemeinsam mit ISO/TC 229 'Nanotechnologies' und CEN/TC 352 'Nanotechnologies' zu neuen Normen führen sollten. Als Beispiel für laufende Nanotechnologie-Projekte mit Koordination aus Deutschland werden MagNaStand (PTB) und nPSize (BAM) gegeben. T2 - Treffen des Normungsausschusses NA 062-08-17 AA Nanotechnologien CY - KIT, Karlsruhe, Germany DA - 07.03.2019 KW - EMPIR KW - Nanoparticles KW - Reference materials KW - Particle size distribution KW - Traceability KW - Standardisation PY - 2019 AN - OPUS4-47859 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Everything SAXS N2 - Introduction keynote for the "Small Angle Scattering Training School 2019", introducing a wide range of aspects around small-angle scattering. T2 - Small Angle Scattering Training School 2019 CY - Diamond Light Source, Didcot, UK DA - 04.06.2019 KW - X-ray scattering KW - Nanostructure KW - Introduction KW - Practical aspects PY - 2019 AN - OPUS4-48191 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Quantitative microstructural analysis - VAMAS/TWA 37 N2 - The 44th Meeting of the Versailles Project on Advanced Materials and Standards (VAMAS) Steering Committee has just taken place at NIST in Boulder (CO, USA). BAM participates with significant contributions in Technical Working Areas on nanoparticle and surface chemistry characterization, but also has positioned itself to new global material challenges and trends in the developement of advanced materials and their characterization, such as thermal properties, self-healing materials, and micro- and nanoplastic. T2 - Annual Meeting of the Versailles Project on Advanced Materials and Standards (VAMAS) Steering Committee CY - Boulder, CO, USA DA - 22.05.2019 KW - VAMAS KW - Nanoparticles KW - Microbeam analysis KW - Advanced materials PY - 2019 AN - OPUS4-48184 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bäßler, Ralph T1 - Factors Influencing Droplet Corrosion in Dense Phase CO2 N2 - This work examined the factors that influence the droplet corrosion of CO2 pipeline steels caused by oxyfuel flue gases in dense phase CO2 at 278 K, simulating the underground transport conditions. The wetting properties were studied by contact angle measurement, revealing pH and time dependency on the reactive wetting behaviors of carbon steel X70. Exposure tests with CO2 saturated water droplet on steel surface showed that the impurities (220 ppmv SO2 and 6700 ppmv O2) diffused into the droplet and then reacted with metal surfaces in dense phase condition, forming the corrosion products. The corrosion rate was confirmed strongly depending on the droplet volume as well as the SO2 concentration. Condensation experiments carried out on freshly polished coupons in CO2 with 200 ppmv H2O, 220 ppmv SO2 and 6700 ppmv O2, showed that the formation and aggregation of droplets is time and temperature dependent. At 278 K, condensation happened stronger and the corrosion products, mainly consisted of dense hydrated FeSO3/FeSO4. While at 288 K, more fluffy corrosion products consisting of iron oxide/hydroxide and hydrated FeSO3/FeSO4 were found. Further exposure tests on carbon steel coupons with different surface roughness did not reveal the difference in weight loss/gain and therefore the corrosion rate. T2 - NACE International Corrosion Conference 2019 CY - Nashville, TN, USA DA - 24.03.2019 KW - Carbon Capture, Utilization and Storage (CCUS) KW - Supercritical/dense phase CO2 KW - Carbon steel KW - Droplet corrosion KW - Condensation PY - 2019 AN - OPUS4-47916 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Aristia, Gabriela T1 - Electrochemical measurement of polyaniline containing coating at high temperature: PROBLEMS AND CHALLENGES N2 - This presentation describes special aspects when performing measurements at high temperatures. Especially electrochemical issues are addressed for impedance spectroscopy, like overlapping time constants, handling of noise etc. T2 - Electrochemical Doctoral School “Corrosion: from analysis to modelling” CY - Brussels Belgium DA - 04.02.2019 KW - Polyaniline KW - Geothermal KW - Electrochemical impedance spectroscopy PY - 2019 AN - OPUS4-47917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - McSAS for SAS analysis: Usage, benefits, and potential pitfalls N2 - Introducing McSAS, the analytical tool (software) we developed for extracting form-free size distributions from X-ray scattering patterns. T2 - Small Angle Scattering Training School 2019 CY - Diamond Light Source, Didcot, UK DA - 04.06.2019 KW - X-ray scattering KW - SAXS KW - Software KW - Monte Carlo KW - Nanocharacterisation KW - Nanostructure PY - 2019 AN - OPUS4-48192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hodoroaba, Vasile-Dan A1 - Unger, Wolfgang A1 - Shard, A. G. ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Conclusions and perspectives N2 - This chapter briefly summarizes the methods selected within this book for the characterization of nanoparticles with regard to commonly accessible properties: nanoparticle size and size distribution, shape, surface area, surface charge, aggregation state, structure, chemical composition, surface chemistry, and nanoparticle number concentration. Current progress of measurement and analysis, as far as possible according to standard operation procedures, has been the focus of this work. A number of new and less commonly used methods have not been covered, and we outline some of these in this chapter. Future challenges such as automated measurement and analysis, read-across approaches for the prediction of properties, knowledge of measurement uncertainties, the need for certified reference materials, and the necessity to complement measurements methods to obtain more reliable results are covered, and the unmet measurement requirements for real-world nanoparticles are described. KW - Physicochemical characterization KW - Standard operation procedures KW - Data correlation KW - Method development KW - Trends PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00006-7 SP - 527 EP - 534 PB - Elsevier CY - Amsterdam AN - OPUS4-50167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Shard, A. G. A1 - Hodoroaba, Vasile-Dan A1 - Unger, Wolfgang ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Introduction N2 - The purpose of this book is to provide a comprehensive collection of analytical methods that are commonly used to measure nanoparticles, providing information on one, or more, property of importance. The chapters provide up-to-date information and guidance on the use of these techniques, detailing the manner in which they may be reliably employed. Within this chapter, we detail the rationale and context of the whole book, which is driven by the observation of a low level of reproducibility in nanoparticle research. The aim of the book is to encourage awareness of both the strengths and weaknesses of the various methods used to measure nanoparticles and raise awareness of the range of methods that are available. The editors of the book have, for many years, been engaged in European projects and standardization activities concerned with nanoparticle analysis and have identified authors who are experts in the various methods included within the book. This has produced a book that can be used as a definitive guide to current best practice in nanoparticle measurement. KW - Nanoparticles KW - Size distribution KW - Shape KW - Chemistry KW - Coating KW - Concentration KW - Standards KW - Charge KW - Characterisation PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00001-8 SP - 1 EP - 6 PB - Elsevier CY - Amsterdam AN - OPUS4-50166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterization of co (polyamide)s N2 - Characterization problems of technically relevant copolyamides applying size exclusion chromatography, interaction chromatography and their combination with MALDI-TOF-MS will be discussed. T2 - 23. Kolloquium Massenspektrometrie und synthetische Polymere CY - Berlin, Germany DA - 14.05.2019 KW - LCCC KW - Mass spectrometry of polymers KW - SEC KW - LC / MALDI-TOF-MS coupling PY - 2019 AN - OPUS4-48221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lugovtsova, Yevgeniya T1 - Analyse der Ausbreitung geführter Wellen in einem Mehrschichtverbund zur Zustandsüberwachung von Composite-Druckbehältern N2 - Composite-Druckbehälter werden für Speicherung und Transport von Gasen unter hohem Druck verwendet. Durch die gewichtssparende Struktur, die aus einem dünnwandigem Metallgefäß und Faserverbundwerkstoff-Ummantelung besteht, sind solche Behälter insbesondere für die Luftfahrt- und Automobilindustrie interessant, z.B. als Wasserstoffspeicher. Die Druckprüfung ist ein konventioneller Test, um die Integrität von Metalldruckbehältern zu bewerten. Im Falle des Composite-Druckbehälters könnte eine solche Prüfung jedoch den Faserverbundwerkstoff überbeanspruchen und somit die verbleibende Lebensdauer der getesteten Komponente verringern. Infolgedessen ist es notwendig, Verfahren zur zerstörungsfreien Prüfung und möglicherweise zur Zustandsüberwachung von Composite-Druckbehältern zu entwickeln. Unser Ansatz verwendet geführte Ultraschallwellen und hat das Potenzial, kritische Schäden wie Risse im Metall und Faserbrüche und Matrixrisse in Faserverbundwerkstoff zu detektieren. In diesem Beitrag wurde die Scaled Boundary Finite Elemente Methode benutzt, um die multimodale, geführte Wellenausbreitung in einem Mehrschichtverbund, der aus Metall und Kohlenfaserverbund entsteht, zu analysieren. Das Verfahren ermöglicht die Identifizierung geeigneter Wellenmoden und die Analyse ihrer Interaktion mit verschiedenen Schäden. Diese Kenntnisse sollen für die Entwicklung von Verfahren zur Zustandsüberwachung von Composite-Druckbehältern angewendet werden. T2 - 22. Kolloquium Schallemission und 3. Anwenderseminar Zustandsüberwachung mit geführten Wellen CY - Karlsruhe, Germany DA - 27.03.2019 KW - Wasserstoffspeicher KW - Automobilindustrie KW - SBFEM KW - Faserverbundwerkstoff KW - Ultraschallwellen PY - 2019 AN - OPUS4-47689 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gao, S. A1 - Hou, J. A1 - Deng, Z. A1 - Wang, T. A1 - Beyer, Sebastian A1 - de Oliveira Guilherme Buzanich, Ana A1 - Richardson, J. J. A1 - Rawal, A. A1 - Seidel, R. A1 - Zulkifli, M. Y. A1 - Li, W. A1 - Bennett, T. D. A1 - Cheetham, A. K. A1 - Liang, K. T1 - Improving the Acidic Stability of Zeolitic Imidazolate Frameworks by Biofunctional Molecules N2 - Zeolitic imidazolate frameworks (ZIFs) have been widely investigated for their use in separation, gas adsorption, catalysis, and biotechnology. Their practical applications, however, can be hampered by their structural instability in humid acidic conditions. Here, guided by density functional theory calculations, we demonstrate that the acidic stability of two polymorphic ZIFs (i.e., ZIF-8 and ZIF-L) can be enhanced by the incorporation of functional groups on polypeptides or DNA. A range of complementary synchrotron investigations into the local chemical structure and bonding environment suggest that the enhanced acidic stability arises from the newly established coordinative interactions between the Zn centers and the inserted carboxylate (for polypeptides) or phosphate (for DNA) groups, both of which have lower pKas than the imidazolate ligand. With functional biomolecular homologs (i.e., enzymes), we demonstrate a symbiotic stability reinforcement effect, i.e., the encapsulated biomolecules stabilize the ZIF matrix while the ZIF exoskeleton protects the enzyme from denaturation. KW - Zeolitic Imidazolate Frameworks KW - Biofunctional Molecules KW - X-ray Absorption Spectroscopy PY - 2019 DO - https://doi.org/10.1016/j.chempr.2019.03.025 VL - 5 IS - 6 SP - 1597 EP - 1608 PB - Elsevier Inc. AN - OPUS4-48702 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Fujimoto, T. T1 - The Surface Analysis Working Group at the Consultative Committee for Amount of Substance, Metrology in Chemistry and Biology: A successful initiative by Martin Seah N2 - Dr Martin Seah, NPL, was the initiator, founder, and first chairman of the Surface Analysis Working Group (SAWG) at the Consultative Committee for Amount of Substance, Metrology in Chemistry and Biology (CCQM) at the Bureau International des Poids et Mesures (BIPM), the international organization established by the Metre Convention. This tribute letter summarizes his achievements during his chairmanship and his long-running impact on the successful work of the group after his retirement. KW - CCQM (Consultative Committee for Amount of Substance) KW - Metrology in Chemistry and Biology KW - Martin Seah KW - Metrology KW - Quantitative surface chemical analysis KW - Surface Analysis Working Group PY - 2021 DO - https://doi.org/10.1002/sia.7033 SN - 0142-2421 VL - 54 IS - 4 SP - 314 EP - 319 PB - John Wiley & Sons Ltd AN - OPUS4-53714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred T1 - EDX-Analysis on medieval glasses and innovative protection of stained glass panels N2 - The church of Koszewko (Poland) is a brick building edified in the 15th century built on cobblestone foundations. There are five windows in the sanctuary. Three of them enclose heraldic panels from the Küssow’s family from the 15th century which are surrounded with Goethe glass from the 18th century to complete the windows. The colored heraldic panels are strongly damaged and corroded with massive paint layer losses, glass- and leadbreakages. Those medieval glass fragments have been shortly discovered and are of particular interest for Poland since only few medieval glazing have been conserved. The damages as well as the glass compositions have been investigated with ESEM/EDX. Two categories of medieval glass compositions have been identified. The blue glass is particularly sensible to corrosion because of his high content in K2O. The colorless and the red glass samples belong to a stable glass type. Due to the thickness of the gel layer, it is easy to see that the degradation is strongly proceeded. The protection of those medieval stained-glass panels is absolute necessary. The medieval panels have been restored and surrounded from a copper frame. Then they have been fixed on the wood frame in the church. The exterior glazing has been closed with a panel of Goethe glass. The gap between the Goethe- and the medieval glass is about 3 cm. The Goethe glass panel has been stabilized with a film based on polyester to protect the medieval glasses against any damages. In this way, a low cost protective glazing has been installed for a long-term conservation of each medieval stained-glass panels. The climate measurements over the period of one year on the restored windows are in process. The temperature and the relative humidity are recorded in the church interior, in the gap between the original and the Goethe glass and outdoors. T2 - 93rd Annual Meeting of DGG and Annual Meeting of USTV CY - Nuremberg, Germany DA - 13.05.2019 KW - Medieval glasses KW - Stained glasses KW - EDX Analysis KW - Corrosion PY - 2019 AN - OPUS4-48025 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guday, G. A1 - Donskyi, Ievgen A1 - Gholami, M. F. A1 - Algara-Siller, G. A1 - Witte, F. A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Paulus, B. A1 - Rabe, J. A1 - Adeli, M. A1 - Haag, R. T1 - Scalable Production of Nanographene and Doping via Nondestructive Covalent Functionalization N2 - A new method for top‐down, one‐pot, gram‐scale production of high quality nanographene by incubating graphite in a dilute sodium hypochlorite solution at only 40 °C is reported here. The produced sheets have only 4 at% oxygen content, comparable with nanographene grown by chemical vapor deposition. The nanographene sheets are covalently functionalized using a nondestructive nitrene [2+1] cycloaddition reaction that preserves their π‐conjugated system. Statistical analyses of Raman spectroscopy and X‐ray photoelectron spectroscopy indicate a low number of sp3 carbon atoms on the order of 2% before and 4% after covalent functionalization. The nanographene sheets are significantly more conductive than conventionally prepared nanographene oxide, and conductivity further increases after covalent functionalization. The observed doping effects and theoretical studies suggest sp2 hybridization for the carbon atoms involved in the [2+1] cycloaddition reaction leading to preservation of the π‐conjugated system and enhancing conductivity via n‐type doping through the bridging N‐atom. These methods are easily scalable, which opens the door to a mild and efficient process to produce high quality nanographenes and covalently functionalize them while retaining or improving their physicochemical properties. KW - Graphene KW - XPS KW - NEXAFS PY - 2019 DO - https://doi.org/10.1002/smll.201805430 VL - 15 IS - 12 SP - 1805430 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-48021 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rühle, Bastian A1 - Krumrey, Julian Frederic A1 - Hodoroaba, Vasile-Dan T1 - Workflow towards automated segmentation of agglomerated, non‑spherical particles from electron microscopy images using artificial neural networks N2 - We present a workflow for obtaining fully trained artificial neural networks that can perform automatic particle segmentations of agglomerated, non-spherical nanoparticles from scanning electron microscopy images “from scratch”, without the need for large training data sets of manually annotated images. The whole process only requires about 15 minutes of hands-on time by a user and can typically be finished within less than 12 hours when training on a single graphics card (GPU). After training, SEM image analysis can be carried out by the artificial neural network within seconds. This is achieved by using unsupervised learning for most of the training dataset generation, making heavy use of generative adversarial networks and especially unpaired image-to-image translation via cycle-consistent adversarial networks. We compare the segmentation masks obtained with our suggested workflow qualitatively and quantitatively to state-of-the-art methods using various metrics. Finally, we used the segmentation masks for automatically extracting particle size distributions from the SEM images of TiO2 particles, which were in excellent agreement with particle size distributions obtained manually but could be obtained in a fraction of the time. KW - Electron microscopy KW - Neural networks KW - Artificial intelligence KW - Image segmentation KW - Automated image analysis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522454 DO - https://doi.org/10.1038/s41598-021-84287-6 VL - 11 IS - 1 SP - 4942 PB - Springer Nature AN - OPUS4-52245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stelzner, Ludwig A1 - Weise, Frank A1 - Oesch, Tyler A1 - Dlugosch, R. A1 - Powierza, Bartosz T1 - Transport and reconfiguration of moisture in HPC due to unilateral heating N2 - Explosive spalling is caused by, among others, the thermohydraulic spalling mechanism. During this process, vaporization, dehydration, moisture-transport and condensation processes interact. As a result, a drying and dehydration zone as well as a saturated zone, known as a moisture clog, are observed inside the unilaterally-heated concrete. The presented research is focused on the experimental investigation of the underlying thermohydraulic processes. To investigate these, a test methodology based on X-ray computed tomography (CT) and nuclear magnetic resonance (NMR) was developed. Thereby, the X-ray CT scans are carried out simultaneously during the application of a defined unilateral-heating regime on a specially-constructed specimen. This miniaturized specimen, equipped with a double-layer casing, reproduces the condition within a planar, unilaterally-heated building component. A preliminary test methodology and the first experimental results were presented at the 5th International Workshop on Concrete Spalling in Borås, Sweden (2017). The contribution for the upcoming workshop presents an improved version of this test methodology and new results for a high-performance concrete (HPC) mixture exposed to temperatures up to 500 °C. Regarding the CT measurements, a higher time-resolution of 15 min was achieved and a quantification of the moisture changes was implemented. Due to an increase in signal quality of the NMR measurements, a pore-size specific moisture distribution can now be resolved. This allows to conclude about the moisture reconfiguration between small gel pores and larger interhydrate pores. Additionally, the NMR measurement are no longer limited to first 2.5 cm below the heated surface but a one-dimensional moisture distribution can now be estimated over the whole 10 cm long specimen. The presented results demonstrate that the combination of X-ray CT and NMR measurements enables to image and quantify the thermally-induced moisture transport and reconfiguration from small gel pores up to macro pores. This provides important insights into the thermohydraulic damage mechanism and leads to a better understanding of spalling avoidance strategies, like the addition of polypropylene fibres. T2 - 6th International Workshop on Concrete Spalling due to fire exposure CY - Sheffield, UK DA - 19.09.2019 KW - Moisture clog KW - X-ray CT KW - NMR KW - Moisture transport KW - HPC PY - 2019 UR - https://firespallingworkshop2019.group.shef.ac.uk/wp-content/uploads/2019/09/Fire-Spalling-Workshop_Proceedings.pdf SN - 978-1-5272-4135-0 SP - 181 EP - 190 CY - Sheffield AN - OPUS4-49161 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf A1 - Pohl, Rainer A1 - Lohde, Sebastian A1 - Aydoğdu, M. T1 - Zerstörungsfreie Prüfung von Composite-Druckgefäßen mit konventioneller und hochfrequenter Wirbelstromtechnik N2 - Composite-Druckgefäße für den Gefahrguttransport sowie für Wasserstoff- und Erdgasfahrzeuge bestehen aus einem lasttragenden Composite und einer gasdichten, metallischen oder polymeren Barriereschicht (Liner). Zur Untersuchung des Alterungsverhaltens solcher Composite-Druckgefäße wurde in der BAM das interdisziplinäre Themenfeldprojekt COD-AGE durchgeführt. Ziel des Projektes war die Entwicklung von Methoden und Modellen zur Beschreibung und Bestimmung des Alterungsverhaltens von Carbonfaser-Compositen am Beispiel von Druckgefäßen, um eine bessere Vorhersage der Alterung und der sicheren Gebrauchsdauer zu ermöglichen. Ein Schwerpunkt in diesem Projekt war die Bereitstellung geeigneter ZfP-Methoden. Dabei ging es sowohl um versuchsbegleitende Prüfungen, als auch um die mögliche Entwicklung von Prüfeinrichtungen für den späteren praktischen Gebrauch. In dem Vortrag werden Prüfergebnisse der alterungsbegleitenden Wirbelstromprüfung an Composite-Druckgefäßen vorgestellt. In Alterungsversuchen wurden Druckgefäße aus einem ca. 4 mm dicken Aluminiumliner und ca. 8 mm dicker CFK-Ummantelung untersucht. Typisches Einsatzgebiet solcher Druckgefäße sind Atemschutzgeräte der Feuerwehr. Die Druckgefäße wurden sowohl mit konventioneller Wirbelstromtechnik von außen und von innen als auch mit hochfrequenter Wirbelstromtechnik von außen geprüft. Es konnten sowohl Beschädigungen des metallischen Liners, als auch Strukturen des CFK-Geflechts nachgewiesen werden. Eine besondere mechanische Herausforderung bestand in der Prüfung der Innenseite der Liner, da hier eine zylindrische Fläche mit einem Innendurchmesser von 150 mm durch einen Zugang von nur 15 mm Durchmesser geprüft werden muss. T2 - DACH-Jahrestagung CY - Friedrichshafen, Germany DA - 26.05.2019 KW - Wirbelstromprüfung KW - COD-AGE KW - Composite-Druckgefäß KW - CFK PY - 2019 AN - OPUS4-48123 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Combined cell and nanoparticle models for TOPAS to study radiation dose enhancement by Monte-Carlo based particle scattering Simulations N2 - Dose enhancement by gold nanoparticles (AuNP) increases the biological effectiveness of radiation damage in biomolecules and tissue. To apply them effectively during cancer therapy their influence on the locally delivered dose has to be determined.[1] Hereby, the AuNP locations strongly influence the energy deposit in the nucleus, mitochondria, membrane and the cytosol of the targeted cells. To estimate these effects, particle scattering simulations are applied. In general, different approaches for modeling the AuNP and their distribution within the cell are possible. In this work, two newly developed continuous and discrete-geometric models for simulations of AuNP in cells are presented. [2] These models are applicable to simulations of internal emitters and external radiation sources. Most of the current studies on AuNP focus on external beam therapy. In contrast, we apply the presented models in Monte-Carlo particle scattering simulations to characterize the energy deposit in cell organelles by radioactive 198AuNP. They emit beta and gamma rays and are therefore considered for applications with solid tumors. Differences in local dose enhancement between randomly distributed and nucleus targeted nanoparticles are compared. Hereby nucleus targeted nanoparticels showed a strong local dose enhancement in the radio sensitive nucleus. These results are the foundation for ongoing experimental work which aims to obtain a mechanistic understanding of cell death induced by radioactive 198Au. T2 - #RSCposter 2023 CY - Online meeting DA - 28.02.2023 KW - AuNP KW - Beta decay KW - Brachytherapy KW - Cancer treatment KW - Clustered nanoparticles KW - DNA KW - DNA damage KW - Dosimetry KW - Energy deposit KW - Geant4 KW - Geant4-DNA KW - Gold Nanoparticles KW - LEE KW - Livermore model KW - Low energy electrons KW - MCS KW - Microdosimetry KW - Monte-Carlo simulation KW - NP KW - OH radical KW - Penelope model KW - Radiation damage KW - Radiation therapy KW - Radiationtherapy KW - Radiotherapy KW - Radioactive decay KW - Radiolysis KW - Simulation KW - TOPAS KW - TOPAS-nbio KW - beta particle KW - particle scattering PY - 2023 AN - OPUS4-57060 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas A1 - Hodoroaba, Vasile-Dan T1 - Correlative Analysis by Raman and other Micro & Nanospectroscopic Imaging Techniques N2 - In the present talk the basics of the Raman spectroscopy and particularly of Raman microscopy are explained. Advantages and disadvantages of the method are highlighted through selected case studies. In the second part of the lecture examples of correlative imaging with electron, X-ray, ion and optical microscopies from micro- to the nanoscale are highlighted. T2 - Charisma School on Raman Harmonisation CY - Turin, Italy DA - 19.10.2022 KW - Raman KW - Correlative Imaging KW - Microscopy KW - Hyperspectral imaging PY - 2022 UR - https://amdgroup.inrim.it/events/vamas-sc-meeting-47/program-sc47 AN - OPUS4-56094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wegner, Karl David T1 - Luminescent Quantum dots – the next-generation nano light bulbs N2 - Fluorescent semiconductor nanocrystals, also known as quantum dots (QDs), enabled many advancements in biotechnology, photovoltaics, photocatalysis, quantum computing and display devices. The high versatility of this nanomaterial is based on their unique size-tunable photoluminescence properties, which can be adjusted from the visible to the near-infrared range. In contrast to other nanomaterials, QDs made the transition from a laboratory curiosity to the utilization in commercial products, like the QLED television screen or in smartphone displays. The best investigated QDs are composed of heavy metals like cadmium or lead, which is not the best choice in terms of toxicity and environmental pollution. A more promising material is Indium Phosphide (InP), which is also currently used by Samsung, Sony and co. in the QLED displays. In this contribution, I would like to give you a sneak peek behind the curtains of nanomaterial synthesis and show how this material is produced, how to stabilize their structural properties, and assess their toxicity in environmentally relevant conditions. Furthermore, I would like to present a synthesis method to accomplish the last open challenge in display technology of a blue luminescent LED based on QDs by introducing a new element to the InP QDs. T2 - The Berlin Postdoc Day CY - Berlin, Germany DA - 03.11.2022 KW - InP KW - Quantum dots KW - Fluorescence KW - Aging KW - Doping KW - Nanomaterial KW - Cytotoxicity PY - 2022 AN - OPUS4-56194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumacher, David T1 - Wind turbine rotor blade testing by dual-energy laminography N2 - Modern wind turbine rotor blades consist of sandwich shell segments made from glass fiber reinforced polymers. During manufacturing, defects can arise which could lead to failure of the whole component under dynamic mechanical and thermal loads. Hence during operation defects can arise which, if detected, can be repaired locally and in-situ by applying repair patches instead of taking the whole rotor blade down and repair it remotely. This method is much more time and cost effective, since the shut-down time of the energy converter is limited to a minimum. These repair patches can, however, also lead to new defects if not applied optimally. Therefore, it is necessary to control the quality of the repair patches to ensure the best possible restoration of structural integrity of the component. As a rotor blade is an object with a large aspect ratio, X-ray laminography is predestined to provide 3D information of the objective volume. To enhance the amount of information gained from laminographic reconstruction, we use in this study a photon counting and energy discriminating X-ray detector and apply a material decomposition algorithm to the data. By inherently separating the incident spectra within the detection process into two distinct energy bins, the basis material decomposition can provide material resolved images. Choosing glass and epoxy resin as basis materials and numerically solving the inverse dual-energy equation system, the reconstructed laminographic datasets contain highly valuable information about the distribution of the basis materials within the structure. Furthermore, cross- artifacts arising from the limited angle of the projection data can be reduced by this method which allows to investigate structures that were hidden underneath the artefacts. T2 - 1st International Symposium on Photon Counting Technologies & Applications CY - München, Germany DA - 05.07.2019 KW - Laminography KW - Wind energy KW - Fiber reinforced polymer KW - Photon counting detector KW - Dual-energy PY - 2019 AN - OPUS4-48440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - New reference material candidates for traceable size measurement of nonspherical nanoparticles N2 - Size measurement of nanoparticles (NP) becomes a challenging analytical problem when non-spherical shapes must be traceably measured. However, most industrial NPs have irregular shapes and broad size distribution making it often more complex to follow European regulatory to identify a material as a nanomaterial according to which accurate measurement of the smallest dimension and its size Distribution is necessary. The European research project nPSize - Improved traceability chain of nanoparticle size measurements aims to fill this gap by developing potential non-spherical reference nanoparticles, measurement procedures and physical modelling to improve the traceability chain, comparability and compatibility for NP size measurements between different methods. Therefore, new model NP with well-controlled shape has been synthesized and are supposed to be systematically characterized using the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering. Following NP candidates are under investigation with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-100 nm lateral), (ii) titania bipyramides (~60 nm length x 40 nm width), (iii) titania acicular particles (100 nm length x 15-20 nm width; aspect ratio 5.5/6), (iv) gold nanorods (~10 nm width x 30 nm length), and (v) gold nanocubes (~55 nm x 55 nm x 55 nm). In addition, sample preparation procedures as well as measurement analysis procedures with evaluation of appropriate measurands and descriptors for each material class and method are being developed to support standardization. To underpin the traceability of the size measurement of nonspherical NP, physical modelling of the signals in e.g. electron microscopy techniques will be used and in combination, the implementation of machine learning is aimed to facilitate measurement Analysis procedures, especially regarding the accurate thresholding/segmentation of the NPs. T2 - European Conference on Applications of Surface and Interface Analysis ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Nanoparticles KW - Size distribution KW - Electron microscopy KW - Certified reference materials KW - Traceability PY - 2019 AN - OPUS4-49227 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stelzner, Ludwig T1 - Transport and reconfiguration of moisture in HPC due to unilateral heating N2 - Explosive spalling is caused by, among others, the thermohydraulic spalling mechanism. During this process, vaporization, dehydration, moisture-transport and condensation processes interact. As a result, a drying and dehydration zone as well as a saturated zone, known as a moisture clog, are observed inside the unilaterally-heated concrete. The presented research is focused on the experimental investigation of the underlying thermohydraulic processes. To investigate these, a test methodology based on X-ray computed tomography (CT) and nuclear magnetic resonance (NMR) was developed. Thereby, the X-ray CT scans are carried out simultaneously during the application of a defined unilateral-heating regime on a specially-constructed specimen. This miniaturized specimen, equipped with a double-layer casing, reproduces the condition within a planar, unilaterally-heated building component. A preliminary test methodology and the first experimental results were presented at the 5th International Workshop on Concrete Spalling in Borås, Sweden (2017). The contribution for the upcoming workshop presents an improved version of this test methodology and new results for a high-performance concrete (HPC) mixture exposed to temperatures up to 500 °C. Regarding the CT measurements, a higher time-resolution of 15 min was achieved and a quantification of the moisture changes was implemented. Due to an increase in signal quality of the NMR measurements, a pore-size specific moisture distribution can now be resolved. This allows to conclude about the moisture reconfiguration between small gel pores and larger interhydrate pores. Additionally, the NMR measurement are no longer limited to first 2.5 cm below the heated surface but a one-dimensional moisture distribution can now be estimated over the whole 10 cm long specimen. The presented results demonstrate that the combination of X-ray CT and NMR measurements enables to image and quantify the thermally-induced moisture transport and reconfiguration from small gel pores up to macro pores. This provides important insights into the thermohydraulic damage mechanism and leads to a better understanding of spalling avoidance strategies, like the addition of polypropylene fibres. T2 - 6th International Workshop on Concrete Spalling due to fire exposure CY - Sheffield, UK DA - 19.09.2019 KW - Moisture clog KW - X-ray CT KW - NMR KW - Moisture transport KW - HPC PY - 2019 AN - OPUS4-49159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Langklotz, U. T1 - FT-IR spectroscopy of corrosion products formed on zinc under atmospheric conditions N2 - Zinc materials are of high importance in the field of corrosion protection. For example, almost half of the annual production of zinc is used as anti-corrosive layer for steel components, particularly under atmospheric conditions. The corrosion protection is frequently ascribed to zinc carbonate species with low solubility which form on the metal surface under atmospheric conditions. Due to the technological importance and wide use of zinc materials, its corrosion behavior and the formation of reaction products has been intensively investigated over decades. Assuming atmospheric corrosion conditions, an initial native passive film of few nanometers thickness forms spontaneously. It consists of zinc oxide and hydroxide, transforming into various species in dependence of the surrounding atmospheric conditions. This study focusses on the investigation of corrosion product layers on massive titanium-zinc sheets, formed during short- and mid-term exposure experiments by Fourier-transformed infrared spectroscopy. This method enables the investigation of extremely thin native passive films which form during the initial hours of exposure. Furthermore, aged surface layers are analyzed which were formed by transformation of initial passive layers over the time of several weeks. The spectroscopic investigations are complemented by scanning electron microscopy (SEM/EDX) in order to obtain information on the chemical composition and morphology of the corrosion products. The combination of both methods offers a comprehensive view on the processes occurring in the early stages of zinc corrosion. T2 - EUROCORR 2019 CY - Sevilla, Spain DA - 09.09.2019 KW - Zinc coatings KW - FT-IR KW - Layer formation PY - 2019 AN - OPUS4-49132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühle, Bastian A1 - Hodoroaba, Vasile-Dan T1 - Automatic Image Segmentation and Analysis using Neural Networks N2 - We present a workflow for obtaining fully trained artificial neural networks that can perform automatic particle segmentations of agglomerated, non-spherical nanoparticles from electron microscopy images “from scratch”, without the need for large training data sets of manually annotated images. This is achieved by using unsupervised learning for most of the training dataset generation, making heavy use of generative adversarial networks and especially unpaired image-to-image translation via cycle-consistent adversarial networks. The whole process only requires about 15 minutes of hands-on time by a user and can typically be finished within less than 12 hours when training on a single graphics card (GPU). After training, SEM image analysis can be carried out by the artificial neural network within seconds, and the segmented images can be used for automatically extracting and calculating various other particle size and shape descriptors. T2 - Machine Learning Workshop CY - Online Meeting DA - 18.03.2021 KW - Electron Microscopy KW - Neural Networks KW - Artificial Intelligence KW - Image Segmentation KW - Automated Image Analysis PY - 2021 AN - OPUS4-52304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Data processing and nonlinear curve Fitting with fityk N2 - A brief introduction into fityk is given. The introduction is followed by a pratical session. Fityk is a versatile data processing tool for nonlinear curve fitting. T2 - AFM Data analysis seminar CY - Online meeting DA - 23.02.2021 KW - Fityk KW - Curve fitting KW - Analysis KW - Raman KW - IR KW - XPS PY - 2021 AN - OPUS4-52154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian T1 - Zerstörungsfreie Charakterisierung der Alterung additiv gefertigter Kunststoffbauteile N2 - Es wurden mittels Fused Layer Modeling (FLM) Probekörper aus ABS und mittels Laser Sintering (LS) Probekörper aus PA 12 hergestellt, die anschließend für drei Monate einer künstlichen Bewitterung unterzogen wurden. Die dabei erzeugte definierte Alterung wurde nach drei Zeitabschnitten jeweils mit zerstörungsfreien Methoden charakterisiert. Dabei wurde neben den spektroskopischen Standardmethoden auch die aktive Thermografie eingesetzt. Die Ergebnisse zeigen, dass sich mittels der Thermografie sowohl chemische Veränderungen als auch mechanische Schädigungen (Fehlstellen) darstellen lassen. Die Bewitterung beeinflusst die Teiltransparenz der Proben zumindest im sichtbaren Spektralbereich, was bei der Charakterisierung der Fehlstellen, die mittels optisch angeregter aktiver Thermografie detektiert wurden, berücksichtigt werden muss. Die Erkenntnisse dienen für die Entwicklung einer Strategie für eine Qualitätskontrolle von additiv gefertigten Kunststoffteilen. T2 - DACH-Jahrestagung 2019 - Zerstörungsfreie Materialprüfung CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Additive Fertigung KW - Künstliche Bewitterung KW - Thermografie KW - Zerstörungsfreie Prüfung KW - additive manufacturing KW - Kunststoffe PY - 2019 AN - OPUS4-48331 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kovacevic, E. A1 - Strunskus, T. A1 - Santhosh, N. M. A1 - Zavasnik, Z. A1 - Unger, Wolfgang A1 - Sauvage, T. A1 - Ammar, M.-R. A1 - Cvelbar, U. A1 - Berndt, J. T1 - Thermal stability studies of plasma deposited hydrogenated carbon nitride nanostructures N2 - Thermally stable carbon nitride nanostructures have potential applications in surface coatings and automotive fields. In this work, hydrogenated nitrogen-rich carbon nitride nanoparticles have been synthesised via low-pressure low-power plasma vapour deposition technique from methane/Nitrogen gas mixture in a dry process. Thermal stability of the initially prepared hydrogenated carbon Nitride structures has been analysed by near-edge X-ray absorption fine-structure spectroscopy (NEXAFS, insitu), Raman spectroscopy, scanning and transmission electron microscopy and nuclear reaction Analysis (NRA). Thermal studies reveal the excellent stability of the material and nitrogen-rich characteristics (N/C ratio 0.5e0.2 ± 0.01). The obtained results suggest transformation of sp3-rich as-deposited carbon Nitride into sp2-carbon phase with more graphitic features upon thermal annealing. Such in-situ thermal studies of plasma deposited carbon nitrides confirm the conversion of sp3-rich phase to sp2-rich carbon phase at the critical temperature (about 450 K), without a huge loss in nitrogen content. The analysis revealed that the material is a stable plasma deposit after this critical temperature up to >1100 K. Additionally, super hydrophilic carbon nitride nanostructure transforms into a hydrophobic surface after thermal annealing. These thermally stable hydrophobic carbon nitride nanoparticles could be used as a promising material for the hydrophobic coatings for various applications, especially for harsh conditions. KW - Carbon nanoparticles KW - Hydrogenated nanostructures KW - Plasma deposition KW - NEXAFS KW - Thermal annealing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536163 DO - https://doi.org/10.1016/j.carbon.2021.08.008 SN - 0008-6223 VL - 184 SP - 82 EP - 90 PB - Elsevier Ltd. AN - OPUS4-53616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hörenz, Christoph A1 - Tache, O. A1 - Bartczak, D. A1 - Nunez, S. A1 - Abad Alvaro, I. A1 - Goenaga-Infante, H. A1 - Hodoroaba, Vasile-Dan T1 - A Study on the Analysis of Particle Size Distribution for Bimodal Model Nanoparticles by Electron Microscopy N2 - The present study addresses the capability of measurement of relative particle number concentration by scanning electron microscopy for model bimodal silica and gold samples prepared in the frame of the European research project “nPSize - Improved traceability chain of nanoparticle size measurements” as candidate reference nanoparticles. KW - Nanoparticles KW - Particle size distribution KW - Bimodal size distribution KW - Traceability PY - 2020 DO - https://doi.org/10.1017/S1431927620021054 VL - 26 IS - S2 SP - 2282 EP - 2283 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Kulow, Anicó A1 - Kabelitz, Anke A1 - Grunewald, C. A1 - Seidel, R. A1 - Chapartegui-Arias, Ander A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Emmerling, Franziska A1 - Beyer, S. T1 - Observation of early ZIF-8 crystallization stages with X-ray absorption spectroscopy N2 - The present study investigates early stages of ZIF-8 crystallization up to 5 minutes post mixing of precursor solutions. Dispersive X-ray Absorption Spectroscopy (DXAS) provides a refined understanding of the evolution of the coordination environment during ZIF-8 crystallization. Linear Combination Fiting (LCF) suggests tetrakis(1-methylimidazole)zinc2+ to be a suitable and stable mononuclear structure analogue for some early stage ZIF-8 intermediates. Our results pave the way for more detailed studies on physico-chemical aspects of ZIF-8 crystallization to better control tailoring ZIF-8 materials for specific applications. KW - In-situ KW - XANES KW - ZIF-8 KW - Crystallization PY - 2020 DO - https://doi.org/10.1039/D0SM01356K SN - 1744-6848 VL - 17 IS - 2 SP - 331 EP - 334 PB - Royal Scociety of Chemistry AN - OPUS4-51723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lutz, C. A1 - Hampel, S. A1 - Ke, X. A1 - Beuermann, S. A1 - Turek, T. A1 - Kunz, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Fittschen, U. T1 - Evidence for redox reactions during vanadium crossover inside the nanoscopic water-body of Nafion 117 using X-ray absorption near edge structure spectroscopy N2 - A major source of capacity fade of the common vanadium redox flow battery (VRFB) is the vanadium ion transport through the separator. However, different transport models disagree significantly in the diffusion coefficient for the different V species and the influence of different transport mechanisms. The underlying hypothesis of this work is that reactions inside the membrane are partly responsible for these discrepancies. Accordingly, it was investigated if redox reactions inside the nanoscopic water body of Nafion 117 can occur. X-ray absorption near edge structure spectroscopy (XANES) was used to distinguish between the different V species inside hydrated Nafion 117 and novel PVDF-based membranes. It was validated that the speciation of vanadium can be performed using the pre-edge peak energy and intensity. The experiments were performed as follows: strips of the membrane were exposed from one site to a V3+ solution (green) and from the other site to a VO2+ solution (yellow). The ions could diffuse into the membrane from both sides. A change of color of the membrane strip was observed. The blue color in the middle of the strip indicated that VO2+ was formed where V3+ and VO2+ got in contact. Using XANES this reaction inside Nafion was proven. KW - PVDF-Based membrane KW - VRFB KW - Vanadium speciation KW - XANES KW - Nafion 117 PY - 2020 DO - https://doi.org/10.1016/j.jpowsour.2020.229176 VL - 483 SP - 229176 PB - Elsevier B.V. AN - OPUS4-51719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Baer, D. R. A1 - Cant, D. J. H. A1 - Castner, D. G. A1 - Ceccone, G. A1 - Engelhard, M. H. A1 - Karakoti, A. S. A1 - Müller, Anja ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Preparation of nanoparticles for surface analysis N2 - A variety of methods used to prepare nano-objects for surface analysis are described along with information about when they might be best applied. Intrinsic properties of NPs which complicate their characterization and need to be considered when planning for surface or other analyses of NPs are identified, including challenges associated with reproducible synthesis and functionalization of the particles as well as their dynamic nature. The relevant information about the sample preparation processes, along with analysis details and data that need to be added to the collection of material provenance information is identified. Examples of protocols that have been successfully used for preparation of nano-objects for surface analysis are included in an annex. KW - Sample preparation KW - Nanoparticles KW - Surface chemistry KW - XPS KW - Dynamic behavior KW - Nano-object KW - Surface analysis PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00018-3 SP - 295 EP - 347 PB - Elsevier CY - Amsterdam AN - OPUS4-50186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mech, A. A1 - Rauscher, H. A1 - Rasmussen, K. A1 - Babick, F. A1 - Hodoroaba, Vasile-Dan A1 - Ghanem, A. A1 - Wohlleben, W. A1 - Marvin, H. A1 - Brüngel, R. A1 - Friedrich, C. M. T1 - The NanoDefine Methods Manual - Part 2: Evaluation of methods N2 - The present series of reports, the NanoDefine Methods Manual, has been developed within the NanoDefine project 'Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial', funded by the European Union's 7th Framework Programme, under grant agreement 604347. In 2011 the European Commission (EC) published a recommendation for a definition of the term 'nanomaterial', the EC NM Definition, as a reference to determine whether an unknown material can be considered as a 'nanomaterial' for regulatory purposes1. One challenge is the development of methods that reliably identify, characterize and quantify nanomaterials (NM) both as substances and in various products and matrices. The overall goal of NanoDefine was to support the implementation of the EC NM Definition. It can also support the implementation of any NM definition based on particle size. The project has developed an integrated approach, which allows identifying any material as a nano- or not a nanomaterial according to the EC NM Definition. NanoDefine explicitly supported the governance challenges associated with the implementation of legislation concerning nanomaterials by: - addressing the issues on availability of suitable measuring techniques, reference materials, validated methods, acceptable to all stakeholders (authorities, policy makers, commercial firms), - developing an integrated and interdisciplinary approach and a close international co-operation and networking with academia, commercial firms and standardization bodies. Thus, the NanoDefine Methods Manual provides guidance on practical implementation of the EC NM Definition throughout the nanomaterial characterization process, and on the characterization techniques employed as well as their application range and limits. It assists the user in choosing the most appropriate measurement method(s) to identify any substance or mixture for a specific purpose, according to the EC NM Definition of a nanomaterial. The NanoDefine project also explored how to assess a material against the criteria of the definition through proxy solutions, i.e. by applying measurement techniques that indirectly determine the x50. Those findings were developed through empirically based scientific work and are included in Part 1 of this Manual. As they go beyond the text of the EC NM Definition, they may be used as practical approach to indicate whether a material is a nanomaterial or not, but keeping in mind that they should not be taken as recommendation for the implementation of the EC NM Definition in a regulatory context. The NanoDefine Methods Manual consists of the following three parts:  Part 1: The NanoDefiner Framework and Tools  Part 2: Evaluation of Methods  Part 3: Standard Operating Procedures (SOPs) Part 1 covers the NanoDefiner framework, general information on measurement methods and performance criteria and tools developed by NanoDefine such as a materials categorisation system, a decision support flow scheme and an e-tool. Part 2 discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size. Part 3 presents the 23 Standard Operating Procedures developed within the NanoDefine project. The current document is part 2. KW - Nanomaterial KW - Nanoparticles KW - NanoDefine KW - Particle size distribution KW - Nanomaterial classification PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503708 SN - 978-92-76-11953-1 DO - https://doi.org/10.2760/071877 SN - 1831-9424 VL - JRC117501 SP - 1 EP - 133 PB - Publications Office of the European Union CY - Luxembourg AN - OPUS4-50370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rühle, Bastian A1 - Hodoroaba, Vasile-Dan T1 - Towards Automated Electron Microscopy Image Segmentation for Nanoparticles of Complex Shape by Convolutional Neural Networks N2 - In this contribution different ways are explored with the aim to generate suitable training data for ‘non-ideal’ samples using various approaches, e.g., computer-generated images or unsupervised learning algorithms such as generative adversarial networks (GANs). We used these data to train simple CNNs to produce segmentation masks of SEM images and tested the trained networks on real SEM images of complex nanoparticle samples. The novel use of CNN for the automated analysis of the size of nanoparticles of complex shape and with a high degree of agglomeration has proved to be a promising tool for the evaluation of particle size distribution on a large number of constituent particles. Further development and validation of the preliminary model, respectively larger training and validation data sets are necessary. KW - Nanoparticles KW - Convolutional neural networks KW - Image segmentation KW - Electron microscopy KW - Automatisation PY - 2020 DO - https://doi.org/10.1017/S1431927620017262 VL - 26 IS - S2 SP - 1188 EP - 1189 PB - Cambridge University Press CY - Cambridge, UK AN - OPUS4-51773 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Clifford, C. A1 - Stintz, M. A1 - Hodoroaba, Vasile-Dan A1 - Unger, Wolfgang A1 - Fujimoto, T. ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - International standards in nanotechnologies N2 - This chapter provides an overview of what standards are, why they are important, and how they are developed. There is a focus on the work of standards committees relevant to nanotechnology measurement and characterization with tables detailing the standards that are currently available for a large number of different techniques, materials, and applications at the nanoscale. KW - Standards KW - Nanotechnology KW - Reproducibility KW - ISO KW - CEN KW - VAMAS PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00026-2 SP - 511 EP - 525 PB - Elsevier CY - Amsterdam AN - OPUS4-50165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Unger, Wolfgang A1 - Wirth, Thomas A1 - Hodoroaba, Vasile-Dan ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Auger electron spectroscopy N2 - An introduction in the application of Auger Electron Spectroscopy to surface chemical analysis of nanoparticles is given. Auger Electron Spectroscopy is a mature method in the field of surface chemical analysis. The chapter addresses the physical basis of the method, the principal design of recent instruments together with modes of operation and options for the presentation of spectra, as well as different approaches for qualitative (including identification of chemical species) and quantitative surface analysis of elements. An application paragraph on surface chemical analysis of nanoparticles by AES or SAM introduces the different measurement approaches and sample preparation strategies applied by analysts. The analysis of nanoparticle ensembles, the so-called selected point analysis where a narrow primary electron beam is centered on an individual nanoparticle, and chemical mapping of individual nanoparticles (or a line scan across) are addressed. Existing literature is reviewed and informative case studies presented. Limitations and pitfalls in the application of AES in surface chemical analysis of nanoparticles are also addressed. KW - Auger Electron Spectroscopy KW - Surface chemical analysis KW - Imaging surface chemical analysis KW - Nanoparticles KW - Nanotechnology PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00020-1 SP - 373 EP - 395 PB - Elsevier CY - Amsterdam AN - OPUS4-50119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mech, A. A1 - Rauscher, H. A1 - Babick, F. A1 - Hodoroaba, Vasile-Dan A1 - Wohlleben, W. A1 - Marvin, H. A1 - Weigel, S. A1 - Brüngel, R. A1 - Friedrich, C. M. T1 - The NanoDefine Methods Manual - Part 1: The NanoDefiner Framework and Tools N2 - The present series of reports, the NanoDefine Methods Manual, has been developed within the NanoDefine project 'Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial', funded by the European Union's 7th Framework Programme, under grant agreement 604347. In 2011 the European Commission (EC) published a recommendation for a definition of the term 'nanomaterial', the EC NM Definition, as a reference to determine whether an unknown material can be considered as a 'nanomaterial' for regulatory purposes1. One challenge is the development of methods that reliably identify, characterize and quantify nanomaterials (NM) both as substances and in various products and matrices. The overall goal of NanoDefine was to support the implementation of the EC NM Definition. It can also support the implementation of any NM definition based on particle size. The project has developed an integrated approach, which allows identifying any material as a nano- or not a nanomaterial according to the EC NM Definition. NanoDefine explicitly supported the governance challenges associated with the implementation of legislation concerning nanomaterials by: - addressing the issues on availability of suitable measuring techniques, reference materials, validated methods, acceptable to all stakeholders (authorities, policy makers, commercial firms), - developing an integrated and interdisciplinary approach and a close international co-operation and networking with academia, commercial firms and standardization bodies. Thus, the NanoDefine Methods Manual provides guidance on practical implementation of the EC NM Definition throughout the nanomaterial characterization process, and on the characterization techniques employed as well as their application range and limits. It assists the user in choosing the most appropriate measurement method(s) to identify any substance or mixture for a specific purpose, according to the EC NM Definition of a nanomaterial. The NanoDefine project also explored how to assess a material against the criteria of the definition through proxy solutions, i.e. by applying measurement techniques that indirectly determine the x50. Those findings were developed through empirically based scientific work and are included in Part 1 of this Manual. As they go beyond the text of the EC NM Definition, they may be used as practical approach to indicate whether a material is a nanomaterial or not, but keeping in mind that they should not be taken as recommendation for the implementation of the EC NM Definition in a regulatory context. The NanoDefine Methods Manual consists of the following three parts:  Part 1: The NanoDefiner Framework and Tools  Part 2: Evaluation of Methods  Part 3: Standard Operating Procedures (SOPs) Part 1 covers the NanoDefiner framework, general information on measurement methods and performance criteria and tools developed by NanoDefine such as a materials categorisation system, a decision support flow scheme and an e-tool. Part 2 discusses the outcome of the evaluation of the nanomaterials characterisation methods for measuring size. Part 3 presents the 23 Standard Operating Procedures developed within the NanoDefine project. The current document is part 1. KW - Nanomaterial KW - Nanoparticles KW - NanoDefine KW - Nanoparticle size distribution KW - Nanomaterial classification KW - Framework KW - Tools PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503699 SN - 978-92-76-11950-0 DO - https://doi.org/10.2760/55181 SN - 1831-9424 SP - 1 EP - 89 PB - Publications Office of the European Union CY - Luxembourg AN - OPUS4-50369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Niemz, P. A1 - Baensch, Franziska A1 - Brunner, A. J. ED - Pavalache-Ilie, M. ED - Curtu, A. L. T1 - Acoustic Emission Analysis And Synchrotron-based Microtomography of glued shear strength samples from spruce wood N2 - To better understanding the failure of adhesive joints tensile tests were carried out on miniature test specimens from Norway spruce in the synchrotron. Urea-formaldehyde resin was used as adhesive. e. For comparison purposes, tensile tests were carried out on solid wood and on bonded miniature tensile shear samples with acoustic emission. The acoustic emission signals of all the experiments occurred with classified pattern recognition. This resulted in two classes of signals for each two frequency peaks. One class consisted of the low-frequency and the other of the higher-frequency peak of higher intensity, but this was essentially independent from the structure (solid wood or plywood) and size scale of the test specimens. The influence of the adhesive layers was determined on wood test specimens on laboratory scale and on miniature test specimens with an adhesive layer and selected fiber orientations. This gave evidence that the sound emission signals from the failure of the adhesive layer presumably of the class with low frequency signals peak in the range of services can be assigned. KW - Wood KW - Bondline KW - In-situ test KW - Acoustic emission KW - Synchrotron tomography PY - 2020 DO - https://doi.org/10.31926/but.fwiafe.2020.13.62.1.7 VL - 13 IS - 62 Part 1 SP - 81 EP - 88 PB - Transilvania University Press, Brasov, Romania CY - Brasov AN - OPUS4-51010 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Mast, J. A1 - Verleysen, E. A1 - Hodoroaba, Vasile-Dan A1 - Kaegi, R. ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Characterization of nanomaterials by transmission electron microscopy - Measurement procedures N2 - In this chapter, approaches are proposed for the descriptive and quantitative characterization of nano-objects with nanometer resolution. Measurements are based on the analysis of the characteristics of 2D projections of individual particles visualized on transmission electron micrographs. Incorporation of spectroscopic methods (EDS and EELS) for elemental analysis of nano-objects is recommended to identify subpopulations of nano-objects in mixtures based on their chemical composition. The focus lies on the determination of physicochemical properties which are essential in a legislatory and regulatory context to define the material as a nanomaterial (NM), and to assess its safety and toxicological potential, using widely accessible equipment. KW - Nanoparticles KW - Sample preparation KW - Image analysis KW - Transmission electron microscopy PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00004-3 SP - 29 EP - 48 PB - Elsevier CY - Amsterdam AN - OPUS4-50121 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Vladár, A. E. A1 - Hodoroaba, Vasile-Dan ED - Hodoroaba, Vasile-Dan ED - Unger, Wolfgang ED - Shard, A. G. T1 - Characterization of nanoparticles by scanning electron microscopy N2 - In this chapter sample preparation, image acquisition, and nanoparticle size and shape characterization methods using the scanning electron microscope (SEM) in reflective and transmitted working modes are described. These help in obtaining reliable, highly repeatable results. The best solutions vary case-by-case and depend on the raw (powdered or suspension) nanoparticle material, the required measurement uncertainty and on the performance of the SEM. KW - Nanoparticles KW - Sample preparation KW - Electron microscopy KW - SEM KW - Size measurement KW - Shape KW - Threshold PY - 2020 SN - 978-0-12-814182-3 DO - https://doi.org/10.1016/B978-0-12-814182-3.00002-X SP - 7 EP - 27 PB - Elsevier CY - Amsterdam AN - OPUS4-50120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Zuverlässigkeitsbetrachtungen bei der Ultraschallprüfung von Radsatzwellen im Ausbildungsbetrieb N2 - Im Rahmen des UT1 E W im Ausbildungszentrum Wittenberge der DGZfPwurden statistische Untersuchungen am Beispiel der Radsatzwellenprüfung mit Testradsatzwellen durchgeführt. Diese Untersuchungen hatten zum Ziel, die wesentlichen Einflussparameter bei der Handprüfung auf das Prüfergebnis zu evaluieren. Im Rahmen der Zuverlässigkeitsbetrachtung wurden die ProbabilityofDetection(POD) und die Nachweisgrenzen ermittelt.Die durchgeführte Studie zeigt, dass die Bewertung der gesamten Zuverlässigkeit der ZfP komplex ist. Dieses verlangt eine detaillierte Versuchsplanung und die Einbeziehung von unterschiedlichen Faktoren, von den Anwendungsparametern bis hin zu den komplexen menschlichen und organisatorischen Faktoren. Die im Rahmen der Studie ermittelten Ergebnisse lassen aufgrund der geringen Anzahl an Testreflektoren keine allgemeingültige Übertragung auf beliebige Korbbogen-geometrienund Reflektorgeometrienzu. T2 - DGZfP DACH Tagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Ausbildung KW - Wellenprüfung KW - Ultraschall KW - Zuverlässigkeit KW - POD PY - 2019 AN - OPUS4-49683 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bäßler, Ralph T1 - Review: Polymer Coatings ‐ A Guide to Chemistry, Characterization, and Selected Applications N2 - This book grew out of a course on polymer coatings held by the author at the university. It shall serve as an introduction to the wide field of polymer coatings. It is not intended to cover completely all facts on polymer coatings. All chapters are well structured. Selected figures and formulas illustrate the content and contribute to a good understandability. At the end of each chapter some hints for further reading are provided. Finally, the book fulfills its intention to introduce into the topic by providing basics on science and technology of polymer coatings, suitable for chemists in industry, materials scientists, polymer chemists and physical chemists. KW - Corrosion KW - Coating KW - Polymer PY - 2020 DO - https://doi.org/10.1002/maco.202070024 SN - 1521-4176 SN - 0947-5117 VL - 71 IS - 2 SP - 321 EP - 322 PB - WILEY‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - Development of amorphous silica particle based reference materials for surface functional group quantification N2 - Functionalized nanomaterials (NM) with their unique size-dependent properties are of increasing relevance for current and future developments in various fields such as medical and pharmaceutical industry, computing, electronics or food and consumer products. The performance and safety of NM are determined by the sum of their intrinsic physicochemical properties.1 Besides other key parameters, the particle surface chemistry, which is largely controlled by the chemical nature and density of functional groups and ligands, must be considered for a better performance, stability, and processibility of NM, as well as their interaction with the environment. Thus, particle standards with well-designed surfaces and methods for functional group quantification can foster the sustainable development of functional and safe(r) NM.2 Here we provide a brief overview of the ongoing research in division Biophotonics to design tailored amorphous silica reference particles with bioanalytically relevant functional groups and ligands, for the development of standardized and validated surface functional group quantification methods. T2 - Workshop NanoRiskSD project CY - Berlin, Germany DA - 09.06.2022 KW - Nanoparticle KW - Surface analysis KW - Silica KW - Fluorescence KW - Assay PY - 2022 AN - OPUS4-55004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoell, A. T1 - On the usage of anomalous SAXS to analyzethe structure and composition of bimetallic nanoparticles and quantum dots N2 - Tailor-made nanoparticles are of increasing interest in e.g. catalysis, as sensor materials, analytical assays, or can have superior photophysical properties. A major issue concerning the preparation of high-quality and functional nanoparticles is a good control of particle size, shape, polydispersity, and composition. Small Angle X-ray Scattering (SAXS) is a non-destructive method for the analysis of nanostructures in a wide variety of materials. This method allows determining averaged structural parameters on a length scale from just above atomic sizes up to several 100 nanometers such as sizes, size distributions, volume fractions, and inner surface sizes. Moreover, anomalous Small Angle X-ray Scattering (ASAXS) exploits the anomalous dispersion of the scattering amplitudes near the X-ray absorption edges of the elements contained in the sample. These element sensitive contrast variations can be used to analyse average composition fluctuations on the nm scale. Two kinds of nanoparticles are chosen here to elaborate the advantages of ASAXS in the analysis of complex materials. A facile and efficient methodology is developed for the thermal synthesis of size-tunable, stable, and uniform bimetallic NiCu core–shell nanoparticles (NPs) for various application in catalysis. Their diameter can be tuned in a range from 6 nm to 30 nm and the Ni:Cu ratio is adjustable in a wide range from 1:1 to 30:1. The NPs are structurally characterized by a method combination of transmission electron microscopy, anomalous small-angle X-ray scattering (ASAXS), X-ray absorption fine structure, and X-ray photoelectron spectroscopy. Here, we focus on the ASAXS method and its ability to analyses nanostructure parts and their compositions at once. As a result, a NiCu alloyed core surrounded by a Ni enriched shell and an outer NiO shell was found. Semiconductor nanocrystals (quantum dots, QDs) are well known for their superior photophysical properties and enabled advancements in several key technologies of the 21st century and numerous technological applications like in photovoltaics, LED displays, photocatalysis, and biosensing. To achieve high photoluminescence quantum yields (PLQY) and enhanced photostability the QD core needs to be passivated by a second semiconductor, which possess a larger band gap to confine the charges within the QD core. An important parameter is thereby the lattice mismatch between the core and shell. To avoid strong lattice strain, which would alter the photophysical properties, an intermediary shell can be used as a lattice adapter between the core and the outer shell leading to core/shell/shell systems. These systems have shown to possess high PLQYs combined with a strong long-term stability and can be found in modern QLED displays. ASAXS was used here to better understand the core/shell/shell structure of InP/ZnSe/ZnS QDs to enable a correlation between their structural and photophysical properties. T2 - IUCr - International Union of Crystallography CY - Melbourne, Australia DA - 22.08.2023 KW - ASAXS KW - Quantum dot KW - Core/shell materials KW - Safer by design PY - 2023 AN - OPUS4-58812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - Amorphous, fluorescent silica particles for bioimaging applications N2 - Nowadays amorphous silica nanoparticles (SiO2 NP) are one of the most abundant engineered nanomaterials, with an annual production of hundreds of thousands of tons, that are used in a broad field of industrial products and processes. Since SiO2 NP are highly stable and easily produced on a large scale at low cost, they are widely employed as fillers for rubbers and composites, absorbents, catalysts, advanced coating additives as well as plant growth agents in agriculture, anti-caking agents in food products, or as carrier material in cosmetic industry. Moreover, they are promising candidates for colloidal scaffolds in biomedical applications like bioimaging, sensing or controlled drug delivery. SiO2 NP modified with luminescent chromophores have several advantages as compared to conventional molecular probes like enhanced brightness, ease of designing ratiometric systems, and increased photostability. Here we present our work on multicolored SiO2 NP for imaging and sensing applications. T2 - FUNGLASS Workshop CY - Berlin, Germany DA - 06.03.2024 KW - Sensors KW - Nano KW - Particles KW - Silica KW - Luminescence KW - Fluorescence KW - Quality assurance KW - Method KW - Synthesis KW - Dye KW - pH KW - Surface analysis PY - 2024 AN - OPUS4-62167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, Hans R. A1 - Weidner, Steffen M. A1 - Scheliga, Felix T1 - Polycondensation of L-lactic acid: a deeper look into solid state polycondensation N2 - L-Lactic acid (LA) was condensed in the presence of SnCl2 or 4-toluenesulfonic acid (TSA) at 140 °C, and chain growth without cyclization was observed. In addition, poly(L-lactic acid)s (PLAs) with a degree of polymerization (DP) of 25, 50 or 100 were prepared by water-initiated ring-opening polymerization (ROP). These PLAs were annealed in the solid state at 140 °C and 160 °C in the presence of tin(II) 2-ethylhexanoate (SnOct2, SnCl2 or TSA). The changes in the molar mass distribution and in the topology were characterized by means of matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry and size exclusion chromatography (SEC). With increasing time, fewer side reactions caused higher molar masses and increasing fractions of cyclic polylactides (cPLA) were obtained. Their “saw tooth” pattern in the MALDI-TOF mass spectra indicated the formation of extended ring crystallites in the solid state. TSA was the most active catalyst and caused fewer side reactions than SnCl2, which was the least reactive catalyst. Acetylation of the CH-OH end groups hindered polycondensation and prevented the formation of cPLAs. Reaction mechanisms will be discussed. KW - MALDI-TOF MS KW - Polycondensation KW - Polylaktide KW - Solid state PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625271 DO - https://doi.org/10.1039/d4py01191k SN - 1759-9962 SP - 1 EP - 9 PB - Royal Society of Chemistry (RSC) AN - OPUS4-62527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falkenhagen, Jana A1 - Dalgic, Mete-Sungur A1 - Weidner, Steffen M. T1 - Quantitative MALDI-TOF Mass Spectrometry of Star-Shaped Polylactides Based on Chromatographic Hyphenation N2 - The end groups of three- and four-arm star-shaped polylactides (PLA) with trimethylolpropane and pentaerythritol core structures were functionalized with acetic acid. Reaction products with different degrees of functionalization were analyzed by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry. Additional gradient elution liquid adsorption chromatography (GELAC) measurements were performed to determine the degree of functionalization. This technique enabled clear separation and sufficient quantification of the formed species. These chromatographic data could be used inversely to quantify mass spectrometric results, which are usually biased by the unknown ionization probabilities of different polymer end group structures. Our results showed that, in this particular case, the peak intensity in the MALDITOF mass spectra can be used to semiquantitatively determine the degree of functionalization in incompletely functionalized multiarm PLA. KW - Polylactides KW - MALDI-TOF-MS KW - Gradient elution liquid adsorption chromatography PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625292 DO - https://doi.org/10.1021/jasms.4c00491 SN - 1879-1123 SP - 1 EP - 9 PB - American Chemical Society (ACS) AN - OPUS4-62529 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martynec, T. A1 - Karapanagiotis, Christos A1 - Klapp, S. H. L. A1 - Kowarik, S. T1 - Machine learning predictions of surface migration barriers in nucleation and non-equilibrium growth N2 - Machine learning is playing an increasing role in the discovery of new materials and may also facilitate the search for optimum growth conditions for crystals and thin films. Here, we perform kinetic Monte-Carlo simulations of sub-monolayer growth. We consider a generic homoepitaxial growth scenario that covers a wide range of conditions with different diffusion barriers (0.4–0.55 eV) and lateral binding energies (0.1–0.4 eV). These simulations are used as a training data set for a convolutional neural network that can predict diffusion barriers and binding energies. Specifically, a single Monte-Carlo image of the morphology is sufficient to determine the energy barriers with an accuracy of approximately 10 meV and the neural network is tolerant to images with noise and lower than atomic-scale resolution. We believe this new machine learning method will be useful for fundamental studies of growth kinetics and growth optimization through better knowledge of microscopic parameters. KW - Machine learning KW - Surface migration barriers KW - Material engineering PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532523 UR - https://www.nature.com/articles/s43246-021-00188-1 DO - https://doi.org/10.1038/s43246-021-00188-1 SN - 2662-4443 VL - 2 SP - 1 EP - 9 PB - Springer Nature CY - London AN - OPUS4-53252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Maack, Stefan A1 - Benner, Philipp A1 - Kröll, Mirco A1 - Prager, Jens A1 - Daum, Werner A1 - Casperson, Ralf A1 - Heckel, Thomas A1 - Spaltmann, Dirk A1 - et al., ED - Wahlster, W. ED - Winterhalter, C. T1 - Deutsche Normungsroadmap künstliche Intelligenz T1 - German standardization roadmap on artificial intelligence N2 - Im Auftrag des Bundesministeriums für Wirtschaft und Klimaschutz haben DIN und DKE im Januar 2022 die Arbeiten an der zweiten Ausgabe der Deutschen Normungsroadmap Künstliche Intelligenz gestartet. In einem breiten Beteiligungsprozess und unter Mitwirkung von mehr als 570 Fachleuten aus Wirtschaft, Wissenschaft, öffentlicher Hand und Zivilgesellschaft wurde damit der strategische Fahrplan für die KI-Normung weiterentwickelt. Koordiniert und begleitet wurden diese Arbeiten von einer hochrangigen Koordinierungsgruppe für KI-Normung und -Konformität. Mit der Normungsroadmap wird eine Maßnahme der KI-Strategie der Bundesregierung umgesetzt und damit ein wesentlicher Beitrag zur „KI – Made in Germany“ geleistet. Die Normung ist Teil der KI-Strategie und ein strategisches Instrument zur Stärkung der Innovations- und Wettbewerbsfähigkeit der deutschen und europäischen Wirtschaft. Nicht zuletzt deshalb spielt sie im geplanten europäischen Rechtsrahmen für KI, dem Artificial Intelligence Act, eine besondere Rolle. N2 - On behalf of the German Federal Ministry of Economic Affairs and Climate Action, DIN and DKE started work on the second edition of the German Standardization Roadmap Artificial Intelligence in January 2022. With the broad participation and involvement of more than 570 experts from industry, science, the public sector and civil society, the strategic Roadmap for AI standardization was thus further developed. This work was coordinated and accompanied by a high-level coordination group for AI standardization and conformity. The standardization roadmap implements a measure of the German government’s AI Strategy and thus makes a significant contribution to “AI – Made in Germany”. Standardization is part of the AI Strategy and is a strategic instrument for strengthening the innovation and competitiveness of the German and European economies. Not least for this reason, standardization plays a special role in the planned European legal framework for AI, the Artificial Intelligence Act. KW - Digitalisierung KW - Künstliche Intelligenz KW - Datenwissenschaft KW - Normung Roadmap KW - Data science KW - Artificial intelligence KW - Standardization roadmap KW - Digitization PY - 2022 UR - https://www.din.de/resource/blob/1072988/20bf33d405710a703aa26f81362493bb/ausgabe-2-nrm-ki-data.pdf UR - https://www.dke.de/de/arbeitsfelder/core-safety/normungsroadmap-ki SP - 1 EP - 448 PB - Deutsches Institut für Normung (DIN) CY - Berlin ET - 2. AN - OPUS4-56576 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karapanagiotis, Christos A1 - Hicke, Konstantin A1 - Krebber, Katerina T1 - Eine Sammlung durch Maschinelles Lernen unterstützter Verteilter Faseroptischer Sensoren für Infrastrukturmonitoring T1 - A collection of machine learning assisted distributed fiber optic sensors for infrastructure monitoring N2 - In this paper, we present a collection of machine learning assisted distributed fiber optic sensors (DFOS) for applications in the field of infrastructure monitoring. We employ advanced signal processing based on artificial neural networks (ANNs) to enhance the performance of the dynamic DFOS for strain and vibration sensing. Specifically, ANNs in comparison to conventional and computationally expensive correlation and linearization algorithms, deliver lower strain errors and speed up the signal processing allowing real time strain monitoring. Furthermore, convolutional neural networks (CNNs) are used to denoise the dynamic DFOS signal and enable useable sensing lengths of up to 100 km. Applications of the machine learning assisted dynamic DFOS in road traffic and railway infrastructure monitoring are demonstrated. In the field of static DFOS, machine learning is applied to the well-known Brillouin optical frequency domain analysis (BOFDA) system. Specifically, CNN are shown to be very tolerant against noisy spectra and contribute towards significantly shorter measurement times. Furthermore, different machine learning algorithms (linear and polynomial regression, decision trees, ANNs) are applied to solve the well-known problem of cross-sensitivity in cases when temperature and humidity are measured simultaneously. The presented machine learning assisted DFOS can potentially contribute towards enhanced, cost effective and reliable monitoring of infrastructures. N2 - In diesem Beitrag stellen wir eine Sammlung von verteilten faseroptischen Sensoren (DFOS) vor, die mit Hilfe von Maschinellem Lernen arbeiten und für Anwendungen im Bereich der Infrastrukturüberwachung geeignet sind. Wir setzen hierbei fortschrittliche Signalverarbeitung auf der Grundlage Künstlicher Neuronaler Netze ein, um die Leistungsfähigkeit dynamischer DFOS für die Messung von Dehnungen und Vibrationen zu verbessern. Insbesondere Künstliche Neuronale Netze (ANNs) liefern im Vergleich zu konventionellen und rechenintensiven Korrelations- und Linearisierungsalgorithmen geringere Dehnungsfehler und beschleunigen die Signalverarbeitung, so dass eine Dehnungsüberwachung in Echtzeit möglich ist. Darüber hinaus wenden wir Convolutional Neural Networks (CNNs) an, um dynamische DFOS-Signale zu entrauschen und damit nutzbare Messlängen von bis zu 100 km zu ermöglichen. Es werden Anwendungsbeispiele dieser durch Maschinelles Lernen unterstützten dynamischen DFOS in den Bereichen des Straßenverkehrsmonitorings und der Zug- und Gleisüberwachung aufgezeigt. Im Bereich der statischen DFOS wird Maschinelles Lernen auf das Verfahren der Optischen Brillouin-Frequenzbereichsanalyse (BOFDA) angewendet. Insbesondere CNN erweisen sich hier als sehr robust gegenüber verrauschten Spektren und tragen zu deutlich kürzeren Messzeiten bei. Darüber hinaus werden verschiedene Algorithmen des maschinellen Lernens (lineare und polynome Regression, Entscheidungsbäume, ANNs) angewandt, um das bekannte Problem der Querempfindlichkeit bei DFOS in den Fällen zu lösen, in denen Temperatur und Feuchtigkeit gleichzeitig gemessen werden sollen. Die hier vorgestellten, durch Maschinelles Lernen unterstützten, DFOS können zu einer verbesserten, kostengünstigen und zuverlässigen Überwachung von Infrastrukturen beitragen. KW - Artificial neural networks KW - Brillouin sensing KW - Distributed acoustic sensing KW - Fibre optic sensors KW - Infrastructure monitoring PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569044 DO - https://doi.org/10.1515/teme-2022-0098 SN - 0171-8096 SP - 1 EP - 19 PB - De Gruyter AN - OPUS4-56904 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Küttenbaum, Stefan A1 - Maack, Stefan A1 - Braml, T. A1 - Taffe, A. A1 - Haslbeck, M. T1 - Bewertung von Bestandsbauwerken mit gemessenen Daten. Teil 1: Konzept, Messungen und Leistungsfähigkeit der ZfP‐Verfahren N2 - Gegenüber dem Neubauentwurf können bei der Bewertung von bestehender Bausubstanz Sicherheitsreserven genutzt werden, da Unsicherheiten, die beim Bau auftreten können, besser bekannt oder nicht mehr vorhanden sind. Können solche Unsicherheiten genauer bewertet werden, z. B. durch die Feststellung der genauen Lage der Spannglieder bei einer Spannbetonbrücke, so können Sicherheitsbeiwerte reduziert werden, ohne dass es dabei zu Auswirkungen auf das normativ festgelegte Zuverlässigkeitsniveau kommt. Mittlerweile sind Prüfmethoden an Bauwerken wirtschaftlich einsetzbar und auch so leistungsfähig, dass die für die Tragfähigkeit und Gebrauchstauglichkeit wesentlichen Parameter identifiziert werden können. Ein wesentlicher Punkt ist hierbei die Integration derartiger Messergebnisse in Rechenmodelle, die für die Nachrechnung des Bauwerks verwendet werden. Dies können sowohl semiprobabilistische Rechenmodelle als auch vollprobabilistische Modelle sein. Bei semiprobabilistischen Methoden können aus den Messergebnissen Teilsicherheitsbeiwerte berechnet und abgeleitet werden, die dann in den bekannten Nachweisformaten gemäß den Eurocodes und der Nachrechnungsrichtlinie berücksichtigt werden. Bei vollprobabilistischen Nachweisen können die Messdaten in Form von Verteilungsdichtefunktionen mit gemessenen Variationskoeffizienten direkt in das Rechenmodell eingehen. In einer dreiteiligen Aufsatzreihe werden die Messverfahren und die Nutzung der Ergebnisse bei der Nachrechnung vorgestellt. Der vorliegende Teil 1 zeigt die Möglichkeiten des Einsatzes von zerstörungsfreien Prüfverfahren und bewertet deren Leistungsfähigkeit. Messen heißt wissen. Dieses Wissen spiegelt die Realität wider und soll den Tragwerksplaner bei der Entscheidungsfindung über die Sicherheit und Zuverlässigkeit von Bestandsbauwerken unterstützen. KW - Nachrechnung KW - Zerstörungsfreie Prüfung KW - Messunsicherheit KW - Brücken KW - Beton PY - 2019 DO - https://doi.org/10.1002/best.201900002 SN - 1437-1006 VL - 114 IS - 6 SP - 370 EP - 382 PB - Ernst & Sohn Verlag für Architektur und technische Wissenschaften GmbH & Co. KG CY - Berlin AN - OPUS4-48156 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Sebastian A1 - Selleng, C. A1 - Meng, Birgit T1 - Prompt phase analyses of ultrahigh-performance concrete N2 - Powder X-ray diffraction is a time-consuming and challenging task, especially for preparation of sensitive phases like ettringite and calcium-silicate-hydrate (C-S-H) phases. Fine-grained ultrahigh-performance concrete (UHPC) with an average grain size <100 μm could be investigated directly without time-consuming milling. As a proof of concept, small UHPC cylinders with plain surfaces were investigated with a newly designed sample holder. The comparison with conventionally prepared powder shows the feasibility of fast qualitative phase analysis using this approach. As a great benefit, a depth-dependent analysis, as well as a comparison of surface layers and core material, was carried out. KW - Ultrahigh-performance concrete (UHPC) KW - X-ray diffraction (XRD) KW - Sample holder KW - Fast measurement KW - Spatial analyses PY - 2018 DO - https://doi.org/10.1061/(ASCE)MT.1943-5533.0002163 SN - 1943-5533 SN - 0899-1561 VL - 30 IS - 3 SP - 06018001, 1 EP - 06018001, 5 PB - American Society of Civil Engineers CY - Reston, VA, USA AN - OPUS4-43879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan A1 - Maack, Stefan T1 - ZfP Statik – Zuverlässigkeitsbewertung von Bestandsbauwerken mit ZfP-Ergebnissen N2 - Messen heißt wissen. Dieses Wissen spiegelt die Realität wider und soll den Statiker eines bestehenden Bauwerkes bei der Entscheidungsfindung über die Sicherheit und Zuverlässigkeit der Konstruktion unterstützen. Gegenüber dem Neubauentwurf können bei der Bewertung von bestehender Bausubstanz Sicherheitsreserven genutzt werden, da Unsicherheiten, die beim Bau auftreten können, besser bekannt oder nicht mehr vorhanden sind. Können solche Unsicherheiten genauer bewertet werden, z. B. durch die Feststellung der genauen Lage der Spannglieder bei einer Spannbetonbrücke, so können Sicherheitsbeiwerte reduziert werden, ohne dass es dabei zu Auswirkungen auf das normativ festgelegte Zuverlässigkeitsniveau kommt. Mittlerweile sind Prüfmethoden an Bauwerken wirtschaftlich einsetzbar und auch so leistungsfähig, dass die für die Tragfähigkeit und Gebrauchstauglichkeit wesentlichen Parameter identifiziert werden können. Ein wesentlicher Punkt ist hierbei die Integration derartiger Messergebnisse in Rechenmodelle, die für die Nachrechnung des Bauwerks verwendet werden. Dies können sowohl semiprobabilistische Rechenmodelle als auch vollprobabilistische Modelle sein. Bei semiprobabilistischen Methoden können aus den Messergebnissen Teilsicherheitsbeiwerte berechnet und abgeleitet werden, die dann in den bekannten Nachweisformaten gemäß den Eurocodes und der Nachrechnungsrichtlinie berücksichtigt werden. Bei vollprobabilistischen Nachweisen können die Messdaten in Form von Verteilungsdichtefunktionen mit gemessenen Variationskoeffizienten direkt in das Rechenmodell eingehen. T2 - Abteilungsseminar der Abteilung 8 CY - Online meeting DA - 28.04.2021 KW - Bestandsbauwerke KW - Zuverlässigkeitsbewertung KW - Nachrechnung KW - Zerstörungsfreie Prüfung KW - Messunsicherheit PY - 2021 AN - OPUS4-52531 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karapanagiotis, Christos T1 - Evaluation of the generalization performance of a CNN-assisted BOFDA system N2 - Brillouin Optical Frequency Domain Analysis (BOFDA) is a powerful and well-established method for static distributed sensing of temperature and strain. Recently, we demonstrated a BOFDA system based on convolutional neural network which shortens the measurement time considerably. In this paper, we apply leave-one-out cross validation to evaluate the generalization performance and provide an unbiased and reliable machine learning model for a time-efficient BOFDA system. T2 - 21. ITG/GMA Fachtagung Sensoren und Messsysteme 2022 CY - Nuremberg, Germany DA - 10.05.2022 KW - Fiber optics sensors KW - BOFDA KW - Brillouin distributed sensing KW - Machine learning PY - 2022 UR - https://www.ama-science.org/direct/tagungsband-sensoren-und-messsysteme-2022 SN - 978-3-8007-5835-7 SP - 289 EP - 292 PB - VDE VERLAG GMBH AN - OPUS4-55183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Adaption of fluidic devices for SHM of hydrogen tanks N2 - Frequency analysis of the tank during every filling Passive actuator is integrated inside filling nozzle/ pressure vessel Frequency from 5 kHz to 150 kHz Frequency sweep (Chirp) can be performed Works with every fluid: air, hydrogen, oxygen, argon, water. T2 - H2Safety Kompetenzzentrum CY - BAM Berlin, Germany DA - 07.07.2021 KW - Fluidic device KW - Structural health monitoring KW - Hydrogen tank KW - Ultrasound PY - 2021 AN - OPUS4-52930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wosniok, Aleksander T1 - Brillouin optical frequency-domain analysis for structural health monitoring N2 - We present our achievements in the development of distributed fiber optic sensing systems based on Brillouin optical frequency-domain analysis for structural health monitoring. The focus of the applications is on the gapless monitoring of geotechnical structures, large area infrastructures and electrical grids. The work includes the latest use of machine learning algorithms to reduce measurement time by coexistent increasing the measurement accuracy. T2 - 4th Workshop on Optomechanics and Brillouin Scattering CY - Erlangen, Germany DA - 14.06.2022 KW - Distributed sensing KW - BOFDA KW - Optical fiber sensor KW - Brillouin distributed fiber sensor PY - 2022 AN - OPUS4-55173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Maack, Stefan A1 - Bertovic, Marija A1 - Radtke, Martin A1 - et al., ED - Wahlster, W. ED - Winterhalter, C. T1 - Deutsche Normungsroadmap künstliche Intelligenz N2 - Rund ein Jahr haben DIN und DKE in einem gemeinsamen Projekt mit dem Bundesministerium für Wirtschaft und Energie und zusammen mit ca. 300 Fachleuten aus Wirtschaft, Wissenschaft, öffentlicher Hand und Zivilgesellschaft an der Normungsroadmap Künstliche Intelligenz gearbeitet. Eine hochrangige Steuerungsgruppe unter dem Vorsitz von Prof. Wolfgang Wahlster hat die Erarbeitung koordiniert und begleitet. Ziel der Roadmap ist die frühzeitige Entwicklung eines Handlungsrahmens für die Normung und Standardisierung, der die internationale Wettbewerbsfähigkeit der deutschen Wirtschaft unterstützt und europäische Wertmaßstäbe auf die internationale Ebene hebt. KW - Künstliche Intelligenz KW - Normung KW - Roadmap PY - 2020 UR - https://www.din.de/resource/blob/772438/ecb20518d982843c3f8b0cd106f13881/normungsroadmap-ki-data.pdf VL - 2020 SP - 1 EP - 232 PB - Deutsches Institut für Normung (DIN) CY - Berlin ET - 1. AN - OPUS4-51733 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karapanagiotis, Christos T1 - Time-efficient CNN-assisted BOFDA N2 - Brillouin Optical frequency domain analysis (BOFDA) is a well-known technique in distributed Fiber sensing for temperature and strain monitoring. In this study, we applied a signal post-processing method based on convolutional neural networks (CNNs) and we show that in comparison to conventional methods based on Lorentzian curve fitting (LCF), our CNN model is more robust against noise and can shorten the measurement time by more than 9 times. This will open the way for applications, where faster monitoring is needed. T2 - Machine learning workshop CY - Online meeting DA - 18.03.2021 KW - Temperature and strain sensing KW - Machine learning KW - Distributed fiber-optic sensors PY - 2021 AN - OPUS4-52305 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Johann, Sergej A1 - Strangfeld, Christoph A1 - Müller, Maximilian A1 - Mieller, Björn A1 - Bartholmai, Matthias ED - Emri, I. T1 - RFID sensor systems embedded in concrete – requirements for long–term operation N2 - Structural Health Monitoring (SHM) is an important topic for Industry 4.0. More and more systems are embedded in different materials and are connected to each other. To embed sensors for a long time in concrete, an exact preparation is required. In this paper, we identify Radio-Frequency Identification (RFID) as promising technology for monitoring of concrete structures. This paper present the concept for long term monitoring, defines the requirements and shows first development steps, for example, the system design, the possibilities of sensor connection, and an encapsulation for embedding in concrete. T2 - 33nd Danubia Adria Symposium on Advances in Experimental Mechanics CY - Portoroz, Slovenia DA - 20.09.2016 KW - RFID sensors KW - Long-term requirements KW - Structural health monitoring KW - Passive RFID KW - Sensor requirements KW - Sensors in concrete KW - Smart structures PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S2214785317308283 DO - https://doi.org/10.1016/j.matpr.2017.06.053 SN - 2214-7853 VL - 4 IS - 5, Part 1 SP - 5827 EP - 5832 PB - Elsevier Ltd. AN - OPUS4-41581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hase, Felix T1 - Design und Aufbau verschiedener Messysteme zur Ermittlung des Feuchtigkeitsprofiles von Estrich N2 - Zur Bestimmung des Feuchtigkeitsgehalts von Fußbodenstrich werden bis zu diesem Zeitpunkt hauptsächlich die Calcium-Carbid Methode (CM) oder das thermogravimetrische Darr-Verfahren angewendet. Für die Anwendung beider Methoden muss der Estrich zerstört werden. Die aus der Messung gewonnenen Messdaten sind jedoch nur einmalig und punktuell. Damit sind diese Verfahren nur bedingt aussagefähig. Des Weiteren variieren die Messdaten von Estrichtyp zu Estrichtyp. Zusammen mit Partnern aus der Forschung und Industrie wird an der Bundesanstalt für Materialforschung und -prüfung (BAM) eine Messkampagne durchgeführt, mit dem Ziel, verschiedene Prüfverfahren zur Bestimmung des Feuchtigkeitsgehalts hinsichtlich ihrer Genauigkeit und Sensitivität zu untersuchen. Hierfür sind zwei neue Messsysteme entwickelt worden, welche auf der zerstörungsfreien Messung basieren. Dafür werden in den Estrich zum einen Sensoren, welche die relative Luftfeuchte messen und zum anderen eine Multiringelektrode, eingebettet. Die Messungen finden in verschiedenen Estricharten und Materialdicken statt, welche bei Normklima mit einer Temperatur von 23 °C und einer relativen Luftfeuchtigkeit von 50 % trocknen. Aus den erhaltenen Messdaten kann ein zeitliches und tiefenabhängiges Feuchtigkeitsprofil des Estrichs erstellt werden. KW - Korrespondierende relative Luftfeuchte KW - Ausgleichsfeuchte KW - Estrichfeuchte KW - Feuchtemesstechnik PY - 2016 SP - 1 CY - Berlin AN - OPUS4-37698 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gebauer, D. A1 - Gutierrez, B. A1 - Marx, S. A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Pirskawetz, Stephan A1 - Breit, W. A1 - Mechtcherine, V. A1 - Grahl, K. A1 - Thiel, T. A1 - Schickert, M. A1 - Krüger, M. T1 - Interrelated data set from nondestructive and destructive material testing of concrete compressive strength specimens N2 - This data set contains three different data types obtained from concrete specimens. For each specimen, the rebound numbers, ultrasonic data (ultrasonic velocity, time of flight), and destructive concrete strength are given. Two kind of specimen geometries were tested: cubes and drilled cores. The files are labeled according to the specimen geometry as "cube" or "core" and the type of measurement data as "compressive_strength", "rn_R" and "rn_Q" for rebound numbers as well as "us" for ultrasonic data. The ultrasonic data were generated by six independent laboratories, the rebound numbers by five independent laboratories and the destructive tests by one laboratory. The designation of each specimen establishes the relationship between the different data types. KW - Non-destructive testing KW - Rebound number KW - Ultrasonic pulse velocity KW - Compressive concrete strength KW - Interlaboratory comparison PY - 2023 DO - https://doi.org/10.7910/DVN/AFCITK PB - Harvard College CY - Cambridge, MA, USA AN - OPUS4-57499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine T1 - Interpretation of NMR signals from partly saturated sandstones N2 - The development of prevention methods and the detection of moisture related damages in buildings and transport infrastructure at an early stage are current issues in the field of non-destructive testing in civil engineering. Especially the subject of partial saturation requires further research since it is more likely to occur than full saturation of the material. In fact, partial saturation in porous media is even more complicated because both fully and partly saturated pores (i.e. pores in which the surfaces are covered with thin water layers) are present. As the non-destructive method nuclear magnetic resonance (NMR) enables the measurement and quantification of relative low moisture contents, it is suitable for the investigation of partly saturated porous building materials. Nevertheless, the differentiation between partly and fully saturated pores is still a challenge. Therefore, in this study, we investigate two sandstones types (Bozanov and Schönbrunner sandstone) at various defined saturation states by using NMR. Furthermore, we measure the relative humidities within the samples and compute the water layer thicknesses (WLT) along the pore walls of all pore sizes to calculate the corresponding degree of pore saturation. To finally assign the NMR signals to pore sizes and to differentiate between partly and fully saturated pores, the water content distribution obtained from the WLT calculation is used for calibration of the relaxation-time distribution. In this extended abstract, selected results only for Schönbrunner sandstone are presented. T2 - ISEMA 2021 CY - Online meeting DA - 26.07.2021 KW - NMR KW - Relative humidity KW - Water layer thickness KW - Partial pore saturation KW - Pore-size distribution PY - 2021 SN - 978-1-7281-8736-5 VL - 2021 SP - 111 EP - 115 PB - IEEE AN - OPUS4-53045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stroh, Julia A1 - Meng, Birgit A1 - Emmerling, Franziska T1 - Deterioration of hardened cement paste under combined sulphatechloride attack investigated by synchrotron XRD N2 - The exact mechanisms of the phase transitions caused by a combined sulphate-chloride attack are discussed controversially. The main points concern the mutual influences of sulphate and chloride ions during the secondary binding processes of these anions within cement hydrate phases. We simulated combined sulphate-chloride attack under laboratory conditions using solutions containing NaCl and Na2SO4 in different concentrations. Three sample compositions were used for the preparation of the specimens. In two of them, 30% of Portland cement was replaced by supplementary cementitious materials (fly ash, slag). The phase distribution in the samples was determined using synchrotron X-ray diffraction. The analysis with high spatial resolution allows the localisation of the secondary phase formation in the microstructural profile of the sample. A mechanism of the phase developments under combined sulphate-chloride attack is derived. KW - Cement paste KW - Sulphate-chloride attack KW - Portland cement KW - Mineral additions PY - 2016 DO - https://doi.org/10.1016/j.solidstatesciences.2016.04.002 IS - 56 SP - 29 EP - 44 PB - Elsevier Masson SAS CY - Issy les Moulineaux cedex; France AN - OPUS4-35936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim T1 - Multivariate Auswertung von Radarsignalen zur Bestimmung typischer Feuchteschäden in Fußböden N2 - Leitungswasserschäden nahmen im Jahr 2018 mit rund 2,9 Milliarden Euro den größten Posten bei Gebäudeversicherungen ein und verursachten damit mehr Kosten, als Elementar-, Feuer, Sturm- und Hagelschäden zusammen. Neutronensonden helfen hier bereits bei der horizontalen Eingrenzung eines Feuchteschadens, wobei die vertikale Unterscheidung betroffener Schichten nur durch die zerstörende Entnahme von Bohrkernen vorgenommen werden kann. Der parallele Einsatz des Radarverfahrens soll hier mit seiner hohen Sensitivität für Wasser künftig zu einem erhöhten Informationsgehalt beitragen und eine kostengünstigere Schadensdiagnose und Planung der Reparaturmaßnahmen ermöglichen. In einem laufenden Forschungsvorhaben werden in systematischen Laborstudien gängige Schadensfälle an häufig anzutreffenden Fußbodenaufbauten simuliert und deren Einfluss auf das Radarverfahren untersucht. Die Bewertung der Schadensträchtigkeit zugeführter Wassermengen erfolgt mithilfe von Luftfeuchtesensoren, welche in der Dämmebene platziert sind. Beim Aufbau der Fußbodenstrukturen kommen Zement- und Anhydritestriche, sowie die Dämmmaterialen Styropor, Styrodur, Glaswolle und Perlite-Schüttung mit variierenden Schichtdicken zum Einsatz. Die Robustheit der zu entwickelnden Messmethode gegenüber derartig verschiedenen und in der Praxis häufig unbekannten Schichtstrukturen stellt eine besondere Herausforderung dar und soll durch den Einsatz multivariater Datenauswertung erhöht werden. Diesbezüglich empfehlen bisherige Ergebnisse die Betrachtung der örtlichen Verteilungen qualitativer Signalmerkmale wie Amplituden, Laufzeiten und Frequenzen im Radargramm (B-Scan). Deren Eignung für reale Schadensfälle außerhalb der Laborumgebung wird hierbei stets kritisch hinterfragt und soll weiterführend an Praxiseinsätzen validiert werden. T2 - 80. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Online Meeting DA - 18.05.2020 KW - Radar KW - Feuchte KW - Fußboden KW - Multivariate Datenauswertung PY - 2020 AN - OPUS4-50862 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Willms, Thomas A1 - Kryk, Holger A1 - Hampel, Uwe T1 - An improved method for the analysis of the reaction products of the partial isobutane oxidation by gas chromatography using a green solvent N2 - In the present work, an improved GC/MS method for the analysis of the reaction products of the non-catalytic partial oxidation of isobutane at a starting temperature of 25°C has been developed and compared to a previously published method. Two green GC-solvents (dimethyl carbonate (DMC), diethyl carbonate (DEC)) and several internal standards (hexane, benzene, toluene, DEC) have been tested. The separation of the products at low retention times (methanol, isobutane, isobutene) could be significantly improved. For the liquid main products t-butyl hydroperoxide (TBHP), di-t-butyl peroxide (DTBP), t-butanol (TBA), propanone and most trace products (isopropanol, isobutanal, methyl formate, isopropyl formate, t-butyl formate and some acetates – 24 compounds in total), a coefficient of determination CoD > 0.999 has been achieved. For all weighing and GC/MS measurements uncertainties have been calculated. The peaks of the peak pair t-butyl formate (CoD >0.999) and isobutanol (CoD >0.99), have been simulated and used for calibrations. DEC gave a decomposition of TBHP on the column. With DMC, a problem of peak purity of TBHP appeared but could be resolved. The use of the green solvent DMC, compared to also studied traditional solvents like heptane and toluene, proved to be very beneficial, since it also permitted to determine polar compounds, e. g. carbon dioxide and formic acid. KW - GC/MS KW - Green solvent KW - Method development KW - Peroxide KW - Measurement uncertainties KW - Oxidation products KW - Simulation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632026 DO - https://doi.org/10.1016/j.chroma.2025.465892 SN - 0021-9673 VL - 1753 SP - 1 EP - 16 PB - Elsevier CY - Amsterdam AN - OPUS4-63202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Anwendung von ZFP-Verfahren zur Material- und Feuchtezustands-Charakterisierung im Bauwesen N2 - Zu viel Feuchte im Unterboden führt zu Schäden an teuren Oberböden wie z. B. Parkett, Laminat, Fliesen, etc. Zum Testen der Restfeuchte existieren in Deutschland zwei anerkannte zerstörende Verfahren, die CM- und die Darr-Methode. Die BAM testet und validiert einige zerstörungsfreie Messverfahren und vergleicht diese mit gravimetrischen und zerstörenden Prüfungen. Weiterhin wird mittels eingebetteter Luftfeuchte-Sensoren der Trocknungsverlauf verfolgt. Weiterhin wird gezeigt, dass mit Kenntnis der Porenvolumenverteilung und der Kelvin-Gleichung die Luftfeuchte in die absolute Massenfeuchte überführt werden kann. T2 - Deutsche Sachverständigentag für Parkett, Fussbodentechnik und Unterböden CY - Kassel, Germany DA - 31.05.2017 KW - Belegreife KW - Feuchte KW - Sorptions-Isotherme KW - Embedded Sensors KW - Estrich PY - 2017 AN - OPUS4-40504 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Ladu, Luana A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in Africa N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in Africa. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2023. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. This study is part of a global project that covers various other countries (see www.qi-fokus.de). KW - Testing KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - TIC KW - Quality infrastructure PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588625 UR - https://www.qi-fokus.de SP - 1 EP - 45 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-58862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Digitalization in conformity assessment in North Macedonia - A QI-FoKuS study N2 - This report summarizes findings from the first comprehensive study on digitalization in conformity assessment in North Macedonia. The reults are based on data from a survey among conformity assessment bodies (CABs) conducted in 2022. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. This study is part of a global project that covers various other countries (see www.qi-fokus.de). KW - COVID-19 KW - Calibration KW - Certification KW - Conformity assessment KW - Conformity assessment body KW - Digital transformation KW - Digitalization KW - Laboratory KW - Quality infrastructure KW - TIC KW - Testing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565986 UR - https://www.qi-fokus.de SP - 1 EP - 44 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-56598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Studying cellular uptake and processing of nanoparticles by LA-ICP-MS N2 - In recent years, elemental imaging of biological samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining in importance. Latest improvements regarding spatial resolution (down to 1 µm) and washout time make LA-ICP-MS particularly interesting for single cell analysis. Many current nanomaterials can serve as contrast agents in cellular or tissue imaging, drug delivery vehicles or therapeutics, whereas others can cause toxic effects. In order to evaluate nano-bio interactions, the number of nanoparticles (NPs) inside cells as well as their localisation within cellular substructures is of particular interest. LA-ICP-MS was used to study the NP pathway from uptake, via intracellular processing up to cell division. Fibroblast cells were incubated with different metallic NPs under varying experimental conditions. For LA analysis the cells were fixed with formaldehyde and dried. Our results show that LA-ICP-MS is able to localise NP aggregates within cellular substructures. The NPs accumulate in the perinuclear region in the course of intracellular processing, e.g. multivesicular fusion and endosomal maturation, but do not enter the nucleus [1, 2]. A strong dependence of NP uptake on concentration and incubation time was found. Additionally, the number of NPs internalized by individual cells was determined and variations within the cell population became visible. A new laser ablation system providing a short washout time (50 ms) together with small spot sizes (< 4 µm) and high repetition rates allows high spatial resolution applications. First results of cell imaging will be shown. The findings demonstrate the potential of LA-ICP-MS enabling insight into NP uptake and intracellular distribution dependent on experimental parameters. T2 - 8th Nordic Conference on Plasma Spectrochemistry CY - Loen, Norway DA - 05.06.2016 KW - Imaging KW - LA-ICP-MS KW - Cell KW - Nanoparticles PY - 2016 AN - OPUS4-36500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia A1 - Ladu, Luana A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. ED - Jakobs, K. ED - Kim, D.-h. T1 - Digital maturity in the conformity assessment industry: An explorative study from Germany N2 - The services of Conformity Assessment Bodies (CABs) are essential to provide for trust in and safety of digital products and services by demonstrating that requirements from standards are met. Thus, it is vital that CABs are ready to fulfil their tasks also in the digital transformation, having the necessary capabilities and resources. Our study is the first to comprehensively assess the digital maturity in the CA industry and to provide some insights into the readiness of the industry to support and at the same time benefit from the digital age. To this end, we developed and implemented a digital maturity model tailored to the CA industry. In this paper, we present first results from our survey among 354 accredited CABs in Germany. With our research we contribute to better understand the digital transformation and maturation of CABs along distinctive stages. The findings suggest that the transformation process in the CA industry is just at the beginning, with the majority of CABs still in early stages of digital maturity. Also, only a few of them already exploit the latest digital technologies and applications like artificial intelligence, blockchain or big data analytics. Nevertheless, CABs regard digitalization as a big opportunity – for themselves and their industry. T2 - 26th EURAS Annual Standardisation Conference – Standards for Digital Transformation: Blockchain and Innovation CY - Glasgow, Great Britain DA - 08.06.2022 KW - Digital maturity KW - Digital transformation KW - Digitalization KW - Quality infrastructure KW - Conformity assessment KW - Conformity assessment body KW - Testing KW - Certification KW - Inspection KW - Laboratory PY - 2022 SN - 978-3-95886-446-7 SP - 253 EP - 272 PB - Verlag Mainz CY - Mainz AN - OPUS4-55065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braml, T. A1 - Wimmer, J. A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Kuhn, T. A1 - Reingruber, M. A1 - Gordt, A. A1 - Hamm, J. ED - Krieger, J. T1 - Datenablage als Grundlage für den digitalen Zwilling eines Bauwerks – Verwaltungsschale BBox N2 - Der Beitrag stellt die Entwicklung und die Systemarchitektur der BBox am Beispiel von 2 Projekten dar. T2 - 1. Fachkongress Digitale Transformation im Lebenszyklus der Verkehrsinfrastruktur CY - Esslingen, Germany DA - 29.06.2021 KW - Digitaler Zwilling KW - Bestandsbauwerke KW - Physikalisches Modell PY - 2021 SN - 978-3-8169-3530-8 SP - 75 EP - 84 PB - expert Verlag CY - Tübingen AN - OPUS4-52938 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Bartolac, M. A1 - Bien, J. A1 - Górski, M. A1 - Keßler, S. A1 - Küttenbaum, Stefan A1 - Kuzawa, M. A1 - Ley, J. A1 - Maack, Stefan A1 - Mendler, A. A1 - Ryjáček, P. A1 - Santos, L. A1 - Verstrynge, E. ED - Keßler, S. ED - Limongelli, M. P. ED - Apostolidi, E. T1 - Chapter 2: Condition survey - Testing and monitoring methods N2 - The through-life management of our constantly ageing infrastructure is a basic requirement in order to ensure their structural safety and serviceability. Each structure experiences deterioration processes with time leading to a decrease of structural safety and serviceability. The design of new structures considers the expected deterioration for a defined period, the design service life. However, a frequent survey of structural safety controlling structural condition should be mandatory and a maintenance plan should be an integral part of the design. In addition, many structures have exceeded their design service life already or are very close to it leading to an increasing demand for condition assessment. On the one hand, assumptions made during design are not valid any more due to change of the loads, e.g., increasing traffic loads in terms of number and weights. On the other hand, design codes evolved over time in such a way that existing structures do not comply with today’s standards. In all these cases, the through-life management is an important tool to maintain the accessibility of existing structures with known reliability. In line with the new Model Code for Concrete Structures, which includes guidance for both – design of new structures and assessment of existing structures, the Task Group 3.3 focused on the compilation of a state-of-the-art guideline for the through-life management of existing concrete structures, including: Data acquisition by testing and monitoring techniques; Condition assessment for the evaluation of existing structures; Performance prediction using advanced methods; Decision-making procedures to perform a complete assessment of existing structure. The overall objective of the through-life management is the assessment of the current condition and the estimation of the remaining service life under consideration of all boundary conditions. KW - Life management KW - Concrete KW - Non-destructive testing KW - Structural health monitoring KW - State-of-the-art PY - 2023 UR - https://doi.org/10.35789/fib.BULL.0109 SN - 978-2-88394-172-4 DO - https://doi.org/10.35789/fib.BULL.0109.Ch02 SN - 1562-3610 VL - fib Bulletin 109 SP - 16 EP - 38 PB - Fédération internationale du béton (fib) CY - Lausanne AN - OPUS4-59110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bartelmeß, Jürgen A1 - Zimmek, David A1 - Bartholmai, Matthias A1 - Strangfeld, Christoph A1 - Schäferling, M. T1 - Fibre optic ratiometric fluorescence pH sensor for monitoring corrosion in concrete N2 - In this communication a novel concept for pH sensing is introduced which is specifically adapted to monitor carbonation induced corrosion in concrete structures. The method is based on a ratiometric measurement principle, exploiting the pH sensitive colour switching of thymol blue in the basic pH regime and the emissive properties of two different (Zn)CdSe/ZnS core shell quantum dots. The transition point of thymol blue in a Hydrogel D4 matrix was determined to be at around pH 11.6, which fits ideally to the intended application. Next to the fundamental spectroscopic characterization of the ratiometric response, a new design for a sensor head, suitable for the incorporation into concrete matrices is presented. Toward this, a manufacturing process was developed which includes the preparation of a double layer of polymers containing either thymol blue or a quantum dot mixture inside a porous ceramic tube. Results of a proof-of-priciple performance test of the sensor head in solutions of different pH and in cement specimens are presented, with encouraging results paving the way for future field tests in concrete. KW - Fiber optic sensing KW - PH monitoring in concrete KW - Embedded sensors KW - Ratiometric fluorescence PY - 2020 DO - https://doi.org/10.1039/c9an02348h VL - 145 IS - 6 SP - 2111 EP - 2117 PB - Royal Society of Chemistry AN - OPUS4-50381 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia A1 - Asna Ashari, Parsa T1 - Impact of the COVID-19 Pandemic on Conformity Assessment: Insights from a Multinational Study N2 - The COVID-19 pandemic has posed new and manifold challenges to organizations and their operations worldwide. Conformity assessment bodies (CABs), such as testing or medical laboratories, certification, and inspection bodies, are also affected by the associated disruptions. Their situation in this crisis is highly relevant, as CABs are essential pillars of the quality infrastructure: Their activities ensure that products and services meet requirements as defined in standards and regulations, thereby contributing to their safety and reliability. Considering the roles and functions of CABs in economy, health, and innovation, the question arises how CABs and their operations were affected by the pandemic and how they responded. To this end, we present the results of an international survey of 986 CABs of all types in Germany, the UK, Italy, and New Zealand. Overall, CABs reported on average a negative development of demand during the pandemic, facing restrictions in all countries. In addition, the pandemic had overall negative impact on the CABs’ investment and innovation activities. However, investments in digital infrastructure were increased as countermeasure, with CABs reporting an increased need for digitalization. Resources relevant to organizational resilience were available to different extents, affecting the speed of response to the challenges of the pandemic. The paper highlights and discusses results from in-depth analyses, which are relevant for policy makers and industry alike. T2 - 25th EURAS Annual Standardisation Conference – Standardisation and Innovation CY - Online meeting DA - 06.09.2021 KW - Conformity assessment KW - Resilience KW - Digitalization KW - Crisis KW - Pandemic KW - Corona KW - COVID-19 KW - Laboratory KW - Quality infrastructure PY - 2021 AN - OPUS4-53225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Vertrauen in Qualität und Sicherheit in der Digitalisierung. QI-Digital: Eine Initiative der zentralen Akteure der Qualitätsinfrastruktur in Deutschland N2 - „Made in Germany“ steht für Vertrauen in Qualität und Sicherheit, das auch in der digitalen und grünen Transformation gelten soll.  In einer zunehmend digitalisierten Welt muss auch die Qualitätssicherung von Produkten, Prozessen und Dienstleistungen neu gedacht werden. Ziel der Initiative QI-Digital ist es, die bewährte Qualitätsinfrastruktur (QI) noch besser zu machen. Für eine moderne und effiziente Qualitätssicherung. Die zentralen Akteure der deutschen QI haben sich in QI-Digital zusammengeschlossen, um konkrete Lösungen für innovative Anwendungsfälle zu entwickeln. Dabei ist ein ganzheitlicher und praxisbezogener Ansatz wichtig, in dem ein weiter Kreis interessierter Stakeholder aktiv eingebunden wird. Im Kurzvortrag wird die Initiative, inkl. ihrer Akteure, Ziele, Projekte und Beteiligungsmöglichkeiten vorgestellt. T2 - Treffen BDI Arbeitskreis Technikpolitik CY - Berlin, Germany DA - 06.09.2022 KW - Qualitätsinfrastruktur KW - Digitalisierung KW - Wasserstofftankstelle KW - Additive Fertigung KW - QI-Cloud KW - digitale Transformation PY - 2022 AN - OPUS4-55635 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weise, Frank T1 - AKR unter kombinierten Einwirkungen - Rissbildungs- und Transportmechanismen N2 - Die vorstehend dargestellten Untersuchungen lassen sich wie folgt zusammenfassen: • Mit dem für die mechanische Vorschädigung entwickelten Versuchsstand und gewählten Prüfregime können die für die ermüdungsinduzierte Schadensevolution typische stabilisierende und stabile Phase in der auf Zug beanspruchten Betonrandzone gut abgebildet werden. So wurde dort zum Beispiel, ausgehend von dem hier gewählten praxisnahen Belastungsregime, mit Ultraschall in der Ruhephase durch das Trockenschwingen ein maximaler Abfall des relativen dynamischen E-Moduls von ca. 8 - 10 % ermittelt. • Mit aufbauenden kapillaren Aufsaugversuchen wurde gezeigt, dass die erzeugte Betondegradation zu einer moderaten Erhöhung der Aufnahme des Prüfmediums führt. • Zur Bewertung der Auswirkungen einer alleinigen Vorschädigung (Trockenschwingen) auf die schädigende AKR mittels Performance-Prüfung ist die Klimawechsellagerung aufgrund der einseitigen Tausalzbeaufschlagung am besten geeignet. Die hier ermittelten Dehnungsverläufe lassen auf einen moderaten Einfluss der mechanischen Vorschädigung auf die AKR schließen. • Die zusätzlich im Kontext der Nasschwingversuche durchgeführten 60°C Betonversuche zeigen, dass die zyklische Beanspruchung vor und nach dem Aufbringen der Tausalzlösung die schädigende AKR gleichfalls moderat erhöht. In derzeit laufenden ergänzenden Untersuchungen wird der separate Einfluss der ermüdungsinduzierten Rissbildung auf die schädigende AKR an homogen, stärker geschädigten Prüfkörpern mit einem hohen inneren AKR-Schädigungspotenzial im 60°C Betonversuch grundhaft analysiert. Zusätzlich wird gegenwärtig der Einfluss der degradierten Betonrandzone auf die Dehnungsverteilung an großformatigen Prüfkörpern über die Höhe im 40°C Betonversuch vertiefend für die makroskopische Modellierung untersucht. T2 - 20. Internationale Baustofftagung ibausil CY - Weimar, Germany DA - 12.09.2018 KW - Betonfahrbahndecke KW - Alkali-Kieselsäure-Reaktion KW - Tausalz KW - LIBS KW - MRFA KW - Nasschemie KW - ZfP PY - 2018 AN - OPUS4-46189 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia A1 - Asna Ashari, Parsa T1 - National Quality Infrastructures in the COVID-19 Pandemic: Insights from a Multinational Study on Impacts and Institutional Responses of Conformity Assessment Bodies N2 - The COVID-19 pandemic has posed new and manifold challenges to organizations and their operations worldwide. Conformity assessment bodies (CABs), such as testing or medical laboratories, certification, and inspection bodies, which are a key part of the Quality Infrastructure and constitute central pillars for trade, health and the innovation system, are also affected by the associated disruptions. However, their services matter more than ever. We present the results of an international survey of 986 CABs of all types in Germany, the UK, Italy, and New Zealand to highlight and compare economic impacts, the resilience of this industry as well as issues of digitalization. T2 - Eu-SPRI 2021 Conference: Science and innovation - an uneasy relationship? CY - Online meeting DA - 09.06.2021 KW - Konformitätsbewertung KW - COVID-19 KW - Corona KW - Qualitätsinfrastruktur KW - Conformity Assessment KW - Certification KW - Testing KW - Resilience PY - 2021 AN - OPUS4-52789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braml, T. A1 - Wimmer, J. A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Kuhn, T. A1 - Reingruber, M. A1 - Gordt, A. A1 - Hamm, J. ED - Krieger, J. T1 - Datenablage als Grundlage für den digitalen Zwilling eines Bauwerks – Verwaltungsschale BBox N2 - Der Weg zur digitalen Brücke ist eingeschlagen. Im Bereich der Planung, Bauüberwachung und -ausführung wird aktuell das Building Information Modelling (BIM) eingeführt. Ist eine Brücke in der Baulast von Bund und Ländern errichtet, wird ihr Zustand im Zuge von wiederkehrenden Bauwerksprüfungen nach DIN 1076 lückenlos überwacht. Abgespeichert werden die Informationen der Überwachung in einer Datenbank (ASB-ING Teilsystem Bauwerksdaten). Aus dieser Datenbank können anschließend relevante Informationen in ein objektspezifisches Bauwerksbuch überführt werden. In dieser Datenbank werden im Vorfeld definierte Daten abgespeichert. Reine Messdaten oder aber auch die verwendeten ingenieurtechnisch-physikalischen Modelle verbleiben in der Regel bei den beauftragen Dienstleistern. Zusammengefasst existieren verschiedene parallele Insellösungen der Informationsablage. Gegenstand verschiedener Forschungsanstrengungen ist es nun Lösungen zu finden, die einen ganzheitlichen Ansatz für den Informationsfluss von der Errichtung über den Betrieb bis hin zum Abbruch eines Bauwerkes sicherstellen. Im Rahmen einer prototypischen Entwicklung wird auf Grundlage, des für die Industrie 4.0 entwickelten open source Software Framework Eclipse BaSyx, ein möglicher Lösungsansatz – die Verwaltungsschale BBox (Bridge Box) - präsentiert. Dieser Lösungsansatz stellt das physikalisch-ingenieurtechnische Modell zur Zustandsbewertung der Brücke gedanklich in den Mittelpunkt. Unter der Voraussetzung einer durchgängigen Digitalisierung der gesamten Prozessschritte innerhalb der Lebensdauer der Brücke, kann jeder Planungs- und Fertigungsschritt, die Instandhaltung einschließlich des Rückbaus erfasst werden. Das Besondere hierbei ist, dass auch die Grundlagen der Bewertung, wie Messdaten, mit abgespeichert werden. Die Modellstruktur der Verwaltungsschale erlaubt hierbei eine bedarfsgerechte Granularität hinsichtlich der Messdaten auf allen virtuellen Ebenen, um das physikalisch-ingenieurtechnisch Modell mit Daten zu versorgen. Die gewählte Form der Datenablage bildet den Grundstein für zukünftige KI-Auswertungen z.B. mit den Methoden des Maschinellen Lernens (ML). Der Zugriff auf die dafür jeweils benötigten Daten wird durch die Ablage der Daten einschließlich Metadaten und den Einsatz einer Standard S3 Schnittstelle stark vereinfacht. Der Beitrag stellt die Entwicklung und die Systemarchitektur der BBox am Beispiel von 2 Projekten dar. T2 - 1. Fachkongress Digitale Transformation im Lebenszyklus der Verkehrsinfrastruktur CY - Esslingen, Germany DA - 29.05.2021 KW - Brücke KW - Digitalisierung KW - Digitaler Zwilling KW - Datenablage PY - 2021 UR - https://elibrary.narr.digital/article/99.125005/dtv202110075 SN - 2748-9221 IS - 1 SP - 75 EP - 84 PB - expert verlag AN - OPUS4-56159 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Bundesanstalt für Materialforschung und –prüfung (BAM) - Round table presentation N2 - Vorstellung der Tätigkeit der BAM und des FB 8.2 im Rahmen einer geplanten Greminentätigkeit im fib - Action Group 9. T2 - 2nd meeting fib Action Group 9 'Testing and SHM’ CY - München, Germany DA - 14.06.2018 KW - Zerstörungsfreie Prüfung KW - Bauwesen PY - 2018 AN - OPUS4-45215 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weise, Frank A1 - Krütt, Enno A1 - Meng, Birgit T1 - AKR unter kombinierten Einwirkungen - Rissbildungs- und Transportmechanismen N2 - Die vorstehend dargestellten Untersuchungen lassen sich wie folgt zusammenfassen: • Mit dem für die mechanische Vorschädigung entwickelten Versuchsstand und gewählten Prüfregime können die für die ermüdungsinduzierte Schadensevolution typische stabilisierende und stabile Phase in der auf Zug beanspruchten Betonrandzone gut abgebildet werden. So wurde dort zum Beispiel, ausgehend von dem hier gewählten praxisnahen Belastungsregime, mit Ultraschall in der Ruhephase durch das Trockenschwingen ein maximaler Abfall des relativen dynamischen E-Moduls von ca. 8 - 10 % ermittelt. • Mit aufbauenden kapillaren Aufsaugversuchen wurde gezeigt, dass die erzeugte Betondegradation zu einer moderaten Erhöhung der Aufnahme des Prüfmediums führt. • Zur Bewertung der Auswirkungen einer alleinigen Vorschädigung (Trockenschwingen) auf die schädigende AKR mittels Performance-Prüfung ist die Klimawechsellagerung aufgrund der einseitigen Tausalzbeaufschlagung am besten geeignet. Die hier ermittelten Dehnungsverläufe lassen auf einen moderaten Einfluss der mechanischen Vorschädigung auf die AKR schließen. • Die zusätzlich im Kontext der Nasschwingversuche durchgeführten 60°C Betonversuche zeigen, dass die zyklische Beanspruchung vor und nach dem Aufbringen der Tausalzlösung die schädigende AKR gleichfalls moderat erhöht. In derzeit laufenden ergänzenden Untersuchungen wird der separate Einfluss der ermüdungsinduzierten Rissbildung auf die schädigende AKR an homogen, stärker geschädigten Prüfkörpern mit einem hohen inneren AKR-Schädigungspotenzial im 60°C Betonversuch grundhaft analysiert. Zusätzlich wird gegenwärtig der Einfluss der degradierten Betonrandzone auf die Dehnungsverteilung an großformatigen Prüfkörpern über die Höhe im 40°C Betonversuch vertiefend für die makroskopische Modellierung untersucht. T2 - 20. Internationale Baustofftagung ibausil CY - Weimar, Germany DA - 12.09.2018 KW - Betonfahrbahndecke KW - Alkali-Kieselsäure-Reaktion KW - Tausalz KW - LIBS KW - MRFA KW - Nasschemie KW - ZfP PY - 2018 SN - 978-3-00-059950-7 SP - 1 EP - 13 AN - OPUS4-46174 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Global status and trends of Digital Transformation in conformity assessment - Insights from our QI-FoKuS study N2 - This presentation summarizes major findings from an international study in 16 countries and regions on digital transformation in conformity assessment bodies such as testing and calibration laboratories or certification and inspection bodies. It draws from survey data of 1.476 participants and specifically highlights findings on the digital maturity of the organizations, providing an international comparison. T2 - 5º Simposio Latinoamericano de Laboratorios de Calibración y Ensayos - ASOCEC 2022 CY - Online meeting DA - 22.11.2022 KW - Quality Infrastructure KW - Digitalization KW - Testing laboratories KW - Conformity assessment KW - Certification KW - Digital transformation KW - TIC PY - 2022 AN - OPUS4-56385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Global Status and Trends in Digital Transformation and Conformity Assessment – The Case of Germany N2 - This presentation summarizes findings from the first comprehensive study on digitalization in conformity assessment worldwide. The reults are based on data from a survey among conformity assessment bodies (CABs) in Germany conducted in 2022, as well as some first insights from Latin American countries. It highlights the digital maturity of the organizations, the motives, benefits and obstacles of digital transformation as well as the actual technology trends. The study on CABs is part of a global project that covers various countries (see www.qi-fokus.de). T2 - IAAC webinar Digital Transformation in Accreditation CY - Online meeting DA - 28.07.2022 KW - Quality Infrastructure KW - Digitalization KW - Testing laboratories KW - Conformity assessment KW - Certification KW - Digital transformation PY - 2022 UR - www.qi-fokus.de AN - OPUS4-55400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Digitalisierung in der Konformitätsbewertung - Wo stehen wir in Deutschland? Aktuelle Einblicke aus unserer Studie N2 - Im Vortrag werden Erkenntnisse aus einer Umfrage unter deutschen Konformitätsbewertungsstellen (KBS) zum Stand der digitalen Transformation vorgestellt, inkl. deren digitaler Reifegrad, Vorteile und Hindernisse sowie aktuelle Technologietrends. Ein Schwerpunkt liegt dabei auf den Prüflaboratorien. T2 - VUP Jahrestagung der Laborbranche 2022: Laborbranche Digital - Gemeinsam in die Zukunft CY - Leipzig, Germany DA - 23.06.2022 KW - Qualitätsinfrastruktur KW - Digitalisierung KW - Prüflaboratorien KW - Konformitätsbewertung KW - Zertifizierungsstellen KW - Digitale Transformation KW - Digitaler Reifegrad PY - 2022 UR - www.qi-fokus.de AN - OPUS4-55401 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Schumacher, David T1 - Zerstörungsfreie Prüfung mit photonenzählenden und spektralauflösenden Röntgenmatrixdetektoren am Beispiel von Werkstoffverbunden N2 - Diese Arbeit beschäftigt sich mit den Eigenschaften der photonenzählenden und spektralauflösenden Detektortechnik und möglichen Anwendungsgebieten in der zerstörungsfreien Prüfung. Dabei wurden konventionelle und photonenzählende Detektortechniken hinsichtlich der Bildqualität und Anwendbarkeit bei unterschiedlichen Prüfaufgaben verglichen und untersucht, inwiefern sich die Energieschwellwertsetzung auf die erreichbare Bildqualität und eine Materialdiskriminierbarkeit bei verschiedenen radiographischen Verfahren auswirkt. Anhand von Anwendungsbeispielen wurden diese Eigenschaften und deren Auswirkung auf das Messergebnis analysiert. Neben der Radiographie wurden auch dreidimensionale Verfahren wie CT und Laminographie berücksichtigt. Als eine der wichtigsten Eigenschaften der photonenzählenden Detektortechnik wurden zunächst die Energieauflösung des photonenzählenden Detektors und die Homogenität der Energieantwort über größere Detektorbereiche bestimmt. Dabei stellte sich heraus, dass die Energieauflösung eines abgegrenzten Detektorbereichs ca. 32 % bei 60 keV beträgt und die Streuung in der Energieantwort der einzelnen Detektorbereiche ca. 12 % ausmacht, woraus sich eine Gesamtunsicherheit in der spektralen Detektorantwort von ca. 44 % ergibt. Die geringe Energieauflösung und das stark heterogene Verhalten der Detektorbereiche ergeben sich vor allem aus der Detektorelektronik, welche nur eine globale Energieschwellwertsetzung zulässt. Trotz dieser Einschränkungen konnte demonstriert werden, dass auch konventionelle radiographische Verfahren, wie Radiographie oder CT, vom Einsatz der photonenzählenden Technik profitieren. So ist es mit dieser Technik möglich, bei sehr geringen Dosisleistungen (z.B. aufgrund der Durchstrahlung großer Wandstärken von dichten Materialien) noch sehr gute Bildqualitäten zu erreichen. Die hohe Dynamik und Kontrastempfindlichkeit dieser Technik begünstigen die Inspektion von Leichtbauwerkstoffen wie Faserverbunde, was anhand von Vergleichen mit herkömmlicher Detektortechnik und anderen ZfP-Verfahren gezeigt werden konnte. Daneben konnte durch den Einsatz der Energieschwellwertsetzung der Einfluss von nicht bildzeichnender Streustrahlung im Röntgenbild um bis zu 20 % reduziert werden. Die Auswirkungen von Aufhärtungseffekten in der CT konnten sogar um bis zu Faktor 1 000 (in der mittleren quadratischen Abweichung), im Vergleich zu herkömmlicher Detektortechnik, reduziert werden. Der Einsatz von photonenzählender Detektortechnik mit Röntgenblitzröhren ist hingegen nicht sinnvoll, da aufgrund der hohen Photonendichte pro Puls und einer endlichen Totzeit des Detektors in der Größenordnung der Pulsbreite eines Blitzes nur ein geringes Signal detektiert werden kann. Im Hinblick auf eine Materialdiskriminierbarkeit konnte demonstriert werden, dass im Fall einer Radiographie anhand der Energieschwellwertsetzung im Detektor eine materialstärkenunabhängige Diskriminierung zwischen zwei Materialien (hier: Al und Fe) erzielt werden kann. Unter Einsatz mehrerer Energiefenster und eines Verfahrens der explorativen und multivariaten Datenanalyse konnte eine materialaufgelöste CT eines Multi-Material-Phantoms erreicht werden, wobei die Schwächungskoeffizienten der enthaltenen Materialien im relevanten Energieberiech teilweise sehr dicht beieinander lagen. Neben Radiographie und CT wurde auch die Möglichkeit einer materialaufgelösten Laminographie am Beispiel eines glasfaserverstärkten Rotorblatts untersucht. Anhand der Energieschwellwertsetzung war nicht nur eine eindeutige Trennung der Glasfasern von der Epoxidharzmatrix möglich, sondern auch eine signifikante Reduzierung der durch die Laminographie entstandenen Artefakte. Der damit verbundene Gewinn an Information führt zu einer verbesserten Aussagefähigkeit des Untersuchungsergebnisses, was letztendlich eine gesteigerte Betriebssicherheit zur Folge hat. N2 - This thesis investigates the properties of photon counting and energy discriminating digital detector arrays and possible applications in the field of non-destructive testing. Conventional integrating detector technology was compared with photon counting technology in terms of image quality and applicability in different inspection tasks. The impact of internal energy thresholding on material discriminability and achievable image quality was investigated for different radiological methods. The properties of photon counting detectors and their impact on the measurement result were analyzed for different applications including three-dimensional methods such as CT and laminography in addition to radiographic testing. Energy resolution is one of the most important properties of photon counting technology. Therefore, energy resolution was initially determined in addition to the homogeneity of the energy Response across the detector. It was found that the energy resolution amounts to approx. 32 % for a 60 keV monoenergetic spectrum (241Am). In combination with the variance in the response of single detector tiles of approx. 12 % the total uncertainty in the detector energy response appears to approx. 44 %. This low energy resolution and strongly heterogenous detector response result mainly from the detector electronics which only allow setting global energy thresholds. Despite these limitations it was demonstrated that even conventional single energy techniques, such as radiography or CT, benefit from photon counting technology. Thus, this technology allows to gain high quality images even at very low dose rates which might occur e.g. at high wall thickness Penetration of dense materials. The high dynamic range and high contrast sensitivity facilitate the inspection of lightweight materials such as fiber composites which was shown by comparison with integrating technology and other NDT methods. Furthermore, the use of energy thresholding enables to reduce the influence of non-imaging scattered radiation within the X-ray image by about 20 %. The impact of beam hardening artefacts in CT was reduced even up to a factor of 1 000, compared to conventional integrating detector technology. In contrast, the use of photon counting technology with x-ray flash tubes is not useful, since the high photon density within a single flash and a finite dead time of the detector only yield a very low signal. In terms of material discriminability, it was shown that due to energy thresholding a thickness Independent material separation between two materials (here: Al and Fe) can be achieved in the case of a radiography. By using more than two energy windows in combination with multivariate methods of data analysis, a material resolved CT of a multi-material phantom was performed in which six materials were separated distinctly despite very close attenuation coefficients in the relevant energy range. In addition to radiography and CT, the possibility of a material resolved laminography was investigated by means of a glass fiber reinforced wind turbine blade. In addition to a distinct separation between glass fibers and resin matrix, a significant reduction of cross artefacts that inherently arise from the laminography could be achieved. This gain in information yields a higher significance of the measurement and hence an increased reliability of the component or the whole system. T3 - BAM Dissertationsreihe - 165 KW - Zerstörungsfreie Prüfung KW - Photonenzählende Detektoren KW - Radiographie KW - Laminographie KW - Computer-Tomographie KW - Dual-Energy KW - Nondestructive testing KW - Photon counting detectors KW - Radiography KW - Laminography KW - Computed tomography KW - Dual energy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500327 SN - 1613-4249 VL - 165 SP - 1 EP - 172 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-50032 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taffe, A. A1 - Küttenbaum, Stefan A1 - Maack, Stefan T1 - Verwendung von Messergebnissen zerstörungsfreier Prüfverfahren im Bauwesen in statischen Nachweisen - Statistisch abgesicherte Messgrößen beschreiben dem Prüfingenieur die tatsächlich ausgeführte Konstruktion N2 - Zerstörungsfreie Prüfverfahren (ZfPBau-Verfahren) sind auch im Bauwesen stets an praxisrelevante Prüfaufgaben gekoppelt. Die Ermittlung beispielsweise eines Ist-Zustandes im Vorfeld einer Betoninstandsetzung oder die Ermittlung von Schadensursache und Schadensumfang als Folge wiederkehrender Untersuchungen von Brücken nach DIN 1076 sind etablierte Anwendungsgebiete der ZfPBau. Mit der Einführung der Nachrechnungsrichtlinie für Straßenbrücken im Jahr 2011 hat die Nachfrage nach ZfPBau-Dienstleistungen einerseits stark zugenommen, andererseits eröffnet sie Möglichkeiten, in statischen Nachweisen die tatsächlichen Eigenschaften bestehender Konstruktionen rechnerisch anzusetzen. Dazu aber müssen Messergebnisse statistisch bewertet werden können. Dies geschieht durch eine einheitliche Ermittlung der Messunsicherheit, mit der die Voraussetzungen geschaffen werden, um Messergebnisse von ZfPBau-Verfahren in statischen Berechnungen verwenden zu können. Im folgenden Beitrag wird gezeigt, wie Messgrößen der ZfPBau als (stochastische) Basisvariablen in probabilistische Nachweise zur Berechnung der Zuverlässigkeit einfließen können, indem Grenzzustandsgleichungen modifiziert werden. Mit dieser Vorgehensweise sind weitere Schlussfolgerungen aus den Ergebnissen möglich. KW - Bestandsbauwerke KW - Zerstörungsfreie Prüfung KW - Probabilistik KW - Statischer Nachweis KW - Brücken PY - 2018 UR - http://www.bvpi.de/bvpi-content/ingenieur-box/pruefingenieur.htm SN - 1430-9084 VL - 05 IS - 52 SP - 46 EP - 53 PB - Bundesvereinigung der Prüfingenieure für Bautechnik e.V. CY - Berlin AN - OPUS4-45477 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Non-Destructive Testing of Composite Pressure Vessels using Conventional and High-Frequency Eddy Current Technique N2 - Composite-Druckgefäße für den Gefahrguttransport sowie für Wasserstoff- und Erdgasfahrzeuge bestehen aus einem lasttragenden Composite und einer gasdichten, metallischen oder polymeren Barriereschicht (Liner). Zur Untersuchung des Alterungsverhaltens solcher Composite-Druckgefäße wurde in der BAM das interdisziplinäre Themenfeldprojekt COD-AGE durchgeführt. Ziel des Projektes war die Entwicklung von Methoden und Modellen zur Beschreibung und Bestimmung des Alterungsverhaltens von Carbonfaser-Compositen am Beispiel von Druckgefäßen, um eine bessere Vorhersage der Alterung und der sicheren Gebrauchsdauer zu ermöglichen. Ein Schwerpunkt in diesem Projekt war die Bereitstellung geeigneter ZfP-Methoden. Dabei ging es sowohl um versuchsbegleitende Prüfungen, als auch um die mögliche Entwicklung von Prüfeinrichtungen für den späteren praktischen Gebrauch. In dem Vortrag werden Prüfergebnisse der alterungsbegleitenden Wirbelstromprüfung an Composite-Druckgefäßen vorgestellt. In Alterungsversuchen wurden Druckgefäße aus einem ca. 4 mm dicken Aluminiumliner und ca. 8 mm dicker CFK-Ummantelung untersucht. Typisches Einsatzgebiet solcher Druckgefäße sind Atemschutzgeräte der Feuerwehr. Die Druckgefäße wurden sowohl mit konventioneller Wirbelstromtechnik von außen und von innen als auch mit hochfrequenter Wirbelstromtechnik von außen geprüft. Es konnten sowohl Beschädigungen des metallischen Liners, als auch Strukturen des CFK-Geflechts nachgewiesen werden. Eine besondere mechanische Herausforderung bestand in der Prüfung der Innenseite der Liner, da hier eine zylindrische Fläche mit einem Innendurchmesser von 150 mm durch einen Zugang von nur 15 mm Durchmesser geprüft werden muss. N2 - Composite pressure vessels for transporting dangerous goods and for hydrogen and natural gas vehicles consist of a load-bearing composite and a gas-tight, metallic or polymeric barrier layer (liner). To investigate the aging behavior of such composite pressure vessels, BAM carried out the interdisciplinary project COD-AGE. The aim of the project was the development of methods and models for the description and determination of the aging behavior of carbon fiber composites using the example of pressure vessels in order to better predict aging and safe working life. One focus of this project was the provision of suitable NDT methods. These included both test-related tests and the possible development of test equipment for later practical use. In the lecture, test results of the age-related eddy current test on composite pressure vessels are presented. In aging tests, pressure vessels made of an approximately 4 mm thick aluminum liner and approx. 8 mm thick CFRP layer were examined. Typical application of such pressure vessels are respiratory protective devices of the fire department. The pressure vessels were tested using conventional eddy current technology from the outer and inner side as well as with high-frequency eddy current technology. Both damage to the metallic liner and structures of the CFRP could be detected. A particular mechanical challenge was the inspection of the inside of the liners, since a cylindrical surface with an inside diameter of 150 mm has to be tested with an access of only 15 mm diameter. T2 - TAHYA-Workshop CY - Berlin, Germany DA - 27.11.2019 KW - NDT KW - Composite pressure vessel KW - CFRP KW - Eddy current testing PY - 2019 AN - OPUS4-49829 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - X-ray generation N2 - This talk was recorded during the 2020 Better with Scattering workshop held at BAM in Berlin. This educational talk explains the various ways in which X-rays can be generated in the lab as well as at the synchrotron, with benefits and drawbacks for all. T2 - Better with Scattering workshop 2020 CY - BAM, Berlin, Germany DA - 16.03.2020 KW - Small angle scattering KW - X-ray instrumentation KW - X-ray generation PY - 2020 UR - https://www.youtube.com/watch?v=Hze3PvcK7es AN - OPUS4-51016 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - Neue ICP-MS basierte Methoden zur Analyse von Nano- und Mikropartikeln in der Umwelt N2 - In den vergangen Jahren hat das Umweltbewusstsein in der Bevölkerung stark zugenommen und somit auch das Interesse an der Vermeidung von anthropogenen (Schad-)Stoffen in der Umwelt. Eine (neue) Substanzklasse, deren Umweltauswirkungen noch nicht vollständig untersucht sind und die in den vergangenen Jahren immer mehr an Bedeutung gewonnen hat, sind (metallbasierte) Nanomaterialien. Im Gegensatz zu bspw. Elementspezies weisen Nanomaterialien eine Vielzahl von Eigenschaften auf und lassen sich nicht über nur ein Merkmal beschreiben - dies stellt eine große analytische Herausforderung dar. Hier haben sich vor allem die Feld-Fluss-Fraktionierung (AF4) und die single-particle-ICP-MS als leistungsstarke analytische Methoden herausgestellt. In (aquatischen) Umweltmatrizes (z.B. Oberflächengewässern) liegen neben artifiziellen auch natürliche Partikel vor, was eine weitere große Herausforderung für den Nachweis von Nanomaterialien darstellt. Neben dem Nachweis von anthropogenen Stoffen in der Umwelt ist zudem deren ökotoxikologische Bewertung wichtig. In der aquatischen Ökotoxikologie werden hierzu Testorganismen mit den jeweiligen Substanzen über die Wasserphase exponiert. Effektkonzentrationen (EC50) werden dabei auf Basis der Konzentrationen in der Wasserphase abgeleitet - tatsächlich bioakkumulierte Mengen werden hierbei jedoch meist nicht ermittelt; eine weitere große Herausforderung besteht zudem in der Bewertung von Mischungstoxizitäten. Gängige Testorganismen sind u.a. Kieselalgen (Diatomeen). Diatomeen stehen am Anfang der Nahrungskette - toxikologisch relevante Metalle/Nanomaterialien können sich hierüber im Nahrungsnetz der Oberflächengewässer anreichern und ggf. nachhaltig auswirken. Im ersten Teil des Vortrages werden zunächst neue elementanalytische Methoden zum Nachweis von metallbasierten Nanopartikeln in Umweltmatrizes auf Basis der AF4/ICP-SFMS sowie stabilen Isotopenlabeln am Beispiel von Eisennanopartikeln vorgestellt. Im zweiten Teil wird eine neue elementanalytische Methode als komplementäre Technik zur ökotoxikologischen Bewertung von (Schad-)Stoffen vorgestellt. Die neue Methode basiert auf der on-line Kopplung von HPLC mit der single-cell-ICP-(ToF)-MS (sc-ICP-(ToF)-MS) [1, 3-5]. Hierüber konnten wir erfolgreich die automatisierte Multielementanalytik einzelner Diatomeen realisieren und zur Analyse von mit Metallen inkubierten Diatomeen (cyclotella meneghiniana) einsetzen. Wir konnten zeigen, dass die sc-ICP-ToF-MS zukünftig eine leistungsstarke, komplementäre Technik in der aquatischen Ökotoxikologie zum z.B. Test von Metallen und Nanomaterialien darstellt. T2 - GDCh Wissenschaftsforum Chemie CY - Aachen, Germany DA - 17.09.2019 KW - ICP-MS KW - Nanomaterialien KW - Single particle-ICP-ToF-MS KW - Single cell-ICP-ToF-MS PY - 2019 AN - OPUS4-49743 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meermann, Björn T1 - New icp-(Tof)-MS based Methods for Material- and Environmental Analysis N2 - Entwicklung von ICP-(ToF)-MS basierten Methoden für die Spezies und Einzelorganismen und -Partikelanalytik an der Schnittstelle Material-Umwelt T2 - Analytisch Chemisches Kolloquium Uni Duisburg-Essen CY - Essen, Germany DA - 04.11.2019 KW - CE-ICP-MS KW - single cell-ICP-ToF-MS KW - single particle-ICP-ToF-MS KW - Speciation analysis PY - 2019 AN - OPUS4-49747 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Untersuchung lokaler Korrosionsprozesse mittels kombinierter elektrochemischer und mikroskopischer Methoden N2 - Forschungsarbeiten des Fachbereichs auf dem Gebiet "Methoden für die Analyse der lokalen Korrosionsprozesse". T2 - ProcessNet-Arbeitsausschuss Elektrochemische Prozesse (AA ECP) CY - DECHEMA, Frankfurt am Main, Germany DA - 21.01.2019 KW - Scanning electrochemical microscope (SECM) KW - Atomic Force Microscopy (AFM) KW - Multielectrode based sensors PY - 2019 AN - OPUS4-49751 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - A brief history of scattering N2 - Recorded on the first day of the Better with Scattering workshop. In this video, I explore some of the highlights of the development of small-angle X-ray scattering over its long history. I discuss developments on the technical side, analytical methods, detectors, data quality and data management. T2 - Better with Scattering workshop 2020 CY - BAM, Berlin, Germany DA - 16.03.2020 KW - Small angle scattering KW - History PY - 2020 UR - https://www.youtube.com/watch?v=mFH6P4tZbyM AN - OPUS4-51015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stawski, Tomasz T1 - Scattering is a powerful tool to follow nucleation and growth of minerals from solutions N2 - In recent years, we have come to appreciate the astounding intricacy of the processes leading to the formation of minerals from ions in aqueous solutions. The original, and rather naive, ‘textbook’ image of these phenomena, stemming from the adaptation of classical nucleation and growth theories, has increased in complexity due to the discovery of a variety of precursor and intermediate species. These include solute clusters (e.g. prenucleation clusters, PNCs), liquid(-like) phases, as well as amorphous and nanocrystalline solids etc.. Does it, however, mean that all the minerals grow through intermediate phases, following a non-classical pathway? In general, the precursor or intermediate species constitute different, often short-lived, points along the pathway from dissolved ions to the final solids (typically crystals in this context). In this regard synchrotron-based scattering (SAXS/WAXS/total scattering) appears to be the perfect tool to follow in situ and in a time-resolved manner the crystallization pathway because of the temporal and spatial length scales that can be directly accessed with these techniques. In this presentation we show how we used scattering to probe the crystallisation mechanisms of calcium sulfate, This system contains minerals that are widespread in diverse natural environments, but they are also important in various industrial settings. Our data demonstrate that calcium sulfate precipitation involves formation and aggregation of sub-3 nm anisotropic primary species. The actual crystallisation and formation of imperfect single crystals of calcium sulfate phases, takes place from the inside of the in itial aggregates. Hence, calcium sulfate follows a non-classical pathway. T2 - X-ray Powder Diffraction at DESY - new opportunities for research and industry CY - Online meeting DA - 22.06.2020 KW - Nucleation KW - Calcium sulfate KW - Diffraction KW - Scattering KW - Synchrotron KW - SAXS/WAXS PY - 2020 AN - OPUS4-50943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Simulaciónes de Montecarlo II: El scoring en las superficies N2 - En esta presentación desarrollaremos un ejemplo de aplicación para la dispersión de partículas utilizando el método de simulación de Monte- Carlo. Se discutirá el caso de las nanopartículas de oro radiactivo y como obtener informacions sobre diferente tipos de particulas pasando las superfices. T2 - Seminar of the bioanalysis group CY - Universidad Nacional de Colombia, Medellin, Colombia DA - 16.03.2020 KW - Geant4 KW - Geant4-DNA KW - MCS KW - Particle scattering simulation KW - Particle scattering simulations KW - Radioactive decay KW - Radioactive nanoparticle KW - Desintegracion radioactiva KW - Geant4 KW - Monte-Carlo simulations KW - Método de Montecarlo KW - Topas KW - nanoparticula PY - 2020 AN - OPUS4-50564 LA - spa AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bennet, Francesca T1 - Microprinting and SEM analysis for quantitative evaluation of nanoparticles in solution N2 - Nanoparticle suspensions were microprinted onto TEM grids for subsequent analysis by SEM/TSEM and evaluation of particle numbers using Image J software. Various nanoparticle types, concentrations and printing conditions (temperature, rel. humidity) were evaluated in order to determine the optimal conditions for producing a uniform distribution of particles on the substrate and eliminating the coffee ring effect. T2 - H2020 ACEnano Project Meeting CY - Amsterdam, Netherlands DA - 04.03.2020 KW - Nanoparticle KW - Imaging KW - Microprinting KW - Homogeneous deposition PY - 2020 AN - OPUS4-50584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Setup of a Particle Scattering Simulation environment N2 - A step by step introduction to the setup of a particle scattering simulation is given. Followed by an installation session. T2 - Seminar of the bioanalysis group CY - Universidad Nacional de Colombia, Medellin, Columbia DA - 12.02.2020 KW - Geant4 KW - Geant4-DNA KW - MCS KW - Monte-Carlo simulations KW - Particle scattering simulations KW - Scattering KW - Simulations KW - Debian KW - Linux KW - Topas KW - C++ KW - Topas-nbio KW - Git KW - Cmake PY - 2020 AN - OPUS4-50366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Basics and applications of good SAXS: Quantifying the fine structure of lots of materials N2 - In contrast to the crisp, clear images you can get from electron microscopy, small-angle X-ray scattering (SAXS) patterns are rather featureless. These patterns, however, contain averaged structural information of all of the finest material structures that were illuminated by the X-ray beam. With careful and precise investigation, and supplementary information from complementary techniques, this bulk material structure can be quantified to reveal structural information spanning four or even five decades in size. Additionally, while the data correction and analysis is complex, sample preparation is very straightforward, also allowing for in-situ and operando measurements to be performed without breaking a sweat. In the right hands, then, this technique can be the most powerful tool in your analytical arsenal. T2 - OpTecBB webinar within the scope of the focus area Optical Analytics CY - Online meeting DA - 27.05.2020 KW - Small-angle scattering KW - Introduction KW - Application KW - Saxs KW - Nanomaterials KW - Nanostructure PY - 2020 UR - https://www.youtube.com/watch?v=mXkYL3dSsTY UR - https://optecbb.de/veranstaltungen/veranstaltung/webinar-basics-and-applications-of-good-saxs-1238/ AN - OPUS4-50879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - View into the Depths of Copolymer Microstructure N2 - For different kinds of polymers it will be shown how it could be realized to obtain information on small, sometimes isomeric topological heterogeneities by coupling UPLC / ESI-TOF-MS and LC /MALDI-TOF-MS. T2 - DSM, Fall Meeting CY - Breda, The Netherlands DA - 07.11.2019 KW - Microstructure KW - LC-MS KW - Copolymer PY - 2019 AN - OPUS4-49587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Ejemplos de simulaciónes de Montecarlo La desintegración radioactiva N2 - A walkthrough how to setup radioactive sources in monte-carlo particle scattering simulations and perform different types of scorings. N2 - En esta presentación desarrollaremos un ejemplo de aplicación para la dispersión de partículas utilizando el método de simulación de Monte- Carlo. Se discutirá el caso de las nanopartículas de oro radiactivo y los diferentes tipos del scoring. T2 - Seminar of the bioanalysis group CY - Universidad Nacional de Colombia, Medellin, Columbia DA - 27.02.2020 KW - MCS KW - Geant4-DNA KW - Geant4 KW - Radioactive nanoparticle KW - Radioactive decay KW - Particle scattering simulations KW - Particle scattering simulation KW - Topas KW - Monte-Carlo simulations KW - Desintegracion radioactiva KW - Método de Montecarlo KW - Geant4 KW - nanoparticula PY - 2020 AN - OPUS4-50472 LA - spa AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Marcoulaki, E. A1 - van Duuren, B T1 - Testing and benchmarking nanosafety services N2 - One of the objectives of the EU Project EC4SafeNano (European Centre for Risk Management and Safe Innovation in Nanomaterials & Nanotechnologies) was to test and benchmark the services in order to check their relevance to address identified stakeholder needs, but also to evaluate the governance of the structure delivering the proposed services. The aim is to demonstrate the technical relevance of the services and the overall open structure organisation, including governance rules and operating procedures, by answering relevant identified questions (case studies) selected by a panel of stakeholders. Therefore, a significant part of the project will be devoted to this demonstration of the operational and functional basis of the organized network. T2 - Review Meeting EC4SafeNano CY - Brussels, Belgium DA - 16.01.2020 KW - Nanosafety KW - EC4SafeNano KW - Nanosafety services KW - EU KW - Case studies PY - 2020 AN - OPUS4-50273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - In situ imaging of corrosion processes N2 - The presentation summarizes our recent results on the coupled electrochemical methods for high resolution corrosion studies. The combination of Scanning Electrochemical Microscopy (SECM) and multielectrode (MMA) based real-time corrosion monitoring was presented as a new method for achieving high time resolution in local electrochemical analysis. Correlative imaging by means of Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM) was demonstrated as a tool for the investigation of local corrosion processes initiated by the intermetallic particles (IMPs) on AA2024-T3 aluminium alloy. T2 - BAM-IfW Workshop CY - Dresden, Germany DA - 28.03.2019 KW - MIC KW - Atomic Force Microscopy (AFM) KW - Corrosion monitoring KW - Corrosion PY - 2019 AN - OPUS4-50291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Application of atomic force microscopy (AFM) for in situ corrosion studies of thin film covered AA2024 T3 aluminium alloy surface N2 - The performance of functional coatings and adhesively joined hybrid components relies strongly on the stability of the polymer-metal interface. With the increasing utilization of multi-material structures in the automotive and aerospace industry, it is of great scientific and technical interest to understand the processes leading to interface degradation and to develop novel strategies to increase corrosion and delamination resistance. The aim of this project is to develop thin epoxy-based films and their carbon nanofiller loaded composites on aluminium alloy AA2024-T3 as a model system and to investigate their interfacial stability under corrosive and coupled corrosive-mechanical load. Spin coating was used for the layer-by-layer deposition of poly[(o-cresyl glycidyl ether)-co-formaldehyde] and poly-(ethylenimine) bi-layers. Atomic force microscopy (AFM) results indicate a very homogeneous and dense film with low surface roughness. Carbon nanofillers were introduced either by mixing into the coating components or in between individual layers to control the separation between the carbon nanofillers and alloy surface. The film chemistry and barrier properties were characterized by means of spectroscopic and electrochemical methods, respectively. The degradation and delamination behavior of the epoxy-based films was characterized by means of in situ AFM corrosion experiments. The quantitative imaging (QI) mode allowed the observation of hydrogen-generation induced blister formation during exposure to corrosive electrolyte and how the local corrosion processes evolved with exposure time. Complementary energy dispersive X-ray spectroscopy (EDX) analysis was performed to correlate the corrosion behavior with the different intermetallic particle chemistries and distributions. The presentation will summarize our results on the effect of interface chemistry and carbon nanofiller – alloy separation on the initiation of local corrosion processes on thin film covered AA2024-T3 aluminium alloys. T2 - EuroCorr2019 CY - Sevilla, Spain DA - 09.09.2019 KW - Corrosion KW - Atomic Force Microscopy (AFM) PY - 2019 AN - OPUS4-50293 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Özcan Sandikcioglu, Özlem T1 - Coupled electrochemical, microscopic and spectroscopic techniques for the analysis of local corrosion and mic processes N2 - Summary of the research topics of the division 6.2 and recent results T2 - HZDR-IRE Institutscolloquium CY - Dresden, Germany DA - 24.09.2019 KW - MIC KW - Localised corrosion KW - Corrosion monitoring KW - Biofilmbildung KW - Atomic Force Microscopy (AFM) PY - 2019 AN - OPUS4-50295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian T1 - Zerstörungsfreie Charakterisierung additiv gefertigter Kunststoffbauteile und ihres Alterungsverhaltens sowie zerstörende Prüfungen N2 - Es wurden Prüfkörper aus additiver Fertigung mittels Laser Sinter Verfahren (Polyamid 12, PA 12) und Fused Layer Modeling (Acrylnitril-Butadien-Styrol, ABS) sowie Prüfkörper aus dem Kunststoff-Spritzguss Verfahren (PA 12 und ABS) über 2000 Stunden künstlich bewittert. Vor, während und nach der Bewitterung erfolgte eine zerstörungsfreie Prüfung mittels Thermografie, optischer Mikroskopie und spektralen Methoden (UV/VIS-Spektroskopie und spektrale Reflexion), um den Alterungsfortschritt zu untersuchen und Schäden durch die künstliche Bewitterung sowie eingedruckte Defekte zu identifizieren und zu detektieren. Zusätzlich wurden zerstörende Zugprüfungen vorgenommen, welche mit einer IR-Kamera verfolgt wurden. Auf diese Weise konnten lokale Temperaturänderungen, hervorgerufen durch elastische sowie plastische Verformungen, zeitaufgelöst erfasst und ausgewertet werden. T2 - Sitzung des DGM Fachausschusses Polymerwerkstoffe CY - Würzburg, Germany DA - 14.11.2019 KW - Additive Fertigung KW - Thermografie KW - Kunststoffe KW - Zugprüfungen KW - Künstliche Bewitterung PY - 2019 AN - OPUS4-49820 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Challenges in Traceable Size Measurement of Non-Spherical, Non-Monodisperse Nanoparticles - nPSize N2 - Size measurement of nanoparticles (NP) becomes a challenging analytical problem when non-spherical shapes must be traceably measured. However, most industrial NPs have irregular shapes and broad size distribution making it often more complex to follow European regulatory to identify a material as a nanomaterial according to which accurate measurement of the smallest dimension and its size Distribution is necessary. The European research project nPSize - Improved traceability chain of nanoparticle size measurements aims to fill this gap by developing potential non-spherical reference nanoparticles, measurement procedures and physical modelling to improve the traceability chain, comparability and compatibility for NP size measurements between different methods. Therefore, new model NP with well-controlled shape has been synthesized and are supposed to be systematically characterized using the traceable methods scanning/transmission electron microscopy, atomic force microscopy and small angle X-ray scattering. Following NP candidates are under investigation with respect to their homogeneity and stability: (i) titania nanoplatelets (10-15 nm thickness x 50-100 nm lateral), (ii) titania bipyramides (~60 nm length x 40 nm width), (iii) titania acicular particles (100 nm length x 15-20 nm width; aspect ratio 5.5/6), (iv) gold nanorods (~10 nm width x 30 nm length), and (v) gold nanocubes (~55 nm x 55 nm x 55 nm). In addition, sample preparation procedures as well as measurement analysis procedures with evaluation of appropriate measurands and descriptors for each material class and method are being developed to support standardization. To underpin the traceability of the size measurement of nonspherical NP, physical modelling of the signals in e.g. electron microscopy techniques will be used and in combination, the implementation of machine learning is aimed to facilitate measurement Analysis procedures, especially regarding the accurate thresholding/segmentation of the NPs.zeige mehr T2 - Nanoparticle Reference Materials - Production and Cerification Training Course CY - London, UK DA - 10.12.2019 KW - Nanoparticles KW - Traceability KW - Particle size distribution KW - Electron microscopy KW - Reference materials KW - Non-spherical shape PY - 2019 AN - OPUS4-50040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hörenz, Christoph T1 - Preparation of Nanoparticulate Samples for Electron Microscopy N2 - This presentation addresses the importance of proper sample preparation to obtain suitable samples for electron microscopic measurements. The objective as well as the requirements are discussed. Further, different sample deposition methods for various types of nanoparticulate samples are shown. T2 - nPSize Web Conference CY - Online meeting DA - 23.07.2020 KW - Nanoparticles KW - Electron microscopy KW - Sample preparation KW - Particle size distribution KW - Particle number concentration PY - 2020 AN - OPUS4-51047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Feltin, N. T1 - Hybrid metrology for microscopy of nanoparticles N2 - This presentation is structured in two parts: i) Hybrid metrology by combining SEM with AFM (N. Feltin) and ii) hybridization and corelative microscopy by SEM, STEM-in-SEM, TEM, EDS, Auger Electron Microscopy, TKD and more (D. Hodoroaba). The first part is focused on the metrological part of the hybrid measurement SEM-AFM, the second part offers some further possibilities of correlative microscopy of nanoparticles based on practical examples. T2 - EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy" CY - Online meeting DA - 27.10.2020 KW - Nanoparticles KW - SEM KW - AFM KW - Metrology KW - Particle size distribution KW - Correlative imaging KW - STEM-in-SEM (TSEM) PY - 2020 AN - OPUS4-51476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize Improved Traceability Chain of Nanoparticle Size Measurement - Outcomes for the Strategy/Metrology Groups of ISO/TC 229 Nanotechnologies N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, VAMAS inter-laboratory comparisons) to be standardized and implemented in accredited analytical laboratories is discussed. Complementation and/or filling gaps of published and ongoing standardisation projects on size, shape and number concentration measurements under ISO/TC 229/JWG 2 are offered. T2 - Annual Meeting of ISO/TC 229 Nanotechnologies - Strategy and Metrology Groups CY - Online meeting DA - 06.11.2020 KW - Nanoparticles KW - Size KW - nPSize KW - Inter-laboratory comparison KW - ISO/TC 229 KW - VAMAS PY - 2020 AN - OPUS4-51544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - EMPIR nPSize - Improved Traceability Chain of Nanoparticle Size Measurement; nPSize offer after 2 Ys N2 - The main outcomes of the EMPIR project nPSize are presented and the suitability of the new capabilities (e.g. reference materials, measurement procedures, VAMAS inter-laboratory comparisons) to be standardized and implemented in accredited analytical laboratories is discussed. T2 - EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy" CY - Online meeting DA - 27.10.2020 KW - Nanoparticles KW - Size KW - Shape KW - Traceability KW - EMPIR KW - Reference materials KW - VAMAS PY - 2020 AN - OPUS4-51477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Design and Quantitative Characterization of Functional Molecular Chromophores and Nanomaterials with UV/vis/NIR/IR Emission and Traceable Optical Measurements N2 - Research of division Biophotonics at the Federal Institute for Materials Research and Testing (BAM) covers several topics including photophysics of molecular and nanocrystalline emitters, the development of signal enhancement, multiplexing, and barcoding strategies, surface group quantification, the rational design of different types of stimuli-responsive optical probes, and concepts and reference materials for the validation of optical-spectroscopic measurements. In the following representative examples for each of these topics are given. Also, current developments like single particle spectroscopy and flow cytometry with lifetime detection and newly certified fluorescence quantum yield standards are presented. T2 - Kolloquium BfR CY - Berlin, Germany DA - 12.10.2020 KW - Fluorescence KW - Quantitative spectroscopy KW - Single particle spectroscopy KW - Multiplexing KW - Reference materials KW - Optical probes KW - Sensor molecules KW - Assay KW - Dye KW - Quantum yield KW - Method development KW - surface group analysis KW - synthesis KW - fluorescence standards PY - 2020 AN - OPUS4-51449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Quantitative Microstructural Analaysis under VAMAS/TWA 37 N2 - The progress in activities on Microbeam Analysis under VAMAS/TWA 37 is reviewed. Particularly the liaison with the new projects within the ISO technical committee TC 202 is presented and discussed with respect to the possibility of identifying and launching related VAMAS projects. Need of more promotion for the engagement of more participants from industry and academia at national, European and international level is highlighted. Also, the competition with the other technical working areas (on 'nano' or materials-related) is critically discussed. T2 - Versailles Project on Advanced Materials and Standards (VAMAS) 45th Steering Committee Meeting CY - Online meeting DA - 30.09.2020 KW - VAMAS KW - Microbeam analysis KW - Inter-laboratory comparison KW - EBSD KW - FIB PY - 2020 UR - http://www.vamas.org/ AN - OPUS4-51360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska T1 - Wenn es im Holz knackt. Über die Herausforderung, kritische Versagensvorgänge in Holzstrukturen mittels Schallemissionsanalyse zu identifizieren N2 - Um die Versagensabläufe über die verschiedenen Skalen im Holzwerkstoff verfolgen zu können, werden Zugversuche an Lagenhölzern mittels Schallemissionsmessung überwacht. Synchron erfolgen In-situ-Messungen mit Digitaler Bildkorrelation bzw. Synchrotron-Mikro-Computertomographie. Die Kombination aller Ergebnisse wie auch die Anwendung der frequenzbasierten Mustererkennung und die Simulation ausgewählter Versuche zielen auf die Identifizierung zugrunde liegender Mechanismen hin. Abschließend werden Ansätze für ein Monitoring von Holzstrukturen diskutiert. T2 - 419. Sitzung AK Berlin der DGZFP CY - Online meeting DA - 15.09.2020 KW - Acoustic Emission (AE) KW - Holzwerkstoffe KW - Mustererkennung KW - Monitoring Konzept PY - 2020 AN - OPUS4-51361 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Everything and the kitchen sink: correcting X-ray data for everything N2 - Recorded at the Better with Scattering workshop 2020, this talk highlights the complete set of data correction steps that we do for the MAUS, and how they can be used elsewhere too. This links well with the talk in this series by Dr. Tim Snow, and also highlights the details of the background subtraction that needs to be done. T2 - Better with Scattering workshop 2020 CY - BAM, Berlin, Germany DA - 16.03.2020 KW - Small angle scattering KW - Data corrections PY - 2020 UR - https://www.youtube.com/watch?v=Hp4qziOxZFk AN - OPUS4-51018 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karapanagiotis, Christos A1 - Krebber, Katerina T1 - Machine Learning Approaches in Brillouin Distributed Fiber Optic Sensors N2 - This paper presents reported machine learning approaches in the field of Brillouin distributed fiber optic sensors (DFOSs). The increasing popularity of Brillouin DFOSs stems from their capability to continuously monitor temperature and strain along kilometer-long optical fibers, rendering them attractive for industrial applications, such as the structural health monitoring of large civil infrastructures and pipelines. In recent years, machine learning has been integrated into the Brillouin DFOS signal processing, resulting in fast and enhanced temperature, strain, and humidity measurements without increasing the system’s cost. Machine learning has also contributed to enhanced spatial resolution in Brillouin optical time domain analysis (BOTDA) systems and shorter measurement times in Brillouin optical frequency domain analysis (BOFDA) systems. This paper provides an overview of the applied machine learning methodologies in Brillouin DFOSs, as well as future perspectives in this area. KW - Distributed fiber optic sensors KW - BOTDA KW - BOFDA KW - Machine learning KW - Strain and temperature measurements KW - Artificial neural networks PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580145 DO - https://doi.org/10.3390/s23136187 VL - 23 IS - 13 SP - 1 EP - 26 PB - MDPI AN - OPUS4-58014 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Terzioglu, T. A1 - Karthik, M. A1 - Hurlebaus, S. A1 - Hueste, M. A1 - Maack, Stefan A1 - Wöstmann, Jens A1 - Wiggenhauser, Herbert A1 - Krause, M. A1 - Miller, P. A1 - Olson, L. T1 - Nondestructive evaluation of grout defects in internal tendons of posttensioned girders N2 - Post-tensioning systems provide safe and efficient construction solutions for long span bridges. Despite the improved grouting practices over the past decade, existing post-tensioning systems may have significant amount of grout defects, which could lead to corrosion of the strands. Condition assessment of post-tensioning systems is necessary to allow bridge owners to take timely, proactive actions to mitigate or prevent further Deterioration and unanticipated tendon failures. A detailed experimental study conducted to assess the performance of nondestructive evaluation techniques in detecting grout defects within internal tendons is presented herein. Nondestructive evaluation techniques that include Ground Penetrating Radar, Impact Echo, Ultrasonic Tomography, and Ultrasonic Echo are evaluated in terms of detecting the location and severity of fabricated grout defects in a full-scale post-tensioned U-girder mock-up specimen. While Ground Penetrating Radar can identify the location and profile of the internal tendons, particularly metal ducts due to strong reflections, this method did not provide any information about the defect conditions within the tendon. Both Impact Echo and Ultrasonic Echo techniques are effective in identifying the Location of grout defects, but could not differentiate between water, void, or compromised grout conditions. The study clearly demonstrates the need for NDE techniques that are applicable to anchorage regions, and that are capable of estimating the severity and nature of grout defects in internal tendons. KW - Zerstörungsfreie Prüfung KW - Nondestructive testing KW - Ground penetrating radar KW - Impact Echo KW - Ultrasonic tomography KW - Ultrasonic echo KW - Bridge inspection PY - 2018 UR - https://www.sciencedirect.com/science/article/pii/S0963869517305996?via%3Dihub DO - https://doi.org/10.1016/j.ndteint.2018.05.013 SN - 0963-8695 VL - 99 SP - 23 EP - 35 PB - Elsevier Ltd. AN - OPUS4-45218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karapanagiotis, Christos A1 - Hicke, Konstantin A1 - Krebber, Katerina T1 - Machine learning assisted BOFDA for simultaneous temperature and strain sensing in a standard optical fiber N2 - We report, to our knowledge for the first time on simultaneous distributed temperature and strain sensing in a standard telecom optical fiber using a machine learning assisted Brillouin frequency domain analysis (BOFDA) system. The well-known temperature and strain cross-sensitivity problem is addressed by developing a BOFDA system with a high signal-to-noise ratio and applying machine learning. The spectrum consists of four highly resolved peaks, whose Brillouin frequency shifts are extracted and serve as features for the machine learning algorithms. The spectra result from a 450-m standard SMF-28 optical fiber, and particularly from a segment of 30 m. This fiber segment is coiled around a stretcher and placed in a climate chamber. The applied temperature and strain values range from 20 °C to 40 °C and from 0 µɛ to 1380 µɛ, respectively. The total measurement time to achieve a high SNR and resolve four peaks with a spatial resolution of 6 m is 16 min. To discriminate temperature and strain effects, simple frequentist and more sophisticated Bayesian-based algorithms are employed with the powerful Gaussian process regression (GPR) delivering the best performance in terms of temperature and strain errors, which are found to be 2 °C and 45 µɛ, respectively. These errors are calculated using leave-one-out cross-validation, so that an unbiased estimation of the sensor’s performance is provided. KW - Machine learning KW - Brillouin distributed fiber optic sensors KW - Temperature and strain sensing KW - BOFDA PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569155 DO - https://doi.org/10.1364/OE.480224 SN - 1094-4087 VL - 31 IS - 3 SP - 5027 EP - 5041 PB - OPTICA AN - OPUS4-56915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karapanagiotis, Christos A1 - Wosniok, Aleksander A1 - Hicke, Konstantin A1 - Krebber, Katerina T1 - Time-Efficient Convolutional Neural Network-Assisted Brillouin Optical Frequency Domain Analysis N2 - To our knowledge, this is the first report on a machine-learning-assisted Brillouin optical frequency domain analysis (BOFDA) for time-efficient temperature measurements. We propose a convolutional neural network (CNN)-based signal post-processing method that, compared to the conventional Lorentzian curve fitting approach, facilitates temperature extraction. Due to its robustness against noise, it can enhance the performance of the system. The CNN-assisted BOFDA is expected to shorten the measurement time by more than nine times and open the way for applications, where faster monitoring is essential. KW - Fiber-optic sensors KW - Machine learning KW - Temperature and strain monitoring KW - Brillouin distributed sensing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524631 DO - https://doi.org/10.3390/s21082724 VL - 21 IS - 8 SP - 2724 PB - MDPI AN - OPUS4-52463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karapanagiotis, Christos A1 - Hicke, Konstantin A1 - Wosniok, Aleksander A1 - Krebber, Katerina T1 - Distributed humidity fiber-optic sensor based on BOFDA using a simple machine learning approach N2 - We report, to our knowledge for the first time, on distributed relative humidity sensing in silica polyimide-coated optical fibers using Brillouin optical frequency domain analysis (BOFDA). Linear regression, which is a simple and well-interpretable algorithm in machine learning and statistics, is utilized. The algorithm is trained using as features the Brillouin frequency shifts and linewidths of the fiber’s multipeak Brillouin spectrum. To assess and improve the effectiveness of the regression algorithm, we make use of machine learning concepts to estimate the model’s uncertainties and select the features that contribute most to the model’s performance. In addition to relative humidity, the model is also able to simultaneously provide distributed temperature information addressing the well-known cross-sensitivity effects. KW - Fiber optics sensors KW - Machine learning KW - Brillouin distributed sensing KW - Humidity sensing KW - Simultaneous temperature and humidity sensing PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546294 DO - https://doi.org/10.1364/OE.453906 VL - 30 IS - 8 SP - 12484 EP - 12494 PB - OPTICA AN - OPUS4-54629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy T1 - Ermittlung des Flüssigwasseranteils in Sandsteinen mittels NMR und relativer Luftfeuchte N2 - Die zerstörungsfreie Erfassung der Feuchteverteilung im Porensystem eines Baustoffes ist in der zerstörungsfreien Prüfung (ZfP) von großer Bedeutung, da Feuchte (i. d. R. in Form von Flüssigwasser) ein hohes Schadenspotential für die Materialien und Konstruktionen aufweist. Für die Lokalisierung möglicher Schad- oder Risikostellen und die Einleitung von Präventionsmaßnahmen sind vor allem Kenntnisse über das Porengefüge und Feuchtetransportmechanismen im Baustoff erforderlich. Derzeit besteht allerdings eine wesentliche Problematik in der Erfassung und Quantifizierung von Feuchteverteilungen bei Teilsättigung. In der ZfP stellt die Nuklear Magnetische Resonanz (NMR) ein geeignetes Verfahren zur Feuchtedetektion dar. Mit diesem Verfahren lassen sich prinzipiell Relaxationszeiten von Wasserstoffprotonen in Abhängigkeit von ihrer Bindungsart und der Porenumgebung messen. In Baustoffen dominieren jedoch die Signalanteile des freien (schadensträchtigen) Wassers zumeist stark. Und eine derzeit noch ungeklärte Frage ist, ob bei Materialien mit sehr breiten Porengrößenverteilungen größere teilgesättigte von kleineren vollgesättigten Poren durch unterschiedliches Relaxationsverhalten unterschieden werden können. In dieser Arbeit wird die Eignung von NMR für die Ermittlung von Feuchteverteilungen in Naturstein sowohl bei Voll- als auch bei Teilsättigung untersucht. Die Bestimmung des Flüssigwasseranteils in teilgesättigten Poren soll dabei durch eine Korrelation von NMR und relativen Luftfeuchten erfolgen. Dazu werden 12 verschiedene Sandsteinproben, deren Poren(eingangs-)größenverteilungen mit der Quecksilberporosimetrie bereits ermittelt wurden, untersucht. Die Proben werden in einem Klimaschrank bei 23°C und relativen Luftfeuchten von 40 bis 90% schrittweise aufgesättigt. Nach Abschluss jedes Aufsättigungsschrittes werden mit der NMR-Relaxometrie die T2-Relaxationszeitenverteilungen bestimmt. Durch die Nutzung eines weiterentwickelten Ansatzes von Hillerborg lassen sich schließlich zu jeder Luftfeuchte die adsorbierte Wasserfilmdicke und somit der Porensättigungsgrad berechnen. Mithilfe dieser Zusatzinformation ist eine genauere Analyse der Relaxationszeitenverteilungen bei Teilsättigung möglich. Am Ende dieser Arbeit soll erstmals der Zusammenhang des Wassersignals und dem Porensystem eines Baustoffes mit multimodaler Porengrößenverteilung bei Teilsättigung aufgezeigt werden. T2 - 70. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Brunswick, Germany DA - 04.03.2019 KW - Relative Luftfeuchte KW - Sandstein KW - Nuklear magnetische Resonanz KW - Porengrößenverteilung PY - 2019 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-47513 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Franziska A1 - Scholz, G. A1 - Batzdorf, Lisa A1 - Wilke, Manuel A1 - Emmerling, Franziska T1 - Synthesis, structure determination, and formation of a theobromine: oxalic acid 2:1 cocrystal N2 - The structure and the formation pathway of a new theobromine : oxalic acid (2 : 1) cocrystal are presented. The cocrystal was synthesised mechanochemically and its structure was solved based on the powder X-ray data. The mechanochemical synthesis of this model compound was studied in situ using synchrotron XRD. Based on the XRD data details of the formation mechanism were obtained. The formation can be described as a self-accelerated ('liquid like') process from a highly activated species. KW - ssNMR spectroscopy KW - Synchrotron measurements KW - API molecule PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-331567 DO - https://doi.org/10.1039/c4ce02066a SN - 1466-8033 VL - 17 IS - 4 SP - 824 EP - 829 CY - London, UK AN - OPUS4-33156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krause, Christina A1 - Zorn, R. A1 - Frick, B. A1 - Schönhals, Andreas T1 - Quasi- and inelastic neutron scattering to investigate the molecular dynamics of discotic molecules in the bulk N2 - In- and quasielastic neutron scattering is employed to investigate both the vibrational density of states and the molecular dynamics of two homologous discotic liquid crystals (DLC) with different length of the alkyl side chain based on a triphenylene derivate. For both compounds characteristic low frequency excess contributions to the vibrational density of states are found. Therefore it is concluded that these liquid crystals show a glass-like behaviour. Elastic scans further show that in these materials a rich molecular dynamics takes place. T2 - QENS/WINS 2014 - 11th International Conference on Quasielastic Neutron Scattering and 6th International Workshop on Inelastic Neutron Spectrometers CY - Autrans, France DA - 2014-05-11 PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-325477 DO - https://doi.org/10.1051/epjconf/20158302017 SN - 2100-014X VL - 83 SP - 02017-1 EP - 02017-4 PB - EDP Sciences CY - Les Ulis AN - OPUS4-32547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ressnig, A. A1 - Corbiere, T. A1 - Lunkenbein, T. A1 - Braun, Ulrike A1 - Willinger, M. G. A1 - Antonietti, M. T1 - Decomposition synthesis of tuneable, macroporous carbon foams from crystalline precursors via in situ templating N2 - A flexible, sustainable, one-step thermal decomposition route for the synthesis of hierarchical, heteroatom doped carbon foams is presented. Task-specific semi-organic crystals combine functions for three different purposes: the carbon and heteroatom source, a foaming agent (CO2) and an in situ generable template (NaCl). Insights to the decomposition pathway were gained through FTIR/MS coupled TGA and an ultrafast out-of-furnace heating procedure and the products were analysed with (HR)SEM/TEM, EELS, FTIR, and N2 sorption. The resulting macroporous carbon foams are excellent supports for metallic nanoparticles due to their hierarchical structure, high surface area and tuneable heteroatom contents. This was demonstrated for catalytically active copper or the magnetic CoNi alloy for water purification. KW - macroporous carbon KW - thermal decomposition KW - synthesize heteroatom KW - in situ template (NaCl) PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-318641 DO - https://doi.org/10.1039/c4ta03646h SN - 2050-7496 SN - 2050-7488 VL - 2 IS - 42 SP - 18076 EP - 18081 PB - RSC CY - London [u.a.] AN - OPUS4-31864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wrobel, Norma A1 - Kolkoori, Sanjeevareddy A1 - Zscherpel, Uwe A1 - Ewert, Uwe T1 - Innovative X-ray backscatter technique for security applications: Detection of dangerous materials N2 - Radiological inspections, in general, are NDT&E methods to detect the bulk of explosives without invasion into the object of analysis. In contrast to personal luggage, cargo or structural components constitute a complexity that may significantly hamper the detection of a threat by conventional transmission radiography. A novel approach of interrogating a large object to a certain depth only with a single sided access will be presented. It consists of an X-ray backscatter camera with a special twisted slit collimator for imaging backscattered objects. The new X-ray backscatter camera is not only imaging the objects due to their densities but also by taking into account the influences of surrounding objects. Additionally, it does not only image illuminated features but also depicts shadows from absorbing materials. This is a unique characteristic of the developed X-ray backscatter camera. Experimental mock-ups are conducted imitating container with threats among a complex packing as they may be encountered in reality. At the end, the significant advantages of the presented X-ray backscatter camera in the context of aviation and port security will be discussed. T2 - ECNDT 2014 - 11th European conference on non-destructive testing CY - Prague, Czech Republic DA - 06.10.2014 KW - Radiography KW - X-ray backscatter imaging KW - Irradiation geometry KW - Detection of dangerous materials KW - Security applications PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-322429 UR - https://www.ndt.net/?id=16432 SN - 1435-4934 VL - 19 IS - 12 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-32242 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schick, D. A1 - Herzog, M. A1 - Bojahr, A. A1 - Leitenberger, W. A1 - Hertwig, Andreas A1 - Shayduk, R. A1 - Bargheer, M. T1 - Ultrafast lattice response of photoexcited thin films studied by X-ray diffraction N2 - Using ultrafast X-ray diffraction, we study the coherent picosecond lattice dynamics of photoexcited thin films in the two limiting cases, where the photoinduced stress profile decays on a length scale larger and smaller than the film thickness. We solve a unifying analytical model of the strain propagation for acoustic impedance-matched opaque films on a semi-infinite transparent substrate, showing that the lattice dynamics essentially depend on two parameters: One for the spatial profile and one for the amplitude of the strain. We illustrate the results by comparison with high-quality ultrafast X-ray diffraction data of SrRuO3 films on SrTiO3 substrates. KW - Festkörperphysik KW - Dünnschichttechnik KW - Ellipsometrie KW - Röntgenbeugung KW - Optische Konstanten PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-322471 DO - https://doi.org/10.1063/1.4901228 SN - 2329-7778 VL - 1 IS - 6 SP - 064501-1 - 064501-13 PB - AIP Publishing LLC CY - Melville, NY AN - OPUS4-32247 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolkoori, Sanjeevareddy A1 - Wrobel, Norma A1 - Zscherpel, Uwe A1 - Ewert, Uwe T1 - New X-ray backscatter imaging technique for nondestructive testing of aerospace components N2 - Critical parts in aircraft manufacturing such as stringers are very commonly used in modern aircraft structures to resist the compressive loads caused by the aerodynamic effects. They are generally made-up of thin aluminium (Al) metal sheets and are one of the key components in the aircraft wings. Any defects in the stringer leads to weakening of the stiffness of the whole wing structure and consequently, failures may occur. Hence, the structural integrity of the stringers should be evaluated using reliable non-destructive testing (NDT) methods. Due to the complex shaped structure of the stringer, the one-sided access NDT method such as X-ray backscatter technique is more preferable for the non-destructive imaging. In this paper, we present a new X-ray backscatter technique to image the internal sections of the stringer with only a single-sided access. The whole object was inspected by changing the viewing direction of the X-ray backscatter camera. For the first time, the X-ray backscatter measurements were conducted using high-energy (> 0.5MeV) X-rays and proved the applicability of the present technique to inspect thick carbon-fiber laminated components. In order to improve the inspection time and image quality of the backscatter image, we used high-resolution (180ìm) digital detector arrays (DDAs). At the end, important applications of the presented X-ray backscatter technique to the aerospace industry are discussed. T2 - ECNDT 2014 - 11th European conference on non-destructive testing CY - Prague, Czech Republic DA - 06.10.2014 KW - X-ray backscatter imaging KW - Twisted-slit collimator KW - NDT KW - Digital detector array (DDA) KW - Stringer KW - Aerospace applications PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-322376 UR - https://www.ndt.net/?id=16431 SN - 1435-4934 VL - 19 IS - 12 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-32237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolkoori, Sanjeevareddy A1 - Wrobel, Norma A1 - Deresch, Andreas A1 - Redmer, Bernhard A1 - Ewert, Uwe T1 - Dual high-energy X-ray digital radiography for material discrimination in cargo containers N2 - In this contribution, we present a dual high-energy X-ray imaging technique for cargo container inspection using the 'spectral high-energy X-ray attenuation method'. This method is based on attenuation of continuous highenergy spectra. The developed experimental technique consists of a betatron as high-energy (up to 7.5 MeV) X-ray source and a matrix detector with high spatial resolution (400 ìm) for digital X-ray imaging. In order to evaluate the material discrimination capability using dual high-energy X-ray imaging, a test specimen is proposed, comprising step wedges of different low and high atomic number (Z) materials. The selected X-ray spectra for the dual-energy experiments correspond to 3 MV and 7.5 MV acceleration potential of the betatron. We evaluated the ratio between low- and high-energy X-ray attenuation coefficients quantitatively based on simulated poly-energetic high-energy X-ray source spectra and the detector sensitivity using the 'analytical Radiographic Testing inspection simulation tool' (aRTist) developed at BAM. The simulated effective attenuation coefficients are compared with corresponding experimental results in order to establish a method for identification of low- and high-Z materials in the container. Finally, important applications of the proposed technique in the context of aviation security are discussed. T2 - ECNDT 2014 - 11th European conference on non-destructive testing CY - Prague, Czech Republic DA - 06.10.2014 KW - Digital radiography KW - NDT KW - High-energy X-ray imaging KW - Betatron KW - Digital detector array (DDA) KW - Container inspection KW - Material discrimination KW - Effective attenuation coefficient PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-322394 UR - https://www.ndt.net/?id=16430 SN - 1435-4934 VL - 19 IS - 12 SP - 1 EP - 10 PB - NDT.net CY - Kirchwald AN - OPUS4-32239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kreutzbruck, Marc A1 - Bauer, P. A1 - Caspers, F. A1 - Heck, S. A1 - Müller, F. A1 - Pohl, Rainer A1 - Scheuerlein, C. A1 - Sickert, Roland A1 - Maierhofer, Christiane A1 - Brackrock, Daniel T1 - Sensoren für Verbunddrähte aus Niob-Titan und Kupfer N2 - Der Large Hadron Collider (LHC) des europäischen Kernforschungszentrums CERN ist einer der weltweit größten und leistungsfähigsten Teilchenbeschleuniger. Um den Teilchenstrahl auf seiner Kreisbahn zu halten, werden mit Hilfe supraleitender Spulen sehr starke Magnetfelder erzeugt. Die hierzu benötigten hohen Ströme werden über Verbunddrähte aus Niob-Titan und Kupfer geleitet. Die Drähte werden u.a. durch Ultraschallschweißungen miteinander verbunden. Eine mangelhafte Verbindung kann zur Erwärmung der Kontaktstelle und in Folge davon zum Zusammenbruch der Supraleitung führen. Auf Anfrage des CERN wurden an der BAM Untersuchungen zur Prüfbarkeit solcher Verbindungen bei Umgebungstemperatur durchgeführt. Es gelang, für einen Verbindungstypen einen Wirbelstromsensor für eine manuelle Prüfung zu entwickeln. Ein Prototyp des Sensors befindet sich beim CERN in der praktischen Erprobung. Das Sensorprinzip sowie Prüfergebnisse aus Labor und Praxis werden vorgestellt. T2 - DGZfP-Jahrestagung 2014 CY - Potsdam, Germany DA - 26.05.2014 KW - Ultraschallprüfung mit Matrix-Sensoren KW - Aktive Thermografie KW - Gabelsensor PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-319785 SN - 978-3-940283-61-0 VL - 148 SP - 1 EP - 12 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-31978 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guo, Y. A1 - Lippitz, Andreas A1 - Saftien, P. A1 - Unger, Wolfgang A1 - Kemnitz, E. T1 - Tuning the surface properties of novel ternary iron(III) fluoride-based catalysts using the template effect of the matrix N2 - Sol–gel prepared ternary FeF3–MgF2 materials have become promising heterogeneous catalysts due to their porosity and surface Lewis/Brønsted acidity (bi-acidity). Despite the good catalytic performance, nanoscopic characterisations of this type of material are still missing and the key factors controlling the surface properties have not yet been identified, impeding both a better understanding and further development of ternary fluoride catalysts. In this study, we characterised the interaction between the bi-acidic component (FeF3) and the matrix (MgF2) on the nano-scale. For the first time, the formation pathway of FeF3–MgF2 was profiled and the template effect of MgF2 during the synthesis process was discovered. Based on these new insights two novel materials, FeF3–CaF2 and FeF3–SrF2, were established, revealing that with decreasing the atomic numbers (from Sr to Mg), the ternary fluorides exhibited increasing surface acidity and surface area but decreasing pore size. These systematic changes gave rise to a panel of catalysts with tuneable surface and bulk properties either by changing the matrix alkaline earth metal fluoride or by adjusting their ratios to Fe or both. The template effect of the alkaline earth metal fluoride matrix was identified as the most probable key factor determining the surface properties and further influencing the catalytic performance in ternary fluoride based catalysts, and paves the way to targeted design of next-generation catalysts with tunable properties. KW - Catalysis KW - Surface analysis KW - XPS PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-327410 DO - https://doi.org/10.1039/c4dt03229b SN - 1477-9226 SN - 1477-9234 SN - 1364-5447 VL - 44 IS - 11 SP - 5076 EP - 5085 PB - RSC CY - Cambridge AN - OPUS4-32741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhne, Christian A1 - Boehm, Rainer A1 - Prager, Jens T1 - Detektion der Einhüllenden in SAFT-Daten durch Anwendung multidimensionaler analytischer Signale mit single-orthant-Spektren N2 - Die Synthetic Aperture Focusing Technique (SAFT) ist ein Verfahren zur Verarbeitung von HF-Bildern, die an unterschiedlichen Prüfkopfpositionen aufgenommen wurden. Es wird in der zerstörungsfreien Werkstoffprüfung genutzt, um eine Abbildung von Materialfehlern innerhalb des Gebietes zu erstellen, auf das die Rekonstruktion angewandt wird. Die nach Abschluss der SAFT-Rekonstruktion zusammengestellten Informationen über Reflektoren liegen zunächst nach wie vor in Form von HF-Daten vor. Die Interpretierbarkeit der SAFT-Bilder ist im Allgemeinen davon abhängig, wie diese Daten vor der endgültigen Darstellung aufbereitet werden. Die Bildung der Amplitudeneinhüllenden aus dem zugehörigen analytischen Signal stellt eine Möglichkeit einer solchen Aufbereitung nach Anwendung des SAFT-Algorithmus dar. Sie ist jedoch nur im eindimensionalen Fall eindeutig definiert. In diesem Beitrag wird das Konzept der analytischen Signale mit single-orthant-Spektren aufgegriffen, um eine Detektion der Einhüllenden an mehrdimensionalen HF-Daten durchzuführen. Dabei wird über die Betragsquadrate aller möglichen nach dieser Definition zu bildenden analytischen Signale gemittelt. Es wird gezeigt, dass die Anwendung des beschriebenen Verfahrens einem Separationsansatz entspricht. Außerdem wird eine Möglichkeit aufgezeigt die Gültigkeit dieses Ansatzes anhand der totalen und partiellen Hilberttransformationen des Signals im konkreten Fall zu überprüfen. Die Ergebnisse dieser Methode zur Verbesserung von SAFT Bildern werden unter Verwendung synthetischer und experimenteller Daten an rekonstruierten Abbildungen verschiedener Reflektorarten beispielhaft dargestellt. T2 - DACH-Jahrestagung 2012 CY - Graz, Austria DA - 17.09.2012 KW - Ultrasonic testing (UT) KW - Synthetic aperture focusing technique (SAFT) KW - Analytic signal PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-327039 UR - https://www.ndt.net/search/docs.php3?id=14341 SN - 1435-4934 VL - 18 IS - 5 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-32703 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hemmann, Felix A1 - Jäger, Christian A1 - Kemnitz, E. T1 - Comparison of acidic site quantification methods for a series of nanoscopic aluminium hydroxide fluorides N2 - Quantitative determination of acidic surface sites is highly important for the characterization of solid acids because the activity of a catalyst is often related to the concentration of these sites. A recently developed method using 15N Nuclear Magnetic Resonance spectroscopy (NMR) for the quantification of acidic Lewis and Brønsted sites has been tested for a series of nanoscopic aluminum hydroxide fluorides. Comparison with other methods for the quantitative determination of acidic sites shows that this 15N NMR quantification method is a promising technique for the comprehensive investigation of acidic sites. Three different acidic sites, one Brønsted and two Lewis sites, can be distinguished by their 15N chemical shifts of pyridine and simultaneously quantified under conditions corresponding to catalytic reaction conditions. Determination of the individual concentrations of acidic sites allows further insight into the catalytic process. It was found that the concentration of Brønsted sites correlates with catalyzed conversion of citronellal to isopulegol in the investigated series of catalysts. Additionally, investigations indicate that one of the Lewis sites become blocked during the reaction of citronellal. KW - Solid acids KW - TOF KW - NH3-TPD KW - Progressive catalyst poisoning KW - FTIR KW - Quantitative NMR KW - Solid state NMR PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-323280 DO - https://doi.org/10.1039/c4ra09477h SN - 2046-2069 VL - 4 IS - 100 SP - 56900 EP - 56909 PB - RSC Publishing CY - London AN - OPUS4-32328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Buzanich, Günter A1 - Curado, Jessica A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Scharf, O. T1 - Slicing - a new method for non destructive 3D elemental sensitive characterization of materials N2 - Recent advances in synchrotron sources and detector technology have led to substantial improvements in spatial resolution and detection limits for X-ray fluorescence analysis (XRF). However, the non-destructive three-dimensional elemental sensitive characterization of samples remains a challenge. We demonstrate the use of the so-called 'Color X-ray Camera' (CXC) for 3D measurements for the first time. The excitation of the sample is realized with a thin sheet-beam. The stepwise movement of the sample allows getting the elemental distribution for each layer with one measurement. These layers can be combined to a full 3D dataset for each element afterwards. Since the information is collected layer by layer, there is no need to apply reconstruction techniques, which quite often are the reason for artifacts in the results achieved by computed tomography (CT). The field of applications is wide, as the 3D elemental distribution of a material contains clues to processes inside the samples from a variety of origins. The technique is of special interest and well suited for biological specimens, because their light matrix minimizes restricting absorption effects. Measurement examples of a hornet and the teeth of a Sorex araneus are shown. KW - SR-microXRF KW - 3D KW - CXC PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-324330 DO - https://doi.org/10.1039/c4ja00085d SN - 0267-9477 SN - 1364-5544 VL - 29 IS - 8 SP - 1339 EP - 1344 PB - Royal Society of Chemistry CY - London AN - OPUS4-32433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zscherpel, Uwe A1 - Schumacher, David A1 - Redmer, Bernhard A1 - Ewert, Uwe A1 - Ullberg, C. A1 - Weber, N. A1 - Pantsar, T. T1 - Digital radiology with photon counting detectors N2 - The progress in X-ray detector electronics (sensitivity and speed) allows meanwhile fast single photon detection by a matrix detector. Combined photon counting and energy discrimination is implemented in the electronic circuit of each detector pixel. The company XCounter developed detectors based on CdTe single crystals, which can be tiled to larger areas and have a pixel size of 100ìm. The largest area available in beginning of 2014 is 50x75 mm². These detectors have very promising properties, which make them very suitable for NDT applications: 1. A CdTe attenuation layer of 750 µm thickness allows efficient X-ray detection up to ca. 300 keV. In counting mode only photon noise is important; no other detector noise sources need to be considered. There is no Offset signal without radiation. 2. Each of the detector pixels has two energy thresholds. These can be used for dual energy imaging for materials separation. Also the suppression of scattered radiation by energy thresholding will improve the image contrast sensitivity. First experiments will be presented which demonstrate the advantages of this new detector technology over the conventional charge integrating detectors. A challenge is the development of a modified detector calibration procedure, which becomes critical at longer exposure times. T2 - ECNDT 2014 - 11th European conference on non-destructive testing CY - Prague, Czech Republic DA - 06.10.2014 KW - Materials characterization KW - Radiographic testing (RT) KW - Digital detector array KW - Photo counting KW - Image quality KW - Calibration KW - Dual-energy KW - Energy discrimination KW - Digital radiology KW - Detectors PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-323063 UR - https://www.ndt.net/?id=16709 SN - 1435-4934 N1 - Geburtsname von Schumacher, David: Walter, D. - Birth name of Schumacher, David: Walter, D. VL - 19 IS - 12 SP - 1 EP - 8 PB - NDT.net CY - Kirchwald AN - OPUS4-32306 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schumm, A. A1 - Martin, E. A1 - Beaumont, M. A1 - Ewert, Uwe A1 - Kolkoori, Sanjeevareddy A1 - Zscherpel, Uwe A1 - Wrobel, Norma A1 - Redmer, Bernhard T1 - A comparative study on the performance of digital detector systems for high energy applications N2 - For cast components reaching or exceeding total material thicknesses of 150mm, high energy sources such as linear accelerators or Betatrons are required in order to obtain reasonable exposure times. In this study, the performance of digital detector systems, involving imaging plates (IP) and digital detector arrays (DDA), was evaluated with respect to the testing class B requirements as formulated in the standard EN ISO 17636-2. As a reference, traditional radiographic film and a Cobalt-60 source was used. With film exposures, testing class B was achieved with Co-60 and Betatron (7.5 MV) at longer exposure times. The preliminary results show that the testing class B was not obtained with the examined digital detector arrays (DDA) and the high resolution imaging plates (IP) , even at 40, 60 and 80 minutes exposure time with a 7.5 MV Betatron. Class A was achieved using high resolution imaging plates with optimized metal filters between object and IPs and a high resolution DDA with intermediate Cu filters. Class A was also achieved applying a DDA with lower basic spatial resolution than required by Table B.13 of EN ISO 17636-2, but using the compensation principle as described in this standard. The next generation of digital detector arrays might potentially be able to obtain class B performance with the expected spatial resolution and sensitivity improvements. T2 - ECNDT 2014 - 11th European conference on non-destructive testing CY - Prague, Czech Republic DA - 06.10.2014 KW - Radiography KW - Image quality KW - Betatron KW - Digital detector array (DDA) KW - Casting KW - Standards KW - High energy radiography KW - Comparison of detectors KW - Steel weldment PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-323075 UR - https://www.ndt.net/?id=16394 SN - 1435-4934 VL - 19 IS - 12 SP - 1 EP - 6 PB - NDT.net CY - Kirchwald AN - OPUS4-32307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ewert, Uwe A1 - Zscherpel, Uwe T1 - Minimum requirements for digital radiography equipment and measurement procedures by different industries and standard organizations N2 - The digital photography has almost completely substituted the film photography. The film replacement is also fast progressing in medical X-ray radiography. This process is slower in NDT and especially in Europe. Reasons for the hesitating change to digital radiography (RT-D) in NDT are the necessary time for adoption of standards and the conservative request for film RT by auditors and NDT managers for applications in large plants and at construction areas. The fast serial inspection for small castings is already almost completely dominated by RT-D due to the cost effective short exposure and interpretation times. Standards were developed in parallel at CEN, ISO, ASTM and ASME. Unfortunately, the standard practices are different and the requirements on image quality and useable hardware are different too. The first standard series on Computed Radiography were developed and published by CEN and ASTM in 2005. Harmonized classification and qualification standards are available but the published practices are different. ASTM has developed the first standards for application of Digital Detector Arrays (DDA) in 2010. The first digital RT ISO standard practice is ISO 17636-2 (2013), which describes the practice for application of DDAs and Imaging Plates for weld inspection. At the first time this standard provides requirements for the selection of suitable hardware. Minimum image quality requirements are specified in analogy to film radiography and 3 Compensation Principles are defined to enable the application of a wider range of digital detectors. A comparison of the different international digital RT standards is given and first experiences with ISO 17636-2 are discussed. New standards on RT wall thickness and corrosion measurements (EN 16407, film and digital) have been developed recently. T2 - ECNDT 2014 - 11th European conference on non-destructive testing CY - Prague, Czech Republic DA - 06.10.2014 KW - NDT KW - X-Ray KW - Digital detectors KW - Standards KW - Radiographic procedures KW - Unsharpness KW - Basic spatial resolution KW - Requirements KW - Digital industrial radiology PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-323081 UR - https://www.ndt.net/?id=16708 SN - 1435-4934 VL - 19 IS - 12 SP - 1 EP - 18 PB - NDT.net CY - Kirchwald AN - OPUS4-32308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinrich, Thomas A1 - Traulsen, Christoph Hans-Henning A1 - Darlatt, Erik A1 - Richter, S. A1 - Poppenberg, J. A1 - Traulsen, N.L. A1 - Linder, I. A1 - Lippitz, Andreas A1 - Dietrich, Paul A1 - Dib, B. A1 - Unger, Wolfgang A1 - Schalley, C.A. T1 - The versatility of 'Click' reactions at surfaces: Molecular recognition at interfaces N2 - In order to investigate molecular recognition on surfaces, an azide-functionalized monolayer was deposited on gold. The monolayer was characterized by X-ray photoelectron spectroscopy (XPS) and angle-resolved near-edge X-ray absorption fine structure (NEXAFS) experiments and the decomposition of the azide upon irradiation with X-ray beams was investigated. Subsequently, various alkyne-functionalized host and guest molecules were attached to the azide by 1,3-dipolar cycloaddition. These modified surfaces and their host–guest chemistry were analysed by XPS and angle-resolved NEXAFS. The reversibility of guest binding was shown for one example as a proof of principle. KW - 'Click' reaction KW - Azide-terminated surfaces KW - SAMs KW - Host guest molecules KW - Molecular recognition at interfaces PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-306463 DO - https://doi.org/10.1039/C4RA01730G SN - 2046-2069 VL - 4 IS - 34 SP - 17694 EP - 17702 PB - RSC Publishing CY - London AN - OPUS4-30646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ehlert, Christopher A1 - Unger, Wolfgang A1 - Saalfrank, P. T1 - C K-edge NEXAFS spectra of graphene with physical and chemical defects: a study based on density functional theory N2 - Recently, C K-edge Near Edge X-ray Absorption Fine Structure (NEXAFS) spectra of graphite (HOPG) surfaces have been measured for the pristine material, and for HOPG treated with either bromine or krypton plasmas (Lippitz et al., Surf. Sci., 2013, 611, L1). Changes of the NEXAFS spectra characteristic for physical (krypton) and/or chemical/physical modifications of the surface (bromine) upon plasma treatment were observed. Their molecular origin, however, remained elusive. In this work we study by density functional theory, the effects of selected point and line defects as well as chemical modifications on NEXAFS carbon K-edge spectra of single graphene layers. For Br-treated surfaces, also Br 3d X-ray Photoelectron Spectra (XPS) are simulated by a cluster approach, to identify possible chemical modifications. We observe that some of the defects related to plasma treatment lead to characteristic changes of NEXAFS spectra, similar to those in experiment. Theory provides possible microscopic origins for these changes. KW - Graphene KW - NEXAFS KW - Spectrum simulation KW - Density functional theory PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-309658 DO - https://doi.org/10.1039/c4cp01106f SN - 1463-9076 SN - 1463-9084 VL - 16 IS - 27 SP - 14083 EP - 14095 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-30965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg A1 - von der Ehe, Kerstin A1 - Jaunich, Matthias A1 - Schade, U. A1 - Aziz, E. F. A1 - Wolff, Dietmar T1 - Fourier-spektroskopische Untersuchungen im mittleren- und fernen Infrarotbereich an Co-60 bestrahlten und thermisch belasteten ultrahochmolekularen Polyethylen-Proben N2 - Fourier-Spektroskopische Untersuchungen von hochmolekularem Polyethylen (HMW-PE) und ultrahochmolekularem Polyethylen (UHMW-PE) im Mittleren - und Fernen Infrarotbereich können Veränderungen der molekularen Strukturen nachweisen, die durch Co60 γ-Strahlung und Rekristallisationsprozesse initiiert werden. UHMW-PE und HMW-PE sind im gewählten IR-Bereich unterscheidbar. Die integrale Absorption der B1u – Gitterschwingungen im Fernen Infrarotbereich (THz-Bereich) ermöglichen die quantitative Beschreibung des Kristallinitätsgrades und dessen Abbau. Die Bildung ungesättigter Vinylengruppen und der Abbau ungesättigter Methylengruppen können im Mittleren Infrarotbereich nachgewiesen werden. T2 - DGZfP-Jahrestagung 2014 CY - Potsdam, Germany DA - 26.05.2014 KW - Infrared and far-infrared spectroscopy KW - Polyethylene KW - Co-60 irradiation PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-313317 SN - 978-3-940283-61-0 VL - 148 SP - 1 EP - 7 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-31331 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Franziska A1 - Scholz, G. A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Evaluation of the formation pathways of cocrystal polymorphs in liquid-assisted syntheses N2 - The synthesis of the polymorphic cocrystal caffeine:anthranilic acid was investigated to obtain a better understanding of the processes leading to the formation of different polymorphic forms. In the case of these cocrystal polymorphs synthesized by liquid-assisted grinding a distinct influence of the dipole moment of the solvent was found. A pre-coordination between the solvent molecules and the caffeine:anthranilic acid cocrystal could be identified in the formation of form II. In the case of form II the solvent can be regarded as a catalyst. The formation pathway of each polymorph was evaluated using synchrotron X-ray diffraction. KW - cocrystal KW - synchrotron X-ray diffraction KW - caffeine PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-313222 DO - https://doi.org/10.1039/c4ce00472h SN - 1466-8033 VL - 16 IS - 35 SP - 8272 EP - 8278 CY - London, UK AN - OPUS4-31322 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Bennetts, V.H. A1 - Lilienthal, A.J. A1 - Bartholmai, Matthias T1 - From insects to micro air vehicles - a comparison of reactive plume tracking strategies N2 - Insect behavior is a common source of inspiration for roboticists and computer scientists when designing gas-sensitive mobile robots. More specifically, tracking airborne odor plumes, and localization of distant gas sources are abilities that suit practical applications such as leak localization and emission monitoring. Gas sensing with mobile robots has been mostly addressed with ground-based platforms and under simplified conditions and thus, there exist a significant gap between the outstanding insect abilities and state-of-the-art robotics systems. As a step toward practical applications, we evaluated the performance of three biologically inspired plume tracking algorithms. The evaluation is carried out not only with computer simulations, but also with real-world experiments in which, a quadrocopter-based micro Unmanned Aerial Vehicle autonomously follows a methane trail toward the emitting source. Compared to ground robots, micro UAVs bring several advantages such as their superior steering capabilities and fewer mobility restrictions in complex terrains. The experimental evaluation shows that, under certain environmental conditions, insect like behavior in gas-sensitive UAVs is feasible in real-world environments. T2 - IAS13 - 13th International conference on intelligent autonomous systems CY - Padova, Italy DA - 2014-07-15 KW - Autonomous micro UAV KW - Mobile robot olfaction KW - Gas source localization KW - Reactive plume tracking KW - Biologically inspired robots PY - 2016 SN - 978-3-319-08338-4; 978-3-319-08337-7 DO - https://doi.org/10.1007/978-3-319-08338-4_110 SN - 2194-5357 SP - 1533 EP - 1548 PB - Springer Verlag CY - Berlin, Germany AN - OPUS4-31526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ecker, Melanie A1 - Pretsch, Thorsten T1 - Novel design approaches for multifunctional information carriers N2 - Two design approaches for multifunctional information carriers are introduced. In the first one, quick response (QR) code carriers, which were composed of poly(ester urethane) (PEU) and microencapsulated thermochromic pigments (T-PIGs), differing in color and color switching temperature (CST), were prepared. The obtained material systems exhibited machine-readable QR codes at 23 °C and a two-stage decolorization when heated, culminating in unreadable QR codes at temperatures above the highest CST of the employed T-PIGs. In the second scenario, information carriers were sealed with a dark, thermochromic PEU layer. As a result, the QR codes were hidden at 23 °C and became readable upon heating due to color fading. Beyond the characterization of the employed components, preparation methods, functionality analyses and durability investigations are reported. When heated after thermo-mechanical programming, pronounced shape memory properties could be verified. The thermo-responsiveness of such multifunctional material systems may qualify them for usage in anti-counterfeiting applications. KW - Poly(ester urethane) KW - Shape memory polymer KW - Thermo-responsiveness KW - Information carrier KW - QR code carrier KW - Thermochromic properties KW - Microencapsulated thermochromic pigments KW - Anti-counterfeiting KW - Smart label KW - Difficult-to-copy KW - Durability KW - Multifuncitonal material systems PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-315176 DO - https://doi.org/10.1039/c4ra08977d SN - 2046-2069 VL - 4 IS - 87 SP - 46680 EP - 46688 PB - RSC Publishing CY - London AN - OPUS4-31517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Vogl, Jochen A1 - Rosner, M. ED - Babbi, A. ED - Peltz, U. T1 - Bleiisotopenanalyse der römischen >Tabella Defixionis< N2 - Blei weist in der Natur die vier stabilen Isotope 204Pb, 206Pb, 207Pb und 208Pb auf, mit den entsprechenden Isotopenhäufigkeiten von 1,4%, 24,1 %, 22,1 % und 52,4 %686. Dabei sind 206Pb, 207Pb und 208Pb radiogene Isotope, welche als Endglieder der natürlichen Zerfallsreihen von 238U, 235U und 232Th entstanden sind. 204Pb ist ein sogenanntes primordiales Isotop, welches bereits vor Entstehung der Erde vorhanden war. Aufgrund dieser Prozesse weisen Gesteine, Mineralien und Erze eine charakteristische Bleiisotopenzusammensetzung auf, die von der Ausgangskonzentration an Blei, Thorium und Uran sowie von der seit der Gesteinsgenese vergangenen Zeit abhängt. Diese Eigenschaft bleibt auch während der Bleigewinnung aus dem Erz, meist Galenit, erhalten, auch wenn das Silber vorher durch Kupellation abgetrennt wurde687. Das in Silbererzen enthaltene Blei war ein willkommenes Nebenprodukt der Erzverhüttung und wurde zur Herstellung von Bleiobjekten verwendet. Artefakte, die aus dem so gewonnenen Blei gefertigt wurden, spiegeln daher die Bleiisotopenzusammensetzung der verwendeten Rohmaterialien wider. KW - Blei KW - Isotopenzusammensetzung KW - Fluchtafel KW - Herkunft PY - 2013 SN - 978-3-88467-207-5 SN - 0171-1474 N1 - Serientitel: Monographien des Römisch-Germanischen Zentralmuseums – Series title: Monographien des Römisch-Germanischen Zentralmuseums VL - 109 SP - 182 EP - 184 PB - Verlag des Römisch-Germanischen Zentralmuseums CY - Mainz AN - OPUS4-29842 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Redmer, Bernhard A1 - Föllner, Maik ED - Babbi, A. ED - Peltz, U. T1 - Radiographische Untersuchungen der Bronzeobjekte N2 - Ziel der Durchstrahlung war es, anhand von Bearbeitungsspuren am Objekt auf die Fertigungstechnologie und damit auf die Formgebung des Gegenstandes schließen zu können. Dazu wurde die technische Radiographie mit Speicherfolientechnik als zerstörungsfreies und bildgebendes Prüfverfahren angewendet. KW - Kunst KW - Bronze KW - Röntgentechnik KW - Computer-Radiographie PY - 2013 SN - 978-3-88467-207-5 SN - 0171-1474 N1 - Serientitel: Monographien des Römisch-Germanischen Zentralmuseums – Series title: Monographien des Römisch-Germanischen Zentralmuseums IS - 109 SP - 165 EP - 172 PB - Verlag des Römisch-Germanischen Zentralmuseums CY - Mainz AN - OPUS4-29786 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neffe, A.T. A1 - Von Ruesten-Lange, M. A1 - Braune, S. A1 - Lützow, K. A1 - Roch, T. A1 - Richau, K. A1 - Krüger, A. A1 - Becherer, T. A1 - Thünemann, Andreas A1 - Jung, F. A1 - Haag, R. A1 - Lendlein, A. T1 - Multivalent grafting of hyperbranched oligo- and polyglycerols shielding rough membranes to mediate hemocompatibility N2 - Hemocompatible materials are needed for internal and extracorporeal biomedical applications, which should be realizable by reducing protein and thrombocyte adhesion to such materials. Polyethers have been demonstrated to be highly efficient in this respect on smooth surfaces. Here, we investigate the grafting of oligo- and polyglycerols to rough poly(ether imide) membranes as a polymer relevant to biomedical applications and show the reduction of protein and thrombocyte adhesion as well as thrombocyte activation. It could be demonstrated that, by performing surface grafting with oligo- and polyglycerols of relatively high polydispersity (>1.5) and several reactive groups for surface anchoring, full surface shielding can be reached, which leads to reduced protein adsorption of albumin and fibrinogen. In addition, adherent thrombocytes were not activated. This could be clearly shown by immunostaining adherent proteins and analyzing the thrombocyte covered area. The presented work provides an important strategy for the development of application relevant hemocompatible 3D structured materials. KW - Nanotechnology KW - thrombocyte adhesion KW - biomedical applications PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-308196 DO - https://doi.org/10.1039/c4tb00184b SN - 2050-750X SN - 2050-7518 VL - 2 IS - 23 SP - 3626 EP - 3635 PB - Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-30819 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Feuchtemessung im Bauwesen - Ein Überblick N2 - Ein Großteil der Schäden im Baubereich ist auf feuchteinduzierte Prozesse zurückzuführen. Der Erhaltungsaufwand allein im Hochbau wurde bereits vor einiger Zeit auf jährlich ca. 35 Mrd. Euro geschätzt. Aus diesem Grund hat die Feuchtemessung in der Bauwerksdiagnose eine sehr hohe Bedeutung - und im Idealfall sollte sie natürlich alles können: schnell sein, wiederholbar und zerstörungsfrei anwendbar. Zwar gibt es eine Vielzahl an verfügbaren Feuchtemesstechniken, oft fällt es Anwendern aber schwer, einzuschätzen welches die richtige Prüfmethode für ihr Problem ist. Genormt sind nur direkte und zerstörende Verfahren, die zwar teils hochgenau, aber doch nur stichprobenartig Aussagen liefern können. Die anderen, zerstörungsfreien Methoden basieren auf der Änderung feuchteabhängiger physikalischer Materialeigenschaften. Ihre Grundlagen, sowie Vor- und Nachteile werden hier näher dargestellt. T2 - Fachtagung Bauwerksdiagnose 2014 CY - Berlin, Germany DA - 13.02.2014 KW - Feuchtemessung KW - Zerstörungsfreie Prüfung KW - Baustoffe PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-311672 UR - http://www.bauwerksdiagnose2014.de/portals/bwd2014/BB/vortrag%205.pdf UR - http://www.bauwerksdiagnose2014.de/Berichtsband SN - 978-3-940283-56-6 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-31167 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bald, Ilko A1 - Keller, A. T1 - Molecular processes studied at a single-molecule level using DNA origami nanostructures and atomic force microscopy N2 - DNA origami nanostructures allow for the arrangement of different functionalities such as proteins, specific DNA structures, nanoparticles, and various chemical modifications with unprecedented precision. The arranged functional entities can be visualized by atomic force microscopy (AFM) which enables the study of molecular processes at a single-molecular level. Examples comprise the investigation of chemical reactions, electron-induced bond breaking, enzymatic binding and cleavage events, and conformational transitions in DNA. In this paper, we provide an overview of the advances achieved in the field of single-molecule investigations by applying atomic force microscopy to functionalized DNA origami substrates. KW - DNA origami KW - atomic force microscopy KW - single-molecule analysis KW - DNA radiation damage KW - protein binding KW - enzyme reactions KW - G quadruplexes PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-314343 DO - https://doi.org/10.3390/molecules190913803 SN - 1420-3049 VL - 19 IS - 9 SP - 13803 EP - 13823 PB - MDPI CY - Basel AN - OPUS4-31434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane T1 - Measurement of the radiative energy output of flash lamps by means of thermal thin probes N2 - Flash lamps are widely used excitation sources in the field of non-destructive testing with active thermography. Though the realized energy density in front of the investigated object is a significant factor with regard to detection sensitivity, only few data concerning this issue have been published so far. It is shown here that local energy densities can be estimated by means of a simple metal plate, which exhibits a certain temperature increase after flash excitation. After discussing the underlying calorimetric principle the sensor concept is reviewed using constant blackbody radiation and short laser pulses, since both kinds of sources generate known energy densities. The relative uncertainty of measurements of the energy density is found to be in the range of 10%. The last part of the present paper describes an application for characterizing the radiation of a usual 6 kJ flash lamp. The energy conversion efficiency was found to be only about 11%. KW - Flash thermography KW - Flash lamp KW - Energy sensor KW - Calorimetric principle KW - Conversion efficiency PY - 2014 DO - https://doi.org/10.1016/j.infrared.2014.07.012 SN - 1350-4495 VL - 67 SP - 363 EP - 370 PB - Elsevier CY - Amsterdam AN - OPUS4-31436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krause, Christina A1 - Zorn, R. A1 - Emmerling, Franziska A1 - Falkenhagen, Jana A1 - Frick, B. A1 - Huber, P. A1 - Schönhals, Andreas T1 - Vibrational density of states of triphenylene based discotic liquid crystals: dependence on the length of the alkyl chain N2 - The vibrational density of states of a series of homologous triphenylene-based discotic liquid crystals HATn (n = 5, 6, 8, 10, 12) depending on the length of the aliphatic side chain is investigated by means of inelastic neutron scattering. All studied materials have a plastic crystalline phase at low temperatures, followed by a hexagonally ordered liquid crystalline phase at higher temperatures and a quasi isotropic phase at the highest temperatures. The X-ray scattering pattern for the plastic crystalline phase of all materials shows a sharp Bragg reflection corresponding to the intercolumnar distance in the lower q-range and a peak at circa 17 nm-1 related to intracolumnar distances between the cores perpendicular to the columns as well as a broad amorphous halo related to the disordered structure of the methylene groups in the side chains in the higher q-range. The intercolumnar distance increases linearly with increasing chain length for the hexagonal columnar ordered liquid crystalline phase. A similar behaviour is assumed for the plastic crystalline phase. Besides n = 8 all materials under study exhibit a Boson peak. With increasing chain length, the frequency of the Boson peak decreases and its intensity increases. This can be explained by a self-organized confinement model. The peaks for n = 10, 12 are much narrower than for n = 5, 6 which might imply the transformation from a rigid system to a softer one with increasing chain length. Moreover the results can also be discussed in the framework of a transition from an uncorrelated to a correlated disorder with increasing n where n = 8 might be speculatively considered as a transitional state. KW - X-ray scattering KW - Neutron scattering KW - Differential scanning calorimetry PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-304789 DO - https://doi.org/10.1039/c3cp55303e SN - 1463-9076 SN - 1463-9084 VL - 16 IS - 16 SP - 7324 EP - 7333 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-30478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agirrezabal-Telleria, Iker A1 - Guo, Y. A1 - Hemmann, Felix A1 - Arias, P. L. A1 - Kemnitz, E. T1 - Dehydration of xylose and glucose to furan derivatives using bifunctional partially hydroxylated MgF2 catalysts and N2-stripping N2 - The current furfural production yield is low due to the use of non-selective homogeneous catalysts and expensive separation. In this work, partially hydroxylated MgF2 catalysts, synthesized using different water contents, were screened during xylose dehydration in water–toluene at 160 °C. The different Lewis/Brønsted ratios on the MgF2 catalysts showed that under-coordinated Mg can isomerize xylose to xylulose, whilst the surface OH-groups were responsible for the dehydration reactions. The presence of glucose as a co-carbohydrate reduced the furfural selectivity from 86 to 81%, whilst it also led to high 5-hydroxymethylfurfural selectivity. The tests catalyzed by MgF2 in combination with simultaneous N2-stripping showed that a furfural selectivity of 87% could be achieved using low xylose loadings. Moreover, the catalysts regenerated by H2O2 showed high activity during the dehydration tests in water–toluene at 160 °C. KW - Bifunctional MgF2 KW - Lewis/Bronsted KW - Carbohydrates KW - Furan derivatives KW - N2-stripping PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-305441 DO - https://doi.org/10.1039/c4cy00129j SN - 2044-4753 SN - 2044-4761 VL - 4 IS - 5 SP - 1357 EP - 1368 PB - RSC Publ. CY - Cambridge AN - OPUS4-30544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szczerba, Wojciech A1 - Schott, M. A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas A1 - Kurth, D.G. T1 - Thermally induced structural rearrangement of the Fe(II) coordination geometry in metallo-supramolecular polyelectrolytes N2 - Rigid rod-type metallo-supramolecular coordination polyelectrolytes with Fe(II) centres (Fe-MEPEs) are produced via the self-assembly of the ditopic ligand 1,4-bis(2,2':6',2''-terpyridine-4'-yl)benzene (tpy-ph-tpy) and Fe(II) acetate. Fe-MEPEs exhibit remarkable electrochromic properties; they change colour from blue to transparent when an electric potential is applied. This electrochemical process is generally reversible. The blue colour in the ground state is a result of a metal-to-ligand charge transfer at the Fe(II) centre ion in a quasi-octahedral geometry. When annealed at temperatures above 100 °C, the blue colour turns into green and the formerly reversible electrochromic properties are lost, even after cooling down to room temperature. The thermally induced changes in the Fe(II) coordination sphere are investigated in situ during annealing of a solid Fe-MEPE using X-ray absorption fine structure (XAFS) spectroscopy. The study reveals that the thermally induced transition is not accompanied by a redox process at the Fe(II) centre. From the detailed analysis of the XAFS spectra, the changes are attributed to structural changes in the coordination sphere of the Fe(II) site. In the low temperature state, the Fe(II) ion rests in a quasi-octahedral coordination environment surrounded by six nitrogen atoms of the pyridine rings. The axial Fe–N bond length is 1.94 Å, while the equatorial bond length amounts to 1.98 Å. In the high temperature state, the FeN6-site exhibits a distortion with the axial Fe–N bonds being shortened to 1.88 Å and the equatorial Fe–N bonds being elongated to 2.01 Å. KW - Metallo-supramolecular polyelectrolytes KW - Electrochromism KW - XANES KW - EXAFS KW - Local structure KW - Thermal stability PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-317331 DO - https://doi.org/10.1039/c4cp01187b SN - 1463-9076 SN - 1463-9084 VL - 16 IS - 36 SP - 19694 EP - 19701 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-31733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stoch, P. A1 - Szczerba, Wojciech A1 - Bodnar, W. A1 - Ciecinska, M. A1 - Stoch, A. A1 - Burkel, E. T1 - Structural properties of iron-phosphate glasses: spectroscopic studies and ab initio simulations N2 - Vitrification is the most effective method for the immobilization of hazardous waste by incorporating toxic elements into a glass structure. Iron phosphate glasses are presently being considered as matrices for the storage of radioactive waste, even of those which cannot be vitrified using conventional borosilicate waste glass. In this study, a structural model of 60P2O5–40Fe2O3 glass is proposed. The model is based on the crystal structure of FePO4 which is composed of [FeO4][PO4] tetrahedral rings. The rings are optimized using the DFT method and the obtained theoretical FTIR and Raman spectra are being compared with their experimental counterparts. Moreover, the proposed model is in very good agreement with X-ray absorption fine structure spectroscopy (XANES/EXAFS) and Mössbauer spectroscopy measurements. According to the calculations the Fe3+ is in tetrahedral and five-fold coordination. The maximal predicted load of waste constituents into the glass without rebuilding of the structure is 30 mol%. Below this content, waste constituents balance the charge of [FeO4]- tetrahedra which leads to their strong bonding to the glass resulting in an increase of the chemical durability, transformation and melting temperatures and density. KW - Glass KW - Iron KW - DFT simulations KW - Mössbauer spectroscopy KW - XANES/EXAFS KW - FTIR spectroscopy KW - Raman spectroscopy KW - Coordination PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-317351 DO - https://doi.org/10.1039/c4cp03113j SN - 1463-9076 SN - 1463-9084 VL - 16 IS - 37 SP - 19917 EP - 19927 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-31735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Isleyen, A. T1 - Matrix reference materials for environmental analysis N2 - Reliable analysis of chemical indicators in water, sediment and soil samples for the purpose of environmental pollution assessment poses one of the greatest analytical challenges, having in mind the complexity of sample matrix and low concentrations of pollutants. Organics (pesticides, PAHs, PCBs, etc.) and heavy metals (Hg, Cd, Ni, Pb and As) represent target parameters. Laboratories performing sampling and tests in this field regulated by respective EU directives [1], need strong support in terms of providing them with appropriate matrix CRMs enabling the process of quality control. NMIs and DIs with proven metrological capabilities for the production and certification of such materials are necessary for the provision of quality data. This project is aiming to develop capacity to produce CRMs for environmental analysis by transferring the theoretical and practical know-how between the partners and combining their skills to focus on environmental CRM production in accordance with ISO Guide 34 [2]. Production process includes good manufacturing practices for processing materials, method development and validation for homogeneity, stability and characterisation tests, characterisation of selected analytes together with additional information about matrix constituents, the calculation of individual uncertainties (between units inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. Inter laboratory comparison registered as EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills. T2 - 9th International Conference on Instrumental Methods of Analysis: Modern Trends and Applications CY - Kalamata, Greece DA - 20.09.2015 KW - PFOS KW - Environment KW - CRM KW - Soil KW - Heavy metal KW - PFOA PY - 2015 UR - http://www.ima2015.teikal.gr/images/IMA-2015_book_of_abstracts.pdf AN - OPUS4-38799 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Isleyen, A. T1 - A Joint Research Project for the Sustainable Production of Certified Matrix Reference Materials for Environmental Analysis N2 - Reliable analysis of chemical indicators in water, sediment and soil samples for the purpose of environmental pollution assessment poses one of the greatest analytical challenges, having in mind the complexity of sample matrix and low concentrations of pollutants. Organics (pesticides, PAHs, PCBs, etc.) and heavy metals (Hg, Cd, Ni, Pb and As) represent target parameters. Laboratories performing sampling and tests in this field regulated by respective EU directives, need strong support in terms of providing them with appropriate matrix CRMs enabling the process of quality control. NMIs and DIs with proven metrological capabilities for the production and certification of such materials are necessary for the provision of quality data. This project is aiming to develop capacity to produce CRMs for environmental analysis by transferring the theoretical and practical know-how between the partners and combining their skills to focus on environmental CRM production in accordance with ISO Guide 34. Production process includes good manufacturing practices for processing materials, method development and validation for homogeneity, stability and characterisation tests, characterisation of selected analytes together with additional information about matrix constituents, the calculation of individual uncertainties (between units inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. Inter laboratory comparison registered as EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills. T2 - BERM-14 International Symposium on Biological and Environmental Reference Materials CY - National Harbor, Maryland, USA DA - 12.10.2015 KW - Soil KW - Heavy metal KW - Environment KW - CRM KW - PFOA KW - PFOS PY - 2015 AN - OPUS4-38800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Manso, M. T1 - Assessment of heavy metals and hazardous substances in tattoo inks N2 - Tattooing practice is adopted worldwide and represents a socio-cultural phenomenon, but the injection into the skin of coloring agents, such as metals might pose a serious health problem. Tattoo ink compounds are in general not officially controlled. Moreover, the origins as well as the chemical and toxicological specifications of these coloring agents are hardly known by the producers, the tattooists and by the consumers. In this view, the aim of this study was to characterize the metal composition of tattoo inks available in the market and to draw attention to the associated risk for human health. A set of tattoo inks from the brand Kuro Sumi was analyzed by means of Synchrotron-based X-ray Fluorescence spectrometry (Sy-XRF) at BAMline @ BESSY II and Raman Spectroscopy using the XploRA confocal Raman microscope (785 nm laser) at the LIBPhys-UNL. Carbon black, rutile, phtalo blue, phtalo green, helizarin red, helizarin yellow and dioxazine violet were respectively identified in black, white, blue, green, red, yellow and violet inks. However, a wide range of transition and heavy metals, potentially hazardous was revealed by Sy-XRF. A semi-quantitative evaluation has revealed, in some inks, amounts of Cr, Cu, Zn and Pb higher than the allowed according to the resolution adopted by the Council of Europe on the safety of tattoos and permanent make-up. T2 - European Conference on X-Ray Spectrometry (EXRS) CY - Gothenburg, Schweden DA - 19.06.2016 KW - Synchrotron KW - XRF KW - Tattoo PY - 2016 AN - OPUS4-38804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Manso, M. T1 - Toxic metals in tattoo inks N2 - Tattooing practice is adopted worldwide and represents a socio-cultural phenomenon, but the injection into the skin of coloring agents, such as metals might pose a serious health problem. Tattoo ink compounds are in general not officially controlled. Moreover, the origins as well as the chemical and toxicological specifications of these coloring agents are hardly known by the producers, the tattooists and by the consumers. In this view, the aim of this study was to characterize the metal composition of tattoo inks available in the market and to draw attention to the associated risk for human health. A set of tattoo inks from the brand Kuro Sumi was analyzed by means of Synchrotron-based X-ray Fluorescence spectrometry (Sy-XRF) at BAMline @ BESSY II and Raman Spectroscopy using the XploRA confocal Raman microscope (785 nm laser). Carbon black, rutile, phtalo blue, phtalo green, helizarin red, helizarin yellow and dioxazine violet were respectively identified in black, white, blue, green, red, yellow and violet inks. However, a wide range of transition and heavy metals, potentially hazardous was revealed by Sy-XRF. A semi-quantitative evaluation has revealed, in some inks, amounts of Cr, Cu, Zn and Pb higher than the allowed according to the resolution adopted by the Council of Europe on the safety of tattoos and permanent make-up (PMU. T2 - Heavy Metals: from the Environment to the Man CY - Lissabon, Portugal DA - 21.03.2016 KW - Synchrotron KW - BAMline KW - XRF KW - Tattoo PY - 2016 AN - OPUS4-38806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - First in situ measurements with a newly developed SR-based ‘Single-shot‘ EXAFS set-up N2 - The newly developed EXAFS set-up comprises both time- and spatially-resolved EXAFS information simultaneously in a single-shot. This facile, stable and scanningless set-up was tested at the BAMline @ BESSY-II (Berlin, Germany). The primary broadband beam is generated by a filter/X-ray-mirror combination (bandpass). The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by an area sensitive detector based on a CCD camera, in a theta - 2 theta geometry. The first in situ measurements were successfully carried out and hereby presented. The case-study involved a well known reaction, in which structural changes are induced over time, and continuously measured. We were able to track structural changes within a 1s time resolution. T2 - European Conference on X-Ray Spectrometry (EXRS) CY - Gothenburg, Sweden DA - 19.06.2016 KW - Synchrotron KW - BAMline KW - EXAFS PY - 2016 AN - OPUS4-38807 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Online low-field NMR spectroscopy in modular plants for chemical production N2 - Die Online-Reaktionsverfolgung ist der Schlüssel zur chemischen Prozesskontrolle. Heute werden in diesem Bereich hauptsächlich Methoden der optischen Spektroskopie eingesetzt. Durch aktuelle Entwicklungen im Bereich kompakter Niederfeld-NMR-Spektrometer auf Basis von Permanentmagnetsystemen ist erstmals auch die Integration unmittelbar in einer industriellen Produktionsumgebung möglich. Diese Geräte sind robuste und relativ preiswerte Analysatoren, welche die Vorteile eines wartungsfreundlichen Betriebs ohne Notwendigkeit von kryogenen Flüssigkeiten, sowie eine einfache Handhabung vereinen. Aktuell auf dem Markt verfügbare Geräte sind jedoch ausschließlich auf den Einsatz im Laborbetrieb ausgerichtet. Für die Kopplung als Online-Methode im Prozesseinsatz ist die Entwicklung geeigneter Durchflusszellen notwendig. Diese ermöglichen idealerweise ein gutes Signal-Rausch-Verhältnis, eine ausreichende Robustheit und müssen die Anforderungen an die Integration in industrielle Anlagen erfüllen (z.B. Explosionsschutz, Temperierung). Intensivierte kontinuierliche Prozesse stehen im Fokus der aktuellen Forschung. Im Vergleich zu etablierten Batch-Verfahren besteht in modularen chemischen Anlagen die Möglichkeit durch kurze Umrüstzeiten zwischen Kampagnen effektiv auf die Marktentwicklung zu reagieren. Bei kontinuierlicher Prozessführung sind Online-Sensoren und eine zuverlässige und schnelle Regelung der Produktqualität essentiell. Andernfalls besteht ein großes Risiko, große Mengen nicht-spezifikationskonformer Produkte zu erhalten. Dies wird im Rahmen des Forschungsprojekts CONSENS (Integrated Control and Sensing) der Europäischen Union durch die Entwicklung und Integration intelligenter Sensormodule zur Prozessüberwachung und -steuerung in modularen Anlagenkonzepten thematisiert. Das vorgestellte NMR-Analysatormodul mit der Baugröße von 57 x 57 x 85 cm basiert auf einem kompakten 43,5-MHz-NMR-Spektrometer. Dieses ist zusammen mit einem Akquisitionsrechner und einer programmierbaren Steuerung für die automatisierte Daten-aufbereitung (Phasing, Baseline-Korrektur) und Auswertung in ein explosionsgeschütztes Gehäuse integriert. Für die automatisierte Datenanalyse kommt die Methode des Indirect Hard Modelings (IHM) zum Einsatz. Die entwickelten IHM-Modelle werden mittels Online-Hochfeld-NMR-Spektroskopie als Referenzverfahren in einem Versuchsaufbau zur Überwachung kontinuierlicher Reaktionen auf Basis eines mit Spritzenpumpen betriebenen 1/8" Rohrreaktors validiert. N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and relatively inexpensive analysers, which feature advantages like low cost, low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, sufficient robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. If these are not available, there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Union’s Research Project CONSENS (Integrated Control and Sensing [3]) by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. The presented NMR module is provided in an explosion proof housing of 57 x 57 x 85 cm module size and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling (IHM) was selected for data analysis of the low-field NMR spectra. A set-up for monitoring continuous reactions in a thermostated 1/8” tubular reactor using automated syringe pumps was used to validate the IHM models by using high-field NMR spectroscopy as analytical reference method. T2 - Praktische Probleme der Kernresonanzspektroskopie CY - Erlangen, Germany DA - 16.01.2017 KW - Online NMR spectroscopy KW - Automated data evaluation KW - NMR sensor KW - Process control PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-389819 AN - OPUS4-38981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Hodoroaba, Vasile-Dan A1 - Mielke, Johannes T1 - Templates for nanomaterial characterisation of tier 1 and tier 2 measurement methods N2 - The EU FP7 NanoDefine project was launched in November 2013 and will run until October 2017. The Project is dedicated to support the implementation of the EU Recommendation on the Definition of Nanomaterial by the provision of the required analytical tools and respective guidance. Main goal is to develop a novel tiered approach consisting of (i) rapid and cost-efficient screening methods and (ii) confirmatory measurement methods. The "NanoDefiner" eTool will guide potential end-users, such as concerned industries and regulatory bodies as well as enforcement and contract laboratories, to reliably classify if a material is nano or not. To achieve this objective, a comprehensive inter-laboratory evaluation of the performance of current characterisation techniques, instruments and software is performed. Instruments, software and methods are further developed. Their capacity to reliably measure the size of particulates in the size range 1-100 nm and above (according to the EU definition) is validated. Technical reports on project results are published to reach out to relevant stakeholders, such as policy makers, regulators, industries and the wider scientific community, to present and discuss our goals and results, to ensure a continuous exchange of views, needs and experiences obtained from different fields of expertise and application, and to finally integrate the resulting feedback into our ongoing work on the size-related classification of nanomaterials. KW - Nanomaterial KW - Measurement method KW - Screening methods KW - Confirmatory methods PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-389827 UR - http://www.nanodefine.eu/index.php/downloads/nanodefine-technical-reports SP - 1 EP - 74 PB - The NanoDefine Consortium CY - Wageningen, The Netherlands AN - OPUS4-38982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Thünemann, Andreas A1 - Emmerling, Franziska A1 - Hodoroaba, Vasile-Dan T1 - Review of existing calibration or reference N2 - We report on calibration standards of nanoparticles meeting the definition of a nanomaterial given by the European Commission (EU 2011) which are relevant for the characterisation methods applied in the NanoDefine project. We found that the Impact of nanoparticles is outstanding in the scientific literature. A number of 270.000 paper titles on nanoparticles are listed in the Web of Science data base. But surprisingly, the availability of suitable certified standard reference materials is scarce. Only a few sources were found. For example, BAM provides the database Nanoscaled Reference Materials at http://www.nano-refmat.bam.de/en/ in cooperation with the ISO/TC 229 Nanotechnologies. In addition, two publications from 2013 on nanoscale reference materials are available. Candidates of nano-(certified) reference materials from other ongoing or just finished FP6 and FP7 nano-metrology projects have been extracted from the Compendium of Projects in the European NanoSafety Cluster (Compendium NSC, 2013). Recommendations for selection of representative test materials and calibration standards for NanoDefine internal tasks, respectively, are also given. KW - Nanomaterial KW - Reference materials KW - Certified reference materials PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-389836 UR - http://www.nanodefine.eu/index.php/downloads/nanodefine-technical-reports SP - 1 EP - 18 CY - Wageningen, The Netherlands AN - OPUS4-38983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feller, Viktor A1 - Mielentz, Frank A1 - Klewe, T. A1 - Orglmeister, R. T1 - Codierte Sendesignale für die Ultraschallprüfung von Betonbauteilen T1 - Coded transmission in ultrasonic testing of concrete components N2 - Es wurden Untersuchungen hinsichtlich der Eignung und der praktischen Relevanz von codierten Sendesignalen als Anregungsimpulse für die Ultraschallprüfung von Betonbauteilen durchgeführt. Anhand von synthetischen Daten werden die theoretischen Vorteile der codierten Impulssequenzen gezeigt. Im Anschluss werden Barker- und Golay-codierte Sendesignale an einer Betonstufenplatte mit einem Größtkorn von 16 mm getestet. Es zeigt sich das große Potenzial dieses Verfahrens, insbesondere bei Verwendung von Golay-Sequenzen als Anregung für die Ultraschallprüfköpfe. Es ergibt sich ein deutlich verbessertes Signal-Stör-Verhältnis im Vergleich zu den herkömmlichen bipolaren Rechteckimpulsen. KW - Ultraschall KW - Codierte Sendesignale KW - Korrelationsanalyse KW - Bauwesen PY - 2017 DO - https://doi.org/10.1515/teme-2016-0026 SN - 2196-7113 SN - 0171-8096 VL - 84 IS - 4 SP - 234 EP - 240 PB - Oldenbourg Verlag CY - München AN - OPUS4-38934 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, R. T1 - SEM or TEM for the characterization of nanoparticles? N2 - Scanning Electron Microscopy (SEM) or Transmission Electron Microscopy (TEM) ? This is a question, nowadays discussed in EM labs of research and industry involved in the characterization and metrology of nanoparticles. The Scanning principle is adapted to TEM, the Transmission mode is adapted to Ultra High Resolution SEM. Can modern SEM replace TEM, reach atomic resolution even without Cs corrector or nm lateral resolution for X-ray Spectroscopy (EDX)? Due to the development of a New Cold Field Emission (NCFE) electron source Hitachi SEMs SU9000 and SU8200 can deliver routinely sub-nm image resolution and EDX mappings at very high count rates and a lateral EDX resolution of a few nm. A TiO2 sample provided by BAM was analysed at 30 kV using low kV STEM – simultaneously with the Through-the-lens (TTL) SE detector, the Bright Field transmission and Dark Field transmission signals. By this method a pixel-precise information of the particle’s surface using SE, its chemical nature using DF-STEM and its crystalline structure using Bright Field signal is given in one 40sec scan. The advantage of this observation mode compared to Ultra Low Voltage imaging is outlined. T2 - 7. NRW Nano-Konferenz CY - Münster, Germany DA - 07.12.2016 KW - SEM KW - TEM KW - Nanoparticles PY - 2016 AN - OPUS4-38936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - van de Kreeke, Johannes T1 - EPTIS presentation for CNAS and RMPT workshop, Beijing 2016 N2 - Introduction to EPTIS for Chinese and regional audience T2 - RMPT workshop 2016 CY - Beijing, China DA - 20.09.2016 KW - EPTIS KW - Ringversuche KW - Proficiency testing KW - PT KW - ILC PY - 2016 AN - OPUS4-39004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Procop, Mathias A1 - Hodoroaba, Vasile-Dan A1 - Terborg, R. A1 - Berger, D. T1 - Determination of the Effective Detector Area of an Energy-Dispersive X-Ray Spectrometer at the Scanning Electron Microscope Using Experimental and Theoretical X-Ray Emission Yields N2 - A method is proposed to determine the effective detector area for energy-dispersive X-ray spectrometers (EDS). Nowadays, detectors are available for a wide range of nominal areas ranging from 10 up to 150mm2. However, it remains in most cases unknown whether this nominal area coincides with the “net active sensor area” that should be given according to the related standard ISO 15632, or with any other area of the detector device. Moreover, the specific geometry of EDS installation may further reduce a given detector area. The proposed method can be applied to most scanning electron microscope/EDS configurations. The basic idea consists in a comparison of the measured count rate with the count rate resulting from known X-ray yields of copper, titanium, or silicon. The method was successfully tested on three detectors with known effective area and applied further to seven spectrometers from different manufacturers. In most cases the method gave an effective area smaller than the area given in the detector description. KW - Energy-dispersive X-ray spectrometer (EDS) KW - EDX KW - Effective area KW - X-ray emission yield KW - Geometrical collection efficiency PY - 2016 UR - https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/div-classtitledetermination-of-the-effective-detector-area-of-an-energy-dispersive-x-ray-spectrometer-at-the-scanning-electron-microscope-using-experimental-and-theoretical-x-ray-emission-yieldsdiv/E15B2E67C349201CF323E778EB9C6D94 DO - https://doi.org/10.1017/S1431927616011788 VL - 22 IS - 6 SP - 1360 EP - 1368 PB - Cambridge University Press CY - New York, NY, USA AN - OPUS4-38858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Unger, Wolfgang T1 - Non-destructive surface measurements N2 - Materials and chemical producers require detailed knowledge of surface chemistry for research into new products. One way to understand a surface without damaging it is to bombard it with an electron beam, causing its atoms to emit characteristic X-rays enabling identification. The measurement of these must be precise as many elements emissions are close in energy – traceable reference materials will ensure instruments using this technique are stable and accurate. KW - Metrology KW - EDS KW - EDX PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-388647 UR - http://www.euramet.org/metrology-for-societys-challenges/metrology-for-industry/impact-case-studies-emrp-industry-theme/ SP - 1 EP - 2 CY - Teddington AN - OPUS4-38864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Unger, Wolfgang T1 - Measuring organic layers N2 - Many innovative products - from touchscreens to solar panels to pharmaceuticals – utilise multiple organic layers to create complex functionality. New techniques have been developed to remove and measure layers individually enabling improved product development and assisting with quality assurance. However, manufacturers cannot be certain of the depth of layer being removed and new reference materials for these techniques are needed to increase uptake, and remove a major barrier to innovation. KW - Organic layers KW - XPS KW - SIMS PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-388656 UR - http://www.euramet.org/metrology-for-societys-challenges/metrology-for-industry/impact-case-studies-emrp-industry-theme/ SP - 1 EP - 2 CY - Teddington AN - OPUS4-38865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Unger, Wolfgang T1 - Surface analysis for Alzheimer’s N2 - Modifying or controlling surface chemistry is important in new product development, quality control and research. This is particularly true where functionality of surfaces, thin films and interfaces are key to the application, such as organic solar cells and devices for medical diagnostics. Surface chemical analysis aims to provide quantitative elemental, chemical state and functional group information from the surface of materials, but requires comparable test data and improved measurement traceability. KW - Liposomes KW - Proteins KW - ToF-SIMS KW - Peptides KW - Mapping PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-388663 UR - http://www.euramet.org/metrology-for-societys-challenges/metrology-for-industry/impact-case-studies-emrp-industry-theme/ SP - 1 EP - 2 CY - Teddington AN - OPUS4-38866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Hiratsuka, M. T1 - Interlaboratory comparison: optical property classification of carbon-based films by ellipsometry N2 - The paper addresses the “INTERLABORATORY COMPARISON: OPTICAL PROPERTY CLASSIFICATION OF CARBON-BASED FILMS BY ELLIPSOMETRY” and the following points are discussed in more detail: Established classification for mechanical properties, Complementary classification for optical properties, Ellipsometry for determination of optical constants n-k plane as material fingerprint, Samples, participants & set-ups (samples: Japan, participants: Japan, Germany, France, set-ups: Japan, Germany, USA) and Results of interlaboratory comparison: thickness, n & k. T2 - ISO TC 107 Meeting Tokyo CY - Tokio, Japan DA - 17.01 2017 KW - Interlaboratory Comparison KW - Optical Property KW - Carbon-based Films KW - Ellipsometry PY - 2017 AN - OPUS4-39028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paul, Andrea A1 - Meyer, Klas A1 - Ruiken, Jan-Paul A1 - Illner, M. A1 - Müller, D.-N. A1 - Esche, E. A1 - Wozny, G. A1 - Westad, Frank A1 - Maiwald, Michael T1 - Process spectroscopy in microemulsions — Raman spectroscopy for online monitoring of a homogeneous hydroformylation process N2 - A major industrial reaction based on homogeneous catalysis is hydroformylation for the production of aldehydes from alkenes and syngas. Hydroformylation in microemulsions, which is currently under investigation at Technische Universität Berlin on a mini-plant scale, was identified as a cost efficient approach which also enhances product selectivity. Herein, we present the application of online Raman spectroscopy on the reaction of 1-dodecene to 1-tridecanal within a microemulsion. To achieve a good representation of the operation range in the mini-plant with regard to concentrations of the reactants a design of experiments was used. Based on initial Raman spectra partial least squares regression (PLSR) models were calibrated for the prediction of 1-dodecene and 1-tridecanal. Limits of predictions arise from nonlinear correlations between Raman intensity and mass fractions of compounds in the microemulsion system. Furthermore, the prediction power of PLSR models becomes limited due to unexpected by-product formation. Application of the lab-scale derived calibration spectra and PLSR models on online spectra from a mini-plant operation yielded promising estimations of 1-tridecanal and acceptable predictions of 1-dodecene mass fractions suggesting Raman spectroscopy as a suitable technique for process analytics in microemulsions. KW - Raman KW - Online KW - Chemometrics KW - Hydroformylation KW - Mini-plant KW - Microemulsion PY - 2017 DO - https://doi.org/10.1088/1361-6501/aa54f0 SN - 1361-6501 SN - 0957-0233 VL - 28 IS - 3 SP - 035502-1 EP - 035502-11 PB - IOP Publishing Ltd CY - UK AN - OPUS4-39032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waiblinger, H. U. A1 - Brockmeyer, J. A1 - Bruenen-Nieweler, C. A1 - Busch, U. A1 - Haase, I. A1 - Hahn, A. A1 - Haarmann, M. A1 - Hauser, W. A1 - Huber, I. A1 - Jany, K. D. A1 - Kirmse, N. A1 - Lindeke, S. A1 - Neumann, K. A1 - Naumann, H. A1 - Paschke, A. A1 - Pietsch, K. A1 - Pöpping, B. A1 - Reiting, R. A1 - Schroeder, U. A1 - Schwägele, F. A1 - Weller, Michael G. A1 - Zagon, J. T1 - Methoden zur Differenzierung von Tierarten in Lebensmitteln – Status quo N2 - Nicht zuletzt bedingt durch den Pferdefleischskandal im Jahr 2013 wurden in Deutschland die Aktivitäten bei der Methodenstandardisierung im Bereich der Tierarten-Differenzierung in den vergangenen Jahren intensiviert. Wenn auch positive Befunde bei dem Nachweis von Bestandteilen aus Pferd in Lebensmitteln wie Lasagne derzeit so gut wie nicht mehr anzutreffen sind, so hat die Tierartendifferenzierung insgesamt beim Nachweis von Verfälschungen in Lebensmitteln einen hohen Stellenwert. Diese Arbeit fasst daher den aktuellen Stand der Analytik in Deutschland mit Schwerpunkt bei der Standardisierung zusammen. Sie wurde erstellt durch die Arbeitsgruppe „Biochemische und molekularbiologische Analytik“ der Lebensmittelchemischen Gesellschaft mit Unterstützung von Experten der Arbeitsgruppe „Molekularbiologische Methoden zur Pflanzen- und Tierartendifferenzierung“ (§ 64 LFGB) sowie der ALTS-Arbeitsgruppe „Immunologie und Molekularbiologie“ (jeweils D). KW - ELISA KW - PCR KW - Multiplex KW - DNA-Chip KW - Fischarten KW - Standardisierung KW - Molekularbiologie KW - Immunoassay KW - Hybridisierung KW - Digitale PCR KW - LC-MS/MS KW - Massenspektrometrie KW - Schnellmethoden KW - Screening KW - Milch KW - Microarray KW - LAMP KW - Laborvergleichuntersuchungen KW - Referenzmaterialien KW - Standardverfahren PY - 2017 SN - 0015-363X IS - 1 SP - 97 EP - 102 PB - Deutscher Fachverlag GmbH CY - Frankfurt AN - OPUS4-39038 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Measurement and calculation of multimodal material VSSA N2 - In order to ground the debate on the metrics that apply for VSSA determined by adsorption isotherms and to illustrate the consequences of real bimodality for VSSA screening, a bimodal mixture has been selected for systematic investigations. A sample of BaSO4 fine was spiked with 10% g/g of BaSO4 ultrafine. The ultrafine grade is a clear nanomaterial (NM) according to the size criterion with a median Feretmin of 27 nm and the fine grade is clearly a non-NM with a median Feretmin of 249 nm. Because of the number ratio of 300:1, the mixture has to be a NM according to the size criterion. Three independent BET measurements were performed on the mixture by two different labs and resulted in a mean VSSA of 23 m2/cm3 with a standard deviation of 3.3 m2/cm3, which leads to a dminVSSA of 258 nm, and, therefore, would falsely classify the material as a non-NM. This effect was predicted earlier by calculated examples (Roebben et al. 2014) and demonstrates that mixtures of nano- and non-nano multimodal materials very likely lead to false negative classifications. Moreover, the measured VSSA values for the mixture of 23 m²/cm³ are in excellent accord with the value of 24.6 m²/cm³ predicted from the TEM size distributions of the individual materials according to the model described by JRC (Roebben et al. 2014), but are significantly different from the prediction of 309 m²/cm³ obtained from the same TEM size distribution by a particle number weighted approach (Lecloux 2015). The same is true for a 50% g/g mixture. We conclude that the mass-based VSSA approach (Roebben et al. 2014) is equal to the VSSA that is measurable by adsorption isotherms, such as from standardized BET. T2 - NANoREG Technical Meeting on VSSA discussion CY - Schiphol, The Netherlands DA - 26.09.2016 KW - VSSA KW - Nanomaterial KW - Electron microscopy KW - Particle size distribution PY - 2016 AN - OPUS4-38914 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Babick, F. A1 - Mielke, Johannes A1 - Hodoroaba, Vasile-Dan A1 - Weigel, St. A1 - Wohlleben, W. T1 - Critical review manuscript with real-world performance data for counting, ensemble and separating methods including in-build mathematical conversion to number distributions submitted for publication N2 - The content of the paper is the assessment of the performance of (conventional) measurement techniques (MTs)with respect to the classification of disperse materials according to the EC recommendation for a definition of nanomaterial. This performance essentially refers to the accurate assessment of the number weighted median of (the constituent) particles. All data and conclusions are based on the analytical study conducted as real-world performance testing. It comprised different types of MTs (imaging, counting, fractionating, spectroscopic and integral) as well as different types of materials. Beside reference materials with well-defined size distribution the study also included several commercial powders (variation of particle composition, morphology, coating, size range and polydispersity). In order to ensure comparability of measurement results, the participants were guided to use uniform protocols in sample preparation, conducting measurements, data analysis and in reporting results. Corresponding documents have been made public, in order to support the reviewing process of the paper, respectively to ensure the reproducibility of data by other users under the same conditions. The scientific paper relies on a comprehensive set of revised measurement data reported in uniform templates, completely describes the experimental procedures and discusses the MTs’ performance for selected materials in detail. Even more, the study is summarised and evaluated, which leads to recommendations for the use of MTs within a tiered approach of NM characterisation. In addition, the paper critically examines the factors that may affect the outcome of such a comparison among different MTs. KW - Nanomaterial KW - Measurement techniques KW - EC definition of nanomaterial KW - Nanoparticles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-389646 UR - http://www.nanodefine.eu/index.php/downloads/nanodefine-technical-reports UR - http://www.nanodefine.eu/publications/reports/NanoDefine_TechnicalReport_D3.3.pdf SP - D3.3, 1 EP - 72 PB - The NanoDefine Consortium CY - Wageningen, The Netherlands AN - OPUS4-38964 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana T1 - Process monitoring of an intensified continuous production unit with compact NMR spectroscopy N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and inexpensive analysers, which feature advantages like low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. Otherwise there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Union’s Research Project CONSENS by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. The presented NMR module is provided in an explosion proof housing with a module size of 57 x 57 x 85 cm and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling (IHM) was selected for data analysis of the low-field NMR spectra. A set-up for monitoring continuous reactions in a thermostated 1/8” tubular reactor using automated syringe pumps was used to validate the IHM models by using high-field NMR spectroscopy as analytical reference method. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 19.01.2017 KW - Online NMR spectroscopy PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-390117 AN - OPUS4-39011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online spectroscopy in micellar systems – A process analytical approach for a hydroformylation mini-plant N2 - Within the Collaborative Research Center InPROMPT a novel process concept for the hydroformylation of long-chained olefins is studied in a mini-plant, using a rhodium complex as catalyst in the presence of syngas. Recently, the hydroformylation in micro¬emulsions, which allows for the efficient recycling of the expensive rhodium catalyst, was found to be feasible. However, the high sensitivity of this multi-phase system with regard to changes in temperature and composition demands a continuous observation of the reaction to achieve a reliable and economic plant operation. For that purpose, we tested the potential of both online NMR and Raman spectroscopy for process control. The lab-scale experiments were supported by off-line GC-analysis as a reference method. A fiber optic coupled probe of a process Raman spectrometer was directly integrated into the reactor. 25 mixtures with varying concentrations of olefin (1-dodecene), product (n-tridecanal), water, n-dodecane, and technical surfactant (Marlipal 24/70) were prepared according to a D-optimal design. Online NMR spectroscopy was implemented by using a flow probe equipped with 1/16” PFA tubing serving as a flow cell. This was hyphenated to the reactor within a thermostated bypass to maintain process conditions in the transfer lines. Partial least squares regression (PLSR) models were established based on the initial spectra after activation of the reaction with syngas for the prediction of unknown concentrations of 1-dodecene and n-tridecanal over the course of the reaction in the lab-scale system. The obtained Raman spectra do not only contain information on the chemical composition but are further affected by the emulsion properties of the mixtures, which depend on the phase state and the type of micelles. Based on the spectral signature of both Raman and NMR spectra, it could be deduced that especially in reaction mixtures with high 1-dodecene content the formation of isomers as a competitive reaction was dominating. Similar trends were also observed during some of the process runs in the mini-plant. The multivariate calibration allowed for the estimation of reactants and products of the hydroformylation reaction in both laboratory setup and mini-plant. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 19.01.2017 KW - Online reaction monitoring PY - 2017 AN - OPUS4-39012 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Simon, Franz-Georg T1 - PEREBAR - Long-Term Performance of Permeable Reactive Barriers Used for the Remediation of Contaminated Groundwater N2 - Contaminated land, landfills and sediments pose a serious environmental threat by polluting groundwater in the surrounding area. In 14 European countries contamination caused by uranium represents a particularly serious danger where drinking water resources might be affected. Other heavy metals and organic pollutants can also have a strongly deleterious effect on groundwater. Available technologies (e.g. pump- and-treat) fall short of solving the problem because their performance is not yet adequate for effective remediation. The aim of the project is to elaborate the scientific basis for laboratory and pilot-scale testing of and the practical application of a considerably more efficient and cost-effective in-situ reactive barrier technology targeting the above contaminants. The primary model test site will be an area in Southern Hungary contaminated by uranium mining- thus including a region which is due to become part of the European Union. The approach taken to meet the project objectives was the characterisation of different reactive materials and relevant attenuation processes in the reactive matrix of the permeable barrier with special respect to their long-term behaviour. The experimental work included laboratory experiments at different scales, going from bench-scale tests up to pilot-scale, and field-scale experiments. Experimental conditions were predetermined by the characteristics of the model site, such as geologic and hydrogeological settings, soil composition, and type, extent and spreading of the contamination. Technological methods to enhance the long-term efficacy and cost-effectiveness of permeable reactive barrier systems were developed and tested under realistic conditions. KW - Ground water pollution KW - Contaminated sites KW - Environmental pollution KW - Permeable reactive barrier systems PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-390231 UR - http://www.eugris.info/displayproject.asp?Projectid=4290 SP - 1 EP - 9 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Heinrich, Thomas T1 - Switchable Surfaces: Mono- and Multilayers of Stimuli-Responsive Supramolecules on Solid Supports N2 - Rotaxanes are mechanically interlocked molecules (MIMs) that are considered to be excellent prototypes for the development of molecular machines. They comprise a discrete number of molecules that are bound to each other via non-covalent interactions. Mechanically interlocked means that a covalent bond must be broken in order to separate the molecules from another. If the rotaxanes are furthermore provided with different binding sites, they can perform a con-formational change and thus a nanoscopic movement by the application of an external stimu-lus. However, this movement is not directed in solution and a macroscopic effect is therefore, if at all, very difficult to realize. The integration of rotaxanes into a reference system by, for example, the immobilization on a surface is regarded as a promising approach to convert the generated nanoscopic motion into a macroscopic effect. The present work describes the immobilization of chloride-switchable rotaxanes onto surfaces using a variety of methods. In detail, the applied methods are the metal-mediated layer-by-layer (LbL) self-assembly and the covalent deposition using click chemistry, which can be con-sidered as separate approaches. Before the rotaxanes were immobilized, the deposition meth-ods were first established and gradually improved on the basis of earlier results by using dif-ferent macrocycle and guest molecules. Various template layers – so-called self-assembled monolayers (SAMs) – were used. These are terminated with pyridine or terpyridine for the metal-induced LbL deposition. Azide-terminated SAMs are used for the covalent deposition. In the course of that, the following objectives were achieved: The deposition of diterpyridin functionalized macrocycles in multilayers with a preferential orientation was investigated and verified by transmission-UV/Vis, X-ray photoelectron spectroscopy (XPS) as well as near edge X-ray absorption fine structure (NEXAFS). In order to produce the multilayer, metal-ions and macrocycles were alternately deposited onto various SAMs. To enable further process control for the LbL deposition, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) has been extended by use of Principal Component Analysis (PCA) which is capable of analyzing even very small changes in the deposition procedure. By using two different macrocycles and four metals, a mixed multilayer was fabricated that can be programmed by its deposition sequence. The treatment of the multilayers with appropriate guest molecules showed that they are on one hand addressable to the lowest layer by an external stimulus and that they are on the other hand able to incorporate a relatively large amount of the guest. Additionally, the covalently deposited supramolecules are also able to bind guests and to adapt to their structures. In both cases, the reversibility could be shown by appropriate experiments. Finally, the introduction of pyridine-functionalized nanoparticles into the multilayers led to a higher guest uptake, which can be explained by the reduction of the macrocycle-order due to the uneven surface of the nanoparticles. KW - Layer-by-layer deposition KW - XPS KW - NEXAFS KW - ToF SIMS KW - Switchable rotaxane PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:188-fudissthesis000000103658-0 SP - 1 EP - 139 PB - Freie Unversität CY - Berlin AN - OPUS4-39614 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Traulsen, Christoph T1 - Programmierbare supramolekulare (Komposit-)Multischichten auf Gold- und Siliziumoberflächen N2 - The present doctoral thesis focuses on the deposition of programmable supramolecular multilayers and composite-multilayers on gold and silicon substrates using a layer-by-layer selfassembly approach which is based on coordination chemistry. For this purpose, a variety of pyridine- and terpyridine-terminated self-assembled monolayers has been developed and deposited on gold and silicon substrates. Multitechnique analysis was carried out using X-ray photoelectron spectroscopy (XPS), (angle-dependent) near-edge Xray-absorption fine-structure spectroscopy (NEXAFS spectroscopy), time-of-flight secondaryion mass spectrometry (ToF-SIMS), transmissions UV/Vis spectroscopy as well as atomic force microscopy (AFM). By optimization of the deposition procedure, highly-ordered monomolecular and binary monolayers were deposited. As a proof of principle, transition metal-ions and appropriately labeled test-ligands were deposited on top of the functional monolayers. Furthermore, monolayers of terpyridine-terminated tetralactam macrocycles and the corresponding ether rotaxanes have been immobilized using coordination chemistry. In order to enhance the macrocycle surface coverage, the deposition procedure has been optimized as well. Multilayers consisting of diterpyridine-terminated tetralactam macrocycles have been deposited using either Fe(II) or alternatingly Fe(II) and Ni(II) metal-ions. The surface analysis proved a regular layer growth and a remarkable orientation of the macrocycles within the layer stacks. The applicability of the deposition procedure was expanded to a programmable layer stack by implementing pyridine-terminated macrocycles. The monodentate ligands led to an additional coordination sphere and thus to the application of a different transition metal-ion. The macrocycles and metal-ions were programmed according to the deposition sequence applied. The corresponding layer stack exhibited a linear dichroism of the π*-resonance corresponding to a preferential orientation of the macrocycles. Furthermore, the concept was extended to the deposition of composite multilayers consisting of pyridine-functionalized macrocycles and gold-nanoparticles which were synthesized during this thesis as well. Finally, reversible on-surface host-guest complex formation N2 - Die vorliegende Dissertation befasst sich mit der Herstellung von programmierbaren, supramolekularen Multischichten und Komposit-Multischichten auf Gold- und Siliziumoberflächen durch Anwendung eines koordinationschemischen Schicht-auf-Schicht-Selbstorganisationsverfahrens und den damit verbundenen Synthesen, Beschichtungen und Analysen. Um dieses Ziel zu erreichen, wurde zunächst eine Vielzahl von pyridin- und terpyridinterminierten selbstorganisierten Monoschichten (SAM) hergestellt und auf Gold- und Siliziumoberflächen abgeschieden. Die Abscheideprozedur wurde optimiert wobei zur Analytik der Oberflächen Röntgenphotoelektronenspektroskopie (XPS), winkelabhängiger kantennaher Röntgenabsorptionsfeinstrukturspektroskopie (NEXAFS-Spektroskopie), Flugzeit-Sekundärionen-Massenspektrometrie (ToF-SIMS), Transmissions-UV/Vis-Spektroskopie sowie Rasterkraftmikroskopie (AFM) eingesetzt wurde. Es konnte gezeigt werden, dass sich hochgeordnete monomolekulare und gemischte Monoschichten erzeugen lassen. Die terminalen funktionellen Gruppen dieser SAMs konnten als Ligand zur Komplexbildung mit Übergangsmetallionen verwendet werden. Diese koordinative Haftschicht wurde zur Verknüpfung zunächst von Testliganden und später von terpyridin-terminierten Tetralactam-Makrozyklen (TLM) und darauf basierenden Etherrotaxanen verwendet. Hierbei wurden ebenfalls die Beschichtungsbedingungen optimiert, um einen vollständigen Bedeckungsgrad zu erreichen. Unter Verwendung dieser Bedingungen wurden anschließend Multischichten aus TLMs und Fe(II)-Ionen sowie alternierend Fe(II) und Ni(II) abgeschieden. Die Analyse der hergestellten Multischichten zeigte reproduzierbar ein regelmäßiges, kontrollierbares Wachstum und eine Vorzugsorientierung. Durch den Einsatz von pyridin- und terpyridin-terminierten TLMs mit variierenden Metallionen konnte gezeigt werden, dass es möglich ist, die Abfolge verschiedener Schichten der Multischicht gezielt festzulegen. Im weiteren Verlauf der Arbeit wurden pyridin-terminierte Goldnanopartikel hergestellt und in die Multischichten integriert, um so Komposit-Multischichten herzustellen. Letztlich konnte gezeigt werden, dass die erzeugten Multischichten genutzt werden können, um über nicht-kovalente Wechselwirkungen reversibel Gastmoleküle zu binden und freizusetzten. KW - Layer-by-layer deposition KW - XPS KW - NEXAFS KW - ToF SIMS KW - Progammable rotaxane stacks PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:188-fudissthesis000000096664-6 SP - 1 EP - 141 PB - Freie Universität CY - Berlin AN - OPUS4-39615 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madkour, Sherif T1 - Unveiling the heterogeneous structure of miscible polymer blend confined in ultrathin films via nanosized relaxation spectroscopy N2 - Advances in functional coatings, batteries, innovative organic electronics, and hybrid materials depend strongly on polymeric materials confined in thin films or adsorbed at surfaces. Subsequently, understanding the materials behavior under confinement and the deviations, from the bulk, that might arise is necessary for optimized technological applications. In the nanometer vicinity, solid interfaces and free surfaces could alter for instance entanglements, glassy dynamics (α-relaxation), and the thermal glass transition temperature (Tg), compared to the bulk behavior. Consequently, this could change macroscopic quantities of thin films like adhesion, wettability, friction, reactivity, and biocompatibility, which are topical problems for hybrid materials. In fact, despite the intense investigations on thin homopolymers films, little is known about polymer blend thin films and how blending affect glass dynamics and glass transition, under confinement. This work discusses the glassy dynamics of thin films of Poly (vinyl methyl ether) (PVME) with special focus to the dynamics near the interfaces. Further, PVME is then blended with the well-studied polystyrene (PS) in two concentrations; 50:50 and 25:75 wt-%, which are miscible in bulk. The glass dynamics of thin films of both blend concentration are then investigated. Here, a combination of nanosized relaxation spectroscopies; broadband dielectric spectroscopy (BDS) and specific heat spectroscopy (SHS); employing AC nanochip calorimetry, was utilized to probe the glassy dynamics of the thin films, thickness: 7nm – 200 nm. It should be noted that both methods are sensitive to different probes; where SHS senses entropy fluctuations while BDS measures dipole fluctuations. For BDS measurements, a recently developed nano-structured electrode sample arrangement was employed; where ultra-thin films are spin-coated on an ultra-flat highly conductive silicon wafer, sandwiched between a wafer with nanostructured SiO2 nano-spacers with heights between 35 nm and 70 nm. Furthermore, these measurements are then combined with surface analytical techniques; ellipsometry and AFM, for controlled film thickness and topography. Probing of PVME thin films revealed the existence of an adsorbed layer with a restricted mobility at the polymer/substrate interface, which is independent from the bulk-like behavior and thickness independent. As for PVME/PS thin films, it was shown that the overall segmental dynamics of both blends are strongly affected by a fine counter-balance between a free surface layer at the polymer/air interface, which is PVME-rich layer, and an adsorbed layer at the polymer/substrate interface, which is PS-rich. This is the first example where confinement induced changes were observed by BDS for ultra-thin films. All results were analyzed in details and will be comprehensively discussed. T2 - Seminar at University of Pennsylvania CY - Philadelphia, USA DA - 21.03.2017 KW - Ultra-thin polymer films PY - 2017 AN - OPUS4-39621 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - SETNanoMetro advances: Fabrication and measurement of TiO2 engineered nanoparticles N2 - The press conference on the results of the European Project FP7 constitutes a dissemination event dedicated to the production and characterization of "Shape-engineered TiO2 nanoparticles for metrology of functional properties: setting design rules from material synthesis to nanostructured devices" with the main large-scale applications in the three reference sectors: energy, health and environment. T2 - Press conference on the results of the European Project FP7 CY - Istituto Nazionale di Ricerca Metrologica (INRiM), Torino, Italy DA - 31.03.2017 KW - TiO2 KW - Nanoparticles KW - Measurement KW - Metrology KW - Shape-enegineered nanoparticles PY - 2017 AN - OPUS4-39622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Asadujjaman, Asad A1 - Bertin, Annabelle A1 - Schönhals, Andreas T1 - Dielectric analysis of the upper critical solution temperature behaviour of a poly(acrylamide-coacrylonitrile) copolymer system in water N2 - A copolymer consisting of acrylamide (AAm) and acrylonitrile (AN) in aqueous solution was investigated using broadband dielectric spectroscopy at frequencies between 10⁻¹ Hz and 10⁶ Hz in the temperature range from 2 °C to 60 °C. This system shows an UCST phase behavior. The phase transition and aggregation behavior is monitored by both the temperature and frequency dependence of the complex conductivity σ*(f, T), where the AN fraction and the concentration of the solution were varied. Additionally, the dielectric data are compared with the results obtained from dynamic light scattering measurements. The temperature dependence of the DC conductivity (σDC) of the copolymer solution is monitored and the phase transition temperature (PTT) of the poly(AAm-co-AN) copolymer is deduced from a change in the T-dependence of the DC conductivity. The change in σDC can be explained by decreased effective charge carrier mobility and a reduction of the effective charge number density at temperatures below the phase Transition temperature of the poly(AAm-co-AN) solution. A pronounced interfacial polarization effect on the frequency dependence of the real part of the conductivity (σ') is observed at temperatures below the phase Transition temperature. The charge carriers are blocked at the formed aggregates giving rise to this interfacial polarization. The dependence of the interfacial polarization on the acrylonitrile fraction in the copolymer and the concentration of the solution is studied in detail and conclusions concerning the internal structures of the copolymer aggregates are drawn. KW - Thermoresponsive polymres PY - 2017 DO - https://doi.org/10.1039/c6sm02684b SN - 1744-6848 SN - 1744-683X VL - 13 IS - 12 SP - 2384 EP - 2393 PB - Royl Society of Chemistry Publishing AN - OPUS4-39556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias A1 - Stegemann, Robert T1 - GMR Sensor Arrays for High-Spatial Resolution Measurements in NDT-Applications N2 - Magneto resistive (MR) sensors are suited for a wide range of different applications. Especially due to their small sizes and their frequency-independent behaviour, they are eligible candidates for non-destructive testing methods where high spatial resolution is required. The use of specialized magnetic field probes enables not only a defect evaluation, but also a localized characterization of ferromagnetic materials. This paper presents some NDT (non-destructive testing) examples concerning magnetic flux leakage applications (MFL) and eddy current testing (ET). For MFL-testing we used an NDT-adapted GMR (Giant MR) sensor array for the detection of small inclusions in thin steel sheets. We also investigated the effects of microstructure on magnetic properties using GMR sensors. The ET-example describes an MR array probe consisting of 32 MR-elements, an ASIC, subsequent readout components and a one-wire excitation to generate eddy currents inside the material (developed in the EU-funded IMAGIC-project, 2011-2014, 7th Framework Programme). Using this MR-probe we achieved results with a better spatial resolved defect detection of neighbouring boreholes compared to “conventional” ET-probes. T2 - 14th Symposium Magnetoresistive Sensors and Magnetic Systems CY - Wetzlar, Germany DA - 21.03.2017 KW - GMR KW - Eddy current testing KW - Magnetic flux leakage PY - 2017 SP - 146 EP - 153 AN - OPUS4-39557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Schick, Ch. A1 - Schönhals, Andreas T1 - Unexpected behavior of ultra-thin films of blends of polystyrene/poly(vinyl methyl ether) studied by specific heat spectroscopy N2 - Specific heat spectroscopy (SHS) employing AC nanochip calorimetry was used to investigate the glassy dynamics of ultra-thin films (thicknesses: 10 nm–340 nm) of a polymer blend, which is miscible in the bulk. In detail, a Poly(vinyl methyl ether) (PVME)/Polystyrene (PS) blend with the composition of 25/75 wt. % was studied. The film thickness was controlled by ellipsometry while the film topography was checked by atomic force microscopy. The results are discussed in the framework of the balance between an adsorbed and a free surface layer on the glassy dynamics. By a self-assembling process, a layer with a reduced mobility is irreversibly adsorbed at the polymer/substrate interface. This layer is discussed employing two different scenarios. In the first approach, it is assumed that a PS-rich layer is adsorbed at the substrate. Whereas in the second approach, a PVME-rich layer is suggested to be formed at the SiO2 substrate. Further, due to the lower surface tension of PVME, with respect to air, a nanometer thick PVME-rich surface layer, with higher molecular mobility, is formed at the polymer/air interface. By measuring the glassy dynamics of the thin films of PVME/PS in dependence on the film thickness, it was shown that down to 30 nm thicknesses, the dynamic Tg of the whole film was strongly influenced by the adsorbed layer yielding a systematic increase in the dynamic Tg with decreasing the film thickness. However, at a thickness of ca. 30 nm, the influence of the mobile surface layer becomes more pronounced. This results in a systematic decrease in Tg with the further decrease of the film thickness, below 30 nm. These results were discussed with respect to thin films of PVME/PS blend with a composition of 50/50 wt.%as well as literature results. KW - Ultra thin polymer films PY - 2017 DO - https://doi.org/10.1063/1.4978505 SN - 0021-9606 SN - 1089-7690 VL - 146 IS - 20 SP - 203321-1 EP - 203321-9 PB - AIP Publishing AN - OPUS4-39558 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - GMR Sensor Arrays for High-Spatial Resolution Measurements in NDT-Applications N2 - Magneto resistive (MR) sensors are suited for a wide range of different applications. Especially due to their small sizes and their frequency-independent behaviour, they are eligible candidates for non-destructive testing methods where high spatial resolution is required. The use of specialized magnetic field probes enables not only a defect evaluation, but also a localized characterization of ferromagnetic materials. This paper presents some NDT (non-destructive testing) examples concerning magnetic flux leakage applications (MFL) and eddy current testing (ET). For MFL-testing we used an NDT-adapted GMR (Giant MR) sensor array for the detection of small inclusions in thin steel sheets. We also investigated the effects of microstructure on magnetic properties using GMR sensors. The ET-example describes an MR array probe consisting of 32 MR-elements, an ASIC, subsequent readout components and a one-wire excitation to generate eddy currents inside the material (developed in the EU-funded IMAGIC-project , 2011-2014, 7th Framework Programme). Using this MR-probe we achieved results with a better spatial resolved defect detection of neighbouring boreholes compared to “conventional” ET-probes. T2 - 14th Symposium Magnetoresistive Sensors and Magnetic Systems CY - Wetzlar, Germany DA - 21.03.2017 KW - GMR KW - Eddy current testing KW - Magnetic flux leakage PY - 2017 AN - OPUS4-39560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Ehlert, Christopher T1 - Simulationen von Röntgenabsorptionsprozessen zur Charakterisierung von Systemen in kondensierter Phase N2 - Diese Doktorarbeit ist das Resultat einer intensiven und fruchtbaren Zusammenarbeit zwischen dem Fachbereich 6.1 (Oberflächenanalytik und Grenzflächenchemie) der Bundesanstalt für Materialforschung und -prüfung (BAM) sowie der Arbeitsgruppe Theoretische Chemie von Professor Saalfrank an der Universität Potsdam. Zusammen haben wir die Strukturaufklärung von Systemen in kondensierter Phase unter Verwendung der Röntgenabsorptionsspektroskopie betrieben. Von Seiten der BAM wurden experimentelle Röntgenabsorptionsspektren hoher Auflösung an modernen Synchrotroneinrichtungen (BESSY II, Berlin) aufgenommen. Die Theoretische Chemie liefert, unter Verwendung quantenchemischer Methoden, die Möglichkeit die Spektren zu simulieren. Bei der Röntgenabsorption wird ein Photon hoher Energie von einem molekularen System absorbiert und in einen angeregten Zustand versetzt. Die Intensität der Absorption ist stark abhängig von der eingestrahlten Photonenenergie. Das resultierende Absorptionsspektrum enthält eine Vielzahl von Informationen. Meine Aufgabe bestand darin, die untersuchten Systeme am Computer zu modellieren. KW - XPS KW - NEXAFS KW - Spektrensimulation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:517-opus4-104844 SP - 1 EP - 142 PB - Universität Potsdam CY - Potsdam AN - OPUS4-39562 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Asadujjaman, Asad T1 - Functional polymer based on 2,6-diaminopyridine with tunable UCST behaviour in water/alcohol mixture N2 - Thermoresponsive polymers are of great importance in numerous applications such as bioseparation, drug delivery, diagnostic and microfluidic applications.[1-2] Only a few thermoresponsive polymers have been reported that present an Upper Critical Solution Temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range and “green” solvents such as water or ethanol.[3] Indeed, polymers with UCST behavior below 60°C in alcohol or water/alcohol mixtures are extremely promising for the preparation of “smart” materials for sensing. In this work, two novel functional polymers of based on a 2,6-diaminopyridine motif were synthesized by free-radical polymerization. Their UCST-type transition temperature is tunable by varying either their concentration in solution or the type of solvent. Insights into this phenomenon are investigated using turbidimetry and temperature dependent dynamic light scattering. T2 - Konferenz CY - Lisbon, Portugal DA - 06.03.2017 KW - Thermoresponsive polymers KW - UCST-type polymers PY - 2017 AN - OPUS4-39579 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madkour, Sherif T1 - Unveiling the Dynamics of Self-Assembled Layers of Thin Films of PVME by Nanosized Relaxation Spectroscopy N2 - In thin polymer films, little is known about the dynamics of the adsorbed layers, despite their importance in innovative applications. Here, Broadband Dielectric Spectroscopy (BDS) was utilized to investigate the glassy dynamics of thin films of a low MW Poly (vinyl methyl ether) (PVME) (thicknesses: 7 – 160 nm). A recently developed nano-structured capacitor arrangement was employed; where a silicon wafer with nanostructured SiO2 nano-spacers, with heights of 35 nm and 70 nm, is placed on top of a thin film spin coated on an ultra-flat highly conductive silicon wafer. Further, PVME/SiO2 interactions was confirmed by contact angle measurements, hence an adsorbed layer is allowed to form. For films with thicknesses smaller than 50 nm, BDS measurements showed two relaxation processes. The first process coincided, in its position and temperature dependence, with the -relaxation of bulk PVME, thus it was assigned to the -relaxation of a bulk-like layer. The second process showed a different temperature dependence and was ascribed to the relaxation of polymer segments adsorbed at the substrate. Both processes showed no thickness dependence. The results will be discussed in detail. To our knowledge, this is the first study of the segmental dynamics of an adsorbed layer in thin films. T2 - Marchmetting American Physical Society CY - New Orleans, USA DA - 13.03.2017 KW - Ultra thin polymer films PY - 2017 AN - OPUS4-39592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - How far does the light shine? A check-up of quantitative high and low field NMR spectroscopy N2 - The Royal Society of Chemistry NMR Discussion Group and Molecular Spectroscopy Group would like to invite you to the 2017 Spring Meeting, which will be held at GlaxoSmithKline (GSK), Stevenage. The theme for the meeting is “Low level detection and quantification by NMR” and different NMR technologies, including solution state NMR, solid state NMR and benchtop/low field NMR will be discussed. The presentations will cover a range of NMR related disciplines, including conventional low level detection and quantification, the use of cryoprobes, quantification of polymorphism using ssNMR and also methods for spectral simplification. Recent developments and applications of hyperpolarisation techniques, within both solution state and solid state NMR, will be presented in conjunction with the effect these sensitivity enhancements have with respect to quantification and limits of detection. T2 - NMR Discussion Group and Molecular Spectroscopy Group Spring Meeting: "Low Level Detection and Quantification by NMR Spectroscopy" CY - Stevenage, UK DA - 29.03.2017 KW - Online NMR Spectroscopy KW - Quantitative NMR Spectroscopy KW - qNMR KW - Indirect Hard Modeling KW - Limit of Detection KW - NMR Spectroscopy KW - Metrology PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-395936 AN - OPUS4-39593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Szczerba, Wojciech A1 - Costo, R. A1 - Veintemillas-Verdaguer, S. A1 - del Puerto Morales, M. A1 - Thünemann, Andreas T1 - SAXS analysis of single- and multi-core iron oxide magnetic nanoparticles N2 - This article reports on the characterization of four superparamagnetic iron oxide nanoparticles stabilized with dimercaptosuccinic acid, which are suitable candidates for reference materials for magnetic properties. Particles p1 and p2 are single-core particles, while p3 and p4 are multi-core particles. Small-angle X-ray scattering analysis reveals a lognormal type of size distribution for the iron oxide cores of the particles. Their mean radii are 6.9 nm (p1), 10.6 nm (p2), 5.5 nm (p3) and 4.1 nm (p4), with narrow relative distribution widths of 0.08, 0.13, 0.08 and 0.12. The cores are arranged as a clustered network in the form of dense mass fractals with a fractal dimension of 2.9 in the multi-core particles p3 and p4, but the cores are well separated from each other by a protecting organic shell. The radii of gyration of the mass fractals are 48 and 44 nm, and each network contains 117 and 186 primary particles, respectively. The radius distributions of the primary particle were confirmed with transmission electron microscopy. All particles contain purely maghemite, as shown by X-ray absorption fine structure spectroscopy KW - Superparamagnetic nanoparticles KW - Iron oxide KW - Reference materials KW - SAXS KW - Small-angle x-ray scattering KW - XANES KW - X-ray absorption near-edge structure KW - X-ray absorption fine structure PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-395948 DO - https://doi.org/10.1107/S1600576717002370 SN - 1600-5767 VL - 50 IS - Part 2 SP - 481 EP - 488 PB - (IUCr) International Union of Crystallography AN - OPUS4-39594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sturm, Heinz T1 - Improving polymer matrix additives for composite structures: a focus on boehmite N2 - The aims of the Research Unit „Acting Principles of Nano-Scaled Matrix Additives for Composite Structures“ (DFG FOR 2021) are based on different synergetic pathways. Challenges are to achieve an improved damage tolerance combined with unchanged processability and a proof of the nano-based effect from molecular scale up to structural level. First of all, a comprehensive understanding of the acting mechanisms of nano-scaled ceramic additives onto polymer matrices of continuous fibre reinforced polymer composites with respect to improved matrix dominated properties is in focus. To proof of the nanoscopic and microscopic effects up to structural level; experimental investigations start on the functional correlation between the particle properties and the resulting properties of the epoxy as suspension and in the solid state. This includes tests for the resulting composite structures as well. Along the entire process chain different multi-scale simulations are performed from molecular modelling up to the macroscopic, structural level. The combination of experimental investigations and simulation methods enables a holistic understanding of the acting principles and basic mechanisms. Specialized techniques based on Scanning Force Microscopy are the basis of our analysis of physicochemical properties of the boehmite nanoparticles and their polymer environment. A surface map of mechanical properties as an input for simulations facilitate a deeper understanding of such composites across all scales. This enables us to understand the macroscopic structure-property relationship and to predict failure mechanisms as well as routes for optimization. T2 - 92nd DKG annual meeting and symposium on high performance ceramics CY - Berlin, Germany DA - 19.03.2017 KW - Boehmite nanoparticle KW - Intermodulation AFM KW - Composite structures KW - Pull-out test KW - Thermoset KW - Crack propagation energy PY - 2017 AN - OPUS4-39519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramos, Inês I. A1 - Carl, Peter A1 - Schneider, Rudolf A1 - Segundo, Marcela A. T1 - Development of automated immunosensing methods for clinical and environmental Analysis using lab-on-valve platforms N2 - The lab-on-valve (LOV) is a mesofluidic platform that has been recently exploited for the automation and miniaturization of bioanalytical assays, resorting namely to molecular recognition schemes based on immunosensing. Due to its high versatility for reagent accommodation, it is possible to establish immunoassays under several formats (eg. direct competitive ELISA, sandwich ELISA or even label-free immunoaffinity chromatography). For instance, the LOV has been used as a manifold for UV-vis micro-Bead Injection Spectroscopy (μ-BIS), a technique that involves the quantification of the target analyte by direct measurement on the surface of a solid phase capable of retaining the target analyte by molecular recognition. The μ-BIS-LOV strategy affords several analytical advantages, namely short time-toresult intervals (3 to 15 min), low sample volume (1-20 μL), automated solution handling and washing steps, downscaling of reagents’ consumption, low-cost analysis and little generation of waste. Additionally, the solid support is renewed before each determination, minimizing surface fouling, cross-contamination issues and functional group deactivation. No sample clean-up steps are required because interferences are separated from the target analyte upon quantification mediated by a molecular recognition element attached to the micro-bead column. The portability of the LOV device makes it compatible with point-of-care testing. To our knowledge, this technique has been mainly employed for the evaluation and optimization of bioaffinity processes, but its potential for clinical and environmental analysis remains underexploited. Hence, in this communication, different immunosensing strategies using the LOV platform will be addressed, namely the determination of autoimmune IgG in human serum, and the assessment of drug (carbamazepine) levels in wastewater samples. T2 - EBS 2017 CY - Potsdam, Germany DA - 20.03.2017 KW - Lab-on-valve KW - Automation KW - Immunoassay PY - 2017 AN - OPUS4-39521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Analysis of TiO2 nanoparticles – Various activities at BAM N2 - The presentation goes into the characterization of TiO2 engineered nanoparticles within EU/FP7 SETNanoMetro Project and the nanomaterial classification according to the EC definition tested within EU/FP7 NanoDefine Project. Further, ISO/TC 229/JWG 2 activities related on ISO standards in development and inter-laboratory comparisons on measurement of nanoparticle size and shape distribution by SEM and TEM are discussed. T2 - Seminar CY - PTB Braunschweig, Germany DA - 23.03.2017 KW - Nanoparticles KW - Electron microscopy KW - Nanomaterial KW - Standardization KW - Inter-laboratory comparison PY - 2017 AN - OPUS4-39527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Vorversuche zur Ultraschallprüfung an Groutverbindungen N2 - Im rahmen des themenfeldprojektes LEBEWIND wurden Vorversuche zur Ultraschallprüfung von Groutverbindungen an Offshore-Windenergieanlagen gemacht. Die Experimente mit kommerzieller Prüftechnik in Echo und Transmission durch die Stahlwandung hindurch bestätigten, dass diese Bauweise so nicht prüfbar ist. T2 - Workshop "Grout in der Betriebsphase" CY - Berlin, Germany DA - 22.03.2017 KW - Windenergieanlagen KW - Grout KW - Ultraschall PY - 2017 AN - OPUS4-39541 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Messunsicherheiten in Messungen und Oberflächencharakterisation: Ellipsometrie, Härte und Haftprüfung N2 - Die Angabe der Messunsicherheit wird im Rahmen von Konformitätsbewertungen gefordert. Die Messunsicherheit gibt an, wie sicher der wahre Wert der Messgröße getroffen wird. Für ihre Ermittlung gibt es unterschiedliche Ansätze, allen voran der „Guide to the Expression of Uncertainty in Measurement“ (GUM). In der geplanten Auditoren- und Bewerterschulung sollen in einem Übersichtsvortrag "Uncertainty Budgets in Measurement and Testing for Surface Characterization: Ellipsometry, Hardness and Adhesion Testing" Herangehensweisen und Methoden zur Ermittlung der Messunsicherheit vorgestellt und anschließend anhand beispielhafter Anwendungen aus den Arbeitsbereichen der BAM erklärend untersetzt werden. Mit dieser Schulung sollen die Auditoren und Bewerter der BAM befähigt werden, geltende Anforderungen zur Messunsicherheit handhaben und beurteilen zu können. T2 - Auditoren- und Bewerterschulung CY - BAM, Berlin, Germany DA - 05.04.2017 KW - GUM KW - Messunsicherheit KW - Oberflächencharakterisierung KW - Ellipsometrie, Härte,und Haftung KW - Härte KW - Haftung PY - 2017 AN - OPUS4-39767 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Air-coupled ultrasonics: theory N2 - This presentation is an overview of the basics of air-coupled ultrasonic testing. The emphasis is on transducers and wave propagation, illustrated by examples from non-destructive testing. T2 - Non-destructive testing of fiber reinforced polymers. Training course ultrasonics and active thermography CY - Berlin, Germany DA - 28.03.2017 KW - Air-coupled ultrasonic testing KW - Carbon-fiber-reinforced plastic KW - Transducer PY - 2017 AN - OPUS4-39768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas T1 - Sinn und Unsinn dichter Messraster bei Radaruntersuchungen von Betonbauteilen N2 - Schlaffe und vorgespannte Bewehrungen in Stahlbetonbauwerken lassen sich in einer Tiefe von etwa 30 – 35 cm gut mit dem Radarverfahren orten. In der Praxis zeigt sich aber häufig, daß der zeitliche Aufwand für eine Radarmessung stark variieren kann. Gründe dafür sind zum einen die Komplexität der Bewehrung im Betonbauteil, zum anderen aber auch die Unsicherheit des Anwenders bei der Durchführung der Radarmessung. Die Frage, ob die Bewehrung schon mit der Messung entlang einer einzelnen Messlinie gefunden werden kann, oder ob eine flächige Messung notwendig ist, kann häufig nicht schnell und einfach beantwortet werden. Bei flächigen Radarmessungen ist ein wesentlicher Punkt dabei die Frage, wie dicht das Messraster sein soll. In der Praxis stellt sich häufig im Nachhinein heraus, daß ein weniger dichtes Raster mit einem Messlinienabstand von 10 cm oder 20 cm statt eines dichteren Rasters von z. B. 5 cm Messlinienabstand keine merkliche Verschlechterung des Ergebnisses beim Orten der Bewehrung liefert. Der zeitliche Aufwand für eine Radarmessung kann sich deshalb bei einer aufgabenbezogenen Wahl des Messrasters im Vergleich zur ursprünglichen Messung um deutlich mehr als die Hälfte verringern. Seltener tritt in der Praxis der Fall auf, daß ein Messraster zu groß gewählt wurde. Anhand von Praxisbeispielen werden die Unterschiede von Radarergebnissen bei einer Variation von Messrastern gezeigt. Die Wahl eines aufgabenbezogenen Messrasters wird ebenso wie die Wahl einer geschickten Antennenpolarisation bei der Ortung vorgespannter Bewehrung betrachtet und der Einfluss der Antennenpolarisation auf den Aufwand der Radarmessung diskutiert. Abschließend wird ein kurzer Ausblick gegeben, was für ein Potential dichte Messraster trotzdem in der Forschung haben können. T2 - Fachtagung Bauwerksdiagnose 2014 der DGZfP CY - Berlin, Germany DA - 13.02.2014 KW - Radar KW - Zerstörungsfreie Prüfung KW - Stahlbeton PY - 2014 AN - OPUS4-39820 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas T1 - Ortung von Spanngliedern zum schadensfreien Bohren im Rahmen von Ertüchtigungsmaßnahmen N2 - Am Beispiel der Ertüchtigung einer Brücke in Bremen wird gezeigt, wie mit den zerstörungsfreien Prüfverfahren (ZfP) Radar- und Ultraschall die genau Lage vorgespannte Bewehrung gefunden bzw. bestätigt werden kann. Im Rahmen von Ertüchtigungsmaßnahmen an Spannbetonbrücken werden häufig Kernbohrungen durchgeführt, die die vorhandenen Spannbewehrungen nicht beschädigen dürfen. Es wird die Vorgehensweise beschrieben, wie mit ZfP ein wesentlicher Beitrag geleistet wird, das Risiko einer Beschädigung zu minimieren und somit eine bessere Planungssicherheit für die Ertüchtigungsmaßnahmen zu schaffen. Dabei werden auch die Grenzen der bei den Verfahren aufgezeigt. T2 - Fachtagung Bauwerksdiagnose 2012, Praktische Anwendungen Zerstörungsfreier Prüfungen und Zukunftsaufgaben CY - Berlin, Germany DA - 23.02.2012 KW - Radar KW - Zerstörungsfreie Prüfung KW - Stahlbeton KW - Ultraschall PY - 2012 AN - OPUS4-39821 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas T1 - Ortung von Spanngliedern zum schadensfreien Bohren im Rahmen von Ertüchtigungsmaßnahmen N2 - Am Beispiel der Ertüchtigung einer Brücke in Bremen wird gezeigt, wie mit den zerstörungsfreien Prüfverfahren (ZfP) Radar- und Ultraschall die genau Lage vorgespannte Bewehrung gefunden bzw. bestätigt werden kann. Im Rahmen von Ertüchtigungsmaßnahmen an Spannbetonbrücken werden häufig Kernbohrungen durchgeführt, die die vorhandenen Spannbewehrungen nicht beschädigen dürfen. Es wird die Vorgehensweise beschrieben, wie mit ZfP ein wesentlicher Beitrag geleistet wird, das Risiko einer Beschädigung zu minimieren und somit eine bessere Planungssicherheit für die Ertüchtigungsmaßnahmen zu schaffen. Dabei werden auch die Grenzen der beiden Verfahren aufgezeigt. T2 - Fachtagung Bauwerksdiagnose 2012 - Praktische Anwendungen zerstörungsfreier Prüfungen und Zukunftsaufgaben CY - Berlin, Germany DA - 23.02.2012 KW - Radar KW - Zerstörungsfreie Prüfung KW - Stahlbeton KW - Ultraschall PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-398225 SN - 978-3-940283-40-5 VL - 134 (Vortrag 11) SP - 1 EP - 7 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin, Germany AN - OPUS4-39822 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas T1 - Gleisbettschotteruntersuchung mit der Impulsradar Array - Technik N2 - Das ZfP Verfahren Impulsradar wird bei der Untersuchung des Schotterunterbaus von Schienen wegen unterstützend eingesetzt, um deren Struktur und Materialeigenschaften zu bestimmen. Eingesetzt werden kann dieses Verfahren sowohl für die Qualitätskontrolle beim Neubau von Schienenwegen als auch für die Bedarfsermittelung von Instandsetzungsarbeiten aufgrund von Schotterverunreinigungen. Kosten können eingespart werden durch eine Verlängerung der Reinigungszyklen und der Lebensdauer des Schotters. Ein Antennenarray für die Ermittlung der Ausbreitungsgeschwindigkeit wurde entwickelt und aufgebaut. Ergebnisse von Schottermessungen im Labor werden vorgestellt. T2 - Fachtagung Bauwerksdiagnose - Praktische Anwendungen Zerstörungsfreier Prüfungen und Zukunftsaufgaben CY - Berlin, Germany DA - 21.02.2008 KW - Radar KW - Zerstörungsfreie Prüfung PY - 2008 SN - 978-3-940283-08-5 VL - 112 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung CY - Berlin AN - OPUS4-39823 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas T1 - Entwicklung eines Radarantennenarrays zur Untersuchung des Untergrundes im Schottergleisbett N2 - Die Erarbeitung der Grundlagen für effiziente und bedarfsgerechte Instandsetzungsmaßnahmen an Schottergleisbetten ist das Ziel des Projektes „SafeRail“. Das Impulsradarverfahren wird als zerstörungsfreie Methode für die Zustandsbestimmung des Schotters verwendet, um entsprechend den hohen Anforderungen der Netzbetreiber Unterbrechungen des Schienenverkehrs weitgehend zu vermeiden. Für eine automatisierte Bewertung der Vermischung des Schotters mit dem Untergrund sowie des Abnutzungszustandes des Schotters wird ein Antennenarray entwickelt, das bezüglich seiner Messgeometrie optimiert wird. T2 - Fachtagung Bauwerksdiagnose 2006 - Praktische Anwendungen zerstörungsfreier Prüfungen und Zukunftsaufgaben CY - Berlin, Germany DA - 23.02.2006 KW - Radar KW - Zerstörungsfreie Prüfung PY - 2006 SN - 3-931381-71-4 VL - 100 SP - 1 EP - 6 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-39824 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas A1 - Maierhofer, Christiane T1 - Railway Ballast Fouling Inspection by Monitoring the GPR Propagation Velocity with a Multi-Offset Antenna Array N2 - In this paper, a new method for the investigation of the degradation of ballast railway track beds is proposed. An array of antennas is used for simultaneous acquisition of reflected radar impulses, which have been transmitted from different sending positions. This array setup allows an automated CMP-measurement, which enables a direct calibration of the ballast thickness. These multiple offset measurements using the array setup are well suited for fast railway inspections. The method offers the possibility to visualize the state of degradation of the ballast in a velocity spectrum. T2 - 11th International Conference on Ground Penetrating Radar, the Ohio State University CY - Columbus, Ohio, USA DA - 19.06.2006 KW - Radar KW - Non-destructive testing KW - Railroad PY - 2006 SP - 1 EP - 4 CY - Columbus, Ohio AN - OPUS4-39825 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas T1 - Multi-offset impulse radar for the inspection of railway ballast N2 - A multi-offset radar system will be presented that features the possibility to get quantitative information about the wave propagation velocity as a measure of the ballast quality. This goes beyond the regular application of conventional radar systems offering only qualitative structural information. The new approach provides a fast NDT method for the classification of ballast fouling. A main advantage of the multi-offset radar is that regular ballast digging for velocity evaluation can be avoided and travel time can be directly transformed into an equivalent depth by using the automatically evaluated velocity. The maintenance cost and interruption time can be significantly decreased by this method. The application of velocity evaluation method is common in geophysical applications but it is used for ballast inspection for the first time. T2 - 9th International Congress Railway Engineering CY - University of Westminster, London, UK DA - 20.06.2007 KW - Radar KW - Non-destructive testing KW - Railroad PY - 2007 SN - 0-947644-61-10 VL - 2007 SP - 1 EP - 7 AN - OPUS4-39826 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas T1 - GPR antenna array for the inspection of railway ballast N2 - A GPR antenna array was investigated for automated measurement of wave propagation velocity as a measure of the ballast quality. This goes beyond the regular application of conventional radar systems offering only qualitative structural information. The new approach provides a fast NDT method for the classification of ballast fouling. A main advantage of the multi-offset radar is that regular ballast digging for velocity evaluation can be avoided and travel time can be directly transformed into an equivalent depth by using the automatically evaluated velocity. Fast monitoring of ballast fouling condition can reduce maintenance cost significantly by supporting the works necessary for ballast cleaning and furthermore this method reduces interruption time for a better railway service. T2 - National Seminar & Exhibition on Non-Destructive Evaluation, NDE 2011 of the INDIAN SOCIETY FOR NONDESTRUCTIVE TESTING (ISNT) CY - Chennai, India DA - 08.12.2011 KW - Radar KW - Non-destructive testing KW - Railroad PY - 2011 AN - OPUS4-39811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kind, Thomas T1 - GPR Development and Applications in Germany N2 - The presentation was an invited talk for the final meeting of the Mara Nord Project. Projects purpose is to demonstrate the potential of GPR method use in road condition measurement and rehabilitation planning to the Nordic market. This will be achieved through cooperation between Finland, Sweden and Norway. The presentation gives an overview of road condition measurement and rehabilitation planning in Germany and several different kind of GPR applications in Germany. T2 - Ground Penetrating Radar in Road Monitoring and Evaluation Now and the Future - Seminar (Mara Nord Project) CY - Trondheim, Norway DA - 18.04.2012 KW - Radar KW - Road inspection KW - Non-destructive testing PY - 2012 AN - OPUS4-39816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kind, Thomas A1 - Wöstmann, Jens A1 - Feistkorn, Sascha A1 - Trela, Christiane ED - Meßinger, Jens T1 - Radar in der Baupraxis: Lokalisierung von zweilagig vorgespannter Bewehrung in Beton N2 - Die Ermittlung der genauen Bewehrungslage ist von großem Interesse bei der Instandsetzung und Ertüchtigung von Stahlbetonbauwerken. Denn nur wenn die Lage der für die Standsicherheit wichtigen Bewehrung bekannt ist, können Kernbohrungen oder Sägearbeiten schadensfrei durchgeführt werden. Das Bodenradar als zerstörungsfreie Methode ist wegen des einfachen Verfahrens der Antenne entlang einer Messspur für eine solche Aufgabenstellung sehr gut geeignet. Die Anwendung kann aber eingeschränkt werden, wenn die gesuchte Bewehrung zu tief liegt oder durch eine davor liegende Bewehrung abgeschattet wird. Bei der Ortung mehrlagiger Bewehrung ist es wichtig, einen mehrstufigen und effizienten Messplan zu erstellen, der den Aufwand auf einem vertretbaren Maß beschränkt und die Möglichkeit bietet, beim Erreichen der Verfahrensgrenzen rechtzeitig die Untersuchung abzubrechen. Am Beispiel einer Stahlbetonbrücke, die nachträglich mit externen Spanngliedern versehen wurde, wird das Vorgehen beim Orten von mehrlagiger Bewehrung gezeigt. T2 - Georadar - Erfahrungen und Perspektiven CY - Freiberg, Germany DA - 24.09.2009 KW - Radar KW - Zerstörungsfreie Prüfung KW - Stahlbeton PY - 2010 SN - 0947-1944 VL - I SP - 1 EP - 6 PB - Dt. Geophysikalische Ges. CY - Potsdam AN - OPUS4-39827 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geißler, Daniel T1 - Assessment of Particle-based Luminescent Reporters in Sandwich Immunoassays N2 - Immunoassays are an important field of in vitro diagnostics, as they allow for a fast and highly sensitive detection of many biologically and diagnostically relevant analytes such as proteins, hormones, and pharmaceuticals. Fluorescence immunoassays (FIA), where the antibodies and/or antigens are labeled with luminescent reporters, can be easily read out directly by measuring the intensity, decay time, or polarization of the emitted light. Moreover, FIA enable the simultaneous detection of different analytes within a single sample (multiplexing) and are particularly suited for point-of-care (POC) diagnostics and high throughput screening (HTS). The application of luminescent nanoparticles as reporters in FIA could further improve assay sensitivity, as several 100 to 1000 luminophores can be incorporated or attached to such nanoscale carriers, thereby amplifying their absorption and/or emission signals simply by increasing the number of dye molecules. Although dye-loaded polymeric and silica nanoparticles have been increasingly used as reporters in immunoassays, achievable signal amplification factors related to the use of particle reporters are still difficult to predict and quantify, which also hampers the comparability of different nanoscale reporters. To overcome this challenge, we performed a systematic comparison of spectroscopically and analytically well characterized particle labels in a homogeneous sandwich immunoassay format for the detection of the common inflammation biomarker C-reactive protein (CRP). Hereby, we studied the influence of particle parameters like size, surface chemistry, and dye loading concentration for different dye classes, i.e. organic dyes and metal ligand complexes, varying in their signal-relevant spectroscopic properties (molar absorption coefficients, photoluminescence quantum yields, Stokes shifts, and emission decay times), for different detection schemes (direct read-out vs. dye extraction). The emitters applied were chosen to be commercially available for a reasonable price, to absorb between 400 nm and 450 nm, and to emit in the visible region, as these parameters are accessible with most established microplate readers. Based upon our findings, we highlight the advantages and limitations of nanoscale reporters with respect to the choice of suitable particles, encoding dyes, and detection strategies, and compare the achievable sensitivities and dynamic ranges for our CRP model immunoassay. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Immunoassay KW - Nanoparticle KW - Luminescence PY - 2017 AN - OPUS4-39784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saravanan, S. A1 - Balamurugan, M. A1 - Lippitz, Andreas A1 - Fonda, E. A1 - Swaraj, Sufal T1 - XANES studies of titanium dioxide nanoparticles synthesized by using Peltophorum pterocarpum plant extract N2 - The preparation and characterization of a Titanium dioxide (TiO2) by a simple, cost effective, facile and eco-friendly green synthesis method using Peltophorum pterocarpum plant extract is presented. The green synthesized nanoparticles were characterized using X-ray diffraction (XRD), Raman spectroscopy, High-resolution transmission electron microscopy (HR-TEM) and X-ray absorption near edge spectroscopy (XANES). XRD results show that the prepared TiO2 NPs were significantly crystalline with various percentages of anatase and rutile phases. The nanoparticles were found to have different diameters ranging from 20 to 80 nm. No evidence of any intermediate or different TiO2 phases were found in XANES measurements performed at the Ti K- and L-edge. It is shown that the TiO2 NPs with high uniformity, high surface area and minimum aggregation can be prepared with relative ease and the desired anatase: rutile phase ratio can be obtained by controlling the experimental conditions. KW - XANES KW - Raman KW - XRD KW - NEXAFS KW - Titanium dioxide PY - 2016 UR - http://www.sciencedirect.com/science/article/pii/S0921452616304197 DO - https://doi.org/10.1016/j.physb.2016.09.011 SN - 0921-4526 IS - 503 SP - 86 EP - 92 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-39805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya T1 - Optical Methods for the Quantification of Functional Groups on Particle Surfaces N2 - Polymer nanoparticles are of increasing importance for a wide range of applications in the material and life sciences. This includes their application as carriers for e.g., analyte-responsive ligands for DNA sequencing platforms, drugs as well as dye molecules for use as multichromophoric reporters for signal enhancement in optical assays or the fabrication of nanosensors and targeted probes in bioimaging studies. Application-relevant properties of nanometer- and micrometer-sized particles (NP) include their size (and size distribution), colloidal stability, biocompatibility, and ease of subsequent functionalization, e.g., with linkers, sensor molecules, and targeting ligands. In this respect, the knowledge of the chemical nature, the total number of surface groups and the number of groups accessible for subsequent coupling reactions with differently sized optical labels or biomolecules is mandatory. This requires robust, reliable and validated methods, which can be employed for the characterization of a broad variety of particle systems independent of their optical properties, i.e., scattering or the presence of encoding dyes, and can be preferably performed specifically, sensitively, and fast with inexpensive equipment. Particularly attractive methods are here straightforward colorimetric, and fluorometric assays. In this respect, we studied a variety of conventional labels for optical readout, utilizing e.g., a change in intensity and/or color of absorption and/or emission. While in common assays, most reporters are measured directly at the particle surface, which can easily lead to signal distortions by scattering and encoding dyes, we focus on the development of cleavable and multimodal labels. These labels are detectable both bound at the particle surface and after cleavage of a linker unit in the supernatant with different analytical methods like fluorometry together with elemental analysis, ICP-OES or ICP-MS for straightforward method validation by method comparison. Here, we present our newly-synthesized cleavable labels and their application for photometric quantification of amino, thiol and carboxy surface groups on different types of nanomaterials and compare the results obtained from surface group analysis relying on conventional labels. T2 - First European / 10th German BioSensor Symposium CY - Potsdam, Germany DA - 20.03.2017 KW - Optical quantification KW - Surface functional groups KW - Nanoparticle PY - 2017 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-39788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 12, Ausgabe 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2004 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 12 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40060 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 12, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 12, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2004 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 12 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40061 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Guehrs, E. A1 - Schneider, M. A1 - Günther, Ch. M. A1 - Hessing, P. A1 - Heitz, K. A1 - Wittke, D. A1 - López-Serrano Oliver, Ana A1 - Jakubowski, Norbert A1 - Plendl, J. A1 - Eisebitt, S. A1 - Haase, A. T1 - Quantification of silver nanoparticle uptake and distribution within individual human macrophages by FIB/SEM slice and view N2 - Quantification of nanoparticle (NP) uptake in cells or tissues is very important for safety assessment. Often, electron microscopy based approaches are used for this purpose, which allow imaging at very high resolution. However, precise quantification of NP numbers in cells and tissues remains challenging. The aim of this study was to present a novel approach, that combines precise quantification of NPs in individual cells together with high resolution imaging of their intracellular distribution based on focused ion beam/ scanning electron microscopy (FIB/SEM) slice and view approaches. KW - Nanoparticles KW - FIB/SEM slice and view KW - Absolute dose KW - Cellular internalization KW - Macrophage PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-400626 DO - https://doi.org/10.1186/s12951-017-0255-8 SN - 1477-3155 VL - 15 SP - Article 21, 1 EP - 11 AN - OPUS4-40062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 13, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 13, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2005 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 13 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40065 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Millar, Steven A1 - Günther, Tobias A1 - Wilsch, Gerd T1 - Revealing hidden spectral information of chlorine and sulfur in data of a mobile Laser-induced Breakdown Spectroscopy system using chemometrics N2 - For the damage assessment of reinforced concrete structures the quantified ingress profiles of harmful species like chlorides, sulfates and alkali need to be determined. In order to provide on-site analysis of concrete a fast and reliable method is necessary. Low transition probabilities as well as the high ionization energies for chlorine and sulfur in the near-infrared range makes the detection of Cl I and S I in low concentrations a difficult task. For the on-site analysis a mobile LIBS-system (k = 1064 nm, Epulse ≤ 3 mJ, t = 1.5 ns) with an automated scanner has been developed at BAM. Weak chlorine and sulfur signal intensities do not allow classical univariate analysis for process data derived from the mobile system. In order to improve the analytical performance multivariate analysis like PLS-R will be presented in this work. A comparison to standard univariate analysis will be carried out and results covering important parameters like detection and quantification limits (LOD, LOQ) as well as processing variances will be discussed (Allegrini and Olivieri, 2014 [1]; Ostra et al., 2008 [2]). It will be shown that for the first time a low cost mobile system is capable of providing reproducible chlorine and sulfur analysis on concrete by using a low sensitive system in combination with multivariate evaluation. KW - LIBS KW - Chemometrics KW - Building materials PY - 2017 DO - https://doi.org/10.1016/j.sab.2017.04.001 SN - 0584-8547 VL - 132 SP - 43 EP - 49 PB - Elsevier B.V. AN - OPUS4-40066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schürmann, Robin A1 - Bald, Ilko T1 - Effect of adsorption kinetics on dissociation of DNA-nucleobases on gold nanoparticles under pulsed laser illumination N2 - Photothermal therapy is a novel approach to destroy cancer cells by an increase of temperature due to laser illumination of gold nanoparticles (GNPs) that are incorporated into the cells. Here, we study the decomposition of DNA nucleobases via irradiation of gold nanoparticles with ns-laser pulses. The kinetics of the adsorption and decomposition process is described by a theoretical model based on the Langmuir assumptions and correlated with experimentally determined reaction rates revealing a strong influence of the nucleobase specific adsorption. Beside the four nucleobases, their brominated analogs, which are potential radiosensitizers in cancer therapy, are also investigated and show a significant modification of the decomposition rates. The fastest decomposition rates are observed for adenine, 8-bromoadenine, 8-bromoguanine and 5-bromocytosine. These results are in good agreement with the relative adsorption rates that are determined from the aggregation kinetics of the GNPs taking the effect of an inhomogeneous surface into account. For adenine and its brominated analog, the decomposition products are further analyzed by surface enhanced Raman scattering (SERS) indicating a strong fragmentation of the molecules into their smallest subunits. KW - Gold nanoparticle KW - DNA damage KW - Kinetics KW - Pulsed Laser KW - Physical Chemistry PY - 2017 DO - https://doi.org/10.1039/c6cp08433h SN - 1463-9076 SN - 1463-9084 VL - 19 IS - 17 SP - 10796 EP - 10803 AN - OPUS4-40070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wlonka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 13, Ausgabe 3 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 13, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2005 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 13 IS - 3 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40087 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 5, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 5, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1997 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 5 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40142 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 5, Ausgabe 3 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 5, edition 3 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1997 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 5 IS - 3 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40143 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 6, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 6, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1998 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 6 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40146 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 6, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 6, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1998 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 6 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40147 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 6, Ausgabe 3 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 6, edition 3 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1998 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 6 IS - 3 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40148 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 7, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 7, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1999 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 7 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40151 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 7, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 7, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1999 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 7 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40152 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 7, Ausgabe 3 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 7, edition 3 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1999 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 7 IS - 3 SP - 1 EP - 8 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40153 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Electron beam therapy: Microdosimetric calculations for the quantification of fundamental damaging processes N2 - Electron beam therpy is used to treat tumor cells by irradiation with high energy electrons (HEE). The irradiation is performed by medical linear accelerators. By interaction of the HEE with the irradiated tissue a broad spectra of secondary electrons and water dissoziation products is generated. These products interact with biomolecules, especially DNA, by various processes. The disentanglement of the resulting direct- and indirect damage to DNA and other cellular components is still under debate. To increase the efficiency of future therapies a better understanding of the microscopic damaging processes is highly important. Especially the various contributions of the secondary species produced, such as low energy electrons (LEE) and radicals is far from understood and quantified. To increase the understanding we present a combination of a microdosimetric simulations and experiments to quantify the damage by means of electron scattering and diffusion simulations within the Geant4-DNA framework. In combination with in-liquid irradiation of plasmid DNA it possible to determine microdosimetric quantities for biomolecules in liquid environment. The presented method was applied to the irradiation of plasmid DNA (pUC19) in water. This opens up new possibilities in radiation research to quantify the dosage-damage relationship for microscopic plasmid volumes under well defined physiological condition. T2 - IWBBIO17 CY - Granada. Spain DA - 25.04.2017 KW - DNA KW - Dosimetry KW - Monte-Carlo simulation KW - Electron irradiation KW - Microdosimetry PY - 2017 AN - OPUS4-40043 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 11, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 11, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2003 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 11 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40049 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swart, C. A1 - Jakubowski, Norbert T1 - Update on the status of metrology for metalloproteins N2 - Metalloproteins, which represent about 30 % of the total proteome, are often important markers for distinguishing between healthy and diseased states of patients. As such markers have become increasingly important in clinical diagnostics, some of these proteins are routinely analysed in clinical laboratories. Reliable and comparable results are the basis for the investigation of changes in the proteome due to different health conditions. Nevertheless, for many proteins the results achieved with different routine measurement procedures or in different laboratories vary widely, thus hampering medical insights and the development of treatments. Reference measurement procedures with results traceable to the International System of Units (SI) will also help to greatly improve the performance of routine measurement procedures and, this way, they support the understanding of changes in the metallome. KW - Metalloproteins KW - Traceability KW - Standardization KW - Quantitative proteomics PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-400522 DO - https://doi.org/10.1039/c6ja00181e IS - 9 SP - 1756 EP - 1765 PB - Royal Society of Chemistry (RSC) AN - OPUS4-40052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 11, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 11, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2003 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 11 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40057 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer T1 - Standardization of NDT Methods and Operational Procedures - Active Thermography N2 - Starting with a general consideration of standards the different kinds and levels of standards are compiled. The procedure of initiating a standard is described. An overview about all existing standards for TT (Thermographic Testing) is given with a special focus on ASTM standards. T2 - Training Course: Non-destructive testing of fiber reinforced polymers CY - Berlin, Germany DA - 28.03.2017 KW - Standardization KW - Non-destructive testing KW - Thermographic testing PY - 2017 AN - OPUS4-40107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer T1 - Basics of active thermography applied to CFRP and GFRP N2 - Starting with some examples from the VITCEA project, which gives the framework of the training course, the physical basis of active thermography is demonstrated. It consists of the physical phenomena heat conduction and thermal radiation. The contrast mechanism is explained by means of a simple 1-dimensional approach. This leads to the concept of thermal thickness which is essential for active thermography. Later, the influence of the surface properties reflectivity and emissivity is considered more in detail. T2 - Training Course: Non-destructive testing of fiber reinforced polymers CY - Berlin, Germany DA - 28.03.2017 KW - Heat conduction KW - Thermographic inspection KW - Thermal radiation KW - Emissivity PY - 2017 AN - OPUS4-40108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Analytical applications of high resolution continuum source molecular absorption spectrometry N2 - High-resolution continuum source molecular absorption spectrometry (HR-CS-MAS) has been apply for the determination of non-metals and isotope analysis, extending so the application range of atomic absorption spectrometry (AAS). This seminar is divides in two main parts. First, here is presented a comprehensive mechanistic study of molecule formation in graphite furnaces, a key step into the recovery of analytical signals in AAS and MAS. Therefore, a well-known system for fluorine determination was studied: the molecule formation of CaF, with Zr as permanent modifier. Through a kinetic approach, an Arrhenius behaved pseudo first order reaction respect to F- was observed and by spectroscopic methods (XPS, XAS, EDX) an intermediate state was possible to be elucidated. Here it is proposed a mechanism, where zirconium works as heterogeneous catalyst: after a pyrolytic step, it is activated the intermediate ZrO(OCaF) and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. Second, we have developed analytical methods using HR-CS-MAS as detector for quantification of fluorine in consume-care products with declared per-fluorinated ingredients. Ad, the high resolution of the instrumentation allows identify isotopic shifts in some observed molecular spectra. Consequently, the molecular spectra of enriched isotopes of B were investigated and so the potential of HR-CS-MAS for the determination of isotopic ratios is established. T2 - Brown Bag Lecture SALSA Humboldt Universität zu Berlin CY - Berlin, Germany DA - 18.04.2017 KW - Fluorine KW - Molecular absorption KW - Graphite furnace KW - Isotopes KW - Boron PY - 2017 AN - OPUS4-40075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wlonka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 13, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 13, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2005 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 13 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40085 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 3, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 3, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1995 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 3 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40133 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Glaus, Reto A1 - Gornushkin, Igor B. A1 - Nagli, L. T1 - Stimulated emission in aluminum laser-induced plasma: an experimental study N2 - The stimulated emission (SE) in aluminum laser-induced plasma pumped in resonance with the 3s23p − 3s24s aluminum transition at 266.04 nm is investigated experimentally. It is shown that the population Inversion between the 3s23p and 3s24s states can be created by weak pumping at several microjoule to millijoule pulse energies and result in high gain. The intensity of the SE at 396.15 nm is related to the number density of Al Atoms via absorption measurements. It is found that the SE in forward and backward directions with respect to the pumping laser is different in terms of the line shape and intensity that is attributed to inhomogeneity in a gain coefficient across the plasma plume. KW - Spectroscopy KW - Lasers KW - Laser induced breakdown PY - 2017 DO - https://doi.org/10.1364/AO.56.003699 SN - 1559-128X SN - 0003-6935 SN - 1539-4522 VL - 56 IS - 13 SP - 3699 EP - 3702 PB - Optical Society of America CY - Washington, DC, USA AN - OPUS4-40134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 4, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 4, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1996 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 4 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40139 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 4, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 4, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1996 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 4 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40140 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 5, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 5, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1997 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 5 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40141 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hornemann, A. A1 - Eichert, D. A1 - Flemig, Sabine A1 - Hoehl, A. A1 - Ulm, G. A1 - Beckhoff, B. ED - Shen, Q. ED - Nelson, C. T1 - Probing biolabels for high throughput biosensing via synchrotron radiation SEIRA technique N2 - Bio-diagnostic assays of high complexity rely on nanoscaled assay recognition elements that can provide unique selectivity and design-enhanced sensitivity features. High throughput performance requires the simultaneous detection of various analytes combined with appropriate bioassay components. Nanoparticle induced sensitivity enhancement, and subsequent multiplexed capability Surface-Enhanced InfraRed Absorption (SEIRA) assay formats are fitting well these purposes. SEIRA constitutes an ideal platform to isolate the vibrational signatures of targeted bioassay and active molecules. The potential of several targeted biolabels, here fluorophore-labeled antibody conjugates, chemisorbed onto low-cost biocompatible gold nano-aggregates substrates have been explored for their use in assay platforms. Dried films were analyzed by synchrotron radiation based FTIR/SEIRA spectro-microscopy and the resulting complex hyperspectral datasets were submitted to automated statistical analysis, namely Principal Components Analysis (PCA). The relationships between molecular fingerprints were put in evidence to highlight their spectral discrimination capabilities. We demonstrate that robust spectral encoding via SEIRA fingerprints opens up new opportunities for fast, reliable and multiplexed high-end screening not only in biodiagnostics but also in vitro biochemical imaging. T2 - 12th International Conference on Synchrotron Radiation Instrumentation (SRI) CY - New York, NY, USA DA - 06.07.2015 KW - Biolabels KW - High throughput biosensing KW - Synchrotron radiation KW - SEIRA Technique PY - 2016 DO - https://doi.org/10.1063/1.4952927 VL - 1741 SP - Article Number: 050007 PB - AIP Conference Proceedings AN - OPUS4-40113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reinmuth-Selzle, K. A1 - Kampf, C. J. A1 - Lucas, K. A1 - Lang-Yona, N. A1 - Fröhlich-Nowoisky, J. A1 - Shiraiwa, M. A1 - Lakey, P. S. J. A1 - Lai, S. A1 - Liu, F. A1 - Kunert, A. T. A1 - Ziegler, K. A1 - Shen, F. A1 - Sgarbanti, R. A1 - Weber, B. A1 - Bellinghausen, I. A1 - Saloga, J. A1 - Weller, Michael G. A1 - Duschl, A. A1 - Schuppan, D. A1 - Pöschl, U. T1 - Air pollution and climate change effects on allergies in the anthropocene: Abundance, interaction, and modification of allergens and adjuvants N2 - Air pollution and climate change are potential drivers for the increasing burden of allergic diseases. The molecular mechanisms by which air pollutants and climate parameters may influence allergic diseases, however, are complex and elusive. This article provides an overview of physical, chemical and biological interactions between air pollution, climate change, allergens, adjuvants and the immune system, addressing how these interactions may promote the development of allergies. We reviewed and synthesized key findings from atmospheric, climate, and biomedical research. The current state of knowledge, open questions, and future research perspectives are outlined and discussed. The Anthropocene, as the present era of globally pervasive anthropogenic influence on planet Earth and, thus, on the human environment, is characterized by a strong increase of carbon dioxide, ozone, nitrogen oxides, and combustion- or traffic-related particulate matter in the atmosphere. These environmental factors can enhance the abundance and induce chemical modifications of allergens, increase oxidative stress in the human body, and skew the immune system toward allergic reactions. In particular, air pollutants can act as adjuvants and alter the immunogenicity of allergenic proteins, while climate change affects the atmospheric abundance and human exposure to bioaerosols and aeroallergens. To fully understand and effectively mitigate the adverse effects of air pollution and climate change on allergic diseases, several challenges remain to be resolved. Among these are the identification and quantification of immunochemical reaction pathways involving allergens and adjuvants under relevant environmental and physiological conditions. KW - Allergie KW - Klimaveränderung KW - Luftverschmutzung KW - Partikel KW - Ozon KW - Stickoxide KW - Allergene KW - Adjuvantien KW - PALM KW - DAMP PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404531 DO - https://doi.org/10.1021/acs.est.6b04908 SN - 1520-5851 SN - 0013-936X VL - 51 IS - 8 SP - 4119 EP - 4141 PB - American Chemical Society (ACS) CY - Washington AN - OPUS4-40453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis T1 - A Simple Model of a Contact Acoustic Nonlinearity (CAN) with Scaled Boundary Finite Element Method (SBFEM) N2 - In this contribution, we present a short introduction into the basics of SBFEM formulation of the dynamic elastic wave equation. The SBFEM is then extended for modelling the non-linear behavior of crack clapping. T2 - GAMM 2017 CY - Weimar, Germany DA - 06.03.2017 KW - Scaled Boundary Finite Element Method KW - SBFEM KW - Contact Acoustic Nonlinearity (CAN) PY - 2017 AN - OPUS4-40463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Juribašić, M. A1 - Halasz, I. A1 - Budimir, A. A1 - Užarević, K. A1 - Lukin, S. A1 - Monas, A. A1 - Emmerling, Franziska A1 - Plavec, J. A1 - Ćurić, M. T1 - Reversible Gas−Solid Ammonia N−H Bond Activation Mediated by an Organopalladium Complex N2 - N−H bond activation of gaseous ammonia is achieved at room temperature in a reversible solvent-free reaction using a solid dicyclopalladated azobenzene complex. Monitoring of the gas−solid reaction in real-time by in situ solid-state Raman spectroscopy enabled a detailed insight into the stepwise activation pathway proceeding to the final amido complex via a stable diammine intermediate. Gas−solid synthesis allowed for isolation and subsequent structural characterization of the intermediate and the final amido product, which presents the first dipalladated complex with the PdII−(μ-NH2)−PdII bridge. Gas−solid reaction is readily followed via color changes associated with conformational switching of the palladated azobenzene backbone. The reaction proceeds analogously in solution and was characterized by UV−vis and NMR spectroscopies showing the same stepwise route to the amido complex. Combining the experimental data with density functional theory calculations we propose a stepwise mechanism of this heterolytic N−H bond activation assisted by exogenous ammonia. KW - In situ KW - Mechanochemistry PY - 2017 DO - https://doi.org/10.1021/acs.inorgchem.7b00422 VL - 56 SP - 5342 EP - 5351 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-40464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - LAYER-based Sensors for Monitoring: Surface Plasmon Resonance, Air-coupled UltraSonics, Magneto-optical Coupling N2 - The talk addresses layer-based sensors for monitoring applications. In particular, sensor principles surface plasmon resonance (SPR), air-coupled ultrasonic, and magneto-optical coupling are discussed. Optical sensors on planar substrates are prepared by sol-gel, CVD- and PVD deposition techniques, ultrasonic sensors on planar and curved substrates are made by means of PVD processes, and magnetostrictive coatings for magneto-optical sensors are deposited on fibre-based Bragg gratings (FBGs) using PVD and ECD techniques. For all kinds of sensors design and function are explained and discussed, i.e. regarding sensitivity. It is shown that a) SPR enhanced ellipsometry is a promising tool for gas monitoring of hazardous gases, that b) thermos-acoustic and piezo-electric pulse-echo techniques are relevant for damage inspection of hidden volume defects of CFRPs, and that c) magnetostrictive-optical sensors with self-calibrating (magnetic reference field) function are useful for structural health monitoring in terms of strain sensors. T2 - Vortrag im National Institute of Standards and Technology, Ceramics Division, Nanoscale Strength Measurement and Standards CY - NIST Gaithersburg, Maryland, USA DA - 28.04.2017 KW - Layer-based sensors KW - Surface plasmon resonance (SPR), KW - Air-coupled ultrasonics KW - Magneto-optical coupling KW - Gas monitoring KW - Damage inspection KW - Structural health monitoring PY - 2017 AN - OPUS4-40465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nützmann, Kathrin T1 - Depth dependent phase identification of corrosion zones in ferritic alloys by micro-X-ray absorption near edge structure spectroscopy N2 - Ferritic steels with chromium contents up to 13 wt% are used as materials for power plant components as boiler materials (< 2 wt% Cr) and super heater tubes (> 9 wt% Cr). These materials are subject to aggressive corrosion caused by hot gases such as CO2, H2O, O2 and SO2. Especially SO2 causes fatal corrosion even as a minor component. To examine sulfurous corrosion mechanisms, experiments with pure SO2 were conducted. A proper analysis of the material changes requires phase identification and quantification with a high lateral resolution within the corrosion scale. T2 - ANAKON2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Corosion KW - Steel KW - XANES PY - 2017 AN - OPUS4-40415 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Asadujjaman, Asad A1 - Ahmadi, Vahid A1 - Yalcin, M. A1 - ten Brummelhuis, N. A1 - Bertin, Annabelle T1 - Thermoresponsive functional polymers based on 2,6-diaminopyridine motif with tunable UCST behaviour in water/alcohol mixtures N2 - 2,6-Diaminopyridine based functional polymers poly N-(6-aminopyridin-2-yl)acrylamide) (PNAPAAm) and poly(N-(6-acetamidopyridin-2-yl)acrylamide) (PNAcAPAAm) were synthesized via free radical polymerization and in addition PNAcAPAAm was synthesized by reversible addition–fragmentation chain transfer (RAFT) polymerization for comparison. The obtained polymers displayed upper critical solution temperature (UCST)-type reversible thermoresponsiveness in water/alcohol mixtures. The UCST Phase transition behaviour of the obtained functional polymers was studied using temperature dependent turbidimetry, dynamic light scattering and 1H-NMR measurements. The phase transition temperature of the polymers was tunable by varying either the concentration of the polymer solution, the nature of the alcohol or the composition of the solvent mixture. The cloud Point temperature of PNAcAPAAm was found to decrease with increasing alcohol content (MeOH, EtOH and iPrOH) in water/alcohol mixtures. Past a critical amount of EtOH or iPrOH in water, the cloud point temperature of PNAcAPAAm increased upon further addition of EtOH or iPrOH. Such functional polymers with tunable UCST behaviour can be applicable in drug delivery, sensing, personal care and microfluidic applications. KW - UCST polymer KW - 2,6-diaminopyridine KW - Cosolvency PY - 2017 DO - https://doi.org/10.1039/c7py00539c SN - 1759-9954 SN - 1759-9962 VL - 8 IS - 20 SP - 3140 EP - 3153 PB - RSC AN - OPUS4-40417 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Available particle-sizing techniques at work for the classification as a nanomaterial - How reliable it really is? N2 - The capability of currently available particle sizing techniques for reliable classification of materials that potentially fall under the EU Definition of a nanomaterial is discussed. A systematic quantitative evaluation of the sizing techniques is presented together with representative case studies of analysis of industrially relevant materials. Recommendations on the most appropriate and efficient use of techniques for different types of material are given. T2 - Frontiers of Nanomaterial Characterization CY - Tokyo, Japan DA - 28.05.2017 KW - Nanomaterial classification KW - Nanoparticles KW - Number-weighted median size KW - Particle size analysis KW - Characterization techniques PY - 2017 AN - OPUS4-40474 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - NanoDefine – a brief overview N2 - The large European nanometrology Project NanoDefine is presented briefly with respect to the challenges of measurement of particle size distribution for complex nanoparticulate materials. The methods chosen for a tiered approach for the classification of a nanomaterial are discussed with regard to their peformance. Representative resuls on real life, complex shaped nanoparticulate materials are shown. The recently initiated VAMAS inter-laboratory comparisons to determine the reproducibility necessary for international standardisation have been also presented. T2 - Metrology Study Group of ISO/TC 229 Nanotechnologies /JWG2 'Measurement and Characterization' CY - Tokyo, Japan DA - 31.05.2017 KW - EU definition of a nanomaterial KW - Nanomaterial classification KW - Nanoparticles KW - Nanoparticle size distribution KW - VAMAS inter-laboratory comparison KW - Particle sizing techniques PY - 2017 AN - OPUS4-40475 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Inter-laboratory Comparison on Shape of Bipramidal TiO2 Nanoparticles by Transmission Electron Microscopy - First Results N2 - First results of an inter-laboratory comparsion launched in the frame of ISO/TC 229 'Nanotechnologies' / JWG 2 'Measurement and Characterization' are presented and the further data treatment discussed. Feret min, Feret and Aspect Ratio of bipyramidal TiO2 nanoparticles as determined according to the measurememnt protocol distributed by BAM are compared for all 17 participants for the first time. The inclusion of the case study into the ongoing ISO/TC 229/JWG 2 project on Measurement of size and shape distribution of nanoparticles by TEM is discussed. T2 - Meeting of ISO/TC 229 'Nanotechnologies' CY - Tokyo, Japan DA - 29.05.2017 KW - Inter-laboratory comparison KW - Particle size and shape distribution KW - Bipyramidal TiO2 nanoparticles KW - ISO/TC 229 KW - TEM PY - 2017 AN - OPUS4-40476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Marc Benjamin A1 - Meyer, Susann A1 - Kunte, Hans-Jörg A1 - Solomun, Tihomir A1 - Sturm, Heinz T1 - Measurements and simulations of microscopic damage to DNA in water by 30 keV electrons: A general approach applicable to other radiation sources and biological targets N2 - The determination of the microscopic dose-damage relationship for DNA in an aqueous environment is of a fundamental interest for dosimetry and applications in radiation therapy and protection. We combine geant4 particle-scattering simulations in water with calculations concerning the movement of biomolecules to obtain the energy deposit in the biologically relevant nanoscopic volume. We juxtaposition these results to the experimentally determined damage to obtain the dose-damage relationship at a molecular level. This approach is tested for an experimentally challenging system concerning the direct irradiation of plasmid DNA (pUC19) in water with electrons as primary particles. Here a microscopic target model for the plasmid DNA based on the relation of lineal energy and radiation quality is used to calculate the effective target volume. It was found that on average fewer than two ionizations within a 7.5-nm radius around the sugar-phosphate backbone are sufficient to cause a single strand break, with a corresponding median lethal energy deposit being E1/2=6±4 eV. The presented method is applicable for ionizing radiation (e.g., γ rays, x rays, and electrons) and a variety of targets, such as DNA, proteins, or cells. KW - DNA KW - Radiation damage KW - Dosimetry KW - DNA radiation damage KW - Single-strand break (SSB) KW - Double-strand break (DSB) KW - Low energy electrons KW - Monte Carlo simulation KW - Radiation damage to biomolecules KW - Plasmid DNA in water KW - Lethal dose KW - Solutions (pH, salinity, cosolutes) KW - Geant4 KW - Microdosimetry PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404244 DO - https://doi.org/10.1103/PhysRevE.95.052419 SN - 2470-0045 SN - 2470-0053 VL - 95 IS - 5 SP - 052419-1 EP - 052419-8 PB - American Physical Society CY - USA AN - OPUS4-40424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred T1 - SEM and Micro-XRF analysis to investigate stained glass windows N2 - Several restoration projects of stained-glass windows have been performed in Poland since 2010.Chemical analysis of glass samples was performed with SEM/EDX on a FEI ESEM-XL 30, (EDX-EDAX) and with Micro-XRF (M4 Tornado, Bruker).The chemical composition of medieval glass samples and of glass samples of the 19th Century have been determined. T2 - Technart2017 CY - Bilbao, Spain DA - 02.05.2017 KW - SEM KW - Micro-XRF KW - Glass composition PY - 2017 AN - OPUS4-40435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Nowak, S. H. A1 - Petric, M. A1 - Buchriegler, J. A1 - Bjeoumikhov, A. A1 - Bjeoumikhova, Z. A1 - von Borany, J. A1 - Munnik, F. A1 - Radtke, Martin A1 - Renno, A. D. A1 - Reinholz, Uwe A1 - Scharf, O. A1 - Tilgner, J. A1 - Wedell, R. T1 - Road to micron resolution with a color X-ray camera - Polycapillary optics characterization N2 - In a color X-ray camera spatial resolution is achieved by means of a polycapillary optic conducting X-ray photons from small regions on a sample to distinct energy dispersive pixels on a CCD matrix. At present, the resolution limit of color X-ray camera systems can go down to several microns and is mainly restricted by Pixel dimensions. The recent development of an efficient subpixel resolution algorithm allows a release from pixel size, limiting the resolution only to the quality of theoptics. In this work polycapillary properties that influence the spatial resolution are systematized and assessed both theoretically and experimentally. It is demonstrated that with the current technological Level reaching one micron resolution is challenging, but possible. KW - Color X-ray camera KW - Polycapillary optics PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404404 DO - https://doi.org/10.48550/arXiv.1705.08939 SN - 2331-8422 SP - 1 EP - 11 PB - Cornell University CY - Ithaca, NY AN - OPUS4-40440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Prager, Jens T1 - Einfluss der Aufbaurichtung und Porosität additiv gefertigter Stahl- und Aluminiumwerkstoffe auf lokale akustische Eigenschaften N2 - Die Ultraschallprüfung additiv gefertigter Metallbauteile setzt eine genaue Kenntnis der akustischen Eigenschaften des Werkstoffs voraus. Insbesondere bei bildgebenden Rekonstruktionsverfahren müssen Anisotropien berücksichtigt werden, um ausreichende Abbildungsgenauigkeit zu erhalten. Es ist davon auszugehen, dass der lagenweise Aufbau des Werkstoffs beim selektiven Laserschmelzen eine bevorzugte Kornorientierung erzeugt, die sich in einer akustischen Anisotropie widerspiegelt. Zudem wird erwartet, dass die besondere Kornstruktur Einfluss auf die Schallschwächung hat. Ziel der vorliegenden Untersuchungen war es, die akustischen Eigenschaften verschiedener additiv gefertigter Werkstoffe zu analysieren und die Ergebnisse mit konventionell gefertigten Werkstoffen zu vergleichen. In die Untersuchungen wurden verschiedene Stahl- und Aluminiumproben mit unterschiedlicher Aufbaurichtung einbezogen. Die Ergebnisse, sowohl aus Tauchtechnik als auch aus Kontakttechnikuntersuchungen, zeigen eine signifikante Abhängigkeit der Schallausbreitungsgeschwindigkeit von der Aufbaurichtung. Zudem werden örtliche Schwankungen der gemessenen Schallgeschwindigkeiten sowie ein Einfluss auf die Schallschwächung sichtbar. T2 - DGZfP Jahrestagung CY - Koblenz, Germany DA - 22.05.2017 KW - Additive Fertigung KW - Ultraschallprüfung PY - 2017 AN - OPUS4-40405 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Prager, Jens T1 - Akustische Eigenschaften additiv gefertigter Werkstoffe N2 - Die Ultraschallprüfung additiv gefertigter Metallbauteile setzt eine genaue Kenntnis der akustischen Eigenschaften des Werkstoffs voraus. Insbesondere bei bildgebenden Rekonstruktionsverfahren müssen Anisotropien berücksichtigt werden, um ausreichende Abbildungsgenauigkeit zu erhalten. Es ist davon auszugehen, dass der lagenweise Aufbau des Werkstoffs beim selektiven Laserschmelzen eine bevorzugte Kornorientierung erzeugt, die sich in einer akustischen Anisotropie widerspiegelt. Zudem wird erwartet, dass die besondere Kornstruktur Einfluss auf die Schallschwächung hat. Ziel der vorliegenden Untersuchungen war es, die akustischen Eigenschaften verschiedener additiv gefertigter Werkstoffe zu analysieren und die Ergebnisse mit konventionell gefertigten Werkstoffen zu vergleichen. In die Untersuchungen wurden verschiedene Stahl- und Aluminiumproben mit unterschiedlicher Aufbaurichtung einbezogen. Die Ergebnisse, sowohl aus Tauchtechnik- als auch aus Kontakttechnikuntersuchungen, zeigen eine signifikante Abhängigkeit der Schallausbreitungsgeschwindigkeit von der Aufbaurichtung. Zudem werden örtliche Schwankungen der gemessenen Schallgeschwindigkeiten sowie ein Einfluss auf die Schallschwächung sichtbar T2 - DGZfP Jahrestagung CY - Koblenz, Germany DA - 22.05.2017 KW - Additive Fertigung KW - Ultraschallprüfung PY - 2017 AN - OPUS4-40406 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Numerische Untersuchungen zur Luftultraschallprüfung von faserverstärkten Kunststoffen N2 - Luftultraschall wird immer häufiger für die Prüfung von anisotropen Faserverbunden eingesetzt. Meistens wir in Durchschallung geprüft, aber bei der einseitigen Zugänglichkeit muss eine Art Tandemtechnik mit Anregung von geführten Wellen angewendet werden. Bei beiden Techniken ist der Signal-Rausch-Abstand wegen der niedrigen akustischen Impedanz der Luft deutlich kleiner als bei einer typischen Prüfung in Kontakttechnik. Bei der Tandemtechnik wird das Signal zusätzlich durch eine größere Divergenz und Dämpfung geschwächt. Deshalb ist es wichtig, die Anregung, Ausbreitung und Detektion von geführten Wellen in Faserverbunden zu verstehen. In diesem Beitrag wird ein Finite-Elemente-Modell für die Simulation von luftgekoppelter Anregung und Ausbreitung von geführten Wellen in Faserverbunden vorgestellt und mit Messungen verglichen. Insbesondere wurde die Wellenausbreitung und Modenkonversion in der Nähe von Schäden in mehreren Parameterstudien untersucht. T2 - DGZfP-Jahrestagung CY - Koblenz, Germany DA - 22.5.2017 KW - FEM KW - Luftultraschall KW - Faserverstärkter Kunststoff KW - Prüfung KW - Simulation PY - 2017 AN - OPUS4-40407 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Gegenüberstellung von Wirbelstromprüfung und aktiver Thermografie an CFK-Versuchskörpern N2 - In vielen Bereichen der Technik haben Konstruktionen unter Einsatz von CFK-Bauteilen und Komponenten die klassischen Metalle abgelöst. Die zerstörungsfreie Prüfung solcher CFK-Bauteile gewinnt somit zunehmend an Bedeutung. Ein mögliches Prüfverfahren ist dabei die Wirbelstromprüfung. Aufgrund der relativ geringen elektrischen Leitfähigkeit von CFK-Komponenten kommt hierbei häufig die sogenannte HF-Wirbelstromprüfung zum Einsatz. In verschiedenen Untersuchungen der BAM konnten jedoch auch mit Wirbelstromprüfsystemen in niedrigen Frequenzbereichen gute Ergebnisse erzielt werden. Um die Möglichkeiten und Grenzen dieser konventionellen Wirbelstromprüfung auszuloten, wurden Messungen an Versuchskörpern durchgeführt, welche bereits bei der Validierung der Blitz- und Lock-in-Thermografie für neue Verfahrensnormen erfolgreich eingesetzt wurden. Ein Typ dieser Versuchskörper sind Flachproben aus CFK von 6 mm Dicke. In diesen wurden Flachbodenbohrungen mit Durchmessern zwischen 4 mm und 24 mm eingebracht. Die Restwandstärken liegen zwischen 0,06 mm und 3,66 mm. Ein weiterer CFK-Versuchskörper hat die Geometrie eines Stufenkeiles. Bei verschiedenen Stufenkeilen sind Wanddicken zwischen 1,4 mm und 5,4 mm realisiert worden. In diesen wurden künstliche quadratische Delaminationen mit Kantenlängen zwischen 2 mm und 20 mm eingebracht. Die Ergebnisse der Wirbelstromprüfung werden denen der aktiven Thermografie gegenübergestellt. Zur Nachbildung von Kompositwerkstoffen wurden die flachen Versuchskörper mit geeigneten Versuchskörpern aus Aluminium und Stahl kombiniert. Die Wirbelstromprüfungen wurden mit einem handelsüblichen Prüfgerät im Frequenzbereich zwischen 500 Hz und 3 MHz und entsprechend angepassten Sensoren durchgeführt. T2 - DGZfP Jahrestagung CY - Koblenz, Germany DA - 22.05.2017 KW - Wirbelstromprüfung KW - Thermografie KW - CFK PY - 2017 AN - OPUS4-40408 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kästner, Claudia A1 - Lichtenstein, Dajana A1 - Lampen, Alfonso A1 - Thünemann, Andreas T1 - Monitoring the fate of small silver nanoparticles during artificial digestion N2 - The report on the results of an in vitro digestion study of silver nanoparticles in presence and absenceof food. The particles were poly(acrylic acid) stabilized ultra-small silver nanoparticles with a radius of 3.1 nm and a relative size distribution width of 0.2. As food components oil, starch, skimmed milk powderand a mixture thereof were chosen. Aggregation of the particles was quantified with small-angle X-rayscattering in terms of log-normal radii distributions. Complete aggregation of the primary particles wasdetermined in the absence of food. In contrast, the presence of oil and starch initiates a disaggregationin the intestine. Only small aggregates of 6 nm radii and aggregation numbers of 7 were found in thepresence of milk powder. It prevents primary particles from etching in the gastric and intestinal juice.Our results indicate that the silver nanoparticles can pass the digestion process in a nanoscale form butundergo a strong and food-dependent transformation in their state of aggregation. KW - Small-angle X-ray scattering KW - SAXS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404099 DO - https://doi.org/10.1016/j.colsurfa.2016.08.013 SN - 0927-7757 SN - 1873-4359 VL - 526 SP - 76 EP - 81 PB - Elsevier B.V. AN - OPUS4-40409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf A1 - Pohl, Rainer T1 - Zerstörungsfreie Prüfung mit Wirbelstrom zur Qualitätskontrolle beim Schienenschleifen N2 - In verlegten Eisenbahnschienen entstehen durch Rollkontaktermüdung rissartige Oberflächenschädigungen. Der geschädigte Bereich wird im Rahmen der Schieneninstandhaltung regelmäßig abgetragen, um zu verhindern, dass durch unkontrolliertes Risswachstum schwerwiegende Schienenschäden entstehen. Hierzu werden u. A. Schienenschleifzüge eingesetzt. Früher wurde das Schleifergebnis einer Sichtprüfung unterzogen. Es kommt jedoch vor, dass Risse in der Oberfläche beim Schleifen zugeschmiert oder durch Schleifriefen maskiert werden, so dass diese nicht mehr sichtbar obwohl noch vorhanden sind. An der BAM wurde ein Wirbelstromprüfsystem entwickelt, das sowohl zur Planung als auch der Qualitätskontrolle der Schieneninstandhaltung genutzt wird. Dieses System ist in der Lage, Schädigungen zu detektieren und deren Schädigungstiefe zu bestimmen, selbst dann, wenn optisch keine Schädigung zu erkennen ist. Seit 2013 ist die Qualitätskontrolle mit Wirbelstromprüfsystemen bei der Schienenbearbeitung fest im Regelwerk der DB verankert. T2 - Schleiftagung 2017 CY - Stuttgart, Germany DA - 01.02.2017 KW - Zerstörungsfreie Prüfung KW - Wirbelstromprüfung KW - Schienenschleifen PY - 2017 AN - OPUS4-40379 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Wohlleben, W. A1 - Mielke, Johannes A1 - Hodoroaba, Vasile-Dan A1 - Zimathies, Annett A1 - Bianchin, A. A1 - Lecloux, A. A1 - Roebben, G. A1 - Rauscher, H. A1 - Gibson, N. T1 - Development of an integrated approach based on validated and standardized methods to support the implementation of the EC recommendation for a definition of nanomaterial N2 - The VSSA approach has the important advantage over classifying, imaging and counting techniques that it does not involve dispersion protocols. Further, the BET technique as the basis for VSSA determination it is in widespread use, generates low costs and is specified for many commercial materials. Finally, the same equipment allows for a deeper analysis by full isotherm evaluation. The present deliverable assesses all NanoDefine powders, supplemented by further real-world materials (in total 26 powders), and quantitatively compares the relationship between the median size (by Electron Microscopy – considered as benchmark for the EC nanomaterial definition) vs. the size derived from VSSA. The VSSA method mitigates the challenges of EM to assess the thickness of platelets, but worked as well on fibbers and particles of irregular shapes. A screening strategy is proposed. If applied to the further data from real-world materials as validation set, this screening does achieve a correct classification, leaving only borderline materials for tier 2 assessment. KW - Nanomaterial KW - Classification KW - Regulation KW - VSSA KW - Size measurement KW - Particle size PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-398938 DO - https://doi.org/10.1007/s11051-017-3741-x SP - 1 EP - 26 PB - The NanoDefine Consortium CY - Wageningen, The Netherlands AN - OPUS4-39893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zeynalov, Eldar A1 - Wagner, M. A1 - Friedrich, Jörg Florian A1 - Magerramova, M. A1 - Salmanova, N. A1 - Hidde, Gundula A1 - Meyer-Plath, A. T1 - The peculiar behavior of functionalized carbon nanotubes in hydrocarbons and polymeric oxidation environments N2 - It has been shown that selected types of substituents are able to vary the oxidative behavior of multi-walled carbon nanotubes. Such substituents investigated were sterically hindered secondary amino groups bonded in grafted piperidine units and covalently bonded bromine groups. Their interference and activity was preliminary determined in the model cumene and then in oil diesel fraction and low density polyethylene oxidation reactions. Results obtained indicate that chemical linking of amine moieties containing –NH groups directly to the carbon nanotubes core significantly increases their intrinsic anti-oxidative capacity while the grafting of Br-groups provokes the opposite functioning of the pristine samples. This inference was proved by thermogravimetric and differential thermal analysis of the polyethylene composites and experiments on profound aerobic oxidation of petroleum naphthenic fraction derived from the commercial Baku oils blend diesel cut. KW - Multi-walled carbon nanotubes KW - Amine derivatives KW - Plasma-chemical technique KW - Brominated carbon nanotubes KW - Rate of model oxidation KW - Anti-oxidative efficiency KW - Catalytic activity KW - Inhibition rate constant KW - Photoelectron spectroscopy KW - Oxidation KW - Polyethylene composites KW - Oil diesel fraction PY - 2016 DO - https://doi.org/10.1080/01694243.2016.1239304 SN - 0169-4243 SN - 1568-5616 VL - 31 IS - 9 SP - 988 EP - 1006 AN - OPUS4-39894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hyppänen, I. A1 - Perälä, N. A1 - Arppe, Riika A1 - Schäferling, Michael A1 - Soukka, T. T1 - Environmental and excitation power effects on the ratiometric upconversion luminescence based temperature sensing using nanocrystalline NaYF4:Yb3+,Er3+ N2 - The luminescence intensity ratio (LIR) of the green emissions of the near-infrared excited NaYF4:Yb3+,Er3+ nanocrystals is a promising method for temperature sensing. Here, the influence of excitation power density, excitation pulse length, excitation wavelength, silica shell, and solvent on the LIR and its temperature response is reported. The primary objective is to study the LIR mechanism and the impact of measurement and environmental parameters on the calibration and precision of the LIR. The LIR value is demonstrated to be unaffected by the excitation intensity in the studied range. This result is essential, considering the application feasibility of the LIR method as temperature sensor, where the effective excitation power density depends on the sample matrix and the distance excitation light travels in the sample. The pulsed excitation, however, results in an increase in the LIR value upon short pulse width. Silanization of bare nanocrystals has no effect on the LIR values, but the local warming of H2O samples under laser exposure results in slightly increased LIR values compared to other solvents; D2O, oleic acid, and dimethyl sulfoxide. The thermal quenching of luminescence lifetimes of Er3+ emission is proved to be too weak for sensing applications. KW - Photon upconversion KW - Temperature sensing KW - Luminescence intensity ratio KW - Excitation intensity PY - 2017 UR - http://onlinelibrary.wiley.com/doi/10.1002/cphc.201601355/epdf DO - https://doi.org/10.1002/cphc.201601355 SN - 1439-4235 SN - 1439-7641 VL - 18 IS - 6 SP - 692 EP - 701 PB - Wiley-VCH CY - Weinheim AN - OPUS4-39899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hyppänen, Iko A1 - Höysniemi, Niina A1 - Arppe, Riika A1 - Schäferling, Michael A1 - Soukka, Tero T1 - Environmental impact on the excitation path of the red upconversion emission of nanocrystalline NaYF4:Yb3+,Er3+ N2 - The mechanism for red upconversion luminescence of Yb−Er codoped materials is not generally agreed on in the literature. Both two-photon and three-photon processes have been suggested as the main path for red upconversion emission. We have studied β-NaYF4:Yb3+,Er3+ nanoparticles in H2O and D2O, and we propose that the nanoparticle environment is a major factor in the selection of the preferred red upconversion excitation pathway. In H2O, efficient multiphonon relaxation (MPR) promotes the two-photon mechanism through green emitting states, while, in D2O, MPR is less effective and the three-photon path involving back energy transfer to Yb3+ is the dominant mechanism. For the green upconversion emission, our results suggest the common two-photon path through the 4F9/2 energy state in both H2O and D2O. KW - Photon upconversion KW - Three photon excitation KW - Multiphonon relaxation KW - Excitation intensity PY - 2017 UR - http://pubs.acs.org/doi/pdf/10.1021/acs.jpcc.7b01019 DO - https://doi.org/10.1021/acs.jpcc.7b01019 SN - 1932-7447 SN - 1932-7455 VL - 121 IS - 12 SP - 6924 EP - 6929 PB - ACS Publications AN - OPUS4-39900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - A proposed mechanism of action of permanent modifiers for molecular absorption spectrometry: the case of calcium monofluoride N2 - High-Resolution Continuum Source Molecular Absorption Spectrometry (HR-CS-MAS) with graphite furnace atomizers has been successfully used for the analytical determination of non-metals. The use of permanent modifiers (or coatings) for molecule formation is necessary, but their mechanisms of action remain unclear. In order to understand and improve the current analytical methods, we present a comprehensive mechanistic study of molecule formation in graphite furnaces: a key step into the recovery of analytical signals. Therefore, a well-known system for fluorine determination was studied: the molecule formation of CaF, with Zr as permanent modifier. Through a kinetic approach, an Arrhenius plot showed a pseudo first order reaction respect to F-. By spectroscopic methods (XPS, XAS, EDX) it was possible to elucidate an intermediate state. Here a mechanism is proposed, where ZrO2 works as heterogeneous catalyst: after a pyrolytic step, it is activated to the intermediate state of ZrO(OCaF) and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. With this analytical information, improved surface modifications and coatings for graphite furnaces can be designed and some of them, for example with Zr nanoparticle and Zr xerogels are here presented. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Fluorine KW - High-resolution continuum source Molecular Absorption Spectrometry KW - HR-CS-MAS KW - Zirconium oxide KW - Modifier KW - Coating PY - 2017 AN - OPUS4-39902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, F. A1 - Lai, S. A1 - Tong, H. A1 - Lakey, P. S. J. A1 - Shiraiwa, M. A1 - Weller, Michael G. A1 - Pöschl, U. A1 - Kampf, C. J. T1 - Release of free amino acids upon oxidation of peptides and proteins by hydroxyl radicals N2 - Hydroxyl radical-induced oxidation of proteins and peptides can lead to the cleavage of the peptide, leading to a release of fragments. Here, we used high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) and pre-column online ortho-phthalaldehyde (OPA) derivatization-based amino acid analysis by HPLC with diode array detection and fluorescence detection to identify and quantify free amino acids released upon oxidation of proteins and peptides by hydroxyl radicals. Bovine serum albumin (BSA), ovalbumin (OVA) as model proteins, and synthetic tripeptides (comprised of varying compositions of the amino acids Gly, Ala, Ser, and Met) were used for reactions with hydroxyl radicals, which were generated by the Fenton reaction of iron ions and hydrogen peroxide. The molar yields of free glycine, aspartic acid, asparagine, and alanine per peptide or protein varied between 4 and 55%. For protein oxidation reactions, the molar yields of Gly (∼32-55% for BSA, ∼10-21% for OVA) were substantially higher than those for the other identified amino acids (∼5-12% for BSA, ∼4-6% for OVA). Upon oxidation of tripeptides with Gly in C-terminal, mid-chain, or N-terminal positions, Gly was preferentially released when it was located at the C-terminal site. Overall, we observe evidence for a site-selective formation of free amino acids in the OH radical-induced oxidation of peptides and proteins, which may be due to a reaction pathway involving nitrogen-centered radicals. KW - Peptides KW - Proteins KW - Oxidation KW - Hydroxyl radicals KW - LC-MS KW - Amino acid analysis KW - Bovine serum albumin KW - Ovalbumin KW - Tripeptides KW - Ortho-Phthalaldehyde KW - AAA KW - Degradation KW - Fragmentation KW - Mechanism PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-398714 UR - http://link.springer.com/article/10.1007%2Fs00216-017-0188-y DO - https://doi.org/10.1007/s00216-017-0188-y SN - 1618-2650 SN - 1618-2642 VL - 409 IS - 9 SP - 2411 EP - 2420 PB - Springer CY - Heidelberg AN - OPUS4-39871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Braun, B. A1 - Wedler, C. A1 - Theil, F. T1 - Synthesis of M + 4 stable isotopomers of ergometrine and ergometrinine N2 - The priority ergot alkaloids ergometrine and ergometrinine are highly toxic mycotoxins naturally occurring in different types of grains (i.e. rye, wheat, rice), as well as grain-based foods and, therefore, have gained increasing importance for food safety over the last years. The application of HPLC-MS/MS for the analysis of ergot alkaloids in food presupposes the availability of isotopically labelled internal standards. Thus, a multistep synthesis was developed for ergometrine-(N-13CD3) and its epimer ergometrinine-(N-13CD3) with a mass shift of four units compared with the parent compounds. The synthesis is based on the preparation of stable isotope labelled lysergic acid that was coupled with (S)-alaninol. The chemical synthesis of both compounds has been achieved in six steps with an overall yield of 1 % (ergometrine-(N-13CD3)) and 0.6 % (ergometrinine-(N-13CD3)), respectively. Structural identification was performed by MS analysis as well as 1H and 13C NMR. KW - Ergometrine-(N-13CD3) KW - Ergometrinine-(N-13CD3) KW - Mycotoxin KW - Ergot alkaloids KW - Analytical standard KW - Stable isotope dilution analysis (SIDA) PY - 2017 SN - 1934-578X SN - 1555-9475 VL - 12 IS - 3 SP - 373 EP - 376 PB - NPC CY - Westerville, Ohio, USA AN - OPUS4-39874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian T1 - Bleifreie Sanitärwerkstoffe auf Kupferbasis - Zertifiziertes Referenzmaterial für die Analyse von Messing N2 - Für den Einsatz in der Funkenemissionsspektrometrie und Röntgenfluoreszenzanalyse hat die Bundesanstalt für Materialforschung und -prüfung (BAM) das zertifizierte Referenzmaterial (ZRM) ERM-EB393a für die Analyse von bleifreiem Messing (CuZn21Si3P) herausgegeben. Zertifiziert wurden die Massenanteile der Legierungselemente Kupfer, Silicium und Phosphor sowie der Spuren Blei, Eisen, Zinn, Aluminium, Chrom, Mangan, Nickel, Arsen und Cadmium. Die Charakterisierung des ZRM erfolgte nasschemisch im Ringversuch mit erfahrenen Laboratorien aus der Nichteisenmetallindustrie. KW - Zertifiziertes Referenzmaterial KW - ECOBRASS KW - Bleifreies Messing KW - Sanitärwerkstoff PY - 2017 VL - 71 IS - 3 SP - 79 EP - 81 PB - GDMB Verlag GmbH AN - OPUS4-39679 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buckle, T. A1 - van der Wal, S. A1 - van Malderen, S. A1 - Müller, Larissa A1 - Kuil, J. A1 - van Unen, V. A1 - Peters, R. A1 - van Bemmel, M. A1 - McDonnell, L. A1 - Velders, A. A1 - Koning, F. A1 - Vanhaeke, F. A1 - van Leeuwen, F. T1 - Hybrid imaging labels: providing the link between mass spectrometry-based molecular pathology and theranostics N2 - Development of theranostic concepts that include inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) imaging can be hindered by the lack of a direct comparison to more standardly used methods for in vitro and in vivo evaluation; e.g. fluorescence or nuclear medicine. In this study a bimodal (or rather, hybrid) tracer that contains both a fluorescent dye and a chelate was used to evaluate the existence of a direct link between mass spectrometry (MS) and in vitro and in vivo molecular imaging findings using fluorescence and radioisotopes. At the same time, the hybrid label was used to determine whether the use of a single isotope label would allow for MS-based diagnostics. KW - Imaging KW - Laser Ablation ICP-MS KW - Diagnostics PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-396813 DO - https://doi.org/10.7150/thno.17484 VL - 7 IS - 3 SP - 624 EP - 633 PB - IvySpring AN - OPUS4-39681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietrich, Paul A1 - Treu, Dieter A1 - Kalbe, Henryk A1 - Krumrey, M. A1 - Gross, Thomas A1 - Marti, K. A1 - Unger, Wolfgang T1 - Experimental determination of the effective attenuation length of palladium 3d 5/2 photoelectrons in a magnetron sputtered Pd nanolayer N2 - An electron effective attenuation length (EAL) of 1.68nm for Al Kα excited Pd 3d 5/2 photoelectrons with a kinetic energy of 1.152 keV has been determined experimentally using a sputtered Pd film deposited on an ultra flat fused quartz substrate. The film thickness was reduced by Ar ion sputtering several times in order to obtain different Pd film thicknesses which are used to determine experimental EAL values. These results are compared to data generated by using a Simulation of Electron Spectra for Surface Analysis (SESSA) simulation using an inelastic mean free path (IMFP) calculated with the Tanuma–Powell–Penn (TPP)-2M formula and with ‘elastic scattering on and off’. Contributions to the uncertainty budget related to the experimental approach are discussed in detail. Proposals on how to further improve the approach are suggested. KW - Pd 3d KW - Electron effective attenuation length KW - XPS PY - 2017 UR - http://onlinelibrary.wiley.com/doi/10.1002/sia.6141/abstract?campaign=woletoc DO - https://doi.org/10.1002/sia.6141 SN - 0142-2421 SN - 1096-9918 VL - 49 IS - 5 SP - 464 EP - 468 PB - John Wiley & Sons, Ltd AN - OPUS4-39682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Die neue ISO 20339 N2 - Ein Vergleich der neuen ISO 20339 "Non-destructive testing — Equipment for eddy current examination — Array probe characteristics and verification" mit der ISO 15548-2 "Non-destructive testing – Equipment for eddy current examination – Part 2: Probe characteristics and verification". Es wird gezeigt, dass beide Normen weitgehend identisch sind und in der neuen ISO 20339 die Besonderheiten von Arrays unzureichend berücksichtigt werden. T2 - DGZfP Fachausschuss Oberflächenrissprüfung (FA OFR) CY - Ismaning, Germany DA - 28.03.2017 KW - Wirbelstromprüfung KW - Norm KW - Arraysonde PY - 2017 AN - OPUS4-39654 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 1, Ausgabe 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. PY - 1993 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 VL - 1 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39932 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 17, Ausgabe 3 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 17, edition 3 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2009 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 17 IS - 3 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40222 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 18, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 18, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2010 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 18 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40223 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 8, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 8, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2000 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 8 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40224 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 10, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 10, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2002 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 10 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40225 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Maiwald, Michael T1 - Proceedings of 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) N2 - EuroPACT 2017 is the fourth European Conference on Process Analytics and Control Technology. The conference covered new technologies in process analytics, the implementation of these technologies in various fields and the transformation of data into knowledge. The conference was supported by an exhibition of instrumentation, applications and data evaluation tools. EUROPACT 2017 provided a meeting and a discussion forum for scientists and users of process analytics from academia and industry. The conference programme includes plenary lectures and discussion during poster sessions. The conference took place 10-12 May 2017 in Potsdam (nearby Berlin), Germany. T2 - 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) CY - Potsdam, Germany DA - 10.05.2017 KW - EuroPACT KW - EuroPACT 2017 KW - Prozessanalytik KW - Process Analytical Technology KW - Process control KW - Control Technology KW - Chemometrics PY - 2017 UR - http://dechema.de/europact17.html SP - 1 EP - 176 CY - Frankfurt a. M. AN - OPUS4-40227 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Paul, Andrea A1 - Ruiken, J.-P. A1 - Westad, Frank A1 - Illner, M. A1 - Müller, D. A1 - Esche, E. A1 - Repke, J.-U. A1 - Maiwald, Michael T1 - Online Spectroscopy in Microemulsions – A Process Analytical Approach for a Hydroformylation Mini-plant N2 - Within the Collaborative Research Center InPROMPT a novel process concept for the hydroformylation of long-chained olefins is studied in a mini-plant, using a rhodium complex as catalyst in the presence of syngas. Recently, the hydroformylation in micro¬emulsions, which allows for the efficient recycling of the expensive rhodium catalyst, was found to be feasible. However, the high sensitivity of this multi-phase system with regard to changes in temperature and composition demands a continuous observation of the reaction to achieve a reliable and economic plant operation. For that purpose, we tested the potential of both online NMR and Raman spectroscopy for process control. The lab-scale experiments were supported by off-line GC-analysis as a reference method. A fiber optic coupled probe of a process Raman spectrometer was directly integrated into the reactor. 25 mixtures with varying concentrations of olefin (1-dodecene), product (n-tridecanal), water, n-dodecane, and technical surfactant (Marlipal 24/70) were prepared according to a D-optimal design. Online NMR spectroscopy was implemented by using a flow probe equipped with 1/16” PFA tubing serving as a flow cell. This was hyphenated to the reactor within a thermostated bypass to maintain process conditions in the transfer lines. Partial least squares regression (PLSR) models were established based on the initial spectra after activation of the reaction with syngas for the prediction of unknown concentrations of 1-dodecene and n-tridecanal over the course of the reaction in the lab-scale system. The obtained Raman spectra do not only contain information on the chemical composition but are further affected by the emulsion properties of the mixtures, which depend on the phase state and the type of micelles. Based on the spectral signature of both Raman and NMR spectra, it could be deduced that especially in reaction mixtures with high 1-dodecene content the formation of isomers as a competitive reaction was dominating. Similar trends were also observed during some of the process runs in the mini-plant. The multivariate calibration allowed for the estimation of reactants and products of the hydroformylation reaction in both laboratory setup and mini-plant. T2 - 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) CY - Potsdam, Germany DA - 10.05.2017 KW - Microemulsions KW - Process Analytical Technology KW - Reaction Monitoring KW - Online NMR Spectroscopy KW - Online Raman Spectroscopy PY - 2017 SP - 64 EP - 64 CY - Frankfurt a. M. AN - OPUS4-40228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Paul, Andrea A1 - Wander, Lukas A1 - Gräßer, Patrick A1 - Maiwald, Michael T1 - Design and Validation of a Compact NMR Analyser N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and relatively inexpensive analysers, which feature advantages like low cost, low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, sufficient robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. If these are not available, there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Unionʼs Research Project CONSENS (Integrated Control and Sensing) by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. The presented NMR module is provided in an explosion proof housing of 57 x 57 x 85 cm module size and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling (IHM) was selected for data analysis of the low-field NMR spectra. A set-up for monitoring continuous reactions in a thermostated 1/8” tubular reactor using automated syringe pumps was used to validate the IHM models by using high-field NMR spectroscopy as analytical reference method. T2 - 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) CY - Potsdam, Germany DA - 10.05.2017 KW - Prozessanalytik KW - Reaction Monitoring KW - Online NMR Spectrsocopy KW - Process Analytical Technology KW - Industrie 4.0 KW - EuroPACT PY - 2017 SP - 72 EP - 73 CY - Frankfurt a. M. AN - OPUS4-40229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illner, M. A1 - Meyer, Klas A1 - Paul, Andrea A1 - Esche, E. A1 - Maiwald, Michael A1 - Repke, J.-U. T1 - Operation and Optimal Control of Multiphase Systems – Hydroformylation in Microemulsions on the Mini-plant Scale N2 - Hydroformylation of short-chained olefins has been established as a standard industrial process for the production of C2 to C6 aldehydes. Using aqueous solutions of transition metal complexes these processes are carried out homogeneously catalyzed. A biphasic approach allows for highly efficient catalyst recovery. Regarding renewable feedstocks, the hydroformylation of long-chained alkenes (> C10) in a biphasic system, using highly selective rhodium catalysts has yet not been shown. Therefore, the Collaborative Research Center SFB/TR 63 InPROMPT develops new process concepts, involving innovative tuneable solvent systems to enable rather difficult or so far nonviable synthesis paths. One possible concept is the hydroformylation of long-chained alkenes in microemulsions. For this, a modular mixer-settler concept was proposed, combining high reaction rates and efficient catalyst recycling via the application of technical grade surfactants. The feasibility of such a concept is evaluated in a fully automated, modular mini-plant system within which the characteristics of such a multiphase system pose several obstacles for the operation. Maintaining a stable phase separation for efficient product separation and catalyst recycling is complicated by small and highly dynamic operation windows as well as poor measurability of component concentrations in the liquid phases. In this contribution, a model-based strategy is presented to enable concentration tracking and phase state control within dynamic mini-plant experiments. Raman spectroscopy is used as an advanced process analytical tool, which allows for online in-situ tracking of concentrations. Combined with optical and conductivity analysis optimal plant trajectories can be calculated via the solution of dynamic optimization problem under uncertainty. Applying these, a stable reaction yield of 40 % was achieved, combined with an oil phase purity of 99,8 % (total amount of oily components in the oil phase) and catalyst leaching below 0.1 ppm. T2 - 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) CY - Potsdam, Germany DA - 10.05.2017 KW - Hydroformylation KW - Micoemulsion KW - Dispersion KW - Process Analytical Technology KW - Mini-plant KW - EuroPACT PY - 2017 SP - 92 EP - 92 CY - Frankfurt a. M. AN - OPUS4-40230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 15, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 15, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2007 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 15 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40208 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertin, Annabelle T1 - Upper Critical Solution Temperature (UCST)-type thermoresponsive polymers from acrylamide-based monomers N2 - UCST-type thermoresponsive polymers that phase separate from solution upon cooling present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol. In this context, acrylamide-based monomers can be very useful building blocks for designing novel UCST-type polymers because of their hydrophilic nature (with the right side chain) and propensity to form hydrogen bonds. We want to present our latest results on the copolymer poly(acrylamide-co-acrylonitrile) (P(AAm-co-AN)) that present a UCST in water as well as on two homopolymers based on an acrylamide derivative of 2,6-diaminopyridine, namely poly(N-(6-aminopyridin-2-yl)acrylamide) (PNAPAAm) and poly(N-(6-acetamidopyridin-2-yl)acrylamide) (PNAcAPAAm) that show UCST-type thermoresponsiveness in water/alcohol mixtures. Our focus for P(AAm-co-AN)) is its aggregation behaviour above and below its phase transition temperature as the size of thermoresponsive polymeric systems is of prime importance for biomedical applications (as size dependent processes take place in the body) and is linked to the optical properties of a material that matter in materials science. In the case of PNAPAAm and PNAcAPAAm, we focused on the co-solvency/co-non solvency effect on the phase transition temperature in water/alcohol mixture. Indeed, polymers with UCST behavior below 60°C in water/alcohol mixtures are extremely promising for the preparation of “smart” materials for sensing. T2 - Soft smart responsive materials workshop: Fundamentals and applications (SmartCECAM) CY - Mainz, Germany DA - 11.05.2017 KW - Thermoresponsive polymers KW - UCST-type polymers KW - poly(acrylamide-co-acrylonitrile) KW - 2,6-diaminopyridine-based polymers KW - co-solvency in water/acohol mixture PY - 2017 AN - OPUS4-40211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 16, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 16, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2008 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 16 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40214 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 16, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 16, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2008 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 16 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40216 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 17, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 17, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2009 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 17 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40218 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 17, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 17, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2009 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 17 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40220 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Joseph, A. A1 - Bernardes, C. E. S. A1 - Druzhinina, A. I. A1 - Varushchenko, R. M. A1 - Nguyen, Thi Yen A1 - Emmerling, Franziska A1 - Yuan, L. A1 - Dupray, V. A1 - Coquerel, G. A1 - Minas da Piedade, M. E. T1 - Polymorphic phase transition in 4′-hydroxyacetophenone: Equilibrium temperature, kinetic barrier, and the relative stability of Z′=1 and Z′=2 forms N2 - Particularly relevant in the context of polymorphism is understanding how structural, thermodynamic, and kinetic factors dictate the stability domains of polymorphs, their tendency to interconvert through phase transitions, or their possibility to exist in metastable states. These three aspects were investigated here for two 4′-hydroxyacetophenone (HAP) polymorphs, differing in crystal system, space group, and number and conformation of molecules in the asymmetric unit. The results led to a ΔfGm°-T phase diagram highlighting the enantiotropic nature of the system and the fact that the Z′=1 polymorph is not necessarily more stable than its Z′=2 counterpart. It was also shown that the form II → form I transition is entropy driven and is likely to occur through a nucleation and growth mechanism, which does not involve intermediate phases, and is characterized by a high activation energy. Finally, although it has been noted that conflicts between hydrogen bond formation and close packing are usually behind exceptions from the hypothesis of Z′=1 forms being more stable than their higher Z′ analogues, in this case, the HAP polymorph with stronger hydrogen bonds (Z′=2) is also the one with higher density. KW - Polymorphism KW - Polymorphic transition KW - 4'-hydroxyacetophenone PY - 2017 DO - https://doi.org/10.1021/acs.cgd.6b01876 SN - 1528-7483 SN - 1528-7505 VL - 17 IS - 4 SP - 1918 EP - 1932 PB - ACS AN - OPUS4-40167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krome, Fabian A1 - Gravenkamp, H. T1 - A semi-analytical curved element for linear elasticity based on the scaled boundary finite element method N2 - This work introduces a semi-analytical formulation for the simulation and modeling of curved structures based on the Scaled Boundary Finite Element Method (SBFEM). This approach adapts the fundamental idea of the SBFEM concept to scale a boundary to describe a geometry. Until now, scaling in SBFEM has exclusively been performed along a straight coordinate which enlarges, shrinks or shifts a given boundary. In this novel approach, scaling is based on a polar or cylindrical coordinate system such that a boundary is shifted along a curved scaling direction. The derived formulations are used to compute the static and dynamic stiffness matrices of homogeneous curved structures. The resulting elements can be coupled to general SBFEM or FEM domains. For elastodynamic problems computations are performed in the frequency domain. Results of this work are validated using the Global Matrix Method and Standard Finite Element analysis. KW - Scaled boundary finite element method KW - Elasticity KW - Curved structures PY - 2017 DO - https://doi.org/10.1002/nme.5306 SN - 0029-5981 SN - 1097-0207 VL - 109 IS - 6 SP - 790 EP - 808 PB - WILEY-BLACKWELL AN - OPUS4-40170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Telgmann, L. A1 - Lindner, U. A1 - Lingott, J. A1 - Jakubowski, Norbert T1 - Analysis and speciation of lanthanoides by ICP-MS N2 - Inductively coupled plasma mass spectrometry (ICP-MS) is based on formation of positively charged atomic ions in a high-frequency inductively coupled Argon plasma at atmospheric pressure. The ions are extracted and transferred from the plasma source into a mass analyzer operated at high vacuum via an interface equipped with a sampling and a skimmer cone. The ions are separated in the mass analyzer according to their charge to mass ratio. The ions are converted at a conversion dynode and are detected by use of a secondary electron multiplier or a Faraday cup. From an analytical point of view, ICP-MS is a well-established method for multi-elemental analysis in particular for elements at trace- and ultra-trace levels. Furthermore, methods based on ICP-MS offer simple quantification concepts, for which usually (liquid) standards are applied, low matrix effects compared to other conventional analytical techniques, and relative limits of detection (LODs) in the low pg g−1 range and absolute LODs down to the attomol range. For these applications, ICP-MS excels by a high sensitivity which is independent of the molecular structure and a wide linear dynamic range. It has found acceptance in various application areas and during the last decade ICP-MS is also more and more applied for detection of rare earth elements particularly in the life sciences. Due to the fact that all molecules introduced into the high temperature of the plasma in the ion source were completely dissociated and broken down into atoms, which are subsequently ionized, all elemental species information is completely lost. However, if the different species are separated before they enter the plasma by using adequate fractionation or separation techniques, then ICP-MS can be used as a very sensitive element-specific detector. We will discuss this feature of ICP-MS in this chapter in more detail at hand of the speciation of gadolinium-containing contrast agents. KW - Analysis of lanthanoides KW - ICP-MS KW - Speciation of Gd-containing MRI contrast agents PY - 2016 UR - http://adsabs.harvard.edu/abs/2016PhSRv...1...58T DO - https://doi.org/10.1515/psr-2016-0058 SN - 2365-659X SN - 2365-6581 VL - 1 IS - 11 SP - id. 58, 1 EP - 20 AN - OPUS4-40176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online spectroscopy in microemulsions – A process analytical approach for a hydroformylation mini-plant N2 - Within the Collaborative Research Center InPROMPT a novel process concept for the hydroformylation of long-chained olefins is studied in a mini-plant, using a rhodium complex as catalyst in the presence of syngas. Recently, the hydroformylation in micro¬emulsions, which allows for the efficient recycling of the expensive rhodium catalyst, was found to be feasible. However, the high sensitivity of this multi-phase system with regard to changes in temperature and composition demands a continuous observation of the reaction to achieve a reliable and economic plant operation. For that purpose, we tested the potential of both online NMR and Raman spectroscopy for process control. The lab-scale experiments were supported by off-line GC-analysis as a reference method. A fiber optic coupled probe of a process Raman spectrometer was directly integrated into the reactor. 25 mixtures with varying concentrations of olefin (1-dodecene), product (n-tridecanal), water, n-dodecane, and technical surfactant (Marlipal 24/70) were prepared according to a D-optimal design. Online NMR spectroscopy was implemented by using a flow probe equipped with 1/16” PFA tubing serving as a flow cell. This was hyphenated to the reactor within a thermostated bypass to maintain process conditions in the transfer lines. Partial least squares regression (PLSR) models were established based on the initial spectra after activation of the reaction with syngas for the prediction of unknown concentrations of 1-dodecene and n-tridecanal over the course of the reaction in the lab-scale system. The obtained Raman spectra do not only contain information on the chemical composition but are further affected by the emulsion properties of the mixtures, which depend on the phase state and the type of micelles. Based on the spectral signature of both Raman and NMR spectra, it could be deduced that especially in reaction mixtures with high 1-dodecene content the formation of isomers as a competitive reaction was dominating. Similar trends were also observed during some of the process runs in the mini-plant. The multivariate calibration allowed for the estimation of reactants and products of the hydroformylation reaction in both laboratory setup and mini-plant. T2 - 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) CY - Potsdam, Germany DA - 10.05.2017 KW - Process analytical technology KW - Online NMR spectroscopy KW - Online Raman spectroscopy KW - Microemulsions PY - 2017 AN - OPUS4-40185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illner, M. T1 - Operation and optimal control of multiphase systems – Hydroformylation in microemulsions on the mini-plant scale N2 - develops new process concepts, involving innovative tuneable solvent systems to enable rather difficult or inapplicable synthesis paths. One possible concept is the hydroformylation of long-chained alkenes in microemulsions. For this, a modular mixer-settler concept was proposed, combining high reaction rates and efficient catalyst recycling via the application of technical grade surfactants. The feasibility of such a concept is evaluated in a fully automated, modular mini-plant system within which the characteristics of such a multiphase system pose several obstacles in operating this mini-plant. Maintaining a stable phase separation for efficient product separation and catalyst recycling is complicated by small and highly dynamic operation windows as well as poor measurability of component concentrations in the liquid phases. In this contribution, a model-based strategy is presented to enable concentration tracking and phase state control within dynamic mini-plant experiments. Raman spectroscopy is used as an advanced process analytical tools, which allows for online in-situ tracking of concentrations. Combined with optical and conductivity analysis optimal plant trajectories can be calculated, solving a dynamic optimization problem under uncertainty. Applying these, a stable reaction yield of 40 % was achieved, combined with an oil phase purity of 99,8 % (total amount of oily components in the oil phase) and a catalyst leaching below 0.1 ppm. T2 - 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) CY - Potsdam, Germany DA - 10.05.2017 KW - Process monitoring KW - Hydroformylation KW - Mini-plant KW - Process control KW - Process analytical technology KW - EuroPACT KW - InPROMPT PY - 2017 UR - http://dechema.de/en/europact17.html AN - OPUS4-40233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Telgmann, L. A1 - Lindner, U. A1 - Lingott, J. A1 - Jakubowski, Norbert ED - Prof. Dr. Golloch, Alfred T1 - Analysis and speciation of lanthanoides by ICP-MS N2 - Inductively coupled plasma mass spectrometry (ICP-MS) is based on formation of positively charged atomic ions in a high-frequency inductively coupled Argon plasma at atmospheric pressure. The ions are extracted and transferred from the plasma source into a mass analyzer operated at high vacuum via an interface equipped with a sampling and a skimmer cone. The ions are separated in the mass analyzer according to their charge to mass ratio. The ions are converted at a conversion dynode and are detected by use of a secondary electron multiplier or a Faraday cup. From an analytical point of view, ICP-MS is a well-established method for multi-elemental analysis in particular for elements at trace- and ultra-trace levels. Furthermore, methods based on ICP-MS offer simple quantification concepts, for which usually (liquid) standards are applied, low matrix effects compared to other conventional analytical techniques, and relative limits of detection (LODs) in the low pg g−1 range and absolute LODs down to the attomol range. For these applications, ICP-MS excels by a high sensitivity which is independent of the molecular structure and a wide linear dynamic range. It has found acceptance in various application areas and during the last decade ICP-MS is also more and more applied for detection of rare earth elements particularly in the life sciences. Due to the fact that all molecules introduced into the high temperature of the plasma in the ion source were completely dissociated and broken down into atoms, which are subsequently ionized, all elemental species information is completely lost. However, if the different species are separated before they enter the plasma by using adequate fractionation or separation techniques, then ICP-MS can be used as a very sensitive element-specific detector. We will discuss this feature of ICP-MS in this chapter in more detail at hand of the speciation of gadolinium-containing contrast agents. KW - Analysis of lanthanoides KW - ICP-MS KW - Speciation of Gd-containing MRI contrast agents PY - 2017 SN - 978-3-11-036523-8 SP - Chapter 5, 124 EP - 144 PB - De Gruyter AN - OPUS4-40238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 14, Ausgabe 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2006 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 14 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40199 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Bewertung von Anzeigen in Faserverbundwerkstoffen mit aktiver Thermographie und Ultraschall N2 - Es wurden ausgewählte Ergebnisse aus dem EU-Vorhaben VITCEA vorgestellt. T2 - Sitzung des Fachausschusses Faserverbundwerkstoffe der DGZfP CY - Stade, Germany DA - 11.5.2017 KW - Faserverbundwerkstoffe KW - Ultraschallprüfung KW - Thermographie PY - 2017 AN - OPUS4-40202 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 14, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 14, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2006 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 14 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40204 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 15, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 15, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2007 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 15 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40205 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Improved Deposition of Nanoparticles vy Electrospray Analaysis with SEM/TEM and EDS N2 - Although there are many experimental techniques for measuring particle sizes and size distributions, electron microscopy (EM) is still considered as the gold standard in this field, especially when it comes to particle sizes in the nanorange (1 nm – 100 nm). Furthermore, high-resolution X-ray spectroscopy (EDS) can be applied to individual nanoparticles. To be able to extract accurate information from the EM micrographs and EDS elemental maps that are representative for the material under investigation, one needs to assure the representativity of the particles as sampled on the substrate and their homogeneous spatial distribution, to avoid operator bias when selecting the imaged area. Furthermore, agglomeration should be avoided as far as possible. Several sample preparation techniques exist since a long time, the most common way being suspending the particles in a liquid and depositing them on the grid. However, this procedure includes the drying of larger solvent amounts on the substrate itself, which can affect the spatial distribution of the deposited particles. One possibility to overcome this problem is the use of an electrospray system, where the suspension of particles is sprayed onto the substrate in charged droplets that are so small that they either dry off on the substrate immediately without affecting the position of particles, or even already during their flight time to the substrate. No dedicated commercial instruments are available for the preparation of TEM grids yet, only electrostatic deposition of aerosols on TEM grids has been reported so far. To test the prototype and assess its performance, several materials have been sprayed onto TEM grids and the resulting particle distributions were compared to more traditional sample preparation strategies like the “drop on grid” method. Operation parameters such as the sample flow-rate, capillary – substrate distance, electric field strength and sampling period length have been optimised. It was found that the particles deposited by electrospray generally show a much more homogeneous spatial distribution on the substrate and a substantial increase of the number of single particles, which are much better suited to an automatic image evaluation procedure than the agglomerated particles observed otherwise. The applicability of the technique to a broad range of materials is demonstrated by various examples, but also the influence of the substrate, the choice of the particular TEM grid, on the obtained spatial particle distribution is assessed. T2 - EMAS 2017 - 15th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS and IUMAS-7 Meeting CY - Konstanz, Germany DA - 07.05.2017 KW - Electrospray deposition KW - TEM grids KW - Nanoparticles KW - Agglomeration PY - 2017 AN - OPUS4-40257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - Kratzbeständigkeit – Prüfmethoden und deren Praxistauglichkeit N2 - Der Vortrag widmet sich modifizierten Oberflächen zur Erhöhung der Kratzbeständigkeit sowie entspre-chenden Prüfmethoden und bewertet deren Praxis-tauglichkeit. Nach einer Übersicht zu Begriffen und Definitionen wird die wirtschaftliche Bedeutung der Kratzbeständigkeit aufgezeigt. Neben generellen Anforderungen an Mess-und Prüfverfahren hinsicht-lich Einsatzbereichen, Messunsicherheit und Validie-rung werden diverse Verfahren zur Erzeugung und Bewertung Einzel- und Vielfach-Kratzern nebst ent-sprechenden Normen vorgestellt. Die analytische Charakterisierung, werkstofftechnische Gesichts-punkte und eine Zusammenstellung aktuell gültiger Normen zur Kratzbeständigkeit schließen den Vortrag ab. T2 - Seminar: Modifikation der Kratz- und Abriebsbeständigkeit von Kunststoffen CY - SKZ – KFE GmbH Peine, Germany DA - 09.05.2017 KW - Kunststoff-Oberflächen KW - Kratzbeständigkeit KW - Härte KW - Abrieb KW - Prüfverfahren KW - Normung PY - 2017 AN - OPUS4-40258 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietzsch, Michael A1 - Andrusenko, Iryna A1 - Branscheid, Robert A1 - Emmerling, Franziska A1 - Kolb, Ute A1 - Tremel, Wolfgang T1 - Snapshots of calcium carbonate Formation - a step by step analysis N2 - Recent advances in our understanding of CaCO, nucleation from solution have provoked new and challenging questions. We have studied CaC03 formation using precipitation by carbonate ester hydrolysis which ensures precipitation from a strictly homogeneous solution state and allows “titrating” carbonate to a solution with a given Ca2+ concentration on a timescale suited for kinetic studies. Nucleation and crystallization were traced by combining dynamic light Scattering (DLS) and transmission electron microscopy (TEM). DLS served as in situ technique to identify the nucleation time, to monitor particle size evolution, to discriminate different precipitation mechanisms and to validate reproducibility. TEM snapshots taken during different stages of the precipitation process identified different phases and morphologies. At a high level of supersaturation homogeneous nucleation in solution led to the formation of amorphous CaC03 particles (diameter=30 nm), which transformed via vaterite to calcite. Nucleation occurred uniformly in solution which appears to be unique for the CaC03 System. In the presence of Na-polymethacrylate (Na-PMA), heterogeneous nucleation was suppressed and Ca-polymer aggregates were formed in the prenucleation stage. Beyond a critical threshold supersaturation CaC03 particles formed in solution outside of these aggregates. The nucleation process resembled that without additive, indicating that Na-PMA exerts only a minor effect on the CaC03 nucleation. In the postnucleation stage, the polymer led to the formation of extended liquid-like networks, which served as a precursor phase for solid ACC particles that formed alongside the network. KW - biomineralization KW - calcium carbonate KW - nucleation KW - polymer additives PY - 2017 DO - https://doi.org/10.1515/zkri-2016-1973 SN - 2194-4946 SN - 2196-7105 VL - 232 IS - 1-3 SP - 255 EP - 265 PB - De Gruyter CY - Berlin AN - OPUS4-39863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 22. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik: Polyzyklische aromatische Kohlenwasserstoffe (PAK) in Boden, Mineralölkohlenwasserstoffe (MKW) in Boden, Elemente in Sediment und Gesamtcyanid in Boden. KW - Eignungsprüfung KW - Boden KW - Spurenelemente KW - Gesamtcyanid KW - MKW KW - PAK PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-398676 SP - 1 EP - 261 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39867 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 2, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 2, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1994 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 2 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39955 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija T1 - NDE reliability and the influence of human factors N2 - The presentation highlights the need for human factors research in the field of non-destructive testing (NDT) and presents a review of factors affecting human performance in NDT with examples of own research studies and previous studies in the field. T2 - IAEA Technical Meeting on the Optimization of Non-Destructive Examination and In-Service Inspection to Improve Nuclear Power Plant Performance CY - Espoo, Finland DA - 04.04.2017 KW - Human factors KW - Non-destructive testing KW - Reliability KW - Nuclear PY - 2017 UR - https://www.iaea.org/NuclearPower/Meetings/2017/2017-04-04-04-07-NPES.html UR - https://www.iaea.org/NuclearPower/Downloadable/Meetings/2017/2017-04-04-04-07-NPES/1_NDE_Reliability_and_the_influenceof_human_factors_Marija_Bertovic.pdf AN - OPUS4-39956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Mirtschin, Nikolaus T1 - Thermomechanisches Verhalten von semikristallinem Polyester-Urethan N2 - Formgedächtnispolymere werden durch thermomechanische Vorbehandlung, die Programmierung, in eine temporäre Form überführt. In die Ursprungsform kehren sie dann erst nach externer Stimulierung, durch Auslösen des Formgedächtniseffekts, wieder zurück. Um diesen Effekt zu optimieren, werden in dieser Arbeit thermomechanische Designoptionen analysiert und Stellschrauben der Programmierung diskutiert. Quantifiziert wird das Materialverhalten eines physikalisch vernetzten Polyurethans mit semikristalliner Polyester-Weichsegmentphase (PEU) in thermomechanischen Messungen, in denen das Polymer Dehnungen bis über 1000% fixiert. Deformationen im breiten Schmelzübergangsbereich der Weichsegmentphase ermöglichen die präzise Kontrolle über die Temperaturen der Dehnungs- und Spannungsrückstellung, den bekannten Temperaturgedächtniseffekt (TGE). Erst durch eine neuartige Programmierung wird jedoch der Beginn der Rückstellung einstellbar. Für diesen Onset-TGE wird das PEU direkt nach dem Recken entlastet und danach unter die Kristallisationstemperatur abgekühlt. In situ Röntgenstreuung zeigt, dass durch den frühen Entlastungszeitpunkt nur der Teil der kristallinen Weichsegmentphase zur Fixierung beiträgt, der auch beim Recken kristallin ist. Die Kristallinität bietet daher eine Stellschraube, um das thermomechanische Verhalten zu veredeln. Über die Optimierungsparameter Reckrate, Temperaturhaltezeit und maximale Dehnung erzielt das PEU hohe Fixierbarkeiten und Rückstellspannungen, ohne die Rückstellung und den Onset-TGE zu beeinträchtigen. Durch die Erweiterung der Programmierung des Onset-TGEs hin zu einer zweiten Deformation und Entlastung innerhalb des Schmelzübergangs zeigt das PEU einen bisher nicht berichteten zweistufigen Spannungsanstieg während der Rückstellung. Ein Temperaturlimit für den Onset-TGE stellt die Peak-Schmelztemperatur aus der dynamischen Differenzkalorimetrie dar. Durch die verbleibende Kristallinität oberhalb dieser Temperatur führt die Deformation und Entlastung direkt zur thermoreversiblen Aktuation mit Dehnungsänderungen bis zu 28%. Die Ergebnisse werden auf einen Miniaturisierungsansatz für schaltbare Informationsträger übertragen, mit denen eine maschinenlesbare Information von nichtlesbar nach lesbar geschaltet werden kann. In einer Machbarkeitsstudie wird der für Sensoranwendungen vielversprechende Onset-TGE genutzt, um die Lesbarkeit der Informationsträger bei einer vordefinierten Temperatur zu schalten. Das erweitert das potentielle Anwendungsfeld der Technologie vom Produkt- und Markenschutz zur Überwachung von Kühlketten. N2 - Shape memory polymers are able to change their shape upon application of an external stimulus. This behavior requires a thermomechanical treatment, so-called programming, to establish a temporary shape. To optimize the shape memory performance, thermomechanical design options will be analyzed and programming parameters discussed in the present thesis. The material behavior of a physically crosslinked polyurethane with semicrystalline polyester soft segments (PEU) is quantified by thermomechanical measurements, where the polymer fixes strains of above 1000%. The deformation within the broad melting transition of the soft segment phase enables the precise control over the temperatures of strain and stress recovery, also known as temperature-memory effect (TME). But only the herein introduced programming route, consisting in elongation and unloading prior to cooling below the crystallization transition, allows for fine-tuning the beginning of recovery. For the resulting onset-TME in situ X-ray scattering indicates that only soft segment crystals contribute to fixation, which are crystalline during deformation. Therefore, the crystallinity opens the door for gaining precisely control over the thermomechanical behavior. Optimization parameters for reaching high strain fixities and recovery stresses without compromising recovery nor the onset-TME are found in the strain rate, temperature holding time and maximum strain. When extending the programming route for onset-TMEs towards a second deformation and unloading step of PEU within the melting transition, an unreported two-step stress recovery is rendered possible. However, the peak melting temperature determined from differential scanning calorimetry represents a temperature limit for the onset control. Through the residual crystallinity above that temperature, deformation and unloading yield thermoreversible actuation with strain changes up to 28%. The findings are transferred to a miniaturization approach for switchable information carriers for switching encoded information from machine-unreadable to readable. In a proof-of-concept study the onset-TME – promising for sensor applications – can be exploited in order to predefine a temperature threshold value for readability of information carriers. This behavior widen their potential applicability from product and brand protection to cold chain supervision. T3 - BAM Dissertationsreihe - 156 KW - Formgedächtnispolymere KW - Temperaturgedächtnispolymere KW - Polyester-Urethan KW - Thermomechanische Eigenschaften KW - Programmierung PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-399648 SN - 978-3-9818270-5-7 SN - 1613-4249 VL - 156 SP - iii EP - 150 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39964 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kind, Thomas T1 - Amplitudes variation of GPR rebar reflection due to the influence of concrete aggregate scattering N2 - Dense GPR measurements of rebar reflection amplitudes Show relative variations, which can be in the order of more than 10% - 20%. Former investigations demonstrated that these variations are caused by the heterogeneity of concrete, i.e. due to the inclusion of aggregates in concrete. These amplitude variations make it difficult to analyse single reflection amplitudes in order to determine the rebar diameter or to estimate the concrete deterioration state. In a systematic study we have quantified the statistical variation of the rebar reflection amplitude for concrete covers of 6 cm, 9 cm, 12 cm, 15 cm and 18 cm, for two different grading curves and for the rebar diameters 12 mm and 28 mm. Also the influence of the wavelength has been investigated by using antennas with different centre frequencies in relation to the aggregate size. The results are discussed with regard to a quantitative amplitude evaluation of GPR measurements and also the potential of using these variations for a characterization of concrete material properties. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - Ground penetrating radar KW - Concrete KW - Rebar KW - Aggregate scattering PY - 2015 UR - http://www.ndt.net/?id=18402 SN - 1435-4934 VL - 20 IS - 11 SP - 412 EP - 420 PB - NDT.net CY - Kirchwald AN - OPUS4-40007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Würth, Christian T1 - Scattering of Particles N2 - Introduction to theory and applications of light scattering T2 - Cost-action Training school CY - Turku, Finland DA - 03.04.2017 KW - Light scattering PY - 2017 AN - OPUS4-40010 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Konopelko, L.A. A1 - Kolobova, A.V. A1 - Rozhnov, M.S. A1 - Melnyk, D.M. A1 - Petryshyn, P.V. A1 - Shpilnyi, S.A. A1 - Iakubov, S.E. A1 - Bakovec, N. V. A1 - Kluchits, A.S. A1 - Kipphardt, Heinrich A1 - Aleksandrov, V. V. T1 - COOMET.QM-S5 (COOMET project № 576/RU/12) : “Supplementary comparison of national standards in the field of analysis of gas mixtures containing СО2, СО, С3Н8 in nitrogen (“automotive” gas mixtures)” N2 - The relevance of the COOMET.QM-S5 comparison is founded on tightening of requirements to a control of automobile emissions (realization of environmental standards of EURO 4, EURO-5). Participating laboratories: VNIIM, BAM, BelGIM, Ukrmetrteststandart, KazInMetr. This comparison was carried out in 2013-2014. This supplementary comparison supports CMC claims for: CO2 in the range (4–16) 10⁻² mol/mol; CO in the range (0.5–5) 10⁻² mol/mol; C3H8 in the range (0.01–0.3) 10⁻² mol/mol. Results: Component CO: All laboratories identified the values of carbon monoxide mole fraction in the gas mixture within ±0.9134%. Component CO2: All laboratories identified the values of carbon dioxide mole fraction in the gas mixture within ±0.3042%. Component C3H8: All laboratories identified the values of propane mole fraction in the gas mixture within ±0.443%. KW - COOMET.QM-S5 KW - Gas analysis PY - 2016 UR - http://kcdb.bipm.org/appendixB/KCDB_ApB_info.asp?cmp_idy=1401&cmp_cod=COOMET.QM-S5&prov=exalead SN - 1681-7575 SN - 0026-1394 VL - 53 IS - Technical Supplement SP - Article 08004, 1 EP - 33 PB - IOP publishing AN - OPUS4-40015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 8, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 8, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2000 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 8 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40018 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 2, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 2, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1994 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 2 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40019 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 3, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 3, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 1995 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 3 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40020 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 8, Ausgabe 3 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 8, edition 3 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2000 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 8 IS - 3 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40021 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 9, Ausgabe 1 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 9, edition 1 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2001 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 9 IS - 1 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40022 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 9, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 9, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2001 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 9 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40023 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Wloka, Monika T1 - DAR-aktuell - Kurzinformation - Akkreditierung, Zertifizierung, Prüfung - Jahrgang 10, Ausgabe 2 T1 - DAR-aktuell - newsletter - accreditation, certification, testing - volume 10, edition 2 N2 - Die hier vorliegende Kurzinformation hat das Ziel, über Neues auf dem Gebiet der Akkreditierung, Zertifizierung und Prüfung in Deutschland und Europa sowie über Inhalte und Ergebnisse der Arbeit verschiedener auf diesem Sektor tätigen Organisationen zu informieren. N2 - The aim of this newsletter is to inform about new developments in the area of accreditation, certification and testing in Germany and Europe as well as about topics and results of the work of several organisations that are active in this sector. PY - 2002 SN - 1436-154X SN - 1436-1558 SN - 1436-2082 N1 - Volltext (PDF) in deutsch und englisch - Full text (PDF) in German and English VL - 10 IS - 2 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40025 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - „Prozess-Sensoren 4.0“ – Chancen für neue Automatisierungskonzepte und neue Geschäftsmodelle in der Prozessindustrie N2 - Prozess-Sensoren 4.0 vereinfachen ihre Einbindung über Plug and Play, obwohl sie komplexer werden. Sie bieten Selbstdiagnose, Selbstkalibrierung und erleichterte Parametrierung. Über die Konnektivität ermöglichen die Prozess-Sensoren den Austausch ihrer Informationen als Cyber-physische Systeme mit anderen Prozess-Sensoren und im Netzwerk. Der Aufbruch von der aktuellen Automation zum smarten Sensor hat bereits begonnen. Automatisierungstechnik und Informations- und Kommunikationstechnik (IKT) verschmelzen zunehmend. Wenn die Prozessindustrie dieses nicht definiert, tun es andere. Für die weitere Entwicklung von der Ist‐Situation zu einer Industrie-4.0-Welt in der Prozessindustrie werden mehrere Szenarien diskutiert. Diese reichen vom erleichterten Abruf sensorbezogener Daten über zusätzliche Kommunikationskanäle zwischen Sensor und mobilen Endgeräten über vollständig bidirektionale Kommunikation bis hin zur Einbindung der Cloud und des Internets in virtualisierte Umgebungen. Um zu einer störungsfreien Kommunikation aller Sensoren untereinander zu kommen, muss mindestens ein einheitliches Protokoll her, das alle Sensoren sprechen und verstehen. Der derzeit greifbarste offengelegte Standard, der moderne Kommunikationsanforderungen erfüllt, ist OPC Unified Architecture (OPC-UA). Viele halten das Sortieren der Kommunikationsstandards für eines der wesentlichen Errungenschaften von Industrie 4.0. Eine Topologie für smarte Sensoren, das Zusammenwirken mit daten- und modellbasierte Steuerungen bis hin zur Softsensorik sowie weitere Anforderungen an Sensoren sind jedoch heute noch nicht angemessen beschrieben. Wir müssen jetzt schnell die Weichen für eine smarte und sichere Kommunikationsarchitektur stellen, um zu einer störungsfreien Kommunikation aller Sensoren auf Basis eines einheitlichen Protokolls zu kommen, welches alle Sensoren ausgeben und verstehen. Aktuelle und zukünftige öffentliche Förderung von Industrie 4.0-Projekten sind eine gute Investition. Wegen der hohen Komplexität und Interdisziplinarität gelingt die Umsetzung nur gemeinsam zwischen Anwendern aus der Prozessindustrie, Software- und Geräteherstellern und Forschungsgruppen. Anwender sind gefragt, diese neue Technologie durch eine beschleunigte Validierung und Akzeptanz umzusetzen. Sie erhalten die einzigartige Chance, ihre Prozesse und Anlagen wettbewerbsfähig zu halten. Kooperativ betriebenen F&E-Zentren und gemeinsam anerkannten Applikationslaboren kommt dafür eine hohe Bedeutung zu. T2 - Tagung Industrie 4.0 - "Safety und Security - Mit Sicherheit gut vernetzt", Hochschule für Technik und Wirtschaft CY - Berlin, Germany DA - 28.04.2017 KW - Prozessanalytik KW - Prozess-Sensoren 4.0 KW - Prozessindustrie KW - Smarte Sensoren KW - Automation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-400262 AN - OPUS4-40026 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Isleyen, A. T1 - Matrix reference materials for environmental analysis N2 - Reliable analysis of chemical indicators in water, sediment and soil samples for the purpose of environmental pollution assessment poses one of the greatest analytical challenges, having in mind the complexity of sample matrix and low concentrations of pollutants. Organics (pesticides, PAHs, PFOS, etc.) and heavy metals (Hg, Cd, Ni, Pb and As) represent target parameters. Laboratories performing sampling and tests in this field regulated by respective EU directives, need strong support in order to establish a quality system. It is necessary to provide appropriate calibrators i.e. matrix CRMs relates to the unique sample matrices representing typical samples in the geomorphological and anthropological sense. In addition to that, bearing in mind the complexity and instability of environmental samples, it is very difficult to obtain appropriate referents materials with no local providers. Our project is aiming to develop capacity to produce CRMs for environmental analysis by transferring the theoretical and practical know-how between the partners and combining their skills to focus on environmental CRM production in accordance with ISO Guide 34. Our project will have an impact on environmental monitoring in the partnering countries and on the scientific community, who will use the newly developed reference materials. Furthermore, partners will develop strategies for producing new CRMs either on their own or in cooperation. This will lead to regional CRM producers serving scientific and official laboratories. T2 - 2nd International Congress of Chemists and Chemical Engineers of Bosnia and Herzegovina CY - Sarajevo, Bosnia and Herzegovina DA - 21.10.2016 KW - CRM KW - Environmental analysis KW - Quality system PY - 2016 AN - OPUS4-40028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - IDMS Training N2 - Based on its proven records especially in reference material certification, isotope dilution mass spectrometry (IDMS) is considered as one of the most powerful and most accurate methods for determining amounts of substance. Contrary to other calibration approaches, IDMS does not directly suffer from long-time changes or drifts in instrument sensitivity. Moreover, provided isotopic exchange between the sample and spike is ensured, losses of analyte do not affect the analytical result. Both advantages are based on the fact that IDMS only requires isotope ratio measurements and isotope ratios are largely unaffected by instrumental drift, setup or by matrix, unless an isobaric interference is present. The Consultative Committee for Amount of Substance (CCQM), the world's highest institution for metrology in chemistry, considers IDMS as the most important “Primary Method of Measurement” for amount determination. The total combined uncertainty, according to ISO and EURACHEM guidelines, can easily be calculated via the IDMS equations. Applying it correctly, IDMS has the potential to be a primary method of measurement yielding SI traceable values in the most direct way with combined uncertainties significantly smaller than obtainable by other methods. In general it can be stated that IDMS is the most important reference method for elemental and elemental species analysis, offering highest accuracy and precision or smallest measurement uncertainties, when properly applied. Thus IDMS represents by far the best suited reference method for RM characterisation. Due to its universal applicability IDMS offers sufficient potential to follow future needs in analytical chemistry as well as in the RM sector. This presentation will demonstrate the basic principle of IDMS and will show its Pros and Cons as well as its pitfalls. Possible sources of errors and bias are mentioned and correction models will be discussed. Notice will be given to metrological aspects such as traceability and uncertainty. Differences in the application of thermal ionization mass spectrometry and inductively coupled plasma mass spectrometry are discussed as well as differences between different types of mass spectrometers. This will be illustrated by practical examples from various fields. T2 - Workshop and practical training on isotope dilution mass spectrometry CY - Berlin, Germany DA - 22.02.2016 KW - Isotope dilution mass spectrometry KW - Primary method of measurement KW - Certification PY - 2016 AN - OPUS4-40029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Isotope analysis N2 - The variation of isotope ratios is increasingly used to unravell natural and technical questions. In the past the investigation and interpretation of such variations was the field of a limited number of experts. With new upcoming techniques and research topics in the last decades, such as provenance and authenticity of food, the number of published isotope data strongly increased. Instrumental developments such as the enhancement of inductively coupled plasma mass spectrometers (ICPMS) from an instrument for simple quantitative analysis to highly sophisticated isotope ratio machines influenced this process significantly. While in former times only experts in mass spectrometry were able to produce reliable isotope data, nowadays many laboratories, never been in touch with mass spectrometry before, produce isotope data with an ICPMS. Especially for such user isotope reference materials (IRM) are indispensible to enable a reliable method validation. The fast development and the broad availability of ICPMS also lead to an expansion of the classical research areas and new elements are under Investigation. This presentation shows the basics and principles for isotope ratio determination using ICP-MS. Additionally, it provides three specific examples for isotope Ratio applications: isotope dilution mass spectrometry; provenancing of archaeoligical artifeacts by lead isotope Ratio Analysis and studies on boron uptake in bell pepper plants. T2 - ICP-MS Kurs (BAM Akademie) CY - Berlin, Germany DA - 19.04.2017 KW - Lead isotopes KW - Delta values KW - Boron isotopes KW - Archaeology KW - Plant metabolism PY - 2017 AN - OPUS4-40030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Implementation of ISO Guide 34 into the quality management system of BAM N2 - Presentation of the BAM quality management System with focus on the ISO Guide 34 implementation. This presentation is one part of the re-evaluation of BAM carried out by the Technical Committee of EURAMET. T2 - TC-Q Meeting CY - Dublin, Ireland DA - 12.04.2017 KW - Quality system KW - Re-evaluation KW - Metrology in chemistry KW - EURAMET KW - CCQM PY - 2017 AN - OPUS4-40031 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schäferling, Michael T1 - Sensing and Imaging of Intracellular pH Using Photon Upconversion Based Nanoprobes N2 - Sensing of intracellular pH is of particular interest in biomedical research since structure and function of biomolecules strongly depend on the concentration of protons in their environment. We have functionalized photon upconversion nano-particles (UCNPs) with pH responsive dyes to achieve nanoprobes for intracellular pH determination. The sensing mechanism is based on a resonance energy transfer (UC-RET) from the 550 nm emission of hexagonal nanocrystals of NaYF4: Yb3+,Er3+ to the pH-sensitive fluorophore pHrodoTM Red. The nanocrystals were coated with thin shells of aminosilane or highly branched polyethylenimine (PEI) with several nanometer layer thickness for coupling of the pH indicator. The nanoprobes are calibrated by ratiometric dual wavelength readout at 550 nm (reference signal) and 590 nm (sensor signal) and visualized using a scanning confocal fluorescence microscope with 980 nm excitation wavelength. It was found that PEI coating enables a higher coupling of indicator molecules on the particle surface, better signal to reference ratios in ratiometric readout and an improved cellular uptake compared to the aminosilane coated particles due to a more positive zeta potential. We studied the cellular uptake efficacy of the nanoprobes and determined to which type of compartment, lysosomes, endosomes or cytosol, the probes are targeted to by measuring the pH of their microenvironment. An in situ control was performed in live cells by a treatment with nigericin, whereby the pH of all intracellular compartments is set at extracellular level. Finally, we will show new strategies for the preparation of UCNP-dye conjugates with improved UC-RET efficiency to achieve higher acceptor (sensor) emission. T2 - 1st European / 10th German Biosensor Symposium CY - Potsdam, Germany DA - 20.03.2017 KW - Photon Upconversion KW - Nanoprobes KW - Chemical Sensing KW - PH KW - Live cell imaging PY - 2017 AN - OPUS4-40032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kage, Daniel T1 - Dye-stained lifetime-encoded polymer microbeads for application in time-resolved flow cytometry N2 - Flow cytometry is a standard analytical tool for biological research and in medical applications. There are different requirements triggering recent device and method development depending on the desired field of application. One trend is governed by the need for an increasing number of simultaneously detectable codes, i.e., fluorescent labels. The other one focuses on cost-effective methods and development of miniaturized, portable devices. Fluorophore encoding is usually based on spectral encoding. However, this approach is hampered by, e.g., spectral crosstalk. Additionally, the sensitivity of fluorescence intensity measurements to fluctuations in excitation light intensity and dye concentration limits the achievable number of detection channels. Moreover, spectral multiplexing typically requires several costly excitation light sources. Lifetime multiplexing and the discrimination between different encoding fluorophores and carrier beads based on their fluorescence decay kinetics could present an innovative alternative. Encoded beads, i.e., beads with lifetime codes corresponding to the surface chemistry, have been employed to evaluate the feasibility of this approach with a custom designed flow cytometer equipped with a pulsed light source and a fast detector for time-resolved measurements in a flow. In a first step, we used steady state and time-resolved photoluminescence measurements for the spectroscopic characterization of micrometer-sized dye-stained PMMA beads. Subsequently, the potential use of these microbeads for flow cytometry applications was analyzed with a prototype flow cytometer with lifetime detection. With our proof-of-concept studies, we could demonstrate that lifetime discrimination and simultaneous readout of a ligand fluorescence signal for analyte quantification is feasible with a set of dye-stained polymer microbeads at single wavelength excitation. These studies are expected to pave the road for new applications of fluorescence lifetime multiplexing in time-domain flow cytometry and bead-based assays in general. T2 - DBS/EBS 2017 CY - Potsdam, Germany DA - 20.03.2017 KW - Flow cytometry KW - Fluorescence KW - Life sciences KW - Lifetime encoding KW - Polymer particles PY - 2017 AN - OPUS4-39996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Bach, S. A1 - Gorelik, T. A1 - Kolb, U. A1 - Tremel, W. A1 - Emmerling, Franziska T1 - Divalent metal phosphonates – new aspects for syntheses, in situ characterization and structure solution N2 - Divalent metal phosphonates are promising hybrid materials with a broad field of application. The rich coordination chemistry of the phosphonate linkers enables the formation of structures with different dimensionalities ranging from isolated complexes and layered structures to porous frameworks incorporating various functionalities through the choice of the building blocks. In brief, metal phosphonates offer an interesting opportunity for the design of multifunctional materials. Here, we provide a short review on the class of divalent metal phosphonates discussing their syntheses, structures, and applications. We present the advantages of the recently introduced mechanochemical pathway for the Synthesis of divalent phosphonates as a possibility to generate new, in certain cases metastable compounds. The benefits of in situ investigation of synthesis mechanisms as well as the implementation of sophisticated methods for the structure analysis of the resulting compounds are discussed. KW - Metal phosphonate KW - Mechanochemistry PY - 2017 DO - https://doi.org/10.1515/zkri-2016-1971 SN - 2194-4946 SN - 2196-7105 VL - 232 IS - 1-3 SP - 209 EP - 222 PB - De Gruyter AN - OPUS4-40003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Behnke, Thomas T1 - Spectroscopic quantification of surface groups on micro- and nanoparticles N2 - Nanometer- and micrometer-sized particles are of increasing importance for a wide range of applications in the material and life sciences. This includes carriers for, e.g., drugs as well as dye molecules for use as multichromophoric reporters for signal enhancement in optical assays, platforms for DNA sequencing, and the fabrication of nanosensors and targeted probes for bioimaging studies. Application-relevant properties of such particles include their size (and size distribution), shape, colloidal stability, biocompatibility, and ease of subsequent functionalization, e.g., with linkers, sensor molecules, and targeting ligands. The latter requires knowledge of the number of groups effectively accessible for subsequent coupling reactions and hence, selective and sensitive methods of analysis, which can be ideally employed for the characterization of a broad variety of particle systems independent of their optical properties, i.e., scattering or the presence of encoding dyes. For product control, robust, reliable and fast methods performable with inexpensive equipment are prefered. In this respect, we studied a variety of conventional labels for optical readout, utilizing changes in intensity and/or color of absorption and/or emission. In addition, we developed a platform of cleavable and multimodal labels for optical assays which consist of a cleavable linker and an optically active reporter moiety. In contrast to conventional reporters measured directly at the particle surface, which are prone to signal distortions by scattering and encoding dyes, these cleavable labels can be detected colorimetrically or fluorometrically both bound at the particle surface and after quantitative cleavage of the linker in the transparent supernatant. Moreover, they enable straightforward validation by method comparison with elemental analysis, ICP-OES or ICP-MS. Here, we present representative examples of newly synthesized cleavable labels and their application for the quantification of amino, thiol and carboxy surface groups on different nanomaterials and compare these results with measurements using conventional optical labels. T2 - 253rd ACS National Meeting CY - San Francisco, CA, USA DA - 02.04.2017 KW - Nanoparticles KW - Microparticles KW - Surface groups KW - Quantification KW - Cleavable linker PY - 2017 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-40004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trela, Christiane T1 - Ground penetrating radar in reflection vs transmission mode for void detection in concrete structures N2 - The concreting of prefabricated concrete structures can lead to insufficient bonding or even to remaining cavities. Honeycombs (aggregate clusters without cement) represent potential weakening of the structure and need to be detected non-destructively. In our study we tested the capability of ground penetrating radar (GPR) techniques for this purpose. We applied GPR in reflection mode and zero-offset profiling (ZOP) transmission mode on a precast concrete twin wall with built-in honeycombs. GPR measurements were performed as two channel measurement with ground coupled antennas with centre frequencies of 1.5 GHz and 2.6 GHz mounted to an automated scanner system. Our findings show that ZOP transmission measurements are a more efficient method to detect voids in reinforced concrete structures compared to reflection mode measurements. This holds for both the effort needed for the measurement and the evaluation as well as the validity of the data. Honeycombs (basically representing voids) are usually characterized by strongly reduced amplitudes and earlier arrivals of the transmitted wave. T2 - International Symposium Non-Destructive Tesing in Civil Engineering (NDT-CE 2015) CY - Berlin, Germany DA - 15.09.2015 KW - Void detection KW - Ground penetrating radar KW - Reflection KW - Transmission KW - Reinforced concrete KW - Prefabricated wall PY - 2015 AN - OPUS4-40005 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trela, C. A1 - Kind, Thomas A1 - Günther, Martin T1 - Ground penetrating radar in reflection vs transmission mode for void detection in concrete structures N2 - The concreting of prefabricated concrete structures can lead to insufficient bonding or even to remaining cavities. Honeycombs (aggregate clusters without cement) represent potential weakening of the structure and need to be detected non-destructively. In our study we tested the capability of ground penetrating radar (GPR)techniques for this purpose. We applied GPR in reflection mode and zero-offset profiling (ZOP) Transmission mode on a precast concrete twin wall with built-in honeycombs. GPR measurements were performed as twochannel measurement with ground coupled antennas with centre frequencies of 1.5 GHz and 2.6 GHz mounted to an automated scanner system. Our findings show that ZOP transmission measurements are a more efficient method to detect voids in reinforced concrete structures compared to reflection mode measurements. This holds for both the effort needed for the measurement and the evaluation as well as the validity of the data. Honeycombs (basically representing voids) are usually characterized by strongly reduced amplitudes and earlier arrivals of the transmitted wave. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - Ground penetrating radar KW - Reflection KW - Transmission KW - Reinforced concrete KW - Prefabricated wall KW - Void detection PY - 2015 SN - 1435-4934 SP - 324 EP - 344 PB - Technische Universität Berlin / Bundesanstalt für Materialforschung und -prüfung CY - Berlin, Germany AN - OPUS4-40006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - CCQM-P149 Statistical evaluation of results N2 - The results for CCQM-P149 "Purity Determination of high purity zinc" are displayed and three different statistical approaches for the calculation of the reference value are compared. T2 - CCQM IAWG Meeting CY - Paris, France DA - 24.04.2017 KW - Purity KW - Metrology KW - Comparison KW - Impurities PY - 2017 AN - OPUS4-40033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen T1 - Roadmap for the purity determination of pure metallic elements N2 - High purity materials can serve as a realisation of the Système International d’Unitès (SI) unit amount of substance for the specific element. Solutions prepared from such high purity materials using gravimetric preparation and the concept of molar mass are used as calibration solutions in many fields of analytical chemistry. Calibration solutions prepared this way provide the traceability to the SI and are the metrological basis in elemental analysis. The preparation and characterization of such primary pure substances, representing the realisation of the SI unit amount of substance, is undertaken only by a small number of National Metrology Institutes (NMI) and Designated Institutes (DI). Many other NMIs and DIs, however, prepare elemental calibration solutions as calibrants for their measurement services, such as the certification of matrix Reference Materials or the provision of reference values for Proficiency Testing schemes. The elemental calibration solutions used for this purpose are not a direct service to customers, such as preparing secondary calibration solutions, but provide the source of traceability for the other services. Hence, it is necessary for the NMI or DI to obtain data on the purity of the pure metals or other materials used to prepare the solutions with measurement uncertainties meeting the needs of the above described services. This is commonly undertaken as a “fit for purpose” assessment, appropriate for the uncertainty requirement of the service provided to customers. As a consequence, total purity measurements are a long-term strategy of CCQM-IAWG. Several studies were conducted (CCQM-P107, CCQM-K72 and CCQM-P149) on the measurement of the purity of zinc. From these studies, several conclusions can be drawn for the purity assessment of a pure (metallic) element. These conclusions will be put together in this document in order to assist all NMIs/DIs in performing a purity assessment, whenever needed. T2 - CCQM IAWG Meeting CY - Paris, France DA - 24.04.2017 KW - CCQM KW - Metrology KW - Purity assessment PY - 2017 AN - OPUS4-40034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas T1 - Angewandte Raman-mikrospektroskopische Bildgebung in der Materialanalytik N2 - Ramanmikroskopie kombiniert den chemischen Informationsgehalt von Ramanspektren mit einer Ortsauflösung im Mikrometer- bis Sub-Mikrometerbereich und eignet sich daher hervorragend zur Analyse mikrostrukturell und chemisch komplexer Materialien. Zemente des 19. Jahrhunderts sind chemisch wie mikrostrukturell wesentlich komplexer als die heute aus definierten Rohmaterialien unter optimalen Bedingungen erbrannten Mörtelbinder. Der erstmalige Einsatz bildgebender Ramanmikroskopie im Bereich zementbasierter Materialien zeigte das Potential dieser Analytik auf. Gezieltes, flächendeckendes Abrastern von Klinkerrelikten in der hydratisierten Zementmatrix ermöglicht die Bestimmung von Silikaten, Aluminaten, Ferriten und anderer Phasen inklusive polymorpher Formen und Änderungen der Zusammen-setzung innerhalb von Mischkristallreihen und aufgrund des Einbaus von Fremdionen, wobei auch mikropartikuläre Bestandteile erfasst werden, deren Konzentrationen unter der Nachweisgrenze makroskopischer Analyseverfahren liegen. So lassen sich Rückschlüsse auf die verwendeten Rohmaterialien und die Herstellungsbedingungen ziehen, was die Bestimmung des verwendeten Zementtyps zulässt und damit Auswirkungen auf die Auswahl von Restaurierungsmaterialien hat. Möglichkeiten zur quantitativen Verteilungsanalyse von Kristallorientierungen und mechanischer Spannungen zeigten sich bei der Untersuchung von Dünnschicht-Solarzellen-Absorbern wie Cu(In,Ga)Se2 und daraus abgeleiteter Materialien. Die direkte Kompatibilität mit Lichtmikroskopie-Proben und die hohe chemisch-strukturelle Spezifizität von Ramanspektren kamen der Untersuchung naturhistorischer Mikroskopiepräparate aus Museumssammlungen zugute. Sowohl das Eindeckmedium und seine aktuelle Zusammensetzung (z.B. bezüglich leichtflüchtiger Bestandteile) als auch durch Alterung entstandene Schäden lassen sich mit der Technik zerstörungsfrei erfassen. Damit können in Zukunft Beiträge zum Erhalt der weltweit mehrere Millionen Proben umfassenden naturhistorischen Sammlungen geleistet werden. Die in der Forschung gesammelte Erfahrung fließt in der BAM direkt in die Sonder-probenanalytik für Industriekunden ein, wo Ramanbildgebung, eingebettet in ein Arsenal komplementärer Methoden, ebenfalls häufig eine zentrale Rolle spielt. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Ramanmikroskopie KW - Anorganische Materialien KW - Organische Materialien PY - 2017 AN - OPUS4-40037 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Ferruginous phases in 19th century lime and cement mortars: A Raman microspectroscopic study N2 - Raman microscopic imaging was just recently introduced into the analysis of residual Roman and Portland cement grains in 19th century cement stone, displaying evidence of the experimental adaptation of contemporary technological knowledge and practice to local circumstance. Beyond calcium ferrites, this study deals with ferruginous clinker phases that are atypical compared to present-day commercial conditions of manufacture, such as iron oxides, clinopyroxenes or pyroxenoids. Analog, microtexture, mineralogy and chemical composition of pulverized ferrosilicate slag used in the course of the 19th century as mineral additive in lime mortar reflect local resource utilization, recording the melting history within the furnace and the effectiveness of the reduction process of a single smelting event. In the case of the discussed example, chemical imaging by Raman microscopy allowed deducing a lime-rich, low-silica melt exposed to fairly reducing conditions because of the detection of the pyrometallurgic phases fayalite (Fe2SiO4), kirschsteinite (CaFeSiO4) and calcioolivine (Ca2SiO4) in zoned olivine laths and (with the melilite gehlenite, Ca2Al2SiO7) in the Interstitial matrix, cross-cut by dendritic wuestite (FeO). The presented analytical approach faces the high spatial complexity of such mortar samples by microspectroscopic imaging with micrometer lateral resolution and their chemical complexity by extracting the rich chemical information content from Raman spectra. Intensity maps of marker bands provide spatial phase distributions. Furthermore, maps of peak positions can give access to the dissemination of spectroscopically similar phases of solid solution series (e.g., olivine and calcium Aluminate ferrite) as well as varying amounts of incorporated foreign cations (e.g., in hematite). KW - Residual cement grains KW - Ferrite KW - Iron oxide KW - Slag KW - Olivine KW - Raman microspectroscopy PY - 2017 DO - https://doi.org/10.1016/j.matchar.2017.04.009 SN - 1044-5803 SN - 1873-4189 VL - 129 SP - 9 EP - 17 PB - Elsevier AN - OPUS4-40039 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lauer, Franziska T1 - Artificial pollen grain mixtures analyzed with multivariate MALDI-TOF MS imaging N2 - Anemophilous plants produce pollen grains, which have to be monitored to provide an information network for persons suffering from an allergy. The current conventional characterization and identification of pollen is performed by time-consuming microscopic examinations on the basis of the genus-specific pollen shape and size. These examinations are in need of proficient researchers, are not statistically validated, and additionally rely on relatively inaccurate observations of the pollination process. A variety of new analytical approaches have been proposed in order to develop a fast and reliable pollen identification using specific molecular information. Recently, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) was initially applied for the rapid investigation of such complex biological samples. The combination of the obtained patterns of pollen mass spectra and multivariate statistics provide a powerful tool for identifying taxonomic relationships. Here promising results obtained by the reduction and optimization of sample preparation prior to MALDI-TOF MS mapping are presented. Based on a novel application of conductive carbon tape as target, the signal information of the species-specific mass peak patterns of pollen was enhanced. This leads to a clear separation in a subsequent pattern analysis, which is important when analyzing pollen grains in natural species mixtures. As a proof-of-concept, artificial pollen mixtures were investigated by MALDI imaging and evaluated by innovative multivariate data analysis strategies, to assign individual pollen species in the mixtures. Our results can be used to improve the taxonomic differentiation and identification of pollen species and might be useful for the development of a routine method to identify pollen based on mass spectrometry. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Sample pretreatment KW - MALDI-TOF MS KW - HCA and PCA imaging KW - Pollen PY - 2017 AN - OPUS4-39989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Canning, S. A1 - Voskuil, J. A1 - Weller, Michael G. T1 - An author and reviewer in conversation – reproducibility and antibody validation N2 - A recent Opinion Article by Jan Voskuil (JV), Aeonian Biotech, discussed the challenges in validation of research antibodies. It was openly peer reviewed by Michael Weller (MW), Federal Institute for Materials Research and Testing (BAM), Germany. In this blog, both discuss these challenges, the reproducibility crisis and open data. DA - 19 May, 2017 KW - Antibodies KW - Monoclonal KW - Antibody ID KW - Quality control KW - Open data KW - Reproducibility KW - Peer review PY - 2017 UR - https://blog.f1000.com/2017/05/19/an-author-and-reviewer-in-conversation-reproducibility-and-antibody-validation SN - 2051-9796 SP - 1 EP - 5 PB - F1000 Research Ltd. CY - London AN - OPUS4-40310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dippong, Martin A1 - Carl, Peter A1 - Lenz, C. A1 - Schenk, J. A. A1 - Hoffmann, Katrin A1 - Schwaar, Timm A1 - Schneider, Rudolf A1 - Kuhne, Maren T1 - Hapten-specific single-cell selection of hybridoma clones by fluorescence-activated cell sorting for the generation of monoclonal antibodies N2 - The conventional hybridoma screening and subcloning process is generally considered to be one of the most critical steps in hapten-specific antibody production. It is time-consuming, monoclonality is not guaranteed, and the number of clones that can be screened is limited. Our approach employs a novel hapten-specific labeling technique of hybridoma cells. This allows for fluorescence-activated cell sorting (FACS) and single-cell deposition and thereby eliminates the above-mentioned problems. A two-step staining approach is used to detect antigen specificity and antibody expression: in order to detect antigen specificity, hybridoma cells are incubated with a hapten−horseradish peroxidase conjugate (hapten−HRP), which is subsequently incubated with a fluorophore-labeled polyclonal anti-peroxidase antibody (anti-HRP−Alexa Fluor 488). To characterize the expression of membrane-bound immunoglobulin G (IgG), a fluorophore-labeled anti-mouse IgG antibody (anti-IgG−Alexa Fluor 647) is used. Hundreds of labeled hybridoma cells producing monoclonal antibodies (mAbs) specific for a hapten were rapidly isolated and deposited from a fusion mixture as single-cell clones via FACS. Enzyme-linked immunosorbent assay (ELISA) measurements of the supernatants of the sorted hybridoma clones revealed that all hapten-specific hybridoma clones secrete antibodies against the target. There are significant improvements using this high-throughput technique for the generation of mAbs including increased yield of antibody-producing hybridoma clones, ensured monoclonality of sorted cells, and reduced development times. KW - Monoclonal antibodies KW - FACS KW - Hybridoma cells PY - 2017 DO - https://doi.org/10.1021/acs.analchem.6b04569 SN - 0003-2700 SN - 1520-6882 VL - 89 IS - 7 SP - 4007 EP - 4012 PB - ACS Publications AN - OPUS4-40320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Altenburg, Simon ED - Bison, P. ED - Burleigh, D. T1 - Direct comparison of two pyrometers and a low-cost thermographic camera for time resolved LWIR temperature measurements N2 - Contactless temperature sensing is state of the art and essential part of countless applications in the field of process control and automation. This contribution presents the case of a nondestructive thickness measurement method for polymeric coatings on concrete ground. Two pyrometers and a low-cost infrared camera were taken into account. The particular measurement results were compared with those of a more sophisticated infrared camera. It was found that the low-cost infrared camera has a lower noise level than the pyrometers, even for a single pixel. The opportunity to average over a large number of pixels and to establish a bias correction enables a further noise reduction by almost factor of 10. Furthermore, the temporal resolution of the infrared camera was investigated by means of a well-defined thermal oscillation. It could be demonstrated that the averaged time stamps are correct and the requirement of a Minimum framerate of 50 Hz is met. Finally, the temperature transient on a polymer coated concrete block during and after a 10 s heating period was recorded with a pyrometer and the infrared camera. This experiment confirmed the suitability of the camera for the intended measurement method. T2 - Thermosense: Thermal Infrared Applications CY - Anaheim, CA, USA DA - 10.04.2017 KW - Contactless temperature measurement KW - Layer thickness KW - Pyrometer KW - Infrared camera KW - Nondestructive testing PY - 2017 SN - 978-1-5106-0929-7 SN - 978-1-5106-0930-3 DO - https://doi.org/10.1117/12.2261074 SN - 0277-786X SN - 1996-756X VL - 10214 SP - Article 1021414, 1 EP - 10 AN - OPUS4-40291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc T1 - Spurenfeuchtemessung in technischen Gasen mit coulometrischen Sensoren N2 - Die Messung der Gasfeuchte im Spurenbereich in unterschiedlichen technisch und medizinisch relevanten Gasen erfolgte mit Sensoren, die auf dem coulometrischen Messprinzip basieren. Die verwendeten planaren coulometrischen Sensoren wurden im Frostpunkttemperaturbereich von -70 °C bis -30 °C in synthetischer Luft, Wasserstoff, Stickstoff und Distickstoffmonoxid (Lachgas) untersucht. Als Referenz für die Messungen wurde ein Präzisionstaupunktspiegel-Hygrometer verwendet. Die Gasfeuchte kann mit Hilfe der Sensoren in allen untersuchten Gasen, aber mit geänderten Kalibrierfunktionen, mit einer erweiterten Unsicherheit von kleiner als 2,1 K bestimmt werden. Für die Messungen in unterschiedlichen Gasen muss also der Einfluss der Gasmatrix auf das Sensorsignal berücksichtigt werden. So ist zum Beispiel bei Messungen in befeuchtetem Wasserstoff, aufgrund von Rekombinationseffekten, ein signifikant geändertes Sensorsignal zu beobachten. T2 - Temperatur 2017 CY - Berlin, Germany DA - 17.05.2017 KW - Spurenfeuchte KW - Coulometrische Sensoren KW - Technische Gase PY - 2017 AN - OPUS4-40292 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Detjens, Marc A1 - Hübert, Thomas A1 - Banach, Ulrich T1 - Spurenfeuchtemessung in unterschiedlichen Gasen mit coulometrischen Sensoren N2 - Die Messung der Gasfeuchte im Spurenbereich in unterschiedlichen technisch und medizinisch relevanten Gasen erfolgte mit Sensoren, die auf dem coulometrischen Messprinzip basieren. Die verwendeten planaren coulometrischen Sensoren wurden im Frostpunkttemperaturbereich von -70 °C bis -30 °C in synthetischer Luft, Wasserstoff, Stickstoff und Distickstoffmonoxid (Lachgas) untersucht. Als Referenz für die Messungen wurde ein Präzisionstaupunktspiegel-Hygrometer verwendet. Die Gasfeuchte kann mit Hilfe der Sensoren in allen untersuchten Gasen, aber mit geänderten Kalibrierfunktionen, mit einer erweiterten Unsicherheit von kleiner als 2,1 K bestimmt werden. Für die Messungen in unterschiedlichen Gasen muss also der Einfluss der Gasmatrix auf das Sensorsignal berücksichtigt werden. So ist zum Beispiel bei Messungen in befeuchtetem Wasserstoff, aufgrund von Rekombinationseffekten, ein signifikant geändertes Sensorsignal zu beobachten. T2 - Temperatur 2017 CY - Berlin, Germany DA - 17.05.2017 KW - Spurenfeuchte KW - Coulometrische Sensoren KW - Technische Gase PY - 2017 SN - 978-3-944659-04-6 SP - 247 EP - 252 AN - OPUS4-40293 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bandow, Nicole T1 - Auswahl von Passivsammlermaterialien für NSO-Heterocyclen im Grundwasser N2 - NSO-Heterocyclen (NSO-H) finden sich zusammen mit polycyklischen aromatischen Kohlenwasserstoffen (PAK) überwiegend an Teer- und Teeröl kontaminierten Standorten im Boden und Grundwasser. NSO-H sind ähnlich toxisch wie PAK, aber polarer und damit hydrophiler. Da NSO-H an kontaminierten Standorten lediglich einen geringen Anteil des Schadstoffinventars ausmachen, wurde ihnen in der Vergangenheit wenig Aufmerksamkeit zuteil und sie werden im Gegensatz zu PAK nicht routinemäßig erfasst. Aufgrund ihrer teilweise ausgeprägten Persistenz und der vergleichsweisen guten Wasserlöslichkeit bilden sie trotz der eher geringen Anfangskonzentrationen große Schadstofffahnen mit geringen Konzentrationen aus. Mikrobielle Abbauprozesse bewirken dabei im Verlauf der Fahne Veränderungen der Anteile der Einzelsubstanzen zueinander. In der Nähe des Schadensherdes dominieren meist PAK, im Abstrom sinkt deren Konzentration allerdings schneller, so dass hier die NSO-H die dominierende Schadstoffgruppe darstellen. Auf Grund des unterschiedlichen Abbauverhaltens kann die NSO-HBelastung über den PAK Summenparameter nicht zuverlässig bestimmt werden. T2 - Innovationstag Mittelstand 2017 CY - Berlin, Germany DA - 18.05.2017 KW - Passivsammler KW - Adsorbentien KW - NSO-Heterocyclen KW - Grundwasser PY - 2017 AN - OPUS4-40294 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Aktuelle Herausforderungen für die Prozessanalytik – von der Online-NMR-Spektroskopie im Feld bis zum Plasmaspektrometer auf dem Acker N2 - Der Vortrag stellt einige aktuelle Herausforderungen für die Prozessanalytik und mögliche Antworten vor. Gepulste Raman-Spektrometer akkumulieren das Raman-Signal mit Hilfe schneller optischer Schalter im Picosekunden-Bereich, bevor langlebigere Fluoreszenzanregung entsteht. Damit lassen sich stark fluoreszierende Materialien untersuchen, die bislang nicht zugänglich sind. Eine weitere interessante Entwicklung ist etwa die Shifted excitation Raman difference spectroscopy (SERDS) die besonders für biologische Anwendungen interessant ist. Flexible, modulare Produktionsanlagen stellen einen vielversprechenden Ansatz für die kontinuierliche Produktion von Fein- und Spezialchemikalien dar. In einem EU-Projekt wird derzeit die Feldintegration eines Online-NMR-Sensormoduls als smartes Modul für die Prozesskontrolle vorangebracht. Dieses Modul basiert auf einem kommerziell erhältlichen Niederfeld-NMR-Spektrometer, welche zurzeit für die Anwendung im Laborbereich erhältlich ist. Für die Feldintegration wurde ein ATEX-zertifiziertes, explosionsgeschütztes Gehäuse entwickelt sowie Automationsschemen für den unbeaufsichtigten Betrieb und für die spektrale Datenauswertung erstellt. Eine sehr gut anwendbare analytische Messtechnik zur Kontrolle der elementaren Zusammensetzung von verschiedensten Materialien ist die laserinduzierte Plasmaspektroskopie (LIPS, engl. LIBS - Laser-induced Breakdown Spectroscopy). Bei der LIBS wird ein kurz gepulster Laser auf eine Probe fokussiert, um ein Leuchtplasma zu erzeugen. Das dabei erzeugte Atomemissionsspektrum ermöglicht eine qualitative und quantitative Analyse der Zusammensetzung der Probe bezüglich praktisch aller Elemente des Periodensystems. In einem aktuellen Projekt wird diese Methode neben anderen zur Online-Analyse von Ackerböden für die ortsspezifischer Bewirtschaftung (Precision Agriculture) weiterentwickelt und bewertet. T2 - Vortragsreihe Analytik, Merck KGaA CY - Darmstadt, Germany DA - 19.05.2017 KW - Prozessanalytik KW - Reaction Monitoring KW - Online NMR Spektroskopie KW - LIBS KW - RFA KW - Raman-Spektroskopie KW - BONARES KW - CONSENS PY - 2017 AN - OPUS4-40328 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haas, Marko T1 - Damit Berichte etwas berichten N2 - Der Vortrag "Damit Berichte etwas berichten" wurde anlässlich des 22. Controller-Erfahrungsaustausches der Bundesbehörden am 17.05.2017 gehalten. Er beschäftigt sich mit wesentlichen Grundlage für die professionelle Darstellung von Daten für Controller, aber auch für Wissenschaftlerinnen und Wissenschaftler. Dabei werden die Grundsätze einer aussagekräftigen Darstellung anhand des Akronyms "MEHR Güte" entwickelt und dargestellt. T2 - 22. Erfahrungsaustausch KLR/Controlling der Bundesbehörden CY - Berlin, Germany DA - 17.05.2017 KW - Präsentieren KW - Datenaufbereitung KW - Grafik PY - 2017 AN - OPUS4-40347 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel A1 - Gohlke, Dirk A1 - Meinig, Silvia A1 - Kaszemeikat, T. T1 - Hochauflösende Reinheitsgradbestimmung - Fertigung von Referenzfehlern N2 - Regelwerke zur zerstörungsfreien Bestimmung des Reinheitsgrades wie das SEP 1927 und die ASTM E588 erreichen ihre Vergleichbarkeit unter Anwendung von - vergleichsweise einfachen - Referenzfehlern. Hinsichtlich Realisierbarkeit wird somit der Kompromiss zwischen Herstellung des Referenzfehlers und der erreichbaren Nachweisgrenze gefunden. Zur Weiterentwicklung über die Grenzen der SEP1927 hinaus, wurde der Versuch unternommen Fehler kleiner 500 μm herzustellen - welche aufgrund der geringen geometrischen Ausdehnung fertigungsbedingt schwierig zu realisieren sind. Bei den vergleichenden Untersuchungen kristallisierten sich zwei Fertigungsverfahren, Funkenerosion (EDM: electrical discharge maching) und die Fertigung der Bohrungen unter Verwendung eines Hochleistungslasers, als vielversprechend heraus. Zunächst wurden die Fehler mit beiden Verfahren in unterschiedlichen Größen (100, 250 und 100 μm) und Tiefen (1, 1,5 und 2 mm) unter Anwendung von computertomographischen Verfahren der Röntgenprüfung, die Geometrie der eingebrachten Fehlstellen und anschließend durch hochauflösende Tauchtechnikmessungen das Reflektionsverhalten charakterisiert. T2 - DGZfP Jahrestagung CY - Koblenz, Germany DA - 22.05.2017 KW - Materialcharakterisierung KW - Reinheitsgradbestimmung KW - Ultraschalltauchtechnik PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-403505 SN - 978-3-940283-85-6 SP - P20, 1 EP - 2 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) AN - OPUS4-40350 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Signalverarbeitung zur hochauflösenden Reinheitsgradbestimmung N2 - Basierend auf aktuellen Regelwerken (SEP1927 und ASTM E588) stehen Möglichkeiten zur nichtinvasiven Beurteilung des zu untersuchenden Werkstoffes, in verschiedenen Qualitätsstufen bis zu einer Vergleichsfehlergröße von bis zu 300 Mikrometer zur Verfügung. Allerdings ist der realistische Nachweis und die Beurteilung von künstlichen sowie von natürlichen Fehlern kleiner 500 Mikrometer nur unter optimalen Voraussetzungen (bspw. Wahl des Prüfkopfes, Geometrie des Prüfobjektes, orts- bzw. zeitliche Auflösung der Messdatenaufnahme) und unter Einsatz von geeigneten Signalverarbeitungsalgorithmen möglich. Im Rahmen von Ringversuchen wurden daher verschiedene Methoden zur Aufbereitung der zu erfassenden Messdaten entwickelt und an verschiedenen Bauteilgeometrieen und Werkstoffen getestet. Dabei stellten sich der spektrale Tiefenausgleich (SDAC) und die nichtlineare Bewertung einzelner Frequenzkomponenten des Nutzsignals als sehr vielversprechend heraus und die Nachweisbarkeit kleiner Fehler - im Bereich von 100 - 500 μm - konnte erfolgreich gesteigert werden. T2 - DGZfP Jahrestagung CY - Koblenz, Germany DA - 22.05.2017 KW - Materialcharakterisierung KW - Reinheitsgradbestimmung KW - Ultraschalltauchtechnik PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-403523 AN - OPUS4-40352 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rades, Steffi T1 - Tracing fluorine at the surface and in the bulk of TiO2 nanoplatelets by means of SEM-EDX, AES and ToF-SIMS N2 - The synthesis of TiO2 nanoplatelets with fluorine-containing reactants is carried out using titanium (IV) butoxide as precursor and concentrated HF as shape controller, the final product requires a working up in order to eliminate or at least to reduce the amount of residual fluorides, which is realized here by well-defined thermal treatment of the samples. Bulk and surface sensitive methods namely scanning electron microscopy with energydispersive X-ray spectroscopy (SEM-EDX), Auger electron spectroscopy (AES) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) have been applied to trace the presence of any fluorides in dependence on different information depths and measurement sensitivities of these methods. T2 - EMAS 2017 - 15th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS and IUMAS-7 Meeting CY - Konstanz, Germany DA - 07.05.2017 KW - Nanoparticles KW - Surface analysis KW - ToF-SIMS KW - AES KW - SEM-EDX PY - 2017 AN - OPUS4-40265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rades, Steffi T1 - Surface and in-depth analysis of functionalization of TiO2 nanoparticles for self-assembly in multiple layers N2 - Parameters of TiO2 coatings can greatly influence their final performance in largescale applications such as photocatalytic measurements, orthopedic and/or dental prostheses, cell cultures, and dye-sensitized solar cells. From different film deposition procedures, self-assembly of TiO2 NPs in multiple layers was selected for systematic characterization. EDX, AES and ToF-SIMS analysis have been carried out in order to evaluate the functionalization of several types of TiO2 NPs differing in size, shape and surface area. T2 - EMAS 2017 - 15th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS and IUMAS-7 Meeting CY - Constance, Germany DA - 07.05.2017 KW - Functionalization KW - Surface analysis KW - Nanoparticles KW - Thin films PY - 2017 AN - OPUS4-40266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hübert, Thomas T1 - Hydrogen sensor deployment N2 - Presentation of BAM test facility. Presentation of previous analysis of sensor performance in relation to application requirements and sensor data base. The main topics of sensor metrological, deployment and operational metrics were discussed. T2 - Hydrogen Sensor Workshop CY - Brussels, Belgium DA - 10.05.2017 KW - Hydrogen sensors KW - Sensor deployment PY - 2017 AN - OPUS4-40270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, F. A1 - Reinmuth-Selzle, K. A1 - Lai, S. A1 - Weller, Michael G. A1 - Pöschl, U. A1 - Kampf, C. J. T1 - Simultaneous determination of nitrated and oligomerized proteins by size exclusion high-performance liquid chromatography coupled to photodiode array detection N2 - Chemical modifications such as nitration and cross-linking may enhance the allergenic potential of proteins. The kinetics and mechanisms of the underlying chemical processes, however, are not yet well understood. Here, we present a size-exclusion chromatography/spectrophotometry method (SEC-HPLC-DAD) that allows a simultaneous detection of mono-, di-, tri-, and higher protein oligomers, as well as their individual nitration degrees (NDs). The ND results of proteins from this new method agree well with the results from an alternative well-established method, for the analysis of tetranitromethane (TNM)- and nitrogen dioxide and ozone (NO2/O3)-nitrated protein samples. Importantly, the NDs for individual oligomer fractions can be obtained from the new method, and also, we provide a proof of principle for the calculation of the concentrations for individual protein oligomer fractions by their determined NDs, which will facilitate the investigation of the kinetics and mechanism for protein tyrosine nitration and cross-linking. KW - Size exclusion chromatography KW - HPLC-DAD KW - Protein nitration degree KW - Protein oligomer analysis KW - Nitrotyrosine KW - Dimer KW - Trimer KW - Oligomer KW - Protein KW - Tetranitromethane KW - BSA KW - Albumin KW - Air pollution KW - Nitrogen oxides PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0021967317303795 DO - https://doi.org/10.1016/j.chroma.2017.03.015 SN - 0021-9673 VL - 1495 SP - 76 EP - 82 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-40304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Metrology for spatially resolved chemical analysis at the micro and nanometre scales - Surface analysis working group (SAWG) - Report for 15th meeting (2016/17) N2 - CCQM has established a framework of comparisons to demonstrate the international comparability of chemical measurements. The key point is the establishment of comparable measurements, with traceability to internationally or nationally stated references. Originally initiated by Dr Martin P Seah, NPL, the Surface Analysis Working Group (SAWG) has been formally founded in 2003. The following terms of reference were presented to CCQM in April 2002. CCQM ratified the group as a full working group of CCQM in April 2003 with these terms of reference: - to develop pilot studies and carry out key comparisons of national measurement standards for surface and micro/nano-analysis; - to assist in identifying and establishing inter-laboratory work to improve the traceability of surface and micro/nano-analysis; - to establish and update a work plan to be adopted by CCQM; - to discuss and review the scope of the working group and to liase with other working groups related to nanotechnology. Following the 2016 meeting, the Key Comparison K-129 "Measurement of atomic fractions in Cu(In,Ga)Se2 Films" lead by KRISS and the Key Comparison K-136 on "BET specific surface area of nanoporous Al2O3" lead by UNIIM&BAM have been finished in 2016. The 15th meeting of SAWG will focus on - survey on CMC claim submitted with reference to K-129 and K-136. - the overall and SAWG specific aspects of the CCQM Strategy process, - a joint meeting with the Inorganic Working Group addressing number concentrations of nano particles, - discussion of future comparisons. T2 - CCQM Plenary Meeting at BIPM 2017 CY - Paris, France DA - 27.4.17 KW - Metrology KW - Comparisons KW - CCQM PY - 2017 AN - OPUS4-40277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thiel, Erik A1 - Ziegler, Mathias T1 - Subsurface defect localization by structured heating using laser projected photothermal thermography N2 - The presented method is used to locate subsurface defects oriented perpendicularly to the surface. To achieve this, we create destructively interfering thermal wave fields that are disturbed by the defect. This effect is measured and used to locate the defect. We form the destructively interfering wave fields by using a modified projector. The original light engine of the projector is replaced with a fiber-coupled high-power Diode laser. Its beam is shaped and aligned to the projector's spatial light modulator and optimized for optimal optical throughput and homogeneous projection by first characterizing the beam profile, and, second, correcting it mechanically and numerically. A high-performance infrared (IR) camera is set up according to the tight geometrical situation (including corrections of the geometrical image distortions) and the requirement to detect weak temperature oscillations at the sample surface. Data acquisition can be performed once a synchronization between the individual thermal wave field sources, the scanning stage, and the IR camera is established by using a dedicated experimental setup which needs to be tuned to the specific material being investigated. During data post-processing, the relevant information on the presence of a defect below the surface of the sample is extracted. It is retrieved from the oscillating part of the acquired thermal radiation coming from the so-called depletion line of the sample surface. The exact location of the defect is deduced from the analysis of the spatial-temporal shape of these oscillations in a final step. The method is reference-free and very sensitive to changes within the thermal wave field. So far, the method has been tested with steel samples but is applicable to different materials as well, in particular to temperature sensitive materials. KW - Active thermography KW - Structured heating KW - Digital micromirror device KW - Thermal wave field KW - Photothermal PY - 2017 UR - https://www.jove.com/video/55733 DO - https://doi.org/10.3791/55733 SN - 1940-087X IS - 123 SP - e55733-1 EP - e55733-13 PB - MyJoVE Corp. AN - OPUS4-40281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Design and validation of a compact NMR analyser N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and relatively inexpensive analysers, which feature advantages like low cost, low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, sufficient robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. If these are not available, there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Union’s Research Project CONSENS (Integrated Control and Sensing) by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. The presented NMR module is provided in an explosion proof housing of 57 x 57 x 85 cm module size and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling (IHM) was selected for data analysis of the low-field NMR spectra. A set-up for monitoring continuous reactions in a thermostated 1/8” tubular reactor using automated syringe pumps was used to validate the IHM models by using high-field NMR spectroscopy as analytical reference method. T2 - EuroPACT 2017 CY - Potsdam, Germany DA - 10.05.2017 KW - Online reaction monitoring KW - NMR spectroscopy PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-402822 AN - OPUS4-40282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Hochauflösende Reinheitsgradbestimmung – Fertigung von Referenzfehlern N2 - Regelwerke zur zerstörungsfreien Bestimmung des Reinheitsgrades wie das SEP 1927 und die ASTM E588 erreichen ihre Vergleichbarkeit unter Anwendung von - vergleichsweise einfachen - Referenzfehlern. Hinsichtlich Realisierbarkeit wird somit der Kompromiss zwischen Herstellung des Referenzfehlers und der erreichbaren Nachweisgrenze gefunden. Zur Weiterentwicklung über die Grenzen der SEP1927 hinaus, wurde der Versuch unternommen Fehler kleiner 500 μm herzustellen - welche aufgrund der geringen geometrischen Ausdehnung fertigungsbedingt schwierig zu realisieren sind. Bei den vergleichenden Untersuchungen kristallisierten sich zwei Fertigungsverfahren, Funkenerosion (EDM: electrical discharge maching) und die Fertigung der Bohrungen unter Verwendung eines Hochleistungslasers, als vielversprechend heraus. Zunächst wurden die Fehler mit beiden Verfahren in unterschiedlichen Größen (100, 250 und 100 μm) und Tiefen (1, 1,5 und 2 mm) unter Anwendung von computertomographischen Verfahren der Röntgenprüfung, die Geometrie der eingebrachten Fehlstellen und anschließend durch hochauflösende Tauchtechnikmessungen das Reflektionsverhalten charakterisiert. T2 - DGZfP Jahrestagung CY - Koblenz, Germany DA - 22.05.2017 KW - Materialcharakterisierung KW - Reinheitsgradbestimmung KW - Ultraschalltauchtechnik PY - 2017 AN - OPUS4-40353 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf A1 - Munzke, Dorit A1 - Pohl, Rainer T1 - Wirbelstromprüfung an Composite-Druckgefäßen N2 - Composite-Druckgefäße für den Gefahrguttransport sowie für Wasserstoff- und Erdgasfahrzeuge bestehen aus einem lasttragenden Composite und einer gasdichten, metallischen oder polymeren Barriereschicht (Liner). Zur Untersuchung des Alterungsverhaltens solcher Composite-Druckgefäße wird in der BAM das interdisziplinäre Themenfeldprojekt COD-AGE durchgeführt. Ziel des Projektes ist die Entwicklung von Methoden und Modellen zur Beschreibung und Bestimmung des Alterungsverhaltens von Carbonfaser-Compositen (CFK) am Beispiel von Druckgefäßen, um eine bessere Vorhersage der Alterung und der sicheren Gebrauchsdauer zu ermöglichen. Ein Schwerpunkt in diesem Projekt ist die Bereitstellung geeigneter ZfP-Methoden. Dabei geht es sowohl um versuchsbegleitende Prüfungen, als auch um die mögliche Entwicklung von Prüfeinrichtungen für den späteren praktischen Gebrauch. In diesem Vortrag werden Prüfsysteme und Prüfergebnisse der „konventionellen“ Wirbelstromprüfung vorgestellt. In einem ersten Schritt wurden Versuche an bereits geschädigten Druckgefäßen durchgeführt. Dabei wurden Druckgefäße mit den Materialpaarungen Stahl-CFK, Aluminium-CFK und Kunststoff-CFK untersucht. Die Dicken der CFK-Schichten reichten hierbei von ca. 4 mm bis ca. 8 mm. Anfangs wurden die Gefäße mit verschiedenen Sensoren von außen geprüft. Es konnten sowohl Beschädigungen des metallischen Liners, als auch Strukturen des CFK-Geflechts nachgewiesen werden. In einem zweiten Schritt wurden die Gefäße von innen geprüft. Hierbei bestand die besondere Herausforderung in der Prüfung eines Zylinders von 150 mm Durchmesser durch einen Zugang von nur 15 mm Durchmesser. Mit den bei diesen Vorversuchen optimierten Prüfsystemen wurden dann begleitende Prüfungen bei Alterungsversuchen durchgeführt. In den Alterungsversuchen wurden Druckbehälter mit einem ca. 4 mm dicken Aluminiumliner und ca. 3,5 mm dicker CFK-Ummantelung untersucht. Typisches Einsatzgebiet solcher Flaschen sind Atemschutzgeräte bei der Feuerwehr. Die verschiedenen Prüfsysteme und die mit ihnen erzielten Ergebnisse werden vorgestellt. T2 - DGZfP-Jahrestagung 2017 CY - Koblenz, Germany DA - 22.05.2017 KW - Composite-Druckgefäß KW - Wirbelstromprüfung KW - CFK PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-403577 SN - 978-3-940283-85-6 VL - 162 SP - 1 EP - 9 PB - DGZfP e.V. AN - OPUS4-40357 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Wirbelstromprüfung an Composite-Druckgefäßen N2 - Composite-Druckgefäße für den Gefahrguttransport sowie für Wasserstoff- und Erdgasfahrzeuge bestehen aus einem lasttragenden Composite und einer gasdichten, metallischen oder polymeren Barriereschicht (Liner). Zur Untersuchung des Alterungsverhaltens solcher Composite-Druckgefäße wird in der BAM das interdisziplinäre Themenfeldprojekt COD-AGE durchgeführt. Ziel des Projektes ist die Entwicklung von Methoden und Modellen zur Beschreibung und Bestimmung des Alterungsverhaltens von Carbonfaser-Compositen (CFK) am Beispiel von Druckgefäßen, um eine bessere Vorhersage der Alterung und der sicheren Gebrauchsdauer zu ermöglichen. Ein Schwerpunkt in diesem Projekt ist die Bereitstellung geeigneter ZfP-Methoden. Dabei geht es sowohl um versuchsbegleitende Prüfungen, als auch um die mögliche Entwicklung von Prüfeinrichtungen für den späteren praktischen Gebrauch. In diesem Vortrag werden Prüfsysteme und Prüfergebnisse der „konventionellen“ Wirbelstromprüfung vorgestellt. In einem ersten Schritt wurden Versuche an bereits geschädigten Druckgefäßen durchgeführt. Dabei wurden Druckgefäße mit den Materialpaarungen Stahl-CFK, Aluminium-CFK und Kunststoff-CFK untersucht. Die Dicken der CFK-Schichten reichten hierbei von ca. 4 mm bis ca. 8 mm. Anfangs wurden die Gefäße mit verschiedenen Sensoren von außen geprüft. Es konnten sowohl Beschädigungen des metallischen Liners, als auch Strukturen des CFK-Geflechts nachgewiesen werden. In einem zweiten Schritt wurden die Gefäße von innen geprüft. Hierbei bestand die besondere Herausforderung in der Prüfung eines Zylinders von 150 mm Durchmesser durch einen Zugang von nur 15 mm Durchmesser. Mit den bei diesen Vorversuchen optimierten Prüfsystemen wurden dann begleitende Prüfungen bei Alterungsversuchen durchgeführt. In den Alterungsversuchen wurden Druckbehälter mit einem ca. 4 mm dicken Aluminiumliner und ca. 3,5 mm dicker CFK-Ummantelung untersucht. Typisches Einsatzgebiet solcher Flaschen sind Atemschutzgeräte bei der Feuerwehr. Die verschiedenen Prüfsysteme und die mit ihnen erzielten Ergebnisse werden vorgestellt. T2 - DGZfP-Jahrestagung 2017 CY - Koblenz, Germany DA - 22.05.2017 KW - Composite-Druckgefäß KW - Wirbelstromprüfung KW - CFK PY - 2017 AN - OPUS4-40359 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pohl, Rainer A1 - Casperson, Ralf A1 - Maierhofer, Christiane A1 - Müller, Jan A1 - Pelkner, Matthias T1 - Gegenüberstellung von Wirbelstromprüfung und aktiver Thermografie an CFK-Versuchskörpern N2 - In vielen Bereichen der Technik haben Konstruktionen unter Einsatz von CFK-Bauteilen und Komponenten die klassischen Metalle abgelöst. Die zerstörungsfreie Prüfung solcher CFK-Bauteile gewinnt somit zunehmend an Bedeutung. Ein mögliches Prüfverfahren ist dabei die Wirbelstromprüfung. Aufgrund der relativ geringen elektrischen Leitfähigkeit von CFK-Komponenten kommt hierbei häufig die sogenannte HF-Wirbelstromprüfung zum Einsatz. In verschiedenen Untersuchungen der BAM konnten jedoch auch mit Wirbelstromprüfsystemen in niedrigen Frequenzbereichen gute Ergebnisse erzielt werden. Um die Möglichkeiten und Grenzen dieser konventionellen Wirbelstromprüfung auszuloten, wurden Messungen an Versuchskörpern durchgeführt, welche bereits bei der Validierung der Blitz- und Lock-in-Thermografie für neue Verfahrensnormen erfolgreich eingesetzt wurden. Ein Typ dieser Versuchskörper sind Flachproben aus CFK von 6 mm Dicke. In diesen wurden Flachbodenbohrungen mit Durchmessern zwischen 4 mm und 24 mm eingebracht. Die Restwandstärken liegen zwischen 0,06 mm und 3,66 mm. Ein weiterer CFK-Versuchskörper hat die Geometrie eines Stufenkeiles. Bei verschiedenen Stufenkeilen sind Wanddicken zwischen 1,4 mm und 5,4 mm realisiert worden. In diesen wurden künstliche quadratische Delaminationen mit Kantenlängen zwischen 2 mm und 20 mm eingebracht. Die Ergebnisse der Wirbelstromprüfung werden denen der aktiven Thermografie gegenübergestellt. Zur Nachbildung von Kompositwerkstoffen wurden die flachen Versuchskörper mit geeigneten Versuchskörpern aus Aluminium und Stahl kombiniert. Die Wirbelstromprüfungen wurden mit einem handelsüblichen Prüfgerät im Frequenzbereich zwischen 500 Hz und 3 MHz und entsprechend angepassten Sensoren durchgeführt. T2 - DGZfP Jahrestagung 2017 CY - Koblenz, Germany DA - 22.05.2017 KW - Wirbelstromprüfung KW - Aktive Thermografie KW - CFK PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-403607 SN - 978-3-940283-85-6 VL - 162 SP - 1 EP - 10 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-40360 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pellegrino, F. A1 - Pellutiè, L. A1 - Sordello, F. A1 - Minero, C. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Maurino, V. T1 - Influence of agglomeration and aggregation on the photocatalytic activity of TiO2 nanoparticles N2 - Particle aggregation and agglomeration influence the optical properties of materials and therefore theirability to absorb and scatter the incoming radiation, also affecting their photocatalytic activity. Wehave studied the correlation between aggregation and photocatalytic activity for titanium dioxide bymeans of experimental measurements of extinction and photocatalytic activity and calculations of theiroptical properties (extinction, absorption and scattering cross-sections). This approach can be adoptedto quantitatively assess the quantum yields of the heterogeneous photocatalytic systems. The study wasperformed on TiO2PC105 Cristal ACTiVTM, made of aggregated (and agglomerated) primary particles of anatase. The size of the aggregates has been reduced with ultra-sonication. Aqueous suspensions of the obtained materials were characterized by measuring the optical properties (UV–vis extinction), the sizing properties (DLS) and the photocatalytic activity (degradation of phenol under standard con-ditions). The extinction and absorption spectra of the suspensions were derived from the calculatedcoefficients, considering also the size distributions measured with DLS, and revealed that light absorptionis maximized when particle aggregation and agglomeration are avoided, while diffusion of the incomingradiation dominates when large aggregates and agglomerates are present. The present paper represents a valuable approach to the accurate and reproducible measurement of the photocatalytic activity ofTiO2nanoparticles suspensions, thus allowing a more reliable comparison of the properties of different materials. KW - Titanium dioxide KW - Nanoparticles KW - Agglomeration/aggregation KW - Photocatalysis KW - Quantum yield PY - 2017 DO - https://doi.org/10.1016/j.apcatb.2017.05.046 SN - 0926-3373 SN - 1873-3883 VL - 216 SP - 80 EP - 87 PB - Elsevier B.V. AN - OPUS4-40477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grulke, E. A. A1 - Yamamoto, K. A1 - Kumagai, K. A1 - Häusler, Ines A1 - Österle, Werner A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Brown, S. C. A1 - Chan, C. A1 - Zheng, J. A1 - Yamamoto, K. A1 - Yashiki, K. A1 - Song, N. W. A1 - Kim, Y. H. A1 - Stefaniak, A. B. A1 - Schwegler-Berry, D. A1 - Coleman, V. A. A1 - Jämting, Å. K. A1 - Herrmann, J. A1 - Arakawa, T. A1 - Burchett, W. W. A1 - Lambert, J. W. A1 - Stromberg, A. J. T1 - Size and shape distributions of primary crystallites in titania aggregates N2 - The primary crystallite size of titania powder relates to its properties in a number of applications. Transmission electron microscopy was used in this interlaboratory comparison (ILC) to measure primary crystallite size and shape distributions for a commercial aggregated titania powder. Data of four size descriptors and two shape descriptors were evaluated across nine laboratories. Data repeatability and reproducibility was evaluated by analysis of variance. One-third of the laboratory pairs had similar size descriptor data, but 83% of the pairs had similar aspect ratio data. Scale descriptor distributions were generally unimodal and were well-described by lognormal reference models. Shape descriptor distributions were multi-modal but data visualization plots demonstrated that the Weibull distribution was preferred to the normal distribution. For the equivalent circular diameter size descriptor, measurement uncertainties of the lognormal distribution scale and width parameters were 9.5% and 22%, respectively. For the aspect ratio shape descriptor, the measurement uncertainties of the Weibull distribution scale and width parameters were 7.0% and 26%, respectively. Both measurement uncertainty estimates and data visualizations should be used to analyze size and shape distributions of particles on the nanoscale. KW - Measurement uncertainty KW - Size distribution KW - Shape distribution KW - TEM KW - Titania PY - 2017 DO - https://doi.org/10.1016/j.apt.2017.03.027 SN - 0921-8831 VL - 28 IS - 7 SP - 1647 EP - 1659 PB - Elsevier B.V. AN - OPUS4-40478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Using Smart Sensors and Modular Production Units for Sustainable and Flexible Production of High Quality Chemicals and Pharmaceuticals N2 - The talk reflects how PAT could be applied in future developments ofpharma manufacturing. It shows the benefits, increase quality, size and increasing speed of production with significant reduction of quality costs, which are possible. Using Smart Sensors and model based data evaluation methods are the key to reduce set-up times and costs. Industry 4.0 will help shape the Pharmaceutical industry of tomorrow. This is demonstrated by an example using modular production units for Continuous Manufacturing. The development of a smart online NMR analyser is shown. T2 - Pharma Talk 2017 CY - Berlin, Germany DA - 08.06.2017 KW - Process Monitoring KW - CONSENS KW - Online NMR Spectroscopy KW - Continuous Manufacturing KW - Pharmaceutical Production PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-405039 AN - OPUS4-40503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred A1 - Feldmann, Ines A1 - Knabe, Nicole A1 - Toepel, J. T1 - Organic surface coatings on medieval stained glass and microbiological investigation N2 - Mediaeval stained glass has been treated with Polymethylmetacrylate coatings by Kwiatkowski in Poland during the 1950th. Such treated panels were found in the Johannis Church of Toruń (without protective glazing), in the Cathedral of Włocławek (behind a protective glazing), and on glass kept in exhibition cases in the museum of Toruń. Surface coatings have been detected and analyzed. There was no extensive contamination by fungi or bacteria if the glass was either coated or not. T2 - Glass Science in Art and Conservation 2017 CY - Lisbon, Portugal DA - 06.06.2017 KW - Microbiological investigation KW - Medieval stained glass KW - SEM analysis PY - 2017 SN - 978-989-99528-3-6 SP - 112 EP - 113 PB - NOVA:FCT Editorial CY - Lisbon AN - OPUS4-40568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Torge, Manfred T1 - Organic surface coatings on medieval stained glass and microbiological investigation N2 - Mediaeval stained glass has been treated with Polymethylmetacrylate coatings by Kwiatkowski in Poland during the 1950th. Such treated panels were found in the Johannis Church of Toruń (without protective glazing), in the Cathedral of Włocławek (behind a protective glazing), and on glass kept in exhibition cases in the museum of Toruń. Surface coatings have been detected and analyzed. There was no extensive contamination by fungi or bacteria if the glass was either coated or not. T2 - Glass Science in Art and Conservation 2017 CY - Lisbon, Portugal DA - 06.06.2017 KW - Microbiological investigation KW - Medieval stained glass KW - SEM analysis PY - 2017 AN - OPUS4-40573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Isotope analysis by molecular absorption spectrometry N2 - The use of molecular absorption spectrometry (MAS) for the determination of isotope amount ratios is here discussed. Preliminary results on the determination of isotope ratios of boron, copper and magnesium in reference materials are here presented and compared with their certificates. T2 - Adlershofer Kolloquium Analytik CY - Berlin, Germany DA - 13.06.2017 KW - Isotope KW - Molecular absorption KW - HR-CS-MAS KW - Isotopic shift KW - Spectrometry KW - Isotope ratio PY - 2017 AN - OPUS4-40574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Bridge Monitoring by Passive Seismic Data, First tests at the BLEIB reference structure N2 - Seismic wave velocities are related to elastic moduli and other properties and can serve as indicators for changes in the material. They are conventionally determined by active measurements. Using ideas from seismic interferometry determination from stacked cross-correlations of registrations of man-made and natural noise (“passive seimics“) is an effective alternative, as these data might be available from vibration monitoring anyway. The validity of this approach is demonstrated by a simple experiment based on recordings of man made noise using accelerometers at the reference structure. The s-wave (or more probable. guided wave) velocity was determined to be 2100 m/s in both active and passive experiments. T2 - Passive Imaging and monitoring in wave physics: from seismology to ultrasound CY - Cargese, France DA - 05.06.2017 KW - Bridge monitoring KW - Passive seismics KW - Ambient noise KW - Interferometry KW - Elastic wave velocity PY - 2017 AN - OPUS4-40577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bennetts, V.H. A1 - Neumann, Patrick P. T1 - Probabilistic air flow modelling using turbulent and laminar characteristics for ground and aerial robots N2 - For mobile robots that operate in complex, uncontrolled environments, estimating air flow models can be of great importance. Aerial robots use air flow models to plan optimal navigation paths and to avoid turbulence-ridden areas. Search and rescue platforms use air flow models to infer the location of gas leaks. Environmental monitoring robots enrich pollution distribution maps by integrating the information conveyed by an air flow model. In this paper, we present an air flow modelling algorithm that uses wind data collected at a sparse number of locations to estimate joint probability distributions over wind speed and direction at given query locations. The algorithm uses a novel extrapolation approach that models the air flow as a linear combination of laminar and turbulent components. We evaluated the prediction capabilities of our algorithm with data collected with an aerial robot during several exploration runs. The results show that our algorithm has a high degree of stability with respect to parameter selection while outperforming conventional extrapolation approaches. In addition, we applied our proposed approach in an industrial application, where the characterization of a ventilation system is supported by a ground mobile robot. We compared multiple air flow maps recorded over several months by estimating stability maps using the Kullback-Leibler divergence between the distributions. The results show that, despite local differences, similar air flow patterns prevail over time. Moreover, we corroborated the validity of our results with knowledge from human experts. T2 - IEEE International Conference on Robotics and Automation (ICRA) CY - Singapore DA - 29.05.2017 KW - Mapping KW - Field robots KW - Environment monitoring and management KW - Aerial systems KW - Perception and autonomy PY - 2017 AN - OPUS4-40548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bennetts, V.H. A1 - Neumann, Patrick P. T1 - Probabilistic air flow modelling using turbulent and laminar characteristics for ground and aerial robots N2 - For mobile robots that operate in complex, uncontrolled environments, estimating air flow models can be of great importance. Aerial robots use air flow models to plan optimal navigation paths and to avoid turbulence-ridden areas. Search and rescue platforms use air flow models to infer the location of gas leaks. Environmental monitoring robots enrich pollution distribution maps by integrating the information conveyed by an air flow model. In this paper, we present an air flow modelling algorithm that uses wind data collected at a sparse number of locations to estimate joint probability distributions over wind speed and direction at given query locations. The algorithm uses a novel extrapolation approach that models the air flow as a linear combination of laminar and turbulent components. We evaluated the prediction capabilities of our algorithm with data collected with an aerial robot during several exploration runs. The results show that our algorithm has a high degree of stability with respect to parameter selection while outperforming conventional extrapolation approaches. In addition, we applied our proposed approach in an industrial application, where the characterization of a ventilation system is supported by a ground mobile robot. We compared multiple air flow maps recorded over several months by estimating stability maps using the Kullback-Leibler divergence between the distributions. The results show that, despite local differences, similar air flow patterns prevail over time. Moreover, we corroborated the validity of our results with knowledge from human experts. T2 - IEEE International Conference on Robotics and Automation (ICRA) CY - Singapore DA - 29.05.2017 KW - Mapping KW - Field robots KW - Environment monitoring and management KW - Aerial systems KW - Perception and autonomy PY - 2017 AN - OPUS4-40549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bennetts, V.H. A1 - Kucner, T.P. A1 - Schaffernicht, E. A1 - Neumann, Patrick P. A1 - Fan, H. A1 - Lilienthal, A.J. T1 - Probabilistic Air Flow Modelling Using Turbulent and Laminar Characteristics for Ground and Aerial Robots N2 - For mobile robots that operate in complex, uncontrolled environments, estimating air flow models can be of great importance. Aerial robots use air flow models to plan optimal navigation paths and to avoid turbulence-ridden areas. Search and rescue platforms use air flow models to infer the location of gas leaks. Environmental monitoring robots enrich pollution distribution maps by integrating the information conveyed by an air flow model. In this paper, we present an air flow modelling algorithm that uses wind data collected at a sparse number of locations to estimate joint probability distributions over wind speed and direction at given query locations. The algorithm uses a novel extrapolation approach that models the air flow as a linear combination of laminar and turbulent components. We evaluated the prediction capabilities of our algorithm with data collected with an aerial robot during several exploration runs. The results show that our algorithm has a high degree of stability with respect to parameter selection while outperforming conventional extrapolation approaches. In addition, we applied our proposed approach in an industrial application, where the characterization of a ventilation system is supported by a ground mobile robot. We compared multiple air flow maps recorded over several months by estimating stability maps using the Kullback-Leibler divergence between the distributions. The results show that, despite local differences, similar air flow patterns prevail over time. Moreover, we corroborated the validity of our results with knowledge from human experts. T2 - IEEE International Conference on Robotics and Automation (ICRA) CY - Singapore DA - 29.05.2017 KW - Mapping KW - Field Robots KW - Environment Monitoring and Management KW - Aerial Systems KW - Perception and Autonomy PY - 2017 SN - 978-1-5090-4632-4 SP - 1 EP - 7 PB - IEEE AN - OPUS4-40544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalinka, Gerhard A1 - ElAbshihy, K. T1 - Circumventing boundary effects while characterizing epoxy/copper interphases using nanoindentation N2 - Characterization of the size and mechanical properties of interphases is essential when designing multicomponent materials. When nanoindentation is used to investigate the size and mechanical properties of an interphase, a common challenge is that the indenter or the stress zone formed around it are often restricted by the reinforcement, making it difficult to distinguish the mechanical property variations caused by the interphase itself from those caused by the boundary effect. In this work, a testing system was developed that allows determining the indent affected zone and accounting for it in the interphase measurements of an epoxy/Cu system. Using finite element analysis, we confirmed the validity of the proposed system. Nanoindentation was used to investigate the Interphase between copper and two different epoxy systems; amine-cured and anhydride-cured. Nanoindentation results showed that a copper layer that is only 10 nm thick still exhibits a constriction effect on the indentations in its vicinity. The amine-cured epoxy did not show any sign of interphase existence using the introduced method. However, a soft interphase with a thickness of ~1.7 μm was measured on theanhydride-cured epoxy. Furthermore, we show that the proposed system can be used to determine the interphase thickness as well as its relative mechanical properties regardless of the indentation depth. This system can be further used for investigating other polymer/metal interphases to better understand the factors influencing them, thus helping engineer the interphase size and properties to enhance composite performance. KW - Interphase KW - Polymer-metal KW - Epoxy KW - Copper KW - Composites KW - Nanoindentation PY - 2017 DO - https://doi.org/10.1080/09276440.2017.1286878 SN - 0927-6440 SN - 1568-5543 VL - 24 IS - 9 SP - 833 EP - 848 PB - Taylor & Francis CY - UK AN - OPUS4-39128 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mitzkus, Anja A1 - Sahre, Mario A1 - Reinstädt, Philipp A1 - Griepentrog, Michael A1 - Beck, Uwe A1 - Köppe, Enrico A1 - Bartholmai, Matthias A1 - Basedau, Frank A1 - Hofmann, Detlef A1 - Gong, Xin A1 - Schukar, Vivien T1 - Altbekannter Watts-Elektrolyt, junge Hightech-Anwendung, Nickel- und Nickel-Eisen-Schichten als magnetostriktive Aktorschicht auf faseroptischen Sensoren N2 - Durch faseroptische Sensoren können Bauteile im Einsatz kontinuierlich überwacht und frühzeitig Informationen über Materialveränderungen gewonnen werden. Mittels einer magnetostriktiven Aktorschicht, welche den Sensor umhüllt, kann nun auch die korrekte Sensorfunktion jederzeit kontrolliert werden. Als Aktorschicht eignet sich galvanisch abgeschiedenes reines Nickel oder Nickel-Eisen in der Zusammensetzung 50:50. Um diese haftfest mit dem Sensor zu verbinden wurde ein ECD/PVD-Kombinationsschichtsystem entwickelt. Die mechanischen Eigenschaften der ECD-Schicht können sowohl mit einer auf die Fasergeometrie angepassten instrumentierten Eindringprüfung als auch einem 2-Punkt-Biegeversuch bestimmt werden. KW - Faseroptik-Sensoren KW - ECD-Aktorschicht KW - PVD-Haftfestigkeit KW - Nickel-/Nickel-Eisen- Magnetostriktion PY - 2016 SN - 2195-5891 SN - 2195-5905 VL - 12 SP - 1 EP - 4 AN - OPUS4-39129 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pogány, A. A1 - Balslev-Harder, D. A1 - Braban, Ch. F. A1 - Cassidy, N. A1 - Ebert, V. A1 - Ferracci, V. A1 - Hieta, T. A1 - Leuenberger, D. A1 - Martin, N. A. A1 - Pascale, C. A1 - Peltola, J. A1 - Persijn, S. A1 - Tiebe, Carlo A1 - Twigg, M. M. A1 - Vaittinen, Olavi A1 - van Wijk, J. A1 - Wirtz, K. A1 - Niederhauser, B. T1 - A metrological approach to improve accuracy and reliability of ammonia measurements in ambient air N2 - The environmental impacts of ammonia (NH3) in ambient air have become more evident in the recent decades, leading to intensifying research in this field. A number of novel analytical techniques and monitoring instruments have been developed, and the quality and availability of reference gas mixtures used for the calibration of measuring instruments has also increased significantly. However, recent inter-comparison measurements show significant discrepancies, indicating that the majority of the newly developed devices and reference materials require further thorough validation. There is a clear need for more intensive metrological research focusing on quality assurance, intercomparability and validations. MetNH3 (Metrology for ammonia in ambient air) is a three-year project within the framework of the European Metrology Research Programme (EMRP), which aims to bring metrological traceability to ambient ammonia measurements in the 0.5–500 nmol mol−1 amount fraction range. This is addressed by working in three areas: (1) improving accuracy and stability of static and dynamic reference gas mixtures, (2) developing an optical transfer standard and (3) establishing the link between high-accuracy metrological standards and field measurements. In this article we describe the concept, aims and first results of the project. KW - Ammonia in ambient air KW - Traceability KW - Reference gas standards KW - Optical transfer standard KW - Validation and testing infrastructure PY - 2016 DO - https://doi.org/10.1088/0957-0233/27/11/115012 SN - 0957-0233 VL - 27 IS - 11 SP - 115012 EP - 115026 PB - IOP Publishing Ltd. AN - OPUS4-39130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Nanoscience, SAXS and you N2 - A presentation demonstrating small-angle x-ray scattering and its applications. T2 - Invited talk CY - Deutsches GeoForschungsZentrum, Potsdam, Germany DA - 19.01.2017 KW - SAXS KW - Nanoscience PY - 2017 AN - OPUS4-39136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Unger, Wolfgang T1 - IND15 JRP SurfChem: Traceable quantitative surface chemical analysis for industrial applications N2 - The SurfChem project has made a significant contribution to traceable quantitative surface chemical analysis for industrial applications by delivering new certified reference materials and test samples for specific technical applications. Regular performance tests of instruments, metrological methodology for the detection of (bio)organic surface species, ambient and non-destructive surface chemical analysis for in-line process control and new in situ characterisation techniques of catalytically active surfaces have been achieved. KW - Surface analysis KW - Metrology KW - Euramet EMRP PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-388673 UR - http://www.euramet.org/research-innovation/search-research-projects/details/?eurametCtcp_project_show%5Bproject%5D=1115&eurametCtcp_project%5Bback%5D=893&cHash=5fd23fc7f759db18176584b5d8a5fe89 SP - 1 EP - 39 CY - Teddington AN - OPUS4-38867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Inter-laboratory comparison on shape of bipyramidal TiO2 nanoparticles by TEM N2 - The TiO2 material selected for the present inter-laboratory comparison (ILC) was the bipyramidal anatase UT001 batch synthesized hydrothermally by University of Turin in the frame of the EU/FP7 Project SETNanoMetro and carefully prepared on TEM grids by BAM to be distributed to the ILC participants. A clear measurement protocol including data analysis and reporting (including an xls reporting template) has been also prepared by BAM. 14 of 18 participants have measured and reported results which have been already checked by BAM as being conform to the agreed protocol. After receiving the last results (of 4 participants) the ILC data evaluation will be carried out by BAM in line with agreed ISO/TC229 procedures as for the other case sudies. T2 - Annual Meeting of ISO/TC 229 Nanotechnologies CY - Singapore, Republic of Singapore DA - 07.11.2016 KW - TiO2 KW - Nanoparticles KW - Inter-laboratory comparison KW - Shape KW - TEM KW - Particle size distribution PY - 2016 AN - OPUS4-38868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Kanzler, Daniel T1 - Zuverlässigkeitsanalyse von digitalen Radiographie-Systemen bei der Prüfung von realen Materialdefekten N2 - Die zerstörungsfreie Prüfung (ZfP) ist aus solchen Bereichen unseres Lebens nicht mehr wegzudenken, in denen Schäden mit hohen Folgekosten oder Gefährdungen von Menschenleben entstehen können (Beispiele: Transportwesen, Energieerzeugung, Chemieindustrie). In der Praxis kann ein Prüfsystem an seine Grenzen geraten, z.B. bei kleinen Defekten. Defekte mit kritischer Größe werden möglicherweise nicht detektiert. Daher müssen probabilistische Bewertungsverfahren das Prüfsystem beschreiben. Es wird eine objektive Qualitätskennzahl gesucht, auf deren Basis die Anwendbarkeit der Prüfmethode definiert werden soll. Die Auffindwahrscheinlichkeit (engl. probability of detection - POD) erfüllt diese Anforderung. Die POD zeigt auf Basis des Zusammenhangs und der Streuung der Daten, ob das Verfahren für die Prüftätigkeit akzeptiert werden kann oder noch verbessert werden muss. Das ursprüngliche POD-Verfahren wurde für quasi eindimensionale Defekte in dünnen Luftfahrtbauteilen entwickelt. In der industriellen Realität ist diese Bewertung ein Balanceakt zwischen Statistik und Durchführbarkeit: Die Prüfung soll mit realen Defektdaten für die spätere Produktion des Bauteils (bzw. wiederkehrende Wartungsprüfung) bewertet werden. Doch die notwendige Gegenüberstellung zwischen Schliffdaten, für die Erfassung der wahren Defektgröße von räumlich ausgeprägten Defekten und dem Signal eines ZfP-Systems stellt sich als herausfordernde und kostenintensive Aufgabe heraus. Sowohl die Aufstellung eines gemeinsamen Koordiantensystems als auch die Beschreibung und Angleichung der Daten stellen eine notwendige Vorarbeit dar. In dieser Arbeit wird ein mögliches Vorgehen entwickelt, dass im Weiteren eingesetzt werden kann. Während in der Literatur zum Thema POD häufig die Begrenzung des Einsatzes einer eindimensionalen POD (POD mit einem Defektparameter) für reale Defekte bereits erkannt wurde, soll außerdem in dieser Arbeit das Verfahren auf der Signalseite umfassender erweitert werden, um die Einbeziehung realer Defekte in die POD-Bewertung zu ermöglichen. Hierfür werden mit Hilfe dieser Arbeit zwei wesentliche Neuerungen in der POD-Bewertung eingeführt: 1. Die Anzeigenfläche wird als wichtiges Indiz zur Detektion in die Bewertung eingeführt. Dabei zeigt der Ansatz einer Observer-POD, bei dem der Detektierbarkeit eines Defekts beschrieben wird, eine Möglichkeit in die Bewertung zu erweitern. Jedoch wird die notwendige Datenanzahl die für eine Observer-POD selten mit Experimenten erreicht. Daher schlagen wir die Einführung eines Glättungsalgorithmus vor, um auch auf der Basis von wenigen Daten die Flächenabhängigkeit zu erfassen. Der Algorithmus wird hierbei durch simulierte Daten auf seine Funktionsfähigkeit überprüft, bevor er auf reale Defekte angewendet wird. Gleichzeitig helfen die simulierten Daten einen Vergleich zu den vorhergegangenen Ansätzen zu ermöglichen. 2. Darüber hinaus reichen die Daten der realen Defekte häufig nicht aus, um die statistische Forderung zu gewährleisten, so dass es notwendig, wird künstliche Defekte mit einzubeziehen. Deshalb sollen die vorhanden künstlichen Defekte in Form von Referenzdefekten mit einbezogen werden, um die statistische Grundlage zu erhöhen. Für die Prüfung von Referenzdefekten sind jedoch wichtige Einflussgrößen (z.B. Oberflächenrauhigkeit) nicht vorhanden. Wegen der unterschiedlichen Aussagekraft der Daten und zur Vermeidung einer zu optimistischen Abschätzung, ist eine einfache Mischung der Daten ausgeschlossen. Um realen Defekten eine Möglichkeit dafür zu schaffen, dass die Eigenschaften der realen Defekte angemessen auf das Ergebnis der Bewertung des Verfahrens Einfluss nehmen können, wird eine gewichtete Kombination der Defektdaten für die Bewertung vorgestellt. Das Vorgehen wird am Beispiel der radiographischen Prüfung einer elektronenstrahlgeschweißten Naht durchgeführt. Die Schweißnaht verbindet den Deckel zur Außenwand eines Kupferbehältern, der für die spätere Endlagerung von verbrauchten Brennstäben aus Kernkraftwerken entwickelt wurde. Die Messergebnisse stammen aus von der Firma Posiva Oy, dem zuständigen Unternehmen für die Endlagerung von verbrauchten Brennstäben aus Kernkraftwerken in Finnland. Hierbei stellt die POD-Bewertung ein wichtiges Element in der Gesamtrisikobewertung für das Endlagersystem dar. T3 - BAM Dissertationsreihe - 153 KW - Radiographie KW - POD KW - Zuverlässigkeit KW - Zerstörungsfreie Prüfung (ZfP) KW - Probabilistische Bewertung PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-388723 SN - 978-3-9818270-1-9 SN - 1613-4249 VL - 153 SP - iii EP - 134 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38872 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oberleitner, Lidia A1 - Garbe, L.-A. A1 - Dahmen-Levison, Ursula A1 - Schneider, Rudolf T1 - Improved strategies for selection and characterization of new monoclonal anticarbamazepine antibodies during the screening process using feces and fluorescence polarization immunoassay N2 - Immunoassays are suitable tools for high-throughput screenings. The prerequisite for accurate determinations by these methods is the selection of an excellent antibody. The production and selection of monoclonal antibodies is usually a tedious process. In this study, new strategies for improving antibody production and characterization were applied. This includes the monitoring of the immunization progress in mice through antibodies extracted from feces, which allows a time-resolved and animal-friendly monitoring of the immune response. Additionally, fluorescence polarization immunoassay (FPIA) could be successfully applied for fast and easy examination of cell culture supernatants and the investigation of antibody/antigen interactions including kinetics and fluorescence properties. These methods simplify the selection of the optimal antibody. As a target analyte, carbamazepine was chosen. This is a widely used antiepileptic drug which also frequently occurs in the environment. The new antibody enables CBZ determination in the concentration range 0.66–110 µg L-1 within 10 min using a high-throughput microtiter plate-based FPIA, and between 1.4 and 79 µg L-1 within 5 min applying an automated cuvette-based FPIA instrument, and from 0.05–36 µg L-1 using ELISA. The measurements were performed at a non-equilibrium state which improved the sensitivity and selectivity of the assays. Due to low cross-reactivity especially towards the main CBZ metabolite and other pharmaceuticals (<1%), this antibody gives the opportunity for application in medical and environmental analyses. KW - Antikörper KW - Emerging Pollutants KW - Schadstoffe KW - Monoklonal KW - Pharmazeutika KW - Arzneistoffe KW - Assay KW - Pesticide parathion-methyl KW - Waste-water KW - Samples KW - Pharmaceuticals KW - Quantification PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-392473 DO - https://doi.org/10.1039/c6ay01968d SN - 1759-9660 VL - 8 SP - 6883 EP - 6894 PB - Royal Society of Chemistry CY - London AN - OPUS4-39247 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kuhne, Maren A1 - Schneider, Rudolf T1 - Verfahren zur Charakterisierung und Selektion Hapten-spezifischer Hybridomazellen und Herstellung hochaffiner monoklonaler anti-Hapten-Antikörper N2 - Die vorliegende Erfindung liegt auf dem Gebiet der Herstellung hochaffiner anti-Hapten-Antikörper. Ferner befasst sich die vorliegende Erfindung mit einem Markierungsverfahren zur durchflußzytometrischen Charakterisierung und Selektion Hapten-spezifischer Hybridomazellen KW - Patent KW - Antikörper KW - Monoklonal KW - Durchflußzytometrie KW - Markierung KW - Label PY - 2016 VL - DE 10 2014 114 522 A1 2016.04.07 SP - 1 EP - 16 CY - München AN - OPUS4-39248 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Illerhaus, Bernhard T1 - Hinweis zum Betrieb von Mikrofokusröntgenröhren N2 - Beim Betrieb von µFokus-Röntgenröhren entsprechend der Betriebsanleitung können schwerwiegende Schäden auftreten. KW - Hochspannungsüberschlag PY - 2017 UR - http://www.dgzfp.de/Portals/24/Zeitung/Ausgaben/Zeitung153.pdf IS - 153 SP - 18 EP - 18 PB - DGZfP AN - OPUS4-39249 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Oberleitner, Lidia T1 - Immunochemical determination of caffeine and carbamazepine in complex matrices using fluorescence polarization N2 - Pharmacologically active compounds are omnipresent in contemporary daily life, in our food and in our environment. The fast and easy quantification of those substances is becoming a subject of global importance. The fluorescence polarization immunoassay (FPIA) is a homogeneous mix-and-read format and a suitable tool for this purpose that offers a high sample throughput. Yet, the applicability to complex matrices can be limited by possible interaction of matrix compounds with antibodies or tracer. Caffeine is one of the most frequently consumed pharmacologically active compounds and is present in a large variety of consumer products, including beverages and cosmetics. Adverse health effects of high caffeine concentrations especially for pregnant women are under discussion. Therefore, and due to legal regulations, caffeine should be monitored. Automated FPIA measurements enabled the precise and accurate quantification of caffeine in beverages and cosmetics within 2 min. Samples could be highly diluted before analysis due to high assay sensitivity in the low μg/L range. Therefore, no matrix effects were observed. The antiepileptic drug carbamazepine (CBZ) is discussed as a marker for the elimination efficiency of wastewater treatment plants and the dispersion of their respective effluents in surface water. The development of a FPIA for CBZ included the synthesis and evaluation of different tracers. Using the optimum tracer CBZ-triglycine-5-(aminoacetamido) fluorescein, CBZ concentrations in surface waters could be measured on different platforms: one sample within 4 min in tubes or 24 samples within 20 min on microtiter plates (MTPs). For this study, a commercially available antibody was used, which led to overestimations with recovery rates up to 140% due to high cross-reactivities towards CBZ metabolites and other pharmaceuticals. For more accurate CBZ determination, a new monoclonal antibody was produced. In this attempt, methods for improving the monitoring during the production process were successfully applied, including feces screening and cell culture supernatant screening with FPIA. The new monoclonal antibody is highly specific for CBZ and showed mostly negligible cross-reactivities towards environmentally relevant compounds. Measurements at non-equilibrium state improved the sensitivity and selectivity of the developed FPIA due to slow binding kinetics of the new antibody. Additionally, this measure enables for CBZ determination over a measurement range of almost three orders of magnitude. The comprehensively characterized antibody was successfully applied for the development of sensitive homogeneous and heterogeneous immunoassays. The new antibody made the development of an on-site measurement system for the determination of CBZ in wastewater possible. After comprehensive optimization, this automated FPIA platform allows the precise quantification of CBZ in wastewater samples only pre-treated by filtration within 16 min. Recovery rates of 61 to 104% were observed. Measurements in the low μg/L range are possible without the application of tedious sample preparation techniques. Different FPIA platforms including MTPs, cuvettes and tubes were successfully applied. For the choice of the right format, the application field should be considered, e.g. desired sample throughput, usage for optimization or characterization of antibodies or if a set-up for routine measurements is sought for. For high sample throughput and optimization, FPIA performance on MTPs is advantageous. The best results for the application to real samples were obtained using kinetic FP measurements in cuvettes. T3 - BAM Dissertationsreihe - 154 KW - Antibody KW - Coffee KW - ELISA KW - Fluorophore tracer KW - Wastewater PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-392506 SN - 978-3-9818270-2-6 SN - 1613-4249 VL - 154 SP - 1 EP - 124 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39250 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Wilke, Manuel A1 - Fischer, Franziska A1 - Röllig, Mathias A1 - Maierhofer, Christiane A1 - Emmerling, Franziska T1 - Warming up for mechanosynthesis – temperature development in ball mills during synthesis N2 - We present a first direct measurement of the temperature during milling combined with in situ Raman spectroscopy monitoring. The data reveal a low temperature increase due to the mechanical impact and clear temperature increases as a consequence of the reaction heat. Based on the data, temperature rises as postulated in the magma plasma and hot spot theory can be excluded for soft matter milling syntheses. KW - Thermography KW - Milling KW - Mechanochemistry KW - Soft matter PY - 2017 DO - https://doi.org/10.1039/c6cc08950j SN - 1364-548X SN - 1359-7345 SN - 0009-241X VL - 53 IS - 10 SP - 1664 EP - 1667 AN - OPUS4-39251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ewert, Uwe T1 - Progress in digital industrial radiology - Part 1: Radiographic techniques-film replacement and backscatter imaging N2 - Similar to the success story of digital photography a major upheaval has been observed in digital industrial radiology. This paper is split into 3 parts: Part 1: Film Replacement and Backscatter Imaging: Computed radiography with phosphor imaging plates substitutes film applications. Digital Detector Arrays enable an extraordinary increase of contrast sensitivity in comparison to film radiography. The increased sensitivity of digital detectors enables the efficient usage for dimensional measurements and functionality tests substituting manual maintenance. The digital measurement of wall thickness and corrosion status is state of the art in petrochemical industry. Photon counting and energy discriminating detectors are applied up to 300 Kv provide increased thickness dynamic and material discrimination by synchronously acquisition of images of the high and low energy part of the spectrum. X-ray back scatter techniques have been applied in safety and security relevant applications with single sided access of source and detector. First inspections of CFRP in aerospace industry were successfully conducted with newly designed back scatter cameras. Numeric modeling is used to design X-Ray optics and inspection scenarios as well as conducting RT training. Part 2: Computed tomography (CT) Part 3: Micro Radiography and Micro CT. KW - Digital radiography KW - Computed tomography KW - Laminography KW - Imaging plates KW - Digital detector arrays KW - Photon counting detectors KW - Back scatter KW - Numeric modelling KW - CFRP KW - Welding KW - Corrosion PY - 2016 VL - 1-2 SP - 37 EP - 43 AN - OPUS4-39163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Esteban-Fernandez, Diego A1 - Traub, Heike A1 - Hutchinson, R. T1 - High resolution laser ablation NWRimage system for single cell imaging N2 - The traceability and availability of nanoparticles enables their use to enhance a variety of nano-biological and nano-medicinal applications. The particular size and shape of nanoparticles determine the uptake rate and pathway into the cell, and therefore impact specific cell components and processes. Selecting specific particle types allows researchers to target the process or structure of interest, with minimal additional impact. This can be used for drug or DNA delivery, and is being explored for use in oncology. Understanding the different uptake mechanisms and impacted processes requires sub-cellular Imaging resolution to determine, for example, whether or not the nanoparticles are reaching the nucleus. Sub-cellular imaging has traditionally been challenging to achieve with laser ablation ICP-MS due to a lack of sensitivity at small spots. Bioimaging using LA-ICP-MS is a well-established technique, but usually applied on the tissue scale, which depends on larger spot areas where sensitivity is less problematic. The improved sensitivity and washout from the NWRimage has allowed faster imaging of smaller spots. The NWRimage also provides the possibility of true sub-micron spot sizes. This work compares the capabilities of standard laser Ablation (NWR213 system) with results from the NWRimage platform, which has been optimized for imaging applications. T2 - European Winter Conference on Plasma Spectrochemistry CY - St. Anton, Austria DA - 19.02.2017 KW - Laser ablation KW - Imaging KW - Nanoparticle PY - 2017 AN - OPUS4-39281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Franziska A1 - Emmerling, Franziska T1 - Synthesen in der Kugelmühle N2 - Wärme, Licht und Elektrizität sind die typischen Energiequellen chemischer Synthesen. In den letzten Jahren haben sich aber auch mechanische Kräfte etabliert: Mechanochemie braucht kein Lösungsmittel und funktioniert bei Raumtemperatur. Über die zugrundeliegenden Prozesse ist bislang wenig bekannt. KW - Mechanochemie PY - 2016 DO - https://doi.org/10.1002/nadc.20164046717 SN - 1439-9598 SN - 1868-0054 VL - 64 IS - 5 SP - 509 EP - 513 AN - OPUS4-39282 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Franziska T1 - Geschüttelt, nicht gerührt - Chemie in der Kugelmühle N2 - Chemie kann so einfach sein: Zwei Pulver in eine Kugelmühle geben, kräftig schütteln und schon entsteht eine neue Verbindung. Dr. Franziska Fischer konnte durch Echtzeitüberwachung die Reaktionswege solcher mechanochemischen Synthesen aufdecken. Ihre Dissertation am Institut für Chemie der Humboldt-Universität und an der Bundesanstalt für Materialforschung und -prüfung leistet einen entscheidenden Beitrag zur Entwicklung umweltverträglicher und kosteneffizienter Synthesemethoden. T2 - Dissertationspreis Adlershof für 2016 CY - Berlin, Germany DA - 15.02.2017 KW - Mechanochemie PY - 2017 AN - OPUS4-39283 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lauer, Franziska A1 - Seifert, Stephan A1 - Kneipp, Janina A1 - Weidner, Steffen T1 - Simplifying the Preparation of Pollen Grains for MALDI-TOF MS Classification N2 - Matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) is a well-implemented analytical technique for the investigation of complex biological samples. In MS, the sample preparation strategy is decisive for the success of the measurements. Here, sample preparation processes and target materials for the investigation of different pollen grains are compared. A reduced and optimized sample preparation process prior to MALDI-TOF measurement is presented using conductive carbon tape as target. The application of conductive tape yields in enhanced absolute signal intensities and mass spectral pattern information, which leads to a clear separation in subsequent pattern analysis. The results will be used to improve the taxonomic differentiation and identification, and might be useful for the development of a simple routine method to identify pollen based on mass spectrometry. KW - PCA KW - MALDI-TOF MS KW - Conductive carbon tape KW - Pollen KW - Sample pretreatment PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-392885 UR - http://www.mdpi.com/1422-0067/18/3/543/ DO - https://doi.org/10.3390/ijms18030543 SN - 1422-0067 VL - 18 IS - 3 SP - 543 EP - 554 PB - MDPI AG CY - Basel, Switzerland AN - OPUS4-39288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ehlert, Christopher A1 - Kröner, D. A1 - Saalfrank, P. T1 - A combined quantum chemical/molecular dynamics study of X-rayphotoelectron spectra of polyvinyl alcohol using oligomer models N2 - X-ray photoelectron spectroscopy (XPS) is a powerful tool for probing the local chemical environment ofatoms near surfaces. When applied to soft matter, such as polymers, XPS spectra are frequently shifted andbroadened due to thermal atom motion and by interchain interactions. We present a combined quantummechanical QM/molecular dynamics (MD) simulation of X-ray photoelectron spectra of polyvinyl alcohol(PVA) using oligomer models in order to account for and quantify these effects on the XPS (C1s) signal. Inour study, molecular dynamics at finite temperature were performed with a classical forcefield and by abinitio MD (AIMD) using the Car–Parrinello method. Snapshots along the trajectories represent possibleconformers and/or neighbouring environments, with different C1s ionization potentials for individualC atoms leading to broadened XPS peaks. The latter are determined by Δ-Kohn Sham calculations. Wealso examine the experimental practice of gauging XPS (C1s) signals of alkylic C-atoms in C-containingpolymers to the C1s signal of polyethylene. We find that (i) the experimental XPS (C1s) spectra of PVA (position and width) can be roughly repre-sented by single-strand models, (ii) interchain interactions lead to red-shifts of the XPS peaks by about0.6 eV, and (iii) AIMD simulations match the findings from classical MD semi-quantitatively. Further, (iv)the gauging procedure of XPS (C1s) signals to the values of PE, introduces errors of about 0.5 eV. KW - XPS KW - Quantummechanical molecular dynamics simulation KW - Polyvinyl alcohol PY - 2015 DO - https://doi.org/10.1016/j.elspec.2014.12.007 SN - 0368-2048 VL - 199 SP - 38 EP - 45 PB - Elsevier B.V. AN - OPUS4-39290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kästner, Claudia T1 - Tuning the catalytic activity of silver nanoparticles N2 - The use of silver nanoparticles in consumer related products has significantly increased over the last decade, especially due to their antimicrobial properties. Today they are used in a variety of products, which range from textiles to dietary supplements. Thus, investigations on nanoscale silver become increasingly important in many fields like biomedicine or catalysis. Unfortunately, the results of these studies are extremely diverse and do not lead to a consistent evaluation of the toxicity of silver nanoparticles. The main problem is the use of nonuniform and poorly characterized particles with broad size distributions. To overcome this problem we modified the known polyol process to synthesize ultra-small core-shell silver nanoparticles in a large scale. The particles are highly stable and show no aggregation for more than six months. Small-angle X-ray scattering analysis reveals a narrow size distribution of the silver cores with a mean radius of 3 nm and a distribution width of 0.6 nm. Dynamic light scattering provides a hydrodynamic radius of 10.0 nm and a PDI of 0.09. The stabilizing ligand PAA can be easily exchanged by biomolecules to modify the surface functionality. Replacements of PAA with glutathione and bovine serum albumin have been successfully performed. To demonstrate the broad applicability of our particles we performed catalysis experiments with the reduction of 4-nitrophenol as model reaction. The PAA-stabilized particles show a catalytic activity of (436 ± 24) L g-1 s-1, which is the highest reported in literature for silver nanoparticles. In contrast, GSH and BSA passivate the surface substantially resulting in lower catalytic activities. T2 - Australian Colloid and Interface Symposium 2017 CY - Coffs Harbour, New South Wales, Australia DA - 29.01.2017 KW - SAXS KW - Protein coating KW - Catalysis PY - 2017 AN - OPUS4-39203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kästner, Claudia T1 - Food-dependent aggregation of silver nanoparticles during an artificial digestion N2 - In the last decade the utilization of silver nanoparticles in consumer related products is strongly enhanced. Therefore, many studies focus on investigations regarding their toxicological potential. This includes investigations concerning uptake, distribution and excretion of the particles. However, little attention was paid to changes of physical and chemical properties of the particles in the human body. A major question is if the particles are size and shape persistent and can survive the digestion process. In this study we analytically monitored the changes in the size distribution of colloidal silver during an artificial digestion process with the help of small angle X-ray scattering. We synthesized poly(acrylic acid) stabilized ultra-small silver nanoparticles with a radius of 3.1 nm and a size distribution width of 20%. The artificial digestion process mimics the gastro-intestinal passage and simulates the oral, gastric and small intestinal conditions. Additionally, we used as food components oil, starch, skimmed milk powder and mixture thereof to provide a preferably realistic environment. Large aggregates of up to 56 nm were determined in the absence of food additives. In contrast, the presence of oil and starch limit the radii of aggregates to about 10 nm. Only small aggregates of 6 nm radii were found in the presence of milk powder. It prevents primary particles from etching in the intestinal juice. Our results indicate that the silver nanoparticles can pass the digestion process in a nanoscale form but undergo a strong and food-dependent transformation in their state of aggregation. T2 - Australian Colloid and Interface Symposium 2017 CY - Coffs Harbour, New South Wales, Australia DA - 29.01.2017 KW - SAXS KW - Food additives KW - Aggregation PY - 2017 AN - OPUS4-39204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Vogl, Jochen A1 - Becker, Dorit A1 - Koenig, Maren A1 - Yim, Y.-H. A1 - Lee, K.-S. A1 - Goenaga-Infante, H. A1 - Malinowskiy, D. A1 - Hill, S. A1 - Ren, T. A1 - Wang, J. A1 - Vocke, R. D. A1 - Murphy, K. A1 - Nonose, N. A1 - Rienitz, O. A1 - Noordmann, J. T1 - Certification Report for the Isotopic Reference Materials ERM-AE142 and ERM-EB400 N2 - Lead (Pb) isotope amount ratios are commonly used in applications ranging from archaeology and forensic sciences to terrestrial and extra-terrestrial geochemistry. Despite their utility and frequency of use, only three certified isotope amount ratio reference materials are currently available for Pb: NIST SRMs 981, 982 and 983. Because SRM 981 has a natural Pb isotopic composition, it is mainly used for correcting instrumental mass discrimination or fractionation. This means that, at present, there are no other certified isotope reference materials with natural Pb isotopic composition that could be used for validating or verifying an analytical procedure involving the measurement of Pb isotope amount ratios. To fill this gap, two new reference materials, both certified for their Pb isotopic composition, have been produced together with a complete uncertainty assessment. These new reference materials offer SI traceability and an independent means of validating or verifying analytical procedures used to produce Pb isotope amount ratio measurements. ERM-EB400 is a bronze material containing a nominal Pb mass fraction of 45 mg/kg. ERM-AE142 is a high purity solution of Pb with a nominal mass fraction of 100 mg/kg. Both materials have been specifically produced to assist analysts in verifying or validating their analytical procedures. Note that while one of these reference materials requires the chemical separation of Pb from its matrix (ERM-EB400), the other does not (ERM-AE142). Details on the certification of these isotope reference materials are provided in this report. KW - Lead isotopic composition KW - Isotope ratio KW - Reference material KW - Mass spectrometry PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-392060 SP - 1 EP - 16 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Waiblinger, H. U. A1 - Bartsch, D. A1 - Brockmeyer, J. A1 - Bruenen-Nieweler, C. A1 - Busch, U. A1 - Haase, I. A1 - Hahn, A. A1 - Haarmann, M. A1 - Hauser, W. A1 - Huber, I. A1 - Jany, K. D. A1 - Kirmse, N. A1 - Lindeke, S. A1 - Neumann, K. A1 - Naumann, H. A1 - Paschke, A. A1 - Pietsch, K. A1 - Pöpping, B. A1 - Reiting, R. A1 - Schroeder, U. A1 - Schwägele, F. A1 - Weller, Michael G. A1 - Zagon, J. T1 - Methods of differentiating animal species in foods – Status quo N2 - Work on standardising methods in the field of animal species differentiation has been intensified in Germany in recent years, not least due to the horsemeat scandal in 2013. Even though there are now hardly ever any positive findings any more in examinations to detect horse adulterations in foods such as lasagne, animal species differentiation altogether ranks high in detecting adulteration of foods. This article therefore summarises the current status of analytical techniques used in Germany with standardisation at German level. It has been established by the working group “Biochemical and Molecular Biological Analytics” of the Lebensmittelchemische Gesellschaft (Food Chemistry Society within the German Chemical Society) with support of experts in the working group “Molecular biology techniques for differentiating plant and animal species” (§ 64 of the German Food and Feed Code – LFGB) and the “Immunology and molecular biology” task force of the food hygiene and Food of animal origin working group (ALTS), both from Germany. KW - Animal species differentiation KW - Fish species KW - PCR KW - Standardisation KW - DNA chip KW - Multiplex methods KW - Digital PCR KW - ELISA methods KW - Immunoassays KW - LC-MS/MS KW - Reference materials KW - Microarrays KW - LAMP KW - Interlaboratory studies PY - 2017 SN - 0179-2415 VL - 97 IS - 1 SP - 50 EP - 55 PB - Deutscher Fachverlag GmbH CY - Frankfurt AN - OPUS4-39264 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ertel, Jens-Peter A1 - Niederleithinger, Ernst A1 - Grohmann, Maria ED - Stahlmann, J. T1 - Das PileInspect-Projekt: Pfahlintegritätsprüfung durch Schwinganregung mittels eines elektrodynamischen Shakers N2 - Pfahlintegritätsprüfung von Bohrpfählen durch Messung der Impulsantwort mittels Schwinganregung und regularisierter Dekonvolution. T2 - Pfahlsymposium 2017 CY - Braunschweig, Germany DA - 23.02.2017 KW - Pfahlintegritätsprüfung KW - Tikhonov KW - Dekonvolution KW - PileInspect KW - Shaker PY - 2017 VL - 2017 IS - 102 SP - 217 EP - 235 PB - Eigenverlag Institut für Grundbau und Bodenmechanik - Technische Universität Braunschweig CY - Braunschweig AN - OPUS4-39272 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - 30 years LC-MS of synthetic macromolecules – an old story or something left to discover? N2 - Structure elucidation of complex synthetic copolymers still represents a challenge. A one-dimensional separation technique cannot give the answer to the question: What are the molar mass distribution (MMD), the functionality distribution (FTD), the chemical composition distribution (CCD), the monomer sequence distribution (MSD), the topology differences within a single broad distributed polymer sample? Is the coupling of liquid chromatographic separation techniques to mass spectrometry able to fill the gaps to a certain degree? Different LC separation techniques as size exclusion chromatography (SEC), liquid adsorption chromatography (LAC), liquid chromatography at critical conditions (LCCC) and gradient elution liquid chromatography (GELC) combined with Matrix assisted Laser Desorption Ionization (MALDI) respectively Electrospray Ionization (ESI) Time of Flight (TOF) mass spectrometry are able to give information which otherwise are completely inaccessible. In some cases, CID tandem mass spectrometry is applied. Fragmentation of suitable precursor ions resulted in typical fragment ion patterns. This technique enables an additional information on e.g. sequences, structural defects and topology of complex polymer mixtures. Often the deficiencies of stand-alone methods can be bridged. LC, blind to structural information needs mass spectrometry as one of the most powerful detectors able to give detailed information on e.g. the repeat units, functionalization or copolymer composition of the chromatographic separated constituents. A separation prior to MS reduces radical the dispersity which is one of the reasons for failing of MS. Also problems with different ionization probabilities in complex mixtures can partly be overcame. The lecture will provide a series of examples where LC-MS has been applied to evaluate complex macromolecules and mixtures of these. On- and offline coupling principles will be compared and the pros and cons of both mass spectrometric techniques will be discussed. T2 - SCM-8; International Symposium on the CY - Amsterdam, The Netherlands DA - 30.01.2017 KW - Characterization of polymers KW - HPLC KW - UPLC/ESI-TOF-MS KW - LC/MALDI-TOF-MS KW - Coupling techniques PY - 2017 AN - OPUS4-39276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baumann, Maria T1 - Characterization of poly(carbonate-dimethylsiloxane)-copolymers via LC, MALDI-TOF mass spectrometry and FTIR N2 - Copolymers made of polycarbonate (PC) and polydimethylsiloxane (PDMS) are broadly applied in material science. High impact-stability and transparency are the marks of bisphenol-A polycarbonate. PDMS on the other hand excels in thermal stability, flame resistance and weatherability. Combining those favourable characteristics in a copolymer yields in a ductile but impact-resistant and flame retardant material. In order to understand the synthesis process and to improve the quality and characteristics of a copolymer, knowing its structure is essential. The challenge lies in the variety of heterogeneities like molecular mass-, block-size- and block-distribution. This study addresses the structural characterization of PC-PDMS-copolymers using different liquid chromatographic techniques, including two dimensional combinations, hyphenated to MALDI-mass spectrometry and FTIR. The large difference in polarities of PC and PDMS is a challenge for liquid chromatography as well as ionization in MALDI. Nevertheless, we were able to differentiate between homopolymer and actual copolymer, clarify the presence of cyclic structures and gain information about the PDMS blocks T2 - SCM-8; International Symposium on the CY - Amsterdam, The Netherlands DA - 30.01.2017 KW - Copolymer characterization KW - Liquid chromatography KW - FTIR KW - MALDI-TOF-MS KW - LCCC PY - 2017 AN - OPUS4-39277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Weller, Michael G. T1 - Interview with Dr Michael G. Weller N2 - This author interview is by Dr Michael G. Weller, Head of Division 1.5 Protein Analysis at Federal Institute for Materials Research and Testing (BAM). BAM (www.bam.de/en) is a senior scientific and technical institute with responsibility to the German Federal Ministry for Economic Affairs and Energy. Dr Weller's review paper, Quality issues of research antibodies is available for download in Analytical Chemistry Insights. KW - Antibodies KW - Quality KW - Reproducibility PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-392326 UR - http://insights.sagepub.com/la_press_news.php?pa=view&news_item_id=4025 SP - 1 PB - SAGE CY - London AN - OPUS4-39232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Low field NMR spectroscopy for sustainable and flexible production of high quality chemical products N2 - The main development goal of process industries is to advance the continuous production of high-value products that meet high quality demands in flexible intensified continuous plants by introducing novel online sensing equipment and closed-loop control (CONSENS – integrated control and sensing- is funded from the European Union’s Horizon 2020 research and innovation programme). Therefore, we present the field integration of a benchtop NMR instrument into a modular production environment, focussing on suitable equipment for operation in hazardous areas with risk of explosive atmospheres. We investigated a pharmaceutical reaction step in order to describe challenges for the experimental design, the evaluation of complex NMR spectra and demonstrate automated data analysis tools. T2 - 5th Panic - Practical Applications of NMR in Industry Conferece CY - Hilton Head Island, SC 29928, USA DA - 20.02.2017 KW - Online NMR spectroscopy KW - Automated data evaluation KW - Process control PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-392333 AN - OPUS4-39233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Quantitative NMR spectroscopy for gas metrology – applications in liquefied petroleum gases N2 - The field of gas metrology is dealing with the development and improvement of gas analytical methods, as well as production of highly accurate primary reference standards. These are prepared at national metrological institutes (NMI) and represent the highest national level of traceability. Used for certification of secondary standards provided by specialty gas distributors these are very important for a high number of industrial sectors, which have to proof traceability due to legal or regulatory affairs, e.g., natural gas suppliers. Thus, improvements in the production and certification of these mixtures will have a direct influence on gas industry. Due to its direct correlation to the number of spins within active sample volume quantitative NMR spectroscopy (qNMR) is a highly promising method with absolute comparison abilities in complex systems. Especially for liquefied petroleum gases (LPG) it has the ability of studying the unmodified sample at same conditions like in the cylinder. In contrast to gas chromatography no preparation steps and no changes like evaporation of the sample are necessary. In this work we show the most recent results of our investigations on highly accurate LPG mixtures provided in constant-pressure piston cylinders. A dynamic pressure-resistant setup allows for sampling and circulation of the samples to ensure a homogeneous withdrawal from the cylinder. This is presented on examples of a commercial multicomponent LPG mixture obtained from specialty gas distributor, as well as two cylinders from the key comparison CCQM-K119 at highest level of international metrology. T2 - 5th Panic - Practical Applications of NMR in Industry Conferece CY - Hilton Head Island, SC 29928, USA DA - 20.02.2017 KW - Quantitative NMR spectroscopy KW - Gas metrology KW - Liquefied petroleum gas PY - 2017 AN - OPUS4-39234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Thin film analysis by SEM/EDX (EPMA) N2 - A short overview of thin film analysis by SEM/EDX is presented. Relevant steps such as optimization of instrumnetal parameters, extraction of net peak areas, use of standards, calculation of k-values and quantification with the dedicated thin film analysis software (Stratagem) are explained. Examples of different layered aystems are given together with validation of the results. T2 - Seminar Max-Planck-Institut fur Mikrostrukturphysik, Department Nano-Systems from ions, spins and electrons CY - Halle (an der Saale), Germany DA - 23.02.2017 KW - Thin film analysis KW - SEM/EDX KW - EPMA KW - k-values PY - 2017 AN - OPUS4-39235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mielke, Johannes A1 - Dohányosová, P. A1 - Müller, P. A1 - López-Vidal, S. A1 - Hodoroaba, Vasile-Dan T1 - Evaluation of electrospray as a sample preparation tool for electron microscopic investigations: Toward quantitative evaluation of nanoparticles N2 - The potential of electrospray deposition, for the controlled preparation of particles for imaging in electron microscopes, is evaluated on various materials: from mono-modal suspensions of spherical particles to multimodal suspensions and to real-world industrial materials. It is shown that agglomeration is reduced substantially on the sample carrier, compared with conventional sample preparation techniques. For the first time, it is possible to assess the number concentration of a tri-modal polystyrene suspension by electron microscopy, due to the high Deposition efficiency of the electrospray. We discovered that some suspension stabilizing surfactants form artifact particles during electrospraying. These can be avoided by optimizing the sprayed suspension. KW - Electrospary KW - Nanoparticles KW - Sample preparation KW - TEM grid KW - SEM PY - 2017 DO - https://doi.org/10.1017/S1431927616012587 SN - 1431-9276 SN - 1435-8115 VL - 23 IS - 1 SP - 163 EP - 172 PB - Cambridge University Press AN - OPUS4-39244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rabin, Ira ED - Elgvin, Torleif ED - Langlois, Michael ED - Davis, Kipp T1 - Material analysis of the fragments N2 - The International Qumran project conducted at the BAM Federal Institute for Materials Research and Testing in 2007–10 aimed at establishing an optimal methodology for an accurate characterization of the Dead Sea Scrolls to address such questions as archaeological provenance, origin, and attribution of fragments to a specific sheet (Rabin 2013). Using equipment of various degrees of complexity we have shown that part of the historic information stored in the material can be revealed by proper characterization of the material. The on-site investigation of the Dead Sea Scrolls fragments from The Schøyen Collection in October 2012 offered the first chance to test this methodology in a field study. For the first time, we used mobile and non-invasive technology exclusively, since we could not transport all of our laboratory equipment to Norway for this project. Moreover, besides the technical limitations dictated by the available equipment, we had to cope with limited time: it was impossible to perform the number of scans required for optimal characterization of over 30 fragments within the fourteen days available. Nevertheless this study presents an important step in the material analysis of the Dead Sea Scrolls, since the devices we used are easily transportable, well known, and easily accessible throughout the world. KW - Archaeometry KW - Cultural heritage KW - Dead Sea scrolls PY - 2016 SN - 978-0-5671-1300-9 SN - 978-0-5672-8571-3 VL - 71 SP - 61 EP - 77 PB - Bloomsbury T&T Clark Series CY - New York; NY 10018 USA AN - OPUS4-39246 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Bellon, Carsten T1 - Schlussbericht zum MNPQ-Projekt 18/11 - Simulationsbasierte Effizienzsteigerung bei Nanofokus-Röntgenröhren für höchstauflösende Materialprüfung N2 - Ziel des Projektes war, mit Hilfe von Computersimulationen die Brennfleckgröße, das Spektrum und die erreichbare Dosisleistung von Transmissionsröhren vorherzusagen sowie diese Kenngrößen zu optimieren. Hierbei sollten insbesondere die Materialien und Schichtdicken von Substrat und strahlungserzeugender Schicht untersucht werden. Eine Voraussetzung für die Überprüfung der Ergebnisse ist die reproduzierbare, korrekte messtechnische Erfassung von Brennfleckgrößen unterhalb 5 μm. KW - Brennfleckgröße KW - Röntgenröhre KW - Transmissionstarget KW - Computersimulation KW - Dosisleistung PY - 2015 SP - 1 EP - 13 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39192 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rauwolf, M. A1 - Turyanskaya, A. A1 - Roschger, A. A1 - Prost, J. A1 - Simon, R. A1 - Scharf, O. A1 - Radtke, Martin A1 - Schoonjans, Tom A1 - de Oliveira Guilherme Buzanich, Ana A1 - Klaushofer, K. A1 - Wobrauschek, P. A1 - Hofstaetter, J. G. A1 - Roschger, P. A1 - Streli, C. T1 - Synchrotron radiation micro X-ray fluorescence spectroscopy of thin structures in bone samples: comparison of confocal and color X-ray camera setups N2 - In the quest for finding the ideal synchrotron-radiation-induced imaging method for the investigation of trace element distributions in human bone samples, experiments were performed using both a scanning confocal synchrotron radiation micro X-ray fluorescence (SR-mXRF) (FLUO beamline at ANKA) setup and a full-field color X-ray camera (BAMline at BESSY-II) setup. As zinc is a trace element of special interest in bone, the setups were optimized for its detection. The setups were compared with respect to count rate, required measurement time and spatial resolution. It was demonstrated that the ideal method depends on the element of interest. Although for Ca (a major constituent of the bone with a low energy of 3.69 keV for its K alpha XRF line) the color X-ray camera provided a higher resolution in the plane, for Zn (a trace element in bone) only the confocal SR-µXRF setup was able to sufficiently image the distribution. KW - Synchrotron KW - BAMline KW - BESSY KW - XRF KW - X-ray Color Camera PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-391944 DO - https://doi.org/10.1107/S1600577516017057 SN - 1600-5775 VL - 24 SP - 307 EP - 311 PB - International Union of Crystallography AN - OPUS4-39194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krause, B. T1 - Detection of aluminum nanoparticles in biological media and in vitro N2 - Aluminum is the third most abundant element in the earth crust and therefore ubiquitously detectable in the environment. Mostly found in the form of derivatives such as silicates or oxides, it also occurs as metallic aluminum for example as colorant in sweets or in aluminum foil. With regard to potential toxicological effects, the different solubility of metallic aluminum nanoparticles compared to Al2O3 is of high relevance. Formation of ions may facilitate the crossing of blood-tissue barriers. Distribution towards other organs and subsequent re-formation of particulate aluminum due to milieu changes might occur. Therefore, the determination of solubility is required for proper risk assessment. Inductively coupled plasma mass spectrometry (ICP-MS) allows determination of aluminum with a detection limit of about 6 ppb. It could be proven that dissolution and solubility of metallic aluminum is significantly different when compared to Al2O3. Using ICP-MS in the single particle mode, a significant change in the behavior of both aluminum species was detected after undergoing the artificial digestion. Nearly unchanged in the saliva, particles show dissolution and high agglomeration during the gastric state before deagglomerating again in the intestine. Further analysis by time-of-flight secondary ion mass spectrometry (ToF-SIMS) revealed the uptake of both aluminum forms by proliferating and differentiated Caco-2 cells. For both particle forms different ions could be detected. Several aluminum-amino acid complex-derived ions from serine and valine were identified. In the case of Al2O3, Al2O2+, AlOH+, AlH2O+ and Al[(H2O)6]3+ were the main ions found co-localizing within treated cells. T2 - European Winter Conference for Plasma Spectrochemistry 2017 CY - Sankt Anton, Austria DA - 19.02.2017 KW - Aluminum KW - SP-ICP-MS KW - SAXS KW - Artificial digestion KW - Cellular uptake PY - 2017 AN - OPUS4-39201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - CT for additive manufacturing process characterisation: assessment of melt strategies on defect population N2 - Selective Electron Beam Melting (SEBM) is a promising powder bed Additive Manufacturing (AM) technique for near net-shape manufacturing of high-value titanium components. However, as with every emerging technique, the manufacturing processes can still be greatly improved and optimised. In particular, the links between AM settings and the resulting sample porosity is of great interest, as the fatigue life of SEBM parts is currently dominated by the presence of porosity. In this study, the size, volume fraction, and spatial distribution of the pores in model samples have been characterised in 3D, using X-ray Computed Tomography (CT), and correlated to the SEBM process variables. A strong relationship was found with the different beam strategies used to contour, and infill by hatching, a part section. The majority of pores were found to be small spherical gas pores, concentrated in the infill hatched region. Rarer irregular shaped pores were mostly located in the contour region and have been attributed to a lack of fusion between powder particles. T2 - Conference on Industrial Computed Tomography iCT2016 CY - Wels, Austria DA - 09.02.2016 KW - Titanium KW - Additive Manufacture KW - Selective Electron Beam Melting KW - Pores KW - Defects KW - X-ray Computed Tomography PY - 2016 AN - OPUS4-39186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bennetts, V.H. A1 - Kucner, T.P. A1 - Schaffernicht, E. A1 - Neumann, Patrick P. A1 - Fan, H. A1 - Lilienthal, A.J. T1 - Probabilistic air flow modelling using turbulent and laminar characteristics for ground and aerial robots N2 - For mobile robots that operate in complex, uncontrolled environments, estimating air flow models can be of great importance. Aerial robots use air flow models to plan optimal navigation paths and to avoid turbulence-ridden areas. Search and rescue platforms use air flow models to infer the location of gas leaks. Environmental monitoring robots enrich pollution distribution maps by integrating the information conveyed by an air flow model. In this paper, we present an air flow modelling algorithm that uses wind data collected at a sparse number of locations to estimate joint probability distributions over wind speed and direction at given query locations. The algorithm uses a novel extrapolation approach that models the air flow as a linear combination of laminar and turbulent components. We evaluated the prediction capabilities of our algorithm with data collected with an aerial robot during several exploration runs. The results show that our algorithm has a high degree of stability with respect to parameter selection while outperforming conventional extrapolation approaches. In addition, we applied our proposed approach in an industrial application, where the characterization of a ventilation system is supported by a ground mobile robot. We compared multiple air flow maps recorded over several months by estimating stability maps using the Kullback-Leibler divergence between the distributions. The results show that, despite local differences, similar air flow patterns prevail over time. Moreover, we corroborated the validity of our results with knowledge from human experts. T2 - IEEE International Conference on Robotics and Automation (ICRA) CY - Singapore DA - 29.05.2017 KW - Mapping KW - Field robots KW - Environment monitoring and management KW - Aerial systems KW - Perception and autonomy PY - 2017 DO - https://doi.org/10.1109/LRA.2017.2661803 SN - 2377-3766 VL - 2 IS - 2 SP - 1117 EP - 1123 PB - IEEE AN - OPUS4-39218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rabin, Ira ED - Elgvin, Torleif ED - Langlois, Michael ED - Davies, Kipp T1 - Ink Sample from Inkwell MS 1655/2 N2 - We have obtained a minute amount of dry ink scratched from the bronze inkwell MS 1655/2. The powder was stored between two glass slides to minimize contamination. For micro analysis by FTIR a sample of the ink powder was transferred into a diamond cell while for confocal Raman spectroscopy a micro sample was placed onto sticky tape. The same portion of the sample was also investigated by scanning electron microscopy, where the elements distribution was determined by EDX. KW - Archaeometry KW - Cultural heritage KW - Dead Sea scrolls PY - 2016 SN - 978-0-5671-1300-9 SN - 978-0-5672-8571-3 VL - 71 SP - 463 EP - 466 PB - Bloomsbury T&T Clark Series CY - New York, NY, USA AN - OPUS4-39225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Weller, Michael G. T1 - Referee Report 06 March 2017 N2 - This article is a valuable and welcome contribution to the ongoing discussion of antibody quality. The suggestion of a two-tier approach is helpful to distinguish between simple descriptive data and the validation of an antibody for a specified application. KW - Antibody KW - Validation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-393333 UR - https://f1000research.com/articles/6-161/v1#referee-response-20349 DO - https://doi.org/10.5256/f1000research.11700.r20349 SN - 2046-1402 SP - 6 EP - 7 PB - F1000 Research Ltd. CY - London AN - OPUS4-39333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Heídari, M. A1 - von Klitzing, R. A1 - Schönhals, Andreas T1 - Unveiling the dynamics of self-assembled layers of thin films of poly(vinyl methyl ether) (PVME) by nanosized relaxation spectroscopy N2 - A combination of nanosized dielectric relaxation (BDS) and thermal spectroscopy (SHS) was utilized to characterize the dynamics of thin films of Poly(vinyl methyl ether) (PVME) (thicknesses: 7 nm – 160 nm). For the BDS measurements, a recently designed nano-structured electrode system is employed. A thin film is spin-coated on an ultra-flat highly conductive silicon wafer serving as the bottom electrode. As top electrode, a highly conductive wafer with non-conducting nanostructured SiO2 nano-spacers with heights of 35 nm or 70 nm is assembled on the bottom electrode. This procedure results in thin supported films with a free polymer/air interface. The BDS measurements show two relaxation processes, which are analyzed unambiguously for thicknesses smaller than 50 nm. The relaxation rates of both processes have different temperature dependencies. One process coincidences in its position and temperature dependence with the glassy dynamics of bulk PVME and is ascribed to the dynamic glass transition of a bulk-like layer in the middle of the film. The relaxation rates were found to be thickness independent as confirmed by SHS. Unexpectedly, the relaxation rates of the second process obey an Arrhenius-like temperature dependence. This process was not observed by SHS and was related to the constrained fluctuations in a layer, which is irreversibly adsorbed at the substrate with a heterogeneous structure. Its molecular fluctuations undergo a confinement effect resulting in the localization of the segmental dynamics. To our knowledge, this is the first report on the molecular dynamics of an adsorbed layer in thin films. KW - Broadband dielectric spectroscopy KW - AC-nanochip calorimetry KW - Nanostructured capacitors KW - Thin films PY - 2017 UR - http://pubs.acs.org/doi/pdf/10.1021/acsami.6b14404 DO - https://doi.org/10.1021/acsami.6b14404 SN - 1944-8244 VL - 9 IS - 8 SP - 7535 EP - 7546 PB - ACS Publications CY - Washington DC AN - OPUS4-39291 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane T1 - 3D Rekonstruktionsverfahren für die aktive Thermografie N2 - Aktive Thermografie wird zunehmend für die zerstörungsfreie Prüfung insbesondere von dünnwandigen Bauteilen eingesetzt. Neben der Ortung und der Bestimmung der lateralen Ausdehnung von Fehlstellen und Inhomogenität in der Ebene parallel zur Oberfläche sind in den Messdaten auch Informationen über die Tiefe bzw. Überdeckung von Fehlstellen enthalten. In der Vergangenheit wurden verschiedene analytische Ansätze zur Rekonstruktion dieser Tiefeninformationen umgesetzt: - Bestimmung der Blindfrequenz über die Phaseninformationen der Puls-Phasen-Thermografie - Bestimmung des Phasenkontrastes bei der Lockin Thermografie - Bestimmung der Fehlstellentiefe mittels Thermal Signal Reconstruction (TSR), d. h. aus dem doppeltlogarithmisch dargestellten zeitlichen Verlauf der Abkühlung nach impulsartiger Erwärmung Nachteil aller bisherigen analytischer Verfahren basierend auf eindimensionalen Modellen ist, dass der Einfluss lateraler Wärmeleitungseffekte nicht berücksichtigt wird. Dieser kann jedoch bei kleineren Fehlstellen nicht mehr vernachlässigt werden, wozu bisher jedoch nur teilempirische Ansätze realisiert wurden. Erst numerische Rekonstruktionsverfahren ermöglichen eine Rekonstruktion auch komplexerer Defektgeometrien unter Berücksichtigung lateraler Wärmeleitungsprozesse sowie anisotroper thermischer Materialeigenschaften. In diesem B eitrag werden die verschiedenen Ansätze in der 3D-Datenanalyse der aktiven Thermografie miteinander verglichen und die Möglichkeiten und Grenzen der Verfahren vorgestellt. T2 - Heidelberger Bildverarbeitungsfortum 2017 CY - Fürth, Germany DA - 07.03.2017 KW - Aktive Thermografie KW - 3D Rekonstruktion KW - Faserverbundwerkstoffe KW - Analytische Modelle KW - Numerische Modelle PY - 2017 AN - OPUS4-39301 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane T1 - Validated inspection techniques for composites in energy applications - The EMRP-project VITCEA N2 - Presentation of results of the EMRP-Project VITCEA T2 - 29. Sitzung des DIN NMP NA 062-08-20 AA „Zerstörungsfreie Prüfung, Obleuteausschuss“ CY - Berlin, Germany DA - 21.02.2017 KW - Fibre reinforced composites KW - Active thermography KW - Ultrasonics PY - 2017 AN - OPUS4-39303 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bäßler, Ralph T1 - Aktivitäten des ISO/TC 265 "Carbon dioxide capture, transportation and geological storage" N2 - Im ISO/TC 265 werden Normen zur Entwicklung, Konstruktion, Betrieb, Umweltplanung und -Management, Risikomanagement, Quantifizierung, Monitoring und Verifizierung sowie weitere Aktivitäten für die einzelnen Stufen der CCS-Prozesskette erstellt. Als neuer Aspekt wurde die Zusammensetzung des CO2-Stroms angesprochen. In Form eines "State-of-the-Art-Reports" soll der derzeitige Kenntnisstand zusammengestellt werden. Dieses soll für einen späteren Normenentwurf als Grundlage dienen. T2 - Projekttreffen, CLUSTER-Verbundvorhaben CY - Halle, Germany DA - 2.3.2017 KW - CCS KW - CO2 KW - Normung PY - 2017 AN - OPUS4-39306 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kage, Daniel T1 - Luminophores for time-resolved flow cytometry N2 - For the application of time-resolved detection in the framework of flow cytometry, suitable luminescence lifetime code carriers are required. Here we report on our achievements concerning strategies to increase the accessible range of lifetime values and to realize continuously tunable lifetimes. To that end, we investigated polymer (PMMA) microbeads stained with mixtures of dyes exhibiting different fluorescence decay kinetics. At the expense of spectrally varying decay kinetics, it is possible to modify the lifetime by changing the dye concentration ratio. Moreover, semiconductor quantum dots incorporated into polymer beads were studied as alternative luminophores outperforming organic dyes with respect to long luminescence lifetimes, flexible choice of excitation wavelength and narrow spectral emission width. Our experiments demonstrate that lifetime adaption with dye mixing is basically feasible and semiconductor quantum dots represent promising candidates for long-lifetime codes. T2 - FLiMFlow meeting CY - Münster, Germany DA - 03.03.2017 KW - Flow cytometry KW - Fluorescence KW - Life sciences KW - Lifetime encoding KW - Polymer particles PY - 2017 AN - OPUS4-39307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bierstedt, Andreas T1 - Improving the performance of the laser-spark ion source for the detection of volatile organic compounds under ambient conditions N2 - Recently, a novel ionization scheme for ambient MS has been introduced. It is based on a quasi-continuous laser induced plasma (LIP), ignited in front of the MS inlet. This setup comprises the advantages of an ambient probe, electro neutrality, a sufficient duty cycle, a ubiquitous plasma medium, low power consumption, the absence of solvents and high sensitivity. To assess its future applicability for the detection of volatile organic compounds, plasma properties and operating conditions are investigated to understand the processes, that lead to the unexpected formation of intact molecular ions. Comprehensive studies include optical Emission spectroscopy, shadowgraphic shockwave visualization and time-of-flight mass spectrometry. T2 - 50. Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie CY - Kiel, Germany DA - 05.03.2017 KW - Laser-spark KW - Laser induced plasma KW - Mass spectrometry KW - Ambient ionization PY - 2017 AN - OPUS4-39309 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Z. A1 - Gao, S. A1 - Brand, U. A1 - Hiller, K. A1 - Wollschläger, Nicole A1 - Pohlenz, F. T1 - Note: Nanomechanical characterization of soft materials using a micro-machined nanoforce transducer with an FIB-made pyramidal tip N2 - The quantitative nanomechanical characterization of soft materials using the nanoindentation technique requires further improvements in the performances of instruments, including their force Resolution in particular. A micro-machined silicon nanoforce transducer based upon electrostatic comb drives featuring the force and depth resolutions down to 1 nN and 0.2 nm, respectively, is described. At the end of theMEMStransducer’s main shaft, a pyramidal tip is fabricated using a focused ion beam facility. A proof-of-principle setup with this MEMS nanoindenter has been established to measure the mechanical properties of soft polydimethylsiloxane. First measurement results demonstrate that the prototype measurement system is able to quantitatively characterize soft materials with elastic moduli down to a few MPa. KW - MEMS KW - Indentation KW - Soft material PY - 2017 DO - https://doi.org/10.1063/1.4977474 SN - 0034-6748 SN - 1089-7623 VL - 88 IS - 3 SP - 036104-1 EP - 036104-3 PB - AIP Publishing AN - OPUS4-39313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Beck, Uwe A1 - Lohse, V. A1 - Negendank, D. A1 - Kormunda, M. A1 - Esser, N. T1 - Thin SnOx films for surface plasmon resonance enhanced ellipsometric gas sensing (SPREE) N2 - Background: Gas sensors are very important in several fields like gas monitoring, safety and environmental applications. In this approach, a new gas sensing concept is investigated which combines the powerful adsorption probability of metal oxide conductive sensors (MOS) with an optical ellipsometric readout. This concept Shows promising results to solve the problems of cross sensitivity of the MOS concept. Results: Undoped tin oxide (SnOx) and iron doped tin oxide (Fe:SnOx) thin add-on films were prepared by magnetron sputtering on the top of the actual surface plasmon resonance (SPR) sensing gold layer. The films were tested for their sensitivity to several gas species in the surface plasmon resonance enhanced (SPREE) gas measurement. It was found that the undoped tin oxide (SnOx) shows higher sensitivities to propane (C3H8) then to carbon monoxide (CO). By using Fe:SnOx, this relation is inverted. This behavior was explained by a change of the amount of binding sites for CO in the layer due to this iron doping. For hydrogen (H2) no such relation was found but the sensing ability was identical for both layer materials. This observation was related to a different sensing mechanism for H2 which is driven by the Diffusion into the layer instead of adsorption on the surface. Conclusion: The gas sensing selectivity can be enhanced by tuning the properties of the thin film overcoating. A relation of the binding sites in the doped and undoped SnOx films and the gas sensing abilities for CO and C3H8 was found. This could open the path for optimized gas sensing devices with different coated SPREE sensors. KW - Doped tin oxide KW - Ellipsometry KW - Gas sensing KW - Surface plasmon KW - Resonance KW - Thin films KW - Transparent conductive oxides PY - 2017 DO - https://doi.org/10.3762/bjnano.8.56 SN - 2190-4286 VL - 8 SP - 522 EP - 529 AN - OPUS4-39391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuroiwa, T. A1 - Zhu, Y. A1 - Inagaki, K. A1 - Long, S. A1 - Christopher, S. A1 - Puelles, M. A1 - Porinsky, M. A1 - Hatamleh, N. A1 - Murby, J. A1 - Merrick, J. A1 - White, I. A1 - Saxby, D. A1 - Caciano de Sena, R. A1 - Dominguez de Almeida, M. A1 - Vogl, Jochen A1 - Phukphatthanachai, Pranee A1 - Fung, W.-H. A1 - Yau, H.-P. A1 - Okumu, T. O. A1 - Kang'iri, J. N. A1 - Tellez, J. A. S. A1 - Campos, E. Z. A1 - Galvan, E. C. A1 - Kaewkhomdee, N. A1 - Taebunpakul, S. A1 - Thiengmanee, U. A1 - Yafa, C. A1 - Tokman, N. A1 - Tunc, M. A1 - Can, S. Z. T1 - Report of the CCQM-K123: trace elements in biodiesel fuel N2 - The CCQM-K123 key comparison was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of sodium, calcium, potassium, magnesium phosphorous and sulfur in biodiesel fuel (BDF). The National Metrology Institute of Japan (NMIJ) and National Institute of Standards and Technology (NIST) acted as the coordinating laboratories. Results were submitted by 11 NMIs and DIs. The participants used different measurement methods, though most of them used inductively coupled plasma-mass spectrometry (ICP-MS), isotope dilution technique with ICP-MS and inductively coupled plasma-optical emission spectrometry (ICP-OES) with microwave acid digestion. The material was quite challenging and a number of questions were raised at the IAWG meeting. Concerning S, the variation in S results between participants, particularly those using IDMS methods was discussed at the IAWG meeting. BAM, NIST and NMIJ reviewed their experimental conditions, results and/or uncertainty calculations for IDMS. According to the additional evaluation and investigation, the variances between the revised results became smaller than the original one, the revised results were overlapping between IDMS measurements of S content at the k=2 level. It is not possible to calculate a KCRV with values being modified after submission. It was concluded that this KC does not support S measurements. Accounting for relative expanded uncertainty, comparability of measurement results for each of Na, Ca, K, Mg and P was successfully demonstrated by the participating NMIs or DIs. It is expected that sodium, calcium, potassium, magnesium and phosphorus at mass fractions greater than approximately 0.1 mg/kg, 0.1 mg/kg, 0.05 mg/kg, 0.05 mg/kg and 0.1 mg/kg respectively in biodiesel fuel and similar matrices (fuels and oils etc.) can be determined by each participant using the same technique(s) employed for this key comparison to achieve similar uncertainties mentioned in the present report. Furthermore, the results of this key comparison can be utilized along with the IAWG core capability approach. KW - Biodiesel KW - Fuel KW - Sulphur KW - Reference measurement PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-393941 UR - http://iopscience.iop.org/article/10.1088/0026-1394/54/1A/08008/meta DO - https://doi.org/10.1088/0026-1394/54/1A/08008 SN - 0026-1394 SN - 1681-7575 VL - 54 SP - Tech. Suppl. 2017, 08008, 1 EP - 47 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-39394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online spectroscopy in micellar systems – A process analytical approach for a hydroformylation mini-plant N2 - Within the Collaborative Research Center InPROMPT a novel process concept for the hydroformylation of long-chained olefins is studied in a mini-plant, using a rhodium complex as catalyst in the presence of syngas. Recently, the hydroformylation in micro¬emulsions, which allows for the efficient recycling of the expensive rhodium catalyst, was found to be feasible. However, the high sensitivity of this multi-phase system with regard to changes in temperature and composition demands a continuous observation of the reaction to achieve a reliable and economic plant operation. For that purpose, we tested the potential of both online NMR and Raman spectroscopy for process control. The lab-scale experiments were supported by off-line GC-analysis as a reference method. A fiber optic coupled probe of a process Raman spectrometer was directly integrated into the reactor. 25 mixtures with varying concentrations of olefin (1-dodecene), product (n-tridecanal), water, n-dodecane, and technical surfactant (Marlipal 24/70) were prepared according to a D-optimal design. Online NMR spectroscopy was implemented by using a flow probe equipped with 1/16” PFA tubing serving as a flow cell. This was hyphenated to the reactor within a thermostated bypass to maintain process conditions in the transfer lines. Partial least squares regression (PLSR) models were established based on the initial spectra after activation of the reaction with syngas for the prediction of unknown concentrations of 1-dodecene and n-tridecanal over the course of the reaction in the lab-scale system. The obtained Raman spectra do not only contain information on the chemical composition but are further affected by the emulsion properties of the mixtures, which depend on the phase state and the type of micelles. Based on the spectral signature of both Raman and NMR spectra, it could be deduced that especially in reaction mixtures with high 1-dodecene content the formation of isomers as a competitive reaction was dominating. Similar trends were also observed during some of the process runs in the mini-plant. The multivariate calibration allowed for the estimation of reactants and products of the hydroformylation reaction in both laboratory setup and mini-plant. T2 - 11. Doktorandenseminar 2017 des Arbeitskreis Prozessanalytik der GDCh und DECHEMA CY - Berlin, Germany DA - 12.03.2017 KW - Online reaction monitoring PY - 2017 AN - OPUS4-39398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Automated data preparation and spectral modeling N2 - For reaction monitoring and process control using NMR instruments, in particular, after acquisition of the FID the data needs to be corrected in real-time for common effects using fast interfaces and automated methods. Conventionally, sensors have to be calibrated in a first step to find a response curve between the sensor signal and physical or chemical properties of the sample. In a second step, a model of the response between these parameters (e.g., concentrations) and the targeted quality specifications is needed. Thanks to the direct proportionality of the molar concentrations and the NMR signal, it could directly be used in the near future to relate the process target quality specification to sensor data – also in combination with multiple other sensor or process information. T2 - qNMR Summit 2017 CY - Berlin, Germany DA - 16.03.2017 KW - Quantitative NMR spectroscopy KW - Automated data evaluation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-393998 AN - OPUS4-39399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lazik, D. A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias T1 - Characteristic length measurement of a subsurface gas anomaly - an integrating monitoring approach over heterogeneous distributed gas flow paths N2 - Geogenic gases such as CH4 or CO2 from natural sources, gases (CCS-CO2, H2, Natural gas, City gas …) from a geological repository, or a leaking gas pipeline can present serious risks in industrial and urban areas where the density of infrastructural elements increases as well as above and below ground. To extend the lead time for risk treatment in such critical regions, reliable detection of gases within the shallow subsurface is required to observe critical gas accumulations before degassing into the atmosphere. A near real-time monitoring approach is introduced to determine the volumetric expansion of such a gas escaping from a leak in the subsurface. Considering the pressure relaxation with the ambient air pressure, the approach enables the forecasting of the final size of a pressurized gas body in terms of characteristic lengths. According to theoretical basics, such a characteristic length, which allows to perform a gas (safety) measurement based on a purely geometrical measure, behaves independently of subsurface properties, i.e., it enables a reliable quantification of the escaping gas, irrespective of its heterogeneous flow path distribution. A field test for a 10 l/min pinhole leakage of CO2 injected in an unsaturated Chernozemic soil (agricultural test field Bad Lauchstädt)that was equipped with linear gas sensors demonstrates the lateral-vertical volumetric gas expansion along the environment of these gas sensors, and confirms the applicability of the new characteristic length approach. T2 - UFZ EnergyDays 2017 CY - Leipzig, Germany DA - 15.03.2017 KW - CO2 KW - Carbon capture and storage KW - Leakage KW - Monitoring PY - 2017 AN - OPUS4-39400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Barnefske, Lena T1 - PDMS-POS capsules for prospective self-healing materials N2 - In this presentation the synthesis and characterisation of PDMS-POS capsules is described and discussed. T2 - 5th International Conference on Multifuctional and Hybrid Nanomaterials CY - Lisbon, Portugal DA - 06.03.2017 KW - Capsules KW - Self-healing KW - PDMS PY - 2017 AN - OPUS4-39404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Klas A1 - Ruiken, J.-P. A1 - Illner, M. A1 - Paul, Andrea A1 - Müller, D. A1 - Esche, E. A1 - Wozny, G. A1 - Maiwald, Michael T1 - Process spectroscopy in microemulsions - setup and multi-spectral approach for reaction monitoring of a homogeneous hydroformylation process N2 - Reaction monitoring in disperse systems, such as emulsions, is of significant technical importance in various disciplines like biotechnological engineering, chemical industry, food science, and a growing number other technical fields. These systems pose several challenges when it comes to process analytics, such as heterogeneity of mixtures, changes in optical behavior, and low optical activity. Concerning this, online nuclear magnetic resonance (NMR) spectroscopy is a powerful technique for process monitoring in complex reaction mixtures due to its unique direct comparison abilities, while at the same time being non-invasive and independent of optical properties of the sample. In this study the applicability of online-spectroscopic methods on the homogeneously catalyzed hydroformylation system of 1-dodecene to tridecanal is investigated, which is operated in a mini-plant scale at Technische Universität Berlin. The design of a laboratory setup for process-like calibration experiments is presented, including a 500 MHz online NMR spectrometer, a benchtop NMR device with 43 MHz proton frequency as well as two Raman probes and a flow cell assembly for an ultraviolet and visible light (UV/VIS) spectrometer. Results of high-resolution online NMR spectroscopy are shown and technical as well as process-specific problems observed during the measurements are discussed. KW - Online-spectroscopy KW - Quantitative NMR spectroscopy KW - Process analytical technology KW - Microemulsions PY - 2017 DO - https://doi.org/10.1088/1361-6501/aa54f3 SN - 0957-0233 SN - 1361-6501 VL - 28 IS - 3 SP - 035501-1 EP - 035501-11 PB - IOP Publishing Ltd. AN - OPUS4-39091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Meyer, Klas T1 - Hochdruck NMR-Spektroskopie N2 - Der Einsatz der quantitativen Kernspinresonanzspektroskopie (NMR-Spektroskopie) in technischen Mischungen stellt einen vielversprechenden Ansatz für die Verfolgung und Kontrolle von Abläufen innerhalb chemischer Produktionsprozesse dar. Die Möglichkeit der direkten Relativquantifizierung ohne Notwendigkeit der Zugabe von Standards oder einer vorherigen Kalibrierung, vergleichbar mit einem simplen „Zählen“ von Kernspins im Messvolumen, macht die Methode darüber hinaus besonders interessant für metrologische Fragestellungen. Im ersten Teil dieser Dissertation wird die Entwicklung von Hochdruckmethoden für Anwendungen in der Gasmetrologie thematisiert. Als ergänzende Analysenmethode liefert die NMR-Spektroskopie hier wichtige Erkenntnisse zur Unterstützung der Herstellung hochgenauer Gas- und Flüssiggasgemische. Der zweite Teil beinhaltet Anwendungsbeispiele für die Prozessanalytik an technischen Systeme auf Basis von Online-NMR- und -Raman-Spektroskopie anhand der industriell relevanten Verfahren der CO2 Absorption in wässrigen Alkanolaminlösungen, sowie der Hydroformylierung langkettiger Alkene in einer Mikroemulsion. KW - Hochdruck NMR-Spektroskopie KW - Quantitative NMR-Spektroskopie KW - Gasphasen NMR-Spektroskopie KW - Prozessanalytik PY - 2017 SN - 9783736994621 SP - 1 EP - 180 PB - Cuvillier CY - Göttingen AN - OPUS4-39092 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Almeida, Ângela A1 - Calisto, Vânia A1 - Domingues, M. Rosário M. A1 - Esteves, Valdemar I. A1 - Schneider, Rudolf A1 - Soares, Amadeu M.V.M. A1 - Figueira, Etelvina A1 - Freitas, Rosa T1 - Comparison of the toxicological impacts of carbamazepine and a mixture of its photodegradation products in Scrobicularia plana N2 - In the aquatic environment, pharmaceutical drugs are submitted to degradation processes, where pho-todegradation is one of the most important mechanisms affecting the fate, persistence and toxicity of thecompounds. Carbamazepine, a widely used antiepileptic, is known to suffer photodegradation in waterbodies and generate photoproducts, some of them with higher potential toxicity than the parent com-pound. Therefore, to evaluate the toxic effects of CBZ when combined with its photoproducts, an acuteexposure (96 h) with the edible clam Scrobicularia plana was performed using environmental concentra-tions of CBZ (0.00–9.00 µg/L) irradiated (and non-irradiated) with simulated solar radiation. The analysisof the irradiated CBZ solutions by mass spectrometry revealed the formation of 5 photoproducts, includ-ing acridine (a compound known to be carcinogenic). Oxidative stress results showed that the exposureto CBZ photoproducts did not increase the toxicity to clams, by comparison with the parent compound. KW - Pharmaceutical drugs KW - Photodegradation KW - Biomarkers KW - Oxidative stress KW - Bivalves PY - 2017 DO - https://doi.org/10.1016/j.jhazmat.2016.05.009 VL - 323 SP - 220 EP - 232 PB - Elsevier B.V. AN - OPUS4-39151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oberleitner, Lidia A1 - Dahmen-Levison, U. A1 - Garbe, L.-A. A1 - Schneider, Rudolf T1 - Application of fluorescence polarization immunoassay for determination of carbamazepine in wastewater N2 - Carbamazepine is an antiepileptic drug that can be used as a marker for the cleaning efficiency of wastewater treatment plants. Here, we present the optimization of a fast and easy on-site measurement system based on fluorescence polarization immunoassay and the successful application to wastewater. A new monoclonal highly specific anti-carbamazepine antibody was applied. The automated assay procedure takes 16 min and does not require sample preparation besides filtration. The recovery rates for carbamazepine in wastewater samples were between 60.8 and 104% with good intra- and inter-assay coefficients of variations (less than 15 and 10%, respectively). This automated assay enables for the onsite measurement of carbamazepine in wastewater treatment plants. KW - On-site measurement KW - Wastewater treatment plant KW - Fluorescence polarization immunoassay KW - Assay optimization KW - Mix-and-read assay PY - 2017 DO - https://doi.org/10.1016/j.jenvman.2017.01.063 SN - 0301-4797 SN - 1095-8630 VL - 193 SP - 92 EP - 97 PB - Elsevier Ltd. AN - OPUS4-39152 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zydziak, N. A1 - Konrad, W. A1 - Feist, F. A1 - Afonin, S. A1 - Weidner, Steffen A1 - Barner-Kowollik, C. T1 - Coding and decoding libraries of sequence-defined functional copolymers synthesized via photoligation N2 - Designing artificial macromolecules with absolute sequence order represents a considerable challenge. Here we report an advanced light-induced avenue to monodisperse sequencedefined functional linear macromolecules up to decamers via a unique photochemical approach. The versatility of the synthetic strategy—combining sequential and modular concepts—enables the synthesis of perfect macromolecules varying in chemical constitution and topology. Specific functions are placed at arbitrary positions along the chain via the successive addition of monomer units and blocks, leading to a library of functional homopolymers, alternating copolymers and block copolymers. The in-depth characterization of each sequence-defined chain confirms the precision nature of the macromolecules. Decoding of the functional information contained in the molecular structure is achieved via tandem mass spectrometry without recourse to their synthetic history, showing that the sequence information can be read.We submit that the presented photochemical strategy is a viable and advanced concept for coding individual monomer units along a macromolecular chain. KW - Photoligation KW - Copolymer sequence KW - MALDI-TOF MS/MS PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-391542 DO - https://doi.org/10.1038/ncomms13672 SN - 2041-1723 VL - 7 SP - Artikel Nr. 13672 AN - OPUS4-39154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Véliz Montes, Cinthya A1 - Memczak, H. A1 - Gyssels, E. A1 - Torres, T. A1 - Madder, A. A1 - Schneider, Rudolf T1 - Photoinduced cross-linking of short Furan-modified DNA on surfaces N2 - We report for the first time the formation of sitespecific interstrand cross-linked (ICL) surface-immobilized furanmodified DNA duplexes via singlet oxygen. 1O2, necessary for effecting furan-mediated ICL formation, was produced in situ using methylene blue or a zinc phthalocyanine derivative (TT1) as a photosensitizer. Via surface plasmon resonance spectroscopy, we show that surface ICL was achieved, and a robust link formed that enhances the stability of the 12-mer duplex even after surface regeneration. The described method represents a novel platform technology based on surfaces with addressable and stable DNA duplexes requiring only short oligonucleotides. KW - DNA interstrand cross-link (ICL) KW - Furanmodified DNA duplexes KW - Surface plasmon resonance spectroscopy PY - 2017 DO - https://doi.org/10.1021/acs.langmuir.6b03855 SN - 0743-7463 SN - 1520-5827 VL - 33 IS - 5 SP - 1197 EP - 1201 PB - ACS Publications AN - OPUS4-39155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Comparative visualization of the geometry of a hollow box girder using 3D-Lidar Part 2: Reconstruction of 3D Geometric Modell N2 - With the mandatory introduction of the May 2011 directive for reassessment of bridges in Germany, the administrations of the federal and state governments have the duty to prove the stability of their bridge stock. Verification of bridge stability will be realized with consideration of the newly increased traffic loads. Particularly in older bridges, the verification can only be achieved if calculative surplus load capacity of the original structural design is taken into account in the recalculation. One option for considering these reserves is the exact determination of the dead weight of the bridge. Within this case study, it will be demonstrated how the problem can be practically solved. In order to determine the dead weight of a concrete bridge, its volume has to be calculated. as a first step, a 3D laser scanner is used to record the internal geometry of a hollow box bridge girder. For the determination of the thickness of the concrete member, the non-destructive technique ultrasonic echo is applied. The construction must be segmented in approximately equidistant parts in order to be able to carry out an economic and efficient investigation. The description of the segmentation of the point cloud, carried out in a 2D model, was presented in the first part of the publication. The subject of this presentation is the merging of 2D cross sections into a 3D model, from which the weight of the bridge can be calculated. T2 - IS&T International Symposium on Electronic Imaging 2017 CY - San Francisco, CA, USA DA - 29.01.2017 KW - Zerstörungsfreie Prüfung im Bauwesen KW - LiDAR KW - NDT PY - 2017 AN - OPUS4-39156 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Philipp, Rosemarie T1 - 16RPT02 ALCOREF - Certified forensic alcohol reference materials N2 - The presentation shows the outline of a new project on certified reference materials for the calibration of evidential breath alcohol analyzers in the 2016 EMPIR Research Potential call. T2 - EURAMET TC-MC Meeting CY - Warsaw, Poland DA - 31.01.2017 KW - Breath alcohol KW - Certified reference material KW - EMPIR PY - 2017 AN - OPUS4-39158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leng, Jing A1 - Kang, N. A1 - Wang, D.-Y. A1 - Wurm, Andreas A1 - Schick, C. A1 - Schönhals, Andreas T1 - Crystallization behavior of nanocomposites based on poly(L-lactide) and MgAl layered double hydroxides - Unbiased determination of the rigid amorphous phases due to the crystals and the nanofiller N2 - Semicrystalline polymers have to be described by a three phase model consisting of a mobile amorphous (MAF), a crystalline (CF), and a rigid amorphous fraction (RAF). For nanocomposites based on a semicrystalline polymer the RAF is due to both the crystallites (RAFcrystal) and the filler (RAFfiller). Polymer nanocomposite based on poly(L-lactide) and MgAl layered double hydroxide nanofiller were prepared. Due to the low crystallization rate of PLA ist crystallization can be suppressed by a high enough cooling rate, and the RAF is due only to the nanofiller. The MAF, CF, and RAF were estimated by Temperature Modulated DSC. For the first time CF, MAF, RAFcrystal, and RAFfiller could be estimated. It was found, that RAFfiller increases linearly with the concentration of the nanofiller for this system. Furthermore, RAFcrystal is only slightly influenced by the presence of the nanofiller. KW - Polymer based nanocomposites PY - 2017 DO - https://doi.org/10.1016/j.polymer.2016.11.065 SN - 0032-3861 SN - 1873-2291 VL - 108 SP - 257 EP - 264 PB - Elesevier AN - OPUS4-39052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Hodoroaba, Vasile-Dan A1 - Mielke, Johannes T1 - Techniques evaluation report for selection of characterisation methods N2 - This report is the result of a comprehensive study on the available CMs which come potentially in question for the reliable analysis of the number based size distribution of a nanomaterial according to the EC recommendation for a definition of nanomaterial. Based on the performance criteria already established in NanoDefine the potential CMs are evaluated according to studies available in the literature as well as following the expertise of the NanoDefine consortium partners. The specific advantages and disadvantages of each method with respect to its applicability to the scope of NanoDefine are particularly highlighted. An CM evaluation table is produced so that the mostly suited CMs with respect to the EC definition can be grouped and recommended to the corresponding NanoDefine work packages for further specific development (improvement and adaption), or for direct validation and standardisation, respectively. The actual evaluation report including the recommended CMs will be revised and, if necessary, eventually updated at the mid time of the project. The update will be jointly discussed in the NanoDefine consortium on the basis of the results of testing the methods on the NanoDefine real world materials. KW - Nanomaterial KW - Characterization method KW - EC definition PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-389473 UR - http://www.nanodefine.eu/publications/reports/NanoDefine_TechnicalReport_D3.1.pdf SP - D3.1, 1 EP - 57 CY - Wageningen, The Netherlands AN - OPUS4-38947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Man proposes, God disposes – The Way from Reaction Monitoring to Industrial Automation N2 - Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction and process control. An increasing number of applications are reported. Robust field integration of NMR systems have to face explosion protection or integration into process control systems with short set-up times. Tis paves the way for industrial automation in real process environments. Automated data preparation and analysis are cornerstones for a breakthrough of NMR techniques for process control. Particularly, robust chemometrics as well as automated signal processing methods have to be (further) developed especially for NMR spectroscopy in process control. This becomes even more important for so called “smart sensors” providing the basis for the future project “Industrie 4.0”, and Industrial Internet of Things (IIoT), along with current requirements to process control, model based control, or soft sensing. Data analysis techniques are available but currently mostly used for off-line data analysis to detect the causes of variations in the product quality. The talk presents current research activities towards process control with compact NMR and reflects “cultural differences” between the interdisciplinary parties involved. T2 - Symposium NMRPM - Quantitative NMR Methods for Reaction and Process Monitoring CY - Kaiserslautern, Germany DA - 19.01.2017 KW - Reaction Monitoring KW - Process Analytical Technology KW - Smart Sensors KW - Process Control KW - Industrie 4.0 KW - Online NMR Spectroscopy PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-389940 AN - OPUS4-38994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Näreoja, T A1 - Deguchi, T A1 - Christ, S. A1 - Peltomaa, R A1 - Prabhakar, N A1 - Fazeli, E A1 - Perälä, N A1 - Rosenholm, J A1 - Arppe, Riika A1 - Soukka, T A1 - Schäferling, Michael T1 - Ratiometric Sensing and Imaging of Intracellular pH Using Polyethylenimine-Coated Photon Upconversion Nanoprobes N2 - Measurement of changes of pH at various intracellular compartments has potential to solve questions concerning the processing of endocytosed material, regulation of the acidification process, and also acidification of vesicles destined for exocytosis. To monitor these events, the nanosized optical pH probes need to provide ratiometric signals in the optically transparent biological window, target to all relevant intracellular compartments, and to facilitate imaging at subcellular resolution without interference from the biological matrix. To meet these criteria we sensitize the surface conjugated pH sensitive indicator via an upconversion process utilizing an energy transfer from the nanoparticle to the indicator. Live cells were imaged with a scanning confocal microscope equipped with a low-energy 980 nm laser excitation, which facilitated high resolution and penetration depth into the specimen, and low phototoxicity needed for long-term imaging. Our upconversion nanoparticle resonance energy transfer based sensor with polyethylenimine-coating provides high colloidal stability, enhanced cellular uptake, and distribution across cellular compartments. This distribution was modulated with membrane integrity perturbing treatment that resulted into total loss of lysosomal compartments and a dramatic pH shift of endosomal compartments. These nanoprobes are well suited for detection of pH changes in in vitro models with high biological background fluorescence and in in vivo applications, e.g., for the bioimaging of small animal models. KW - PH sensing KW - Upconversion KW - Nanoparticles KW - Fluorescecne imaging PY - 2017 UR - http://pubs.acs.org/doi/abs/10.1021/acs.analchem.6b03223 DO - https://doi.org/10.1021/acs.analchem.6b03223 SN - 0003-2700 SN - 1520-6882 VL - 89 IS - 3 SP - 1501 EP - 1508 PB - American Chemical Society CY - Washington AN - OPUS4-39083 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Khani, M. A1 - Mehdipour, E. A1 - Faghani, A. A1 - Guday, G. A1 - Donskyi, Ievgen A1 - Haag, R. A1 - Adeli, M. T1 - Preparation of graphene oxide by cyanuric chloride as an effective and non-corrosive oxidizing agent N2 - In this work, we report a new method for the synthesis of graphene oxide (GO) using cyanuric chloride as a non-corrosive oxidizing agent. The mild conditions, simple purification, and scalability of this method are significant advantages over common approaches in which harsh oxidizing agents are used. Moreover, a major drawback with the Hummers' method, the production of toxic gases, is not an issue with this process. This method is a safe and large-scale alternative for the production of GO under mild conditions. KW - Graphene oxide KW - Synthesis KW - XPS KW - AFM KW - IR KW - TGA PY - 2016 DO - https://doi.org/10.1039/c6ra23702a SN - 2046-2069 VL - 6 IS - 116 SP - 115055 EP - 115057 PB - The Royal Society of Chemistry AN - OPUS4-39111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Near ambient pressure X-ray photoelectron spectroscopy on biofilms N2 - Overview of measurements and future work regarding near ambient pressure XPS on biofilms relevant for the EMPIR-project MetVBadBugs- Quantitative measurement and imaging of drug-uptake by bacteria with antimicrobial resistance. T2 - MetVBadBugs 9M Meeting CY - Turin, Italy DA - 02.02.2017 KW - XPS KW - Bacteria KW - Alginate KW - Biofilm PY - 2017 AN - OPUS4-39120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saywell, A. A1 - Bakker, A. A1 - Mielke, Johannes A1 - Kumagai, T. A1 - Wolf, M. A1 - García-López, V. A1 - Chiang, P.-T. A1 - Tour, J. M. A1 - Grill, L. T1 - Light-Induced Translation of Motorized Molecules on a Surface N2 - Molecular machines are a key component in the vision of molecular nanotechnology and have the potential to transport molecular species and cargo on surfaces. The motion of such machines should be triggered remotely, ultimately allowing a large number of molecules to be propelled by a single source, with light being an attractive stimulus. Here, we report upon the photoinduced translation of molecular machines across a surface by characterizing single molecules before and after illumination. Illumination of molecules containing a motor unit results in an enhancement in the diffusion of the molecules. The effect vanishes if an incompatible photon energy is used or if the motor unit is removed from the molecule, revealing that the enhanced motion is due to the presence of the wavelength-sensitive motor in each molecule. KW - Diffusion KW - Molecular devices KW - Molecular motor KW - Scanning probe microscopy KW - Photoexcitation KW - Photochemistry KW - Molecular machines PY - 2016 UR - http://pubs.acs.org/doi/abs/10.1021/acsnano.6b05650 DO - https://doi.org/10.1021/acsnano.6b05650 VL - 10 IS - 12 SP - 10945 EP - 10952 PB - ACS Publications AN - OPUS4-39095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Neuartige Wandler für die Luftultraschallprüfung N2 - Es werden Luftultraschallwandler für zerstörungsfreie Prüfung vorgestellt. Im Mittelpunkt des Vortrags stehen Ferroelektret-Wandler und thermoakustische Wandler. T2 - DGZfP Arbeitskreis Zwickau-Chemnitz CY - Zwickau, Germany DA - 24.01.2017 KW - Luftultraschall KW - Ultraschallprüfung KW - Ferroelektret KW - Thermoakustik KW - Wandler PY - 2017 AN - OPUS4-39055 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rietz, U. T1 - Validierung der Verbund-, Kleb- und Haftfestigkeit von optischen Schichten mittels Zentrifugentechnologie N2 - Der Vortrag widmet sich der Validierung der Verbundfestigkeit von optischen Schicht-/Substrat-systemen mittels Zentrifugentechnologie und diskutiert Versagensbilder und gemessene Werte der Verbundfestigkeit ausgewählter feinoptischer bzw. ophtalmischer Schichten in Abhängigkeit von den plasto-elastischen Eigenschaften und der Dicke der Substrate. T2 - 15. Praxisseminar KLEBEN, Günter-Köhler-Institut für Fügetechnik und Werkstoffprüfung GmbH CY - Jena, Germany DA - 25.01.2017 KW - Zentrifugentechnologie KW - Verbundfestigkeit KW - Haftfestigkeit KW - Feinoptische Schichten KW - Augenoptische Schichten PY - 2017 AN - OPUS4-39059 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Winkelmann, Aimo T1 - Crystallometric and projective properties of Kikuchi diffraction patterns N2 - Kikuchi diffraction patterns can provide fundamental information about the lattice metric of a crystalline phase. In order to improve the possible precision and accuracy of lattice parameter determination from the features observed in Kikuchi patterns, some useful fundamental relationships of geometric crystal-lography are reviewed, which hold true independently of the actual crystal symmetry. The Kikuchi band positions and intersections and the Kikuchi band widths are highly interrelated, which is illustrated by the fact that all lattice plane trace positions of the crystal are predetermined by the definition of only four traces. If, additionally, the projection centre of the gnomonic projection is known, the lattice parameter ratios and the angles between the basis vectors are fixed. A further definition of one specific Kikuchi band width is sufficient to set the absolute sizes of all lattice parameters and to predict the widths of all Kikuchi bands. The mathematical properties of the gnomonic projection turn out to be central to an improved interpretation of Kikuchi pattern data, emphasizing the importance of the exact knowledge of the projection centre. KW - EBSD KW - Crystallography KW - Kikuchi patterns KW - Projective geometry PY - 2017 DO - https://doi.org/10.1107/S1600576716017477 SN - 1600-5767 VL - 50 IS - Part 1 SP - 102 EP - 119 PB - International Union of Crystallography AN - OPUS4-39061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Kern, Simon T1 - Process monitoring of an intensified continuous production unit with compact NMR spectroscopy N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and inexpensive analysers, which feature advantages like low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. Otherwise there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Union’s Research Project CONSENS by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. The presented NMR module is provided in an explosion proof housing with a module size of 57 x 57 x 85 cm and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling (IHM) was selected for data analysis of the low-field NMR spectra. A set-up for monitoring continuous reactions in a thermostated 1/8” tubular reactor using automated syringe pumps was used to validate the IHM models by using high-field NMR spectroscopy as analytical reference method. T2 - Workshop for Process Industry - Tackling the Future of Plant Operation CY - Frankfurt am Main, Germany DA - 25.01.2017 KW - Online NMR spectroscopy KW - Process analytical technology KW - Prozessanalytik KW - Process control KW - CONSENS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-391386 AN - OPUS4-39138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wohlleben, W. A1 - Mielke, Johannes A1 - Bianchin, A. A1 - Ghanem, A. A1 - Freiberger, H. A1 - Rauscher, H. A1 - Gemeinert, Marion A1 - Hodoroaba, Vasile-Dan T1 - Reliable nanomaterial classification of powders using the volume-specific surface area method N2 - The volume-specific surface area (VSSA) of a particulate material is one of two apparently very different metrics recommended by the European Commission for a definition of "nanomaterial" for regulatory purposes: specifically, the VSSA metric may classify nanomaterials and non-nanomaterials differently than the median size in number metrics, depending on the chemical composition, size, polydispersity, shape, porosity, and aggregation of the particles in the powder. Here we evaluate the extent of agreement between classification by electron microscopy (EM) and classification by VSSA on a large set of diverse particulate substances that represent all the anticipated challenges except mixtures of different substances. EM and VSSA are determined in multiple labs to assess also the level of reproducibility. Based on the results obtained on highly characterized benchmark materials from the NanoDefine EU FP7 project, we derive a tiered screening strategy for the purpose of implementing the definition of nanomaterials. We finally apply the Screening strategy to further industrial materials, which were classified correctly and left only borderline cases for EM. On platelet-shaped nanomaterials, VSSA is essential to prevent false-negative classification by EM. On porous materials, approaches involving extended Adsorption isotherms prevent false positive classification by VSSA. We find no false negatives by VSSA, neither in Tier 1 nor in Tier 2, despite real-world industrial polydispersity and diverse composition, shape, and coatings. The VSSA screening strategy is recommended for inclusion in a technical guidance for the implementation of the definition. KW - Nanomaterial KW - Nanomaterial classification KW - Regulation KW - VSSA KW - Size measurement KW - Particle size PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-391450 DO - https://doi.org/10.1007/s11051-017-3741-x SN - 1388-0764 SN - 1572-896X VL - 19 IS - 2 SP - Article 61, 1 EP - 16 PB - Springer Nature AN - OPUS4-39145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Proposal of an inter-laboratory comparison on shape of bipyramidal TiO2 nanoparticles by TEM N2 - A proposal of an inter-laboratory study (ILC) on determination of size and shape distribution of TiO2 nanoparticles (NPs) by transmission electron microscopy is presented. The anatase NPs synthesized in a controllable fashion within the EU/FP7 project SETNanoMetro can be considered as shape-defined (bipyramidal) and are offered to complete the list of case studies already in progress within ISO/TC229/JWG2. The main points of the measurement procedure are presented as well as a proposed procedure to evaluate the size and shape according to the standard operation procedure already developed within SETNanoMetro is discussed. Potential ILC participants and a plan with next step to be carried out are proposed. T2 - Joint Meeting IEC TC 113 'Nanotechnology for electrotechnical products and systems' and ISO/TC229/JWG2 'Nanotechnologies'/'Measurement and characterization' CY - Lowell, MA, USA DA - 09.05.2016 KW - Nanoparticles KW - TiO2 KW - TEM KW - Shape KW - Inter-laboratory comparison KW - ISO PY - 2016 AN - OPUS4-38900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Streeck, C. T1 - A liquid cell for the analysis of biomolecules (e.g. proteins, chlorophyll) using soft X-ray excitation N2 - For versatile applications, including vacuum instrumentation, a liquid cell was developed. Using ultra-thin windows, this cell enables X-ray Absorption spectrometry in the soft X-ray range which is in particular interesting for the analysis of organic molecules in liquids or at the solid-liquid interface. NEXAFS of a protein at N K-edge and of chlorophyll a at Mg K-edge is demonstrated. T2 - 8th Jouint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 7.12.2016 KW - XAS KW - NEXAFS KW - Liquid cell KW - Chlorophyll PY - 2016 AN - OPUS4-38711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Behavior of Ultra-Thin POLYMER Films investigated by Nanosized Relaxation Spectroscopy N2 - The glass transition behavior of ultra-thin polymer films is discussed in detail. Further nanosized relxation spectroscopy is introduced in the form of AC chip calorimetry and dielectric spectroscopy employing nanostructured electrodes. These methods arre applied to ultra-thin films. T2 - Soft Matter Seminar Jülich CY - Jülich, Germany DA - 15.12.2016 KW - Ultra-thin polymer films PY - 2016 AN - OPUS4-38714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Following Pt in gold Byzantine tesserae: towards provenance and chronology with SR-XRF N2 - Gold mosaics, made from gold and glass, are one of the best expressions of Late Antique Byzantine and Early Islamic art. The gold alloys, whose composition seems to indicate that gold coins were re-used to fabricate the tesserae, can be used to provide information on the mosaics chronology. Monetary Byzantine gold is in fact characterized by the presence of Pt, which contents in the gold alloy change over time, but Pt must be measured in 0.2-0.4 µm thickness gold leaves that were beaten to be sandwiched between two glass layers. To analyze this samples the D²XRF set-up at the BAMline at the BESSY synchrotron in Berlin was used. The combination of a crystal for wavelength dispersion and an energy resolving single photon counting pnCCD allows the realization of this very simple wavelength dispersive detection system. With this system an MDL of 1 μg/g for the determination of Pt in Au under optimal conditions can be reached. Gold leaf tesserae from nine archaeological sites, covering the period that goes from the 5th c. to the 8th c., were analyzed. The presence of Pt in the majority of the samples confirmed the re-use of coins. The Pt contents separate the samples in three groups, one of which having the same chemical characteristics as the Byzantine gold could be compared to dated coins for chronology. The higher Pt contents for one of other groups suggest T2 - Synchrotron Radiation and Neutrons in Art & Archaeology (SR2A) CY - Chicago, USA DA - 06.09.2016 KW - Synchrotron KW - BAMline KW - XRF KW - Archaeometry KW - D2XRF PY - 2016 AN - OPUS4-38808 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Es ist nicht alles Gold was glänzt - Die Analyse von Gold mit Synchrotronstrahlung N2 - Gold ist eines der sieben schon im Altertum bekannten Metalle und wurde wg. seines Glanzes und seiner Seltenheit von alters her als Tauschmittel und zur Herstellung von Schmuck benutzt. Außerdem ist es einfach bearbeitbar und weitestgehend gegen chemische Einflüsse resistent. Die Untersuchungen von Gold mit synchrotronstrahlungsangeregter Röntgenfluoreszenzanalyse sind zerstörungsfrei und geben Auskunft über die in der untersuchten Probe vorhandenen chemischen Elemente. Bei den hier vorgestellten Untersuchungen an der BAMline stehen Fragestellungen wie Herkunft, Herstellungsverfahren und Zusammengehörigkeit von Goldfunden im Vordergrund. Die verschiedenen Fragestellungen werden an einer Reihe von Beispielen erläutert die vom Wikingerschatz aus Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten langen. Zusätzlich werden die modernen Messmethoden vorgestellt, die am Synchrotron heutzutage zur Verfügung stehen. T2 - Vortragsreihe „Naturwissenschaftliche Einsichten in Kunst- und Kulturgut" CY - Dresden, Germany DA - 13.10.2016 KW - Synchrotron KW - BAMline KW - Gold KW - XRF PY - 2016 AN - OPUS4-38809 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - Von Ägypten bis Hiddensee – Analyse von Gold mit Synchrotronstrahlung N2 - Gold ist eines der sieben schon im Altertum bekannten Metalle und wurde wg. seines Glanzes und seiner Seltenheit von alters her als Tauschmittel und zur Herstellung von Schmuck benutzt. Außerdem ist es einfach bearbeitbar und weitestgehend gegen chemische Einflüsse resistent. Die Untersuchungen von Gold mit synchrotronstrahlungsangeregter Röntgenfluoreszenzanalyse sind zerstörungsfrei und geben Auskunft über die in der untersuchten Probe vorhandenen chemischen Elemente. Bei den hier vorgestellten Untersuchungen an der BAMline stehen Fragestellungen wie Herkunft, Herstellungsverfahren und Zusammengehörigkeit von Goldfunden im Vordergrund. Die verschiedenen Fragestellungen werden an einer Reihe von Beispielen erläutert die vom Wikingerschatz aus Hiddensee über die Himmelsscheibe von Nebra bis hin zu Funden aus Ägypten langen. Zusätzlich werden die modernen Messmethoden vorgestellt, die am Synchrotron heutzutage zur Verfügung stehen. T2 - Vorlesung FU Berlin Einführung in die Archäometrie CY - Berlin, Germany DA - 04.11.2016 KW - Synchrotron KW - BAMline KW - Gold KW - XRF PY - 2016 AN - OPUS4-38810 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radtke, Martin T1 - The Colour X-ray Camera – Basics and Applications of a 2D X-ray Detector N2 - The Color X-ray Camera CXC or SLcam® is an energy-resolving X-ray camera capable of energy- and space-resolved measurements. It consists of a high-speed CCD detector coupled to a polycapil-lary optic that conducts the X-ray photons from the probe to distinct pixels onto the detector. The camera is capable of fast acquisition of spatially and energy resolved fluorescence images. A dedicated software enables the acquisition and the online processing of the spectral data for all 69696 pixels, leading to a real-time visualization of the elements distribution in a sample. It was developed in a joint project with BAM, IFG Berlin and PN Sensors. In this contribution we will mainly discuss the use of the CXC at our beamline, the BAMline at BESSY II and imaging applications of the CXC from different areas, like biology and archaeometry. Additionally new developments for the use of the detector without optics, like wavelength dispersive detection or 1shot-XANES, will be presented. T2 - Seminar Strahlenphysikalische Anwendungen in Technik und Medizin CY - Wien, Austria DA - 20.01.2016 KW - Synchrotron KW - BAMline KW - XRF PY - 2016 AN - OPUS4-38811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ostermann, Markus A1 - Herzel, Hannes A1 - Adam, Christian A1 - Kühn, A. A1 - Wedell, R. A1 - Mory, D. T1 - Integrierte Systeme (RFA und LIBS) zur Düngemittelgewinnung und zum Management der Bodenfruchtbarkeit N2 - Aufgrund der natürlichen und vom Menschen verursachten Heterogenität von Böden erfordert der Erhalt und die Verbesserung ihrer Fruchtbarkeit durch landwirtschaftliche Bewirtschaftungsmaßnahmen sorgfältig geplante Ent-scheidungen, die auf einer detaillierten Erfassung der Bodeneigenschaften und einem vertieften Verständnis der Bodenprozesse beruhen. Es ist bekannt, dass die konventionelle, flächen-einheitliche Bewirtschaftung Ertragsver-luste durch zu geringe Bewirtschaftungsintensität (z. B. Düngung) auf einen Teil der Fläche verursacht, während andere Teile des Feldes zu hohe Dosen erhalten und es dadurch zu Verschwendung von Ressourcen und zu Um-weltbelastungen kommt. Trotz der Verfügbarkeit von Technologien für ortsspezifische Düngung ist die Akzeptanz ortsspezifischer Bewirtschaftung (Precision Agriculture) in der Praxis noch gering. Ein wesentlicher Grund dafür ist das Fehlen von kostengünstigen Methoden zur Erfassung der bewirtschaftungsrelevanten Bodenmerkmale. So-wohl für die elementanalytische Untersuchung von Böden als auch für die Untersuchung von Ausgangsmaterialien (z.B. Klärschlammaschen) für ihre Verwendung als Dünger ist eine zuverlässige Analytik und Prozessüberwachung erforderlich. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Wien, Austria DA - 30.11.2015 KW - LIBS KW - Online-RFA KW - Düngemittelgewinnung KW - Bodenfruchtbarkeit KW - BONARES PY - 2015 SP - 23 EP - 24 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38843 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krämer, D. A1 - Violet, N. A1 - Paul, Andrea A1 - Maiwald, Michael A1 - King, R. T1 - Robustification of partial least squares predictions based on near infrared spectroscopy trough nonlinear state estimation N2 - The Cultivation of “Saccharomyces cerevisiae” for enzyme production was monitored using Near-infrared spectroscopy. An inline NIR optrode was therefore immersed in a 15 L vessel. The calibration was done using a Partial Least Squares (PLS) model with reference measurements of glucose, ammonium, phosphate, ethanol, and optical density. A nonlinear biological process model based on an extended Kalman Filter (EKF) was used to describe the fermentation behavior. It was found that EKF corrects inaccurate PLS predictions. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Wien, Austria DA - 30.11.2015 KW - PLS-R KW - Near infrared spectroscopy KW - Prozess-Spektroskopie KW - Process analytical technology KW - Fermentation PY - 2015 SP - 77 EP - 77 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Ruiken, J.-P. A1 - Illner, M. A1 - Müller, D. A1 - Esche, E. A1 - Paul, Andrea A1 - Wozny, G. A1 - Maiwald, Michael T1 - Online spectroscopy in microemulsions – A process analytical approach for hydroformylation miniplant I – Experimental setup and NMR reaction monitoring N2 - Hydroformylation represents an important homogeneous catalyzed process, which is widely used within chemical industry. Usually applied with simple alkenes like Propene and Butene aldehydes obtained from alkenes >C6 are relevant intermediates in production of plasticizers, surfactants and polymers. Today the active catalyst species is often based on valuable Rhodium complexes in aqueous solution. This implies the problem of limited water solubility of the reactands, which is acceptable for short chain lengths, but states a problem in case of higher alkenes. Along with that efficient separation and recycling of the catalyst becomes more complicated. There are different approaches tackling this problem, e.g., by using of salt formation in the BASF process or downstream distillation within the Shell process T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Wien, Austria DA - 30.11.2015 KW - Prozessanalytik KW - Process analytical technology KW - Emuslions KW - Hydroformylation KW - Online NMR spectroscopy KW - Reaction monitoring PY - 2015 SP - 51 EP - 51 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea A1 - Ruiken, J.-P. A1 - Meyer, Klas A1 - Westad, Frank A1 - Illner, M. A1 - Müller, D. A1 - Wozny, G. A1 - Maiwald, Michael T1 - Online spectroscopy in microemulsions – A process analytical approach for hydroformylation miniplant II - Calibration and prediction by Raman spectra N2 - The Collaborative Research Center InPROMPT aims to establish a novel process concept for the hydroformylation of long-chained olefins, using a rhodium complex as catalyst in the presence of syngas. Recently, the hydroformylation in micro-emulsions, which allows for the efficient recycling of the expensive rhodium catalyst, was found to be feasible. However, the temperature and concentration sensitive multi-phase system demands a continuous observation of the reaction to achieve an operational and economically feasible plant operation. For that purpose, we tested the potential of both NMR and Raman spectroscopy for process control assistance. The lab-scale experiments were supported by sampling for off-line GC-analysis as reference analytics. The results of the NMR experiments will be part of another contribution. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Wien, Austria DA - 30.11.2015 KW - Prozessanalytik KW - Process analytical technology KW - Prozess-Spektroskopie KW - Emulsions KW - Hydroformylation KW - Reaction monitoring KW - Raman spectroscopy PY - 2015 SP - 66 EP - 67 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea A1 - Heilmann, M. T. A1 - Schmid, Thomas A1 - Maiwald, Michael T1 - Multivariate classification of Raman spectra from synthetic polymers – an approach for the improved detection of microplastics N2 - The increasing pollution of terrestrial and aquatic ecosystems with plastic debris, which leads to the accumulation of microscopic plastic particles of still unknown fate, is an upcoming problem of our time. In order to monitor the degree of contamination and to understand the underlying processes of degradation and internalization of plastic debris, analytical methods are urgently needed, which help to identify and quantify microplastics. Currently, expensive collected and purified materials enriched on filters are investigated by (micro) infrared spectroscopy (FTIR). Few studies using micro-Raman spectroscopy have been published as well. In contrast to FTIR, Raman spectroscopy can handle wet samples, but it suffers from interference of fluorescent materials. Both micro-FTIR- and micro-Raman, always include time consuming scanning and mapping procedures followed by the manual inspection and measurement of selected particles. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Wien, Austria DA - 30.11.2015 KW - Prozessanalytik KW - Microplastics KW - Mikroplastik KW - Raman-Spektroskopie KW - Polymers KW - Multivariate classification PY - 2015 SP - 80 EP - 81 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38847 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Maiwald, Michael A1 - Guthausen, G. T1 - Abschlussbericht „Prozesskontrolle mittels Niederfeld-NMR-Spektroskopie“ N2 - Die Online-medium-resolution-NMR-Spektroskopie wurde als neue Technik zur Überwachung verfahrenstechnischer Prozesse weiterentwickelt. Entlang der Prozesskette wurden an den verschiedenen Elementen der Online-Spektroskopie gearbeitet. Ein temperierbarer und druckfester Bypass erlaubt, die reagierende Mischung bei Reaktionsbedingungen über eine Pumpe in die NMR-Messzelle zu fördern, für die verschiedene Versionen von temperatur-isolierten NMR-Durchflusszellen berechnet, realisiert und mittels MRI hinsichtlich ihrer strömungsdynamischen und NMR-Eigenschaften charakterisiert wurden. Austauschbare Polymerleitungen für robuste, industrielle Anwendungen kamen ebenso zum Einsatz wie maßgeschneiderte Flusszellen zur Reduktion der Verweilzeitverteilung und des Stoffdurchsatzes. Bewertungsverfahren für MR-NMR-Spektrometer und Durchflusszellen auf Basis leicht verfügbarer Flüssigkeiten (wie z. B. Aceton, Ethanol, Wasser) wurden abgeleitet, Mindestspezifikationen für die Anwendbarkeit der MR-NMR im Prozessmonitoring wurden erarbeitet. Auf der Basis des Bypasssystems konnten einige verschiedene chemische Reaktionen im Bereich einiger 10 s zeitaufgelöst gemessen und ihre Kinetik auch im Fall von Nichtgleichgewichtsmagnetisierung und schneller Strömung analysiert werden. Voraussetzung ist eine stabile und automatisierte Datenbearbeitung, die sich nahtlos in den Workflow von der Datenakquisition bis zur Datenanalyse einbindet. Daher war ein weiteres Augenmerk auf die Datenvorbehandlung gelegt. Bekannte Algorithmen wie die automatisierte Phasenkorrektur entlang der „Minimum Entropy“ Methode und der Maximierung des Realteilspektrums wurden zusammen mit neuen Methoden wie dem Softewarelock implementiert und angewandt. Zur Bestimmung der Konzentrationen wurden verschiedene Verfahren wie die direkte Integration, die Spektrenmodellierung mit und ohne Vorkenntnisse sowie statistische Methoden der Chemometrie angewandt und verglichen. Ebenso ließen sich erstmalig quasiparallel akquirierte 1H- und 19F-MR-NMR-Spektren für die Prozesskontrolle mit gutem Ergebnis analysieren. Die erarbeiteten Konzepte und Verfahren sind unabhängig von der Hard- und -Software des MR-NMR Geräts und damit allgemein einsetzbar. Während des Projektverlaufs kamen Benchtop-Laborgeräte von einer wachsenden Zahl an Herstellern auf den Markt, die immer besser den Anforderungen der Spektroskopie gerecht werden. Online-MR-NMR-Spektroskopie erweitert die Prozessanalytik um eine bislang nur im Labor bekannte chemische Sensitivität gegenwärtig mit der Fähigkeit zur Unterscheidung von beispielsweise Aliphaten, Olefinen oder Aromaten (z. B. Hydrierung) oder Strukturänderungen (z. B. Isomerisierung), bei denen klassische Techniken an ihre Grenzen stoßen. Sie stellt nun eine Alternative für die Prozessanalyse dar, insbesondere wenn schnelle, zerstörungsfreie und integral arbeitende Methoden erforderlich sind. KW - Prozess-Sensoren KW - DFG KW - NMR-Spektroskopie PY - 2015 SP - 1 EP - 15 AN - OPUS4-38852 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mayer, K. A1 - Krause, Martin A1 - Ibrahim, M. A1 - Schubert, Marcus T1 - Requirements for a Small Size Ultrasonic Imaging System for Inspection of Concrete Elements N2 - Ultrasonic imaging systems usually require an array of ultrasonic transducers for data acquisition on a wide area on top of an object under investigation. The goal of an imaging algorithm is the use of reflected ultrasound data to form a recognizable image. Conventional algorithms like SAFT are based on an inverse Huygens' principle and need therefore a dense measurement grid. This requires a big effort in data capturing. For simple and inexpensive measurement different strategies of imaging with reduced amount of data and examples with a manual scanning device on concrete elements are presented. T2 - 19th World Conference on Non-Destructive Testing 2016 CY - Munich, Germany DA - 13.06.2016 KW - NDT-CE KW - Ultrasonic echo KW - SAFT PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-388548 SP - 1245 EP - 1254 PB - DGZfP CY - Bad Breising, Germany AN - OPUS4-38854 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krause, Martin T1 - LAUS – Large Aperture Ultraschall N2 - Prinzip und erste Anwendungsbeispiele eines neu entwickelten Ultraschall-Arrays für die bildgebende Echomessung an sehr dicken Betonbauteilen T2 - Fachtagung Bauwerksdiagnose CY - Berlin, Germany DA - 25.02.2016 KW - Ultraschall-Echo KW - Beton KW - Ultraschall-Array KW - Abbildungsverfahren PY - 2016 AN - OPUS4-38855 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mäder, M. T1 - Pokal der Dresdner Goldschmiedeinnung - Eine naturwissenschaftliche Spurensuche N2 - Die Mitte des 16. Jahrhunderts gegründete Dresdener Goldschmiedeinnung, geriet im 19. Jahrhundert in wirtschaftliche Schwierigkeiten, was letztendlich zu ihrer Auflösung führte. Im Zuge dessen wurde 1872 auch der historische Innungspokal für 80 Taler an das Grüne Gewölbe in Dresden verkauft. Sowohl das Empfehlungsschreiben des damaligen Direktors als auch die Zustimmung zum zügigen Ankauf dürften Beleg dafür sein, dass man damals der festen Überzeugung war, ein etwa 250 Jahre altes, authentisches Silbergefäß erworben zu haben. Die aktuelle kunstwissenschaftliche Begutachtung des Innungspokals lässt begründete Fragen zum Alter und zur Originalität des Objektes, welches heute in der Sammlung des Grünen Gewölbes präsentiert wird, aufkommen. Die kunst-wissenschaftliche und kunsttechnologische Expertise reicht hier allein ftir eine gesicherte Altersbestimmung nicht aus und soll deshalb durch naturwissenschaftliche Untersuchungen zur Materialzusammensetzung unterstützt werden. T2 - Archäometrie und Denkmalpflege 2016 CY - Göttingen, Germany DA - 28.09.2016 KW - Synchrotron KW - BESSY KW - BAMLine KW - XRF PY - 2016 AN - OPUS4-38755 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hachmöller, O. T1 - Elemental bioimaging for the diagnosis of Wilson´s disease by means of LA-ICP-MS N2 - Wilson´s disease, a rare genetic disorder of the copper metabolism, causes the copper accumulation in various organs, leading to manifold hepatic, neurological and psychiatric symptoms. To study the elemental distribution, human Wilson´s disease liver samples were analyzed by means of LA-ICP-MS. Results demonstrated an inhomogeneous copper and iron distribution in human liver with hotspots of very high intensities. Both elements were quantified by an external calibration using matrix-matched standards made of gelatin, showing concentrations up to several thousand micrograms per gram. Additionally, results were validated by means of synchrotron radiation based μXRF at the BAMline at BESSYII (Helmholtz-Zentrum Berlin). T2 - Anwenderttreffen Plasmaspektroskopie CY - Berlin, Germany DA - 22.02.2016 KW - Synchrotron KW - BESSY KW - BAMline KW - XRF PY - 2016 AN - OPUS4-38759 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hachmöller, O. T1 - Investigating Wilson´s disease by elemental bioimaging and speciation analysis using LA-ICP-MS, μXRF and XANES N2 - Wilson´s disease (WD) is a rare genetic disorder of the copper metabolism, causing the accumulation of copper in different organs, including the liver, the central nervous system and cornea. This way, WD initiates manifold hepatic, neurological or psychiatric symptoms. To learn about the elemental distribution and present species in WD, liver samples were analyzed by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS), micro X-ray fluorescence (μXRF) and X-ray absorption near edge structure spectroscopy (XANES). Within this work, LA-ICP-MS was applied to study the distribution of copper and iron in human liver samples, which were collected by a liver biopsy of WD and control patients within a medical investigation. The analysis by LA-ICP-MS was performed with a 213 nm Nd:YAG laser using a spatial resolution of 10 μm and a scan rate of 20 μm/s. In a next step, copper and iron were quantified by LA-ICP-MS using homemade matrix-matched standards made of gelatin. Results showed an inhomogeneous copper and iron distribution in human liver with hotspots up to several thousand micrograms per gram liver within the hepatocytes. Additionally, results for the elemental distribution in WD were validated by means of synchrotron radiation-based μXRF with a beam size of 4 μm at the BAMline at BESSYII (Helmholtz-Zentrum Berlin). Furthermore, XANES was performed to identify the present oxidation states of copper in WD, indicating a mixture of copper(I) and copper(II) within the liver tissue. In the contemporary medicine, rhodanine staining is routinely used to determine the copper distribution in liver tissues. Nevertheless, this method does not provide results with a high sensitivity in comparison to LA-ICP-MS. Therefore, the presented LA-ICP-MS method offers a new possible diagnostic tool. These results may also contribute to a better understanding of Wilson´s disease and its development. T2 - Interdisziplinäres Doktorandenseminar des DAAS CY - Ulm, Germany DA - 06.04.2016 KW - Synchrotron KW - BAMline KW - BESSY KW - XRF KW - XANES PY - 2016 AN - OPUS4-38761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Prost, J. T1 - SR-TXRF-XANES of indoor aerosol samples at BESSY II and ELETTRA N2 - Airborne particulate matter is an issue of growing concern in industrialized countries. Particles with diameters of less than 10 μm, in particular those with less 2.5 μm, are of special concern, as they can enter the human lungs and contribute to various cardiovascular and respiratory diseases. As the composition and health effects of airborne particles in urban, rural and industrial outdoor air has been studied abundantly, our focus lies on the analysis of airborne particle samples collected indoors, which may also have a significant effect on human health, depending on the chemical composition of the particles and the chemical bonding state, in which elements are present. This chemical speciation can be obtained using X-ray absorption near edge structure (XANES) analysis, which requires a tunable excitation source and therefore has to be carried out at synchrotron facilities. For this work, samples were collected in office rooms of the Atominstitut building. The BAMline at BESSYII, Berlin, features a double-multilayer monochromator (DMM) and a double-crystal monochromator (DCM). The DCM offers an energy resolution E/ΔE of around 103, which makes it suitable for X-ray absorption fine structure (XAFS) applications. The Atominstitut SR-TXRF vacuum chamber, formerly located at HASYLAB, Beamline L, is now available at the BAMline. The chamber offers a sample changer for up to 8 quartz carriers suitable for total reflection X-ray fluorescence analysis (TXRF) and was equipped with a 30 mm² silicon drift detector (SDD). Aerosol samples were produced using a modified three-stage Dekati™ impactor. For this work, only the coarse (2.5 to 10 μm, Stage 2) and the fine particle fraction (1 to 2.5 μm, Stage 3), were of interest. XANES analysis was performed for the elements Cr, Cu and Zn. Oxidation states of these 3 elements will be presented. The X-ray Fluorescence beamline at ELETTRA operates in partnership with the IAEA an ultra-high vacuum instrument with a 7-axis manipulator suitable for a variety of X-ray analytical techniques, such as grazing incidence X-ray fluorescence analysis (GI-XRF), TXRF, X-ray reflectometry (XRR) and XANES. Samples were produced using a four-stage Sioutas Personal Cascade Impactor. With this impactor, it is possible to produce sizefractionated samples down to the sub-μm range (Stages: A > 2.5 μm, B 1 to 2.5 μm, C 0.5 to 1 μm and D 0.25 to 0.5 μm). Direct sampling was performed on siliconized 25 mm Si wafers suitable for TXRF. Cu-K edge SR-TXRF-XANES analysis was carried out for samples of all impactor stages. Results of these experiments will be shown. T2 - Denver X-ray Conference CY - Rosemont, Illinois, USA DA - 01.08.2016 KW - Synchrotron KW - BAMline KW - XANES KW - Aerosol PY - 2016 AN - OPUS4-38762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Gräßer, Patrick A1 - Zientek, Nicolai A1 - Maiwald, Michael T1 - First steps towards field integration of benchtop NMR spectroscopy for online monitoring and process control N2 - Online monitoring and process control requires fast and noninvasive analytical methods, which are able to monitor the concentration of reactants in multicomponent mixtures with parts-per-million resolution. Online NMR spectros-copy can meet these demands when flow probes are directly coupled to reactors, since this method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical com-parison method being independent on the matrix. Due to improved magnet design and field shimming strategies portable and robust instruments have been introduced to the market by several manufacturers during the last few years. First studies with this technology showed promising results to monitor chemical reaction in the laboratory. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Wien, Austria DA - 30.11.2015 KW - Online NMR Spectroscopy KW - Smart Sensors KW - Prozess-Spektroskopie KW - Process Analytical Technology KW - Process control PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-388411 SP - 43 EP - 44 AN - OPUS4-38841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Die neue Technologie-Roadmap „Prozess-Sensoren 4.0“ N2 - Derzeit finden gravierende Veränderungen im Umfeld der Informations- und Kommunikationstechnik statt, die eine große Chance für die optimierte Prozessführung und Wertschöpfung mit darauf abgestimmten vernetzt kommunizierenden Sensoren bieten. Diese Art „smarter“ Sensoren stellen Dienste innerhalb eines Netzwerks bereit und nutzen Informationen daraus. Dadurch ergibt sich aktuell die Notwendigkeit, die Anforderungen an Prozess-Sensoren sowie an deren Kommunikationsfähigkeiten detaillierter zu beschreiben – vom einfachen Temperatursensor bis über heute in Entwicklung befindlichen Mess-Systemen hinaus – da diese Technologieentwicklungen rasant voranschreiten. Vernetzte Sensoren sind die Voraussetzung für die Realisierung von Cyber-physischen Produktionssystemen (CPPS) und zukünftiger Automatisierungskonzepte für die Prozessindustrie, wie sie auch durch das Zukunftsprojekt „Industrie 4.0“ adressiert werden. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Wien, Austria DA - 30.11.2015 KW - Roadmap KW - Prozess-Sensoren 4.0 KW - Smart Sensors KW - Smarte Sensoren KW - Prozessanalytik KW - Prozessindustrie PY - 2015 SP - 26 EP - 27 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38842 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strüder, L. A1 - Hartmann, R. A1 - Holl, P. A1 - Ihle, S. A1 - Huth, M. A1 - Schmidt, J. A1 - Tham, Ch. A1 - Kanngießer, B. A1 - Baumann, J. A1 - Renno, A. A1 - Grenzer, J. A1 - Radtke, Martin A1 - Abboud, A. A1 - Pietsch, U. A1 - Soltau, H. T1 - High Speed, High Resolution imaging spectrometers based on pnCCDs for XRF and XRD applications N2 - For many years pnCCDs have been well known as X-ray detectors for spectroscopic imaging in many fields of science: X-Ray Fluorescence analysis (XRF), X-ray Diffraction (XRD) with light sources in large accelerator facilities as well as with laboratory light sources or with X-rays from celestial sources in X-ray astronomy. A brief introduction in GEXRF (Grazing Emission XRF) measurements with a laboratory laser produced plasma source will be given, PIXE (Particle Induced X-ray Emission) measurements and D2XRF (Double Dispersive X-Ray Fluorescence) and Slicing experiments with pnCCDs coupled to polycapillary optics performed at the BESSY synchrotron will be shown. Energy-dispersive Laue diffraction with ultra-hard X-rays for the analysis of defects in metals will conclude the overview of spectroscopic X-ray imaging measurements in the field of structure and dynamics of matter. KW - PnCCD KW - Synchrotron KW - XRF PY - 2016 DO - https://doi.org/10.1017/S1431927616001355 VL - 22 IS - S3 SP - 100 EP - 101 AN - OPUS4-38884 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strüder, L. T1 - High Speed X-ray Imaging and Spectroscopy with pnCCDs: XRF, XRD and PIXE measurements (and others) N2 - For many years pnCCDs have been well known as X-ray detectors for spectroscopic imaging in many fields of science: X-Ray Fluorescence analysis (XRF), X-ray Diffraction (XRD) with light sources in large accelerator facilities as well as with laboratory light sources or with X-rays from celestial sources in X-ray astronomy. A brief introduction in GEXRF (Grazing Emission XRF) measurements with a laboratory laser produced plasma source will be given, PIXE (Particle Induced X-ray Emission) measurements and D2XRF (Double Dispersive X-Ray Fluorescence) and Slicing experiments with pnCCDs coupled to polycapillary optics performed at the BESSY synchrotron will be shown. Energy-dispersive Laue diffraction with ultra-hard X-rays for the analysis of defects in metals will conclude the overview of spectroscopic X-ray imaging measurements in the field of structure and dynamics of matter. T2 - Microscopy & Microanalysis 2016 Meeting CY - Columbus, Ohio, USA DA - 24.07.2016 KW - PnCCD KW - BAMline KW - Synchrotron KW - XRF KW - XRD KW - PIXE PY - 2016 AN - OPUS4-38885 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - WP3 (A 3.3.5 / 3.3.6) electron spectroscopy of core/shell nanoparticles N2 - The presentation summarizes the progress of activity 3.3.5 and 3.3.6 of the Innanopart project. These activities focus on the investigation of different core@shell nanoparticles using synchrotron-radiation-XPS and AES. T2 - Innanopart 18 Months Meeting (EMPIR) CY - Vienna, Austria DA - 31.10.2016 KW - XPS KW - Synchrotron KW - Depth-Profiling KW - AES KW - Core@Shell Nanoparticles PY - 2016 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-38792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina T1 - In situ investigation of mechanochemical syntheses of metal phosphonates N2 - We report on the in situ investigation of mechanochemical syntheses of metal phosphonates. The metal phosphonates are formed in milling reactions starting from a metal acetate and a phosphonic acid. The conversions are observed by synchrotron PXRD and Raman spectroscopy to shed light on the reaction mechanisms including possible intermediates. T2 - 8th HZB User Meeting CY - Berlin, Germany DA - 07.12.2016 KW - Mechanochemistry KW - In situ KW - Metal phosphonates KW - XRD KW - Raman spectroscopy PY - 2016 AN - OPUS4-38780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Barth, Enrico A1 - Homann, Tobias A1 - Prager, Jens T1 - Einpunkt-Laser-Doppler-Vibrometer für die mehrdimensionale Analyse des Schwingungsverhaltens auf Festkörperoberflächen im MHz-Bereich N2 - Zur messtechnischen Analyse des Schwingungsverhaltens von Festkörpern kann die Bewegung der Oberfläche mit einem Laservibrometer vermessen werden. Für bestimmte Anwendungen, beispielsweise bei der Charakterisierung von anisotropen Werkstoffeigenschaften, ist eine mehrdimensionale Bestimmung der Schwingungskomponenten notwendig. Zur Umsetzung des Messprinzips wird ein Ansatz mit einem Einpunkt-Vibrometer verfolgt, welcher sequenziell die Messpunkte aus mehreren Winkeln analysiert und unter Verwendung der Winkelbeziehungen die Normal- und In-Plane-Komponenten der Schwingung berechnet. Die exakte Positionierung des Lasers aus verschiedenen Winkeln stellt durch die hohen Frequenzen und die damit verbundenen Wellenlängen im mm-Bereich die wesentliche Herausforderung bei der Umsetzung des Messverfahrens dar. Bereits kleine Abweichungen führen zu einem hohen Phasenversatz und somit zu nicht tolerierbaren Messfehlern. Unter Berücksichtigung schwer zu ermittelnder Geometrieinformationen wurde ein Verfahren entwickelt, mit dem eine ausreichende Positionierungsgenauigkeit gewährleistet werden kann. Im Vortrag werden zunächst die Fehlereinflüsse analysiert und die Umsetzung des Messverfahrens detailliert vorgestellt. Es wird gezeigt, dass die Schwingungskomponenten bis zu einer Frequenz von 1 MHz mit ausreichender Genauigkeit bestimmt werden können. Zusätzlich wird der Einfluss verschiedener Möglichkeiten zur Erhöhung der Reflektivität der Oberfläche auf die Ergebnisse untersucht. T2 - 43. Jahrestagung für Akustik (DAGA) CY - Kiel, Germany DA - 06.03.2017 KW - ZFP Schweißnaht Ultraschall PY - 2017 SN - 978-3-939296-12-6 SP - 448 EP - 451 AN - OPUS4-39421 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Barth, Enrico T1 - Einpunkt-Laser-Doppler-Vibrometer für die mehrdimensionale Analyse des Schwingungsverhaltens auf Festkörperoberflächen im MHz-Bereich N2 - Zur messtechnischen Analyse des Schwingungsverhaltens von Festkörpern kann die Bewegung der Oberfläche mit einem Laservibrometer vermessen werden. Für bestimmte Anwendungen, beispielsweise bei der Charakterisierung von anisotropen Werkstoffeigenschaften, ist eine mehrdimensionale Bestimmung der Schwingungskomponenten notwendig. Zur Umsetzung des Messprinzips wird ein Ansatz mit einem Einpunkt-Vibrometer verfolgt, welcher sequenziell die Messpunkte aus mehreren Winkeln analysiert und unter Verwendung der Winkelbeziehungen die Normal- und In-Plane-Komponenten der Schwingung berechnet. Die exakte Positionierung des Lasers aus verschiedenen Winkeln stellt durch die hohen Frequenzen und die damit verbundenen Wellenlängen im mm-Bereich die wesentliche Herausforderung bei der Umsetzung des Messverfahrens dar. Bereits kleine Abweichungen führen zu einem hohen Phasenversatz und somit zu nicht tolerierbaren Messfehlern. Unter Berücksichtigung schwer zu ermittelnder Geometrieinformationen wurde ein Verfahren entwickelt, mit dem eine ausreichende Positionierungsgenauigkeit gewährleistet werden kann. Im Vortrag werden zunächst die Fehlereinflüsse analysiert und die Umsetzung des Messverfahrens detailliert vorgestellt. Es wird gezeigt, dass die Schwingungskomponenten bis zu einer Frequenz von 1 MHz mit ausreichender Genauigkeit bestimmt werden können. Zusätzlich wird der Einfluss verschiedener Möglichkeiten zur Erhöhung der Reflektivität der Oberfläche auf die Ergebnisse untersucht. T2 - 43. Jahrestagung für Akustik (DAGA) CY - Kiel, Germany DA - 06.03.2017 KW - Schweißnaht KW - ZFP KW - Ultraschall PY - 2017 AN - OPUS4-39422 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guhl, Svetlana T1 - Online NMR spectroscopy for process monitoring in intensified continuous production plants N2 - Die Überwachung chemischer Reaktionen ist der Schlüssel zur chemischen Prozesskontrolle. Die quantitative NMR-Spektroskopie besitzt ein hohes Potential für das kontinuierliche Prozessmonitoring. Sie arbeitet zerstörungsfrei mit geringen Probenmengen, kommt durch den direkten Nachweis der Kernspins ohne Kalibrierung aus und weist auch in Konzentrationsrandbereichen eine sehr hohe Linearität auf. Durch Innovationen im Bereich der Niederfeld-NMR-Spektroskopie sind seit kurzem kompakte Benchtop-Laborgeräte von einer wachsenden Zahl an Herstellern kommerziell erhältlich. Neben der Verwendung für Lehre und Forschung im Labor besteht ein potentieller Markt für prozesstaugliche Analysatoren auf Basis dieser Technologie. Für die Integration in eine industrielle Umgebung werden hohe Anforderungen an die Robustheit und Sicherheit entsprechender Systeme gestellt. Dies umfasst neben einem zuverlässigen, vollautomatisierten Betrieb vor allem die Konformität mit ATEX-Richtlinien für den Einsatz in den zumeist als explosionsgefährdet geltenden Produktionsbereichen [2]. Insbesondere im Fall kontinuierlicher Prozesse sind Online-Sensoren und eine unmittelbar rückwirkende Regelung (Closed-loop-control) im laufenden Betrieb zur Sicherstellung der Produktqualität zwingend erforderlich. Andernfalls besteht ein hohes Risiko, große Mengen von nicht spezifikationskonformen, sog. Out-of-Spec-Produkten (OOS) zu produzieren, die aufwändig aufbereitet oder schlimmstenfalls verworfen werden müssen. Im Rahmen des EU-Projekts CONSENS (Integrated Control and Sensing) wird ein prozesstauglicher Analysator für den Einsatz in modularen Produktionsanlagen auf Basis eines kommerziell erhältlichen Niederfeld-NMR-Spektrometers entwickelt. Zur Validierung und Verbesserung der Systemintegration dieses Moduls wird eine kontinuierlich betriebene Teilreaktion aus einem pharmazeutischen Produktionsprozess untersucht. Hierbei handelt es sich um die Kopplung der aromatischen Systeme Anilin und o-Fluornitrobenzol unter Verwendung eines Lithiumorganyls. Die hohe Reaktionsgeschwindigkeit dieses Prozessbeispiels erlaubt jedoch keine kinetischen Studien des Reaktionsverlaufs, sodass dies am technisch relevanten Beispiel der katalytischen Hydrierung von 2-Butin-1,4-diol oder weiteren pharmazeutischen Reaktionen demonstriert wird. Im Rahmen dieser Prozessanwendungen ist auch der direkte Vergleich mit etablierten spektroskopischen Verfahren wie UV/VIS-, NIR- und Raman-Spektroskopie geplant. N2 - Process analytical techniques are extremely useful tools for chemical production and manufacture and are of particular interest to the pharmaceutical, food and (petro-) chemical industries. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and relatively inexpensive analysers, which feature advantages like low cost, low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, sufficient robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. A major advantage of NMR spectroscopy is that the method features a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical comparison method which is independent of the matrix. This is an important prerequisite for robust data evaluation strategies within a control concept and reduces the need for extensive maintenance of the evaluation model over the time of operation. Additionally, NMR spectroscopy provides orthogonal, but complimentary physical information to conventional, e.g., optical spectroscopy. It increases the accessible information for technical processes, where aromatic-to-aliphatic conversions or isomerisation’s occur and conventional methods fail due to only minor changes in functional groups. As a technically relevant example, the catalytic hydrogenation of 2-butyne-1,4-diol and further pharmaceutical reactions were studied using an online NMR sensor based on a commercially available low-field NMR spectrometer within the framework of the EU project CONSENS (Integrated Control and Sensing). T2 - 11. Interdisziplinäres Doktorandenseminar CY - Berlin, Germany DA - 12.03.2017 KW - Niederfeld-NMR-Spektroskopie KW - Zerstörungfreie Analytik KW - Online NMR Spektroskopie PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394241 AN - OPUS4-39424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - High-pressure qNMR spectroscopy in condensed- and gas-phase towards determination of impurities and compositions of gas mixtures N2 - Recent technical developments of NMR instruments such as in acquisition electronics and probe design allow detection limits of components in liquid mixtures in the lower ppm range (approx.. 5–10ppm amount of substance). The major advantage of quantitative NMR spectroscopy (qNMR) is that it is a direct ratio method of analysis without the need of calibration. This means that the signal for a specific NMR-active nucleus (e.g., a proton) in an analyte can be compared and quantified by reference to a different nucleus of a separate compound, comparable to a counting of spins in the active volume of the spectrometer. A special application of qNMR in technical mixtures is the observation in the gas phase, which is rarely applied compared to liquid and solid NMR studies. Because of the low density it results in a reduced sensitivity, which can be improved by applying pressure. Therefore a high-pressure NMR setup was developed based on a commercially available NMR tube made of zirconia. This is currently tested up to 20 MPa, but can be extended up to 100 MPa with regard to pressure rating of its components. This work shows results of gas-phase application on natural-gas like reference gas mixtures produced at BAM, as well as investigations on liquefied petroleum gas mixtures (LPG) with high accuracy provided in constant pressure piston cylinders. T2 - qNMR Summit 2017 CY - Berlin, Germany DA - 16.03.2017 KW - Quantitative NMR spectroscopy KW - Gas-phase NMR KW - Reference gas mixtures KW - Liquefied petroleum gas PY - 2017 AN - OPUS4-39425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Glaus, Reto A1 - Nagli, L. A1 - Gornushkin, Igor B. T1 - Stimulated emission in aluminum laser-induced N2 - The stimulated emission (SE) in aluminum laser-induced plasma pumped in resonance with the 3s²3p-3s²4s aluminum transition at 266.04 nm is modeled. A collisional-radiative plasma model based on kinetic equations is proposed to explain the creation of the population inversion and lasing. The model predicts fast depopulation of the ground 3s²3p state by the absorption of resonant laser light at 266 nm and very fast population of the excited 3s²4s state by the cascade transitions from the laser-pumped level, which is driven optically and by collisions. The SE of the 3s²3p-3s²4s transition at 396.15 nm is studied and possible SE at 1.3 and 2.1 μm is predicted. It is confirmed by calculations that the population inversion between the 3s²3p and 3s²4s states can be created by weak pumping at several microjoule–millijoule pulse energies and results in high gain. KW - Lasers KW - Spectroscopy KW - Atomic KW - Laser induced breakdown PY - 2017 DO - https://doi.org/10.1364/AO.56.000695 VL - 56 IS - 3 SP - 695 EP - 701 PB - Optical Society of America AN - OPUS4-39427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Seismic methods for ultrasonic testing in Civil Engineering N2 - Invited presentation on the use of seismic imaging and monitoring technologies in civil engineering T2 - Geophysikalisches Kolloquium der ETH CY - Zürich, Switzerland DA - 17.03.2017 KW - Seimic KW - Ultrasound KW - Monitoring KW - Imaging KW - Concrete PY - 2017 AN - OPUS4-39428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - REFUND: Untersuchung von Bestandsfundamenten und Entscheidungsbäume zur optimierten Weiter- und Nachnutzung N2 - Vor einer geplanten Weiter- oder Wiedernutzung von Bestandsfundamenten stellt sich die Frage nach deren Lage, Geometrie und Zustand im Untergrund. Hierfür gibt es verschiedene Prüfverfahren. Im Projekt REFUND (2014-2016) wurden unter Berücksichtigung der aktuellen Normen und des Standes der Technik Ablaufdiagramme für die Planung der Wiedernutzung und die Untersuchung des Bestandes entwickelt. Dies geschah getrennt für Einzel- und Streifenfundamente, Platten und Pfähle. An zwei Praxisbeispielen wurden die Abläufe getestet und optimiert. Die Ergebnisse wurden in einem Handbuch kompiliert, das bei der TU Darmstadt erscheint. T2 - 24. Darmstädter Geotechnik-Kolloquium CY - Darmstadt, Germany DA - 16.03.2017 KW - Fundamente KW - Wiedernutzung KW - Ablaufdiagramme KW - Planung KW - Prüfung PY - 2017 AN - OPUS4-39429 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lauer, Franziska T1 - Simplifying the preparation of pollen samples for MALDI-TOF MS classification N2 - Matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) is a well-implemented analytical technique for the investigation of complex biological samples. In MS, the sample preparation strategy is decisive for the success of the measurements. Here, sample preparation processes and target materials for the investigation of different pollen grains are compared. A reduced and optimized sample preparation process prior to MALDI-TOF measurement is presented using conductive carbon tape as target. The application of conductive tape yields in enhanced absolute signal intensities and mass spectral pattern information, which leads to a clear separation in subsequent pattern analysis T2 - 11. Interdisziplinäres Doktorandenseminar - GdCH Arbeitskreis Prozessanalytik CY - BAM Adlershof, Berlin, Germany DA - 12.03.2017 KW - Sample pretreatment KW - Conductive carbon tape KW - MALDI-TOF MS KW - PCA KW - Pollen PY - 2017 AN - OPUS4-39439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Dietrich, P. A1 - Thissen, A. A1 - Kulak, N. A1 - Kjaervik, Marit A1 - Unger, Wolfgang T1 - XPS surface chemical analysis of aqueous solutions with EnviroESCA N2 - Water and aqueous reagents are essential in any biological process or system. But apart from a few special low vapor-pressure cases, liquids have not been accessible to any technique requiring UHV conditions. EnviroESCA opens up this exciting field of applications. In this paper first results from water based samples are presented as a proof of concept to demonstrate the special capabilities of EnviroESCA analyzing liquid samples. The following solutions were investigated under near ambient pressure conditions: i.) water, ii.) brine, iii.) an oil in water dispersion, iv.) aqueous iron(II) sulfate heptahydrate, and v.) a suspension of nano silver particles in water. KW - Surface Analysis KW - Near Ambient Pressure XPS KW - Aqueous Solutions PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394603 UR - http://www.enviro.specs.de/cms/upload/bilder/EnviroESCA/Applications/Liquids/Application-Note_EnviroESCA_Aqueous_Solutions.pdf N1 - BAM Mitarbeiter Beitrag im Acknowledgement definiert. IS - #000394 SP - 1 PB - SPECS CY - Berlin AN - OPUS4-39460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertin, Annabelle T1 - Temperature Sensitive Aggregation Behavior of Poly(Acrylamide-co-Acrylonitrile) in Water N2 - Thermoresponsive polymers have shown great potential in applications such as bioseparation, drug delivery and diagnostic. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range have been reported so far. Herein, a robust UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain transfer (RAFT) polymerization and its thermo-induced aggregation behavior in aqueous media was studied. We propose a model for the temperature-induced aggregation behaviour of UCST-type poly(AAm-co-AN) copolymer in aqueous solution on the basis of turbidity measurements, SLS, DLS, SANS and cryo-TEM. T2 - German Physical Society - Spring Meeting 2017 CY - Dresden, Germany DA - 19.03.2017 KW - Thermoresponsive polymers KW - UCST-type copolymer PY - 2017 AN - OPUS4-39465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertin, Annabelle T1 - Functional polymer based on 2,6-diaminopyridine with tunable UCST behaviour in water/alcohol mixture N2 - Thermoresponsive polymers are of great importance in numerous applications such as bioseparation, drug delivery, diagnostic and microfluidic applications. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST), i.e. phase separate from solution upon cooling, in a relevant temperature range and green solvents such as water or ethanol have been reported. Indeed, polymers with UCST behavior below 60°C in alcohol or water/alcohol mixtures are extremely promising for the preparation of smart materials for sensing. In this work two novel functional polymers of based on a 2,6-diaminopyridine motif were synthesized by free radical polymerization. Their UCST-type transition temperature is tunable by varying either their concentration in solution or the type of solvent. Insights into this phenomenon will be given based on turbidimetry and temperature dependent dynamic light scattering T2 - German Physical Society - Spring Meeting 2017 CY - Dresden, Germany DA - 19.03.2017 KW - Thermoresponsive polymers KW - USCT-type polymers KW - Polymers based on 2,6-diaminopyridine PY - 2017 AN - OPUS4-39466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abbas, F. A1 - Donskyi, Ievgen A1 - Gholami, M. A1 - Ziem, B. A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Böttcher, C. A1 - Rabe, J. A1 - Haag, R. A1 - Adeli, M. T1 - Controlled covalent functionalization of thermally reduced graphene oxide to generate defined bifunctional 2D nanomaterials N2 - A controlled, reproducible, gram-scale method is reported for the covalent functionalization of graphene Sheets by a one-pot nitrene [2+1] cycloaddition reaction under mild conditions. The reaction between commercially available 2,4,6-trichloro-1,3,5-triazine and sodium azide with thermally reduced graphene oxide (TRGO) results in defined dichlorotriazine-functionalized sheets. The different reactivities of the chlorine substituents on the functionalized graphene allow stepwise post-modification by manipulating the temperature. This new method provides unique access to defined bifunctional 2D nanomaterials, as exemplified by chiral surfaces and multifunctional hybrid architectures. KW - Graphene oxide KW - Bifunctional 2D nanomaterials KW - XPS KW - NEXAFS KW - AFM PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-394789 DO - https://doi.org/10.1002/ange.201612422 SN - 1433-7851 VL - 56 IS - 10 SP - 2675 EP - 2679 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-39478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nguyen, Thi Yen A1 - Roessler, Ernst A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - Control of organic polymorph formation: crystallization pathways in acoustically levitated droplets N2 - Theoretical and experimental studies indicate that crystal nucleation can take more complex pathways than expected on the ground of the classical nucleation theory. Among these pathways are the formation of pre-nucleation clusters and amorphous precursor phases. A direct in situ observation of the different pathways of nucleation from solution is challenging since the paths can be influenced by heterogeneous nucleation sites, such as container walls. Here, we provide insights into the crystallization process using the in situ combination of an acoustic levitator, Raman spectroscopy, and X-ray scattering. The contactless sample holder enables the observation of homogeneous crystallization processes and the detection of intermediates and final crystalline forms. We provide evidence for the existence of multiple pathways of nucleation based on the investigation of the crystallization of organic molecules from different solvents. Starting from a diluted solution, a supersaturation is reached during the experiment due to the evaporation of the solvent. The highly supersaturated solution reveals different pathways of crystallization. Depending on the degree of supersaturation either the thermodynamically stable or the metastable crystal form is observed. KW - Crystallization KW - In situ XRD KW - Polymorphism KW - Polyamorphism KW - Raman spectroscopy PY - 2017 DO - https://doi.org/10.1515/zkri-2016-1964 SN - 2194-4946 SN - 2196-7105 VL - 232 IS - 1-3 SP - 15 EP - 24 PB - De Gruyter CY - Berlin AN - OPUS4-39708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernsmeier, D. A1 - Bernicke, M. A1 - Ortel, Erik A1 - Bergmann, A. A1 - Lippitz, Andreas A1 - Nissen, J. A1 - Schmack, R. A1 - Strasser, P. A1 - Polte, J. A1 - Kraehnert, R. T1 - Nafion-free carbon-supported electrocatalysts with superior hydrogen evolution reaction performance by soft templating N2 - Efficient water electrolysis requires electrode coatings with high catalytic activity. Platinum efficiently catalyzes the hydrogen evolution reaction in acidic environments, but is a rare and expensive metal. The activity achieved per metal atom can be increased if small Pt particles are dispersed onto electrically conductive, highly accessible and stable support materials. However, the addition of Nafion, a typical binder material used in the manufacture of electrode coatings, can decrease catalytic activity by the blocking of pores and active surface sites. A new approach is reported for the direct synthesis of highly active Nafion-free Pt/C catalyst films consisting of small Pt nanoparticles supported in size-controlled mesopores of a conductive carbon film. The synthesis relies on the co-deposition of suitable Pt and C precursors in the presence of polymer micelles, which act as pore templates. Subsequent carbonization in an inert atmosphere produces porous catalyst films with controlled film thickness, pore size and particle size. The catalysts clearly outperform all Nafion-based Pt/C catalysts reported in the literature, particularly at high current densities. KW - XPS KW - SEM KW - TEM KW - SAXS KW - Catalysis KW - Electrochemistry PY - 2017 DO - https://doi.org/10.1002/celc.201600444 SN - 2196-0216 VL - 4 IS - 1 SP - 221 EP - 229 PB - Wiley Online Library CY - Weinheim AN - OPUS4-39733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liehr, Sascha A1 - Breithaupt, Mathias A1 - Krebber, Katerina T1 - Distributed humidity sensing in PMMA optical fibers at 500 nm and 650 nm wavelengths N2 - Distributed measurement of humidity is a sought-after capability for various fields of application, especially in the civil engineering and structural health monitoring sectors. This article presents a method for distributed humidity sensing along polymethyl methacrylate (PMMA) polymer optical fibers (POFs) by analyzing wavelength-dependent Rayleigh backscattering and attenuation characteristics at 500 nm and 650 nm wavelengths. Spatially resolved humidity sensing is obtained from backscatter traces of a dual-wavelength optical time domain reflectometer (OTDR). Backscatter dependence, attenuation dependence as well as the fiber length change are characterized as functions of relative humidity. Cross-sensitivity effects are discussed and quantified. The evaluation of the humidity-dependent backscatter effects at the two wavelength measurements allows for distributed and unambiguous measurement of relative humidity. The technique can be readily employed with low-cost standard polymer optical fibers and commercial OTDR devices. KW - Optical fiber sensor KW - Humidity sensor KW - Distributed sensor KW - Polymer optical fiber KW - Rayleigh scattering PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-396363 UR - http://www.mdpi.com/1424-8220/17/4/738 DO - https://doi.org/10.3390/s17040738 SN - 1424-8220 VL - 17 IS - 4 SP - Article 738, 1 EP - 12 PB - MDPI CY - Basel, Switzerland AN - OPUS4-39636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, J. A1 - Rankovic, M. A1 - Milosavljevic, A. A1 - Bald, Ilko T1 - A novel setup for the determination of absolute cross sections for low-energy electron induced strand breaks in oligonucleotides – The effect of the radiosensitizer 5-fluorouracil N2 - Low-energy electrons (LEEs) play an important role in DNA radiation damage. Here we present a method to quantify LEE induced strand breakage in well-defined oligonucleotide single strands in terms of absolute cross sections. An LEE irradiation setup covering electron energies <500 eV is constructed and optimized to irradiate DNA origami triangles carrying well-defined oligonucleotide target strands. Measurements are presented for 10.0 and 5.5 eV for different oligonucleotide targets. The determination of absolute strand break cross sections is performed by atomic force microscopy analysis. An accurate fluence determination ensures small margins of error of the determined absolute single strand break cross sections σSSB. In this way, the influence of sequence modification with the radiosensitive 5-Fluorouracil (5FU) is studied using an absolute and relative data analysis. We demonstrate an increase in the strand break yields of 5FU containing oligonucleotides by a factor of 1.5 to 1.6 compared with non-modified oligonucleotide sequences when irradiated with 10 eV electrons. KW - DNA origami KW - DNA radiation damage KW - Radiosensitizer KW - AFM KW - Fluorouracil PY - 2017 UR - http://epjd.epj.org/articles/epjd/abs/2017/02/d160608/d160608.html DO - https://doi.org/10.1140/epjd/e2016-70608-4 VL - 71 SP - 32 PB - Springer CY - New York, NY, USA AN - OPUS4-39643 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schürmann, Robin A1 - Bald, Ilko T1 - Real-time monitoring of plasmon induced dissociative electron transfer to the potential DNA radiosensitizer 8-bromoadenine N2 - The excitation of localized surface plasmons in noble metal nanoparticles (NPs) results in different nanoscale effects such as electric field enhancement, the generation of hot electrons and a temperature increase close to the NP surface. These effects are typically exploited in diverse fields such as surface-enhanced Raman scattering (SERS), NP catalysis and photothermal therapy (PTT). Halogenated nucleobases are applied as radiosensitizers in conventional radiation cancer therapy due to their high reactivity towards secondary electrons. Here, we use SERS to study the transformation of 8-bromoadenine (8BrA) into adenine on the surface of Au and AgNPs upon irradiation with a low-power continuous wave laser at 532, 633 and 785 nm, respectively. The dissociation of 8BrA is ascribed to a hot-electron transfer reaction and the underlying kinetics are carefully explored. The reaction proceeds within seconds or even milliseconds. Similar dissociation reactions might also occur with other electrophilic molecules, which must be considered in the interpretation of respective SERS spectra. Furthermore, we suggest that hot-electron transfer induced dissociation of radiosensitizers such as 8BrA can be applied in the future in PTT to enhance the damage of tumor tissue upon irradiation. KW - SERS KW - Nanoparticles KW - Hot electrons KW - Bromoadenine KW - Catalysis PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-396469 DO - https://doi.org/10.1039/C6NR08695K SN - 2040-3364 SN - 2040-3372 VL - 9 IS - 5 SP - 1951 EP - 1955 PB - RSC AN - OPUS4-39646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Spranger, Holger A1 - Beckmann, Jörg T1 - THz-SAFT Rekonstruktion von HDPE-Bauteilen N2 - Obwohl THz-TDS-Systeme vielfältige Qualitätsparameter von Dielektrika ermitteln können, ist deren industrielle Nutzung im Bereich der zerstörungsfreien Bauteilprüfung noch nicht anerkannter Stand der Technik. Ein pragmatischer Weg, TDS-Systeme neben traditionellen Prüfverfahren zu etablieren, sind systematische Untersuchungen an Modellbauteilen, mit dem Ziel einer Methodenentwicklung zur zuverlässigen berührungslosen Prüfung von Dielektrika. Anhand von THz-TDS-Messungen an Polyethylen-Testkörpern mit künstlich eingebauten Fehlstellen werden anfänglich die Möglichkeiten der Laufzeitmessung zur Ermittlung von Tiefenlagen von Ungänzen in Testkörpern präsentiert. Im weitern Teil wird gezeigt, wie durch eine veränderte Versuchsdurchführung und Verwendung eines modifizierten SAFT-Rekonstruktions-Algorithmus Tomogramme berechnet werden können, in denen die künstlich eingebrachten Fehlstellen hinsichtlich ihrer Größe und Lage geometrisch richtig dargestellt werden. T2 - 3. Fachseminar des FA MTHz Mikrowellen- und Terahertz-Prüftechnik in der Praxis CY - Würzburg, Germany DA - 05.04.2017 KW - THz KW - THz-SAFT KW - THz-TDS KW - SAFT KW - HDPE PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-396883 SN - 978-3-940283-84-9 VL - 161 SP - 1 EP - 9 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-39688 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Spranger, Holger T1 - THZ-SAFT Rekonstruktion von HDPE-Bauteilen N2 - Obwohl THz-TDS-Systeme vielfältige Qualitätsparameter von Dielektrika ermitteln können, ist deren industrielle Nutzung im Bereich der zerstörungsfreien Bauteilprüfung noch nicht anerkannter Stand der Technik. Ein pragmatischer Weg, TDS-Systeme neben traditionellen Prüfverfahren zu etablieren, sind systematische Untersuchungen an Modellbauteilen, mit dem Ziel einer Methodenentwicklung zur zuverlässigen berührungslosen Prüfung von Dielektrika. Anhand von THz-TDS-Messungen an Polyethylen-Testkörpern mit künstlich eingebauten Fehlstellen werden anfänglich die Möglichkeiten der Laufzeitmessung zur Ermittlung von Tiefenlagen von Ungänzen in Testkörpern präsentiert. Im weitern Teil wird gezeigt, wie durch eine veränderte Versuchsdurchführung und Verwendung eines modifizierten SAFT-Rekonstruktions-Algorithmus Tomogramme berechnet werden können, in denen die künstlich eingebrachten Fehlstellen hinsichtlich ihrer Größe und Lage geometrisch richtig dargestellt werden. T2 - 3. Fachseminar Mikrowellen- und Terahertz-Prüftechnik in der Praxis CY - Würzburg, Germany DA - 05.04.2017 KW - THz KW - THz-SAFT KW - HDPE PY - 2017 AN - OPUS4-39689 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online spectroscopy in microemulsions – Process analytical technology for a hydroformylation mini-plant N2 - Within the Collaborative Research Center InPROMPT a novel process concept for the hydroformylation of long-chained olefins is studied in a mini-plant, using a rhodium complex as catalyst in the presence of syngas. Recently, the hydroformylation in micro¬emulsions, which allows for the efficient recycling of the expensive rhodium catalyst, was found to be feasible. However, the high sensitivity of this multi-phase system with regard to changes in temperature and composition demands continuous observation of the reaction to achieve a reliable and economic plant operation. For that purpose, we tested the potential of online NMR and Raman spectroscopy for process control. The lab-scale experiments were supported by data of offline GC analysis. A fiber optic coupled probe of a process Raman spectrometer was directly integrated into the reactor. 25 mixtures with varying concentrations of olefin (1-dodecene), product (n-tridecanal), water, n-dodecane, and technical surfactant (Marlipal 24/70) were prepared according to a D-optimal design. Online NMR spectroscopy was implemented by using a flow probe equipped with 1/16” PFA tubing serving as a flow cell. This was hyphenated to the reactor within a thermostated bypass to maintain process conditions. Partial least squares regression (PLSR) models were established based on the initial spectra after activation of the reaction with syngas for the prediction of unknown concentrations of 1-dodecene and n-tridecanal over the course of the reaction in the lab-scale system. The obtained Raman spectra do not only contain information on the chemical composition but are further affected by the emulsion properties of the mixtures, which depend on the phase state and the type of micelles. Based on the spectral signature of both Raman and NMR spectra, it could be deduced that especially in reaction mixtures with a high content of 1-dodecene the formation of isomers based on a competitive reaction was dominating. Similar trends were also observed during some of the process runs in the mini-plant. The multivariate calibration allowed for the estimation of reactants and products of the hydroformylation reaction in the laboratory setup, as well as in the field during the conducted mini-plant operation studies. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Prozessanalytik KW - Online-NMR-Spektroskopie KW - Online-Raman-Spektroskopie KW - Mikroemulsionen PY - 2017 AN - OPUS4-39691 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Design and validation of a compact NMR analyser N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and inexpensive analysers, which feature advantages like low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. Otherwise there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Union’s Research Project CONSENS by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. The presented NMR module is provided in an explosion proof housing with a module size of 57 x 57 x 85 cm and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling (IHM) was selected for data analysis of the low-field NMR spectra. A set-up for monitoring continuous reactions in a thermostated 1/8” tubular reactor using automated syringe pumps was used to validate the IHM models by using high-field NMR spectroscopy as analytical reference method. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Online NMR spectroscopy KW - Low-Field NMR spectroscopy KW - Modular production plants KW - Process analytical technology PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-396960 AN - OPUS4-39696 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Werkstoffprüfung mittels Ultraschall - …was kann Plasma dort beitragen? N2 - Übersichtsvortrag über die Herausforderungen der Luftultraschallprüfung und welche Möglichkeiten sich durch den Einsatz von Plasmawandler ergeben. T2 - Arbeitsgruppenseminar der AG Plasmatechnologie CY - Kiel, Germany DA - 06.04.2017 KW - Plasma KW - Luftultraschall KW - Dielectric barrier discharge KW - Micro hollow cathode KW - Ultraschallprüfung PY - 2017 AN - OPUS4-39699 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane T1 - A round robin test of flash thermography – detectability and quantification of artificial and natural defects in CFRP and metal structures N2 - Within the scope of a DIN INS project, a flash thermography round robin test that evaluates reliability, comparability, and efficiency of different testing situations was organized. The results give information about the detectability of defects, e.g. depending on their size and depth, the evaluation methods and the materials used. Besides, the influences of equipment and parameters used by the participants on the results were analysed. All of the quantitative results as well as the feedback given by the participants will be presented in a DIN committee in order to contribute to a flash thermography standard. T2 - Conference QIRT 2016 CY - Gdansk, Poland DA - 04.07.2016 KW - Active thermography KW - Round robin test KW - CFRP KW - Metal KW - Flash excitation PY - 2016 AN - OPUS4-37511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Neutron and dielectric spectroscopy - taking advantage of the strengths of each technique in confinement studies: Vibrational and molecular dynamics of nanoconfined liquid crystals N2 - The effect of a nanometre confinement on the molecular dynamics of liquid crystals was studied by broadband dielectric and neutron spectroscopy. As confining host the molecular sieve Al-MCM-41 (Si/Al=60) with a mean pore diameter of 3 nm was selected. As guest the liquid crystals 8CB and E7 were chosen where the latter does not crystallize but undergoes a glass transition forming a nematic glass. Dielectric spectroscopy shows that for the confined systems one relaxation process is observed. Ist characteristic relaxation time is much lower compared to that of the bulk. No signature of the Phase transition characteristics of the bulk liquid crystal is detected. The temperature dependence of the relaxation time of this relaxation process has to be described by the Vogel-Fulcher-Tammann equation and thus shows similarities to glassy dynamics. The vibrational density of states measured by neutron spectroscopy (IN6, ILL; TOFTOF, MLZ) Shows excess contributions with respect to the Debye density of states (boson peak). For the confined systems the low frequency contributions of the boson peak are suppressed, an effect which is also found for conventional glass forming systems. In addition elastic scans were carried out at the backscattering spectrometer (BS) IN10 at ILL. Such measurements provide an overview about the temperature dependence of the microscopic dynamics. Assuming a Gaussian form for the elastically scattered intensities the effective mean square displacement was calculated. For the nanoconfined samples the mean square displacement is strongly reduced in comparison to the bulk. Also these measurements show the signature of a glass Transition indicated by a change in the temperature dependence of the mean square displacement. For confined E7 the extracted glass transition temperature is shifted by more than 20 K to higher temperatures. Broadband inelastic neutron scattering was carried out by combining time-of-flight (IN6, ILL; TOFTOF, MLZ) and backscattering (IN10, ILL; SPHERES, MLZ) experiments in the time domain. The time dependence of the incoherent intermediate scattering function Sinc(q,t) shows two Relaxation processes which were quantitatively analyzed by fitting the KWW function to the data. The process at shorter times shows a close similarity the methyl group rotation found for polymeric systems. The process at longer times was assigned to glassy dynamics. The obtained data are compared in detail in their temperature dependence to the dielectric results. T2 - Deutsche Neutronenstreutagung 2016 CY - Kiel, Germany DA - 20.09.2016 KW - Neutron scattering KW - Broadband dielectric spectroscopy PY - 2016 AN - OPUS4-37516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Cheng-Chieh T1 - Determination of an approximate anisotropic model for a given geometrical complex isotropic structure by means of finite element method and least-squares adjustment N2 - Many engineering structures are made of composite materials or metal foam. To simulate the deformational behaviour of these structures often requires a high number of discretisation elements. This in turn yields a very large system of linear equations that are extremely time and memory consuming or practically impossible to solve. It is therefore desirable to find an approach to overcome this obstacle. T2 - PhD Day 2016 CY - Berlin, Germany DA - 01.09.2016 KW - Least-Squares Adjustment KW - Inverse Analysis KW - Finite Element Method PY - 2016 AN - OPUS4-37521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Cheng-Chieh T1 - Ersatzmodell von komplexen geometrischen Strukturen für FEA N2 - Der Grad der Finite-Elemente-Diskretisierung wird vom Verhältnis der Details zur Objektgröße bestimmt. Die Diskretisierung eines großen Objektes mit vielen kleinen Details führt zu einer hohen Anzahl an Elementen bzw. Knotenpunkten. Die Berechnung solcher Körper erfordern nicht nur sehr hohe Rechenzeit, sondern was die Berechnung unmöglich macht, ist der sehr hohe Speicherbedarf. Mit Hilfe eines Ersatzkörpers wird dieses Problem umgangen. T2 - VDI/VDE-GMA Fachausschuss 2.12 "Strukturanalyse und -überwachung in der Bautechnik im Fachbereich Prozessmesstechnik und Strukturanalyse" CY - Darmstadt, Germany DA - 08.09.2016 KW - Ausgleichungsrechnung KW - Inverse Analysis KW - Finite-Elemente-Method PY - 2016 AN - OPUS4-37522 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Cheng-Chieh T1 - Approximate model for geometrical complex structures N2 - Many engineering structures are made of composite materials or metal foam. To simulate the deformational behaviour of these structures often requires a high number of discretisation elements. This in turn yields a very large system of linear equations that are extremely time and memory consuming or practically impossible to solve. It is therefore desirable to find an approach to overcome this obstacle. T2 - 33rd Danubia- Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Inverse analysis KW - Finite element method KW - Least-squares adjustment PY - 2016 AN - OPUS4-37523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Lange, Thorid A1 - Hielscher, Stefan A1 - Rietz, Uwe A1 - Lerche, D. A1 - Pfuch, A. T1 - Multiple-sample approach for bonding and testing: validation of bonding strength of adhesive-bonded joints and adhesive tapes N2 - The multiple-sample approach by means of centrifugal adhesion testing (CAT-technology) allows the determination of bonding strength of adhesive-bonded joints on a statistical basis of up to eight samples. Therefore, it is obvious to ensure the continuous handling and identical processing of an octet of samples within the entire process chain of wet-chemical cleaning, plasma-chemical pre-treatment, bonding of samples, and testing of bonding strength. Within the multiple-sample bonding set-up (MPKV-technology) a defined bonding pressure can be adjusted regardless the actual number of samples. A comparison of single- and multiple-sample approach is made for bonding strength of selected adhesives, double-sided adhesive tapes and different material combinations [stainless steel (V2A) vs. stainless steel, polyamide (PA), or polypropylene (PP)]. It is shown that both technologies improve reliability of results T2 - EURADH 2016 Adhesion ´16 CY - Glasgow, UK DA - 21.09.2016 KW - Multiple-sample bonding KW - Multiple-sample testing KW - Bonding strength KW - Adhesives and adhesive tapes PY - 2016 SP - 162 EP - 166 AN - OPUS4-37588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thiel, Erik A1 - Kreutzbruck, M. A1 - Ziegler, Mathias T1 - Laser-projected photothermal thermography using thermal wave field interference for subsurface defect characterization N2 - The coherent superposition of two anti-phased thermal wave fields creates a zone of destructive interference which is extremely sensitive to the presence of defects without any reference measurements. Combining a high power laser with a spatial light modulator allows modulating phase and amplitude of an illuminated surface that induces spatially and temporally controlled thermal wave fields. The position and depth of defects are reconstructed from analysis of the Amplitude and Phase of the resulting photothermal signal. The proposed concept is experimentally validated and supported by numerical modeling. KW - Thermal waves KW - Active thermography KW - DMD KW - Spatial light modulator KW - Subsurface defects PY - 2016 UR - http://scitation.aip.org/search?value1=laser+projected+photothermal&option1=all&option912=resultCategory&value912=ResearchPublicationContent&operator8=AND&option8=pub_serialIdent&value8=aip%2Fjournal%2Fapl&qs=true DO - https://doi.org/10.1063/1.4963139 SN - 0003-6951 VL - 109 IS - 12 SP - 123504-1 EP - 123504-4 PB - AIP Publishing CY - Melville, New York AN - OPUS4-37590 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Cheng-Chieh T1 - Approximate model for geometrical complex structures N2 - Many engineering structures are made of composite materials or metal foam. To simulate the deformational behaviour of these structures often requires a high number of discretisation elements. This in turn yields a very large system of linear equations that are extremely time and memory consuming or practically impossible to solve. It is therefore desirable to find an approach to overcome this obstacle. T2 - 33rd Danubia- Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Inverse analysis KW - Finite element method KW - Least-squares adjustment PY - 2016 AN - OPUS4-37524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bresch, Harald A1 - Lexow, Jürgen A1 - Sturm, Heinz A1 - Packroff, R. A1 - Völker, D. A1 - Mutz, D. A1 - Bosse, H. A1 - Gebel, T. A1 - Pipke, R. A1 - Marx, R. A1 - Plitzko, S. A1 - Niesmann, K. A1 - Meyer-Plath, A. A1 - Burgdorf, T. A1 - Engel, N. A1 - Epp, A. A1 - Haase, A. A1 - Herzberg, F. A1 - Laux, P. A1 - Oberemm, A. A1 - Sommer, Y. A1 - Tentschert, J. A1 - Ulm, G. A1 - Schwirn, K. A1 - Liesegang, C. T1 - Nanomaterialien und andere innovative Werkstoffe: anwendungssicher und umweltverträglich T1 - Nanomaterials and other advanced materials: application safety and environmental compatibility N2 - Mit einer langfristigen Forschungsstrategie begleiten die für die Sicherheit von Mensch und Umwelt zuständigen Bundesoberbehörden (Umweltbundesamt, Bundesinstitut für Risikobe-wertung, Bundesanstalt für Arbeitsschutz und Arbeitsmedizin, Bundesanstalt für Materialfor-schung und -prüfung und Physikalisch-Technische Bundesanstalt) die rasch voranschreiten-de Entwicklung neuer Materialien unter den Gesichtspunkten des Arbeits-, Verbraucher- und Umweltschutzes. Die Strategie steht daher in enger Verbindung zu den öffentlichen Förder-programmen für Nanomaterialien und andere innovative Werkstoffe, z. B. des BMBF („Vom Material zur Innovation“) und der EU („Horizon 2020“). Die Forschungsstrategie baut auf den bisherigen Ergebnissen der 2008 begonnenen und 2013 erstmals bilanzierten gemeinsamen Forschungsstrategie der Bundesoberbehörden „Nanotechnologie - Gesundheits- und Umweltrisiken von Nanomaterialien"1 auf und erweitert den Blickwinkel auch auf andere Materialinnovationen, bei denen vergleichbare Risiken für Mensch und Umwelt bestehen oder abgeklärt werden müssen. Darüber hinaus greift sie die Idee „anwendungssichere chemische Produkte“2 aus der Initiative „Neue Qualität der Arbeit“ (INQA) des Bundesministeriums für Arbeit und Soziales (BMAS) und das Konzept der nach-haltigen Chemie3 auf, das vom Bundesministerium für Umwelt, Naturschutz, Bau und Reak-torsicherheit (BMUB) unterstützt wird. Durch eine anwendungssichere und umweltverträgli-che Gestaltung innovativer Materialien und ihrer Folgeprodukte sollen nicht akzeptable Risi-ken für Mensch und Umwelt von Anfang an weitgehend ausgeschlossen werden. Dies kann erreicht werden durch 1. die Verwendung sicherer Materialien ohne Gefahreneigenschaften für Mensch und Umwelt (direkte Anwendungssicherheit) oder 2. eine Produktgestaltung, die über den gesamten Lebenszyklus emissionsarm und umweltverträglich ist (integrierte Anwendungssicherheit) oder 3. eine Unterstützung des Anwenders (product stewardship) durch den Hersteller bei technischen, organisatorischen und persönlichen Schutzmaßnahmen zur sicheren Verwendung und Entsorgung des Produktes (unterstützte Anwendungssicherheit). Die Fortschreibung der Forschungsstrategie soll als Bestandteil des Nanoaktionsplans 2020 der Bundesregierung Beiträge der Ressortforschung zu folgenden Schwerpunkten leisten: • Charakterisierung und Bewertung der Risiken von Materialinnovationen • Unterstützung von Forschungseinrichtungen und Unternehmen • Fortschreiben von Rechtsvorschriften und Praxisempfehlungen 1 http://www.baua.de/nn_47716/de/Themen-von-A-Z/Gefahrstoffe/Nanotechnologie/pdf/Forschungsstrategie.pdf 2 http://www.baua.de/de/Themen-von-A-Z/Gefahrstoffe/Nachhaltige-Chemie/Nachhaltige-Chemie.html 3 http://www.umweltbundesamt.de/themen/chemikalien/chemikalien-management/nachhaltige-chemie 2 • Gesellschaftliche Akzeptanz Die Forschungsstrategie soll mit Projekten und anderen forschungsnahen Aktivitäten umge-setzt werden. Dies umfasst die eigene Forschung der Häuser, die extramurale Ausschrei-bung und Vergabe von Forschungsdienstleistungen sowie die Beteiligung an vorwiegend öffentlich geförderten Drittmittelprojekten. Hinzu kommen Aktivitäten im Rahmen der Politik-beratung und der hoheitlichen Aufgaben. Mit inter- und transdisziplinären Ansätzen soll die Risiko- und Sicherheitsforschung enger mit der Innovationsforschung und Materialentwick-lung verknüpft werden. Die Forschungsstrategie ist aufgrund der raschen Entwicklungen auf diesem Gebiet für den Zeitraum bis 2020 angelegt. Die Forschungsziele adressieren die in diesem Zeitraum voraussichtlich umsetzbaren Forschungsansätze. Die Forschungsstrategie wird durch einen Arbeitskreis begleitet und spätestens mit Ablauf des Nanoaktionsplans 2020 evaluiert und angepasst. KW - Forschungsstrategie KW - Bundesoberbehörden KW - Nanomaterialien KW - Innovative Werkstoffe KW - Nano PY - 2016 UR - https://www.bam.de/_SharedDocs/DE/Downloads/nano-forschungsstrategie-2016.pdf?__blob=publicationFile&v=3 UR - http://www.baua.de/de/Themen-von-A-Z/Gefahrstoffe/Nanotechnologie/pdf/Fortschreibung-Forschungsstrategie.pdf?__blob=publicationFile&v=3 UR - http://www.bmub.bund.de/fileadmin/Daten_BMU/Download_PDF/Nanotechnologie/forschungsstrategie_bundesoberbehoerden_de_bf.pdf SP - 1 EP - 28 PB - UBA/BfR/BAuA/BAM/PTB CY - Berlin AN - OPUS4-37526 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madkour, Sherif T1 - Dielectric investigations on carbon nanomembranes N2 - Multilayer carbon nanomembrances (CNMs) could pave the way for a new ultrathin functional conductive coatings with tunable electrical, optical, and chemical properties. Due to their molecular thickness, they can also be regarded as “interfaces without bulk” separating regions of different gaseous, liquid, or solid components and controlling the materials exchange between them, making them optimal materials for membranes applications. Furthermore, their physical and chemical properties depend strongly on their structure, molecular composition, and the surroundings of either sides, thus allowing for tailored properties. Here, nanolayers of Aromatic p-terphenylthiol (TPT) self-assembled into 2D carbon monolayers (thickness - 1.6 nm) were synthesized and further crosslinked by ion bombardment, forming CNMs. Here, though a recently developed multilayer nanosheets routine, stacks of 5, 10, 15 and 20 TPT sheets where transferred on top of each other forming a multilayered CNMs. However, this transfer routine could introduce some intrinsic defects to the sheets, which would alter the molecular composition and / or structure, thus consequently the CNMs properties. Therefore, it is essential to characterize defects in “pure” TPT nanomembranes, before tailoring the molecular compositions, e.g. adding functional groups. For this reason, broadband dielectric spectroscopy (BDS) was utilized to characterize any defects that could be rasied during preparation. Due the structure of pure TPT membranes, no dipole moment should exsist. However, the presence of other elements, e.g. water or sulphur, would result in a dipole moment that could be probed by BDS. As a main result, for all different stacked-layer numbers, a clear relaxation process is seen, which moves to higher frequencies with increasing the temperature. The temperature dependence of the relaxation rate of this process is independent of film thickness and can be well described by a common VFT function, hence a corporative motion. This relaxation process was assigned to intrinisic defects in the membranes, introduced during preparation, which was further confimed by a detailed anaylsis of the dielectric strength. This is the first BDS measurment on TPT CNMs. T2 - 9th International Conference on Broadband Dielectric Spectroscopy and its Applications CY - Pisa, Italy DA - 11.09.2016 KW - Carbon nanomembranes PY - 2016 AN - OPUS4-37527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Cheng-Chieh A1 - Weisbrich, S. A1 - Neitzel, F. ED - Aulova, Alexandra ED - Rogelj Ritonja, Alenka ED - Emri, Igor T1 - Approximate model for geometrical complex structures N2 - Many engineering structures are made of composite materials or metal foam. To simulate the deformational behaviour of these structures often requires a high number of discretisation elements. This in turn yields a very large system of linear equations that are extremely time and memory consuming or practically impossible to solve. It is therefore desirable to find an approach to overcome this obstacle. T2 - 33rd Danubia- Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Inverse analysis KW - Finite element method KW - Least-squares adjustment PY - 2016 SN - 978-961-94081-0-0 SP - 52 EP - 53 CY - Ljubljana AN - OPUS4-37529 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer T1 - Punktuelle Bestimmung der tatsächlichen Energieabgabe von Blitzlampen N2 - Der Beitrag beschreibt Untersuchungen und Entwicklungsarbeiten für einen technisch einfach zu realisierenden Sensor, der die breitbandige kurzzeitige Energieabgabe von Blitzlampen punktuell bestimmen kann. Solche Lampen werden in der zerstörungsfreien Prüfung als Energiequelle für thermografische Untersuchungen genutzt. Dabei soll die zeitliche Entwicklung der Oberflächentemperatur des Sensors mit der ohnehin vorhandenen IR-Kamera aufgenommen und danach ausgewertet werden. Hierzu wurden zwei Konzepte betrachtet: thermisch dünne und thermisch dicke Proben. Der direkte Vergleich zeigt die Vorteile von thermisch dicken Proben, die in der Physik der beteiligten Wärmeausgleichsprozesse begründet sind. T2 - 18. Fachtagung Sensoren und Messsysteme 2016 CY - Nürnberg, Germany DA - 10.05.2016 KW - Blitz-Thermografie KW - Zerstörungsrfreie Prüfung KW - Blitzlampen KW - Energieabgabe KW - Energiesensor PY - 2016 AN - OPUS4-37531 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Helmerich, Rosemarie T1 - Long-Term measurement of vertical displacements at the outer concrete bridges of the Berlin Main Station N2 - The Berlin Main Station was built between 2000 and 2006. At the occasion of the 10th anniversary after the Berlin Main Station was officially opened to train traffic, a view back on eight years of monitoring was given. For the period of the construction with different load cases, the monitoring system was required by the Railway Authorities (Eisenbahnbundesam, EBA) to survey differential vertical displacements between neighbouring supports of the glas roof and the partially prestressed middle bridges. 128 sensors were installed.The data was published in the Internet with access restricted to the BAM scientists and the owner of the station, the German Railways DB AG. T2 - 33rd Danubia- Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Strain measurements KW - Monitoring KW - Differential displacements KW - Berlin Main Station KW - Hydraulic levelling system KW - Laser-based displacement measuring system PY - 2016 AN - OPUS4-37540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Villatoro, J. A1 - Zühlke, M. A1 - Riebe, D. A1 - Riedel, Jens A1 - Beitz, T. A1 - Löhmannsröben, H.-G. T1 - IR-MALDI ion mobility spectrometry N2 - The novel combination of infrared matrix-assisted laser dispersion and inization (IR-MALDI) with ion mobility (IM) spectrometry makes it possible to investigate biomolecules in their natural environment, liquid water. As an alternative to an ESI source, the IR-MALDI source was implemented in an in-house-developed ion mobility (IM) spectrometer. The release of ions directly from an aqueous solution is based on a phase explosion, induced by the absorption of an IR laser pulse (λ = 2.94 μm, 6 ns pulse width), which disperses the liquid as nano- and micro-droplets. The prerequisites for the application of IR-MALDI-IM spectrometry as an analytical method are narrow analyte ion signal peaks for a high spectrometer resolution. This can only be achieved by improving the desolvation of ions. One way to full desolvation is to give the cluster ions sufficient time to desolvate. Two methods for achieving this are studied: the implementation of an additional drift tube, as in ESI-IM-spectrometry, and the delayed extraction of the ions. As a result of this optimization procedure, limits of detection between 5 nM and 2.5 μMas well as linear dynamic ranges of 2–3 orders of magnitude were obtained for a number of substances. The ability of this method to analyze simple mixtures is illustrated by the separation of two different surfactant mixtures. KW - Ion mobility KW - Spectrometry KW - IR-MALDI KW - Laser PY - 2016 DO - https://doi.org/10.1007/s00216-016-9739-x SN - 1618-2650 SN - 1618-2642 VL - 408 IS - 23 SP - 6259 EP - 6268 PB - Springer-Verlag CY - Heidelberg AN - OPUS4-37615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bach, S. A1 - Panthöfer, M. A1 - Bienert, Ralf A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska A1 - Tremel, W. T1 - Role of water during crystallization of amorphous cobalt phosphate nanoparticles N2 - The transformation of amorphous precursors into crystalline solids and the associated mechanisms are still poorly understood. We illuminate the formation and reactivity of an amorphous cobalt phosphate hydrate precursor and the role of water for its crystallization process. Amorphous cobalt phosphate hydrate nanoparticles (ACP) with diameters of ∼20 nm were prepared in the absence of additives from aqueous solutions at low concentrations and with short reaction times. To avoid the kinetically controlled transformation of metastable ACP into crystalline Co₃(PO₄)₂ × 8H₂O (CPO) its separation must be fast. The crystallinity of ACP could be controlled through the temperature during precipitation. A second amorphous phase (HT-ACP) containing less water and anhydrous Co₃(PO₄)₂ was formed at higher temperature by the release of coordinating water. ACP contains approximately five molecules of structural water per formula unit as determined by thermal analysis (TGA) and quantitative IR spectroscopy. The Co²+ coordination in ACP is tetrahedral, as shown by XANES/EXAFS spectroscopy, but octahedral in crystalline CPO. ACP is stable in the absence of water even at 500 °C. In the wet state, the transformation of ACP to CPO is triggered by the diffusion and incorporation of water into the structure. Quantitative in situ IR analysis allowed monitoring the crystallization kinetics of ACP in the presence of water. KW - Fluorapatite-gelatin nanocomposites KW - Calcium-carbonate KW - Zinc phosphate KW - Crystal-growth KW - Nucleation KW - Polymorphism PY - 2016 DO - https://doi.org/10.1021/acs.cgd.6b00208 SN - 1528-7483 SN - 1528-7505 VL - 16 IS - 8 SP - 4232 EP - 4239 PB - ACS Publications AN - OPUS4-37616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Bartusch, Jürgen A1 - Schadow, Florian A1 - Beck, Uwe A1 - Daschewski, M. A1 - Kreutzbruck, M. T1 - Airborne ultrasonic systems for one-sided inspection using thermoacoustic transmitters N2 - Airborne ultrasonic inspection is performed in through transmission, where the test piece (e.g. adhesive joint or polymer-based composite plate) is placed between the transmitter and the receiver. However, many structures with difficult shapes allow only one-sided inspection. The strong reflection of the signal from the surface overshadows the signals from the inside, so that broadband pulses are required. Thermoacoustic transmission, where the thermal energy of an electrically heated electrode is transformed into the acoustic energy of an ultrasonic wave, opens the possibility to excite broadband pulses and thus to inspect objects with one-sided access. We present various thermoacoustic transducers consisting of an electrically conductive film on a solid substrate. The first type of transducer is a transmitter with an indium-tin-oxide electrode on a glass substrate combined with a laser Doppler vibrometer as a receiver. The second type of transducer combines thermoacoustic transmission and piezoelectric reception, having a titanium electrode as a transmitter deposited onto charged cellular polypropylene serving as a piezoelectric receiver. Using a focusing thermoacoustic transmitter and a separate cellular polypropylene receiver, a through-transmission inspection of a 4 mm thick CFRP test piece with inserts as small as 1 mm was performed. The same emitter and a laser vibrometer as a receiver were used for a one-sided inspection of a Plexiglas block with a cross hole at 15 mm depth. A twin probe consisting of a thermoacoustic transmitter on a cellular polypropylene receiver was applied to a profile measurement on a step wedge with flat bottom holes. The smallest detected diameter of a flat bottom hole was 1 mm. Sound pressure level above 140dB was achieved with each of these transmitters. Thermoacoustic transmitters enable a step towards one-sided air-coupled ultrasonic inspection. T2 - IEEE International Ultrasonics Symposium CY - Tours, France DA - 18.09.2016 KW - Airborne KW - Air-coupled KW - Ultrasonic transducer KW - Thermoacoustic KW - Ferroelectret PY - 2016 SN - 978-1-4673-9897-8 SN - 1948-5719 SP - (online publication) 1 EP - 4 AN - OPUS4-37620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Airborne ultrasonic systems for one-sided inspection using thermoacoustic transmitters N2 - Airborne ultrasonic inspection is performed in through transmission, where the test piece (e.g. adhesive joint or polymer-based composite plate) is placed between the transmitter and the receiver. However, many structures with difficult shapes allow only one-sided inspection. The strong reflection of the signal from the surface overshadows the signals from the inside, so that broadband pulses are required. Thermoacoustic transmission, where the thermal energy of an electrically heated electrode is transformed into the acoustic energy of an ultrasonic wave, opens the possibility to excite broadband pulses and thus to inspect objects with one-sided access. We present various thermoacoustic transducers consisting of an electrically conductive film on a solid substrate. The first type of transducer is a transmitter with an indium-tin-oxide electrode on a glass substrate combined with a laser Doppler vibrometer as a receiver. The second type of transducer combines thermoacoustic transmission and piezoelectric reception, having a titanium electrode as a transmitter deposited onto charged cellular polypropylene serving as a piezoelectric receiver. Using a focusing thermoacoustic transmitter and a separate cellular polypropylene receiver, a through-transmission inspection of a 4 mm thick CFRP test piece with inserts as small as 1 mm was performed. The same emitter and a laser vibrometer as a receiver were used for a one-sided inspection of a Plexiglas block with a cross hole at 15 mm depth. A twin probe consisting of a thermoacoustic transmitter on a cellular polypropylene receiver was applied to a profile measurement on a step wedge with flat bottom holes. The smallest detected diameter of a flat bottom hole was 1 mm. Sound pressure level above 140dB was achieved with each of these transmitters. Thermoacoustic transmitters enable a step towards one-sided air-coupled ultrasonic inspection. T2 - IEEE International Ultrasonics Symposium CY - Tours, France DA - 18.9.2016 KW - Airborne KW - Air-coupled KW - Ferroelectret KW - Thermoacoustic KW - Ultrasonic transducer PY - 2016 AN - OPUS4-37621 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griepentrog, Michael T1 - Kratzbeständigkeit Prüfmethoden und deren Bewertung N2 - Der Vortrag widmet sich der Kratzbeständigkeit-Prüfmethoden und deren Bewertung und beschreibt Begriffe/Definitionen, Wirtschaftliche Bedeutung der Kratzbeständigkeit, Mess- und Prüfverfahren – allgemein (Anwendbarkeit, Messunsicherheit, Validierung), Mess- und Prüfverfahren – speziell die Erzeugung, Prüfverfahren von Einzel- und Vielfach-Kratzern, die Charakterisierung von Verkratzungen und eine zusammenfassende Bewertung im Einzelnen T2 - SKZ-Seminare für die Kunststoff-Branche: Modifikation der Kratz- und Abriebbeständigkeit CY - Peine, Germany DA - 19.04.2016 KW - Kratzfestigkeit KW - Haftfestigkeit KW - Ritztest KW - Instrumentierte Eindringprüfung KW - Normung PY - 2016 AN - OPUS4-37598 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Westphal, Anja T1 - Altbekannter Watts-Elektrolyt, junge Hightech-Anwendung: Ni- und NiFe-Schichten als magnetostriktive Aktorschicht auf faseroptischen Sensoren N2 - Durch den Einsatz von eingebetteten faseroptischen Sensoren können Bauteile überwacht und frühzeitig Informationen über Materialveränderungen gewonnen werden. Um die Zuverlässigkeit eines solchen Sensors gewährleisten zu können, ist es wichtig, die korrekte Funktion des Sensors im Verbund mit einer Werkstoff-Matrix on-line und in-situ überwachen zu können. Im Rahmen des DFG-Projekts FAMOS² (FAser-basierter Magneto-Optischer SchichtSensor) wurde ein selbstdiagnose-fähiger Schichtsensor entwickelt, welcher mit Hilfe einer magnetostriktiven Aktorschicht validiert werden kann. Durch eine Kombination aus PVD (physical vapour deposition) und ECD (electro-chemical deposition) wird die Aktorschicht auf faseroptischen Sensoren haftfest abgeschieden. Ein äußeres Magnetfeldes dehnt die Aktorschicht und damit auch die Faser reversibel. Diese Dehnung führt zu einer Verschiebung der Bragg-Wellenlänge, welche direkt mit der Stärke des zu messenden Magnetfeldes korreliert. Ein etwa 100 Nanometer dünnes PVD-Schichtsystem aus Chrom und Kupfer dient zunächst als Haftvermittler zwischen Glasfaser und ECD-Schicht. Um eine rotationssymmetrische Schichtabscheidung zu erhalten, erfolgt während der PVD-Beschichtung eine Rotation der Faser. In einem klassischen Watts-Elektrolyten wird dann im zweiten Schritt die eigentliche etwa 30 Mikrometer dicke ECD-Aktorschicht auf die PVD-Schicht abgeschieden. Reine Ni-Schichten werden mit NiFe-Legierungen verglichen. Die Geometrie der Faser stellt für die Herstellung und Charakterisierung der Schichten auf der einen Seite eine besondere Herausforderung dar, bietet aber zugleich auch neue experimentelle Möglichkeiten. So kann ggf. die Entstehung von Spannungen in der Schicht während der ECD-Abscheidung in-situ verfolgt werden, indem die Wellenlängenverschiebung aufgrund der Dehnung des Bragg-Gitters optisch gemessen wird. Die Anpassung der Beschichtungsverfahren an die Fasergeometrie sowie die Charakterisierung und die Eigenschaften der ECD-Schicht werden diskutiert. Insbesondere wird auf den Elastizitätsmodul der Aktorschicht eingegangen, wobei Werte aus der Nanoindentation und dem 2-Punkt-Biegeversuch mit der beschichteten Faser als Biegebalken verglichen werden. T2 - ZVO-Oberflächentage CY - Garmisch-Partenkirchen, Germany DA - 21.09.2016 KW - Selbstdiagnosefähiger FBG-Sensor KW - ECD/PVD-Kombinations-Schichtsystem KW - Magnetostriktive Ni- und NiFe-Schicht KW - Nanoindentation KW - 2-Punkt-Biegeversuch PY - 2016 AN - OPUS4-37505 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Lateral resolution delivered by imaging surface-analytical instruments as SIMS, AES and XPS: Application of the BAM-L200 Certified Reference Material and related ISO Standards N2 - The certified reference material BAM-L200, a nanoscale stripe pattern for length calibration and specification of lateral resolution, is described. BAM-L200 is prepared from a cross-sectioned epitaxially grown layer stack of AlxGa1-xAs and InxGa1-xAs on a GaAs substrate. The surface of BAM-L200 provides a flat pattern with stripe widths ranging down to 1 nm. Calibration distances, grating periods and stripe widths have been certified by TEM with traceability to the length unit. The combination of gratings, isolated narrow stripes and sharp edges of wide stripes offers a plenty of options for the determination of lateral resolution, sharpness and calibration of length scale at selected settings of imaging surface analytical instruments. The feasibility of the reference material for an analysis of the lateral resolution is demonstrated in detail by evaluation of ToF-SIMS, AES and EDX images. Other applications developed in the community are summarized, too. BAM-L200 fully supports the implementation of the revised International Standard ISO 18516 (in preparation) which is based on knowledge outlined in the Technical Report ISO/TR 19319:2013. Fundamental approaches to determination of lateral resolution and sharpness in beam-based methods T2 - SIMS Europe 2016 CY - Münster, Germany DA - 18.09.2016 KW - ISO standards KW - XPS KW - AES KW - SIMS KW - Lateral resolution PY - 2016 AN - OPUS4-37507 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane A1 - Rothbart, Nick A1 - Goldammer, M. A1 - Hohlstein, F. A1 - Koch, J. A1 - Kryukov, I. A1 - Mahler, G. A1 - Stotter, B. A1 - Walle, G. A1 - Oswald-Tranta, B. A1 - Sengebusch, M. T1 - A round robin test of flash thermography – detectability and quantification of artificial and natural defects in CFRP and metal structures N2 - Within the scope of a DIN INS project, a flash thermography round robin test that evaluates reliability, comparability, and efficiency of different testing situations was organized. The results give information about the detectability of defects, e.g. depending on their size and depth, the evaluation methods and the materials used. Besides, the influences of equipment and parameters used by the participants on the results were analysed. All of the quantitative results as well as the feedback given by the participants will be presented in a DIN committee in order to contribute to a flash thermography standard. T2 - Conference QIRT 2016 CY - Gdansk, Poland DA - 04.07.2016 KW - Active thermography KW - Flash excitation KW - Round robin test KW - CFRP KW - Metal PY - 2016 UR - http://qirt.gel.ulaval.ca/archives/qirt2016/papers/075.pdf DO - https://doi.org/10.21611/qirt.2016.075 SN - 2371-4085 SP - Paper 075, 517 EP - 526 CY - Quebec, Canada AN - OPUS4-37510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grauel, Bettina T1 - Nd-sensitized tri-doped UCNP systems N2 - This presentation gives a short overview of the PhD student's research topics and interests, within the scope of the 2016 UPCON Spring School. T2 - UPCON 2016 Spring School CY - Breslau, Poland DA - 25.05.2016 KW - UCNP KW - Nd-sensitizer PY - 2016 AN - OPUS4-37223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grauel, Bettina T1 - Nd as sensitizer in NaYF4:Yb,Er,Nd tri-doped upconversion nanocrystals N2 - In recent years, upconversion nanocrystals (UCNC) have shown great promise for biological and medical applications, mainly because of their excitation in the NIR region, which provides minimum fluorescence background and a rather deep penetration into biological samples, as opposed to excitation in the visible or UV region. Moreover, they show a multitude of characteristic narrow emission bands as basis for ratiometric measurements. Commonly, Yb is the sensitizer of choice, because of a comparatively high absorption cross section, simple energy scheme, and rather efficient energy transfer to the activator, mostly Er, Tm or Ho. A main disadvantage of the use of Yb as sensitizer for biological and medical applications is its absorption band at 976 nm and hence the use of an excitation wavelength at which water has a non-negligible absorption. This can lead to significant sample heating, especially at long illumination times or high excitation power densities, and thus, tissue damage or even cell death. A possible solution is the tri-doping of UCNC with Nd as sensitizer, which can be excited efficiently at around 800 nm, where water absorption is at minimum. The use of Nd as a sensitizer and Yb as a bridge between Nd and the activator Er in NaYF₄ nanocrystals is a relatively new way to overcome the problems of heating of samples in an aqueous environment. Disadvantages can arise from the tri-doping, which can favor non-radiative relaxation due to the more complicated excitation process compared to e.g., simple Yb,Er-doped UCNC, which might lower the upconversion quantum yields in these tri-doped systems. In order to quantify clear advantages, NaYF₄:Yb,Er,Nd nanoparticles were synthesized and spectroscopically studied using an 8 W 804 nm laser diode and a custom-designed Edinburgh instruments FSP980 spectrometer. Wavelength-dependent studies of the emission intensities and the decay kinetics of these tri-doped UCNC at different excitation power densities and excitation pulse widths revealed the clear advantages of preventing water absorption on measurable luminescence signals. We were able to show the influence of pulse width and excitation power density on the luminescence intensities and decay kinetics lifetimes at different emission wavelengths. Additionally, we can clearly discern power density-dependent and independent peaks in the emission spectra. In summary, we demonstrate that the tri-doping of NaYF₄:Yb,Er,Nd nanoparticles is a very promising approach to render UCNC more efficient and to make them better suitable for biological and medical applications requiring measurements in aqueous environment. T2 - UPCON 2016 Conference CY - Breslau, Poland DA - 23.05.2016 KW - UCNP KW - Nd-sensitizer KW - excitation power density PY - 2016 AN - OPUS4-37224 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Frenzel, Florian T1 - Spectroscopic study of plasmon enhanced upconversion nanoparticles N2 - The presentation gave an overview of the topic, the aims and the task allocation of the M-ERA.NET founded project named “Nanohype”. In this project four research teams working hand in hand on computational modeling, synthesis and experimental validation to design novel metal-shelled Upconversion-NP combining plasmonic interactions. As Ph.D. student at the BAM I am responsible for the optical characterization (measurements of lifetimes, Quantum Yields and PL emissions ) of these promising novel systems. T2 - SpringSchool, UpCon2016 CY - Wrocław (Breslau), Polen DA - 25.05.2016 KW - Field Enhancement KW - Upconversion KW - Core-Shell KW - FRET KW - Plasmonic PY - 2016 AN - OPUS4-37225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stockmann, Jörg M. T1 - Visualization of low-contrast surface modifications: thin films, printed pattern, laser-induced changes, imperfections, impurities, and degradation N2 - Industrial quality control (QC) nowadays requires the visualization of surface modifications from the macro-scopic to the microscopic or even nanoscopic scale. This is a prerequisite to the evaluation of functionality and reliability, the detection of defects and their separation of artefacts. The diversity of applications ranges from low-E glazings and solar panels, micro- and optoelectronics, micro- and smart devices to sensor-on-chip and lab-on-chip systems [1]. Optical microcopy (light, confocal laser scanning, white light interference) as established QC-tool is operated at normal incidence, i.e. p- and s-polarization are undistinguishable. Either light-intensity in terms of grey scale and colour or intensity-correlated effects of phase shifts are used. In case of ellipsometry, operated at oblique incidence, p- and s-polarization matter, and amplitude ratios and phase shifts upon reflection are measured. Hence, information content must be much higher. The visualization of surface modifications may be very challenging for coating/substrate systems of either al-most identical optical constants, e.g. transparent films on substrates of the same material, or minor film thick-ness, substance quantity and affected area, e.g. ultra-thin or island films. Ellipsometry gives access to the con-trast of intensity (I), amplitude ratio (Ψ), and phase shift (Δ) with nanometer-scaled vertical and micrometer-scaled lateral sensitivity, one is able to identify tiny changes within an unmodified surface. As both mapping ellipsometry (ME) and imaging ellipsometry (IE) are operated in the optical far-field, surface inspection is also possible on the macroscopic scale. Near the Brewster-angle of the bare, undamaged, clean, and fresh substrate, the contrast to add-on and sub-off features is superior. Fig. 1 shows three examples of ellipsometric imaging, i.e. a thin SnO:Ni film on SiO2/Si (Fig. 1a), a dried stain of an anti-body solution on cyclo-olefin-polymer (COP) shown in Fig. 1b, and a polyimide film residue on SiO2/Si (Fig. 1c). For all of these examples, ellipsometry provides much better contrast between substrate and surface modification than optical microscopy, sometimes primarily caused by the oblique incidence (Figs. 1a and 1c), in other cases related to the phase sensitivity of ellipsometry (Fig. 1b). Other examples are laser surface modifications and the corrosion of glass. In these cases, optical microscopy and IE yield to similar results, how-ever only ellipsometry gives access to modelling. Further investigated coating/substrate systems are 100Cr6 steel, native oxide on silicon, borosilicate glass, and the polymer polycarbonate with deposited films of graphene and ta-C:H, printed and dried pattern of liquids such as water, cleaning agents, and dissolved silicone. Besides imaging ellipsometry, referenced spectral ellipsometry (RSE) has been applied, combining the advantages of both optical microscopy (fast measurement) and ellipsometry (high sensitivity to tiny modifications). T2 - International Conference on Spectroscopic Ellipsometry (ICSE-7) CY - Berlin, Germany DA - 06.06.2016 KW - Ellipsometry KW - Thin films KW - Impurities KW - Degradation PY - 2016 AN - OPUS4-37068 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Standardization of fluorescence measurements: Design, development, validation, and fabrication of format-adaptable fluorescence standards for intensity, spectral, and temporal quantities N2 - Photoluminescence techniques are amongst the most widely used tools in the material and life sciences, with new and exciting applications continuously emerging, due to their many advantages like comparative ease of use, unique sensitivity, non-invasive character, and potential for multiplexing, remote sensing, and miniaturization. Drawbacks are , however, signals, that contain unwanted wavelength- and polarization contributions from instrument-dependent effects, which are time-dependent due to the aging of instrument components, and difficulties to measure absolute fluorescence intensities. Thus, there is a considerable need for standards for intensity, spectral, and temporal fluorescence quantities to meet the increasing need for instrument performance validation and global trends to harmonize physicochemical measurements. In this respect, instrument calibration strategies together with different types of fluorescence standards are presented as well as design concepts for robust, easy-to-use, and format-adaptable fluorescence standards useable for the determination of different fluorescence parameters and a broad variety of fluorescence techniques. T2 - SALSA-Kolloquien CY - Berlin, Germany DA - 07.06.2016 KW - Fluorescence KW - Standard KW - Quality assurance KW - Spectral correction KW - Quantum yield PY - 2016 AN - OPUS4-37070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Siegel, G. A1 - Mockenhaupt, F.H.M.E. A1 - Behnke, A.-L. A1 - Ermilov, Eugeny A1 - Winkler, K. A1 - Pries, A.R. A1 - Malmsten, M. A1 - Hetzer, R. A1 - Saunders, R. A1 - Lindman, B. T1 - Lipoprotein binding to anionic biopolyelectrolytes and the effect of glucose on nanoplaque formation in arteriosclerosis and Alzheimer's disease N2 - Arteriosclerosis with its clinical sequelae (cardiac infarction, stroke, peripheral arterial occlusive disease) and vascular/Alzheimer dementia not only result in far more than half of all deaths but also represent dramatic economic problems. The reason is, among others, that diabetes mellitus is an independent risk factor for both disorders, and the number of diabetics strongly increases worldwide. More than one-half of infants in the first 6 months of life have already small collections of macrophages and macrophages filled with lipid droplets in susceptible segments of the coronary arteries. On the other hand, the authors of the Bogalusa Heart Study found a strong increase in the prevalence of obesity in childhood that is paralleled by an increase in blood pressure, blood lipid concentration, and type 2 Diabetes mellitus. Thus, there is a clear linkage between arteriosclerosis/Alzheimer's disease on the one hand and diabetes mellitus on the other hand. Furthermore, it has been demonstrated that distinct apoE isoforms on the blood lipids further both arteriosclerotic and Alzheimer nanoplaque formation and therefore impair flow-mediated vascular reactivity as well. Nanoplaque build-up seems to be the starting point for arteriosclerosis and Alzheimer's disease in their later full clinical manifestation. In earlier work, we could portray the anionic biopolyelectrolytes syndecan/perlecan as blood flow sensors and lipoprotein receptors in cell membrane and vascular matrix. We described extensively molecular composition, conformation, form and function of the macromolecule heparan sulfate proteoglycan (HS-PG). In two supplementary experimental settings (ellipsometry, myography),we utilized isolated HS-PG for in vitro nanoplaque investigations and isolated human coronary artery segments for in vivo tension measurements. With the ellipsometry-based approach, we were successful in establishing a direct connection on a molecular level between diabetes mellitus on the one side and arteriosclerosis/Alzheimer's disease on the other side. Application of glucose at a concentration representative for diabetics and leading to glycation of proteins and lipids, entailed a significant increase in arteriosclerotic and Alzheimer nanoplaque formation. IDLapoE4/E4 was by far superior to IDLapoE3/E3 in Plaque build-up, both in diabetic and non-diabetic patients. Recording vascular tension of flow-dependent reactivity in blood substitute solution and under application of different IDLapoE isoforms showed an impaired vasorelaxation for pooled IDL and IDLapoE4/E4, thus confirming the ellipsometric investigations. Incubation in IDLapoE0/E0 (apoE “knockout man”), however, resulted in a massive flowmediated contraction, also complemented by strongly aggregated nanoplaques. In contrast, HDL was shown to present a powerful protection against nanoplaque formation on principle, both in the in vitro model and the in vivo scenario on the endothelial cell membrane. The competitive interplay with LDL is highlighted through the flow experiment, where flow-mediated, HDL-induced vasodilatation remains untouched by additional incubation with LDL. This is due to the four times higher affinity for the proteoglycan receptor of HDL as compared to LDL. Taken together, the studies demonstrate that while simplistic, the ellipsometry approach and the endothelialmimicking proteoglycan-modified surfaces provide information on the initial steps of lipoprotein-related Plaque formation, which correlates with findings on endothelial cells and blood vessels, and afford insight into the role of lipoprotein deposition and Exchange phenomena at the onset of these pathophysiologies. KW - Diabetes mellitus and Alzheimer's disease KW - HS-PG flow sensor and lipoprotein receptor KW - Glucose and nanoplaque formation KW - IDLapoE3/E3 and IDLapoE4/E4 isoforms KW - HDL protection KW - β-amyloid (1–42) PY - 2016 DO - https://doi.org/10.1016/j.cis.2016.02.001 SN - 0001-8686 VL - 232 SP - 25 EP - 35 AN - OPUS4-37078 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hollamby, M. J. A1 - Aratsu, K. A1 - Pauw, Brian Richard A1 - Rogers, S. E. A1 - Smith, A. J. A1 - Yamauchi, M. A1 - Lin, X. A1 - Yagai, S. T1 - Simultaneous SAXS and SANS Analysis for the Detection of Toroidal Supramolecular Polymers Composed of Noncovalent Supermacrocycles in Solution N2 - Molecular self-assembly primarily occurs in solution. To better understand this process, techniques capable of probing the solvated state are consequently required. Smallangle scattering (SAS) has a proven ability to detect and characterize solutions, but it is rarely applied to more complex assembly shapes. Here, small-angle X-ray and neutron scattering are applied to observe toroidal assemblies in solution. Combined analysis confirms that the toroids have a core–shell structure, with a p-conjugated core and an alkyl shell into which solvent penetrates. The dimensions determined by SAS agree well with those obtained by (dried-state) atomic force microscopy. Increasing the number of naphthalene units in the molecular building block yields greater rigidity, as evidenced by a larger toroid and a reduction in solvent penetration into the shell. The detailed structural analysis demonstrates the applicability of SAS to monitor complex solution-based selfassembly. KW - Nanorings KW - Self-assembly KW - Small-angle scattering KW - Supramolecular chemistry KW - Toroids PY - 2016 DO - https://doi.org/10.1002/anie.201603370 SN - 1433-7851 SN - 1521-3773 IS - 128 SP - 10044 EP - 10047 PB - Wiley-VCH Verlag GmbH CY - Weinheim AN - OPUS4-37144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - ICP-MS with Sector Field Devices N2 - This lecture is an introduction to ICP-MS with a double focusing magnetic sector mass analyzer. It offers fundamental background, a thorough discussion of analytical features, and state of the art information on applications. Different types of double focusing instruments also are considered. Specific topics include fundamental aspects of ICP-MS (physical properties of a double focusing instrument, operational characteristics in comparison with quadrupole instruments); analytical characteristics (spectral and non-spectral interferences, figures of merit in low and high resolution modes, blanks and memory effects, HPLC and GC interfaces), and applications (industrial including ultra-pure reagents and alloys, environmental, geological, and biomedical materials). T2 - Winter Conference on Plasma Spectrochemistry CY - Tucson, Arizona, USA DA - 10.01.2016 KW - High-resolution ICP-MS KW - Figures of merit KW - Interfaces KW - Applications KW - Ultra-trace analysis PY - 2016 AN - OPUS4-37148 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weller, Andreas T1 - Induced polarization and pore radius - a discussion N2 - Permeability estimation from spectral induced polarization (SIP) measurements is based on a fundamental premise that the characteristic relaxation time (t) is related to the effective hydraulic radius (reff) controlling fluid flow. The approach requires a reliable estimate of the diffusion coefficient of the ions in the electrical double layer. Others have assumed a value for the diffusion coefficient, or postulated different values for clay versus clay-free rocks. We examine the link between t and reff for an extensive database of sandstone sampleswhere mercury porosimetry data confirm that reff is reliably determined from a modification of the Hagen-Poiseuille equation assuming that the electrical tortuosity is equal to the hydraulic tortuosity. Our database does not support the existence of 1 or 2 distinct representative diffusion coefficients but instead demonstrates strong evidence for 6 orders of magnitude of variation in an apparent diffusion coefficient that is well correlated with both reff and the specific surface area per unit pore volume (Spor). Two scenarios can explain our findings: (1) the length-scale defined by t is not equal to reff and is likely much longer due to the control of pore surface roughness; (2) the range of diffusion coefficients is large and likely determined by the relative proportions of the different minerals (e.g. silica, clays) making up the rock. In either case, the estimation of reff (and hence permeability) is inherently uncertain from SIP relaxation time. T2 - IP Workshop 2016 CY - Aarhus, Denmark DA - 06.06.2016 KW - pore radius KW - mercury intrusion capillary pressure KW - spectral induced polarization KW - relaxation time PY - 2016 AN - OPUS4-37116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H. R. A1 - Weidner, Steffen T1 - Dispersities of Polyesters of Various Diphenols Prepared by Irreversible Polycondensations N2 - Polyesters of bisphenol-A, bisphenol-P, catechol, and sebacic acid are prepared and different synthetic methods are compared. The diphenols are condensed with sebacoyl chloride either in dichloromethane/pyridine or in refl uxing chlorobenzene without HCl-acceptor. Further- more, bisphenol-A acetate is polycondensed with sebacic acid in bulk. All experiments are worked up so that fractionation is avoided. The extent of cyclization is estimated by matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS) and the molar mass distribution by size exclusion chromatography (SEC). Polycondensations in solution yield larger fractions of cyclics and higher dispersities (up to 11). Polycondensations in bulk give lower fractions of cycles and dispersities from 4.6 to 6.3 for high molar mass polyesters or 2.8 to 3.5 for low molar mass products. Characteristic curves describing the dependence of the dispersity on the initial monomer concentration are elaborated. KW - cyclization KW - dispersity KW - mass spectra KW - polycondensation KW - polyesters PY - 2016 DO - https://doi.org/10.1002/macp.201600004 IS - 217 SP - 1361 EP - 1369 PB - Wiley-VCH Verlag CY - Weinheim AN - OPUS4-37120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kage, Daniel T1 - Lifetime-encoded microparticles - application to flow cytometry N2 - Analytical methods require efficient and versatile strategies to measure an increasing number of analytes that can be used in conjunction with established platforms like flow cytometry. Spectral multiplexing suffers from problems such as spectral crosstalk and often requires different excitation light sources increasing instrumentation costs. Thus, the number of distinguishable reporters with intensity-based barcodes is limited. An alternative can be lifetime encoding for discrimination of fluorophores based on their fluorescence decay kinetics. We report on the suitability of µm-sized polymer particles stained with organic dyes for lifetime encoding. These dyes are excitable at a standard laser diode wavelength and detectable within a single spectral window. For lifetime-based discrimination, these dyes display sufficiently different luminescence decay kinetics. We present the spectroscopic properties of these beads and address challenges like the limited number of detectable photons in a flow for the reliable discrimination. These studies are expected to pave the road to new applications of fluorescence lifetime multiplexing for time-domain flow cytometry. T2 - DPG Spring Meeting 2016 CY - Regensburg, Germany DA - 06.03.2016 KW - flow cytometry KW - lifetime encoding KW - life sciences KW - fluorescence KW - polymer particles PY - 2016 AN - OPUS4-37153 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hsiao, I.-L. A1 - Bierkandt, Frank A1 - Reichardt, Ph. A1 - Luch, A. A1 - Huang, Y.-J. A1 - Jakubowski, Norbert A1 - Tentschert, J. A1 - Haase, A. T1 - Quantification and visualization of cellular uptake of TiO2 and Ag nanoparticles: comparison of different ICP-MS techniques N2 - Safety assessment of nanoparticles (NPs) requires techniques that are suitable to quantify tissue and cellular uptake of NPs. The most commonly applied techniques for this purpose are based on inductively coupled plasma mass spectrometry (ICP-MS). Here we apply and compare three different ICP-MS methods to investigate the cellular uptake of TiO2 (diameter 7 or 20 nm, respectively) and Ag (diameter 50 or 75 nm, respectively) NPs into differentiated mouse neuroblastoma cells (Neuro-2a cells). Cells were incubated with different amounts of the NPs. Thereafter they were either directly analyzed by laser ablation ICP-MS (LA-ICP-MS) or were lysed and lysates were analyzed by ICP-MS and by single particle ICP-MS (SP-ICP-MS). KW - Nanoparticles KW - Single particle ICP-MS KW - Laser ablation ICP-MS KW - Cellular internalization KW - Neurons PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-371620 DO - https://doi.org/10.1186/s12951-016-0203-z SN - 1477-3155 VL - 14 SP - Article 50 AN - OPUS4-37162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mielke, Johannes A1 - Martınez-Blanco, J. A1 - Peters, M. V. A1 - Hecht, S. A1 - Grill, L. T1 - Observing single-atom diffusion at a molecule-metal interface N2 - The dynamics at the interface between a close-packed porphyrin monolayer and Au(111) is investigated by time-dependent scanning tunneling microscopy, detecting the motion of single-interface adatoms in real space. Imaging sequences reveal predominant switching of the molecular appearance in adjacent molecules, pointing to a spatial correlation that is consistent with adatom diffusion from one molecule to the next. In some cases, the number of switching molecules is drastically increased, indicating collective switching events. In addition to the thermally induced motion of adatoms at the interface, also voltage pulses from the microscope tip can induce the process—revealing different yields in agreement with the model of adatom hopping. KW - STM KW - molecular switch KW - single molecule KW - switching dynamics KW - porphyrin KW - Au(111) PY - 2016 UR - http://journals.aps.org/prb/abstract/10.1103/PhysRevB.94.035416 DO - https://doi.org/10.1103/PhysRevB.94.035416 VL - 94 IS - 3 SP - 035416-1 EP - 035416-7 PB - American Physical Society AN - OPUS4-37177 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppe, Enrico A1 - Bartholmai, Matthias A1 - Daum, Werner A1 - Gong, Xing A1 - Hofmann, Detlef A1 - Basedau, Frank A1 - Schukar, Vivien A1 - Westphal, Anja A1 - Sahre, Mario A1 - Beck, Uwe T1 - New self - diagnostic fiber optical sensor technique for structural health monitoring N2 - Fiber optic sensors have gained increasing importance in recent years and are well established in many areas of industrial applications. In this paper, we introduce a concept of a self-diagnostic fiber optic sensor. The presented sensor is to resolve the problems of embedded fiber optic sensors in complex structures and to enable the validation under operational conditions. For this purpose, different magnetostrictive coated fiber optic sensors were developed and various experiments were performed to verify their mode of Operation and to determine the respective reproducibility. The measuring principle is illustrated by obtained experimental results, which showed a change in wavelength from 1 pm at a magnetic field strength change of 0.25 mT. In addition, the temperature characteristics of the implemented magnetostrictive sensor were analyzed and an experimental factor of 1.5 compared to a reference fiber optic sensor was determined. T2 - 32nd DANUBIA ADRIA SYMPOSIUM on Advances in Experimental Mechanics CY - Starý Smokovec, Slovakia DA - 22.09.2015 KW - Self-diagnostic fiber optical sensor KW - Magnetostrictive metal coating KW - Magnetic field KW - Fiber bragg grating PY - 2016 DO - https://doi.org/10.1016/j.matpr.2016.03.038 SN - 2214-7853 VL - 3 IS - 4 SP - 1009 EP - 1013 AN - OPUS4-37131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altenburg, Simon A1 - Krankenhagen, Rainer A1 - Weber, H. T1 - Thickness determination of semitransparent isolated solids using the flash method and an analytical model N2 - As groundwork for thickness determination of polymeric surface protection systems for concrete, we present a method for measuring the thickness of isolated semitransparent solids using pulse thermography both in Transmission and reflection geometry. Since standard models do not capture semitransparency, an advanced analytical model by Salazar et al. is applied. Physical material parameters are deduced by fitting experimental data from samples of well-known thickness. Using those, the thickness of samples of the material can be obtained by fitting, as demonstrated for different semitransparent polymer materials. T2 - QIRT 2016 CY - Gdańsk, Poland DA - 04.07.2016 KW - Analytical model KW - Concrete KW - Flash thermography KW - Semitransparency KW - Surface protection KW - Thermography KW - Thickness PY - 2016 DO - https://doi.org/10.21611/qirt.2016.001 SN - 2371-4085 VL - 2016 SP - 71 EP - 78 AN - OPUS4-37200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhiem, S. A1 - Barthel, Anne-Kathrin A1 - Meyer-Plath, A. A1 - Hennig, M. P. A1 - Wachtendorf, Volker A1 - Sturm, Heinz A1 - Schäffer, A. A1 - Maes, H. M. T1 - Release of 14C-labelled carbon nanotubes from polycarbonate composites N2 - Waste disposal of carbon nanotube (CNT) containing products is expected to be the most important pathway for release of CNTs into the environment. In the present work, the use of radiolabelled CNTs (14C-CNT) for polycarbonate polymer nanocomposites with 1 wt% 14C-CNT content allowed for the first time to quantify and differentiate the CNT release according to the type of impact along the materials' ageing history. After an initial exposure of the nanocomposite by solar-like irradiation, further environmental impacts were applied to composite material. They aimed at mimicking disposal site conditions that may induce further ageing effects and CNT release. This study included shaking in water, rapid temperature changes, soaking in humic acid solution as well as waste water effluent, and, finally, gentle mechanical abrasion. All ageing impacts were applied sequentially, both on pristine (control) and on solar-irradiated nanocomposites. All experiments were accompanied by absolute quantification of radioactive release as well as chemical and morphological analyses of the nanocomposite surfaces using infra-red (IR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The morphological analysis showed that spectral irradiation can uncover CNT networks on the outer nanocomposite surface layers by polymer degradation. After having subjected the solar-irradiated nanocomposite to all studied disposal site effect, the total radioactive release was quantified to amount to 64 mg CNT/m2, whereas only 0.8 mg CNT/m2 were found for the un-irradiated control sample. Solar degradation of polymers was thus found to significantly increase the propensity of the studied polymer nanocomposites to release CNTs during ageing effects at the product's end-of-life typical for disposal sites. KW - Weathering KW - Carbon nanotubes KW - Nanocomposites KW - Release KW - Quantification PY - 2016 UR - http://www.sciencedirect.com/science/article/pii/S0269749116303748 DO - https://doi.org/10.1016/j.envpol.2016.04.098 SN - 0269-7491 VL - 215 IS - August SP - 356 EP - 365 PB - Elsevier Ltd. CY - Paris AN - OPUS4-36899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel T1 - Reference block design for high resolution ultrasound immersion tank N2 - In respect of modern approaches in material sciences and highly increased requirements on materials on safety relevant components, quality management and non-destructive testing reclaims a steadily increased meaning. The destructive meaning of measuring the degree of purity is defined in DIN EN 10247 through metallurgical investigations, especially microsections. For and comparable, but non-destructive testing due ultrasonic testing, the material the SEP 1927 is a well-defined industry standard. A novel and alternative way of reference block construction was focused by this work. The proposed amendments, regarding the manufactoring and machining, are less time and cost consuming. Verified by measurements the presented reference block fits the same acoustical characteristics and the requirements of the guideline. T2 - World Conference on Non-Destructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Immersion tank testing KW - SEP 1927 KW - Degree of purity KW - High resolution ultrasonic testing PY - 2016 AN - OPUS4-36850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotschate, Daniel A1 - Gohlke, Dirk A1 - Eisentraut, Mark T1 - Reference block design for high resolution ultrasound immersion tank N2 - In respect of modern approaches in material sciences and highly increased requirements on materials on safety relevant components, quality management and non-destructive testing reclaims a steadily increased meaning. The destructive meaning of measuring the degree of purity is defined in DIN EN 10247 through metallurgical investigations, especially microsections. For and comparable, but non-destructive testing due ultrasonic testing, the material the SEP 1927 is a well-defined industry standard. A novel and alternative way of reference block construction was focused by this work. The proposed amendments, regarding the manufacturing and machining, are less time and cost consuming. Verified by measurements the presented reference block fits the same acoustical characteristics and the requirements of the guideline. T2 - 19th World Conference on Non-Destructive Testing CY - Munich, Germany DA - 13.06.2016 KW - SEP 1927 KW - Degree of purity KW - High resolution ultrasonic testing KW - Immersion tank testing PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-368512 VL - 2016 SP - Paper X15, 1 EP - 4 AN - OPUS4-36851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, J.-Y. A1 - Hou, X.-N. A1 - Tian, Y. A1 - Jiang, L. A1 - Deng, S. A1 - Röder, B. A1 - Ermilov, Eugeny T1 - Photoinduced energy and charge transfer in a bis(triphenylamine)-BODIPY-C60 artificial photosynthetic system N2 - Triphenylamines (TPAs), boron dipyrromethenes (BODIPYs) and fullerenes C60 are excellent building blocks for the design of artificial photosynthetic systems. In the present work, we report the synthesis, characterization and detailed photophysical studies of a novel (TPA)2–BODIPY–C60 tetrad in polar and nonpolar solvents. The absorption spectrum of this compound covered virtually the entire visible Region (350–700 nm) and could be interpreted as a superposition of the spectra of individual components. Upon TPA-part excitation, a fast and very efficient excitation energy transfer (EET) delivers the excitation to the BODIPY moiety resulting in complete quenching of the TPA first excited singlet state as well as the appearance of the BODIPY fluorescence. The efficiency of EET process was estimated to be 1. Direct or indirect (via EET) excitation of the BODIPY-part of the tetrad is followed by photoinduced charge transfer to the charge-separated state BODIPY+–C60- irrespective of the solvent used. In polar N,N-dimethylformamide (DMF)charge recombination occurs directly to the ground state with the Charge recombination rate, kCR, slower than 108 s-1, whereas in nonpolar toluene (TOL) a small energy gap between the charge-separated state and first excited singlet state of the BODIPY moiety facilitates the back charge transfer process. The latter results in the appearance of thermally activated delayed fluorescence. The rate of charge separation was found to be ca. 2 times faster in TOL than in DMF. KW - Charge transfer KW - Energy transfer KW - Artificial photosynthesis KW - BODIPY KW - TPA KW - Fullerene C60 PY - 2016 DO - https://doi.org/10.1039/c6ra06841c SN - 2046-2069 VL - 6 IS - 62 SP - 57293 EP - 57305 AN - OPUS4-37080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Emmerling, Franziska T1 - Time- & spatial-resolved X-ray absorption fine structure (XAFS) spectroscopy in a single-shot – new analytical possibilities for in situ material characterization N2 - A new concept that comprises both time- and lateral-resolved X-ray absorption fine-structure information simultaneously in a single shot is presented. This uncomplicated set-up was tested at the BAMline at BESSY-II (Berlin, Germany). The primary broadband beam was generated by a double multilayer monochromator. The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by either an energy-sensitive area detector, the so-called color X-ray camera, or by an area-sensitive detector based on a CCD camera, in θ-2θ geometry. The first tests were performed with thin metal foils and some iron oxide mixtures. A time resolution of lower than 1 s together with a spatial resolution in one dimension of at least 50 µm is achieved. KW - Time resolution KW - Single-shot XAFS PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370892 DO - https://doi.org/10.1107/S1600577516003969 SN - 1600-5775 IS - 23 SP - 769 EP - 776 PB - International Union of Crystallography CY - Chester, UK AN - OPUS4-37089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Mieller, Björn A1 - Noordmann, J. A1 - Rienitz, O. A1 - Malinovskiy, D. T1 - Characterization of a series of absolute isotope reference materials for magnesium: ab initio calibration of the mass spectrometers, and determination of isotopic compositions and relative atomic weights N2 - For the first time, an ab initio calibration for absolute Mg isotope ratios was carried out, without making any a priori assumptions. All quantities influencing the calibration such as the purity of the enriched isotopes or liquid and solid densities were carefully analysed and their associated uncertainties were considered. A second unique aspect was the preparation of three sets of calibration solutions, which were applied to calibrate three multicollector ICPMS instruments by quantifying the correction factors for instrumental mass discrimination. Those fully calibrated mass spectrometers were then used to determine the absolute Mg isotope ratios in three candidate European Reference Materials (ERM)-AE143, -AE144 and -AE145, with ERM-AE143 becoming the new primary isotopic reference material for absolute isotope ratio and delta measurements. The isotope amount ratios of ERM-AE143 are n(25Mg)/n(24Mg) = 0.126590(20) mol/mol and n(26Mg)/n(24Mg) = 0.139362(43) mol/mol, with the resulting isotope amount fractions of x(24Mg) = 0.789920(46) mol/mol, x(25Mg) = 0.099996(14) mol/ mol and x(26Mg) = 0.110085(28) mol/mol and an atomic weight of Ar(Mg) = 24.305017(73); all uncertainties were stated for k = 2. This isotopic composition is identical within uncertainties to those stated on the NIST SRM 980 certificate. The candidate materials ERM-AE144 and -AE145 are isotopically lighter than ERM-AE143 by 1.6 ‰ and 1.3 ‰, respectively, concerning their n(26Mg)/n(24Mg) ratio. The relative combined standard uncertainties are ≤0.1 ‰ for the isotope ratio n(25Mg)/n(24Mg) and ≤0.15 ‰ for the isotope ratio n(26Mg)/ n(24Mg). In addition to characterizing the new isotopic reference materials, it was demonstrated that commonly used fractionation laws are invalid for correcting Mg isotope ratios in multicollector ICPMS as they result in a bias which is not covered by its associated uncertainty. Depending on their type, fractionation laws create a bias up to several per mil, with the exponential law showing the smallest bias between 0.1 ‰ and 0.7 ‰. KW - isotope reference material KW - absolute measurements KW - mass spectrometry KW - atomic weight KW - magnesium PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370931 DO - https://doi.org/10.1039/C6JA00013D SN - 0267-9477 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. VL - 31 IS - 7 SP - 1440 EP - 1458 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-37093 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ortel, Erik A1 - Hertwig, Andreas A1 - Berger, D. A1 - Esposito, P. A1 - Rossi, A. M. A1 - Kraehnert, R. A1 - Hodoroaba, Vasile-Dan T1 - New approach on quantification of porosity of thin films via electron-excited X‑ray spectra N2 - One of the crucial characteristics of functionalized thin films is their porosity (i.e., the ratio between the pore volume and the volume of the whole film). Due to the very low amount of material per coated area corresponding to thin films, it is a challenge for analytics to measure the film porosity. In this work, we present an Approach to determine the porosity of thin films by means of electron probe microanalysis (EPMA) either by wavelength-dispersive X-ray spectrometry (WDX) or by energy-dispersive X-ray spectrometry (EDX) with a scanning electron microscope (SEM). The procedure is based on the calculation of the film mass deposition from electron-excited X-ray spectra. The mass deposition is converted into film density by division of measured film thickness. Finally, the film porosity is calculated from the measured film density and the density of bulk, nonporous film material. The general applicability of the procedure to determine the porosity is demonstrated on thin templated mesoporous TiO₂ films, dip-coated on silicon wafer, with controlled porosity in the range of 15 to 50%. The high accuracy of the mass deposition as determined from X-ray spectra was validated with independent methods (ICP-OES and weighing). Furthermore, for the validation of the porosity results, ellipsometry, interference fringes method (IFM), and focused ion beam (FIB) cross sectioning were employed as independent techniques. Hence, the approach proposed in the present study is proven to be suited as a new analytical tool for accurate and relatively fast determination of the porosity of thin films. KW - Porosity KW - X-rays KW - EDX KW - Thin film KW - TiO2 KW - Density KW - Mass deposition KW - STRATAGem PY - 2016 UR - http://pubs.acs.org/doi/abs/10.1021/acs.analchem.6b00847 DO - https://doi.org/10.1021/acs.analchem.6b00847 VL - 88 IS - 14 SP - 7083 EP - 7090 PB - ACS Publications CY - 1155 Sixteenth Street N.W., Washington, DC 20036 AN - OPUS4-36911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Holzweber, Markus A1 - Unger, Wolfgang A1 - Hodoroaba, Vasile-Dan T1 - Ionic liquids as a reference material candidate for the quick performance check of energy dispersive X-ray spectrometers for the low energy range below 1 keV N2 - Ionic liquids (ILs) are proposed as simple and efficient test materials to evaluate the performance of energy dispersive X-ray spectrometers (EDS) in the low energy range below 1 keV. By only one measurement, C Kα, N Kα, O Kα, and F Kα X-ray lines can be excited. Additionally, the S Kα line at 2.3 keV and, particularly, the S L series at 149 eV complete the picture with X-ray lines offered by the selected ILs. The well-known (certifiable) elemental composition of the ILs selected in the present study can be used to check the accuracy of results produced with the available EDS quantification routines in the low energy range, simultaneously, for several low atomic number elements. A comparison with other reference materials in use for testing the performance of EDS in the low energy range is included. KW - Ionic liquids KW - EDX KW - CRM KW - Reference material KW - Low energy KW - X-rays PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-369120 DO - https://doi.org/10.1021/acs.analchem.6b01444 SN - 0003-2700 SN - 1520-6882 VL - 88 IS - 14 SP - 6967 EP - 6970 PB - ACS Publications CY - Columbus, Ohio AN - OPUS4-36912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Boehm, Rainer T1 - Automatisierte Prüfung von Radsatzwellen im eingebauten Zustand N2 - Der einwandfreie Zustand der Radsätze von Schienenfahrzeugen ist von größter Bedeutung für den sicheren Betrieb. Die Radsatzwellen werden durch eine große Zahl von Lastwechseln individuell unterschiedlich beansprucht. Dabei spielen viele Einflüsse wie äußere statische und dynamische Lasten, innere Lasten aufgrund von Unwuchten und inneren Spannungen und Umweltbedingungen entscheidende Rollen. Eine regelmäßige Prüfung ist daher obligatorisch. BTD entwickelt im Rahmen eines MNPQ-Projektes in Kooperation mit der BAM eine Phased Array Technik zur automatisierten Prüfung von Radsatzwellen im eingebauten Zustand. Die schwierigen Ankoppelbedingungen aufgrund der begrenzten Zugänglichkeit, der komplexen Geometrie und möglicherweise vorhandener Farbschichten und Schmutz auf der Radsatzwelle stellen hierbei große Herausforderungen dar. Um diesen zu begegnen, werden neben optimierten Prüfköpfen, einer in die Wasservorlaufstrecke integrierten akustischen Linse und einer speziellen Ankoppeltechnik auch Signalverarbeitungsalgorithmen eingesetzt. Die Darstellung der Signalverarbeitung ist der Schwerpunkt dieses Beitrages. Mit Hilfe von Messdatensätzen präparierter Testwellen werden verschiedene Algorithmen erprobt und hinsichtlich der Stabilität, dem Verhalten bezüglich der Ankoppelschwankungen und veränderter Wellengeometrien und der Fähigkeit zur automatischen Unterscheidung von Fehler- und Formanzeigen bewertet. Letztlich wird die beste Lösung im entwickelten Prüfsystem eingesetzt. T2 - 9. Fachtagung ZfP im Eisenbahnwesen CY - Wittenberge, Germany DA - 15.03.2016 KW - Automatisierte Ultraschallprüfung KW - Radsatzwellen KW - Signalverarbeitung KW - Akustische Linse PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370545 AN - OPUS4-37054 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaenisch, Gerd-Rüdiger T1 - Simulation and experimental results of manual UT-testing of hollow wheel set axles during the education of operators N2 - The reliability of wheel set axle testing is of high importance because small discontinuities caused during manufacturing or rock fall impacts during operation might cause growing cracks during the operation load cycles. While most of the axles are tested by automated UT-systems today, the basic education of railway NDT operators is still manual testing providing the basic understanding and skills for the operators. In Germany it is a common rule that NDT operators in the railway branch need to refresh their knowledge and skills every five years including a refresh examination. The testing results from these exercises and from a parallel round robin test have been sampled at the DGZfP Railway Education Centre in Wittenberge for a period of about 5 years. The results of the operators written in test record sheets were compared with the “true” test crack or notch position in the axles used for examination. In this way the testing results could be categorized into “hits” and “misses” and the “hits” were further evaluated due to correct position and adequate amplitude height. Considering some thousand indications documented by the operators during the refresh examination and comparing transition bow, shaft and seat it was a highlight to see that the operators reach their best detection rate in the transition bow of the wheel axle set while this is often the most difficult part concerning the UT-echoes. Fortunately this is due to their raised awareness in the transition bow region because this is the most dangerous region with respect to fracture mechanics. For two selected axles the experimental set up of 45° and 70° inward and outward UT-testing were also simulated showing clearly the difficulties of the UT-echoes detection of some specific test defects. T2 - XXII Saint-Petersburg Conference on Ultrasonic Testing of Metals and Advanced Materials (UTM 2016) CY - St. Petersburg, Russia DA - 24.05.2016 KW - Ultrasound KW - Manual testing KW - NDT reliability KW - Fault tree analysis KW - Education of NDT personnel PY - 2016 AN - OPUS4-37013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hesse, Almut A1 - Weller, Michael G. T1 - Protein Quantification by Derivatization-Free High-Performance Liquid Chromatography of Aromatic Amino Acids N2 - Amino acid analysis is considered to be the gold standard for quantitative peptide and protein analysis. Here, we would like to propose a simple HPLC/UV method based on a reversed-phase separation of the aromatic amino acids tyrosine (Tyr), phenylalanine (Phe), and optionally tryptophan (Trp) without any derivatization. The hydrolysis of the proteins and peptides was performed by an accelerated microwave technique, which needs only 30 minutes. Two internal standard compounds, homotyrosine (HTyr) and 4-fluorophenylalanine (FPhe) were used for calibration. The limit of detection (LOD) was estimated to be 0.05 µM (~10 µg/L) for tyrosine and phenylalanine at 215 nm. The LOD for a protein determination was calculated to be below 16 mg/L (~300 ng BSA absolute). Aromatic amino acid analysis (AAAA) offers excellent accuracy and a precision of about 5% relative standard deviation, including the hydrolysis step. The method was validated with certified reference materials (CRM) of amino acids and of a pure protein (bovine serum albumin, BSA). AAAA can be used for the quantification of aromatic amino acids, isolated peptides or proteins, complex peptide or protein samples, such as serum or milk powder, and peptides or proteins immobilized on solid supports. KW - Protein analysis KW - Proteomics KW - Peptides KW - Metrology KW - Certified reference materials KW - Amino acid analysis KW - Hydrolysis KW - Microwave KW - Tyrosine KW - Phenylalanine KW - Tryptophan PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370215 DO - https://doi.org/10.1155/2016/7374316 SN - 2090-0112 SN - 2090-0104 VL - 2016 SP - Article 7374316, 1 EP - 8 PB - Hindawi CY - Cairo, London, New York AN - OPUS4-37021 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hielscher, Stefan T1 - Haftfestigkeit optischer und ophthalmischer Schichten auf Polymeren und Glas T1 - Adhesive strength of optical coatings on glass and ophthalmic coatings on polymers N2 - Die quantitative Bestimmung der Haftfestigkeit von Beschichtungen ist von entscheidender Bedeutung sowohl für die Entwicklung als auch für die Qualitätssicherung. In einer Vergleichsstudie zur Haftfestigkeit von optischen und ophthalmischen Schichten wurde mit Hilfe der Zentrifugentechnologie der Einfluss verschiedener Parameter (Substratdicke, Oberflächenvorbehand-lung, Haftvermittler) auf die Haftfestigkeit optischer Schichten auf silikatischen und ophthalmischer Schichten auf polymeren Substraten untersucht. Zur Bestimmung der Haftfestigkeit in der physikalisch korrekten Dimension Kraft pro Fläche im Stirnabzug stehen die Ein-Proben-Prüfung mit der Zugprüfmaschine und die Mehr-Proben-Prüfung mittels Zentri- fugentechnologie zur Verfügung. Die Zentrifugentechnologie wurde ausgewählt, da die Prüfung von bis zu acht Proben unter nahezu identischen Versuchsbedingungen und somit eine statistisch gesicherte Bestimmung der Haftfestigkeit möglich sind. Es konnte nachgewiesen werden, dass die Substratdicke einen erheblichen Einfluss auf die gemessene Haftfestigkeit hat. Dies entspricht den Erwartungen, da es sich bei der Haftfestigkeit um eine System- eigenschaft des Schicht-Substrat-Systems handelt. Bei den Delaminationsbrüchen (DF) konnte zwischen Delamination des metallischen Reflektors (DF-R) und Delamination des Dielektrikums (DF-D) unter- schieden werden. Im Fall hinreichender Haftfestigkeit der Beschichtung traten auch Adhäsionsbrüche am Interface zum und Kohäsionsbrüche im Klebstoff auf. Nachfolgende Untersuchungen werden sich mit alternativen Klebstoffen und weiterentwickelten Fügestrategien befassen. N2 - The quantitative determination of adhesive strength of coatings is essential for both R&D and quality assurance. In a comparative study on adhesive strength of optical and ophthalmic coatings, centrifuge technology has been used for the investigation of the influence of certain parameters (e.g. substrate thickness, surface-pretreatment and adhesion promoters) on adhesive strength of optical coatings on silicate and ophthalmic coatings on polymer substrates. For determination of adhesive strength in the correct dimension force per area in the pull-off test, only two tests are available, the single-sample test in a tensile testing machine and the multi-sample test by means of centrifuge technology. The centrifuge technology has been chosen because up to eight samples can be tested under almost identical testing conditions at the same time. Hence, a statistical evaluation of adhesive strength is feasible. It has been shown that substrate thickness has a remarkable influence on the measured adhesive strength. This fulfils the expectations as adhesive strength is a system property of the coating-substrate system. Regarding delamination failure (DF) it could be differentiated between the delamination of reflective coatings (DF-R) and delamination of dielectric coatings (DF-D). In case of sufficient adhesive strength of the coating, adhesion failure at the interface of and cohesion failure within the adhesive were also observed. Following studies will address alternative adhesives and advanced bonding strategies. T2 - Werkstoffprüfung 2015 CY - Bad Neuenahr, Germany DA - 03.12.2015 KW - Haftfestigkeit KW - Optische Schichten KW - Ophthalmische Schichten KW - Zentrifugentechnologie KW - Mehr-Proben-Prüfung PY - 2015 AN - OPUS4-37022 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Halisch, M. ED - Kruschwitz, Sabine ED - Schmitt, M. ED - Weller, Andreas T1 - Quantification of rock structures with high resolution X-ray μ-CT for laboratory SIP measurements N2 - Spectral Induced Polarization (SIP) measurements are used in many different ways to characterize natural rocks and soils. Main foci of interest are the enhanced characterization of the causes of IP-effects in clastic rocks (especially sandstones), the interactions between the matrix-fluid-system and within the electrical double layers as well as the correlation with “classical” petrophysical parameters, such as specific surface area, permeability, mercury intrusion capillary pressure (MICP) and others. Nevertheless, for all of these investigations, knowledge of the inner structure of the sample material is essential in order to create reliable and validated models as well as to interpret and to assess the data most completely. Unfortunately, many of the methods used, to get access to the inner structure of rocks are destructive (e.g. MICP, thin sectioning, etc.) and the valuable sample is lost. In addition, data is either of volume integrated nature or only available for the 2D case and the usage of sister cores does not necessarily lead to reliable results. In this paper, the authors showcase the possibilities of non-destructive and three dimensional X-ray computed tomography and of enhanced image analysis capabilities for the quantification of rock structures at the pore scale. T2 - IP Workshop 2016 CY - Aarhus, Denmark DA - 06.06.2016 KW - μ-CT imaging, KW - Rock structure KW - Digital image analysis KW - Pore geometry KW - Grain geometry KW - SIP PY - 2016 SP - 1 EP - 4 CY - Aarhus, Denmark AN - OPUS4-37024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Götschel, S. A1 - Höhne, Christian A1 - Kolkoori, Sanjeevareddy A1 - Mitzscherling, Steffen A1 - Prager, Jens A1 - Weiser, M. T1 - Ray tracing boundary value problems: simulation and SAFT reconstruction for ultrasonic testing N2 - The application of advanced imaging techniques for the ultrasonic inspection of inhomogeneous anisotropic materials like austenitic and dissimilar welds requires information about acoustic wave Propagation through the material, in particular travel times between two Points in the material. Forward ray tracing is a popular approach to determine traveling paths and arrival times but is ill suited for inverse problems since a large number of rays have to be computed in order to arrive at prescribed end points. In this contribution we discuss boundary value problems for acoustic rays, where the ray path between two given points is determined by solving the Eikonal equation. The implementation of such a two Point boundary value ray tracer for sound field simulations through an austenitic weld is described and its efficiency as well as the obtained results are compared to those of a forward ray tracer. The results are validated by comparison with experimental results and commercially available UT simulation tools. As an application, we discuss an implementation of the method for SAFT (Synthetic Aperture Focusing Technique) reconstruction. The ray tracer calculates the required travel time through the anisotropic columnar grain structure of the austenitic weld. There, the formulation of ray tracing as a boundary value Problem allows a straightforward derivation of the ray path from a given transducer Position to any pixel in the reconstruction area and reduces the computational cost considerably. T2 - 19th World Conference on Non-Destructive Testing 2016 CY - München, Germany DA - 13.06.2016 KW - Ultrasonic testing KW - SAFT KW - Ray tracing KW - Simulation PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370494 UR - www.ndt.net/?id=19437 SP - ID 19437, 1 EP - 8 AN - OPUS4-37049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Boehm, Rainer T1 - What is the benefit of the total focussing method and full matrix capture for ultrasonic imaging using the phased array technique N2 - In the last two decades automated ultrasonic inspection devices took over a lot of applications that prior have been carried out using manual inspection with the evaluation of A-scans only. In parallel phased array systems have been developed and brought to the market which offer detailed and fast control over the sound field. When applying automated inspection phased array systems for UT measurements imaging of the recorded data in combination with the probe positioning data is used for the evaluation of inspections. B-Scan, C-Scan and S-Scan images are typically used with this setup. For more sophisticated applications with linear arrays echo tomography and syntethic aperture focusing technique (SAFT) are well known methods and often applied for high resolution image reconstruction. Since channel count of phased array systems is constantly rising, matrix arrays with up to 256 elements entered the market. Signal processing in the matrix domain became 3D. Since some years the Total Focusing Method (TFM) is an additional imaging tool for these type of application. It is based on the Full Matrix Capture (FMC) using the elements of phased array probes as separate transmitters and receivers. In this contribution we discuss the common ground of SAFT and TFM as well as the differences between these imaging tools. The combined use of automated inspection, matrix arrays and signal processing for high resolution measurements is a challenging task where a very long parameter list has to be taken into account. Under which conditions which elements of the full matrix should be taken for the reconstruction for best results? Based on examples taken from measured and simulated echo signals it will be shown how image resolution can be optimized in dependence of different parameters like the distance between transmitters and receivers and their directivity patterns, the depth of echo source and the specimen geometry. T2 - 19th World Conference on Non-Destructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Ultrasonic testing KW - Ultrasonic imaging KW - Phased array KW - Total focussing method KW - Full matrix capture PY - 2016 UR - https://www.wcndt2016.com/programme AN - OPUS4-37051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Götschel, S. T1 - Ray tracing boudary value problems: simulation and SAFT reconstruction for ultrasonic testing N2 - The application of advanced imaging techniques for the ultrasonic inspection of inhomogeneous anisotropic materials like austenitic and dissimilar welds requires information about acoustic wave propagation through the material, in particular travel times between two points in the material. Forward ray tracing is a popular approach to determine traveling paths and arrival times but is ill suited for inverse problems since a large number of rays have to be computed in order to arrive at prescribed end points. In this contribution we discuss boundary value problems for acoustic rays, where the ray path between two given points is determined by solving the eikonal equation. The implementation of such a two point boundary value ray tracer for sound field simulations through an austenitic weld is described and its efficiency as well as the obtained results are compared to those of a forward ray tracer. The results are validated by comparison with experimental results and commercially available UT simulation tools. As an application, we discuss an implementation of the method for SAFT (Synthetic Aperture Focusing Technique) reconstruction. The ray tracer calculates the required travel time through the anisotropic columnar grain structure of the austenitic weld. There, the formulation of ray tracing as a boundary value problem allows a straightforward derivation of the ray path from a given transducer position to any pixel in the reconstruction area and reduces the computational cost considerably. T2 - 19th World Conference on Non-Destructive Testing 2016 CY - Munich, Germany DA - 13.06.2016 KW - Ultrasonic testing KW - SAFT KW - Ray tracing KW - Simulation PY - 2016 UR - www.ndt.net/?id=19437 UR - https://www.wcndt2016.com/portals/wcndt/bb/Fr1H4.pdf AN - OPUS4-37052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Habel, Wolfgang R. A1 - Krebber, Katerina A1 - Daum, Werner T1 - Results in standardization of FOS to support the use of SHM systems N2 - Measurement and data recording systems are important parts of a holistic Structural Health Monitoring (SHM) system. New sensor technologies such as fiber-optic sensors are often used; however, standards (or at least guidelines) are not yet available or internationally approved. This lack in standardization makes the acceptance of FOS technologies in complex SHM systems substantially difficult. A standard family for different FOS technologies is therefore being developed that should help to design SHM systems in an optimal way. International standardization activities take place in several standardization bodies such as IEC and ASTM, and within SHM societies such as ISHMII. The paper reports on activities in standardization of fiber-optic sensors, on results already achieved, and on newly started projects. Combined activities of fiber sensor experts and SHM experts from Civil Engineering are presented. These contributions should help owners of structures as well as developers of sensors and monitoring systems to select effective and validated sensing technologies. Using these standards, both parties find recommendations how to proceed in development of SHM systems to evaluate the structural behavior based on e.g. standardized fiber optic sensors, and to derive necessary measures, e.g. the optimal maintenance strategy. T2 - Sixth European Workshop on Optical Fibre Sensors CY - Limerick, Ireland DA - 30.05.2016 KW - Fiber-optic sensor KW - Standard KW - Temperature KW - Strain KW - Monitoring KW - Structural health KW - Application PY - 2016 DO - https://doi.org/10.1117/12.2236863 SN - 0277-786X VL - 9916 SP - 991625-1 EP - 991625-4 AN - OPUS4-37053 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Characterization of nanocrystalline particles with NIR emission - Spectroscopic properties and surface group analysis N2 - There is an increasing interest in optical reporters like semiconductor quantum dots and upconversion nanocrystals with emission > 800 nm for bioanalysis, medical diagnostics, and safety barcodes. Prerequisites for the comparison of material performance, the mechanistic understanding of nonradiative decay channels, and the rational design of new nanomaterials with improved properties are reliable fluorescence measurements and validated methods for the assessment of their surface chemistry. The latter is of special relevance for nanocrystalline emitters, where surface states and the accessibility of emissive states by quenchers largely control accomplishable photoluminescence quantum yields and hence, signal sizes and detection sensitivities from the reporter side. Here, we present the design of integrating sphere setups for the excitation power density-dependent absolute measurement of emission spectra and photoluminescence quantum yields in the wavelength region of 350 to 1600 nm and results from spectroscopic studies of semiconductor quantum dots and upconversion nanocrystals of different size and surface chemistries in various environments. Subsequently, examples for simple approaches to surface group and ligand analysis are presented. T2 - 1st International Biophotonics Conference CY - Singapure DA - 25.07.2016 KW - Fluorescence KW - Integrating sphere spectroscopy KW - Quantum yield KW - NIR KW - IR KW - Optical spectroscopy KW - Nanomaterials KW - Semiconducor nanocrystals KW - Surface analysis KW - Ligand analysis KW - Optical assay PY - 2016 AN - OPUS4-36998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Neue Konzepte für die zerstörungsfreie Prüfung und die Zustandsüberwachung von Eisenbahnradsätzen mit Ultraschall N2 - Die regelmäßige Überprüfung von Eisenbahnradsatzwellen auf betriebsbedingte Schädigungen ist ein fester Bestandteil des Instandhaltungskonzeptes von Eisenbahnfahrzeugen. Insbesondere bei hohen Achslasten und hohen Rotationsgeschwindigkeiten ist eine detaillierte regelmäßige Prüfung notwendig. In den letzten Jahren wurden für diese Prüfaufgabe mechanisierte Ultraschallprüfsysteme entwickelt, erfolgreich eingeführt und etabliert. Für eine Weiterentwicklung dieser Technologie stehen die Themen Erhöhung der Auflösung, Reduzierung von Oberflächen- und Störeinflüssen, Verkürzung von Prüfzeiten, Verbesserung der POD, Verlängerung von Inspektionsintervallen, Vereinfachung der Auswertung und die Möglichkeit der Durchführung von Analyseprüfungen im Vordergrund. Es werden Ansätze und neue Konzepte zur Lösung dieser Herausforderungen vorgestellt. T2 - 9. Fachtagung Zerstörungsfreie Prüfung im Eisenbahnwesen CY - Wittenberge, Germany DA - 15.03.2016 KW - Zerstörungsfreie Prüfung KW - Eisenbahn KW - Radsatzwelle KW - Ultraschall KW - POD PY - 2016 AN - OPUS4-37006 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Increasing the sensitivity of ultrasonic phased array wheel set axle inspection by using signal processing N2 - Der einwandfreie Zustand der Radsätze von Schienenfahrzeugen ist von größter Bedeutung für den sicheren Betrieb. Die Radsatzwellen werden durch eine große Zahl von Lastwechseln individuell unterschiedlich beansprucht. Dabei spielen viele Einflüsse wie äußere statische und dynamische Lasten, innere Lasten aufgrund von Unwuchten und inneren Spannungen und Umweltbedingungen entscheidende Rollen. Eine regelmäßige Prüfung ist daher obligatorisch. BTD entwickelt im Rahmen eines MNPQ-Projektes in Kooperation mit der BAM eine Phased Array Technik zur automatisierten Prüfung von Radsatzwellen im eingebauten Zustand. Die schwierigen Ankoppelbedingungen aufgrund der begrenzten Zugänglichkeit, der komplexen Geometrie sowie Farbschichten und Schmutz auf der Radsatzwelle stellen hierbei große Herausforderungen dar. Zu deren Bewältigung werden neben optimierten Prüfköpfen, einer in die Wasservorlaufstrecke integrierten akustischen Linse und einer speziellen Ankoppeltechnik auch Signalverarbeitungsalgorithmen eingesetzt. Die Darstellung der Signalverarbeitung ist der Schwerpunkt dieses Beitrages. Mit Hilfe von Messdatensätzen präparierter Testwellen werden verschiedene Algorithmen erprobt und hinsichtlich der Stabilität, dem Verhalten bezüglich der Ankoppelschwankungen und veränderter Wellengeometrien und der Fähigkeit zur automatischen Unterscheidung von Fehler- und Formanzeigen bewertet. Letztlich wird die beste Lösung im entwickelten Prüfsystem eingesetzt. T2 - 19th WCNDT - World Conference on Non Destructive Testing CY - München, Germany DA - 13.06.2016 KW - Ultrasound KW - Phased array KW - Wheelset KW - Railway KW - Signal processing PY - 2016 AN - OPUS4-37008 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altenburg, Simon T1 - Thermografische Schichtdickenbestimmung von Oberflächenschutzsystemen für Beton N2 - Im Bauwesen werden Polymerbeschichtungen häufig eingesetzt um einerseits ein bestimmtes Aussehens zu schaffen oder andererseits das Bauteil vor Alterung, Verschleiß oder Schädigung zu schützen. Bei praktisch allen Arbeitszielen ist deren Wirkung von der eigens dafür definierten Schichtdicke der Polymerbeschichtung abhängig. Daher wird die Dicke der Beschichtung nach erfolgtem Schichtauftrag überprüft. Für den in diesem Zusammenhang anspruchsvollen mineralischen Untergrund Beton stehen bislang allerdings nur zerstörende Prüfverfahren zur Verfügung. Aus diesem Grund soll im Rahmen des Projektes in Kollaboration mit der IBOS GmbH ein auf aktiver Thermografie basierendes Verfahren sowie ein Gerät für den vor-Ort-Einsatz entwickelt werden, mit dessen Hilfe eine zerstörungsfreie Schichtdickenbestimmung möglich ist. Der Vortrag gibt einen kurzen Überblick über die Schichtdickenbestimmung mit Hilfe aktiver Thermografie und erläutert die speziellen Herausforderungen an die Thermografie für die in diesem Projekt zu charakterisierenden Polymerwerkstoffe. Zudem wird auf die Anforderungen an die zu entwickelnde Methode, den aktuellen Stand der Entwicklung sowie auf erste Ergebnisse des Projektes eingegangen. T2 - Abteilungsseminar der Abteilung 8 CY - Berlin, Germany DA - 02.05.2016 KW - Thermografie KW - Analytisches Modell KW - Oberflächenschutzsystem KW - Beton KW - Teiltransparenz KW - Dickenbestimmung PY - 2016 AN - OPUS4-36991 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Esteban-Fernandez, Diego A1 - Traub, Heike T1 - High resolution laser ablation NWRimage system for single cell imaging N2 - This work demonstrates the sub-cellular resolution bio-imaging capabilities of the NWRimage system with Dual Concentric Injector (DCI) technology in a practical application. 3T3 fibroblast cells incubated with gold nanoparticles were imaged, demonstrating the sub-cellular imaging capabilities. A laser ablation system specifically designed for rapid, high resolution imaging was employed. The system´s optical layout is optimized to minimize crater diameters. Sensitivity and speed were achieved using the DCI technology for ultra-fast washout times. T2 - 13th European Workshop on Laser Ablation CY - Ljubljana, Slovenia DA - 12.07.2016 KW - Laser ablation KW - Bio-imaging KW - Nanoparticle PY - 2016 AN - OPUS4-36996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kästner, Claudia T1 - Coating-tuned catalytic activity of silver nanoparticles N2 - The use of silver nanoparticles in consumer related products has significantly increased over the last decade, especially due to their antimicrobial properties. Today they are used in a variety of products, which range from textiles over children toys and dietary supplements. Therefore, research on silver in a nanoscale form becomes increasingly important for a high amount of studies. Unfortunately the results of these studies are extremely diverse and do not lead to a consistent evaluation of the toxicity of silver nanoparticles. The central problem lies in the utilization of a wide range of silver nanoparticles, which show a broad size distribution. To overcome this problem we synthesized ultra-small core-shell silver nanoparticles by an up-scaled modification of the polyol process. The particles are highly stable and show no aggregation for more than six months. Small-angle X-ray scattering (SAXS) analysis reveal a narrow size distribution of the silver cores with a mean radius of RC = 3.0 nm and a distribution width of 0.6 nm. Dynamic light scattering (DLS) provides a hydrodynamic radius of RH = 10.0 nm and a PDI of 0.09. The surface of the particles is covered with poly(acrylic acid) (PAA) forming a shell with a thickness of 7.0 nm, which provides colloidal stability lasting for more than six months at ambient conditions. It is foreseen to use these thoroughly characterized particles as reference material to compare the catalytic and biological properties of functionalized silver nanoparticles. The stabilizing ligand PAA can be easily exchanged by biomolecules to modify the surface functionality. Replacements of PAA with glutathione (GSH) and bovine serum albumin (BSA) have been performed as examples. We demonstrate that the particles effectively catalyze the reduction of 4-nitrophenol to 4-aminophenol with sodium borohydride. With PAA as stabilizer, the catalytic activity of (436 ± 24) L g-1 s-1 is the highest reported in literature for silver nanoparticles. GSH and BSA passivate the surface substantially resulting in lower catalytic activities of (77.6 ± 0.9) L g-1 s-1 and (3.47 ± 0.50) L g-1 s-1, respectively. The ultra-small particles were already used in the Nano Define project. Due to their small size it is possible to investigate the detection limits of different analytical techniques like electron microcopy, field flow fractionation or single particle tracking. In this project they serve as the calibration standard with the smallest radius. T2 - International summer school “Nanoscience meets Metrology” CY - Turin, Italy DA - 04.09.2016 KW - Protein coating KW - SAXS KW - Ligand exchange PY - 2016 AN - OPUS4-37352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Klas A1 - Kern, Simon A1 - Zientek, Nicolai A1 - Guthausen, G. A1 - Maiwald, Michael T1 - Process control with compact NMR N2 - Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction and process control. An increasing number of applications are reported. To build an interdisciplinary bridge between “process control” and “compact NMR”,we give a short overviewon current developments in the field of process Engineering such as modern process design, integrated processes, intensified processes along with requirements to process control, model based control, or soft sensing. Finally, robust field integration of NMR systems into processes environments, facing explosion protection or Integration into process control systems, are briefly discussed. KW - Prozessanalytik KW - Quantitative NMR-Spektroskopie KW - Industrie 4.0 KW - Reaction monitoring KW - Process control KW - Online NMR spectroscopy KW - Compact NMR PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-373562 UR - http://www.sciencedirect.com/science/article/pii/S0165993616300073 DO - https://doi.org/10.1016/j.trac.2016.03.016 SN - 0165-9936 VL - 83 IS - Part A / SI SP - 39 EP - 52 PB - Elsevier AN - OPUS4-37356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hübert, Thomas T1 - Gas sensors for technical safety and process control N2 - The presentation gives an overview on sensor principles and materials. Examples for sensor application in technical safety and process control were presented and the contribution of BAM in sensor testing, validation and standadization are discussed. T2 - Vortrag in der Abteilung Physik des ITS (Institute Technology Surabaya) CY - Surabaya, Indonesia DA - 29-08-2016 KW - Gas sensor KW - Safety KW - Process control PY - 2016 AN - OPUS4-37358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Köppe, Enrico T1 - Magnetic field detection with an advanced FBG-based sensor device N2 - A high-performance fiber Bragg grating-based (FBG) sensor device for the detection of small magnetic fields has been developed. Based on a smart multilayer coating exposed over the physical length of the FBG, magnetic fields exhibited by rotating machine parts, power generators or current cable can easily be detected, analysed and evaluated. Consequently, this innovative, in-process and non-contact inspection method leads to an increase in quality and reliability of high-performing machine parts, devices and cables. The basic physical concept is based on a magnetostrictive multilayer coating system that strains the high-resolution FBG element. Subsequently, a fixed relationship between induced magnetic field and wavelength change of the FBG element forms the characteristic sensitivity curve. Intensive tests regarding the characterisation of the magnetic field FBG sensor have been carried out and its performance has been evaluated. T2 - EuroSensors XXX 2016 CY - Budapest, Hungary DA - 04.09.2016 KW - Strain KW - Fiber Bragg grating KW - Magnetostriction KW - Magnetic field PY - 2016 AN - OPUS4-37364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Preissel, Marcel A1 - Vrana, J. T1 - Ermittlung der Auffindwahrscheinlichkeit von Reflektoren in Abhängigkeit der Rastergröße bei der Ultraschallprüfung großer Schmiedestücke N2 - Die Auswirkung des Prüfrasters nach der DGZfP Richtlinie US 07:2014 auf die Auffindwahrscheinlichkeit von Reflektoren wird untersucht. Hierzu werden Simulationsrechnungen durchgeführt, mit dem Ziel, die Abhängigkeit der Unterbewertung von Größe und Tiefenlage von Reflektoren in Bezug auf das Prüfraster zu ermitteln und experimentell zu überprüfen. In zwei Simulationsreihen wird der Einfluss des Prüfrasters auf die Suche von Anzeigen und auf die Bewertung von Anzeigen ermittelt und bewertet. Auf Basis der Simulationsrechnungen wird eine POD-Analyse mit dem Ziel durchgeführt, die Auffindwahrscheinlichkeit von Reflektoren in Bezug zur Rastergüte Rn zu setzten und die Nachweisgrenze zu ermitteln. KW - Schmiedeteile KW - Ultraschall KW - Probability of detection KW - Prüfraster PY - 2016 UR - http://www.dgzfp.de/Dienste/ZfP-Zeitung IS - 150 SP - 52 EP - 57 AN - OPUS4-37032 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Daniel T1 - Ellipsometric characterization of metal doped SnOx thin films for SPREE-based gas sensors N2 - Gas sensors are an important tool in various areas for example in industrial process control as well as Gas sensors are an important tool in various areas for example in industrial process control as well as safety applications or in research. A useful gas detector should be selective, precise, stable and cost-effective. In the present research a surface based gas detection technique is investigated using the SPR effect with ellipsometric readout. This technique is called surface plasmon resonance enhanced ellipsometry (SPREE). The sensor consists of a gold layer (40 nm) top-coated with a doped metal-oxide (M:SnOₓ, 5 nm). The coating is added by magnetron sputtering with doped targets with different doping concentrations. It could be shown that, without the top-coating, these type of sensors can detect various gases, e.g. CO, H2, O2, O3, He, N2, with sensitivities down to the ppm range (in air). The goal of the present study is to characterize the additional coating materials in dependence of the coating conditions. With the help of the doped-metal oxide, the sensitivity increases dramatically by a factor of 100. Additionally, a selectivity for specific gases is observed which depends on the doping conditions of the coating. Changing the properties of the plasma coating process and the doping metal gives access to a variety of different layers and enables us to find the best conditions. T2 - Leibniz Institut für Analytische Wissenschaften ISAS e.V. - Kolloqium CY - Berlin, Germany DA - 05.05.2016 KW - Ellipsometry KW - SPR effect KW - SnOx KW - Gas sensors PY - 2016 AN - OPUS4-37034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pech, Anja A1 - Wilke, Olaf A1 - Horn, Wolfgang A1 - Jann, Oliver T1 - Analysis of very volatile organic compounds (VVOC) with thermal desorption GC-MS N2 - Most VVOC were rarely considered in the evaluation of construction products. (Salthammer, 2014) In Germany this will change because the latest version of the German AgBB scheme for health evaluation (2015) now include VVOC, e.g. ethyl acetate and ethanol. In this study selected compounds were tested with the procedure described in ISO 16017 and a method for measuring VVOC with thermal desorption was developed. Three different adsorbents Tenax TA, Carbograph 5TD and Carbopack X were tested to analyse VVOC according to ISO 16017. For the tested VVOC, Carbograph 5TD showed the best results under the chosen analytical conditions. T2 - Indoor Air 2016, The 14th international conference of Indoor Air Quality and Climate CY - Gent, Belgium DA - 03.07.2016 KW - Thermal desorption KW - VVOC KW - Carbograph 5TD KW - Carbopack X PY - 2016 SP - Paper 889, 1 EP - 2 AN - OPUS4-37035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzweber, M. T1 - Ionische Flüssigkeiten als Referenzmaterial in der Oberflächenanalytik N2 - Energiedispersive Röntgenspektroskopie (EDX) ist eine der meist verbreiteten Methoden zur Bestimmung der chemischen Zusammensetzung von Festkörpern und dünnen Schichten. Durch die technologische Weiterentwicklung energiedispersiver Röntgenspektrometer wurde die Leistungsfähigkeit auch im niederenergetischen Bereich unter 1 keV verbessert. Geeignete Testmaterialien zur Überprüfung der Leistungsfähigkeit im niederenergetischen Bereich in Übereinstimmung mit ISO 15632 sind kaum vorhanden und basieren hauptsächlich auf C K und F K Linien. Um gültige Resultate aus akkreditierten und zertifizierten Prüf- und Kalibrierlaboratorien in Übereinstimmung mit ISO/IEC 17025 zu gewährleisten sind regelmäßige Funktionsprüfungen der Spektrometer notwendig. In einer Machbarkeitsstudie wurde die Eignung einer bestimmten Substanz-klasse, nämlich ionische Flüssigkeiten, als Referenzmaterial zur routinemäßi-gen Überprüfung der Energieskala, der Energieauflösung und der Spektrometer Effizienz untersucht. Es kann gezeigt werden, dass mit einer einzigen Messung an einem einzigen Referenzmaterial mehrere Geräteparameter überprüft werden können. Damit ist es im niederenergetischen Bereich möglich regelmäßige Funktionsprüfungen von Spektrometern durchzuführen, aber auch die Leistungsfähigkeit verschiedener Spektrometer zu vergleichen. Beides kann sehr effizient durch einen einfachen qualitativen Vergleich mehrerer Spektren erreicht werden. Durch die Verwendung von ionischen Flüssigkeiten als Referenzmaterial, deren Stöchiometrie genau bekannt ist bzw. zertifiziert werden kann, können eventuell sogar die gängigen Modelle zur Matrixkorrektur validiert werden. Auch wäre eine Neubewertung von Fundamentalparametern (Fluoreszenzausbeute, Massenschwächungskoeffizienten usw.) von Elementen niedriger Ordnungszahl möglich. T2 - 19. Arbeitstagung Angewandte Oberflächenanalytik (AOFA) CY - Soest, Germany DA - 05.09.2016 KW - Ionische Flüssigkeiten KW - Referenzmaterial KW - Oberflächenanalytik PY - 2016 UR - http://www.awz-soest.fraunhofer.de/de/aofa2016.html AN - OPUS4-37322 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kardjilov, N. A1 - Hilger, A. A1 - Manke, I. A1 - Banhart, J. A1 - Griesche, Axel T1 - Imaging with Cold Neutrons at the CONRAD-2 Facility N2 - CONRAD-2 is an imaging instrument using low-energy (cold) neutrons. The instrument is installed at the end of a curved neutron guide which avoids the direct line of sight towards the reactor core. This ensures a very low background of high-energy neutrons and. photons at the sample position. The cold neutron beam provides a wavelength range which is suitable for phase-and diffraction-contrast imaging such as grating interferometry and Bragg edge mapping. The instrument is well suited for high resolution imaging due to the high efficiency of the very thin scintillators that can be used for the detection of cold neutrons. An instrument upgrade was performed recently as a part of an upgrade program for the cold neutron instrumentation at HZB. The parameters of the instrument as well as some research highlights will be presented. T2 - 10th World Conference on Neutron Radiography (WCNR) CY - Grindelwald, SWITZERLAND DA - 05.10.2014 KW - iron embrittlement KW - neutron imaging KW - neutron instrumentation KW - cold neutrons PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-373239 DO - https://doi.org/10.1016/j.phpro.2015.07.008 SN - 1875-3892 VL - 69 SP - 60 EP - 66 PB - Elsevier B.V. CY - Amsterdam, NL AN - OPUS4-37323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Nanoparticles and films characterization: Electron microscopy and related techniques N2 - Scanning Electron Microscopy (SEM) represents the mostly widespread method available in analytical laboratories dedicated to the characterization of physical properties such as morphology of various solid materials from ‘micro-’ down to the nanometre scale. The use of secondary electrons excited by a sharply, nm-focussed primary electron beam enables at any modern SEM to image objects with high in-depth and lateral sensitivity, i.e. with high spatial resolution. Hence, e. g. nanoparticles (NPs) are able to be easily characterized with respect to their individual size and shape, but also to the morphology of their surface. By preparing the nano-objects on thin membranes as electron transparent samples it is possible to perform electron microscopy in the transmission mode (TEM and TSEM). The corresponding transmission (i.e. mass-thickness) contrast reveals in-depth information, but is also well suited for dimensional measurements in the 2D projection image. Both the surface sensitive mode and the transmission one are meanwhile available at any modern SEM. If an X-ray spectrometer is attached to an electron microscope, it is possible to analyse the characteristic X-rays induced by electron bombardment. Most electron microscopes have attached an energy dispersive X-ray spectrometer (EDX) so that EDX elemental maps can be carried out. Recent technological developments of high throughput EDS detectors and their advantages regarding high-resolution X-ray analysis down to the nm range are reviewed. High-resolution micrographs (SEM, TSEM, TEM) and corresponding X-ray elemental maps on various representative nanoparticles, but also layered samples prepared in cross-section, will be presented and discussed. The importance of selecting the best suited analysis conditions will be highlighted. Also other, often challenging, topics such as sample preparation and image data processing will be critically addressed by practical examples. Further analytical techniques able to be employed at an electron microscope, like cathodoluminescence (CL) or micro-X-ray fluorescence (µXRF) will be briefly surveyed. T2 - Nanoscience Meets Metrology - Synthesis, Characterization, Testing and Applications of Validated Nanoparticles - International Summer School CY - Turin, Italy DA - 04.09.2016 KW - Nanoparticles KW - Electron microscopy KW - High-resolution KW - Thin films KW - X-ray spectroscopy PY - 2016 UR - http://www.setnanometro.eu/events/ AN - OPUS4-37325 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lichtenstein, D. T1 - Core or coating material – What dictates the uptake and translocation of nanoparticles in vitro? N2 - Nanoparticle size and shape are crucial parameters regarding the potential of nanoparticles to penetrate cell membranes and epithelial barriers. Current research in this field additionally focuses on the particle coating material. In order to distinguish between core- and coating-related effects in nanoparticle uptake and translocation behavior, this study investigated two nanoparticles equal in size, coating and charge but different in core material. Silver and iron oxide coated with poly (acrylic acid) (PAS) were extensively characterized by TEM (transmission electron microscopy), SAXS (Small-Angle X-ray Scattering), ZetasizerTM and NanoSightTM. For uptake and transport studies the widely used human intestinal Caco-2 model in a TranswellTM-system with subsequent elemental analysis (AAS) was used. For evaluation and particle visualization transmission electron microscopy (TEM) and Ion Beam Microscopy (IBM) were conducted. Although similar in size, charge and coating material, the behavior of particles in Caco-2 cells was quite different. The internalized amount was comparable, but PAA-coated iron oxide nanoparticles were additionally transported through the cells. By contrast, PAA-coated silver nanoparticles remained in the cells. Our findings suggest that the coating material influenced only the uptake of the nanoparticles whereas the translocation was determined by the core material. In summary, a core-dependent effect on nanoparticle translocation was revealed. Both the uptake and transport of nanoparticles in and through cells should be considered when discussing nanoparticle fate and safety. T2 - Eurotox 2016 CY - Seville, Spain DA - 04.09.2016 KW - Cellular uptake KW - SAXS PY - 2016 AN - OPUS4-37338 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Färber, C. A1 - Titschack, J. A1 - Schönberg, Chr. H. L. A1 - Ehrig, Karsten A1 - Boos, K. A1 - Illerhaus, Bernhard A1 - Asgaard, U. A1 - Bromley, R. G. A1 - Freiwald, A. A1 - Wisshak, M. ED - Bahn, M. ED - Fennel, K. ED - Kesselmeier, J. ED - Naqvi, S. W. A. T1 - Long-term macrobioerosion in the Mediterranean Sea assessed by micro-computed tomography N2 - Biological erosion is a key process for the recycling of carbonate and the formation of calcareous sediments in the oceans. Experimental studies showed that bioerosion is subject to distinct temporal variability, but previous long-term studies were restricted to tropical waters. Here, we present results from a 14-year bioerosion experiment that was carried out along the rocky limestone coast of the island of Rhodes, Greece, in the Eastern Mediterranean Sea, in order to monitor the pace at which bioerosion affects carbonate substrate and the sequence of colonisation by bioeroding organisms. Internal macrobioerosion was visualised and quantified by micro-computed tomography and computer-algorithm-based segmentation procedures. Analysis of internal macrobioerosion traces revealed a dominance of bioeroding sponges producing eight types of characteristic Entobia cavity networks, which were matched to five different clionaid sponges by spicule identification in extracted tissue. The morphology of the entobians strongly varied depending on the species of the producing sponge, its ontogenetic stage, available space, and competition by other bioeroders. An early community developed during the first 5 years of exposure with initially very low macrobioerosion rates and was followed by an intermediate stage when sponges formed large and more diverse entobians and bioerosion rates in-creased. After 14 years, 30 % of the block volumes were occupied by boring sponges, yielding maximum bioerosion rates of 900 g m. KW - Bioerosion KW - Computed tomography KW - Carbonate substrate PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-372709 UR - http://www.biogeosciences.net/13/3461/2016/bg-13-3461-2016.pdf DO - https://doi.org/10.5194/bg-13-3461-2016 VL - 13 IS - 11 SP - 3461 EP - 3474 PB - Copernicus Publications CY - Göttingen AN - OPUS4-37270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bierstedt, Andreas T1 - Development and characterization of an airborne laser-spark ion source for ambient desorption / ionization mass spectrometry N2 - A novel direct sampling ionization scheme for ambient mass spectrometry is presented. Desorption and ionization is achieved by a quasi-continuous laser induced plasma in air. Since there are no solid or liquid electrodes involved the ion source does not suffer from chemical interferences or fatigue originating from erosive burning or from electrode consumption. A laser plasma was ignited under ambient conditions in front of a modified TOF MS atmospheric pressure interface, using a high repetition rate DPSS laser operating at 532 nm and 26 kHz and an aspherical lens with a focal length of 8 mm. Emission spectroscopy (40-1100 nm) and time resolved studies on specific plasma parameters revealed insight into the physical and chemical plasma properties. Plasma ignition can be performed in rare gases and under ambient conditions. The hot plasma zone was kept at a certain distance from the sample region. Thus, effective collisional cooling seemed to prevent thermal fragmentation. Every single spark generates a shockwave, providing new reactive species, which expands concentrically from the hot region. Under ambient conditions primary charge carriers (ions and electrons) as well as VUV radiation initialize reaction cascades equivalent to other ambient ionization methods, such as DART or DBD. Mass spectra of polar/nonpolar hydrocarbons, sugars, pharmaceuticals and natural biomolecules in food were observed. Comprehensive emission spectroscopic measurements and time resolved electron current studies revealed insight into some plasma properties, such as the emitted high energetic radiation and the time evolution of the expanding plume. T2 - International Mass Spectrometry Conference 2016 CY - Toronto, ON, Canada DA - 20.08.2016 KW - laser-spark KW - laser-induced plasma KW - ambient mass spectrometry KW - emission spectroscopy PY - 2016 AN - OPUS4-37281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schäferling, Michael T1 - Nanoprobes for sensing and imaging of intracellular pH based on polyethyleneimide-coated photon upconversion nanoparticles conjugated to a pH sensitive rhodamine dye N2 - Lanthanide-doped photon upconversion nanoparticles (UCNPs) exhibit many advantages compared to Stokes-shifted luminescent probes (organic dyes, quantum dots). Due to the upconversion process, the limitations of photobleaching, autofluorescence and low penetration depths in tissue shown by classical fluorescent probes are avoided. This makes UCNPs particularly useful for applications in complex biological samples. Sensing of intracellular pH is of particular interest in biomedical research since structure and function of biomolecules strongly depend on the concentration of protons in their environment. T2 - UPCON 2016 CY - Wroclaw, Poland DA - 23.05.2016 KW - upconversion KW - nanoprobes KW - chemical sensing PY - 2016 AN - OPUS4-37282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schäferling, Michael T1 - Sensing and Imaging of Intracellular pH Using Polyethyleneimine-coated Photon Upconversion Based Nanoprobes N2 - Lanthanide-doped photon upconversion nanoparticles (UCNPs) exhibit many advantages compared to conventional Stokes-shifted luminescent probes such as organic dyes and quantum dots. Due to the upconversion (UC) process, which describes the conversion of NIR light into shorter wavelength radiation, the limitations of photobleaching, autofluorescence and low penetration depths in tissue shown by classical fluorescent probes absorbing in the UV/vis range are avoided. This makes UCNPs particularly useful for applications in complex samples occurring in bioanalysis, biomedicine and imaging. Sensing of intracellular pH is of particular interest in biomedical research since structure and function of biomolecules strongly depend on the concentration of protons in their environment. We described previously a UCNP nanosensor for pH based on a resonance energy transfer from hexagonal nanocrystals of NaYF4: Yb3+,Er3+ to a pH-sensitive fluorophore (pHrodoTM Red).[1] The nanocrystals were coated with a thin shell of aminosilane with several nanometer layer thickness for coupling of the pH indicator. In this contribution we present a new generation of UC nanoprobes that are coated with a layer of highly branched polyethylenimine (PEI). The PEI coating enables a higher coupling of indicator molecules on the particle surface, better signal to reference ratios in ratiometric readout and an improved cellular uptake compared to the aminosilane coated particles due to a more positive zeta potential. Again, pHrodoTM Red is used as pH indicator, sensitized by the 550 nm emission of the UCNPs. The nanoprobes are calibrated by ratiometric dual wavelength readout at 550 nm (reference signal) and 590 nm (sensor signal) and visualized using a scanning confocal fluorescence microscope with 980 nm excitation wavelength. We studied the cellular uptake efficacy of the nanoprobes and determined to which type of compartment, lysosomes, endosomes or cytosol, the probes are targeted to by measuring the pH of their microenvironment. An in situ control was performed in live cells by a treatment with nigericin, whereby the pH of all intracellular compartments is set at extracellular level. Our results suggest that the PEI coating facilitated endosomal escape of the nanoprobes. T2 - Europtrode XIII CY - Graz, Austria DA - 20.03.2016 KW - upconversion KW - chemical sensing KW - nanoprobes PY - 2016 AN - OPUS4-37283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bierstedt, Andreas A1 - Riedel, Jens T1 - Airborne laser-spark for ambient desorption/ionisation N2 - A novel direct sampling ionisation scheme for ambient mass spectrometry is presented. Desorption and ionisation are achieved by a quasi-continuous laser induced plasma in air. Since there are no solid or liquid electrodes involved the ion source does not suffer from chemical interferences or fatigue originating from erosive burning or from electrode consumption. The overall plasma maintains electro-neutrality, minimising charge effects and accompanying long term drift of the charged particles trajectories. In the airborne plasma approach the ambient air not only serves as the plasma medium but at the same time also slows down the nascent ions via collisional cooling. Ionisation of the analyte molecules does not occur in the plasma itself but is induced by interaction with nascent ionic fragments, electrons and/or far ultraviolet photons in the plasma vicinity. At each individual air-spark an audible shockwave is formed, providing new reactive species, which expands concentrically and, thus, prevents direct contact of the analyte with the hot region inside the plasma itself. As a consequence the interaction volume between plasma and analyte does not exceed the threshold temperature for thermal dissociation or fragmentation. Experimentally this indirect ionisation scheme is demonstrated to be widely unspecific to the chemical nature of the analyte and to hardly result in any fragmentation of the studied molecules. A vast ensemble of different test analytes including polar and non-polar hydrocarbons, sugars, low mass active ingredients of pharmaceuticals as well as natural biomolecules in food samples directly out of their complex matrices could be shown to yield easily accessible yet meaningful spectra. Since the plasma medium is humid air, the chemical reaction mechanism of the ionisation is likely to be similar to other ambient ionisation techniques. N2 - Wir stellen hier eine neue Ionisationsmethode für die Umgebungsionisation (ambient ionisation) vor. Sowohl die Desorption als auch die Ionisation erfolgen hierbei durch ein laserbetriebenes Luftplasma. Die Abwesenheit fester oder flüssiger Elektroden hat zur Folge, dass die Methode weder unter chemischen Interferenzen noch unter Verschleiß durch Korrosionsbrand oder abgetragenes Elektrodenmaterial leidet. Insgesamt betrachtet herrscht in dem Plasma Elektroneutralität, wodurch Aufladungseffekte minimiert werden, die andernfalls zu einer langfristigenÄderung der Flugbahnen von Ionen während der Experimente führen kann. In dem Ansatz eine freischwebende Luftentladung bei Atmosphärendruck zu verwenden agiert die Luft nicht nur als Plasmamedium sondert dient zusätzlich als Badgas für die stoßinduzierte Kühlung der entstehenden Ionen. Die Ionisierung der Analytmoleküle erfolgt nicht unmittelbar im Plasma sondern in dessen direkter Umgebung durch Wechselwirkung mit freigesetzten ionischen Luftspezies, freien Elektronen oder Photonen im kurzwelligen ultravioletten Bereich. Jede Laserentladung erzeugt eine hörbare Stoßwelle, in welcher neu produzierte reaktive Spezies freigesetzt werden, welche sich konzentrisch ausbreiten, so dass eine Diffusion der Analytmoleküle ins heiße Innere des Plasmas verhindert wird. Daraus folgt, dass im Interaktionsvolumen zwischen Plasma und Analyt der Temperaturgrenzwert für eine thermische Dissoziation oder Fragmentierung der Moleküle nicht überschritten wird. Experimentell konnte belegt werden, dass das vorgestellte Ionisierungsschema sehr unselektiv bezüglich der chemischen Analytklasse ist und kaum Fragmentierungsprodukte beobachtet werden können. Messungen einer breitgefächerten Auswahl unterschiedlicher Testsubstanzen, wie beispielsweise polarer und unpolarer Kohlenwasserstoffe, Zuckern, niedermolekularer pharmazeutischer Wirkstoffe, sowie natürlicher Biomoleküle in Lebensmittelproben unmittelbar aus ihren komplexen Matrizes, führten zu aussagekräftigen Massenspektren. Zumal das Lasermedium feuchte Luft ist, scheint der Reaktionsmechanismus dem anderer Atmosphärendruckionisierungsmethoden zuähneln. KW - Laser-spark KW - Laser-induced plasma KW - DPSS laser KW - High repetition rate KW - Ambient mass spectrometry KW - Time-of-flight mass spectrometry KW - Ionisation PY - 2016 DO - https://doi.org/10.1255/ejms.1417 SN - 1469-0667 VL - 22 IS - 3 SP - 105 EP - 114 PB - IM Publications LLP CY - Chichester, UK AN - OPUS4-37286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pollakowski, B. T1 - Qualifying PDMS deposited on silicon wafer surfaces as calibration standard for organic matter by X-ray spectrometry and XPS N2 - Polydimethylsiloxane (PDMS)is one of the most appearing contamination of medical devices.Dedicated analysis of PDMS on surfaces necessary, but the lack of calibration samples provides a bottle neck. There is a demand for metrological tools ensuring traceable and reliable analysis of mass deposition and of the chemical species of contaminants. Photoelectron spectroscopy (PES) and reference-free GIXRF can be used to qualify bench top instrumentation. Comparison of PES data and GIXRF data enable the establishment of a traceability chain. T2 - EXRS 2016, European Conference on X - ray Spectrometry CY - Gothenburg, Sweden DA - 19.06.2016 KW - Silicone analysis KW - XPS KW - GIXRF PY - 2016 AN - OPUS4-37295 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rackwitz, J. A1 - Kopyra, J. A1 - Dabkowska, I. A1 - Ebel, K. A1 - Rankovic, M. A1 - Milosavljevic, A. R. A1 - Bald, Ilko T1 - Sensitizing DNAtowards low-energy electrons with 2-fluoroadenine N2 - 2-Fluoroadenine (2FA) is a therapeutic agent, which is suggested for application in cancer radiotherapy. The molecular mechanism of DNA radiation damage can be ascribed to a significant extent to the action of low-energy (<20 eV) electrons (LEEs), which damage DNA by dissociative electron attachment. LEE induced reactions in 2FA are characterized both isolated in the gas phase and in the condensed phase when it is incorporated into DNA. Information about negative ion resonances and anion-mediated fragmentation reactions is combined with an absolute quantification of DNA strand breaks in 2FA-containing oligonucleotides upon irradiation with LEEs. The incorporation of 2FA into DNA results in an enhanced strand breakage. The strand-break cross sections are clearly energy dependent, whereas the strand-break enhancements by 2FA at 5.5, 10, and 15 eV are very similar. Thus, 2FA can be considered an effective radiosensitizer operative at a wide range of electron energies. KW - Ab initio calculations KW - Dissociative electron attachment KW - DNA origami KW - DNA radiation damage KW - Fludarabine PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/anie.201603464/full DO - https://doi.org/10.1002/anie.201603464 SN - 1433-7851 SN - 1521-3773 VL - 55 IS - 35 SP - 10248 EP - 10252 AN - OPUS4-37372 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe ED - Baier, Jennifa ED - Sahre, Mario ED - Weise, Matthias ED - Dähne, L. ED - Lerche, K.-H. T1 - Plasma Compatibility of Particles for Functional PVD-coatings by ex-situ Injection - Stability of Particles under Plasma Conditions N2 - The validation of the plasma compatibility of particles is a prerequisite for their application in plasma dispersion layers. The goal is the realization of functional add-on features on surfaces, in films and coatings. Although intended applications primarily address nanoparticles, the compatibility tests were carried out at first with particles in the lower micrometer range in order to investigate material-, fluorescent marker- or surface-based degradation effects in a simple manner. Plasma compatibility implies at least the short-term acceptance of charged species, plasma-UV radiation, vacuum and elevated temperatures. Otherwise, effects on geometrical dimensions, chemical bonds, fluorescence efficiency and plastic-elastic properties are expected. The plasma compatibility of monodisperse fluorescent-labeled particles to microwave excitation was evaluated by means of microscopic and spectroscopic investigation methods (light, fluorescence, confocal, atomic force microscopy and FTIR). This study comprises particles of different materials (SiO2, PMMA, PS, MF) and sizes (from 50 nm to 10 μm). A special preparation technique ensures that smallest geometry changes of particles can be measured by atomic force microscopy. For the selected plasma conditions (P = 600 W, f = 2.46 GHz, d = 10 cm) and an exposure time of 10 minutes, the geometry of SiO2 particles (approx. 1.7 μm) remains nearly unchanged, whereas PS particles shrink in diameter by 6% and PMMA particles by 11%. For selected core-particles (SiO2, MF) with fluorescencemarked (rhodamine) shell-polyelectrolytes no remarkable plasma degradation of the fluorescence intensity was observed for the above mentioned plasma conditions, however a doubling of exposure time already results in a significant decrease in intensity. Two different injection systems have been studied for the particle injection into the plasma deposition process. One of the selected systems also proves process compatibility regarding the expected pressure differences upon injection. T2 - PARTEC 2016, International Congress on Particle Technology CY - Nürnberg, Germany DA - 19.04.2016 KW - plasma dispersion layers KW - functional PVD coatings KW - particle injection PY - 2016 SN - 978-3-18-092283-6 SN - 0083-5560 SP - 6. Applications of Particle Technology/6.11_Beck_Uwe PB - VDI Wissensforum GmbH CY - Düsseldorf AN - OPUS4-37265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Ruiken, J.-P. A1 - Illner, M. A1 - Paul, Andrea A1 - Müller, D. A1 - Esche, E. A1 - Repke, J.-U. A1 - Maiwald, Michael T1 - Prozessanalytik für die moderne Verfahrenstechnik – Online-NMR- und -Raman-Spektroskopie im mizellaren Stoffsystem N2 - Homogen katalysierte Reaktionen sind wichtige Werkzeuge der chemischen Industrie. Milde Reaktionsbedingungen und hohe Selektivitäten führen zu einer energie- und ressourcenschonenden Produktion. Ein bedeutender Prozessschritt ist die Hydroformylierung. Hier kommen Kobalt- und Rhodiumkomplexe mit mehrzähnigen Liganden zum Einsatz, die zumeist in wässriger Lösung vorliegen. Die Anwendbarkeit beschränkt sich demnach auf kurzkettige Edukte mit hinreichender Wasserlöslichkeit. T2 - ProcessNet-Jahrestagung und 32. DECHEMA-Jahrestagung der Biotechnologen 2016 CY - Aachen, Germany DA - 12.09.2016 KW - Hydroformylierung KW - Prozessanalytik KW - Prozess-Spektroskopie KW - NMR-Spektroskopie KW - Raman-Spektroskopie KW - Mizellen PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/cite.201650219/epdf DO - https://doi.org/10.1002/cite.201650219 SN - 1522-2640 VL - 88 SP - 1304 EP - 1317 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-37316 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Meyer, Klas A1 - Paul, Andrea A1 - Maiwald, Michael T1 - Ugly Spectra and Lousy interfaces – Challenges for Compact NMR Spectroscopy in Process Control N2 - With the introduction of advanced process analytical technology, the closeness of key process variables to their limits can be directly controlled and the product can be classified or even released in real time. Compact NMR instruments can make NMR spectroscopy accessible in industrial and harsh environments for process control. T2 - ProcessNet-Jahrestagung und 32. DECHEMA-Jahrestagung der Biotechnologen 2016 CY - Aachen, Germany DA - 12.09.2016 KW - Online NMR Spectroscopy KW - Smart Sensors KW - Industrie 4.0 KW - Reaction Monitoring PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/cite.201650243/full DO - https://doi.org/10.1002/cite.201650243 SN - 1522-2640 VL - 88 SP - 1304 EP - 1317 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-37317 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moser, Marko T1 - Spectroscopic Quantification of Thiol Groups and Ligands on Nanomaterials N2 - Thiols have a high binding affinity to noble metals and semiconductor (SC) materials. Thiol ligands enable size control and tuning of the surface during the synthesis of nanoparticles (NP), significantly influence their physico-chemical and optical properties, and allow for their bioconjugation via further functional groups. Thus, simple, inexpensive, robust, and fast methods for the quantification of thiol groups and the characterization of thiol-modified or - stabilized nanomaterials including polymers are of considerable importance. T2 - Innovation Forum Senftenberg 2016 CY - Senftenberg, Germany DA - 01.06.2016 KW - Thiols KW - Ellman KW - Aldrithiol PY - 2016 AN - OPUS4-37243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moser, Marko T1 - Spectroscopic Quantification of Thiol Groups and Ligands on Nanomaterials N2 - Thiols have a high binding affinity to noble metals and semiconductor (SC) materials. Thiol ligands enable size control and tuning of the surface during the synthesis of nanoparticles (NP), significantly influence their physico-chemical and optical properties, and allow for their bioconjugation via further functional groups. Thus, simple, inexpensive, robust, and fast methods for the quantification of thiol groups and the characterization of thiol-modified or - stabilized nanomaterials including polymers are of considerable importance. T2 - Innovation Forum Senftenberg 2016 CY - Senftenberg, Germany DA - 01.06.2016 KW - Ellman KW - Aldrithiol KW - Thiols PY - 2016 AN - OPUS4-37245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moser, Marko T1 - Quantification of PEG-Maleimide Ligands and Coupling Efficiencies on Nanoparticles with Ellman’s Reagent N2 - Emissive nanoparticles (NP) are of ever increasing importance in nanotechnology, optical industries, and life sciences. Applicationrelevant properties determining particle performance and biocompatibility depend mainly on surface functional groups or ligands. Coating with polyethylene glycol (PEG) ligands enhances hydrophilicity and biocompatibility of nanomaterials, and enables subsequent binding of biomolecules. Hence, PEGylated particles must be carefully engineered and monitored with simple and fast methods. T2 - 9th Meeting of Engineering of Functional Interfaces CY - Wildau, Germany DA - 03.07.2016 KW - PEG-Maleimide KW - Ellman PY - 2016 AN - OPUS4-37247 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winkelmann, Aimo T1 - Improved analysis of EBSD patterns N2 - The presentation demonstrates how crystal structures can be derived from EBSD patterns. T2 - EBSD Meeting CY - London, UK DA - 31.03.2014 KW - Electron backscatter diffraction KW - Kikuchi pattern KW - Crystal structure analysis PY - 2014 AN - OPUS4-37893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - Symmetry and Euler angles N2 - The relationship between Euler angles and symmetry-equivalent descriptions of crystal orientations are explained. T2 - EBSD Meeting CY - London, UK DA - 31.03.2014 KW - Electron backscatter diffraction KW - Crystal orientation KW - Euler angles KW - Crystal symmetry PY - 2014 AN - OPUS4-37894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Payton, E. A1 - Nolze, Gert T1 - The Backscatter Electron Signal as an Additional Tool for Phase Segmentation in Electron Backscatter Diffraction N2 - The advent of simultaneous energy dispersive X-ray spectroscopy (EDS) data collection has vastly improved the phase separation capabilities for electron backscatter diffraction (EBSD) mapping. A major problem remains, however, in distinguishing between multiple cubic phases in a specimen, especially when the compositions of the phases are similar or their particle sizes are small because the EDS interaction volume is much larger than that of EBSD, and the EDS spectra collected during spatial mapping are generally noisy due to time limitations and the need to minimize sample drift. The backscatter electron (BSE) signal is very sensitive to the local composition due to its atomic number (Z) dependence. BSE imaging is investigated as a complimentary tool to EDS to assist phase segmentation and identification in EBSD through examination of specimens of meteorite, Cu dross, and steel oxidation layers. The results demonstrate that the simultaneous acquisition of EBSD patterns, EDS spectra, and the BSE signal can provide new potential for advancing multiphase material characterization in the scanning electron microscope. KW - Electron backscatter diffraction KW - Energy dispersive x-ray spectroscopy KW - Scanning electron microscopy KW - Multiphase microstructure KW - Phase identification KW - Backscattered electron imaging KW - Meteorite KW - Monte Carlo simulation PY - 2013 DO - https://doi.org/10.1017/S1431927613000305 VL - 19 IS - 4 SP - 929 EP - 941 AN - OPUS4-37895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Schäfer, N. A1 - Abou-Ras, D. T1 - Raman microspectroscopy provides access to compositional and microstructural details of polycrystalline materials N2 - This overview article provides insight into how to apply Raman spectroscopy in combination with a confocal, optical microscope setup on polycrystalline material systems, in order to obtain quantitative information on phase distribution, grain sizes, crystal orientations and microstrain. Although the present work uses Cu(In,Ga)(S,Se)₂ absorber layers in corresponding thin-film solar cells as a model system to demonstrate the capabilities of Raman microspectroscopy, the approaches discussed may be applied to any organic or inorganic, polycrystalline materials system. KW - Raman microscopy KW - Microstructure KW - Microspectroscopic imaging KW - Polycrystalline materials PY - 2016 SN - 0966-0941 VL - 28 IS - 5 SP - 16 EP - 20 PB - Wiley AN - OPUS4-37929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stockmann, Jörg M. T1 - Conventional Single-Sample vs. Multiple-Sample Hardness Testing: Tensile Testing Machine vs. Centrifuge N2 - The paper addresses the “Conventional Single-Sample vs. Multiple-Sample Hardness Testing: Hardness Testing Machine vs. Centrifuge” and the follow points are discussed in more detail: Principle of the centrifuge test, components of the centrifuge test, indenter geometries, microscopic measurement of Brinell and Vickers indents, and hardness testing: conventional vs. centrifuge. T2 - LUM, International Workshop Dispersion Analysis & Materials Testing 2016 CY - Berlin, Germany DA - 26.10.2016 KW - Hardness testing KW - Brinell KW - Vickers KW - Centrifuge technology PY - 2016 AN - OPUS4-37930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Hielscher, R. A1 - Winkelmann, Aimo T1 - Electron backscatter diffraction beyond the mainstream N2 - We present special applications of electron backscatter diffraction (EBSD) which aim to overcome some of the limitations of this technique as it is currently applied in the scanning electron microscope. We stress that the raw EBSD signal carries additional information which is useful beyond the conventional orientation determination. The background signal underlying the backscattered Kikuchi diffraction (BKD) patterns reflects the chemical composition and surface topography but also contains channeling-in information which is used for qualitative real-time orientation imaging using various backscattered electron signals. A significantly improved orientation precision can be achieved when dynamically simulated pattern are matched to the experimental BKD patterns. The breaking of Friedel’s rule makes it possible to obtain orientation mappings with respect to the point-group symmetries. Finally, we discuss the determination of lattice parameters from individual BKD patterns. Subgrain structure in a single quartz grain. The increased noise level in the left map reflects the lower precision of a standard orientation determination using band detection by the Hough transform. The right map results from the same experimental raw data after orientation refinement using a pattern matching approach. The colors correspond an adapted inverse pole figure color key with a maximum angular deviation of about 2° from the mean orientation. KW - Electron backscatter diffraction PY - 2017 DO - https://doi.org/10.1002/crat.201600252 SN - Online 1521-4079 VL - 52 IS - 1 SP - Special Issue - Article Number: UNSP 1600252, 1 EP - 24 PB - WILEY-VCH AN - OPUS4-37935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Siebler, Daniel A1 - Heinze, K. T1 - Conformational stability of oligoferrocene oligoamide foldamers N2 - Organometallic oligoamides built from three to four ferrocene amino acid units (H-Fca-OH,1-amino-1'-ferrocene carboxylic acid) fold into hydrogen bonded secondary structures featuring eight-membered rings by cooperative hydrogen bonds. NMR studies and DFT calculations (CAM-B3LYP, LANL2DZ, IEFPCM (THF) reveal that the organometallic zigzag foldamer structures are highly resistant toward denaturation by hydrogen bond acceptors such as dimethyl sulfoxide and 2,4-lutidine. Replacing one ferrocene amino acid unit by the organic alpha-amino acid glycine at the C-terminal end (Fca goes to Gly) significantly destabilizes the secondary zigzag structure facilitating denaturation by DMSO. Highly stabilized ordered poly(Fca) architectures are very attractive for future applications of switchable hydrogen-bonded redox-active materials. KW - Secondary structure KW - Conformational analysis KW - Ferrocene KW - Foldamers KW - Hydrogen bonds PY - 2016 DO - https://doi.org/10.1016/j.organchem.2016.02.032 SN - 0022-328X VL - 821 SP - 19 EP - 24 PB - Elsevier B.V. AN - OPUS4-37961 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dippong, Martin T1 - Fraunhofer Life Science Day N2 - Their high affinity, selectivity and specificity make monoclonal antibodies (mAbs) very important tools in research, diagnostics and therapy. The production of mAbs is routinely performed by hybridoma technique. Hybridomas are generated by fusing antibody-producing B cells with indefinitely proliferating myeloma cells. Both, cell fusion and the indispensable identification and isolation of the desired antibody-producing hybridoma clone is still far from being trivial. We describe a novel method that should help to optimize the cell fusion, and the screening for antibody-secreting hapten-specific hybridoma cells by using fluorescence activated cell sorting and single-cell fusion. Hybridoma cells specific for a hapten were incubated with a hapten-peroxidase conjugate (hapten-HRP), which was subsequently incubated with a fluorophore-labeled polyclonal anti-peroxidase antibody (anti-HRP-Alexa Fluor® 488). To characterize the expression of membrane-bound immunoglobulin G (IgG) a fluorophore-labeled anti-mouse IgG antibody (anti-IgG-Alexa Fluor® 647) was used. Successful staining was verified by confocal laser scanning microscopy (CLSM). We show that it is possible to specifically label hapten-specific hybridoma cells. It should also be possible to use this labelling approach for the isolation of hapten-specific B cells from the spleen and use these cells for single-cell fusion. Parallelized cell fusion chips were developed to increase fusion efficiencies. T2 - Fraunhofer Life Science Day 2015 CY - Leipzig, Germany DA - 03.07.2015 KW - Single-cell fusion KW - Hybridoma KW - Monoclonal antibodies PY - 2015 AN - OPUS4-37872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martin, S. A1 - Walnsch, A. A1 - Nolze, Gert A1 - Leineweber, A. A1 - Léaux, F. A1 - Scheuerlein, C. T1 - The crystal structure of (Nb0.75Cu0.25)Sn-2 in the Cu-Nb-Sn system N2 - During the processing of superconducting Nb3Sn wire, several intermediate intermetallic phases including a previously encountered Cu-Nb-Sn phase show up. The yet unknown crystal structure of this phase is now identified by a combination of different experimental techniques and database search to be of the hexagonal NiMg2 type with a proposed composition of about (Nb0.75Cu0.25)Sn2. The structure determination started from an evaluation of the lattice parameters from EBSD Kikuchi patterns from quenched material suggesting hexagonal or orthorhombic symmetry. A database search then led to the hexagonal NiMg2 type structure, the presence of which was confirmed by a Rietveld analysis on the basis of high energy synchrotron X-ray powder diffraction data. Assuming a partial substitution of Nb in orthorhombic NbSn2 by Cu, the change of the valence electron concentration provokes a structural transformation from the CuMg2 type for NbSn2 to the NiMg2 type for (Nb0.75Cu0.25)Sn2. In the previous literature the (Nb0.75Cu0.25)Sn2 phase described here has occasionally been referred to as Nausite. KW - Electron backscatter diffraction KW - X-ray diffraction KW - Intermetallic compound KW - Structure solution KW - Superconductor PY - 2017 DO - https://doi.org/10.1016/j.intermet.2016.09.008 SN - 0966-9795 SN - 1879-0216 VL - 80 SP - 16 EP - 21 PB - Elsevier Ltd. AN - OPUS4-37874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - Computational Advances N2 - The EBSD signal provides more information than the used Kikuchi pattern. The presentation discusses several parts of the detected signal and how they can be interpreted. T2 - EBSD 2014 CY - Pittsburgh, Pennsylvania, USA DA - 17.06.2014 KW - Electron backscatter diffraction KW - Simulation KW - Kikuchi pattern KW - Magnetite KW - Maghemite KW - Hematite PY - 2014 AN - OPUS4-37899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - Fast Orientation Projection using OpenGL N2 - Electron backscatter diffraction produces an enormous number of single orientation data which need to be processed but also visualized. The presentation shows that standard hardware can be used to increase the presentation speed considerably. T2 - EBSD 2012 CY - Pittsburgh, Pennsylvania, USA DA - 19.06.2012 KW - electron backscatter diffraction KW - OpenGL KW - crystal orientation KW - pole figure PY - 2012 AN - OPUS4-37900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Payton, E. T1 - The BSE signal as an additional tool for phase assignment in EBSD N2 - The presentation demonstrates how the background signal of EBSD patterns can be used for a rough assignment of phases which cannot distinguished by the diffraction signal. T2 - EBSD 2012 CY - Pittsburgh, Pennsylvania, USA DA - 19.06.2012 KW - Electron backscatter diffraction KW - Backscattered electrons KW - Kikuchi pattern KW - Phase distribution KW - Phase separation KW - Phase recognition PY - 2012 AN - OPUS4-37901 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lahcini, M. A1 - Weidner, Steffen A1 - Oumayama, J. A1 - Scheliga, F. A1 - Kricheldorf, H. R. T1 - Unsaturated Copolyesters of Lactide N2 - Four classes of unsaturated copolyesters of L-lactide were prepared either from isosorbide or bis(hydroxymethyl)tricyclodecane in combination with fumaric acid or from 1,4-butenediol or 1,4- butynediol with terephthalic acid. All syntheses were performed in such a way that lactide was oligomerized with a diol as the initiator and the resulting oligomers were polycondensed with a dicarboxylic acid dichloride either in a one-pot synthesis or in a two-step procedure. For most copolyesters the SEC measurements gave weight average molecular weights in the range of 30–60 kg mol⁻1 and dispersities in the range of 4.2–6.2. The MALDI-TOF mass spectra displayed a high content of cycles and indicated an irreversible kinetic course of all polycondensations. Glass-transition temperatures (Tg) above 90 °C were only found for two copolyesters of isosorbide. Addition of bromine to copolyesters of 1,4-butenediol yielded flame retarding biodegradable polymers. KW - Copolyester KW - MALDI-TOF MS KW - SEC KW - Lactide PY - 2016 DO - https://doi.org/10.1039/c6ra16008e VL - 2016/6 IS - 96 SP - 93496 EP - 93504 PB - Royal Society of Chemistry AN - OPUS4-37913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Siebler, Daniel A1 - Rohwetter, Philipp A1 - Brusenbach, R. A1 - Plath, R. T1 - Optical-only detection of partial discharge with fluorescent polymer optical fiber sensors N2 - This paper reflects recent progress in the field of fluorescent polymer optical fiber sensors (F-POF) for partial discharge (PD) detection in high voltage (HV) cable accessories using optical-only PD detection by coincidence single photon counting. In experiments with artificial PD sources these sensors show the ability to detect optical emissions from picocoulomb-level PDs in a real-scale model of a translucent high voltage cable accessory. False positives (caused by detector noise) are efficiently suppressedwhile maintaining sufficient sensitivity,even when the sensor is located in an unfavorable position. T2 - EUROSENSORS 2015 CY - Freiburg, Germany DA - 06.09.2015 KW - Partial discharge KW - Silicone rubber KW - High voltage cable accessories KW - Polymer optical fiber POF KW - Fluorescence KW - Coincidence PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-337881 DO - https://doi.org/10.1016/j.proeng.2015.08.711 SN - 1877-7058 VL - 120 SP - 845 EP - 848 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-33788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klykov, Oleg A1 - Weller, Michael G. T1 - Quantification of N-hydroxysuccinimide and N-hydroxysulfosuccinimide by hydrophilic interaction chromatography (HILIC) N2 - N-Hydroxysuccinimide (NHS) esters are the most important activated esters used in many different bioconjugation techniques, such as protein labelling by fluorescent dyes and enzymes, surface activation of chromatographic supports, microbeads, nanoparticles, and microarray slides, and also in the chemical synthesis of peptides. Usually, reactions with NHS esters are very reliable and of high yield, however, the compounds are sensitive to air moisture and water traces in solvents. Therefore, the quantification of NHS would be a very helpful approach to identify reagent impurities or degradation of stored NHS esters. No robust and sensitive method for the detection of NHS (or the more hydrophilic sulfo-NHS) has been reported yet. Here, a chromatographic method based on HILIC conditions and UV detection is presented, reaching a detection limit of about 1 mg L-1, which should be sensitive enough for most of the applications mentioned above. Exemplarily, the hydrolytic degradation of a biotin-NHS ester and a purity check of a fluorescent dye NHS ester are shown. An important advantage of this approach is its universality, since not the structurally variable ester compound is monitored, but the constant degradation product NHS or sulfo-NHS, which avoids the necessity to optimize the separation conditions and facilitates calibration considerably. KW - NHS KW - Sulfo-NHS KW - NHS-Ester KW - Qualitätskontrolle KW - Reinheitsbestimmung KW - HPLC PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-337833 DO - https://doi.org/10.1039/c5ay00042d SN - 1759-9660 SN - 1759-9679 VL - 7 IS - 15 SP - 6443 EP - 6448 PB - RSC Publ. CY - Cambridge AN - OPUS4-33783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Dohse, Elmar A1 - Bartusch, Jürgen A1 - Kreutzbruck, Marc T1 - Luftultraschallprüfung von CFK mit planaren und fokussierenden Wandlern N2 - Für die Prüfung von Leichtbaustrukturen ist in den letzten Jahren ein vermehrter Einsatz der Luftultraschallprüfung zu verzeichnen. Insbesondere eignet sich Luftultraschall für die Prüfung von Faserkunststoffverbunden und hybrider Werkstoffverbunde, die ihre Anwendung in der Automobilindustrie und Luftfahrt finden. Für den Bau von marktüblichen Luftultraschall-Wandlern werden Piezokomposite mit Anpassschichten versehen. Ihre Herstellung ist allerdings sehr anspruchsvoll und die erreichbaren Signal-Rausch-Abstände sind für viele Prüfprobleme als noch nicht ausreichend einzustufen. Zwecks gesteigerter Effizienz beim Schallübertrag in die Luft wurden Luftultraschall-Sender und -Empfänger aus zellulärem Polypropylen entwickelt. Dieses piezoelektrische Material ist aufgrund seiner geringer Dichte und seiner sehr geringen Schallgeschwindigkeit an die niedrige akustische Impedanz der Luft deutlich besser angepasst, als die üblicherweise verwendeten Anpassschichten. Letztere können bei Polypropylen-Wandlern daher gänzlich vermieden werden. In diesem Beitrag wird Luftultraschall-Prüfung an zwei verschiedenen CFK-Testkörpern vorgestellt: an einer Platte mit T-Stringern aus dem Seitenleitwerk eines Flugzeugs und an einer Platte mit künstlich eingebrachten Fehlern. Es wurde mit unterschiedlichen planaren und fokussierenden Wandlern geprüft. Marktübliche Wandler mit Anpassschichten wurden mit den selbstentwickelten Wandlern aus zellulärem Polypropylen verglichen. Der Signal-Rausch-Abstand und die laterale Auflösung wurden sowohl im Prüfaufbau mit senkrechter Einschallung als auch mit Schrägeinschallung gemessen. Die Ergebnisse zeigen, dass die Schrägeinschallung zwar den Signal-Rauschabstand erhöht, aber die laterale Auflösung verschlechtern kann. T2 - DACH Jahrestagung 2015 CY - Salzburg, Austria DA - 11.05.2015 PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-349751 UR - http://jt2015.dgzfp.de/Portals/jt2015/BB/mi1a3.pdf SP - Mi.1.A.3-1 EP - Mi.1.A.3-9 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-34975 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane T1 - Einzelblitz vs. Multiblitz - Blitzthermografie mit mehreren Blitzen N2 - Die Blitzthermografie weist eine Reihe von Vorteilen gegenüber anderen Verfahren der aktiven Thermografie auf und hat daher eine relativ große Verbreitung in Forschung und Industrie gefunden. Ein wesentlicher Nachteil ist jedoch die begrenzte Energie, die pro Blitz genutzt werden kann. Es stellt sich die Frage, ob sich durch mehrere kurz hintereinander ausgeführte Blitze eine Verbesserung des Energieeintrags erreichen lässt. Zur experimentellen Untersuchung dieser Frage wurde ein Versuchsstand mit vier Blitzlampen so umgerüstet, dass die Blitzlampen zeitgleich oder nacheinander mit einer regelbaren Verzögerung ausgelöst werden können („Multiblitz“). Als Probekörper dienten Platten aus CFK, an deren Rückseite Flachbodenbohrungen (FBB) eingebracht worden waren. Betrachtet wurde jedoch nur der absolute Temperaturhub am ungestörten Material. Die Experimente zeigen relativ geringe Effekte im Prozentbereich, wie sie auch gemäß einer quantitativen Abschätzung zu erwarten sind. Interessanterweise vergrößerte sich der Einfluss der Multiblitzanregung auf die Energieeinkopplung deutlich bei einem etwas vergrößerten Abstand zwischen Blitzlampen und untersuchter Oberfläche. Die Ursache für diesen Effekt ist derzeit unklar, vermutet werden eine Temperaturabhängigkeit und/oder eine Abstandsabhängigkeit des Wärmübergangskoeffizienten im Konvektionsterm. T2 - Thermographie-Kolloquium 2015 CY - Leinfelden-Echterdingen, Germany DA - 01.10.2015 KW - Thermografie KW - Blitzthermografie KW - Konvektion KW - Wärmeverluste KW - Einkoppeleffizienz KW - Energiekopplung PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-345487 SN - 978-3-940283-74-0 VL - 154 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-34548 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mönch, Bettina A1 - Kraus, Werner A1 - Köppen, Robert A1 - Emmerling, Franziska T1 - The different conformations and crystal structures of dihydroergocristine N2 - The identification of different forms of dihydroergocristine (DHEC) was carried out by crystallization from different organic solvents. DHEC was identified as potential template for molecularly imprinted polymers (MIPs) for the epimeric specific analysis of ergot alkaloids (EAs) in food. DHEC was crystallized from different solvents in order to mimic the typical MIP synthesis conditions. Four new solvatomorphs of DHEC were obtained. All solvatomorphs contain a water molecule in the crystal structure, whereas three compounds contain an additional solvent molecule. Based on the conformation of DHEC a comparison with typical EA molecules was possible. The analysis showed that DHEC is a suitable template for MIPs for EAs. PY - 2016 DO - https://doi.org/10.1016/j.molstruc.2015.10.008 SN - 0022-2860 SN - 1872-8014 SN - 0377-046X VL - 1105 SP - 389 EP - 395 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-35009 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilsch, Gerd A1 - Eichler, T. A1 - Millar, Steven A1 - Gottlieb, Cassian T1 - Quantitative determination of chloride-to-cement content of concrete by laser-induced breakdown spectroscopy (LIBS) N2 - Laser-induced breakdown spectroscopy (LIBS) is a combination of plasma generation on the sample surface by a high power laser pulse and optical emission spectroscopy (OES). It is a direct measurement method without an extensive sample preparation. Concrete is a multi phase system. With LIBS it is possible to distinguish the different phases and based on that to correlate the chloride content to the cement mass. This is done by scanning the surface with a resolution of up to 0.1 mm. The high measurement frequency of 100 Hz or even higher allows the in-situ visualization of the chloride content over the measured area. With a calibration a quantification of chloride concentration is possible. As an example the LIBS measurement on a 50 mm by 70 mm area with a resolution of 0.5 mm and the visualization of the chloride distribution takes only 10 minutes. Additionally it is possible to evaluate the carbonation depth from the same measurement. Examples of practical application to determine the chloride-to-cement-content on concrete samples are presented. The possibilities and the limitations of LIBS are discussed. T2 - CONCREEP 10 - Mechanics and physics of creep, shrinkage, and durability of concrete and concrete structures CY - Vienna, Austria DA - 21.09.2015 KW - LIBS KW - Chlorides KW - Carbonation KW - Heterogeneity KW - Quantitative concentration KW - 2D-map PY - 2015 SP - 815 EP - 822 AN - OPUS4-34677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Krüger, Simone A1 - Raspe, Tina A1 - Despinasse, Marie-Claire A1 - Moritz, W. A1 - Nörthemann, K. T1 - Wasserstoffsensoren zur früheren Branddetektion - Systematische Untersuchungen zur Wasserstoffgenerierung bei Schwelbränden und Entwicklung eines Wasserstoffsensors zur Brandfrüherkennung einschließlich Vergleich mit anderen Branddetektionssystemen N2 - Wasserstoff als Brandprodukt entsteht in einer sehr frühen Brandphase, insbesondere bei Schwelbränden. Durch die Entwicklung eines geeigneten Wasserstoffsensors ist es nicht nur möglich, sehr frühzeitig einen entstehenden Brand zu detektieren, sondern durch die Erkennung eines Entstehungsbrandes und frühzeitiger Löschmaßnahmen ergibt sich eine Vermeidung von Personen- und Sachschäden. Die sich in der Entwicklung befindlichen Wasserstoffsensoren wurden von der TLTS GmbH zur Verfügung gestellt. Im Rahmen dieses Projektes wurden diese Sensoren in verschiedenen Testbränden, d.h. sowohl im Labormaßstab, in der Rauchkammer, als auch in Realbrandszenarien in einer 2-Raum-Containerwohnung mit verschiedenen wohnungstypischen Materialien und Gebrauchsgegenständen getestet, insbesondere in Kombination mit anderen analytischen Methoden und im Vergleich mit anderen Detektionssystemen. Der Schwerpunkt lag in der Rauchgaskomponentendetektion in der frühen Brandphase, insbesondere der Wasserstoffgenerierung in Abhängigkeit des Brandszenarios. Es erfolgten umfangreiche Untersuchungen bezüglich der Korrelation von Brandmaterialien, thermischen Bedingungen, Strömungsverhältnissen und geometrischen Bedingungen zur Wasserstoffgenerierung, ihrem zeitlichen Verlauf und der Relation zu anderen entstehenden Gasen (z.B. Kohlenstoffmonoxid) und der Rauchentwicklung unter exakt definierten (reproduzierbaren) Brandentstehungsbedingungen. Dadurch wurde eine quantifizierbare Bewertung des Wasserstoffsensors gegenüber bestehenden Systemen erreicht. Aus den Untersuchungen sind ebenfalls Schlussfolgerungen zu den Vorteilen und Grenzen der Implementierung von Wasserstoffsensoren in Multisensor-Brandmelder ableitbar. Es konnte anhand der Testbrände gezeigt werden, dass der H2-Sensor bei Schwelbrandversuche von wohnungstypischen Materialien geeignet ist und ein sehr frühzeitiger Nachweis sehr geringer H2-Konzentrationen, noch bevor Rauch und CO detektiert werden können, möglich ist und diese somit eine Alternative oder Ergänzung zu traditionellen Rauch- und CO-Meldern für mehr Sicherheit sind. Für den kommerziellen Einsatz dieser Sensoren müssen die Einflussfaktoren, wie z.B. mit der Luftfeuchtigkeit und Querempfindlichkeiten, wie z.B. mit anderen Brandgasen, wie CO weiter verbessert werden. KW - Wasserstoffsensoren KW - Branddetektion PY - 2016 SN - 978-3-9817502-9-4 VL - 2016 SP - 1 EP - 184 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35773 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Harald T1 - Core-shell systems - different cases N2 - Coating, stabilization layers, functionalization of particles or simple contamination are common variants of a core-shell system. For smaller nanoparticles this is of major importance. A particle with 16 nm diameter and a usual surface layer of 2 nm will have the same volume for the core as for the shell. In this case the material of the particle doesn’t have a clear definition. It is a common case that a particle consists of four different layers: Core, shell, stabilization layer and contamination. The properties of the particles differ according to this structure. For example silver particles might have a different dissolution rate for pure particles and for particles which are grown on top of a core. Different solubility or defined other properties of materials is a common reason for producing core-shell systems. Gold cores are surrounded by silica to stabilize them or to get a defined distance between the cores. Silica might be surrounded by gold and the silica dissolved afterwards. This delivers hollow shells. Another important example for core-shell systems are quantum dots. A small core is surrounded by a different material for increasing the photoluminescence. Furthermore there a stabilization layer is needed. The smallest part of the final particles is the initial core. The photoluminescence is based on this core, but the shells contain much more material. Categorization should address this. Core-shell systems are not covered by most of the existing decision trees for grouping. They are either regarded as special case or a singular layer. This disqualifies core-shell systems for grouping within the common models. There might be a very easy way to avoid this problem and even to combine some of the different decision trees. Starting the decision tree with the solubility of the outer shell and subsequently addressing the inner layers will be a pragmatic approach to solve the problem. If there is no shell, the categorization can start with a tiered approach or with the proposed “stawman” chemical categorization. If a shell is covering the surface there is a need to check if the shell is stable. If it is stable, the particle can be categorized based on this shell. If it is soluble, the ions need to be addressed as in the classic case. Furthermore the shell might increase the uptake by the cells. If the ions and the uptake are not critical the categorization can continue with the next layer. With this not perfect but pragmatic approach, the surface layers can be addressed with very limited additional efforts. Most criteria are based on classically tabulated data. Including a rating system like the precautionary matrix approach might even address the fact that some parameters are not always Yes/No, e.g. solubility, ion toxicity and uptake. T2 - OECD Expert Meeting on Grouping and Read Across for the Hazard Assessment of Manufactured Nanomaterials CY - Brussels, Belgium DA - 13.04.2016 KW - OECD KW - Nanoparticles KW - Nanomaterials KW - Grouping KW - Nano PY - 2016 AN - OPUS4-35774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radtke, Martin A1 - Buzanich, Günter A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Scharf, O. A1 - Scholz, Philipp A1 - Guerra, M.F. T1 - Double Dispersive X-Ray Fluorescence (D2XRF) based on an Energy Dispersive pnCCD detector for the detection of platinum in gold N2 - With the aim of improving limits of detection (LOD) of trace elements in a matrix with adjacent fluorescence energies, a simple double dispersive X-ray fluorescence detection system (D2XRF) was constructed to operate at the beamlines BAMline and the mySpot @ BESSY II. This system is based on the combination of a crystal analyzer with an energy resolving single photon counting pnCCD. Without further collimators, the efficient suppression of the background by the pnCCD and the good energy resolution of the crystal results in improved LOD. In first order reflections, an energy resolution of 13 eV for Cu Kα was reached, and an energy range of 1 keV was covered in one shot. This new system was applied to the detection of platinum (Pt) in gold leaves with a LOD of 0.9 mg/kg, which is the lowest attained by totally non-destructive methods nowadays. The presence of Pt in gilded objects from Abydos and Byzantine mosaics provides vital information, as it indicates the alluvial origin of the gold for these examples. KW - Platinum Wavelength dispersive D2XRF KW - Gold Synchrotron XRF PY - 2016 DO - https://doi.org/10.1016/j.microc.2015.10.039 VL - 125 SP - 56 EP - 61 PB - Elsevier Science CY - Amsterdam AN - OPUS4-35777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sauer, Andreas A1 - Scharf, Holger A1 - Becker, Roland T1 - Bericht zum 17. BAM-Ringversuch "Altlasten" N2 - Präsentation der Ergebnisse eines Ringversuchs zur Kompetenzbewertung von Prüflaboratorien auf dem Gebiet der anorganischen und organischen Bodenanalytik. KW - Eignungsprüfung KW - Boden KW - PAK KW - MKW KW - AOX KW - Spurenelemente KW - Gesamtcyanid KW - Proficiency testing KW - Soil KW - PAH KW - TPH KW - Trace elements KW - Total cyanide PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-357785 SP - 1 EP - 212 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35778 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lehmann, Andreas T1 - Matrixeinflüsse bei der Bestimmung von Arzneimittelrückständen mittels LC-MS/MS in Oberflächenwasserproben bei Konzentrationen im ppt-Bereich N2 - Zur Bestimmung von Arzneimittelrückständen in Oberflächengewässern wird häufig die LC-MS/MS als Methode der Wahl eingesetzt. Obwohl sich dieses Nachweisverfahren durch eine hohe Empfindlichkeit und Selektivität auszeichnet, gibt es vor allem bei geringen Substanzkonzentrationen häufig störende Einflüsse durch Matrixeffekte. Diese Matrixeffekte können unterschiedliche Ursachen haben. Einige Matrixeffekte werden am Beispiel des Wirkstoffs Carbamazepin erläutert. Carbamazepin wird durch Kläranlagen nur partiell aus dem Abwasser entfernt und ist im Spurenbereich auch noch im Trinkwasser nachzuweisen. Wenn für die LC-MS/MS wasserbasierte Anteile in der mobilen Phase genutzt werden, befinden sich trotz Verwendung einer Labor-Reinstwasseranlage in der mobilen Phase noch kleinste Konzentrationen von Carbamazepin, welche einen Blindwert im unteren ppt-Bereich verursachen. Weitere Matrixeffekte treten durch die unterschiedliche Qualität der Oberflächenwasserproben auf. Koelutionen von weiteren Inhaltstoffen zeitgleich mit dem Zielanalyten führen zu einer Diskriminierung des Meßsignals. Verbindungen, die den gleichen Massenübergang bei nahezu identischer Retentionszeit zeigen, erfordern eine reproduzierbare chromatographische Vortrennung oder die Wahl einer alternativen HPLC-Säule. T2 - ANAKON 2015 CY - Graz, Austria DA - 23.03.2015 KW - Arzneimittelrückstände in Oberflächenwasserproben KW - HPLC-MS/MS KW - Massenspektrometrie KW - Carbamazepin PY - 2015 AN - OPUS4-35793 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - From k-values to elemental composition by EMPA (EDX & WDX) N2 - k-values (k-ratio, K-value) is defined as ratio of the X-ray photon intensity I measured for a particular characteristic peak from the unknown sample to the value measured for the same X-ray peak from a reference material of known composition under identical conditions of beam energy, spectrometer efficiency and electron dose. T2 - CCQM - Surface and Micro/Nano Analysis Working Group (SAWG) Meeting for 2016 CY - Paris, France DA - 19.04.2016 KW - k-values KW - EPMA KW - EDX KW - WDX PY - 2016 AN - OPUS4-35794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hea, Y. A1 - Esteban-Fernandez, Diego A1 - Neumann, B. A1 - Bergmann, U. A1 - Bierkandt, Frank A1 - Linscheid, M. W. T1 - Application of MeCAT-Click labeling for protein abundance characterization of E. coli after heat shock experiments N2 - In a proof of concept study, metal-coded affinity tags based on click chemistry (MeCAT-Click) were used to analyze the proteome of Escherichia coli (E. coli) in response to heat stress. This allows high labeling efficiency, high detection sensitivity, and multiplex capabilities, which are pivotal for its application to protein quantification. Two approaches are presented for relative quantification of differentially lanthanide-labeled proteins. The first approach uses isotope-labeling, where ESI-MS was utilized to quantify the differentially labeled proteins from different states of E. coli. With this approach, 14 proteins were found with changed abundance, among them five proteins upregulated. In the second approach, differentially labeled samples were separated by two dimensional gel electrophoresis (2 DE) and scanned by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Comparison of the signal intensities of the different lanthanides was used to quantify different sample states. Based on this information, ESI-MS was used to identify the proteins with different abundance. The sensitivity of LA-ICP-MS allowed us to find one upregulated protein that was nearly invisible by silver staining ("Probable replication endonuclease from retron EC67"). The advantage of this approach is to locate low abundant proteins with differential expression using LA-ICP-MS, which may be overlooked otherwise. Biological significance: This paper demonstrates the successful application of a novel metal labeling strategy to quantify the proteins from complex biological samples. In comparison with former metal labeling strategies, it reduces the steric hindrance and improves the labeling efficiency during the labeling process, which ensure its successful application. This methodology is compatible with both molecular and elemental mass spectrometry. ESI-MS/MS in combination with software-based search allows the identification and relative quantification of labeled proteins. In addition, LA-ICP-MS helps to locate the labeled proteins in 2-DE gels with superior detection capability, thus, target proteins with low abundance can be precisely followed. Its excellent sensitivity allows one to track the proteins of interest that are barely visible by silver staining. KW - Protein quantification KW - Heat shock response KW - Ln-MeCAT-Click labeling KW - nanoLC-ESI-MS/MS KW - 2-D electrophoresis KW - LA-ICP-MS PY - 2016 DO - https://doi.org/10.1016/j.jprot.2015.12.010 SN - 1874-3919 VL - 136 SP - 68 EP - 76 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-35837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hartmann, S A1 - Sturm, Heinz A1 - Blaudeck, T A1 - Hoelck, O A1 - Hermann, S A1 - Schulz, SE A1 - Wunderle, B. T1 - Experimental and computational studies on the role of surface functional groups in the mechanical behavior of interfaces between single-walled carbon nanotubes and metals N2 - To study the mechanical interface behavior of single-walled carbon nanotubes (CNTs) embedded in a noble metal, we performed CNT-metal pull-out tests with in situ scanning electron microscope experiments. Molecular dynamics (MD) simulations were conducted to predict force-displacement data during pull-out, providing critical forces for failure of the system. In MD simulations, we focused on the influence of carboxylic surface functional groups (SFGs) covalently linked to the CNT. Experimentally obtained maximum forces between 10 and 102 nN in palladium and gold matrices and simulated achievable pulling forces agree very well. The dominant failure mode in the experiment is CNT rupture, although several pull-out failures were also observed. We explain the huge scatter of experimental values with varying embedding length and SFG surface density. From simulation, we found that SFGs act as small anchors in the metal matrix and significantly enhance the maximum forces. This interface reinforcement can lead to tensile stresses sufficiently high to initiate CNT rupture. To qualify the existence of carboxylic SFGs on our CNT material, we performed analytical investigation by means of fluorescence labeling of surface species and discuss the results. With this contribution, we focus on a synergy between computational and experimental approaches involving MD simulations, nano scale testing, and analytics (1) to predict to a good degree of accuracy maximum pull-out forces of single-walled CNTs embedded in a noble metal matrix and (2) to provide valuable input to understand the underlying mechanisms of failure with focus on SFGs. This is of fundamental interest for the design of future mechanical sensors incorporating piezoresistive single-walled CNTs as the sensing element. KW - Oxygen-containing functionalities KW - Molecular-dynamics KW - Structural characterization KW - Reinforced composites KW - Raman spectroscopy KW - Shear strength KW - Polymer matrix KW - Pull-out KW - Simulation KW - Purification PY - 2016 DO - https://doi.org/10.1007/s10853-015-9142-6 SN - 0022-2461 SN - 1573-4803 VL - 51 IS - 3 SP - 1217 EP - 1233 AN - OPUS4-35795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer-Plath, Asmus A1 - Beckert, F A1 - Tölle, FJ A1 - Sturm, Heinz A1 - Mülhaupt, R T1 - Stable aqueous dispersions of functionalized multi-layer graphene by pulsed underwater plasma exfoliation of graphite N2 - A process was developed for graphite particle exfoliation in water to stably dispersed multi-layer graphene. It uses electrohydraulic shockwaves and the functionalizing effect of solution plasma discharges in water. The discharges were excited by 100 ns high voltage pulsing of graphite particle chains that bridge an electrode gap. The underwater discharges allow simultaneous exfoliation and chemical functionalization of graphite particles to partially oxidized multi-layer graphene. Exfoliation is caused by shockwaves that result from rapid evaporation of carbon and water to plasma-excited gas species. Depending on discharge energy and locus of ignition, the shockwaves cause stirring, erosion, exfoliation and/or expansion of graphite flakes. The process was optimized to produce long-term stable aqueous dispersions of multi-layer graphene from graphite in a single process step without requiring addition of intercalants, surfactants, binders or special solvents. A setup was developed that allows continuous production of aqueous dispersions of flake size-selected multi-layer graphenes. Due to the well-preserved sp(2)-carbon structure, thin films made from the dispersed graphene exhibited high electrical conductivity. Underwater plasma discharge processing exhibits high innovation potential for morphological and chemical modifications of carbonaceous materials and surfaces, especially for the generation of stable dispersions of two-dimensional, layered materials. KW - Exfoliation KW - Graphene KW - Aqueous dispersion KW - Solution plasma KW - Functionalization KW - Electrohydraulic effect KW - Shear exfoliation KW - Oxide-films KW - Water PY - 2016 DO - https://doi.org/10.1088/0022-3727/49/4/045301 SN - 0022-3727 VL - 49 IS - 4 SP - 045301-1 EP - 045301-11 AN - OPUS4-35796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Marc Benjamin A1 - Solomun, Tihomir A1 - Wellhausen, Robert A1 - Herrmann, S A1 - Seitz, H A1 - Meyer, Susann A1 - Kunte, Hans-Jörg A1 - Zeman, J. A1 - Uhlig, F A1 - Smiatek, J A1 - Sturm, Heinz T1 - Influence of the Compatible Solute Ectoine on the Local Water Structure: Implications for the Binding of the Protein G5P to DNA N2 - Microorganisms accumulate molar concentrations of compatible solutes like ectoine to prevent proteins from denaturation. Direct structural or spectroscopic information on the mechanism and about the hydration shell around ectoine are scarce. We combined surface plasmon resonance (SPR), confocal Raman spectroscopy, molecular dynamics simulations, and density functional theory (DFT) calculations to study the local hydration shell around ectoine and its influence on the binding of a gene-S-protein (G5P) to a single-stranded DNA (dT(25)). Due to the very high hygroscopicity of ectoine, it was possible to analyze the highly stable hydration shell by confocal Raman spectroscopy. Corresponding molecular dynamics simulation results revealed a significant change of the water dielectric constant in the presence of a high molar ectoine concentration as compared to pure water. The SPR data showed that the amount of protein bound to DNA decreases in the presence of ectoine, and hence, the protein-DNA dissociation constant increases in a concentration-dependent manner. Concomitantly, the Raman spectra in terms of the amide I region revealed large changes in the protein secondary structure. Our results indicate that ectoine strongly affects the molecular recognition between the protein and the oligonudeotide, which has important consequences for osmotic regulation mechanisms. KW - Aqueous solution KW - Biological structure KW - Raman spectroscopy KW - Organic osmolytes KW - High throughput KW - Gene-5 protein KW - Amino acid KW - Water structure PY - 2015 DO - https://doi.org/10.1021/acs.jpcb.5b09506 SN - 1520-6106 SN - 1089-5647 SN - 1520-5207 VL - 119 IS - 49 SP - 15212 EP - 15220 AN - OPUS4-35800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Lück, S. A1 - Schmidt, V. A1 - Grothausmann, R. A1 - Hilger, A. A1 - Manke, I. T1 - Missing wedge computed tomography by iterative algorithm DIRECTT N2 - A strategy to mitigate typical reconstruction artefacts in missing wedge computed tomography is presented. These artefacts appear as elongations of reconstructed details along the mean direction (i.e. the symmetry centre of the projections). Although absent in standard computed tomography applications, they are most prominent in advanced electron tomography and also in special topics of X-ray and Neutron tomography under restricted geometric boundary conditions. We investigate the Performance of the DIRECTT (Direct Iterative Reconstruction of Computed Tomography Trajectories) algorithm to reduce the directional artefacts in standard procedures. In order to be sensitive to the anisotropic nature of missing wedge artefacts, we investigate isotropic substructures of metal foam as well as circular disc models. Comparison is drawn to filtered backprojection and algebraic techniques. Reference is made to reconstructions of complete data sets. For the purpose of assessing the reconstruction Quality, Fourier transforms are employed to visualize the missing wedge directly. Deficient reconstructions of disc models are evaluated by a length-weighted boundary orientations. The DIRECTT results are assessd at different signal-to-noise ratios by means of local and integral evaluation Parameters. KW - Tomography KW - Algorithm KW - Reconstruction KW - Computed tomography KW - Electron tomography KW - Image morphology KW - Iterative reconstruction KW - Missing wedge PY - 2016 DO - https://doi.org/10.1111/jmi.12313 SN - 1365-2818 VL - 261 IS - 1 SP - 36 EP - 45 PB - Wiley CY - Hoboken, New Jersey, USA AN - OPUS4-35801 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mielke, Johannes T1 - Evaluation of particle sizing techniques for the implementation of the EC definition of a nanomaterial N2 - What is a nanomaterial? Beyond a pure academic interest, this question has substantial im-plications for consumer protection and regulatory purposes. The European Commission has recommended a definition of nanomaterial (2011/696/EU), which states that a given material is considered a nanomaterial if more than 50 % of the particles in the number size distribution have a smallest dimension between 1 and 100 nm. Although several well established particle sizing techniques exist, the implementation of this definition for any particulate material remains a metrological challenge. The European research project NanoDefine (http://www.nanodefine.eu) has the aim of pro-viding help for the implementation of the definition. One central task is the performance evaluation of the available particle sizing techniques. For this purpose, a wide variety of real world materials has been selected. All available sizing techniques, including imaging, mobility-based and static scattering techniques, independent whether being counting, fractionating, spectroscopic or integrally sizing, will be applied to all of the projects materials to test the techniques performance and to establish their ranges of applicability. Because most of the techniques do not measure in number metrics as required in the nanomaterial definition, the quality of the conversion to the number based particle size distribution is assessed as well. Special care is taken on suitable sample preparation procedures as one of the most chal-lenging issues towards reaching a highly accurate result. Within this contribution, first results of the performance testing of state of the art characterisation techniques on the unique set of NanoDefine real world materials are going to be presented. From these results, first conclu-sions about the material dependent ranges of applicability for the considered particle sizing techniques can be drawn. The technique specific advantages and shortcomings with respect to the application of the EC definition as well as the analytical challenges encountered will be highlighted. Acknowledgements: The research leading to these results has received funding from the European Community's Seventh Framework Programme (FP7/2007-2013) under grant agreement n° 604347. T2 - PARTEC CY - Nürnberg, Germany DA - 19.04.2016 KW - Nanomaterial PY - 2016 AN - OPUS4-35802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böckmann, H. A1 - Liu, S. A1 - Mielke, Johannes A1 - Gawinkowski, S. A1 - Walluk, J. A1 - Grill, L. A1 - Wolf, M. A1 - Kumagai, T. T1 - Direct observation of photoinduced tautomerization in single molecules at a metal surface N2 - Molecular switches are of fundamental importance in nature, and light is an important stimulus to selectively drive the switching process. However, the local dynamics of a conformational change in these molecules remain far from being completely understood at the single-molecule level. Here, we report the direct observation of photoinduced tautomerization in single porphycene molecules on a Cu(111) surface by using a combination of low-temperature scanning tunneling microscopy and laser excitation in the near-infrared to ultraviolet regime. It is found that the thermodynamically stable trans configuration of porphycene can be converted to the metastable cis configuration in a unidirectional fashion by photoirradiation. The wavelength dependence of the tautomerization cross section exhibits a steep increase around 2 eV and demonstrates that excitation of the Cu d-band electrons and the resulting hot carriers play a dominant role in the photochemical process. Additionally, a pronounced isotope effect in the cross section (∼100) is observed when the transferred hydrogen atoms are substituted with deuterium, indicating a significant contribution of zero-point energy in the reaction. Combined with the study of inelastic tunneling electron-induced tautomerization with the STM, we propose that tautomerization occurs via excitation of molecular vibrations after photoexcitation. Interestingly, the observed cross section of ∼10–19 cm2 in the visible–ultraviolet region is much higher than that of previously studied molecular switches on a metal surface, for example, azobenzene derivatives (10–23–10–22 cm2). Furthermore, we examined a local environmental impact on the photoinduced tautomerization by varying molecular density on the surface and find substantial changes in the cross section and quenching of the process due to the intermolecular interaction at high density. KW - STM KW - Pophycene PY - 2016 DO - https://doi.org/10.1021/acs.nanolett.5b04092 SN - 1530-6984 SN - 1530-6992 VL - 16 IS - 2 SP - 1034 EP - 1041 PB - ACS AN - OPUS4-35803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Asadujjaman, Asad T1 - Aggregation behavior of UCST-Type poly(acrylamide-co-acrylonitrile) copolymer across the phase transition temperature N2 - Thermoresponsive polymers have shown great potential in applications such as bioseparation, drug delivery and diagnostic. Only few thermoresponsive polymers that present an upper critical solution temperature (UCST) in a relevant temperature range, i.e. Phase separate from solution upon cooling, have been reported so far. Moreover, the most studied UCST type polymers namely polybetaines are difficult to use under physiological conditions, which significantly restricts their potential applications. Therefore, UCST polymers with sharp and robust phase transition in physiological conditions (in the presence of salts, ions etc.) are highly needed in order to extend the range of applications of this class of polymers. Herein, a robust UCST-type copolymer of acrylamide (AAm) and acrylonitrile (AN) (poly(AAm-co-AN)) was prepared by reversible addition fragmentation chain Transfer (RAFT) polymerization and its thermo-induced aggregation behavior in aqueous media was studied by turbidity and dynamic light scattering measurements. At temperature below the UCST, the poly(AAm-co-AN) copolymer chains were aggregated together. The aggregate size was found to be larger with increasing AN contents and became smaller upon dilution of the copolymer solutions. While above the UCST, the poly(AAm-co-AN) copolymer chains were expanded and weekly associated in solution. The association between the copolymer chains formed smaller aggregates with increasing the AN Contents or the concentration of the solutions. A model is proposed to explain such aggregationassociation behavior of the poly(AAm-co-AN) copolymer depending on the AN Contents and concentration of the solutions. T2 - Berliner Chemie Symposium & Chemie in Praxis 2016 CY - Berlin, Germany DA - 12.04.2016 KW - Polymer KW - UCST PY - 2016 AN - OPUS4-35804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Manuel T1 - Crystallisation of transition metal phosphonates - A mechanochemical approach N2 - Mechanochemistry is a convenient way to form metal phosphonates with neutral and/or monodeprotonated phosphonates, controlled by the stoichiometric. In situ investigation of reactions helps understanding mechanisms and formation of intermediates. The knowledge of intermediates helps to find metastable structures.The diffusion mechanism is most probable for the mechanochemical synthesis of metal phosphonates. T2 - Institutskolloquium CY - Heinrich Heine University Düsseldorf (HHU), Düsseldorf, Germany DA - 28.01.2016 KW - metal phosphonates KW - Mechanochemistry KW - mof PY - 2016 AN - OPUS4-35860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Franziska T1 - Temperature dependent investigation of mechanochemical cocrystallisation N2 - Milling reactions often result in 100% yields of single products, making purifying procedures obsolete. Mech-anochemistry is also a sustainable and eco-friendly method. The ever increasing interest in this method is contrasted by a lack in mechanistic understanding of the mechanochemical reactivity and selectivity. Recent in situ investigations provided direct insight into formation pathways. However, the currently available theories do not predict temperature T as an influential factor. Here, we report the first determination of an activation energy for a mechanochemical reaction. In a temperature-dependent in situ study the cocrystallisation of ibuprofen and nicotinamide was investigated as a model system. These experiments provide a pivotal step towards a comprehensive understanding of milling reaction mechanisms. T2 - BCA Spring Meeting CY - Nottingham UK DA - 04.04.2016 KW - activation energy KW - cocrystal KW - mechanochemistry KW - milling KW - temperature PY - 2016 AN - OPUS4-35863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Die neuen Prozess-Sensoren 4.0 - Selbstdiagnose, Selbstkalibrierung und Selbstkonfiguration stehen im Fokus N2 - Heute wie morgen müssen Prozess-Sensoren zuerst die Aufgabe des Messens und der Generierung von Prozessinformationen erfüllen. Die Mess-Signale gehen in der Regel auf physikalische oder chemische Größen zurück, werden durch eine Kennlinie repräsentiert und lassen sich kalibrieren. Heute muss man dazu einen großen Aufwand betreiben, denn die physikalischen oder chemischen Informationen werden in vielen Fällen nicht direkt gemessen, sondern verbergen sich in Rohdaten, z. B. in einem optischen Spektrum. Diese Kalibrierungen können für komplexe Sensoren teilweise mehr Kostenaufwand bedeuten, als das Messgerät selbst. KW - Prozess-Sensoren KW - Prozess-Sensoren 4.0 KW - Industrie 4.0 KW - Kommunikationsstandards KW - Technologie-Roadmap PY - 2016 SN - 0947-4188 IS - 7-8 SP - 16 EP - 16 PB - Wiley-VCH Verlag GmbH & Co. KGaA AN - OPUS4-35812 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brieger, C. A1 - Melke, J. A1 - van der Bosch, N. A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - de Oliveira Guilherme Buzanich, Ana A1 - Krishna Kayarkatte, M. A1 - Schoeckel, A. A1 - Roth, C. T1 - A combined in-situ XAS-DRIFTS study unraveling adsorbate induced changes on the Pt nanoparticle structure N2 - The adsorption behavior of Platinum nanoparticles was studied for the as-received catalyst (under inert gas), under hydrogen and CO atmosphere using our newly designed in-situ cell. X-ray Absorption Spectroscopy (XAS) and Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) experiments were performed simultaneously with high data quality. Structural information and the type of adsorbate could be revealed via Extended X-ray Absorption Fine Structure (EXAFS) analysis, Dl X-ray Absorption Near Edge Structure analysis (Dl XANES) and in-situ DRIFTS. The as-received catalyst showed sub-surface oxygen and O(n-fold). Under CO atmosphere only CO(atop) was found. Reversible adsorbate induced changes of the Pt nanoparticle structure were derived from changes in the PtAPt coordination number and the corresponding bond distance. Under reducing conditions (H2, CO) a significant increase in both values occurred. Temperature dependent desorption of CO revealed a gradual shift from PtACO to PtAO. Reoxidation was clearly assigned to strong metal support interaction from the SiO2 support. KW - X-ray absorption spectroscopy KW - DRIFTS KW - XANES KW - CO adsorption KW - Platinum KW - Strong metal support interaction KW - Silica support KW - Adsorbates KW - Infrared spectroscopy PY - 2016 DO - https://doi.org/10.1016/j.jcat.2016.03.034 IS - 339 SP - 57 EP - 67 PB - Elsevier Inc. CY - Philadelphia, Pennsylvania, USA AN - OPUS4-35815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nitsche, Michael T1 - Den Akkreditierungsbeirat (AKB) und seine Arbeit verstehen N2 - Dargestellt werden die deutsche Akkreditierungslandschaft, die Aufgaben des AKB, die Mitgliederstruktur und die Möglichkeiten, wie Externe Themen in die Beratungen des Beirates einbringen können. Ferner wird der Prozess der Regelermittlung sowie die Veröffentlichung ermittelter oder bestätigter Regeln durch den Beirat beschrieben. Des Weiteren wird auf einige aktuell im Beirat diskutierte Fragestellungen und Themen eingegangen. T2 - VMPA-Thementag CY - Braunschweig, Germany DA - 13.06.2017 KW - Akkrediterung KW - AKB KW - Regelermittlung PY - 2017 AN - OPUS4-40879 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Caldeira, Rui T1 - Verbesserung der Empfindlichkeit von Ferroelektret-Empfängern für Luftultraschall-Prüfung N2 - Der immer steigende Bedarf nach Prüfungsverfahren von Verbundwerkstoffen eröffnet die Möglichkeit von Prüfverfahren mittels luftgekoppelten Ultraschalls. Die Steigerung der Empfindlichkeit der Luftultraschall-Wandler erhöht deren Einsatzbereich. Die größte Herausforderung des Verfahrens stellt die Impedanzanpassung an die Luft dar. Ende der 1990er Jahre entdeckte man in Ferroelektreten (geladenen zellulären Polymeren) das Potential zur Lösung dieser Problematik. Geladenes zelluläres Polypropylen, mit einer geringen akustischen Impedanz als bei den meist verwendeten piezoelektrischen Materialien, bietet eine deutlich bessere Anpassung an die Luft. Sein piezoelektrisches Verhalten mit einem piezoelektrischen Koeffizient d33 von 200-800 pm/V ähnelt dem von piezoelektrischen Keramiken. Grund für dieses Verhalten sind die polarisierten Zellen, die eine permanente Ladung erzeugen. Die permanente Ladung erzeugt ein starkes elektrisches Feld in der Folie. Eine auf die Oberfläche einwirkende Kraft staucht die Zellen, wodurch sich die eingeschlossenen Ladungsträger im Verhältnis zueinander bewegen. Durch diese Potential- Verschiebung entsteht eine Ladung auf der Oberfläche. Mit angelegter Vorspannung kann die Empfindlichkeit des Wandlers kontrolliert werden, indem die vorgegebene Polarisierung temporär unterstützt oder reduziert wird. In diesem Beitrag ist die Entwicklung eines Ultraschallempfängers aus geladenem zellulärem Polypropylen mit Anwendung der Vorspannung dargestellt. Eine Verbesserung des Signal-Rausch-Abstands bei der Durchschallung eines Testkörpers um 12-15 dB wurde erreicht. T2 - DGZfP-Jahrestagung CY - Koblenz, Germany DA - 22.5.2017 KW - Ultraschall KW - Luftultraschall KW - Ferroelektret KW - Prüfung KW - Sensor PY - 2017 AN - OPUS4-40880 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Höhne, Christian T1 - Multimodal approach for the numerical simulation of ultrasonic guided waves in cylindrical structures of non-constant thickness N2 - Guided waves hold great potential for applications in the field of ultrasonic nondestructive testing. Examples of possible applications are the ultrasonic testing and structural health monitoring of wheelset-axles as used in trains. Depending on the particular type, these axles can be described as either thick cylindrical rods or thick walled hollow cylinders with varying thickness. Wheelset-axles are safety relevant components that have to be inspected on a regular basis. The use of guided waves would allow a full inspection while accessing only the front faces of the axle, thus potentially speeding up the inspection procedure. In order to develop such an inspection technique, however, detailed knowledge of wave propagation through the axle is required. Established mesh-based procedures, like the finite element method, could be used to simulate guided wave propagation in such structures. However, due to the size of the axle itself and the comparatively fine mesh that is dictated by the wavelengths usually applied in ultrasonic testing, these mesh-based procedures would be very expensive in terms of computation times. The multimodal approach seems to be a very promising alternative that can be expected to provide results significantly faster. The multimodal method uses the guided wave modes of a corresponding waveguide with a constant cross-section as basis in which the local sound field at any given position in a waveguide with varying thickness can be expressed. Thereby the numerical effort is reduced to solving the one dimensional differential equations that govern the evolution of the coefficients in the mode spectrum along the waveguide. Once the sound field has been calculated, a time dependence can easily be included, which allows the simulation of pulse propagation through the waveguide. In this thesis, the multimodal approach, as described for the calculation of Lamb-waves in plates with non-constant thickness, is extended to other types of elastic waveguides such as cylindrical rods and thick walled hollow cylinders. For the sake of simplicity, investigations are restricted to axially symmetric wave modes. The results obtained with the multimodal approach are validated against FEM-simulations. It is shown that the multimodal method potentially holds a great advantage in terms of computation time over commercially available software based on the finite element method. Finally, the multimodal method is evaluated with respect to possible future applications on wheelset-axles. KW - Guided waves KW - Wave propagation PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:co1-opus4-41255 SP - 1 EP - 123 PB - Brandenburgische Technische Universität CY - Cottbus AN - OPUS4-40884 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Olejko, Lydia A1 - Bald, Ilko T1 - FRET efficiency and antenna effect in multi-color DNA origami-based light harvesting systems N2 - Artificial light harvesting complexes find applications in artificial photosynthesis, photovoltaics and light harvesting chemical sensors. They are used to enhance the absorption of light of a reaction center which is often represented by a single acceptor. Here, we present different light harvesting systems on DNA origami structures and analyze systematically the light harvesting efficiency. By changing the number and arrangement of different fluorophores (FAM as donor, Cy3 as transmitter and Cy5 as acceptor molecules) the light harvesting efficiency is optimized to create a broadband absorption and to improve the antenna effect 1 (including two energy transfer steps) from 0.02 to 1.58, and the antenna effect 2 (including a single energy transfer step) from 0.04 to 8.7, i.e. the fluorescence emission of the acceptor is significantly higher when the light-harvesting antenna is excited at lower wavelength compared to direct excitation of the acceptor. The channeling of photo energy to the acceptor proceeds by Förster Resonance Energy Transfer (FRET) and we carefully analyze also the FRET efficiency of the different light harvesting systems. Accordingly, the antenna effect can be tuned by modifying the stoichiometry of donor, transmitter and acceptor dyes, whereas the FRET efficiency is mainly governed by the spectroscopic properties of dyes and their distances. KW - DNA origami KW - Light-harvesting KW - FRET KW - Antenna effect PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-405867 UR - http://pubs.rsc.org/en/content/articlelanding/2017/ra/c7ra02114c#!divAbstract DO - https://doi.org/10.1039/C7RA02114C VL - 7 IS - 39 SP - 23924 EP - 23934 PB - The Royal Soc. of Chemistry AN - OPUS4-40586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heck, Christian A1 - Prinz, Julia A1 - Dathe, A. A1 - Merck, V. A1 - Stranik, O. A1 - Fritzsche, W. A1 - Kneipp, Janina A1 - Bald, Ilko T1 - Gold nanolenses self-assembled by DNA origami N2 - Nanolenses are self-similar chains of metal nanoparticles, which can theoretically provide extremely high field enhancements. Yet, the complex structure renders their synthesis challenging and has hampered closer analyses so far. Here, DNA origami is used to self-assemble 10, 20, and 60 nm gold nanoparticles as plasmonic gold nanolenses (AuNLs) in solution and in billions of copies. Three different geometrical arrangements are assembled, and for each of the three designs, surface-enhanced Raman scattering (SERS) capabilities of single AuNLs are assessed. For the design which shows the best properties, SERS signals from the two different internal gaps are compared by selectively placing probe dyes. The highest Raman enhancement is found for the gap between the small and medium nanoparticle, which is indicative of a cascaded field enhancement. KW - DNA origami KW - SERS KW - Gold nanoparticles KW - Plasmonics PY - 2017 UR - http://pubs.acs.org/doi/pdf/10.1021/acsphotonics.6b00946 DO - https://doi.org/10.1021/acsphotonics.6b00946 SN - 2330-4022 VL - 4 IS - 5 SP - 1123 EP - 1130 AN - OPUS4-40587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jakubowski, Norbert T1 - Spectral interferences N2 - ICP-MS is a well-established analytical method which excels by high accuracy, high dynamic range and extremely low limits of detection for most metals. Furthermore ICP-MS offers a very high multi-element coverage so that many elements of the periodic table can be detected simultaneously. In this series of lectures, we want to focus on the historical developments, fundamentals, instrumentation and novel applications of ICP-MS in the life and material sciences. CY - Berlin KW - Spectral interferences KW - High resolution MS KW - Collision and reaction cells PY - 2017 SP - 1 EP - 18 CY - Berlin AN - OPUS4-40866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jakubowski, Norbert T1 - Non-spectral interferences N2 - ICP-MS is a well-established analytical method which excels by high accuracy, high dynamic range and extremely low limits of detection for most metals. Furthermore ICP-MS offers a very high multi-element coverage so that many elements of the periodic table can be detected simultaneously. In this series of lectures, we want to focus on the historical developments, fundamentals, instrumentation and novel applications of ICP-MS in the life and material sciences. KW - Matrix effects KW - Internal standards PY - 2017 SP - 1 EP - 7 CY - Berlin AN - OPUS4-40868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - van de Kreeke, Johannes T1 - CEN/CENELEC - EU project Western Balkans N2 - The presentation provides an introduction to the field of PT. (1) BAM activities on PT, (2) What is PT, (3) PT statistics, (4) Get started yourself. T2 - PT for Western Balkan countries CY - Berlin, Germany DA - 26.06.2017 KW - Proficiency testing KW - Interlaboratory comparisons KW - Round robins PY - 2017 AN - OPUS4-40871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - WP3 (A 3.3.4 / 3.3.5 / 3.3.6) electron spectroscopy of core/shell nanoparticles N2 - The presentation summarizes the progress of activity 3.3.4, 3.3.5 and 3.3.6 of the Innanopart project. These activities focus on the investigation of different core@shell nanoparticles using laboratory-XPS, synchrotron-radiation-XPS and AES. T2 - Innanopart 27 Months Meeting (EMPIR) CY - Berlin, Germany DA - 14.06.2017 KW - AES KW - Core@shell nanoparticles KW - Depth-profiling KW - Synchrotron KW - XPS PY - 2017 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-40874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Palasse, L. A1 - Häusler, Ines A1 - Dirscherl, K. A1 - Oswald, F. A1 - Narbey, S. A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan T1 - Characterization of the inner structure of porous TiO2 nanoparticle films in dye sensitive solar cells (DSSC) by focused ion beam (FIB) tomography and transmission Kikuchi diffraction (TKD) in the scanning electron microscope (SEM) N2 - A combined methodical approach is tested for the first time with respect to the characterization of the inner structure of porous TiO2 layers infiltrated with ruthenium molecular sensitizer as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area ‘offered’ by the pore Network to the dye. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles (NPs) on FTO/glass substrates. The analytical methods exploited in our study are Focused Ion Beam (FIB) slicing followed by 3D reconstruction as well as the new approach transmission Kikuchi diffraction (TKD) technology in the scanning electron microscope (SEM). While the first method results in the visualization of the 3D pore network within the TiO2 layer, the second one can be successfully applied to analyze the crystal orientation of grains (i.e. NPs in our case) in nanometer resolution. Moreover, size and shape distribution of the TiO2 NPs within the layer can be extracted. SEM in transmission mode and atomic force microscopy (AFM) have been used to verify the dimensional data obtained by the new combined methodical approach. Its analytical benefits but also the challenges and limitations are highlighted. KW - Transmission Kikuchi diffraction KW - Focused ion beam tomography KW - Titanium dioxide KW - Nanoparticles KW - Porosity KW - Particle size KW - DSSC PY - 2017 DO - https://doi.org/10.1016/j.matchar.2017.06.030 SN - 1044-5803 SN - 1873-4189 VL - 131 SP - 39 EP - 48 PB - Elsevier AN - OPUS4-40875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beckmann, Jörg T1 - THz applications for NDT N2 - Electromagnetic waves in the frequency range between 0.1 and 10 THz are described as THz-radiation (T-ray). The ability to penetrate dielectric materials, to operate contactless and to be non-ionizing as well as be-ing insensitive to ambient temperatures makes THz technologies for NDT applications attractive especially where other techniques are not available or less suitable. Today T-rays are applied in non-destructive testing for quality control and condition monitoring issues. The operation is based on the combination of both transmission and/or reflection measurements and specially developed reconstruction procedures. Firstly, THz-TDS measurements will be presented to demonstrate the opportunities for spectroscopy and imaging of polymer materials. A SAFT algorithm and an Optical Layer-Model will be presented and discussed in more detail to demonstrate the opportunities of image reconstruction for visualization of the inner structures of op-tically and far infra-red opaque polymer composites. T2 - 2017 Far East Forum On Nondestructive Evaluation/Testing: New Technology & Application CY - XI'an, China DA - 22.06.2017 KW - THz radiation KW - Terahertz synthetic aperture focusing KW - Thickness measurements KW - Image reconstruction KW - Dielectric materials PY - 2017 AN - OPUS4-40799 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR T1 - Amts- und Mitteilungsblatt, Band 47, Heft 2 T3 - Amts- und Mitteilungsblatt der BAM - 2/2017 PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-408040 SN - 0340-7551 VL - 47 IS - 2 SP - 359 EP - 453 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-40804 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühlmann, Madlen T1 - Design of an online-analysis technique for the determination of major and minor nutrients in soils using DP-LIBS N2 - LIBS (laser-induced breakdown spectroscopy) is known as a fast and simultaneous multi-element analysis with little or no sample preparation. Because of that, over the last few years there has been a growing interest in applications of LIBS in the field of agriculture. As part of the National Research Strategy BioEconomy 2030 the German Federal Ministry of Education and Research (BMBF) started an innovation programme called BonaRes. BonaRes consists of ten interdisciplinary research project as-sociations which are dealing with soil as a sustainable resource for the bio-economy. One of these research projects is I4S (intelligence for soil) which has the goal to develop an integrated system for site-specific soil fertility management. This system includes a sensor platform, which contains different sensors, like XRF, VIS-NIR, Gamma and LIBS. The main task of LIBS measurements in this project is the real time determination of the elemental contents of major and minor nutrients in soils, like calcium, magnesium, potassium. For this purpose, a special setup has been designed. The sample uptake operates with the help of a rotatable sample plate, on which the loose soil sample can be placed in form of a track. The sample plate circulates with different velocities to simulate the application on the field. To provide a higher intensity and a better re-producibility of the obtained signal, a double-pulse Nd:YAG laser (1064 nm) was used. In order to minimize dust formation from the soil during the operation of the laser, a dust removal by suction has been integrated When using relative methods such as LIBS, a suitable calibration curve is needed for absolute quantification. Within the I4S project a large number of soil samples from different testing grounds with known data of chemical composition, texture etc. is available. For the first calibration curves seven soil samples from different grounds in Germany were prepared as reference materials and four certified reference materials from China and Canada were purchased. With the help of these reference materials, calibration curves for different elements were initially calculated based on internal standard addi-tion. Copper was used as internal standard because of its low concentration in soils. The complex matrix of soils, as well as the influence of moisture and grain size in soils makes the absolute quantification by LIBS challenging. To overcome these influences, a calibration curve based on multivariate analysis was generated. Therefore, baseline correction on the second derivative with a Savitzky-Golay filter was followed by a partial least squares regression (PLSR). Multivariate analysis leads to noise reduction and neglection of interfering signals. Therefore, a better correlation between signal intensity and nutrient concentration is observed and a robust calibration curve is obtained. T2 - 9. Euro-Mediterranes Symposium LIBS CY - Pisa, Italy DA - 11.06.2017 KW - LIBS KW - Soil KW - Matrix KW - Multi-element PY - 2017 AN - OPUS4-40807 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gebbers, R. T1 - Laser-induced breakdown spectroscopy (LIBS) for efficient quantitative determination of elemental plant nutrients in soils: A contribution to precision agriculture N2 - One important aim of precision agriculture (PA) is the optimization of crop growth by means of site-specific measures, e.g. fertilizer application. Thus, PA should contribute to a resource efficient and ecofriendly soil management. Due to the expenses associated with traditional methods of soil analysis, requiring sample collection and laboratory analysis, PA technologies are still not in widespread use. Therefore, the aim of the project “I4S – Integrated System for Site-Specific Soil Fertility Management” is the development of a field-deployed, sensor-based analysis system offering rapid, cost-effective and spatially-resolved fertilizer recommendations. In this system, laser-induced breakdown spectroscopy (LIBS) could be ideally suited to assessing elemental nutrient contents of soils. In addition to low cost, durability and small size, a reliable quantification procedure is a crucial requirement for such a system. However, the texture as well as the composition of the soil can affect the spectra. This matrix dependence is the key challenge to be addressed in the application of LIBS for soil evaluation. The focus of this work was the establishment of a LIBS method for soil analysis in a laboratory environment for future field application. Natural soil samples of various origins, textures and compositions were used to characterize the matrix dependence of the LIBS spectra. Reference samples were prepared by adding defined amounts of the target elements to the soils (standard addition). Signals not superimposed by peaks of other elements were identified for each element. The reference samples also provided calibration curves for the respective soil type when the initial concentrations in the soils were taken into account. Additionally, the common laboratory method ICP-OES following aqua regia extraction was used to obtain reference values. Various approaches of calibration free evaluation of the data were also evaluated. In addition to traditional single-pulse experiments, the advantages of dual-pulse LIBS in relation to signal intensity, reproducibility as well as overcoming the matrix dependence of soil spectra were investigated. These methods were subsequently applied to validation samples collected on a dense grid within a field. T2 - Pedometrics 2017 CY - Wageningen, The Netherlands DA - 26.06.2017 KW - LIBS KW - Precision KW - Agriculture KW - Soil KW - Site-specific PY - 2017 AN - OPUS4-40808 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer-Tenhagen, C. A1 - Johnen, D. A1 - Heuwieser, W. A1 - Becker, Roland A1 - Schallschmidt, Kristin A1 - Nehls, Irene T1 - Odor Perception by Dogs: Evaluating Two Training Approaches for Odor Learning of Sniffer Dogs N2 - In this study, a standardized experimental set-up with various combinations of herbs as odor sources was designed. Two training approaches for sniffer dogs were compared; first, Training with a pure reference odor, and second, training with a variety of odor mixtures with the target odor as a common denominator. The ability of the dogs to identify the target odor in a new context was tested. Six different herbs (basil, St. John’s wort, dandelion, marjoram, parsley, ribwort) were chosen to produce reference materials in various mixtures with (positive) and without (negative)chamomile as the target odor source. The dogs were trained to show 1 of 2 different behaviors, 1 for the positive, and 1 for the negative sample as a yes/no task. Tests were double blind with one sample presented at a time. In both training approaches, dogs were able to detect chamomile as the target odor in any presented mixture with an average sensitivity of 72% and a specificity of 84%. Dogs trained with odor mixture containing the target odor had more correct indications in the transfer task. KW - dog training KW - herbs KW - reference materials, KW - scent dog KW - smell KW - training model PY - 2017 DO - https://doi.org/10.1093/chemse/bjx020 SN - 1464-3553 SN - 0379-864X VL - 42 IS - 5 SP - 435 EP - 441 PB - Oxford University Press AN - OPUS4-40786 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rietz, U. T1 - Centrifugal Adhesion Testing Technology for adhesive strength determination N2 - The paper addresses the ‘Centrifugal Adhesion Testing Technology for adhesive strength determination´ and the following points are discussed in more detail: Bonding & Adhesive Strength Measurement principle CAT-Technology (Centrifugal Adhesion Testing), Preparation of test specimen, SEPView 7 – Software, Metal coatings on glass and on non-planar polymer substrates, Comparison of adhesive tapes. T2 - The Adhesion Society – 40th Annual Meeting & Short Cours CY - St. Petersburg, Florida, USA DA - 26.02.2017 KW - Centrifugal Adhesion Testing KW - CAT-Technology KW - Adhesive strength determination KW - Bonding KW - Metal coatings PY - 2017 AN - OPUS4-40788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lucassen, F. A1 - Pritzkow, Wolfgang A1 - Rosner, M. A1 - Sepulveda, F. A1 - Vasquez, P. A1 - Wilke, H. A1 - Kasemann, S. A. T1 - The stable isotope composition of nitrogen and carbon and elemental contents in modern and fossil seabird guano from Northern Chile – Marine sources and diagenetic effects N2 - Seabird excrements (guano) have been preserved in the arid climate of Northern Chile since at least the Pliocene. The deposits of marine organic material in coastal areas potentially open a window into the present and past composition of the coastal ocean and its food web. We use the stable isotope composition of nitrogen and carbon as well as element contents to compare the principal prey of the birds, the Peruvian anchovy, with the composition of modern guano. We also investigate the impact of diagenetic changes on the isotopic composition and elemental contents of the pure ornithogenic sediments, starting with modern stratified deposits and extending to fossil guano. Where possible, 14C systematics is used for age information. The nitrogen and carbon isotopic composition of the marine prey (Peruvian anchovy) of the birds is complex as it shows strong systematic variations with latitude. The detailed study of a modern profile that represents a few years of guano deposition up to present reveals systematic changes in nitrogen and carbon isotopic composition towards heavier values that increase with age, i.e. depth. Only the uppermost, youngest layers of modern guano show compositional affinity to the prey of the birds. In the profile, the simultaneous loss of nitrogen and carbon occurs by degassing, and non-volatile elements like phosphorous and calcium are passively enriched in the residual guano. Fossil guano deposits are very low in nitrogen and low in carbon contents, and show very heavy nitrogen isotopic compositions. One result of the study is that the use of guano for tracing nitrogen and carbon isotopic and elemental composition in the marine food web of the birds is restricted to fresh material. Despite systematic changes during diagenesis, there is little promise to retrieve reliable values of marine nitrogen and carbon signatures from older guano. However, the changes in isotopic composition from primary marine nitrogen isotopic signatures towards very heavy values generate a compositionally unique material. These compositions trace the presence of guano in natural ecosystems and its use as fertilizer in present and past agriculture. KW - Isotope ratio KW - VPDB KW - Fishmeal KW - Elemental analyser KW - Vario EL III KW - Casein standard KW - ICP-OES KW - Accelerator mass spectrometry PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-407911 DO - https://doi.org/10.1371/journal.pone.0179440 SN - 1932-6203 VL - 12 IS - 6 SP - Article e0179440, 1 EP - 25 PB - PLOS CY - San Francisco, California, US AN - OPUS4-40791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Barnefske, Lena T1 - PDMS-POS-capsules for prospective self-healing silicone rubber N2 - Capsules made of a polydimethylsiloxane (PDMS) core with a poly(organosiloxane) (POS) shell can be used as a new filler system for self-healing silicone rubber. Synthesis of these PDMS-POS capsules, as well as the characterization based on TGA, SEM and fluorescence spectroscopy is presented. T2 - 6th ICSHM 2017 CY - Friedrichshafen, Germany DA - 25.06.2017 KW - Self-healing KW - Capsules KW - PDMS PY - 2017 AN - OPUS4-40856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Barnefske, Lena T1 - Entwicklung eines mechanisch verstärken und selbstheilenden Silikonelastomers auf Basis eines Kapsel-basierten Ansatzes N2 - Im Arbeitskreis von Herrn Prof. Dr. Menzel (TU Braunschweig) wurde in Sievershausen ein Vortrag zum Thema „Self-healing and mechanically reinforced silicone rubber by the use of multifuctional capsules“ gehalten. Der Vortrag beginnt mit einer kurzen Motivation und einem Überblick über selbstheilende Materialien. Daraufhin werden die Ergebnisse zur Entwicklung eines selbstheilenden Silikonelastomers auf Basis von Kapseln, bestehend aus einem PDMS Kern und einer POS Hülle, dargestellt. Es folgt die Analytik, die auf DLS, TGA, UV/Vis und Fluoreszenzspektroskopie sowie SEM beruht. Der Vortrag endet mit einem Ausblick über zukünftige Arbeiten auf dem Gebiet. T2 - Seminar in Sievershausen CY - Sievershausen, Lehrte, Germany DA - 07.06.2017 KW - Selbstheilung KW - PDMS PY - 2017 AN - OPUS4-40857 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hüllmann, Dino T1 - Aerial Robot Olfaction - Mobile Gas Sensors N2 - An introduction to BAM, gas source localisation and gas distribution mapping is given. Both an example for in-situ and open-path gas sensors is shown. The flight platforms used at BAM are introduced. T2 - Workshop "Drohnen in der Wissenschaft" CY - Potsdam, Germany DA - 30.06.2017 KW - Gassensor KW - Olfaction KW - Multicopter PY - 2017 AN - OPUS4-40858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jakubowski, Norbert T1 - Short course on ICP-MS N2 - ICP-MS is a well-established analytical method which excels by high accuracy, high dynamic range and extremely low limits of detection for most metals. Furthermore ICP-MS offers a very high multi-element coverage so that many elements of the periodic table can be detected simultaneously. In this series of lectures, we want to focus on the historical developments, fundamentals, instrumentation and novel applications of ICP-MS in the life and material sciences. KW - Fundamentals KW - Theory KW - Basics PY - 2017 SP - 1 EP - 33 CY - Berlin AN - OPUS4-40865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geißler, Daniel A1 - Würth, Christian A1 - Wolter, C. A1 - Weller, H. A1 - Resch-Genger, Ute T1 - Excitation wavelength dependence of the photoluminescence quantum yield and decay behavior of CdSe/CdS quantum dot/quantum rods with different aspect ratios N2 - The excitation wavelength (lexc) dependence of the photoluminescence (PL) quantum yield (FPL) and decay behavior (tPL) of a series of CdSe/CdS quantum dot/Quantum rods (QDQRs), consisting of the same spherical CdSe core and rod-shaped CdS shells, with aspect ratios ranging from 2 to 20 was characterized. lexc between 400–565 nm were chosen to cover the first excitonic absorption band of the CdSe core material, the onset of absorption of the CDs shell, and the region of predominant shell absorption. A strong lexc dependence of relative and absolutely measured FPL and tPL was found particularly for the longer QDQRs with higher aspect ratios. This is attributed to combined contributions from a length-dependent shell-to-core exciton localization efficiency, an increasing number of defect states within the shell for the longest QDQRs, and probably also the presence of absorbing, yet non-emitting shell material. Although the FPL values of the QDQRs decrease at shorter wavelength, the extremely high extinction coefficients introduced by the shell outweigh this effect, leading to significantly higher brightness values at wavelengths below the absorption onset of the CdS Shell compared with direct excitation of the CdSe cores. Moreover, our results present also an interesting example for the comparability of absolutely measured FPL using an integrating sphere setup and FPL values measured relative to common FPL standards, and underline the Need for a correction for particle scattering for QDQRs with high aspect ratios. KW - Quantum dot KW - Quantum rod KW - Quantum yield KW - Integrating sphere KW - Decay time PY - 2017 DO - https://doi.org/10.1039/C7CP02142A SN - 1463-9076 SN - 1463-9084 VL - 19 IS - 19 SP - 12509 EP - 12516 PB - Royal Society of Chemistry (RSC) AN - OPUS4-40814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Millar, Steven A1 - Grothe, S. A1 - Wilsch, Gerd T1 - 2D evaluation of spectral LIBS data derived from heterogeneous materials using cluster algorithm N2 - Laser-induced Breakdown Spectroscopy (LIBS) is capable of providing spatially resolved element maps in regard to the chemical composition of the sample. The evaluation of heterogeneous materials is often a challenging task, especially in the case of phase boundaries. In order to determine information about a certain phase of a material, the need for a method that offers an objective evaluation is necessary. This paper will introduce a cluster algorithm in the case of heterogeneous building materials (concrete) to separate the spectral information of non-relevant aggregates and cement matrix. In civil engineering, the information about the quantitative ingress of harmful species like Cl−, Na+ and SO2−4 is of great interest in the evaluation of the remaining lifetime of structures (Millar et al., 2015; Wilsch et al., 2005). These species trigger different damage processes such as the alkali-silica reaction (ASR) or the chloride-induced corrosion of the reinforcement. Therefore, a discrimination between the different phases, mainly cement matrix and aggregates, is highly important (Weritz et al., 2006). For the 2D evaluation, the expectation-maximizationalgorithm (EM algorithm; Ester and Sander, 2000) has been tested for the application presented in this work. The method has been introduced and different figures of merit have been presented according to recommendations given in Haddad et al. (2014). Advantages of this method will be highlighted. After phase separation, non-relevant information can be excluded and only the wanted phase displayed. Using a set of samples with known and unknown composition, the EM-clustering method has been validated regarding to Gustavo González and Ángeles Herrador (2007). KW - LIBS KW - Concrete KW - EM-clustering KW - Heterogeneity PY - 2017 DO - https://doi.org/10.1016/j.sab.2017.06.005 SN - 0584-8547 VL - 2017 IS - 134 SP - 58 EP - 68 PB - Elsevier B.V. AN - OPUS4-40644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Matthias A1 - Mull, Birte A1 - Horn, Wolfgang A1 - Brödner, Doris A1 - Mölders, N. A1 - Renner, M. T1 - Reproducibly emitting reference material on thermoplastic polyurethane basis for quality assurance/quality control of emission test chamber measurements N2 - Volatile Organic Compounds (VOC) are ubiquitous in the indoor air since they are emitted from materials used indoors. Investigations of these materials are mostly carried out in emission test chambers under controlled climatic conditions. Reference materials are an important tool for quality assurance/Quality control of emission test chamber measurements but so far they are not commercially available. In this study, a new approach was tested to develop an appropriate reference material with homogenous and reproducible emission of the VOC with well measurable air concentrations in emission test Chambers larger than 20 L at air change rates of 0.5 - 1 /h. Thermoplastic Polyurethane (TPU) was selected as Matrix material which was impregnated with 2,2,4- trimethyl-1,3-pentanediol monoisobutyrate (texanol) as test VOC using compressed carbon dioxide. An optimization of the impregnation parameters such as temperature, pressure, time, VOC injection volume and TPU sample size was performed until the targeted area specific Emission rate (SERa) value was reached. Further aspects like process control, storage effects and correlation of the sample size to the emission rate were investigated. It was found that the SERa immediately after sample preparation were not reproducible between the batches but became unified 10 days after loading into the test chamber indicating the necessity of aging before use. SERa between 13,000 and 18,000 mg m-2 h-1 were obtained, and the impregnated materials could be well stored in aluminum-coated polyethylene foil for at least seven weeks without significant losses. Furthermore, the impregnation of styrene and the SVOC 2,6-diisopropylnaphthalene was tested. KW - Reference material KW - Emissions testing KW - Volatile organic compounds KW - Polymer material KW - CO2 assisted impregnation PY - 2017 DO - https://doi.org/10.1016/j.buildenv.2017.06.005 SN - 0360-1323 SN - 1873-684X VL - 122 SP - 230 EP - 236 PB - Elsevier AN - OPUS4-40646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Omara, Shereen Shabaan A1 - Turky, G. A1 - Ghoneim, A. A1 - Thünemann, Andreas A1 - Abdel Rehim, M. H. A1 - Schönhals, Andreas T1 - Hyperbranched poly(amidoamine)/kaolinite nanocomposites: Structure and charge carrier dynamics N2 - An ex-situ approach was applied to prepare nanocomposites from hyperbranched poly(amidoamine) and modified kaolinite (Ka-DCA). The structure of the polymer and the corresponding nanocomposites was investigated by FTIR, DSC, SAXS and TEM. SAXS might suggest a partly exfoliated structure of the nanocomposites, which was supported by TEM. The molecular dynamics was studied by means of broadband dielectric spectroscopy (BDS). The dielectric spectra are dominated by a conductivity contribution at higher temperatures for all samples investigated. The obtained results further indicated that DC conductivity is increased by 4 orders of magnitude with increasing concentration of Ka-DCA nanofiller. Further, a significant separation between the conductivity relaxation time and that of segmental dynamics was observed. The decoupling phenomenon and the conductivity mechanism were discussed in detail. This study provides insights about the influence of the nanofiller on the structure and the conductivity contribution of nanocomposites of hyperbranched polymers including the decoupling phenomenon and fragility. KW - Hyperbranched polymers KW - Nanocomposites KW - Conductivity PY - 2017 DO - https://doi.org/10.1016/j.polymer.2017.06.017 SN - 0032-3861 VL - 121 SP - 64 EP - 74 PB - Elsevier Ltd. AN - OPUS4-40648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Chancen für neue Automatisierungskonzepte und neue Geschäftsmodelle in der Prozessindustrie auf Basis von „Prozess-Sensoren 4.0“ und Modularisierung N2 - Für die weitere Entwicklung von der Ist‐Situation zu einer Industrie-4.0-Welt in der Prozessindustrie bestehen recht ähnliche Szenarien. Dazu werden derzeit mehrere Szenarien diskutiert. Diese reichen vom erleichterten Abruf sensorbezogener Daten über zusätzliche Kommunikationskanäle zwischen Sensor und mobilen Endgeräten über vollständig bidirektionale Kommunikation bis hin zur Einbindung der Cloud und des Internets in virtualisierte Umgebungen. Um zu einer störungsfreien Kommunikation aller Sensoren untereinander zu kommen, muss mindestens ein einheitliches Protokoll her, das alle Sensoren sprechen und verstehen. Der derzeit greifbarste offengelegte Standard, der moderne Kommunikationsanforderungen erfüllt, ist OPC Unified Architecture (OPC-UA). Viele halten das Sortieren der Kommunikationsstandards für eines der wesentlichen Errungenschaften von Industrie 4.0. Es gibt viele Parallelen zwischen der Laborgerätewelt und der Prozess-Sensor-Welt, die im Rahmen der Digitalisierung immer näher aneinanderrücken. T2 - SPECTARIS e.V., 3. Treffen Projektgruppe Schnittstellen CY - Berlin, Germany DA - 14.06.2017 KW - Prozess-Sensoren KW - Industrie 4.0 KW - SPECTARIS KW - OPC-UA KW - Automation KW - Smarte Sensoren PY - 2017 AN - OPUS4-40598 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Broadband dielectric spectroscopy as a complementary tool to characterize polymer systems N2 - The basics of broadband dielectric spectroscopy were introduced in detail. The analysis of the data was discussed. As application of broadband dielectric spectroscopy the alpha-relaxation (dynamic glass transition) and the chain dynamics of polymers were ilustrated. Further the application of dielectric spectroscopy to polymerbased nanocomposites and high preformance polymers was discussed in Detail. T2 - International Symposium on Polymer Analyisis and Characterization CY - Linz, Austria DA - 11.06.2017 KW - Broadband dielectric spectroscopy PY - 2017 AN - OPUS4-40602 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Polymer-based nanocomposites – Interplay between interfacial and bulk properties N2 - Different types of polymerbased nanocomposites (matrix materials: polyethylene, polypropylene, polylactide, polycarbonate, polystyrene) with a broad variety of nanofillers (fillers: layered silica, layered doubled hydroxides, POSS) are prepared where the concentration of the particles is varied. For layered fillers TEM images show both an intercalated and exfoliated morphology in dependence on the nanofiller and the matrix. All systems are studied in detail by dielectric spectroscopy (BDS) but also complementary methods like WAXS, SAXS, gas transport measurements, calorimetry, and FTIR spectroscopy are employed. Besides the dispersion, the interfacial region between the nanoparticles and the polymer matrix is crucial for the properties of the nanocomposites. Therefore, attention is paid to investigate this interfacial area by BDS because the polar groups of both the surfactant and compatibilizer are located close to the layers. For some systems it is found that the molecular mobility in the interfacial area is essentially higher than in the matrix. In addition a Maxwell/Wagner/Sillars polarization is found due to the blocking of charges at the layers. The time constant of this MWS-process can be correlated with characteristic length scales in the nanocomposites and provides information about the dispersion of the nanofiller. T2 - International Symaposium on Polymer Ananlysis and Characterization CY - Linz, Austria DA - 11.06.2016 KW - Polymer based nanocomposites KW - Broadband dielectric spectroscopy PY - 2017 AN - OPUS4-40604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf A1 - Heckel, Thomas T1 - New evaluation methods for non-destructive rail inspection using eddy current and ultrasound N2 - Since 1999 there has been a continuous development of non-destructive head check inspection. Especially in case of modern rail inspection systems, high demands on a fast, detailed detection and classification of defects called for improved testing methods. Due to the large amount of different rail types and profiles, the adaptation and optimization of algorithms is still in progress. Additional data analysis is under devel-opment for combined eddy current and ultrasonic inspection methods. This presentation gives an over-view of further enhancement and linking of testing systems as well as data processing. Main foci of the development are an improved sensitivity and an increased reliability of the testing results. Also, addi-tional information can be obtained like determination of local hardness and roughness of the rail as well as an enhanced resolution for locating of defects which will be part of the presented work. T2 - Railway Engineering-2017 CY - Edinburgh, UK DA - 21.06.2017 KW - Eddy current testing KW - Ultrasonic testing KW - Rail inspection KW - Data evaluation KW - Classification PY - 2017 SN - 0-947644-83-0 DO - https://doi.org/10.25084/raileng.2017.0078 SP - 1 EP - 10 AN - OPUS4-40767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Simone T1 - Early fire detection: Are hydrogen sensors able to detect pyrolysis of household materials? N2 - We analysed the hydrogen generation during the smouldering of polymeric materials, which are typically used in the household, in the Smoke Density Chamber coupled to a new developed hydrogen sensor to detect early stages of fires. The results of hydrogen generation were compared with the emission of carbon monoxide and smoke during the fire scenarios. Additionally, the results were compared with parameters used in traditional commercial detection systems. In this scenario, the hydrogen sensor showed encouraging results for the detection of fires in earlier phase compared to traditional detectors. Furthermore, we tested the new developed hydrogen sensor in a real room with different fire scenarios. We have also investigated interferences, e.g. steam and cigarette smoke. The hydrogen sensor could detect hydrogen generation in the earliest stage of fire, even before CO and smoke were developed in detectable amounts. Therefore, the hydrogen sensor can be applied for early fire detection in case of pyrolysis. The sensors are quite good for detecting pyrolysis gases. But when it comes to a fast ignition other techniques are more suitable for it. The sensors are best for combination with other techniques, such as smoke detectors. T2 - 12th IAFSS Conference CY - Lund, Sweden DA - 12.6.2017 KW - Hydogen sensor KW - Smouldering KW - Detection PY - 2017 AN - OPUS4-40688 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riaz, Muhammad T1 - Effect of modification on acidity and porosity of natural zeolite clinoptilolite N2 - 1. Introduction Catalytic processing of heavy feedstock can meet the increased demand of energy up to a great extent. It requires the application of acidic catalysts like zeolites. However, the used synthetic catalysts are difficult to recover and reuse and are mostly spent. The use of natural zeolite as spent catalysts may open new perspectives in the chemical use of heavy feed feedstock by chemical conversion. Natural zeolites are not expensive, widely available and environment friendly. Clinoptilolite is a natural, most abundant medium pore size zeolite, consisting of 2-deminsional pore system containing of oxygen-8- membered and oxygen-10-membered rings.Although clinoptilolite is porous and can be acidified by ion exchange or acid treatment. Samples were characterized by XRD regarding crystallinity and phase composition. The acidity was studied by ammonia-TPD measurements and 1H solid state MAS NMR as well as REDOR experiments. Structure and structural changes caused by applied modifications were studied by 27Al- and 29Si MAS NMR measurements and thermal analysis. 2. Experimental Part The ion exchange behaviour of natural zeolite tuff contained ca. 90 ma. % of clinoptilite was studied in 0.1 and 0.5 M ammonium nitrate solution and for comparison with HCl solution of similar concentration. The activation temperature was varied between 300-600°C.The catalytic test was performed using ca. 0.2 g of the catalyst and ca.10g of the aldehyde and alcohol using toluene as solvent and under reflux. Reaction water was removed via a by-pass. 3. Results and discussion The experiments show that a part of the cations of clinoptilolite readily exchange with ammonium ions and protons supplied by acid treatment. Substitution of the compensating cations by NH4+ followed by calcination and HCl treatment does not produce structural changes in the original material, but it opens the channels and increases acidity and thermal stability. Calcination at higher temperature and exchange with concentrated acid has a more severe impact on the clinoptilolite structure dealumination as indicated by the appearance of 5- and 6-fold coordinated aluminum. Catalytic activity of sample is related to the surface acidity. The presence of acidic protons of medium to strong strength is confirmed by ammonia-TPD and proton NMR measurements. 4. Conclusions Acidic natural clinoptilolite catalysts prepared via ammonium exchange followed by calcination and acid treatment shows a positive influence on acidity and porosity. Modification creates hierarchical micro-nano porosity. The specific surface area varies between ca. 45 m2/g and 245 m2/g. T2 - Catalysis summer school-UK CY - Liverpool, UK DA - 17.07.2017 KW - Natural Zeolite Clinoptilolite PY - 2017 AN - OPUS4-40689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Kazakov, Alexander Ya. T1 - Kinetic model of stimulated emission created by resonance pumping of aluminum laser-induced plasma N2 - Stimulated emission observed experimentally in an aluminum laser induced plasma is modeled via a kinetic approach. The simulated emission at several cascade transitions is created by a pump laser guided through the plasma at several microseconds after its creation and tuned in resonance with the strong 3s²3p-3s²4s transition at 266 nm. A two-dimensional space-time collisional radiative plasma model explains the creation of the Population inversion and lasing at wavelengths of 2100 nm and 396.1 nm. The population inversion for lasing at 2100 nm is created by depopulation of the ground 3s²3p state and population of the 3s²5s state via the absorption of the resonant radiation at 266 nm. The population inversion for lasing at 396.1 nm occurs during the laser pulse via the decay of the population of the pumped 3s²5s state to the excited 3s²4s state via cascade transitions driven optically and by collisions. In particular, efficient are the mixing transitions between neighboring states separated by small gaps on the order of kT at Plasma temperatures of 5000–10 000 K. The model predicts that the population inversion and corresponding gain may reach high values even at very moderate pump energy of several lJ per pulse. The efficiency of lasing at 2100 nm and 396.1 nm is estimated to be ~3% and 0.05%, correspondingly with respect to the pump laser intensity. The gain for lasing at 396.1 nm can reach as high as ~40 cm⁻¹. The polarization effect that the pump radiation at 266 nm imposes on the stimulated emission at 396.1 nm is discussed. The calculated results are favorably compared to experimental data. KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics KW - Lasers PY - 2017 DO - https://doi.org/10.1063/1.4984912 SN - 0021-8979 SN - 1089-7550 VL - 121 IS - 21 SP - 213303-1 EP - 213303-11 AN - OPUS4-40693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Characterization of nanomaterials with VIS/NIR emission - Spectroscopic properties and surface group analysis N2 - Spectroscopic methods for the absolute characterization of the optical properties of different types of vis/NIR-emissive nanomaterials like semiconductor quantum dots, upconversion nanocrystals, and dye-doped polymer nanoparticles will be presented and their relevance for the mechanistic understanding of nonradiative decay channels and the rational design of new nanomaterials will be underpinned. In this respect, also the potential of optical spectroscopy for surface group and ligand analysis surface chemistry will be demonstrated. T2 - Colloquium der Physikalischen und Theoretischen Chemie CY - Berlin, Germany DA - 21.06.2017 KW - Characterization KW - Nanomaterials PY - 2017 AN - OPUS4-40696 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Huang, M. D. A1 - Becker-Ross, H. A1 - Florek, S. A1 - Abad Andrade, Carlos Enrique A1 - Okruss, M. T1 - Investigation of high-resolution absorption spectra of diatomic sulfides of group 14 elements in graphite furnace and the comparison of their performance for sulfur determination N2 - For the purpose of finding suitable molecules applicable to sulfur determination and to compare their analytical sensitivity systematically, high-resolution overview molecular absorption spectra of sulfides of group 14 elements produced in a graphite furnace were investigated. To that end a modular simultaneous echelle spectrograph (MOSES) was used, which allows recording sub-ranges of spectra out of a total wavelength range from 190 nm to 735 nm. The combined overview spectra show a complex structure with many vibrational bands, each of them consisting of a multitude of sharp rotational lines. The absorption of rotational lines of SiS (282.910 nm), GeS (295.209 nm), SnS (271.578 nm), and PbS (335.085 nm) has been analyzed for optimizing the particular experimental conditions regarding to the sulfur determination. Using the commercial CS AAS instrument contrAA 600 under optimized conditions such as the temperature program, the modification of the platform with Zr and the use of chemical modifiers, the achieved characteristic masses for sulfur are 12 ng (CS), 15.7 ng (SiS), 9.4 ng (GeS), 20 ng (SnS), and 220 ng (PbS). The first four sulfides provide an analytical sensitivity with roughly the same level, but the GeS molecule seems to be the best one with respect to analytical sensitivity and flexibility in molecular formation control. The PbS molecule provides the lowest analytical sensitivity, and together with its low bond strength it is not recommended for sulfur determination. KW - Sulfur determination KW - Sulfides of group 14 elements KW - Molecular absorption KW - High-resolution continuum source absorption spectrometry KW - Graphite furnace PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0584854717302215 DO - https://doi.org/10.1016/j.sab.2017.06.012 SN - 0584-8547 VL - 135 SP - 15 EP - 21 PB - Elsevier B.V. CY - Amsterdam, The Netherlands AN - OPUS4-40771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - New Evaluation Methods for Non-Destructive Rail Inspection using Eddy Current and Ultrasound N2 - Since 1999 there has been a continuous development of non-destructive head check inspection. Especially in case of modern rail inspection systems, high demands on a fast, detailed detection and classification of defects called for improved testing methods. Due to the large amount of different rail types and profiles, the adaptation and optimization of algorithms is still in progress. Additional data analysis is under devel-opment for combined eddy current and ultrasonic inspection methods. This presentation gives an over-view of further enhancement and linking of testing systems as well as data processing. Main foci of the development are an improved sensitivity and an increased reliability of the testing results. Also, additional information can be obtained like determination of local hardness and roughness of the rail as well as an enhanced resolution for locating of defects which will be part of the presented work. T2 - Railway Engineering-2017 CY - Edinburgh, UK DA - 21.06.2017 KW - Eddy current testing KW - Ultrasonic testing KW - Rail inspection KW - Data evaluation KW - Classification PY - 2017 AN - OPUS4-40772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - S2XAFS: Time-resolved X-ray absorption spectroscopy in a ‘single-shot’ – First in situ applications N2 - The newly developed EXAFS set-up comprises both time- and spatially-resolved EXAFS information simultaneously in a single-shot. This facile, stable and scanningless set-up was tested at the BAMline @ BESSY-II (Berlin, Germany). The pri-mary broadband beam is generated by a filter/X-ray-mirror combination (bandpass). The transmitted beam through the sample is diffracted by a convexly bent Si (111) crystal, producing a divergent beam. This, in turn, is collected by an area sensitive detector, in a theta - 2 theta geometry. The first in situ measurements were successfully carried out and hereby presented. The case-study deals with research on Zn-based Metal-Organic-Frameworks (MOFs) that have potential for medi-cal/pharmaceutical applications. This hot topic of MOF research targets encapsulation of therapeutically relevant bio-macromolecules (e.g. Enzymes) for drug delivery applications. Questions regarding the influence of proteins on the coor-dination of Zn during MOF crystal growth and within the final MOF can be answered with this new setup. We were able to track structural changes within a 1s time resolution. T2 - CSI XL Conference CY - Pisa, Italy DA - 12.06.2017 KW - Single-shot EXAFS KW - In situ characterization KW - Biomedical applications PY - 2017 AN - OPUS4-40683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Muhammad, Riaz T1 - Effect of the ammonium ion exchange and HCl treatment on the acidity of natural zeolite clinoptilolite N2 - Clinoptilolite is a natural, medium pore size, zeolite. It contains a 2-deminsional pore system containing of oxygen-8- membered and oxygen-10-membered rings. It is one of the most abundant natural zeolites. Clinoptilolite has a crystalline structure showing unique ion exchange and sorption properties. It is mainly used as ion exchanger and adsorbent for removal of toxic elements and compounds from the environment. The use of natural zeolite as spent catalysts may open new perspectives in the chemical use of heavy feed feedstock by chemical conversion. Natural zeolites are not expensive, widely available and environment friendly. Clinoptilolite is the most abundant natural zeolite. Although clinoptilolite is a potential acid catalyst, reports on its application in catalysis are limited so far. This contribution deals with the modification of the acidity of the natural zeolite clinoptilolite, the characterization of the acid sites and the catalytic activity in the Brønsted acid catalyzed acetalization of benzaldehyde with butandiol-1,3. The samples were acidified by via ammonium-ion exchange followed by calcination and acid treatment. The obtained catalysts were characterized by XRD regarding crystallinity and phase composition. The morphology was studied by TEM images The acidity was studied by ammonia-TPD measurements and 1H solid state MAS NMR as well as REDOR experiments. Structure and structural changes caused by applied modifications were studied by 27Al- and 29Si MAS NMR measurements and thermal analysis. The ion experiments show that a part of the cations of clinoptilolite readily exchange with ammonium ions and protons from HCl treatment. The NMR results give first hints for a relation of the catalytic conversion with the presence of 5-fold coordinated aluminum. The results will be discussed in terms of a collaborative action of Brønsted acid sites and 5-fold coordinated aluminum. T2 - Deutsche Zeolith Tagung-2017 CY - Frankfurt Germany DA - 01.03.2017 KW - Natural zeolite clinoptilolite PY - 2017 AN - OPUS4-40684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Muhammad, Riaz T1 - Acidity of natural zeolite clinoptilolite and catalytic performance in the acetalization of benzaldehyde with butandiol-1,3 N2 - 1. Introduction Clinoptilolite is a natural, medium pore size, zeolite. It contains a 2-deminsionalpore system containing of oxygen-8- membered and oxygen-10-membered rings. It is one of the most abundant natural zeolites. It is mainly used as ion exchanger and adsorbent for removal of toxic elements and compounds from the environment. Although clinoptilolite is porous and can be acidified by ion exchange or acid treatment and a potential catalyst, reports on its application in catalysis are limited so far. This contribution deals with acidic modification of a natural zeolite sample, characterization of the nature of acid sites and the catalytic activity in the Brønsted acid catalyzed acetalization of benzaldehyde with butandiol-1,3. The samples were acidified by via ammonium-ion exchange and acid treatment. Samples were characterized by XRD regarding crystallinity and phase composition. The morphology was studied by TEM images The acidity was studied by ammonia-TPD measurements and 1H solid state MAS NMR as well as REDOR experiments. Structure and structural changes caused by applied modifications were studied by 27Al- and 29Si MAS NMR measurements. and thermal analysis. 2. Experimental Part The studied natural zeolite tuff contained ca. 90 ma.-% of clinoptilite. The ion exchange behavior was studied in 0.1 and 0.5 M ammonium nitrate solution and for comparison with HCl solution of similar concentration. The activation temperature was varied between 300-600°C.The catalytic test was performed using ca. 0.1 g of the catalyst and ca.10g of the aldehyde and alcohol using toluene as solvent and under reflux. Reaction water was removed via a by-pass. 3. Results and discussion The ion experiments show that a part of the cations of clinoptilolite readily exchange with ammonium ions and protons supplied by acid treatment. However, exchange with the acid has a more severe impact on the clinoptilolite structure. More severe treatment times leads to a loss of activity in terms of acetal formation: Sample show all high conversions after 4 h of reaction, but show markedly differences after short reaction times. The presence of acidic protons of medium to strong strength is confirmed by ammonia-TPD and proton NMR measurements. The sample activation causes a partial dealumination as indicated by the appearance of 5- and 6-fold coordinated aluminum. Interestingly, the NMR result give first hints for a relation of the catalytic conversion) with the amount of 5-fold coordinated aluminum. The results will be discussed in terms of a collaborative action of Brønsted acid sites and 5-fold coordinated aluminum. 4. Conclusions Acid natural clinoptilolite catalysts were prepared via ammonium and acid treatment. The clinoptilpolite is highly active in acid catalyst acetalization of aldehydes, affine chemical reaction. Activity was markedly influenced by the activation. A cooperative effect of Brønsted sites and 5-fold coordinated Al is discussed to explain the superior performance of the most active catalyst. Acknowledgments (times new roman, 9 pts) We gratefully acknowledge the excellent assistance of Dr. A. Villinger (XRD) and Dr. M. Frank (TEM images). References [1] A.Dziedziecka, B. Sulikowski, : Ruggiero-Mikulajczyk, Catal. Today, 2016, 259, 50-58. T2 - 8th International Symposium on Acid-Base Catalysis CY - Rio de Janeiro, Brazil DA - 07.05.2017 KW - Natural Zeolite Clinoptilolite PY - 2017 AN - OPUS4-40685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riaz, Muhammad T1 - Influence of the acidic, thermal, and water vapour treatment on the catalytic performance of acidic hierarchical structured clinoptilolite N2 - Clinoptilolite is a natural, medium pore size zeolite. It contains a 2-deminsional pore system consisting of oxygen-8- membered and oxygen-10-membered rings. It is one of the most abundant natural zeolites. It is mainly used as ion exchanger and adsorbent for removal of toxic elements and compounds from the environment. Although clinoptilolite is microporous and can be acidified by ion exchange or acid treatment and a potential catalyst, reports on its application in catalysis are limited so far. This contribution deals with modification of a natural zeolite clinoptilolite, and the study of the influence of the textural and acidic properties on the catalytic performance in the acid catalyzed acetalization of bezaldehyde with butandiol-1,3 and the more demanding etherification of glycerol with t-butanol or isomerization of n-hexane. The samples were acidified by via ammonium-ion exchange followed by calcination and acid treatment. Samples were characterized by XRD regarding crystallinity and phase composition, FTIR, and N2-adsorption for porosity. The morphology was studied by TEM images. The acidity was studied by ammonia-TPD measurements and 1H solid state MAS NMR. Structure and structural changes caused by applied modifications were studied by 27Al- and 29Si MAS NMR measurements and TRAPDOR experiments as well as thermal analysis. The studied natural zeolite tuff contained ca. 90 ma.-% of clinoptilolite. The ion exchange behavior was studied with ammonium nitrate solution and for comparison with HCl solution of similar concentration. The cation exchange was followed by AES. The activation temperature was varied between 400-600°C. The catalytic test was performed e.g. using ca. 0.2 g of the catalyst and ca.10g of the aldehyde or alcohol using toluene as solvent and under reflux. Reaction water was removed via a by-pass. The isomerization of n-hexane was performed in a fall stream reactor at elevated temperature at gas phase. Water vapour saturated air was passed over clinoptilolite samples at elevated temperature for different time. The ion exchange experiments shows that ca 45% of the cations of clinoptilolite readily exchange with ammonium ions and protons supplied by acid treatment. However, exchange with the acid has a more severe impact on the clinoptilolite structure. More severe treatment times leads to a loss of activity in terms of acetal formation. Sample show all high conversions after 4 h of reaction, but show markedly differences after short reaction times. The presence of acidic protons of medium to strong strength is confirmed by ammonia-TPD and proton NMR measurements. The sample activation causes a partial dealumination as indicated by the appearance of 5- and 6-fold coordinated aluminum. Interestingly, the NMR results give first hints for a relation of the catalytic conversion with the amount of 5-fold coordinated aluminum. The results will be discussed in terms of a collaborative action of Brønsted acid sites and 5-fold coordinated aluminum. Modified clinoptilpolite is highly active in acid catalyst acetalization of aldehydes, isomerization of n-hexane and etherification of glycerol with t-butanol. Acidic natural clinoptilolite catalysts prepared via ammonium exchange followed by calcination and acid treatment shows a positive influence on acidity and porosity. Modification creates hierarchical micro-nano porosity. The specific surface area varies between ca. 45 m2/g and 257 m2/g. T2 - EUROPA CAT 2017 CY - Florence Italy DA - 27.08.2017 KW - Natural Zeolite Clinoptilolite PY - 2017 AN - OPUS4-40687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Maiwald, Michael T1 - Low field NMR spectroscopy for process control - robust automated data preparation and analysis as prerequisites T1 - Niederfeld NMR-Spektroskopie für die Prozesskontrolle – Robuste und automatisierte Datenvorbehandlung und Datenanalyse als Grundvoraussetzungen N2 - Berichtet wird über die automatisierte und spektral-modellgestützte Datenauswertung quantitativer Online-NMR-Spektren von technischen Systemen, die einen grundlegenden Beitrag zum Thematik Smart Sensors im Sinne kalibrierarmer bzw. kalibrierfreier Verfahren liefern. Die quantitative Online-NMR-Spektroskopie ist besonders reizvoll für diese Thematik: Sie kommt durch den direkten Nachweis der Kernspins ohne Kalibrierung aus und arbeitet auch in Konzentrationsrandbereichen äußerst linear. Als „absolute Vergleichsmethode“ (direkte Proportionalität der Signale zu den Stoffmengen innerhalb eines Spektrums) ist die NMR-Spektroskopie für die durchgeführten Grundlagenuntersuchungen im Zusammenhang mit spektralen Modellen prädestiniert. T2 - Seminar des Institut für Mathematik, Universität Rostock CY - Rostock, Germany DA - 12.07.2017 KW - Prozessanalytik KW - Prozess-Sensoren 4.0 KW - Online NMR Spektroskopie KW - Indirect Hard Modeling PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-409694 AN - OPUS4-40969 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ismail, N. S. A1 - Le, Quynh Hoa A1 - Vu, T. H. A1 - Inoue, Yuki A1 - Yoshikawa, H. A1 - Saito, M. A1 - Tamiya, E. T1 - Electrochemiluminescence Based Enzymatic Urea SensorUsing Nanohybrid of Isoluminol-gold Nanoparticle-graphene Oxide Nanoribbons N2 - This study evaluates on the possibility of using gold nanoparticles functionalizedwith the luminol derivative N-(aminobutyl)-N-(ethylisoluminol)(ABEI) and hybridizedwith graphene oxidenanoribbons on acarbon based screen-printedelectrode (ABEI-AuNP-GONR/SPE) as an enzymaticelectrochemiluminescence (ECL) urea sensor.The electrocatalytic activity and ECL intensity of ABEI-AuNP-GONR/SPE were found to increase proportionally with the concentrationofurea in the analyte sample,owing to the rise in pH value.These phenomena are attributed to increased formation of luminol monoanion precursors for further electrochemical oxidation,which in turn produce eitherluminol radicals or excited3-amino-phthalate molecules.The luminescence is most likely caused by the interaction of luminol radicals with superoxide radicals formed from dissolved oxygen. Thesensitivity of our sensor was determinedtobe 170.58 mM@1 and 16.23 mM@1 for urea concentrations from 2to5.82 mM and from 5.82 to 30 mM, respectively, coveringthe normal urea level in human blood. KW - Nanomaterials KW - Graphene oxide KW - Biosensors PY - 2017 UR - http://onlinelibrary.wiley.com/doi/10.1002/elan.201600477 DO - https://doi.org/10.1002/elan.201600477 SN - 1040-0397 SN - 1521-4109 VL - 29 IS - 4 SP - 938 EP - 943 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-40970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tahri, K. A1 - Tiebe, Carlo A1 - El Bari, N. A1 - Hübert, Thomas A1 - Bouchikhi, B. T1 - Geographical classification and adulteration detection of cumin by using electronic sensing coupled to multivariate analysis N2 - The objective of this work is to report the improvement obtained in the discrimination of complex aroma and taste with subtle differences in odor and flavor, by the use of fast suitable procedures for the cases of measurements in the field demanding decision-making in real time. The proposed electronic sensing systems, formed by an E-nose and VE-tongue, were used to discriminate cumin cultivars from different geographical origins, as well as to quantify the cumin adulteration percentages by using unsupervised and supervised chemometric tools. Thus, the results obtained are sufficiently encouraging as a starting point for the development of new electronic sensing systems with more improvement such the reliability of the sensors’ performance as well as the chemometric tools in order to deal with a complex dataset. KW - VE-tongue KW - E-nose KW - Chemometric tools KW - Cumin discrimination KW - Geographical origins KW - Adulteration detection PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-409735 DO - https://doi.org/10.1016/j.protcy.2017.04.102 SN - 2212-0173 VL - 27 SP - 240 EP - 241 PB - Elsevier B.V. AN - OPUS4-40973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - BAM: Welche Referenzmaterialien produziert und wie sie zertifiziert werden… N2 - Die Bundesanstalt für Materialforschung und -prüfung (BAM) produziert seit über 100 Jahren zertifizierte Referenzmaterialien und ist seit 2016 auch als Referenzmaterialhersteller nach ISO Guide 34 akkredi- tiert. Heute werden eine Vielzahl von Referenzmaterialien aus den Gebieten Eisen/Stahl, Nichteisenmetalle, Keramik, Glas und Umwelt bereitgestellt. Im Vortrag werden die einzelnen Schritte der Referenzmaterialherstellung wie Probenpräparation, Homogenitätsuntersuchung und Zertifizierungsringversuch vorgestellt. Darüber hinaus werden Fragen der Zertifizierungsstrategie und Rückführbarkeit diskutiert. T2 - Seminar "Verbrennungsanalyse" CY - Velen, Germany DA - 20.06.2017 KW - Referenzmaterial KW - Homogenität KW - Rückführbarkeit PY - 2017 AN - OPUS4-40960 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schürmann, Robin A1 - Tanzer, Katrin A1 - Dąbkowska, Iwona A1 - Denifl, Stephan A1 - Bald, Ilko T1 - Stability of the parent anion of the potential radiosensitizer 8 ‑ Bromoadenine formed by low-energy (<3 eV) electron attachment N2 - 8-Bromoadenine (8BrA) is a potential DNA radiosensitizer for cancer radiation therapy due to its efficient interaction with low-energy electrons (LEEs). LEEs are a short-living species generated during the radiation damage of DNA by high-energy radiation as it is applied in cancer radiation therapy. Electron attachment to 8BrA in the gas phase results in a stable parent anion below 3 eV electron energy in addition to fragmentation products formed by resonant exocyclic bond cleavages. Density functional theory (DFT) calculations of the 8BrA– anion reveal an exotic bond between the bromine and the C8 atom with a bond length of 2.6 Å, where the majority of the charge is located on bromine and the spin is mainly located on the C8 atom. The detailed understanding of such long-lived anionic states of nucleobase analogues supports the rational development of new therapeutic agents, in which the enhancement of dissociative electron transfer to the DNA backbone is critical to induce DNA strand breaks in cancerous tissue. KW - Dissociative electron attachment KW - DNA damage KW - Radiosensitization KW - Mass spectrometry PY - 2017 DO - https://doi.org/10.1021/acs.jpcb.7b02130 SN - 1520-6106 VL - 121 IS - 23 SP - 5730 EP - 5734 AN - OPUS4-40963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kapa, Thomas T1 - Distributed Brillouin Sensors N2 - This presentation starts with an overview of various optical sensing applications of Department 8.6 Fiber Optic Sensors. Main topic of presentation is distributed Brillouin sensing of strain and temperature by Brillouin Optical Frequency Domain Analysis (BOFDA). For power grids of offshore wind farms temperature and strain sensing should prevent or rapidly reveal costly break downs. T2 - Seminarvortrag TU Clausthal CY - Goslar, Germany DA - 15.06.2017 KW - Fibre Optic Sensors KW - Stimulated Brillouin Scattering KW - Distributed Sensing PY - 2017 AN - OPUS4-40966 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Passiu, Cristiana A1 - Rossi, Antonella A1 - Bernard, Laetitia A1 - Paul, Dennis A1 - Hammond, John A1 - Unger, Wolfgang A1 - Venkataraman, Nagaiyanallur V. A1 - Spencer, Nicholas D. T1 - Fabrication and Microscopic and Spectroscopic Characterization of Planar, Bimetallic, Micro- and Nanopatterned Surfaces N2 - Micropatterns and nanopatterns of gold embedded in silver and titanium embedded in gold have been prepared by combining either photolithography or electron-beam lithography with a glue-free template-stripping procedure. The obtained patterned surfaces have been topographically characterized using atomic force microscopy and scanning electron microscopy, showing a very low root-mean-square roughness (<0.5 nm), high coplanarity between the two metals (maximum height difference ≈ 2 nm), and topographical continuity at the bimetallic interface. Spectroscopic characterization using X-ray photoelectron spectroscopy (XPS), time-of-flight secondary-ion mass spectrometry (ToF-SIMS), and Auger electron spectroscopy (AES) has shown a sharp chemical contrast between the two metals at the interface for titanium patterns embedded in gold, whereas diffusion of silver into gold was observed for gold patterns embedded in silver. Surface flatness combined with a high chemical contrast makes the obtained surfaces suitable for applications involving functionalization with molecules by orthogonal adsorption chemistries or for instrumental calibration. The latter possibility has been tested by determining the image sharpness and the analyzed area on circular patterns of different sizes for each of the spectroscopic techniques applied for characterization.This is the first study in which the analyzed area has been determined using XPS and AES on a flat surface, and the first example of a method for determining the analyzed area using ToF-SIMS. KW - XPS KW - AES KW - SIMS KW - Lateral resolution KW - Test pattern PY - 2017 UR - http://pubs.acs.org/doi/abs/10.1021/acs.langmuir.7b00942 DO - https://doi.org/10.1021/acs.langmuir.7b00942 SN - 0743-7463 VL - 33 IS - 23 SP - 5657 EP - 5665 PB - ACS AN - OPUS4-40929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Wirbelstromprüfung an Bahnkomponenten N2 - Nach einer kurzen Einführung in die Wirbelstromprüfung werden sowohl die Entwicklungen des FB 8.4 auf dem Gebiet der Wirbelstromprüfung an Bahnkomponenten der letzten Jahre als auch die Pläne für die Zukunft vorgestellt. T2 - BVG-Tag CY - Berlin, Germany DA - 07.07.2017 KW - Wirbelstromprüfung KW - Eisenbahn PY - 2017 AN - OPUS4-40931 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jakubowski, Norbert A1 - Schmidt, B. A1 - Sötebier, C. A1 - Pergantis, S. A1 - Shigeta, K. T1 - Single particle and single cell ICP-MS N2 - ICP-MS is a well-established analytical method which excels by high accuracy, high dynamic range and extremely low limits of detection for most metals. Furthermore ICP-MS offers a very high multi-element coverage so that many elements of the periodic table can be detected simultaneously. In this series of lectures, we want to focus on the historical developments, fundamentals, instrumentation and novel applications of ICP-MS in the life and material sciences. KW - Single particle ICP-MS KW - Single cell ICP-MS PY - 2017 AN - OPUS4-40952 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Progress Talk 1 / Working Group Meeting of Prof. Erhard Kemnitz (Humboldt-Universität zu Berlin) N2 - This presentation deals with the progress between month one and six of my PhD thesis. I prepared it, in order to update my supervisor Prof. Kemnitz and my colleagues from the department of chemistry at the Humboldt-Universität zu Berlin (HU). T2 - Working Group Meeting of Prof. Erhard Kemnitz CY - Humboldt-Universität zu Berlin (HU), Germany DA - 06.02.2017 KW - Core@shell nanoparticles KW - SEM KW - Synchrotron KW - XPS KW - TEM KW - EDX PY - 2017 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-40892 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Progress Talk 2 / Working Group Meeting of Prof. Erhard Kemnitz (Humboldt-Universität zu Berlin) N2 - This presentation deals with the progress between month seven and eleven of my PhD thesis. I prepared it, in order to update my supervisor Prof. Kemnitz and my colleagues from the department of chemistry at the Humboldt-Universität zu Berlin (HU). T2 - Working Group Meeting of Prof. Erhard Kemnitz CY - Humboldt-Universität zu Berlin (HU), Germany DA - 20.06.2017 KW - XPS KW - Synchrotron KW - Core@shell nanoparticles KW - SEM KW - ICP-MS PY - 2017 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-40893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lichtenstein, D. A1 - Böhmert, L. A1 - Meyer, Th. A1 - Sieg, H. A1 - Thünemann, Andreas A1 - Loipis, I. E. A1 - Bäuning, A. A1 - Lampen, A. T1 - Core or coating material? What dictates the uptake and translocation of nanoparticles in vitro? N2 - A core-dependent effect on nanoparticle translocation was revealed. Both the uptake and transport of nanoparticles in and through cells should be considered when discussing nanoparticle fate and safety. T2 - 52nd Congress of the European-Societies-of-Toxicology (EUROTOX) CY - Seville, Spain DA - 04.09.2016 KW - Small-angle X-ray scattering KW - SAXS KW - Silver KW - Nanoparticle PY - 2017 DO - https://doi.org/10.1016/j.toxlet.2016.06.1940 SN - 0378-4274 SN - 1879-3169 VL - 258 SP - S267 EP - S268 PB - Elsevier Ltd. AN - OPUS4-40935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lichtenstein, D. A1 - Meyer, Th. A1 - Böhmert, L. A1 - Sieg, H. A1 - Juling, S. A1 - Thünemann, Andreas A1 - Lopies, I. E. A1 - Bräuning, A. A1 - Lampen, A. T1 - Evidence for particle-specific and coating-related uptake of silver nanoparticles N2 - Present data indicate that the quantification of silver nanoparticle internalization revealed a clear particle-specific and coatingrelated uptake. Furthermore, a high amount of silver nanoparticles is taken up in cell models of higher complexity. Thus, an underestimation of particle effects in vitro might be prevented by considering cell models with greater proximity to the in vivo situation. T2 - 52nd Congress of the European-Societies-of-Toxicology (EUROTOX) CY - Seville, Spain DA - 04.09.2016 KW - Small-angle X-ray scattering KW - SAXS KW - Nanoparticle KW - Silver PY - 2017 DO - https://doi.org/10.1016/j.toxlet.2016.06.1938 SN - 0378-4274 VL - 258 SP - S267 EP - S267 PB - Elsevier Ltd. AN - OPUS4-40936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Material properties and their impact on laserinduced plasmas for concrete analysis N2 - For concrete production aggregates, cement and water are mixed together and after 28 days of hydration a porous and multiphase material is formed. To consider the heterogeneity of concrete a 2D scanning system is used. The coarse aggregates (limit > 2 X d ) can be excluded. laser spot The remaining content is a mixture of flour grains and cement particles (micro heterogeneity). Harmful species like chlorides may penetrate together with water through the capillary pore space. A quantification of Cl regarding to the cement content only (European standard EN 206) is necessary for the damage assessment. A LIBS system operating with a NdCr:YAG laser (pulse energy of 3 mJ, a wavelength of 1064 nm, a pulse width of 1.5 ns, a repetition rate of 100 Hz) and two Czerny-Turner spectrometer (UV and NIR range) have been used. T2 - EMSLIBS Konferenz 2017 CY - Pisa, Italy DA - 12.06.2017 KW - Concrete KW - LIBS KW - Micro-heterogeneity PY - 2017 AN - OPUS4-40938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sieg, H. A1 - Lehmann, C. A1 - Kästner, Claudia A1 - Krause, B. A1 - Burel, A. A1 - Chevance, S. A1 - Böhmert, L. A1 - Lichtenstein, D. A1 - Tentschert, J. A1 - Bräuning, A. A1 - Laux, A. A1 - Thünemann, Andreas A1 - Loipis, I. E. A1 - Fessard, V. A1 - Luch, A. A1 - Lampen, A. T1 - Effects of Al-, Ti- and Zn-containing nanomaterials on cell lines in vitro N2 - Among the different tested endpoints, Al- and Ticontaining nanomaterials did notshowany toxicity in intestinal cell lines in vitro. Nevertheless, this absence of effect was not due to an absence of exposure, since particle-specific uptake was reported. Metal particle uptake over a long time period might therefore be relevant for risk assessment of aluminum- and titanium-containing food products. T2 - 52nd Congress of the European-Societies-of-Toxicology (EUROTOX) CY - Seville, Spain DA - 04.09.2017 KW - Nanoparticles PY - 2017 DO - https://doi.org/10.1016/j.toxlet.2016.06.1954 SN - 0378-4274 VL - 258 SP - S272 PB - Elsevier Ltd. AN - OPUS4-40939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gottlieb, Cassian T1 - Influence of grain sizes on the quantification of libs measurements in concrete influence of grain sizes on the quantification of libs measurements in concrete N2 - Concrete is a multiphase material made of cement, aggregates and water. The heterogeneity of concrete is a result of mixing aggregates (grain size between 0.125 mm to 32 mm) and cement (grain size < 0.04 mm) together. There are always aggregates with a grain size below 0.125 mm (flour grains) therefore the cement matrix is always a mixture of these small particles. Different grain size distributions by making concrete are important to ensure the needed density and com-pressive strength. In order to estimate the remaining lifetime of concrete structures the quantification of element concentra-tions of alkali and chlorides regarding to the cement matrix only (1/3 of the total mass), is a major concern in civil engineer-ing. Due to two-dimensional scanning with LIBS the coarse aggregates can be evaluated and excluded from the analysis. In the case of particles (flour grains and cement) smaller than the laser spot size, the microscopic hetero-geneity influences the laser-plasma interaction and has therefore an impact on the results. In this study the influence of the micro-heterogeneity and the impact on the laser-material interaction is examined. The effect of changing ratios between cement particles and aggregate particles in the laser-induced plasma has been analyzed (see figure 1, right). Therefore, different samples with defined grain sizes are prepared and the obtained distributions were analyzed with x-ray diffraction (XRD). For the LIBS measurements, an automated system that operates with a low energy NdCr:YAG laser (pulse energy of 3 mJ, a wavelength of 1064 nm, a pulse width of 1.5 ns, a repetition rate of 100 Hz) and a NIR Czerny-Turner spectrometer has been used. T2 - EMSLIBS Konferenz 2017 CY - Pisa, Italy DA - 12.06.2017 KW - Grain size KW - LIBS KW - Concrete PY - 2017 AN - OPUS4-40940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Exploring the capabilities of near ambient pressure XPS: Characterisation of biofilms and nanoparticles in solution N2 - Seminar-talk for "Ausgewählte analytische Methoden der Physik " at TU Berlin. A introduction about near-ambient pressure XPS is given, furhter, results from measurements of biofilms and dispersed nanoparticles are presented and discussed. T2 - Seminar AG Kanngießer: Ausgewählte analytische Methoden der Physik CY - Technische Universität, Berlin, Germany DA - 04.07.2017 KW - Alginate KW - NAP-XPS KW - Nanoparticles KW - Biofilms KW - E. coli PY - 2017 AN - OPUS4-40905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Priebe, Nsesheye Susan T1 - Performance of rice husk ash as an alternative binder in a modified cementitious system N2 - The main objective of this project presentation was to evaluate the by-products of paddy farming (in Tanzania) into sustainable building materials optimised for construction of low-cost housing, and suitable to be adopted in rice-producing countries in Africa. In Tanzania, rice husks are seldom used as a fuel – if not burnt or dumped in landfills and there is lack of awareness or active research on optimising the by-product RHA in cement and concrete technology. Scientific research within this field of technology can advance development by obtaining suitable properties of the by-products that can provide an advantageous and alternative measure for their use as SCMs not only in its raw form i.e. husks for low-cost housing but also in its artificial form i.e. RHA as a high-tech as a substitute for cement in Africa. T2 - RICH Africa 1st Bilateral Workshop CY - Dar es Salaam, Tanzania DA - 04.04.2016 KW - Rice husk ash KW - Low-cost housing KW - Sub-Saharan Africa KW - Cement PY - 2016 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. AN - OPUS4-41034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Priebe, Nsesheye Susan T1 - Proceedings of the 3rd symposium knowledge exchange for young scientists (KEYS) - Applicable cement and concrete technology for sub-Saharan Africa - International cooperation, innovation, research and capacity building N2 - This third symposium focuses on applicable cement and concrete technology for sub-Saharan Africa – international cooperation, innovation, research and capacity building. The rise of sub-Saharan Africa’s economies is significant to development. However, such development should be sustainable in order to increase the economic stability of Africa. In terms of sustainability, applicable concrete technology with relevance to the market needs is suitable to build up the infrastructure of a society. In the current sub-Saharan African market, there exists an enormous potential in sustainable research for innovative construction. Education is of key importance to innovation alongside a sound interaction with key players in the construction sector. The symposium includes keynote lectures from 10 international keynote speakers and technical papers from 25 young scientists, who were selected out of a high number of applicants based on the excellence of their scientific writing. The presentations of all participants as well as keynote lectures are represented in these proceedings. T2 - 3rd Symposium on Knowledge Exchange for Young Scientists (KEYS) CY - Johannesburg, South Africa DA - 26.06.2017 KW - Cement and concrete relevant to Africa PY - 2017 SN - 978-3-9818270-7-1 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. VL - 3 SP - 1 EP - 230 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-41037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Applications of X-ray refraction to non-destructive characterization of ceramics and composites N2 - X-ray refraction is analogous to visible light deflection by matter, with two main differences: 1- convex objects cause divergence (i.e., the refraction index n is smaller than 1), and 2- deflection angles are very small, from a few seconds to a few minutes of arc (i.e., n is near to 1). Trivially but importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks, and quantify their densities in bulk (light) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, their detectability is simply limited by the wavelength of the radiation. We will thereby show the application of X-ray refraction 2D mapping (topography) and tomography to different sorts of problems in ceramic science and technology: 1) Sintering of SiC green bodies; 2) Porosity analysis in diesel particulate filter silicates; 3) fiber de-bonding in metal and polymer matrix composites; 4) micro-cracking of glass-precursor -eucryptite. We will see that the use of X-ray refraction analysis yields quantitative results, also directly usable in available models. T2 - FiMPART 2017 CY - Bordeaux, France DA - 09.07.2017 KW - Refraction radiography KW - Ceramics KW - Refraction tomography KW - Composites PY - 2017 AN - OPUS4-41040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Broadband dielectric spectroscopy in comparison to other spectroscopic methods applied to functional materials N2 - The basics of broadband dielectric spectroscopy were introduced in detail. The analysis of the data was discussed. As application of broadband dielectric spectroscopy the alpha-relaxation (dynamic glass transition) and the chain dynamics of polymers were illustrated. Further the application of dielectric spectroscopy to advanced functional materials. T2 - International Summer School on Crystal Growth and Advanced Materials for Energy Conversation CY - Bucharest, Romania DA - 10.07.2017 KW - Broadband dielectric spectroscopy PY - 2017 AN - OPUS4-41024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Effect of electrode configuration on dielectric strength testing N2 - Dielectric strength is a critical property for materials used as electrical insulators. The measurement of dielectric strength is well established and straightforward, but the values determined in a measurement are strongly dependent on the measurement setup and the specimen characteristics. For example, the size of the electrodes has a significant influence on the results. ASTM D149 covers a range of electrode sizes and does not unambiguously prescribe the quality of the electrodes. Thus, different test setups and procedures are used in the field. Consequently, a comparison of dielectric strength values of different origins, for example material supplier and customer, is often not meaningful. To quantify the influence of the test procedure on the dielectric strength values, a batch of industrial thick-film substrates has been tested with different electrode configurations under AC conditions. Opposing cylinders with diameters of 6.4 mm and 25 mm, and a thick-film metallization with a diameter of 25 mm were used in the study. At least 20 specimens were tested with each type of electrodes. The results range from 21.7 ± 0.7 kV/mm measured with printed electrodes to 26.7 ±1.2 kV/mm measured with reused 6.4 mm cylinders. This means a difference of 23 %. Measurements performed with 6.4 mm cylinder electrodes produce significantly lower values (ANOVA, α = 0.01) if a new set of electrodes is used for each measurement instead of reusing the same pair of electrodes for the entire batch. The dielectric strength measured with new 25 mm cylinders is 11.2 % lower than the values determined with new 6.4 mm cylinders. No significant difference (ANOVA, α = 0.01) was found for measurements with printed electrodes and opposing 25 mm cylinders. Weibull evaluation of the data showed that all tested electrode configurations result in a similar reliability of the specimen (Weibull modulus) but in a significantly different characteristic dielectric strength (scale factor, Bonferroni, α = 0.05). This study emphasizes the importance of a thorough and comprehensive documentation and communication of the test procedure for dielectric strength measurements. It further helps to evaluate the significance of differences in dielectric strength data provided by different sources. T2 - 15th Conference & Exhibition of the European Ceramic Society (ECerS2017) CY - Budapest, Hungary DA - 09.07.2017 KW - Dielectric strength KW - Ceramic KW - Insulators KW - Thick-film electrodes PY - 2017 AN - OPUS4-41025 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Priebe, Nsesheye Susan T1 - A modified cementitious system for sub-Saharan Africa N2 - Supplementary cementitious materials (SCMs) are largely used all over the world. The leading SCMs are fly ash (FA) and slag. However, such materials originate from industries that are not well established in sub-Saharan Africa (SSA). Therefore, it becomes extremely challenging and expensive to build up sustainable cement and concrete. For SSA, agriculture is one of the leading economic sectors. Agricultural by-products such as rice husk ash (RHA), can be a potential binder material beneficial for use in a cementitious system. RHA combined with limestone filler (LSF) is an option that can be practised for rice producing countries in Africa. T2 - PhD Day CY - Berlin, Germany DA - 14.07.2015 KW - Supplementary cementitious materials KW - Rice husk as KW - Cement KW - Concrete KW - Sustainable PY - 2015 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. AN - OPUS4-41029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Introduction to multivariate Data Analysis N2 - Multivariate data analysis is a universal tool for the evaluation of process spectroscopic data. In process analytics, huge amounts of information are produced i) by the many variables contained in one spectrum often exceeding 1000 (wavenumbers, wavelength, shifts…), and ii) the high number of spectra that is generated within the measurement period. Multivariate data analysis, often also called Chemometrics, help to extract the relevant information which is needed to examine and even control processes. Therefore, calibration models must be precise and robust, and moreover, must cover a wide range of variation of factors posing an influence on the process. In this pre-conference course an introduction to both, explorative data analysis by PCA (Principal Component Analysis), and regression analysis by the most frequently used method, i.e. PLSR (Partial Least Squares Regression) is given. In principal, all optical spectroscopic methods are suited for multivariate evaluation. It will be demonstrated that under certain preconditions, even process NMR spectra can be predicted by PLSR models. At first, basic principles of multivariate data analysis will be provided. This includes a short introduction into the concept of model building and interpretation of results. Detailed aspects of data pretreatment and calibration & validation strategies for chemometric models will be provided with own data from NIR, Raman and NMR spectroscopy. In a first example, the development of an online compatible method for the quantification of methanol in biodiesel by PLSR is presented. This also includes the classification of biodiesel feedstocks by PCA and statistical tools which allow for the estimation of a full uncertainty budget. The Raman spectroscopic prediction of Hydroformylation reaction in a miniplant is used to discuss shortcomings and pitfalls which may occur with the transfer of off-line models to the real processes. Design of experiment and strategies for suitable lab-scale experiments are presented as a possible way to overcome problems. In a third application the prediction of the reactants of an esterification reaction based on process NMR data is demonstrated. T2 - EuroPACT 2017 4rd European Conference on Process Analytics and Control Technology CY - Potsdam, Germany DA - 10.05.2017 KW - Chemometrics KW - PLSR KW - Spectroscopy PY - 2017 UR - www.euro-pact.de AN - OPUS4-41016 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Usmani, Shirin T1 - Wood protection with nanoparticles: MgF2 and CaF2 N2 - Alkaline earth metal fluoride nanoparticles have been investigated for application in wood protection. Sols of MgF2 and CaF2 were synthesized and their efficacy was tested against fungi and termites (Rehmer 2016, Krahl et al. 2016). The sols were characterized by XRD and SEM. The wood specimens were vacuum impregnated with nanoparticles and then exposed to fungi and termites according to EU certified test conditions. Our results show that wood impregnated with metal fluoride nanoparticles significantly reduce cellulose hydrolysis by fungi and termites. The wood samples were exposed to brown-rot fungi; Coniophora puteana and Poria placenta. Between the two fungi, the overall mass lost due to fungal degradation was lower for treated (MgF2 and CaF2) wood samples exposed to Coniophora puteana. Thus, the metal fluoride nanoparticles impregnated in the wood samples were more efficient in reducing cellulose degradation from Coniophora puteana than from Poria placenta. However the mass loss in samples treated with MgF2 was similar to those treated with CaF2, irrespective of type of fungi. Therefore, it is likely that fungal degradation in treated samples was dependent on the biocidal action of fluorides rather than on the differences in chemical and physical properties of MgF2 and CaF2, respectively. Conversely, for termite exposure, wood samples treated with MgF2 had lower cellulose degradation compared to those treated with CaF2. A possible explanation for this difference in results could be fungi and termites use separate mechanisms for cellulose hydrolysis which will be further investigated. Future experiments include testing the leaching potential of MgF2 and CaF2 nanoparticles from wood. The results from the leaching experiment will test if metal fluoride nanoparticles can provide long-term and environmentally safe protection to wood. T2 - International Research Group (IRG48) Scientific Conference on Wood Protection CY - Ghent, Belgium DA - 04.06.2017 KW - Fluoride KW - Nanoparticles KW - Brown-rot fungi KW - Termites PY - 2017 AN - OPUS4-41019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kulow, Anicó T1 - S²XAFS: A new experimental setup for time-resolved X-ray absorption fine structure spectroscopy in a 'single shot' N2 - A newly developed EXAFS setup is presented. It enables both time- and spatially resolved EXAFS information simul-taneously in a single shot. First tests of this setup were performed at the BAMline @ BESSY-II (Berlin, Germany). A primary broadband beam generated by a filter/X-ray-mirror combination passes through the sample and is then dif-fracted by a convexly bent Si (111) crystal. This results in a divergent beam which is collected by an area sensitive detector, in a θ-2θ-geometry. Beside tests on metal foils the first in situ measurements were successfully carried out. The case-study deals with research on Zn-based Metal-Organic-Frameworks (MOF) with medical/pharmaceutical applications. This hot topic of MOFs research concerns drug delivery and encapsulation of therapeutically relevant proteins (e.g. BSA). Questions like how does a certain protein influences the coordination of Zn can be answered with this new setup. We were able to track structural changes within a 1s time resolution. T2 - CSI XL CY - Pisa, Italy DA - 11.06.2017 KW - XAFS KW - Time-resolved KW - Dispersive KW - In-situ measurement PY - 2017 AN - OPUS4-41052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Redmer, Bernhard T1 - Mobile Tomographic X-Ray Inspection N2 - A special 3D tomographic algorithm was developed for mobile inspection of large objects. The method is based on a coplanar movement of an X-ray tube parallel to the surface of a digital detector array (DDA). Two different designs were developed and applied for 3D testing of welded pipes in nuclear power plants and large aircraft components made from carbon fiber reinforced polymers (CFRP). The reconstructed tomo-graphic images permit the detection, characterization and measurement of the dimensions of flaws with en-hanced sensitivity compared to conventional radiography and UT. T2 - Far East NDT New Technology & Application Forum 2017 CY - Xi'an, Shaanxi province, China DA - 22.06.2017 KW - Computed tomography KW - Laminography KW - Weld inspection KW - Fibre composites KW - Aircrafts PY - 2017 AN - OPUS4-41055 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Swaraj, S. A1 - Dietrich, Paul A1 - Unger, Wolfgang T1 - Simultaneous surface and bulk sensitive XAS measurements of magnetic particle clusters N2 - Magnetic iron oxide nanoparticle clusters (mnpc) coated with organic stabilizers were investigated using scanning transmission x-ray microscopy (STXM). Simultaneous surface and bulk sensitive Fe L₃ edge absorption spectra, obtained using a photomultiplier tube and a channeltron, were used to detect subtle changes in the oxidation state in the surface and bulk of Iron Oxide mnpc. The effectiveness of this mode of STXM operation is demonstrated for these nanoparticle clusters. T2 - X-Ray Microscopy Conference 2016 (XRM 2016) CY - Oxford, UK DA - 15.08. 2016 KW - Fe L3 edge absorption spectra KW - Scanning transmission x- ray microscopy KW - Magnetic iron oxide nanoparticle clusters KW - XAS PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-410576 UR - http://iopscience.iop.org/article/10.1088/1742-6596/849/1/012014/pdf DO - https://doi.org/10.1088/1742-6596/849/1/012014 SN - 1742-6588 VL - 849 SP - 012014, 1 EP - 012014, 5 PB - IOP Publishing AN - OPUS4-41057 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Stability and homogeneity of alginate samples N2 - Overview of measurements and future work regarding near ambient pressure XPS on alginate samples relevant for the EMPIR-project MetVBadBugs- Quantitative measurement and imaging of drug-uptake by bacteria with antimicrobial resistance. T2 - MetVBadBugs 18M Meeting CY - PTB, Berlin, Germany DA - 17.07.2017 KW - Alginate KW - NAP-XPS KW - Biofilms PY - 2017 AN - OPUS4-41077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Thiel, Erik T1 - Thermal Wave Interference with High-Power VCSEL Arrays For Locating Vertically Oriented Subsurface Defects N2 - Among the photothermal methods, full-field thermal imaging is used to characterize materials, to determine thicknesses of layers, or to find inhomogeneities such as voids or cracks. The use of classical light sources such as flash lamps (impulse heating) or halogen lamps (modulated heating) led to a variety of nondestructive testing methods, in particular lock-in and flash-thermography. In vertical cavity surface emitting lasers (VCSELs), laser light is emitted perpendicular to the surface with a symmetrical beam profile. Due to the vertical structure, they can be arranged in large arrays of many thousands of individual lasers, which allows power scaling into the kilowatt range. Recently, a high-power yet very compact version of such a VCSEL-array became available that offers both the fast timing behavior of a laser as well as the large illumination area of a lamp. Moreover, it allows a spatial and temporal control of the heating because individual parts of the array can be controlled arbitrarily in frequency, amplitude, and phase. In conjunction with a fast infrared camera, such structured heating opens up a field of novel thermal imaging and testing methods. As a first demonstration of this approach, we chose a testing problem very challenging to conventional thermal infrared testing: The detection of very thin subsurface defects perpendicularly oriented to the surface of metallic samples. First, we generate destructively interfering thermal wave fields which are then affected by the presence of defects within their reach. It turned out that this technique allows highly sensitive detection of subsurface defects down to depths in excess of the usual thermographic rule of thumb, with no need for a reference or surface preparation T2 - QNDE 2017 CY - Provo, Utah, USA DA - 17.07.2017 KW - Thermal Wave KW - Photothermal KW - Active Thermography KW - VCSEL KW - Subsurface Defect PY - 2017 AN - OPUS4-41078 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Daly, M. A1 - Burnett, T. L. A1 - Pickering, E. J. A1 - Tuck, O. C. G. A1 - Léonard, Fabien A1 - Kelley, R. A1 - Withers, P. J. A1 - Sherry, A. H. T1 - A multi-scale correlative investigation of ductile fracture N2 - The use of novel multi-scale correlative methods, which involve the coordinated characterisation of matter across a range of length scales, are becoming of increasing value to materials scientists. Here, we describe for the first time how a multi-scale correlative approach can be used to investigate the nature of ductile fracture in metals. Specimens of a nuclear pressure vessel steel, SA508 Grade 3, are examined following ductile fracture using medium and high-resolution 3D X-ray computed tomography (CT) analyses, and a site-specific analysis using a dual beam plasma focused ion beam scanning electron microscope (PFIB-SEM). The methods are employed sequentially to characterise damage by void nucleation and growth in one volume of interest, allowing for the imaging of voids that ranged in size from less than 100 nm to over 100 mm. This enables the examination of voids initiated at carbide particles to be detected, as well as the large voids initiated at inclusions. We demonstrate that this multi-scale correlative approach is a powerful tool, which not only enhances our understanding of ductile failure through detailed characterisation of microstructure, but also provides quantitative information about the size, volume fractions and spatial distributions of voids that can be used to inform models of failure. It isfound that the vast majority of large voids nucleated at MnS inclusions, and that the volume of a void varied according to the volume of its initiating inclusion raised to the power 3/2. The most severe voiding was concentrated within 500 mm of the fracture surface, but measurable damage was found to extend to a depth of at least 3 mm. Microvoids associated with carbides (carbide-initiated voids) were found to be concentrated around larger inclusion-initiated voids at depths of at least 400 mm. Methods for quantifying X-ray CT void data are discussed, and a procedure for using this data to calibrate parameters in the Gurson-Tvergaard Needleman (GTN) model for ductile failure is also introduced. KW - Gurson model KW - SA508 KW - Correlative tomography KW - Void nucleation & growth KW - X-ray computed tomography PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-414547 UR - http://www.sciencedirect.com/science/article/pii/S1359645417302203?via%3Dihub DO - https://doi.org/10.1016/j.actamat.2017.03.028 VL - 130 SP - 56 EP - 68 PB - Elsevier AN - OPUS4-41454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Pelkner, Matthias A1 - Kreutzbruck, Marc ED - Fermon, C. ED - Van de Voorde, M. H. T1 - Spin Electronics for Non Destructive Testing N2 - Electromagnetic methods are widely used in Non-destructive Testing industries (NDT). In order to meet the requirements, safety-relevant products and structures have to be tested reliably during production or within subsequent maintenance cycles. For this purpose industrial users call for adapted testing methods which allow the detection of relevant defects such as cracks and pore in ferromagnetic or conductive materials. Automated testing systems and the application of sensor arrays are of great interest in order to enhance inspection quality and to decrease testing time and costs. Magneto resistance (MR) sensors like giant magneto resistance (GMR) or tunnel magneto resistance sensor (TMR) have proofed their suitability in many NDT-applications due to their extraordinary properties which combine high field sensitivity, a high spatial resolution and low costs. Due to their small size these sensors can be useful – in addition to the pure detection task – for a more detailed defect characterization and defect reconstruction providing defect size, orientation and geometry. This chapter gives a brief introduction of electromagnetic testing methods, i.e., magnetic particle inspection (MPI) and eddy current testing (ET), followed by two different approaches for which MR sensor arrays were successfully adapted. KW - Magneto resistance KW - GMR KW - TMR KW - Non-destructive testing KW - Magnetic flux leakage KW - Eddy current PY - 2017 SN - 978-3-527-33985-3 SP - 81 EP - 102 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-41463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - Benefits of GMR sensors adapted for NDT applications N2 - Main concept of magnetism and, therefore, of magnetic imaging can be subdivided into different levels, macroscopic, magnetic domain, and atomic. While conventional sensor solutions cover only the macroscopic level, the spatial resolution of GMR (Giant Magneto Resistance) sensors go down to the domain scale. In addition, those low cost sensors are well suited for automotive and industrial applications, particularly high-speed solutions. Main reason is their outstanding performance in terms of high spatial resolution, high accuracy, high bandwidth combined with field sensitivity, energy efficiency and durability. In contrast to industrial use, down to the present day GMR sensors do not get beyond scientific scope in case of non-destructive testing (NDT) applications. Nevertheless, there are scientific and industrial NDT applications in which adapted GMR sensor can be promising compared to the conventional NDT methods. This contribution summarizes findings at the BAM over the last decade which demonstrates the preeminent properties of GMR-based testing solutions. This comprises the active and passive testing of different materials with hidden defects and flaws near geometric boundaries like edges where conventional methods meet their limits. Another promising application for adapted GMR sensors is the characterization of magnetic materials, where the sensors provide additional information on microstructure, mechanical stress state, phase transformations and their interaction with magnetic fields. The examples show the need and benefit of NDT adapted GMR sensors. T2 - QNDE - 44th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Provo, Utah, USA DA - 16.07.2017 KW - NDT KW - GMR KW - Magnetic flux leakage KW - Eddy current KW - Residual stress PY - 2017 AN - OPUS4-41465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - Eddy Current testing of Composite Pressure Vessels N2 - The use of composite pressure vessels instead of conventional vessels made of steel or aluminum grew strongly over the last decade. The reason for this trend is the tremendous weight saving in case of composite vessels. However, the long-time behavior is not fully understood for filling and discharging cycles and creep strength and their influence on the CFRP coating (carbon fiber reinforced plastics) and the internal liner (steel, aluminum, or plastics) [1]. The CFRP ensures the pressure resistance while the inner liner is used as container for liquid or gas. To overcome the missing knowledge of ageing BAM started an internal project to investigate degradation of these material systems [2]. Therefore, applicable testing methods are needed. Normally, high-frequency eddy current testing (HF-ET, f > 10 MHz) is deployed for CFRP due to its low conductivity of the fiber, which is in the order of 0.01 MS/s, and the capacitive coupling between the fibers. Nevertheless, in some cases conventional ET can be applied. We show a concise summary of studies on the application of conventional ET of composite pressure vessels. T2 - QNDE - 44th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Provo, Utah, USA DA - 16.07.2017 KW - eddy current KW - composites KW - pressure vessels KW - CFRP PY - 2017 AN - OPUS4-41466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Thorid T1 - Mehr-Proben-Kleb-Technologie zur Validierung der Klebfestigkeit N2 - Mit der Verfügbarkeit der Mehr-Proben-Prüfung von bis zu 8 Klebverbunden mittels CAT-Technologie (CAT: centrifugal adhesion testing) wurde im Forschungsvorhaben OKTETT ein durchgehendes Mehr-Proben-Konzept zur Validierung der Klebfestigkeit angewendet. Dazu gehört ein universeller Probenteller zur Mehr-Proben-Handhabung bei Vorbehandlung, Lagerung, Transport und Klebung. Für das Mehr-Proben-Kleben wurde die MSB-Technologie (MSB: multiple sample bonding) unter Verwendung einer instrumentierten hydraulischen Mehr-Proben-Klebvorrichtung entwickelt. Damit kann der Klebandruck für bis zu 8 Prüfkörper über einen Drucksensor definiert eingestellt und die gesamte Vorrichtung beim Kleben Temperatu-ren von bis zu 180°C ausgesetzt werden. T2 - 12. ThGOT Thementage Grenz- und Oberflächentechnik und 5. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 14.03.2017 KW - Zentrifugentechnologie KW - Mehr-Proben-Kleben (MSB) KW - Mehr-Proben-Prüfen (CAT) KW - Haftfestigkeit KW - Verbundfestigkeit PY - 2017 SN - 978-3-00-055614-2 SP - 1 EP - 2 AN - OPUS4-41467 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Sensor Roadmap 4.0 – Prospects towards a uniform topology for process control and smart sensor networks N2 - Smart functions of sensors simplify their use and enable plug-and-play, even though they are more complex. This is particularly important for, self-diagnostics, self-calibration and self-configuration/parameterization. Intelligent field devices, digital field networks, Internet Protocol (IP)-enabled connectivity and web services, historians, and advanced data analysis software are providing the basis for the future project “Industrie 4.0” and Industrial Internet of Things (IIoT). Important smart features include connectivity and communication ability according to a unified protocol (OPC-UA currently most widely discussed), maintenance and operating functions, traceability and compliance, virtual description to support a continuous engineering, and well as interaction capabilities between sensors. This is a prerequisite for the realization of Cyber Physical Systems (CPS) within these future automation concepts for the process industry. Therefore, smart process sensors enable new business models for users, device manufacturers, and service providers. The departure from current automation to smart sensor has already begun. Further development is based on the actual situation over several steps. Possible perspectives will be via additional communication channels to mobile devices, bidirectional communication, integration of the cloud and virtualization. The integration of virtual runtime environments can provide a more flexible topology for process control environments. The talk summarizes the currently discussed requirements to process sensors 4.0 and introduces an online NMR sensor as an example, which was developed in the EU project CONSENS. T2 - Swiss Chemical Society Fall Meeting, Symposium on PAT & Industry 4.0 CY - Bern, Switzerland DA - 21.08.2017 KW - Process Monitoring KW - Smart Sensors KW - Reaction Monitoring KW - Indirect Hard Modeling KW - Online NMR Spectroscopy KW - Industrie 4.0 PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-414683 AN - OPUS4-41468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Kabelitz, Anke A1 - Zimathies, Annett A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Crystal structure and in situ investigation of a mechanochemical synthesized 3D zinc N-(phosphonomethyl)glycinate N2 - The mechanochemical synthesis of the zinc N-(phosphonomethyl)glycinate Zn(O₃PCH₂NH₂CH₂CO₂) H₂O is presented. The structure was solved from powder X-ray diffraction (PXRD) data. In the three-dimensional pillared structure, the Zn atoms are coordinated tetrahedrally. In situ investigations of the reaction process with synchrotron PXRD and Raman spectroscopy reveal a two-step process including the formation of an intermediate. KW - Mechanochemistry KW - Metal phosphonate KW - In situ PY - 2017 DO - https://doi.org/10.1007/s10853-017-1121-7 SN - 0022-2461 SN - 1573-4803 VL - 52 IS - 20 SP - 12013 EP - 12020 PB - Springer CY - New York AN - OPUS4-41490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, G. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinsch, Stefan A1 - Kemnitz, E. A1 - Emmerling, Franziska T1 - Ca- and Sr- tetrafluoroisophthalates: mechanochemical synthesis, characterization, and ab initio structure determination N2 - New fluorinated coordination polymers were prepared mechanochemically by milling the alkaline earth metal hydroxides MII(OH)2·xH2O (MII: Ca, Sr) with tetrafluoroisophthalic acid (H2mBDC-F4). The structures of [{Ca(mBDC-F4)(H2O)2}·H2O] and [{Sr(mBDC-F4)(H2O)2}·H2O] were determined based on ab initio calculations and their powder X-ray diffraction (PXRD) data. The compounds are isomorphous and crystallize in the orthorhombic space group P212121. The determined structures were validated by using extended X-ray absorption (EXAFS) data. The new materials were thoroughly characterized using elemental analysis, thermal analysis, magic angle spinning NMR, and attenuated total reflection-infrared spectroscopy. Further characterization methods such as BET, dynamic vapor sorption, and scanning electron microscopy imaging were also used. Our investigations indicate that mechanochemistry is an efficient method for preparing such materials. KW - Mechanochemistry KW - In situ KW - XRD KW - Coordination polymers PY - 2017 UR - http://pubs.rsc.org/-/content/articlehtml/2017/dt/c7dt00734e DO - https://doi.org/10.1039/c7dt00734e VL - 46 IS - 18 SP - 6003 EP - 6012 AN - OPUS4-41516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matoga, D. A1 - Roztocki, K. A1 - Wilke, Manuel A1 - Emmerling, Franziska A1 - Oszajca, M. A1 - Fitta, M. A1 - Bałanda, M. T1 - Crystalline bilayers unzipped and rezipped: solid-state reaction cycle of a metal–organic framework with triple rearrangement of intralayer bonds N2 - We present a series of remarkable structural transformations for a family of layered metal–organic frameworks (MOFs) in a three-step solid-state reaction cycle. The cycle represents new dynamic behavior of 2D coordination polymers and involves the sequence of reactions: {[Mn2(ina)4(H2O)2]·2EtOH}n (JUK-1) → {(NH4)2[Mn(ina)2(NCS)2]}n·xH2O (JUK-2) → {[Mn2(ina)2(Hina)2(NCS)2]}n (JUK-3) → JUK-1 (Hina = isonicotinic acid), each accompanied by rearrangement of intralayer coordination bonds and each induced by a different external stimulus. In situ investigation of the first step of the cycle by combined synchrotron X-ray diffraction and Raman spectroscopy reveals direct mechanochemical unzipping of JUK-1 bilayers to respective JUK-2 layers with reaction rates dependent on the milling conditions. In contrast, the reverse zipping of JUK-2 layers involves two steps and proceeds through a new MOF (JUK-3) whose structure was elucidated by powder X-ray diffraction. Magnetic measurements confirm conversions of manganese nodes in the reaction cycle. The findings indicate the possibility of developing coordination-based assemblies with large structural responses for use in smart stimuli-responsive systems and sensor technologies. KW - Mechanochemistry KW - In situ KW - XRD KW - MOF PY - 2017 UR - http://pubs.rsc.org/is/content/articlehtml/2017/ce/c7ce00655a DO - https://doi.org/10.1039/C7CE00655A VL - 19 SP - 2987 EP - 2995 AN - OPUS4-41517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pavlovic, Mato A1 - Zoëga, Andreas A1 - Kurz, J. H. A1 - Zanotelli, Christina T1 - Investigations to introduce the probability of detection method for ultrasonic inspection of hollow axles at Deutsche Bahn N2 - The vast experience with the automated, ultrasonic system for the inspection of hollow railway axles used by Deutsche Bahn shows that much smaller flaws are detectable than required. This results in a number of false calls. False calls lead to unnecessary demounting and disassembling of wheelsets, which generates unnecessary additional costs. In order to adjust the sensitivity of the inspection system to reduce the number of false calls without compromising safety, the capability of the system to detect cracks needs to be comprehensively established. This capability can be quantified by using probability of detection (POD) curves for the system. The multi-parameter POD model makes it possible to include several factors that influence the crack detection in the analysis. The analysis presented in this paper shows that crack position, orientation, depth extension, and shape as well as the geometry of the axle all have influence on the ultrasonic response amplitude. For future work, calculation of the POD using multi-parameter POD model with these parameters is planned. T2 - ESIS TC24 Workshop "Integrity of Railway Structures" CY - Leoben, Austria DA - 24.10.2016 KW - Crack KW - Reliability KW - POD KW - Axle KW - Ultrasonic PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-415201 DO - https://doi.org/10.1016/j.prostr.2017.07.002 SN - 2452-3216 VL - 4 SP - 79 EP - 86 PB - Elsevier, B.V. AN - OPUS4-41520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Analysis of fluorine traces in TiO2 nanoplatelets by SEM/EDX, AES and TOF-SIMS N2 - Hydrothermal synthesis of anatase TiO2 nanosheets with a high fraction of exposed {001} facets and related high photocatalytic activity - as an alternative to bipyramidal anatase TiO2 nanoparticles mainly exposing the {101} facets. The scope of the material preparation work is the thermal reduction of residual fluorides from HF (capping agent) induced during the synthesis of TiO2 nanosheets by calcination at 873K. The analytical task consists of detection and localization of fluorine present at the surface and/or in the bulk of TiO2 nanosheets before and after calcination by SEM/EDX, Auger electron spectroscopy and ToF-SIMS. T2 - Microscopy & Microanalysis 2017 Meeting CY - St. Louis, MO, USA DA - 06.08.2017 KW - Nanoplatelets KW - Fluorine KW - SEM/EDX KW - Auger electron spectroscopy KW - ToF-SIMS KW - TiO2 PY - 2017 AN - OPUS4-41579 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schukar, Vivien A1 - Köppe, Enrico A1 - Hofmann, Detlef A1 - Mitzkus, Anja A1 - Gong, Xin A1 - Sahre, Mario A1 - Bartholmai, Matthias A1 - Beck, Uwe ED - Emri, Igor T1 - A contribution to intelligent automatic validation of structure-integrated fibre optic strain sensors N2 - An auto-validation tool for the reliability quantification of materials integrated fiber Bragg grating (FBG) strain sensors have been developed and tested. The FBG strain sensor was jacketed with a magnetostrictive layer based on iron-nickel which, when excited by a specific magnetic field, adds an artificial strain to the sensor. The fixed relationship between magnetic induction and wavelength shift of the FBG strain sensor characterizes the bond strength and adhesion between the sensor and the surrounding structure. Due to an easily applicable magnetic field, it is possible to validate the sensor performance in a non-contact, fast way without disturbing the data-acquisition process. T2 - 33nd Danubia Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Fiber Bragg grating KW - Self-diagnosis KW - Magnetostriction KW - Strain KW - Auto-validation PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S2214785317308489 DO - https://doi.org/10.1016/j.matpr.2017.06.073 SN - 2214-7853 VL - 4 IS - 5, Part 1 SP - 5935 EP - 5939 PB - Elsevier Ltd. AN - OPUS4-41583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Lazik, D. A1 - Bartholmai, Matthias ED - Emri, Igor T1 - Validation of membrane-based linear soil gas sensors under field conditions N2 - A 400 m2 soil test field with gas injection system was built up, which enables an experimental validation of linear membrane-based gas sensors – a sensor technology which was developed based on the selective permeation of gases through membranes. Several soil watering and injection experiments with carbon dioxide at different days with varying boundary conditions were performed showing that the sensor behaves mostly insensitive to the environmental conditions investigated, i.e., barometric pressure fluctuations, soil temperature, air temperature and humidity, sun duration, and wind speed. Furthermore, depending on water infiltration, a gas phase displacement could be observed in-situ based on the changed measurement signal. The results of the validation experiments highlight the potential of the method for rapid leak detection and localization qualifying the sensor particularly for safety applications, e.g., in underground gas storage areas. T2 - 33nd Danubia Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Distributed linear sensor KW - Membrane-based gas sensing KW - Subsurface monitoring KW - Gas storage areas KW - Validation PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S2214785317308404 DO - https://doi.org/10.1016/j.matpr.2017.06.065 SN - 2214-7853 VL - 4 IS - 5, Part 1 SP - 5893 EP - 5897 PB - Elsevier Ltd. AN - OPUS4-41584 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bagcioglu, M. A1 - Kohler, A. A1 - Seifert, Stephan A1 - Kneipp, Janina A1 - Zimmermann, B. T1 - Monitoring of plant-environment interactions by high-throughput FTIR spectroscopy of pollen N2 - 1. Fourier transform infrar ed (FTIR) spectroscopy enables chemical analysis of pollen samples for plant phenotyping to stud y plant–environment interactions, such as influence of climate change or pathogens. However, current approach, such as microspectrosc opy and attenuated total refle ction spectrosco py, doe s not allow fo r high-throughput protocols. This st udy at hand suggests a new sp ectroscopic method for high-throughp ut characterization of pollen. 2. Samples were measured as thin films of pollen fragments using a Bruker FTIR spe ctrometer with a high-throughput eXTension (HTS-XT) unit employing 384-well plates. In total, 146 pollen samples, belonging to 31 different pollen species of Fagaceae and Betulaceae and collected during three consecutive years (2012–2014) at locations in Croatia, Germany and Norway, were analysed. Critical steps in the sample preparation and measurement, such as variabilities between technical replicates, between microplates and between spectrometers, were studied. 3. Measurement variations due to sample preparation, microplate holders and instrumentation were low, and thus allowed differentiation of samples with respect to phylogeny and biogeography. The spectral variability for a ran ge of Fagales spec ies (Fagus, Quercus, Betula, Corylus, Alnus and Ostrya) showed high-species-specific differences in pollen’s chemical composition due to eithe r location or year. Statistically significant inter-annual and locational differences in the pollen spectra indicate that pollen chemical composition has high phenotypic plasticity and is influenced by local climate conditions. The variations in composition are connected to lipids, proteins, carbohydrates and sporopollenins that play crucial ro les in cold and desiccation tolerance, protection against UV radiation and as material and energy reserves. 4. The results of this study demonstrate the value of high-throughput FTIR approach for the systematic collection of data on ecosystems. The novel FTIR approach offers fast, reliable and economical screening of large number of samples by semi-automated methodology. The high-throughput approach could provide crucial understanding on plant–climate interactions with respect to biochemical variation within genera, species and populations. KW - Ecology and environmental sciences KW - Infrared spectroscopy KW - Pollen PY - 2017 UR - http://onlinelibrary.wiley.com/doi/10.1111/2041-210X.12697/epdf DO - https://doi.org/10.1111/2041-210X.12697 VL - 8 IS - 7 SP - 870 EP - 880 PB - British Ecological Society CY - London, UK AN - OPUS4-41540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Gräßer, Patrick A1 - Wander, Lukas A1 - Zientek, Nicolai A1 - Guhl, Svetlana A1 - Meyer, Klas A1 - Kern, Simon T1 - Strangers in the Night—Smart Process Sensors in Our Current Automation Landscape N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Smart sensors enable concepts like self-diagnostics, self-calibration, and self-configuration/parameterization whenever our current automation landscape allows it. Here we summarize the currently discussed general requirements for process sensors 4.0 and introduce a smart online NMR sensor module as example, which was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). T2 - Eurosensors 2017 Conference CY - Paris, France DA - 03.09.2017 KW - Process Monitoring KW - Smart Sensors KW - CONSENS KW - Online NMR Spectroscopy KW - Mini-plant PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-415772 UR - http://www.mdpi.com/2504-3900/1/4/628 DO - https://doi.org/10.3390/proceedings1040628 VL - 1 SP - 628 EP - 631 PB - MDPI CY - Basel AN - OPUS4-41577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Electrospray as a sample preparation tool for electron microscopic investigations: Toward quantitative evaluation of nanoparticles N2 - The potential of electrospray deposition, for the controlled preparation of particles for imaging in electron microscopes, is evaluated on various materials: from mono-modal suspensions of spherical particles to multimodal suspensions and to real-world industrial materials. It is shown that agglomeration is reduced substantially on the sample carrier, compared with conventional sample preparation techniques. For the first time, it is possible to assess the number concentration of a tri-modal polystyrene suspension by electron microscopy, due to the high Deposition efficiency of the electrospray. We discovered that some suspension stabilizing surfactants form artifact particles during electrospraying. These can be avoided by optimizing the sprayed suspension. T2 - Microscopy & Microanalysis 2017 Meeting CY - St. Louis, MO, USA DA - 06.08.2017 KW - Electrospray deposition KW - Nanoparticles KW - Electron microscopy KW - Sample preparation KW - TEM KW - SEM PY - 2017 AN - OPUS4-41578 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kaiser, M. A1 - Würth, Christian A1 - Kraft, Marco A1 - Hyppänen, I. A1 - Soukka, T. A1 - Resch-Genger, Ute T1 - Power-dependent upconversion quantum yield of NaYF4:Yb3+,Er3+ nano- and micrometer-sized particles – measurements and simulations N2 - Photophysical studies of nonlinear lanthanide-doped photon upconverting nanoparticles (UCNPs) increasingly used in biophotonics and photovoltaics require absolute measurements of the excitation power density (P)-dependent upconversion luminescence (UCL) and luminescence quantum yields (ΦUC) for quantifying the material performance, UCL deactivation pathways, and possible enhancement factors. We present here the P-dependence of the UCL spectra, ΦUC, and slope factors of the different emission bands of representative 25 nm-sized oleate-capped β-NaYF4:17% Yb3+, 3% Er3+ UCNPs dispersed in toluene and as powder as well as ΦUC of 3 μm-sized upconversion particles (UCμP), all measured with a newly designed integrating sphere setup, enabling controlled variation of P over four orders of magnitude. This includes quantifying the influence of the beam shape on the measured ΦUC and comparison of experimental ΦUC with simulations utilizing the balancing power density model of the Andersson-Engels group and the simulated ΦUC of UCμP from the Berry group, underpinned by closely matching decay kinetics of our UC material. We obtained a maximum ΦUC of 10.5% for UCμP and a ΦUC of 0.6% and 2.1% for solid and dispersed UCNPs, respectively. Our results suggest an overestimation of the contribution of the purple and an underestimation of that of the red emission of β-NaYF4:Yb3+,Er3+: microparticles by the simulations of the Berry group. Moreover, our measurements can be used as a guideline to the absolute determination of UCL and ΦUC KW - Upconversion KW - Photophysics KW - Nanoparticles PY - 2017 DO - https://doi.org/10.1039/c7nr02449e VL - 9 IS - 28 SP - 10051 EP - 10058 PB - The Royal Society of Chemistry AN - OPUS4-41550 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tütken, T. A1 - Tatzel, Michael A1 - Vogl, Jochen A1 - Rosner, M. T1 - Assessing δ26Mg in bioapatite as proxy for faunivory N2 - Knowledge about feeding behavior is essential to determine trophic interactions and reconstruct predator-prey relationships in modern and past foodwebs. Traditionally, nitrogen isotopes (δ15N) of collagen are used to quantify the ingestion of animal protein, however collagen usually does not preserve over geological time scales. To infer the diet of extinct vertebrates from fossil material more resistant dietary proxies such as Ca and Mg isotopes are needed, which are major elements in the bioapatite of bones and teeth. Magnesium is a bio-essential element that replaces calcium in the bioapatite lattice and bone and enamel δ26Mg values of extant mammals increase systematically along the foodchain [1, 2]. The existing δ26Mg data, however, is scarce, in particular with respect to carnivores, thus still limiting the capability of this dietary proxy to reliably determine trophic differences between plant- and animal-feeders. To better constrain trophic-level effects recorded in Mg isotopes, we analyzed δ26Mg of bioapatite from modern mammals with a focus on faunivores, both carnivores and as yet unexplored insectivores. The trophic level effect of δ26Mg is influenced by the geological substrate which causes isotope variability in δ26Mg of faunal remains between different ecosystems [1, 2]. Therefore, as first-order proxy for sample provenance and to assess potential influences of the bedrock substrate of the animals´ habitats on δ26Mg of bones and teeth, we measured the 87Sr/86Sr on the same specimens. This information will enable us to refine trophic level effects and determine whether δ26Mg can be used to distinguish different faunivores isotopically. This will be of paramount importance for dietary reconstructions of trophic niches in fossil foodwebs. [1] Martin et al. (2014) Geochmica Cosmochimica Acta 130, 12-20. [2] Martin et al. (2015) Proceedings of the National Academy of Sciences 112, 430-435. T2 - Goldschmidt CY - Paris, France DA - 13.08.2017 KW - Magnesium stable isotopes KW - Isotope fractionation KW - Trophic level KW - 87Sr/86Sr KW - Provenance PY - 2017 AN - OPUS4-41535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Complementary methodical approach for the analysis of a perovskite solar cell layered system N2 - Loss in efficiency of perovskite solar cells may be caused by structural and/or chemical alterations of the complex layered system. As these changes might take place either in the bulk and/or on the surface of the stratified material, analytical tools addressing both key issues are selected and combined. SEM/EDX combined with XPS were chosen as appropriate methodical approach to characterise perovskite laboratory cells in depth and complementary on top, before and after light exposure. The layered perovskite system investigated here is based on glass covered with fluorine doped tin oxide (FTO), followed by three porous thin films of TiO2, ZrO2 and a thick monolithic carbon. The TiO2 film is subdivided into a dense layer covered by a porous one constituted of nanoparticles with a truncated bipyramidal shape. This layered system serves as the matrix for the perovskite. After infiltration of perovskite solution and annealing, EDX spectral maps on cross-sections of the specimen have been measured. The distribution of relevant elements – Si, Sn, Ti, Zr and C – correlates conclusively with layers visible in the acquired SEM images. Lead and iodine are distributed throughout the porous layers C, ZrO2 and TiO2. In a SEM micrograph taken of the cross-section of a sample after illumination, the glass substrate and all layers FTO, TiO2, ZrO2 as well as C are clearly identified. By EDX it was found that several weeks of ambient daylight did not change significantly the qualitative elemental composition of lead and iodine throughout the solar cell system. It was confirmed with EDX that nanoparticles identified in high-resolution SEM micrographs contain mainly Pb and I, indicating these to be the perovskite crystals. However, a time-dependent compositional and chemical altering was observed with XPS for the near-surface region of the outermost ~10 nm after two months of illumination. T2 - Microscopy & Microanalysis 2017 Meeting CY - St. Louis, MO, USA DA - 06.08.2017 KW - Thin films KW - EDX KW - XPS KW - SEM KW - Nanoparticles KW - Perovskite KW - TiO2 PY - 2017 AN - OPUS4-41664 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Analysis of the operation of accreditation bodies N2 - Project objective: The aim of this project is to develop a tool based on objective criteria and indicators which can be used to analyze the operations of accreditation bodies. The tool will be used to systematically assess several European accreditation bodies, enabling a comparative analysis to be made. By investigating current practices, the analysis will generate discussion amongst accreditation bodies on how to improve the efficiency and effectiveness of operations. Methodology: The tool is based on parameters that enable comparison of various accreditation bodies, despite different operational processes and organizational forms. These parameters will be derived from operational processes with high relevance for accreditation bodies, and mapped to a universal process map which enables comparison between institutions. The processes will be characterized using data from internal databases, reports, financial audits etc., and will be supported by feedback from a qualitative self-evaluation of process maturity, carried out by the accreditation bodies themselves. The criteria for evaluating process maturity are based on those used in the excellence model of the European Foundation for Quality Management (EFQM), and are applied to the processes identified in the process map. The tool will be validated through application to various accreditation bodies in Europe. Project outline: The pilot phase of project comprises three stages. In the first stage the processes of accreditation bodies were systematically analyzed through the development of the process map. Nine processes of special relevance are identified and underpinned by indicators as described above. In the second step the tool was applied to the German accreditation body, DAkkS, in order to check and modify the indicators. The third stage will verify the transferability of the model by extending analysis to selected European accreditation bodies, again refining and optimizing the tool based on this analysis. Finally, after successful conduction of the pilot phase it is planned to extend the analysis to other European accreditation bodies interested in participation in 2018. T2 - Kick-Off Meeting at SWEDAC CY - Boras, Sweden DA - 24.01.17 KW - Accreditation KW - EFQM-excellence-model PY - 2017 AN - OPUS4-41672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfram T1 - Mathematical and statistical tools for online NMR spectroscopy in chemical processes N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied, which are calibration intensive. NMR spectroscopy has a high potential for direct loop process control while exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environments for advanced process monitoring and control. Within the European Union’s Research Project CONSENS (Integrated CONtrol and SENsing by development and integration of a smart NMR module for process monitoring was designed and delivers online spectra of various reactions. The presented NMR module is provided in an explosion proof housing of 57 x 57 x 85 cm module size and involves a compact spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction), and evaluation. For reaction monitoring and process control using NMR instruments after acquisition of the FID the data needs to be corrected in real-time for common effects using fast interfaces and automated methods. When it comes to NMR data evaluation under industrial process conditions, the shape of signals can change drastically due to nonlinear effects. Additionally, the multiplet structure becomes more dominant because of the comparably low-field strengths which results in overlapping of multiple signals. However, the structural and quantitative information is still present but needs to be extracted by applying predictive models. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). By using the benefits of traditional qNMR experiments data analysis models can meet the demands of the PAT community (Process Analytical Technology) regarding low calibration effort/calibration free methods, fast adaptions for new reactants, or derivatives and robust automation schemes. T2 - Advanced Mathematical and Computational Tools in Metrology and Testing XI (AMCTM) CY - Glasgow, UK DA - 29.08.2017 KW - Process Monitoring KW - CONSENS KW - Online NMR Spectroscopy KW - Indirect Hard Modeling KW - Data Analysis PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-416560 AN - OPUS4-41656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Characterization of Porous, TiO2 Nanoparticle Films Using On-Axis TKD in SEM – a New Nano-Analysis Tool for a Large-Scale Application N2 - A combined methodical approach is tested with respect to the characterization of the inner structure of porous TiO2 layers as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area of the pore network. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles on FTO/glass substrates. The analytical methods exploited in our study are Focused Ion Beam (FIB) slicing followed by 3D reconstruction as well as the new approach transmission Kikuchi diffraction (TKD) technology in the scanning electron microscope (SEM). Size and shape distribution of the TiO2 NPs within the layer can be extracted. SEM in transmission mode and atomic force microscopy (AFM) have been used to verify the dimensional data obtained by the new combined methodical approach. Its analytical benefits but also the challenges and limitations are highlighted. T2 - Microscopy & Microanalysis 2017 Meeting CY - St. Louis, MO, USA DA - 06.08.2017 KW - Porous layers KW - TiO2 KW - Nanoparticles KW - Size and shape distribution KW - TKD KW - SEM PY - 2017 AN - OPUS4-41660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Organic surface modification and analysis of TiO2 nanoparticles for self-assembly in multiple layers N2 - Parameters of TiO2 coatings can greatly influence their final performance in largescale applications such as photocatalytic measurements, orthopedic and/or dental prostheses, cell cultures, and dye-sensitized solar cells. From different film deposition procedures, self-assembly of TiO2 NPs in multiple layers was selected for systematic characterization. EDX, AES and ToF-SIMS analysis have been carried out in order to evaluate the functionalization of several types of TiO2 NPs differing in size, shape and surface area. T2 - Microscopy & Microanalysis 2017 Meeting CY - St. Louis, MO, USA DA - 06.08.2017 KW - TiO2 KW - Nanoparticles KW - EDX KW - ToF-SIMS KW - XPS KW - Auger electron spectroscopy KW - Functionalization PY - 2017 AN - OPUS4-41662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Analysis of the operation of accreditation bodies N2 - Project objective: The aim of this project is to develop a tool based on objective criteria and indicators which can be used to analyze the operations of accreditation bodies. The tool will be used to systematically assess several European accreditation bodies, enabling a comparative analysis to be made. By investigating current practices, the analysis will generate discussion amongst accreditation bodies on how to improve the efficiency and effectiveness of operations. Methodology: The tool is based on parameters that enable comparison of various accreditation bodies, despite different operational processes and organizational forms. These parameters will be derived from operational processes with high relevance for accreditation bodies, and mapped to a universal process map which enables comparison between institutions. The processes will be characterized using data from internal databases, reports, financial audits etc., and will be supported by feedback from a qualitative self-evaluation of process maturity, carried out by the accreditation bodies themselves. The criteria for evaluating process maturity are based on those used in the excellence model of the European Foundation for Quality Management (EFQM), and are applied to the processes identified in the process map. The tool will be validated through application to various accreditation bodies in Europe. Project outline: The pilot phase of project comprises three stages. In the first stage the processes of accreditation bodies were systematically analyzed through the development of the process map. Nine processes of special relevance are identified and underpinned by indicators as described above. In the second step the tool was applied to the German accreditation body, DAkkS, in order to check and modify the indicators. The third stage will verify the transferability of the model by extending analysis to selected European accreditation bodies, again refining and optimizing the tool based on this analysis. Finally, after successful conduction of the pilot phase it is planned to extend the analysis to other European accreditation bodies interested in participation in 2018. T2 - Kick-Off Meeting at RvA (Raad voor Accreditatie) CY - Utrecht, The Netherlands DA - 24.04.2017 KW - Accreditation KW - EFQM-excellence-model PY - 2017 AN - OPUS4-41686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Analysis of the operation of accreditation bodies N2 - Project objective: The aim of this project is to develop a tool based on objective criteria and indicators which can be used to analyze the operations of accreditation bodies. The tool will be used to systematically assess several European accreditation bodies, enabling a comparative analysis to be made. By investigating current practices, the analysis will generate discussion amongst accreditation bodies on how to improve the efficiency and effectiveness of operations. Methodology: The tool is based on parameters that enable comparison of various accreditation bodies, despite different operational processes and organizational forms. These parameters will be derived from operational processes with high relevance for accreditation bodies, and mapped to a universal process map which enables comparison between institutions. The processes will be characterized using data from internal databases, reports, financial audits etc., and will be supported by feedback from a qualitative self-evaluation of process maturity, carried out by the accreditation bodies themselves. The criteria for evaluating process maturity are based on those used in the excellence model of the European Foundation for Quality Management (EFQM), and are applied to the processes identified in the process map. The tool will be validated through application to various accreditation bodies in Europe. Project outline: The pilot phase of project comprises three stages. In the first stage the processes of accreditation bodies were systematically analyzed through the development of the process map. Nine processes of special relevance are identified and underpinned by indicators as described above. In the second step the tool was applied to the German accreditation body, DAkkS, in order to check and modify the indicators. The third stage will verify the transferability of the model by extending analysis to selected European accreditation bodies, again refining and optimizing the tool based on this analysis. Finally, after successful conduction of the pilot phase it is planned to extend the analysis to other European accreditation bodies interested in participation in 2018. T2 - Kick-Off Meeting at ENAC (Entidad Nacional de Acreditación) CY - Madrid, Spain DA - 17.01.2017 KW - Accreditation KW - EFQM-excellence-model PY - 2017 AN - OPUS4-41692 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Bundesanstalt für Materialforschung und -prüfung - Welcome N2 - Vorstellung der BAM sowie der Abteilung S und eines TZ-Projekts mit Bezug zu Qualitätsinfrastruktur im Rahmen eines Gastvortrags im Rahmen der Veranstaltungsreihe Quality Infrastructure Management an der TU Berlin N2 - Presentation of the BAM as well as the Department S and a technical cooperation project related to quality infrastructure within the framework of a guest lecture within the the Quality Infrastructure Management lecture series at the TU Berlin. T2 - Guest lecture at Quality Infrastructure Management (6 ECTS) - WS 2016/2017 at TU Berlin, Fachgebiet Innovationsökonomie CY - TU Berlin, Berlin, Germany DA - 03.11.2016 KW - Quality infrastructure PY - 2016 AN - OPUS4-41693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Vergleich der Arbeitsweise von Akkreditierungsstellen in Europa N2 - Project objective: The aim of this project is to develop a tool based on objective criteria and indicators which can be used to analyze the operations of accreditation bodies. The tool will be used to systematically assess several European accreditation bodies, enabling a comparative analysis to be made. By investigating current practices, the analysis will generate discussion amongst accreditation bodies on how to improve the efficiency and effectiveness of operations. Methodology: The tool is based on parameters that enable comparison of various accreditation bodies, despite different operational processes and organizational forms. These parameters will be derived from operational processes with high relevance for accreditation bodies, and mapped to a universal process map which enables comparison between institutions. The processes will be characterized using data from internal databases, reports, financial audits etc., and will be supported by feedback from a qualitative self-evaluation of process maturity, carried out by the accreditation bodies themselves. The criteria for evaluating process maturity are based on those used in the excellence model of the European Foundation for Quality Management (EFQM), and are applied to the processes identified in the process map. The tool will be validated through application to various accreditation bodies in Europe. Project outline: The pilot phase of project comprises three stages. In the first stage the processes of accreditation bodies were systematically analyzed through the development of the process map. Nine processes of special relevance are identified and underpinned by indicators as described above. In the second step the tool was applied to the German accreditation body, DAkkS, in order to check and modify the indicators. The third stage will verify the transferability of the model by extending analysis to selected European accreditation bodies, again refining and optimizing the tool based on this analysis. Finally, after successful conduction of the pilot phase it is planned to extend the analysis to other European accreditation bodies interested in participation in 2018. N2 - Projektbeschreibung: Das übergeordnete Ziel des Projekts ist es, ein Werkzeug bereitzustellen, mit dem die Arbeitsweise von Akkreditierungsstellen auf objektiver Grundlage und kennzahlenbasiert analysiert werden kann. Durch Anwendung auf mehrere Akkreditierungsstellen soll zudem eine vergleichende Analyse verschiedener Akkreditierungsstellen ermöglicht werden, die zur Harmonisierung der Arbeitsweise der Akkreditierungsstellen in Europa beiträgt. Mit zunehmender Harmonisierung entsteht zusätzliches Vertrauen in das europäische Konformitätsbewertungssystem. Das Projekt umfasst vier Phasen. In der ersten Phase des Projekts werden die Tätigkeiten von Akkreditierungsstellen und ihre auf gesetzlichen und normativen Anforderungen beruhenden Verpflichtungen systematisch analysiert. Es wird eine mit Kennzahlen unterlegte Prozesslandschaft entwickelt, die ein Modell bildet, dem die implementierten Abläufe und eingesetzten Ressourcen der Akkreditierungsstelle zugeordnet werden können. In der zweiten Phase werden die Prozesse der Deutschen Akkreditierungsstelle DAkkS dem Modell zugeordnet. Dabei werden mit Hilfe der DAkkS internen Datenbank Kennzahlen und Indikatoren erhoben. Die Übertragbarkeit des so erstandenen Modells wird in einem dritten Schritt durch die Erweiterung auf weitere Akkreditierungsstellen im europäischen Raum untersucht. In der vierten Phase wird die Analyse auf weitere europäische Akkreditierungsstellen ausgeweitet. T2 - Kick-Off Veranstaltung bei der DAkkS (Deutsche Akkreditierungsstelle) CY - Berlin, Germany DA - 12.09.2016 KW - Accreditation KW - EFQM-excellence-model PY - 2016 AN - OPUS4-41695 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Vergleich der Arbeitsweise von Akkreditierungsstellen in Europa - Datenerhebung N2 - Project objective: The aim of this project is to develop a tool based on objective criteria and indicators which can be used to analyze the operations of accreditation bodies. The tool will be used to systematically assess several European accreditation bodies, enabling a comparative analysis to be made. By investigating current practices, the analysis will generate discussion amongst accreditation bodies on how to improve the efficiency and effectiveness of operations. Methodology: The tool is based on parameters that enable comparison of various accreditation bodies, despite different operational processes and organizational forms. These parameters will be derived from operational processes with high relevance for accreditation bodies, and mapped to a universal process map which enables comparison between institutions. The processes will be characterized using data from internal databases, reports, financial audits etc., and will be supported by feedback from a qualitative self-evaluation of process maturity, carried out by the accreditation bodies themselves. The criteria for evaluating process maturity are based on those used in the excellence model of the European Foundation for Quality Management (EFQM), and are applied to the processes identified in the process map. The tool will be validated through application to various accreditation bodies in Europe. Project outline: The pilot phase of project comprises three stages. In the first stage the processes of accreditation bodies were systematically analyzed through the development of the process map. Nine processes of special relevance are identified and underpinned by indicators as described above. In the second step the tool was applied to the German accreditation body, DAkkS, in order to check and modify the indicators. The third stage will verify the transferability of the model by extending analysis to selected European accreditation bodies, again refining and optimizing the tool based on this analysis. Finally, after successful conduction of the pilot phase it is planned to extend the analysis to other European accreditation bodies interested in participation in 2018. N2 - Projektbeschreibung: Das übergeordnete Ziel des Projekts ist es, ein Werkzeug bereitzustellen, mit dem die Arbeitsweise von Akkreditierungsstellen auf objektiver Grundlage und kennzahlenbasiert analysiert werden kann. Durch Anwendung auf mehrere Akkreditierungsstellen soll zudem eine vergleichende Analyse verschiedener Akkreditierungsstellen ermöglicht werden, die zur Harmonisierung der Arbeitsweise der Akkreditierungsstellen in Europa beiträgt. Mit zunehmender Harmonisierung entsteht zusätzliches Vertrauen in das europäische Konformitätsbewertungssystem. Das Projekt umfasst vier Phasen. In der ersten Phase des Projekts werden die Tätigkeiten von Akkreditierungsstellen und ihre auf gesetzlichen und normativen Anforderungen beruhenden Verpflichtungen systematisch analysiert. Es wird eine mit Kennzahlen unterlegte Prozesslandschaft entwickelt, die ein Modell bildet, dem die implementierten Abläufe und eingesetzten Ressourcen der Akkreditierungsstelle zugeordnet werden können. In der zweiten Phase werden die Prozesse der Deutschen Akkreditierungsstelle DAkkS dem Modell zugeordnet. Dabei werden mit Hilfe der DAkkS internen Datenbank Kennzahlen und Indikatoren erhoben. Die Übertragbarkeit des so erstandenen Modells wird in einem dritten Schritt durch die Erweiterung auf weitere Akkreditierungsstellen im europäischen Raum untersucht. In der vierten Phase wird die Analyse auf weitere europäische Akkreditierungsstellen ausgeweitet. T2 - Vorstellung des Interviewleitfadens bei der DAkkS CY - Berlin, Germany DA - 14.06.2016 KW - Accreditation KW - EFQM-excellence-model PY - 2016 AN - OPUS4-41696 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Bundesanstalt für Materialforschung und -prüfung - Welcome N2 - Vorstellung der BAM, der Abteilung S und speziell der BAM-Zertifizierungsstelle im Rahmen eines Gastvortrags im Rahmen der Veranstaltungsreihe Strategic Standardisation an der TU Berlin, Fachgebiet Innovationsökonomie N2 - Presentation of the BAM as well as the Department S and a technical cooperation project related to quality infrastructure within the framework of a guest lecture within the the Quality Infrastructure Management lecture series at the TU Berlin. T2 - Guest lecture at Strategic Standardization - SoSe 2016 CY - TU Berlin, Berlin, Germany DA - 17.05.2016 KW - Product certification KW - BAM certification body PY - 2016 AN - OPUS4-41697 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Analysis of the operation of accreditation bodies N2 - Project objective: The aim of this project is to develop a tool based on objective criteria and indicators which can be used to analyze the operations of accreditation bodies. The tool will be used to systematically assess several European accreditation bodies, enabling a comparative analysis to be made. By investigating current practices, the analysis will generate discussion amongst accreditation bodies on how to improve the efficiency and effectiveness of operations. Methodology: The tool is based on parameters that enable comparison of various accreditation bodies, despite different operational processes and organizational forms. These parameters will be derived from operational processes with high relevance for accreditation bodies, and mapped to a universal process map which enables comparison between institutions. The processes will be characterized using data from internal databases, reports, financial audits etc., and will be supported by feedback from a qualitative self-evaluation of process maturity, carried out by the accreditation bodies themselves. The criteria for evaluating process maturity are based on those used in the excellence model of the European Foundation for Quality Management (EFQM), and are applied to the processes identified in the process map. The tool will be validated through application to various accreditation bodies in Europe. Project outline: The pilot phase of project comprises three stages. In the first stage the processes of accreditation bodies were systematically analyzed through the development of the process map. Nine processes of special relevance are identified and underpinned by indicators as described above. In the second step the tool was applied to the German accreditation body, DAkkS, in order to check and modify the indicators. The third stage will verify the transferability of the model by extending analysis to selected European accreditation bodies, again refining and optimizing the tool based on this analysis. Finally, after successful conduction of the pilot phase it is planned to extend the analysis to other European accreditation bodies interested in participation in 2018. T2 - Kick-Off Meeting at Norwegian Accreditation CY - Lillestrom, Norway DA - 07.02.2017 KW - EFQM-Excellence-Model KW - Accreditation PY - 2017 AN - OPUS4-41675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Analysis of the operation of accreditation bodies N2 - Project objective: The aim of this project is to develop a tool based on objective criteria and indicators which can be used to analyze the operations of accreditation bodies. The tool will be used to systematically assess several European accreditation bodies, enabling a comparative analysis to be made. By investigating current practices, the analysis will generate discussion amongst accreditation bodies on how to improve the efficiency and effectiveness of operations. Methodology: The tool is based on parameters that enable comparison of various accreditation bodies, despite different operational processes and organizational forms. These parameters will be derived from operational processes with high relevance for accreditation bodies, and mapped to a universal process map which enables comparison between institutions. The processes will be characterized using data from internal databases, reports, financial audits etc., and will be supported by feedback from a qualitative self-evaluation of process maturity, carried out by the accreditation bodies themselves. The criteria for evaluating process maturity are based on those used in the excellence model of the European Foundation for Quality Management (EFQM), and are applied to the processes identified in the process map. The tool will be validated through application to various accreditation bodies in Europe. Project outline: The pilot phase of project comprises three stages. In the first stage the processes of accreditation bodies were systematically analyzed through the development of the process map. Nine processes of special relevance are identified and underpinned by indicators as described above. In the second step the tool was applied to the German accreditation body, DAkkS, in order to check and modify the indicators. The third stage will verify the transferability of the model by extending analysis to selected European accreditation bodies, again refining and optimizing the tool based on this analysis. Finally, after successful conduction of the pilot phase it is planned to extend the analysis to other European accreditation bodies interested in participation in 2018. T2 - Kick-Off-Meeting bei UKAS (United Kingdom Accreditation Service) CY - Staines-opon-Thames, UK DA - 20.02.2017 KW - EFQM-Excellence-Model KW - Accreditation PY - 2017 AN - OPUS4-41676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Analysis of the operation of accreditation bodies N2 - Project objective: The aim of this project is to develop a tool based on objective criteria and indicators which can be used to analyze the operations of accreditation bodies. The tool will be used to systematically assess several European accreditation bodies, enabling a comparative analysis to be made. By investigating current practices, the analysis will generate discussion amongst accreditation bodies on how to improve the efficiency and effectiveness of operations. Methodology: The tool is based on parameters that enable comparison of various accreditation bodies, despite different operational processes and organizational forms. These parameters will be derived from operational processes with high relevance for accreditation bodies, and mapped to a universal process map which enables comparison between institutions. The processes will be characterized using data from internal databases, reports, financial audits etc., and will be supported by feedback from a qualitative self-evaluation of process maturity, carried out by the accreditation bodies themselves. The criteria for evaluating process maturity are based on those used in the excellence model of the European Foundation for Quality Management (EFQM), and are applied to the processes identified in the process map. The tool will be validated through application to various accreditation bodies in Europe. Project outline: The pilot phase of project comprises three stages. In the first stage the processes of accreditation bodies were systematically analyzed through the development of the process map. Nine processes of special relevance are identified and underpinned by indicators as described above. In the second step the tool was applied to the German accreditation body, DAkkS, in order to check and modify the indicators. The third stage will verify the transferability of the model by extending analysis to selected European accreditation bodies, again refining and optimizing the tool based on this analysis. Finally, after successful conduction of the pilot phase it is planned to extend the analysis to other European accreditation bodies interested in participation in 2018. T2 - Kick-Off Meeting at Akkredittierung Austria CY - Wien, Austria DA - 01.03.2017 KW - EFQM-Excellence-Model KW - Accreditation PY - 2017 AN - OPUS4-41679 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Analysis of the operation of accreditation bodies N2 - Project objective: The aim of this project is to develop a tool based on objective criteria and indicators which can be used to analyze the operations of accreditation bodies. The tool will be used to systematically assess several European accreditation bodies, enabling a comparative analysis to be made. By investigating current practices, the analysis will generate discussion amongst accreditation bodies on how to improve the efficiency and effectiveness of operations. Methodology: The tool is based on parameters that enable comparison of various accreditation bodies, despite different operational processes and organizational forms. These parameters will be derived from operational processes with high relevance for accreditation bodies, and mapped to a universal process map which enables comparison between institutions. The processes will be characterized using data from internal databases, reports, financial audits etc., and will be supported by feedback from a qualitative self-evaluation of process maturity, carried out by the accreditation bodies themselves. The criteria for evaluating process maturity are based on those used in the excellence model of the European Foundation for Quality Management (EFQM), and are applied to the processes identified in the process map. The tool will be validated through application to various accreditation bodies in Europe. Project outline: The pilot phase of project comprises three stages. In the first stage the processes of accreditation bodies were systematically analyzed through the development of the process map. Nine processes of special relevance are identified and underpinned by indicators as described above. In the second step the tool was applied to the German accreditation body, DAkkS, in order to check and modify the indicators. The third stage will verify the transferability of the model by extending analysis to selected European accreditation bodies, again refining and optimizing the tool based on this analysis. Finally, after successful conduction of the pilot phase it is planned to extend the analysis to other European accreditation bodies interested in participation in 2018. T2 - Kick-Off Meeting at LATAK (Latvian National Accreditation Bureau) CY - Riga, Latvia DA - 04.04.2017 KW - Accreditation KW - EFQM-Excellence-Model PY - 2017 AN - OPUS4-41680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Hesse, Almut T1 - Entwicklung immunchemischer Methoden zur Spurenanalytik der Sprengstoffe Nitropenta und Trinitrotoluol N2 - Pentaerythrityltetranitrat (PETN), ein in jüngster Vergangenheit häufig von Terroristen verwendeter Sprengstoff, ist äußerst schwer zu detektieren. Ein verbesserter Antikörper gegen PETN wurde durch Anwendung des Konzepts des bioisosteren Ersatzes entwickelt,indem ein Nitroester durch einen Carbonsäurediester ersetzt wurde. Biostere Moleküle haben eine ähnliche Struktur wie die Referenzsubstanz und zeigen eine vergleichbare biologische Wirkung. Dieser Ansatz führte zu polyklonalen Antikörpern mit extrem guter Selektivität und Sensitivität. Die Nachweisgrenze des Enzyme-Linked Immunosorbent Assays (ELISAs) beträgt 0,15 μg/L. Der Messbereich des Immunassays liegt zwischen 1 und 1000 μg/L. Die Antikörper sind sowohl hinreichend pH-stabil als auch robust gegen Lösungsmittelzusätze. Das Antiserum könnte auch für Schnelltests, Biosensoren, Mikro-Arrays und andere analytische Methoden verwendet werden. Für die Umweltanalytik von Trinitrotoluol (TNT) wurde eine Hochdruckflüssigkeitschromatographie (HPLC)-kompatible Affinitätssäule hergestellt. Druckbeständiges, poröses Glas hat sich als ein hervorragendes Trägermaterial herauskristallisiert. Um selektive anti-TNT-Antikörper für die Herstellung der Affinitätssäule aus den beiden verwendeten TNT-Seren zu isolieren, wurde eine Trennung an einer Dinitrophenyl-Affinitätssäule durchgeführt. Zur Optimierung der Immobilisierungsmethode wurden orangefarbene Dabsyl -Proteine synthetisiert und auf der Oberfläche gebunden. Die Färbung wurde als Indikator für die Immobilisierungsdichte verwendet. Wegen der hohen Affinitätskonstanten der polyklonalen anti-TNT-Antikörper der beiden Seren (5,1 bzw. 2,3∙109 L/mol) lässt sich TNT durch eine typische saure Elution der TNT-Affinitätssäule nur schwer eluieren. Aus diesem Grund wurde eine neuartige Elutionsmethode entwickelt, die irreversible, denaturierende, thermische Online -Elution. Diese eröffnet ein weites Anwendungsfeld, da so Affinitäten, die klass ischerweise aufgrund zu hoher Bindungskonstanten zwischen Ligand und Rezeptor nicht für die Affinitätschromatographie genutzt werden können, für die Analytik besser handhabbar werden. Die maximale Kapazität einer im Rahmen dieser Arbeit hergestellten Affinitätssäule (64,8 μL) betrug 650 ng TNT bzw. 10 μg/mL Säulenvolumen. Um die Immobilisierungsdichte der produzierten Affinitätssäulen zu bestimmen, wurde ein neues Verfahren entwickelt, da die üblichen spektroskopischen Proteinbestimmungsmethoden aufgrund der hohen unspezifischen Wechselwirkung mit dem Trägermaterial zur Proteinbestimmung nicht geeignet waren. Zur Quantifizierung von Proteinen oder Peptiden,die auf festen Trägern immobilisiert sind, wurde auf Grundlage einer HPLC-Trennung der aromatischen Aminosäuren Tyrosin (Tyr) und Phenylalanin (Phe) ohne vorherige Derivatisierung eine gegenüber der klassischen Aminosäureanalytik vereinfachte HPLC/UV-Methode entwickelt. Die Hydrolyse der Proteine und Peptide wurde durch Einsatz von Mikrowellentechnik beschleunigt, sodass nur 30 Minuten statt ca. 22 Stunden für das Standardprotokoll benötigt wurden, bei dem ein Hydrolyseröhrchen verwendet wird. Zur internen Kalibrierung wurden zwei Standardverbindungen, Homotyrosin (HTyr) und 4-Fluorphenylalanin (FPhe) verwendet. Die Nachweisgrenze (limit of detection, LOD) bei 215 nm ist sowohl für Tyr als auch für Phe 0,05 μM (~ 10 μg/L). Dieses neue Verfahren, das als Aromatische Aminosäureanalyse (Aromatic Amino Acid Analysis, AAAA) bezeichnet werden kann, wurde zur Proteinbestimmung von homogenen Proben mit Rinderserumalbumin (BSA) des Nationalen Instituts für Standards und Technologie der USA (NIST) validiert, wobei die Nachweisgrenze für Proteine mit 16 mg/L (~ 300 ng BSA) mit gängigen spektroskopischen Verfahren vergleichbar ist. Es liefert incl. der Hydrolysestufe eine verbesserte Genauigkeit mit einer relativen Standardabweichung von ca. 5%. T3 - BAM Dissertationsreihe - 158 KW - Affinitätschromatographie KW - Affinity chromatography KW - Polyklonale TNT-Antikörper KW - Immunassay KW - Aromatische Aminosäureanalyse KW - Polyclonal TNT-antibodies KW - Polyclonal PETN-antibodies KW - Immunoassay KW - Aromatic amino acid analysis KW - Polyklonale PETN-Antikörper PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-417566 SN - 1613-4249 VL - 158 SP - I EP - 234 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-41756 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Denkler, Tilman T1 - Guest lecture: Quality infrastructure & sustainability N2 - Gastvortrag an der TU Berlin zu Qualitätsinfrastruktur und Nachhaltigkeit, gehalten im Rahmen der Veranstaltungsreihe Sustainable Innovation N2 - Guest lecture at the TU Berlin on quality infrastructure and sustainability, held as part of the Sustainable Innovation lecture series. T2 - Guest lecture at Sustainable Innovation - WS 2015/2016 CY - TU Berlin, Berlin, Germany DA - 01.12.2015 KW - Quality infrastructure KW - Sustainability PY - 2015 AN - OPUS4-41699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gorris, H.H. A1 - Resch-Genger, Ute T1 - Perspectives and challenges of photon-upconversion nanoparticles - Part II: Bioanalytical applications N2 - In Part II of this Review series on lanthanide-doped photon-upconversion nanoparticles (UCNPs), we present and critically discuss the Performance and suitability of UCNPs as background-free luminescent Reporters in bioimaging and bioanalytical applications. The preparation of a biocompatible nanoparticle surface is an integral step for all life - science-related applications. UCNPs have found their way into a large number of diagnostic platforms, homogeneous and heterogeneous assay formats, and sensor applications. Many bioanalytical detection schemes involve Förster resonance energy transfert (FRET), which is still debated for UCNPs and Needs to be much improved. The Need for dedicated and standardized instruments as well as recent studies on the Dissolution and potential toxicity of UCNPs are addressed. Finally we outline future Trends and challenges in the field of upconversion. KW - Fluorescence KW - Lanthanide KW - Upconversion KW - Brightness KW - Quantification KW - Nanoparticle KW - Absolute fluorometry KW - NIR KW - IR KW - Quantum yield KW - Assay KW - Bioconjugation KW - Imaging KW - FRET KW - Sensor PY - 2017 DO - https://doi.org/10.1007/s00216-017-0482-8 SN - 1618-2650 SN - 1618-2642 VL - 409 IS - 25 SP - 5875 EP - 5890 PB - Springer AN - OPUS4-41706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dörfel, Ilona T1 - Microstructure of alumina coating on steel P92 after thermal cycling N2 - 1. Introduction Alumina coatings are one possibility to increase the corrosion resistance, lifetime and application range of thermally loaded steel components, e.g. in modern power plants where the use of the Oxy-fuel technology corrosive fuel gas (H2O-CO2-O2-SO2 at 650 °C) affects the steel parts. In previous investigations the efficacy of protective alumina coatings on steel P 92 under those conditions was demonstrated. A shutdown and re-start of power plants or parts of them causes thermal stresses of the components which can cause detrimental effects like microstructural changes in the steel itself, changes in its oxidation behavior, delamination or microstructural changes in the coating. All those effects can lead to failure of the components, resulting in lifetime reduction. 2. Objectives As a first step, we concentrate on the influence of thermal cycling tests and observe the impact on the microstructure of the coating and the interface in laboratory air. These investigations will help understanding the processes which occur, show directions of potentially necessary changes of the coating due to improved thermal stress behaviour. 3. Materials & methods P 92 is a ferritic-martensitic steel, containing 9% Cr which forms protective Cr-oxide-rich scales in dry environments and non-protective ones in water-containing environments. Coupons of P 92, having ground surfaces, were dip-coated via a sol-gel process and subjected to thermal cycling for 500 h (1000 cycles) in laboratory air in a temperature range between room temperature and 660° C. The resulting mass loss was determined by weighing. Samples for TEM investigations were produced as cross sections normal to the sample surface by FIB preparation (Quanta 3D, (FEI)). The TEM/STEM investigations were performed using a JEM2200FS (JEOL) operated at 200 kV. The microstructure of the coating and the interface after cycling tests was characterized via TEM, HREM, and STEM images, electron diffraction as well as EDX and EFTEM methods. 4. Results At steep edges in the surface profile the coating was imperfect and cracks have formed during the thermal cycling. Flat surface regions are well-covered. The whole interface region between the steel and the coating shows a dense Cr-oxide-rich zone, which can form protective regions in case of local failure. The Cr-oxide zone is followed by a region of mixed oxides, containing Cr, Mn, Fe, and Al in variable composition, to which a porous δ-Al2O3 zone is joined. 5. Conclusions • Alumina coatings promote the formation of dense, Cr-rich zones at the interface, which makes the system self-healing. • These zones are stable during thermal stresses, even in regions with cracked coatings. • They cause reduction of outward diffusion and mass loss during thermal cycling. T2 - MC2017 CY - Lausanne, Switzerland DA - 21.08.2017 KW - Coating KW - Thermal cycling KW - TEM PY - 2017 UR - https://www.mc2017.ch/general-information/downloads/ AN - OPUS4-41724 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lauer, Franziska A1 - Seifert, Stephan A1 - Kneipp, Janina A1 - Weidner, Steffen T1 - Simplifying the preparation of pollen grains for MALDI-TOF MS classification N2 - Matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) is a well-implemented analytical technique for the investigation of complex biological samples. In MS, the sample preparation strategy is decisive for the success of the measurements. Here, sample preparation processes and target materials for the investigation of different pollen grains are compared. A reduced and optimized sample preparation process prior to MALDI-TOF measurement is presented using conductive carbon tape as target. The application of conductive tape yields in enhanced absolute signal intensities and mass spectral pattern information, which leads to a clear separation in subsequent pattern analysis. The results will be used to improve the taxonomic differentiation and identification, and might be useful for the development of a simple routine method to identify pollen based on mass spectrometry. KW - MALDI KW - Conductive carbon tape KW - Pollen KW - Sample pretreatment KW - Principal component analysis PY - 2017 DO - https://doi.org/10.3390/ijms18030543 SN - 1422-0067 SN - 1661-6596 VL - 18 IS - 3 SP - 543-1 EP - 543-11 PB - MDPI AN - OPUS4-41733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jakubowski, Norbert T1 - Lecture 7: Speciation N2 - ICP-MS is a well-established analytical method which excels by high accuracy, high dynamic range and extremely low limits of detection for most metals. Furthermore ICP-MS offers a very high multi-element coverage so that many elements of the periodic table can be detected simultaneously. In this series of lectures, we want to focus on the historical developments, fundamentals, instrumentation and novel applications of ICP-MS in the life and material sciences. KW - Speciation KW - SDS-PAGE KW - GC-ICP-MS PY - 2017 SP - 1 EP - 74 CY - Berlin AN - OPUS4-41721 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Haferkamp, Sebastian T1 - In situ investigations of mechanochemical Knoevenagel condensations N2 - Mechanaochemistry is an effecthive method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions. T2 - INCOME2017 CY - Kosice, Slovakia DA - 03.09.2017 KW - C-C coupling KW - Mechanochemistry KW - Knoevenagel condensation KW - Synchrotron KW - In situ PY - 2017 AN - OPUS4-41845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, F. A1 - Lakey, P. S. J. A1 - Berkemeier, T. A1 - Tong, H. A1 - Kunert, A. T. A1 - Meusel, H. A1 - Cheng, Y. A1 - Su, H. A1 - Fröhlich-Nowoisky, J. A1 - Lai, S. A1 - Weller, Michael G. A1 - Shiraiwa, M. A1 - Pöschl, U. A1 - Kampf, C. J. T1 - Atmospheric protein chemistry influenced by anthropogenic air pollutants: nitration and oligomerization upon exposure to ozone and nitrogen dioxide N2 - The allergenic potential of airborne proteins may be enhanced via post-translational modification induced by air pollutants like ozone (O3) and nitrogen dioxide (NO2). The molecular mechanisms and kinetics of the chemical modifications that enhance the allergenicity of proteins, however, are still not fully understood. Here, protein tyrosine nitration and oligomerization upon simultaneous exposure of O3 and NO2 were studied in coated-wall flow-tube and bulk solution experiments under varying atmospherically relevant conditions (5–200 ppb O3, 5–200 ppb NO2, 45–96% RH), using bovine serum albumin as a model protein. Generally, more tyrosine residues were found to react via the nitration pathway than via the oligomerization pathway. Depending on reaction conditions, oligomer mass fractions and nitration degrees were in the ranges of 2.5–25% and 0.5–7%, respectively. The experimental results were well reproduced by the kinetic multilayer model of aerosol surface and bulk chemistry (KM-SUB). The extent of nitration and oligomerization strongly depends on relative humidity (RH) due to moisture-induced phase transition of proteins, highlighting the importance of cloud processing conditions for accelerated protein chemistry. Dimeric and nitrated species were major products in the liquid phase, while protein oligomerization was observed to a greater extent for the solid and semi-solid phase states of proteins. Our results show that the rate of both processes was sensitive towards ambient ozone concentration but rather insensitive towards different NO2 levels. An increase of tropospheric ozone concentrations in the Anthropocene may thus promote pro-allergic protein modifications and contribute to the observed increase of allergies over the past decades. KW - Oxidation KW - Nitration KW - Cross-linking KW - Ozone KW - Nitrogen dioxide KW - Dimer KW - Air pollution KW - Diesel KW - Aeroallergens KW - Pollen KW - Tyrosine KW - Nitrotyrosine KW - BSA KW - Albumin PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-418482 DO - https://doi.org/10.1039/c7fd00005g SN - 1359-6640 VL - 200 SP - 413 EP - 427 PB - Royal Society of Chemistry CY - London AN - OPUS4-41848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schürmann, Robin Mathis A1 - Tsering, Thupten A1 - Tanzer, Katrin A1 - Denifl, Stephan A1 - Kumar, S.V.K. A1 - Bald, Ilko T1 - Resonant Formation of Strand Breaks in Sensitized Oligonucleotides Induced by Low-Energy Electrons (0.5–9 eV) N2 - Halogenated nucleobases are used as radiosensitizers in cancer radiation therapy, enhancing the reactivity of DNA to secondary low-energy electrons (LEEs). LEEs induce DNA strand breaks at specific energies (resonances) by dissociative electron attachment (DEA). Although halogenated nucleobases show intense DEA resonances at various electron energies in the gas phase, it is inherently difficult to investigate the influence of halogenated nucleobases on the actual DNA strand breakage over the broad range of electron energies at which DEA can take place (<12 eV). By using DNA origami nanostructures, we determined the energy dependence of the strand break cross-section for oligonucleotides modified with 8-bromoadenine ((8Br)A). These results were evaluated against DEA measurements with isolated (8Br)A in the gas phase. Contrary to expectations, the major contribution to strand breaks is from resonances at around 7 eV while resonances at very low energy (<2 eV) have little influence on strand breaks. KW - Dissociative electron attachment KW - DNA damage KW - DNA nanotechnology KW - Low energy electrons PY - 2017 DO - https://doi.org/10.1002/anie.201705504 SN - 1433-7851 SN - 1521-3773 VL - 56 IS - 36 SP - 10952 EP - 10955 PB - Wiley AN - OPUS4-41850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schürmann, Robin A1 - Tsering, Thupten A1 - Tanzer, Katrin A1 - Denifl, Stephan A1 - Kumar, S.V.K. A1 - Bald, Ilko T1 - Resonante Bildung von Strangbrüchen in sensibilisierten Oligonukleotiden induziert durch niederenergetische Elektronen (0.5–9.0 eV) N2 - In der Krebs-Strahlentherapie werden halogenierte Nukleinbasen als Radiosensibilisatoren eingesetzt, um die Reaktivität der DNA gegenüber niederenergetischen Elektro- nen (NEEs) zu erhöhen. NEEs erzeugen DNA-Strangbrüche bei spezifischen Energien (Resonanzen) durch dissoziative Elektronenanlagerung (DEA). Obwohl halogenierte Nukle- inbasen intensive DEA-Resonanzen bei verschiedenen Elek-tronenenergien in der Gasphase aufweisen, kann der Einfluss der halogenierten Nukleinbasen auf tatsächliche DNA-Strangbrüche grundsätzlich nur schwer über den Energiebereich, in dem DEA stattfindet (< 12 eV), untersucht werden. Mithilfe von DNA-Origami-Nanostrukturen haben wir die Energieabhängigkeit der Wirkungsquerschnitte für DNA-Strangbrüche von Oligonukleotiden bestimmt, die mit 8- Bromadenin (8BrA) modifiziert wurden. Diese Ergebnisse wurden mit DEA-Messungen an isoliertem 8BrA in der Gas-phase verglichen. Entgegen der Erwartungen wird der Großteil der Strangbrüche durch Resonanzen um 7 eV hervorgerufen, wohingegen der Einfluss von Resonanzen bei sehr niedrigen Energien (< 2eV) auf die Strangbrüche gering ist. KW - DNA Schäden KW - Niederenergetische Elektronen KW - DNA Nanotechnologie KW - Dissoziative Elektronen Anlagerung PY - 2017 DO - https://doi.org/10.1002/ange.201705504 SN - 1521-3757 SN - 0044-8249 VL - 129 IS - 36 SP - 11094 EP - 11098 PB - Wiley AN - OPUS4-41851 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Strangers in the Night – Smart Process Sensors in Our Current Automation Landscape N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors will simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. This is particularly important for concepts like self-diagnostics, self-calibration and self-configuration/parameterization. Intelligent field devices as parts of digital field networks, Inter-net Protocol (IP)-based connectivity and web interfaces, as well as advanced data analysis soft-ware will provide the basis for future projects like Industrie 4.0, Factory of the Future, or Industrial Internet of Things (IIoT). The talk summarizes the currently discussed general requirements for process sensors 4.0 and introduces an online NMR sensor as example. This sensor was developed to provide integrated control and sensing for sustainable operation of flexible intensified processes (CONSENS) funded by the European Union’s Horizon 2020 research and innovation programme. T2 - Eurosensors 2017 Conference CY - Paris, France DA - 03.09.2017 KW - Process Monitoring KW - Smart Sensors KW - Online NMR Spectroscopy KW - Indirect Hard Modeling KW - Industrie 4.0 KW - Eurosensors PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-418271 UR - http://www.eurosensors2017.eu/ AN - OPUS4-41827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Locating subsurface defects with structured heating using high-power VCSEL-laser arrays N2 - Among the photothermal methods, full-field thermal imaging is used to characterize materials, to determine thicknesses of layers, or to find inhomogeneities such as voids or cracks. The use of classical light sources such as flash lamps (impulse heating) or halogen lamps (modulated heating) led to a variety of nondestructive testing methods, in particular lock-in and flash-thermography. In vertical cavity surface emitting lasers (VCSELs), laser light is emitted perpendicular to the surface with a symmetrical beam profile. Due to the vertical structure, they can be arranged in large arrays of many thousands of individual lasers, which allows power scaling into the kilowatt range. Recently, a high-power yet very compact version of such a VCSEL-array became available that offers both the fast timing behavior of a laser as well as the large illumination area of a lamp. Moreover, it allows a spatial and temporal control of the heating because individual parts of the array can be controlled arbitrarily in frequency, amplitude, and phase. In conjunction with a fast infrared camera, such structured heating opens up a field of novel thermal imaging and testing methods. As a first demonstration of this ansatz, we chose a testing problem very challenging to conventional thermal infrared testing: The detection of very thin subsurface defects perpendicularly oriented to the surface of metallic samples. First, we generate destructively interfering thermal wave fields which are then affected by the presence of defects within their reach. It turned out that this technique allows highly sensitive detection of subsurface defects down to depths in excess of the usual thermographic rule of thumb, with no need for a reference or surface preparation. T2 - 19th International Conference on Photoacoustic and Photothermal Phenomena CY - Bilbao, Spain DA - 16.07.2017 KW - Thermografie KW - Laser KW - Zerstörungsfreie Prüfung KW - Thermography KW - Non-destructive testing PY - 2017 AN - OPUS4-41829 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Das VCSEL-Laser Array – Durch strukturierte Erwärmung mit einer neuartigen Hochleistungslichtquelle verdeckte Defekte thermografisch detektieren N2 - Vertical Cavity Surface Emitting Lasers (VCSELs) sind Diodenlaser, welche Laserstrahlung mit gutem Strahlprofil senkrecht zur Chipoberfläche emittieren. Aufgrund dieser vertikalen Bauweise können sie in großen Arrays zu vielen tausenden einzelnen Lasern zusammengefasst werden. Solch ein VCSEL-Array vereint das schnelle zeitliche Verhalten eines Diodenlasers mit der hohen optischen Bestrahlungsstärke und dem großen Beleuchtungsbereich von Blitzlampen oder LEDs und kann damit potentiell alle herkömmlichen Lichtquellen der Thermografie ersetzen. Darüber hinaus kann der Prüfkörper mithilfe dieser Lichtquelle strukturiert erwärmt werden, da einzelne Bereiche des VCSEL-Arrays unabhängig voneinander angesteuert werden können. Dieser neue Freiheitsgrad ermöglicht die Entwicklung neuer thermografischer ZfP-Verfahren. Wir demonstrieren diesen Ansatz anhand eines für die konventionelle Thermografie nur sehr bedingt lösbaren Prüfproblems, der Detektion vertikal zur Oberfläche ausgerichteter, sehr dünner, verdeckter Defekte in metallischen Werkstoffen. Wir erzeugen hierzu destruktiv interferierende thermische Wellenfelder. Defekte im Einflußbereich dieser thermischen Wellenfelder stören die destruktive Interferenz und erlauben eine hochsensible Detektion bis in Tiefen jenseits der üblichen thermografischen Faustformel, ohne Referenz und ohne Oberflächenbehandlung. T2 - DGZfP-Jahrestagung 2017 CY - Koblenz, Germany DA - 22.05.2017 KW - Thermografie KW - Laser KW - Zerstörungsfreie Prüfung PY - 2017 AN - OPUS4-41834 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meißner, G. A1 - Dirican, D. A1 - Jäger, Christian A1 - Braun, T. A1 - Kemnitz, E. T1 - Et3GeH versus Et3SiH: controlling reaction pathways in catalytic C–F bond activations at a nanoscopic aluminum chlorofluoride† N2 - Catalytic C–F bond activation reactions of mono- and polyfluoroalkanes at Lewis acidic amorphous aluminum chlorofluoride (ACF) are presented. The hydrogen sources Et3GeH or Et3SiH control the selectivity of the conversions. The immobilization of Et3GeH at ACF resulted in catalytic dehydrohalogenation reactions to yield olefins under very mild conditions. In contrast, if Et3SiH is immobilized at ACF, C–C coupling occured and the formation of Friedel–Crafts products was observed. MAS NMR spectroscopic studies revealed information about the surface binding of the substrates. KW - Vapor-phase hydrofluorination KW - Carbon-fluorine bonds KW - Vinyl fluoride KW - Phosphine-ligands KW - Room-temperature KW - Building-blocks KW - Etal-complexes KW - Germylium ions KW - Lewis-acids KW - Hydrodefluorination PY - 2017 DO - https://doi.org/10.1039/c7cy00845g SN - 2044-4753 SN - 2044-4761 VL - 7 IS - 15 SP - 3348 EP - 3354 PB - The Royal Society of Chemistry AN - OPUS4-41836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bagcioglu, M. A1 - Kohler, A. A1 - Seifert, St. A1 - Kneipp, Janina A1 - Zimmermann, B. T1 - Monitoring of plant–environment interactions by high-throughput FTIR spectroscopy of pollen N2 - 1. Fourier transform infrared (FTIR) spectroscopy enables chemical analysis of pollen samples for plant phenotyping to study plant–environment interactions, such as influence of climate change or pathogens.However, current approach, such as microspectroscopy and attenuated total reflection spectroscopy, does not allow for highthroughput protocols. This study at hand suggests a new spectroscopic method for high-throughput characterization of pollen. 2. Samples were measured as thin films of pollen fragments using a Bruker FTIR spectrometer with a highthroughput eXTension (HTS-XT) unit employing 384-well plates. In total, 146 pollen samples, belonging to 31 different pollen species of Fagaceae and Betulaceae and collected during three consecutive years (2012–2014) at locations in Croatia, Germany and Norway, were analysed. Critical steps in the sample preparation and measurement, such as variabilities between technical replicates, between microplates and between spectrometers, were studied. 3. Measurement variations due to sample preparation, microplate holders and instrumentation were low, and thus allowed differentiation of samples with respect to phylogeny and biogeography. The spectral variability for a range of Fagales species (Fagus, Quercus, Betula, Corylus, Alnus and Ostrya) showed high-species-specific differences in pollen’s chemical composition due to either location or year. Statistically significant inter-annual and locational differences in the pollen spectra indicate that pollen chemical composition has high phenotypic plasticity and is influenced by local climate conditions. The variations in composition are connected to lipids, proteins, carbohydrates and sporopollenins that play crucial roles in cold and desiccation tolerance, protection against UVradiation and asmaterial and energy reserves. 4. The results of this study demonstrate the value of high-throughput FTIR approach for the systematic collection of data on ecosystems. The novel FTIR approach offers fast, reliable and economical screening of large number of samples by semi-automated methodology. The high-throughput approach could provide crucial understanding on plant–climate interactions with respect to biochemical variation within genera, species and populations. KW - Alnus KW - Betula KW - Betulaceae KW - Corylus KW - Ecology and environmental sciences KW - Fagaceae KW - Fagus KW - Infrared spectroscopy KW - Pollen KW - Quercus PY - 2017 DO - https://doi.org/10.1111/2041-210X.12697 VL - 2017 IS - 8 SP - 870 EP - 880 PB - British Ecological Society AN - OPUS4-41838 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis A1 - Prager, Jens A1 - Krome, Fabian T1 - Application of the scaled boundary finite element method (SBFEM) for a numerical simulation of ultrasonic guided waves N2 - This paper addresses the computation of dispersion curves, mode shapes and propagation of elastic guided waves. It summarizes the approaches based on the Scaled Boundary Finite Element Method. Descriptions for plates, rods, pipelines and waveguides with an arbitrary cross section are included. The important steps for the approximation of the displacement in bounded and unbounded domains are stated. The grid generation process is explained. It is highlighted that the Scaled Boundary Finite Element Method is very efficient, if large portions of the domain are either straight or with a constant curvature. The computation of dispersion curves for layered structures is presented. T2 - Sensor + Test CY - Nürnberg, Germany DA - 30.05.2017 KW - Ultrasonic guided waves KW - Non-destructive testing KW - Scaled boundary finite element method (SBFEM) PY - 2017 SN - 978-3-9816876-4-4 VL - 2017 SP - C5.4, 376 EP - 381 AN - OPUS4-41876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wanka, Antje Jutta T1 - Novel antibody tagging strategy using lanthanide loaded NHS-dota-ester for the application in highly selective LA-ICP-MS-based immunoassays N2 - Using metal tagged antibodies for multiplex immunoassays is an important aspect in the research field of bioanalytics. Various tagging strategies have been published, however the formed antibody conjugates were described only rudimentarily. We present an inexpensive, simple and fast DOTA-NHS-ester tagging strategy and the characterization of the conjugates. The monoclonal anti-beta-actin-antibody was used as model system and was modified with the bifunctional ligand DOTA-NHS-ester complexing monoisotopic lanthanide ions. In contrast to the antibody tagging with other tags based on maleimide chemistry the DOTA-NHS-ester reacts with unprotonated amino groups instead of free sulfhydryl groups. The great advantage of this is that a partially reduction of the antibody is not required and therefore the antibody remains intact. The characterization of the conjugates by different analytical techniques demonstrates that no antibody fragments are formed. A mean tagging degree of 8 tags/antibody was determined. The applicability of this tagging strategy is shown in first results of an Alzheimer’s disease study in a mouse model. We have chosen three different NHS-DOTA-ester tagged antibodies for multielement LA-ICP-MS based bioimaging of mice brain tissue. The artificial introduced lanthanides as well as naturally occurring elements were analyzed simultaneously and differences between transgenic and wild-type animals are presented. T2 - Metallomics CY - Wien, Austria DA - 13.08.2017 KW - Antibody tagging KW - LA-ICP-MS based immunoassays PY - 2017 AN - OPUS4-41877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis T1 - Application of the scaled boundary finite element method (SBFEM) for numerical simulation of ultrasonic guided waves N2 - The application of waveguides for acoustic measuring technologies and the development of non-destructive evaluation techniques with guided ultrasonic waves for plate like materials like carbon fiber reinforced plastic shells and layered structures require a good understanding of acoustic wave propagation inside the material. The well-known Finite Element Method can be used for simulations, however at least for higher frequencies, the ratio of wavelength and geometrical dimension demands a time-consuming fine grid. Using commercial simulation tools the computational costs increase considerably for ultrasonic frequencies. In the recent years, the Federal Institute for Materials Research and Testing has developed a very efficient alternative for simulating acoustic wave propagation particularly in wave guides by extending the Scaled Boundary Finite Element Method (SBFEM). The SBFEM as a semi-analytical method has one main advantage over the classical Finite Element Method: It only demands a discretization of the boundary instead of the whole domain. This is pictured in the figures below. The method is still related to the Finite Element Method and uses their well-known solving strategies. SBFEM is shown to be highly efficient, especially in the frequency domain. Additionally, the efficiency can be increased by using higher-order spectral elements. In plates and cylinders, the SBFEM can be used to animate propagating modes and computes their wavenumber. In this contribution, we present a short introduction into the basics of SBFEM formulation of the dynamic elastic wave equation. The applicability and efficiency of the approach is demonstrated by applying the method to layered structures and different wave guide geometries. As one example we present the wave propagation in a typical adhesive joint of different metal sheets as common in new designs in automotive industry. The analysis comprises the computation of dispersion curves as starting point of every development of non-destructive testing techniques for inspecting such structures as well as the analysis of the propagating modes. Additional examples presented handle special cases for axis-symmetric geometries, such as pipes and cylindrical rods which are common in various acoustic measurement applications. T2 - Sensor + Test CY - Nürnberg, Germany DA - 30.05.2017 KW - Ultrasound KW - Guided waves KW - Numerical simulation KW - Scaled boundary finite element method PY - 2017 AN - OPUS4-41879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bulling, Jannis T1 - The scaled boundary finite element method to model contact acoustic nonlinearity N2 - In Non-Destructive Testing, ultrasonic waves are commonly used to identify flaws and cracks. In plates, shells, pipes and other geometries guided waves can be used to test the whole structure at once. In these tests, the input and response signal can have a nonlinear relationship due to cracks. At least for higher deflections, the propagating wave excites each side of the crack in such a way that it hits the other side. This clapping generally leads to a generation of higher harmonic waves and is referred to Contact Acoustic Nonlinearity (CAN). To get a better insight into the salient physics of the effect numerical simulations are necessary. In the recent years, the Scaled Boundary Finite Element Method (SBFEM) was introduced to efficiently simulate wave propagation. The main advantage of the method is an easy grid generation process because the domain is discretized with arbitrary polygons instead of the triangles and rectangles. Another advantage is the possibility to model crack tips elegantly without additional workload. The SBFEM approach is still related to the Finite Element Method and uses similar techniques. The method is very efficient using high-order-spectral elements. In this contribution, we present a short introduction into the basics of SBFEM formulation of the dynamic elastic wave equation. The SBFEM is then extended for modeling the non-linear behavior of crack clapping. Different approaches with increasing complexity are presented and assessed with respect to numerical stability. T2 - ICTCA 2017 CY - Wien, Austria DA - 31.07.2017 KW - Contact acoustic nonlinearity KW - Scaled boundary finite element method PY - 2017 AN - OPUS4-41880 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane T1 - A multi-parameter probability of detection (POD) model for flash thermography N2 - In most cases where a POD is calculated based on continuous data obtained by active thermography, the signal-to-noise ratio (SNR) of the signal, the difference of the defect signal to the background or the absolute signal is analyzed as a function of the aspect ratio (ratio of the size of a defect to its overage), although a distinct linear relationship on a linear or logarithmic scale could not be satisfactorily shown and is also not expected. Therefore, a multi-parameter probability of detection (POD) model was developed, where an â versus a continuous signal analysis was based on the linear relationship between the SNR and a multi-parameter a. This POD model is based on data which were recorded within a flash thermography round robin test with nine participants. Metal test specimens with flat bottom holes (FBHs) were analyzed by calculating the SNR of the defect signatures in the thermograms as well as in the phase images as a function of defect parameters. The linear relationship of the experimental data to the multi-parameter a was verified by comparison to data obtained from an analytical model that is considering lateral thermal heat diffusion as well as to data obtained by numerical simulation. The resulting POD curves for the thermograms and phase images give an estimation for the detectability of the FBHs with known geometry in steel using different equipment and obtained by different participants. By comparing the SNRs of FBHs with similar geometries, this POD model was transferred to aluminum and copper as well. T2 - 7th European-American Workshop on Reliability of NDT CY - Potsdam, Germany DA - 05.09.2017 KW - NDT KW - Active thermography KW - POD model KW - Standardization PY - 2017 AN - OPUS4-41882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Dielectric relaxation of discotic liquid crystals N2 - The molecular dynamics of the discotic liquid crystals like pyrene-1,3,6,8-tetracarboxylic tetra(2-ethylhexyl) ester is studied by dielectric relaxation spectroscopy. Dielectric spectroscopy shows 3 processes: a b-relaxation at low temperatures and an a-relaxation in the temperature range of the mesophases followed by conductivity. The dielectric a-relaxation is assigned to a restricted glassy dynamics in the plastic crystal as well as in the liquid crystalline phase. T2 - 16th International Symposium on Electretes CY - Leuven, Belgium DA - 04.09.2017 KW - Discotic liquid crystals PY - 2017 AN - OPUS4-41887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krüger, Simone A1 - Despinasse, Marie-Claire A1 - Raspe, Tina A1 - Nörthemann, K. A1 - Moritz, W. T1 - Early fire detection: Are hydrogen sensors able to detect pyrolysis of house hold materials? N2 - We analysed the hydrogen generation during the smouldering of polymeric materials, which are typically used in the household, in the Smoke Density Chamber coupled to a new developed hydrogen sensor to detect early stages of fires. The results of hydrogen generation were compared with the emission of carbon monoxide and smoke during the fire scenarios. Additionally, the results were compared with parameters used in traditional commercial detection systems. In this scenario, the hydrogen sensor showed encouraging results for the detection of fires in earlier phase compared to traditional detectors. Furthermore, we tested the new developed hydrogen sensor in a real room with different fire scenarios. We have also investigated interferences, e.g. steam and cigarette smoke. The hydrogen sensor could detect hydrogen generation in the earliest stage of fire, even before CO and smoke were developed in detectable amounts. Therefore, the hydrogen sensor can be applied for early fire detection in case of pyrolysis. The sensors are quite good for detecting pyrolysis gases. But when it comes to a fast ignition other techniques are more suitable for it. The sensors are best for combination with other techniques, such as smoke detectors. T2 - IAFSS 12th Symposium 2017 CY - Lund, Sweden KW - Fire chemistry KW - Hydrogen sensor PY - 2017 DO - https://doi.org/10.1016/j.firesaf.2017.04.035 SN - 0379-7112 SN - 1873-7226 VL - 91 SP - 1059 EP - 1067 PB - Elsevier AN - OPUS4-41895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sahre, Mario T1 - Electroplated magnetostrictive actuator layer enabling the external diagnosis of strain sensors N2 - Embedded fibre-opticaloptical strain sensors are suitable for structural health monitoring. In order to validate long-term performance (e.g.sensors integrated in airplane wings or wind power turbine blades) an external diagnostics is required. A strain-detecting region of the optical fibre, the fibre Bragg grating (FBG, is encased by a magnetostrictive layer system serving as actuator. For the validation of the correct sensor function, an external magnetic field introduces mechanical strain resulting in a defined shift of the Bragg wavelength. The layer system is realized by acombined PVD /ECD process optimized regarding magnetostrictive and mechanical properties. The long -term stability of layer adhesion and actuator function has been verified. T2 - 12. Thementage Grenz- und Oberflächentechnik (ThGOT) und das 5. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Germany DA - 14.03.2017 KW - Magnetostrictive actuator layer KW - PVD /ECD process KW - Magnetostrictive layer KW - Strain sensors PY - 2017 AN - OPUS4-41800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zeegers, G. P. A1 - Steinhoff, R. F. A1 - Weidner, Steffen A1 - Zenobi, R. T1 - Evidence for laser-induced redox reactions in matrix-assisted laserdesorption/ionization between cationizing agents and target plate material: a study with polystyrene and trifluoroacetate salts N2 - Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is often applied to assess the dispersity and the end groups of synthetic polymers through the addition of cationizing agents. Here weaddress how these cation adducts are formed using polystyrene (PS) as a model polymer. We analyzed PSby MALDI-MS with a 2-[(2E)-3-(4-tert-butylphenyl)-2-methylprop-2-enylidene]malononitrile (DCTB) as the matrix and a range of trifluoroacetate (TFA) salts as cationizing agents on a range of different targetplate materials (copper, 1.4301 stainless steel, aluminum, Inconel 625, Ti90/Al6/V4 and chromium-, gold-and silver-plated stainless steel). It was found that on a stainless steel substrate the metal cations Al+,Li+, Na+, Cu+and Ag+formed polystyrene adducts, whereas K+, Cs+, Ba2+, Cr3+, Pd2+, In3+, or their lower oxidation states, did not. For the copper and silver substrates, PS and DCTB adduct formation with cations liberated from these target plate materials was observed upon addition of a cationizing agent, which indicates the occurrence of redox reactions between the added TFA salts and the target plate material. Judging from their standard electrode potentials, these redox reactions would not normally occur, i.e.,they require an additional energy input, strongly suggesting that the observed redox reactions are laser-induced. Furthermore, copper granules were found to successfully sequester PS from a tetrahydrofuran(THF) solution, consistent with the view complex formation with the copper target plate can take place prior to the MALDI-MS measurement. KW - Polymer MALDI KW - Cationization KW - Polystyrene KW - Laser-induced redox reactions KW - Target plate material PY - 2017 DO - https://doi.org/10.1016/j.ijms.2016.10.007 SN - 1387-3806 SN - 1873-2798 VL - 416 SP - 80 EP - 89 PB - Elsevier B.V. AN - OPUS4-41146 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Boehm, Rainer A1 - Heckel, Thomas T1 - Simulation of sparse matrix array designs N2 - Matrix phased array probes become more and more prominent to be used in industrial applications. The main drawbacks, using probes incorporating a very large number of transducer elements, are the needs for an appropriate cabling and an ultrasonic device offering many parallel channels. Matrix arrays designed for extended functionality feature at least 64 or more elements. Typical arrangements are square matrices, e.g. 10 by 10 or 11 by 11 or rectangular matrices, e.g. 8 by 16 or 10 by 12 to fit a 128-channel phased array system. In some phased array systems, the number of simultaneous active elements is limited to a certain number, e.g. 32 or 64. Those setups do not allow to run the probe with all elements active which may cause a significant change in the directivity pattern of the resulting sound beam. When only a subset of elements is possible to use during a single acquisition, different strategies may be applied to collect enough data for rebuilding the missing information from the echo signal. Omission of certain elements may be one approach, overlay of subsequent shots with different active areas may be another one. This paper presents the influence of decreased number of active elements on the sound field and their distribution on the array. An example for 16 active elements out of 121 is given in Figure 1. The sound field divergence and its shape basically remain the same, while the sensitivity is reduced and the amplitudes of the speckle-like side lobes increase significantly. Solutions using subsets with different element activity patterns on matrix arrays and their advantages and disadvantages concerning the sound field are evaluated using semi-analytic simulation tools. Sound field criteria regarding the consequences for NDT test results and the system setup are discussed. T2 - QNDE 2017 CY - Provo, UT, USA DA - 17.07.2017 KW - Ultrasound KW - Sparse array KW - Simulation PY - 2017 AN - OPUS4-41149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Non-Destructive ultrasonic investigations on FRP structures N2 - Components made of fibre-reinforced plastic are a prominently used material in modern safety-relevant structures. Periodic in-service non-destructive inspection of these structures is necesary. The EMRP-funded project VITCEA aims on the evaluation of the performance of various non-destructive testing methods on the inspection of fibre-reinforced plastics. The physical layout of fibre layers leads to complex structures of fibre-reinforced plastic parts. Furthermore different material properties of the fibre and the resin cause anisotropic behaviour of the material.This poses a challenge for ultrasonic NDT by causing a complex acoustical response. The acoustical behaviour of fibre-reinforced plate materials has been simulated. Specimens with artificial flaws for the evaluation of the detection thresholds have been designed and manufactured. Mechanized ultrasonic testing methods using phased-array sensors, air-coupled transducers, immersion tank testing and contact technique have been evaluated on the specimen. In this talk results of different ultrasonic testing methods will be compared and discussed. T2 - VITCEA Steakholder Workshop CY - NPL, London, UK DA - 7.6.2017 KW - FRP KW - Fiber reinforced platic KW - Ultrasound KW - Matrix array KW - ACUT KW - Air coupled KW - Non-destructive testing PY - 2017 AN - OPUS4-41153 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schlegel, Moritz-Caspar T1 - Nano-porous Materials - Introduction into Metal-organic Frameworks N2 - Metallic organic frameworks are the materials stirring great interest by their large variety of structure types and chemical composition as well as low density and very high surface area, which are desirable properties for gas storage such as for hydrogen, methane or carbon dioxide. Using different so called secondary building units offer an opportunity to form tunable structures with channels of various geometry and allow in this way to study the absorption of the molecular hydrogen, methane or carbon dioxid in the systematic way. T2 - Neutron Scattering Application to Hydrogen Storage Materials CY - Berlin, Germany DA - 07.08.2017 KW - MOFs KW - Hydrogen KW - Crystallography PY - 2017 AN - OPUS4-41285 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Thorid T1 - Mehr-Proben-Kleb-Vorrichtung (MPKV) zur Validierung der Klebfestigkeit N2 - Mit der Verfügbarkeit der Mehr-Proben-Prüfung von bis zu 8 Klebverbunden mittels CAT-Technologie (CAT: centrifugal adhesion testing) wurde im Forschungsvorhaben OKTETT ein durchgehendes Mehr-Proben-Konzept zur Validierung der Klebfestigkeit angewendet. Dazu gehört ein universeller Probenteller (Abb.1) zur Mehr-Proben-Handhabung bei Vorbehandlung, Lagerung, Transport und Klebung. Für das Mehr-Proben-Kleben wurde die MSB-Technologie (MSB: multiple sample bonding) unter Verwendung einer instrumentierten hydraulischen Mehr-Proben-Kleb-vorrichtung entwickelt. Damit kann der Klebandruck für bis zu 8 Prüfkörper über einen Drucksensor definiert eingestellt und die gesamte Vorrichtung beim Kleben Temperaturen von bis zu 180°C ausgesetzt werden. T2 - 12. Thementage Grenz- und Oberflächentechnik (ThGOT) und das 5. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Gemany DA - 14.03.2017 KW - Zentrifugentechnologie KW - Mehr-Proben-Kleben (MSB) KW - Mehr-Proben-Prüfen (CAT) KW - Haftfestigkeit KW - Verbundfestigkeit PY - 2017 AN - OPUS4-41291 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Complex dynamics of ultra-thin films of blends of polystyrene/ poly(vinyl methyl ether) by nanosized relaxation spectroscopy N2 - In the course of miniaturizing modern technology down to the molecular scale, understanding the materials behavior has to be investigated and deviations from the bulk have to be understood. A combination of nano-sized relaxation spectroscopies (Broadband Dielectric Spectroscopy (BDS) and Specific Heat Spectroscopy (SHS)) employing AC nanochip calorimetry were utilized to investigate the glassy dynamics of ultra-thin films of blends of Poly (vinyl methyl ether) (PVME) / Polystyrene (PS) (50:50 and 25/75 wt-%), which are miscible in the bulk (thicknesses: 8nm - 200nm, film thickness was controlled by ellipsometry, film topography by AFM). Both methods are sensitive to different probes; where SHS senses entropy fluctuations BDS measures dipole fluctuations. For BDS measurements, a recently developed nano-structured electrode sample arrangement is employed. By measuring the dynamic glass transition in dependence of the film thickness, SHS showed that the Tg of the whole film was strongly influenced by a nanometer-thick surface layer at the polymer/air interface due to a self-assembling process. Compared to the SHS results the BDS measurements show a completely different behavior. At high temperatures the temperature dependence of the relaxation times of the films follows that of bulk-like PS/PVME obeying the VFT-law. With decreasing temperature the temperature dependence deviates from the VFT to an Arrhenius law where the apparent activation energy decreases with decreasing film thickness. This is the first example were confinement induced changes were observed by BDS for ultra-thin films. All results were analyzed in detail in a comprehensive discussion. T2 - 8th International Discussion Meeting Relaxation in Complex Systems CY - Wisla, Poland DA - 23.07.2017 KW - Ultra thin polymer films PY - 2017 AN - OPUS4-41171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yildirim, Arda T1 - Structure, Dynamics and Phase Behavior of a Discotic Liquid Crystal Confined in Nanoporous Anodic Aluminum Oxide Membranes N2 - Discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to organize and stack themselves into columns in a hexagonal columnar mesophase, a mesophase in between the plastic crystalline and isotropic phase, driven by the overlap of the π orbitals of their aromatic core. This leads to a high charge-carrier mobility along the column axis. Further, these columns could then be considered as “molecular nanowires”. Spatial confinement of soft matter in nanoporous media influences its structure, thermodynamic properties, and mobility. Embedding liquid crystals and polymers into nanopores of anodic aluminum oxide (AAO) results in a 2D nanoconfinement of these materials. This confinement affects their properties, compared to the bulk, such as phase transition temperatures and enthalpies, molecular mobility, and architecture of the crystallization. In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6), a triphenylene-based DLC, was confined into nanoporous AAO membranes. The structure, dynamics and the phase behavior of the confined HAT6 were investigated by broadband dielectric spectroscopy (BDS) and differential scanning calorimetry (DSC). HAT6 was embedded into nanoporous AAO membranes by melt infiltration in the isotropic phase under argon atmosphere. The membranes have parallel aligned cylindrical nanopores, with different pore diameters in the range of 10-180 nm. Bulk HAT6 forms a hexagonal columnar phase; in between the isotropic phase above 371 K and the plastic crystalline phase below 340 K. Unlike the bulk, the confined HAT6 split the phase transitions in two or more, which might be interpret as different phase structures; close to the wall and at the pore center. Moreover, the phase transitions of the confined HAT6 shifted, with decreasing pore diameter, to lower temperatures. The dependencies of the phase transition temperatures on the pore size was well-described by the Landau-de Gennes model. Furthermore, pore surfaces of a series of membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. HAT6 was embedded into the modified membranes by the same aforementioned preparation. The influence of the changed host-guest-interaction, on the structure, dynamics, and the phase behavior of HAT6 confined in the modified membranes, was also investigated by BDS and DSC. T2 - Liquids 2017 – 10. Liquid Matter Conference CY - Ljubljana, Slovenia DA - 17.07.2017 KW - Discotic Liquid Crystals KW - Nanoconfinement PY - 2017 AN - OPUS4-41178 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler T1 - X-Ray Computed Tomography as a Tool for Calibration and Validation of Numerical Simulations N2 - This presentation includes the results of a number of case studies of concrete properties using computed tomography (CT) in combination with various in-situ testing techniques, including those of mechanical loading, water transport, and fire. The results of these case studies demonstrate the potential of CT as an approach for obtaining unique, quantitative data about the structure of materials. This data can serve as the basis for calibrating and validating a new generation of numerical models that have a stronger foundation in micromechanical theory. This will contribute to the development of more accurate and versatile simulation approaches for concrete and other building materials. T2 - International Workshop: Micromechanics of Rocks and Concrete CY - Berlin, Germany DA - 21.07.2017 KW - Computed tomography (CT) KW - In-situ testing KW - Case studies PY - 2017 AN - OPUS4-41104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nguyen, Thi Yen T1 - Guided crystallization: The influence of solvent and concentration N2 - Theoretical and experimental studies indicate that crystal nucleation can take more complex pathways than expected on the ground of the classical nucleation theory. A direct in situ observation of the different pathways of nucleation from solution is challenging since the paths can be influenced by heterogeneous nucleation sites, such as container walls. The custom-made acoustic levitator using in these experiments regulates the influence that solid surfaces, temperature, and humidity have on the crystallization process. The investigations of the crystallization process of paracetamol were performed with in situ analytical techniques and theoretical simulations to gain a comprehensive insight into processes, occurring intermediates, and required reaction conditions. The targeted choice of the solvent and the concentration enabled the guidance of the pathways, therefore, resulting in the isolation of one desired crystalline structure. T2 - Annual COST meeting CY - Lincoln, United Kingdom DA - 25.06.2017 KW - Crystallization KW - Polymorphism KW - Molecular dynamic simulation KW - Pair distribution function analysis KW - XRD PY - 2017 AN - OPUS4-41111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Industrielle Durchstrahlungsprüfung mit Filmen und digitalen Detektoren N2 - Der Vortrag stellt Grundlagen und Anwendungen der industriellen Durchstrahlungsprüfung vor. Ausgehend von den Röntgenfilmen und ihren Eigenschaften werden moderne Technologien zum Filmersatz erläutert. Das sind die Computerradiographie mit Speicherfolien oder digitale Matrixdetektoren (DDA). Zentrale Frage in der industriellen Radiographie ist die erreichbare Bildqualität. Als Anwendungen werden die Korrosionsprüfung von Rohrleitungen mit CR und die Hoch-Kontrastempfindlichkeits-Radiographie mit DDAs präsentiert. T2 - 65. Radiometrisches Seminar Theuern "Bildgebende Verfahren mit ionisierender Strahlung in nicht-medizinischen Anwendungen" CY - Theuern, Germany DA - 12.05.2017 KW - DDA KW - ZfP KW - Radiographie KW - CR KW - FIlm PY - 2017 AN - OPUS4-41131 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Alte Bekannte im neuen Gewand: zertifizierte BAM-Schwärzungstreppen zur Densitometerkalibrierung N2 - Es wird die Entwicklung der BAM-Schwärzungstreppen von ihren Anfängen Ende der 1970er Jahre bis zum heutigen Referenzmaterial "Filmtreppe optischer Dichten für die technische Radiographie" dargestellt, dessen BAM-Zertifizierung vor dem Abschluß steht. T2 - DGZfP-Jahrestagung 2017 CY - Koblenz, Germany DA - 22.05.2017 KW - Optische Dichte KW - ZfP KW - Radiographie KW - Röntgenfilm PY - 2017 AN - OPUS4-41132 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Recent developments of photon counting and energy discriminating detectors for radiographic testing N2 - The direct detection of X-ray photons into electrical signals is enabled by usage of highly absorbing photo conducting materials (e.g. CdTe) as detection layer of an underlying CMOS semiconductor X-ray image detector. If the read-out speed is high enough (ca. 50 – 100 ns dead time) single X-ray photons can be counted and their energy measured. Read-out noise and dark image correction can be diminished. By setting energy thresholds, selected energy ranges of the X-ray spectrum can be detected or suppressed. This allows material discrimination or reduction of scattered radiation, which results in an enhanced contrast sensitivity. T2 - 2017 Far East Forum on Nondestructive Evaluation & Testing CY - Xi`an, China DA - 21.06.2017 KW - Industrial X-ray imaging KW - Direct detection KW - Photon counting KW - Energy discrimination KW - Dual energy imaging PY - 2017 AN - OPUS4-41133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zscherpel, Uwe T1 - Annual report of sub-commission V-A "Radiography based weld inspection" N2 - Annual report on activities of sub-commission V-A of the International Institute of Welding given by its chairman. T2 - Annual Assembly of IIW CY - Shanghai, China DA - 25.06.2017 KW - Radiographic testing KW - International Institute of Welding PY - 2017 AN - OPUS4-41135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mooshofer, H. A1 - Boehm, Rainer A1 - Heinrich, W. A1 - Fendt, K. A1 - Goldammer, M. A1 - Kolk, K. A1 - Vrana, J. T1 - Amplitudenbasierte Fehlergrößenbewertung mit SAFT: Auf dem Weg von der bildlichen Darstellung zum Messverfahren N2 - Die Größenbewertung von Anzeigen und die Bestimmung der Nachweisgrenze spielen bei der Ultraschallprüfung eine zentrale Rolle: Sie stellen sicher, dass kritische Ungänzen erfasst und bruchmechanisch behandelt werden können. Bei SAFT wurde bisher die Größe von Ungänzen dadurch bestimmt, dass die räumliche Anzeigenausdehnung im Rekonstruktionsergebnis ausgewertet wird, d.h. die Anzahl von Voxel über die sich eine Anzeige erstreckt. Auf diese Weise lassen sich jedoch nur Defektanzeigen bewerten, die größer oder gleich der Wellenlänge sind. Bei kleinen Defekten versagt diese Methode, d.h. es ist keine Größenbewertung möglich. Außerdem bietet diese Methode keine Aussage über die Nachweisgrenze des Verfahrens. Ein Hauptvorteil von SAFT gegenüber der konventionellen Ultraschallprüfung ist aber gerade die Verbesserung der Nachweisgrenze, denn SAFT steigert das Signal-Rausch-Verhältnis (SNR) gegenüber dem Gefügerauschen und reduziert statistisches Rauschen. Um diesen Hauptvorteil nutzen (und quantifizieren) zu können, wird für SAFT eine Methode zur Nachweisgrenzenbestimmung und zur Größenbewertung der Anzeigen kleiner Ungänzen benötigt. Neben ihrer räumlichen Ausdehnung lassen sich Anzeigen im SAFT-Ergebnis auch durch ihre Amplitude charakterisieren, wenn die Prüfkopfeigenschaften und die geometrischen Verhältnisse beim Scan berücksichtigt werden. Genauer gesagt durch die Amplitudensumme, in die - neben der Echoamplitude - auch die winkelabhängige Streucharakteristik eingeht. Im Folgenden wird dargelegt, dass sich die Amplitudensumme zur Nachweisgrenzenbestimmung und zur Größenbewertung kleiner Ungänzen eignet. Es wird der Zusammenhang zwischen der Amplitudensumme und der Größe von Ungänzen dargestellt, und es wird gezeigt, dass auch die Anzeigenposition und die Form des Prüfobjektes eine Rolle spielen können. Auf dieser Basis wird eine Methode zur Größenbestimmung kleiner Anzeigen im SAFT-Ergebnis entwickelt. Damit lässt sich das SAFT-Ergebnis als Ersatzfehlergröße darstellen, so wie das bei konventioneller Ultraschallprüfung z.B. mit Hilfe von AVG-Diagrammen erfolgt. Durch die Vervollständigung um die Größenbewertung ist SAFT nicht mehr nur ein bildgebendes Verfahren, sondern es kann vielmehr als vollwertiges Messverfahren dienen. T2 - DGZfP-Jahrestagung 2017 CY - Koblenz, Germany DA - 22.05.2017 KW - Synthetic aperture focussing technique (SAFT) KW - Defektgrößenbewertung KW - Gewichtete Amplitudensumme KW - Kleine Reflektoren PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-411571 SN - 978-3-940283-85-6 VL - 162 SP - 1 EP - 9 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-41157 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuchenbecker, Petra T1 - Ringversuch: Partikelgrößenbestimmung von keramischen Pulvern mittels Laserstreulichtverfahren nach ISO 13320 N2 - Der Vortrag gibt anhand eines konkreten Beispiels einen Überblick über die notwendigen, umfangreichen Schritte zur Vorbereitung, Durchführung und Auswertung von Ringversuchen nach DIN EN ISO 17043. T2 - Sitzung des Fachausschuss 2 (Rohstoffe) der DKG CY - Meißen, Germany DA - 21.06.2017 KW - Ringversuch KW - Partikelgröße KW - DIN EN ISO 17043 PY - 2017 AN - OPUS4-41158 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Quantitation of luminescent properties of Yb and Ho co-doped NaYF4 colloidal nanoparticles - novel active-core-active-shell materials and novel characterization methods N2 - At the core of luminescence color and lifetime tuning of rare earth doped upconverting nanoparticles (UCNPs) is the understanding of the impact of the particle architecture for commonly used sensitizer (S) and activator (A) ions. In this respect, we present here a series of core@shell NaYF4 UCNPs doped with Yb3+ and Ho3+ ions, where the same dopant concentrations were distributed in different particle architectures following the scheme: YbHo core and YbHo@..., …@YbHo, Yb@Ho, Ho@Yb, YbHo@Yb, and Yb@YbHo core-shell NPs. As revealed by quantitative steady state and time-resolved luminescence studies, the relative spatial distribution of the A and S ions in the UCNPs and their protection from surface quenching has critical impact on their luminescent characteristics. Interestingly, although the increased amount of Yb3+ ions boosts UCNP performance by increasing the absorption, the Yb3+ ions can also dissipate the energy stored in the material through energy migration to surface, thereby reducing the overall energy transfer efficiency to the activator ions. T2 - COST Workshop CY - Aveiro, Portugal DA - 30.06.2017 KW - Upconversion KW - Nanoparticle KW - Flourescence KW - Core-shell architecture KW - NIR KW - Absolute flourometry KW - Integrating sphere spectroscopy KW - Ho(III) KW - Yb(III) PY - 2017 AN - OPUS4-41161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin A1 - Solomun, Tihomir A1 - Meyer, Susann A1 - Kunte, Hans-Jörg A1 - Schröter, Maria-Astrid A1 - Sturm, Heinz T1 - Development of a standard procedure for the irradiation of biomolecules N2 - In dosimetry the determination of the effectiveness of the damaging processes is standardized and accounted for by the radiation and tissue weighting factor. For the underlying constituents of the tissue, that is the various biomolecules, such a systematic approach doesn't exist. This makes it difficult to compare results obtained under different experimental conditions. In the following work, we will describe a method to obtain comparable values for the radiation-biomolecule interaction, measured under different conditions. This approach can lead to standardization of dosedamage relationship at the molecular level. Such approach is necessary for a better understanding of the relations between the damage of the single constituents of biological tissue and the whole – finally gaining a more complete picture of irradiation damage. T2 - 14th International Congress of the International Raditation Protection Association (IRPA) CY - Cape Town, South Africa DA - 09.05.2016 KW - Dosimetry PY - 2017 VL - 14 SP - 1 EP - 5 AN - OPUS4-41164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Online-qNMR-Spektroskopie zur Charakterisierung des Lösungsverhaltens von pharmazeutischen Wirkstoffen und Formulierungen N2 - Nur weit weniger als ein Prozent aller pharmazeutischen Wirkstoffe finden den Weg in die Anwendung. Grund dafür sind in fast allen Fällen die äußerst schlechten biopharmazeutischen Eigenschaften der Wirkstoffe, wie ihre Löslichkeit, Stabilität und – bei festen Darreichungsformen – ihre Kristalleigenschaften, auch wenn die Wirkstoffe eine gute Wirksamkeit oder gute toxikologische Eigenschaften aufweisen. Mit dem Trend zu höheren Molmassen bei chemischen Wirkstoffen nimmt ihre Löslichkeit in wässrigen Systemen rapide ab. Verbesserungen der Löslichkeit und des Auflösungsverhalten stellen heute die zentrale Herausforderung bei der Entwicklung neuer Arzneimittel dar und liegen im Fokus der aktuellen pharmazeutischen Forschung und Entwicklung. Für eine Verbesserung der physikalisch chemischen Eigenschaften werden verschiedene Verfahren beforscht: Mikronisierung, gezielte Salzbildung bzw. Salzscreening, Solubilisierung mit Cosolventien oder die Nutzung von Polymeren als mögliche Transportwege. Pharmazeutische Cokristalle bestehen aus einem Wirkstoff und einem sogenannten Cokri-stall-Bildner. Bei letzterem handelt es sich typischerweise um ein organisches Molekül, das ähnliche Struktureigenschaften wie der pharmazeutische Wirkstoff aufweist. Die Synthese und Charakterisierung von pharmazeutischen Cokristallen ist von patentrechtlicher Relevanz und Gegenstand aktueller Forschungen, da die Bildung solcher Cokristalle häufig mit einer Verbesserung der physikochemischen Eigenschaften der enthaltenen Wirkstoffe einhergeht. In den letzten Jahren ist es gelungen, insbesondere das Auflösungsverhalten der pharmazeutischen Wirkstoffe gezielt zu verbessern und dadurch eine optimierte Bioverfügbarkeit zu realisieren. Um einige Einschränkungen der Methoden UV/VIS-Detektion und HPLC zu umgehen, verfolgen wir das Auflösungsverhalten der Cokristalle mittels Online-NMR-Spektroskopie als ein direktes Verfahren: Die Methode erlaubt zum einen die direkte Beobachtung und Quantifizierung individueller Species, die bei der Auflösung beteiligt sind, d. h. Wirkstoff(e), Cokristallbildner und Lösungsmittel lassen sich getrennt voneinander mit einer hohen zeitlichen Auflösung und spektraler Dispersion beobachten. Ferner kommt diese Me-thode ohne Kalibrierung aus, da die NMR-Spektroskopie eine "absolute Vergleichsmethode" ist. Darüber hinaus kann die absolute Konzentration gemessen werden, wenn gegen Standards gearbeitet wird. Der Einsatz dieses Verfahrens zum Studium des Auflösungsverhaltens ist völlig neu. Perspektivisch reizvoll ist die Weiterentwicklung zu einem mikroanalytischen Verfahren, das mit äußerst geringen Substanzmengen auskommt. T2 - Institutskolloquium Pharmazie und Lebensmittelchemie, Julius-Maximilians-Universität Würzburg CY - Würzburg, Germany DA - 27.07.2017 KW - Pharmazeutische Wirkstoffe KW - Pharmazeutische Formulierungen KW - Cokristalle KW - qNMR-Spektroskopie KW - Quantitative NMR-Spektroskopie KW - Auflösungsverhalten PY - 2017 AN - OPUS4-41166 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yildirim, Arda T1 - Structure, Dynamics and Phase behavior of bulk and confined liquid crystals N2 - In this study, the molecular dynamics of two linear-shaped tetramethylated guanidinium triflates ionic liquid crystals were investigated by a combination of Broadband Dielectric Spectroscopy (BDS) and Specific Heat Spectroscopy (SHS). Three processes were detected by BDS; at low temperature γ-process, at higher temperatures α-process and at even higher temperatures conductivity. The γ-process indicates localized fluctuations, and the α-process designates cooperative fluctuations. Slightly different restrictions were found for conductivity processes of LC536 and LC537 due to the slightly different lengths of alky chains. Furthermore, the cooperative dynamics were also probed by SHS. The cooperative dynamics probed by the different techniques (BDS and SHS) compared, and assigned to the different restrictions on the cooperativity due to the difference in the sensitivity of the techniques. T2 - Seminar Vortrag Universität Stuttgart CY - Stuttgart, Germany DA - 24.07.2017 KW - Discotic Liquid Crystals PY - 2017 AN - OPUS4-41179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sentker, K. A1 - Yildirim, Arda T1 - Characterization of the thermotropic phase behavior and microscopic structure of a confined discotic liquid crystal N2 - Discotic liquid crystals (DLC) filled into cylindrical nanopores exhibit a liquid crystalline phase with their molecules arranged in hexagonal columns. The columns orient perpendicular (radially) or parallel (axially) with respect to the pore axis depending on surface anchoring conditions and pore size. Axially oriented columns enable the fabrication of organic nanowires utilizing the high conductivity in the stacking direction due to overlapping π-electrons. This leads to interesting applications in e.g. organic semiconductorbased devices. The molecular ordering of the liquid crystalline columns can be probed by temperature dependent optical retardation measurements supplemented by X-ray diffraction sensitive to the translational order. We investigated the DLC 2, 3, 6, 7, 10, 11 - hexakis [hexyloxy] triphenylene (HAT6) embedded in nanoporous alumina and silica membranes as function of the pore diameter (12 nm - 180 nm). Due to their hydrophilic nature porous membranes enforce face-on anchoring leading to a radial orientation. To obtain edge-on anchoring conditions, and thus favoring axial orientation, the silica membrane surface is chemically modified. The optical retardation measurements show that the columns orient radially in these membranes independent of the anchoring conditions. Interestingly, a quantized phase transition of each molecular layer is found indicated by a distinct increase of the optical orientation. Additionally, an axial orientation of HAT6 filled into alumina membranes with a pore diameter of 25 nm is achieved. A Landau-de Gennes ansatz semi-quantitatively describes the phase transition behavior observed. X-ray diffraction experiments performed at the 3rd generation synchrotron radiation source PETRA III at DESY giving detailed information about the translational order support these findings. Summarizing, this study shows the existence of a phase transition in the molecular range as well as the suitability of the membrane with 25 nm pores as a template for preparing organic nanowires. T2 - Liquids 2017 – 10th Liquid Matter Conference CY - Ljubljana, Slovenia DA - 17.07.2017 KW - Discotic Liquid Crystals PY - 2017 AN - OPUS4-41180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koegler, M. T1 - Time-gated Raman spectroscopy and SERS as advanced technologies in bioprocess monitoring N2 - Raman spectroscopy is becoming a powerful process analytical technology (PAT) tool. Until now Raman technology has not shown its full potential in bioprocess on-line monitoring due to several technical challenges. Because of only small? interference from water molecules, Raman-spectroscopy is in contrast to IR spectroscopy able to follow changes of metabolite concentrations in dilute aqueous solutions. Results from common CCD-based process Raman-spectrometers reveal only barely identifiable peaks with a dominating (fluorescence) background. To solve this, Raman spectroscopy needs: (A) an enhancement to increase the limit of detection (LOD), and (B) a reliable method to distinguish the Raman signal from the sample-related auto-fluorescence. SERS (surface enhanced Raman spectroscopy) acts as an optical "nano-antenna"-effect. It causes a dipolar localized surface Plasmon resonance effect due to noble metallic nanoparticles or roughened metal and improves the limit of detection (LOD) significantly. Another new process-monitoring technique, which removes the fluorescence background in Raman-measurements is called time-gated Raman spectroscopy. It uses a picosecond pulsed Nd:YVO4-laser as emission source (exc= 532 nm) and a gated SPAD-array (Single Photon Avalanche Detector) detector instead of commonly used CCD (Charged Coupled Device)-detectors and CW (Continues Wave) laser emission. Time-Gate can measure the Raman-signal before the stronger fluorescence signal reaches the detector. In this study we utilized both SERS (Surface Enhanced Raman Spectroscopy) and time-gated Raman spectroscopy (TG-Raman) in combination on cell-free supernatant samples of an Escherichia coli cultivation with mineral salt media and a lactic acid bacteria fermentation with complex media. As a reference method for the estimation of amino acids and other metabolites, HPLC-RID and HPLC-FLD were used to evaluate the Raman-based detection. The quantitative evaluation of Raman data was performed by multivariate data analysis such as principal component analysis (PCA) and partial least squares regression (PLSR). For the first time, we can show that both qualitative and quantitative measurements are conducted successfully with both, SERS and time-gated Raman methods in industrially relevant media, so that a fast and reliable in situ or bypassed concentration measurement becomes feasible. T2 - 2. Photonics Finland, Optics and Photonics Days 2017 CY - Oulu, Finland DA - 29.05.2017 KW - Time-gate Raman KW - PAT KW - Chemometrics PY - 2017 UR - http://www.photonics.fi/event/opd17-optics-photonics-days-2017/ AN - OPUS4-41182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Explosive trace detection by ion mobility spectrometry for air cargo screening N2 - This article describes the application of the ion mobility spectrometry (IMS) as a technical link in the screening within the airfreight transport chain. Air freight is of very important also for German foreign trade. Every year around 4.3 Mt of freight are loaded at German airports and transported by air planes. The average value of a transported metric ton freight was approximately 81,000 € in 2015. Nearly 50 percent of the total air freight is transported in passenger planes as belly freight. Measures are necessary to detect illegal, dangerous items such as weapons, ammunition or improvised explosive devices (IED) to protect against attacks on air traffic security. The aim is to increase security in air traffic and at the same time contemporary increasing or at least unchanged efficiency in the airfreight transport chain. IMS is a suitable instrumental technology for the trace detection of explosives (ETD) and their precursors orthogonal to radiological x-ray measurements on suspicious freight within 30 seconds and per EU regulation 2015/1998, section 6.2. The ECAC* certified ETD system QS-B220 was used. The IMS performance is demonstrated on three target compounds, TNT, RDX and PETN. The results’ evaluation of this semi-quantitative screening is carried out by using statistical methods for reliability assessment, such as probability of detection (POD) and receiver operating characteristic (ROC). Their detection limits with a POD = 0.90 are determined after swab sampling on various surfaces. These screening results provide an objective decision-making aid to responsible control personnel in addition to x-ray measurements, whether there are or are no dangerous substances or objects in the cargo. *) ECAC = European Civil Aviation Conference T2 - 26th International Conference on Ion Mobility Spectrometry CY - Ozarow Mazowiecki (Warsaw), Poland DA - 23.07.2017 KW - Air traffic security KW - Ion mobility spectrometry KW - Explosive trace detection KW - Airfreight transport chain PY - 2017 AN - OPUS4-41188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Madkour, Sherif T1 - In-situ probing of the dynamics of irreversibly adsorbed layers in PVME thin films N2 - For many years now, the so-called three layer model (free-surface, bulk-like, and adsorbed layers) has been commonly used, along with other parameters, to explain the deviations seen in glass transition and glassy dynamics for polymers confined into thin films, compared to their bulk value. Nevertheless, due to the hard accessibility of the adsorbed layers in supported films, little is known about the nature of their dynamics and how they really influences the overall dynamics of the thin films. Here, the irreversibly self-assembled adsorbed layer of a low MW Poly (vinyl methyl ether) (PVME) is solvent-leached from a 200 nm film. The thickness and topography of this layer is checked with Atomic Force Microscopy (AFM), to insure no dewetting and low roughness. Further, the dynamics of the adsorbed layer is then in-situ probed with Broadband Dielectric Spectroscopy (BDS). A recently developed nano-structured capacitor arrangement was employed; where a silicon wafer with nanostructured SiO2 nano-spacers, with heights of 35 nm, is placed on top of a thin film spin coated on an ultra-flat highly conductive silicon wafer. All results will be discussed in detail and quantitatively compared to our recent work on the glassy dynamics of PVME thin films (50 nm- 7nm), where BDS measurements showed two thickness-independent relaxation processes. The first process was assigned to the -relaxation of a bulk-like layer. Whereas the second process showed a different temperature dependence and was ascribed to the relaxation of polymer segments adsorbed at the substrate. To our knowledge, this is the first in-situ study of the dynamics of an irreversibly adsorbed layer. T2 - 8th International Discussion Meeting Relaxation in Complex Systems CY - Wisla, Poland DA - 23.07.2017 KW - Thin films PY - 2017 AN - OPUS4-41190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schwaar, Timm T1 - Particle-based epitope analysis of a monoclonal antibody N2 - A method for the examination of the epitope of a monoclonal antibody against a peptide related to hepcidin-25, known as a biomarker in the ion metabolism, was developed. Characterizing the exact binding site helps to understand the properties of the antibody. A peptide consists of different amino acids, each contributing differently to the binding strength. To examine the influence of the amino acids, each amino acid was subsequently exchanged by glycine. If the respective amino acid is critical for binding to the antibody, a significant drop in the binding affinity should be observed. The epitope screening of monoclonal antibodies is a complex and elaborate procedure. For this approach, variants of the peptides were synthesized by conventional Fmoc-based peptide synthesis. The solid support was chosen to be suitable for the synthesis and additional screening against the antibody. To determine the binding affinity, the bead-bound peptides were incubated with a fluorophore-labeled antibody. After the incubation, the beads were placed on a slide and the fluorescence was detected by a fluorescence scanner. A high fluorescence indicates a high binding affinity and vice versa. T2 - Tag der Chemie 2017 CY - Berlin, Germany DA - 05.07.2017 KW - Antibody KW - Epitope analysis PY - 2017 AN - OPUS4-41191 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abbas, Ioana M. T1 - HPLC-MS/MS quantification of hepcidin-25, a new promising iron biomarker, in human serum samples N2 - Hepcidin-25 has attracted much attention ever since its discovery in 2001. It is widely recognized that this liver produced peptide hormone plays a major role in the regulation of iron levels in mammals. Hepcidin levels could reveal important clinical information about several pathological states in patients suffering from iron-related disorders such as chronic kidney disease (CKD) or hereditary haemochromatosis (HH). Despite significant efforts though, the development of a reliable assay to quantify hepcidin proved to be problematic for the last 15 years. With the aim to tackle the current difficulties in hepcidin quantification and improve the status of this promising biomarker in the clinical field, we developed a rapid and robust analytical strategy for the quantification of hepcidin-25 in human samples based on HPLC-MS/MS (QqQ) to be implemented in routine laboratories. The novelty of the method is the use of special HPLC vials to avoid adsorptive losses due to the basic character of the peptide that causes interaction with the silanol groups of the vial’s glass surface. Up to 90% decrease in the MS/MS signal was observed, when commercial HPLC vials were used, while vials treated with 3-(2-aminoethylamino)propylmethyl-dimethoxysilane or 1H,1H,2H,2H-perfluorooctyltriethoxysilane, leading to no significant losses in the dynamic range of physiological hepcidin-25 mean serum levels (10-20 µg/L). Careful analytical validation was performed for determining the reproducibility, repeatability, limit of quantification (0.5 µg/L) and linearity (0.5-40 µg/L) of the method. Serum samples from 9 healthy volunteers were analyzed with a median hepcidin-25 level of 3.3 µg/L, comparable to results reported in the literature. T2 - Tag der Chemie 2017 CY - Berlin, Germany DA - 05.07.2017 KW - Hepcidin-25 KW - LC-MS/MS KW - Iron biomarker PY - 2017 AN - OPUS4-41193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Thermoakustische Ultraschallwandler für zerstörungsfreie Materialprüfung N2 - Luftgekoppelte Ultraschallwandler werden für die bildgebende Prüfung von Klebeverbindungen und Verbundwerkstoffen eingesetzt. Nach dem heutigen Stand der Technik wird die Prüfung in Durchschallung durchgeführt, d.h. der Prüfling befindet sich zwischen dem Sender und dem Empfänger. Allerdings erlauben komplexere Strukturen wie z.B. Teile einer PKW-Karosserie, nur einen einseitigen Zugang. Für die Prüfung solcher Bauteile sind Wandler von hoher Bandbreite von Vorteil. Thermoakustische Wechselwirkung, wobei thermische Energie einer elektrisch geheizten Elektrode in akustische umgewandelt wird, öffnet die Möglichkeit, extrem breitbandige Pulse zu erzeugen. In unserem Beitrag werden verschiedene thermoakustische Sender vorgestellt. Die meisten bestehen aus einer elektrisch leitenden Schicht auf einem festen Substrat. Der erste Typ ist ein Sender mit einer Elektrode aus Indium-Zinn-Oxid auf Glas-Substrat kombiniert mit einem Laser-Doppler-Vibrometer als Empfänger. Diese Kombination ermöglicht extrem breitbandige Signale. Der zweite Typ kombiniert thermoakustische Emission mit piezoelektrischem Empfang. Dieser Typ besteht aus einer Titan-Elektrode auf geladenem zellulärem Polypropylen, das als piezoelektrischer Empfänger dient. Zelluläres Polypropylen ist mit einem Elastizitätsmodul von ca. 1 MPa bei 250 kHz an die Luft sehr gut angepasst. Der dritte Wandlertyp ist ein Wandler mit elektrostatischen Gasentladung unter Atmosphärendruck. Mit dem fokussierenden thermoakustischen Sender (Typ 1) und einem Polypropylen-Empfänger ist eine Durchschallung einer 4 mm dicken Platte aus carbonfaserverstärktem Kunststoff gelungen. Künstliche Delaminationen mit der Größe 1 mm wurden detektiert. Derselbe Sender kombiniert mit einem Laser-Doppler-Vibrometer als Empfänger wurden für die Prüfung von einem Testkörper aus PMMA mit einseitigem Zugang eingesetzt. Der Wandler bestehend aus einem thermoakustischen Sender auf einem Polypropylen-Empfänger (Typ 2) wurde für die Profilvermessung eines Stufenkeils eingesetzt. Dabei wurden Flachbodenbohrungen mit einem Durchmesser 1 mm abgebildet. Mit diesen beiden Sendern wurde ein Schalldruckpegel über 140dB im Fokus gemessen. Der Wandler mit der Funkenentladung (Typ 3) wurde für die Charakterisierung von Luftultraschallwandlern eingesetzt. Auf Basis dieses Entladungstyps wurde ein Schalldruckpegel über 160dB an einem Abstand von 150 mm gemessen, was deutlich über dem Schallpegel aller bekannten Luftultraschall-Wandler liegt. Die größte Bandbreite von deutlich über 100% der Mittenfrequenz wurde mit dem Wandler Typ 1 erreicht. So große Bandbreiten ermöglichen neue Anwendungen für Luftultraschallwandler, insbesondere wenn kombiniert mit Signalverarbeitungsalgorithmen. T2 - Workshop des Fachausschusses Ultraschall der DEGA e.V. „Schallfeldbasierte Messverfahren - vom Transducer bis zur praktischen Anwendung“ CY - Kloster Drübeck, Germany DA - 11.07.2017 KW - Thermoakustik KW - Ultraschall KW - Wandler KW - Luftultraschall KW - Transducer PY - 2017 AN - OPUS4-41195 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Neuartige Wandler für Luftultraschallprüfung N2 - In diesem Vortrag wurde eine Übersicht über die aktuelle Forschung im Gebiet des Luftultraschalls gegeben. Insbesondere wurden Luftultraschall-Wandler vorgestellt, die nicht wie marktübliche Wandler auf Basis von Piezokeramik gebaut werden, sondern auf anderen Prinzipien basieren. Ferroelektret-Wandler und thermoakustische Wandler werden vorgestellt, sowie Wandler, die auf einer Kombination von diesen zwei Prinzipien basieren. T2 - Sitzung des Arbeitskreises Saarbrücken der DGZfP CY - Saarbrücken, Germany DA - 22.06.2017 KW - Luftultraschall KW - Wandler KW - Ferroelektret KW - Thermoakustik KW - Prüfung PY - 2017 AN - OPUS4-41196 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Fischer, Franziska A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - The effect of the ball to reactant ratio on mechanochemical reaction times studied by in situ PXRD N2 - The effect of the reactant powder mass on reaction times for the mechanochemical formation of a soft matter model system was studied by in situ PXRD. The syntheses were performed at a constant ball mass in a shaker mill with and without glassy SiO2 as an inert additive. Reaction times decreased with the increase of the ball to reactant ratio (BRR). The kinetic influence of the SiO2 powder was excluded. The decrease in the reaction time with decreasing mass of reactants was related to the rise in the stress energy transferred to the powder by a higher ball impact. The BRR had no effect on the induction time. But the product conversion was accelerated by raising the BRR. While a certain temperature is needed for the activation of reactants in the induction phase, the conversion of soft matter reactants is rather controlled by impact than temperature. KW - XRD KW - Mechanochemistry PY - 2017 UR - http://pubs.rsc.org/en/content/articlehtml/2017/ce/c7ce00502d DO - https://doi.org/10.1039/c7ce00502d VL - 19 IS - 28 SP - 3902 EP - 3907 AN - OPUS4-41197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schlegel, Moritz-Caspar A1 - Svetogorov, R. T1 - Crystal structure refinements - Rietveld Method N2 - The talk is an introduction into the Rietveld method and basic aspects concerning powder diffraction analysis. The FOX- and Jana software are explained stepwise which should enable the audiences of the talk to start structure refinements by their own. T2 - Neutron Scattering Application to Hydrogen Storage Materials CY - Berlin, Germany DA - 07.08.2017 KW - Rietveld KW - Refinement KW - FOX KW - Jana2006 PY - 2017 AN - OPUS4-41345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe T1 - ALD-Haftvermittler zur Erhöhung der Haft- bzw. Klebfestigkeit N2 - Zur Erhöhung der Haft- und Klebfestigkeit von Niedrigenergie-Polymeren wie PTFE, PP und PE werden plasmabasierte Aktivierungen (Realisierung von dangling bonds) und Modifizierungen (Realisierung von functional groups) verwendet. Die Effizienz dieser Modifizierungen liegt für technisch raue Oberflächen bei ca. 10%, d. h. nur jedes zehnte C-Atom wird aktiviert oder modifi-ziert, weil sowohl LP- (Low Pressure) als auch AP- (Atmospheric Pressure) Plasmen nicht topo-graphietreu wirksam werden. Zudem ist die Lebensdauer der Aktivierung bzw. Modifizierung oft sehr kurz, liegt im Bereich von wenigen Minuten bis zu mehreren Stunden, d.h. zeitnahe Beschich-tung oder Verklebung in Prozessfolge sind unabdingbar. Im Projekt „HARFE - Haftung, Reproduzierbarkeit, Festigkeit“ soll untersucht werden, in wie weit diese Defizite mittels Atomlagenabscheidung (ALD: Atomic Layer Deposition) vorbeschichteten Polymeren minimiert werden können. ALD-Prozesse sind zum einen topographietreu, zum anderen sowohl ohne als auch mit Plasmaunterstützung realisierbar. T2 - 12. Thementage Grenz- und Oberflächentechnik (ThGOT) und das 5. Kolloquium Dünne Schichten in der Optik CY - Zeulenroda, Gemany DA - 14.03.2017 KW - ALD-Prozess KW - ALD Haftvermittler KW - Haftfestigkeit KW - Klebefestigkeit KW - Verbundfestigkeit KW - Zentrifugentechologie KW - Mehrprobenprüfung PY - 2017 AN - OPUS4-41352 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Marc Benjamin A1 - Susann, Meyer A1 - Schröter, Maria-Astrid A1 - Kunte, Hans-Jörg A1 - Solomun, Tihomir A1 - Sturm, Heinz T1 - DNA protection by ectoine from ionizing radiation: molecular mechanisms N2 - Ectoine, a compatible solute and osmolyte, is known to be an effective protectant of biomolecules and whole cells against heating, freezing and extreme salinity. Protection of cells (human keratinocytes) by ectoine against ultraviolet radiation has also been reported by various authors, although the underlying mechanism is not yet understood. We present the first electron irradiation of DNA in a fully aqueous environment in the presence of ectoine and at high salt concentrations. The results demonstrate effective protection of DNA by ectoine against the induction of single-strand breaks by ionizing radiation. The effect is explained by an increase in low-energy electron scattering at the enhanced free-vibrational density of states of water due to ectoine, as well as the use of ectoine as an ˙OH-radical scavenger. This was demonstrated by Raman spectroscopy and electron paramagnetic resonance (EPR). KW - Ectoine KW - DNA KW - Radiation protection KW - Ionizing radiation KW - Compatible solute KW - Biomolecules KW - Sodium chloride KW - Aqueous solution KW - Hydroxyectoine KW - Raman spectroscopy KW - Electron irradiation KW - Cancer KW - Radical scavenger KW - Low energy electrons KW - Hydroxyl radical KW - OH-radical KW - Ectoin KW - UV radiation KW - Sun KW - Salt KW - Radiation therapy PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-419332 UR - http://pubs.rsc.org/en/content/articlehtml/2017/cp/c7cp02860a DO - https://doi.org/10.1039/C7CP02860A SN - 1463-9076 VL - 19 IS - 37 SP - 25717 EP - 25722 PB - Royal Society of Chemistry CY - United Kingdom AN - OPUS4-41933 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Voigt, Gerrit T1 - Determining moisture in materials and IoT N2 - Knowing the state of the setting process of concrete in buildings or the moisture level of old walls can be crucial in determining further steps in the construction or restoration process. Small 2.4 GHz modules can be either embedded or applied on the surface to determine the moisture distribution in material. Common modules, that are based on the highly available Bluetooth Low Energy standard, emit electromagnetic waves, whose signal strength gets dampened by water molecules. This effect serves as the basis on determining the moisture level in material. We will show how to apply this method in a meshed sensor network for online monitoring. T2 - SMAR2017 CY - Zurich, Switzerland DA - 13.09.2017 KW - Moisture KW - Concrete KW - Radio signals KW - Bluetooth PY - 2017 SP - Paper 152, 1 EP - 6 CY - Zürich, Switzerland AN - OPUS4-41997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ricci, M. A1 - Shegunova, P. A1 - Conneely, P. A1 - Becker, Roland A1 - Torres, M. M. A1 - Osuna, M. A. A1 - On, T.P. A1 - Man, L.H. A1 - Baek, S.-Y. A1 - Kim, B. A1 - Hopley, C. A1 - Liscio, C. A1 - Warren, J. A1 - Le Diouron, V. A1 - Lardy-Fontan, S. A1 - Lalere, B. A1 - Mingwu, S. A1 - Kucklick, J. A1 - Vamathevan, V. A1 - Matsuyama, S. A1 - Numata, M. A1 - Brits, M. A1 - Quinn, L. A1 - Fernandes-Whaley, M. A1 - Gören, A.C. A1 - Binici, B. A1 - Konopelko, L. A1 - Krylov, A. A1 - Mikheeva, A. T1 - CCQM-K102: Polybrominated diphenyl ethers in sediment N2 - The key comparison CCQM-K102: Polybrominated diphenyl ethers in sediment was coordinated by the JRC, Directorate F - Health, Consumers & Reference Materials, Geel (Belgium) under the auspices of the Organic Analysis Working Group (OAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM). Thirteen National Metrology institutes or Designated Institutes and the JRC participated. Participants were requested to report the mass fraction (on a dry mass basis) of BDE 47, 99 and 153 in the freshwater sediment study material. The sediment originated from a river in Belgium and contained PBDEs (and other pollutants) at levels commonly found in environmental samples. The comparison was designed to demonstrate participants' capability of analysing non-polar organic molecules in abiotic dried matrices (approximate range of molecular weights: 100 to 800 g/mol, polarity corresponding to pKow < −2, range of mass fraction: 1–1000 μg/kg). All participants (except one using ultrasonic extraction) applied Pressurised Liquid Extraction or Soxhlet, while the instrumental analysis was performed with GC-MS/MS, GC-MS or GC-HRMS. Isotope Dilution Mass Spectrometry approach was used for quantification (except in one case). The assigned Key Comparison Reference Values (KCRVs) were the medians of thirteen results for BDE 47 and eleven results for BDE 99 and 153, respectively. BDE 47 was assigned a KCRV of 15.60 μg/kg with a combined standard uncertainty of 0.41 μg/kg, BDE 99 was assigned a KCRV of 33.69 μg/kg with a combined standard uncertainty of 0.81 μg/kg and BDE 153 was assigned a KCRV of 6.28 μg/kg with a combined standard uncertainty of 0.28 μg/kg. The k-factor for the estimation of the expanded uncertainty of the KCRVs was chosen as k = 2. KW - Intercomparison KW - Traceability KW - Nation metrology institutes PY - 2017 DO - https://doi.org/10.1088/0026-1394/54/1A/08026 SN - 0026-1394 SN - 1681-7575 VL - 54 SP - 08026, 1 EP - 82 AN - OPUS4-41998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Voigt, Gerrit T1 - Determining moisture in materials and IoT N2 - Knowing the state of the setting process of concrete in buildings or the moisture level of old walls can be crucial in determining further steps in the construction or restoration process. Small 2.4 GHz modules can be either embedded or applied on the surface to determine the moisture distribution in material. Common modules, that are based on the highly available Bluetooth Low Energy standard, emit electromagnetic waves, whose signal strength gets dampened by water molecules. This effect serves as the basis on determining the moisture level in material. We will show how to apply this method in a meshed sensor network for online monitoring. T2 - Fourth Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures CY - Zurich, Switzerland DA - 13.09.2017 KW - Moisture KW - Concrete KW - Radio signals KW - Bluetooth PY - 2017 AN - OPUS4-41999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Akhmetova, Irina T1 - In situ investigation of mechanochemical syntheses of manganese phosphonates N2 - The exploration of metal phosphonates chemistry has gained great interest during the last decades, because of their structural diversity. Transition metal phosphonates are promising candidates for an application as electrocatalysts in oxygen reduction reactions (ORR). Here, we present the in situ investigation of mechanochemical syntheses of two different manganese phosphonates by synchrotron X-ray diffraction. Nitrilotri(methylenephosphonic acid) and N,N-Bis(phosphonomethyl)glycine were chosen as ligands. The liquid-assisted milling process can be divided into three steps, including an amorphous stage. One of the products has not been obtained by classical solution chemistry before. These metal phosphonates and/or their derivatives are considered to be active in electrochemical energy conversion. The verification of their applicability is one of the topics of our resent research. T2 - 9th International Conference on Mechanochemistry and Mechanical Alloying CY - Kosice, Slovakia DA - 03.09.2017 KW - Mechanochemistry KW - In situ KW - Metal phosphonate KW - XRD PY - 2017 AN - OPUS4-41920 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Häusler, Ines A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Palasse, L. A1 - Dirscherl, K. T1 - Characterization of porous, TiO2 nanoparticle films using on-axis TKD in SEM – a new nano-analysis tool for a large-scale application N2 - A combined methodical approach is tested with respect to the characterization of the inner structure of porous TiO2 layers as typically used in modern dye sensitized solar cells (DSSC). Their performance is directly linked to the surface area of the pore network. The micrometer thick layer employed was manufactured by screen-printing of a starting TiO2 powder constituted of shape-controlled, bipyramidal anatase nanoparticles on FTO/glass substrates. The analytical methods exploited in our study are Focused Ion Beam (FIB) slicing followed by 3D reconstruction as well as the new approach transmission Kikuchi diffraction (TKD) technology in the scanning electron microscope (SEM). Size and shape distribution of the TiO2 NPs within the layer can be extracted. SEM in transmission mode and atomic force microscopy (AFM) have been used to verify the dimensional data obtained by the new combined methodical approach. Its analytical benefits but also the challenges and limitations are highlighted. KW - TiO2 KW - TKD KW - Particle size distribution KW - Nanoparticles KW - Porous film PY - 2017 UR - https://www.cambridge.org/core/services/aop-cambridge-core/content/view/8A8B29335A2F4D0CB6922F6F5A19C5DC/S1431927617003397a.pdf/characterization_of_porous_tio2_nanoparticle_films_using_onaxis_tkd_in_sem_a_new_nanoanalysis_tool_for_a_largescale_application.pdf DO - https://doi.org/10.1017/S1431927617003397 VL - 23 IS - S1 (July) SP - 542 EP - 543 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-41924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Oswald, F. A1 - Narbey, S. A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Complementary methodical approach for the analysis of a perovskite solar cell layered system N2 - Loss in efficiency of perovskite solar cells may be caused by structural and/or chemical alterations of the complex layered system. SEM/EDX combined with XPS were chosen as appropriate methodical approach to characterise perovskite laboratory cells in depth and complementary on top, before and after light exposure. The layered perovskite system investigated here is based on glass covered with fluorine doped tin oxide (FTO), followed by three porous thin films of TiO2, ZrO2 and a thick monolithic carbon. This layered system serves as the matrix for the perovskite. After infiltration of perovskite solution and annealing, EDX spectral maps on cross-sections of the specimen have been measured. The distribution of relevant elements – Si, Sn, Ti, Zr and C – correlates conclusively with layers visible in the acquired SEM images. Lead and iodine are distributed throughout the porous layers C, ZrO2 and TiO2. By EDX it was found that several weeks of ambient daylight did not change significantly the qualitative elemental composition of lead and iodine throughout the solar cell system. It was confirmed with EDX that nanoparticles identified in high-resolution SEM micrographs contain mainly Pb and I, indicating these to be the perovskite crystals. However, a time-dependent compositional and chemical altering was observed with XPS for the near-surface region of the outermost ~10 nm after two months of illumination. KW - Pervskite solar cells KW - TiO2 KW - Porous layer KW - SEM/EDX KW - XPS PY - 2017 UR - https://www.cambridge.org/core/services/aop-cambridge-core/content/view/0E9E937542BC8B5535900B53B7F667E9/S1431927617010558a.pdf/complementary_methodical_approach_for_the_analysis_of_a_perovskite_solar_cell_layered_system.pdf DO - https://doi.org/10.1017/S1431927617010558 VL - 23 IS - S1 (July) SP - 1978 EP - 1979 PB - Cambridge University Press CY - New York, NY, U.S.A. AN - OPUS4-41925 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hübert, Thomas A1 - Majewski, Jacek T1 - Transient response time measurement of hydrogen sensors N2 - The efficiency of gas sensor application for facilitating the safe use of hydrogen depends considerably on the sensor response to a change in hydrogen concentration. Therefore, the response time has been measured for five different-type commercially available hydrogen sensors. Experiments showed that all these sensors surpass the ISO 26142 standard; for the response times t90 values of 2 s to 16 s were estimated. Results can be fitted with an exponential or sigmoidal function. It can be demonstrated that the results on transient behaviour depend on both the operating parameters of sensors and investigation methods, as well as on the experimental conditions: gas change rate and concentration jump. T2 - 7th International Conference on Hydrogen Safety (ICHS 2017) CY - Hamburg, Germany DA - 11.09.2017 KW - Response time measurement KW - Sensor characteristics KW - Hydrogen sensors PY - 2017 AN - OPUS4-41928 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Caldeira, Rui A1 - Bartusch, Jürgen A1 - Kupnik, M. T1 - Air-coupled ultrasonic ferroelectret receiver with additional DC voltage N2 - Highly sensitive air-coupled ultrasonic sensors are essential for various applications such as testing of composite materials. One of the major challenges for the development of air-coupled ultrasonic sensors is the impedance matching to air. With a lower acoustic impedance than the usual piezoelectric materials, charged cellular polypropylene film (cPP) offers better matching to air with a similar piezoelectric coefficient. The piezoelectric behaviour demonstrated by cPP comes from polarized air cells that create a permanent internal voltage. The sensitivity of the sensor varies with the application of an additional DC bias voltage. Thus, this work presents a cPP ultrasonic sensor with an improvement of up to 15 ± 1 dB on the signal-to-noise ratio. T2 - Eurosensors 2017 CY - Paris, France DA - 3.9.2017 KW - Ultrasonic KW - Air-coupled KW - Cellular polypropylene KW - Transducer KW - Ferroelectret PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-419009 DO - https://doi.org/10.3390/proceedings1040362 VL - 1 IS - 4 SP - Article 362, 1 EP - 4 AN - OPUS4-41900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Air-coupled ultrasonic ferroelectret receiver with additional DC voltage N2 - Highly sensitive air-coupled ultrasonic sensors are essential for various applications such as testing of composite materials. One of the major challenges for the development of air-coupled ultrasonic sensors is the impedance matching to air. With a lower acoustic impedance than the usual piezoelectric materials, charged cellular polypropylene film (cPP) offers better matching to air with a similar piezoelectric coefficient. The piezoelectric behaviour demonstrated by cPP comes from polarized air cells that create a permanent internal voltage. The sensitivity of the sensor varies with the application of an additional DC bias voltage. Thus, this work presents a cPP ultrasonic sensor with an improvement of up to 15 ± 1 dB on the signal-to-noise ratio. T2 - Eurosensors 2017 CY - Paris, France DA - 3.9.2017 KW - Ultrasonic KW - Ferroelectret KW - Transducer KW - Air-coupled KW - Cellular polypropylene PY - 2017 AN - OPUS4-41901 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertin, Annabelle T1 - Upper critical solution temperature (UCST)- type thermoresponsive polymers from acrylamide-based monomers N2 - UCST-type thermoresponsive polymers that phase separate from solution upon cooling present a tremendous potential not only in aqueous media where they can be used in drug delivery, diagnostic and microfluidic applications, but also in water/alcohol mixtures, where they can be used for instance in sensing systems for alcohol-soluble drugs. However, only a few thermoresponsive polymers have been reported that present an UCST in a relevant temperature range and “green” solvents such as water or ethanol. In this context, acrylamide-based monomers can be very useful building blocks for designing novel UCST-type polymers because of their hydrophilic nature (with the right side chain) and propensity to form hydrogen bonds. We want to present our latest results on the copolymer poly(acrylamide-co-acrylonitrile) (P(AAm-co-AN)) that present a UCST in water as well as on two homopolymers based on an acrylamide derivative of 2,6-diaminopyridine, namely poly(N-(6-aminopyridin-2-yl)acrylamide) (PNAPAAm) and poly(N-(6-acetamidopyridin-2-yl)acrylamide) (PNAcAPAAm) that show UCST-type thermoresponsiveness in water/alcohol mixtures. Our focus for P(AAm-co-AN)) is its aggregation behaviour above and below its phase transition temperature as the size of thermoresponsive polymeric systems is of prime importance for biomedical applications (as size dependent processes take place in the body) and is linked to the optical properties of a material that matter in materials science. In the case of PNAPAAm and PNAcAPAAm, we focused on the co-solvency/co-non solvency effect on the phase transition temperature in water/alcohol mixture. Indeed, polymers with UCST behavior below 60°C in water/alcohol mixtures are extremely promising for the preparation of “smart” materials for sensing. T2 - 31st Conference of the European Colloid and Interface Society (ECIS 2017) CY - Madrid, Spain DA - 03.09.2017 KW - Thermoresponsive polymers KW - UCST polymers KW - Acrylamide based polymers PY - 2017 AN - OPUS4-41902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Quantitative online NMR spectroscopy for industrial reaction and process monitoring N2 - Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction and process control. An increasing number of applications are reported. Robust field integration of NMR systems have to face explosion protection or integration into process control systems with short set-up times. Tis paves the way for industrial automation in real process environments. Automated data preparation and analysis are cornerstones for a breakthrough of NMR techniques for process control. Particularly, robust chemometrics as well as automated signal processing methods have to be (further) developed especially for NMR spectroscopy in process control. This becomes even more important for so called “smart sensors” providing the basis for the future project “Industrie 4.0”, and Industrial Internet of Things (IIoT), along with current requirements to process control, model based control, or soft sensing. Data analysis techniques are available but currently mostly used for off-line data analysis to detect the causes of variations in the product quality. T2 - Syngenta Face to Face Meeting Process Analytical Technology CY - Münchwilen, Switzerland DA - 12.09.2017 KW - Process monitoring KW - Online NMR spectroscopy KW - Reaction monitoring KW - Hydroformylation KW - Gas analysis KW - CONSENS KW - Indirect hard modeling PY - 2017 AN - OPUS4-41946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Design and validation of a compact online NMR module N2 - Monitoring chemical reactions is the key to process control. Today, mainly optical online methods are applied, which are calibration intensive. NMR spectroscopy has a high potential for direct loop process control while cutting the calibration and validation needs to an minimum and thus exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environments for advanced process monitoring and control. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. Data analysis techniques are available but currently mostly used for off-line data analysis to detect the causes of variations in the product quality. This is addressed within the EU’s Research Project CONSENS by the development and integration of a smart NMR module for process monitoring. The presented NMR module is provided in a mobile explosion proof housing and involves a compact spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction), and evaluation. Such “smart sensors” provide the basis for the future project “Industrie 4.0”, and Industrial Internet of Things (IIoT), along with current requirements to process control, model based control, or soft sensing. The module transforms the acquired online spectra of various technically relevant reactions to either conventional 4‒20 mA signals as well as WiFi based OPC-UA communication protocols, which enables NMR-based advanced process control and funny discussions with plant managers along with automation and safety engineers. T2 - Small Molecule NMR Conference (SMASH) CY - Baveno, Italy DA - 17.09.2017 KW - Online NMR spectroscopy KW - CONSENS KW - Reaction monitoring KW - Process control KW - Process analytical technology KW - Indirect hard modeling KW - Industrie 4.0 KW - Smart sensors KW - SMASH PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-419473 UR - http://www.smashnmr.org/conference/program AN - OPUS4-41947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas T1 - Assessment and validation of various flow cell designs for quantitative online NMR spectroscopy N2 - Compact nuclear magnetic resonance (NMR) instruments make NMR spectroscopy and relaxometry accessible in industrial and harsh environments for reaction and process control. Robust field integration of NMR systems have to face explosion protection or integration into process control systems with short set-up times. This paves the way for industrial automation in real process environments. The design of failsafe, temperature and pressure resistant flow through cells along with their NMR-specific requirements is an essential cornerstone to enter industrial production plants and fulfill explosion safety requirements. NMR-specific requirements aim at full quantitative pre-magnetization and acquisition with maximum sensitivity while reducing sample transfer times and dwell-times. All parameters are individually dependent on the applied NMR instrument. Luckily, an increasing number of applications are reported together with an increasing variety of commercial equipment. However, these contributions have to be reviewed thoroughly. The performance of sample flow cells commonly used in online analytics and especially for low-field NMR spectroscopy was experimentally and theoretically investigated by 1H-NMR experiments and numerical simulations. Here, we demonstrate and discuss an automated test method to determine the critical parameters of flow through cells for quantitative online NMR spectroscopy. The setup is based on randomized setpoints of flow rates in order to reduce temperature related effects. Five flow cells and tubings were assessed and compared for high-field as well as low-field NMR spectrometers. T2 - Small Molecule NMR Conference (SMASH) CY - Baveno, Italy DA - 17.09.2017 KW - Online NMR spectroscopy KW - Reaction monitoring KW - Flow cell KW - Process control KW - SMASH PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-419485 UR - http://www.smashnmr.org/conference/program AN - OPUS4-41948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Reading between the lines – Automated data analysis for low field NMR spectra N2 - For reaction monitoring and process control using NMR instruments, in particular, after acquisition of the FID the data needs to be corrected in real-time for common effects using fast interfaces and automated methods. When it comes to NMR data evaluation under industrial process conditions, the shape of signals can change drastically due to nonlinear effects. Additionally, the multiplet structure becomes more dominant because of the comparably low-field strengths which results in overlapping of multiple signals. However, the structural and quantitative information is still present but needs to be extracted by applying predictive models. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modeling). By using the benefits of traditional qNMR experiments data analysis models can meet the demands of the PAT community (Process Analytical Technology) regarding low calibration effort/calibration free methods, fast adaptions for new reactants, or derivatives and robust automation schemes. T2 - Small Molecule NMR Conference (SMASH) CY - Baveno, Italy DA - 17.09.2017 KW - Online NMR spectroscopy KW - Data analysis KW - Chemometrics KW - Indirect hard modeling KW - Spectral modeling KW - Line prediction KW - CONSENS KW - SMASH PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-419498 UR - http://www.smashnmr.org/conference/program AN - OPUS4-41949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mull, Birte A1 - Sauerwald, T. A1 - Schultealbert, C. A1 - Horn, Wolfgang A1 - Brödner, Doris A1 - Richter, Matthias T1 - Reproducibly emitting reference materials for volatile and semi-volatile organic compounds—using finite element modeling for emission predictions N2 - Recent research into emissions of (semi-)volatile organic compounds [(S)VOC] from solid materials has focused on the development of suitable reference materials for quality assurance/quality control of emission test chamber measurements, which fulfill requirements such as homogenous and reproducible (S)VOC release. The approach of this study was to find a method for preparation of a material with predictable (S)VOC emission rates. AVOC (styrene) and an SVOC (2,6-diisopropylnaphthalene, DIPN), loaded into either vacuum grease or a 1:1 mixture of paraffin/squalane, have been tested. For the prediction of the emission rates, a model using the finite element method (FEM) was created to simulate the (S)VOC emission profiles. Theoretical and experimental results obtained in a Micro-Chamber/Thermal Extractor (μ-CTE™) and in 24 L emission test chamber measurements were in good agreement. Further properties were investigated concerning the material applicability, such as shelf life and inter-laboratory comparability. The maximum relative standard deviation in the inter-laboratory study was found to be 20%. KW - Emitting reference material KW - Emission test chamber KW - Micro-chamber KW - FEM model PY - 2017 DO - https://doi.org/10.1007/s11869-017-0508-6 SN - 1873-9318 SN - 1873-9326 VL - 10 IS - 10 SP - 1237 EP - 1246 PB - Springer Science+Business Media B.V. AN - OPUS4-41951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lehmann, Jens A1 - Leonhard, H. T1 - Unsichtbares sichtbar machen - Oberflächenschnelltest auf Korrosionsgefahr N2 - Eine Passivschicht schützt die Oberfläche nichtrostender Stähle vor Materialauflösung. Sie darf nicht unvollständig oder beschädigt sein. Sonst drohen Schadensfälle durch Korrosion an Rohrsystemen und Behältern. TÜV SÜD Chemie Service zeigt ein von der Bundesanstalt für Materialforschung und -prüfung (BAM) entwickeltes Verfahren zur Überprüfung der Passivschicht. Der Test nimmt nur 15 Minuten in Anspruch. KW - Nichtrostender Stahl KW - Korrosionsschnelltest KW - KorroPad KW - Passivschicht PY - 2017 SN - 1436-2597 VL - 20 IS - 9 SP - 53 EP - 54 PB - Wiley-VCH Verlag GmbH & Co. KGaG CY - Weinheim AN - OPUS4-41911 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kratzig, Andreas A1 - Le, Quynh Hoa T1 - Korrosion von Stählen in flüssigen und überkritischen CO2–Strömen unter realitätsnahen Bedingungen N2 - CCUS-Technologie gilt als eine vielversprechende Methode zur Abschwächung des Beitrags von fossilen Emissionen zur globalen Erwärmung. Dabei wird das in den Verbrennungsprozessen entstandene Treibhausgas aufgefangen, zu verschiedenen Lagerstätten transportiert und langzeitig gespeichert bzw. einer chemischen Nutzung zugeführt. CO2-Transport-Pipelines sind potentiell gefährdet, wenn sie korrosiven Begleitstoffen des CO2-Stroms, wie SOx, NOx bei einem hohen Wasserdampfanteil ausgesetzt sind. Screening-Tests zeigten, dass bei einer Konzentration von 1000 ppmv H2O die Reaktionen und Kondensation von SO2 und NO2 mit O2 und H2O zu Säuretropfen (pH ~ 0,5) auf der Oberfläche von Metall-Prüfkörpern und Gefäßen führen. Die Werkstoffe 1.4313 1.8977 und 1.4562 wurden in CO2-Atmosphäre mit unterschiedlichen Verhältnissen der säurebildenden Komponenten SO2, NO2, H2S mit H2O untersucht. Diese Studien zeigten grundsätzlich den Mechanismus sowie die Rolle jedes CO2-Strom-Begleitstoffes auf den Korrosionsprozess. T2 - CLUSTER-Projektreffen CY - Halle/Wittenberge, Germany DA - 02.03.2017 KW - Korrosion KW - Pipeline-Transport KW - Säurekondensation KW - CLUSTER PY - 2017 AN - OPUS4-41917 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kratzig, Andreas A1 - Le, Quynh Hoa A1 - Bettge, Dirk A1 - Bäßler, Ralph A1 - Kranzmann, Axel ED - EUROCORR, T1 - Interaction of oxidizing and reductive components in CO2 fluids in transport pipelines at low and high pressure and low temperature N2 - Carbon Capture Utilization and Storage (CCUS) is a promising technology for the reduction of CO2 emissions, e.g. from fossil-fuel operated power plants or cement mills. Crucial points for a sustainable and future-proof CCUS procedure are reliability and cost efficiency of the pipeline transport network. Due to the absence of certified benchmarks for upper limits, systematic experiments with impurities in the CO2 stream were carried out. For oxidation processes SO2 and NO2 acted as corrosive components, and for reductive atmosphere H2S. Carbon steel L485MB (pipeline), martensitic steel 1.4313 (compression) and austenitic steel 1.4562 (injection) were selected as specimens. Experiments were performed at 0 bar or 100 bar and within a temperature range 278 K ≤ T ≤ 313 K. High-alloyed Cr-Ni steels revealed no corrosion (1.4562, 1.4313), while for carbon steel considerable corrosion was observed. The type and intensity of corrosion was strongly coupled with the applied corrosive species and the level of humidity in the CO2 stream, leading to different compositions of acidic condensates. Applying a reducing atmosphere results in very little corrosion rates, but provokes pitting corrosion. In contrast, oxidizing or mixed settings lead to a clearly increased growth of the corrosion layer, but exhibit shallow uniform corrosion. Exceptional nitric acid results in intergranular corrosion. Investigations on the specimens were carried out by optical microscopy, XRD, SEM/EDX, and AAS/IC. T2 - EUROCORR 2017 CY - Prague, Czech Republic DA - 03.09.2017 KW - CCS KW - Pipeline transport KW - CO2 corrosion KW - Carbon steels KW - Condensation PY - 2017 SP - Paper 80181, 1 EP - 4 AN - OPUS4-41918 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kratzig, Andreas T1 - Interaction of oxidizing and reductive components in CO2 fluids in transport pipelines (X70) at low temperature N2 - Carbon Capture Utilization and Storage (CCUS) is a promising technology for the reduction of CO2 emissions, e.g. from fossil-fuel operated power plants or cement mills. Crucial points for a sustainable and future-proof CCUS procedure are reliability and cost efficiency of the pipeline transport network. Due to the absence of certified benchmarks for upper limits, systematic experiments with impurities in the CO2 stream were carried out. For oxidation processes SO2 and NO2 acted as corrosive components, and for reductive atmosphere H2S. Carbon steel L485MB (pipeline), martensitic steel 1.4313 (compression) and austenitic steel 1.4562 (injection) were selected as specimens. Experiments were performed at 1 bar or 100 bar and within a temperature range 278 K ≤ T ≤ 313 K. High-alloyed Cr-Ni steels revealed no corrosion (1.4562, 1.4313), while for carbon steel considerable corrosion was observed. The type and intensity of corrosion was strongly coupled with the applied corrosive species and the level of humidity in the CO2 stream, leading to different compositions of acidic condensates. Applying a reducing atmosphere results in very little corrosion rates, but provokes pitting corrosion. In contrast, oxidizing or mixed settings lead to a clearly increased growth of the corrosion layer, but exhibit shallow uniform corrosion. Exceptional nitric acid results in intergranular corrosion. T2 - EUROCORR 2017 CY - Prague, Czech Republic DA - 03.09.2017 KW - CCS KW - Pipeline transport KW - CO2 corrosion KW - Condensation KW - Carbon steel PY - 2017 AN - OPUS4-41919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, Katrin T1 - New NIR fluorescence reference materials and quantum yield standards for standardization of fluorescence-based measurements N2 - Luminescence techniques are amongst the most commonly used analytical methods in the life and the material sciences due to their sensitivity and nondestructive character. All photoluminescence signals are, however, affected by wavelength-, polarization- and time-dependent instrument-related effects. Furthermore, substantial challenges to measure absolute luminescence intensities complicate the comparison of data recorded with different instruments and on the same instrument at different times. These problems can be easily resolved with fluorescence standards used for instrument performance validation (IPV) and determination of instrument-to-instrument variations, which allow to measure, quantify, and monitor the wavelength-dependent spectral responsivity for typically used instrument settings. For example, a set of liquid fluorescence standards, the BAM Kit F001-F005, and a ready-to-use glass-based fluorescence standard BAM F-012 developed and certified by BAM enable the characterization of many fluorescence parameters in the UV/vis wavelength range. For the increasingly used near infrared (NIR) region, standards and calibration tools are still very rare. Reliable spectral fluorescence standards and intensity or quantum yield standards are currently not available for the NIR, even though in biology, molecular imaging, and clinical diagnostics fluorescence labels absorbing and emitting in the long wavelength region beyond 650 nm are being increasingly used. This limitation hampers the reliability and comparability of fluorescence measurements in the NIR and calls for simple fluorescence standards for instrument characterization and for the quantification of fluorescence intensities and efficiencies to improve the comparability of the emission measurements in the NIR. This encouraged us to assess the potential of several NIR-emitting materials as spectral fluorescence standards, thereby extending the BAM Kit from the UV/vis into the NIR up to 950 nm. Moreover, we currently certify quantum yield standards for the UV/vis/NIR to improve the reliability of relative measurements of this spectroscopic key quantity particularly > 650 nm. These tools enable an instrument characterization, signal referencing, quality assurance, traceability, and method validation now also for wavelengths > 650 nm, thereby improving the reliability of fluorescence data in pharmaceutical research, medical and clinical diagnostics, material analysis, and environmental monitoring. T2 - 15th Conference on Methods and Applications in Fluorescence (MAF) CY - Brugge, Belgium DA - 10.09.2017 KW - Fluorescence reference materials KW - Quantum yield standard KW - Glass-based fluorescence standard PY - 2017 AN - OPUS4-41990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Naresh-Kumar, G. A1 - Vilalta-Clemente, A. A1 - Jussila, H. A1 - Winkelmann, Aimo A1 - Nolze, Gert A1 - Vespucci, S. A1 - Nagarajan, S. A1 - Wilkinson, A. J. A1 - Trager-Cowan, C. T1 - Quantitative imaging of anti-phase domains by polarity sensitive orientation mapping using electron backscatter diffraction N2 - Advanced structural characterisation techniques which are rapid to use, non-destructive and structurally definitive on the nanoscale are in demand, especially for a detailed understanding of extended-defects and their influence on the properties of materials. We have applied the electron backscatter diffraction (EBSD) technique in a scanning electron microscope to non-destructively characterise and quantify antiphase domains (APDs) in GaP thin films grown on different (001)Si substrates with different offcuts. We were able to image and quantify APDs by relating the asymmetrical intensity distributions observed in the EBSD patterns acquired experimentally and comparing the same with the dynamical electron diffraction simulations. Additionally mean angular error maps were also plotted using automated cross-correlation based approaches to image APDs. Samples grown on substrates with a 4° offcut from the [110] do not show any APDs, whereas samples grown on the exactly oriented substrates contain APDs. The procedures described in our work can be adopted for characterising a wide range of other material systems possessing non-centrosymmetric point groups. KW - Polarity KW - Semiconductor KW - Antiphase boundary PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-420167 SN - 2045-2322 VL - 7 SP - Article 10916, 1 EP - 10 AN - OPUS4-42016 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bartoschewitz, R. A1 - Appel, P. A1 - Barrat, J.-A. A1 - Bischoff, A. A1 - Caffee, M.W. A1 - Franchi, I.A. A1 - Gabelica, Z. A1 - Greenwood, R.C. A1 - Harir, M. A1 - Harries, D. A1 - Hochleitner, R. A1 - Hopp, J. A1 - Laubenstein, M. A1 - Mader, B. A1 - Marques, R. A1 - Morlok, A. A1 - Nolze, Gert A1 - Prudêncio, M.I. A1 - Rochette, P. A1 - Ruf, A. A1 - Schmitt-Kopplin, P. A1 - Seemann, E. A1 - Szurgot, M. A1 - Tagle, R. A1 - Wach, R.A. A1 - Welten, K. C. A1 - Weyrauch, M. A1 - Wimmer, K. T1 - The Braunschweig meteorite − a recent L6 chondrite fall in Germany N2 - On April 23rd 2013 at 2:07 a.m., a 1.3 kg meteorite fell in the Braunschweig suburb Melverode (52° 13′ 32.19″ N. 10° 31′ 11.60″ E). Its estimated velocity was 250 km/h and it formed an impact pit in the concrete fall site with a diameter of 7 cm and a depth of 3 cm. Radial dust striae are present around the impact pit. As a result of the impact, the meteorite disintegrated into several hundred fragments with masses up to 214 g. The meteorite is a typical L6 chondrite, moderately shocked (S4) – but with a remarkably high porosity (up to 20 vol%). The meteorite was ejected from its parent body as an object with a radius of about 10–15 cm (15–50 kg). The U,Th-He gas retention age of ∼550 Ma overlaps with the main impact event on the L-chondrite parent body ∼470 Ma ago that is recorded by many shocked L chondrites. The preferred cosmic-ray exposure age derived from production of radionuclides and noble gas isotopes is (6.0 ± 1.3) Ma. KW - Braunschweig meteorite KW - L chondrite KW - Fall reconstruction KW - Petrology and mineralogy KW - Organic matter KW - IR spectroscopy KW - Bulk chemistry KW - Radionuclides KW - Noble gas isotopes KW - Specific heat PY - 2016 DO - https://doi.org/10.1016/j.chemer.2016.10.004 SN - 0009-2819 SN - 1611-5864 VL - 77 IS - 1 SP - 207 EP - 224 AN - OPUS4-42018 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard T1 - Einsatz von mobilen Röntgenuntersuchungsmethoden im Museum - Zwei Fallbeispiele N2 - Zwei Bildhauermodelle aus dem Georg-Kolbe-Museum Berlin standen zur Restaurierung an. Das kleinere, 'Lucino' (1920), 41cm, wurde hochauflösend mit CT gemessen, da mittels CT sowohl der Herstellungsprozeß einer Gipsstatue als auch der innere Zustand, wie Ergänzungen, Klebungen und Armierungen, festgestellt werden können. Aus den CT Bildern ergab sich eine für die vorher vermutete Gipszusammensetzung ungewöhnliche innere Struktur. Mit einer Freihand bedienten Röntgenpistole zur Messung der Röntgenfluoreszenz wurde daraufhin die Zusammensetzung des Materials der Statuette als Terracotta bestimmt. Durch den Einsatz von Helium als Spülmittel konnten auch leichte Materialien nachgewiesen und so eine Unterscheidung zwischen Gips und gebranntem Ton durchgeführt werden. Aus den CT Daten wurde eine virtuelle Darstellung der äußeren Geometrie gewonnen. Ein damit versuchsweise erstelltes Replik (Rapid Prototyping, 3D-Drucker, TU-Berlin) entsprach nicht den Anforderungen des Museums zur Erstellung einer Gußform für eine Bronzekleinserie der Statuette. Die zweite Statue, die 'Große Nacht' (1930) ist mit ihrer Größe von 2,12m und aufgrund des durch korrodierende Metallarmierung verursachten Schadensbildes nicht mehr transportfähig. Eine in-situ Untersuchung mit dem mobilen Tomographen, der in den 1980ern zur Untersuchung von Bäumen gebaut und jetzt mit einem modernen Flachdetektor und einer Röntgenröhre ausgestattet ist, wird vorgestellt. Die Möglichkeiten acder in-situ CT für große Skulpturen werden anhand der Ergebnisse diskutiert. T2 - DGZfP-Jahrestagung 2010 CY - Erfurt, Germany DA - 10.05.2010 KW - Mobile CT KW - Mobile RFA PY - 2010 AN - OPUS4-21316 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dey, Anika A1 - Casperson, Ralf A1 - Pohl, Rainer A1 - Thomas, Hans-Martin T1 - Die Wirbelstromprüfung als Hilfsmittel für die Schieneninstandhaltung N2 - Die zerstörungsfreie Oberflächenprüfung an verlegten Eisenbahnschienen mit Wirbelstrom hat in den letzten Jahren durch ständige Weiterentwicklung und Verifizierung enorm an Bedeutung gewonnen. Es wurde u.a. angestrebt zuverlässige Planungsgrößen für den Einsatz von Instandhaltungsmaßnahmen zu erhalten, durch deren gezielten Einsatz Risswachstum unterbunden werden kann. Die Ursache für das Wachstum von Rissen in der Schiene liegt in der Materialermüdung des Werkstoffes infolge der Betriebsbelastungen im RadSchiene-Kontakt. Nach einer gewissen Beanspruchungsdauer kommt es an den Kontaktflächen der Fahrkante zu einer Kaltverfestigung des Schienenstahls. Durch fortschreitende Verfestigung des kontaktbeanspruchten Oberflächenbereichs der gehärteten Schicht wird der Werkstoff spröde und es bilden sich feine Risse aus. Die Risse wachsen anfangs unter einem flachen Winkel in das Schieneninnere hinein, neigen dann aber ab einem gewissen Stadium dazu in das Innere des Schienenkopfes abzukippen, was im Extremfall zu einem Schienenbruch führen kann. Diese Rollkontaktermüdungsrisse, auch genannt Head Checks, entstehen bevorzugt in der Fahrkante von bogenäußeren Schienen. Die Anwendung der Wirbelstromprüfung an der Schiene wurde bisher zur Ermittlung der Schädigungstiefe dieser Rollkontaktermüdungsrisse eingesetzt. Das Wirbelstromverfahren besitzt die Eigenschaft, sehr empfindlich auf alle Veränderungen der Materialeigenschaften an der Oberfläche zu reagieren. Daher wurde festgestellt, dass sich neben der Detektion von Rissen auch Fehler wie Eindrückungen oder Schlupfwellen, bis hin zu Materialveränderungen durch Schweißen oder Aufhärtungen in der Schienenoberfläche bestimmen lassen. Die Wirbelstromprüfung besitzt daher das Potenzial, mögliche Orte der Entstehung von Ermüdungsrissen in einem extrem frühzeitigen Stadium nachzuweisen. Ziel ist es, die rissgefährdeten Zonen schon im Zustand der Kaltverfestigung zu identifizieren. Dadurch können sich neue Aspekte für die präventive Schieneninstandhaltung ergeben. T2 - DGZfP-Jahrestagung 2010 - Zerstörungsfreie Materialprüfung ZfP in Forschung, Entwicklung und Anwendung CY - Erfurt, Germany DA - 10.05.2010 PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-214813 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-21481 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Einfluss lokaler Aufhärtung ferritischer Stähle auf die Risstiefenbestimmung mit dem Wirbelstromprüfverfahren N2 - Mechanische Belastung wie z. B. der Rollkontakt zwischen den Rollen und Lagerringen eines Wälzlagers oder der Rad-Schiene-Kontakt bei der Eisenbahn führen bei ferritischen Stählen zu einer Aufhärtung der Oberfläche. Die mit der Aufhärtung verbundene Versprödung begünstigt die Entstehung von Ermüdungsrissen. Zur Risstiefenbestimmung mit dem Wirbelstromprüfverfahren werden in der Regel Kalibrierkörper mit künstlichen Testfehlern aus dem Grundwerkstoff des Prüfteils verwendet. Die betriebsbedingte Aufhärtung der Prüfteiloberfläche bleibt bei der Kalibrierung unberücksichtigt. Die lokale Aufhärtung der Oberfläche führt zu einem ortsabhängigen Offset des Wirbelstromsignals in Richtung der Rissanzeigen und somit zu einer Überbewertung der Risstiefe. Bei einzelnen Rissen lässt sich der Effekt kompensieren, in dem das Wirbelstromgerät neben jedem Riss abgeglichen bzw. die Differenz zwischen dem Offset und der Rissanzeige berechnet wird. In der Realität liegen die Ermüdungsrisse jedoch oft so dicht nebeneinander, dass auf Grund der Überlagerung benachbarter Rissanzeigen weder ein Abgleich zwischen den Rissen noch eine Bestimmung des Offsets möglich ist. Finite-Elemente-Berechnungen ermöglichen es, die in der Realität stets kombiniert auftretenden Wirbelstromsignale der Ermüdungsrisse und der Oberflächenaufhärtung getrennt zu simulieren, um Erkenntnisse für eine Verbesserung der Risstiefenbestimmung zu erlangen. T2 - DGZfP-Jahrestagung 2010 Zerstörungsfreie Materialprüfung ZfP in Forschung, Entwicklung und Anwendung CY - Erfurt, Germany DA - 10.05.2010 PY - 2010 AN - OPUS4-21482 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shokouhi, Parisa A1 - Zoëga, Andreas A1 - Wiggenhauser, Herbert T1 - Nondestructive investigation of stress-induced damage in concrete N2 - The changes in the sonic surface wave velocity of concrete under stress were investigated in this paper. Surface wave velocities at sonic frequency range were measured on a prismatic concrete specimen undergoing several cycles of uniaxial compression. The loading was applied (or removed) gradually in predefined small steps (stress-controlled). The surface wave velocity was measured at every load step during both loading and unloading phases. Acoustic Emission (AE) test was conducted simultaneously to monitor the microcracking activities at different levels of loading. It was found that the sonic surface wave velocity is highly stress dependent and the velocity-stress relationship follows a particular trend. The observed trend could be explained by a combination of acoustoelasticity and microcracking theories, each valid over a certain range of applied stresses. Having measured the velocities while unloading, when the material suffers no further damage, the effect of stress and damage could be differentiated. The slope of the velocity-stress curves over the elastic region was calculated for different load cycles. This quantity was normalized to yield a dimensionless nonlinear parameter. This parameter generally increases with the level of induced damage in concrete. KW - Nondestructive testing (NDT) KW - Surface wave velocity KW - Concrete KW - Acoustoelasticity KW - Microcracking PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-215943 UR - http://downloads.hindawi.com/journals/ace/2010/740189.pdf DO - https://doi.org/10.1155/2010/740189 SN - 1687-8094 SN - 1687-8086 VL - 2010 IS - Article ID 740189 SP - 1 EP - 9 PB - Hindawi Publ. Corp. CY - New York, NY, USA AN - OPUS4-21594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pretsch, Thorsten T1 - Review on the functional determinants and durability of shape memory polymers N2 - Shape memory polymers (SMP) belong to the class of stimuli-responsive materials and have generated significant research interest. Their capability to retain an imposed, temporary shape and to recover the initial, permanent shape upon exposure to an external stimulus depends on the "functional determinants", which in simplistic terms, can be divided into structural/morphological and processing/environmental factors. The primary aim of the first part of this review is to reflect the knowledge about these fundamental relationships. In a next step, recent advances in shape memory polymer composites are summarized. In contrast to earlier reviews, studies on the impairment of shape memory properties through various factors, such as aging, compression and hibernation, lubricants, UV light and thermo-mechanical cycling, are extensively reviewed. Apart from summarizing the state-of-the-art in SMP research, recent progress is commented. KW - Shape memory polymer KW - Active polymer KW - Shape memory polymer composite KW - Shape memory properties KW - Functionality KW - Degradation KW - Aging KW - Functional determinants KW - Thermo-mechanical testing KW - Durability PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-217390 UR - http://www.mdpi.com/2073-4360/2/3/120/pdf DO - https://doi.org/10.3390/polym2030120 SN - 2073-4360 VL - 2 IS - 3 SP - 120 EP - 158 PB - MDPI CY - Basel AN - OPUS4-21739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Christina T1 - Modulare Analyse der Zuverlässigkeit von ZfP-Systemen mit dem Werkzeug der Systemtheorie - Eine gute Balance zwischen Sicherheit und Ökonomie N2 - Untersucht wird die Modulare Validierung, die Mechanisierte Durchstrahlungsprüfung und die Wirbelstromprüfung an hoch beanspruchten Teilen aus der Luftfahrt. T2 - DGZfP-JAHRESTAGUNG 2002 CY - Weimar, Germany DA - 06.05.2002 PY - 2002 AN - OPUS4-19972 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lück, S. A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Schmidt, V. T1 - Statistical analysis of tomographic reconstruction algorithms by morphological image characteristics N2 - We suggest a procedure for quantitative quality control of tomographic reconstruction algorithms. Our task-oriented evaluation focuses on the correct reproduction of phase boundary length and has thus a clear implication for morphological image analysis of tomographic data. Indirectly the method monitors accurate reproduction of a variety of locally defined critical image features within tomograms such as interface positions and microstructures, debonding, cracks and pores. Tomographic errors of such local nature are neglected if only global integral characteristics such as mean squared deviation are considered for the evaluation of an algorithm. The significance of differences in reconstruction quality between algorithms is assessed using a sample of independent random scenes to be reconstructed. These are generated by a Boolean model and thus exhibit a substantial stochastic variability with respect to image morphology. It is demonstrated that phase boundaries in standard reconstructions by filtered backprojection exhibit substantial errors. In the setting of our simulations, these could be significantly reduced by the use of the innovative reconstruction algorithm DIRECTT. KW - Tomography KW - Computed tomography KW - Reconstruction algorithm KW - Morphological image analysis KW - Phase boundary KW - Metrology KW - Non-destructive testing PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-210710 DO - https://doi.org/10.5566/ias.v29.p61-77 SN - 1580-3139 SN - 1854-5165 VL - 29 SP - 61 EP - 77 CY - Ljubljana, Slovenia AN - OPUS4-21071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schukar, Vivien T1 - Experimental Validation Technique for Strain Transfer Characterisation of Fibre Bragg Grating based Strain Sensors N2 - This examination deals with the validation faciliy KALFOS and the ESPI reference system. T2 - Photonics 2010, International Conference on Fiber Optics and Photonics CY - Guwahati, India DA - 11.12.2010 PY - 2010 AN - OPUS4-22421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moreira, E.V. A1 - Rabello, J.M.B. A1 - Pereira, M.d.S. A1 - Lopes, R.T. A1 - Zscherpel, Uwe T1 - Digital radiography using digital detector arrays fulfills critical applications for offshore pipelines N2 - Digital radiography in the inspection of welded pipes to be installed under deep water offshore gas and oil pipelines, like a presalt in Brazil, in the paper has been investigated. The aim is to use digital radiography for nondestructive testing of welds as it is already in use in the medical, aerospace, security, automotive, and petrochemical sectors. Among the current options, the DDA (Digital Detector Array) is considered as one of the best solutions to replace industrial films, as well as to increase the sensitivity to reduce the inspection cycle time. This paper shows the results of this new technique, comparing it to radiography with industrial films systems. In this paper, 20 test specimens of longitudinal welded pipe joints, specially prepared with artificial defects like cracks, lack of fusion, lack of penetration, and porosities and slag inclusions with varying dimensions and in 06 different base metal wall thicknesses, were tested and a comparison of the techniques was made. These experiments verified the purposed rules for parameter definitions and selections to control the required digital radiographic image quality as described in the draft international standard ISO/DIS 10893-7. This draft is first standard establishing the parameters for digital radiography on weld seam of welded steel pipes for pressure purposes to be used on gas and oil pipelines. KW - Zerstörungsfreie Prüfung von Schweißnähten KW - Durchstrahlungsprüfung KW - Digitale Radiologie PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-225319 DO - https://doi.org/10.1155/2010/894643 SN - 1687-6172 VL - 2010 IS - Article ID 894643 SP - 1 EP - 7 PB - Hindawi Publ. CY - New York, NY, USA AN - OPUS4-22531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Karrasch, Andrea A1 - Wawrzyn, Eliza A1 - Schartel, Bernhard A1 - Jäger, Christian T1 - Solid-state NMR on thermal and fire residues of bisphenol A polycarbonate/silicone acrylate rubber/bisphenol A bis(diphenyl-phosphate)/(PC(SiR/BDP) and PC/SiR/BDP/zinc borate (PC/SiR/BDP/ZnB) - Part 1: PC charring and the impact of BDP and ZnB N2 - Structural changes in the condensed phase of bisphenol A polycarbonate (containing 0.45 wt% poly (tetrafluoroethylene))/silicone acrylate rubber/bisphenol A bis(diphenyl-phosphate) (PC/SiR/BDP) and PC/SiR/BDP/zinc borate (PC/SiR/BDP/ZnB) during thermal treatment in nitrogen atmosphere and in fire residues were investigated by solid-state NMR. H-1, B-11, C-13 and P-31 NMR experiments using direct excitation with a single pulse and H-1-P-31 cross-polarization (CP) were carried out including 31P(1 H) and C-13{P-31}double-resonance techniques (REDOR: Rotational Echo Double Resonance) on a series of heat-treated samples (580 K-850 K). Because many amorphous phases occur in the solid residues, and solid-state NMR spectroscopy addresses the most important sites carbon, phosphorus and boron, this paper is the key analytical approach for understanding the pyrolysis and flame retarding phenomenon in the condensed phase of PC/SiR/BDP and PC/SiR/BDP/ZnB. For the system PC/SiR/BDP it is shown that (i) at temperatures around 750-770 K (main decomposition step) carbonaceous charring of PC occurs and arylphosphate structures are still present, reacted in part with the decomposing PC; (ii) for higher temperatures from 770 K the phosphorus remaining in the solid phase increasingly converts to amorphous phosphonates and inorganic orthophosphates with a minor amount of crystalline orthophosphates; and (iii) H-1-P-31{H-1} CP REDOR and H-1-C-13{P-31} CP REDOR NMR experiments suggest that the phosphates and phosphonates are bound via oxygen to aromatic carbons, indicating the interaction with the carbonaceous char. When ZnB is added to the system PC/SiR/BDP, (i) ZnB leads to a slightly enhanced PC decomposition for temperatures below 750 K; (ii) alpha-Zn-3(PO4)(2) and borophosphate (BPO4) are formed in small amounts at high temperatures suggesting a reaction between BDP and ZnB during thermal decomposition; and (iii) most of the borate remains in the solid residues, forming an amorphous pure borate network, with the BO3/BO4 ratio increasing with higher temperatures. The NMR data of thermal and fire residues are highly correlated, underlining the importance of this work for understanding the pyrolysis and flame retardancy mechanisms in the condensed phase during the burning of the PC/SiR blends. (C) 2010 Elsevier Ltd. All rights reserved. KW - Flame retardance KW - NMR KW - Polycarbonate (PC) blends KW - Bisphenol-A bis(diphenyl)phosphate (BDP) KW - Zinc borate PY - 2010 DO - https://doi.org/10.1016/j.polymdegradstab.2010.07.034 SN - 0141-3910 SN - 1873-2321 VL - 95 IS - 12 SP - 2525 EP - 2533 PB - Applied Science Publ. CY - London AN - OPUS4-22647 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Buchholz, Uwe T1 - Material Characterisation of Cross-linked Polyethylene (XLPE) and Liquid Silicone Rubber (LSR) by means of Ultrasonic Spectroscopy N2 - For prediction of wave propagation in multilayered structures it is necessary to know the material properties. Important parameters are sound velocity (c) and attenuation ( ). Values found in the literature were not satisfactory mainly due to insufficient accuracy of measured attenuation. Experiments were carried out in Division VI.3 - Durability of Polymers. The ultrasonic test equipment was provided by Divisions VIII.1 - Measurement and Testing Technology; Sensors and VIII.4 - Acoustical and Electromagnetical Methods. T2 - ETG-Kongress 2009, Fachtagung 4: Diagnostik CY - Düsseldorf, Germany DA - 27.10.2009 PY - 2009 AN - OPUS4-20479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schukar, Marcus T1 - Climatic investigations of microstructured polymer optical fibers N2 - - Behaviour of MPOF under climatic influences (e.g. temperature, humidity) is an important criterium for the use of MPOF as sensors or for communication - Different types of MPOF with varying hole structures were tested: I. Multimode MPOF (type 1) II. Graded index MPOF (type 2) T2 - 18th International Conference on Plastic Optical Fibers CY - Sydney, Australia DA - 07.09.2009 PY - 2009 AN - OPUS4-20485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pohl, Rainer A1 - Thomas, Hans-Martin A1 - Casperson, Ralf T1 - Mögliche Fehlerquellen und deren Einflüsse bei der Risstiefenbestimmung mit Wirbelstrom N2 - Mit der Wirbelstromprüfung ist die Bestimmung der Tiefe offener Risse in Metallen prinzipiell möglich und wird auch in unterschiedlichen Anwendungen durchgeführt. Hierbei haben die jeweiligen praktischen Prüfbedingungen jedoch erheblichen Einfluss auf die Qualität der Prüfaussage. Es werden einige grundlegende Effekte erläutert, die bei der Risstiefenbestimmung mit Wirbelstrom zu beachten sind. Ein spezieller Labormessplatz wird unter dem Aspekt möglicher Fehlbewertungen vorgestellt und Schlussfolgerungen für die praktische Anwendung werden gezogen. Anhand praktischer Beispiele aus der Schienenprüfung mit Wirbelstrom werden die Auswirkungen verschiedener Fehlereffekte bei der Risstiefenbestimmung gezeigt. T2 - DGZfP-Jahrestagung 2009 CY - Münster, Deutschland DA - 18.05.2009 KW - Head Check KW - Wirbelstromprüfung KW - Risstiefenbestimmung PY - 2009 SN - 978-3-940283-16-0 IS - DGZfP-BB 115 (Di.2.B.2) SP - 1 EP - 11 AN - OPUS4-20514 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dey, Anika A1 - Casperson, Ralf A1 - Pohl, Rainer A1 - Thomas, Hans-Martin T1 - Die Klassifizierung von Oberflächenfehlern in Schienen mit der Wirbelstromprüfung N2 - Die Rissbildung durch Rollkontaktermüdung, der Materialverschleiß oder die Bildung von Einzelfehlern – aufgrund solcher Schädigungsarten wird die Lebensdauer der Schiene signifikant verkürzt. Mit entsprechenden Methoden der ZfP können diese Schäden an Schienen erkannt und bewertet werden. Ein sehr geeignetes Verfahren zur Feststellung von Schädigungen und Unregelmäßigkeiten in der Oberfläche ist die Wirbelstromprüfung. Die zerstörungsfreie Prüfung der Schienenoberfläche durch das Wirbelstromverfahren wurde ursprünglich zur Detektion von Rollkontaktermüdungsrissen entwickelt. Anhand von Ergebnissen aus zahlreichen Prüfeinsätzen in den letzten Jahren wurde außerdem festgestellt, dass unter anderen auch Fehler wie Squats, Belgrospis, Eindrückungen oder Riffel in den Wirbelstromsignalen erkannt werden können. Aufgrund dieser Erfahrungen ist es möglich geworden, den Oberflächenfehlern in der Schiene ein charakteristisches Wirbelstromsignal zuzuordnen. Somit eröffnet sich die Möglichkeit die Wirbelstromprüfung an Schienen nicht ausschließlich zur Detektion von Rollkontaktermüdungsris-sen zu verwenden, sondern auch zur Feststellung von Einzelfehlern oder Materialveränderungen in der Oberfläche. Zusätzlich besteht das Potential durch Ultraschall erfasste Anzeigen, wie z.B. Schweißnähte, Squats etc. mit der Wirbelstromprüfung zu bestätigen und die Aussagesicherheit und Qualität dieser Prüfmethoden noch zu erhöhen. T2 - DGZfP-Jahrestagung 2009 CY - Münster, Deutschland DA - 18.05.2009 KW - Wirbelstromprüfung KW - Rollkontaktermüdung KW - Schienenfehler KW - Eisenbahnschiene PY - 2009 SN - 978-3-940283-16-0 IS - DGZfP-BB 115 (Di.2.B.3) SP - 1 EP - 9 AN - OPUS4-20512 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pawlowski, Kristin A1 - Schartel, Bernhard A1 - Fichera, Mario Augusto A1 - Jäger, Christian T1 - Flame retardancy mechanisms of bisphenol A bis(diphenyl phosphate) in combination with zinc borate in bisphenol A polycarbonate/Acrylonitrile-butadiene-styrene blends N2 - Bisphenol A polycarbonate/acrylonitrile–butadiene–styrene (PC/ABS) with and without bisphenol A bis(diphenyl phosphate) (BDP) and 5 wt.% zinc borate (Znb) were investigated. The pyrolysis was studied by thermogravimetry (TG), TG-FTIR and NMR, the fire behaviour with a cone calorimeter applying different heat fluxes, LOI and UL 94. Fire residues were examined with NMR. BDP affects the decomposition of PC/ABS and acts as a flame retardant in the gas and condensed phases. The addition of Znb results in an additional hydrolysis of PC. The fire behaviour is similar to PC/ABS, aside from a slightly increased LOI and a reduced peak heat release rate, both caused by borates improving the barrier properties of the char. In PC/ABS + BDP + Znb, the addition of Znb yields a borate network and amorphous phosphates. Znb also reacts with BDP to form alpha-zinc phosphate and borophosphates that suppress the original flame retardancy mechanisms of BDP. The inorganic–organic residue formed provides more effective flame retardancy, in particular at low irradiation in the cone calorimeter, and a clear synergy in LOI, whereas for more developed fires BDP + Znb become less effective than BDP in PC/ABS with respect to the total heat evolved. KW - Flame retardancy KW - PC/ABS KW - Aryl phosphate KW - Zinc borate KW - Flammability PY - 2010 DO - https://doi.org/10.1016/j.tca.2009.10.007 SN - 0040-6031 SN - 1872-762X VL - 498 IS - 1-2 SP - 92 EP - 99 PB - Elsevier CY - Amsterdam AN - OPUS4-20746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dey, Anika A1 - Casperson, Ralf A1 - Pohl, Rainer A1 - Thomas, Hans-Martin T1 - Die Wirbelstromprüfung als Hilfsmittel für die Schieneninstandhaltung N2 - Die zerstörungsfreie Oberflächenprüfung an verlegten Eisenbahnschienen mit Wirbelstrom hat in den letzten Jahren durch ständige Weiterentwicklung und Verifizierung enorm an Bedeutung gewonnen. Es wurde u.a. angestrebt zuverlässige Planungsgrößen für den Einsatz von Instandhaltungsmaßnahmen zu erhalten, durch deren gezielten Einsatz Risswachstum unterbunden werden kann. Die Ursache für das Wachstum von Rissen in der Schiene liegt in der Materialermüdung des Werkstoffes infolge der Betriebsbelastungen im Rad-Schiene-Kontakt. Nach einer gewissen Beanspruchungsdauer kommt es an den Kontaktflächen der Fahrkante zu einer Kaltverfestigung des Schienenstahls. Durch fortschreitende Verfestigung des kontaktbeanspruchten Oberflächenbereichs der gehärteten Schicht wird der Werkstoff spröde und es bilden sich feine Risse aus. Die Risse wachsen anfangs unter einem flachen Winkel in das Schieneninnere hinein, neigen dann aber ab einem gewissen Stadium dazu in das Innere des Schienenkopfes abzukippen, was im Extremfall zu einem Schienenbruch führen kann. Diese Rollkontaktermüdungsrisse, auch genannt Head Checks, entstehen bevorzugt in der Fahrkante von bogenäußeren Schienen. Die Anwendung der Wirbelstromprüfung an der Schiene wurde bisher zur Ermittlung der Schädigungstiefe dieser Rollkontaktermüdungsrisse eingesetzt. Das Wirbelstromverfahren besitzt die Eigenschaft, sehr empfindlich auf alle Veränderungen der Materialeigenschaften an der Oberfläche zu reagieren. Daher wurde festgestellt, dass sich neben der Detektion von Rissen auch Fehler wie Eindrückungen oder Schlupfwellen, bis hin zu Materialveränderungen durch Schweißen oder Aufhärtungen in der Schienenoberfläche bestimmen lassen. Die Wirbelstromprüfung besitzt daher das Potenzial, mögliche Orte der Entstehung von Ermüdungsrissen in einem extrem frühzeitigen Stadium nachzuweisen. Ziel ist es, die rissgefährdeten Zonen schon im Zustand der Kaltverfestigung zu identifizieren. Dadurch können sich neue Aspekte für die präventive Schieneninstandhaltung ergeben. T2 - DGZfP-Jahrestagung 2010 CY - Erfurt, Deutschland DA - 10.05.2010 KW - Wirbelstromprüfung KW - Rollkontaktermüdung KW - Schienenfehler KW - Eisenbahnschiene PY - 2010 SN - 978-3-940283-26-9 IS - DGZfP-BB 122 (P68) SP - 1 EP - 7 CY - Berlin AN - OPUS4-21886 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf A1 - Dey, Anika A1 - Pohl, Rainer A1 - Reimund, Verena A1 - Thomas, Hans-Martin T1 - Einfluss lokaler Aufhärtung ferritischer Stähle auf die Risstiefenbestimmung mit dem Wirbelstromprüfverfahren N2 - Mechanische Belastung wie z. B. der Rollkontakt zwischen den Rollen und Lagerringen eines Wälzlagers oder der Rad-Schiene-Kontakt bei der Eisenbahn führen bei ferritischen Stählen zu einer Aufhärtung der Oberfläche. Die mit der Aufhärtung verbundene Versprödung begünstigt die Entstehung von Ermüdungsrissen. Zur Risstiefenbestimmung mit dem Wirbelstromprüfverfahren werden in der Regel Kalibrierkörper mit künstlichen Testfehlern aus dem Grundwerkstoff des Prüfteils verwendet. Die betriebsbedingte Aufhärtung der Prüfteiloberfläche bleibt bei der Kalibrierung unberücksichtigt. Die lokale Aufhärtung der Oberfläche führt zu einem ortsabhängigen Offset des Wirbelstromsignals in Richtung der Rissanzeigen und somit zu einer Überbewertung der Risstiefe. Bei einzelnen Rissen lässt sich der Effekt kompensieren, in dem das Wirbelstromgerät neben jedem Riss abgeglichen bzw. die Differenz zwischen dem Offset und der Rissanzeige berechnet wird. In der Realität liegen die Ermüdungsrisse jedoch oft so dicht nebeneinander, dass auf Grund der Überlagerung benachbarter Rissanzeigen weder ein Abgleich zwischen den Rissen noch eine Bestimmung des Offsets möglich ist. Finite-Elemente-Berechnungen ermöglichen es, die in der Realität stets kombiniert auftretenden Wirbelstromsignale der Ermüdungsrisse und der Oberflächenaufhärtung getrennt zu simulieren, um Erkenntnisse für eine Verbesserung der Risstiefenbestimmung zu erlangen. T2 - DGZfP-Jahrestagung 2010 CY - Erfurt, Deutschland DA - 10.05.2010 PY - 2010 SN - 978-3-940283-26-9 IS - DGZfP-BB 122 (P25) SP - 1 EP - 5 CY - Berlin AN - OPUS4-21887 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Brink, Arne T1 - Anwendung der Impuls-Thermografie als zerstörungsfreies Prüfverfahren im Bauwesen N2 - Ziel der Untersuchungen ist die Weiterentwicklung der Impuls-Thermografie als quantitatives zerstörungsfreies Prüfverfahren zur Ortung oberflächennaher Inhomogenitäten in Bauteilen und Bauwerken. Zur Zeit werden Putzablösungen auf Mauerwerk bzw. Beton, Hohlstellen und Kiesnester in Beton, Ablösungen und Hohlstellen bei Spaltklinkern im Dickbettmörtel auf Beton, Verbundprobleme von CFK-Laminaten auf Beton sowie Ablösungen von Bitumen-Abdichtungsbahnen auf Stahl untersucht. T2 - Fachtagung (BAUFACH) "Bauwerksdiagnose - Praktische Anwendungen zerstörungsfreier Prüfungen" CY - Leipzig, Germany DA - 25.10.2001 KW - Mauerwerk KW - Hohlstellen KW - CFK-Laminate PY - 2001 AN - OPUS4-3300 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Munz, Martin A1 - Sturm, Heinz T1 - Structure formation on the surface of indium phosphide irradiated by femtosecond laser pulses N2 - Laser-induced periodic surface structures (LIPSS; ripples) with different spatial characteristics have been observed after irradiation of single-crystalline indium phosphide (c-InP) with multiple linearly polarized femtosecond pulses (130 fs, 800 nm) in air. With an increasing number of pulses per spot, N, up to 100, a characteristic evolution of two different types of ripples has been observed, i.e., (i) the growth of a grating perpendicular to the polarization vector consisting of nearly wavelength-sized periodic lines and (ii), in a specific pulse number regime (N = 5-30), the additional formation of equally oriented ripples with a spatial period close to half of the laser wavelength. For pulse numbers higher than 50, the formation of micrometer-spaced grooves has been found, which are oriented perpendicular to the ripples. These topographical surface alterations are discussed in the frame of existing LIPSS theories. KW - Femtosecond laser irradiation KW - Indium phosphide KW - Microstructure KW - Laser induced periodic surface structures KW - LIPSS KW - SEM PY - 2005 DO - https://doi.org/10.1063/1.1827919 SN - 0021-8979 SN - 1089-7550 VL - 97 SP - 1 EP - 9 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-5992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Dilz, K. A1 - Pohl, J. A1 - Rühe, S. A1 - Thomas, Hans-Martin A1 - Casperson, Ralf T1 - Online-Schweißnahterkennung von Schienenprüfzügen mittels Wirbelstromverfahren N2 - Zur Detektion von Schweißnähten an verlegten Schienen gehört deren Identifikation und Lokalisation. Die Aufgabe, Schweißnähte derart zu detektieren, stellt sich bei der Prüfung eines Gleisnetzes auf Schädigungen, aber auch unabhängig davon. T2 - Jahrestagung Zerstörungsfreie Materialprüfung 2003 CY - Mainz, Deutschland DA - 26.05.2003 PY - 2003 UR - http://www.ndt.net/article/dgzfp03/papers/v07/v07.htm SN - 3-931381-47-1 N1 - Serientitel: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. – Series title: Berichtsband / Deutsche Gesellschaft für zerstörungsfreie Prüfung e. V. IS - 83-CD SP - 1 EP - 4 PB - DGZfP CY - Berlin AN - OPUS4-3491 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Streicher, Doreen A1 - Krause, Martin T1 - Ultraschallecho an Beton - Definition von Kenngrößen zur Beurteilung der Leistungsfähigkeit von bildgebenden Verfahren N2 - Für die Strukturaufklärung von Betonbauteilen existieren mehrere bildgebende Ultraschallecho-Verfahren, u. a. mit Nutzung des Prinzips der synthetischen Apertur. Die Ergebnisse werden mit unterschiedlichen Verfahren, mit oder ohne Anwendung von Rekonstruktionsrechnungen, ausgewertet und in der Regel als B- bzw. C-Bilder dargestellt. Ziel ist es, die unterschiedlichen Verfahren anhand von Messreihen an Testkörpern mit bekannten Prüfobjekten in Hinblick auf Ihre Leistungsfähigkeit quantitativ zu fassen und zu vergleichen, um den Einsatz der Prüfverfahren bei Untersuchungen unbekannter Objekte zu optimieren. Dazu wurden drei Kenngrößen definiert. Als erster Schritt erfolgte die Anwendung der Definitionen auf vorliegende Messergebnisse zu einer in einem 50 cm dicken Betontestkörper parallel zur Messfläche eingebrachten Bohrung. T2 - DGZfP-Jahrestagung 2002: ZfP in Anwendung, Entwicklung und Forschung CY - Weimar, Germany DA - 06.05.2002 KW - Strukturaufklärung KW - Rekonstruktionsrechnungen KW - Betontestkörper PY - 2002 AN - OPUS4-3896 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lausch, Regine T1 - Geometrieeffekte und Hüllrohrortung bei der Impaktecho-Prüfung von Betonbauteilen - Experimentelle und modelltheoretische Ergebnisse N2 - Das Impaktecho-Verfahren wird seit vielen Jahren zur zerstörungsfreien Untersuchung von Betonbauteilen eingesetzt. Um die Mechanismen der elastischen Wellenausbreitung besser zu verstehen und den Einfluss von Geometrieeffekten auf das Messergebnis herauszuarbeiten, wurden Messungen und numerische Simulationen an einer Betonplatte mit drei innenliegenden Hüllrohren durchgeführt. T2 - DGZfP-Jahrestagung 2002: ZfP in Anwendung, Entwicklung und Forschung CY - Weimar, Germany DA - 06.05.2002 KW - Numerische Simulation KW - Betonplatte KW - Hüllrohre PY - 2002 AN - OPUS4-3886 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krause, Martin T1 - Hohlstellenortung in Holzbalken mit dem Ultraschallverfahren N2 - Zusammenfassung: Sehr klares Echo - der Rückwand - der künstlich eingebrachten Fehlstellen - der Schäden in Faserrichtung (Kernfäulenachbildung) T2 - DGZfP-Jahrestagung 2002: ZfP in Anwendung, Entwicklung und Forschung CY - Weimar, Germany DA - 06.05.2002 KW - Kernfäule KW - Standsicherheit KW - Schadenserkennung PY - 2002 AN - OPUS4-3883 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Wirbelstromprüfung an Eisenbahnschienen - Integration der Wirbelstromtechnik in Ultraschallprüfzüge N2 - Eisenbahnschienen sind betriebsbedingt hohen mechanischen Belastungen ausgesetzt. Es ist notwendig, Schädigungen möglichst frühzeitig zu detektieren und hinsichtlich ihrer Schädigungstiefe zu bewerten, um sie durch gezielte Schienenbearbeitung (Schleifen, Hobeln, Fräsen) rechtzeitig zu beseitigen. Mit der bisher in Schienenprüfzügen eingesetzten Ultraschalltechnik lassen sich die Oberflächenfehler nur schwer detektieren. Eine Bewertung der Schädigungstiefe ist nicht möglich. Die Wirbelstromtechnik stellt als oberflächennahes Verfahren der zerstörungsfreien Prüfung eine ideale Ergänzung zur volumenhaften Ultraschallprüfung dar. Es wurde ein Wirbelstromprüfsystem entwickelt, das eine Detektion und Tiefenbewertung von Oberflächenfehlern bei einer Prüfgeschwindigkeit von bis zu 100 km/h und einem Messpunktabstand von 1 mm ermöglicht. Das Wirbelstromsystem kann in das vorhandene Ultraschallsystem integriert werden. Dieses beginnt mit der Übernahme der Dateinamen zur Speicherung der Messdaten, dem synchronen Start und Stopp der Messung, Ortssynchronisation über gemeinsamen Wegtakt und externe Kilometrierung bis hin zur gemeinsamen Darstellung der Prüfergebnisse. Die unterschiedlichen Ultraschallsysteme der verschiedenen Prüfzüge erfordern eine flexible Konfigurierbarkeit der Schnittstelle (Digital-IO, LAN). Wegen des enormen Umfanges der Urdaten ist es erforderlich, die Auswertung der Wirbelstromdaten so weit wie möglich zu automatisieren. Als Ergebnis der automatisierten Auswertung erhält der Prüfer Angaben über Lage, Art und Häufigkeit von Fehlern sowie die maximale Schädigungstiefe. Nebenbei ist das Wirbelstromsystem auch in der Lage, Schweißnähte in den Schienen zu detektieren. Da die Schweißnähte auch optisch zu erkennen sind, stellen sie ein wichtiges Merkmal zum Auffinden von Fehlstellen dar. T2 - DACH-Jahrestagung 2004: ZfP in Forschung, Entwicklung und Anwendung CY - Salzburg, Austria DA - 17.05.2004 PY - 2004 AN - OPUS4-4083 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Urs T1 - The micro X-Ray fluorescence analysis (MXRF) T2 - Stand H23/R012, BAM CY - Berlin, Germany DA - 2006-05-02 PY - 2006 AN - OPUS4-12484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Farooq, M. U. A1 - Klement, U. A1 - Nolze, Gert T1 - Microstructural characterisation of a Co-Cr-Mo laser clad applied on railway wheels N2 - A Co-Cr-Mo laser cladding applied on railway wheels is characterised by a combination of EBSD and EDX. A complete pass of the cladding is investigated to achieve a better understanding of the microstructure evolution during laser cladding. A microstructure with columnar grains extending over the whole thickness of the cladding is observed. The grains have a <001>-fibre texture with the fibre axis parallel to the normal of the substrate surface, and a substructure consisting of cells/dendrites. During the cladding process, two different kinds of precipitates form in the cell walls, which can be identified as M6C and a non-equilibrium phase. Furthermore, stacking faults are observed to occur in the cladding grains and are discussed with respect to the laser cladding process. KW - Laser cladding KW - Co-Cr-Mo KW - EBSD KW - Carbides PY - 2006 DO - https://doi.org/10.3139/146.101312 SN - 1862-5282 VL - 97 IS - 6 SP - 838 EP - 844 PB - Hanser CY - München AN - OPUS4-13973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Farooq, M. U. A1 - Klement, U. A1 - Nolze, Gert T1 - EBSD and EDX analysis at the cladding - Substrate interface of a laser clad railway wheel N2 - Electron backscatter diffraction and energy-dispersive X-ray spectrometry were used to investigate the intermixed interface produced during laser cladding of a Co-Cr-Mo alloy on a steel substrate. A multi-component system and rapid solidification conditions together lead to a complex microstructure at the interface. The solidification of the cladding starts with the formation of an interface layer, which is about 75µm in thickness and consists of randomly oriented equiaxed grains of Co-Cr-Fe solid solution and martensite. Orientation analysis of the grains in the interface layer revealed that some grains have a special orientation relationship with the former austenite grains in the heat affected zone but the cladding is not formed by epitaxial growth on the substrate. Intermixing of the materials at the interface is providing a strong bond between the substrate and the cladding. For a grain from the interface layer to emerge as columnar grain in the cladding, it was determined that its <001> crystallographic direction is not supposed to deviate more than 25° from the sample normal direction. KW - EBSD KW - Laser cladding KW - Interface KW - Orientation KW - Nishiyama - Wassermann relationship PY - 2006 DO - https://doi.org/10.3139/146.101413 SN - 1862-5282 VL - 97 IS - 11 SP - 1512 EP - 1518 PB - Hanser CY - München AN - OPUS4-14425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wosniok, Aleksander T1 - Dyke monitoring using fiber sensor-based geosynthetics N2 - Dyke breaks - caused by e.g. Overflows or Slop breaks during long lasting high water gauge - Play a great role in a failure potential of extreme flood Events. Using conventional dyke condition Monitoring dyke messengers can undertake only a visual surface inspection. Thus defective Areas can oftentimes be discovered too late. A critical area in which failures due to soil displacement and moisture Penetration become more significant is located at a landside dyke foot. Geotextiles are integrated here as a Drainage in case of modern three-zone type of dyke. T2 - European Symposium on Flood Risk Management Research (EFRM 2007) CY - Dresden, Germany DA - 26.02.2007 PY - 2007 AN - OPUS4-14571 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cervino, C. A1 - Knopp, D. A1 - Weller, Michael G. A1 - Niessner, R. T1 - Novel Aflatoxin derivatives and protein conjugates N2 - Aflatoxins, a group of structurally related mycotoxins, are well known for their toxic and carcinogenic effects in humans and animals. Aflatoxin derivatives and protein conjugates are needed for diverse analytical applications. This work describes a reliable and fast synthesis of novel aflatoxin derivatives, purification by preparative HPLC and characterisation by ESI-MS and one- and two-dimensional NMR. Novel aflatoxin bovine serum albumin conjugates were prepared and characterised by UV absorption and MALDI-MS. These aflatoxin protein conjugates are potentially interesting as immunogens for the generation of aflatoxin selective antibodies with novel specificities. KW - Aflatoxin KW - Mycotoxin KW - Hapten KW - Protein conjugation KW - Immunogen KW - Antigen KW - Antibody PY - 2007 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-147572 UR - http://www.mdpi.org/molecules/papers/12030641.pdf UR - http://www.mdpi.org/molecules/papers/12030641sm.pdf DO - https://doi.org/10.3390/12030641 SN - 1420-3049 VL - 12 IS - 3 SP - 641 EP - 653 PB - MDPI CY - Basel AN - OPUS4-14757 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilder, Constanze T1 - Bohrpfahlüberwachung mit strukturintegrierten faseroptischen Sensoren N2 - - Zuverlässiger Nachweis der Tragfähigkeit und Strukturintegrität von Bohr- und Rammpfählen - Nur ein Sensor für alle Pfahlprüfmethoden - Umfassendere Aussagen über Boden-Bauwerks-Interaktion und Gebrauchstauglichkeit durch Nutzung von Sensorketten - Langzeitüberwachung tragender Bauwerkselemente T2 - Sensor+Test 2011 CY - Nuremberg, Germany DA - 07.06.2011 PY - 2011 AN - OPUS4-24058 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Witt, Jens T1 - Fiber optic heart rate sensor for integration into personal protective equipment N2 - The European research project i-Protect “Intelligent PPE system for personnel in high-risk and complex environments”, supported by the EU 7th Framework Programme, develops an advanced personal protective equipment (PPE) system that will ensure active protection and information support for personnel operating in high risk and complex environments in fire fighting, chemical and mining rescue operations. Within the project an intelligent underwear for monitoring the rescuers heart rate, body temperature, and respiratory rate will be developed. T2 - BioPhotonics Workshop CY - Parma, Italy DA - 08.06.2011 PY - 2011 AN - OPUS4-24062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Erhard, Anton A1 - Goedecke, Thomas A1 - Menrad, Andreas A1 - Bethke, John T1 - Application of nondestructive testing - Methods for packaging examination N2 - Nondestructive testing (NDT) methods are applicable in many ways for defect detection as well as optimization of packaging production processes. The visual inspection method is the technique which is mostly used, although neither the customer nor a skilled inspector may be aware of this. Techniques like ultrasound for wall thickness measurement, the application of x-ray techniques or the use of dye penetrant techniques for crack detection are rather well known to the NDT family. However, acoustic emission techniques can also be helpful for the characterization of packaging materials. In this paper the employment of x-ray computer tomography (CT) for measurement of wall thickness in plastic jerrycans, especially on the edges, and its possible optimization of production processes will be discussed. A comparison of the CT and ultrasonic examinations of wall thickness and the reliability of this measured data are also important points for the discussion, especially if some safety factors can be derived from the results. The leakage test is also good for jerrycans, IBCs or other kinds of drums for the transportation and storage of dangerous goods. The disadvantage of this kind of test is that a lack of quality, e.g. wall thickness deterioration, cannot be detected if the wall thickness withstands the internal pressure. Therefore, especially for Quality assurance, the other, previously mentioned techniques are better for a statistical assessment of a batch. This paper is focused on the comparison of different NDT results with special emphasis on the large range of material mechanical properties. T2 - 25th IAPRI Symposium on Packaging CY - Berlin, Germany DA - 16.05.2011 KW - Materialeigenschaft KW - Zerstörungsfreie Prüfung KW - Computertomographie KW - Kunststoffbehälter PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-239191 SN - 978-3-940283-31-3 VL - 126 SP - 1 EP - 7 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-23919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard A1 - Badde, Aurelia A1 - Michaelis, Matthias A1 - Berger, U. A1 - Onel, Yener A1 - Meinel, Dietmar A1 - Goebbels, Jürgen T1 - Einsatz von mobilen Röntgenuntersuchungsmethoden im Museum - Zwei Fallbeispiele N2 - Zwei Bildhauermodelle aus dem Georg-Kolbe-Museum Berlin standen zur Restaurierung an. Das kleinere, 'Lucino' (1920), 41cm, wurde hochauflösend mit CT gemessen, da mittels CT sowohl der Herstellungsprozeß einer Gipsstatue als auch der innere Zustand, wie Ergänzungen, Klebungen und Armierungen, festgestellt werden können. Aus den CT Bildern ergab sich eine für die vorher vermutete Gipszusammensetzung ungewöhnliche innere Struktur. Mit einer Freihand bedienten Röntgenpistole zur Messung der Röntgenfluoreszenz wurde daraufhin die Zusammensetzung des Materials der Statuette als Terracotta bestimmt. Durch den Einsatz von Helium als Spülmittel konnten auch leichte Materialien nachgewiesen und so eine Unterscheidung zwischen Gips und gebranntem Ton durchgeführt werden. Aus den CT Daten wurde eine virtuelle Darstellung der äußeren Geometrie gewonnen. Ein damit versuchsweise erstelltes Replik (Rapid Prototyping, 3D-Drucker, TU-Berlin) entsprach nicht den Anforderungen des Museums zur Erstellung einer Gußform für eine Bronzekleinserie der Statuette. Die zweite Statue, die 'Große Nacht' (1930) ist mit ihrer Größe von 2,12m und aufgrund des durch korrodierende Metallarmierung verursachten Schadensbildes nicht mehr transportfähig. Eine in-situ Untersuchung mit dem mobilen Tomographen, der in den 1980ern zur Untersuchung von Bäumen gebaut und jetzt mit einem modernen Flachdetektor und einer Röntgenröhre ausgestattet ist, wird vorgestellt. Die Möglichkeiten acder in-situ CT für große Skulpturen werden anhand der Ergebnisse diskutiert. T2 - DGZfP-Jahrestagung 2010 CY - Erfurt, Deutschland DA - 10.05.2010 KW - Mobile CT KW - Mobile RFA PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-246956 UR - https://www.ndt.net/?id=10149 SN - 978-3-940283-26-9 VL - 122 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-24695 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane A1 - Ziegler, Mathias A1 - Kunert, M. A1 - Goldammer, M. T1 - Entwicklung von Referenzprobekörpern für die Standardisierung der Blitzthermografie N2 - Die aktive Thermografie wird in der Industrie zunehmend in verschiedenen Bereichen zur Qualitätssicherung, Zustandsdiagnose und Zustandsüberwachung eingesetzt. Bestehende Normen zur Thermografie beschreiben die Grundlagen, Geräte und Begriffe. In diesem Beitrag wird über ein Projekt berichtet, dessen Ziel die Erarbeitung einer Prüfnorm zur Blitzthermografie ist. Diese sollte neben der Auswahl geeigneter Gerätekomponenten, der Auswertungsverfahren und der Vorgehensweise bei der Prüfung auch die Beschreibung geeigneter Referenzprobekörper enthalten, die eine Bewertung der Messapparatur und eine Qualitätssicherung der Prüfung ermöglichen. T2 - Thermographie-Kolloquium 2011 CY - Stuttgart, Germany DA - 29.09.2011 KW - Aktive Thermografie KW - Blitzanregung KW - Prüfnorm KW - Referenzprobekörper PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-246230 SN - 978-3-940283-36-8 VL - 130 SP - 1 EP - 7 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-24623 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lai Wai-Lok, Wallace A1 - Kind, Thomas A1 - Wiggenhauser, Herbert T1 - A study of concrete hydration and dielectric relaxation mechanism using ground penetrating radar and short-time fourier transform N2 - Ground penetrating radar (GPR) was used to characterize the frequency-dependent dielectric relaxation phenomena in ordinary Portland cement (OPC) hydration in concrete changing from fresh to hardened state. The study was experimented by measuring the changes of GPR A-scan waveforms over a period of 90 days, and processed the waveforms with short-time Fourier transform (STFT) in joint time-frequency analysis (JTFA) domain rather than a conventional time or frequency domain alone. The signals of the direct wave traveled at the concrete surface and the reflected wave from an embedded steel bar were transformed with STFT, in which the changes of peak frequency over ages were tracked. The peak frequencies were found to increase with ages and the patterns were found to match closely with primarily the well-known OPC hydration process and secondarily, the evaporation effect. The close match is contributed to the simultaneous effects converting free to bound water over time, on both conventional OPC hydration and dielectric relaxation mechanisms. KW - Soil water content KW - Wet soil KW - Microwave KW - Moisture KW - GPR KW - Dispersion PY - 2010 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-239723 DO - https://doi.org/10.1155/2010/317216 SN - 1687-6172 IS - Article ID 317216 SP - 1 EP - 14 PB - Hindawi Publ. CY - New York, NY, USA AN - OPUS4-23972 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Liehr, Sascha T1 - A dynamic fiber optic strain and power change sensor N2 - A dynamic and quasi-distributed sensor principle for simultaneous measurement of length changes and optical power changes between reflection points in an optical fiber is presented. The technique is based on the incoherent optical frequency domain reflectometry (I-OFDR). The calculation of phase and amplitude changes from few measurement points in the frequency domain yields precise and dynamic length and optical power change results up to 2 kHz and μm-resolution. Test results showing the deformation of a masonry building under seismic load are presented. Promising fields of application for this technique are the structural health monitoring sector and chemical process control. T2 - 21st International Conference on Optical Fiber Sensors CY - Ottawa, Canada DA - 15.05.2011 PY - 2011 AN - OPUS4-24930 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Feigl, Michael T1 - Electrochemical evaluation of corrosion behaviour of sol-gel alumina coated steel AlSl304 and Ni-base alloy Inconel-718 T2 - Eurocorr 2011 CY - Stockholm, Sweden DA - 05.09.2011 PY - 2011 AN - OPUS4-24870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertovic, Marija A1 - Gaal, Mate A1 - Müller, Christina A1 - Fahlbruch, B. A1 - Schombach, D. T1 - Einfluss des Zeitdrucks auf die manuelle Ultraschallprüfung. Untersuchung zu menschlichen Faktoren auf die Ergebnisse zerstörungsfreier Prüfungen N2 - Die übergeordnete Zielsetzung unserer Untersuchung bestand darin, am Beispiel von Prüfungen mit Ultraschall eine belastbare Aussage zum Einfluss der Arbeitsbedingungen des Prüfers auf die Qualität der Ergebnisse von zerstörungsfreien Prüfungen zu ermitteln und Möglichkeiten zur Minimierung ungünstiger Einflussfaktoren aufzuzeigen. Der Schwerpunkt der Untersuchung wurde auf die manuelle Ultraschallprüfung gelegt und der Faktor 'Zeitdruck' (in drei Stufen variiert) als die zu variierende physische Einflussgröße gewählt. Die Variation des Faktors Zeitdruck wurde gemäß dem Prozessmodell von der Erhebung psychologischer Faktoren, die das Individuum und die Organisation beschreiben, begleitet. Die Ultraschallprüfungen erfolgten mit zehn Prüfern am Großbehälter und an Vergleichskörpern mit eingebrachten Testfehlern (Nuten, Risse). Die ausgewählten Fehler waren typisch für Prüfaufgaben, die bei wiederkehrenden Ultraschallprüfungen in Kernkraftwerken von den Prüfern zu lösen sind. Die Prüfaufgabe bestand darin, die in den vorgegebenen Prüfabschnitten vorhandenen Reflektoren aufzufinden und deren Amplituden, Ortskoordinaten und Längenerstreckungen zu ermitteln. Als Bewertungsmaßstab für die Qualität der Prüfaussage und für den Einfluss des menschlichen Faktors diente die Präzision der gemessenen Werte. Die Ergebnisse zeigen einen hohen Einfluss des menschlichen Faktors auf das Prüfergebnis und eine Einwirkung des Zeitdrucks besonders auf die Präzision der Messwerte. Hierbei war die Wirkung des individuell wahrgenommenen Zeitdrucks zusammen mit der psychischen Arbeitsbeanspruchung signifikant. Es wurde unter anderem herausgearbeitet, dass durch eine gute Vorbereitung auf die Prüfung, z.B. durch die sorgfältige Einweisung und ein vorgeschaltetes Fertigkeitstraining an Vergleichskörpern, die Zuverlässigkeit der Prüfergebnisse verbessert werden kann. Insgesamt hatte der Faktor 'Organisation' neben der 'Erfahrung' einen hohen Einfluss auf das Leistungsvermögen der Prüfer. Die Projektergebnisse wurden im Abschlussbericht des Forschungsvorhabens SR2514 dargestellt, es wurden drei Empfehlungen zur Vorbereitung und Einweisung der Prüfer, zur Stärkung der Verantwortung der Prüfaufsicht und zum 4-Augen-Prinzip formuliert. Die Empfehlungen wurden in der KTA- Regel 3201.4 'Komponenten des Primärkreises von Leichtwasserreaktoren; Teil 4: Wiederkehrende Prüfungen und Betriebsüberwachung (RÄE Fassung 2010-11)', umgesetzt. T2 - DGZfP-Jahrestagung 2011 CY - Bremen, Germany DA - 30.05.2011 KW - Human factors KW - ZfP KW - Ultraschallprüfung KW - UT KW - Zeitdruck PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-251610 UR - http://jt2011.dgzfp.de/Portals/jt2011/BB/mi2c3.pdf SN - 978-3-940283-33-7 IS - DGZfP-BB 127 (Mi.2.C.3) SP - 1 EP - 9 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-25161 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dey, Anika A1 - Casperson, Ralf A1 - Pohl, Rainer A1 - Thomas, Hans-Martin A1 - Heyder, R. T1 - Erfahrungen mit der Wirbelstromprüfung beim Einsatz an unterschiedlichen Schienenstahlsorten N2 - Die steigenden Anforderungen im Schienenverkehr haben u. a. wachsende Betriebsbeanspruchungen für das Führungselement Schiene zur Folge. Auf Strecken mit hohen Belastungen wird dadurch die Entstehung von Rollkontaktermüdungsrissen, den sog. Head Checks, begünstigt. Für die Quantifizierung von Schäden im Hinblick auf eine optimierte Instandhaltung, setzt die DB AG daher seit einigen Jahren die Wirbelstromprüfung an Schienen ein. Es wurde ein Wirbelstromprüfsystem speziell für die Detektion und Bewertung von Head Checks auf der Schienenstahlsorte R260 entwickelt. Um den Instandhaltungsaufwand möglichst gering zu halten, unterliegen Eisenbahnschienen einer ständigen technologischen Weiterentwicklung durch die Hersteller. Durch Verbesserung der Schienenstahlsorten soll ein größerer Widerstand gegen die Bildung von Rollkontaktermüdungsrissen erreicht werden. Anhand von Streckenversuchen der DB AG in den letzten Jahren konnte festgestellt werden, dass tatsächlich eine Verminderung der Risswachstumsgeschwindigkeit erzielt wurde. Dafür zeigten sich im Vergleich zur Stahlsorte R260 abweichende Rissgeometrien, geringere Abstände zwischen den Ermüdungsrissen und somit eine größere Dichte des Rissfeldes. Die daraus resultierenden Folgen für die Ergebnisse der Wirbelstromprüfung werden hier erläutert. Praktische Prüferfahrungen an Schienenstahlsorten mit höherer Festigkeit werden vorgestellt. T2 - DGZfP-Jahrestagung 2011 CY - Bremen, Germany DA - 30.05.2011 KW - Wirbelstromprüfung KW - Rollkontaktermüdung KW - Schienenstahlsorten KW - Schienenfehler KW - Eisenbahnschiene PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-252793 SN - 978-3-940283-33-7 IS - DGZfP-BB 127 (Di.2.A.4) SP - 1 EP - 10 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) AN - OPUS4-25279 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weller, Michael G. T1 - A unifying review of bioassay-guided fractionation, effect-directed analysis and related techniques N2 - The success of modern methods in analytical chemistry sometimes obscures the problem that the ever increasing amount of analytical data does not necessarily give more insight of practical relevance. As alternative approaches, toxicity- and bioactivity-based assays can deliver valuable information about biological effects of complex materials in humans, other species or even ecosystems. However, the observed effects often cannot be clearly assigned to specific chemical compounds. In these cases, the establishment of an unambiguous cause-effect relationship is not possible. Effect-directed analysis tries to interconnect instrumental analytical techniques with a biological/biochemical entity, which identifies or isolates substances of biological relevance. Successful application has been demonstrated in many fields, either as proof-of-principle studies or even for complex samples. This review discusses the different approaches, advantages and limitations and finally shows some practical examples. The broad emergence of effect-directed analytical concepts might lead to a true paradigm shift in analytical chemistry, away from ever growing lists of chemical compounds. The connection of biological effects with the identification and quantification of molecular entities leads to relevant answers to many real life questions. KW - Toxicity KW - Drug discovery KW - Natural products KW - Environmental analysis KW - Lead identification PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-262960 DO - https://doi.org/10.3390/s120709181 SN - 1424-8220 VL - 12 IS - 7 SP - 9181 EP - 9209 PB - MDPI CY - Basel AN - OPUS4-26296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Osterloh, Kurt A1 - Ewert, Uwe A1 - Zvizdic, D. A1 - Krstelj, V. T1 - Die EFNDT Arbeitsgruppe 5 'Öffentliche Sicherheit mit ZfP-Techniken' neu formiert N2 - Für die öffentliche Sicherheit wird gesorgt, indem Gefahren rechtzeitig entdeckt werden. Deren Ursprung kann im technischen oder menschlichen Versagen liegen, womit im englischen Sprachraum zwischen 'Safety' und 'Security' unterschieden wird. Hinsichtlich der Folgen verschwimmt aber dieser Unterschied, obwohl für deren Verhinderung unterschiedliche Zuständigkeiten existieren. Bezüglich des gemeinsamen Interesses und auch überlappender Methoden und Vorgehensweisen würden beide Seiten gewinnen können, wenn es eine Brücke zwischen ihnen gäbe. Eine solche zu schaffen hat sich die EFNDT Arbeitsgruppe (Working Group) 5 zur Aufgabe gestellt. Gestaltet werden soll sie durch gemeinsame Veranstaltungen und Seminaren, die zur Bildung von Konsortien und der Durchführung gemeinsamer Projekte führen sollen. T2 - DGZfP-Jahrestagung 2011 CY - Bremen, Germany DA - 03.05.2011 KW - EFNDT Working Group 5 KW - Technische und öffentliche Sicherheit KW - Gemeinsamkeiten in ZfP und öffentlicher Sicherheit KW - Brückenbildung zwischen Zuständigkeitsbereichen PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-250631 SN - 978-3-940283-33-7 VL - 127 SP - 1 EP - 5 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-25063 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Osterloh, Kurt A1 - Fratzscher, Daniel A1 - Zscherpel, Uwe A1 - Ewert, Uwe A1 - Hasenstab, A. A1 - Bücherl, T. A1 - Schillinger, B. T1 - Partielle Tomographie mit Neutronen zur Beurteilung von Leimschichten in Holz N2 - Verleimte Holzproben wurden je nach Größe mit thermischen (ANTARES) bzw. schnellen Neutronen (NECTAR) an der Forschungs-Neutronenquelle Heinz Maier-Leibnitz (FRM II) der Technischen Universität München in Garching untersucht. Entweder ließen die durchstrahlbare Schichtdicke oder die eingeschränkte Strahlgeometrie es nicht zu, das Probenteil allseitig zu durchstrahlen. Um dennoch innere Strukturen wie Leimschichten zumindest mit einem eingeschränkten Winkelbereich tomographisch darzustellen, wurde mit Hilfe des Slice-Theorems erfolgreich rekonstruiert. Ein Brett von 2 cm Dicke wurde mit thermischen Neutronen erfolgreich untersucht, ein größeres mit schnellen. T2 - DGZfP-Jahrestagung 2011 CY - Bremen, Germany DA - 30.05.2011 KW - Neutronentomographie KW - Eingeschränkter Winkelbereich KW - Holz PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-250649 SN - 978-3-940283-33-7 VL - 127 SP - 1 EP - 6 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-25064 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Osterloh, Kurt A1 - Fratzscher, Daniel A1 - Jechow, Mirko A1 - Bücherl, T. A1 - Schillinger, B. A1 - Hasenstab, A. A1 - Zscherpel, Uwe A1 - Ewert, Uwe T1 - Limited view tomography of wood with fast and thermal neutrons N2 - Neutrons are absorbed particularly by hydrogen containing materials so they can be used as a tool for visualising heterogeneous density distributions of organic materials. Penetration limits are set by the layer thicknesses and the neutron energies applied. In case of specimens with a flat shape the situation may be encountered that the object only could be penetrated in selected directions. In addition, the overall size may exceed the beam diameter and thus the viewing window if a certain region of interest should be studied by tomography without destroying the integrity of the specimen. This study shows the capabilities and limits of thermal and fast neutrons to investigate flat wooden specimens such as boards and girders by neutron tomography under such circumstances. Taking projections was impaired either by the limits of penetrability or by the total size of the object. As a consequence, projections were included for reconstruction only from a limited angular range of 90°. It could be shown that an approach based on the slice theorem was capable to visualise structural features along the beam directions while simply omitting the perpendicular ones without causing additional artefacts. Small samples with a thickness of up to 2 cm but several times broader could be studied with the ANTARES facility of the FRM II neutron source in Garching providing thermal neutrons while larger objects required a beam of higher energy as available in the NECTAR facility of the same institution. The fast (fission) neutrons (1.5 – 2 MeV) of this site allowed investigating an area of interest inside a girder with a cross section of 23.5 x 49 cm². Internal features such as inclusions could be detected as well as a heterogeneous density distribution in glue layers. T2 - International symposium on digital industrial radiology and computed tomography CY - Berlin, Germany DA - 20.06.2011 KW - Computed tomography KW - Slice theoreme KW - Limited angle tomography PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-250663 SN - 978-3-940283-34-4 VL - 128 SP - 1 EP - 5 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-25066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Bobe, U. A1 - Beck, Uwe A1 - Wegwerth, Tillmann A1 - Sahre, Mario A1 - Weise, Matthias A1 - Strauß, Birgid A1 - Reetz, Susanne A1 - Schondelmaier, D. A1 - Kutz, O. A1 - Winzer, B. A1 - Schaule, G. T1 - Nanotechnologische Entwicklung von "easier-to-clean"- Oberflächenstrukturen für eine zukünftig gesteigerte Lebensmittel- und Produktsicherheit - Abschlussbericht AiF-Vorhaben Nr.: 210 ZN III N2 - Reinigung wird in der Lebensmittel- und Pharmaindustrie aufgrund des stetig steigenden Kosten- und Zeitdrucks sowie der hohen Verbrauchererwartungen hinsichtlich Produktsicherheit und -haltbarkeit ein immer zentraleres Thema. Eine verbesserte Reinigbarkeit bedeutet für die produzierende Industrie eine Steigerung der Effizienz der Produktionsanlage. Besonders in der heutigen medienintensiven Zeit kommt ein "Lebensmittelskandal" durch ein unsicheres Produkt einem finanziellen Desaster und immensem Imageverlust gleich. Aus diesem Grund ist die Reinigbarkeit der produktberührenden Oberflächen stets ein wichtiges Kriterium für die Werkstoffauswahl. Basierend auf den Theorien zu Schmutzhaftung und -entfernung wurde im Rahmen dieser Arbeit überprüft, ob und wie die theoretisch relevanten Parameter auch in den Experimenten den Reinigungserfolg beeinflussen. Der Schwerpunkt wurde auf die Einflussgrößen des Werkstoffes gelegt, um herauszufinden, wie stark eine Oberfläche selbst zu ihrer Reinigbarkeit beitragen kann (self-cleaning). In den durchgeführten Versuchen hat sich gezeigt, dass die Oberflächenrauheit lediglich bei der Reinigung von kohäsiven Schmutzfilmen eine entscheidende Rolle gespielt hat. Hingegen ist ihr Einfluss auf das Reinigungsergebnis von sich auflösenden Schmutzfilmen und Partikeln nur begrenzt bis gar nicht zur Geltung gekommen. Das Oberflächenmaterial hatte keinen starken, aber dennoch signifikanten Einfluss auf die Reinigbarkeit der untersuchten Oberflächen. Dass die Reinigbarkeit einer Oberfläche keine Materialkonstante sein kann, wurde unter Verwendung spezieller Oberflächen mit definiert geätzten Rauheitsstrukturen nachgewiesen. Der Reinigungserfolg hängt immer auch von der Verunreinigungsart ab, was sich auch in vergleichbaren Versuchen der Einzelpartikelablösung mittels AFM in dem Einfluss der Elastizität bzw. Plastizität der Partikeln geäußert hat. Praxistaugliche Empfehlungen gehören mit zu den wichtigsten Zielen dieser Arbeit gewesen. Mit Fokus auf die Oberflächenparameter und auf Basis der durchgeführten Untersuchungen wurde zur Optimierung der Reinigung produktberührender Oberflächen für bekannte Kontaminationen eine Checkliste als Orientierungshilfe erarbeitet. Ist die Verunreinigungsart dennoch unbekannt, so sollte der "Grenzwert" von Ra = 1 µm unterschritten werden, um bei Vorhandensein filmartiger Verschmutzungen keine negativen Auswirkungen auf die Reinigbarkeit zu haben. Die Notwendigkeit nach hochpolierten Oberflächen (Ra < 0,3 µm) aus Reinigbarkeitsgründen kann aufgrund der Untersuchungen nicht nachvollzogen werden. Das Ziel des Vorhabens wurde erreicht. PY - 2007 SP - I EP - 148 PB - TU München CY - Weihenstephan AN - OPUS4-25430 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pelkner, Matthias A1 - Neubauer, Andreas A1 - Reimund, Verena A1 - Kreutzbruck, Marc T1 - Routes for GMR-sensor design in non-destructive testing N2 - GMR sensors are widely used in many industrial segments such as information technology, automotive, automation and production, and safety applications. Each area requires an adaption of the sensor arrangement in terms of size adaption and alignment with respect to the field source involved. This paper deals with an analysis of geometric sensor parameters and the arrangement of GMR sensors providing a design roadmap for non-destructive testing (NDT) applications. For this purpose we use an analytical model simulating the magnetic flux leakage (MFL) distribution of surface breaking defects and investigate the flux leakage signal as a function of various sensor parameters. Our calculations show both the influence of sensor length and height and that when detecting the magnetic flux leakage of µm sized defects a gradiometer base line of 250 µm leads to a signal strength loss of less than 10% in comparison with a magnetometer response. To validate the simulation results we finally performed measurements with a GMR magnetometer sensor on a test plate with artificial µm-range cracks. The differences between simulation and measurement are below 6%. We report on the routes for a GMR gradiometer design as a basis for the fabrication of NDT-adapted sensor arrays. The results are also helpful for the use of GMR in other application when it comes to measure positions, lengths, angles or electrical currents. KW - Giant magneto resistance KW - Non-destructive testing KW - Magnetic flux leakage KW - Sensor array PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-271325 DO - https://doi.org/10.3390/s120912169 SN - 1424-8220 VL - 12 IS - 9 SP - 12169 EP - 12183 PB - MDPI CY - Basel AN - OPUS4-27132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hanelt, Sven A1 - Friedrich, Jörg Florian A1 - Meyer-Plath, Asmus T1 - UV spectrometric indirect analysis of brominated MWCNTs with UV active thiols and an alkene-reaction kinetics, quantification and differentiation of adsorbed bromine and oxygen N2 - Indirect UV-absorption spectrometry was shown to be a valuable tool for chemical characterization of functionalized carbon nanotubes (CNTs). It complements data from X-ray photoelectron spectroscopy (XPS) or FTIR analysis since it helps to clarify the type and concentration of functional groups. The principles of indirect application of UV-spectrometry and its mathematical interpretation are discussed. Their facile application, together with their adequate sensitivity and high flexibility, make UV-absorption-based approaches a valuable alternative to fluorescence spectrometry. Here, the approach was applied to the chemical analysis of oxidizing substances on CNTs. For this, pristine CNTs of low but finite oxygen content as well as brominated CNTs were analyzed by reaction in suspension with UV-active thiol reagents and a styrene derivative. It was shown that carefully selected reagents allow differentiation and quantification of bromine and generally oxidizing entities like oxygen. For brominated CNTs, it was shown that physisorbed bromine may dominate the overall bromine content. KW - Carbon nanotubes KW - CNTs KW - UV-spectrometry KW - Bromination KW - Thiols KW - Mercaptans KW - Disulfides KW - Quantification KW - Kinetics PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-289077 DO - https://doi.org/10.3390/ma6083035 SN - 1996-1944 VL - 6 IS - 8 SP - 3035 EP - 3063 PB - MDPI CY - Basel AN - OPUS4-28907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf A1 - Eckey, Andreas A1 - Pohl, Rainer A1 - Allner, C. A1 - Beilken, D. T1 - Wirbelstromprüfsystem für Schienenbearbeitungsmaschinen N2 - PLR Prüftechnik Linke & Rühe Magdeburg und die BAM Bundesanstalt für Materialforschung und -prüfung Berlin haben in Zusammenarbeit mit anderen Partnern im Laufe der letzten Jahre verschiedene Wirbelstromsysteme zur Prüfung verlegter Schienen auf rissartige Fehler des Typs Head Checks entwickelt. Die Entwicklung dieser Systeme erfolgte mit dem Ziel, ein Hilfsmittel für die Planung von Schieneninstandhaltungsmaßnahmen zu schaffen. Die Systeme haben sich im praktischen Prüfeinsatz bewährt. Hierzu wurde regelmäßig auf den vorhergehenden Tagungen berichtet. Bei der Schieneninstandhaltung kommen unterschiedliche Typen von Schienenbearbeitungsmaschinen zum Einsatz, z. B. Schienenfräs- und Schleifzüge. Seit einiger Zeit wird von Seiten der Schienennetzbetreiber vermehrt ein Qualitätsnachweis nach erfolgter Schienenbearbeitung gefordert. Hierzu wurde ein Wirbelstromprüfsystem entwickelt, dass speziell an die Erfordernisse der Qualitätsüberwachung in Schienenbearbeitungsmaschinen angepasst ist. Das Prüfsystem wird vorgestellt und über erste Erfahrungen aus dem praktischen Einsatz wird berichtet. T2 - DGZfP-Jahrestagung 2013 CY - Dresden, Germany DA - 06.05.2013 KW - Wirbelstromprüfung KW - Schienenbearbeitung KW - ZfP KW - Eisenbahn PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-290651 SN - 978-3-940283-49-8 IS - Poster 62 SP - 1 EP - 6 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung e.V. (DGZfP) AN - OPUS4-29065 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dörfel, Ilona T1 - TEM Investigations of Alumina Coatings after Corrosion Experiments T2 - MC2013 CY - Regensburg, Germany DA - 25.08.2013 PY - 2013 AN - OPUS4-29169 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Casperson, Ralf T1 - Wirbelstromprüfsystem für Schienenbearbeitungsmaschinen N2 - PLR Prüftechnik Linke & Rühe Magdeburg und die BAM Bundesanstalt für Materialforschung und -prüfung Berlin haben in Zusammenarbeit mit anderen Partnern im Laufe der letzten Jahre verschiedene Wirbelstromsysteme zur Prüfung verlegter Schienen auf rissartige Fehler des Typs Head Checks entwickelt. Die Entwicklung dieser Systeme erfolgte mit dem Ziel, ein Hilfsmittel für die Planung von Schieneninstandhaltungsmaßnahmen zu schaffen. Die Systeme haben sich im praktischen Prüfeinsatz bewährt. Hierzu wurde regelmäßig auf den vorhergehenden Tagungen berichtet. Bei der Schieneninstandhaltung kommen unterschiedliche Typen von Schienenbearbeitungsmaschinen zum Einsatz, z. B. Schienenfräs- und Schleifzüge. Seit einiger Zeit wird von Seiten der Schienennetzbetreiber vermehrt ein Qualitätsnachweis nach erfolgter Schienenbearbeitung gefordert. Hierzu wurde ein Wirbelstromprüfsystem entwickelt, dass speziell an die Erfordernisse der Qualitätsüberwachung in Schienenbearbeitungsmaschinen angepasst ist. Das Prüfsystem wird vorgestellt und über erste Erfahrungen aus dem praktischen Einsatz wird berichtet. T2 - DGZfP-Jahrestagung 2013 CY - Dresden, Germany DA - 06.05.2013 PY - 2013 AN - OPUS4-28480 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pohl, Rainer A1 - Casperson, Ralf A1 - Eckey, Andreas A1 - Sickert, Roland T1 - Passiver induktiver Sensor zur Zustandsüberwachung rotierender metallischer Bauteile N2 - Häufig müssen rotierende metallische Bauteile im Betrieb auf das Entstehen rissartiger Fehler überwacht werden. Hierbei besteht im Allgemeinen die Anforderung, trotz extrem schwieriger Umweltbedingungen eine sichere Prüfaussage zu gewährleisten. Es wurden Untersuchungen durchgeführt, inwieweit passive induktive Sensoren in der Lage sind, diese Anforderungen zu erfüllen. Hierzu wurden verschiedene einfache Sensormodelle aufgebaut und an verschiedenen Vergleichsfehlern erprobt. Die Ergebnisse der Untersuchungen werden vorgestellt. Insbesondere die Möglichkeiten und Grenzen dieser einfachen Sensortypen werden herausgearbeitet. T2 - DGZfP-Jahrestagung 2013 CY - Dresden, Germany DA - 06.05.2013 KW - Induktiver Sensor KW - Rotierendes Bauteil PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-285552 SN - 978-3-940283-49-8 IS - P30 SP - 1 EP - 8 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung e.V. (DGZfP) AN - OPUS4-28555 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Orts Gil, Guillermo A1 - Natte, Kishore A1 - Österle, Werner T1 - Multi-parametric reference nanomaterials for toxicology: state of the art, future challenges and potential candidates N2 - A major requirement for the validation of methods assessing the risk associated with engineered nanoparticles (ENPs) is the use of reference materials (RMs). In the present contribution we review available RMs, ongoing projects and characterisation trends in the field. The conclusion is that actual approaches to RMs mostly deal with metrological considerations about single properties of the ENPs, typically their primary size, which can hardly be representative of nanoparticles characteristics in real testing media and therefore, not valid for reliable and comparable toxicological studies. As an alternative, we discussed the convenience and feasibility of establishing multi-parametric RMs for a series of ENPs, focusing on silica nanoparticles (SNPs). As a future perspective, the need to develop RMs based on hybrid nanoparticles is also discussed. KW - Referenzmaterialien KW - Nanopartikel KW - Toxikologie KW - Metrologie PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-292997 DO - https://doi.org/10.1039/c3ra42112k SN - 2046-2069 VL - 3 IS - 40 SP - 18202 EP - 18215 PB - RSC Publishing CY - London AN - OPUS4-29299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weller, Michael G. T1 - Immunoassays and biosensors for the detection of cyanobacterial toxins in water N2 - Algal blooms are a frequent phenomenon in nearly all kinds of fresh water. Global warming and eutrophication by waste water, air pollution and fertilizers seem to lead to an increased frequency of occurrence. Many cyanobacteria produce hazardous and quite persistent toxins, which can contaminate the respective water bodies. This may limit the use of the raw water for many purposes. The purification of the contaminated water might be quite costly, which makes a continuous and large scale treatment economically unfeasible in many cases. Due to the obvious risks of algal toxins, an online or mobile detection method would be highly desirable. Several biosensor systems have been presented in the literature for this purpose. In this review, their mode of operation, performance and general suitability for the intended purpose will be described and critically discussed. Finally, an outlook on current developments and future prospects will be given. KW - Algal toxins KW - Cyanotoxins KW - Biotoxins KW - Blue-green algae KW - Harmful algal blooms KW - Microcystins KW - Nodularins KW - Anatoxin-a KW - Anatoxin-a(s) KW - Cylindrospermopsin KW - Saxitoxins PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-294728 DO - https://doi.org/10.3390/s131115085 SN - 1424-8220 VL - 13 IS - 11 SP - 15085 EP - 15112 PB - MDPI CY - Basel AN - OPUS4-29472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mielentz, Frank A1 - Milmann, Boris A1 - Krause, Martin A1 - Müller, W. A1 - Crail, S. T1 - Zerstörungsfreie Risscharakterisierung in Betonbauteilen mit Ultraschall N2 - Die Risstiefenbestimmung in Festen Fahrbahnen ist hinsichtlich der Dauerhaftigkeit der Konstruktion von wesentlichem Interesse. Im Rahmen eines gemeinsamen Forschungsvorhabens mit der DB AG wurden aus der Literatur bekannte Ansätze bewertet und darauf aufbauend ein Verfahren zur bildgebenden Rissdarstellung entwickelt. Rissüberbrückende Bewehrung sowie Kontaktstellen zwischen den Rissflanken wirken als Schallbrücken und erschweren die Risscharakterisierung, wie bei einem Einsatz an einer Betriebserprobungsstrecke festgestellt wurde. Ein aus der Literatur bekanntes Verfahren der einfachen Laufzeitmessung erwies sich für die Tiefenbestimmung von realen verunreinigten Rissen als ungeeignet. T2 - Fachtagung Bauwerksdiagnose - Praktische Anwendungen Zerstörungsfreier Prüfungen CY - Leipzig, Germany DA - 25.10.2001 PY - 2001 VL - 76-CD SP - 1 EP - 10 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-1188 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mittag, Kornelia A1 - Colla, Camilla A1 - Krause, Martin A1 - Maierhofer, Christiane A1 - Mielentz, Frank A1 - Milmann, Boris A1 - Schneider, Gerhard A1 - Wöstmann, Jens A1 - Wiggenhauser, Herbert T1 - Zerstörungsfreie Messungen zur Beurteilung des inneren Zustandes fester Fahrbahnen der Deutschen Bahn AG: Vergleichsmessungen an Probeaufbauten im Labor N2 - Im Rahmen eines FE-Projektes “Inspektion Fester Fahrbahnen“ der BAM und der Deutschen Bahn AG geht es um die Anwendung und weitere Entwicklung zerstörungsfreier Messverfahren zur Beurteilung des Zustandes Fester Fahrbahnen. Nach ersten Versuchsreihen direkt im Gleis wurden für verschiedene Bauarten die charakteristischen Herstellungsbedingungen simuliert und systematisch untersucht. Die kombinierte Anwendung der drei Messverfahren Ultraschall-Array-, Impakt-Echo- und Impuls-Radar-Verfahren wird hier an dem Beispiel “Betonschwelle in Betoneinbettung” dargestellt. T2 - Fachtagung Bauwerksdiagnose - Praktische Anwendungen Zerstörungsfreier Prüfungen CY - Leipzig, Germany DA - 25.10.2001 KW - Impakt-Echo-Messverfahren KW - Impuls-Radar-Messverfahren KW - Ultraschall-Array-Messverfahren PY - 2001 VL - 76-CD SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-1201 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wehrstedt, A. A1 - Ullner, Christian T1 - Erfolgreicher Abschluss der Normungsarbeit "Instrumentierte Eindringprüfung" - ISO 14577 ist veröffentlicht N2 - Im Oktober 2002 fand die Normungsarbeit zur „Instrumentierten Eindringprüfung“ mit der Veröffentlichung von ISO 14577 mit den drei Teilen: - Teil 1: Prüfverfahren - Teil 2: Prüfung und Kalibrierung der Prüfmaschinen - Teil 3: Kalibrierung von Referenzproben ihren erfolgreichen Abschluss. KW - Härteprüfung KW - Eindringtechnik KW - Mechanische Eigenschaften KW - Schichtprüfung KW - Prüfmaschine PY - 2002 SN - 0011-4952 VL - 81 IS - 10 SP - 684 EP - 689 PB - Beuth-Vertrieb CY - Berlin AN - OPUS4-1739 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Colla, Camilla A1 - Krause, Martin A1 - Maierhofer, Christiane A1 - Höhberger, H.-J. A1 - Sommer, H. T1 - Combination of NDT techniques for site investigation of non-ballasted railway tracks N2 - Today's civil engineering NDT needs are for quantitative, fast to apply and easy to interpret methods. They are required on site both for evaluation of existing structures/infrastructure and for quality control in new construction. With this purpose, BAM has carried out in-situ feasibility studies, using radar, impact-echo and ultrasonic-echo methods. Two examples are given of their combined application on different railway slab–track constructions, using high frequency radar, scanning impact-echo and ultrasonic array methods. The aim was to evaluate limitations and advantages, comparability and complementarity of these methods. The on-site measurements demonstrated the possibility to investigate, with good accuracy via NDT, the bonding conditions between sleepers and slab, to locate voids and measure layer thickness. The acoustic and electromagnetic methods used, were found to be complementary. KW - Concrete KW - NDT KW - Impact echo KW - Ultrasonics KW - Radar KW - Railway PY - 2002 DO - https://doi.org/10.1016/S0963-8695(01)00033-0 SN - 0963-8695 VL - 35 SP - 95 EP - 105 PB - Butterworth-Heinemann CY - Oxford AN - OPUS4-1858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Entwicklung eines luftgekoppelten Ultra-schall-Echo-Prüfverfahrens mittels fluidischer Anregung N2 - In vielen technischen Bereichen werden Ultraschallverfahren zur zerstörungsfreien Werkstoffprüfung eingesetzt. Dabei wird ein Schallpuls von einem Prüfkopf in ein Prüfobjekt eingebracht. Der Puls kann unter anderem durch Membranen oder Pie-zoelemente erzeugt werden und wird in der Regel durch direkten Kontakt oder über ein Koppelmittel an das Objekt übertragen. Luftgekoppelter Ultraschall spielt in kommerziellen Anwendungen bisher eine untergeordnete Rolle, da die Differenz der akustischen Impedanzen von Luft und Festkörpern immense Verluste beim Über-gang des Schallsignals hervorruft. In diesem Beitrag soll ein neuartiges Anregungsprinzip vorgestellt werden, mit dem ein Großteil dieser Verluste vermieden wird. Anstelle eines Festkörpers soll mit Hilfe einer fluidischen Düse Druckluft zur Signalerzeugung eingesetzt werden. In dieser Düse wird eine selbsterhaltende Strömungsinstabilität erzeugt, die einen Schallpuls von bis zu 100 kHz hervorruft, sodass der Impedanzverlust in die Umge-bungsluft entfällt. Da die charakteristische Frequenz eines fluidisch generierten Pul-ses maßgeblich von der Bauform der Düse und dem anliegenden Druck abhängt, lässt sich mittels einer geeigneten Strömungsregelung ein breiter Frequenzbereich zur Abtastung nutzen. Die so emittierten Pulse werden auf das Prüfobjekt gerichtet und die reflektierten Signale mit einem Laservibrometer an der Oberfläche des Objekts im Echo-Verfahren abgetastet. Von drei signalmindernden Materialübergängen bei gewöhnlichem luftgekoppeltem Ultraschall bleibt in dem hier vorgeschlagenen Mes-system lediglich die Grenzfläche von Luft zu Prüfkörper, sodass eine höhere Signal-ausbeute als bisher erwartet werden kann. T2 - DACH-Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Berührungsloser Ultraschall KW - Fluidische Oszillatoren KW - ZfP im Bauwesen KW - Beton PY - 2019 AN - OPUS4-50569 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weigel, Sandra A1 - Sielaff, S. A1 - Kunsic-Nowak, T. A1 - Nytus, N. A1 - Schwettmann, K. A1 - Schulze, C. A1 - Wetekam, J. T1 - Die FTIR-Untersuchung von Bitumen: Chancen, Durchführung und Präzision N2 - Die Fourier-Transformations-Infrarot-Spektroskopie (FTIR-Spektroskopie) stellt eine innovative und wirkungsvolle Methode zur Charakterisierung von Bitumen und bitumenhaltigen Bindemitteln dar. So erlaubt die FTIRCharakterisierung nicht nur eine Bewertung des Alterungsfortschritts eines Bindemittels, sondern zudem auch die Identifizierung von im Bitumen enthaltenen Additiven und Schadstoffen wie z. B. polyzyklischen aromatischen Kohlenwasserstoffen (PAK), die Ableitung verschiedener physikalischer und chemischer Kennwerte sowie weiterhin eine Klassifizierung von Bindemitteln nach verschiedenen übergeordneten Eigenschaften wie der Raffinerie, dem Alterungszustand und auch der Alterungsempfindlichkeit. KW - Bitumen und bitumenhaltige Bindemittel KW - FTIR-Spektroskopie KW - Anwendungsmöglichkeiten KW - Vergleichuntersuchung KW - Arbeitsanleitung KW - Präzision PY - 2023 UR - https://www.kirschbaum.de/fachzeitschriften/strasse-und-autobahn/strasse-und-autobahn/aktuelles-heft-17.html DO - https://doi.org/10.53184/STA8-2023-4 VL - 74/8 SP - 630 EP - 642 PB - KIRSCHBAUM VERLAG GmbH CY - Bonn AN - OPUS4-59049 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture transport and measurements at BAM N2 - An overview over material moisture measurements and modelling of building materials at BAM. T2 - Rilem TC MMS Constituent meeting CY - Rabat, Morocco DA - 09.03.2023 KW - Material moisture KW - Moisture transport KW - Sorption isotherm KW - Sorption theory KW - Diffusion coefficient KW - NMR KW - Knudsen effect PY - 2023 AN - OPUS4-57141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Imaging of nanoparticles in cells by LA-ICP-MS N2 - Studying the interaction of nanoparticles (NPs) with cells has become a growing field of interest. Research topics are ranging from nanotoxicology to medical applications e.g. as theranostic agents. In order to evaluate nano-bio interactions, the number of NPs inside cells as well as their localisation within cellular substructures is of particular interest. In recent years, elemental imaging of biological samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining more and more importance. Latest instrumental developments regarding spatial resolution (down to 1 µm) and detection efficiency make LA ICP-MS particularly interesting for single cell analysis. Here, we have applied LA-ICP-MS for sub-cellular scale imaging of individual cells to study the NP pathway from uptake, via intracellular processing up to cell division. Furthermore, the local distribution of naturally occurring elements in cells like P was measured to indicate the cell morphology. Murine fibroblast cells were incubated with different metal-containing NPs under varying experimental conditions. For LA analysis, the cells were fixed and dried. Sub-cellular resolution was achieved by careful optimisation of the laser ablation parameters. By rastering with the laser beam across the sample, a two-dimensional image of the elemental distribution can be received. Our results show that LA-ICP-MS is able to localise NP aggregates within cellular substructures. The studied NPs accumulate in the perinuclear region in the course of intracellular processing, e.g. multivesicular fusion and endosomal maturation, but do not enter the nucleus. The uptake depends on the physico-chemical properties of the nanostructures and on the incubation conditions like concentration and incubation time. Additionally, the number of NPs internalized by individual cells was determined and variations within a cell population became visible. The findings demonstrate the potential of LA-ICP-MS providing insight into NP uptake and intracellular distribution dependent on experimental parameters. T2 - Euroanalysis 2017 CY - Stockholm, Sweden DA - 28.08.2017 KW - Laser ablation KW - Nanoparticle KW - ICP-MS KW - Imaging KW - Cell PY - 2017 AN - OPUS4-41884 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Standardization in Emerging Technologies - The Case of Additive Manufacturing N2 - Additive Manufacturing provides an important enabling technology for the digital transformation of the economy. As an emerging technology it has seen a remarkable development over the last three decades. Nevertheless, it is far from a broad adoption with several barriers to overcome yet. One of the major challenges is the lack of standards. The critical role of standardization for innovation is generally recognized, still the topic too often has been neglected in strategic roadmapping exercises for emerging technologies. Too little is known about the complex dynamics and interrelations of standardization and innovation. The anticipation of standardization needs and the timely and efficient implementation of standards is challenging. This paper aims at contributing to a better understanding of the role that standards play in the multi-dimensional system of innovation. It analyzes the trajectories of innovation in Additive Manufacturing in a systematic and holistic way, focusing on standardization activities with regard to coordination, stakeholders involved, the timing and types of standards developed. Putting standardization in context of the multi-dimensional innovation system of Additive Manufacturing the research shows where standards can support the diffusion of an emerging technology. T2 - ITU Kaleidoscope Academic Conference: Challenges for a data-driven society CY - Nanjing, China DA - 27.11.2017 KW - Additive Manufacturing KW - Emerging technologies KW - Technological innovation KW - Standards KW - Standardization KW - 3D-Printing PY - 2017 SN - 978-92-61-24291-6 SN - 978-92-61-24281-7 SN - 978-92-61-24301-2 SP - 193 EP - 200 CY - Geneva AN - OPUS4-43501 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Johann, Sergej A1 - Strangfeld, Christoph ED - Chan, T. ED - Mahini, S, T1 - Embedded wireless sensor systems for long-term SHM and corrosion detection in concrete components N2 - State-of-the-art communication standards like RFID and Bluetooth Low Energy enable the development of sensor systems which can be completely embedded into concrete components for long-term SHM and early damage detection. Objective of the project KonSens which is carried out at BAM is the development, implementation, and validation of sensors for measuring of Parameters relevant for corrosion, like moisture, pH value, and electrical conductivity, inside steel reinforced concrete components. The primarily addressed application is detection and evaluation of corrosion processes in concrete bridges. In contrast to cable connected sensors, embedded wireless sensors avoid any pathways for intrusion of moisture and chemicals, e.g., chlorides which could trigger corrosion activity. To allow for long-term, ideally life-time operation, the once embedded sensor systems must work highly energy efficient. One option are passive RFID sensor systems, which work without battery. The energy is transmitted to the system through the electromagnetic field, even to operate sensors. A crucial parameter is the transmission depth in concrete. First experiments with RFID sensors working at frequencies of 13.56 MHz (HF) and 868 MHz (UHF) embedded in concrete specimen resulted positive for transmission depths of up to 13 cm, which is quite promising, considering that corrosion would appear first at the top level of rebars. A second generation of passive RFID sensor systems has been implemented with improved antenna design. Current experiments using these systems focus on the Transmission characteristics in terms of transmission depths and the impact of concrete moisture. Low-energy humidity sensors are used and analysed regarding their capability for measuring the material moisture. Additionally, a relation between transmitted power to the embedded sensor and the moisture content of the concrete specimen caused by energy absorption can be presumed and is under systematic investigation. T2 - International Conference on Structural Health Monitoring of Intelligent Infrastructure 2017 CY - Brisbane, Australia DA - 05.12.2017 KW - RFID sensors KW - Structural health monitoring KW - Sensors in concrete KW - Smart structures PY - 2017 SN - 978-1-925553-05-5 SP - 1 EP - 7 AN - OPUS4-43492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias T1 - Embedded wireless sensor systems for long-term SHM and corrosion detection in concrete components N2 - State-of-the-art communication standards like RFID and Bluetooth Low Energy enable the development of sensor systems which can be completely embedded into concrete components for long-term SHM and early damage detection. Objective of the project KonSens which is carried out at BAM is the development, implementation, and validation of sensors for measuring of Parameters relevant for corrosion, like moisture, pH value, and electrical conductivity, inside steel reinforced concrete components. The primarily addressed application is detection and evaluation of corrosion processes in concrete bridges. In contrast to cable connected sensors, embedded wireless sensors avoid any pathways for Intrusion of moisture and chemicals, e.g., chlorides which could trigger corrosion activity. To allow for long-term, ideally life-time operation, the once embedded sensor systems must work highly energy efficient. One option are passive RFID sensor systems, which work without battery. The energy is transmitted to the system through the electromagnetic field, even to operate sensors. A crucial parameter is the transmission depth in concrete. First experiments with RFID sensors working at frequencies of 13.56 MHz (HF) and 868 MHz (UHF)embedded in concrete specimen resulted positive for transmission depths of up to 13 cm, which is quite promising, considering that corrosion would appear first at the top level of rebars. A second generation of passive RFID sensor systems has been implemented with improved antenna design. Current experiments using these systems focus on the transmission characteristics in terms of transmission depths and the impact of concrete moisture. Low-energy humidity sensors are used and analysed regarding their capability for measuring the material moisture. Additionally, a relation between transmitted power to the embedded sensor and the moisture content of the concrete specimen caused by energy absorption can be presumed and is under systematic investigation. T2 - Structural Health Monitoring of Intelligent Infrastructure Conference 2017 CY - Brisbane, Australia DA - 05.12.2017 KW - RFID sensors KW - Structural health monitoring KW - Sensors in concrete KW - Smart structures PY - 2017 AN - OPUS4-43491 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kruschwitz, Sabine A1 - Munsch, Sarah Mandy A1 - Strangfeld, Christoph A1 - Wöstmann, Jens A1 - Borchardt, Kerstin T1 - Eignung zerstörungsfreier Messtechnik für die Bestimmung der Belegreife von Estrichen N2 - Die Bestimmung der Belegreife von Estrichen erfolgt im Bauwesen meist unter Verwendung von zerstörenden Verfahren, die Probenentnahmen erfordern und nur punktuelle Daten liefern. Bei anhydritgebundenen Estrichen gelten 0,5 M% und bei zementgebundenen ca. 3,5 M% und höher als belegreifer Feuchtegehalt. Die Belegreife wird als Feuchtegehalt in Masseprozent (M%) bezogen auf die Trockenmasse des Baustoffes angegeben. Zur zerstörungsfreien Feuchtemessung existieren verschiedene einfach zu bedienende Handgeräte, die u. a. auf elektrischen, elektromagnetischen und kapazitiven Methoden beruhen. In dieser Arbeit wurden ein kapazitives (Kugelsonde), ein elektromagnetisches (Mikrowellensensoren) und ein elektrisches Messverfahren (Vierelektroden-Sonde) untersucht. Mit Ausnahme der Vierelektroden-Sonde weisen die Handgeräte keine ausreichende Sensitivität in Bereichen niedriger Feuchtegehalte unterhalb von 1 M% auf und scheinen somit nicht für anhydritgebundene Estriche geeignet zu sein. Für zementgebundene Estriche lassen sich hingegen mit allen getesteten Geräten Änderungen in dem Bereich der Belegreife erfassen. In dieser Arbeit wird zusätzlich die Wasserabgabe in g/m²/Tag als Bezugsgröße herangezogen. Die Wasserabgabe stellt ein geeigneteres Maß für die Schadensträchtigkeit dar und ermöglicht direkte Vergleiche unabhängig von der verwendeten Estrichart. Für alle getesteten Estriche konnte eine Wasserabgabe von ca. 8-10 g/m²/Tag als Belegreifegrenzwert bestimmt werden. N2 - The determination of the readiness for covering of screeds in the construction industry is usually carried out by using destructive methods, which require sampling and only provide punctual data. As non-destructive testing methods, various hand tools exist, which are based on electrical and capacitive methods and are easy to handle. In this study, a capacitive spherical probe, a 4-Electrode probe in Wenner configuration and microwave probes were tested. With the exception of the 4-Electrode probe, the hand instruments do not have sufficient sensitivity in ranges of low humidity below 1 M%, and therefore do not appear to be suitable for anhydrite-bound screeds with a readiness of covering at 0.5 M%. On the other hand, for cement-bound screeds, it is possible to record changes in the range of the readiness of covering. The readiness of covering is usually stated and determined in reference to the relative moisture content. For the purpose of really assessing the risk of damage, we suggest to rather use the “water loss” in g/m²/day. Our results show in direct comparisons that value of approximately 8-10 g/m²/day is a reliable indicator for the readiness for covering of all tested screed types. KW - Estrich KW - Feuchte KW - Zerstörungsfreie Prüfung KW - Calcium-Carbid-Methode KW - Mikrowellensensoren KW - Vierelektroden-Sonde KW - Kapazitive Kugelsonde KW - Screed KW - Moisture KW - Readiness for covering KW - Non-destructive testing KW - Calcium carbide method KW - Microwave KW - 4-electrode probe KW - Capacitive spherical probe PY - 2017 DO - https://doi.org/10.1002/bate.201700051 SN - 1437-0999 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. VL - 95 IS - 4 SP - 265 EP - 274 PB - Ernst & Sohn AN - OPUS4-43169 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine A1 - Munsch, Sarah Mandy A1 - Wöstmann, Jens A1 - Strangfeld, Christoph T1 - Zerstörungsfreie Feuchtemessungen an Estrichen mittels der geophysikalischen Methoden Georadar und NMR N2 - Die Ermittlung der Belegreife von Fußbodenestrichen ist im Bauwesen von hoher Bedeutung, da es bei dem Verlegen von Parkett oder anderen Bodenbelägen auf Estrichen zu erheblichen feuchtigkeitsbedingten Schäden kommen kann, wenn diese noch nicht hinreichend getrocknet sind. Für die Messung des Feuchtegehalts wird üblicherweise auf zerstörende Methoden wie das Darr- und CM-Verfahren zurückgegriffen, die Probennahmen erfordern und nur punktuelle Informationen liefern. Ziel dieser Forschungsstudie ist die Untersuchung der Eignung und Anwendbarkeit des Georadars und der Kernspinresonanz (NMR) zur zerstörungsfreien und flächendeckenden Feuchtemessung von Estrichen. Dazu wurden Messungen mit beiden Verfahren an einer Gruppe zementgebundener (CT) und einer Gruppe anhydritgebundener (CA) Estriche während ihres Austrocknungsprozesses bei einem Konstant-Klima durchgeführt. Bei dem Radarverfahren werden Amplitude und Laufzeit elektromagnetischer Reflexionen, die durch den Wassergehalt beeinflusst werden, gemessen. Die Radarmessungen erfolgten auf jeder Probe entlang von zwei senkrechten Profilen mit einer 2GHz-Antenne. Die Kernspinresonanz steht aufgrund ihrer Abhängigkeit zur magnetischen Kernresonanz der 1H-Wasserstoffatomen in Relation mit dem Wassergehalt in dem Messvolumen der zu untersuchenden Probe. Die Untersuchungen erfolgten mit dem NMR MOUSE System in Aufsatztechnik. Dabei liegt die Eindringtiefe bei 24,8 mm. Bei den Untersuchungen lässt sich für CT-Estriche ein starker vertikaler Feuchtegradient feststellen. Die CA-Estriche weisen hingegen nur einen schwachen Feuchtegradienten bis nahezu konstante Amplituden über die gesamte Tiefe auf. Nach Erreichen einer Amplitude von ca. 5-8 lässt sich keine weitere Amplitudenveränderung registrieren bzw. sind ab diesen Zeitpunkt die Änderungen im Wassergehalt zu gering, um von der NMR aufgelöst zu werden. In den Ergebnissen des Radarverfahrens lässt sich ebenfalls ein von dem Feuchtegehalt abhängiges Verhalten der Messparameter beobachten. Mit zunehmender Trocknung kann man eine Abnahme der Laufzeit zwischen direkter und an der Rückwand reflektierter Welle messen. Die Amplituden beider Wellen hingegen nehmen während des Austrocknungsprozesses zu. Im Gegensatz zur NMR erhält man keine tiefenbezogenen Informationen. Es lassen sich aber Rückschlüsse auf den Feuchtegehalt im Gesamtvolumen ziehen. T2 - 77. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Potsdam, Germany DA - 27.03.2017 KW - Feuchtemessung KW - Estrich KW - Georadar KW - NMR PY - 2017 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-43245 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Johann, Sergej A1 - Müller, Maximilian A1 - Bartholmai, Matthias T1 - Embedded passive RFID-based sensors for moisture monitoring in concrete N2 - Damages in infrastructure due to moisture amount to billions of Euros every year. For a more predictive structural health monitoring in civil engineering, the detection and monitoring of hazardous moisture in steel reinforced concrete constructions is of high interest. The sensors have to be wireless, elsewise they weaken the concrete cover of the rebars. The lifetime of such constructions is normally decades, thus the sensors have to be battery-free and fully passive. Considering these requirements, passive RFID-based sensors are developed. Communication and energy supply are realized wireless via the electromagnetic field of a RFID transmitter. The passive RFIDbased sensors are embedded into the concrete to enable the monitoring of moisture transport in porous materials. Results of the hydration process are shown. T2 - IEEE Sensors 2017 CY - Glasgow, Scotland, UK DA - 30.10.2017 KW - Embedded sensors KW - Wireless sensors KW - Passive sensors KW - RFID-based sensors KW - Structural health monitoring KW - Moisture PY - 2017 SN - 978-1-5386-4056-2 DO - https://doi.org/10.1109/ICSENS.2017.8234166 SP - 870 EP - 872 PB - IEEE AN - OPUS4-43033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture testing and mapping N2 - Non-destructive testing of moisture in building materials T2 - NDT&E Advanced Training Workshop CY - Berlin, Germany DA - 27.06.2018 KW - Building materials KW - Concrete KW - Moisture measurement PY - 2018 AN - OPUS4-45348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Studying nanoparticle-cell interaction by ICP-MS based techniques N2 - Nanoparticles (NPs) have found a wide range of applications in research and industry. Thereby the interaction of NPs with biological systems like cells has become a major field of interest, ranging from medical applications to nanotoxicology. Size, shape and surface modification of the nanomaterials determine the uptake rate and pathway into the cells, and therefore impact specific cell components and processes. Inductively coupled plasma mass spectrometry (ICP-MS) is a well-established analytical method offering high sensitivity and multi-element capability. By coupling a laser ablation (LA) system to an ICP-MS the analysis of different kinds of solid samples is possible. In recent years, it was shown that LA-ICP-MS can provide quantitative as well as distribution information of metal containing nanoparticles (NPs) in cell samples. Here LA-ICP-MS was applied for the imaging of individual fibroblast cells to study the uptake and intracellular processing of NPs. Our results show that LA-ICP-MS can be used to localize nanoparticle aggregates within cellular compartments. The studied NPs accumulate in the perinuclear region in the course of intracellular processing, but do not enter the cell nucleus. The uptake efficiency depends strongly on the physico-chemical properties of the nanostructures as well as on the incubation conditions like concentration and incubation time. ICP-MS was used to determine the composition of the nanomaterials as well as the number of NPs in cells after acid digestion of the samples. T2 - Workshop on Reference Nanomaterials CY - Berlin, Germany DA - 14.05.2018 KW - ICP-MS KW - Laser ablation KW - Nanoparticle KW - Cell PY - 2018 AN - OPUS4-45073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Feuchtemessverfahren N2 - Discussion and presentation of different methods for moisture measurements in civil Engineering. T2 - Vorlesung Diagnostik und Ertüchtigung von Bauwerken CY - TU Berlin, Germany DA - 16.05.2018 KW - Material moisture KW - Moisture measurements PY - 2018 AN - OPUS4-44944 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Strangfeld, Christoph A1 - Maack, Stefan T1 - Verfahren und Vorrichtung zur Untersuchung einer Probe N2 - Ein Verfahren zur Untersuchung einer Probe (50) weist die Schritte des Anregens einer sich ausbreitenden mechanische Deformation (2) in der Probe (50) mittels eines fluidischen Oszillators (10), und des Bestimmens einer Charakteristik der mechanischen Deformation (2) auf. KW - Luftgekoppelter Ultraschall KW - Fluidischer Oszillator KW - Zerstörungsfreie Prüfung KW - Beton PY - 2018 SP - 1 EP - 23 CY - Berlin AN - OPUS4-44945 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Grotelüschen, Bjarne A1 - Bartholmai, Matthias A1 - Strangfeld, Christoph ED - Kossa, A. ED - Kiss, R. T1 - Towards Autonomous NDT Inspection: Setup and Validation of an Indoor Localization System N2 - Monitoring and maintenance of civil infrastructure are of great importance, as any undetected damage can cause high repair costs, unintended deadtime, or endanger structural integrity. The inspection of large concrete structures such as bridges and parking lots is particularly challenging and time-consuming. Traditional methods are mostly manual and involve mapping a grid of measurement lines to record the position of each measurement. Current semi-automated methods, on the other hand, use GPS or tachymeters for localization but still require trained personnel to operate. An entirely automated approach using mobile robots would be more cost- and time-efficient. While there have been developments in using GPS-enabled mobile robots for bridge inspection, the weak signal strength in indoor areas poses a challenge for the automated inspection of structures such as parking lots. This paper aims to develop a solution for the automated inspection of large indoor concrete structures by addressing the problem of robot localization in indoor spaces and the automated measurement of concrete cover and rebar detection. T2 - 39th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Siófok, Hungary DA - 26.09.2023 KW - NDT Inspection KW - Mobile Robot KW - Indoor Localization KW - Setup and Validation PY - 2023 SN - 978-963-421-927-9 SP - 88 EP - 89 PB - Hungarian Scientific Society of Mechanical Engineering (GTE) CY - Siófok, Hungary AN - OPUS4-58660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Tobias T1 - Classification of cement pastes with laser-induced breakdown spectroscopy N2 - In civil engineering, the investigation of existing infrastructure is of major importance for maintaining and ensuring stability of the structures. To ensure durability, uniform regulations and standards apply e.g. the European standard EN 206-1. In some countries, the EN-standard is supplemented by additional standards, as in Germany with DIN 1045-2. Here, specific application rules are described, e.g. for the cement type, to ensure the resistant to different exposures. Therefore, the knowledge of the materials originally used is important in assessing the condition of existing concrete structure. Unfortunately, these are often unknown and must be determined retrospectively. Therefore, we present the application of the laser-induced breakdown spectroscopy to distinguish between different types of cement. Spectral information’s are used to build a classification model. First, the accuracy of the classification is analyzed on ten pure laboratory cement samples. To investigate possible sources of error, the model was then applied to cement samples with different moisture content. The study shows that LIBS is a promising tool for distinguishing between cement types. For further industrial application, however, factors influencing the LIBS signal must be included to ensure a robust model. T2 - 10th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy CY - Brno, Czech Republic DA - 08.09.2019 KW - Spectroscopy KW - LIBS KW - Cement KW - Classification PY - 2019 AN - OPUS4-49253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Imaging of nanoparticles in cells by LA-ICP-MS N2 - The interaction of nanoparticles (NPs) with cells has become a major field of interest, ranging from therapeutic applications to nanotoxicology. The cellular uptake depends on the primary characteristics of the NPs (e.g. size, shape, surface modification) and on the cells interacting with the particles. Thereby the quantification of NPs in cells is of particular importance to obtain information under different experimental conditions. Presently, the number of NPs internalized is often determined by inductively coupled plasma (ICP) optical emission spectrometry (OES) or ICP mass spectrometry (MS) after acid digestion of a cell suspension or a cell pellet. The result is an average value and no information about the distribution among cells or within a cell is available. Therefore we developed a method based on laser ablation (LA) in combination with ICP-MS to localise and quantify metallic NPs in single cells. LA-ICP-MS is a powerful analytical method which offers excellent sensitivity at high spatial resolution and multielement capability without time-consuming sample preparation steps. Recently, LA-ICP-MS was established for elemental mapping of biological samples like tissues. In our experiments, fibroblast cells were incubated with gold or silver containing nanoparticles and grown on sterile coverslips under standard conditions. For LA analysis the cells were fixed with formaldehyde and dried. Subcellular resolution is achived by careful optimisation of laser energy, ablation frequency and scan speed. The elemental distribution was determined by continuous ablation line by line of cells incubated with NPs. Our results show that LA-ICP-MS is able to detect NP aggregates within cellular substructures. After 24 h of incubation the NPs were found in the cytosol, preferencially in the perinuclear region, but do not enter the nucleus. Additionally, a quantification strategy at single-cell level was developed. For this purpose nitrocellulose membrane was spiked with Ag or Au nanoparticle suspension at different concentration levels and analysed by LA-ICP-MS. Based on this calibration the number of NPs taken up by individual cells was determined and variations within the cell population become visible. The cells show a strong dependence of NP uptake on concentration and incubation time. Our results demonstrate the potential of LA-ICP-MS providing insight into NP uptake and intracellular distribution dependent on experimental parameters. T2 - Erfahrungsaustausch LA-ICP-MS mit Bayer AG CY - Berlin, Germany DA - 11.09.2017 KW - LA-ICP-MS KW - Bioimaging KW - Nanoparticles KW - Cell PY - 2017 AN - OPUS4-42575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture testing and mapping N2 - Discussion and presentation of different methods for moisture measurements in civil Engineering. T2 - NDT&E Advanced Training Workshop CY - Berlin, Germany DA - 05.07.2017 KW - Moisture measurement KW - Building materials KW - Concrete PY - 2017 AN - OPUS4-42623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Validierung und Vergleich verschiedener Methoden zur Bestimmung von Flüssigwasser in Baustoffen N2 - Darstellung der aktuellen Feuchtemesstechnik im Bauwesen. Erklärung der Grundlagen über die Sorptionsisotherme und den Wasserdampfpartialdruck. Vorstellung der Ergebnisse der korrespondierenden relativen Luftfeuchtemessungen. T2 - Abteilungsseminar der Abteilung 8, BAM CY - BAM, Berlin, Germany DA - 06.11.2017 KW - Concrete KW - Material moisture KW - Moisture measurements KW - Moisture in civil engineering KW - Corresponding relative humidity PY - 2017 AN - OPUS4-42744 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - RFID based sensors in civil engineering N2 - Damages in infrastructure due to moisture amount to billions of Euros every year. For a more predictive structural health monitoring in civil engineering, the detection and monitoring of hazardous moisture in steel reinforced concrete constructions is of high interest. The sensors have to be wireless, elsewise they weaken the concrete cover of the rebars. The lifetime of such constructions is normally decades, thus the sensors have to be battery-free and fully passive. Considering these requirements, passive RFID-based sensors are developed. Communication and energy supply are realized wireless via the electromagnetic field of a RFID transmitter. The passive RFID based sensors are embedded into the concrete to enable the monitoring of moisture transport in porous materials. Results of the hydration process are shown. T2 - RFID tomorrow & wireless IoT CY - Düsseldorf, Germany DA - 27.09.2017 KW - RFID based sensors KW - Moisture monitoring KW - Concrete KW - Embedded sensors PY - 2017 AN - OPUS4-42622 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture testing and mapping N2 - Discussion and presentation of different methods for moisture measurements in civil engineering. T2 - NDT&E Advanced Training Workshop CY - Berlin, Germany DA - 05.07.2017 KW - Building materials KW - Moisture measurements KW - Concrete PY - 2017 SP - 87 EP - 107 CY - Berlin, Germany AN - OPUS4-42624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wiggenhauser, Herbert A1 - Kind, Thomas A1 - Mielentz, Frank A1 - Strangfeld, Christoph A1 - Völker, Christoph A1 - Wilsch, Gerd T1 - Non-destructive testing in civil engineering at BAM N2 - Research and Development in Non-Destructive Testing in Civil Engineering at BAM has de-veloped over more than two decades. Highlights of present research are ultrasound phase array probes, ground penetrating radar applications for the assessment of existing structures and Laser Induced Breakdown Spec-troscopy (LIBS) to determine which chemical elements on the surface of a specimen are. RFID sensor devel-opments for wireless moisture monitoring and data fusion for the combined analysis of sensor data are fast developing areas. In addition, a selection of application cases is briefly described. T2 - Vortrag über die Aktivitäten des Fachbereichs 8.2 in der zerstörungsfreien Prüfung im Bauwesen. KW - Ultrasonic testing KW - RFID-sensors KW - Data fusion KW - Ground penetrating radar KW - LIBS PY - 2017 SP - 1 EP - 10 CY - Berlin AN - OPUS4-44132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kowarik, Stefan T1 - Artificial intelligence, the end of the world, and surface science N2 - Artificial intelligence (AI), machine learning, and neural networks have revolutionized fields such as self-driving cars or machine translation. Indeed, AI has progressed so far that scientists such as Stephen Hawking now fear that it may destroy humankind altogether. So, let’s get started and use AI in surface science. Here we train neural networks to use raw measurement data as input and immediately return the desired output parameters. We discuss the example of X-ray reflectivity measurements of ultrathin films, which contain reciprocal space information and must traditionally be fitted with dynamic scattering theory. Instead, we train the neural network with simulated X-ray data of multilayer structures and then apply it to measurement data. The neural network yields high accuracy results, is robust against noise, and performs significantly faster than fitting algorithms in real-time experiments. The presented neural network data analysis is becoming increasingly attractive, because free software has become very accessible and specialized computer chips (NPU) are currently being rolled out. T2 - DPG Früjahrstagung CY - Berlin, Germany DA - 12.03.2018 KW - X-ray reflectivity KW - AI KW - Machine learning KW - Neural network PY - 2017 AN - OPUS4-44602 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Luftgekoppelter Ultraschall mittels fluidischer Oszillatoren N2 - Das Ultraschallprüfverfahren wird im Bauwesen für die zerstörungsfreie Prüfung von Bauwerken eingesetzt, insbesondere für Strukturuntersuchungen. Dadurch sollen Lage und Größe von Bauschäden detektiert werden, um geeignete und kostengünstige Sanierungsmaßnahmen ergreifen zu können. Da in der Praxis meist nur eine einseitige Zugänglichkeit gegeben ist (z. B. Betonverschalung eines Tunnels), wird im Impuls-Echoverfahren gemessen. Dies bedeutet, dass ein Ultraschallsignal erzeugt und dessen Echo aufgenommen wird. Prüfköpfe, welche einen Oberflächenkontakt benötigen, erhöhen die benötigte Messzeit dramatisch. Mittels luftgekoppeltem Ultraschall können viele naupraktische Problem umgangen werden und die Messzeit kann deutlich reduziert werden. Als Möglichkeit zur Anregung eines luftgekoppeltem Ultraschallsignals werden fluidische Bauteile diskutiert T2 - Abteilungsseminar 8. CY - BAM, Berlin, Germany DA - 05.03.2018 KW - Luftgekoppelter Ultraschall KW - Zerstörungsfreie Prüfung im Bauwesen KW - Betonprüfung KW - Fluidische Oszillatoren PY - 2018 AN - OPUS4-44413 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia ED - Jakobs, K. ED - O'Connor, R. V. T1 - Standardization for the Industrial Internet of Things: Engagement by China, Germany and the USA N2 - Standardization is a major challenge for a successful digital transformation of manufacturing. Industry and governments have put this topic on their agenda and stakeholders worldwide are engaged in various Standard Development Organizations, consortia and fora, seeking to shape the standards for the Industrial Internet of Things (IIoT). This paper for the first time analyzes how well participants from the USA, China and Germany are actually represented and engaged in standards development for the IIoT. Using quantitative metrics, the study specifically investigates standardization activities for Wireless Sensor Networks at the Internet Engineering Taskforce (IETF). The results are divergent: Measuring the authorships of IETF Internet-Drafts, China’s successful catch-up in international standardization is confirmed, having even outperformed the USA. When it comes to the authorship of the actual standards at IETF, China could not assert its top position. Here, US authors are leading, followed by German participants. The paper discusses different engagement patterns in depth and analyzes the national economic, institutional and political backgrounds that influence them. T2 - 23rd EURAS Annual Standardisation Conference "Standards for a Smarter Future" CY - Dublin, Irland DA - 13.06.2018 KW - Wireless Sensor Networks KW - IETF KW - Standards PY - 2018 SN - 978-3-95886-229-6 SP - 145 EP - 164 PB - Verlagshaus Mainz GmbH Aachen CY - Aachen AN - OPUS4-45496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Standardization for the Industrial Internet of Things: Engagement by China, Germany and the USA N2 - Standardization is a major challenge for a successful digital transformation of manufacturing. Industry and governments have put this topic on their agenda and stakeholders worldwide are engaged in various Standard Development Organizations, consortia and fora, seeking to shape the standards for the Industrial Internet of Things (IIoT). This paper for the first time analyzes how well participants from the USA, China and Germany are actually represented and engaged in standards development for the IIoT. Using quantitative metrics, the study specifically investigates standardization activities for Wireless Sensor Networks at the Internet Engineering Taskforce (IETF). The results are divergent: Measuring the authorships of IETF Internet-Drafts, China’s successful catch-up in international standardization is confirmed, having even outperformed the USA. When it comes to the authorship of the actual standards at IETF, China could not assert its top position. Here, US authors are leading, followed by German participants. The paper discusses different engagement patterns in depth and analyzes the national economic, institutional and political backgrounds that influence them. T2 - The 3rd International Symposium on Standardization and Governance CY - Changsha, China DA - 10.07.2018 KW - Wireless Sensor Networks KW - Standards KW - IETF PY - 2018 AN - OPUS4-45498 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Standardization for the Industrial Internet of Things: Engagement by China, Germany and the USA N2 - Standardization is a major challenge for a successful digital transformation of manufacturing. Industry and governments have put this topic on their agenda and stakeholders worldwide are engaged in various Standard Development Organizations, consortia and fora, seeking to shape the standards for the Industrial Internet of Things (IIoT). This paper for the first time analyzes how well participants from the USA, China and Germany are actually represented and engaged in standards development for the IIoT. Using quantitative metrics, the study specifically investigates standardization activities for Wireless Sensor Networks at the Internet Engineering Taskforce (IETF). The results are divergent: Measuring the authorships of IETF Internet-Drafts, China’s successful catch-up in international standardization is confirmed, having even outperformed the USA. When it comes to the authorship of the actual standards at IETF, China could not assert its top position. Here, US authors are leading, followed by German participants. The paper discusses different engagement patterns in depth and analyzes the national economic, institutional and political backgrounds that influence them. T2 - 23rd EURAS Annual Standardisation Conference "Standards for a Smarter Future" CY - Dublin, Irland DA - 13.06.2018 KW - Wireless Sensor Networks KW - Standards KW - IETF PY - 2018 AN - OPUS4-45497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan A1 - Braml, T. A1 - Maack, Stefan T1 - Refining stochastic models for the reassessment of bridges using advanced NDT-methods N2 - Increasing requirements on the infrastructure caused by more and heavier traffic coincide with both the aging and the progressive degradation of bridge constructions. These exemplary issues lead to a non-negligible need for reassessments of existing bridges. Compared to the new building design, safety reserves can be used in the evaluation of such existing structures, since uncertainties that may arise during the design, construction and previous Service time are better known or no longer present. Uncertainties can be evaiuated more precisely by measurements. In the meantime, the application of advanced NDT-methods on concrete structures have become so capable, that crucial structure Parameters like certain material properties or geometrical dimensions can be quantified without significant destructive interventions. The measured data can be explicitly incorporated into the probabilistic computation models used for the bridge reassessment in form of random variables. Therewith, a previously insufficient model can be refined to achieve a higher level of approximation. This contribution emphasises two fundamental steps of the measured data based probabilistic reassessment: The sensitivity analyses to identify the cruciai Parameters and the needed accuracy of the related information as well as the comparison with expected uncertainties of non-destructively measured Parameters. T2 - 17th International Probabilistic Workshop CY - Edinburgh, UK DA - 11.09.2019 KW - Measurement KW - Reassessment KW - NDT KW - Concrete bridges PY - 2019 SP - 99 EP - 105 AN - OPUS4-48998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Refining stochastic models for the reassessment of bridges using NDT-methods N2 - Increasing requirements on the infrastructure caused by more and heavier traffic coincide with both the aging and the progressive degradation of bridge constructions. These exemplary issues lead to a non-negligible need for reassessments of existing bridges. Compared to the new building design, safety reserves can be used in the evaluation of such existing structures, since uncertainties that may arise during the design, construction and previous Service time are better known or no longer present. Uncertainties can be evaiuated more precisely by measurements. In the meantime, the application of advanced NDT-methods on concrete structures have become so capable, that crucial structure Parameters like certain material properties or geometrical dimensions can be quantified without significant destructive interventions. The measured data can be explicitly incorporated into the probabilistic computation models used for the bridge reassessment in form of random variables. Therewith, a previously insufficient model can be refined to achieve a higher level of approximation. This contribution emphasises two fundamental steps of the measured data based probabilistic reassessment: The sensitivity analyses to identify the cruciai Parameters and the needed accuracy of the related information as well as the comparison with expected uncertainties of non-destructively measured Parameters. T2 - 17th International Probabilistic Workshop CY - Edinburgh, UK DA - 11.09.2019 KW - Measurement KW - Reassessment KW - Structural safety KW - Concrete bridges KW - NDT PY - 2019 AN - OPUS4-48999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Standardization in emerging technologies - The case of additive manufacturing N2 - Additive Manufacturing provides an important enabling technology for the digital transformation of the economy. As an emerging technology it has seen a remarkable development over the last three decades. Nevertheless, it is far from a broad adoption with several barriers to overcome yet. One of the major challenges is the lack of standards. The critical role of standardization for innovation is generally recognized, still the topic too often has been neglected in strategic roadmapping exercises for emerging technologies. Too little is known about the complex dynamics and interrelations of standardization and innovation. The anticipation of standardization needs and the timely and efficient implementation of standards is challenging. This paper aims at contributing to a better understanding of the role that standards play in the multi-dimensional system of innovation. It analyzes the trajectories of innovation in Additive Manufacturing in a systematic and holistic way, focusing on standardization activities with regard to coordination, stakeholders involved, the timing and types of standards developed. Putting standardization in context of the multi-dimensional innovation system of Additive Manufacturing the research shows where standards can support the diffusion of an emerging technology. T2 - ITU Kaleidoscope Academic Conference: Challenges for a data-driven society CY - Nanjing, China DA - 27.11.2017 KW - 3D-Printing KW - Additive Manufacturing KW - Emerging technologies KW - Standardization KW - Standards KW - Technological innovation PY - 2017 AN - OPUS4-49082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej T1 - Smart electronic helper for long term monitoring of bridges and building structures N2 - Increasing traffic volume on the one hand and ageing infrastructure on the other hand have created many new challenges for maintenance and structural health monitoring of roads and bridges. In the past, many bridges and road structures have been neglected, often resulting in traffic congestion, road closure, and increased repair costs. This research is concerned with the development of a system to improve the challenge of maintenance and early detection of damage, particularly moisture penetration and corrosion of steel reinforced concrete components. The objective is to develop a method that will also work after 30 years and longer. Many new IoT solutions are equipped with internal energy storage elements (accumulators or batteries) which are inappropriate here, since most relevant signs of concrete degradation occur after decades, where the functioning of such elements are more than questionable. The presented technology approach uses radio-frequency identification (RFID) and enables connectivity to sensors. It offers the advantage of an passive, completely independent energy supply without any energy storage components. Since the system should be permanently embedded in concrete, it is crucial to develop a long-term stable device which is adapted to the environmental influences of the structure, e.g., long-term resistance in very alkaline environment of pH 13. In numerous experiments, the robustness of the system was tested and evaluated. Various tests with encapsulations to protect the electronics were performed, and for long-term validation different concrete specimens were instrumented with RFID-sensor-systems. Their operating time is now around two years and investigations for signs of fatigue and damage to the encapsulation and the electronics are ongoing. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures (SMAR 2019) CY - Potsdam, Germany DA - 27.08.2019 KW - Passive RFID KW - Sensors KW - SHM KW - Long term monitoring KW - Smart structures PY - 2019 AN - OPUS4-48832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia A1 - Blind, K. ED - Jakobs, K. ED - Morone, P. T1 - Testbeds for standardization in the IIoT N2 - In the paper, we discuss the role and impacts of testbeds in standardization for the industrial internet of things. Based on a multiple case study, four different approaches were identified followed in the testbeds with regard to their standardization activities. T2 - 24th EURAS Annual Standardisation Conference CY - Rom, Italy DA - 13.06.2019 KW - IIoT KW - Industrie 4.0 KW - Normen KW - Standards KW - Normung KW - Standardization KW - Agile KW - Testbed PY - 2019 SN - 978-3-95886-282-1 SP - 215 EP - 234 PB - Verlagshaus Mainz CY - Aachen AN - OPUS4-49121 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dudek, Gabriele T1 - Accreditation, conformity assessment and national Quality Infrastructure - The system in Germany and areas of research N2 - The presntation gives an overview of the QI System in Germany and Europe, especially accreditation and conformity assessment. It further highlights some areas of research conducted in BAM with regard to elements of QI. T2 - National Quality Infrastructure • Beijing Forum CY - Peking, People's Republic of China DA - 08.01.2019 KW - QI KW - Accreditation KW - Quality infrastructure KW - Qualitätsinfrastruktur KW - Conformity assessment KW - Konformitätsbewertung KW - Akkreditierung PY - 2019 AN - OPUS4-49123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona T1 - Vorstellung BAM-Initiative QI-FoKuS N2 - Vorstellung der BAM und der Initiative QI-FoKuS bei dem VDA mit einem Schwerpunkt auf die am 30.09.2019 startende Unternehmensbefragung zu Nutzung und Wirkung von Managementsystemen T2 - VDA: Sitzung III / 2019 des Ausschusses Qualitätsmanagement (QMA) CY - Berlin, Germany DA - 25.09.2019 KW - Konformitätsbewertung KW - Managementsysteme KW - ISO/IEC 27001 PY - 2019 AN - OPUS4-49116 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Accreditation, conformity assessment and national quality infrastructure - The system in Germany and areas of research N2 - The presentation gives an overview and some examples of research projects conducted at BAM (Department S.2) in the field of QI T2 - National Quality Infrastructure • Beijing Forum CY - Peking, People's Republic of China DA - 08.01.2019 KW - QI KW - Qualitätsinfrastruktur KW - Quality infrastructure KW - Conformity assessment KW - Konformitätsbewertung KW - Standardization KW - Normung KW - Akkreditierung KW - Accreditation PY - 2019 AN - OPUS4-49124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Water content in construction materials N2 - Discussion of material moisture and moisture transport in liquid and vapour phase. Prediction of the pore saturation in partially saturated pores in building materials. T2 - 5. Herbstschule Competence Center for Material Moisture CY - Ettlingen, Germany DA - 08.10.2019 KW - Material moisture KW - Building materials KW - Embedded sensors KW - Partially saturated pores PY - 2019 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-49260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Correlation between the electric impedance and the water layer thickness in partially saturated screed samples N2 - Discussion of material moisture in liquid and vapour phase. Prediction of the pore saturation in partially saturated pores in building materials. Correlation between the electric impedance and the water layer thickness in partially saturated screed samples. T2 - 10. CMM Tagung CY - Ettlingen, Germany DA - 10.10.2019 KW - Embedded sensors KW - Corresponding relative humidity KW - Electrical impedance KW - Material moisture KW - Building materials KW - Partiallly saturated pores PY - 2019 AN - OPUS4-49261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Alhadad, Mohamad Saddik T1 - Entwicklung und Validierung eines luftgekoppelen Impakt-Echo-Messverfahrens mittels fluidischer Anregung N2 - Die steigende Nachfrage von zerstörungsfreien Prüfverfahren, welche die Zeitinvestition verbessern und eine kontinuierliche Messung ermöglichen, erfordert die Entwicklung des luftgekoppltes Impakt-Echo-Messverfahrens. Diese Entwicklung kann durch die fluidische Anregung ermöglicht werden. Das Ziel dieser vorliegenden Arbeit war der Aufbau einer Messapparatur, die auf Schnelligkeit setzt und kontinuierlich misst. Nach der Durchführung der fluidischen Anregung wurden mit Hilfe eines Laservibrometers die Daten aufgenommen. Zur Analysierung der auf diese Weise erhobenen Messwerte wurden sie mittels der Fast-Fourier-Transformation in den Frequenzbereich transformiert. Für den Zweck der Validierung wurden Zylinder-Probekörper und Platten-Probekörper wurden verwendet. Die Messungen an den Zylinder-Probekörpern lieferten erfolgreiche Ergebnisse, während die Messungen an den Platten-Probekörpern weitere Untersuchung und Entwicklung benötigten werden. KW - Bauwesen KW - Delamination KW - Kontaktloses Impakt-Echo KW - Dickenbestimmung PY - 2019 SP - 1 EP - 87 CY - Berlin AN - OPUS4-50320 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hauke, Max T1 - Entwicklung eines Versuchsstandes zur Dickenbestimmung von Werkstoffen mithilfe von frequenzmoduliertem Ultraschall N2 - Die vorliegende Arbeit beschäftigt sich mit der Entwicklung eines Versuchsstandes zur Di-ckenbestimmung von Werkstoffen mithilfe von frequenzmoduliertem luftgekoppelten Ultra-schall. Zur Erzeugung des frequenzmoduliertem Signals wird ein fluidischer Oszillator ver-wendet. Die Schwingungsfrequenz des Oszillators ist von der Größe, der Geometrie und den Druckverhältnissen im Oszillator abhängig, welche durch ein Druckventil veränderbar sind. Zur Datenfassung dienen zwei Laservibrometer. Weiterhin soll die schlussendliche Dicken-bestimmung mithilfe eines Kreuzkorrelationsverfahrens erreicht werden. Während der Ent-wicklung wurden Messungen im Medium Luft, als auch mit Polyamid-Probekörpern durchge-führt. Für die Luftmessungen wurde das Ultraschallsignal an zwei Messpunkten erfasst und der Abstand zwischen diesen Messpunkten daraufhin versucht zu ermitteln. Diese Abstand-messungen wurden mit unterschiedlichen Abständen von 6 bis 15 Zentimeter durchgeführt, wobei der Abstand anhand der Daten mit einer Abweichung von unter einem Zentimeter er-folgreich bestimmt werden konnte. Die Messungen am Probekörper waren weniger Erfolg-reich, da keine reproduzierbare Dickenbestimmung erreicht werden konnte. Trotzdem kann die Entwicklung aufgrund der erfolgreichen Abstandmessung in der Luft sowie den neuen Erkenntnissen aus den Messungen am Probekörper als Erfolg betrachtet werden. KW - Berührungsloser Ultraschall KW - Bauwesen KW - Frequenzmodulation KW - Fluidische Anregung PY - 2019 SP - 1 EP - 74 CY - Berlin AN - OPUS4-50219 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Testbeds for standardization in the IIoT N2 - The poster presents our research findings on the role and impacts of testbeds in standardization for the industrial internet of things. Based on a multiple case study, four different approaches were identified followed in the testbeds with regard to their standardization activities. T2 - EU BRIDGIT2 Project - National Event Bridging the Innovation Gap Between Research & Market Impact using Standardisation CY - Dublin, Ireland DA - 11.09.2019 KW - Normen KW - Normung KW - Standards KW - Standardization KW - Industrie 4.0 KW - Testumgebung KW - IIoT KW - Testbed PY - 2019 AN - OPUS4-50086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - The German Conformity Assessment Panel N2 - The presentation summarizes the economic research activities at Department S concerning Quality Infrastructure. It introduces the new tool "QI-FoKuS" - an annual company survey in Germany, seeking to provide data on conformity assessment and accreditation in Germany. The first company survey deals with the use and certification of management systems with a special focus on information security and the criteria for the selection of certification bodies. T2 - Visit & Workshop at CCAI CY - Beijing, China DA - 10.01.2019 KW - Confromity Assessment KW - Konformitätsbewertung KW - Umfrage KW - Certification KW - Zertifizierung KW - Qualitätsinfrastruktur KW - QI-FoKuS PY - 2019 AN - OPUS4-50089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim A1 - Strangfeld, Christoph A1 - Ritzer, Tobias A1 - Kruschwitz, Sabine ED - Littmann, K. T1 - Zerstörungsfreie Lokalisierung von Flüssigwasser in Fußböden durch Kombination von Radar und Neutronensonde N2 - Das Neutronensondenverfahren wird bereits seit vielen Jahren erfolgreich zur Eingrenzung und Quantifizierung auftretender Feuchteschäden an Fußböden eingesetzt. Hierzu bedarf es jedoch einer Vielzahl zerstörender Sondierungsbohrungen, welche die gewonnenen Messdaten kalibrieren und eine Tiefenzuordnung des Flüssigwassers zulassen. Dadurch entsteht ein zeitlicher und finanzieller Aufwand, der durch den parallelen Einsatz des elektromagnetischen Radarverfahrens vermieden werden könnte. Mit seiner hohen Sensitivität für Wasser bietet diese Messmethode die Möglichkeit der vertikalen Lokalisierung von Feuchte, was zu einer automatisierten Klassifizierung typischer Schadensfälle beitragen soll. In einem laufenden Forschungsvorhaben werden in systematischen Laborstudien gängige Schadensfälle an häufig anzutreffenden Fußbodenaufbauten simuliert und deren Einfluss auf die genannten Verfahren untersucht. Hierbei kommen Zement- und Anhydritestriche, sowie unterschiedliche Dämmmaterialen mit variierenden Schichtdicken zum Einsatz. Wesentlicher Bestandteil der Auswertung ist die Extraktion signifikanter Signalmerkmale des Radarverfahrens, welche Rückschlüsse auf den Schadensfall und ggf. die Wassermenge zulassen. Weiterführend sollen die Kombinationsmöglichkeiten der verschiedenen Signalmerkmale und der Neutronensondendaten durch Methoden der multivariaten Datenauswertung und des maschinellen Lernens geprüft werden. Die Unabhängigkeit gegenüber wechselnden Schichtdicken und Materialien steht hierbei besonders im Fokus und soll anhand der erzielten Ergebnisse evaluiert werden. T2 - 10. Kolloquium Industrieböden - Fachtagung über stark beanspruchte Bodenkonstruktionen CY - Esslingen, Germany DA - 03.03.2020 KW - Radar KW - Feuchte KW - Neutronensonde PY - 2020 SN - ISBN 978-3-8169-8505-1 (ePDF) SN - ISBN 978-3-8169-3505-6 (Print) SP - 179 EP - 185 PB - Expert Verlag CY - Tübingen AN - OPUS4-50589 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Zerstörungsfreie Prüfung im Bauwesen - eine zuverlässige Informationsquelle N2 - Inhalt der Präsentation: - Einführung in das Prinzip der Laufzeitmessung - Vorteile bei der Anwendung von Volumenverfahren an Spannbetonbrücken - Möglichkeiten zur Beurteilung der Leistungsfähigkeit von ZfP-Verfahren und zur Verwendung der Messergebnisse in probabilistischen Nachweisen von Bestandstragwerken T2 - Fachtagung ZfPStatik 2020 CY - Munich, Germany DA - 18.02.2020 KW - Zerstörungsfreie Prüfung im Bauwesen KW - Messunsicherheit KW - Nachrechnung KW - Beurteilung von Bestandstragwerken PY - 2020 AN - OPUS4-50417 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Zerstörungsfreie Lokalisierung von Flüssigwasser in Fußböden durch Kombination von Radar und Neutronensonde N2 - Das Neutronensondenverfahren wird bereits seit vielen Jahren erfolgreich zur Eingrenzung und Quantifizierung auftretender Feuchteschäden an Fußböden eingesetzt. Hierzu bedarf es jedoch einer Vielzahl zerstörender Sondierungsbohrungen, welche die gewonnenen Messdaten kalibrieren und eine Tiefenzuordnung des Flüssigwassers zulassen. Dadurch entsteht ein zeitlicher und finanzieller Aufwand, der durch den parallelen Einsatz des elektromagnetischen Radarverfahrens vermieden werden könnte. Mit seiner hohen Sensitivität für Wasser bietet diese Messmethode die Möglichkeit der vertikalen Lokalisierung von Feuchte, was zu einer automatisierten Klassifizierung typischer Schadensfälle beitragen soll. In einem laufenden Forschungsvorhaben werden in systematischen Laborstudien gängige Schadensfälle an häufig anzutreffenden Fußbodenaufbauten simuliert und deren Einfluss auf die genannten Verfahren untersucht. Hierbei kommen Zement- und Anhydritestriche, sowie unterschiedliche Dämmmaterialen mit variierenden Schichtdicken zum Einsatz. Wesentlicher Bestandteil der Auswertung ist die Extraktion signifikanter Signalmerkmale des Radarverfahrens, welche Rückschlüsse auf den Schadensfall und ggf. die Wassermenge zulassen. Weiterführend sollen die Kombinationsmöglichkeiten der verschiedenen Signalmerkmale und der Neutronensondendaten durch Methoden der multivariaten Datenauswertung und des maschinellen Lernens geprüft werden. Die Unabhängigkeit gegenüber wechselnden Schichtdicken und Materialien steht hierbei besonders im Fokus und soll anhand der erzielten Ergebnisse evaluiert werden. T2 - 10. Kolloquium Industrieböden CY - Esslingen, Germany DA - 03.03.2020 KW - Radar KW - Feuchte KW - Neutronensonde PY - 2020 AN - OPUS4-50590 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ecke, Alexander A1 - Bell, Jérémy A1 - Schneider, Rudolf T1 - A three-dimensional microfluidic flow cell and system integration for improved electrochemical substrate detection in HRP/TMB-based immunoassays N2 - Immunoassays, based on the recognition and capture of analytes by highly selective antibodies, are now used extensively in all areas of diagnostics, but the challenge is to further integrate them into online sensors. To improve the transition from laboratory immunoassays to immunosensors, we have developed a complete flow system, based on a microfluidic core flow cell to enable automated detection of one of the most commonly used immunoassay substrates, TMB, by chronoamperometry. The architecture and fluidic optimisation of the system showed that a specially designed 3D flow cell allows higher flow rates (500 μL min−1) than a standard enlarged microfluidic channel (50 μL min−1) resulting in a significantly shorter detection time of 30 seconds per sample and making the system more robust against interferences due to bubble formation in the chip. The electrochemical measurements showed an improved signal-to-noise ratio (SNR) and thus higher sensitivity for a model immunoassay for diclofenac (SNR = 59), compared to the analytical performance of a conventional laboratory microplate-based assay with optical detection (SNR = 19). In general, this system facilitates the conversion of any conventional immunoassay into an immunosensor with automatic and continuous detection. KW - Microfluidic KW - Immunoassay KW - Electrochemical KW - Mikrofluidik KW - Immunassay KW - Elektrochemie PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580159 DO - https://doi.org/10.1039/d3sd00095h VL - 2 SP - 887 EP - 892 PB - Royal Society of Chemistry CY - London, United Kingdom AN - OPUS4-58015 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reuter, T. A1 - Borges de Oliveira, F. A1 - Abt, Ch. A1 - Ballach, F. A1 - Bartscher, M. A1 - Bellon, Carsten A1 - Dennerlein, F. A1 - Fuchs, P. A1 - Günnewig, O. A1 - Hausotte, T. A1 - Hess, J. A1 - Kasperl, S. A1 - Maass, N. A1 - Kimmig, W. A1 - Schielein, R. A1 - von Schmid, M. A1 - Suppes, A. A1 - Wagner, G. A1 - Watzl, Ch. A1 - Wohlgemuth, F. T1 - Introduction to “Realistic Simulation of real CT systems with a basic-qualified Simulation Software - CTSimU2“ N2 - The lack of traceability to meter of X-ray Computed Tomography (CT) measurements still hinders a more extensive acceptance of CT in coordinate metrology and industry. To ensure traceable, reliable, and accurate measurements, the determination of the task-specific measurement uncertainty is necessary. The German guideline VDI/VDE 2630 part 2.1 describes a procedure to determine the measurement uncertainty for CT experimentally by conducting several repeated measurements with a calibrated test specimen. However, this experimental procedure is cost and effort intensive. Therefore, the simulation of dimensional measurement tasks conducted with X-ray computed tomography can close these drawbacks. Additionally, recent developments towards a resource and cost-efficient production (“smart factory”) motivate the need for a corresponding numerical model of a CT system (“digital twin”) as well. As there is no standardized procedure to determine the measurement uncertainty of a CT system by simulation at the moment, the project series CTSimU was initiated, aiming at this gap. Concretely, the goal is the development of a procedure to determine the measurement uncertainty numerically by radiographic simulation. The first project (2019-2022), "Radiographic Computed Tomography Simulation for Measurement Uncertainty Evaluation - CTSimU" developed a framework to qualify a radiographic simulation software concerning the correct simulation of physical laws and functionalities. The most important outcome was a draft for a new guideline VDI/VDE 2630 part 2.2, which is currently under discussion in the VDI/VDE committee. The follow-up project CTSimU2 "Realistic Simulation of real CT systems with a basic-qualified Simulation Software" will deal with building and characterizing a digital replica of a specific real-world CT system. The two main targets of this project will be a toolbox including methods and procedures to configure a realistic CT system simulation and to develop tests to check if this replica is sufficient enough. The result will be a draft for a follow-up VDI/VDE guideline proposing standardized procedures to determine a CT system's corresponding characteristics and test the simulation (copy) of a real-world CT system which we call a "digital twin". T2 - 12th Conference on Industrial Computed Tomography (iCT) 2023 CY - Fürth, Germany DA - 27.02.2023 KW - dXCT KW - X-ray computed tomography KW - Simulation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-589204 DO - https://doi.org/10.58286/27715 VL - 28 IS - 3 SP - 1 EP - 5 PB - NDT.net AN - OPUS4-58920 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruibal, C. A1 - Gueidan, C. A1 - Selbmann, L. A1 - Gorbushina, Anna A1 - Crous, P.W. A1 - Groenewald, J.Z. A1 - Muggia, L. A1 - Grube, M. A1 - Isola, D. A1 - Schoch, C.L. A1 - Staley, J.T. A1 - Lutzoni, F. A1 - De Hoog, G.S. T1 - Phylogeny of rock-inhabiting fungi related to Dothideomycetes N2 - The class Dothideomycetes (along with Eurotiomycetes) includes numerous rock-inhabiting fungi (RIF), a group of ascomycetes that tolerates surprisingly well harsh conditions prevailing on rock surfaces. Despite their convergent morphology and physiology, RIF are phylogenetically highly diverse in Dothideomycetes. However, the positions of main groups of RIF in this class remain unclear due to the lack of a strong phylogenetic framework. Moreover, connections between rock-dwelling habit and other lifestyles found in Dothideomycetes such as plant pathogens, saprobes and lichen-forming fungi are still unexplored. Based on multigene phylogenetic analyses, we report that RIF belong to Capnodiales (particularly to the family Teratosphaeriaceae s.l.), Dothideales, Pleosporales, and Myriangiales, as well as some uncharacterised groups with affinities to Dothideomycetes. Moreover, one lineage consisting exclusively of RIF proved to be closely related to Arthoniomycetes, the sister class of Dothideomycetes. The broad phylogenetic amplitude of RIF in Dothideomycetes suggests that total species richness in this class remains underestimated. Composition of some RIF-rich lineages suggests that rock surfaces are reservoirs for plant-associated fungi or saprobes, although other data also agree with rocks as a primary substrate for ancient fungal lineages. According to the current sampling, long distance dispersal seems to be common for RIF. Dothideomycetes lineages comprising lichens also include RIF, suggesting a possible link between rock-dwelling habit and lichenisation. KW - Arthoniomycetes KW - Capnodiales KW - Dothideomycetes KW - Evolution KW - Extremotolerance KW - Multigene phylogeny KW - Rock-inhabiting fungi PY - 2009 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-219821 DO - https://doi.org/10.3114/sim.2009.64.06 SN - 0166-0616 VL - 64 IS - 1 SP - 123 EP - 133 PB - Centraalbureau voor Schimmelcultures CY - Utrecht, The Netherlands AN - OPUS4-21982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Urban, Klaus A1 - Ackerhans, C. A1 - Gorbushina, Anna T1 - Analysis of Carbon and Nitrogen from Atmospheric Sources by Bulk Deposition Sampling at various locations in Germany N2 - Atmospheric deposition of particulate matter is an important indicator of air pollution and a significant factor in material surface fouling. The elemental composition of this nutrient-containing dust depends largely on the exposure region and time as well as on climate. Therefore, in this paper we report an analysis of atmospheric pollutions with a self-made low-cost bulk deposition sampler directed at sampling deposition via air transport and rainfall. We used the device in diverse environments - thus comparing an urban region, an area surrounded by forest and an area mainly dominated by agriculture. The total organic carbon (TOC) and total nitrogen (TN) amounts were selected as indicator parameters and analyzed in a biweekly rhythm for three and a half and two years, respectively. The TOC value responded to particulate matter in the urban area, especially significant were the influences of the New Year's firework in urban and pollen in the rural forest area. In contrast, the TN value was more under the influence of the nitrogen emissions in the agriculture-dominated area. However, the TN value did not correlate with the NOx values in the urban area because the atmospheric nitrogen emissions in the city might originate from various emission sources. Summarizing, the TOC and TN values of the self-made low-cost bulk deposition sampler were in good agreement with environmental events of their immediate surrounding. Moreover, the selected containers and sampling procedures are universally applicable to monitor and analyze organic as well as inorganic parameters (e.g. metal ions) of atmospheric deposition. KW - Passive sampling KW - Biomonitoring KW - Air Analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-609373 DO - https://doi.org/10.1016/j.envadv.2024.100583 SN - 2666-7657 VL - 17 SP - 1 EP - 9 PB - Elsevier Ltd. AN - OPUS4-60937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Standardization in emerging technologies - The case of additive manufacturing N2 - Additive Manufacturing provides an important enabling technology for the digital transformation of the economy. As an emerging technology it has seen a remarkable development over the last three decades. Nevertheless, it is far from a broad adoption with several barriers to overcome yet. One of the major challenges is the lack of standards. The critical role of standardization for innovation is generally recognized, still the topic too often has been neglected in strategic roadmapping exercises for emerging technologies. Too little is known about the complex dynamics and interrelations of standardization and innovation. The anticipation of standardization needs and the timely and efficient implementation of standards is challenging. This paper aims at contributing to a better understanding of the role that standards play in the multi-dimensional system of innovation. It analyzes the trajectories of innovation in Additive Manufacturing in a systematic and holistic way, focusing on standardization activities with regard to coordination, stakeholders involved, the timing and types of standards developed. Putting standardization in context of the multi-dimensional innovation system of Additive Manufacturing the research shows where standards can support the diffusion of an emerging technology. T2 - 22nd EURAS Annual Standardisation Conference: Digitalisation: Challenge and Opportunity for Standardisation CY - Berlin, Germany DA - 28.06.2017 KW - 3D Printing KW - Additive manufacturing KW - Emerging technologies KW - Innovation KW - Standards PY - 2017 AN - OPUS4-46032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Standardization in emerging technologies - The case of additive manufacturing N2 - Additive Manufacturing provides an important enabling technology for the digital transformation of the economy. As an emerging technology it has seen a remarkable development over the last three decades. Nevertheless, it is far from a broad adoption with several barriers to overcome yet. One of the major challenges is the lack of standards. The critical role of standardization for innovation is generally recognized, still the topic too often has been neglected in strategic roadmapping exercises for emerging technologies. Too little is known about the complex dynamics and interrelations of standardization and innovation. The anticipation of standardization needs and the timely and efficient implementation of standards is challenging. This paper aims at contributing to a better understanding of the role that standards play in the multi-dimensional system of innovation. It analyzes the trajectories of innovation in Additive Manufacturing in a systematic and holistic way, focusing on standardization activities with regard to coordination, stakeholders involved, the timing and types of standards developed. Putting standardization in context of the multi-dimensional innovation system of Additive Manufacturing the research shows where standards can support the diffusion of an emerging technology. T2 - ITU Kaleidoscope Academic Conference: Challenges for a data-driven society CY - Nanjing, China DA - 27.11.2017 KW - 3D-Printing KW - Additive Manufacturing KW - Emerging technologies KW - Standardization KW - Standards KW - Technological innovation PY - 2017 AN - OPUS4-46033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weise, Frank A1 - Millar, Steven A1 - Wilsch, Gerd T1 - Analyse des Tausalzeintrags in Fahrbahndeckenbetone mit neuartiger Prüftechnik T1 - Analysis of De-icing Salt in Concrete Pavement with a new type of Test Technology N2 - In den letzten Jahren sind im deutschen Bundesautobahnnetz vermehrt AKR-Schäden an Betonfahrbahndecken aufgetreten. Ursächlich hierfür ist die Verwendung alkaliempfindlicher Gesteinskörnung. Dies führt bei gleichzeitiger Anwesenheit von Wasser infolge der Exposition der Fahrbahndecke und des alkalischen Milieus durch den Einsatz alkalireicher Portlandzemente bei der Betonherstellung zu einer Alkali-Kieselsäure-Reaktion (AKR). Zusätzlich wird der AKR-Schädigungsprozess in Betonfahrbahndecken durch den externen Tausalzeintrag (primär NaCl) im Winter begünstigt. Vor diesem Hintergrund kommt der Ermittlung des Tausalzeintrags in den Fahrbahndeckenbeton eine große Bedeutung zu. Die Analyse des Tausalzeintrags erfolgte bisher ausschließlich nasschemisch an gemahlenen Bohrkernsegmenten. Nachteilig sind hierbei der relativ hohe prüftechnische Aufwand und die eingeschränkte Ortsauflösung. Der alternative Einsatz von LIBS (Laser-induced breakdown spectroscopy) eröffnet in diesem Kontext neue Möglichkeiten. So wird in diesem Beitrag anhand von Bohrkernen aus einem repräsentativen AKR-geschädigten BAB-Abschnitt exemplarisch die Vorgehensweise bei der LIBS-Analyse zur Ermittlung der Na- und Cl-Verteilung an vertikalen Schnittflächen von Bohrkernen aufgezeigt. Da der Tausalzeintrag primär über den Zementstein erfolgt, wurde der verfälschende Na-Grundgehalt der Gesteinskörnung mittels eines Ausschlusskriteriums (Ca-Gehalt) eliminiert. Vergleichend durchgeführte Cl-Mappings mit Mikroröntgenfluoreszenzanalyse sowie nasschemische Analysen belegen die Güte der durchgeführten LIBS-Messungen. Allerdings bedarf es bei der quantitativen Ermittlung des Natriumgehaltes in der Betonfahrbahndecke noch weitergehender Untersuchungen. N2 - Analysis of the intrusion of de-icing salt into concrete pavements by a novel test method In recent years the German motorway network has seen an increase in the occurrence of damage in concrete pavements. This has been caused by the use of alkali-sensitive aggregates. Given the exposure of the concrete pavement to water and the alkaline environment caused by the use of Portland cement during concrete mixing, this environment can lead to an alkali-silica reaction (ASR) process. This ASR-damage process in concrete pavements is further exacerbated by the external application of de-icing salt in winter. Against this background, the evaluation of the intrusion of de-icing salt becomes of great importance. Until now, the analysis of the intrusion of de-icing salt was carried out in a wet-chemistry process on finely ground segments of drilling cores. The disadvantages of this method are the relatively arduous testing process and the limited depth resolution. The alternative application of LIBS (laser-induced breakdown spectroscopy) offers new possibilities in this context. In this paper, the procedure for the LIBS analysis of sodium and chloride distribution on vertical cut surfaces of drilling cores taken from representative ASR-damaged concrete pavements is presented. Because the intrusion of de-icing salt takes place primarily in the cement matrix, the distorting effect of the sodium content in the aggregates was eliminated by an exclusion criteria (namely, the calcium content). The comparable chloride mappings by micro X-ray fluorescence spectroscopy and wet-chemical analysis confirm the quality of the LIBS measurements. However, additional investigations are necessary for the quantitative analysis of sodium content in concrete pavements. KW - Betonfahrbahndecke KW - Alkali-Kieselsäure-Reaktion KW - Tausalz KW - LIBS KW - MRFA KW - Nasschemie KW - ZfP PY - 2018 DO - https://doi.org/10.1002/best.201800033 SN - 0005-9900 SN - 1437-1006 VL - 113 IS - 9 SP - 656 EP - 666 PB - Wilhelm Ernst & Sohn, Verlag für Architektur und technische Wissenschaften GmbH & Co. KG CY - Berlin AN - OPUS4-46171 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Küttenbaum, Stefan A1 - Maack, Stefan A1 - Taffe, A. T1 - Structural safety referring to ultrasound on concrete bridges N2 - Measuring means knowing. The structural engineer’s Knowledge about structures is vitally important for the assessment of their structural safety. This contribution shows, how non-destructive testing methods can be used to collect valuable Information about existing structures. This value is expressed in this paper by the usability in probabilistic assessments and thus by the reliability of the information. The development of non-destructive testing methods in civil-engineering allows the realistic measurement and visualization of inner constructions of concrete components with a minimum of destructive interventions. The evaluation of the quality of measurement data is of fundamental importance for quantitative measurements in order to ensure the objectivity of testing and evaluation and to assess the reliability of the knowledge acquired. Both systematic and random deviations must be identified, quantified and taken into account to obtain statistically sound data. The Focus of this contribution is on the methodical path, how displayed measurement data can be processed into reliable knowledge. It is not about developing assessment methods but about providing necessary knowledge to increase their operational usability. T2 - 16th International Probabilistic Workshop CY - Vienna, Austria DA - 12.09.2018 KW - NDT KW - Reassessment KW - Probabilistic KW - Non-destructive testing in civil engineering PY - 2018 DO - https://doi.org/10.1002/best.201800034 SN - 1437-1006 VL - 113 IS - S2 SP - 7 EP - 13 PB - Ernst & Sohn Verlag für Architektur und technische Wissenschaften GmbH & Co. KG CY - Berlin AN - OPUS4-46143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Structural safety referring to ultrasound on concrete bridges N2 - Measuring means knowing. The structural engineer’s Knowledge about structures is vitally important for the assessment of their structural safety. This contribution shows, how non-destructive testing methods can be used to collect valuable Information about existing structures. This value is expressed in this paper by the usability in probabilistic assessments and thus by the reliability of the information. The development of non-destructive testing methods in civil-engineering allows the realistic measurement and visualization of inner constructions of concrete components with a minimum of destructive interventions. The evaluation of the quality of measurement data is of fundamental importance for quantitative measurements in order to ensure the objectivity of testing and evaluation and to assess the reliability of the knowledge acquired. Both systematic and random deviations must be identified, quantified and taken into account to obtain statistically sound data. The Focus of this contribution is on the methodical path, how displayed measurement data can be processed into reliable knowledge. It is not about developing assessment methods but about providing necessary knowledge to increase their operational usability. T2 - 16th International Probabilistic Workshop CY - Vienna, Austria DA - 12.09.2018 KW - NDT KW - Reassessment KW - Probabilistic KW - Non-destructive testing in civil engineering KW - Existing bridges PY - 2018 AN - OPUS4-46144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Reliability assessment of existing bridges based on NDT-results N2 - The non-destructive testing methods available for civil engineering (NDT-CE) enable the measurements of quantitative parameters, which realistically describe the characteristics of existing buildings. In the past, methods for quality evaluation and concepts for validation expanded into NDT-CE to improve the objectivity of measured data. Thereby, a metrological foundation was developed to collect statistically sound and structurally relevant information about the inner construction of structures without destructive interventions. More recently, the demand for recalculations of structural safety was identified. This paper summarizes a basic research study on structural analyses of bridges in combination with NDT. The aim is to use measurement data of nondestructive testing methods as stochastic quantities in static calculations. Therefore, a methodical interface between the guide to the expression of uncertainty in measurement and probabilistic approximation procedures (e.g. FORM) has been proven to be suitable. The motivation is to relate the scientific approach of the structural analysis with real information coming from existing structures and not with those found in the literature. A case study about the probabilistic bending proof of a reinforced concrete bridge with statistically verified data from ultrasonic measurements shows that the measuring results fulfil the requirements concerning precision, trueness, objectivity and reliability. T2 - 5th ICCRRR 2018 - International Conference on Concrete Repair, Rehabilitation and Retrofitting CY - Cape Town, South Africa DA - 19.11.2018 KW - NDT KW - Concrete KW - Stochastic model KW - Reassessment KW - Reliability PY - 2018 AN - OPUS4-46768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Zerstörungsfreie Prüfungen an Konstruktionen aus Beton - Stand der Technik – Stand der Forschung N2 - Übersichtsvortrag zur Anwendung zerstörungsfreier Prüfverfahren für das Bauwesen mit Schwerpunkt auf den Baustoff Beton. T2 - Hausinterne Fortbildungsmaßnahme - Hessen Mobil - Straßen- und Verkehrsmanagement CY - Dillenburg/Hessen, Germany DA - 15.01.2019 KW - Zerstörungsfreie Prüfung KW - Beton KW - Stand der Technik KW - Brücken PY - 2019 AN - OPUS4-47234 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Weathering scenarios – Changes in polymer surface morphologies and leaching of brominated flame retardants N2 - In addition to previously reported results on the simulated aging of polystyrene samples (PS) containing 1 wt. % hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene (PP)-samples containing 0.1 wt. % BDE-209. All studied polymer samples were exposed to a defined weathering schedule in a climate chamber in accordance to regulation EN ISO 4892-3:2006.For the determination of BDE-209 in the collected rain water samples derived from the used climate chamber, the samples were prepared in accordance with a validated protocol. Before the analyses, each sample was spiked with 2 µL of isotopically labeled BDE-209 (13C10-BDE-209) to serve as internal standard (ISTD) in the performed stable isotope dilution analysis. Subsequently the samples were extracted with isooctane, the obtained aliquots of the extracts were concentrated to 200 µL and 2 µL of the resulting solution were injected to the GC/MS for quantification. Additionally, the total bromine contents are monitored for the aged and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) as well as X-ray fluorescence analysis (XRF) as non-destructive and rapid method. Furthermore, results from surface analysis using environmental scanning electron microscopy (ESEM) for morphological characterization of the aged and untreated samples were presented and discussed. In general, the resulting data from the accelerated aging will be compared to those from the natural weathering experiments (“atmospheric exposure”, in soil). The atmospheric exposure was performed by placing the samples on a weathering rack, which is aligned in SW direction (in a 45° angle to the horizon). The weathering data were regularly recorded by Deutscher Wetterdienst at this site. The surfaces of the test specimens (aged and stored references) were analyzed by ESEM as well as by LA-ICP-MS and by XRF. The surface of PS and PP specimens aged outdoors present the aging under real conditions and allow the comparison to the accelerated aged specimens by means of the weathering chamber. This way, we explore the efficiency of the accelerated aging procedure, which provides the advantage of well-defined and reproducible conditions compared to natural weathering, as a tool for testing different plastic materials. Additionally “in soil” experiments were conducted in-door in a well characterized testing soil. The soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining concrete basin inside of an air-conditioned room. In this manner, TOC, water capacity and humidity are recorded parameters. To assure a washing out process from the samples by the raining water, the target water content is calculated to 8%. The actual humidity is measured by a tensiometer, assuring the duration of the raining period. The water content is additionally monitored by weight of the basin, capturing water from raining periods. The correct humidity is a fundamental parameter for biological activity. Samples of PS resp. PP were of dimension 10x1cm and 5 specimens were placed up to the half in the soil per basin. Microbial activity of the soil, monitored by the reference polyurethane, sets HBCD resp. BDE-209 of the samples free and will be leached from the samples by raining water. Thereafter these will be captured by passive samplers placed in a distinct distance to the samples in the soil. The “in soil” experiments are complementary to the weathering experiments due to the biological activity in the soil. These experiments simulate the fate of the brominated flame retardants in the biosphere. T2 - Umwelt 2018 CY - Münster, Germany DA - 09.09.2018 KW - BFR KW - Weathering KW - PP KW - PS PY - 2018 AN - OPUS4-47029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim T1 - Untersuchung von Signalmerkmalen des Radarverfahrens zur Feuchtemessung an Estrichen N2 - Das elektromagnetische Radarverfahren ist mit seiner starken Sensitivität für Wasser längst eine etablierte Methode zur zerstörungsfreien Feuchtemessung. Besonders bei geophysikalischen Aufgabenstellungen erfreut es sich großer Beliebtheit, doch auch an Baustoffen wird es immer häufiger zur Ortung von schadensträchtigem Wasser eingesetzt. Somit liefert die Literatur bereits zahlreiche Signalmerkmale, welche einen Rückschluss auf die Feuchte des untersuchten Mediums zulassen. Die Eignung dieser Signalmerkmale zur Messung an Estrichen wurde in Laborstudien anhand des Austrocknungsprozesses nach der Herstellung untersucht. Hierbei kamen zement- und anhydritgebundene Estriche unterschiedlicher Schichtdicke zum Einsatz, wobei die Darr- und die Calciumcarbid-Methode als Referenzverfahren dienten. In der Auswertung erwiesen sich besonders die klassischen Merkmale aus dem Zeitbereich (Amplitude, Laufzeit) als robuste Methoden zur Feuchtemessung. Bei kleinen Schichtdicken und niedrigen Feuchtegehalten ist die Auswertung der klassischen Merkmale jedoch fehleranfällig, v.a. weil die (automatisierte) Separierung von direkter und Reflexionswelle nicht mehr eindeutig ist. Dies wirkt sich besonders auf die jeweiligen Frequenzanteile aus, die i.d.R. nicht zu den klassischen Feuchte-Merkmalen gehören. In weiterführenden Untersuchungen soll der Mehrwert durch multivariate Datenauswertung und Ansätze des maschinellen Lernens geprüft werden. Übergeordnetes Ziel ist der Einsatz des Radarverfahrens an geschichteten Fußbodenaufbauten zur automatisierten und zerstörungsfreien Lokalisierung von Feuchteschäden. T2 - 79. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Brunswick, Germany DA - 04.03.2019 KW - Radar KW - Feuchte KW - Fußboden KW - Signalmerkmale PY - 2019 AN - OPUS4-47525 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Zerstörungsfreie Prüfung an Bestandsbrücken aus Beton – Fallbeispiele aus Nachrechnung und Ertüchtigung N2 - Vorstellung von zerstörungsfreien Prüfverfahren und deren Anwendung an konkreten Fallbeispielen der Praxis. T2 - VSVI-Seminar 12/2019 "Brücken- und Ingenieurbau" CY - Braunschweig, Germany DA - 18.03.2019 KW - Zerstörungsfreie Prüfung KW - Brückenbauwerke KW - Nachrechnungsrichtlinie PY - 2019 AN - OPUS4-47566 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Neumann, Patrick P. T1 - Informations-Austausch zu mobilen autonomen Roboterplattformen N2 - Abteilungsübergreifender Informations-Austausch zu mobilen autonomen Roboterplattformen T2 - Informations-Austausch zu mobile autonomen Roboterplattformen CY - BAM, Berlin, Germany DA - 01.03.2019 KW - Mobile Plattform KW - Roboter KW - Autonome Systeme PY - 2019 AN - OPUS4-47475 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ritzer, Tobias A1 - Klewe, Tim T1 - Radarwellen und Neutronenstrahlung - Die Lösung für den Großschaden? Ergebnisse aus dem Forschungsprojekt zur Feuchtebestimmung von schwimmenden Bodenaufbauten N2 - Die Idee des Dissertationsprojekts ist der parallele Einsatz des Radarverfahrens und der Neutronensonde zur Lokalisierung von Feuchteschäden in Fußbodenaufbauten. Hierbei soll die integrale Messweise der Neutronensonde durch die vertikale Information des Radarsignals ergänzt werden, um zukünftig auf zerstörende Sondierungsbohrungen verzichten zu können. Primäres Ziel ist eine automatisierte und zerstörungsfreie Klassifizierung und Quantifizierung verschiedener Schadensfälle im Fußboden, welche zur Abschätzung und Auswahl des Sanierungsaufwands dienen soll. In systematischen Laborstudien an modular aufgebauten Referenzprobekörpern werden die Nachweisgrenzen der beiden Verfahren für unterschiedliche, häufig anzutreffende Fußbodenaufbauten untersucht. Hierfür wurde ein Satz verschiedenster Estrichprobekörper gefertigt und deren Hydratisierungsprozess gravimetrisch und mit den benannten Feuchtemessverfahren beobachtet. In der laufenden Auswertung konnten bereits signifikante Signalmerkmale der Radarmessungen extrahiert, sowie dessen Korrelation zum Feuchteverlauf der Proben gezeigt werden. Der modulare Aufbau der Fußbodenschichten zur Simulation von gängigen Feuchteschäden folgt im Anschluss. Über Datenfusion und Signalverarbeitung sollen so innovative Auswertungsansätze entwickelt und deren Validität an realen Schadensfällen geprüft werden. T2 - Messekongress Schadenmanagement und Assistance CY - Leipzig, Germany DA - 26.03.2019 KW - Radar KW - Neutronensonde KW - Feuchte KW - Schichtaufbau PY - 2019 AN - OPUS4-47684 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan A1 - Maack, Stefan A1 - Taffe, A. A1 - Braml, T. T1 - Non-destructive testing in civil engineering: A valuable source of information for reliability assessments N2 - The reassessment of bridges is becoming increasingly important. The basic requirement for analyses of structural safety is reliable knowledge about individual structures. This paper introduces the new approach to evaluate the quality of measured data gained from non-destructive testing (NDT) to provide reliable, objective, and relevant information about existing bridges. The purpose is to relate this validated knowledge to probabilistic analyses. Bridging the gap between NDT and numerical reassessments indicates reduced numerical uncertainties and residual service time extensions. This paper deals with an application of this approach using measurement data collected by ultrasonic technique at a prestressed concrete bridge. T2 - IABSE Symposium 2019 CY - Guimarães, Portugal DA - 27.03.2019 KW - NDT KW - Measurement KW - Structural safety KW - Uncertainty KW - Existing bridges PY - 2019 SN - 978-3-85748-163-5 VL - 112 SP - 1132 EP - 1139 PB - IABSE (International Association for Bridge and Structural Engineering) CY - Zurich, Switzerland AN - OPUS4-47815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zoega, A. A1 - Krause, Martin A1 - Kurz, J. A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Boßmann, N. T1 - Ultraschalluntersuchungen zur Rissdetektion an Spannbetonschwellen N2 - Im deutschen Eisenbahnnetz sind ca. 80 Millionen Spannbetonschwellen verbaut. Analog zu anderen Bauwerken werden Wpannbetonschwellen regelmäßig visuell inspiziert. Die Rissbildung ist bei diesen Inspektionen ein Kriterium für die Schädigung einer Spannbetonschwelle. Durch Rissbildung kann es passieren, dass Betonschwellen ihre Nutzungsdauer nicht erreichen. KW - ZfPBau KW - Spannbeton PY - 2017 VL - März 2017 IS - Ernst & Sohn Special 2017 SP - 20 EP - 22 PB - Ernst & Sohn Verlag für Architektur und technische Wissenschaften GmbH & Co. KG CY - Berlin AN - OPUS4-48112 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Elemental imaging by laser ablation ICP-MS N2 - Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is nowadays an established multi-elemental analysis and mapping technique. It was shown that LA-ICP-MS can visualize the elemental distribution within tissue thin sections or cell samples. Quantification is possible by using appropriate matrix-matched calibration samples. Besides naturally occurring elements and metals from contrast agents, biomolecules using metal-tagged antibodies were detected in different bio-medical samples. By combining the results with findings from histology, magnetic resonance imaging (MRI) and other techniques disease related changes like alterations of the extracellular matrix can be investigated. T2 - 4th Colloquium of CRC 1340 "Matrix in Vision" CY - Berlin, Germany DA - 09.04.2019 KW - Laser ablation KW - ICP-MS KW - Imaging PY - 2019 AN - OPUS4-47752 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Küttenbaum, Stefan A1 - Braml, T. A1 - Taffe, A. A1 - Maack, Stefan ED - Pellegrino, C. ED - Faleschini, F. ED - Zanini, M.A. ED - Matos, J.C. ED - Casas, J.R. ED - Strauss, A. T1 - From Uncertainty in Measurement to Certainty in Bridge Reassessment N2 - "The reassessment of bridges continues to take great importance both nationally and internationally. A major challenge is to find computation models reflecting the actual properties of the considered structures sufficiently accurate. Besides regular inspections, the conduction of advanced measurements is suitable to generate reliable information about a structure to be assessed. Prior to incorporating measurement results in reassessment, the relevance, the trueness, and the precision of the measured information needs to be stated. On the one hand, the use of information whose quality has not been assessed can lead to errors with serious consequences. On the other, the measurement of irrelevant information is inefficient. Although the use of measured data in assessment is currently mostly unregulated, their appreciation in reliability analyses is beneficial since the built environment can be assessed more realistically. Utilizing NDT in reassessment has the potential to extend remaining lifetimes of a structure, save resources, and improve infrastructural availabilities. The power of judgment regarding the decision on the reliability of an existing structure can be increased. In this contribution, an approach is outlined to process non-destructively gathered measurement data in a comparableway in order to include themeasured information in probabilistic reliability assessments of existing structures. An essential part is the calculation of measurement uncertainties. The effect of incorporating evaluated NDT-results is demonstrated by means of a prestressed concrete bridge and GPR measurements conducted on this bridge as a case-study. The bridge is assessed regarding SLS Decompression using the NDT-results." KW - Reliability KW - Assessment KW - Existing structures KW - NDT KW - Concrete PY - 2022 DO - https://doi.org/10.1007/978-3-030-91877-4_58 VL - 200 SP - 509 EP - 517 PB - Springer CY - Cham AN - OPUS4-54019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braml, T. A1 - Wimmer, J. A1 - Varabei, Y. A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Kuhn, T. A1 - Reingruber, M. A1 - Gordt, A. A1 - Hamm, J. T1 - Digitaler Zwilling: Verwaltungsschale BBox als Datenablage über den Lebenszyklus einer Brücke T1 - Digital twin: Asset administration shell BBox as data storage over the life cycle of a bridge N2 - Auf dem Weg zur digitalen Brücke existieren bereits erste Lösungen, die den Lebenszyklus einer Brücke abbilden können. Für die Planung, den Bau und den Unterhalt stehen unterschiedlichste Werkzeuge, z. B. BIM, DIN 1076, SIB-Bauwerke, Monitoring etc. zur Verfügung, die jeweils mit unterschiedlichen Datenformaten arbeiten. Für ein intelligentes Erhaltungsmanagement müssen aber alle Daten mit den verschiedenen Datenformaten zusammengeführt, abgelegt und so verwaltet werden können, dass über den gesamten Lebenszyklus einer Brücke die Abbildung eines ganzheitlichen digitalen Zwillings eines Bauwerks möglich ist. Die Autoren haben dafür mit BBox den Prototyp einer Verwaltungsschale (VWS) auf Grundlage von Industrie 4.0 entwickelt. Damit wird das physikalisch-ingenieurtechnische Modell zur Zustandsbewertung der Brücke in den Mittelpunkt gestellt und der gesamte Lebenszyklus einer Brücke kann unabhängig von Datenformaten digital erfasst werden. Da der Aufbau der VWS durch die Granularität optimal strukturiert ist, bietet die Ablage und Einspeisung von Messdaten sowohl die Grundlage eines Live-Monitorings als auch den Grundstein für maschinelles Lernen (ML). Der Datenzugriff via S3-Schnittstelle erleichtert die Entwicklung von eigenen Prognosemodellen mit Informationsmustern (SHIP – Structural Health Information Pattern). Am Beispiel der Heinrichsbrücke Bamberg wird die praktische intelligente Umsetzung des Bauwerksmonitorings inkl. VWS mit Informationsmustern und ML gezeigt. N2 - On the way to the digital bridge, initial solutions already exist that can map the life cycle of a bridge. A wide variety of tools are available for planning, construction and maintenance, e. g. BIM, DIN 1076, SIB structures, monitoring etc., each of which works with different data formats. For an intelligent maintenance management, however, all data with the different data formats must be merged, stored, and managed in such a way that the mapping of a holistic digital twin of a structure is possible over the entire life cycle of a bridge. For this purpose, the authors have developed BBox, a prototype of an asset administration shell (AAS) based on Industry 4.0. This places the physical-engineering model for assessing the condition of the bridge at the center, and the entire life cycle of a bridge can be digitally recorded independently of data formats. Since the structure of the AAS is optimally structured through granularity, the storage and feeding of measurement data provides both the basis of live monitoring and the cornerstone for machine learning (ML). The data access via S3 interface facilitates the development of own prognosis models with information patterns (SHIP – Structural Health Information Pattern). Using the Heinrichsbrücke Bamberg as an example, the practical intelligent implementation of structural monitoring incl. AAS with information patterns and ML is shown. KW - Digitaler Zwilling KW - Lebenszyklus KW - Bauwerksmonitoring KW - Industrie 4.0 KW - Maschinelles Lernen KW - Digital twin KW - Life cycle KW - Structural health monitoring KW - Industry 4.0 KW - Machine learning PY - 2021 DO - https://doi.org/10.1002/bate.202100094 SN - 1437-0999 SP - 1 EP - 9 PB - Ernst & Sohn CY - Berlin AN - OPUS4-54017 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bühling, Benjamin A1 - Maack, Stefan A1 - Strangfeld, Christoph T1 - Using sonic crystals to separate the acoustic from the flow field of a fluidic transducer N2 - Ultrasonic testing is a widely applied measurement method in materials research and medicine. Commonly, a transducer is coupled to the specimen directly or via a liquid coupling agent. While reducing acoustic transmission losses significantly, this procedure is time-consuming and cannot be used for sensitive specimens. Air-coupled ultrasound is a viable alternative in such cases, although suffering from very high acoustic transmission losses between transducer, air and specimen. The recently introduced fluidic transducer (FT) generates ultrasound by utilizing the instability of a supersonic air jet switched inside a fluidic amplifier. Since only air is used as the working medium and no vibrating surfaces are used for ultrasound generation, the transducer is able to efficiently generate large acoustic pressure amplitudes. The resulting acoustic field shares its directivity with the ejected high-velocity air jet. Thus, the acoustic energy needs to be redirected from the jet axis in order to make the fluidic transducer applicable to sensitive specimens. In this study, the effectivity of using sonic crystals (SCs) for this redirection is investigated using acoustic and flow measurements. SCs are air-permeable while being reflective to large acoustic frequency bands. It was shown that both a defect waveguide and a mirroring strategy successfully redirected the acoustic field from the air jet. Furthermore, the interaction of flow and SC showed strong acoustic quenching if the SC was placed too close to the FT outlet. Blockage of the jet entrainment due to the SC may result in slightly higher off-axis flow velocities locally, which should be considered in sensitive applications. KW - Air-coupled ultrasound KW - Sonic crystal KW - Fluidics KW - Non-destructive testing KW - Metamaterial KW - Bandgap quenching PY - 2022 DO - https://doi.org/10.1016/j.apacoust.2021.108608 SN - 0003-682X VL - 189 SP - 1 EP - 7 PB - Elsevier CY - Amsterdam AN - OPUS4-54205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - QI-DIGITAL - Eine moderne Qualitätsinfrastruktur in Zeiten zunehmender Digitalisierung N2 - QI-Digital ist eine Initiative der BAM gemeinsam mit den zentralen Akteuren der Qualitätsinfrastruktur (QI) in Deutschland. Sie zielt darauf ab, gemeinsam Lösungen für eine moderne QI vor dem Hintergrund der zunehmenden Digitalisierung zu entwickeln. Im Vortrag wird ein Überblick zu den Zielen und Maßnahmen im Projekt gegeben, insbesondere hinsichtlich der beiden BAM-Use Cases „Additive Fertigung“ und „Sichere und verlässliche Wasserstofftankstelle“ sowie der QI-Cloud, die ein wesentlicher Baustein für das strukturelle Fundament einer QI-Digital darstellt. T2 - Fraunhofer Materials - 7. Verbundinterner Workshop »MDS - Materials Data Space®« CY - Online meeting DA - 26.01.2022 KW - Qualitätsinfrastruktur KW - Digitalisierung KW - Wasserstofftankstelle KW - Additive Fertigung KW - QI-Cloud PY - 2022 AN - OPUS4-54307 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karapanagiotis, Christos T1 - Temperature and humidity discrimination in Brillouin distributed fiber optic sensing using machine learning algorithms N2 - In the last few years, the use of machine learning has emerged in the field of distributed fiber optic sensors as a promising approach to enhance their performance and provide new capabilities. In this study, we use machine learning for simultaneous measurements of temperature and humidity in polyimide (PI)-coated optical fibers based on Brillouin Brillouin optical frequency domain analysis (BOFDA). Different non-linear machine learning algorithms are employed, namely polynomial regression, decision trees and artificial neural networks (ANNs), and their discrimination performance is benchmarked against that of the conventional linear regression. The performance is evaluated using leave-one-out cross-validation to ensure that the models are reliable and able to generalize well on new data. We show that nonlinear machine learning algorithms outperform the conventional linear regression and thus could pave the way towards simultaneous cost-effective temperature and humidity distributed sensing, which has the potential to find attractive new applications in the field of civil and geotechnical engineering, from structural health monitoring of dikes and bridges to subsea cables and long pipelines corrosion detection. T2 - SPIE Photonics Europe CY - Strasbourg, France DA - 03.04.2022 KW - Distributed Brillouin sensing KW - Machine learning KW - Artificial neural networks KW - Humidity sensing KW - Simultaneous temperature and humidity sen PY - 2022 AN - OPUS4-54631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karapanagiotis, Christos A1 - Hicke, Konstantin A1 - Krebber, Katerina T1 - Temperature and humidity discrimination in Brillouin distributed fiber optic sensing using machine learning algorithms N2 - In the last few years, the use of machine learning has emerged in the field of distributed fiber optic sensors as a promising approach to enhance their performance and provide new capabilities. In this study, we use machine learning for simultaneous measurements of temperature and humidity in polyimide (PI)-coated optical fibers based on Brillouin Brillouin optical frequency domain analysis (BOFDA). Different non-linear machine learning algorithms are employed, namely polynomial regression, decision trees and artificial neural networks (ANNs), and their discrimination performance is benchmarked against that of the conventional linear regression. The performance is evaluated using leave-one-out cross-validation to ensure that the models are reliable and able to generalize well on new data. We show that nonlinear machine learning algorithms outperform the conventional linear regression and thus could pave the way towards simultaneous cost-effective temperature and humidity distributed sensing, which has the potential to find attractive new applications in the field of civil and geotechnical engineering, from structural health monitoring of dikes and bridges to subsea cables and long pipelines corrosion detection. T2 - SPIE Photonics Europe 2022 CY - Strasbourg, France DA - 03.04.2022 KW - Distributed Brillouin sensing KW - Machine learning KW - Artificial neural networks KW - Simultaneous temperature and humidity sensing KW - BOFDA PY - 2022 DO - https://doi.org/10.1117/12.2620985 VL - 12139 SP - 1 EP - 7 PB - SPIE AN - OPUS4-54861 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Digitalisierung in der Konformitätsbewertung - Einblicke aus unserer internationalen QI-FoKuS-Studie N2 - Die Präsentation enthält Informationen zur internationalen Studie der BAM zum Thema Digitalisierung in der Konformitätsbewertung, insbesondere erste Ergebnisse aus Deutschland. Sie zeigt u.a. die digitale Reife der teilnehmenden Prüflaboratorien und Zertifizierungsstellen sowie technologische Trends. T2 - 25. Kolloquium von EUROLAB-D CY - Berlin, Germany DA - 11.05.2022 KW - Qualitätsinfrastruktur KW - Digitalisierung KW - Prüflaboratorien KW - Konformitätsbewertung KW - Prüfwesen PY - 2022 AN - OPUS4-54814 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karapanagiotis, Christos T1 - Evaluation of the generalization performance of a CNN-assisted BOFDA system N2 - Brillouin Optical Frequency Domain Analysis (BOFDA) is a powerful and well-established method for static distributed sensing of temperature and strain. Recently, we demonstrated a BOFDA system based on convolutional neural network which shortens the measurement time considerably. In this paper, we apply leave-one-out cross validation to evaluate the generalization performance and provide an unbiased and reliable machine learning model for a time-efficient BOFDA system. T2 - 21. ITG/GMA Fachtagung Sensoren und Messsysteme 2022 CY - Nürnberg, Germany DA - 10.05.2022 KW - Fiber optics sensors KW - BOFDA KW - Convolutional neural networks KW - Machine learning KW - Temperature sensing PY - 2022 AN - OPUS4-54862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia A1 - Asna Ashari, Parsa T1 - Digital Maturity in the Conformity Assessment Industry - An explorative study from Germany N2 - First insights from a survey conducted among German Conformity Assessment Bodies (CABs) to explore their status of digital transformation, incl. their digital maturity, benefits and obstacles as well as actual technology trends. T2 - 26th EURAS Conference CY - Glasgow, Great Britain DA - 08.06.2022 KW - Quality Infrastructure KW - Digitalization KW - Prüflaboratorien KW - Konformitätsbewertung KW - Zertifizierungsstellen KW - Digitalisierung KW - Digitaler Reifegrad KW - Qualitätsinfrastruktur PY - 2022 AN - OPUS4-55049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaenisch, Gerd-Rüdiger T1 - Quantitative simulation of back scatter X-ray imaging and comparison to experiments N2 - X-ray backscatter imaging is a well established NDT technique to inspect complex objects using only a single-sided access. In difference to conventional transmission X-ray radiography, the X-ray backscatter imaging utilizes the scattered radiation caused by the Compton scattering effect. In order to achieve high backscatter intensities from a test object, it is necessary to optimize the backscatter system parameters namely the angle between source and slit camera, the slit collimator system, the shielding between source and scatter camera, and the type of detector. In addition, the scatter phenomena in to the investigated object need to be understood. In this contribution, we present a Monte Carlo model McRay which considers all relevant single and multiple interactions of photons and electrons. This model can be used to simulate back scatter techniques. It allows not only calculating the scatter image for a given experimental setup but also registering the spectrum of the detected scattered photons. Both aspects are important to understand the imaging process, to interpret the results, and to optimize the backscatter camera investigated here. Additionally experimental results will be presented and compared with simulations. T2 - 19th World Conference on Nondestructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Back-scatter techniques KW - Measurements KW - Monte Carlo methods KW - Radiology KW - Simulation PY - 2016 AN - OPUS4-36606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Electrochemical immunosensing with a 3-dimensional microfluidic flow cell N2 - Immunoassays, based on analyte recognition and capture by highly selective antibodies with high affinity, are intensively used in all fields of laboratory diagnostics and in screen-ings of food and environmental samples. Yet, for many purposes, online sensors are desir-able, and, in principle, all immunoassay tech-niques can be integrated into lab-on-chip set-ups that can work as continuous monitoring devices. Yet, the challenge remains to devel-op platforms and elements that are fit for a quick transition of laboratory microplate as-says to immunosensors. T2 - European Biosensor Symposium CY - Aachen, Germany DA - 28.08.2023 KW - Biosensor KW - Antibodies KW - Microfluidics KW - Electrochemical detection PY - 2023 AN - OPUS4-59240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chazeau, E. A1 - Pipier, A. A1 - Wegner, Karl David A1 - Ghiringhelli, F. A1 - Sancey, L. A1 - Paul, C. A1 - Goze, C. T1 - NIR-II aza-BODIPY Platform for the Development of a Fluorescent Antibody Drug Conjugate N2 - Real-time imaging of antibody-drug conjugates (ADCs) offers valuable insights for assessing tumor targeting specificity, monitoring therapeutic efficacy, and detecting off-target accumulation that may cause adverse effects. To enable precise tracking, we developed a versatile fluorescent platform based on an NIR-II emitting aza-BODIPY dye, which can be site-specifically grafted onto an IgG1 antibody to generate well-defined fluorescent ADCs. As a proof of concept, we synthesized an HER2-targeting trastuzumab immunoconjugate bearing a NIR-II aza-BODIPY fluorophore. The cytotoxic monomethyl auristatin E (MMAE) payload was introduced in the final step, resulting in a trackable and homogeneous ADC suitable for both in vitro and in vivo investigations. The resulting Trastu-azaNIRII-MMAE selectively accumulated in HER2-positive subcutaneous tumors, significantly reducing the tumor growth. Using NIR-II optical imaging, a single injection of the NIR-II-ADC allowed for the detection of the conjugate over a period of more than one month, highlighting its potential for long-term tracking and therapeutic applications. KW - NIR-II KW - Fluorescence KW - Quality assurance KW - Antibody drug conjugate KW - In vivo imaging PY - 2025 DO - https://doi.org/10.1021/acs.jmedchem.4c02777 VL - 68 IS - 7 SP - 7232 EP - 7242 PB - ACS Publications AN - OPUS4-63025 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Kick-off meeting DFG OsciFreq N2 - Das Bauwesen erfordert sehr hohe Flächenleistungen, so dass der physische Kontakt zur Oberfläche möglichst vermieden werden sollte, um eine hohe Verfahrgeschwindigkeit der Sensoren zu gewährleisten. Andererseits weisen luftgekoppelte, membranbasierte Aktuatoren durch den Impedanzsprung sehr hohe Verluste auf. Daher stellt das schnelle berührungslose Ultraschallmessen immer noch eine ungelöste Herausforderung im Bauwesen dar. T2 - VH_8294_Kick_off_Meeting_OsciFreq CY - Berlin, Germany DA - 17.06.2022 KW - Fluidic device KW - Beton KW - Luftgekoppelter Ultraschall KW - OsciFreq PY - 2022 AN - OPUS4-55126 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Wie steht es um die Digitalisierung in Prüflaboratorien in Deutschland? Einblicke aus der QI-FoKuS-Studie N2 - Im Vortrag werden Erkenntnisse aus einer Umfrage unter deutschen Konformitätsbewertungsstellen (KBS) zum Stand der digitalen Transformation vorgestellt, inkl. deren digitaler Reifegrad, Vorteile und Hindernisse sowie aktuelle Technologietrends. T2 - Forum Akkreditierung CY - Online meeting DA - 06.09.2022 KW - Qualitätsinfrastruktur KW - Digitalisierung KW - Prüflaboratorien KW - Konformitätsbewertung KW - Prüfung KW - digitale Transformation KW - Digitaler Reifegrad PY - 2022 AN - OPUS4-55634 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ladu, Luana T1 - Digitalization in conformity assessment- an explorative study from Germany N2 - First insights from a survey conducted among German Conformity Assessment Bodies (CABs) to explore their status of digital transformation, incl. their digital maturity, benefits and obstacles as well as actual technology trends. T2 - EU – SPRI 2022 CY - Utrecht, Netherlands DA - 02.06.2022 KW - Digitaler Reifegrad KW - Digitalisierung KW - Konformitätsbewertung KW - Prüflaboratorien KW - Qualitätsinfrastruktur KW - Zertifizierungsstellen PY - 2022 AN - OPUS4-55519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Bühling, Benjamin A1 - Maack, Stefan T1 - OsciCheck - A novel fluidic transducer for air coupled ultrasonic measurements N2 - Ultrasonic measurement technology has become indispensable in NDT-CE. Air-coupled ultrasonic (ACU) measurement techniques promise to reduce measurement time. However, the signal quality suffers from large specific impedance mismatch at the transducer-air and air-specimen interface. Additionally, large pressure amplitudes are necessary for the penetration depth required in NDT-CE applications. To address the specific requirements of ultrasonic testing in NDT-CE, a robust ACU transducer was developed, that generates ultrasound by quickly switching a pressurized air flow. The simple design of the fluidic transducer makes the device maintenance free and resilient against harsh environmental conditions. Since the signal is generated by aeroacoustics, there is no specific impedance mismatch between the transducer and the surrounding air. The ultrasonic signal exhibits frequencies in the 30-60 kHz range and is therefore well suited to penetrate heterogenous materials such as concrete. This contribution gives an introduction in the working principle and signal characteristics of the fluidic transducer. A detailed outlook is given to discuss the future potential of fluidic ultrasonic actuators. T2 - International Symposium Non-Destructive Testing in Civil Engineering CY - Zurich, Switzerland DA - 16.08.2022 KW - Air-coupled ultrasound KW - Nondestructive testing KW - Fluidics KW - Bistable amplifier KW - Aeroacoustics PY - 2022 AN - OPUS4-55529 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Introduction of a monitoring system for Bingham fluids in additive manufacturing with concrete N2 - Freeform additive manufacturing of concrete structures is a rising technology in civil engineering with several fascinating advantages. Nonetheless, to ensure reliability and structural integrity, standards and quality control are required in the future to bring this technology into the market. As the concrete is manufactured continuously, continuous quality control of the printing process is also required, i.e. comprehensive process monitoring. At BAM, a test rig will be installed, enabling the printing of concrete structures with a maximum size of 2 m x 1 m x 1 m (l x w x h). Here, process monitoring is the focus of the test rig. In this study, we show the results of the first pump tests, including the measurement of several parameters such as temperature and pressure along the supply system, i.e. from the concrete pump to the printer head. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Additive manufacturing of concrete KW - Process monitoring KW - Non-destructive testing KW - Bingham fluid PY - 2022 AN - OPUS4-55637 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - On the Treatment of Measurement Uncertainty in Stochastic Modeling N2 - Measurement uncertainty calculations in stochastic moddeling of time-independent, NDT-based random variables to be used in refined assessment of existing structures T2 - International Probabilistic Workshop 2022 (IPW2022) CY - Stellenbosch, South Africa DA - 08.09.2022 KW - Reliability KW - Assessment KW - Existing structures KW - Measurement uncertainty PY - 2022 AN - OPUS4-55657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Towards NDT supported decisions on the reliability of existing bridges N2 - 1) Concept for the NDT-supported assessment of existing structures 2) Demonstration: Shear force analysis of a prestressed concrete bridge T2 - ICOSSAR 2021-2022,13th International Conference on Structural Safety & Reliability CY - Online meeting DA - 13.09.2022 KW - Nachrechnung KW - Zuverlässigkeitsbewertung KW - Messunsicherheit KW - Querkraftnachweis PY - 2022 AN - OPUS4-55796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - On the accuracy of tendon localization in concrete using ultrasound N2 - Approaches to the development of a (GUM-) measurement model for the calculation of measurement uncertainties in the localization of tendons in concrete structures using the ultrasonic echo method including demonstration were presented. T2 - 6th International Conference on Concrete Repair, Rehabilitation and Retrofitting (ICCRRR 2022) CY - Cape Town, South Africa DA - 03.10.2022 KW - Reliability KW - Measurement Uncertainty KW - Non-Destructive Testing KW - Existing Concrete Structures PY - 2022 AN - OPUS4-55991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture distribution in amorphous porous materials N2 - Mesopores dominate the material moisture and influence the gas diffusion through materials such as concrete or sandstone T2 - Nano@bam Round Table Nano Materials CY - Berlin, Germany DA - 14.10.2022 KW - Physisorption KW - Mesopores KW - Amorphous materials PY - 2022 AN - OPUS4-55998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Bühling, Benjamin A1 - Hauke, M. A1 - Schweitzer, T. A1 - Maack, Stefan T1 - Frequency modulated, air-coupled ultrasound generated by fluidic oscillators N2 - The majority of ultrasonic devices used for non-destructive testing in civil engineering require contact with the surface of the concrete (specimen), which significantly increases the time required for the measurement. This makes it impractical for extensive investigation of large-scale structures such as bridge decks, foundations, or tunnels. In a pioneering approach, fluidic oscillators are used as contact free ultrasonic sources to overcome the aforementioned limitations. These robust and cost-effective actuators require only pressurised air and are ideally suited for harsh environments. At a constant supply pressure, they generate a continuous mono-frequent actuation signal. Further, varying the supply pressure via a fast pressure regulator was found to generate a frequency modulated signal which enabled time-of-flight measurement with an added advantage of increased signal to noise ratio. To demonstrate the feasibility of this novel idea of non-contact ultrasound, the results of the initial tests are presented. T2 - IEEE International Ultrasound Symposium CY - Venice, Italy DA - 11.10.2022 KW - Air-coupled ultrasound KW - Frequency modulation KW - Non-destructive testing KW - Civil engineering KW - Building materials KW - Fluidic oscillators PY - 2022 DO - https://doi.org/10.1109/IUS54386.2022.9958740 SP - 1 EP - 4 AN - OPUS4-56073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Frequency modulated, air-coupled ultrasound generated by fluidic oscillators N2 - The majority of ultrasonic devices used for non-destructive testing in civil engineering require contact with the surface of the concrete (specimen), which significantly increases the time required for the measurement. This makes it impractical for extensive investigation of large-scale structures such as bridge decks, foundations, or tunnels. In a pioneering approach, fluidic oscillators are used as contact free ultrasonic sources to overcome the aforementioned limitations. These robust and cost-effective actuators require only pressurised air and are ideally suited for harsh environments. At a constant supply pressure, they generate a continuous monofrequent actuation signal. Further, varying the supply pressure via a fast pressure regulator was found to generate a frequency modulated signal which enabled time-of-flight measurement with an added advantage of increased signal to noise ratio. To demonstrate the feasibility of this novel idea of non-contact ultrasound, the results of the initial tests are presented. T2 - IEEE International Ultrasound Symposium CY - Venice, Italy DA - 11.10.2022 KW - Air coupled ultrasound KW - Frequency modulation KW - Non-destructive testing KW - Civil engineering KW - Building materials KW - Fluidic oscillators PY - 2022 AN - OPUS4-56069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Frequency modulated, air-coupled ultrasound generated by fluidic oscillators N2 - The majority of ultrasonic devices used for non- destructive testing in civil engineering require contact with the surface of the concrete (specimen), which significantly increases the time required for the measurement. This makes it impractical for extensive investigation of large-scale structures such as bridge decks, foundations, or tunnels. In a pioneering approach, fluidic oscillators are used as contact free ultrasonic sources to overcome the aforementioned limi- tations. These robust and cost-effective actuators require only pressurised air and are ideally suited for harsh environments. At a constant supply pressure, they generate a continuous mono- frequent actuation signal. Further, varying the supply pressure via a fast pressure regulator was found to generate a frequency modulated signal which enabled time-of-flight measurement with an added advantage of increased signal to noise ratio. To demonstrate the feasibility of this novel idea of non-contact ultrasound, the results of the initial tests are presented. T2 - IEEE International Ultrasound Symposium CY - Venice, Italy DA - 11.10.2022 KW - Air-coupled ultrasound KW - Frequency modulation KW - Non-destructive testing KW - Civil engineering KW - Building materials KW - Fluidic oscillators PY - 2022 AN - OPUS4-56072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaenisch, Gerd-Rüdiger T1 - Back scatter X-ray imaging with twisted slit collimator – quantitative simulation and comparison to experiments N2 - X-ray backscatter imaging is a well-established NDT technique to inspect complex objects using only a single-sided access. We present a specially designed multi-slit scatter camera consisting of several twisted slits which are parallelly arranged in a metal block. The camera projects one image per slit to the digital detector array, where the images are overlaying each other. The aperture is corrected based on a deconvolution algorithm to focus the overlaying projections into a single representation of the object. In order to achieve high backscatter intensities from an object, it is necessary to optimize the parameters of the backscatter system by simulation. T2 - 2017 Far East Forum on Nondestructive Evaluation & Testing CY - Xi`an, China DA - 21.06.2017 KW - Back scatter imaging KW - Computer simulation KW - Aperture focusing KW - Deconvolution PY - 2017 AN - OPUS4-42084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - aRTist – An Industrial-Radiology Simulator Using Tcl/Tk & VTK N2 - Industrial radiography or Radiographic Testing (RT) is a method of non-destructive testing where many types of manufactured components can be examined to verify the internal structure and integrity of the specimen. The computer program aRTist can generate synthetic radiographs from a virtual RT test set-up. In the field of industrial radiology simulation is used, e.g. to optimize techniques for complex applications, to support the preparation of written procedures, and for education purposes. The simulator aRTist combines analytical and Monte Carlo methods to efficiently model the radiation transport. The program comes with a graphical user interface written in Tcl/Tk. In combination of Tcl/Tk and the 3D capabilities of the visualization toolkit (VTK) a practical and convenient simulator has been realized. This will be illustrated by discussing application scenarios of classical radiography, X-ray computer tomography, and X-ray backscatter imaging. Additionally, some insight to the software implementation of the simulator will be given. T2 - EuroTCL 2017, 15th European Tcl/Tk User Meeting CY - Berlin, Germany DA - 08.07.2017 KW - Simulation KW - Radiography KW - Computed tomography PY - 2017 AN - OPUS4-43153 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Characterisation of biofilms with near-ambient pressure XPS N2 - A drawback for X-ray photoelectron spectroscopy is that the measurements must be performed under ultra-high vacuum, which limits the type of samples which can be studied. However, by applying a differentially pumped aperture positioned close to the surface, even wet samples can be measured at near ambient pressure while the energy analyser is still under ultra-high vacuum, as illustrated below. Successful XPS-measurements with pressure up to 30 mbar have been reported using this approach, which opens up a new world of possibilities for ambient pressure measurements with XPS. While there are examples where NAP-XPS has been used to study electrochemical processes and heterogeneous catalysis, little attention has been paid to its potential use in biological materials. Until now, bacteria have only been characterised with conventional XPS, which requires tedious sample preparation usually involving freeze drying, a treatment that may degrade biological sample constituents. By studying biological samples in their native wet states, new insight about composition, absorption and transport of drugs through cell membranes and extracellular polymeric substance (EPS) layers can be obtained. Both artificial model-films of exopolysaccharides and biofilms of Escherichia Coli have been characterised at pressures ranging from ultra-high vacuum to 15 mbar by using SPECS’ EnviroESCA NAP-XPS instrument and conventional XPS. By applying antimicrobials to model biofilms, some of which are known to be resistant towards the antimicrobial in question, the distribution of antimicrobials in biofilms has been studied. Measurement capabilities and limitations of the approach will be discussed. T2 - European conferene on applications of surface and interface analysis (ECASIA 17) CY - Montpellier, France DA - 25.09.2017 KW - NAP-XPS KW - E. coli KW - Biofilms KW - Alginate PY - 2017 AN - OPUS4-42561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koller, C. S. A1 - Hönow, B. A1 - Bellon, Carsten A1 - Börner, F. D. T1 - Detection of vertical movement of fluids behind the casing of groundwater observation wells N2 - Focus of this work is the detection of vertical movements behind the casing of groundwater observation wells within the seal. A new multi-methodical and azimuthal logging tool, named Azimuthal-Annulus-Convection-Identification (AACI)-Log has been developed and tested. The measurement concept of this probe is based on the combination of three azimuthal measuring logs – contact temperature on the inside of the casing wall, backscattered gamma-rays (gamma-gamma density), and natural radioactivity (gamma ray). Consequently, a direction-oriented image of the annular space can be derived. Not only the reason (void, potential channel) but also the resulting effect (vertical movement of fluids) can be detected with the Azimuthal-Annulus-Convection (AACI) – Log at the same time. KW - Azimuthal temperature field KW - Vertical fluid movement KW - Groundwater observation well KW - Azimuthal well logging KW - Direction-oriented image KW - Annular space PY - 2016 DO - https://doi.org/10.1504/IJHST.2016.079336 SN - 2042-7808 VL - 6 IS - 4 SP - 301 EP - 330 PB - Inderscience Publishers CY - Olney, UK AN - OPUS4-43158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Characterization of biofilms with near ambient pressure XPS N2 - Near Ambient Pressure XPS opens up a new world of possibilities for measurements with XPS. While there are examples where NAP-XPS has been used to study electrochemical processes and heterogeneous catalysis, little attention has been paid to its potential use in biological materials. Until now, bacteria have only been characterised with conventional XPS, which requires tedious sample preparation usually involving freeze drying, a treatment that may degrade biological sample constituents. By studying biological samples in their native wet states, new insight about composition, absorption and transport of drugs through cell membranes and extracellular polymeric substance (EPS) layers can be obtained. Both artificial model-films of exopolysaccharides and biofilms of Escherichia Coli have been characterised at pressures ranging from ultra-high vacuum to 15 mbar by using SPECS’ EnviroESCA NAP-XPS instrument and conventional XPS. By applying antimicrobials to model biofilms, some of which are known to be resistant towards the antimicrobial in question, the distribution of antimicrobials in biofilms has been studied. Capabilities and limitations of the approach will be discussed. T2 - The 4th annual workshop on ambient presssure X-ray photoelectron spectroscopy CY - Shanghai, China DA - 13.12.2017 KW - NAP-XPS KW - Biofilms KW - E. coli PY - 2017 AN - OPUS4-43568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Surface characterisation of biofilms by nearambient pressure X-ray photoelectron spectroscopy N2 - The XPS information depth of approximately 10 nm is in the same size range as the outer membrane of the gram-negative bacteria, which makes XPS a suitable tool for determining the elemental composition of the bacterial surface and monitor changes caused by outer stress like dehydration or exposure to antimicrobials. However, bacteria are inherently in a hydrated state, and therefore only compatible to ultra-high vacuum after extensive sample preparation, which may degrade the sample constituents. This issue is addressed by the development of near-ambient pressure (NAP)-XPS, which enables bacteria and biofilms to be characterised in their native wet state. Artificial biofilms, bacteria and biofilms of Escherichia coli have been characterised with the laboratory NAP-XPS instrument EnviroESCA from SPECS GmbH, at pressures ranging from high vacuum to 12 mbar, and in both humid and dry environment. By studying biological samples in their native wet state, new insight about composition and transport of drugs through cell membranes and the extracellular polymeric substance (EPS) of biofilms can be obtained. T2 - Royal Society of Chemistry Twitter Conference CY - Worldwide (online conference) DA - 06.03.2018 KW - Biofilms KW - E. coli KW - Alginate KW - NAP-XPS PY - 2018 AN - OPUS4-44498 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Progress on characterisation of biofilms by NAP-XPS N2 - Progress talk on characterisation of biofilms by NAP-XPS in the framework of the MetVBadBugs EURAMET-project T2 - MetVBadBugs 24 M project meeting CY - Turin, Italy DA - 06.02.2018 KW - Biofilms KW - E. coli KW - Alginate KW - NAP-XPS PY - 2018 AN - OPUS4-44065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Surface characterisation of biological samples with near-ambient pressure XPS N2 - The principle of NAP-XPS is explained, together with its relevance for biological samples. Further, ongoing work on NAP-XPS measurements on E. coli biofilms is presented. T2 - Seminar AG Weinhart, FU Berlin CY - Freie Universität, Berlin, Germany DA - 05.12.2016 KW - NAP-XPS KW - Biofilms KW - Alginate KW - E. coli PY - 2017 AN - OPUS4-43331 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Seim, C. T1 - EMPIR project Metrology vs. Bad Bugs aims to provide urgently needed metrology to quantitatively measure localization and penetration of antibiotics and biocides in bacteria and biofilms N2 - An overview of ongoing reference-free X-ray spectrometry, near-ambient pressure X-ray photoelectron spectroscopy and Fourier-Transform infrared micro-spectroscopy studies on the penetration of biocides/antibiotics into bacteria and biofilms is given. T2 - Ninth Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Biofilms KW - Alginate KW - XRF KW - FTIR KW - NAP-XPS PY - 2017 AN - OPUS4-43465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tan, K. H. A1 - Sattari, S. A1 - Donskyi, Ievgen A1 - Cuellar-Camacho, J. L. A1 - Cheng, C. A1 - Schwibbert, Karin A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Gorbushina, Anna A1 - Adeli, M. A1 - Haag, R. T1 - Functionalized 2D nanomaterials with switchable binding to investigate graphene–bacteria interactions N2 - Graphene and its derivatives have recently attracted much attention for sensing and deactivating pathogens. However, the mechanism of multivalent interactions at the graphene–pathogen interface is not fully understood. Since different physicochemical parameters of graphene play a role at this interface, control over graphene’s structure is necessary to study the mechanism of these interactions. In this work, different graphene derivatives and also zwitterionic graphene nanomaterials (ZGNMs) were synthesized with defined exposure, in terms of polymer coverage and functionality, and isoelectric points. Then, the switchable interactions of these nanomaterials with E. coli and Bacillus cereus were investigated to study the validity of the generally proposed “trapping” and “nano-knives” mechanisms for inactivating bacteria by graphene derivatives. It was found that the antibacterial activity of graphene derivatives strongly depends on the accessible area, i.e. edges and basal plane of sheets and tightness of their agglomerations. Our data clearly confirm the authenticity of “trapping” and “nano-knives” mechanisms for the antibacterial activity of graphene sheets. KW - XPS KW - Graphene KW - Graphene–bacteria interaction PY - 2018 DO - https://doi.org/10.1039/c8nr01347k SN - 2040-3364 SN - 2040-3372 VL - 10 IS - 20 SP - 9525 EP - 9537 PB - RSC CY - London AN - OPUS4-45084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Dietrich, P. A1 - Beblo-Vranesevic, K. A1 - Kjærvik, Marit A1 - Unger, Wolfgang A1 - Schwibbert, Karin A1 - Hardie, K. A1 - Brown, J. T1 - XPS surface analysis of bacterial samples N2 - This application note presents how EnviroESCA can be used to analyze bacterial samples under near ambient pressure conditions in various states of hydration using different levels of humidity. Such investigations of bacterial cell wall surfaces in their hydrated state are essential for studying biological interfaces at work. The use of innovative near-ambient pressure (NAP-)XPS instrumentation allows the detailed analysis of irregularly-surfaced biofilms. NAP-XPS enables the surface analysis of bacterial samples in their natural hydrated state without complex sample preparation techniques such as freeze-drying or fast-freezing, which are needed for XPS analysis in ultrahigh vacuum. KW - Near ambient pressure XPS KW - Biofilms PY - 2018 UR - http://www.enviroai.com/uploads/1/0/2/8/102861712/xps_surface_analysis_of_bacillus_subtilis_biofilms_final.pdf IS - Application Note #000399 SP - 1 EP - 5 CY - Berlin AN - OPUS4-44588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Surface characterisation of biological samples by near-ambient pressure XPS N2 - A presentation held for the seminar "Ausgewählte analytische Methoden der Physik" hosted by Prof. Birgit Kanngießer at TU Berlin. The first part focus on depth-dependent XPS-measurements (XPS, synchrotron HAXPES) to obtain a concentration profile of iodine in an artificial biofilm. In the second part, NAP-XPS measurements of various bacterial samples are presented. T2 - Forschungsseminar "Ausgewählte analytische Methoden der Physik", TU Berlin CY - Berlin, Germany DA - 17.07.2018 KW - Biofilms KW - Alginate KW - Agarose KW - HAXPES KW - NAP-XPS PY - 2018 AN - OPUS4-45505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Quantitative biocide profile measurements by calibrated NAP-XPS N2 - Progress update for the EMPIR-project MetVBadBugs- Quantitative measurement and imaging of drug-uptake by bacteria with antimicrobial resistance. T2 - MetVBadBugs 26 M project meeting CY - South Mimms, UK DA - 05.07.2018 KW - Biofilms KW - Alginate KW - Antibiotics KW - E. coli KW - XPS PY - 2018 AN - OPUS4-45402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kjaervik, Marit A1 - Schwibbert, Karin A1 - Dietrich, P. A1 - Thissen, A. A1 - Unger, Wolfgang T1 - Near-ambient pressure XPS of hydrated Escherichia coli samples with EnviroESCA N2 - This application note presents how EnviroESCA can be used to analyze E. coli biofilms on silicon under near ambient pressure conditions in various states of hydration. Such investigations of the outer bacterial cell surface in their hydrated state are essential for studying biological interfaces at work. KW - Biofilms KW - E. coli KW - NAP-XPS PY - 2018 UR - http://www.enviroai.com/uploads/1/0/2/8/102861712/nap_xps_of_escherichia_coli_samples.pdf IS - Application Note #000400 SP - 1 EP - 4 CY - Berlin, Germany AN - OPUS4-45720 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Surface characterisation of bacteria and biofilms by NAP-XPS N2 - The XPS information depth of approximately 10 nm is in the same size range as the outer membrane of the gram-negative bacteria, which makes XPS a suitable tool for determining the elemental composition of the bacterial surface and monitor changes caused by outer stress like dehydration or exposure to antimicrobials. However, bacteria are inherently in a hydrated state, and therefore only compatible to ultra-high vacuum after extensive sample preparation, which may degrade the sample constituents. This issue is addressed by the development of near-ambient pressure (NAP)-XPS, which enables bacteria and biofilms to be characterised in their native wet state. Artificial biofilms, bacteria and biofilms of Escherichia coli have been characterised with the laboratory NAP-XPS instrument EnviroESCA from SPECS GmbH, at pressures ranging from high vacuum to 12 mbar, and in both humid and dry environment. By studying biological samples in their native wet state, new insight about composition and transport of drugs through cell membranes and the extracellular polymeric substance (EPS) of biofilms can be obtained. In this contribution, the latest progress on biofilm characterisation by NAP-XPS will be presented, and measurement capabilities and limitations will be discussed. T2 - Die Frühjahrstagung der Deutsche Physikalische Gesellschaft CY - Berlin, Germany DA - 12.03.2018 KW - Biofilms KW - E. coli KW - Alginate KW - NAP-XPS PY - 2018 AN - OPUS4-44500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karapanagiotis, Christos T1 - Machine learning for strain, temperature and humidity discrimination in Brillouin optical frequency domain analysis N2 - We propose to our knowledge for the first time an ensemble of probabilistic machine learning models for strain, temperature and humidity discrimination in Brillouin optical frequency domain analysis (BOFDA) applying a two-fiber configuration. T2 - 28th International Conference on Optical Fiber Sensors CY - Hamamatsu, Japan DA - 20.11.2023 KW - Multiparameter sensing KW - Fiber optic sensors KW - Machine learning KW - Structural health monitoring PY - 2023 AN - OPUS4-59396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - Ways to unlock the potential of NDT for the reliability assessment of existing structures N2 - Vortrag über die Berechnung von Messunsicherheiten und die POD-Analyse zur Aufbereitung von ZfP-Ergebnissen für die Zuverlässigkeitsbewertung bestehender Bauwerke. T2 - 8th International Workshop on Reliability of NDT/NDE @ SPIE Smart Structures + NDE CY - Los Angeles, CA, USA DA - 12.03.2023 KW - Probability of Detection KW - Measurement uncertainty KW - Reliability assessment PY - 2023 AN - OPUS4-57192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Bühling, Benjamin T1 - Low-frequency ultrasound data (pulse-echo technique) with shear horizontal and longitudinal waves on the step-shaped concrete specimen “Pk266” with tendons N2 - This dataset contains raw data acquired in ultrasound measurements on a reference specimen made of concrete at Bundesanstalt für Materialforschung und -prüfung (BAM), Berlin (Germany). The internal specimen identifier is “Pk266”. The measurements were conducted using the pulse-echo method. The upper surface of the specimen was defined as measuring area. The aim of the measurements is to determine both the geometrical dimensions (thickness) and the position of tendons to the measuring area. In addition to this, a second dataset of a second specimen with identifier is existing named “Pk050” has been acquired. Pk050 has the same geometrical dimensions and concrete recipe as Pk266 recipe but does not contain tendons [Reference: https://doi.org/10.7910/DVN/9EID5D]. KW - Ultrasound KW - Pulse echo method KW - Synthetic Aperture Focusing Technique KW - Validation KW - Elastic wave PY - 2023 DO - https://doi.org/10.7910/DVN/NUU0WZ PB - Harvard College CY - Cambridge, MA, USA AN - OPUS4-57232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kanzler, D. A1 - Schmitt, M. A1 - Maack, Stefan A1 - Baensch, F. T1 - Erarbeitung einer Norm für einen standardisierten Prozess zur probabilistischen Bewertung von Prüfverfahren N2 - Im DIN-Normenausschuss Materialprüfung (NMP) wurde das Normungsgremium NA 062-08-28 AA „Qualifizierung von zerstörungsfreien Prüfungen“ reaktiviert. Das Ziel der Reaktivierung ist die Erarbeitung einer Norm für einen standardisierten Prozess zur probabilistischen Bewertung von Prüfverfahren. In der zerstörungsfreien Prüfung (ZfP) führt die Ermittlung von Mess- / Prüfunsicherheiten von Prüfverfahren, in normativer Hinsicht in Deutschland und Europa, noch ein Schattendasein. Die Norm ISO IEC 17025 und auch der VDA-Band 5 wurden weiter in Richtung Messunsicherheit entwickelt, allerdings führt ihre Anwendung in der ZfP zu Problemen. Der Arbeitsausschuss NA 062-08-28 AA soll hier den Brückenschlag zwischen Messunsicherheit, objektiver statistischer Bewertung für ZfP-Verfahren und eine weitere Stärkung der probabilistischen Bruchmechanik erreichen. Geplant ist daher die Erarbeitung einer DIN-Norm, welche die Kriterien für eine korrekte Versuchsplanung, ein praktikables Vorgehen zur Bewertung der Prüfergebnisse und die mathematische Überführung in eine Zuverlässigkeitsaussage enthält. Es soll ein Leitfaden erstellt werden, der für ein möglichst breites Branchenspektrum eingesetzt werden kann, unabhängig von den Besonderheiten verschiedener Industriezweige. Dargestellt werden das relevante Normungsgremium sowie der Hintergrund des zu erstellenden Dokuments. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Validation KW - Normung KW - Probability of Detection PY - 2023 AN - OPUS4-58344 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karapanagiotis, Christos ED - Krebber, Katerina T1 - Machine learning for strain, temperature and humidity discrimination in Brillouin optical frequency domain analysis N2 - We propose to our knowledge for the first time an ensemble of probabilistic machine learning models for strain, temperature and humidity discrimination in Brillouin optical frequency domain analysis (BOFDA) applying a two-fiber configuration. T2 - 28th International Conference on Optical Fiber Sensors CY - Hamamatsu, Japan DA - 20.11.2023 KW - Multiparameter sensing KW - Machine learning KW - Fiber optic sensors KW - Structural health monitoring PY - 2023 SP - 1 EP - 4 PB - Optica Publishing Group AN - OPUS4-59397 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirabella, Francesca T1 - ToF-SIMS as a new tool for nano-scale investigation of ps-laser-generated surface structures on titanium substrates N2 - In recent years, the fabrication of laser-generated surface structures on metals such as titanium surfaces have gained remarkable interests, being technologically relevant for applications in optics, medicine, fluid transport, tribology, and wetting of surfaces. The morphology of these structures, and so their chemistry, is influenced by the different laser processing parameters such as the laser fluence, wavelength, pulse repetition rate, laser light polarization type and direction, angle of incidence, and the effective number of laser pulses per beam spot area. However, the characterization of the different surface structures can be difficult because of constraints regarding the analytical information from both depth and the topographic artifacts which may limit the lateral and depth resolution of elemental distributions as well as their proper quantification. A promising technique to investigate these structures even at the nano-scale is Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS), a very surface sensitive technique that at the same time allows to perform depth-profiling, imaging and 3D-reconstruction of selected ion-sputter fragment distributions on the surface. In this study we combine chemical analyses such as Energy Dispersive X-ray spectroscopy (EDX) and high-resolution scanning electron microscopy (SEM) analyses with ToF-SIMS to fully characterize the evolution of various types of laser-generated micro- and nanostructures formed on Ti and Ti alloys at different laser fluence levels, effective number of pulses and at different pulse repetition rates (1 – 400 kHz), following irradiation by near-infrared ultrashort laser pulses (925 fs, 1030 nm) in air environment or under argon gas flow. We show how this combined surface analytical approach allows to evaluate alteration in the surface chemistry of the laser-generated surface structures depending on the laser processing parameters and the ambient environment. T2 - European Materials Research Society (EMRS) Fall Meeting 2021 CY - Online meeting DA - 20.09.2021 KW - ToF SIMS KW - Nano characterization PY - 2021 AN - OPUS4-53366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bircher, B. T1 - Compensation of machine geometry deviations for dXCT N2 - It is fundamental to determine the machine geometry accurately for dimensional X-ray computed tomography (XCT) measurements. When performing high-accuracy scans, compensation of a non-static geometry, e.g. due to rotary axis errors or drift, might become necessary. Here we provide an overview of methods to determine and account for such deviations on a per projection basis. They include characterisation of stage error motions, in situ geometry measurements, numerical simulations, and reconstruction-based optimization relying on image quality metrics and will be discussed in terms of their metrological performance. Since a radiographic calibration is always required to provide an initial absolute geometry, this method will be presented as well. T2 - dXCT conference 2021 CY - Online meeting DA - 17.05.2021 KW - Computed tomography PY - 2021 AN - OPUS4-54029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Binder, F. T1 - Ein praxisnaher Leitfaden für computertomografische Untersuchungen mit der radiografischen Simulationsumgebung aRTist N2 - Radiografische Simulationswerkzeuge wie aRTist, ScorpiusXLab, SimCT oder CIVA CT verwenden analytische Methoden und physikalische Monte-Carlo-Teilchentransportsimulationen, um die Interaktionsprozesse zwischen Röntgenstrahlung und Materie zu simulieren. Die berechneten Projektionen bilden anschließend unter Berücksichtigung einer definierten Scan-Trajektorie die Basis der Simulation einer röntgencomputertomografischen Untersuchung. Radiografische Simulationswerkzeuge befinden sich in einem stetigen Wandel, beispielsweise durch die Entwicklung neuer Rekonstruktionsmethoden, durch Erweiterung von analytischen Modellen, durch Integration komplexer Trajektorien oder durch Berücksichtigung von prozessbedingten geometrischen Abweichungen. Im laufenden EMPIR-Projekt „AdvanCT“ entsteht deshalb ein „Good Practice Guide“ für die Simulationsumgebung aRTist. Ziel dieses Guides ist es, die mit steigender Komplexität verbundenen Einstiegshürden für Anwender von aRTist zu reduzieren, um damit einen praxisnahen Zugang zur virtuellen Computertomografie zu ermöglichen. Dabei werden anhand von praktisch nachvollziehbaren Beispielen die grundlegenden Mechanismen der Simulationsumgebung erklärt und ein strukturierter Leitfaden zur Simulation röntgencomputertomografischer Untersuchungen mit aRTist vermittelt. In diesem Beitrag werden erste Auszüge des Guides sowie eine Übersicht der weiteren geplanten Themen für die anschließende Diskussion vorgestellt. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Computertomographie Simulation PY - 2021 AN - OPUS4-54030 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - Virtual CT with aRTist N2 - Simulation becomes more and more important in modern CT imaging. It is increasingly used to optimize techniques for complex applications, to support the preparation of written procedures, and for educational purposes. The radiographic simulator aRTist is a modelling tool which simulates X-ray imaging using a hybrid analytical and Monte Carlo method to efficiently model the radiation transport. In addition to the relevant physical effects such as absorption, scattering and fluorescence, simplified fast models are employed to describe the characteristics of the X-ray source and the detector. aRTist is well equipped to model realistic X-ray imaging setups due to the ability to load exported CAD object descriptions. A simple CT scan module is contained in aRTist which allows the simulation of standard (circular cone beam) scanning trajectories. This training session starts with a general introduction to aRTist and will highlight its basic usage. Furthermore, the focus is on the configuration of scan trajectories and batch simulations for virtual CT. The aim is to enable the audience to use the aRTist software for their own experiments in virtual CT. T2 - dXCT conference 2021 CY - Online meeting DA - 17.05.2021 KW - computed tomography simulation PY - 2021 AN - OPUS4-54062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sintschuk, Michael T1 - Work- and Data flow for CT at BAMline II N2 - After a general presentation of the beamline, specifically the workflow for ex-situ CT at BAMline is presented. Although being used in a broad variety of research fields the usual workflow for CT experiments is in most cases similar in terms of sample mounting, tomographic scan and reconstruction. Specific scanning schemes allow for a preview reconstruction carried out during the scan. A detailed description of the used hardware as well as the self-coded programs applied in the data pipeline will be given. This will be accompanied by a practical demonstration of the software involved in the entire process. T2 - Pipeline for XCT data acquisition and reduction workshop CY - Online meeting DA - 22.02.2021 KW - BAMline KW - Synchrotron KW - Tomography PY - 2021 AN - OPUS4-52169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Borges de Oliveira, F. A1 - Reuter, T. A1 - Plotzki, David A1 - Bartscher, M. A1 - Hausotte, T. T1 - Novel reference standards for the qualification of radiography-based computed tomography simulation software N2 - This contribution presents a set of largely novel reference standards specially designed for testing different important physical effects and functionalities of radiography-based computed tomography (CT) simulation software. These standards were developed within the scope of the German cooperation project “CTSimU – Radiographic Computed Tomography Simulation for Measurement Uncertainty Evaluation” [1] and serve as tools for the basic qualification of the sufficient physical correctness and required features of simulation software of CT-based coordinate measurement systems (CMSs) via the analyses either of 2D projection images only or of full CT scans. The results serve as input to the German standardisation committee for the development of a new national VDI/VDE guideline in the series VDI/VDE 2630 dealing with the basic qualification aspect of CT simulation software and shall lay ground for the measurement uncertainty determination of dimensional measurements using CT. T2 - 11th Conference on Industrial Computed Tomography (iCT 2022) CY - Online meeting DA - 08.02.2022 KW - Multi-geometry cuboid KW - Radiographic simulation software KW - Basic qualification KW - CT simulation, spherical step-wedge KW - Conical hole sheet KW - Tungsten-Edge PY - 2022 SP - 1 EP - 12 PB - Research Group Computed Tomography, Upper Austrian University of Applied Sciences (FH OÖ) CY - Wels, Austria AN - OPUS4-54569 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bircher, B. A1 - Meli, F. A1 - Küng, A. A1 - Bellon, Carsten A1 - Evsevleev, Sergei A1 - Katic, M. A1 - Heikkinen, V. A1 - Hemming, B. A1 - Lassila, A. T1 - Traceable determination of non-static XCT machine geometry: New developments and case studies N2 - It is fundamental to determine the machine geometry accurately for dimensional X-ray computed tomography (XCT) measurements. When performing high-accuracy scans, compensation of a non-static geometry, e.g. due to rotary axis errors or drift, might become necessary. Here we provide an overview of methods to determine and account for such deviations on a per projection basis. They include characterisation of stage error motions, in situ geometry measurements, numerical simulations, and reconstruction-based optimization relying on image quality metrics and will be discussed in terms of their metrological performance. Since a radiographic calibration is always required to provide an initial absolute geometry, this method will be presented as well. The improvements of the XCT geometry correction methods are presented by means of case studies. The methods can be applied individually or in combination and are intended to provide a toolbox for XCT geometry compensation. T2 - 11th Conference on Industrial Computed Tomography (iCT 2022) CY - Online meeting DA - 08.02.2022 KW - Radiographic XCT geometry determination KW - Dimensional metrology KW - traceability KW - XCT machine geometry KW - Calibrated reference standards PY - 2022 SP - 1 EP - 10 PB - Research Group Computed Tomography, Upper Austrian University of Applied Sciences (FH OÖ) CY - Wels, Austria AN - OPUS4-54479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Plotzki, David A1 - Hartlaub, Bendix A1 - Borges de Oliveira, F. A1 - Reuter, T. A1 - Wohlgemuth, F. A1 - Bellon, Carsten A1 - Hausotte, T. T1 - The CTSimU software toolbox for CT-related image processing and quality assessment N2 - A software toolbox is introduced that addresses several needs common to computed tomography (CT). Built for the WIPANO CTSimU project to serve as the reference implementation for its image processing and evaluation tasks, it provides a Python 3 interface that is adaptable to many conceivable applications. Foremost, the toolbox features a pipeline architecture for sequential 2D image processing tasks, such as flat field corrections and image binning, and enables the user to create their own processing modules. Beyond that, it provides means to measure line profiles and image quality assessment algorithms to calculate modulation transfer functions (MTF) or to determine the interpolated basic spatial resolution (iSRb) using a duplex wire image. It can also be used to calculate projection matrices for the reconstruction of scans with arbitrary industrial CT geometries and trajectories. The CTSimU project defined a framework of projection- and volume-based test scenarios for the qualification of radiographic simulation software towards its use in dimensional metrology. The toolbox implements the necessary evaluation routines and generates reports for all projection-based tests. T2 - 11th Conference on Industrial Computed Tomography (iCT 2022) CY - Online meeting DA - 08.02.2022 KW - Image processing KW - CT KW - Geometry KW - Software KW - Python PY - 2022 SP - 1 EP - 7 PB - Research Group Computed Tomography, Upper Austrian University of Applied Sciences (FH OÖ) CY - Wels, Austria AN - OPUS4-54476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reuter, T. A1 - Borges de Oliveira, F. A1 - Plotzki, David A1 - Hausotte, T. T1 - Influence of detector misalignments on different geometrical and dimensional measurands using a dedicated test specimen N2 - An important focus of research in Industrial X-ray Computed Tomography (CT) is to determine the task-specific measurement uncertainty of CT measurements numerically by using simulations. For this, all relevant influence factors need to be identified and quantified. It is known, for example, that geometrical misalignments of the detector lead to measurement deviations if the reconstruction does not consider these misalignments. This contribution uses computer simulation of CT data to investigate the influence of geometrical misalignments of the detector on several measurands found in typical measurements tasks in the industry. A newly developed test specimen with a broad variety of features is used for this study. Angular and positional detector deviations are systematically introduced into the simulations and deliberately left uncompensated during the CT reconstruction. The resulting measurement deviations are shown and discussed. T2 - 11th Conference on Industrial Computed Tomography (iCT 2022) CY - Online meeting DA - 08.02.2022 KW - Geometrical misalignment KW - Task specific numerical measurement uncertainty KW - Dimensional metrology PY - 2022 SP - 1 EP - 7 PB - Research Group Computed Tomography, Upper Austrian University of Applied Sciences (FH OÖ) CY - Wels, Austria AN - OPUS4-54568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ecke, Alexander T1 - An Immunosensor for Pharmaceutical Contaminants in Water Supply N2 - Contamination of drinking water with pharmaceuticals is an emerging problem and a potential health threat. Immunochemical methods based on the binding of the analyte to specific antibodies enable fast & cost-effective on-site analyses. Magnetic bead-based immunoassays (MBBAs) allow for implementation into an immunosensor for online testing. Particles are prepared by either coupling the analyte molecule (diclofenac) or the respective antibody (amoxicillin) to the surface. For miniaturization, detection is performed electrochemically (chronoamperometry) on a microfluidic chip. The developed immunosensor will enable detection of pharmaceuticals directly in water supply pipes. T2 - Analytica Conference CY - München, Germany DA - 21.06.2022 KW - Immunosensor KW - Magnetic Particles KW - Microfluidics KW - Amperometry KW - Diclofenac KW - Amoxicillin PY - 2022 AN - OPUS4-55381 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bühling, Benjamin T1 - OsciCheck - Fluidische Erzeugung eines luftgekoppelten Ultraschallpulses N2 - Das ZIM-Projekt OsciCheck wird vorgestellt, die Funktionsweise eines fluidischen Oszillators erläutert und die nächsten Arbeitsschritte im Projekt dargestellt. T2 - Herbstworkshop der jungen DEGA CY - Berlin, Germany DA - 01.11.2019 KW - Fluidischer Oszillator KW - Ultraschall KW - Luftgekoppelter Ultraschall KW - Zerstörungsfreie Prüfung PY - 2019 AN - OPUS4-51294 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Strangfeld, Christoph A1 - Klewe, Tim ED - Rizzo, P. ED - Milazzo, A. T1 - Hygrometric Moisture Measurements Based on Embedded Sensors to Determine the Mass of Moisture in Porous Building Materials and Layered Structures N2 - Subfloors are layered structures, consisting largely of porous building materials, such as screed. They are often suffering damage from tap water leakage, which is a typical problem in buildings, and which has largely contributed to repair costs of almost 3 billion Euro in 2018 alone in Germany. In this context, especially mould plays a role, which is both destroying the structure and posing severe health risks. To determine the damaging effects of moisture, it is necessary to know the respective processes occurring in building materials, especially to quantify the amount of moisture and its progress in the material. In this study, humidity sensors are used to derive the material moisture experimentally. Capacitive sensors recording the relative humidity are embedded into the screed and in the insulation materials such as expanded polystyrene, extruded polystyrene, perlite and glass wool. For the application in screed, the sensors need to be shielded against the aggressive alkaline materials. To ensure an appropriate exchange with the environment, a permeable membrane is requested. Different membrane materials have been investigated regarding their robustness and their permeability. In the first experimental setup, two humidity sensor arrays with seven individual sensors are embedded in homogeneous screed samples. The measured corresponding relative humidity of the screed is converted to the material moisture based on the approach of Hillerborg. In a second experimental setup, a layered structure of a complete subfloor is built in a box of 0.8 m times 0.8 m. The humidity sensors are positioned in the different insulation materials of various thicknesses. By adding water, leakage damage is simulated and its progress and effect is investigated experimentally. The investigations point at the question if the observed moisture is able to generate damage such as mould. The moisture and corresponding humidity values are discussed. It will be shown that this low-cost hygrometric approach can be used easily for moisture monitoring of screed and insulation materials as well KW - Moisture monitoring KW - Material moisture KW - Building materials KW - Embedded humidity sensors PY - 2021 DO - https://doi.org/10.1007/978-3-030-64594-6_22 VL - 1 SP - 213 EP - 225 PB - Springer Nature CY - Cham AN - OPUS4-52013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Millar, Steven A1 - Strangfeld, Christoph A1 - Wilsch, Gerd T1 - Identification of type of cement through laser-induced breakdown spectroscopy N2 - The composition of concrete determines its resistance to various degradation mechanisms such as ingress of ions, carbonation or reinforcement corrosion. Knowledge of the composition of the hardened concrete is therefore helpful to assess the remaining service life of an existing structure or evaluate the damage observed during inspections. For example, for most existing concrete structures the type of cement originally used is not known and must therefore be determined afterwards. This paper presents a preliminary study on the application of laser-induced breakdown spectroscopy (LIBS) to identify the type of cement. For this purpose, ten different types of cement were investigated. For every type, three cement paste prisms were produced: (i) prisms dried, ground and pressed into tablets, (ii) prisms dried and (iii) prisms untreated. LIBS measurements were performed with a diode-pumped low energy laser (1064 nm, 3 mJ, 1.5 ns, 100 Hz) in combination with two compact spectrometers which cover the UV and NIR spectral range. A reduced subset of spectral features was used to build a classification model based on linear discriminant analysis. The results show that the classification of homogenized pressed cement powder samples provides a high accuracy, however, factors such as a different sample matrix and moisture content can affect the accuracy of the classification. The study demonstrates that LIBS is a promising tool to identify the type of cement. KW - Spectroscopy KW - LIBS KW - Cement KW - Classification KW - Identification PY - 2020 DO - https://doi.org/10.1016/j.conbuildmat.2020.120345 VL - 258 SP - 120345 PB - Elsevier Ltd. AN - OPUS4-51157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan A1 - Maack, Stefan T1 - Nutzung von ZfP-Daten bei der Nachrechnung von Spannbetonbrücken N2 - Der Vortrag umfasst methodische Ansätze sowie Fallbeispiele zur Nachrechnung von Betonbrücken unter Einbeziehung von gütebewerteten, zerstörungsfreien Inspektionsergebnissen. T2 - Seminar "Zerstörungsfreie Prüfung" der Technischen Universität München CY - Online meeting DA - 09.07.2020 KW - ZfPStatik KW - Ultraschall KW - Radar KW - Nachrechnung PY - 2020 AN - OPUS4-50999 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia A1 - Mirtsch, Mona T1 - Corona-Monitor - Auswirkungen der Corona-Pandemie auf Konformitätsbewertung und Konformitätsbewertungsstellen in Deutschland: Ergebnispräsentation zur Befragung im Juni 2020 N2 - Im Vortrag wurden die Ergebnisse der von BAM gemeinsam mit der TU Berlin und Fraunhofer ISI durchgeführten Befragung zur Lage der Konformitätsbewertungsstellen während der Corona-Pandemie vorgestellt und mit den Teilnehmer*innen diskutiert. Schwerpunkte lagen auf den wirtschaftlichen Auswirkungen (Aufträge, Arbeitsfähigkeit, Existenz), der Resilienz der Branche sowie den Wirkungen auf die Digitalisierung. Mehr Informationen unter www.qi-fokus.de. T2 - QI-FoKuS - Forschung für Konformitätsbewertung und Sicherheit CY - Online meeting DA - 08.10.2020 KW - Konformitätsbewertung KW - Konformitätsbewertungsstellen KW - Corona KW - COVID-19 KW - Prüfung KW - Zertifizierung KW - Resilienz KW - Digitalisierung KW - QI-FoKuS PY - 2020 UR - http://www.qi-fokus.de AN - OPUS4-51407 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler T1 - Analysis of the porosity of alkali-sensitive aggregates for the assessment of microstructure-dependent solubility in the context of ASR N2 - Intensified Alkali-Silica Reaction (ASR) damage has occurred on German roadways in recent years, leading to requirements for compulsory pre-construction investigation of aggregate alkali sensitivity using concrete tests with external alkali supply. However, since these tests are time-consuming and cost-intensive, there is interest in replacing them with a solubility test on pure aggregate in 0.1 M KOH solution at 80°C with a defined NaCl content (1wt.-%). In this context, the influence of aggregate pore structure on SiO2 and Al2O3 solubility was investigated in this project. This paper compares the results of porosity studies with X-ray Computed Tomography (3D-CT) and the Brunauer-Emmett-Teller (BET) method on individual quarried and river gravel granules of both rhyolite and greywacke. For visualization and quantification of both externally accessible and fully enclosed surfaces of granules using X-ray 3D-CT, special software tools were developed. The results demonstrated that the river gravel granules had significantly larger externally accessible surfaces than the quarried granules. BET measurements on individual stones showed, as expected, that measured surfaces were about three orders of magnitude larger than those from the X-ray 3D-CT analyses due to the higher spatial resolution of BET. There was no apparent correlation between the X-ray 3D-CT and BET surface areas. Mercury porosimetry measurements indicate that this may be due to the presence of significant porosity below the spatial resolution of the X-ray 3D-CT. A comparison of SiO2 and Al2O3 solubility measurements with the X-ray 3D-CT and BET surface area data resulted only in weak, inconclusive correlations, indicating the need for further experimental investigation. T2 - Microdurability Webinar CY - Online meeting DA - 12.10.2020 KW - X-ray Computed Tomography (CT) KW - Brunauer-Emmett-Teller (BET) Method KW - Alkali-Silica Reaction (ASR) KW - Porosity KW - Solubility PY - 2020 AN - OPUS4-51429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bühling, Benjamin T1 - OsciCheck - Fluidic Generation of Ultrasound N2 - The OsciCheck project is presented. The working principle and sound field of a fluidic switch is described. Future goals of the project are presented. T2 - CoDA Summer School 2020 CY - Berchtesgaden, Germany DA - 28.09.2020 KW - Fluidic Switch KW - Air-coupled ultrasound KW - Ultrasound KW - Non-destructive testing KW - Fluidischer Schalter KW - Luftgekoppelter Ultraschall KW - Ultraschall KW - Zerstörungsfreie Prüfung PY - 2020 AN - OPUS4-51380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mirtsch, Mona A1 - Koch, Claudia T1 - Informationssicherheit in deutschen Unternehmen: Ergebnisse der QI-FoKuS Umfrage zur ISO/IEC 27001 N2 - Ergebnisvorstellung im mitgliederexklusiven Webinar der Deutschen Gesellschaft für Qualität (DGQ) zur Studie: "Nutzung und Wirkung von einem ISMS nach ISO/IEC 27001". Neben Zweck und Design der Studie werden sowohl Hürden bei der Implementierung, fördernde Maßnahmen, die Anwender nützlich finden und die Frage, warum Firmen diese Norm nicht nutzen, erörtert. T2 - Nutzung und Wirkung von einem ISMS nach ISO/IEC 27001 CY - Online meeting DA - 15.04.2021 KW - Zertifizierung KW - Informationssicherheit KW - ISO/IEC 27001 KW - Managementsysteme PY - 2021 AN - OPUS4-52485 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Karapanagiotis, Christos T1 - Development of artificial neural networks for real time and high resolution strain sensing N2 - We propose a method based on artificial neural networks to extract strain information from wavelength-scanning coherent optical time domain reflectometry (C-OTDR) data. Our neural network algorithm performs more than two orders of magnitude faster than the conventional approach. This is due to the highly parallel evaluation of the neural networks on a GPU accelerated computer and the fact that conventional correlation and interpolation analysis needs many Iteration steps. This opens the way for real-time C-OTDR strain sensing because the neural Network strain predictions require less time than the measurements themselves. Real-time data Analysis enables long-term sensing e.g. in structural health monitoring, because the large amount of raw data does not have to be stored but can immediately be reduced to the strain data of interest. T2 - Workshop (in collaboration with KIT) CY - Online meeting DA - 27.08.2018 KW - Dynamic strain sensing KW - Machine learning KW - Distributed fiber-optic sensors PY - 2018 AN - OPUS4-52307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - TC 286-GDP STAR - chapter: Modelling moisture transport in porous media N2 - The current content and structure of the chapter "Modelling moisture transport in porous media" of the state of the art report is presented. T2 - RILEM Spring Convention 2021 CY - Online meeting DA - 06.04.2021 KW - Moisture transport KW - Porous media KW - Modelling mass transfer KW - Gas diffusion KW - Concrete PY - 2021 AN - OPUS4-52405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schönsee, Eric T1 - Entwicklung eines Prüfstandes zur Erfassung von Frischbetoneigenschaften während der additiven Fertigung T1 - Development of a test rig for detecting parameters of fresh concrete during additive manufacturing N2 - In den vergangenen Jahren ist die Entwicklung additiver Fertigungsverfahren branchenübergreifend fortgeschritten. In der Industrie ist die Verarbeitung von Polymeren wie z. B. Polylactide (PLA) oder Acrylnitril-Butadien-Styrol-Copolymer (ABS) am weitesten verbreitet, aber auch die Verarbeitung von Metallen nimmt zu. Umfragen des Fraunhofer-Institut für Produktionstechnik und Automatisierung IPA aus dem Jahr 2016 verdeutlichen, wie hoch das Potential additiver Fertigungsverfahren eingeschätzt wird und auch die Anzahl der jährlich angemeldeten Patente im Bereich des 3D-Drucks hat sich in den letzten Jahren vervielfacht. KW - Additive Fertigung KW - 3D Druck von Beton KW - Prozessüberwachung PY - 2021 SP - 1 EP - 145 CY - Berlin AN - OPUS4-52550 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Klewe, Tim T1 - Classification of moisture damage in layered building floors with GPR and neutron probe N2 - In 2019, 3.1 billion Euro of damage was caused by piped water, accounting for the largest share (53%) of building insurance claims in Germany. In the event of damage, the accurate determination and localization of water ingress is essential to plan for and perform efficient renovations. Neutron probes are already applied successfully on building floors to localize the source of damage and other affected areas. However, additional information about the depth of moisture penetration can only be obtained by the destructive extraction of drilling cores, which is a time- and cost-intensive procedure. With its high sensitivity to water and fast measurement procedure, Ground Penetrating Radar (GPR) can serve as a suitable extension to the neutron probe, enabling more precise characterization of common forms of moisture damage. In this research project, we study the influence of common types of moisture damage in differing floor constructions using GPR and a neutron probe. A measurement setup with interchangeable layers is used to vary the screed material (cement or anhydrite) and insulation material (Styrofoam, Styrodur, glass wool, perlite), as well as the respective layer thickness. Every configuration is measured for the following main cases: 1) dry state; 2) with a damaged insulation layer and 3) a damaged screed layer. The evaluation is focused on the extraction of distinctive signal features for GPR, which can be used to classify the underlying case of damage. Furthermore, possible combinations of these features are investigated using multivariate data analysis and machine learning in order to evaluate the influence of different floor constructions. To validate the developed methods, practical measurements on real damage cases in Germany are carried out and compared to reference data obtained from drilling cores. T2 - EGU 21 General Assembly CY - Online meeting DA - 19.04.2021 KW - Radar KW - Moisture KW - Building floors PY - 2021 AN - OPUS4-52532 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bühling, Benjamin T1 - Acoustic and flow data of an ultrasonic fluidic switch and an ultrasonic piezoelectric transducer N2 - This dataset contains acoustic and flow data of an ultrasonic fluidic switch, which have been acquired using a microphone, a hot-wire anemometer and a pitot tube. Furthermore, acoustic data of a commercial piezoelectric transducer is provided. KW - Fluidics KW - Air-coupled ultrasound KW - Ultrasound KW - Non-destructive testing KW - Acoustic-flow interaction KW - Piezoelectric transducer PY - 2020 DO - https://doi.org/10.7910/DVN/OQYPC9 PB - Harvard College CY - Cambridge, MA, USA AN - OPUS4-52392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Munsch, Sarah Mandy T1 - Interpretation of NMR signals from partly saturated sandstones N2 - The development of prevention methods and the detection of moisture related damages in buildings and transport infrastructure at an early stage are current issues in the field of non-destructive testing in civil engineering. Especially the subject of partial saturation requires further research since it is more likely to occur than full saturation of the material. In fact, partial saturation in porous media is even more complicated because both fully and partly saturated pores (i.e. pores in which the surfaces are covered with thin water layers) are present. As the non-destructive method nuclear magnetic resonance (NMR) enables the measurement and quantification of relative low moisture contents, it is suitable for the investigation of partly saturated porous building materials. Nevertheless, the differentiation between partly and fully saturated pores is still a challenge. Therefore, in this study, we investigate two sandstones types (Bozanov and Schönbrunner sandstone) at various defined saturation states by using NMR. Furthermore, we measure the relative humidities within the samples and compute the water layer thicknesses (WLT) along the pore walls of all pore sizes to calculate the corresponding degree of pore saturation. To finally assign the NMR signals to pore sizes and to differentiate between partly and fully saturated pores, the water content distribution obtained from the WLT calculation is used for calibration of the relaxation-time distribution. T2 - ISEMA 2021 CY - Online meeting DA - 26.07.2021 KW - NMR KW - Relative humidity KW - Water layer thickness KW - Partial pore saturation KW - Pore-size distribution PY - 2021 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-53044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan T1 - From uncertainty in measurement to certainty in bridge assessment N2 - In this contribution, an approach is outlined to process non-destructively gath-ered measurement data in a comparable way in order to include the measured information in probabilistic reliability assessments of existing structures. An es-sential part is the calculation of measurement uncertainties. The effect of incor-porating evaluated NDT-results is demonstrated by means of a prestressed con-crete bridge and GPR measurements conducted on this bridge as a case-study. The bridge is assessed regarding SLS Decompression using the NDT-results. T2 - 1st Conference of the European Association on Quality Control of Bridges and Structures – EUROSTRUCT2021 CY - Padova, Italy DA - 29.08.2021 KW - Reliability KW - Assessment KW - Existing structures KW - NDT KW - Concrete PY - 2021 AN - OPUS4-53173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bühling, Benjamin A1 - Schweitzer, T. A1 - Maack, Stefan A1 - Strangfeld, Christoph T1 - Influence of operating conditions on the fluidic ultrasonic transducer signal N2 - While contact and immersion ultrasonic testing are established methods in non-destructive testing (NDT), generating high power air-coupled ultrasound remains a challenging task. Solutions often involve setups that are restricted to lab environments. When field measurements are required, such as in NDT for civil engineering, a handy, robust and safe transducer is needed. For this purpose, an ultrasonic transducer based on a fluidic switch has been developed. A sonic air flow inside the device is switched rapidly so that an ultrasonic signal is generated. Both theory and previous flow simulations suggest that the control flow pressure ramp has only little influence on the switching time of the device. This publication gives an overview over the operating principle of the fluidic ultrasonic transducer and investigates the influence of control tube length and pulsing repetition rate on the ultrasonic pressure amplitude. High repetition rates are found to reduce the signal amplitude, whereas long tubing has only little negative influence on the amplitude while improving signal quality. T2 - 47. Jahrestagung für Akustik (DAGA 2021) CY - Vienna, Austria DA - 15.08.2021 KW - Ultrasound KW - Non-destructive testing KW - Fluidic devices PY - 2021 UR - https://pub.dega-akustik.de/DAGA_2021 SN - 978-3-939296-18-8 SP - 48 EP - 51 CY - Berlin, Germany AN - OPUS4-53493 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bühling, Benjamin T1 - Recent Developments of Fluidic Ultrasonic Transducers at BAM N2 - Ultrasonic measurement technology has become indispensable in NDT. In order to reduce measurement time and extend the application to other materials, contactless ultrasound is the subject of many different research groups. Department 8 has been researching successfully in this field for years. A novel approach is based on so-called fluidic devices. These devices can be used to perform binary logic operations with the help of natural flow instabilities. Hence the abbreviated name, Fluidic (FLUID+LogIC). Only a pressure reservoir of the used fluid is required as energy supply. This enables the production of very robust actuators that generate ultrasonic signals in an extremely energy efficient way. The presentation includes the research results of the ZIM innovation project OsciCheck. The original idea will be presented and its application on different building materials is validated. Beyond this, the possible application areas are much larger and a detailed outlook is given to discuss the future potential of fluidic ultrasonic actuators. T2 - Abteilungsseminar Abteilung 8 CY - Berlin, Germany DA - 23.09.2021 KW - Uultrasound KW - Non-destructive testing KW - Fluidic devices KW - Hydrogen KW - Ranging KW - Harsh environments PY - 2021 AN - OPUS4-53356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bühling, Benjamin T1 - Influence of Operating Conditions on the Fluidic Ultrasonic Transducer Signal N2 - Motivation: • Air-coupled ultrasound (AC-US) enables faster measurements in non-destructive testing for civil engineering • Current state of the art: piezo and capacitive transducers are mostly used for AC US • Currently >99.9% sound intensity loss due to impedance mismatches Innovation: • Fluidic transducers generate US (30-60 kHz) by rapid switching of a supersonic jet • Fluidic transducers rely on external components such as solenoid valves and tubing --> How do repetition time and tube length influence the signal? T2 - DAGA 2021 CY - Vienna, Austria DA - 15.08.2021 KW - Ultrasound KW - Non-destructive testing KW - Fluidic devices PY - 2021 AN - OPUS4-53408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Mirtsch, Mona A1 - Blind, K. A1 - Castka, P. ED - Jakobs, K. T1 - Impact of the COVID-19 Pandemic on Conformity Assessment: Insights from a Multinational Study N2 - The COVID-19 pandemic has posed new and manifold challenges to organizations and their operations worldwide. Conformity assessment bodies (CABs), such as testing or medical laboratories, certification, and inspection bodies, are also affected by the associated disruptions. Their situation in this crisis is highly relevant, as CABs are essential pillars of the quality infrastructure: Their activities ensure that products and services meet requirements as defined in standards and regulations, thereby contributing to their safety and reliability. Considering the roles and functions of CABs in economy, health, and innovation, the question arises how CABs and their operations were affected by the pandemic and how they responded. To this end, we present the results of an international survey of 986 CABs of all types in Germany, the UK, Italy, and New Zealand. Overall, CABs reported on average a negative development of demand during the pandemic, facing restrictions in all countries. In addition, the pandemic had overall negative impact on the CABs’ investment and innovation activities. However, investments in digital infrastructure were increased as countermeasure, with CABs reporting an increased need for digitalization. Resources relevant to organizational resilience were available to different extents, affecting the speed of response to the challenges of the pandemic. The paper highlights and discusses results from in-depth analyses, which are relevant for policy makers and industry alike. T2 - 25th EURAS Annual Standardisation Conference – Standardisation and Innovation CY - Aachen, Germany DA - 05.09.2021 KW - COVID-19 KW - Corona KW - Crisis KW - Digitalization KW - Laboratory KW - Pandemic KW - Quality infrastructure KW - Conformity assessment KW - Resilience PY - 2021 SN - 978-3-95886-421-4 SP - 379 EP - 398 PB - Verlag Mainz AN - OPUS4-53815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Bewitterungsszenarien im Vergleich – Veränderungen in der Oberflächenmorphologie von Polypropylen (PP) und Polystyrol (PS) unter dem Aspekt des Austrags von polybromierten Flammschutzmitteln N2 - In addition to previously reported results on the simulated aging of polystyrene samples (PS) containing 1 wt. % hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene (PP)-samples containing 0.1 wt. % BDE-209. All studied polymer samples were exposed to a defined weathering schedule in a climate chamber in accordance to regulation EN ISO 4892-3:2006.For the determination of BDE-209 in the collected rain water samples derived from the used climate chamber, the samples were prepared in accordance with a validated protocol. Before the analyses, each sample was spiked with 2 µL of isotopically labeled BDE-209 (13C10-BDE-209) to serve as internal standard (ISTD) in the performed stable isotope dilution analysis. Subsequently the samples were extracted with isooctane, the obtained aliquots of the extracts were concentrated to 200 µL and 2 µL of the resulting solution were injected to the GC/MS for quantification. Additionally, the total bromine contents are monitored for the aged and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) as well as X-ray fluorescence analysis (XRF) as non-destructive and rapid method. Furthermore, results from surface analysis using environmental scanning electron microscopy (ESEM) for morphological characterization of the aged and untreated samples were presented and discussed. In general, the resulting data from the accelerated aging will be compared to those from the natural weathering experiments (“atmospheric exposure”, in soil). The atmospheric exposure was performed by placing the samples on a weathering rack, which is aligned in SW direction (in a 45° angle to the horizon). The weathering data were regularly recorded by Deutscher Wetterdienst at this site. The surfaces of the test specimens (aged and stored references) were analyzed by ESEM as well as by LA-ICP-MS and by XRF. The surface of PS and PP specimens aged outdoors present the aging under real conditions and allow the comparison to the accelerated aged specimens by means of the weathering chamber. This way, we explore the efficiency of the accelerated aging procedure, which provides the advantage of well-defined and reproducible conditions compared to natural weathering, as a tool for testing different plastic materials. Additionally “in soil” experiments were conducted in-door in a well characterized testing soil. The soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining concrete basin inside of an air-conditioned room. In this manner, TOC, water capacity and humidity are recorded parameters. To assure a washing out process from the samples by the raining water, the target water content is calculated to 8%. The actual humidity is measured by a tensiometer, assuring the duration of the raining period. The water content is additionally monitored by weight of the basin, capturing water from raining periods. The correct humidity is a fundamental parameter for biological activity. Samples of PS resp. PP were of dimension 10x1cm and 5 specimens were placed up to the half in the soil per basin. Microbial activity of the soil, monitored by the reference polyurethane, sets HBCD resp. BDE-209 of the samples free and will be leached from the samples by raining water. Thereafter these will be captured by passive samplers placed in a distinct distance to the samples in the soil. The “in soil” experiments are complementary to the weathering experiments due to the biological activity in the soil. These experiments simulate the fate of the brominated flame retardants in the biosphere. N2 - Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umweltbeständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polystyrol (PS) und Polypropylen (PP) zum Einsatz, die jeweils mit polybromierten Flammschutzmitteln (PBFSM) versehen sind. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Auch soll mit Hilfe der RFA und der LA-ICP-MS die Abreicherung der PBFSM in den Modellmaterialien beschrieben werden. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden. T2 - 47. Jahrestagung der GUS 2018 CY - Stutensee - Blankenloch, Germany DA - 21.03.2018 KW - Polypropylen KW - Polystyrol KW - Flammschutzmittel KW - XRF KW - LA-ICP-MS PY - 2018 AN - OPUS4-47024 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Kombination von Radar und Neutronensonde zur Bestimmung der Massenfeuchte von Estrichen N2 - Leitungswasserschäden nahmen im Jahr 2016 mit rund 2,6 Milliarden Euro den größten Posten bei Gebäudeversicherungen ein. Die Bestimmung und Lokalisierung des Schadensausmaßes ist dabei ein erster wichtiger Schritt, um die erforderlichen Sanierungsarbeiten abschätzen und effizient vornehmen zu können. Hierfür sind Radar und Neutronensonden bereits etablierte Verfahren. Für verlässliche Aussagen zum quantitativen Feuchtegehalt eines Baustoffes werden jedoch zerstörende Sondierungsbohrungen zur Kalibrierung der aufgenommenen Daten benötigt. Dieser hohe zeitliche und finanzielle Aufwand soll zukünftig durch den parallelen Einsatz der genannten Messverfahren verhindert werden. In der durchgeführten Studie wurden Estrichprobekörper auf Zement- und Anhydritbasis mit variablen Dicken und Festigkeiten hergestellt und deren Austrocknung mit Radar und Neutronensonde über einen Zeitraum von 90 Tagen beobachtet. Als Referenzverfahren zur Ermittlung des Feuchteverlaufs dienten die gravimetrische Darr- und chemische Calcium-Carbid-Methode, welche an kleineren Schwesterproben der gleichen Charge angewendet wurden. Kontinuierliche Wägungen der größeren Probekörper gaben hierbei Aufschluss über den durch Austrocknung schwindende Wasseranteil. Aus dem aufgenommen Radardatensatz konnten anschließend markante Signalmerkmale im Zeit- und Frequenzbereich extrahiert und deren Zusammenhang zum Feuchtegehalt der Estrichtypen untersucht werden. Hierbei wurden gängige Methoden aus der Literatur zur Feuchtemessung mit Radar angewandt, wobei die Kombination dieser und das Hinzuziehen der Neutronensonde mittels Datenfusion zu einem höheren Informationsgehalt beiträgt. Somit kann eine zerstörungsfreie Quantifizierung des Feuchteschadens an schwimmenden Fußbodenaufbauten vorgenommen werden T2 - DACH-Jahrestagung DGZfP 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Radar KW - Feuchte KW - Neutronensonde KW - Datenfusion PY - 2019 AN - OPUS4-48153 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Kombination von Radar und Neutronensonde zur Bestimmung der Massenfeuchte von Estrichen N2 - Leitungswasserschäden nahmen im Jahr 2016 mit rund 2,6 Milliarden Euro den größten Posten bei Gebäudeversicherungen ein. Die Bestimmung und Lokalisierung des Schadensausmaßes ist dabei ein erster wichtiger Schritt, um die erforderlichen Sanierungsarbeiten abschätzen und effizient vornehmen zu können. Hierfür sind Radar und Neutronensonden bereits etablierte Verfahren. Für verlässliche Aussagen zum quantitativen Feuchtegehalt eines Baustoffes werden jedoch zerstörende Sondierungsbohrungen zur Kalibrierung der aufgenommenen Daten benötigt. Dieser hohe zeitliche und finanzielle Aufwand soll zukünftig durch den parallelen Einsatz der genannten Messverfahren verhindert werden. In der durchgeführten Studie wurden Estrichprobekörper auf Zement- und Anhydritbasis mit variablen Dicken und Festigkeiten hergestellt und deren Austrocknung mit Radar und Neutronensonde über einen Zeitraum von 90 Tagen beobachtet. Als Referenzverfahren zur Ermittlung des Feuchteverlaufs dienten die gravimetrische Darr- und chemische Calcium-Carbid-Methode, welche an kleineren Schwesterproben der gleichen Charge angewendet wurden. Kontinuierliche Wägungen der größeren Probekörper gaben hierbei Aufschluss über den durch Austrocknung schwindende Wasseranteil. Aus dem aufgenommen Radardatensatz konnten anschließend markante Signalmerkmale im Zeit- und Frequenzbereich extrahiert und deren Zusammenhang zum Feuchtegehalt der Estrichtypen untersucht werden. Hierbei wurden gängige Methoden aus der Literatur zur Feuchtemessung mit Radar angewandt, wobei die Kombination dieser und das Hinzuziehen der Neutronensonde mittels Datenfusion zu einem höheren Informationsgehalt beiträgt. Somit kann eine zerstörungsfreie Quantifizierung des Feuchteschadens an schwimmenden Fußbodenaufbauten vorgenommen werden T2 - DACH-Jahrestagung DGZfP 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Radar KW - Feuchte KW - Multiple Lineare Regression KW - Neutronensonde KW - Datenfusion PY - 2019 AN - OPUS4-48152 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Ultraschall-Messsystem für die Langzeitüberwachung von Betonkonstruktionen N2 - Ultraschallmessverfahren werden seit Langem erfolgreich für Prüfaufgaben im Bauwesen eingesetzt. Die dauerhafte Überwachung und frühzeitige Erkennung von Schäden an komplexen Neubauten und alternder Infrastruktur kann mittels Ultraschall-Transmissionsmessungen und speziellen Auswertemethoden, wie z. B. Korrelationverfahren und Codawelleninterferometrie, realisiert werden. Für die Dauerüberwachung wurde ein kompaktes System entwickelt, das Ultraschall-Messdaten erfassen und ins Internet auf einen FTP-Server übertragen kann. Es können hierbei alle angeschlossenen Prüfköpfe für jede Messung wahlweise als Sender oder Empfänger geschaltet werden. Es wurden Vorverstärker entwickelt, bei denen die Versorgung mit Strom über die Messleitung erfolgt. Dadurch können die Verstärker nahe am Prüfkopf positioniert werden. Durch Änderungen in den Ultraschall-Signalen können Schädigungen des Bauteils, wie z.B. Risse, in Echtzeit erkannt werden. T2 - DGZfP DACH-Jahrestagung CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Ultraschall KW - Monitoring KW - Codawelleninterferometrie KW - Eingebettete Sensorik PY - 2019 AN - OPUS4-48144 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Ultrasonic methods for quality assurance and condition assessment in nuclear concrete structures – lessons learned N2 - Ultrasonic non-destructive testing methods have found various applications in quality assurance and condition assessment of nuclear concrete structures. This includes but is not limited to the localization of construction features (thickness measurements, reinforcement, tendon ducts, and others) and damage detection (e. g. corrosion or cracks). However, there are still limitations, e. g. limited penetration depth and resolution, issues when testing hybrid steel/concrete structures as well as absence of standards and regulations. This presentation will show progress in some of these issues and will focus on advanced instrumentation and validation of ultrasonic NDT for concrete structures. Ultrasonic echo testing has been limited to a penetration depth of less than one meter in reinforced concrete. The development of the LAUS (Large Aperture Ultrasonic System), using a large array of ultrasonic transducers and wider offsets between transmitter and receiver, allows to reach up to 5 m in reinforced concrete and 9 m in unreinforced concrete. This capability has been demonstrated by collecting data from an engineered salt concrete barrier in an underground nuclear waste storage facility. Due to an increasingly competitive environment, commercial manufacturers will continue to develop equipment with enhanced penetration and/or increased resolution. To quantify the capabilities and reliability of ultrasonic tests, validation mockups with engineered flaws are required. EPRI and BAM have built a large-scale mockup at a test site close to Berlin (BAM-TTS, Horstwalde) using a design which is repeated at other places. This presentation will also cover the methods deployed on engineered flaws and the repeatability of the test results. T2 - NDE in Nuclear CY - Charlotte, NC, USA DA - 25.7.2019 KW - Concrete KW - Nuclear Structures KW - Ultrasound PY - 2019 AN - OPUS4-48690 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Johann, Sergej A1 - Wu, Cheng-Chieh T1 - KonSens - RFID embedded² systems in concrete – validation experiments N2 - Structural Health Monitoring (SHM) is an important part of buildings surveillance and maintenance to detect material failure as early as possible and to contribute in protection of structures and their users. The implementation of Radio Frequency Identification (RFID) sensor systems without cable connection and battery into building components offers innovative possibilities to enable long-term in-situ SHM of addressed structures, bridges. The objectives of the presented study are complete embedding of RFID sensors systems in concrete, full passive communication with the systems, at best for the whole life span of structures. One challenge for this task is the highly alkaline environment in concrete, which requires non-degrading and robust encapsulation. Further Requirements are passive communication and energy supply, appropriate antenna design, placement and fixation in concrete, and the selection and implementation of sensors and connections. The concept is to develop and optimize a simple and robust system, which meets the requirements, as well as comprehensive validation in concrete specimen and real world applications. Two different systems were developed (HF and UHF RFID, respectively). First tasks were the implementation of analog sensors using the superposition principle for the signal adaption. Investigation of suitable materials for robust encapsulation and sensor protection against basic environments. Four materials were investigated in pH 13 solution for 14 days - 3D-Printer-Polymer was completely resolved - PVC has no noticeable decrease in weight - (VitaPro) glass filter for the sensor protector, has weight loss 2.7 % - The epoxy resin has increased by 1.8 % due to moisture expansion Different concrete samples were prepared for the validation of the systems. RFID sensors were embedded in different integration depths. Investigate the energy- and data transfer through concrete, also with varying moisture content. Additionally, signal strength data was used to optimize and validate the antenna characteristics in concrete. Next steps are to guarantee a sufficient energy supply for UHF RFID systems embedded in different concrete mixtures and further embedding the HF and UHF RFID systems in real bridges and buildings to validate the long term monitoring. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures (SMAR 2019) CY - Potsdam, Germany DA - 27.08.2019 KW - Passive RFID KW - RFID sensors KW - Sensors in concrete KW - Smart structures KW - Structural health monitoring PY - 2019 AN - OPUS4-48790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moosavi, Robabeh A1 - Grunwald, Marcel A1 - Redmer, Bernhard A1 - Nerger, Deborah A1 - Hille, Falk A1 - Kühn, T. A1 - Hering, M. T1 - Damage investigations of concrete under impact load using laminography N2 - We examine the behavior of reinforced concrete components subjected to impact induced loading conditions which might be caused by vessels collisions such as aircraft fuel tanks The concrete plates were impact damaged at TU Dresden and shipped to BAM At BAM laminar tomography as the imaging method is used to determine and quantify the damage state An automatic crack detection method based on template matching is applied to find the cracks and we aim to develop a new method using machine learning Algorithms In addition numerical models are developed to understand the experiment and to predict the damage structures based on failure mechanisms. T2 - DCMS Summer School MATERIALS 4.0 CY - Dresden, Germany DA - 10.09.2018 KW - Laminography KW - Crack detection KW - Reinforced concrete KW - 3D imaging PY - 2018 AN - OPUS4-48637 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Testbeds for standardization in the IIoT N2 - The poster presents our research findings on the role and impacts of testbeds in standardization for the industrial internet of things. Based on a multiple case study, four different approaches were identified followed in the testbeds with regard to their standardization activities. T2 - BRIDGIT2 conference at NSAI CY - Dublin, Irland DA - 11.09.2019 KW - IIoT KW - Normen KW - Industrie 4.0 KW - Standards KW - Normung KW - Standardization KW - Testbed PY - 2019 AN - OPUS4-48937 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine A1 - Munsch, Sarah Mandy T1 - Potential automatisierter NMR-Messungen zur Ermittlung von Hydratationseigenschaften - ein Vergleich mit Vicat- und Wärmeflusskalorimetrie-Ergebnissen N2 - Es werden Ergebnisse von 1H-NMR-Relaxometrie-Messungen an Salzbeton und einem alkali-aktivierten Material, die im Rahmen des Themenfeldprojektes Seal Waste Safe durchgeführt werden, vorgestellt. Dabei wird die zeitliche Entwicklung von ausgewählten Merkmalen der ermittelten T2-Relaxationszeitenverteilungen während der Hydratation betrachtet. Als Referenz zur Identifikation von charakteristischen Hydratationsereignissen dienen der Vicat-Nadeleindringversuch und Wärmeflusskalorimetrie. T2 - Online-Workshop „Dauerhafte Verschlussbauwerke für Endlager“ CY - Online meeting DA - 14.02.2022 KW - NMR-Relaxometrie KW - Alkali-aktiviertes Material KW - Salzbeton KW - Seal Waste Safe PY - 2022 AN - OPUS4-54945 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mirtsch, Mona A1 - Koch, Claudia A1 - Asna Ashari, Parsa A1 - Blind, K. A1 - Castka, P. T1 - Quality assurance in supply chains during the COVID-19 pandemic: Empirical evidence on organisational resilience of conformity assessment bodies N2 - Global supply chains rely on the compliance and safety of their products, processes, and facilities. These vital services (often referred to as ‘quality assurance’ or ‘conformity assessment’ services) are provided by Conformity Assessment Bodies (CABs). This empirical study explores the impact of the COVID-19 pandemic on CABs as well as their response to the resulting challenges. Data was gathered through an online survey among all accredited CABs in Germany, which resulted in 555 valid responses. Taking a resilience perspective, we reveal that CABs were hit hard by the disruptions caused by the pandemic, albeit to different degrees, in part due to their type of services, size, and sectors served. Furthermore, we find that contingency plans do not directly cushion order declines (as the main indicator of the economic impact of the pandemic) but rather indirectly through helping CABs respond more quickly, which in turn mitigates their order declines. However, our results show that contingency plans can also have adverse effects if they hinder flexible reaction to the crisis. The findings of our study help managers and policymakers learn from the COVID-19 pandemic and improve the resilience of the conformity assessment sector and quality assurance in the event of future crises. KW - Quality Infrastructure KW - Digitalization KW - Testing laboratories KW - Organizational resilience KW - COVID-19 KW - Conformity assessment PY - 2022 DO - https://doi.org/10.1080/14783363.2022.2078189 SP - 1 EP - 23 PB - Taylor & Francis AN - OPUS4-55066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - García Fernández, J. A1 - Sánchez-González, C. A1 - Bettmer, J. A1 - Llopi, J. A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Montes-Bayón, M. T1 - Quantitative assessment of the metabolic products of iron oxide nanoparticles to be used as iron supplements in cell cultures N2 - Iron nanoparticles (NPs) metabolism is directly associated to human health due to their use as anemia treatment and should be studied in detail in cells. Here we present a speciation strategy for the determination of the metabolic products of iron oxide nanoparticles coated by tartaric and adipic acids in enterocytes-like cell models (Caco-2 and HT-29). Such methodology is based on the use of SDS-modified reversed phase high performance liquid chromatography (HPLC) separation using inductively coupled plasma-mass spectrometry (ICP-MS) as Fe selective detector. Post-column isotope dilution analysis is used as quantification tool by adding Fe-57 as isotopically enriched standard. To assess the separation capability of the method, two different iron nanostructures: iron sucrose nanoparticles -Venofer®- used as model suspension and iron tartrate/adipate-modified nanoparticles, both of about 4 nm (core size) were evaluated. The two nanostructures were injected into the system showing good peak profiles and quantitative elution recoveries (>80%) in both cases. In addition, both nanoparticulate fractions could be based-line separated from ionic iron species, which needed to be complexed with 1mM citrate to elute from the column. Exposed cells up to 0.5mM of iron tartrate/adipate-modified nanoparticles were specifically treated to extract the internalized NPs and the extracts examined using the proposed strategy. The obtained results revealed the presence of three different fractions corresponding to nanoparticle aggregates, dispersed nanoparticles and soluble iron respectively in a single chromatographic run. Quantitative experiments (column recoveries ranging from 60 to 80%) revealed the presence of the majority of the Fe in the nanoparticulated form (>75%) by summing up the dispersed and aggregate particles. Such experiments point out the high uptake and low solubilization rate of the tartrate/adipate NPs making these structures highly suitable as Fe supplements in oral anemia treatments. KW - Fe nanoparticles metabolism KW - Cells KW - HPLC-ICP-MS KW - Species-unspecific on-line isotope dilution PY - 2018 DO - https://doi.org/10.1016/j.aca.2018.08.003 SN - 0003-2670 VL - 1039 SP - 24 EP - 30 PB - Elsevier CY - Amsterdam AN - OPUS4-46817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, Holger T1 - An insight into fractionated environmental water samples to understand matrix effects in immunoassays N2 - N4-acetyl-SMX is the most important cross-reacting compound for the SMX-ELISA with concentrations of 1064 - 2488 ng/L in influent wastewater and 40 - 160 ng/L in effluent wastewater. The ELISAgrams for estrone show less interfering signals than for SMX. ELISAgrams of SMX and estrone display in effluent wastewater more interfering signals than in influent wastewater. T2 - ANAKON CY - Graz, Austria DA - 23.03.2016 KW - Sulfamethoxazole KW - Estrone KW - LC-ELISA KW - Matrix effects PY - 2015 AN - OPUS4-35792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Axel A1 - Altmann, Korinna A1 - Kocher, B. A1 - Braun, U. T1 - Determination of tire wear markers in soil samples and their distribution in a roadside soil N2 - Tire wear (TW) constitutes a significant source of microplastic in terrestrial ecosystems. It is known that particles emitted by roads can have an effect up to 100 m into adjacent areas. Here, we apply for the first-time thermal extraction desorption gas chromatography-mass spectrometry (TED-GC/MS) to determine TW in soil samples by detection of thermal decomposition products of styrene-butadiene rubber (SBR), without additional enrichment. Additionally, zinc contents were determined as an elemental marker for TW. Mixed soil samples were taken along three transects along a German motorway in 0.3, 2.0, and 5.0 m distance from the road. Sampling depths were 0–2, 2–5, 5–10, and 10–20 cm. Four fine fractions, 1 000–500, 500–100, 100–50, and <50 μm, were analyzed. TW contents based on SBR ranged from 155 to 15 898 mg kg−1. TW contents based on zinc were between 413 and 44 812 mg kg−1. Comparison of individual values of SBR and zinc reveals SBR as a more specific marker. Results confirm that most TW ends up in the topsoil within a 2 m distance. The sampling strategy resulted in representative data for a larger area. Standard deviations of quadruple TED-GC/MS determination of SBR were <10% for all grain size fractions. TED-GC/MS is a suitable analytical tool for determining TW in soil samples without the use of toxic chemicals, enrichment, or special sample preparation. KW - Microplastic KW - TED-GC/MS KW - Tire wear PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543344 DO - https://doi.org/10.1016/j.chemosphere.2022.133653 VL - 294 SP - 1 EP - 8 PB - Elsevier Ltd. AN - OPUS4-54334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Oliveira Guilherme Buzanich, Ana A1 - Cakir, Cafer Tufan A1 - Radtke, Martin A1 - Haider, M. Bilal A1 - Emmerling, Franziska A1 - F. M. Oliveira, P. A1 - Michalchuk, Adam T1 - Dispersive x-ray absorption spectroscopy for time-resolved in situ monitoring of mechanochemical reactions N2 - X-ray absorption spectroscopy (XAS) provides a unique, atom-specific tool to probe the electronic structure of solids. By surmounting long-held limitations of powder-based XAS using a dynamically averaged powder in a Resonant Acoustic Mixer (RAM), we demonstrate how time-resolved in situ (TRIS) XAS provides unprecedented detail of mechanochemical synthesis. The use of a custom-designed dispersive XAS (DXAS) setup allows us to increase the time resolution over existing fluorescence measurements from ∼15 min to 2 s for a complete absorption spectrum. Hence, we here establish TRIS-XAS as a viable method for studying mechanochemical reactions and sampling reaction kinetics. The generality of our approach is demonstrated through RAM-induced (i) bottom-up Au nanoparticle mechanosynthesis and (ii) the synthesis of a prototypical metal organic framework, ZIF-8. Moreover, we demonstrate that our approach also works with the addition of a stainless steel milling ball, opening the door to using TRIS-DXAS for following conventional ball milling reactions. We expect that our TRIS-DXAS approach will become an essential part of the mechanochemical tool box. KW - In situ studies KW - Dipsersive XAS KW - Mechanochemistry KW - Time-resolved PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567659 DO - https://doi.org/10.1063/5.0130673 SN - 1089-7690 VL - 157 IS - 21 SP - 1 EP - 12 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-56765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Roesch, Philipp A1 - Wittwer, Philipp A1 - Sommerfeld, Thomas A1 - Riedel, Maren A1 - Leube, Peter A1 - Kalbe, Ute A1 - Schoknecht, Ute A1 - Simon, Franz-Georg T1 - Per- and Polyfluoroalkyl Substances (PFAS) in Ski Waxes and Snow from Cross-Country Skiing in Germany - Comparative study of Sum Parameter and Target Analysis N2 - Per- and polyfluoroalkyl substances (PFAS) are often environmentally exposed via discharge through human consumer products, such as ski waxes. In our study we analyzed various ski waxes from the 1980s and 2020s, to determine both the sum parameter values total fluorine (TF), extractable organically bound fluorine (EOF), hydrolysable organically bound fluorine (HOF) as well as targeted PFAS analysis. This showed that modern high-performance waxes contain up to 6 % TF, but also PFAS-free labelled ski waxes contain traces of PFAS with EOF/HOF values in the low mg kg-1 range. With the ban of all fluorine-based waxes with the start of the 2023/2024 winter season this will probably change soon. Moreover, we applied our analysis methods to snow samples from a frequently used cross country ski trail (Kammloipe) in the Ore Mountain region in Germany, assessing the potential PFAS entry/discharge through ski waxes. Melted snow samples from different spots were analyzed by the adsorbable organically bound fluorine (AOF) sum parameter and PFAS target analysis and confirmed the abrasion of the ski waxes into the snow. Moreover, on a PFAS hotspot also soil samples were analyzed, which indicate that PFAS from the ski waxes adsorb after snow melting into the soil. KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Consumer Products PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612760 DO - https://doi.org/10.1016/j.hazadv.2024.100484 VL - 16 SP - 1 EP - 5 PB - Elsevier B.V. AN - OPUS4-61276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Linberg, Kevin A1 - Röder, Bettina A1 - Al-Sabbagh, Dominik A1 - Emmerling, Franziska A1 - Michalchuk, Adam T1 - Controlling polymorphism in molecular cocrystals by variable temperature ball milling N2 - Mechanochemistry offers a unique opportunity to modify and manipulate crystal forms, often providing new products as compared with conventional solution methods. While promising, there is little known about how to control the solid form through mechanochemical means, demanding dedicated investigations. Using a model organic cocrystal system (isonicotinamide:glutaric acid), we here demonstrate that with mechanochemistry, polymorphism can be induced in molecular solids under conditions seemingly different to their conventional thermodynamic (thermal) transition point. Whereas Form II converts to Form I upon heating to 363 K, the same transition can be initiated under ball milling conditions at markedly lower temperatures (348 K). Our results indicate that mechanochemical techniques can help to reduce the energy barriers to solid form transitions, offering new insights into controlling polymorphic forms. Moreover, our results suggest that the nature of mechanochemical transformations could make it difficult to interpret mechanochemical solid form landscapes using conventional equilibrium-based tools. KW - Mechanochemistry KW - Polymorphism KW - TRIS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564728 DO - https://doi.org/10.1039/d2fd00115b SP - 1 EP - 16 PB - Royal Society of Chemistry AN - OPUS4-56472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Belenguer, A. A1 - Lampronti, G. A1 - Michalchuk, Adam A1 - Emmerling, Franziska A1 - Sanders, J. T1 - Quantitative reversible one pot interconversion of three crystalline polymorphs by ball mill grinding N2 - We demonstrate here using a disulfide system the first example of reversible, selective, and quantitative transformation between three crystalline polymorphs by ball mill grinding. This includes the discovery of a previously unknown polymorph. Each polymorph is reproducibly obtained under well-defined neat or liquid-assisted grinding conditions, revealing subtle control over the apparent thermodynamic stability. We discovered that the presence of a contaminant as low as 1.5% mol mol−1 acting as a template is required to enable all these three polymorph transformations. The relative stabilities of the polymorphs are determined by the sizes of the nanocrystals produced under different conditions and by surface interactions with small amounts of added solvent. For the first time, we show evidence that each of the three polymorphs is obtained with a unique and reproducible crystalline size. This mechanochemical approach gives access to bulk quantities of metastable polymorphs that are inaccessible through recrystallisation. KW - Mechanochemistry KW - Polymorph KW - XRD PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549934 DO - https://doi.org/10.1039/D2CE00393G SP - 1 EP - 7 PB - Royal Society of Chemistry AN - OPUS4-54993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Linberg, Kevin A1 - Emmerling, Franziska A1 - Michalchuk, Adam T1 - Unintended Rate Enhancement in Mechanochemical Kinetics by Using Poly(methyl methacrylate) Jars N2 - Time-resolved in situ (TRIS) X-ray diffraction has changed how mechanochemical transformations are studied but requires the use of X-ray transparent jars often made from poly(methyl methacrylate) (PMMA). However, using PMMA jars can alter the apparent kinetics of mechanochemical polymorphism by an order of magnitude, questioning the interpretability of established TRIS methods. Our results suggest that rate enhancement in PMMA jars may not be dominated by chemical effects of the polymer, but rather a result of different equilibrium temperatures within the jar. These features must be better understood before control over mechanochemical reactions can be achieved. KW - Mechanochemistry KW - Organic compounds KW - Polymers KW - Materials PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565276 DO - https://doi.org/10.1021/acs.cgd.2c01227 SN - 1528-7483 SP - 1 EP - 5 PB - ACS Publications AN - OPUS4-56527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Scholz, Philipp A1 - Kalbe, Ute A1 - Caliebe, W. A1 - Tayal, A. A1 - Vasala, S. J. A1 - Simon, Franz-Georg T1 - Speciation of antimony and vanadium in municipal solid waste incineration ashes analyzed by XANES spectroscopy N2 - The use of ashes from municipal solid waste incineration as secondary building materials is an important pillar for the circular economy in Germany. However, leaching of potential toxic elements from these materials must be at environmentally acceptable levels. Normally, a three-month ageing period immobilizes most hazardous heavy metals, but antimony (Sb) and vanadium (V) showed previously unusual leaching. In order to clarify the mechanisms, we analyzed the Sb and V species in various bottom and fly ashes from municipal waste incineration by XANES spectroscopy. Antimony oxidizes from Sb(+ III) species used as flame retardants in plastics to Sb(+ V) compounds during waste incineration. However, owing to the similarity of different Sb(+ V) compound in the Sb K- and L-edge XANES spectra, it was not possible to accurately identify an exact Sb(+ V) species. Moreover, V is mainly present as oxidation state + V compound in the analyzed ashes. However, the coarse and magnetic fraction of the bottom ashes contain larger amounts of V(+ III) and V(+ IV) compounds which might enter the waste incineration from vanadium carbide containing steel tools. Thus, Sb and V could be critical potential toxic elements in secondary building materials and long-term monitoring of the release should be taken into account in the future. KW - Müllverbrennung KW - XANES spectroscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-599841 DO - https://doi.org/10.1007/s10163-024-01954-2 SN - 1438-4957 VL - 26 SP - 2152 EP - 72158 PB - Springer Science and Business Media LLC AN - OPUS4-59984 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Michalchuk, Adam A1 - Emmerling, Franziska T1 - Manipulating the dynamics of mechanochemical ternary cocrystal formation N2 - The mechanism of ternary cocrystal formation, and the potential role of intermediate binary phases, has been debated for some time. We report here the first in situ real-time monitoring of two prototypic ternary cocrystals. Our results suggest that the question is more complicated than previously considered. The mechanism of mechanochemical ternary cocrystal formation depends on the milling conditions, here the milling frequency and addition of liquid. Binary phases can form under certain conditions, but do not act as intermediates in the formation of the ternary cocrystals. Rather, binary phases are competitive with the ternary phase, and their formation appears to compete with that of the ternary components. The presence of binary phases leads to an increase in the overall reaction time. The results reported here offer the first insights into the true complexities of mechanochemical multi-component synthesis of higher order multi-component crystals and demonstrate a new understanding of the influence of milling condition for the study of mechanisms and kinetics. KW - Mechanochemistry KW - In situ KW - Cocrystal PY - 2019 UR - https://pubs.rsc.org/en/content/articlepdf/2019/cc/c9cc03034d DO - https://doi.org/10.1039/c9cc03034d SN - 1364-548X VL - 55 IS - 66 SP - 9793 EP - 9796 PB - RSC AN - OPUS4-48613 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ketelsen, T. A1 - Wintermann, Carsten A1 - Melzer, C. A1 - Dietz, Georg A1 - Golle, U. A1 - Hahn, Oliver ED - Cole, M. ED - Dogramaci, B. ED - Lehmann, A.-S. ED - Sölch, B. ED - Wedekind, G. T1 - Connoisseurship and the Investigation of Materiality: Four “Rembrandt” Drawings in Weimar N2 - The aim of this paper is to present the productive interplay of connoisseurship and material analysis when dealing with drawings by Rembrandt – or previously attributed to him – in the collection of the Klassik Stiftung Weimar. This concerns the more precise determination of the drawing materials used and the reconstruction of the genesis of the drawings discussed. The material analysis allows us to decide whether and how Rembrandt’s inks can be used to determine authorship at all. The “material turn” in drawing studies thus intervenes in the discussion about authorship and opens up a broader production aesthetic perspective. No longer the “style” but rather the handeling becomes the decisive criterion for answering the question “Rembrandt, or not?” KW - Archaeometry KW - History of Art KW - Drawings KW - Rembrandt PY - 2021 SN - 0044-2992 VL - 84 IS - 4 SP - 483 EP - 518 PB - Deutscher Kunstverlag CY - Berlin/München AN - OPUS4-54342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Hahn, Oliver ED - Danielewski, A. ED - Nöller, Renate ED - Doil, Thorsten T1 - Manuscripta americana - Tras las huellas de los aztecas - La exposición en la Kulturwerk en la Staatsbibliothek zu Berlin - 07 diciembre 2022 hasta el 26 de febrero de 2023 T1 - Manuscripta americana - Den Azteken auf der Spur - Eine Ausstellung im Kulturwerk der Staatsbibliothek zu Berlin - 07. Dezember 2022 bis 26. Februar 2023 N2 - Esta publicación, que acompaña a la exposición Manuscripta americana. Tras las huellas de los aztecas, se ocupa de una colección excepcional de manuscritos mexicanos y sudamericanos. La colección se inició cuando, a principios del siglo XIX, Alexander von Humboldt donó a la Biblioteca Real de Berlín varios fragmentos de manuscritos pictográficos indígenas del siglo XVI procedentes del actual México. Estos documentos, conocidos habitualmente como Fragmentos Humboldt, representan la parte más notable de la colección, que con el tiempo se fue ampliando a través de la adquisición de diferentes manuscritos mesoamericanos, principalmente escritos en lenguas indígenas con caracteres latinos. Entre abril de 2017 y marzo de 2019, la Staatsbibliothek zu Berlin - PK (SBB) y el Bundesanstalt für Materialforschung und -prüfung (BAM) llevaron a cabo un proyecto científico conjunto, financiado generosamente por la Deutsche Forschungsgemeinschaft (DFG) con el nombre de Análisis material y estudios histórico-culturales de manuscritos coloniales mexicanos en Berlín y Cracovia. Los principales objetivos del proyecto fueron determinar la procedencia de los manuscritos americanos y, dado que presentan un alto grado de fragmentación, establecer sus relaciones internas y las que establecen con otros objetos ajenos a la colección. Para ello, se combinaron métodos de análisis de corte etnográfico, cultural e histórico con otros propios de las ciencias naturales. Gracias a la buena cooperación con la Bibliotheka Jagiellońska tuvimos acceso tanto a los Manuscripta americana de Berlín como a los de Cracovia, pudiendo proceder a su examen exhaustivo y realizar exámenes científicos de alta precisión. N2 - Die Publikation befasst sich mit einer einzigartigen Sammlung mexikanischer und südamerikanischer Handschriften, die zu Beginn des 19. Jahrhunderts ins Leben gerufen wurde, als Alexander von Humboldt der Königlichen Bibliothek zu Berlin Fragmente indigener mexikanischer Bilderhandschriften aus dem 16. Jahrhundert schenkte. Sie sind heute auch unter der Bezeichnung Humboldt-Fragmente bekannt und stellen den bedeutendsten Teil der Sammlung dar, die im Laufe der Zeit durch den Ankauf verschiedener Arten von Handschriften aus Mittelamerika, vorwiegend in indigenen Sprachen und lateinischer Schrift, erweitert wurde. In den zwei Jahren von April 2017 bis März 2019 verfolgten die Staatsbibliothek zu Berlin – Preußischer Kulturbesitz (SBB-PK) und die Bundesanstalt für Materialforschung und -prüfung (BAM) ein gemeinsames, von der Deutschen Forschungsgemeinschaft (DFG) großzügig gefördertes wissenschaftliches Projekt: Materialanalysen und kulturgeschichtliche Untersuchungen mexikanischer Handschriften aus der Kolonialzeit in Berlin und Krakau. Die Hauptziele des Projekts bestanden darin, die Provenienz der Manuscripta americana zu ermitteln und, da sie einen hohen Grad an Fragmentierung aufweisen, festzustellen, wie sie untereinander und mit Objekten außerhalb der Sammlung in Beziehung stehen. Zu diesem Zweck wurden ethno-kulturhistorische und naturwissenschaftliche Methoden kombiniert. Dank einer guten Zusammenarbeit mit der Jagiellonen-Bibliothek konnten wir die Manuscripta americana sowohl in Berlin als auch in Krakau sehen und studieren und sie wissenschaftlich vermessen. T2 - Manuscripta americana - Tras las huellas de los aztecas - La exposición en la Kulturwerk en la Staatsbibliothek zu Berlin CY - Berlin, Germany DA - 07.12.2022 KW - Amate KW - Arqueometria KW - Manuscrito KW - Pruebas no destructivas PY - 2022 SN - 2567-1251 N1 - Es gibt parallele Sprachausgaben (deutsch und englisch), Links befinden sich im Feld zugehöriger Identifikator - There are parallel language editions (German and English), links are in the field related identifier VL - 4 SP - 1 EP - 120 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-62427 LA - spa AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Hahn, Oliver ED - Danielewski, A. ED - Nöller, Renate ED - Doil, Thorsten T1 - Manuscripta americana - Fragments of the Aztec legacy - An exhibition at Kulturwerk in the Staatsbibliothek zu Berlin - December 07, 2022 until February 26, 2023 N2 - This publication, which accompanies the exhibition Manuscripta americana - On the traces of the Aztecs, concerns a unique collection of Mexican and South American manuscripts. The collection was established at the beginning of the 19th century, when Alexander von Humboldt donated fragments of 16th century indigenous Mexican pictorial manuscripts to the Royal Library in Berlin. Today these are also known as the Humboldt fragments and represent the most significant part of a collection that was augmented over the years by the purchase of various types of Mesoamerican manuscripts, mainly in indigenous languages with Latin script. During the two year period from April 2017 to March 2019, the Berlin State Library (SBB - SPK) and the Bundesanstalt für Materialforschung und -prüfung (BAM) carried out a joint scientific project funded by the Deutsche Forschungsgemeinschaft (DFG) entitled "Material-analytical and cultural-historical examinations of colonial-period manuscripts from Mexico in Berlin and Cracow." The main objectives of the project were to determine the provenance of the Manuscripta americana and, since they exhibit a high degree of fragmentation, to examine how they are related to each other and to objects outside the collection. The investigation combined ethnocultural-historical and materials science methods of analysis. Thanks to the constructive partnership with the Jagiellonian Library, we were able to see and study the Manuscripta americana in both Kraków and Berlin and to carry out scientific measurements on them. T2 - Manuscripta Americana - Fragments of the Aztec Legacy - An Exhibition at Kulturwerk in the Staatsbibliothek zu Berlin CY - Berlin, Germany DA - 07.12.2022 KW - Amate KW - Archaeometry KW - Manuscripts KW - Nondestructive testing PY - 2022 SN - 2567-1251 N1 - Es gibt parallele Sprachausgaben (deutsch und spanisch), Links befinden sich im Feld zugehöriger Identifikator - There are parallel language editions (German and Spanish), links are in the field related identifier VL - 4 SP - 1 EP - 120 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-62419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steger, Simon A1 - Stege, H. A1 - Bretz, S. A1 - Hahn, Oliver ED - Tomasin, P. T1 - Disclosing glittering and sparkling effects in 20th-century reverse glass paintings: a study of metallic pigments and metal foils by means of in situ XRF and DRIFTS analysis N2 - This work presents a spectroscopic study of metallic pigments and metal foils used in reverse glass paintings that were created between 1912 and 1954. Metallic pigments induce a notable sparkling effect by means of the lateral incidence of light, whereas metal foils enhance the gloss and create a glittering effect when the painting is viewed in reflected light. Both effects were desired features especially in modern reverse paintings on glass and applied by artists in manifold creative manner. The paper gives an overview on the composition of the metalfoils and metal pigments in 14 works as determined in situ by X-ray spectrometry. Metal foils made of tin, brass, aluminium and silver were found in nine paintings. Gold imitating Cu-Zn pigments in different hues and with various Cu/Zn net intensity ratios were recorded for six paintings. Silvery pigments were identified mainly as Al pigments, but also as Cu-Zn-Ni alloy in one case. Other uncommon metallic pigments were detected in Arlequin vindicatif (c. 1925) by Floris Jespers, who used not only Cu-Zn and Al pigments, but also brownish Cu and Cu-Zn-Sn pigments. Non-invasive diffuse reflectance infrared Fourier-transform spectroscopy (DRIFTS) was used to classify the binding media of the metallic pigments. Drying oil and natural resin probably mixed with oil were the most common binding media. A polysaccharide-based binder was found in the silvery Cu-Zn-Ni pigment of Ohne Titel (1954) by Marianne Uhlenhuth. KW - Archaeometry KW - Non-invasive analysis KW - Reverse paintings on glass PY - 2020 DO - https://doi.org/10.1016/j.culher.2020.11.008 SN - 1296-2074 VL - 48 SP - 196 EP - 204 PB - Elsevier Masson SAS CY - Amsterdam AN - OPUS4-54428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reed, B.P. A1 - Radnik, Jörg A1 - Shard, A.G. T1 - Ionic liquid [PMIM]+[NTf2]− (Solarpur®) characterized by XPS N2 - X-ray photoelectron spectroscopy (XPS) was performed on the meniscus of a droplet of ionic liquid 1-propyl-3-methyl-imidazolium bis(trifluoromethylsulfonyl) imide [PMIM]+[NTf2]− (Solarpur®) in ultrahigh vacuum. High-resolution spectra of F 1s, O 1s, N 1s, C 1s, and S 2p are presented along with a survey spectrum and the valence band structure. The spectra presented here were generated using monochromatic Al Kα radiation (1486.6 eV). KW - Ionic liquid KW - 1-propyl-3-methyl-imidazolium bis(trifluoromethylsulfonyl)imide KW - X-ray Photoelectron Spectroscopy PY - 2022 DO - https://doi.org/10.1116/6.0001518 VL - 29 IS - 1 SP - 014001-1 PB - AVS AN - OPUS4-54335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Colours, nano and surface N2 - The basic ideas of colours and pigments are presented. The correlation between nanomaterials and colours are explained. Different methods are presented for investigating nanoparticles and their surface. At the end a case study is presented explaining the importance of coating for the properties of nanoparticles. T2 - Eingeladener Vortrag im Deutschen Lackmuseum (Münster) CY - Online meeting DA - 11.02.2022 KW - Pigments KW - Surface Analytics KW - Coatings PY - 2022 AN - OPUS4-54376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Dietz, Georg A1 - Golle, U. A1 - Hahn, Oliver A1 - Ketelsen, T. A1 - Melzer, C. A1 - Wintermann, Carsten ED - Semff, M. T1 - Der fabelhafte Möglichmacher N2 - Der Beitrag würdigt die Verdienste Wolfgang Hollers bei der Etablierung fächerübergreifender Kooperationen zwischen Natur- und Geisteswissenschaften innerhalb der Zeichnungsforschung. KW - Archäometrie PY - 2022 SN - 978-3-947641-20-8 SP - 370 EP - 371 PB - Sieveking Verlag CY - München AN - OPUS4-54355 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver T1 - Materialität von Musikhandschriften N2 - Die Bezeichnung „Tinte auf Papier“ bietet einen guten Einstieg in die Beschreibung der Materialität von Musikhandschriften; so haben sich zahlreiche Manuskripte erhalten, die mit Eisengallustinte auf Hadernpapier verfasst wurden. Das Papier besteht aus Fasern meist pflanzlicher Herkunft und wird durch Entwässerung einer Fasersuspension auf einem Sieb gebildet. Der Abdruck des Schöpfsiebes (die Papierstruktur) und ein vorhandenes Wasserzeichen bieten Anhaltspunkte für Provenienz und Datierung; daneben erlaubt die Analyse der Fasern, der Füllstoffe und der Leimung eine weitere Charakterisierung des Schriftträgers. Spätestens seit dem Mittelalter sind es Eisengallustinten, die das schwarze bis bräunliche Erscheinungsbild vieler Manuskripte auf Papier hervorrufen. Daneben lassen sich auch schwarze Rußtuschen oder farbige Auszeichnungstuschen nachweisen. Eisengallustinten werden durch Mischung einer eisenhaltigen Komponente mit Gerbstoffen hergestellt. Eisensulfat ist die am häufigsten genannte Eisen liefernde Zutat, daneben sind aber auch eisenhaltige Minerale, Nägel oder Rost denkbar. Die Gallussäure leitet sich ab aus den Galläpfeln, der krankhaften Veränderung einzelner Planzenteile verschiedener Eichenarten. Diese werden durch die Eiablage von Schlupfwespen hervorgerufen. Wie schon beim Papier ermöglicht der materialanalytische Nachweis charakteristischer Beimischungen oder Verunreinigungen innerhalb der Tinten die Beantwortung kulturhistorischer Fragestellungen – gemeint sind hier die Unterscheidung von Original und Korrektur oder die Sichtbarmachung späterer Ergänzungen. T2 - DFG-Rundgespraech zur Thermographie-Digitalisierung von Wasserzeichen in Musikhandschriften CY - Vienna, Austria DA - 23.10.2023 KW - Thermographie KW - Manuskripte KW - Wasserzeichen KW - Papier PY - 2023 AN - OPUS4-58798 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - ToF-SIMS at advanced materials - from nano to energy N2 - The basic principles of ToF-SIMS will be explained. Examples of the use of ToF-SIMS for the investigation of titania and core-shell nanoplastic will be given. Furhtermore, 3d reconstruction is explained for nanoparticle research and energy-related materials. T2 - BUA Summer School Mass Spectrometry CY - Berlin, Germany DA - 04.10.2022 KW - ToF-SIMS KW - Nanomaterials KW - Imaging PY - 2022 AN - OPUS4-55897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Singh, Chandan T1 - Functionalized Titanium Carbide Nanosheets based Biosensor for Detection of the SARS-CoV-2 Nucleocapsid Protein N2 - MXenes are a new family of two-dimensional (2D) transition metal carbides, carbonitrides, and nitrides discovered in 2011. Among many reported family members, titanium carbide is the most widely studied and explored due to the optimized synthesis conditions and promising characteristics like good mechanical strength, solution processability, and excellent conductivity. Here, we report the development of an electrochemical biosensor involving the amine-functionalized Few-Layered-Titanium Carbide Nanosheets and monoclonal antibodies against the SARS-CoV-2 nucleocapsid protein (anti-SARS-CoV-2 mAb) to design a point-of-care device for detection of the SARS-CoV-2 nucleocapsid protein (SARS-CoV-2 NP) antigen. T2 - SALSA's Make and Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - MXenes KW - Titanium Carbide Nanosheets KW - Biosensors KW - Electrochemistry PY - 2022 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. AN - OPUS4-55856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas T1 - Rissentwicklung in CFK-Laminaten nachgewiesen durch in situ Röntgen-Refraktion N2 - In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Röntgen-Refraktion KW - Synchrotronstrahlung KW - CFK KW - Rissentwicklung PY - 2023 AN - OPUS4-57622 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Richard A1 - Oehrl, A. A1 - Wischerhoff, E. A1 - Wosniok, Aleksander A1 - Schukar, Marcus T1 - Fiber-Optic Thermoresponsive Polymer-based Temperature Sensor for Process Monitoring N2 - We present a high-precision fiber-optic temperature sensor based on a polymer possessing a Lower Critical Solution Temperature (LCST) in aqueous solution encapsulated in a capillary. For a temperature higher than the LCST the transparent homogenous polymer solution changes into a suspension which forms an opaque fluid. The resulting temperature-dependent turbidity influences the transmission characteristics measured using a simple fiber-optic system. The presented development provides a small-sized, robust temperature sensor, patented by the BAM (patent nr.: EP 3 043 161 B1), easy to integrate in many application fields, especially for process monitoring. T2 - European Workshop on Optical Fibre Sensors (EWOFS 2023) CY - Mons, Belgium DA - 23.05.2023 KW - Thermoresponsive polymer KW - Aqueous polymer solution KW - Temperature sensor KW - LCST KW - POF PY - 2023 AN - OPUS4-57739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schilling, Richard A1 - Oehrl, A. A1 - Wischerhoff, E. A1 - Schukar, Marcus T1 - A fibre optic temperature sensor based on thermoresponsive polymer N2 - We present a temperature sensor based on a polymer exhibiting a Lower Critical Solution Temperature (LCST) in aqueous solution encapsulated in a capillary. Parameters are chosen such that the solution exhibits a cloud point in a temperature range of 30° C to 39°C. The characteristic of thermoresponsive polymers with an LCST, is that above that temperature phase separation of the polymer takes place which leads to a temperature-dependent formation of a cloudy suspension. An optical intensity measurement over the desired temperature range is established by an increase of optical attenuation inside the polymer solution caused by a rising temperature. For our purpose, the polymer capillary is connected to transmitter and receiver via a Polymer Optical Fibre (POF). Our intensity measurement is, to the best of our knowledge, a novel method and can be considered simple when compared to existing fibre-based temperature measurement techniques. Due to the lack of electrical components at the probe, this sensor is suitable for measurements in strong electromagnetic fields and environments for which flying sparks are hazardous, i.e., inflammable fluids or gases. Furthermore, all manufactured sensors share the same temperature dependence and, therefore, are well-suited for comparative measurement, e.g., flow measurement systems. With the given temperature range, a body temperature measurement is also suitable. T2 - European Workshop on Optical Fibre Sensors (EWOFS 2023) CY - Mons, Belgium DA - 23.05.2023 KW - Thermoresponsive polymer KW - Aqueous polymer solution KW - Temperature sensor KW - LCST KW - POF PY - 2023 DO - https://doi.org/https://doi.org/10.1117/12.2678418 SP - 12643-69 PB - SPIE CY - Bellingham, Wash. AN - OPUS4-57735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Sensoren und Analytik für Sicherheit und Prozesskontrolle in Wasserstofftechnologien N2 - Der Beitrag behandelt verschiedene Themen aus dem H2Safety@BAM-Kompetenzfeld Sensorik, Analytik und zertifizierte Referenzmaterialien (SensRef) mit Schwerpunkt auf Mess- und Prüfverfahren, die verschiedene Analyseverfahren, Sensortechnologien und Ultraschallwellen nutzen. Ein Teil davon ist das Euramet-Vorhaben "MefHySto" zur Metrologie der Wasserstoffspeicherung. Des Weiteren werden Verfahren zur Erkennung von freigesetztem Wasserstoff und zur Bestimmung des Wasserstoff-Luftverhältnisses mithilfe von Gassensoren behandelt. Ein weiterer Aspekt ist die zerstörungsfreie Fehlstellenerkennung mit einem integrierten Zustandsüberwachungssystem, das auf geführten Ultraschallwellen basiert und zur Überwachung der Lebensdauer von Composite-Behältern (Wasserstoffspeicher) dient. Zudem wird die Anwendung faseroptischer Sensorik zur Schadenfrüherkennung an Wasserstoffspeichern diskutiert. Dabei werden erkennbare Dehnungsänderungen an Druckbehältern als Indikatoren genutzt. T2 - DVGW-Kongress "H2 Sicherheit" CY - Online meeting DA - 15.03.2023 KW - Faseroptische Sensorik KW - Gassensorik KW - Geführte Ultraschallwellen KW - Leckdetektion KW - Metrologie zur Wasserstoffspeicherung KW - Structural Health Monitoring (SHM) KW - Zerstörungsfreie Prüfung KW - SensRef KW - H2Safety@BAM PY - 2023 AN - OPUS4-57529 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Per- und polyfluorierte Alkylsubstanzen (PFAS) während der Klärschlammverbrennung – Analytische Methoden zur Überwachung N2 - Per- and polyfluoroalkyl substances (PFAS) are a group of more than 12,000 anionic cationic, zwitterionic and neutral anthropologic substances which have been used extensively in a variety of products and industries due to their lipo- and hydrophobic properties, and inert physical and chemical stability. As a result of continuous use of fluorinated consumer products, effluents and sewage sludge from wastewater treatment plants (WWTPs) have been shown to be an important source of PFAS contamination in the environment. While environmental exposure of organic pollutants like PFAS, pesticides and pharmaceuticals have to be avoided, phosphorus from sewage sludge must be used in Germany among other things to produce high-quality P-fertilizers for a circular economy. However, the fate of legacy and emerging PFAS compounds during sewage sludge incineration or pyrolysis is for the most parts still unknown. In particular, PFAS analysis in exhaust air from industrial facilities has not yet been standardized in Germany, which means that no comparable results are available for possible regulation. T2 - Berliner Klärschlamm Konferenz CY - Berlin, Germany DA - 11.11.2024 KW - Klärschlamm KW - Per- and Polyfluoroalkyl substances (PFAS) PY - 2024 AN - OPUS4-61628 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Glas an der Bundesanstalt für Materialforschung und -prüfung N2 - Im Vortrag wird ein kurzer Überblick über die BAM und die Aktivitäten zum Werkstoff Glas gegeben. T2 - 4. Glashüttentag der Jungen DGG vom 29.09.2016 bis 30.09.2016 in Berlin CY - Berlin, Germany DA - 29.09.2016 KW - Glas PY - 2016 AN - OPUS4-38331 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - High-temperature laser profilometry N2 - Advanced methods for 3D green density characterization like computed tomography and 3D FE sinter modeling can be utilized for increasing the reliability of sintered components. The experimental in situ observation of sintering, however, is currently restricted to silhouette methods, i.e. heating microscopy. For complex shaped samples, in situ shape screening during shrinkage would allow much better validation of 3D sinter simulation models. Further, by revealing temporary sinter warpage, 3D high-temperature shape screening allows to locate potential defects of complex sintered components. Against this background, BAM developed a testing device for in situ 3D high-temperature shape screening for ceramic and glass-ceramic tapes up to 1000°C [1-3]. Current work is focused on dropping this restriction in sample shape and temperature. The poster illustrates the current state of this work and possible applications of the method e.g. in detecting sinter warpage of metallized glass-ceramic LTCC tapes. T2 - SGT Centenary Conference, & ESG 2016 CY - Sheffield, UK DA - 04. 09. 2016 KW - Laser profilometry KW - 3D High-temperature shape screening KW - Sintering PY - 2016 AN - OPUS4-38320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - Absorption and refraction techniques: Characterization and Non-Destructivetesting of materials N2 - X-ray techniques developed and used in BAM FB 8.5 (Micro NDE) for characterization of ceramic materials. T2 - Sitzung der Technischen Kommission des Verbands der Keramischen Industrie CY - Berlin, Gremany DA - 10.3.2017 KW - X-ray KW - X-ray refraction KW - Computed Tomography PY - 2017 AN - OPUS4-39322 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René A1 - Müller, Bernd R. A1 - Kupsch, Andreas T1 - Characterizing damage evolution in metal matrix composites with X-ray refraction topography and in situ tensile loading N2 - In this study a metal-matrix-composite with aluminum matrix and Al2O3 particles was investigated with x-ray refraction topography and in-situ tensile loading. It could be observed that after reaching a certain load the specific surface increased steadily. However, the classical radiographs taken for comparison show no damage in the sample. T2 - 8th Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 07.12.2016 KW - X-ray refraction KW - Metal matrix composites KW - In-situ loading KW - Synchrotron PY - 2016 AN - OPUS4-39113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Marzok, Ulrich T1 - 3D High-temperature laser profilometry during sintering N2 - Most crucial for components of complex shape or heterogeneous micro structure, precise control of sintering has decisive influence on dimensional accuracy, mechanical integrity and reliability of sintered components. In these cases, only in situ 3D high-temperature shape screening during shrinkage would allow revealing temporary sinter warpage and hereby caused potential defects. Against this background, nokra Optische Prüftechnik und Automation GmbH, HTM Reetz GmbH and BAM developed a testing device for in situ 3D shape screening for ceramic and glass-ceramic tapes up to 1000°C by means of high-temperature laser profilometry. The local repeatability of the sample-sensor distance (sample height profile) is 10 µm at 1000°C. Current work is focused on dropping these restrictions in sample shape and temperature. In a second testing device, currently being in development, samples up to 5 cm x 5 cm x 5 cm can be measured at temperatures up to 1500°C.The presentation illustrates the current state of this work and possible applications of the method. T2 - 92. DKG Jahrestagung CY - Berlin, Germany DA - 19. 03. 2017 KW - Laser profilometry KW - 3D High-temperatue shape screening KW - Sintering PY - 2017 AN - OPUS4-40449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Hermann, P. A1 - Kästner, B. A1 - Adamczyk, Burkart A1 - Hoehl, A. A1 - Ulm, G. A1 - Adam, Christian T1 - Air and chlorine gas corrosion of different silicon carbides analyzed by nano-Fourier-transform infrared (nano-FTIR) spectroscopy N2 - The present study shows the potential of high-resolution imaging and nano-Fourier-transform infrared (nano-FTIR) spectroscopy for corrosion science. The protective oxidation layers of different chlorine-gas treated silicon carbides (SiCs) were characterized with these techniques. A nitrified SiC showed the highest resistant strength against chlorine corrosion at 1000 °C compared to the other SiCs. Nano-FTIR spectroscopy with a lateral resolution below 40 nm detected differences in the crystallinity of the bulk-SiC and in the transitional region to the protective layer. Furthermore, high-resolution imaging provides deep insight in the interfacial layer between bulk-SiC and the protective oxidation layer on sub-micrometer scale. KW - Nano-Fourier-transform infrared spectroscopy KW - Scattering-type scanning near-field optical microscopy (s-SNOM) KW - Synchrotron radiation KW - Corrosion KW - Silicon carbide KW - Chlorine PY - 2018 DO - https://doi.org/10.1016/j.corsci.2017.12.002 SN - 0010-938X VL - 131 SP - 324 EP - 329 PB - Elsevier AN - OPUS4-43648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kowarik, Stefan T1 - Neuartiger faseroptischer Temperatursensor basierend auf thermoresponsiven Polymeren N2 - Wir zeigen Resultate für einen faseroptischen Temperatursensor, der auf der temperaturabhängigen Eintrübung einer wässrigen Polymerlösung beruht. Da der Sensor auf dem Phasenübergang der spinodalen Entmischung bei fester Temepratur beruht, kann sich der Sensor selbst kalibrieren und daher für Anwendungen zur absoluten Temperaturmessung eingesetzt werden. T2 - Hybrid Sensor Net CY - Karlsruhe, Germany DA - 22.11.2017 KW - LCST PY - 2017 AN - OPUS4-43310 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René T1 - Distinguishing characteristic defect in additively manufactured Ti-Al6-V4 with synchrotron X-ray refraction radiography N2 - Synchrotron X-ray refraction radiography (SXRR) is proven to identify different kinds of defects in Ti-Al6-V4 samples produces by selective laser melting. Namely, these defect types are empty pores and unprocessed powder, which are characteristic to the regions above and below the optimal laser energy density, respectively. Furthermore, SXRR detects small defects below the spatial resolution. T2 - BESSY User Meeting CY - Berlin, Germany DA - 13.12.2017 KW - Additive manufacturing KW - X-ray refraction KW - Porosity PY - 2017 AN - OPUS4-43446 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Volatile concentration and mobility measured by VHE-MS N2 - Der Vortrag schildert die Funktionsweise und einige ausgewählte Anwendungsmöglichkeieten der Vakuum-Heißextraktion an der BAM. T2 - Seminar Instrumentelle Analytik, Fakultät III Prozesswissenschaften, Lehrstuhl Keramik TU Berlin CY - TU Berlin, Germany DA - 17.2.2017 KW - Gehalt volatiler Spezies KW - Heißextraktion PY - 2017 AN - OPUS4-44212 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cabeza, Sandra A1 - Müller, Bernd R. A1 - Pereyra, R. A1 - Fernández, R. A1 - González-Doncel, G. A1 - Bruno, Giovanni T1 - Evidence of damage evolution during creep of Al–Mg alloy using synchrotron X-ray refraction N2 - In order to provide further evidence of damage mechanisms predicted by the recent solid-state transformation creep (SSTC) model, direct observation of damage accumulation during creep of Al–3.85Mg was made using synchrotron X-ray refraction. X-ray refraction techniques detect the internal specific surface (i.e. surface per unit volume) on a length scale comparable to the specimen size, but with microscopic sensitivity. A significant rise in the internal specific surface with increasing creep time was observed, providing evidence for the creation of a fine grain substructure, as predicted by the SSTC model. This substructure was also observed by scanning electron microscopy KW - Aluminium alloys KW - Creep KW - Damage KW - Synchrotron X-ray refraction KW - Electron microscopy KW - subgrain structure PY - 2018 DO - https://doi.org/10.1107/S1600576718001449 SN - 1600-5767 VL - 51 SP - 420 EP - 427 PB - Wiley AN - OPUS4-44619 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adamczyk, Burkart A1 - Formanek, P. A1 - Meyer, Christian A1 - Krüger, O. A1 - Scharf, Holger A1 - Reinsch, Stefan A1 - Ostermann, Markus A1 - Nofz, Marianne A1 - Jäger, Christian A1 - Adam, Christian A1 - Emmerling, Franziska T1 - Nanocrystalline and stacking-disordered beta-cristobalite AlPO4 chemically stabilized at room temperature: synthesis, physical characterization, and X-ray powder diffraction data N2 - This paper reports the first successful synthesis and the structural characterization of nanocrystalline and stacking-disordered β-cristobalite AlPO4 that is chemically stabilized down to room temperature and free of crystalline impurity phases. Several batches of the title compound were synthesized and thoroughly characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy, selected area electron diffraction, energy dispersive X-ray spectroscopy mapping in SEM, solid-state 31P nuclear magnetic resonance (31P-NMR) spectroscopy including the TRAPDOR method, differential thermal analysis (DTA), gas-sorption methods, optical Emission spectroscopy, X-ray fluorescence spectroscopy, and ion chromatography. Parameters that are critical for the synthesis were identified and optimized. The synthesis procedure yields reproducible results and is well documented. A high-quality XRD pattern of the title compound is presented, which was collected with monochromatic copper radiation at room temperature in a wide 2θ range of 5°–100°. KW - Stabilization of high-temperature phase at RT KW - Nanochrystalline AlPO4 KW - Beta-christobalite structure type KW - High-cristobalite form KW - Aluminium phosphate PY - 2017 DO - https://doi.org/10.1017/S0885715617000537 SN - 1945-7413 SN - 0885-7156 VL - 32 IS - S1 SP - S193 EP - S200 PB - JCPDS-ICDD CY - Cambridge AN - OPUS4-42235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabe, Torsten T1 - Prozessbegleitende Prüfung beim Sintern keramischer Schichtverbunde N2 - Die zuverlässige Herstellung von Bauteilen aus Hochleistungskeramik erfordert den Einsatz von prozessbegleitenden Prüfverfahren in allen Fertigungsstufen. Prozessbegleitende Prüfung umfasst sowohl die Bewertung von Ausgangs- und Zwischenprodukten (Pulver, Suspensionen, Grünkörper) als auch die in-situ Überwachung kritischer Fertigungsstufen (Aufbereitung, Formgebung, Entbinderung, Sinterung). Der Arbeitskreis „Prozessbegleitende Prüfverfahren“ im DKG/DGM-Gemeinschaftsausschuss „Hochleistungskeramik“ bietet eine Plattform zum Informationsaustausch über neue Messverfahren und zur Initiierung von Ringversuchen und Referenzmaterialentwicklung. Als aktuelle Beispiele werden zwei applikationsnahe Verfahren zur in-situ Charakterisierung von Geometrieveränderungen (Schwindung, Verformung) an großformatigen keramischen Schichtverbunden vorgestellt. Die Hochtemperatur-3D-Laserprofilometrie ermöglicht die Visualisierung und Quantifizierung der lokalen Verformung keramischer Multilayer während der drucklosen Sinterung. Beobachtet wurden an LTCC-Multilayern starke Verformungen bereits während der Entbinderung und in der Abkühlphase. Das Wissen um zwischenzeitliche Verformungen erweitert das Verständnis über die Ursachen von Defekten in Multilayer-Bauteilen. Die in-situ Messung der Dickenschwindung an realen, großformatigen LTCC-Bauteilen während der druckunterstützten Sinterung wurde erstmals durch die Entwicklung eines LTCC-kompatiblen Drucksinteraggregat mit integriertem Dilatometer ermöglicht. Zusätzlich wurde das Drucksinteraggregat mit einer prozessbegleitende Mess- und Regelungseinrichtung für den Sauerstoffpartialdruck ausgestattet. Durch ein optimiertes Sauerstoffpartialdruckregime konnte an LTCC-Modulen eine qualitätsgefährdende Silberdiffusion aus den Leiterbahnen in das umgebende keramische Dielektrikum drastisch reduziert werden. Das mit einem industriellen Partner entwickelte Drucksinteraggregat eröffnet unikale Möglichkeiten zur Optimierung von Aufheizgeschwindigkeit, Druck und Sinteratmosphäre in allen Phasen des Sinterprozesses. T2 - Werkstoffwoche CY - Dresden, Germany DA - 27.09.2017 KW - In situ Prüfung KW - Keramische Multilayer KW - Laserprofilometrie KW - Drucksintern PY - 2017 AN - OPUS4-42297 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Bernd R. A1 - Cooper, R.C. A1 - Lange, Axel A1 - Kupsch, Andreas A1 - Wheeler, M. A1 - Hentschel, Manfred P. A1 - Staude, Andreas A1 - Pandey, A. A1 - Shyam, A. A1 - Bruno, Giovanni T1 - Stress-induced microcrack density evolution in β-eucryptite ceramics: Experimental observations and possible route to strain hardening N2 - In order to investigate their microcracking behaviour, the microstructures of several β-eucryptite ceramics, obtained from glass precursor and cerammed to yield different grain sizes and microcrack densities, were characterized by laboratory and synchrotron x-ray refraction and tomography. Results were compared with those obtained from scanning electron microscopy (SEM). In SEM images, the characterized materials appeared fully dense but computed tomography showed the presence of pore clusters. Uniaxial tensile testing was performed on specimens while strain maps were recorded and analyzed by Digital Image Correlation (DIC). X-ray refraction techniques were applied on specimens before and after tensile testing to measure the amount of the internal specific surface (i.e., area per unit volume). X-ray refraction revealed that (a) the small grain size (SGS) material contained a large specific surface, originating from the grain boundaries and the interfaces of TiO2 precipitates; (b) the medium (MGS) and large grain size (LGS) materials possessed higher amounts of specific surface compared to SGS material due to microcracks, which decreased after tensile loading; (c) the precursor glass had negligible internal surface. The unexpected decrease in the internal surface of MGS and LGS after tensile testing is explained by the presence of compressive regions in the DIC strain maps and further by theoretical arguments. It is suggested that while some microcracks merge via propagation, more close mechanically, thereby explaining the observed X-ray refraction results. The mechanisms proposed would allow the development of a strain hardening route in ceramics. KW - Beta-eucryptite KW - Microcracked ceramics KW - X-ray refraction KW - Tensile load KW - Strain hardening KW - Synchrotron KW - BAMline KW - Computed Tomography KW - CT PY - 2018 UR - http://www.sciencedirect.com/science/article/pii/S1359645417308881 DO - https://doi.org/10.1016/j.actamat.2017.10.030 SN - 1359-6454 SN - 1873-2453 VL - 144 IS - Supplement C SP - 627 EP - 641 PB - Elsevier B.V. AN - OPUS4-43024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - Microstructure characterisation of advanced materials via 2D and 3D X-ray refraction techniques N2 - 3D imaging techniques have an enormous potential to understand the microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this conference paper we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. We demonstrate showcases of ceramics and composite materials, where microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. We present in situ analysis of the damage evolution in an Al/Al2O3 metal matrix composite during tensile load and the identification of void formation (different kinds of defects, particularly unsintered powder hidden in pores, and small inhomogeneity’s like cracks) in Ti64 parts produced by selective laser melting using synchrotron X-ray refraction radiography and tomography. T2 - THERMEC'2018 CY - Paris, France DA - 09.07.2018 KW - X-ray-refraction KW - Damage evolution KW - Additive manufacturing KW - Composites KW - Creep PY - 2018 AN - OPUS4-45572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - Microstructure characterization of materials using X-ray refraction techniques N2 - X-ray imaging techniques have an enormous potential to understand the microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this lecture we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining the internal specific surface of materials (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. We demonstrate showcases of ceramics and composite materials, where microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. We present in situ analysis of the damage evolution during tensile load and the identification of void formation in parts produced by selective laser melting. T2 - MIMENIMA Summerschool CY - TU-Bremen, Germany DA - 22.8.2018 KW - X-ray refraction KW - Cracks KW - Pores PY - 2018 AN - OPUS4-45790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Combining diffusive gradients in thin films (DGT) and spectroscopic techniques for the determination of phosphorus species in soils N2 - A wide range of methods are used to estimate the plant-availability of soil phosphorus (P). Published research has shown that the diffusive gradients in thin films (DGT) technique has a superior correlation to plant-available P in soils compared to standard chemical extraction tests. In order to identify the plant-available soil P species, we combined DGT with infrared and P K- and L-edge X-ray adsorption near-edge structure (XANES) spectroscopy. This was achieved by spectroscopically investigating the dried binding layer of DGT devices after soil deployment. All three spectroscopic methods were able to distinguish between different kinds of phosphates (poly-, trimeta-, pyro- and orthophosphate) on the DGT binding layer. However, infrared spectroscopy was most sensitive to distinguish between different types of adsorbed inorganic and organic phosphates. Additionally, also intermediates of the time-resolved hydrolysis of trimetaphosphate in soil could be analyzed. Furthermore, infrared and XANES microspectroscopy make it also possible to analyze P compounds on the binding layer with a lateral resolution down to 1 µm2. Therefore, P species of a spatial soil segment (e.g. rhizosphere) can be mapped and analyzed. T2 - Phosphorus in Soil and Plants (PSP6) CY - Leuven, Belgium DA - 10.09.2018 KW - Soil P species KW - Spectroscopy KW - DGT PY - 2018 AN - OPUS4-45961 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Thoralf T1 - KorroPad - New Test Method for the Investigation of the Passive Layer Stability of Stainless Steels N2 - The KorroPad is a gel-based indicator test designed for the electrochemical determination of the passive layer stability and localization of surfaces of stainless steels threatened by localized corrosion. Different investigations and studies on the performance of the KorroPad as well as field trials by industrial users the have proven the principal suitability of the KorroPad method to assess the passive layer stability of stainless steels. The electrochemical mode of action will be described in detail and also the limitations of the applicability will be demonstrated. The influence of different surface finishes has been investigated and verified by known methods for describing corrosion resistances. As a result, the increased corrosion susceptibility of two ground surfaces has been detected, but also the corrosion resistance of further surface finishes could be confirmed. Furthermore the KorroPad test was used for the investigation of the influence of time and humidity on the passive layer development on different stainless steels. T2 - EuroCorr 2018 CY - Krakow, Poland DA - 09.09.2018 KW - Corrosion KW - KorroPad KW - Stainless Steel KW - Passivity KW - Surface finish PY - 2018 AN - OPUS4-46022 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Drexel, R. T1 - Nano-sized Polypropylene as a Promising Candidate Reference Material: Preparation, Characterization and Stability in Complex Matrices N2 - The lack of nanoplastic (NPs) reference materials capable of mimicking real-world scenarios is currently hampering the development of validated extraction techniques from complex matrices (e.g. soils, sediments, biota), the development of analytical approaches for robust identification and quantification, and the ability to use environmentally relevant test materials in (eco)toxicity testing and hazard assessment [1]. The large body of available data suggests that larger microplastics (MPs) in the natural environment are irregular shaped, partially degraded (chemically and physically), a continuum of sizes, shapes and densities, represent a wide range of polymer types, and acts as a reservoir for thousands of plastic chemicals. Although NPs have been described as being neither MPs nor engineered nanoparticles [2], and while direct measurement data of true NP in the environment remain elusive, they are expected to be as equally diverse as MPs [3]. Here, we present a strategy towards the development of a potential NP reference material based on nano-sized polyproplyene particles (nanoPP) developed within the EURAMET-funded PlasticTrace project (https://plastictrace.eu/). The strategy includes the preparation, the physicochemical characterization and the stability assessment of nanoPP in suspension both in its pristine state, but also when spiked into food (mineral water and milk) and environmental matrices (suspended particulate matter collected from the river Elbe ). Collected experimental data suggests nanoPP to be a promising candidate for a NP reference material. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Nanoplastics KW - Reference materials PY - 2025 AN - OPUS4-63382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Drago, C A1 - Wiesner, Yosri A1 - Braun, U A1 - Giovannozi, A A1 - Fadda, M A1 - Putzu, Mara A1 - Lorenzo, S A1 - Moscoso-Pérez, C A1 - Benismail, N A1 - Palma, C A1 - Almeida, J A1 - Mattarozzi, M A1 - Barbaresi, M A1 - Piergiovanni, M A1 - Masino, M A1 - Bianchi, F A1 - Careri, M A1 - v Bavel, B A1 - Maltseva, A A1 - Sillanpää, M A1 - Pröfrock, D A1 - Wippermann, D A1 - Altmann, Korinna T1 - Harmonisation of sample preparation for microplastic analysis: Recovery rates of tablets containing microplastics as reference material for food and environmental matrix N2 - Microplastic are found ubiquitarians in the environment and food products. Up to now, their impact of risks on health and environment is still controversially discussed, but based on the precautionary principle alone, their presence should be monitored and emission should be reduced (see here also the status of existing EU regulations ). The crucial point is not only the reduction of microplastics pollution but also the introduction of legally binding, standardized procedures for their analysis. The limited availability of certified reference material as well as absence of standard operating procedures to identify, characterize and quantify microplastics according to number and mass have generated lack of comparability between different analytical methods and laboratories; but also, the need of time-consuming development of own protocols for each laboratory. Further on, harmonisation and standardisation of microplastics analysis requires specific reference materials that are used to validate the measurement and to ensure the comparability of results. In the first step, we developed tablets of a water-soluble matrix, containing defined numbers of microplastic particles or mass contents. These can be solved in water and can be handled as reference materials in bottled drinking water without additional sample preparation. These samples can be measured, using mass-based methods as thermo-analytical methods like thermal desorption-gas chromatography-mass spectrometry (TED-GC/MS) or pyrolysis–gas chromatography–mass spectrometry (Py-GC/MS) and using umber-based methods as vibrational spectroscopy like Infrared and Raman directly after filtration. The aim of this work was to delevop standard operating procedure to measure microplastics in more complex matrices and to harmonise and compare different detection and characterization methods. In fact, these matrices require different additional treatments to allow a reliable quantification and identification of microplastics. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Nanoplastics PY - 2025 AN - OPUS4-63366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fernández-González, V. T1 - Innovations in Microplastic Measurement: A Pyrolysis Approach for a Polyethylene Terephthalate Reference Material N2 - In the framework of the PlasticTrace project, in which a reference material for PET microplastics will be proposed, a method using pyrolysis and gas chromatography coupled with mass spectrometry detection (Py-GC-MS) is developed to quantify the mass of PET microplastics (10-100 µm) in tablets at two different concentration levels. The overall aim of this project is to develop international metrological capacity that enables the traceable measurement and characterization of SMPs and NPs in environmental and food samples and the production of suitable reference materials, according to the metrological requirements (https://plastictrace.eu/). The proposed method consists of dissolving the tablet containing the PET microplastics in milli-Q water and filtering the solution using a glass microfiber membrane 13 mm filter size, 1.6 µm pore size. After filtering and several washes to ensure complete dissolution of the tablet and recovery of all PET microplastics, the filter is removed, folded, and placed in a capsule of the pyrolyzer for direct Py-GC/MS analysis. Two main markers were selected for PET quantification: vinyl benzoate and benzoic acid, with consistent concentrations found for both at high PET concentrations (≈400 µg) (24% RSD, n=17), but interferences with the matrix and vinyl benzoate were found at low concentrations (≈17 µg PET), with only benzoic acid being valid as a marker in this case (22% RSD, n=10). As an alternative to the quantification of PET microplastics in tablets at low concentrations, derivatization is proposed, for which tetramethylammonium hydroxide solution (TMAH) is added directly into the pyrolysis cap. The PET marker in this case is dimethyl terephthalate, with which good results have also been found (19.6% RSD, n=10 ). The proposed method is robust, simple, with high automation and very little sample handling and treatment, and allows the analysis of PET microplastics (>10 µm) in tablets with excellent accuracy and precision even at very low concentrations. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Nanoplastics KW - GC/MS PY - 2025 AN - OPUS4-63383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Booth, A. T1 - Production of a 1-10 μm polypropylene reference material for development of analytical methods N2 - The poster is about the preparation of microplastics in the size range of 1-10 µm. These size range of particles can be inhalded and therefore be toxic for humans. The preparation is done by comminution of PP pellets and sieving. Characterisation occured for size with laser diffraction, for type with FTIR and for shape with SEM. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Reference materials PY - 2025 AN - OPUS4-63367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Putzu, Mara T1 - Optimization of production process for microplastics reference materials N2 - Microplastics (MP) are defined as plastic particles mainly consisting of polymers in the size range of 1 to 1000 µm. They can be found in a wide range of environmental matrices but also in food products, indicating a potential risk on humans and environment. Plastic debris in the environment or food chain are extremely complex in terms of size, concentration, polymer type, levels of physiochemical degradation and undefined morphologies which makes their isolation and detection in complex matrices challenging. Analytical detection methods and techniques to identify and quantify microplastics in environmental and food matrices are numerous but validated and standardized methods are currently lacking. To close this research gap, reference materials (RMs) and representative sample preparation approaches are urgently needed. Homogeneity and stability are two crucial characteristics for the certification process of the reference materials. For this purpose, we aim to present ways to prepare reference materials containing very low masses of close-to reality plastic particles with broad size distribution (10-100 µm) that are homogeneously distributed in tablet-to-tablet variation and stable over time. Our work is based on the ISO Guide 30:2015 and ISO Guide 35:2017 to fulfil the criteria set in future standards ISO/DIS 16094-2 and ISO/DIS 16094-3. The property of interest will be the mass detected by thermogravimetric analysis (TGA). Furthermore, informative values will be achieved by mass-based technique TED-GC/MS and spectroscopic microscopy techniques, such as µ-FTIR spectroscopy and µ-Raman. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Reference materials KW - TED-GC/MS PY - 2025 AN - OPUS4-63386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittmar, Stefan A1 - Weyrauch, Steffen A1 - Reemtsma, Thorsten A1 - Eisentraut, Paul A1 - Altmann, Korinna A1 - Ruhl, Aki S. A1 - Jekel, Martin T1 - Settling Velocities of Tire and Road Wear Particles: Analyzing Finely Graded Density Fractions of Samples from a Road Simulator and a Highway Tunnel N2 - The terminal settling velocity is considered the most critical parameter determining the transport of tire and road wear particles (TRWP) in aquatic environments. Nonetheless, no respective empirical data has been reported so far. In this study, particle samples from a road simulator and a highway tunnel were investigated with a validated imaging method. Different density and size fractions of both samples were measured separately, acquiring sizes and settling velocities of more than 30,000 individual particles. In addition, tire marker polymers were analyzed for each fraction via thermal extraction desorption-gas chromatography/mass spectrometry. Finally, the acquired particle data was combined according to the fractions’ estimated tire contents in order to deduce detailed probability distributions of particle size and settling velocity for the actual TRWP from both samples. Weighted by TRWP-incorporated tire mass, median diameters of 54 and 44 μm as well as median settling velocities of 0.65 and 0.22 mm/s were found for TRWP from the road simulator and highway tunnel, respectively. This study thus provides the first ever empirical data on TRWP settling velocities in water, which can be highly valuable input for modeling the environmental transport of TRWP and for dimensioning TRWP retention systems. KW - Microplastics KW - TED-GC/MS KW - Sinking velocities KW - Transport PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635449 DO - https://doi.org/10.1021/acs.est.5c04165 SN - 0013-936X VL - 59 IS - 26 SP - 13434 EP - 13446 PB - American Chemical Society (ACS) AN - OPUS4-63544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rossi, A T1 - Lactose Tablets as Suitable Microplastics Reference Material to Support Validation Studies and Quality Control N2 - One of the main challenges in validating microplastics detection methods is the lack of suitable reference materials that accurately reflect the properties of interest. To bridge this gap, the EU-funded PlasticTrace project has developed water-soluble tablets containing precisely defined amounts of polyethylene terephthalate (PET) particles. Each tablet includes a specific mass (0.2, 18.5, or 400 µg) and particle count (151 or 1764, measured via Raman spectroscopy). Production follows a rigorous solid-phase dilution process, ensuring high reproducibility and quality control. The PET particles used in these tablets have an average size of approximately 40 µm, with a range between 10 and 200 µm, and an irregular, stone-like shape. All measurements align with ISO/TC 147/SC 2 standardization efforts and adhere to ISO/DIS 16094-2 and ISO/DIS 16094-3. To assess tablet homogeneity, the most widely accepted microplastics detection techniques, i.e. µ-FTIR, µ-Raman, Py-GC/MS, and TED-GC/MS, were applied. Different batches were produced, each containing varying particle numbers and masses, reaching the detection limits of the methods used. The results demonstrated excellent consistency between tablets, successfully passing homogeneity tests. Furthermore, no significant changes were observed in the tablets' composition or stability after six months of storage. This innovative reference material represents an important advancement in microplastics analysis, supporting laboratories in meeting EU Commission requirements for the monitoring of microplastics in drinking water and wastewater with greater accuracy and reliability. The production process can be transferred for other plastic particles is this size range. T2 - BERM 16 CY - Halifax, Canada DA - 01.06.2025 KW - Microplastics KW - TED-GC/MS KW - Reference materials KW - Raman microscopy PY - 2025 AN - OPUS4-63403 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Visileanu, Emilia A1 - Altmann, Korinna A1 - Stepa, Raluca A1 - Haiducu, Maria A1 - Miclea, Paul Tiberiu A1 - Vladu, Alina A1 - Dondea, Felicia A1 - Grosu, Marian Catalin A1 - Scarlat, Razvan T1 - Comparative Analysis of Airborne Particle Concentrations in Textile Industry Environments Throughout the Workday N2 - This paper addresses the growing concern surrounding microplastic pollution, particularly within the textile industry, and the associated potential health risks linked to the inhalation and ingestion of microplastic particles. Microplastics, defined as plastic particles smaller than five millimeters, are increasingly found not only in aquatic environments, but also in soils, air, and food. Although research on the health impacts of microplastics is still emerging, early studies indicate that these particles could contribute to health issues, including oxidative stress, inflammation, and cardiovascular diseases. Notably, individuals with higher concentrations of plastics in arterial plaques are more susceptible to heart attacks and strokes. In the textile industry, synthetic fibers such as polyester, nylon, and acrylic release microplastics into the air during production. The paper discusses a study conducted in a textile company that processes polyester yarns, where airborne microplastic concentrations were measured at various locations throughout the day. Particle sizes ranging from 0.3 nm to 10 nm were analyzed, revealing the presence of polyester polymers in the particulate matter. These findings underscore the widespread nature of microplastic pollution, particularly in industrial settings, and raise concerns about the health risks associated with prolonged exposure to airborne microplastics. While further research is necessary to fully understand the extent of these health impacts, preliminary data suggest a troubling link between microplastic inhalation and cardiovascular conditions. KW - Microplastics KW - Textiles KW - Airborne particles PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635269 DO - https://doi.org/10.3390/microplastics4020034 SN - 2673-8929 VL - 4 IS - 2 SP - 1 EP - 17 PB - MDPI AG AN - OPUS4-63526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miclea, P-T T1 - Evaluation of Toxicological Characteristics of Airborne Nano/Microplastic Particles From the Industrial Environment N2 - Micro and nano plastic (MNPs) particles and fibres represent a global scale contamination source with hazard potential. They can be identified all around our environment, even in air, soil and water. One of the major global MNPs polluters is the textile industry, which generates plastic particles (nylon, polyester, polyurethane, polyolefin, acrylic etc.) during the manufacturing processes. The study analyses the level of particle concentration outside a company that processes textile yarns, but also from the proximity of workplaces using an online air samplers with cascade and mono filter holders for silicon (Si) and quartz filters, respectively. A laser detector was used for real- time counting of particles of six size classes (PM0.3-PM10). Silicon (Si) filters with a diameter of 9 mm and pore sizes of 10 µm and 1 µm and quartz filters with a diameter of 25 mm and a pore size of 1.2 µm were used for particle sampling. A special holder was designed and made for selective sampling (PM10 and PM1.0) on Si filters. Quartz filters were pre-calcined (8000C) before collection. Sampling parameters: airflow (GilAir Plus pump) -2 l/m3, collection time -3 hours; starting time 7.00 am (T1)/2.00 pm (T2), intermittent natural ventilation, average temperature and humidity: 23.3 0C, RH: 52.5%. The weight of particles collected (µg) on the quart filters was 4.9E-05 (T1) and 5.1E-05 (T2) and on the Si filters 3,2 E-05(T1) and 5E-06(T2). The total number of the outside particles (PM0,3-PM10) was situated between 3584,58 (T1)-15165,05(T2) and inside 9901(T1) and 12921,61(T2). The highest number of PM 10 particles inside was 72/m3 and of PM0.3 particles 71979/m3. The samples were characterized using electron microscopy and µRaman spectroscopy. All samples showed a high concentration of particles on the filter. Samples show only particles with irregular shapes. The equivalent particle diameter was for PM10: 1-5 µm and PM1<1 µm. The total Ion Chromatogram shows the presence of PET-type polymer and the TED GS-MS analysis shows that the weight of the collected particles is PET. After extracting the particles from the quartz filters, they were tested for evaluation of the cytotoxic potential of preparations on human monocyte-macrophage cell cultures and peripheral lymphocytes. In the first case, the level of cytotoxicity was at the border between non-cytotoxic and cytotoxic and in the second test the result was moderate cytotoxic. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - TED-GC/MS KW - Nanoplastics KW - Raman microscopy PY - 2025 AN - OPUS4-63378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miclea, P.-T. T1 - Novel laser pre-structured silicon filters for microplastics analysis N2 - This research presents a novel laser-assisted approach to silicon filter fabrication, offering an effective alternative to traditional photolithographic processes. By integrating selective femtosecond laser irradiation with photoelectrochemical etching, we achieved precisely controlled pore geometries, overcoming common challenges in filter production for microplastic and nanoscale filtration suitable for microplastic number and mass analysis. T2 - SETAC Europe 2025 CY - Vienna, Austria DA - 11.05.2025 KW - Microplastics KW - Nanoplastics KW - Raman microspectroscopy PY - 2025 AN - OPUS4-63384 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fadda, Marta A1 - Sacco, Alessio A1 - Altmann, Korinna A1 - Ciornii, Dmitri A1 - Milczewski, Frank A1 - Bañares, Miguel A. A1 - Portela, Raquel A1 - Giovannozzi, Andrea Mario A1 - Rossi, Andrea Mario T1 - Tracking nanoplastics in drinking water: a new frontier with the combination of dielectrophoresis and Raman spectroscopy N2 - Detection of micro- (MPs) and nanoplastics (NPs) in food and environmental matrices has been gaining relevance due to their potential toxicological effects on human health. While MPs have been detected in a wide range of complex matrices, suitable methods for the characterization and chemical identification of NPs are still lacking, primarily due to significant methodological challenges associated with their nano-specific physiochemical properties, including size distribution (1 nm – 1 µm), dynamic surface chemical changes, and carbon-based composition, which complicate their detection compared to engineered nanomaterials. To overcome the traditional limitations of spectroscopic techniques in terms of spatial resolution and sensitivity at the sub-micrometer level, a novel label-free methodology is presented for specifically identifying the chemical composition of NPs directly in suspension by combining Raman spectroscopy with dielectrophoresis (DEP). Using a custom-built device, small volumes of NPs are injected into a dielectrophoretic cell and locally trapped by DEP forces to fill the Raman confocal volume, facilitating their detection and identification, and providing high signal-to-noise ratio Raman spectra for more reliable analysis. This approach was successfully applied to both Milli-Q water and a commercial brand of drinking water, enabling the rapid identification of various types of NPs with different sizes and polymer compositions at concentrations as low as 20 µg/mL. These included certified reference polystyrene beads ranging from 800 to 60 nm in diameter, as well as polydisperse NPs, more representative of real samples in terms of size distribution and polymer type, such as polyethylene (450 nm), polypropylene (180 nm), and polyethylene terephthalate (100 nm). Moreover, the chemical fingerprint of each NPs was thoroughly investigated and compared with the corresponding bulk polymers, highlighting possible changes in the Raman bands due to surface oxidation or nanometer-scale effect. Therefore, this innovative method can be considered a valuable approach for addressing gaps in the detection and identification of NPs, as well as for monitoring their dynamic phisiochemical changes in real matrices. KW - Nanoplastics KW - Water contaminants KW - Raman microspectroscopy KW - Dielectrophoresis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-633658 DO - https://doi.org/10.1186/s43591-025-00131-y SN - 2662-4966 VL - 5 IS - 1 SP - 1 EP - 11 PB - Springer Science and Business Media LLC AN - OPUS4-63365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Kupsch, Andreas T1 - Refraction driven X-ray caustics at curved interfaces N2 - X-ray refraction related interaction has received rising interest since about two decades in the field of imaging, beam shaping and analysis although being discovered a century ago. Due to refraction at interfaces in inhomogeneous media X-rays undergo natural focusing (or defocusing) of waves, revealing caustics. Such Kind of intensity patterns are well-known for visible light, but have been sparsely discussed for X-rays. The Variation of irradiation density may be predicted in case of known shapes. Analogously to light optics, the intensity distributions cover several orders of magnitude including complete extinction. The partly convergent (and divergent) caustic stripes originate from narrow zones of typical size of some 10−6 of the boundary curvature radius. For the deflection of plane wave synchrotron radiation (energy in the range of some keV to some ten keV) at rods and tubes of several μm diameter, we find good Agreement between experiments and modeling by ray tracing according to Snell’s law without additional diffraction contributions. Apart from Basic Research implications, caustics may influence the performance of irradiation technologies such as sterilization or molecular cross-linking. KW - X-ray caustics KW - X-ray refraction KW - Irradiation KW - Radiation shielding KW - Synchrotron Radiation PY - 2019 UR - http://www.sciencedirect.com/science/article/pii/S0168900218314591 DO - https://doi.org/10.1016/j.nima.2018.10.152 SN - 0168-9002 SN - 1872-9576 VL - 916 SP - 275 EP - 282 PB - Elsevier AN - OPUS4-46924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Effect of Nitrification Inhibitor on Nitrogen Forms in Soil analyzed by Nitrogen K edge micro XANES Spectroscopy N2 - Specific co-fertilization of nutrients can enhance their plant-availability and thus the yield of plants. To investigate this effect, we performed a pot experiment with three different P-fertilizers and ammonium nitrate sulfate as a co-fertilizer, without and with a nitrification inhibitor (NI), and analyzed the form of nitrogen (N) in the soil via novel X-ray spectroscopic method. The application of NI with the N fertilizer led to a higher dry matter yield of maize. Novel N K-edge micro-X-ray absorption near-edge structure (micro-XANES) spectroscopy identified that the application of a NI promotes the temporary formation of a non-exchangeable N in detectable hot-spots in the soil. The subsequent slow release and prolonged availability of N during plant growth leads to higher yield. It can be concluded that NIs lead to a temporary fixation of ammonium-N in a pool that can be accessed by plant roots. Those types of available nutrient pools meet the idea of so-called “next generation fertilizers” as plants have access to nutrients according to their current demand. T2 - Workshop for X-ray and neutron imaging applications in soil sciences CY - Lund, Sweden DA - 17.06.2019 KW - Nitrogen KW - Phosphorus recycling KW - Fertilizer KW - XANES spectroscopy KW - Pot experiment PY - 2019 AN - OPUS4-48237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Specification of bioavailable nutrients and pollutants in the environment by combining DGT and spectroscopic techniques N2 - Previous research shows that analytical methods based on Diffusive Gradients in Thin films (DGT) provide very good correlations to the amount of bioavailable nutrients and pollutants in the environmental samples. However, these DGT results do not identify which compound of the specific element has the high bioavailability. Using various spectroscopic techniques (infrared, XANES and NMR spectroscopy) to analyze the dried DGT binding layers after deployment could allow us to determine the specific elements or compounds. Nutrients such as phosphorus and nitrogen are often, together with other elements, present as molecules in the environment. These ions are detectable and distinguishable by infrared and NMR spectroscopy, respectively. In addition, XANES spectroscopy allows for the specification of nutrients and pollutants (e.g. chromium) on the DGT binding layer. Furthermore, microspectroscopic techniques make it also possible to analyze compounds on the DGT binding layer with a lateral resolution down to 5 µm2. Therefore, species of elements and compounds of e.g. a spatial soil segment can be mapped and analyzed, providing valuable insight to understand the dynamics of nutrients and pollutants in the environment. Here we will present the advantages and limitations of this novel combination of techniques. T2 - 6th Conference on Diffusive Gradients in Thin Films CY - Vienna, Austria DA - 17.09.2019 KW - Soil P species KW - DGT KW - Infrared spectroscopy PY - 2019 AN - OPUS4-49057 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liens, A. A1 - Reveron, H. A1 - Douillard, T. A1 - Blanchard, N. A1 - Lughi, V. A1 - Sergo, V. A1 - Laquai, René A1 - Müller, Bernd R. A1 - Bruno, Giovanni A1 - Schomer, S. A1 - Fürderer, T. A1 - Adolfsson, E. A1 - Courtois, N. A1 - Swain, M. A1 - Chevalier, J. T1 - Phase transformation induces plasticity with negligible damage in ceria-stabilized zirconia-based ceramics N2 - Ceramics and their composites are in general brittle materials because they are predominantly made up of ionic and covalent bonds that avoid dislocation motion at room temperature. However, a remarkable ductile behavior has been observed on newly developed 11 mol.% ceria-stabilized zirconia (11Ce-TZP) composite containing fine alumina (8 vol.% Al2O3) and elongated strontium hexa-aluminate (8 vol.% SrAl12O19) grains. The as-synthesized composite also has shown full resistance to Low Temperature Degradation (LTD), relatively high strength and exceptionally high Weibull modulus, allowing its use in a broader range of biomedical applications. In this study, to deepen the understanding of plastic deformation in Ce-TZP based composites that could soon be used for manufacturing dental implants, different mechanical tests were applied on the material, followed by complete microstructural characterization. Distinct from pure Ce-TZP material or other zirconia-based ceramics developed in the past, the material here studied can be permanently strained without affecting the Young modulus, indicating that the ductile response of tested samples cannot be associated to damage occurrence. This ductility is related to the stress-induced tetragonal to monoclinic (t-m) zirconia phase transformation, analogue to Transformation-Induced Plasticity (TRIP) steels, where retained austenite is transformed to martensite. The aim of this study is to corroborate if the observed plasticity can be associated exclusively to the zirconia t-m phase transformation, or also to microcraking induced by the transformation. The t-m transformed-zones produced after bending and biaxial tests were examined by X-ray refraction and SEM/TEM coupled with Raman. The results revealed that the observed elastic-plastic behavior occurs without extensive microcracking, confirming a purely elastic-plastic behavior driven by the phase transformation (absence of damage). KW - Zirconia KW - Ceria KW - Ceramic matrix composite KW - Plasticity KW - Phase transformation KW - X-Ray Refraction PY - 2020 UR - http://www.sciencedirect.com/science/article/pii/S1359645419307177 DO - https://doi.org/10.1016/j.actamat.2019.10.046 SN - 1359-6454 VL - 183 SP - 261 EP - 273 PB - Elsevier Ltd. AN - OPUS4-49740 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas T1 - Materialcharakterisierung mittels bildgebender Röntgenstreuverfahren N2 - Die herkömmliche Bildgebung mit Röntgenstrahlung beruht auf unterschiedlicher Absorption durch verschiedene Materialien im Volumen eines Körpers. Es entsteht ein "Massebild". Die hier vorgestellten Verfahren benutzen die Brechung und Beugung von Röntgenstrahlen, um innere Oberflächen oder die Molekulartextur von Materialien und Bauteilen abzubilden. Im Vortrag werden die entsprechenden Messtechniken an der BAM im Labormaßstab sowie an Großforschungseinrichtungen vorgestellt und anhand einiger Anwendungsbeispiele die zusätzlichen Informationen zur herkömmlichen Durchstrahlung diskutiert. T2 - 243. Sitzung DGZfP-Arbeitskreis Thüringen CY - Ilmenau, Germany DA - 11.04.2019 KW - Röntgenrefraktion KW - Röntgenbeugung KW - Diffraction Enhanced Imaging KW - Keramik KW - Polyethylen KW - Metall-Matrix-Komposit PY - 2019 AN - OPUS4-49859 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Paz, B. A1 - Meyer, H.-P. A1 - Varychev, A. A1 - Rosner, M. A1 - Vogl, Jochen A1 - Behrendt, S. ED - Treister, M. ED - Yablonsky, L. T1 - Археометрические исследования стеклянных сосудов из погребений ранних кочевников Южного Приуралья T1 - Archäometrische Untersuchungen an achaimenidischen Glasgefäßen aus den Gräbern der frühen Nomaden des südlichen Urals N2 - Die untersuchten Gläser lassen sich in drei Gruppen einteilen. Die beiden Fragmente aus der Nekropole von Pjatimary deuten auf eine frühe Herstellungszeit hin und lassen sich mit eisenzeitlichen Fragmenten iranischer Herkunft vergleichen. Die Glasfunde aus der Nekropole Filippovka bestehen aus völlig unterschiedlichen Glasmaterialien und müssen einer späteren Herstellungszeit zugeordnet werden. Sowohl die unterschiedlichen Rezepturen als auch der definitive Hinweis auf verschiedene Rohstoffquellen zur Herstellung der untersuchten Gläser, lassen ein breitgefächertes Netz von weitreichenden Handelsbeziehungen erkennen. KW - Archäometrie KW - Isotopenverhältnisse Strontium und Blei KW - Elementanalyse KW - Massenspektrometrie KW - Herkunft PY - 2012 SN - 978-5-903011-85-8 VL - 1 SP - 262 EP - 267 PB - TAUS CY - Moskau AN - OPUS4-26899 LA - rus AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Larissa A1 - Jakubowski, Norbert A1 - Hösl, Simone A1 - Scheler, C. A1 - Roos, P.H. A1 - Linscheid, M.W. T1 - Comparison of different chelates for lanthanide labeling of antibodies and application in a Western blot immunoassay combined with detection by laser ablation (LA-)ICP-MS N2 - We have developed lanthanide labeling strategies for antibodies to adapt conventional biochemical workflows like Western blot immunoassays for detection by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) analysis with a special interest to apply the multi-element capabilities of ICP-MS for the design of multiplexed immunoassays. In this paper the lanthanide labeling of antibodies with MeCAT was investigated and the reaction conditions were optimized for application in a Western blot immunoassay analyzed by LA-ICP-MS. Furthermore, the MeCAT labeling strategy was compared with two other commercially available labeling reagents, MAXPAR™ and SCN-DOTA. As a proof-of-principle experiment chemically induced alterations of cytochrome P450 protein expression were investigated and the suitability of the differentially labeled antibodies for Western blot immunoassays of a complex liver microsomal protein fraction was tested. Limits of detection (LODs) in the lower fmol range were reached in the Western blot application using MeCAT and MAXPAR™ as element labeling reagents, whereas even sub-fmol LODs can be achieved in a dot blot experiment for the pure antibodies. PY - 2012 DO - https://doi.org/10.1039/c2ja30068k SN - 0267-9477 SN - 1364-5544 N1 - Geburtsname von Müller, Larissa: Wäntig, L. - Birth name of Müller, Larissa: Wäntig, L. N1 - Geburtsname von Hösl, Simone: Hardt, S. - Birth name of Hösl, Simone: Hardt, S. VL - 27 IS - 8 SP - 1311 EP - 1320 PB - Royal Society of Chemistry CY - London AN - OPUS4-26256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rienitz, O. A1 - Schiel, D. A1 - Görlitz, V. A1 - Jährling, R. A1 - Vogl, Jochen A1 - Lara-Manzano, J.V. A1 - Zon, A. A1 - Fung, W.-H. A1 - Buzoianu, M. A1 - De Sena, R.C. A1 - Dos Reis, L.A. A1 - Valiente, L. A1 - Yim, Y.-H. A1 - Hill, S. A1 - Champion, R. A1 - Fisicaro, P. A1 - Bing, W. A1 - Turk, G.C. A1 - Winchester, M. R. A1 - Saxby, D. A1 - Merrick, J. A1 - Hioki, A. A1 - Miura, T. A1 - Suzuki, T. A1 - Linsky, M. A1 - Barzev, A. A1 - Máriássy, M. A1 - Cankur, O. A1 - Ari, B. A1 - Tunc, M. A1 - Konopelko, L.A. A1 - Kustikov, Y.A. A1 - Bezruchko, M. T1 - Final report on CCQM-K87: Mono-elemental calibration solutions N2 - The aim of this comparison was to demonstrate the capability of national metrology institutes to measure elemental mass fractions at a level of w(E) ≈ 1 g/kg as found in almost all mono-elemental calibration solutions. These calibration solutions represent an important link in traceability systems in inorganic analysis. Virtually all traceable routine measurements are linked to the SI through these calibration solutions. Every participant was provided with three solutions of each of the three selected elements chromium, cobalt and lead. This comparison was a joint activity of the Inorganic Analysis Working Group (IAWG) and the Electrochemical Analysis Working Group (EAWG) of the CCQM and was piloted by the Physikalisch-Technische Bundesanstalt (PTB, Braunschweig, Germany) with the help of the Bundesanstalt für Materialforschung und -prüfung (BAM, Berlin, Germany), the Centro Nacional de Metrología (CENAM, Querétaro, Mexico) and the National Institute of Standards and Technology (NIST, Gaithersburg, USA). A small majority of participants applied inductively coupled plasma optical emission spectrometry (ICP OES) in combination with a variety of calibration strategies (one-point-calibration, bracketing, calibration curve, each with and without an internal standard). But also IDMS techniques were carried out on quadrupole, high resolution and multicollector ICP-MS machines as well as a TIMS machine. Several participants applied titrimetry. FAAS as well as ICP-MS combined with non-IDMS calibration strategies were used by at least one participant. The key comparison reference values (KCRV) were agreed upon during the IAWG/EAWG meeting in November 2011 held in Sydney as the added element content calculated from the gravimetric sample preparation. Accordingly the degrees of equivalence were calculated. Despite the large variety of methods applied no superior method could be identified. The relative deviation of the median of the participants' results from the gravimetric reference value was equal or smaller than 0.1% (with an average of 0.05%) in the case of all three elements. KW - CCQM KW - Metrology KW - IDMS PY - 2012 DO - https://doi.org/10.1088/0026-1394/49/1A/08010 SN - 0026-1394 SN - 1681-7575 VL - 49 IS - 08010, 1A (Technical Supplement 2012) SP - 1 EP - 104 PB - Inst. of Physics Publ. CY - Bristol AN - OPUS4-30458 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Rosner, Martin T1 - Production and certification of a unique set of isotope and delta reference materials for Boron isotope determination in geochemical, environmental and industrial materials N2 - Isotopic reference materials are essential to enable reliable and comparable isotope data. In the case of boron only a very limited number of such materials is available, thus preventing adequate quality control of measurement results and validation of analytical procedures. To address this situation a unique set of two boron isotope reference materials (ERM-AE102a and -AE104a) and three offset δ11B reference materials (ERM-AE120, -AE121 and -AE122) were produced and certified. The present article describes the production and certification procedure in detail. The isotopic composition of all the materials was adjusted by mixing boron parent solutions enriched in 10B or 11B with a boron parent solution having a natural isotopic composition under full gravimetric control. All parent solutions were analysed for their boron concentration as well as their boron isotopic composition by thermal ionisation mass spectrometry (TIMS) using isotope dilution as the calibration technique. For all five reference materials the isotopic composition obtained on the basis of the gravimetric data agreed very well with the isotopic composition obtained from different TIMS techniques. Stability and homogeneity studies that were performed showed no significant influence on the isotopic composition or on the related uncertainties. The three reference materials ERM-AE120, ERM-AE121 and ERM-AE122 are the first reference materials with natural δ11B values not equal to 0‰. The certified δ11B values are -20.2‰ for ERM-AE120, 19.9‰ for ERM-AE121 and 39.7‰ for ERM-AE122, each with an expanded uncertainty (k = 2) of 0.6‰. These materials were produced to cover about three-quarters of the known natural boron isotope variation. The 10B enriched isotope reference materials ERM-AE102a and ERM-AE104a were produced for industrial applications utilising 10B for neutron shielding purposes. The certified 10B isotope abundances are 0.29995 for ERM-AE102a and 0.31488 for ERM-AE104a with expanded uncertainties (k = 2) of 0.00027 and 0.00028, respectively. Together with the formerly certified ERM-AE101 and ERM-AE103 a unique set of four isotope reference materials and three offset δ11B reference materials for boron isotope determination are now available from European Reference Materials. KW - Boron isotope variations KW - Delta-scale KW - Stable isotopes KW - Isotope reference materials KW - Delta reference materials KW - Metrology in chemistry KW - Absolute isotope abundance PY - 2012 DO - https://doi.org/10.1111/j.1751-908X.2011.00136.x SN - 1639-4488 SN - 1751-908X VL - 36 IS - 2 SP - 161 EP - 175 PB - Blackwell CY - Oxford AN - OPUS4-26260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völling, E. A1 - Reifarth, N. A1 - Vogl, Jochen ED - Nosch, M.-L. ED - Laffineur, R. T1 - The intercultural context of treasure A in Troy - Jewellery and textiles N2 - At the end of May 1873, Heinrich Schliemann recovered Treasure A in Troy. He brought all the metal artifacts illegally to Athens and published his iscoveries one year later. Then he bequeathed the Trojan finds to Berlin where from 1881 onwards, Treasure A was exhibited in the Museum of Arts and Crafts (later Gropius Bau). Hubert. Schmidt inventoried and catalogued the Trojan remains in 1902 without the so-called “Dubletten” (duplicates). The transfer of the Treasure trove in 1945 to former Leningrad (St. Petersburg) and Moscow is well known, but there was a partial restoration of the looted art from the former Soviet Union back to the former GDR: eight out of eleven silver vessels of Treasure A came via Leipzig in 1979 finally back to Berlin’s Museum für Vor- und Frühgeschichte, Stiftung Preussischer Kulturbesitz in 1994. During its safe keeping in Leningrad and Leipzig, these silver jars remained ignored in the boxes in which they were transported, a Situation, which today permits them to be investigated almost in their condition of discovery. The study of the Originals allowed Information to be gleaned about their manufacture and offered opportunities for various analyses. After the gold jewellery came to light, technical data and an archaeological appraisal of the Trojan gold kept in the Pushkin Museum of Fine Arts in Moscow could be published in 1996. The considerable quantity of the outstanding gold artifacts of Treasure A was deposited inside the great silver vessel Sch 5873 and listed by Heinrich Schliemann. T2 - 13th International Aegean Conference CY - Copenhagen, Denmark DA - 21.04.2010 PY - 2012 SN - 978-90-429-2665-3 SP - 531 EP - 538 PB - Peeters Publishers CY - Liège, Belgium AN - OPUS4-26408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen T1 - Measurement uncertainty in single, double and triple isotope dilution mass spectrometry N2 - Triple IDMS has been applied for the first time to the quantification of element concentrations. It has been compared with single and double IDMS obtained on the same sample set in order to evaluate the advantages and disadvantages of triple IDMS over single and double IDMS as an analytical reference procedure. The measurement results of single, double and triple IDMS are indistinguishable, considering rounding due to the individual measurement uncertainties. As expected, the relative expanded uncertainties (k = 2) achieved with double IDMS (0.08 %) are dramatically smaller than those obtained with single IDMS (1.4 %). Triple IDMS yields the smallest relative expanded uncertainties (k = 2, 0.077 %) unfortunately at the expense of a much higher workload. Nevertheless triple IDMS has the huge advantage that the isotope ratio of the spike does not need to be determined. Elements with high memory effects, highly enriched spikes or highest metrological requirements may be typical applications for triple IDMS. KW - Single IDMS KW - Double IDMS KW - Triple IDMS KW - Measurement uncertainty KW - Cd mass fraction PY - 2012 DO - https://doi.org/10.1002/rcm.5306 SN - 0951-4198 SN - 1097-0231 VL - 26 IS - 3 SP - 275 EP - 281 PB - Wiley CY - Chichester AN - OPUS4-25292 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völz, Uwe A1 - Boehm, Rainer A1 - Heckel, Thomas A1 - Spruch, W. ED - Pombo, J. T1 - Ultrasonic testing of hollow axles with a conical rotation scanner phased array probe N2 - This paper describes the investigations, carried out during the ongoing European Project WOLAXIM. It presents the development of the non-destructive testing system for hollow axle inspection. The phased array probe is designed, the inspection parameters are determined and the required test equipment is planned according to the specifications. As a part of the probe design, a detailed model to calculate the sound field of the conical phased array is developed. With this model the optimal geometric parameters for bore diameters from 30mm up to 70mm are determined. The first design of a conical probe with forty-eight elements is realised. Based on this design a mock-up with ten elements is produced. The first practical tests with the calculated delay laws show high sensitivity for small test flaws and offer good agreement with the modelling results. The effectiveness as well as the sensitivity with a good signal to noise ratio is verified. The parameters for a short inspection time less than five minutes per axle are determined. A raw scanning with 1.5° circumferential and 2mm axial resolution is feasible within two minutes. That is significantly faster than comparable mechanically rotated probe systems. The remaining three minutes are sufficient for the other steps in the inspection process. The required features will be fulfilled by the COMPAS® phased array device. The feasibility of the ultrasonic system is shown. The specification and the theoretical probe design are complete and sufficient knowledge is present that the system will be viable. The results of the modelling and first practical tests show a good agreement with the objectives. The determined probe parameters satisfy the requirements. T2 - 1st International Conference on Railway Technology: Research, Development and Maintenance CY - Las Palmas de Gran Canaria, Spain DA - 18.04.2012 KW - Ultrasonic testing KW - Phased array KW - Rotation scanner KW - Hollow axle KW - Sleeve shaft KW - WOLAXIM PY - 2012 SN - 978-1-905088-52-2 DO - https://doi.org/10.4203/ccp.98.86 SN - 1759-3433 N1 - Serientitel: Civil-Comp Proceedings – Series title: Civil-Comp Proceedings VL - 98 SP - 1 EP - 10 PB - Civil Comp Press AN - OPUS4-26275 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Malpass-Evans, R. A1 - McKeown, N. A1 - Tyagi, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Low frequency vibrations and diffusion in disordered polymers bearing an intrinsic microporosity as revealed by neutron scattering N2 - The microscopic diffusion and the low frequency density of states (VDOS) of PIM-EATB(CH3) are investigated by inelastic and quasi-elastic neutron scattering where also the demethylated counterpart of PIM-EA-TB(H2) is considered. These intrinsic microporous polymers are characterized by large BET surface area values of several hundred m2/g and pore sizes between 0.5 and 2 nm. Detailed comparison is made to the archetype of polymers of intrinsic microporosity, PIM-1, and polynorbornenes also bearing a microporosity. Due to the wavelength of neutrons, the diffusion and vibrations can be addressed on microscopic length and time scales. From the inelastic neutron scattering experiments the low frequency density of states (VDOS) is estimated which shows excess contributions to the Debye-type VDOS known as Boson peak. It was found that the maximum frequency of the Boson peak decreases with increasing microporosity characterized by the BET surface area. However, besides the BET surface area, additional factors such as the backbone stiffness govern the maximum frequency of the Boson peak. Further the mean squared displacement related to microscopic motions was estimated from elastic fixed window scans. At temperatures above 175 K, the mean squared displacement PIM-EA-TB(CH3) is higher than that for the demethylated counterpart PIM-EA-TB(H2). The additional contribution found for PIM-EATB(CH3) is ascribed to the rotation of the methyl group in this polymer because the only difference between the two structures is that PIM-EA-TB(CH3) has methyl groups where PIM-EA-TB(H2) has none. A detailed comparison of the molecular dynamics is also made to that of PIM-1 and the microporous polynorbornene PTCNSi1. The manuscript focuses on the importance of vibrations and the localized molecular mobility characterized by the microscopic diffusion on the gas Transport in polymeric separation membranes. In the frame of the random gate model localized fluctuations can open or close bottlenecks between pores to enable the diffusion of gas molecules. KW - Polymer of intrisic microporosity KW - Neutron scattering KW - Boson peak KW - Methyl group rotation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538490 DO - https://doi.org/10.3390/cryst11121482 VL - 11 IS - 12 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-53849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fünning, Tabea A1 - Peczek, Anna A1 - Kroh, Aleksandra A1 - Mai, Christian A1 - Paul, Martin A1 - Thomsen, Florian A1 - Tannenberg, Robert A1 - Schumann, Christoph A1 - Weller, Michael G. A1 - Mai, Andreas A1 - Steglich, Patrick C. ED - Lieberman, Robert A. ED - Baldini, Francesco ED - Homola, Jiri T1 - Optimization of local backside released micro-ring resonators for sensing applications using silicon photonic integrated circuits in a SOI technology N2 - Photonic micro-ring resonators (MRR) are widely studied for their high sensitivity across applications like environmental monitoring, healthcare, and chemical analysis. Their evanescent field sensing requires partially unembedded waveguides compatible with CMOS processing. Our approach uses local backside etching with an additional buried oxide (BOX) etch to release waveguides while preserving the back-end of line (BEOL) structure, enabling spatial separation of the sensing area and electronics. The BOX etch critically affects sensor performance, as waveguide surface roughness can alter MRR properties and coupling. We analyzed MRR design variations, comparing wet and dry etching techniques for their effects on optical performance across rib and strip waveguides in quasi-TE and quasi-TM modes. Wafer-level measurements show that backside-released MRR achieve high extinction ratios with slightly reduced quality factors, advancing high-sensitivity photonic sensors. T2 - SPIE Optics + Optoelectronics 2025 CY - Prague, Czech Republic DA - 23.05.2025 KW - Photonic sensors KW - Micro-ring resonator (MRR) KW - Silicon on insulator (SOI) KW - CMOS KW - Local backside etching PY - 2025 SN - 978-1-5106-8851-3 DO - https://doi.org/10.1117/12.3056481 VL - 13527 SP - 1 EP - 8 PB - SPIE CY - Bellingham, WA , USA AN - OPUS4-63585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tannenberg, Robert A1 - Paul, Martin A1 - Fünning, Tabea A1 - Schuhmann, Christoph A1 - Weller, Michael G. A1 - Steglich, Patrick T1 - Multichannel real-time detection of biomarkers with highly miniaturized photonic microchips N2 - The development of novel photonic integrated microchips (PIC) is a promising approach to allow for the convenient detection of key biomarkers in complex matrices through multichannel real-time analysis in a highly compact package. This study reports the successful development and application of a backside released CMOS chip designed for the multichannel real-time detection of biomarkers. Operating at the C-band at approx. 1550 nm, the microchip features three dedicated detection sensors in addition to a reference sensor, enabling simultaneous analysis of multiple biomarkers. The compact and highly miniaturized design of this microchip, with a footprint of just 1 mm², positions it as promising candidate for point-of-care diagnostics and personalized medicine applications. This technology opens a path to transform biomarker detection across various medical fields, offering rapid, reliable, and cost-effective diagnostic solutions. In conclusion, the presented multichannel photonic microchips signify a substantial leap forward in real-time biomarker detection, providing a highly capable platform for future research and clinical applications. T2 - SPIE Optics + Optoelectronics 2025 CY - Prague, Czech Republic DA - 07.04.2025 KW - Photonic integrated circuit KW - Ring resonator KW - Real-time detection KW - Multiplexing KW - Semiconductor KW - CMOS KW - C-reactive protein KW - CRP KW - Biomarker PY - 2025 SN - 978-1-5106-8850-6 DO - https://doi.org/10.1117/12.3056453 VL - 13527 SP - 1 EP - 6 PB - SPIE CY - Prague, Czech Republic AN - OPUS4-63478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Konnertz, Nora A1 - Ding, Yi A1 - Harrison, W.J. A1 - Budd, P.M. A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Molecular mobility and gas transport properties of nanocomposites based on PIM-1 and polyhedral oligomeric phenethyl-silsesquioxanes (POSS) N2 - Polymers with intrinsic microporosity (PIMs) are of great interest in the field of gas separation membranes. Already the first synthesized PIM-1 shows extraordinary permeability and selectivity. Unfortunately, PIM-1 is susceptible to physical aging and thus gradually loses its outstanding properties. In this study a polyhedral oligomeric silsesquioxane with phenethyl substituents (PhenethylPOSS) was used as a nanofiller (0–40 wt%) in the PIM-1 matrix to potentially improve the gas transport properties and prevent physical aging. The molecular mobility of the solution-cast nanocomposite films was analyzed by Broadband Dielectric Spectroscopy (BDS). Furthermore, gas permeability was determined with the time lag method (0–20 bar upstream pressure) at 35 °C for N2, O2, CH4 and CO2. KW - Broadband Dielectric Spectroscopy KW - Gas separation KW - Gas permeation KW - Polymers of intrinsic microporosity KW - Nanocomposite KW - POSS KW - PIM-1 PY - 2017 DO - https://doi.org/10.1016/j.memsci.2017.02.007 SN - 0376-7388 SN - 1873-3123 VL - 529 SP - 274 EP - 285 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-39169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yin, Huajie A1 - Chapala, P. A1 - Bermeshev, M. A1 - Pauw, Brian Richard A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Influence of Trimethylsilyl Side Groups on the Molecular Mobility and Charge Transport in Highly Permeable Glassy Polynorbornenes N2 - Superglassy polymers with a large fractional free volume have emerged as novel materials with a broad range of applications, especially in the field of membrane separations. Highly permeable addition-type substituted polynorbornenes with high thermal resistance and chemical stability are among the most promising materials. The major obstacle for extending the practical membrane application is their strong tendency to physical aging, leading to a partial decline in their superior transport performance over time. In the present study, broadband dielectric spectroscopy with complementary X-ray scattering techniques were employed to reveal changes in microporous structure, molecular mobility, and conductivity by systematic comparison of two polynorbornenes with different numbers of trimethylsilyl side groups. Their response upon heating (aging) was compared in terms of structure, dynamics, and charge transport behavior. Furthermore, a detailed analysis of the observed Maxwell−Wagner−Sillars polarization at internal interfaces provides unique information about the microporous structure in the solid films. The knowledge obtained from the experiments will guide and unlock potential in synthesizing addition-type polynorbornenes with versatile properties. KW - Dielectric spectroscopy KW - Molecular mobility KW - Electrical conductivity KW - Gas separation membranes PY - 2019 DO - https://doi.org/10.1021/acsapm.9b00092 SN - 2637-6105 VL - 1 IS - 4 SP - 844 EP - 855 PB - ACS CY - Washington DC AN - OPUS4-47838 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Kittner, Maria A1 - Altmann, Korinna A1 - Hamann, Sven A1 - Weyer, Rüdiger A1 - Kalbe, Ute T1 - Bewertung der Freisetzung von Mikroplastik aus Sportböden auf Kunststoffbasis - Abschlussbericht N2 - Die Europäische Kommission hat 2023 ein Verbot zum bewussten Austrag von Mikroplastik (MP) in die Umwelt beschlossen, das auch für die Verwendung von synthetischen Gummi-Granulaten (v. a. EPDM) in Sportböden gilt. In Deutschland gibt es laut DFB ca. 5100 Kunstrasenplätze. In der EU beläuft sich die Anzahl laut ECHA auf 13,000 Kunstrasen- und 47,000 Bolzplätze, Tendenz steigend. Das Hauptziel des Projektes war es daher, eine Massenbilanz für die Freisetzung von MP zu erstellen, um so eine Schätzung des MP-Austrags pro Kunstrasenplatz und Jahr zu ermöglichen. Dafür werden die MP-Emissionen von drei Kunstrasenszenarien in verschiedenen Zuständen (ungealtert, künstlich gealtert und in Echtzeit gealtert) verglichen: die Vergangenheit (Kunstrasen: fossilbasiert, EPDM-Füllung), die Gegenwart (der in Europa am häufigsten installierte Rasen) und die Zukunft (Rasen mit recycelten Grasfasern, keine synthetische Füllung sondern z.B. Quarzsand oder Korkschrott). Dazu werden fabrikneue Kunststoffrasen und EPDM-Granulat unter Laborbedingungen beschleunigt gealtert, um die Freiland-Beanspruchung eines Kunststoffrasens in circa 15 Jahren abzubilden. Die Verwendung spezieller Mikrofiltertiegel in Lysimeter-Experimenten ermöglicht die Abschätzung der Partikelgrößen des emittierten MP, was eine Grundbedingung für die Bewertung einer potenziellen Gesundheitsgefährdung für Menschen ist. Ergänzend wurden weitere umweltrelevante Schadstoffausträge aus den Kunststoffrasen quantifiziert. KW - Mikroplastik KW - Kunststoffrasen KW - Schadstoffe KW - Bewitterung KW - Lysimeter PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-633114 DO - https://doi.org/10.26272/opus4-63311 N1 - Das Projekt wurde gefördert vom Bundesinstitut für Bau-, Stadt- und Raumforschung (BBSR) im Auftrag des Bundesministeriums für Wohnen, Stadtentwicklung und Bauwesen (BMWSB) aus Mitteln des Innovationsprogramms Zukunft Bau. Aktenzeichen: FKZ 10.08.18.7-22.02. Projektlaufzeit: 09.2022 bis 03.2025. SP - 1 EP - 75 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-63311 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalbe, Ute A1 - Piechotta, Christian A1 - Bandow, Nicole T1 - Comparing PFAS analysis in batch leaching and column leaching tests N2 - Laboratory leaching tests are tools to assess the mobility of environmental contaminants released from granular materials. Comparative leaching tests were performed using four PFAS-contaminated soils whose concentration patterns of 10 selected perfluoroalkyl and polyfluoroalkyl substances (PFAS) differed due to the two types of contamination sources. This study aimed to evaluate the equivalence of two usual laboratory-scale leaching test procedures, batch and column percolation tests, at liquid-to-solid ratios (L/S) of 2 l/kg, which is the current practice within the German assessment framework, and 10 l/kg (relevant for some EU regulations such as the landfill directive). The differences between the replicates of leaching tests investigating PFAS were smaller for column percolation tests than for batch tests, probably mainly due to the greater sample size and the better representativeness of the sample portion analyzed. It was observed that batch tests overestimate the release of shorter-chain PFAS, whereby the effect was greater with carboxylic than with sulfonic acids. Currently, the limits of detection of analyses given by the DIN standard with regard to PFCA and PFSA in soils are partly not sufficient to detect very low contents, whereas the detection of selected PFCA and PFSA in eluates is more sensitive, in accordance with the available standards. This results in limitations when calculating mass balances. KW - PFAS KW - Leaching KW - Column percolation test KW - Batch test KW - Soil PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-618187 DO - https://doi.org/10.1007/s11356-024-35510-0 SN - 1614-7499 VL - 31 IS - 57 SP - 65233 EP - 65251 PB - Springer Science and Business Media LLC AN - OPUS4-61818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Algernon, Daniel A1 - Wiggenhauser, Herbert T1 - Impact echo data analysis based on Hilbert-Huang transform N2 - Impact echo is an acoustic method based on the use of transient stress waves generated by an elastic impact; it is used for nondestructive testing of concrete structures. In practical applications, the signals obtained often are superimposed by further mechanical vibrations and the so-called geometry effects, which are caused mainly by surface waves. Because of attenuation in the concrete as well as the divergence of the acoustical waves, impact echo signals are transient. As a result, the frequency content changes over time. Normally the analysis is carried out on the Fourier power spectrum of the signal. However, the Fourier spectrum is still affected by the mentioned effects and has well-known deficiencies for short transient signals within longer time sweeps. Application of the Hilbert-Huang transform is presented as a refined method for the time-frequency analysis of nonstationary impact echo data. The basic properties of the method and its practical application for time-frequency analysis of impact echo data, signal filtering, and pattern identification are presented. KW - Impact echo KW - Hilbert-Huang transformation PY - 2007 DO - https://doi.org/10.3141/2028-16 SN - 0361-1981 VL - 2028 IS - 1 SP - 146 EP - 153 PB - Sage Publishing CY - Thousand Oaks, CA AN - OPUS4-20790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Pauw, Brian Richard A1 - Laskina, Sofya A1 - Naik, Aakash A1 - Smales, Glen Jacob A1 - George, Janine A1 - Breßler, Ingo A1 - Benner, Philipp T1 - "Ultima Ratio": Simulating wide-range X-ray scattering and diffraction N2 - We demonstrate a strategy for simulating wide-range X-ray scattering patterns, which spans the small- and wide scattering angles as well as the scattering angles typically used for Pair Distribution Function (PDF) analysis. Such simulated patterns can be used to test holistic analysis models, and, since the diffraction intensity is on the same scale as the scattering intensity, may offer a novel pathway for determining the degree of crystallinity. The "Ultima Ratio" strategy is demonstrated on a 64-nm Metal Organic Framework (MOF) particle, calculated from Q < 0.01 1/nm up to Q < 150 1/nm, with a resolution of 0.16 Angstrom. The computations exploit a modified 3D Fast Fourier Transform (3D-FFT), whose modifications enable the transformations of matrices at least up to 8000^3 voxels in size. Multiple of these modified 3D-FFTs are combined to improve the low-Q behaviour. The resulting curve is compared to a wide-range scattering pattern measured on a polydisperse MOF powder. While computationally intensive, the approach is expected to be useful for simulating scattering from a wide range of realistic, complex structures, from (poly-)crystalline particles to hierarchical, multicomponent structures such as viruses and catalysts. KW - X-ray KW - Simulation KW - 3D Fourier Transform KW - High resolution KW - XRD KW - SAXS KW - PDF KW - Total scattering KW - X-ray scattering KW - Metal organic framework KW - Electron density map KW - FFT PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572067 DO - https://doi.org/10.48550/arXiv.2303.13435 VL - Cornell University SP - 1 EP - 12 PB - Ithaca, NY AN - OPUS4-57206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - VIDEO A1 - Pauw, Brian Richard T1 - "Ultima Ratio": Multi-scale, high-resolution 3D-FFT scattering pattern simulations N2 - This talk highlights a proof-of-concept that demonstrates the ability to calculate high-resolution Fourier transforms. These can be combined with multi-scale modeling to simulate scattering over a wide range, from small-angle scattering to XRD and PDF. The preprint documenting this is available on the ArXiv here: https://doi.org/10.48550/arXiv.2303.13435 The Jupyter notebook, VASP calculation details and MOUSE measured scattering patterns are available from this Zenodo repository: https://dx.doi.org/10.5281/zenodo.7764045 T2 - Shapespyer/MuSSIC Launch Workshop CY - Didcot, UK DA - 20.02.2023 KW - Video KW - Simulation KW - High-resolution KW - Fourier Transform KW - 3D FFT KW - Nanomaterial KW - Metal organic framework KW - MOF KW - SAXS KW - XRD KW - PDF KW - X-ray diffraction KW - Pair distribution function KW - Small-angle X-ray scattering PY - 2023 UR - https://www.youtube.com/watch?v=lEApkOqR5e8 DO - https://doi.org/10.26272/opus4-57212 PB - YouTube, LLC CY - San Bruno, CA, USA AN - OPUS4-57212 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Data-Driven Spectrochemical Methods for Elemental and Isotopic Analysis N2 - High-resolution optical spectrometers generate spectra containing tens of thousands of data points per sample. Picometre-scale isotope shifts, matrix-induced line broadening, and strong inter-feature correlations render classical peak fitting unreliable. Current analytical challenges, therefore, require rigorous algorithms able to expose latent structure, quantify uncertainty, and remain chemically interpretable. The research program presented in this lecture integrates state-of-the-art spectrochemical instrumentation with mathematically disciplined data models. Principal Component Analysis and Partial Least Squares provide chemically meaningful latent variables, while gradient-boosted decision trees or deep neural networks (ANNDL) capture residual non-linearity without sacrificing traceability. All models are trained on isotope-enriched or synthetically generated spectra and distributed with full validation workflows. T2 - Chemisches Institutskolloquium, Humboldt-Universität zu Berlin CY - Berlin, Germany DA - 21.05.2025 KW - Spectrochemistry KW - Isotopes KW - Machine learning KW - Battery KW - Data fusion PY - 2025 AN - OPUS4-63488 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Olaf A1 - Poelke, Birte A1 - Klein, Luise A1 - Rohloff, Alexander A1 - Hoffmann, Holger T1 - Initial VOC Emissions from Consumer Products Determined in Micro-Scale Test Chambers: Results of a Round Robin Test N2 - Emissions of volatile organic compounds (VOCs) from consumer products may have a negative impact on indoor air quality, potentially also affecting human wellbeing. Since consumers may be exposed to these VOCs immediately after e.g. unwrapping of newly purchased products, reliable analytical methods are needed to determine air concentration profiles in the early phase of VOC emissions. Concerning typical sample sizes of consumer products, micro-scale test chambers (μ-chambers) were considered suitable for this purpose. In addition, compared to medium- or large-scale test chambers, μ-chambers require lower initial investment and operational costs, and offer options for emissions screenings where higher sample throughput is essential. For these reasons, a μ-chamber-based method to determine initial concentrations of VOCs emitting within the first hours of simulated product use was developed. The chamber air was frequently sampled on desorption tubes loaded with Tenax® TA, followed by quantification of emitted VOCs via thermal desorption gas chromatography mass spectrometry (TD-GC-MS). The method was assessed in a round robin test involving eight participating laboratories from 2 countries. Pieces of a rain poncho (sample area A: 2.01·10-4 m2) emitting cyclohexanone, phenol, 2-ethylhexanol, naphthalene and isophorone in significant concentrations were distributed as sample material. Each laboratory conducted triplicate emission tests over a period of 48 h in μ-chambers with volumes of 44 or 114 mL. The loading factors L of 4.57 m2·m-3 (44 mL) or 1.76 m2·m-3 (114 mL) and air flow rates of 24 mL·min-1 resulted in area-specific air flow rates q of 7.17 m3·m-2·h-1 in both chamber types. The temperature was set to 23°C and, if possible, relative humidity was set to approx. 50%. The chamber air was sampled after 0.5, 1, 2, 4, 24 and 48 hours. In addition, to assess the analytical performance, each participating laboratory received two analyte-spiked Tenax® TA-loaded desorption tubes for quality control (QC). Very low relative standard deviations (11–17%) were obtained for the QC test. The results of the emissions tests in the early phase (0.5–4 h) were also adequate, with acceptable z scores (|z|≤2.00) received by six to seven participating laboratories. All eight laboratories obtained acceptable z scores after the longer sampling periods (24 and 48 h). Hence, the inter-laboratory comparability of the results obtained with the developed μ-chamber method was successfully confirmed. T2 - Healthy Buildings Europe 2025 CY - Reykjavik, Iceland DA - 08.06.2025 KW - VOC Emissions KW - Consumer Product KW - Test Chamber KW - Round Robin Test PY - 2025 AN - OPUS4-63706 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Chemometric analysis of High resolution spectra for precise and accurate isotope amount ratio determination N2 - Magnesium is a major element in the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg. It is due to their relatively large mass difference (~8% between) that isotope fractionation leads to slight variations of isotope amount ratios in biological, environmental and geological samples. Traditionally, isotope amount ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation. Recently, an optical spectrometric method has been proposed as faster and low-cost alternative for the analysis of isotope ratios: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). For the determination of Mg isotope ratios in selected rock reference materials, the high-resolution molecular absorption spectrum of in-situ generated MgF molecule was studied applying multivariate analysis and the results compared with MC-ICP-MS. Samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix. The absorption spectra were recorded for MgF for the electronic transition X 2Σ → B 2Σ+. The MgF spectrum is described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS). A PLS model was built and calibrated with enriched isotope spikes and certified reference materials. Spectra data was preprocessed by a derivate of second order and venetian blinds cross-validation was employed for finding the optimum latent variables. Finally, the model was refined by a genetic algorithm which identified the best subset of variables for a precise and accurate regression. Results are compatible with those obtained by MC-ICP-MS with an accuracy of ± 0.3‰ with uncertainties ranging between 0.02 to 0.6‰. T2 - Colloquium Analytische Atomspektroskopie CANAS 2019 CY - Freiberg, Germany DA - 23.09.2019 KW - Isotope analysis KW - Chemometric KW - Multivariate analysis KW - HR-CS-MAS KW - Molecular spectrum KW - Magnesium PY - 2019 AN - OPUS4-49878 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Khanipour, Peyman T1 - Real time mass spectrometry - From Unravelling Electrochemical Reaction Mechanism to Trace Analysis of Impurities in Hydrogen Gas N2 - Climate change and related energy policies, exacerbated by unforeseen geopolitical developments, pose new challenges for gas analytics, such as the use of hydrogen, hydrogen-containing alternative gaseous fuels (NH3, etc.), the use of alternative methane-based energy gases (LNG, LPG, etc.) or decarbonisation via CCSU. In all topics, the quality, i.e. the actual chemical composition of the gases, naturally plays a decisive role. BAM is meeting this strategic importance with the further development of hydrogen analytics and is continuing to develop the methods used in order to support the German economy and research landscape with traceability, reference materials and analytical procedures as quickly as possible. Mass spectrometry plays an important role for trace analysis in hydrogen matrix. The presentation shows first experimental results from the application of PTR-TOF-MS (Proton Transfer Reaction Time-of-Flight Mass Spectrometry). T2 - 11th International GAS Analysis Symosium & Exhibition CY - Paris, France DA - 17.05.2022 KW - Gas Analysis KW - Hydrogen KW - Metrology KW - Mass Spectrometry KW - Trace Analysis PY - 2022 AN - OPUS4-56589 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Lithium isotope fractionation as a diagnostic tool for aging lithium-ion batteries N2 - Lithium-ion batteries (LIBs) are central to modern energy storage technologies, powering applications from portable electronics to electric vehicles and grid storage systems. Their popularity comes from their high energy density, efficiency, and extended cycle life. However, over time, various aging mechanisms lead to capacity loss, increased internal resistance, and, ultimately, battery failure. Understanding and predicting these aging processes is crucial for enhancing the reliability and longevity of LIBs. This necessity makes the development of advanced diagnostic tools essential. This study uses plasma-based spectrometry techniques to explore lithium isotope fractionation (LIF) as a predictive tool for monitoring LIB aging and degradation. Mass spectrometric techniques —including MC-ICP-MS, LA-ICP-MS, and MICAP-MS— were employed to analyze lithium isotopic composition in both new and aged lithium cobalt oxide (LCO) cells, including lab-made coin cells and commercial batteries. An isotopic fractionation was identified during electrochemical cycling: 6Li migrates towards the anode, while 7Li accumulates in the cathode. These isotopic patterns correlate with structural degradation, including solid electrolyte interphase (SEI) growth and crack formation, as confirmed by FIB-SEM, XANES, and EXAFS analyses. This correlation demonstrates that LIF aligns with key aging mechanisms in model coin cells and commercial batteries, such as capacity fade and impedance growth. LIF provides a powerful diagnostic tool for battery health monitoring and aging prediction by linking isotopic fractionation to structural degradation. This approach offers significant potential to extend battery lifespan and improve the reliability of energy storage systems. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Isotope KW - Lithium KW - Battery aging KW - Degradation KW - Fractionation KW - Battery PY - 2025 AN - OPUS4-63487 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael A1 - Soruco Aloisio, Ricardo A1 - Meyer, Klas A1 - Klaus, Christian T1 - Auf dem Weg zu einer digitalen Qualitätsinfrastruktur - Eine Labor-Testplattform für die Integration von Sensoren und Messgeräten N2 - Um die internationale Spitzenposition deutscher Unternehmen der Prozessindustrie auch in Zukunft sicher zu stellen, müssen die Unternehmen ihre Prozesse und Geschäftsabläufe digitalisieren und gemeinsam mit der Forschung innovative neue Methoden, Apparate, Anlagen, Sensoren und Automatisierungstechnik sowie Datenkonzepte entwickeln. All dies erfordert den Aufbau neuer Fähigkeiten, Investition in Talente, interdisziplinäre Kommunikation zwischen verschiedenen Personen und Abteilungen und eine Bereitschaft zur Veränderung. KW - QI-Digital KW - Wasserstofftankstelle KW - IT-OT-Testplattform KW - Prozessindustrie PY - 2023 VL - 67 IS - 9 SP - 20 EP - 23 PB - Wiley-VCH CY - Weinheim AN - OPUS4-58461 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fricke, F. A1 - Brandalero, M. A1 - Liehr, Sascha A1 - Kern, Simon A1 - Meyer, Klas A1 - Kowarik, Stefan A1 - Hierzegger, R. A1 - Westerdick, S. A1 - Maiwald, Michael A1 - Hübner, M. T1 - Artificial Intelligence for Mass Spectrometry and Nuclear Magnetic Resonance Spectroscopy Using a Novel Data Augmentation Method N2 - Mass Spectrometry (MS) and Nuclear Magnetic Resonance Spectroscopy (NMR) are valuable analytical and quality control methods for most industrial chemical processes as they provide information on the concentrations of individual compounds and by-products. These processes are traditionally carried out manually and by a specialist, which takes a substantial amount of time and prevents their utilization for real-time closed-loop process control. This paper presents recent advances from two projects that use Artificial Neural Networks (ANNs) to address the challenges of automation and performance-efficient realizations of MS and NMR. In the first part, a complete toolchain has been realized to develop simulated spectra and train ANNs to identify compounds in MS. In the second part, a limited number of experimental NMR spectra have been augmented by simulated spectra, to train an ANN with better prediction performance and speed than state-of-the-art analysis. These results suggest that, in the context of the digital transformation of the process industry, we are now on the threshold of a strongly simplified use of MS and MRS and the accompanying data evaluation by machine-supported procedures, and can utilize both methods much wider for reaction and process monitoring or quality control. KW - Industry 4.0 KW - Cyber-Physical Systems KW - Artificial Neural Networks KW - Mass Spectrometry KW - Nuclear Magnetic Resonance Spectroscopy KW - Modular Production PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-539412 UR - https://ieeexplore.ieee.org/stamp/stamp.jsp?tp=&arnumber=9638378 DO - https://doi.org/10.1109/TETC.2021.3131371 SN - 2168-6750 VL - 10 IS - 1 SP - 87 EP - 98 PB - IEEE AN - OPUS4-53941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Dariz, P. T1 - Raman Microspectroscopic Imaging of Binder Remnants in Historical Mortars Reveals Processing Conditions N2 - Binder remnants in historical mortars represent a record of the connection between the raw materials that enter the kiln, the process parameters, and the end product of the calcination. Raman microspectroscopy combines high structural sensitivity with micrometre to sub-micrometre spatial resolution and compatibility with conventional thin-sectional samples in an almost unique fashion, making it an interesting complementary extension of the existing methodological arsenal for mortar analysis. Raman spectra are vibrational fingerprints of crystalline and amorphous compounds, and contain marker bands that are specific for minerals and their polymorphic forms. Relative intensities of bands that are related to the same crystalline species change according to crystal orientations, and band shifts can be caused by the incorporation of foreign ions into crystal lattices, as well as stoichiometric changes within solid solution series. Finally, variations in crystallinity affect band widths. These effects are demonstrated based on the analysis of three historical mortar samples: micrometric distribution maps of phases and polymorphs, crystal orientations, and compositional variations of solid solution series of unreacted clinker grains in the Portland cement mortars of two 19th century castings, and the crystallinities of thermal anhydrite clusters in a high-fired medieval gypsum mortar as a measure for the applied burning temperature were successfully acquired. KW - Cement clinker remnants KW - High-fired gypsum KW - Thermal anhydrite KW - Spectroscopic imaging KW - Raman microscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515038 DO - https://doi.org/10.3390/heritage2020102 VL - 2 IS - 2 SP - 1662 EP - 1683 PB - MDPI CY - Basel AN - OPUS4-51503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Villajos Collado, José Antonio T1 - Experimental volumetric hydrogen uptake determination at 77 K of commercially available metal-organic framework materials N2 - Storage is still limiting the implementation of hydrogen as an energy carrier to integrate the intermittent operation of renewable energy sources. Among different solutions to the currently used compressed or liquified hydrogen systems, physical adsorption at cryogenic temperature in porous materials is an attractive alternative due to its fast and reversible operation and the resulting reduction in storage pressure. The feasibility of cryoadsorption for hydrogen storage depends mainly on the performance of the used materials for the specific application, where metal-organic frameworks or MOFs are remarkable candidates. In this work, gravimetric and volumetric hydrogen uptakes at 77 K and up to 100 bar of commercially available MOFs were measured since these materials are made from relatively cheap and accessible building blocks. These materials also show relatively high porous properties and are currently near to large-scale production. The measuring device was calibrated at different room temperatures to calculate an average correction factor and standard deviation so that the correction deviation is included in the measurement error for better comparability with different measurements. The influence of measurement conditions was also studied, concluding that the available adsorbing area of material and the occupied volume of the sample are the most critical factors for a reproducible measurement, apart from the samples’ preparation before measurement. Finally, the actual volumetric storage density of the used powders was calculated by directly measuring their volume in the analysis cell, comparing that value with the maximum volumetric uptake considering the measured density of crystals. From this selection of commercial MOFs, the materials HKUST-1, PCN-250(Fe), MOF-177, and MOF-5 show true potential to fulfill a volumetric requirement of 40 g·L−1 on a material basis for hydrogen storage systems without further packing of the powders. KW - Hydrogen adsorption KW - Commercial metal-organic frameworks KW - Hydrogen uptake reproducibility KW - Volumetric uptake KW - Packing density PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542215 DO - https://doi.org/10.3390/c8010005 SN - 2311-5629 VL - 8 IS - 1 SP - 1 EP - 14 PB - MDPI CY - Basel AN - OPUS4-54221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bornemann-Pfeiffer, Martin A1 - Kern, Simon A1 - Maiwald, Michael A1 - Meyer, Klas T1 - Calibration-Free Chemical Process and Quality Control Units as Enablers for Modular Production N2 - Modular chemical production is a tangible translation of the digital transformation of the process industry for specialty chemicals. In particular, it enables the speeding-up of process development and thus a quicker time to market by flexibly connecting and orchestrating standardised physical modules and bringing them to life (i.e., parameterising them) with digitally accumulated process knowledge. We focus on the specific challenges of chemical process and quality control, which in its current form is not well suited for modular production and provide possible approaches and examples of the change towards direct analytical methods, analytical model transfer or machine-supported processes. KW - Modular Production KW - Chemical Process Control KW - Process Analytical Technology KW - Digital Transformation KW - Industry 4.0 PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517264 DO - https://doi.org/10.1002/cite.202000150 SN - 1522-2640 VL - 93 IS - 1-2 SP - 62 EP - 70 PB - Wiley-VCH CY - Weinheim AN - OPUS4-51726 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Dariz, P. T1 - Editorial for the special issue "Modern Raman spectroscopy of minerals" N2 - Raman spectroscopy provides vibrational fingerprints of chemical compounds enabling their unambiguous identification. The assignment of Raman spectra to minerals is straightforward, if appropriate reference data is accessible. Modern couplings of Raman spectroscopy with microscopy (Raman microspectroscopy) merge the high structural specificity with down to sub-micrometre spatial resolution. This analytical tool has high potential not only in the identification of minerals from natural sources but also for studying the complex microstructure and mineral distribution of both ancient and modern man-made materials. In addition to the chemical identity of minerals, Raman spectra are affected by crystal orientations (varying relative Raman band intensities); (sub)stoichiometric compositional changes (e.g., in solid solution series), traces of foreign ions, strain (the latter three shifting Raman bands); and crystallinity (changing Raman band widths), enabling a comprehensive physico-chemical characterisation of minerals. Thus, Raman spectroscopy – including its in situ measurement capabilities – provides possibilities to study mineral paragenesis in both, natural and man-made samples at the micrometre scale. While in 1928 the first experimental evidence for inelastic light scattering was provided by C. V. Raman and K. S. Krishnan by using sunlight for excitation, filters for selecting the inelastically scattered light, and their eyes for detection (later, photographic plates for acquisition of spectra were employed), modern Raman spectrometers make use of laser excitation, dispersive spectrographs and charge coupled device (CCD) detection. This Special Issue includes technological developments and applications in the field of modern Raman spectroscopy of minerals in a broad sense, from natural mineral deposits and archaeological objects to inorganic phases in man-made materials. The studied minerals include fossil resins, typical rock-forming minerals (calcite, quartz, forsterite), iron-sulphur species (e.g., mackinawite), a range of sulphates (gypsum, bassanite, anhydrite III, anhydrite II, celestine, barite, ternesite), as well as silicate minerals like garnets (e.g., almandine). KW - Raman spectroscopy KW - Raman microspectroscopy KW - Mineral identification KW - Physico-chemical characterisation of minerals KW - Mineral paragenesis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515041 DO - https://doi.org/10.3390/min10100860 VL - 10 SP - 860 PB - MDPI CY - Basel AN - OPUS4-51504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottu Mukkula, A. R. A1 - Kern, Simon A1 - Salge, M. A1 - Holtkamp, M. A1 - Guhl, Svetlana A1 - Fleischer, C. A1 - Meyer, Klas A1 - Remelhe, M. A1 - Maiwald, Michael A1 - Engell, S. T1 - An Application of Modifier Adaptation with Quadratic Approximation on a Pilot Scale Plant in Industrial Environment N2 - The goal of this work is to identify the optimal operating input for a lithiation reaction that is performed in a highly innovative pilot scale continuous flow chemical plant in an industrial environment, taking into account the process and safety constraints. The main challenge is to identify the optimum operation in the absence of information about the reaction mechanism and the reaction kinetics. We employ an iterative real-time optimization scheme called modifier adaptation with quadratic approximation (MAWQA) to identify the plant optimum in the presence of plant-model mismatch and measurement noise. A novel NMR PAT-sensor is used to measure the concentration of the reactants and of the product at the reactor outlet. The experiment results demonstrate the capabilities of the iterative optimization using the MAWQA algorithm in driving a complex real plant to an economically optimal operating point in the presence of plant-model mismatch and of process and measurement uncertainties. KW - Process Analytical Technology KW - Online NMR Spectroscopy KW - Process Industry KW - Iterative real-time optimization KW - Modifier adaptation KW - Plant-model mismatch KW - Reactor control KW - CONSENS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524531 DO - https://doi.org/10.1016/j.ifacol.2020.12.685 SN - 1522-2640 VL - 53 IS - 2 SP - 11773 EP - 11779 PB - Elsevier CY - Amsterdam AN - OPUS4-52453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - Engell, S. A1 - Paul, Andrea A1 - Pereira Remelhe, M. A1 - Maiwald, Michael T1 - Flexible automation with compact NMR spectroscopy for continuous production of pharmaceuticals N2 - Modular plants using intensified continuous processes represent an appealing concept for the production of pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes; besides, it enables plug-and-produce reconfiguration for fast product changes. To facilitate this flexibility by real-time quality control, we developed a solution that can be adapted quickly to new processes and is based on a compact nuclear magnetic resonance (NMR) spectrometer. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including robust evaluation of sensor data. Beyond monitoring the product quality, online NMR data was used in a new iterative optimization approach to maximize the plant profit and served as a reliable reference for the calibration of a near-infrared (NIR) spectrometer. The overall approach was demonstrated on a commercial-scale pilot plant using a metal-organic reaction with pharmaceutical relevance. KW - NMR Spectroscopy KW - NIR Spectroscopy KW - Real-time process monitoring KW - Real-time quality control KW - Continuous processes KW - CONSENS KW - Data Fusion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480623 DO - https://doi.org/10.1007/s00216-019-01752-y SN - 1618-2642 SN - 1618-2650 VL - 411 IS - 14 SP - 3037 EP - 3046 PB - Springer Nature CY - Heidelberg AN - OPUS4-48062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruno, Francesco A1 - Fiorucci, Letizia A1 - Vignoli, Alessia A1 - Meyer, Klas A1 - Maiwald, Michael A1 - Ravera, Enrico T1 - pyIHM: Indirect Hard Modeling, in Python N2 - NMR is a powerful analytical technique that combines an exquisite qualitative power, related to the unicity of the spectra of each molecule in a mixture, with an intrinsic quantitativeness, related to the fact that the integral of each peak only depends on the number of nuclei (i.e., the amount of substance times the number of equivalent nuclei in the signal), regardless of the molecule. Signal integration is the most common approach in quantitative NMR but has several drawbacks (vide infra). An alternative is to use hard modeling of the peaks. In this paper, we present pyIHM, a Python package for the quantification of the components of NMR spectra through indirect hard modeling, and we discuss some numerical details of the implementation that make this approach robust and reliable. KW - Algorithms KW - Chemical Structure KW - Deconvolution KW - Mixtures KW - NMR spectroscopy PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626793 DO - https://doi.org/10.1021/acs.analchem.4c06484 SN - 1520-6882 VL - 97 IS - 8 SP - 4598 EP - 4605 PB - ACS Publications CY - Washington D.C. AN - OPUS4-62679 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sarhan, R. M. A1 - Koopman, W. A1 - Schuetz, R. A1 - Schmid, Thomas A1 - Liebig, F. A1 - Koetz, J. A1 - Bargheer, M. T1 - The importance of plasmonic heating for the plasmondriven photodimerization of 4-nitrothiophenol N2 - Metal nanoparticles form potent nanoreactors, driven by the optical generation of energetic electrons and nanoscale heat. The relative influence of these two factors on nanoscale chemistry is strongly debated. This article discusses the temperature dependence of the dimerization of 4-nitrothiophenol (4-NTP) into 4,4′-dimercaptoazobenzene (DMAB) adsorbed on gold nanoflowers by Surface-Enhanced Raman Scattering (SERS). Raman thermometry shows a significant optical heating of the particles. The ratio of the Stokes and the anti-Stokes Raman signal moreover demonstrates that the molecular temperature during the reaction rises beyond the average crystal lattice temperature of the plasmonic particles. The product bands have an even higher temperature than reactant bands, which suggests that the reaction proceeds preferentially at thermal hot spots. In addition, kinetic measurements of the reaction during external heating of the reaction environment yield a considerable rise of the reaction rate with temperature. Despite this significant heating effects, a comparison of SERS spectra recorded after heating the sample by an external heater to spectra recorded after prolonged illumination shows that the reaction is strictly photo-driven. While in both cases the temperature increase is comparable, the dimerization occurs only in the presence of light. Intensity dependent measurements at fixed temperatures confirm this finding. KW - Nanoparticles KW - Plasmonic heating KW - Raman spectroscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475140 DO - https://doi.org/10.1038/s41598-019-38627-2 SN - 2045-2322 VL - 9 IS - 1 SP - 3060, 1 EP - 8 PB - Nature Publishing Group AN - OPUS4-47514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yadav, Anur A1 - Iost, R. M. A1 - Neubert, T. J. A1 - Baylan, S. A1 - Schmid, Thomas A1 - Balasubramanian, Kannan T1 - Selective electrochemical functionalization of the graphene edge N2 - We present a versatile and simple method using electrochemistry for the exclusive functionalization of the edge of a graphene monolayer with metal nanoparticles or polymeric amino groups. The attachment of metal nanoparticles allows us to exploit surface-enhanced Raman scattering to characterize the chemistry of both the pristine and the functionalized graphene edge. For the pristine patterned graphene edge, we observe the typical edge-related modes, while for the functionalized graphene edge we identify the chemical structure of the functional layer by vibrational fingerprinting. The ability to obtain single selectively functionalized graphene edges routinely on an insulating substrate opens an avenue for exploring the effect of edge chemistry on graphene properties systematically. KW - Graphene KW - Nanoparticles KW - Nanosciences KW - Surface-enhanced Raman scattering KW - Atomic force microscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474357 DO - https://doi.org/10.1039/C8SC04083D SN - 2041-6520 VL - 10 IS - 3 SP - 936 EP - 942 PB - Royal Society of Chemistry AN - OPUS4-47435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Zengchao A1 - Akkus, Asli A1 - Weisheit, W. A1 - Giray, Thorsten A1 - Penk, Sibylle A1 - Buttler, Sabine A1 - Recknagel, Sebastian A1 - Abad Andrade, Carlos Enrique T1 - Multielement analysis in soils using nitrogen microwave inductively coupled atmospheric pressure plasma mass spectrometry N2 - In this study, we employed nitrogen microwave inductively coupled atmospheric-pressure plasma (MICAP) combined with quadrupole mass spectrometry (MS) and a liquid sample introduction system to analyze heavy metals in soils. The vanadium, cobalt, nickel, zinc, copper, chromium, arsenic, lead, and cadmium contents in seven reference and three environmental soil samples determined using MICAP-MS were within the uncertainty of the reference values, indicating that MICAP-MS is promising for soil analysis similar to the conventional inductively coupled plasma mass spectrometry (ICP-MS) technique. In addition, the limits of detection (LODs) and sensitivity of both techniques using N2 and Ar plasma were of the same order of magnitude. Furthermore, the performance of MICAP-MS under different N2 purity was investigated, and we found that the plasma formation and ionization efficiency were not influenced by the impurities in the gas. A prominent advantage of MICAP-MS is the low operating cost associated with gas consumption. In this work, MICAP-MS used nitrogen, which is cheaper than argon, and consumed 25% less gas than ICP-MS. Using low-purity N2 can further reduce the gas cost, making MICAP-MS more cost effective than ICP-MS. These results suggest that MICAP-MS is a promising alternative to ICP-MS for the analysis of heavy metals in the soil. KW - Soil KW - Microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) KW - Nitrogen plasma KW - Multi-element analysis PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561048 DO - https://doi.org/10.1039/d2ja00244b SN - 0267-9477 VL - 37 IS - 12 SP - 2556 EP - 2562 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-56104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - Lopez-Linares, F. A1 - Poirier, L. A1 - Jakubowski, Norbert A1 - Recknagel, Sebastian A1 - Panne, Ulrich T1 - Shake, shut, and go – A fast screening of sulfur in heavy crude oils by highresolution continuum source graphite furnace molecular absorption spectrometry via GeS molecule detection N2 - A fast and simple method for sulfur quantification in crude oils was developed by using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). For this, heavy crude oil samples were prepared as microemulsion (shake) and injected into a graphite furnace (shut). Finally, the concentration of sulfur was determined by monitoring in situ the transient molecular spectrum of GeS at wavelength 295.205nm after adding a germanium solution as molecular forming agent (and go). Zirconium dioxide in the form of nanoparticles (45–55nm) was employed as a permanent modifier of the graphite furnace. Calibration was done with an aqueous solution standard of ammonium sulfate, and a characteristic mass (m0) of 7.5ng was achieved. The effectiveness of the proposed method was evaluated analizing, ten heavy crude oil samples with Sulfur amounts ranging between 0.3 and 4.5% as well as two NIST standard reference materials, 1620c and 1622e. Results were compared with those obtained by routine ICP-OES analysis, and no statistical relevant differences were found. KW - Heavy crude oil KW - Sulfur KW - HR-CS-MAS KW - Germanium sulfide KW - Microemulsion PY - 2019 DO - https://doi.org/10.1016/j.sab.2019.105671 SN - 0584-8547 VL - 160 SP - 105671 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-48747 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Determination of isotope ratios by molecular absorption spectrometry N2 - Boron and Magnesium present two and three stable isotopes respectevely. It is due to their relatively large mass difference (~ 10%) that isotope fractionation leads to considerable isotope amount ratio variations in the nature. These have been used as a proof of provenance of mineral and biological samples, to estimate a contamination source and to the determination of geological processes by erosion or subduction. Additionally, boron is employed in the nuclear industry due to the capability of its isotope 10B to thermal-neutron capture and therefore 10B enriched boric acid solutions are used in the cooling system of thermonuclear facilities and in the alloying of steel and carbides for protective shielding. Traditionally, isotope ratio variations have been determined by mass spectroscopic methods. Here an alternative faster and low cost method for isotope ratio determination is proposed: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Isotope amount ratios have been determined by monitoring the absorption spectrum of boron monohydride (BH) for boron and Magnesium monofluoride (MgF) for magnesium in a graphite furnace HR-CS-MAS. Bands (0→0) and (1→1) were evaluated. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained are metrologically compatible with those reported by mass spectrometric methods. Moreover, a precision and accuracy of the method of ± 0.5 ‰. This accuracy and precision is comparable with those obtained by thermal ionization mass spectrometry (TIMS) and multiple collector inductively coupled plasma mass spectrometry (MC-ICP-MS) for boron isotope ratio measurements T2 - Analytik Jena Days CY - Idstein, Germany DA - 26.06.2019 KW - Isotope anaylsis KW - HR-CS-MAS KW - Boron KW - Magnesium KW - Optical spectroscopy KW - Diatomic molecule PY - 2019 AN - OPUS4-49877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Soruco Aloisio, Ricardo A1 - Klaus, Christian T1 - Auf dem Weg zu einer digitalen Qualitätsinfrastruktur - Use Case Wasserstofftankstelle N2 - Im Rahmen der von der BAM und anderen Partnern ins Leben gerufenen Initiative „Digitale Qualitätsinfrastruktur“ liegt der Fokus u.a. auf der Entwicklung von neuen Zertifizierungsworkflows. Dabei ist eine besondere Bedeutung dem Zusammenführen von Operational Technology (OT) und Informationstechnik (IT) beizumessen. Zur Datenintegration aus der Sensor-Feldebene einer Versuchs-wasserstofftankstelle wurde eine solche Infrastruktur zunächst in einer Laborumgebung aufgebaut. T2 - Hannover Messe 2024 - Speakers Corners CY - Hannover, Germany DA - 23.04.2024 KW - IT KW - OT KW - Infrastruktur KW - Datenintregration KW - VPN KW - Verwaltungsschale KW - Open Source KW - Software PY - 2024 AN - OPUS4-59930 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Jungnickel, Robert A1 - Dariz, P. T1 - Insights into the CaSO4–H2O System: A Raman-Spectroscopic Study N2 - Even though being the subject of natural scientific research for many decades, the system CaSO4–H2O, consisting of the five crystalline phases gypsum, bassanite, and the anhydrites III, II, and I, has left many open questions for research. Raman spectroscopy was used because of its structural sensitivity and in situ measurement capability to obtain further insight by studying phase transitions in both ex situ and in situ experiments. The findings include significant contributions to the completeness and understanding of Raman spectroscopic data of the system. The dehydration path gypsum–bassanite–anhydrite III was shown to have strong parallels to a physical drying process, which depends on many parameters beyond the burning temperature. Raman band width determination was demonstrated to enable the quantitative discrimination of α-bassanite and β-bassanite as well as the postulated three sub-forms of anhydrite II (AII), which are all based on differences in crystallinity. In the latter case, the observed continuous structural variations over increasing burning temperatures were elucidated as a combination of decreasing surface areas and healing of crystal lattice defects. We propose an only two-fold sub-division of AII into reactive “disordered AII” and much less reactive “crystalline AII” with a transition temperature of 650°C ± 50 K. KW - Gypsum KW - Bassanite KW - Hemihydrate KW - Anhydrite KW - Raman spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506701 DO - https://doi.org/10.3390/min10020115 SN - 2075-163X VL - 10 IS - 2 SP - 115, 35 PB - MDPI CY - Basel AN - OPUS4-50670 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martins, Inês C.B. A1 - Al-Sabbagh, Dominik A1 - Meyer, Klas A1 - Maiwald, Michael A1 - Scholz, G. A1 - Emmerling, Franziska T1 - Insight into the Structure and Properties of Novel Imidazole-Based Salts of Salicylic Acid N2 - The preparation of new active pharmaceutical ingredient (API) multicomponent Crystal forms, especially co-crystals and salts, is being considered as a reliable strategy to improve API solubility and bioavailability. In this study, three novel imidazole-based salts of the poorly water-soluble salicylic acid (SA) are reported exhibiting a remarkable improvement in solubility and dissolution rate properties. All structures were solved by powder X-ray diffraction. Multiple complementary techniques were used to solve co-crystal/salt ambiguities: density functional Theory calculations, Raman and 1H/13C solid-state NMR spectroscopies. In all molecular salts, the Crystal packing interactions are based on a common charged assisted +N-H SA)...O-(co-former) hydrogen bond interaction. The presence of an extra methyl group in different positions of the co-former, induced different supramolecular arrangements, yielding salts with different physicochemical properties. All salts present much higher solubility and dissolution rate than pure SA. The most promising results were obtained for the salts with imidazole and 1-methylimidazole co-formers. KW - Salicylic acid KW - Imidazole KW - Salts KW - Powder X-ray diffraction KW - SsNMR KW - DFT PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502825 DO - https://doi.org/10.3390/molecules24224144 VL - 24 IS - 22 SP - 4144 PB - MDPI AN - OPUS4-50282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neamtu, M. A1 - Nadejde, C. A1 - Brinza, L. A1 - Dragos, O. A1 - Gherghel, D. A1 - Paul, Andrea T1 - Iron phthalocyanine-sensitized magnetic catalysts for BPA photodegradation N2 - The catalytic behavior of iron phthalocyanine (FePc)-sensitized magnetic nanocatalysts was evaluated for their application in the oxidative treatment of Bisphenol A (BPA) under mild environmental conditions. Two types of FePc (Fe(II)Pc and Fe(III)Pc), which are highly photosensitive compounds, were immobilized on the surface of functionalized magnetite. The nanomaterials were characterized by high resolution transmission electron microscopy (HR-TEM), X-ray difraction (XRD), Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analyses (TGA). The generation of singlet Oxygen by nanomaterials was also investigated. In the presence of UVA light exposure (365nm) and 15mM H2O2, the M@Fe(III)Pc photocatalyst gave the best results; for a catalyst concentration of 2.0gL −1, around 60% BPA was removed after 120min of reaction. These experimental conditions were further tested under natural solar light exposure, for which also M@Fe(III)Pc exhibited enhanced oxidative catalytic activity, being able to remove 83% of BPA in solution. The water samples were less cytotoxic after treatment, this being confrmed by the MCF-7 cell viability assay. KW - Photosensitization KW - magnetic nanocatalysts KW - BPA removal PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506368 DO - https://doi.org/10.1038/s41598-020-61980-6 VL - 10 IS - 1 SP - 5376 AN - OPUS4-50636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eifert, T. A1 - Eisen, K. A1 - Maiwald, Michael A1 - Herwig, C. T1 - Current and future requirements to industrial analytical infrastructure—part 2: smart sensors N2 - Complex processes meet and need Industry 4.0 capabilities. Shorter product cycles, flexible production needs, and direct assessment of product quality attributes and raw material attributes call for an increased need of new process analytical technologies (PAT) concepts. While individual PAT tools may be available since decades, we need holistic concepts to fulfill above industrial needs. In this series of two contributions, we want to present a combined view on the future of PAT (process analytical technology), which is projected in smart labs (Part 1) and smart sensors (Part 2). Part 2 of this feature article series describes the future functionality as well as the ingredients of a smart sensor aiming to eventually fuel full PAT functionality. The smart sensor consists of (i) chemical and process information in the physical twin by smart field devices, by measuring multiple components, and is fully connected in the IIoT 4.0 environment. In addition, (ii) it includes process intelligence in the digital twin, as to being able to generate knowledge from multi-sensor and multi-dimensional data. The cyber-physical system (CPS) combines both elements mentioned above and allows the smart sensor to be self-calibrating and self-optimizing. It maintains its operation autonomously. Furthermore, it allows—as central PAT enabler—a flexible but also target-oriented predictive control strategy and efficient process development and can compensate variations of the process and raw material attributes. Future cyber-physical production systems—like smart sensors—consist of the fusion of two main pillars, the physical and the digital twins. We discuss the individual elements of both pillars, such as connectivity, and chemical analytics on the one hand as well as hybrid models and knowledge workflows on the other. Finally, we discuss its integration needs in a CPS in order to allow is versatile deployment in efficient process development and advanced optimum predictive process control. KW - Smart sensors KW - Industry 4.0 KW - Digital twins KW - Process intelligence KW - Process analytical technology KW - Physical twin KW - Cyber-physical system PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503980 DO - https://doi.org/10.1007/s00216-020-02421-1 SN - 1618-2642 VL - 412 IS - 9 SP - 2037 EP - 2045 PB - Springer CY - Berlin Heidelberg AN - OPUS4-50398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eisen, K A1 - Eifert, T A1 - Herwig, C A1 - Maiwald, Michael T1 - Current and future requirements to industrial analytical infrastructure—part 1: process analytical laboratories N2 - The competitiveness of the chemical and pharmaceutical industry is based on ensuring the required product quality while making optimum use of plants, raw materials, and energy. In this context, effective process control using reliable chemical process analytics secures global competitiveness. The setup of those control strategies often originate in process development but need to be transferable along the whole product life cycle. In this series of two contributions, we want to present a combined view on the future of PAT (process analytical technology), which is projected in smart labs (part 1) and smart sensors (part 2). In laboratories and pilot plants, offline chemical analytical methods are frequently used, where inline methods are also used in production. Here, a transferability from process development to the process in operation would be desirable. This can be obtained by establishing PAT methods for production already during process development or scale-up. However, the current PAT (Bakeev 2005, Org Process Res 19:3–62; Simon et al. 2015, Org Process Res Dev 19:3–62) must become more flexible and smarter. This can be achieved by introducing digitalization-based knowledge management, so that knowledge from product development enables and accelerates the integration of PAT. Conversely, knowledge from the production process will also contribute to product and process development. This contribution describes the future role of the laboratory and develops requirements therefrom. In part 2, we examine the future functionality as well as the ingredients of a smart sensor aiming to eventually fuel full PAT functionality—also within process development or scale-up facilities (Eifert et al. 2020, Anal Bioanal Chem). KW - Smart test laboratories KW - Laboratory 4.0 KW - Sustainable Production KW - Industry 4.0 PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504020 DO - https://doi.org/10.1007/s00216-020-02420-2 SN - 1618-2642 VL - 412 IS - 9 SP - 2027 EP - 2035 PB - Springer CY - Berlin Heidelberg AN - OPUS4-50402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zettner, Alina A1 - Gojani, Ardian A1 - Schmid, Thomas A1 - Gornushkin, Igor B. T1 - Evaluation of a Spatial Heterodyne Spectrometer for Raman Spectroscopy of Minerals N2 - Spatial heterodyne spectroscopy (SHS) is a novel spectral analysis technique that is being applied for Raman spectroscopy of minerals. This paper presents the theoretical basis of SHS and its application for Raman measurements of calcite, quartz and forsterite in marble, copper ore and nickel ore, respectively. The SHS measurements are done using a broadband (518–686 nm) and resolving power R ≈ 3000 instrument. The spectra obtained using SHS are compared to those obtained by benchtop and modular dispersive spectrometers. It is found that SHRS performance in terms of resolution is comparable to that of the benchtop spectrometer and better than the modular dispersive spectrometer, while the sensitivity of SHRS is worse than that of a benchtop spectrometer, but better than that of a modular dispersive spectrometer. When considered that SHS components are small and can be packaged into a handheld device, there is interest in developing an SHS-based Instrument for mobile Raman spectroscopy. This paper evaluates the possibility of such an application. KW - Forsterite KW - Spatial heterodyne spectrometer KW - Interferometric spectroscopy KW - Fourier transform spectroscopy KW - Raman spectroscopy KW - Calcite KW - Quartz PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504624 DO - https://doi.org/10.3390/min10020202 VL - 10 IS - 2 SP - 202 PB - MDPI CY - Basel, Switzerland AN - OPUS4-50462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Integrated and Networked Systems and Processes—A Perspective for Digital Transformation in Thermal Process Engineering N2 - Separation technology as a sub-discipline of thermal process engineering is one of the most critical steps in the production of chemicals, essential for the quality of intermediate and end products. The discipline comprises the construction of facilities that convert raw materials into value-added products along the value chain. Conversions typically take place in repeated reaction and separation steps—either in batch or continuous processes. The end products are the result of several production and separation steps that are not only sequentially linked, but also include the treatment of unused raw materials, by-products and wastes. Production processes in the process industry are particularly susceptible to fluctuations in raw materials and other influences affecting product quality. This is a challenge, despite increasing fluctuations, to deliver targeted quality and simultaneously meet the increasing dynamics of the market, at least for high value fine chemicals. In order to survive successfully in a changed environment, chemical companies must tread new paths. This includes the potential of digital technologies. The full integration and intelligent networking of systems and processes is progressing hesitantly. This contribution aims to encourage a more holistic approach to the digitalization in thermal process engineering by introduction of integrated and networked systems and processes. KW - Smarter Sensor KW - Digitalisation KW - Digital transformation KW - Process Industry KW - Thermal Process Engineering KW - Digital Twins PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504964 DO - https://doi.org/10.3390/chemengineering4010015 SN - 2305-7084 VL - 4 IS - 15 SP - 1 EP - 9 PB - MDPI CY - Basel AN - OPUS4-50496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thiele, Isabel A1 - Santolin, Lara A1 - Meyer, Klas A1 - Machatschek, Rainhard A1 - Bölz, Uwe A1 - Tarazona, Natalia A. A1 - Riedel, Sebastian L. T1 - Microbially synthesized poly(hydroxybutyrate-co-hydroxyhexanoate) with low to moderate hydroxyhexanoate content: Properties and applications N2 - Plastic pollution is the biggest environmental concern of our time. Breakdown products like micro- and nanoplastics inevitably enter the food chain and pose unprecedented health risks. In this scenario, bio-based and biodegradable plastic alternatives have been given a momentum aiming to bridge a transition towards a more sustainable future. Polyhydroxyalkanoates (PHAs) are one of the few thermoplastic polymers synthesized 100 % via biotechnological routes which fully biodegrade in common natural environments. Poly(hydroxybutyrate-cohydroxyhexanoate) [P(HB-co-HHx)] is a PHA copolymer with great potential for the commodity polymers industry, as its mechanical properties can be tailored through fine-tuning of its molar HHx content. We have recently developed a strategy that enables for reliable tailoring of the monomer content of P(HB-co-HHx). Nevertheless, there is often a lack of comprehensive investigation of the material properties of PHAs to evaluate whether they actually mimic the functionalities of conventional plastics. We present a detailed study of P(HB-co-HHx) copolymers with low to moderate hydroxyhexanoate content to understand how the HHx monomer content influences the thermal and mechanical properties and to link those to their abiotic degradation. By increasing the HHx fractions in the range of 2 – 14 mol%, we impart an extension of the processing window and application range as the melting temperature (Tm) and glass temperature (Tg) of the copolymers decrease from Tm 165 ◦C to 126 ◦C, Tg 4 ◦C to − 5.9 ◦C, accompanied by reduced crystallinity from 54 % to 20 %. Elongation at break was increased from 5.7 % up to 703 % at 14 mol% HHx content, confirming that the range examined was sufficiently large to obtain ductile and brittle copolymers, while tensile strength was maintained throughout the studied range. Finally, accelerated abiotic degradation was shown to be slowed down with an increasing HHx fraction decreasing from 70 % to 55 % in 12 h. KW - Molecular Biology KW - General Medicine KW - Biochemistry KW - Structural Biology PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595636 DO - https://doi.org/10.1016/j.ijbiomac.2024.130188 VL - 263 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-59563 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Villajos Collado, José Antonio A1 - Balderas‐Xicohténcatl, Rafael A1 - Al Shakhs, Ali N. A1 - Berenguer‐Murcia, Ángel A1 - Buckley, Craig E. A1 - Cazorla‐Amorós, Diego A1 - Charalambopoulou, Georgia A1 - Couturas, Fabrice A1 - Cuevas, Fermin A1 - Fairen‐Jimenez, David A1 - Heinselman, Karen N. A1 - Humphries, Terry D. A1 - Kaskel, Stefan A1 - Kim, Hyunlim A1 - Marco‐Lozar, Juan P. A1 - Oh, Hyunchul A1 - Parilla, Philip A. A1 - Paskevicius, Mark A1 - Senkovska, Irena A1 - Shulda, Sarah A1 - Silvestre‐Albero, Joaquin A1 - Steriotis, Theodore A1 - Tampaxis, Christos A1 - Hirscher, Michael A1 - Maiwald, Michael T1 - Establishing ZIF‐8 as a reference material for hydrogen cryoadsorption: An interlaboratory study N2 - AbstractHydrogen storage by cryoadsorption on porous materials has the advantages of low material cost, safety, fast kinetics, and high cyclic stability. The further development of this technology requires reliable data on the H2 uptake of the adsorbents, however, even for activated carbons the values between different laboratories show sometimes large discrepancies. So far no reference material for hydrogen cryoadsorption is available. The metal‐organic framework ZIF‐8 is an ideal material possessing high thermal, chemical, and mechanical stability that reduces degradation during handling and activation. Here, we distributed ZIF‐8 pellets synthesized by extrusion to 9 laboratories equipped with 15 different experimental setups including gravimetric and volumetric analyzers. The gravimetric H2 uptake of the pellets was measured at 77 K and up to 100 bar showing a high reproducibility between the different laboratories, with a small relative standard deviation of 3–4 % between pressures of 10–100 bar. The effect of operating variables like the amount of sample or analysis temperature was evaluated, remarking the calibration of devices and other correction procedures as the most significant deviation sources. Overall, the reproducible hydrogen cryoadsorption measurements indicate the robustness of the ZIF‐8 pellets, which we want to propose as a reference material. KW - Physical and theoretical chemistry KW - Atomic and molecular physics, and optics PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594788 DO - https://doi.org/10.1002/cphc.202300794 SN - 1439-7641 SP - 1 EP - 7 PB - Wiley CY - Weinheim AN - OPUS4-59478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kowalewska, Z. A1 - Abad Andrade, Carlos Enrique A1 - Okruss, M. A1 - Recknagel, Sebastian T1 - Feasibility of high-resolution continuum source molecular absorption spectrometry for vanadium determination N2 - This work aimed to evaluate high-resolution continuum source molecular absorption spectrometry (HR-CS MAS), traditionally used to determine non-metals, for the determination of a new element, metal, vanadium. VO was selected as a target molecule because it is relatively stable and was expected to be spontaneously generated in a flame or a graphite furnace (GF). The high-resolution overview spectra of the molecule were obtained in a wide range of 480–630 nm, and absorption due to the X4Σ−–C4Σ− electronic transition was registered. A unique instrumental setup, comprising a prototype Modular Simultaneous Echelle Spectrograph (MOSES) and a commercial HR-CS MAS apparatus, was applied in the research. Finally, the spectral area centered at 550.6230 nm was selected for analysis. A method was developed to determine V in solutions of catalysts of heavy petroleum oil hydroprocessing using a commercial HR-CS spectrometer in a flame version. Although sensitivity was relatively poor (characteristic concentration 380 mg L−1), an extremely low noise enabled reaching a satisfactory detection limit (20 mg L−1 in solution, i.e. 0.1% m:m in the catalyst). For the first time vanadium was determined using ordinary air-acetylene flame. The obtained results were consistent with the results of atomic absorption spectrometry with N2O-C2H2 flame. Unfortunately, only a small population of VO molecules could have been generated in GF measurements. Furthermore, the observed VO molecules appeared only at unfavorably high temperatures. The work shows the potential of HR-CS MAS as a scientific tool for investigating the mechanism of processes occurring in the GF. This work can inspire other research of new analytes for HR-CS MAS. KW - Vanadium KW - HR-CS-MAS KW - VO KW - High-resolution continuum source molecular absorption spectrometry KW - AAS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569899 DO - https://doi.org/10.1039/D2JA00281G SN - 0267-9477 VL - 38 IS - 2 SP - 472 EP - 483 PB - Royal Society of Chemistry AN - OPUS4-56989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhuang, Y. A1 - Spahr, S. A1 - Lutze, H.V. A1 - Reith, C.J. A1 - Hagemann, N. A1 - Paul, Andrea A1 - Haderlein, S.B. T1 - Persulfate activation by biochar and iron: Effect of chloride on formation of reactive species and transformation of N,N-diethyl-m-toluamide (DEET) N2 - Fenton-like processes using persulfate for oxidative water treatment and contaminant removal can be enhanced by the addition of redox-active biochar, which accelerates the reduction of Fe(III) to Fe(II) and increases the yield of reactive species that react with organic contaminants. However, available data on the formation of non-radical or radical species in the biochar/Fe(III)/persulfate system are inconsistent, which limits the evaluation of treatment efficiency and applicability in different water matrices. Based on competition kinetics calculations, we employed different scavengers and probe compounds to systematically evaluate the effect of chloride in presence of organic matter on the formation of major reactive species in the biochar/Fe(III)/persulfate system for the transformation of the model compound N,N‑diethyl-m-toluamide (DEET) at pH 2.5. We show that the transformation of methyl phenyl sulfoxide (PMSO) to methyl phenyl sulfone (PMSO2) cannot serve as a reliable indicator for Fe(IV), as previously suggested, because sulfate radicals also induce PMSO2 formation. Although the formation of Fe(IV) cannot be completely excluded, sulfate radicals were identified as the major reactive species in the biochar/Fe(III)/persulfate system in pure water. In the presence of dissolved organic matter, low chloride concentrations (0.1 mM) shifted the major reactive species likely to hydroxyl radicals. Higher chloride concentrations (1 mM), as present in a mining-impacted acidic surface water, resulted in the formation of another reactive species, possibly Cl2•−, and efficient DEET degradation. To tailor the application of this oxidation process, the water matrix must be considered as a decisive factor for reactive species formation and contaminant removal. KW - Water treatment KW - Organic contaminants KW - Fenton-like systems KW - Radicals KW - ESR PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608677 DO - https://doi.org/10.1016/j.watres.2024.122267 SN - 0043-1354 VL - 265 SP - 1 EP - 8 PB - Elsevier Ltd. AN - OPUS4-60867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Zengchao A1 - Winckelmann, Alexander A1 - Vogl, Jochen A1 - Recknagel, Sebastian A1 - Abad Andrade, Carlos Enrique T1 - Determination of calcium, iron, and selenium in human serum by isotope dilution analysis using nitrogen microwave inductively coupled atmospheric pressure plasma mass spectrometry (MICAP-MS) N2 - In this study, we demonstrate the applicability of nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) for Ca, Fe, and Se quantification in human serum using isotope dilution (ID) analysis. The matrix tolerance of MICAP-MS in Na matrix was investigated, uncovering that high Na levels can suppress the signal intensity. This suppression is likely due to the plasma loading and the space charge effect. Moreover, 40Ca and 44Ca isotopic fractionation was noted at elevated Na concentration. Nine certified serum samples were analyzed using both external calibration and ID analysis. Overestimation of Cr, Zn, As, and Se was found in the results of external calibration, which might be resulted from C-induced polyatomic interference and signal enhancement, respectively. Further investigations performed with methanol showed a similar enhancement effect for Zn, As, and Se, potentially supporting this assumption. The mass concentrations determined with ID analysis show metrological compatibility with the reference values, indicating that MICAP-MS combined with ID analysis can be a promising method for precise Ca, Fe, and Se determination. Moreover, this combination reduces the influences of matrix effects, broadening the applicability of MICAP-MS for samples with complex matrix. KW - Selenium KW - Nitrogen microwave inductively coupled atmospheric pressure mass spectrometry KW - Isotope dilution KW - Human serum KW - Calcium KW - Iron PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598664 DO - https://doi.org/10.1007/s00216-024-05274-0 SN - 1618-2642 SP - 3117 EP - 3125 PB - Springer CY - Berlin AN - OPUS4-59866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tchipilov, Teodor A1 - Meyer, Klas A1 - Weller, Michael G. T1 - Quantitative 1H nuclear magnetic resonance (qNMR) of aromatic amino acids for protein quantification N2 - Hydrolysis of protein samples into amino acids facilitates the use of NMR spectroscopy for protein and peptide quantification. Different conditions have been tested for quantifying aromatic amino acids and proteins. The pH-dependent signal shifts in the aromatic region of amino acid samples were examined. A pH of 12 was found to minimize signal overlap of the four aromatic amino acids. Several aromatic compounds, such as terephthalic acid, sulfoisophthalic acid, and benzene tricarboxylic acid, were applied as internal standards. The quantification of amino acids from an amino acid standard was performed. Using the first two suggested internal standards, recovery was ~97% for histidine, phenylalanine, and tyrosine at a concentration of approximately 1 mM in solution. Acidic hydrolysis of a certified reference material (CRM) of bovine serum albumin (BSA) and subsequent quantification of Phe and Tyr yielded recoveries of 98% ± 2% and 88% ± 4%, respectively, at a protein concentration of 16 g/L or 250 µM. KW - Amino acid analysis KW - Aromatic amino acid analysis KW - AAA KW - AAAA KW - Protein hydrolysis KW - Hydrochloric acid KW - Metrology KW - Traceability KW - NIST KW - Reference materials KW - Internal standard KW - Calibration KW - Compound-independent calibration KW - Histidine KW - Tyrosine KW - Tryptophan KW - Phenylalanine KW - Terephthalic acid KW - Benzene-1,3,5-tricarboxylic acid KW - Bovine serum albumin (BSA) KW - Quantitative protein analysis KW - Phenylketonuria PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570943 DO - https://doi.org/10.3390/mps6010011 VL - 6 IS - 1 SP - 1 EP - 13 PB - MDPI CY - Basel, Schweiz AN - OPUS4-57094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grimmer, Christoph T1 - Development, application and measurement uncertainty of emission reference materials N2 - Volatile organic compounds (VOCs) emitted by furniture and building materials can cause health issues. For an improvement of indoor air quality low emitting materials should be used. Quality assurance and –control (QA/QC) measures require an emission reference material (ERM) with a predictable emission rate of VOCs. The idea is to use porous materials as ERM, which store the VOCs inside their pores and emit them constantly. T2 - Webinar Metrology for Indoor Air Quality Reference materials for QA/QC of the emission test chamber procedure CY - Online meeting DA - 11.04.2024 KW - Emission reference materials KW - Indoor air quality KW - Materials emissions test KW - VOC PY - 2024 AN - OPUS4-59963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Stable isotope analysis of magnesium by optical spectrometry N2 - Magnesium is a naturally occurring element that can be found in several mineral forms in the earth crust. This element presents three stable isotopes 24Mg, 25Mg and 26Mg with a natural abundance of 79%, 10%, and 11% respectively. It is due to their relatively large mass difference (~8% between 24Mg and 26Mg) that isotope fractionation leads to slight isotope amount ratio variations n(26Mg)/n(24Mg) in biological and geological samples. Traditionally, isotope amount ratios have been measured by mass spectrometric methods. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time-consuming. Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) and laser ablation molecular isotopic spectrometry (LAMIS). For the determination of Mg isotope amount ratios, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied. In the case of HR-CS-GFMAS, the absorption spectrum was recorded for MgF for the electronic transitions X 2Σ → A 2 Πi and X 2Σ → B 2Σ+ around wavelengths 358 nm and 268 nm respectively. In the case of LAMIS, it was studied the MgF molecule for the electronic transitions A 2Πi → X 2Σ as well as the MgO molecule for the electronic transition A 1Π+ → X 1Σ around 500 nm. The MgF and MgO spectra are composed by the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO (F is monoisotopic, and the isotope composition of O is assumed as constant). By HR-CS-GFMAS the analysis of Mg was done by deconvolution of the MgF spectrum by a partial least square regression (PLS) calibrated with enriched isotope spikes. The isotope amount ratios in rock samples with and without matrix separation were analyzed. Resulting delta values were obtained with precisions ranging between 0.2-0.5 ‰. On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of in-situ analysis. Main advantages, limitations, and scopes of both optical techniques are going to be discussed and compared with MC-ICP-MS. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Isotope analysis KW - HR-CS-MAS KW - LIBS KW - MC-ICP-MS KW - Magnesium PY - 2019 AN - OPUS4-49876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Matthias T1 - Metrological sound reference products for quality assurance and quality control measures in material emissions testing N2 - In industrialised countries more than 80% of the time is spent indoors. Products, such as building materials and furniture, emit volatile organic compounds (VOCs), which are therefore ubiquitous in indoor air. Different VOC combinations may, under certain environmental and occupational conditions, result in reported sensory irritation and health complaints. A healthy indoor environment can be achieved by controlling the sources and by eliminating or limiting the release of harmful substances into the air. One way is to use materials proven to be low emitting. Meanwhile, a worldwide network of professional commercial and non-commercial laboratories performing emission tests for the evaluation of products for interior use has been established. Therefore, comparability and metrological traceability of test results must be ensured. A laboratory’s proficiency can be proven by internal and external validation measures that both include the application of suitable reference materials. The emission test chamber procedure according to EN 16516 comprises several steps from sample preparation to sampling of test chamber air and chromatographic analysis. Quality assurance and quality control (QA/QC) must therefore be ensured. Currently, there is a lack of suitable reference products containing components relevant for the health-related evaluation of building products. The EU-funded EMPIR project 20NRM04 MetrIAQ (Metrology for the determination of emissions of dangerous substances from building materials into indoor air) aims to develop 1) gaseous primary reference materials (gPRM), which are used for the certification of gaseous (certified) reference materials (gCRM) and 2) emission reference materials (ERM). Most commercial gas standards of indoor-relevant compounds are not certified due to the lack of primary reference materials to which the project aims to contribute. The gPRM under development is a gas-phase standard containing trace levels of VOCs in nitrogen or air from the check standard according to EN 16516 (n-hexane, methyl isobutyl ketone, toluene, butyl acetate, cyclohexanone, o-xylene, phenol, 1,3,5-trimethylbenzene) with a target uncertainty of 5 %. The gPRM can be sampled into sorbent tubes to obtain transfer standards in the form of gCRM. The well characterised ERM represents a sample of a test specimen, e.g. building material, that is loaded into the emission test chamber for a period of several days and is used to evaluate the whole emission test chamber procedure. It shall have a reproducible and temporally constant compound release of less than 10 % variability over 14 days. Different approaches for retarded VOC release, such as the encapsulation of pure compounds and the impregnation of porous materials, are being tested to reach this aim. Furthermore, the design of the ERM is accompanied by the development of a numerical model for the prediction of the emissions for each of the target VOCs. The current progress of the work on both materials will be presented. T2 - CIM 2023 - 21st International Metrology Congress CY - Lyon, France DA - 07.03.2023 KW - Indoor air quality KW - VOC KW - Materials emissions testing KW - Emission reference material KW - Quality assurance/quality control PY - 2023 AN - OPUS4-57142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grimmer, Christoph T1 - Preparation of novel emission reference materials: μ-capsules & impregnated porous materials N2 - Volatile organic compounds (VOCs) emitted by furniture and building materials can cause health issues. For an improvement of indoor air quality low emitting materials should be used. Quality assurance and –control (QA/QC) measures require an emission reference material (ERM) with a predictable emission rate of VOCs. The idea is to use porous materials as ERM, which store the VOCs inside their pores and emit them constantly. T2 - WORKSHOP: METROLOGY FOR INDOOR AIR QUALITY CY - Mol, Belgium DA - 18.10.2023 KW - Emission reference materials KW - Indoor air quality KW - Materials emissions test KW - VOC PY - 2023 AN - OPUS4-59961 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Matthias T1 - Emission reference materials for indoor air measurements N2 - In industrialised countries more than 80% of the time is spent indoors. Products, such as building materials and furniture, emit volatile organic compounds (VOCs), which are therefore ubiquitous in indoor air. VOC in combination may, under certain environmental and occupational conditions, result in reported sensory irritation and health complaints. Emission concentrations can become further elevated in new or refurbished buildings where the rate of air exchange with fresh ambient air may be limited due to improved energy saving aspects. A healthy indoor environment can be achieved by controlling the sources and by eliminating or limiting the release of harmful substances into the air. One way is to use (building) materials proved to be low emitting. Meanwhile, a worldwide network of professional commercial and non-commercial laboratories performing emission tests for the evaluation of products for interior use has been established. Therefore, comparability of test results must be ensured. A laboratory’s proficiency can be proven by internal and external validation measures that both include the application of suitable emission reference materials (ERM). For the emission test chamber procedure according to EN 16516, no artificial ERM is commercially available. The EU-funded EMPIR project MetrIAQ aims to fill this gap by developing new and improved ERMs. The goal is to obtain a material with a reproducible and temporally constant compound release (less than 10 % variability over 14 days). Two approaches were tested: the impregnation of porous materials with VOC, and the encapsulation of VOC in polymer microcapsules. Impregnation is performed with help of an autoclave and supercritical CO2. The encapsulation is done by interfacial polymerisation on VOC droplets. For both approaches, synthesis and/or material parameters were varied to obtain an optimal ERM. Findings about the optimisation of ERM generation, as well as performance of the best emission reference materials, will be presented. T2 - GAS Analysis 2024 CY - Paris, France DA - 30.01.2024 KW - Emission reference materials KW - Materials emissions test KW - VOC KW - Indoor air quality PY - 2024 AN - OPUS4-59506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Niederfeld-NMR-Spektroskopie: Ein universelles Werkzeug für automatisierte, kontinuierliche Produktion von Chemikalien und Pharmazeutika N2 - Um in einem veränderten Umfeld erfolgreich bestehen zu können, müssen Chemieunternehmen neue Pfade beschreiten. Dazu gehört insbesondere das Potential digitaler Technologien. Mit flexiblen, modularen chemischen Vielzweck-Produktionsanlagen lassen sich häufig wechselnde Produkte mit kürzeren Vorlauf- und Stillstandzeiten zwischen den Kampagnen und dennoch hoher Qualität realisieren. Intensivierte, kontinuierliche Produktionsanlagen erlauben auch den Umgang mit schwierig zu handhabenden Substanzen. Grundvoraussetzung für solche Konzepte ist eine hochautomatisierte "chemische" Prozesskontrolle zusammen mit Echtzeit-Qualitätskotrolle, die "chemische" Informationen über den Prozess bereitstellt. In einem Anwendungsbeispiel wurde eine pharmazeutische Lithiierungsreaktion aus einer modularen Pilot-Anlage betrachtet und dabei die Vorzüge eines vollautomatischen NMR-Sensors untersucht. Dazu wurde ein kommerziell erhältliches Benchtop-NMR-Spektrometer mit Permanentmagnet auf die industriellen Anforderungen, wie Explosionsschutz, Feldkommunikation und vollautomatischer, robuster Datenauswertung angepasst. Der NMR-Sensor konnte schließlich erfolgreich im vollautomatischen Betrieb nach fortschrittlichen Regelkonzepten und für die Echtzeitoptimierung der Anlage getestet werden. Die NMR-Spektroskopie erwies sich als hervorragende Online-Methode und konnte zusammen mit einer modularen Datenauswertung sehr flexibel genutzt werden. Die Methode konnte überdies als zuverlässige Referenzmethode zur Kalibrierung konventioneller Online-Analytik eingesetzt werden. Zukünftig werden voll integrierte und intelligent vernetzte "smarte" Sensoren und Prozesse eine kontinuierliche Produktion von Chemikalien und Pharmazeutika mit vertretbaren Qualitätskosten möglich machen. T2 - GDCh-Kolloquium des Ortsverbands Magdeburg CY - Magdeburg, Germany DA - 04.07.2019 KW - Online-NMR-Spektroskopie KW - Smarte Sensoren KW - Prozessindustrie KW - Digitalisierung KW - Fresenius PY - 2019 AN - OPUS4-48414 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Voll integrierte und intelligent vernetzte Systeme und Prozesse – Perspektive: Smarte Sensorik, Aktorik und Kommunikation N2 - Um in einem veränderten Umfeld erfolgreich bestehen zu können, müssen Chemieunternehmen neue Pfade beschreiten. Dazu gehört insbesondere das Potential digitaler Technologien. Mit flexiblen, modularen chemischen Vielzweck-Produktionsanlagen lassen sich häufig wechselnde Produkte mit kürzeren Vorlauf- und Stillstandzeiten zwischen den Kampagnen und dennoch hoher Qualität realisieren. Intensivierte, kontinuierliche Produktionsanlagen erlauben auch den Umgang mit schwierig zu handhabenden Substanzen. Grundvoraussetzung für solche Konzepte ist eine hochautomatisierte "chemische" Prozesskontrolle zusammen mit Echtzeit-Qualitätskotrolle, die "chemische" Informationen über den Prozess bereitstellt. In einem Anwendungsbeispiel wurde eine pharmazeutische Lithiierungsreaktion aus einer modularen Pilot-Anlage betrachtet und dabei die Vorzüge eines vollautomatischen NMR-Sensors untersucht. Dazu wurde ein kommerziell erhältliches Benchtop-NMR-Spektrometer mit Permanentmagnet auf die industriellen Anforderungen, wie Explosionsschutz, Feldkommunikation und vollautomatischer, robuster Datenauswertung angepasst. Der NMR-Sensor konnte schließlich erfolgreich im vollautomatischen Betrieb nach fortschrittlichen Regelkonzepten und für die Echtzeitoptimierung der Anlage getestet werden. Die NMR-Spektroskopie erwies sich als hervorragende Online-Methode und konnte zusammen mit einer modularen Datenauswertung sehr flexibel genutzt werden. Die Methode konnte überdies als zuverlässige Referenzmethode zur Kalibrierung konventioneller Online-Analytik eingesetzt werden. Zukünftig werden voll integrierte und intelligent vernetzte "smarte" Sensoren und Prozesse eine kontinuierliche Produktion von Chemikalien und Pharmazeutika mit vertretbaren Qualitätskosten möglich machen. T2 - Kolloquium im Rahmen der Innovationskampagne CY - Karlsruhe, Germany DA - 18.07.2019 KW - Prozessanalytik KW - Prozesskontrolle KW - Digitalisierung KW - Prozessindustrie KW - Smarte Sensoren KW - Automation PY - 2019 AN - OPUS4-48513 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - ZRM für die Nichtmetall-Analytik N2 - Die Vorgehensweise bei der Zertifizierung von Referenzmaterialien in der BAM entsprechend den Regeln des ISO-Guide 35 wird an Beispielen beschrieben. Darüber hinaus wird ein umfassender Überblick über Referenzmaterialien zur Analyse der Nichtmetalle Sauerstoff, Wasserstoff, Stickstoff, Kohle und Schwefel gegeben. T2 - Expertentreffen anorganische Materialanalyse CY - Langenselbold, Germany DA - 11.09.2019 KW - ZRM KW - Nichtmetall-Analytik KW - ISO-Guide 35 KW - Referenzmaterialien PY - 2019 AN - OPUS4-49091 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Reference materials for non-metal analysis N2 - The procedure for certification of reference materials in BAM in accordance with the rules of ISO Guide 35 is described using examples. In addition, a comprehensive overview of reference materials for the analysis of non-metals oxygen, hydrogen, nitrogen, coal and sulfur is given. T2 - LECO Workshop: CHNOS determination in inorganic (high tec) materials CY - Berlin, Germany DA - 22.10.2019 KW - CRM KW - Non-metal analysis KW - ISO-Guide 35 KW - Reference materials PY - 2019 AN - OPUS4-49458 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Analysis of dynamic systems N2 - Monitoring specific information (i.e., physico-chemical properties, chemical reactions, etc.) is the key to chemical process control when looking at dynamic systems, and quantitative online NMR spectroscopy is the method of choice for the investigation and understanding of dynamic multi-component systems. NMR provides rapid and non-invasive information, and due to the inherent linearity between sample concentration and signal intensity, peak areas can be directly used for quantification of multiple components in a mixture (without the need for any further calibration). This is one of the most attractive features of quantitative NMR spectroscopy. With the launch of devices covering magnetic field strengths from 40 to 90 MHz, so called compact or benchtop NMR systems, this analytical method is now reaching a sufficient degree of compactness and operability for an application outside of very specialized laboratories. Whilst there are also many other tools available to examine various analytical parameters from dynamic processes, such as mass spectrometry, (near) infrared or Raman spectroscopy, each of these tools can only really be used independently. How can we examine and compare all data describing a particular chemical reaction? How can we visualize information rich, specific, or direct methods together with less specific but established analytical methods? And how can we transfer calibration information to the most appropriate process analytical method or method combination? Quantitative NMR spectroscopy (qNMR) has the potential to substitute offline laboratory analysis for calibration purposes by delivering quantitative reference data as an online method. The workshop briefly presents the current state of the art of the analysis of dynamic systems by online NMR spectroscopy and analytical data fusion, with the remaining time being used for questions and open discussion with the attendees. T2 - SMASH 2019 CY - Porto, Portugal DA - 22.09.2019 KW - Process Analytical Technology KW - Reaction Monitoring KW - Online NMR Spectroscopy KW - Data Analysis KW - SMASH PY - 2019 UR - https://www.smashnmr.org/ AN - OPUS4-49042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Integrated and Networked Systems and Processes – A Perspective for Digital Transformation in (Bio) Process Engineering N2 - The competitiveness of the process industry is based on ensuring the required product quality while making optimum use of equipment, raw materials and energy. Chemical companies have to find new paths to survive successfully in a changing environment, while also finding more flexible ways of product and process development to bring their products to market more quickly – especially high-quality high-end products like fine chemicals or pharmaceuticals. The potential of digital technologies belongs to these. One way is knowledge-based production, taking into account all essential equipment, process and regulatory data of plants and laboratories. Today, the potential of this data is often not yet consistently used for a comprehensive understanding of production. Another approach uses flexible and modular chemical plants, which can produce different high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce the time to market of new products. Digital transformation is enabling completely new production concepts that are being used increasingly. Intensified continuous production plants also allow for difficult to produce compounds. This contribution aims to encourage a more holistic approach to the digitalization and use of machine-assisted methods in (bio) process engineering by introduction of integrated and networked systems and processes, which have the potential to speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - 6th BioProScale Symposium - industrial scale bioprocess intensification from process development to large-scale understanding CY - Online meeting DA - 29.03.2021 KW - Industry 4.0 KW - Biotechnology KW - Bio engineering KW - Process Analytical Technology KW - BioProScale KW - Artificial Neural Networks PY - 2021 UR - https://biotechnologie.ifgb.de/node/648 AN - OPUS4-52371 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Maiwald, Michael ED - Tauschnitz, T. T1 - Erweiterung des NOA-Konzepts - M+O-Sensoren, NE 183 N2 - Der Sensorik kommt bei der Digitalisierung der Prozessindustrie eine Schlüsselrolle zu. Entsprechend ist sie ein zentraler Baustein der NAMUR Open Architecture Konzepts (NOA). M+O-Sensoren (Monitoring + Optimization) - stellen eine neue Geräteklasse für die zusätzliche Überwachung und Optimierung von Anlagen der Prozessindustrie dar. Diese deckt klassische und alternative Messprinzipien bis hin zur Nachbildung der menschlichen Sinne ab. Hier werden die Anforderungen an M+O-Sensoren als Bestandteile der NOA beschrieben. KW - Prozessanalytik KW - Prozessindustrie KW - Sensoren KW - M+O-Sensoren KW - NAMUR Open Architecture KW - NOA PY - 2021 SN - 978-3-8356-7451-6 SP - 39 EP - 45 PB - Vulkan-Verlag GmbH CY - Essen ET - 1 AN - OPUS4-52912 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Fully integrated and intelligently networked systems and processes - Perspective: Smart sensors, actuators and communication N2 - Companies in the chemical industry have to tread new paths in order to survive successfully in a changed environment. This includes, in particular, the potential of digital technologies. The full integration and intelligent networking of systems and processes is making slow progress. This talk is a tribute to the field level. It wants to encourage a more holistic approach to the digitalisation of the process industry based on smart sensors, actuators and communication and provides information on current technical perspectives, such as the "one-network paradigm", ad-hoc networking, edge computing, FPGAs, virtual machines or blockchain. These give smart sensors, actuators and communication a completely new perspective. T2 - 5th European Conference on Process Analytics and Control Technology - EuroPACT 2021 CY - Online meeting DA - 15.11.2021 KW - Process Analytical Technology KW - Smart Sensors KW - Digital transformation KW - Industry 4.0 KW - EuroPact KW - Distributed Networks PY - 2021 UR - https://dechema.de/europact2021.html AN - OPUS4-53754 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Raman spectroscopy for online monitoring of a homogeneous hydroformylation process in microemulsion N2 - An important industrial reaction is hydro¬formylation for the production of aldehydes from alkenes and syngas on the basis of homogeneous catalysis. The main cost factors of the processes currently used are product selectivity and the loss of the catalysts used. Therefore, various concepts for the hydroformylation of long-chain olefins have been developed, including hydroformylation in microemulsions, which is being investigated on a mini-plant scale at the Technical University of Berlin [1]. In this study, online Raman spectroscopy of the reaction of 1-dodecene to 1-tri¬decanal in a microemulsion was performed [2]. First, an experimental design was used to obtain a good representation of the operating range in the mini plant with respect to the concentrations of five reactants in a laboratory setup [3]. Based on the Raman spectra, Partial Least Squares (PLS) models for the prediction of 1-dodecene and 1-tride-decanal were calibrated and with these the reactions were predicted on a laboratory scale. In the next step, the PLS models were applied to online spectra from a mini-plant. This resulted in promising estimates of 1-tridecanal and acceptable predictions of 1-dodecene mass fractions. The predictive power of PLS models in this particular case was limited by unexpected by-product formation which, however, can easily be compensated by an extended calibration. Hence, Raman spectroscopy is a promising technique for process analysis in microemulsions. T2 - EuroPACT2021 CY - Online meeting DA - 15.11.2021 KW - Raman KW - Process analytics KW - Inline measurement PY - 2021 AN - OPUS4-53767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - NIR-Ringversuch II: Erste Ergebnisse N2 - Vorstellung der Ergebnisse des Ringversuchs NIR II für den Analyten Paracetamol. Neben den "S-Shape" Darstellungen für die Levels A, B und C werden En-Werte und eine Darstellung der relativen Unsicherheiten (Horwitz) gezeigt. Alle beteiligten Labors zeichnen sich durch eine hohe Performance aus. T2 - 15. Ttreffen PAT RFA CY - Lonza, Visp, Switzerland DA - 17.09.2019 KW - Nahinfrarotspektroskopie KW - Ringversuch PY - 2019 AN - OPUS4-49043 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Kessler, R. W. A1 - Kessler, W. A1 - Maiwald, Michael ED - Meyers, R. A. T1 - Inline and Online Process Analytical Technology with a Focus on Optical Spectroscopy N2 - Process analytical technology (PAT) is a cross-sectional technology and thus essential for future smart production. While in the past decades, the focus of process optimization strategies was on increasing efficiency, in the future, the focus will be on the sustainability of a production and its products. In addition, products will be increasingly personalized in order to match the property profile exactly to the intended use. PAT is able to provide context-sensitive information at the molecular level for process control. Spectroscopic sensors can determine inline and simultaneously both the chemical composition and its sub-microscopic morphology. The article will focus on the optical spectroscopy and therefore starts with a brief introduction on the basic concepts of molecular spectroscopy. In addition, the particularities of measuring liquids, surfaces, or particulate systems in PAT applications are described. This should enable the reader to select the appropriate method for the specific problem. Many examples from everyday industrial practice illustrate the applications. The areas covered are the manufacturing industry, process and pharmaceutical industry, food industry, as well as biotechnology and medical technology. Future will show that PAT is especially important for applications in the field of medicine (point of care) circular economy (recycling, water–wastewater, etc.). It is important to emphasize that sustainability in industrial production can only be successful with an inter- and transdisciplinary close exchange between the different disciplines. KW - Process Analytical Technology KW - Optical Spectroscopy KW - Encyclopedia of Analytical Chemistry KW - Sensors KW - Process Industry PY - 2022 SN - 978-0-47002-731-8 DO - https://doi.org/10.1002/9780470027318.a9791 SP - 1 EP - 31 PB - JohnWiley & Sons, Ltd. AN - OPUS4-56688 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Vogel, Kristin T1 - Berechnung und Nutzung von Unsicherheiten zertifizierter Werte von Referenzmaterialien N2 - Referenzmaterialien sind entscheidend für die Qualitätssicherung von Laboratorien. Diese nutzen Referenzmaterialien unter anderem zur Validierung von Messverfahren und zur Kalibrierung von Geräten. Dabei ist zu beachten, dass zertifizierte Merkmalswerte stets eine gewisse Unsicherheit aufweisen. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Artikels. Des Weiteren wird ein Vorgehen beschrieben, wie die Unsicherheit von Messverfahren mit Hilfe eines Referenzmaterials bestimmt werden kann. KW - Referenzmaterial KW - Messunsicherheit KW - Qualitätskontrolle PY - 2024 DO - https://doi.org/10.1515/teme-2024-0025 SN - 0171-8096 SP - 1 EP - 7 PB - De Gruyter AN - OPUS4-60564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mangoufis-Giasin, I. A1 - Piqué, O. A1 - Khanipour, Peyman A1 - Mayrhofer, K. J. J. A1 - Calle-Vallejo, F. A1 - Katsounaros, I. T1 - Different promoting roles of ruthenium for the oxidation of primary and secondary alcohols on PtRu electrocatalysts N2 - This study shows remarkably different features between the oxidation of secondary and primary C₃-C₅ alcohols. The oxidation of primary alcohols is controlled by the oxidative removal of blocking adsorbates, such as CO, formed after the dissociative adsorption of alcohol molecules. Conversely, secondary alcohols do not undergo dissociative adsorption and therefore their oxidation is purely controlled by the energetics of the elementary reaction steps. In this respect, a different role of ruthenium is revealed for the electrooxidation of primary and secondary alcohols on bimetallic platinum-ruthenium catalysts. Ruthenium enhances the oxidation of primary alcohols via the established bifunctional mechanism, in which the adsorption of (hydr)oxide species that are necessary to remove the blocking adsorbates is favored. In contrast, the oxidation of secondary alcohols is enhanced by the Ru-assisted stabilization of an O-bound intermediate that is involved in the potential-limiting step. This alternative pathway enables the oxidation of secondary alcohols close to the equilibrium potential. KW - Electrocatalysis KW - Electrochemical energy conversion KW - Direct alcohol fuel cells KW - Alcohol electrooxidation KW - Secondary alcohols KW - 2-propanol oxidation KW - Electrochemical real-time mass spectrometry KW - Density functional theory PY - 2021 DO - https://doi.org/10.1016/j.jcat.2021.05.028 SN - 0021-9517 VL - 400 SP - 166 EP - 172 PB - Elsevier CY - San Diego, Calif. AN - OPUS4-56999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Multi-element analysis in different matrices using nitrogen microwave inductively coupled atmospheric pressure plasma mass spectrometry (MICAP-MS) N2 - Inductively coupled plasma mass spectrometry (ICP-MS) emerged as a powerful technique for trace analysis of soil due to its multi-element capability, high sensitivity and low sample consumption. However, despite its success and widespread use, ICP-MS has several persistent drawbacks, such as high argon gas consumption, argon-based polyatomic interferences and the need for complicated RF-power generators. Unlike argon-based ICP, the nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) uses nitrogen as plasma gas, which eliminates high operating costs associated with argon-gas consumption as well as the argon-based interferences1. In this work, the applicability of MICAP-MS for elemental analysis in different matrices is investigated. For this purpose, reference soil samples and steel samples are digested with aqua regia and used for analysis. Concentrations of selected elements are determined using MICAP-MS and validated with ICP-MS und certified values. Sensitivities, limits of detection and gas consumption for both methods are compared and discussed in detail. Performance of MICAP-MS under different nitrogen plasma gas concentrations is investigated and compared. Moreover, the performance of MICAP-MS in alloy matrices is investigated and discussed. T2 - EWCPS 2023 CY - Ljubljana, Slovenia DA - 29.01.2023 KW - Microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) KW - Multi-element analysis KW - Soil KW - Steel KW - Nitrogen plasma PY - 2023 AN - OPUS4-56994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Laser spectroscopy methods for calcium isotope analysis N2 - Calcium isotope analysis can be an important tool for paleoclimate studies of the carbon cycle, as well in carbon capture technology, but its utility is limited by challenges using conventional mass spectrometry. We propose a new fast, precise, and high-throughput technology based on multiple complementary high-resolution spectroscopies analyzed by machine-learning. T2 - Seminars Chemical Physics Caltech CY - Pasadena, CA, USA DA - 13.04.2022 KW - Calcium KW - Atomic spectroscopy KW - CaF KW - Calcium monofluoride KW - Carbon cycle KW - Doppler effect KW - Sub-doppler spectroscopy KW - Laser spectroscopy PY - 2022 AN - OPUS4-56499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - On developments of continuum source atomic and molecular absorption spectrometry N2 - Der Bunsen-Kirchhoff-Preis 2022 wurde am 23.06.2022 anlässlich der analytica conference in München an Dr. Carlos Abad verliehen - in Anerkennung seiner exzellenten Entwicklungen im Bereich der continuum source atomic absorption spectrometry (CS-AAS). Dr. Carlos Abad ist ein herausragender Experte auf dem Gebiet der Atom- und molekularen Absorptionsspektrometrie. insbesondere trug er maßgeblich zur substanziellen Weiterentwicklung von Echelle-Spektrometern für die CS-AAS bei. So gelang es, einen quantitativen Zugang zu Elementen wie Bor, Chlor, Fluor und Schwefel, mittels AAS zu erreichen. Erstmals demonstriert Dr. Carlos Abad am Beispiel eines Zr-Modifier, dass durch die Zeitauflösung der eingesetzten Echelle-Systeme mechanistische Untersuchungen zur Wirkung des Modifiers im Graphitrohrofen möglich sind. Besonders hervorzuheben sind seine Arbeiten zum Einsatz der CS-AAS für die Analyse von Isotopen, die eine Genauigkeit aufweist, welche an die der Multikollektor-induktiv gekoppelten Plasma-Massenspektrometrie (MC-ICP-MS) heranreicht. Damit ergeben sich völlig neue Einsatzmöglichkeiten für technologisch hochrelevante Applikationen, wie z.B. die Untersuchung der Alterung von Lithium-Batterien oder die Lithium-Analyse in Blutserum. T2 - Analytica Conference: Bunsen-Kirchhoff-Preis 2022 der Deutsche Arbeitskreis für Analytische Spektroskopie (DAAS) CY - Munich, Germany DA - 23.06.2022 KW - Isotopes KW - Fluorine KW - Halogens KW - Non-metals KW - HR-CS-MAS KW - HR-CS-AAS KW - Bunsen-Kirchhoff-Preis KW - Continuum source atomic absorption spectrometry KW - Zr-Modifier KW - Graphite furnace KW - Lithium PY - 2022 AN - OPUS4-56500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Optical spectrometry for isotope analysis N2 - Isotope analysis is a tool for material research. For example, it may provide information about the provenance of a sample or changes in dynamic systems. Here is presented optical spectroscopy as an analytical alternative to mass spectrometry for isotope quantification based on the isotopic shift of atoms and diatomic molecules. T2 - Isotopic Tools for the Investigation of Materials WS 21/22 CY - Leoben, Austria DA - 01.10.2021 KW - Isotopes KW - HR-CS-AAS KW - Lithium KW - Atomic absorption spectrometry KW - Diatomic molecules PY - 2022 AN - OPUS4-56495 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fricke, F. A1 - Mahmood, S. A1 - Hoffmann, J. A1 - Brandalero, M. A1 - Liehr, Sascha A1 - Kern, Simon A1 - Meyer, Klas A1 - Kowarik, S. A1 - Westerdick, S. A1 - Maiwald, Michael A1 - Hübner, M. T1 - Artificial Intelligence for Mass Spectrometry and Nuclear Magnetic Resonance Spectroscopy N2 - Mass Spectrometry (MS) and Nuclear Magnetic Resonance Spectroscopy (NMR) are critical components of every industrial chemical process as they provide information on the concentrations of individual compounds and by-products. These processes are carried out manually and by a specialist, which takes a substantial amount of time and prevents their utilization for real-time closed-loop process control. This paper presents recent advances from two projects that use Artificial Neural Networks (ANNs) to address the challenges of automation and performance-efficient realizations of MS and NMR. In the first part, a complete toolchain has been developed to develop simulated spectra and train ANNs to identify compounds in MS. In the second part, a limited number of experimental NMR spectra have been augmented by simulated spectra to train an ANN with better prediction performance and speed than state-of-theart analysis. These results suggest that, in the context of the digital transformation of the process industry, we are now on the threshold of a possible strongly simplified use of MS and MRS and the accompanying data evaluation by machine-supported procedures, and can utilize both methods much wider for reaction and process monitoring or quality control. T2 - 2021 Design, Automation & Test in Europe Conference & Exhibition (DATE) CY - Grenoble, France DA - 01.02.2021 KW - Industry 4.0, KW - Cyber-physical systems KW - Artificial neural networks KW - Mass spectrometry KW - Nuclear magnetic resonance spectroscopy PY - 2021 DO - https://doi.org/10.23919/DATE51398.2021.9473958 SP - 615 EP - 620 PB - IEEE AN - OPUS4-55360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Integrierte und vernetzte Systeme und Prozesse – Eine Perspektive für das Messen in der Prozessindustrie N2 - Anhand von Beispielen wird in diesem Vortrag ein möglicher ganzheitlicherer Ansatz für die Digitalisierung und den Einsatz maschinengestützter Prozesse bei der Herstellung von Spezialchemikalien und Arzneimitteln durch die Einführung integrierter und vernetzter Systeme und Prozesse skizziert. Ein aktueller Ansatz und ein Beispiel in diesem Vortrag sind flexible und modulare chemische Produktionseinheiten, die Mehrzweckanlagen nutzen, um verschiedene hochwertige Produkte mit kurzen Stillstandszeiten zwischen den Kampagnen herzustellen und die Markteinführungszeit für neue Produkte zu verkürzen. Als zweites Beispiel wird kurz die Testplattform Wasserstofftankstelle vorgestellt, die als moderne Anlage der Prozessindustrie betrachtet werden kann, vergleichbar mit einer Anlage aus der chemischen oder pharmazeutischen Industrie. An ihr lassen sich alle derzeit entlang der Digitalen Transformation diskutierten Konzepte implementieren, um sie zu standardisieren und zu validieren. Dazu gehören Konzepte zur Konnektivität von Sensoren und Aktoren aus der Feldebene in höhere Ebenen der Automatisierung oder zur Einbringung zusätzlicher Sensoren oder Sensornetzwerke, die zunehmend flexibler gestaltet werden soll, die sichere und nachvollziehbare Parametrierung von Automatisierungskomponenten – vielleicht aus einem digitalen Abbild (Verwaltungsschale bzw. „Digitaler Zwilling“) heraus, Konzepte zur vorausschauenden Wartung („Predictive Maintenance“), Konzepte zu digitalen Entscheidungsprozessen, Zertifikaten und Signaturen oder der zunehmende Einsatz von komplexen Auswertungsalgorithmen und Applikationen in der Feldebene („Embedded Computing“) oder der „Kante“ zu Cloudbasierten Systemen der Informationstechnik („Edge-Computing“). Die beiden Beispiele sollen aktuelle Entwicklungsachsen des industriellen Messwesens im Rahmen der industriellen Automation aufzeigen, in denen Messwerte, deren Messunsicherheiten und Kontextinformationen eine wichtige Rolle einnehmen. T2 - 324. PTB-Seminar: Berechnung der Messunsicherheit – Empfehlungen für die Praxis CY - Berlin, Germany DA - 22.05.2023 KW - Messunsicherheit KW - Prozessindustrie KW - Datenerfassung KW - QI-Digital KW - Online-NMR-Spektroskopie PY - 2023 UR - https://www.ptb.de/cms/de/ptb/fachabteilungen/abt8/fb-84/ag-842/seminare/324-ptb-seminar-berechnung-der-messunsicherheit-empfehlungen-fuer-die-praxis.html AN - OPUS4-57533 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Modular process control with compact NMR spectroscopy – From field integration to automated data analysis N2 - Chemical and pharmaceutical companies have to find new paths to survive successfully in a changing environment, while also finding more flexible ways of product and process development to bring their products to market more quickly – especially high-quality high-end products like fine chemicals or pharmaceuticals. A current approach uses flexible and modular chemical production units, which can produce different high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce the time to market of new products. NMR spectroscopy appeared as excellent online analytical tool and allowed a modular data analysis approach, which even served as reliable reference method for further Process Analytical Technology (PAT) applications. Using the available datasets, a second data analysis approach based on artificial neural networks (ANN) was evaluated. Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously. In future, such fully integrated and interconnecting “smart” systems and processes can increase the efficiency of the production of specialty chemicals and pharmaceuticals. T2 - GIDRM Day (Gruppo Italiano Discussione Risonanze Magnetiche) - Data analysis and NMR: from fundamental aspects to health and material applications CY - Online meeting DA - 14.10.2022 KW - Process Control KW - Online NMR Spectroscopy KW - Industry 4.0 KW - Process Analytical Technology KW - Data Analysis KW - Machine-Assisted Workflows PY - 2022 DO - https://doi.org/http://www.gidrm.org/index.php/activities/workshops/2022-workshops/gidrm-day-data-analysis-and-nmr-from-fundamental-aspects-to-health-and-material-applications AN - OPUS4-56002 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Modular process control with compact NMR spectroscopy: From field integration to fully automated data analysis N2 - Chemical and pharmaceutical companies need to find new ways to survive successfully in a changing environment, while finding more flexible ways of product and process development to bring their products to market faster - especially high-value, high-end products such as fine chemicals or pharmaceuticals. This is complicated by changes in value chains along a potential circular economy. One current approach is flexible and modular chemical production units that use multi-purpose equipment to produce various high-value products with short downtimes between campaigns and can shorten time-to-market for new products. Online NMR spectroscopy will play an important role for plant automation and quality control, as the method brings very high linearity, matrix independence and thus works almost calibration-free. Moreover, these properties ideally enable automated and machine-aided data analysis for the above-mentioned applications. Using examples, this presentation will outline a possible more holistic approach to digitalization and the use of machine-based processes in the production of specialty chemicals and pharmaceuticals through the introduction of integrated and networked systems and processes. T2 - Benchtop NMR: From Academia to Industry CY - Online meeting DA - 28.09.2022 KW - Digital Transformatioin KW - Process Industry KW - Benchtop NMR Spectroscopy KW - Procee Analytical Technology KW - Modular Production KW - Specialty Chemicals KW - Industry 4.0 PY - 2022 UR - https://eventos.fct.unl.pt/benchtop_nmr_workshop2022/pages/welcome AN - OPUS4-55850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin T1 - Modular production involving benchtop NMR - Current Application Examples Driven by Digitalization N2 - The demand for increasing product diversity in the chemical and pharmaceutical industry calls for new production processes that enable greater flexibility. Therefore, plants are needed which can be adapted to new processes in a fast manner and be scaled up and down easily to volatile market demands. Modular production techniques in combination with advanced process analytical technology (PAT) are considered as a promising solution able to fulfil these requirements. The success and acceptance of modular concepts in both new and existing plants is dependent of its reliability, easy applicability, and standardization. In recent past, enormous efforts were made to overcome existing barriers in a superordinate level, e.g. DEXPI, ENPRO, or MTP naming just a few. Here, we’d like to present a few, more hands-on, application examples which are shown in Figure 1 aiming to increase process flexibility and applicability. T2 - ProcessNET Jahrestagung 2022 Aachen CY - Aachen, Germany DA - 12.09.2022 KW - Process analytical technology KW - NMR spectroscopy KW - Digitization KW - Additive manufacturing PY - 2022 AN - OPUS4-55975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Benchtop NMR spectroscopy in chemical manufacturing: From hardware field integration to data modeling N2 - The use of benchtop-NMR instruments is constantly increasing during the recent years. Advantages of being affordable, portable and easy-to-operate without the need for trained staff make them especially interesting for industrial applications in quality control. However, applications of NMR spectroscopy as an online PAT tool are still very rare but offer a huge potential for process optimization and control. A key task to exploit this potential is hardware field integration of the lab-instruments in a rough environment of a chemical plant. Additionally, developments in automation and data evaluation are mandatory to ensure a robust unattended operation with low maintenance requirements. Here, we show an approach of a fully automated analyzer enclosure considering explosion safety, field communication, as well as environmental conditions in the field. Temperature sensitivity is still a limitation of benchtop-NMR instruments in flow applications. Recent developments of manufacturers allow for limited operation at static temperature levels, however, a dynamic system for continuous operation is still not available. Using a prototype system offering a larger bore, active temperature shielding studies with thermostated air were performed evaluating the performance. Automated data evaluation of NMR spectra using a modular indirect hard modeling (IHM) approach showed good results and flexibility. A second data analysis approach based on artificial neural networks (ANN) was evaluated.Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously, offering new ways to simultaneously evaluating large numbers of different models. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 24.05.2023 KW - Field integration KW - Benchtop-NMR KW - Process Analytical Technology PY - 2023 AN - OPUS4-57560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin T1 - Modular production involving benchtop NMR Current Application Examples Driven by Digitalization N2 - The demand for increasing product diversity in the chemical and pharmaceutical industry calls for new production processes that enable greater flexibility. Therefore, plants are needed which can be adapted to new processes in a fast manner and be scaled up and down easily to volatile market demands. Modular production techniques in combination with advanced process analytical technology (PAT) are considered as a promising solution able to fulfil these requirements. The success and acceptance of modular concepts in both new and existing plants is dependent of its reliability, easy applicability, and standardization. In recent past, enormous efforts were made to overcome existing barriers in a superordinate level, e.g. DEXPI, ENPRO, or MTP naming just a few. Here, we’d like to present a few, more hands-on, application examples which are shown in Figure 1 aiming to increase process flexibility and applicability. T2 - Achema 2022 CY - Frankfurt a.M., Germany DA - 22.08.2022 KW - Process analytical technology KW - NMR spectroscopy KW - Digitization PY - 2022 AN - OPUS4-55974 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Anwendung von hochauflösender optischer Spektrometrie zur Lithium-Isotopenanalyse N2 - Optische Spektrometrie wird als Alternative zur Massenspektrometrie im Bereich der Lithium-Isotopenanalyse vorgestellt. T2 - 11. Analytische Tage CY - Idstein, Germany DA - 11.05.2023 KW - Lithium KW - Isotopenanalyse KW - Atomabsorptionsspektrometrie KW - Massenspektrometrie PY - 2023 AN - OPUS4-57543 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Compact NMR spectroscopy: A versatile tool for automated continuous-flow production of chemicals and pharmaceuticals N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - GDCh-Seminar der Universität Bielefeld CY - Bielefeld, Germany DA - 17.01.2019 KW - Process analytical technology KW - Process industry KW - Online NMR spectroscopy KW - Indirect hard modeling KW - CONSENS KW - Fresenius lecture PY - 2019 AN - OPUS4-47221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Compact NMR Spectroscopy: A Versatile Tool for Automated Continuous-Flow Production of Chemicals and Pharmaceuticals N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - Seminar of Research Department „Life, Light & Matter“ of the InterdisciplinaryFaculty of the University of Rostock CY - Rostock, Germany DA - 08.01.2019 KW - Process Analytical Technology KW - Low-field NMR Spectroscopy KW - Online NMR Spectroscopy KW - Modular Production KW - Process Industry KW - Fresenius Lecture PY - 2019 AN - OPUS4-47166 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Low-field NMR spectroscopy: Applications in chemical and pharmaceutical process development N2 - Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. The talk also generally covers current aspects of high-field and low-field online NMR spectroscopy for reaction monitoring and process control and gives also an overview on direct dissolution studies of API cocrystals. T2 - Discussion Meeting Pharmaceutical Development Bayer AG Wuppertal CY - Wuppertal, Germany DA - 15.01.2019 KW - Process analytical technology KW - Low-field NMR spectroscopy KW - Online NMR spectroscopy KW - Cocrystals KW - Dissolution KW - CONSENS PY - 2019 AN - OPUS4-47201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Compact NMR spectroscopy: A versatile tool for automated continuous-flow production of chemicals and pharmaceuticals N2 - Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. T2 - Process Development Seminar Bayer AG Dormagen CY - Dormagen, Germany DA - 14.01.2019 KW - Process analytical technology KW - Low-field NMR spectroscopy KW - Online NMR spectroscopy KW - CONSENS PY - 2019 AN - OPUS4-47197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Compact NMR Spectroscopy: A Versatile Tool for Automated Continuous-Flow Production of Chemicals and Pharmaceuticals N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - 2nd Reaction Monitoring Symposium, University of Bath CY - Bath, United Kingdom DA - 28.01.2019 KW - Process Analytical Technology KW - Process Industry KW - Online NMR Spectroscopy KW - CONSENS PY - 2019 AN - OPUS4-47271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - How online NMR spectroscopy accelerates chemical process development and manufacturing – From automated spectral analysis to integrated NMR micro reactors N2 - Accelerating chemical process development and manufacturing along with quick adaption to changing customer needs means consequent transformation of former batch to continuous (modular) manufacturing processes. These are justified by an improved process control through smaller volumes, better heat transfer, and faster dynamics of the examined reaction systems. As an example, for such modular process units we present the design and validation of an integrated nuclear magnetic resonance (NMR) micro mixer tailor‐made for a desired chemical reaction based on computational modelling. The micro mixer represents an integrated modular production unit as an example for the most important class of continuous reactors. The quantitative online NMR sensor represents a smart process analytical field device providing rapid and non‐invasive chemical composition information without need for calibration. We describe the custom design through computational fluid dynamics (CFD) for the demands of the NMR sensor as well as for the given reaction conditions. The system was validated with an esterification reaction as an example for a chemical reaction process. Systems utilizing such an online NMR analyser benefits through short development and set‐up times based on “modular” spectral models. Such models can simply be built upon pure component NMR spectra within minutes to a few hours (i.e., assignment of the NMR signals to the components) instead of tedious DoE calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). The approach was validated for typical industrial reactions, such as hydrogenations or lithiations. This work wants to show the benefit of NMR spectroscopy as online analytical technique in industrial applications for improving process understanding and efficiency. Especially development and set‐up times based on “modular” data analysis models will enable new production concepts, which are currently discussed with respect to digitization of process industry. PANIC is the ideal forum for such discussions in the application of NMR spectroscopy and its data analysis to the everyday problems in process industry. T2 - Practical Applicatiions of NMR in Industry Conference (PANIC) 2019 CY - Hilton Head Island, USA DA - 04.03.2019 KW - Process Analytical Technology KW - Reaction Monitoring KW - Online NMR Spectroscopy KW - Micro Reactor KW - Data Analysis KW - PANIC PY - 2019 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-47488 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Accelerating chemical process development and manufacturing by online NMR spectroscopy N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - Symposium: Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) 2019 CY - Kaiserslautern, Germany DA - 31.01.2019 KW - Process Analytical Technology KW - Process Industry KW - Online NMR Spectroscopy KW - Data Analysis KW - Digitization KW - CONSENS PY - 2019 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-47297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas A1 - Maiwald, Michael T1 - NMR Validation - Measurement Uncertainty N2 - There is a need within the NMR community to progress forward in exploring new facets in which we can use analytical techniques to advance our understanding of various systems. One aspect the NMR community hasn’t fully encompassed is the validation process, which also involves setting reference standards, establishing a common language that directly relates to NMR, communication relating to validation, and much more. This workshopcontribution starts with an overview on international metrology for qNMR spectroscopy. Since NMR is completely described by mathematical equations, the measurement unceartainty can directly be dreived from formula. Examples are presented. These are differentiated between type A and B evaluations. Finally the Expanded Unceartainty is defined. Since the user needs a risk-based unceartainty assessment, different "leagues" for routine, advanced, and high level needs are proposed to make clear, that no all sources of uncertainty have to be taken in considerention at practical levels. T2 - Practical Applications of NMR in Industry Conference (PANIC) 2019 - Validation Workshop CY - Hilton Head Island, USA DA - 04.03.2019 KW - Quantitative NMR Spectroscopy KW - qNMR KW - Uncertainty Evaluation KW - Weighing Uncertainty KW - NMR Method Validation PY - 2019 AN - OPUS4-47509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bernstein, Michael A1 - Diehl, Bernd W. K. A1 - Holzgrabe, Ulrike A1 - Maiwald, Michael A1 - Meyer, Klas A1 - Monakhova, Yulia A1 - Schönberger, Torsten T1 - qNMR - The handbook N2 - Quantitative NMR (qNMR) has been around for a long time, but also has great potential to solve future problems in any quantitative analysis. As a primary method, it differs fundamentally from chromatographic methods: it is better described as a quantum mechanical balance. Succesful implementation of qNMR requires certain attention to detail. "qNMR - the handbook" is intended to be a guide for analysts to help understand the fundamental principles of NMR and the significant points relating to its implementation for quantitation. Regulatory considerations of qNMR adoption are explained. NMR fundamentals are explained to provide understanding. Together with many useful examples, the book is a compelling addition to the laboratory's reference library, providing all the tools that any practitioner should know to successfully implement qNMR. The authors are qNMR pioneers and come from a variety of backgrounds including business, government and academia. KW - Quantitative NMR spectroscopy KW - NMR spectroscopy KW - Handbook KW - qNMR PY - 2023 SN - 978-3-7568-7891-8 SN - 978-3-7583-8050-1 SP - 1 EP - 302 PB - BoD – Books on Demand CY - Norderstedt AN - OPUS4-59839 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Die Digitalisierung der Prozessindustrie – Voll integrierte und intelligent vernetzte Sensoren und Prozesse für die kontinuierliche Produktion von Chemikalien und Pharmazeutika N2 - Um in einem veränderten Umfeld erfolgreich bestehen zu können, müssen Chemie-unternehmen neue Pfade beschreiten. Dazu gehört insbesondere das Potential digi-taler Technologien. Mit flexiblen, modularen chemischen Vielzweck-Produktionsanlagen lassen sich häufig wechselnde Produkte mit kürzeren Vorlauf- und Stillstandzeiten zwischen den Kampagnen und dennoch hoher Qualität realisie-ren. Intensivierte, kontinuierliche Produktionsanlagen erlauben auch den Umgang mit schwierig zu handhabenden Substanzen. Grundvoraussetzung für solche Konzepte ist eine hochautomatisierte "chemische" Prozesskontrolle zusammen mit Echtzeit-Qualitätskotrolle, die "chemische" Informati-onen über den Prozess bereitstellt. In einem Anwendungsbeispiel wurde eine phar-mazeutische Lithiierungsreaktion aus einer modularen Pilot-Anlage betrachtet und dabei die Vorzüge eines vollautomatischen NMR-Sensors untersucht. Dazu wurde ein kommerziell erhältliches Benchtop-NMR-Spektrometer mit Permanentmagnet auf die industriellen Anforderungen, wie Explosionsschutz, Feldkommunikation und voll-automatischer, robuster Datenauswertung angepasst. Der NMR-Sensor konnte schließlich erfolgreich im vollautomatischen Betrieb nach fortschrittlichen Regelkon-zepten und für die Echtzeitoptimierung der Anlage getestet werden. Die NMR-Spektroskopie erwies sich als hervorragende Online-Methode und konnte zusammen mit einer modularen Datenauswertung sehr flexibel genutzt werden. Die Methode konnte überdies als zuverlässige Referenzmethode zur Kalibrierung konventioneller Online-Analytik eingesetzt werden. Zukünftig werden voll integrierte und intelligent vernetzte "smarte" Sensoren und Pro-zesse eine kontinuierliche Produktion von Chemikalien und Pharmazeutika mit ver-tretbaren Qualitätskosten möglich machen. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Digitalisierung KW - Datenauswertung KW - Digitaler Zwilling KW - Prozessindustrie KW - Prozessanalytik PY - 2019 AN - OPUS4-47650 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Quantitative NMR-Spektroskopie – Eine unverzichtbare Methode für die Analytische Chemie N2 - Die NMR-Spektroskopie stellt heutzutage eine der wichtigsten Analysenmethoden in der organischen Chemie dar. Während der Großteil aller Untersuchungen qualitativ mit dem Ziel der Stoffidentifikation und Strukturaufklärung erfolgt, erlangt die quantitative NMR-Spektroskopie (qNMR) zunehmend an Bedeutung in Forschung und Industrie. Der entscheidende Vorteil gegenüber anderen Analysenmethoden liegt in der direkten Proportionalität der Signalfläche zur Anzahl Kernspins im Messvolumen. Dies erlaubt eine kalibrationsfreie Relativquantifizierung. Zur Absolutquantifizierung reicht die Zugabe einer definierten Menge eines vom Analyten unabhängigen NMR-Standards aus. Trotz dieser Vorteile findet sich die qNMR bislang nur vereinzelt in Normen und Standardverfahren wieder. Zahlreiche Ringversuche in Metrologie und Industrie demonstrieren die Leistungsfähigkeit moderner NMR-Spektrometer und stärken das Vertrauen in die Methode. Die Entwicklung von Validierungskonzepten, sowie die kommerzielle Verfügbarkeit geeigneter zertifizierter Referenzmaterialien erleichtern die Anwendung, insbesondere im zumeist stark regulierten industriellen Umfeld. Neben etablierten Hochfeld-NMR Spektrometern hat sich in den letzten Jahren ein stark wachsender Markt für kompakte Benchtop-NMR Geräte auf Permanentmagnetbasis entwickelt. Die geringeren Anschaffungs- und Betriebskosten, sowie die einfache Bedienbarkeit erlaubt es auch kleineren Unternehmen in diese Analysenmethode einzusteigen. Weiterhin besteht die Möglichkeit diese mobilen Systeme näher an die Produktion zu bringen, welches von der klassischen Qualitätskontrolle bis hin zur Online-Prozesskontrolle als vollautomatisierter Analysator reicht. Die geringere Feldstärke der Systeme erfordert hier oft den Einsatz modellbasierter Ansätze zur Spektrenauswertung (z.B. Indirect Hard Modeling). Dieser Beitrag gibt eine Übersicht über aktuelle Anwendungen und Entwicklungen der qNMR von der universellen, hochgenauen Labormethode bis hin zur robusten Anwendung als Online-Analysator im Feld. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - qNMR KW - NMR Spektroskopie KW - Messunsicherheit PY - 2019 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-47661 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Hybridmodell zur Bestimmung des Ligningehalts von Kiefernholz N2 - Die Untersuchungen sind durch das das DFG Schwerpunktprogramm 1374 für Biodiversitätsforschung motiviert. Anhand des überwachten Abbaus von Totholz soll untersucht werden, welche Auswirkung unterschiedliche Formen und Intensitäten der Landnutzung auf die Biodiversität innerhalb von drei Exploratorien zeigen. Bei den vorangegangenen Studien wurden Nahrungs¬netzte auf organismischer Ebene sowie Klima- und Umgebungsdaten untersucht und die Veränderung des ausgebrachten Totholzes als Masseverlust erfasst. Es wird jedoch erwartet, dass in Anhängigkeit der beteiligten Organismen und Umgebungsparameter verschiedene Mechanismen des Holzabbaus vorliegen, die in unterschiedlichen Abbauraten der Holzkomponenten Lignin, Cellulose und Hemicellulose resultieren. Aus diesem Grund ist die quantitative Untersuchung des Ligningehalts an Hölzern ein wesentlicher Schritt für ein verbessertes Verständnis der Biodiversität in den untersuchten Exploratorien. Um der hohen Probenanzahl, die sich aus der Kontrolle von jeweils 100 Proben (Plots) in den drei Exploratorien für Hölzer aus 13 Baumarten ergibt, gerecht zu werden, wird eine schnelle und effiziente Untersuchungsmethode benötigt. Diese wird derzeit in Form einer NIR-spektroskopischen Bestimmung des Ligningehalts entwickelt. Um basierend auf den NIR Spektren vermahlener Holzproben Lignin und weitere Holzkomponenten korrekt vorherzusagen, muss zunächst basierend auf nasschemischen Analysen ein chemometrisches Modell kalibriert werden. Dazu ist die Charakterisierung von mindestens 20 – 30 Proben, die eine hohe Varianz des Ligningehalts aufweisen, notwendig. Im Vortrag werden erste Untersuchungs¬ergebnisse für die Vorhersage des Ligningehalts von Kiefernhölzern, die für ein Jahr in dem Exploratorium Schorfheide exponiert wurden, vorgestellt. Die anschließende explorative Datenanalyse (PCA) unter Verwendung von insgesamt 28 Variablen zur Beschreibung klimatischer und Umgebungsparameter weist eine Reihe interessanter Korrelationen auf. Demnach ist der Ligningehalt auf der ersten Hauptkomponente (29% erklärte Varianz) positiv mit dem C/N-Verhältnis und negativ mit Landnutzungsindex korreliert. Masseverlust und Temperatur hingegen dominieren die zweite Hauptkomponente (12% erklärte Varianz). T2 - 4. Innovationsakademie Lignocellulose CY - Berlin, Germany DA - 11.04.2019 KW - NIR Spektroskopie KW - Lignin KW - Datenanalyse PY - 2019 AN - OPUS4-47963 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas T1 - NMR-Spektroskopie als Online-Referenzmethode in der Prozessindustrie N2 - In der Prozessindustrie findet die optische Spektroskopie (z. B. NIR- und Raman-Spektroskopie) als Online-Analytik zunehmend Anwendung zur Überwachung che-mischer Qualitäts¬attribute in der Produktion. Ihr ganzes Potential entfalten die Methoden aber meist nur in Kombination mit einer aufwendigen, multivariaten Kalibrierung. Diese muss alle relevanten Zustände des Systems abdecken und bedarf einer geeigneten Referenz¬analytik. Moderne instrumentelle Analysengeräte weisen eine hohe Empfind¬lich¬keit und Robustheit auf, sind aber dennoch stark von Fehler und Variabilität der Probennahme beeinflusst, was sich auf die Richtigkeit und Qualität des multivariaten Modells auswirkt. Diese Probleme lassen sich verringern, indem die Referenzanalytik ebenfalls online erfolgt. Eine mögliche Lösung stellt die hochauflösende NMR-Spektroskopie als quanti¬tative Online-Referenzanalytik dar. Insbesondere kom¬pakte NMR-Spektrometer auf Basis von Permanent¬magneten sind für diesen Zweck geeignet. Ausschlusskriterien für herkömmlicher NMR-Systeme, wie der große Wartungs-aufwand (Kryotechnik) und der Platz¬bedarf, werden damit vermieden. Im Rahmen des EU-Projekts CONSENS wurde die Nutzung einer Online-Referenz¬analytik mit NMR-Spektroskopie am Beispiel einer industriellen Pilotanlage erfolgreich realisiert. Untersuchungsgegenstand war die kontinuierliche Synthese eines Aus¬gangsstoffs für die pharmazeutische Industrie. Die enthaltenen metallorganischen Verbindungen sind für die bisher genutzte HPLC Analytik unzu-gänglich und die Analyse ausgewählter Proben erfolgte nach dem Quenchen der Lösung oft mit einem großen zeitlichen Abstand zur Probennahme. Konzen-trationswerte auf Basis von Online-NMR-Spektren standen hingegen mit einer zeitlichen Auflösung von drei Spektren pro Minute über den gesamten Reaktionsverlauf hinweg zur Verfügung. Außerdem konnten durch die NMR-Spektroskopie intermediär auftretende Spezies erstmal quantitativ bestimmt und diese Daten für die Kalibrierung eines NIR-Spektrometers genutzt werden. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - NMR-Spektroskopie KW - Prozessanalytik KW - Online-Referenzmethode PY - 2019 AN - OPUS4-47659 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas T1 - Gips – ein unterschätztes Material N2 - Früh- bis spätmittelalterliche Stuckausstattungen bilden ein regionales, da an Gips-vorkommen korreliertes kunsttechnologisches Spezifikum. Aufgrund der beschränkten Kontrollmöglichkeiten über die in einem Meiler oder Feldofen herrschenden Parameter charakterisiert mittelalterliche Hochbrandgipse ein Phasengemisch aus Calciumsulfat-Hydratstufen und thermisch mehr oder weniger stark geschädigten Nebenbestandteilen aus der Gipslagerstätte. Die Analyse mittelalterlicher Hochbrandgipse erfordert die genaue Kenntnis der Bildungs- und Stabilitätsbereiche der Phasen im System CaSO4–H2O. Gips CaSO4 x 2 H2O entwässert beim Brennen über Halbhydrat CaSO4 x 0.5 H2O zu Anhydrit III CaSO4, welches schließlich in den für mittelalterliche Hochbrandgipse relevanten Anhydrit II (AII) übergeht. Für diesen wurden aufgrund der Abbindeeigenschaften drei bis vor kurzem nicht spektroskopisch unterscheidbare Sub-Phasen postuliert: Anhydrit II schwerlöslich (300-500°C, AII-s), unlöslich (500-700°C, AII-u) und Estrichgips (> 700°C, AII-E). Anhydrit I ist nur über 1180°C stabil. Mittels strukturanalytischer Methoden wie Röntgenbeugung (XRD) und Raman-Spektroskopie lassen sich nur die verschiedenen Hydratstufen sowie AIII, AII und AI eindeutig aufgrund unterschiedlicher Kristallstrukturen identifizieren. Ein neues auf Raman-mikrospektroskopischer Bildgebung basierendes Verfahren ermöglicht den Nachweis verschiedener Brenntemperaturen aufgrund der Auswertung von Raman-Bandenbreiten von AII, welche ein Maß für die mit steigender Brenntemperatur zunehmende Kristallinität der Anhydritkörner sind. Die Anwendung dieser Methode sowie der Nachweis pyrometamorpher Umwandlun-gen von Begleitmineralien aus dem Gipsstein als Mineralthermometer zur Bestimmung von Brenntemperaturen wird anhand von Proben früh- und spätmittelalterlicher Skulpturen und Stuckdekorationen aus Südtirol diskutiert. Außerdem wird gezeigt, wie die Analyse solch komplexer Materialien Rückkopplungen in die Analytische Chemie erzeugen kann, da zur erfolgreichen Analytik eine Möglichkeit zur reproduzierbaren Bestimmung von Ramanbandenbreiten und der Korrektur instrumentenabhängiger Verbreiterung gefunden und optimiert werden musste. Damit sollten überzeugende Belege dafür erbracht werden können, dass die Komplexität des monomineralischen Bindemittels Gips bezüglich der je nach Brandbedingungen unterschiedlichen Eigenschaften und insbesondere bezüglich der Herausforderungen an die Analytische Chemie häufig unterschätzt wird. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Gips KW - Anhydrit KW - Ramanspektroskopie PY - 2019 AN - OPUS4-48101 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin T1 - Flow chemistry using benchtop NMR instruments - Current approaches, chances and limitations N2 - Intensified continuous processes are in focus of current research. Compared to traditional batch processes, intensified continuous production allows the synthesis of new and difficult producible compounds with better product uniformity and reduced consumption of raw materials and energy. Flexible (modular) chemical plants can produce various products using the same equipment with short down-times between campaigns, and quick introduction of new products to the market. Consequently, the demand for powerful Process Analytical Technologies, which can monitor key variables like component concentrations in real-time, is increasing. Low-Field NMR spectroscopy presents itself as such an upcoming smart sensor1,2 (as addressed, e.g., in the CONSENS project3,4). Continuous measurement approaches can usually be differed in On- or In-line which both have advantages and drawbacks. On the one hand On-line measurements are easy to integrate even in existing setups through bypass systems, on the other hand issues like the representativity of the sampling must be considered. In the case of Inline analysis, where the whole fluid stream is analyzed, this issue can be avoided. Nevertheless, homogeneity of the mixture must be assured using NMR spectroscopy. This talk shall give a brief summary of current Online and Inline Low-Field NMR approaches. Furthermore, current research results using a tailor-made flow cell for inline analysis are shown pointing out the working range as well as limitations of these method in combination with NMR spectroscopy. T2 - 13. Interdisziplinäres Doktorandenseminar Berlin CY - Berlin, Germany DA - 18.03.2019 KW - NMR KW - Flow Chemistry KW - Inline KW - PAT KW - Benchtop NMR PY - 2019 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-47567 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Stable isotope analysis of magnesium by optical spectrometry N2 - Magnesium (Mg) is a major element in a range of silicate and carbonate minerals, the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg with natural abundances of 79 %, 10 %, and 11 %, respectively. It is due to their relatively large mass difference (~8% between 24Mg and 26Mg) that isotope fractionation leads to slight variations of isotope amount ratios n(26Mg)/n(24Mg) in biological, environmental and geological samples. Traditionally, isotope ratios are measured by mass spectrometric methods and isotope ratios are expressed as deviation from an internationally agreed upon material, i.e. the zero-point of the δ-value scale. Drawbacks of this method include the high costs for instruments and their operation, experienced operators and elaborate, time-consuming chromatographic sample preparation. Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high- resolution continuum source graphite furnace molecular absorption spectrometry (HR- CS-GFMAS) and laser ablation molecular isotopic spectrometry (LAMIS). For the determination of Mg isotope amount ratios, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied. In the case of HR-CS-GFMAS, the absorption spectrum was recorded for MgF for the electronic transitions X2Σ → A2Πi and X 2Σ → B2Σ+ around wavelengths 358 nm and 268 nm, respectively. In the case of LAMIS, we investigated the MgF molecule for the electronic transition A2Πi → X2Σ as well as the MgO molecule for the electronic transition A1Π+ → X1Σ around 500 nm. The MgF and MgO spectra are described by the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO (F is monoisotopic, and the isotope composition of O is assumed as constant). By HR-CS-GFMAS the analysis of Mg was done by deconvolution of the MgF spectrum by partial least square regression (PLS) calibrated with enriched isotope spikes. Isotope amount ratios in rock samples with and without matrix separation were analyzed. Calculated δ-values were accurate and obtained with precisions ranging between 0.2 ‰ and 0.5 ‰ (1 SD, n = 10). On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of in-situ analysis. Main advantages, limitations, and scopes of both optical techniques are going to be discussed and compared to MC-ICP-MS. T2 - Seminars Earth Surface Geochemistry- Deutsches GeoForschungsZentrum GFZ CY - Potsdam, Germany DA - 06.08.2019 KW - Isotope analysis KW - Magnesium KW - HR-CS-MAS KW - LIBS KW - Diatomic KW - Optical spectroscopy PY - 2019 AN - OPUS4-49904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Critical evaluation of optical spectrometry vs mass spectrometry for stable isotope analysis N2 - Mass spectrometric Methods MC-ICP-MS and TIMS) are without doubt the working horse of stable isotope analysis. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time consuming. Optical spectrometric methods are proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS) and laser ablation molecular isotopic spectrometry (LAMIS). First, stable isotope amount compositions of boron (B) and magnesium (Mg) were determined based on the absorption spectra of in-situ generated heteronuclear diatomic molecules (MH or MX) in graphite furnace HR-CS-MAS. The use of a modular simultaneous echelle spectrograph (MOSES) helps to find the maximal isotope shift in the diatomic molecular spectra produced in a graphite furnace by using isotopic spike solutions. Isotopes of boron (10B and 11B) were studied via their hydrides for the electronic transition X 1Σ+ → A 1Π. The spectrum of a given sample is a linear combination of the 10BH molecule and its isotopologue 11BH. Therefore, the isotopic composition of samples can be calculated by a partial least square regression (PLS). For this, a spectral library was built by using samples and spikes with known isotope composition. Boron isotope ratios measured by HR-CS-MAS are identical with those measured by mass spectrometric methods at the 0.15 ‰ level. Similar results were obtained for a multiple isotope system like Mg (24Mg, 25Mg, and 26Mg), where isotope shifts of their isotopologues can be resolved in the MgF molecule for the electronic transition X 2Σ → A 2 Πi. Finally, the application of molecular spectrometry via emission by LAMIS is compared and discussed. T2 - European Winter Conference on Plasma Spectrochemistry EWCPS 2019 CY - Pau, France DA - 03.02.2019 KW - Isotope analysis KW - HR-CS-MAS KW - LIBS KW - MS-ICP-MS KW - Optical spectroscopy KW - Mass spectrometry PY - 2019 AN - OPUS4-49874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nelson, G. A1 - Boehm, U. A1 - Bagley, S. A1 - Bajcsy, P. A1 - Bischof, J. A1 - Brown, C. M. A1 - Dauphin, A. A1 - Dobbie, I. M. A1 - Eriksson, J. E. A1 - Faklaris, O. A1 - Fernandez-Rodriguez, J. A1 - Ferrand, A. A1 - Gelman, L, A1 - Gheisari, A. A1 - Hartmann, H. A1 - Kukat, C. A1 - Laude, A. A1 - Mitkovski, M. A1 - Munck, S. A1 - North, A. J. A1 - Rasse, T. A1 - Resch-Genger, Ute A1 - Schuetz, L. C. A1 - Seitz, A. A1 - Strambio-De-Castillia, C. A1 - Swedlow, J. R. A1 - Alexopoulos, I. A1 - Aumayr, K. A1 - Avilov, S. A1 - Bakker, G.-J. A1 - Bammann, R. R. A1 - Bassi, A. A1 - Beckert, H. A1 - Beer, S. A1 - Belyaev, Y. A1 - Bierwagen, J. A1 - Birngruber, K. A. A1 - Bosch, M. A1 - Breitlow, J. A1 - Cameron, L. A. A1 - Chalfoun, J. A1 - Chambers, J. J. A1 - Chen, C.-L. A1 - Conde-Sousa, E. A1 - Corbett, A. D. A1 - Cordelieres, F. P. A1 - Del Nery, E. A1 - Dietzel, R. A1 - Eismann, F. A1 - Fazeli, E. A1 - Felscher, A. A1 - Fried, H. A1 - Gaudreault, N. A1 - Goh, W. I. A1 - Guilbert, T. A1 - Hadleigh, R. A1 - Hemmerich, P. A1 - Holst, G. A. A1 - Itano, M. S. A1 - Jaffe, C. B. A1 - Jambor, H. K. A1 - Jarvis, S. C. A1 - Keppler, A. A1 - Kirchenbuechler, D. A1 - Kirchner, M. A1 - Kobayashi, N. A1 - Krens, G. A1 - Kunis, S. A1 - Lacoste, J. A1 - Marcello, M. A1 - Martins, G. G. A1 - Metcalf, D. J. A1 - Mitchell, C. A. A1 - Moore, J. A1 - Mueller, T. A1 - Nelson, M. S. A1 - Ogg, S. A1 - Onami, S. A1 - Palmer, A. L. A1 - Paul-Gilloteaux, P. A1 - Pimentel, J. A. A1 - Plantard, L. A1 - Podder, S. A1 - Rexhepaj, E. A1 - Royon, A. A1 - Saari, M. A. A1 - Schapman, D. A1 - Schoonderwoert, V. A1 - Schroth-Diez, B. A1 - Schwartz, S. A1 - Shaw, M. A1 - Spitaler, M. A1 - Stoeckl, M. T. A1 - Sudar, D. A1 - Teillon, J. A1 - Terjung, S. A1 - Thuenauer, R. A1 - Wilms, C. D. A1 - Wright, G. D. A1 - Nitschke, R. T1 - QUAREP-LiMi: A community-driven initiative to establish guidelines for quality assessment and reproducibility for instruments and images in light microscopy N2 - A modern day light microscope has evolved from a tool devoted to making primarily empirical observations to what is now a sophisticated, quantitative device that is an integral part of both physical and life science research. Nowadays, microscopes are found in nearly every experimental laboratory. However, despite their prevalent use in capturing and quantifying scientific phenomena, neither a thorough understanding of the principles underlying quantitative imaging techniques nor appropriate knowledge of how to calibrate, operate and maintain microscopes can be taken for granted. This is clearly demonstrated by the well-documented and widespread difficulties that are routinely encountered in evaluating acquired data and reproducing scientific experiments. Indeed, studies have shown that more than 70% of researchers have tried and failed to repeat another scientist’s experiments, while more than half have even failed to reproduce their own experiments1. One factor behind the reproducibility crisis of experiments published in scientific journals is the frequent underreporting of imaging methods caused by a lack of awareness and/or a lack of knowledge of the applied technique2,3. Whereas quality control procedures for some methods used in biomedical research, such as genomics (e.g., DNA sequencing, RNA-seq) or cytometry, have been introduced (e.g. ENCODE4), this issue has not been tackled for optical microscopy instrumentation and images. Although many calibration standards and protocols have been published, there is a lack of awareness and agreement on common Standards and guidelines for quality assessment and reproducibility5. In April 2020, the QUality Assessment and REProducibility for instruments and images in Light Microscopy (QUAREP-LiMi) initiative6 was formed. This initiative comprises imaging scientists from academia and industry who share a common interest in achieving a better understanding of the performance and limitations of microscopes and improved quality control (QC) in light microscopy. The ultimate goal of the QUAREP-LiMi initiative is to establish a set of common QC standards, guidelines, metadata models7,8, and tools9,10, including detailed protocols, with the ultimate aim of improving reproducible advances in scientific research. This White Paper 1) summarizes the major obstacles identified in the field that motivated the launch of the QUAREP-LiMi initiative; 2) identifies the urgent need to address these obstacles in a grassroots manner, through a community of Stakeholders including, researchers, imaging scientists11, bioimage analysts, bioimage informatics developers, corporate partners, Funding agencies, standards organizations, scientific publishers, and observers of such; 3) outlines the current actions of the QUAREPLiMi initiative, and 4) proposes future steps that can be taken to improve the dissemination and acceptance of the proposed guidelines to manage QC. To summarize, the principal goal of the QUAREP-LiMi initiative is to improve the overall quality and reproducibility of light microscope image data by introducing broadly accepted standard practices and accurately captured image data metrics. KW - Fluorescence KW - Microscopy KW - Quality assurance KW - Comparability KW - Imaging KW - Standards KW - Reference materials KW - Reliability KW - Data KW - Reference data KW - Biology KW - Medicine KW - Life science PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530629 DO - https://doi.org/10.1111/jmi.13041 SN - 1365-2818 VL - 284 IS - 1 SP - 56 EP - 73 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-53062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Anderhalten, L. A1 - Silva, R. V. A1 - Morr, A. A1 - Wang, S. A1 - Smorodchenko, A. A1 - Saatz, Jessica A1 - Traub, Heike A1 - Mueller, S. A1 - Boehm-Sturm, P. A1 - Rodriguez-Sillke, Y. A1 - Kunkel, D. A1 - Hahndorf, J. A1 - Paul, F. A1 - Taupitz, M. A1 - Sack, I. A1 - Infante-Duarte, C. T1 - Different Impact of Gadopentetate and Gadobutrol on Inflammation-Promoted Retention and Toxicity of Gadolinium Within the Mouse Brain N2 - Objectives: Using a murine model of multiple sclerosis, we previously showed that repeated administration of gadopentetate dimeglumine led to retention of gadolinium (Gd) within cerebellar structures and that this process was enhanced with inflammation. This study aimed to compare the kinetics and retention profiles of Gd in inflamed and healthy brains after application of the macrocyclic Gd-based contrast agent (GBCA) gadobutrol or the linear GBCA gadopentetate. Moreover, potential Gd-induced neurotoxicity was investigated in living hippocampal slices ex vivo. Materials and Methods: Mice at peak of experimental autoimmune encephalomyelitis (EAE; n = 29) and healthy control mice (HC; n = 24) were exposed to a cumulative dose of 20 mmol/kg bodyweight of either gadopentetate dimeglumine or gadobutrol (8 injections of 2.5 mmol/kg over 10 days). Magnetic resonance imaging (7 T) was performed at baseline as well as at day 1, 10, and 40 post final injection (pfi) of GBCAs. Mice were sacrificed after magnetic resonance imaging and brain and blood Gd content was assessed by laser ablation-inductively coupled plasma (ICP)-mass spectrometry (MS) and ICP-MS, respectively. In addition, using chronic organotypic hippocampal slice cultures, Gd-induced neurotoxicity was addressed in living brain tissue ex vivo, both under control or inflammatory (tumor necrosis factor α [TNF-α] at 50 ng/μL) conditions. Results: Neuroinflammation promoted a significant decrease in T1 relaxation times after multiple injections of both GBCAs as shown by quantitative T1 mapping of EAE brains compared with HC. This corresponded to higher Gd retention within the EAE brains at 1, 10, and 40 days pfi as determined by laser ablation-ICP-MS. In inflamed cerebellum, in particular in the deep cerebellar nuclei (CN), elevated Gd retention was observed until day 40 after last gadopentetate application (CN: EAE vs HC, 55.06 ± 0.16 μM vs 30.44 ± 4.43 μM). In contrast, gadobutrol application led to a rather diffuse Gd content in the inflamed brains, which strongly diminished until day 40 (CN: EAE vs HC, 0.38 ± 0.08 μM vs 0.17 ± 0.03 μM). The analysis of cytotoxic effects of both GBCAs using living brain tissue revealed an elevated cell death rate after incubation with gadopentetate but not gadobutrol at 50 mM. The cytotoxic effect due to gadopentetate increased in the presence of the inflammatory mediator TNF-α (with vs without TNF-α, 3.15% ± 1.18% vs 2.17% ± 1.14%; P = 0.0345). Conclusions: In the EAE model, neuroinflammation promoted increased Gd retention in the brain for both GBCAs. Whereas in the inflamed brains, efficient clearance of macrocyclic gadobutrol during the investigated time period was observed, the Gd retention after application of linear gadopentetate persisted over the entire observational period. Gadopentetate but not gadubutrol appeared to be neurotoxic in an ex vivo paradigm of neuronal inflammation. KW - Imaging KW - ICP-MS KW - Gadolinium KW - Contrast agent KW - Laser ablation KW - Brain KW - Multiple sclerosis PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546910 DO - https://doi.org/10.1097/RLI.0000000000000884 SN - 0020-9996/22/0000–0000 VL - 57 IS - 10 SP - 677 EP - 688 PB - Wolters Kluwer N.V. CY - Alphen aan den Rijn, The Netherlands AN - OPUS4-54691 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauli, Jutta A1 - Wycisk, V. A1 - Welker, P. A1 - Justies, A. A1 - Resch-Genger, Ute A1 - Haag, R. A1 - Licha, K. T1 - Glycerol-Based Contrast Agents: A Novel Series of Dendronized Pentamethine Dyes N2 - The synthesis of water-soluble dyes, which absorb and emit in the range between 650 and 950 nm and display high extinction coefficients (ε) as well as high fluorescence quantum yields (Φf), is still a demand for optical imaging. We now present a synthetic route for the preparation of a new group of glycerol-substituted cyanine dyes from dendronized indole precursors that have been functionalized as Nhydroxysuccinimide (NHS) esters. High Φf values of up to 0.15 and extinction coefficients of up to 189 000 L mol−1 cm−1 were obtained for the pure dyes. Furthermore, conjugates of the new dendronized dyes with the antibody cetuximab (ctx) that were directed against the epidermal growth factor receptor (EGFR) of tumor cells could be prepared with dye to protein ratios between 0.3 and 2.2 to assess their potential as imaging probes. For the first time, ctx conjugates could be achieved without showing a decrease in Φf and with an increasing labeling degree that exceeded the value of the pure dye even at a labeling degree above 2. The incorporation of hydrophilically and sterically demanding dendrimers into cyanines prevented dimer formation after covalent conjugation to the antibody. The binding functionality of the resulting ctx conjugates to the EGFR was successfully demonstrated by cell microscopy studies using EGFR expressing cell lines. In summary, the combination of hydrophilic glycerol dendrons with reactive dye labels has been established for the first time and is a promising Approach toward more powerful fluorescent labels with less dimerization. KW - Dye KW - Quantum yield KW - Fluorescence KW - Contrast agent KW - Extinction coefficient PY - 2015 DO - https://doi.org/10.1021/acs.bioconjchem.5b00097 SN - 1043-1802 VL - 26 SP - 773 EP - 781 PB - ACS Publications CY - Washington AN - OPUS4-38880 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalot, G. A1 - Godard, A. A1 - Busser, B. A1 - Pliquett, J. A1 - Broekgaarden, M. A1 - Motto-Ros, V. A1 - Wegner, Karl David A1 - Resch-Genger, Ute A1 - Köster, U. A1 - Denat, F. A1 - Coll, J.-L. A1 - Bodio, E. A1 - Goze, C. A1 - Sancey, L. T1 - Aza-BODIPY: A New Vector for Enhanced Theranostic Boron Neutron Capture Therapy Applications N2 - Boron neutron capture therapy (BNCT) is a radiotherapeutic modality based on the nuclear capture of slow neutrons by stable 10B atoms followed by charged particle Emission that inducing extensive damage on a very localized level (<10 um). To be effcient, a suffcient amount of 10B should accumulate in the tumor area while being almost cleared from the normal surroundings. A water-soluble aza-boron-dipyrromethene dyes (BODIPY) fluorophore was reported to strongly accumulate in the tumor area with high and BNCT compatible Tumor/Healthy Tissue ratios. The clinically used 10B-BSH (sodium borocaptate) was coupled to the water-soluble aza-BODIPY platform for enhanced 10B-BSH tumor vectorization. We demonstrated a strong uptake of the compound in tumor cells and determined its biodistribution in mice-bearing tumors. A model of chorioallantoic membrane-bearing glioblastoma xenograft was developed to evidence the BNCT potential of such compound, by subjecting it to slow neutrons. We demonstrated the Tumor accumulation of the compound in real-time using optical imaging and ex vivo using elemental imaging based on laser-induced breakdown spectroscopy. The tumor growth was significantly reduced as compared to BNCT with 10B-BSH. Altogether, the fluorescent aza-BODIPY/10B-BSH compound is able to vectorize and image the 10B-BSH in the tumor area, increasing its theranostic potential for effcient approach of BNCT. KW - Aza-BODIPY KW - SWIR KW - NIR-I KW - Theranostic KW - Boron compound KW - Optical imaging PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512280 DO - https://doi.org/10.3390/cells9091953 VL - 9 IS - 9 SP - 1953 PB - MDPI AN - OPUS4-51228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyerhofer, F. A1 - Dissinger, F. A1 - Weigert, Florian A1 - Jungclaus, J. A1 - Müller-Caspary, K. A1 - Waldvogel, S. R. A1 - Resch-Genger, Ute A1 - Voss, T. T1 - Citric Acid Based Carbon Dots with Amine Type Stabilizers: pHSpecific N2 - We report the synthesis and spectroscopic characteristics of two different sets of carbon dots (CDs) formed by hydrothermal reaction between citric acid and polyethylenimine (PEI) or 2,3-diaminopyridine (DAP). Although the formation of amide-based species and the presence of citrazinic acid type derivates assumed to be responsible for a blue emission is confirmed for both CDs by elemental analysis, infrared spectroscopy, and mass spectrometry, a higher abundance of sp2-hybridized nitrogen is observed for DAP-based CDs, which causes a red-shift of the n-π* absorption band relative to the one of PEI-based CDs. These CD Systems possess high photoluminescence quantum yields (QY) of ∼40% and ∼48% at neutral pH, demonstrating a possible tuning of the optical properties by the amine precursor. pH-Dependent spectroscopic studies revealed a drop in QY to < 9% (pH ∼ 1) and < 21% (pH ∼ 12) for both types of CDs under acidic and basic conditions. In contrast, significant differences in the pHdependency of the n-π* transitions are found for both CD types which are ascribed to different (de)protonation sequences of the CD-specific fluorophores and functional groups using Zeta potential analysis. KW - Fluorescence KW - Particle KW - Nano KW - Surface group analysis KW - Carbon dot KW - C-dot KW - Fluorescent probe KW - Quantum yield KW - Synthesis KW - IR KW - MS KW - Polymer KW - Ligand PY - 2020 DO - https://doi.org/10.1021/acs.jpcc.9b11732 VL - 124 IS - 16 SP - 8894 EP - 8904 PB - American Chemical Society AN - OPUS4-50813 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kader, A. A1 - Brangsch, J. A1 - Reimann, C. A1 - Kaufmann, Jan Ole A1 - Mangarova, D. B. A1 - Moeckel, J. A1 - Adams, L. C. A1 - Zhao, J. A1 - Saatz, Jessica A1 - Traub, Heike A1 - Buchholz, R. A1 - Karst, U. A1 - Hamm, B. A1 - Makowski, M. R. T1 - Visualization and Quantification of the Extracellular Matrix in Prostate Cancer Using an Elastin Specific Molecular Probe N2 - One of the most commonly diagnosed cancers in men is prostate cancer (PCa). Understanding tumor progression can help diagnose and treat the disease at an early stage. Components of the extracellular matrix (ECM) play a key role in the development and progression of PCa. Elastin is an essential component of the ECM and constantly changes during tumor development. This article visualizes and quantifies elastin in magnetic resonance imaging (MRI) using a small molecule probe. Results were correlated with histological examinations. Using an elastin-specific molecular probe, we were able to make predictions about the cellular structure in relation to elastin and thus draw conclusions about the size of the tumor, with smaller tumors having a higher elastin content than larger tumors. Human prostate cancer (PCa) is a type of malignancy and one of the most frequently diagnosed cancers in men. Elastin is an important component of the extracellular matrix and is involved in the structure and organization of prostate tissue. The present study examined prostate cancer in a xenograft mouse model using an elastin-specific molecular probe for magnetic resonance molecular imaging. Two different tumor sizes (500 mm3 and 1000 mm3) were compared and analyzed by MRI in vivo and histologically and analytically ex vivo. The T1-weighted sequence was used in a clinical 3-T scanner to calculate the relative contrast enhancement before and after probe administration. Our results show that the use of an elastin-specific probe enables better discrimination between tumors and surrounding healthy tissue. Furthermore, specific binding of the probe to elastin fibers was confirmed by histological examination and laser ablation–inductively coupled plasma–mass spectrometry (LA-ICP-MS). Smaller tumors showed significantly higher signal intensity (p > 0.001), which correlates with the higher proportion of elastin fibers in the histological evaluation than in larger tumors. A strong correlation was seen between relative enhancement (RE) and Elastica–van Gieson staining (R2 = 0.88). RE was related to inductively coupled plasma–mass spectrometry data for Gd and showed a correlation (R2 = 0.78). Thus, molecular MRI could become a novel quantitative tool for the early evaluation and detection of PCa. KW - Magnetic resonance imaging KW - MRI KW - Molecular imaging KW - Cancer KW - LA-ICP-MS PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-538410 DO - https://doi.org/10.3390/biology10111217 VL - 10 IS - 11 SP - 1 EP - 14 PB - MDPI CY - Basel AN - OPUS4-53841 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yanbaeva, M. A1 - Soyka, J. A1 - Holthoff, J. M. A1 - Rietsch, P. A1 - Engelage, E. A1 - Ruff, A. A1 - Resch-Genger, Ute A1 - Weiss, R. A1 - Eigler, S. A1 - Huber, S. M. T1 - Dimethylene-Cyclopropanide Units as Building Blocks for Fluorescence Dyes N2 - Many organic dyes are fluorescent in solution. In the solid state, however, quenching processes often dominate, hampering material science applications such as light filters, light-emitting devices, or coding tags. We show that the dimethylene-cyclopropanides caffold can be used to form two structurally different types of chromophores, which feature fluorescence quantum yields up to 0.66 in dimethyl sulfoxide and 0.53 in solids. The increased fluorescence in the solid state for compounds bearing malonate substituents instead of dicyanomethide ones is rationalized by the induced twist between the planes of the cyclopropanide core and a pyridine ligand. KW - Fluorescence KW - Dye KW - Sensor KW - Quantum yield KW - Spectroscopy KW - Photophysics KW - Synthesis KW - Solvatochromism PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614931 DO - https://doi.org/10.1002/chem.202402476 VL - 30 IS - 56 SP - 1 EP - 7 PB - Chemistry - A European Journal AN - OPUS4-61493 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yu, Z. A1 - Musnier, B. A1 - Wegner, Karl David A1 - Henry, M. A1 - Chovelon, B. A1 - Desroches-Castan, A. A1 - Fertin, A. A1 - Resch-Genger, Ute A1 - Bailly, S. A1 - Coll, J.-L. A1 - Usson, Y, A1 - Josserand, V. A1 - Le Gúevel, X. T1 - High-Resolution Shortwave Infrared Imaging of Vascular Disorders Using Gold Nanoclusters N2 - We synthesized a generation of water-soluble, atomically precise gold nanoclusters (Au NCs) with anisotropic Surface containing a short dithiol pegylated chain (AuMHA/TDT). The AuMHA/TDT exhibit a high brightness (QY ∼ 6%) in the shortwave infrared (SWIR) spectrum with a detection above 1250 nm. Furthermore, they show an extended half-life in blood (t1/2ß = 19.54 ± 0.05 h) and a very weak accumulation in organs. We also developed a non-invasive, whole-body vascular imaging system in the SWIR window with high-resolution, benefiting from a series of Monte Carlo image processing. The imaging process enabled to improve contrast by 1 order of magnitude and enhance the spatial Resolution by 59%. After systemic administration of these nanoprobes in mice, we can quantify vessel complexity in depth (>4 mm), allowing to detect very subtle vascular disorders non-invasively in bone morphogenetic protein 9 (Bmp9)-deficient mice. The combination of these anisotropic surface charged Au NCs plus an improved SWIR imaging device allows a precise mapping at high-resolution and an in depth understanding of the organization of the vascular network in live animals. KW - Nanoparticle KW - Nanosensor KW - Fluorescence KW - Metal cluster KW - NIR KW - SWIR KW - Photophysics KW - Ligand KW - Size KW - Surface chemistry KW - Quantum yield KW - Mechanism KW - Lifetime KW - Decay kinetics PY - 2020 DO - https://doi.org/10.1021/acsnano.0c01174 VL - 14 IS - 4 SP - 4973 EP - 4981 PB - ACS Publication AN - OPUS4-50671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fa, X. A1 - Lin, Sh. A1 - Yang, J. A1 - Shen, Ch. A1 - Liu, Y. A1 - Gong, Y. A1 - Qin, A. A1 - Ou, Jun A1 - Resch-Genger, Ute T1 - −808 nm-activated Ca2+ doped up-conversion nanoparticles that release no inducing liver cancer cell (HepG2) apoptosis N2 - Anear-infrared (NIR) light-triggered release method for nitric oxide (NO) was developed utilizing core/shell NaYF4: Tm/Yb/Ca@NaGdF4:Nd/Yb up-conversion nanoparticles (UCNPs) bearing a mesoporous silica (mSiO2) shell loaded with theNOdonor S-nitroso-N-acetyl-DL-penicillamine (SNAP). To avoid overheating in biological samples, Nd3+ was chosen as a sensitizer, Yb3+ ions as the bridging sensitizer, andTm3+ ions as UV-emissive activator while co-doping with Ca2+ was done to enhance the luminescence of the activatorTm3+.NOrelease from SNAP was triggered by an NIR-UV up-conversion process, initiated by 808nmlight absorbed by the Nd3+ ions.NOrelease was confirmed by the Griess method. Under 808nmirradiation, the viability of the liver cancer cell line HepG2 significantly decreased with increasing UCNPs@mSiO2-SNAP concentration. For a UCNPs@mSiO2-SNAP concentration of 200 μgml−1, the cell survival probability was 47%. These results demonstrate that UCNPs@mSiO2-SNAP can induce the release of apoptosis-inducingNOby NIR irradiation. KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - Excitation power density KW - Brightness KW - NIR KW - Mechanism KW - Triggered KW - Release KW - Cell KW - PDT KW - Dye KW - Therapy KW - Surface KW - Coating PY - 2022 DO - https://doi.org/10.1088/2050-6120/ac5524 VL - 10 IS - 2 SP - 1 EP - 9 PB - IOP Publishing AN - OPUS4-54842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Manley, P. A1 - Voigt, R. A1 - Ahiboz, D. A1 - Becker, C. A1 - Resch-Genger, Ute T1 - Metasurface Enhanced Sensitized Photon Upconversion: Toward Highly Efficient Low Power Upconversion Applications and Nanoscale E-Field Sensors N2 - Large-scale nanoimprinted metasurfaces based on silicon photonic crystal slabs were produced and coated with a NaYF4:Yb3+/Er3+ upconversion nanoparticle (UCNP) layer. UCNPs on these metasurfaces yield a more than 500-fold enhanced upconversion emission compared to UCNPs on planar surfaces. It is also demonstrated how the optical response of the UCNPs can be used to estimate the local field energy in the coating layer. Optical simulations using the finite element method validate the experimental results and the calculated spatial three-dimensional field Energy distribution helps us to understand the emission enhancement mechanism of the UCNPs closely attached to the metasurface. In addition, we analyzed the spectral shifts of the resonances for uncoated and coated metasurfaces and metasurfaces submerged in water to enable a prediction of the optimum layer thicknesses for different excitation wavelengths, paving the way to applications such as electromagnetic field sensors or bioassays. KW - Nanoparticles KW - Upconversion KW - Metasurface KW - Field sensor KW - Emission enhancement KW - Photonic crystal PY - 2020 DO - https://doi.org/10.1021/acs.nanolett.0c02548 VL - 20 IS - 9 SP - 6682 EP - 6689 PB - ACS Publications AN - OPUS4-51427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sarif, Raduan A1 - Tiebe, Carlo A1 - Herglotz, Christian T1 - Early Response Prediction for H2 Sensors N2 - Green hydrogen (H2) is essential for the global transition to clean energy; it will significantly reduce emissions from heavy industry and the long-distance transport system. H2 can be used as fuel in fuel cells, storing surplus renewable energy, and as a feedstock in industrial processes. However, H2 faces significant safety challenges during storage and transportation. Accidents due to H2 leakage and explosions raise serious concerns due to its high flammability, rapid diffusion in air, and extremely low ignition energy. To mitigate risks associated with H2 leakages, reliable and automated H2 safety systems are essential for emergency repairs or shutdown. An early response from H2 sensors is crucial for early warning in accidents. The earlier response time of H2 sensors is often constrained by their sensor principle, which is heavily influenced by the sensor material’s properties. This study explores methods for earlier sensor response through predictive algorithms. Specifically, we investigate transient response predictions using a First-Order (FO) model and propose improvements through the First-Order with early response and the First-Order with adapted early response model. Both models can predict the stable value of the H2 sensor response from a small time window, which is 70.89% and 83.72% earlier, respectively, than the time required for the sensor hardware to reach it physically. The model’s performance is evaluated by calculating the fitting error with a 2 % threshold. Our current research lays the groundwork for future advancements in real-time sensor response predictions for hydrogen leakage. T2 - IARIA Congress 2025 : The 2025 IARIA Annual Congress on Frontiers in Science, Technology, Services, and Applications CY - Venice, Italy DA - 06.07.2025 KW - H2 Safety KW - H2 leakage detection KW - First-Order (FO) model KW - H2 Sensor data analysis KW - H2 sensor response predictions PY - 2025 AN - OPUS4-64195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blotevogel, J. T1 - Thermal PFAS Destruction in a Full-Scale Hazardous Waste Incinerator N2 - Incineration is currently the only commercial full-scale technology available to destroy per- and polyfluoroalkyl substances (PFAS) in large solid and liquid waste streams. Given previous experience of dioxin formation during halogenated waste incineration, concerns about the emission of products of incomplete destruction (PIDs) from PFAS incineration exist. The overarching objective of this project is to track the fate of fluorine during full-scale hazardous waste incineration in order to demonstrate the readiness, viability, and level of safety for thermal PFAS destruction in various waste streams. The specific objectives of this project are (1) to enhance our understanding of key variables and conditions on PFAS incineration performance, (2) to identify major PIDs under insufficient treatment conditions, (3) to explore the catalytic role of fly ash and other process-relevant surfaces in thermal PFAS decomposition, and (4) to determine the potential formation of polyfluorinated dibenzodioxins and dibenzofurans. T2 - 2025 SERDP & ESTCP PFAS Project Meeting CY - Long Beach, CA, USA DA - 04.08.2025 KW - PFAS KW - Hazardous waste incineration PY - 2025 AN - OPUS4-64189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - Acoustic Ion Manipulation: Electric-field-free Approach to Gate, Focus, and Separate Ions at Atmospheric Pressure N2 - Approaches to control the motion and direction of ionized particles and mole-cules are an essential aspect of ion-based spectrometries, such as mass spec-trometry (MS) and ion mobility spectrometry (IMS). A wide variety of ion optics exist to reflect, focus, separate, gate, and filter ions based on physical proper-ties. Notably all rely on electric and magnetic fields to alter the trajectory of ionized atoms and molecules. While these optics are quite efficient at low pressures due to the large mean free path, diffusion and electrostatic repulsion between ions dominate at higher pressures. Conventional ion optics, that use electric or magnetic fields, can guide ions at atmospheric pressure (AP), but require high field strengths to overcome the dominating aerodynamic effects. Here, we describe a remarkable phenomenon whereby low-power acoustic fields are used to move, shape, gate, and separate beams of gaseous ions at atmospheric pressure. We refer to this approach as Acoustic Ion Manipulation (AIM). Gaseous ions at AP are directed towards and separated by the presence of the acoustic field. To better understand the phenomenon, an ion-detector array provided a measure of bulk ion movement, while mass spectrometry (MS) offered chemical-specific information. As one example of an AIM setup, a standing acoustic wave was formed with two ultrasonic speakers and placed between an ionization source and ion detector. Ion beams preferentially travel through regions of stable pressure gradients (i.e. nodes) and deflect from un-stable regions (i.e. antinodes). Shadowgraphy revealed that the ions are sepa-rated from a neutral gas stream. Specific examples of ion focusing, gating, and separation (based on ion size) will be shown. In addition, experimental findings will be used to postulate a theory to develop a better understand of the behav-ior of gas-phase ions in acoustic fields. This discovery could have profound im-pacts in IMS/MS instrumentation as well as materials processing and charac-terization. T2 - 56. Jahrestagung der DGMS CY - Göttingen, Germany DA - 04.03.2025 KW - Acoustic Ion Manipulation KW - Mass spectrometry KW - Ultrasound PY - 2025 AN - OPUS4-64208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Grabolle, Markus A1 - Pauli, Jutta A1 - Spieles, Monika A1 - Resch-Genger, Ute T1 - Relative and absolute determination of fluorescence quantum yields of transparent samples N2 - Luminescence techniques are among the most widely used detection methods in the life and material sciences. At the core of these methods is an ever-increasing variety of fluorescent reporters (i.e., simple dyes, fluorescent labels, probes, sensors and switches) from different fluorophore classes ranging from small organic dyes and metal ion complexes, quantum dots and upconversion nanocrystals to differently sized fluorophore-doped or fluorophore-labeled polymeric particles. A key parameter for fluorophore comparison is the fluorescence quantum yield (Φf), which is the direct measure for the efficiency of the conversion of absorbed light into emitted light. In this protocol, we describe procedures for relative and absolute determinations of Φf values of fluorophores in transparent solution using optical methods, and we address typical sources of uncertainty and fluorophore class-specific challenges. For relative determinations of Φf, the sample is analyzed using a conventional fluorescence spectrometer. For absolute determinations of Φf, a calibrated stand-alone integrating sphere setup is used. To reduce standard-related uncertainties for relative measurements, we introduce a series of eight candidate quantum yield standards for the wavelength region of ~350–950 nm, which we have assessed with commercial and custom-designed instrumentation. With these protocols and standards, uncertainties of 5–10% can be achieved within 2 h. PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-294202 DO - https://doi.org/10.1038/nprot.2013.087 SN - 1754-2189 SN - 1750-2799 VL - 8 IS - 8 SP - 1535 EP - 1550 PB - Nature Publishing Group CY - Basingstoke AN - OPUS4-29420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiggenhauser, Herbert A1 - Niederleithinger, Ernst T1 - Innovative ultrasonic techniques for inspection and monitoring of large concrete structures N2 - Ultrasonic echo and transmission techniques are used in civil engineering on a regular basis. New sensors and data processing techniques have lead to many new applications in the structural investigation as well as quality control. But concrete structures in the nuclear sector have special features and parameters, which pose problems for the methods and instrumentation currently available, e.g. extreme thickness, dense reinforcement, steel liners or special materials. Several innovative ultrasonic techniques have been developed to deal with these issues at least partly in lab experiments and pilot studies. Modern imaging techniques as multi-offset SAFT have been used e. g. to map delaminations. Thick concrete walls have successfully been inspected, partly through a steel liner. Embedded ultrasonic sensors have been designed which will be used in monitoring networks of large concrete structures above and below ground. In addition, sensitive mathematical methods as coda wave interferometry have been successfully evaluated to detect subtle changes in material properties. Examples of measurements and data evaluation are presented. KW - Automated scanning systems KW - Multi-Offset Array KW - Enhanced Imaging KW - Embedded ultrasonic sensors PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-290513 DO - https://doi.org/10.1051/epjconf/20135604004 SN - 2100-014X VL - 56 SP - 04004-1 EP - 04004-9 PB - EDP Sciences CY - Les Ulis AN - OPUS4-29051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilhelm, Stefan A1 - Kaiser, Martin A1 - Würth, Christian A1 - Heiland, J. A1 - Carrillo-Carrion, C. A1 - Muhr, V. A1 - Wolfbeis, Otto S. A1 - Parak, W.J. A1 - Resch-Genger, Ute A1 - Hirsch, T. T1 - Water dispersible upconverting nanoparticles: effects of surface modification on their luminescence and colloidal stability N2 - We present a systematic study on the effect of surface ligands on the luminescence properties and colloidal stability of β-NaYF4:Yb3+,Er3+ upconversion nanoparticles (UCNPs), comparing nine different surface coatings to render these UCNPs water-dispersible and bioconjugatable. A prerequisite for this study was a large-scale synthetic method that yields ~2 g per batch of monodisperse oleate-capped UCNPs providing identical core particles. These ~23 nm sized UCNPs display an upconversion quantum yield of ~0.35% when dispersed in cyclohexane and excited with a power density of 150 W cm-2, underlining their high quality. A comparison of the colloidal stability and luminescence properties of these UCNPs, subsequently surface modified with ligand exchange or encapsulation protocols, revealed that the ratio of the green (545 nm) and red (658 nm) emission bands determined at a constant excitation power density clearly depends on the surface chemistry. Modifications relying on the deposition of additional (amphiphilic) layer coatings, where the initial oleate coating is retained, show reduced non-radiative quenching by water as compared to UCNPs that are rendered water-dispersible via ligand exchange. Moreover, we could demonstrate that the brightness of the upconversion luminescence of the UCNPs is strongly affected by the type of surface modification, i.e., ligand exchange or encapsulation, yet hardly by the chemical nature of the ligand. KW - upconverting nanoparticles (UCNPs) KW - Luminescence KW - surface modification PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-324071 DO - https://doi.org/10.1039/c4nr05954a SN - 2040-3364 SN - 2040-3372 VL - 7 IS - 4 SP - 1403 EP - 1410 PB - RSC Publ. CY - Cambridge AN - OPUS4-32407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Neue Ideen für die zerstörungsfreie Prüfung von Beton: Seismische Interferometrie und mehr N2 - Ultraschallverfahren haben sich im Bauwesen in den letzten Jahren immer mehr in der Praxis etabliert. Echomessungen zur Geometriebestimmung sind Stand der Technik. In der Wissenschaft gibt es zahlreiche Ideen, die Messmethodik und die Auswertung weiter zu verbessern sowie den Einsatzbereich zu erweitern. Erste eingebettete Ultraschallsysteme zum Langzeitmonitoring sind installiert, Mehrkanalgeräte ermöglichen immer größere Aperturen und Eindringtiefen, verbesserte Abbildungsverfahren zeigen immer mehr Details. Zusätzlich lassen sich Verfahren aus der Geophysik adaptieren, die weiteren Fortschritt versprechen. Die Seismische Interferometrie dient klassisch dazu, Materialeigenschaften des Erduntergrundes mittels seismischer Wellen zu bestimmen. Derzeitige Anwendungsbereiche sind die Verbesserung seismischer Abbildungsverfahren, Interpolation seismischer Spuren (A-Scans), Bestimmung von Quellparametern oder die Eliminierung unerwünschter Signale in passiven und aktiven Experimenten, hauptsächlich durch Kreuzkorrelation und Bestimmung Greenscher Funktionen. Diese Techniken können auch auf Ultraschalldaten, die an Betonkonstruktionen erfasst wurden, angewendet werden. Moderne Abbildungsverfahren benötigen eine möglichst hohe A-Scan-Dichte und eine genaue Kenntnis des Quellsignals. Beides ist nicht unbedingt gegeben, z. B. wegen der physischen Größe der Sensoren und wechselnder Ankopplungsbedingungen. In simulierten und realen Experimenten wurden interferometrische Methoden zur Lösung dieser Aufgabenstellungen evaluiert. Es zeigt sich, dass fehlende A-Scans kinematisch korrekt interpoliert werden können, wenn ausreichend viele Sender- und Empfängerpositionen genutzt wurden. Amplituden und Signalform sind verändert, können aber durch adaptive Filterung angepasst werden. Die Quellsignalform kann mit hoher Genauigkeit rekonstruiert werden. Die Ergebnisse können potentiell zu einer Verbesserung der Abbildung des Inneren der untersuchten Objekte genutzt werden. T2 - DGZfP-Jahrestagung 2014 CY - Potsdam, Germany DA - 26.05.2014 KW - Zerstörungsfreie Prüfung KW - Geophysik PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-337967 UR - http://www.ndt.net/article/dgzfp2014/papers/di1c1.pdf SN - 978-3-940283-61-0 IS - DGZfP-BB 148 SP - Di.1.C.1, 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-33796 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Douma, J. A1 - Niederleithinger, Ernst A1 - Snieder, R. T1 - Improved focusing using deconvolution within a concrete block N2 - Time reversal techniques are used in ocean acoustics, medical imaging and non-destructive evaluation to backpropagate recorded signals to the source of origin. We demonstrate experimentally a technique which improves the temporal focus achieved at the source location. The experiment consists of propagating a signal from a transducer within a concrete block to a single receiver on the surface, and then applying time reversal or deconvolution to focus the energy back at the source location. The results show that we are able to generate a focus in time at the correct location. The proposed method is simple and proven to be robust. Additionally, its costs are negligible due to deconvolution being a preprocessing step to the recorded data. The technique can be applied for detailed investigation of the source mechanisms (e. g. cracks) but also for monitoring purposes. T2 - DGZfP-Jahrestagung 2014 CY - Potsdam, Germany DA - 26.05.2014 KW - Ultrasonics KW - Acoustic emission KW - Time reversal KW - Deconvolution PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-337953 UR - http://www.ndt.net/article/dgzfp2014/papers/di2c2.pdf SN - 978-3-940283-61-0 IS - DGZfP-BB 148 SP - Di.2.C.2, 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-33795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Clauß, F. A1 - Epple, Niklas A1 - Ahrens, M. A. A1 - Niederleithinger, Ernst A1 - Mark, P. T1 - Correlation of Load-Bearing Behavior of Reinforced Concrete Members and Velocity Changes of Coda Waves N2 - The integral collection of information such as strains, cracks, or temperatures by ultrasound offers the best prerequisites to monitor structures during their lifetime. In this paper, a novel approach is proposed which uses the collected information in the coda of ultrasonic signals to infer the condition of a structure. This approach is derived from component tests on a reinforced concrete beam subjected to four-point bending in the lab at Ruhr University Bochum. In addition to ultrasonic measurements, strain of the reinforcement is measured with fiber optic sensors. Approached by the methods of moment-curvature relations, the steel strains serve as a reference for velocity changes of the coda waves. In particular, a correlation between the relative velocity change and the average steel strain in the reinforcement is derived that covers 90% of the total bearing capacity. The purely empirical model yields a linear function with a high level of accuracy (R 2 =0.99, R2=0.99, RMSE≈90μ RMSE≈90μ strain). KW - Ultrasound KW - Coda Wave Interferometry (CWI) KW - Structural Health Monitoring KW - Reinforced Concrete KW - Embedded Sensors PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542316 DO - https://doi.org/10.3390/ma15030738 VL - 15 IS - 3 SP - 738 PB - MDPI AN - OPUS4-54231 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bastos, V. A1 - Oskoei, P. A1 - Andresen, Elina A1 - Saleh, Maysoon I. A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Oliveira, H. T1 - Stability, dissolution, and cytotoxicity of NaYF4‑upconversion nanoparticles with different coatings N2 - Upconversion nanoparticles (UCNPs) have attracted considerable attention owing to their unique photophysical properties. Their utilization in biomedical applications depends on the understanding of their transformations under physiological conditions and their potential toxicity. In this study, NaYF4: Yb,Er UCNPs, widely used for luminescence and photophysical studies, were modified with a set of four different coordinatively bound surface ligands, i.e., citrate, alendronate (AA), ethylendiamine tetra(methylene phosphonate) (EDTMP), and poly(maleic anhydride-alt-1-octadecene) (PMAO), as well as silica coatings with two different thicknesses. Subsequently, the aging-induced release of fluoride ions in water and cell culture media and their cytotoxic profile to human keratinocytes were assessed in parallel to the cytotoxic evaluation of the ligands, sodium fluoride and the lanthanide ions. The cytotoxicity studies of UCNPs with different surface modifications demonstrated the good biocompatibility of EDTMP-UCNPs and PMAO-UCNPs, which is in line with the low amount of fluoride ions released from these samples. An efficient prevention of UCNP dissolution and release of cytotoxic ions, as well as low cytotoxicity was also observed for UCNPs with a sufficiently thick silica shell. Overall, our results provide new insights into the understanding of the contribution of surface chemistry to the stability, dissolution behavior, and cytotoxicity of UCNPs. Altogether, the results obtained are highly important for future applications of UCNPs in the life sciences and bioimaging studies. KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Excitation power density KW - Surface chemistry KW - Coating PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544681 DO - https://doi.org/10.1038/s41598-022-07630-5 SN - 2045-2322 VL - 12 SP - 1 EP - 13 PB - Springer Nature CY - London AN - OPUS4-54468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chakraborty, J. A1 - Wang, Xin A1 - Stolinski, M. T1 - Analysis of Sensitivity of Distance between Embedded Ultrasonic Sensors and Signal Processing on Damage Detectability in Concrete Structures N2 - Damage detection of reinforced concrete (RC) structures is becoming a more attractive domain due to the safety issues arising in the last few decades. The damage in concrete can be caused by excessive exploitation of the structure or environmental effects. The cracks in concrete can be detected by different nondestructive testing methods. However, the available methods used for this purpose have numerous limitations. The technologies available in the market nowadays have difficulties detecting slowly progressive, locally limited damage. In addition, some of These methods cannot be applied, especially in hard-to-reach areas in the superstructures. In order to avoid these deficiencies, an embedded ultrasonic methodology can be used to detect cracks in RC structures. In this study, the methodology of crack detection supported with the advanced Signal processing algorithm was proposed and verified on RC structures of various types, and cracks occurring between embedded sensors can be detected. Moreover, different pairs of ultrasonic sensors located in the considered structures are used for the analysis of the sensitivity of distance between them. It is shown that the ultrasonic sensors placed in the range of 1.5–2 m can detect cracks, even when the other methods failed to detect changes in the structure. The obtained results confirmed that diffuse ultrasonic sensor methodology is able to monitor real structures more effectively than traditional techniques. KW - Ultrasound KW - Coda wave interferometry KW - Structural health monitoring PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543624 DO - https://doi.org/10.3390/acoustics4010007 VL - 4 IS - 1 SP - 89 EP - 110 PB - MDPI CY - Basel, Schweiz AN - OPUS4-54362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Le Guevel, X. A1 - Wegner, Karl David A1 - Würth, Christian A1 - Baulin, V. A. A1 - Musnier, B. A1 - Josserand, V. A1 - Resch-Genger, Ute A1 - Koll, J-C T1 - Tailoring the SWIR emission of gold nanoclusters by surface ligand rigidification and their application in 3D bioimaging N2 - The influence of solvent polarity and surface ligand rigidification on the SWIR emission profile of gold nanoclusters with an anistropic surface was investigated. A strong enhancement of the SWIR emission band at 1200 nm was observed when measuring in different local environments: in solution, in polymer composites, and in solids. SWIR in vivo imaging of mice assisted by deep learning after intravenous administration of these gold nanoclusters provides high definition pseudo-3D views of vascular blood vessels. KW - Nano KW - Nanomaterial KW - Metal cluster KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - NIR KW - SWIR KW - Ligand KW - Gold KW - Mechanism KW - Charge transfer KW - Enhancement strategy KW - Imaging KW - Application KW - Contrast agent PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543582 DO - https://doi.org/10.1039/D1CC06737K VL - 58 IS - 18 SP - 2967 EP - 2970 PB - RSC AN - OPUS4-54358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kaufmann, Jan Ole A1 - Brangsch, J. A1 - Kader, A. A1 - Saatz, Jessica A1 - Mangarova, D. B. A1 - Zacharias, M. A1 - Kempf, W. E. A1 - Schwaar, T. A1 - Ponader, Marco A1 - Adams, L. C. A1 - Möckel, J. A1 - Botnar, R. M. A1 - Taupitz, M. A1 - Mägdefessel, L. A1 - Traub, Heike A1 - Hamm, B. A1 - Weller, Michael G. A1 - Makowski, M. R. T1 - ADAMTS4-specific MR-probe to assess aortic aneurysms in vivo using synthetic peptide libraries N2 - The incidence of abdominal aortic aneurysms (AAAs) has substantially increased during the last 20 years and their rupture remains the third most common cause of sudden death in the cardiovascular field after myocardial infarction and stroke. The only established clinical parameter to assess AAAs is based on the aneurysm size. Novel biomarkers are needed to improve the assessment of the risk of rupture. ADAMTS4 (A Disintegrin And Metalloproteinase with ThromboSpondin motifs 4) is a strongly upregulated proteoglycan cleaving enzyme in the unstable course of AAAs. In the screening of a one-bead-one-compound library against ADAMTS4, a low-molecular-weight cyclic peptide is discovered with favorable properties for in vivo molecular magnetic resonance imaging applications. After identification and characterization, it’s potential is evaluated in an AAA mouse model. The ADAMTS4-specific probe enables the in vivo imaging-based prediction of aneurysm expansion and rupture. KW - Peptide KW - Peptide library KW - OBOC library KW - Combinatorial chemistry KW - Peptide aptamers KW - Binding molecule KW - Affinity KW - Synthetic peptides KW - Contrast agent KW - Magnetic resonance imaging KW - One-bead-one-compound library KW - On-chip screening KW - Lab-on-a-chip KW - MALDI-TOF MS KW - SPR KW - Surface plasmon resonance KW - Alanine scan KW - Fluorescence label KW - MST KW - Docking KW - Chelate PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-560930 DO - https://doi.org/10.1038/s41467-022-30464-8 N1 - Geburtsname von Ponader, Marco: Wilke, M. - Birth name of Ponader, Marco: Wilke, M. VL - 13 IS - 1 SP - 1 EP - 18 PB - Springer Nature Limited CY - Heidelberg AN - OPUS4-56093 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Knigge, Xenia A1 - Andresen, Elina A1 - Resch-Genger, Ute A1 - Cant, D.J.H. A1 - Shard, A.G. A1 - Clifford, C.A. T1 - Composition, thickness, and homogeneity of the coating of core–shell nanoparticles—possibilities, limits, and challenges of X-ray photoelectron spectroscopy N2 - Core–shell nanoparticles have attracted much attention in recent years due to their unique properties and their increasing importance in many technological and consumer products. However, the chemistry of nanoparticles is still rarely investigated in comparison to their size and morphology. In this review, the possibilities, limits, and challenges of X-ray photoelectron spectroscopy (XPS) for obtaining more insights into the composition, thickness, and homogeneity of nanoparticle coatings are discussed with four examples: CdSe/CdS quantum dots with a thick coating and a small core; NaYF4-based upconverting nanoparticles with a large Yb-doped core and a thin Er-doped coating; and two types of polymer nanoparticles with a poly(tetrafluoroethylene) core with either a poly(methyl methacrylate) or polystyrene coating. Different approaches for calculating the thickness of the coating are presented, like a simple numerical modelling or a more complex simulation of the photoelectron peaks. Additionally, modelling of the XPS background for the investigation of coating is discussed. Furthermore, the new possibilities to measure with varying excitation energies or with hard-energy X-ray sources (hard-energy X-ray photoelectron spectroscopy) are described. A discussion about the sources of uncertainty for the determination of the thickness of the coating completes this review. KW - X-ray spectroscopy KW - Nanoparticles KW - Spectroscopy / Instrumentation KW - Spectroscopy / Theory PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548305 DO - https://doi.org/10.1007/s00216-022-04057-9 VL - 414 IS - 15 SP - 4331 EP - 4345 PB - SpringerNature AN - OPUS4-54830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Cui A1 - Kitzmann, W.R. A1 - Weigert, Florian A1 - Förster, Ch. A1 - Wang, X. A1 - Heintze, K. A1 - Resch-Genger, Ute T1 - Matrix Effects on Photoluminescence and Oxygen Sensitivity of a Molecular Ruby N2 - The molecular ruby analogue [Cr(ddpd)2]3+ (ddpd=N,N’-dimethyl-N,N’-dipyridine-2-ylpyridine-2,6-diamine) exhibits near infrared (NIR) emission with a high photoluminescence (PL) quantum yield ΦPL of 11 % and a lifetime of 898 μs in deaerated water at room temperature. While ligand-based control of the photophysical properties has received much attention, influences of the counter anions and microenvironment are still underexplored. In this study, the luminescence properties of the molecular ruby were systematically examined for the counter anions Cl−, Br−, [BF4]−, [PF6]−, [BPh4]−, and [BArF24]− in acetonitrile (MeCN) solution, in crystals, and embedded into polystyrene nanoparticles (PSNP). Stern-Volmer analyses of the oxygen quenching studies in the intensity and lifetime domain showed the highest oxygen sensitivity of the complexes with the counter anions of [BF4]− and [BArF24]−, which also revealed the longest luminescence lifetimes. Embedding [Cr(ddpd)2][PF6]3 in PSNPs and shielding with poly(vinyl alcohol) yields a strongly NIR-emissive oxygen-insensitive material with a record ΦPL of 15.2 % under ambient conditions. KW - Fluorescence KW - Sensor KW - Oxygen KW - Quantum yield KW - Quality assurance KW - Complex KW - Cr(III) KW - Lifetime KW - Ligand KW - Solid state KW - X-Ray analysis KW - Structure-property relationship KW - Nano KW - Polymer KW - Particle PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546057 DO - https://doi.org/10.1002/cptc.202100296 SN - 2367-0932 VL - 6 IS - 6 SP - 1 EP - 9 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fontoura Barroso, Daniel A1 - Epple, Niklas A1 - Niederleithinger, Ernst T1 - A Portable Low-Cost Ultrasound Measurement Device for Concrete Monitoring N2 - This paper describes a new ultrasonic measuring device called “W-Box”. It was developed based on the requirements of the DFG Forschergruppe (research unit) CoDA for a portable device for monitoring of concrete specimens, models and actual structures using embedded ultrasonic transducers as well as temperature and humidity sensors. The W-Box can send ultrasonic pulses with a variable frequency of 50–100 kHz to one selectable transducer and records signals from up to 75 multiplexed channels with a sample rate of 1 MHz and a resolution of 14 bits. In addition, it measures temperature and humidity with high accuracy, adjustable amplification, restarts automatically after a power failure and can be fully controlled remotely. The measured data are automatically stored locally on-site data quality checks and transferred to remote servers. The comparison of the W-Box with a laboratory setup using commercial devices proves that it is equally reliable and precise, at much lower cost. The W-Box also shows that their measurement capacities, with the used embedded ultrasonic transducers, can reach above 6 m in concrete. KW - Low-cost KW - Coda wave interferometry KW - Ultrasound KW - IoT KW - Non-destructive testing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546756 DO - https://doi.org/10.3390/inventions6020036 SN - 2411-5134 VL - 6 IS - 2 SP - 1 EP - 17 PB - MDPI CY - Basel, Switzerland AN - OPUS4-54675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Bühling, Benjamin A1 - Niederleithinger, Ernst T1 - Low frequency ultrasonic dataset for pulse echo object detection in an isotropic homogeneous medium as reference for heterogeneous materials in civil engineering N2 - The dataset presented contains ultrasonic data recorded in pulse echo mode. The investigated specimen is made of the isotropic homogeneous material polyamide and has a drill hole of constant diameter running parallel to the surface, which was scanned in a point grid using an automatic scanner system. At each measuring position, a pitch-catch measurement was performed using a sampling rate of 2 MHz. The probes used are arrays consisting of a spatially separated receiving and in-phase transmitting unit. The transmitting and receiving sides each consist of 12 point-shaped single probes. These dry-point contact (DPC) probes operate according to the piezoelectric principle at nominal frequencies of 55 kHz (shear waves) and 100 kHz (longitudinal waves), respectively, and do not require a coupling medium. The measurements are performed with longitudinal (100 kHz) and transverse (55 kHz) waves with different geometric orientations of the probe on the measurement surface. The data presented in the article provide a valid source for evaluating reconstruction algorithms for imaging in the low-frequency ultrasound range. KW - Non-destructive testing KW - Ultrasound KW - Pulse-echo method KW - Reference material KW - Reconstruction algorithm KW - Validation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547326 DO - https://doi.org/10.1016/j.dib.2022.108235 VL - 42 SP - 1 EP - 11 PB - Elsevier Inc. AN - OPUS4-54732 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholtz, Lena A1 - Eckert, J. G. A1 - Elahi, T. A1 - Lübkemann, F. A1 - Hübner, Oskar A1 - Bigall, N. C. A1 - Resch-Genger, Ute T1 - Luminescence encoding of polymer microbeads with organic dyes and semiconductor quantum dots during polymerization N2 - Luminescence-encoded microbeads are important tools for many applications in the life and material sciences that utilize luminescence detection as well as multiplexing and barcoding strategies. The preparation of such beads often involves the staining of premanufactured beads with molecular luminophores using simple swelling procedures or surface functionalization with layer-by-layer (LbL) techniques. Alternatively, these luminophores are sterically incorporated during the polymerization reaction yielding the polymer beads. The favorable optical properties of semiconductor quantum dots (QDs), which present broadly excitable, size-tunable, narrow emission bands and low photobleaching sensitivity, triggered the preparation of beads stained with QDs. However, the colloidal nature and the surface chemistry of these QDs, which largely controls their luminescence properties, introduce new challenges to bead encoding that have been barely systematically assessed. To establish a straightforward approach for the bead encoding with QDs with minimized loss in luminescence, we systematically assessed the incorporation of oleic acid/oleylamine-stabilized CdSe/CdS-core/shell-QDs into 0.5–2.5 μm-sized polystyrene (PS) microspheres by a simple dispersion polymerization synthesis that was first optimized with the organic dye Nile Red. Parameters addressed for the preparation of luminophore-encoded beads include the use of a polymer-compatible ligand such as benzyldimethyloctadecylammonium chloride (OBDAC) for the QDs, and crosslinking to prevent luminophore leakage. The physico-chemical and optical properties of the resulting beads were investigated with electron microscopy, dynamic light scattering, optical spectroscopy, and fluorescence microscopy. Particle size distribution, fluorescence quantum yield of the encapsulated QDs, and QD leaking stability were used as measures for bead quality. The derived optimized bead encoding procedure enables the reproducible preparation of bright PS microbeads encoded with organic dyes as well as with CdSe/CdS-QDs. Although these beads show a reduced photoluminescence quantum yield compared to the initially very strongly luminescent QDs, with values of about 35%, their photoluminescence quantum yield is nevertheless still moderate. KW - Polymerization KW - Quantum dots KW - Microbeads KW - Fluorescence PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553430 DO - https://doi.org/10.1038/s41598-022-16065-x SN - 2045-2322 VL - 12 SP - 1 EP - 16 PB - Nature Publishing Group CY - London AN - OPUS4-55343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Clark, P.C.J A1 - Andresen, Elina A1 - Sear, M. J. A1 - Favaro, M. A1 - Girardi, L. A1 - van de Krol, R. A1 - Resch-Genger, Ute A1 - Starr, D.E. T1 - Quantification of the Activator and Sensitizer Ion Distributions in NaYF4:Yb3+, Er3+ Upconverting Nanoparticles Via Depth-Profiling with Tender X-Ray Photoemission N2 - The spatial distribution and concentration of lanthanide activator and sensitizer dopant ions are of key importance for the luminescence color and efficiency of upconverting nanoparticles (UCNPs). Quantifying dopant ion distributions and intermixing, and correlating them with synthesis methods require suitable analytical techniques. Here, X-ray photoelectron spectroscopy depth-profiling with tender X-rays (2000–6000 eV), providing probe depths ideally matched to UCNP sizes, is used to measure the depth-dependent concentration ratios of Er3+ to Yb3+, [Er3+]/[Yb3+], in three types of UCNPs prepared using different reagents and synthesis methods. This is combined with data simulations and inductively coupled plasma-optical emission spectroscopy (ICP-OES) measurements of the lanthanide ion concentrations to construct models of the UCNPs’ dopant ion distributions. The UCNP sizes and architectures are chosen to demonstrate the potential of this approach. Core-only UCNPs synthesized with XCl3·6H2O precursors (β-phase) exhibit a homogeneous distribution of lanthanide ions, but a slightly surface-enhanced [Er3+]/[Yb3+] is observed for UCNPs prepared with trifluroacetate precursors (α-phase). Examination of Yb-core@Er-shell UCNPs reveals a co-doped, intermixed region between the single-doped core and shell. The impact of these different dopant ion distributions on the UCNP's optical properties is discussed to highlight their importance for UCNP functionality and the design of efficient UCNPs. KW - Shell KW - Nanomaterial KW - Nano KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Excitation power density KW - Surface KW - Coating KW - Core-shell KW - XPS KW - Intermixing KW - HAXPES KW - Method PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552075 DO - https://doi.org/10.1002/smll.202107976 SN - 1613-6813 SP - 1 EP - 13 PB - Wiley-VCH-Verlag CY - Weinheim, Germany AN - OPUS4-55207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kader, A. A1 - Kaufmann, Jan Ole A1 - Mangarova, D. B. A1 - Moeckel, J. A1 - Brangsch, J. A1 - Adams, L. C. A1 - Zhao, J. A1 - Reimann, C. A1 - Saatz, Jessica A1 - Traub, Heike A1 - Buchholz, R. A1 - Karst, U. A1 - Hamm, B. A1 - Makowski, M. R. T1 - Iron Oxide Nanoparticles for Visualization of Prostate Cancer in MRI N2 - Prostate cancer (PCa) is one of the most common cancers in men. For detection and diagnosis of PCa, non-invasive methods, including magnetic resonance imaging (MRI), can reduce the risk potential of surgical intervention. To explore the molecular characteristics of the tumor, we investigated the applicability of ferumoxytol in PCa in a xenograft mouse model in two different tumor volumes, 500 mm3 and 1000 mm3. Macrophages play a key role in tumor progression, and they are able to internalize iron-oxide particles, such as ferumoxytol. When evaluating T2*-weighted sequences on MRI, a significant decrease of signal intensity between pre- and post-contrast images for each tumor volume (n = 14; p < 0.001) was measured. We, furthermore, observed a higher signal loss for a tumor volume of 500 mm3 than for 1000 mm3. These findings were confirmed by histological examinations and laser ablation inductively coupled plasma-mass spectrometry. The 500 mm3 tumors had 1.5% iron content (n = 14; sigma = 1.1), while the 1000 mm3 tumors contained only 0.4% iron (n = 14; sigma = 0.2). In vivo MRI data demonstrated a correlation with the ex vivo data (R2 = 0.75). The results of elemental analysis by inductively coupled plasma-mass spectrometry correlated strongly with the MRI data (R2 = 0.83) (n = 4). Due to its long retention time in the blood, biodegradability, and low toxicity to patients, ferumoxytol has great potential as a contrast agent for visualization PCa. KW - Imaging KW - Nanoparticle KW - Cancer KW - Iron oxide KW - ICP-MS KW - Magnetic resonance imaging PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550075 DO - https://doi.org/10.3390/cancers14122909 VL - 14 IS - 12 SP - 1 EP - 13 PB - MDPI CY - Basel, Switzerland AN - OPUS4-55007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kromer, C. A1 - Schwibbert, Karin A1 - Gadicherla, A. K. A1 - Thiele, Dorothea A1 - Nirmalananthan-Budau, Nithiya A1 - Laux, P. A1 - Resch-Genger, Ute A1 - Luch, A. A1 - Tschiche, H. R. T1 - Monitoring and imaging pH in biofilms utilizing a fluorescent polymeric nanosensor N2 - Biofilms are ubiquitous in nature and in the man-made environment. Given their harmful effects on human health, an in-depth understanding of biofilms and the monitoring of their formation and growth are important. Particularly relevant for many metabolic processes and survival strategies of biofilms is their extracellular pH. However, most conventional techniques are not suited for minimally invasive pH measurements of living biofilms. Here, a fluorescent nanosensor is presented for ratiometric measurements of pH in biofilms in the range of pH 4.5–9.5 using confocal laser scanning microscopy. The nanosensor consists of biocompatible polystyrene nanoparticles loaded with pH-inert dye Nile Red and is surface functionalized with a pH-responsive fluorescein dye. Its performance was validated by fluorometrically monitoring the time-dependent changes in pH in E. coli biofilms after glucose inoculation at 37 °C and 4 °C. This revealed a temperature-dependent decrease in pH over a 4-h period caused by the acidifying glucose metabolism of E. coli. These studies demonstrate the applicability of this nanosensor to characterize the chemical microenvironment in biofilms with fluorescence methods. KW - Dye KW - Fluorescence KW - Signal enhancement KW - Sensor KW - Quantum yield KW - Synthesis KW - Nanoparticle KW - Nano KW - Polymer KW - Ph KW - Biofilm KW - MIC KW - Corrosion KW - Microorganism KW - Bacteria PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550751 DO - https://doi.org/10.1038/s41598-022-13518-1 SN - 2045-2322 VL - 12 IS - 1 SP - 1 EP - 10 PB - Nature Publishing Group CY - London AN - OPUS4-55075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Biesen, L. A1 - Krenzer, J. A1 - Nirmalananthan-Budau, Nithiya A1 - Resch-Genger, Ute A1 - Müller, Th. J. J. T1 - Asymmetrically bridged aroyl-S,N-ketene acetalbased multichromophores with aggregationinduced tunable emission N2 - Asymmetrically bridged aroyl-S,N-ketene acetals and aroyl-S,N-ketene acetal multichromophores can be readily synthesized in consecutive three-, four-, or five-component syntheses in good to excellent yields by several successive Suzuki-couplings of aroyl-S,N-ketene acetals and bis(boronic)acid esters. Different aroyl-S,N-ketene acetals as well as linker molecules yield a library of 23 multichromophores with substitution and linker pattern-tunable emission properties. This allows control of different communication pathways between the chromophores and of aggregation-induced emission (AIE) and energy transfer (ET) properties, providing elaborate aggregation-based fluorescence switches. KW - Dye KW - Aggregation KW - Aggregation induced emission KW - Signal enhancement KW - Energy transfer KW - Switch KW - Sensor KW - Quantum yield KW - Lifetime KW - Photophysics KW - Sythesis KW - Nanaoparticle PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550719 DO - https://doi.org/10.1039/d2sc00415a VL - 13 SP - 5374 EP - 5381 PB - Royal Society of Chemistry AN - OPUS4-55071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Golusda, L. A1 - Kühl, A. A. A1 - Lehmann, M. A1 - Dahlke, K. A1 - Mueller, S. A1 - Boehm-Sturm, P. A1 - Saatz, Jessica A1 - Traub, Heike A1 - Schnorr, J. A1 - Freise, C. A1 - Taupitz, M. A1 - Biskup, K. A1 - Blanchard, V. A1 - Klein, O. A1 - Sack, I. A1 - Siegmund, B. A1 - Paclik, D. T1 - Visualization of inflammation in experimental colitis by magnetic resonance imaging using very small superparamagnetic iron oxide particles N2 - Inflammatory bowel diseases (IBD) comprise mainly ulcerative colitis (UC) and Crohn´s disease (CD). Both forms present with a chronic inflammation of the (gastro) intestinal tract, which induces excessive changes in the composition of the associated extracellular matrix (ECM). In UC, the inflammation is limited to the colon, whereas it can occur throughout the entire gastrointestinal tract in CD. Tools for early diagnosis of IBD are still very limited and highly invasive and measures for standardized evaluation of structural changes are scarce. To investigate an efficient non-invasive way of diagnosing intestinal inflammation and early changes of the ECM, very small superparamagnetic iron oxide nanoparticles (VSOPs) in magnetic resonance imaging (MRI) were applied in two mouse models of experimental colitis: the dextran sulfate sodium (DSS)-induced colitis and the transfer model of colitis. For further validation of ECM changes and inflammation, tissue sections were analyzed by immunohistochemistry. For in depth ex-vivo investigation of VSOPs localization within the tissue, Europium-doped VSOPs served to visualize the contrast agent by imaging mass cytometry (IMC). VSOPs accumulation in the inflamed colon wall of DSS-induced colitis mice was visualized in T2* weighted MRI scans. Components of the ECM, especially the hyaluronic acid content, were found to influence VSOPs binding. Using IMC, colocalization of VSOPs with macrophages and endothelial cells in colon tissue was shown. In contrast to the DSS model, colonic inflammation could not be visualized with VSOP-enhanced MRI in transfer colitis. VSOPs present a potential contrast agent for contrast-enhanced MRI to detect intestinal inflammation in mice at an early stage and in a less invasive manner depending on hyaluronic acid content. KW - Inflammation KW - Imaging KW - Immunohistochemistry KW - MRI KW - Nanoparticle KW - Extracellular matrix KW - Laser ablation KW - ICP-MS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555395 DO - https://doi.org/10.3389/fphys.2022.862212 SN - 1664-042X VL - 13 IS - July 2022 SP - 1 EP - 15 PB - Frontiers Research Foundation CY - Lausanne AN - OPUS4-55539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Diewald, F. A1 - Epple, Niklas A1 - Kraenkel, T. A1 - Gehlen, C. A1 - Niederleithinger, Ernst T1 - Impact of External Mechanical Loads on Coda Waves in Concrete N2 - During their life span, concrete structures interact with many kinds of external mechanical loads. Most of these loads are considered in advance and result in reversible deformations. Nevertheless, some of the loads cause irreversible, sometimes unnoticed changes below the macroscopic scale depending on the type and dimension of the impact. As the functionality of concrete structures is often relevant to safety and society, their condition must be known and, therefore, assessed on a regular basis. Out of the spectrum of non-destructive monitoring methods, Coda Wave Interferometry using embedded ultrasonic sensors is one particularly sensitive technique to evaluate changes to heterogeneous media. However, there are various influences on Coda waves in concrete, and the interpretation of their superimposed effect is ambiguous. In this study, we quantify the relations of uniaxial compression and uniaxial tension on Coda waves propagating in normal concrete. We found that both the signal correlation of ultrasonic signals as well as their velocity variation directly reflect the stress change in concrete structures in a laboratory environment. For the linear elastic range up to 30% of the strength, we calculated a velocity variation of −0.97‰/MPa for compression and 0.33%/MPa for tension using linear regression. In addition, these parameters revealed even weak irreversible changes after removal of the load. Furthermore, we show the time-dependent effects of shrinkage and creep on Coda waves by providing the development of the signal parameters over time during half a year together with creep recovery. Our observations showed that time-dependent material changes must be taken into account for any comparison of ultrasonic signals that are far apart in time. The study’s results demonstrate how Coda Wave Interferometry is capable of monitoring stress changes and detecting even small-size microstructural changes. By indicating the stated relations and their separation from further impacts, e.g., temperature and moisture, we anticipate our study to contribute to the qualification of Coda Wave Interferometry for its application as an early-warning system for concrete structures. KW - Ultrasound KW - Coda Wave Interferometry (CWI) KW - Mechanical Load KW - Microstructure KW - Concrete PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556878 DO - https://doi.org/10.3390/ma15165482 SN - 1996-1944 VL - 15 IS - 16 SP - 1 EP - 15 PB - MDPI AN - OPUS4-55687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Niederleithinger, Ernst T1 - Practical procedure for the precise measurement of geometrical tendon positions in concrete with ultrasonic echo N2 - Existing concrete structures were usually designed for lifetimes of several decades. The current and urgently required efforts to increase sustainability and protect the environment will likely result in extended service lives up to 100 years. To achieve such objectives, it is required to assess structures over their entire lifecycles. Non-destructive testing (NDT) methods can reliably support the assessment of existing structures during the construction, operational, and decommissioning phases. One of the most important and safety-relevant components of a prestressed concrete structure are the tendons. NDT methods such as the ultrasonic echo method are suitable for both the detection and the localization of the tendons, i.e., the measurement of their geometrical position inside the component. The uniqueness of structures, concrete heterogeneity, and varying amounts of secondary components such as the reinforcement represent obstacles in the application of these methods in practice. The aim of this contribution is to demonstrate a practicable procedure, that can be used in the field to determine the parameters required for the measuring data analysis without extensive knowledge about the investigated components. For this purpose, a polyamide reference specimen is used to show which steps are required to obtain reliable imaging information on the position of tendons from the measurement data. The procedure is then demonstrated on a concrete test specimen that covers various relevant and practice-oriented test scenarios, such as varying tendon depths and component thicknesses. T2 - International Conference on Concrete Repair, Rehabilitation and Retrofitting (ICCRRR 2022) CY - Cape Town, South Africa DA - 03.10.2022 KW - Validation KW - Non-destructive testing KW - Ultrasonic KW - Reconstruction KW - Concrete KW - Tendon duct PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559979 DO - https://doi.org/10.1051/matecconf/202236403007 SN - 2261-263X SP - 1 EP - 8 AN - OPUS4-55997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Avci, Fatma T1 - Characterization of black mass by X-Ray fluorescence spectroscopy N2 - X-ray fluorescence analysis (XRF) is a method of elemental analysis that is used either as wavelength dispersive XRF (WDXRF) or energy dispersive XRF (EDXRF). Using EDXRF, it is possible to analyze samples within a few minutes without time-consuming sample preparation. This makes the method potentially suitable for analyzing larger sample quantities under industrial conditions. However, the XRF method is matrix-dependent. Depending on the cathode material of the recycled batteries, there are significant differences in the composition of the resulting black mass. This means that specific calibration models must be developed for different types of black mass. The aim of our work is to use the EDXRF method to reliably analyze black mass of different origins with regard to the elements that are particularly interesting for recycling: nickel (Ni), manganese (Mn), cobalt (Co), aluminum (Al), iron (Fe), zinc (Zn), silicon (Si), copper (Cu), and phosphorus (P). Based on the different mass fractions of the elements mentioned, black masses from used lithium-ion batteries can be divided into three groups according to the cathode chemistry: lithium nickel manganese cobalt oxide (NMC), lithium cobalt oxide (LCO), and mixed chemistries (MC), the latter of which may contain lithium iron phosphate (LFP). The division into groups is necessary to determine the matrices and thus select the appropriate calibration model for the analysis of the EDXRF data in order to achieve the most accurate determination of the elemental content possible. Reference analyses are performed using WDXRF. The score plots obtained by PLS-DA of the specific elemental composition of the black masses examined to date by both WDXRF and EDXRF reveal a correct separation of the BM matrix types LCO, NMC, and MC. Our preliminary results with test samples yielded 100 % correct predictions with both data sets. However, only two matrix types, NMC and LCO, have been tested with the EDXRF data so far. Data for MC is pending as work progresses. T2 - Doctoral seminar 2025 - Working Group Chemometrics and Quality Assurance (GDCh) CY - Hamburg, Germany DA - 11.09.2025 KW - Black Mass KW - XRF Spectroscopy KW - Chemometric Modeling KW - PLS-DA PY - 2025 AN - OPUS4-64095 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Current status of monitoring of PFAS release from industrial facilities N2 - Increasing studies report per- and polyfluoroalkyl substances (PFAS) in the ambient air and emissions from diverse industrial sources. Therefore, a comprehensive framework for characterizing PFAS emissions by identifying source-specific chemical fingerprints, evaluating emission pathways and assessing the impact of remediation technologies is needed. Depending on the type of PFAS, dedicated sampling and analytical procedures are required. Here, also the detection of possible PFAS transformation products, so-called products of incomplete combustion (PICs) are more mobile or toxic, is also of great interest to evaluate these technologies in terms of mineralisation potential and fluorine mass balance. T2 - PFAS study and technical exchange tour of MEE-FECO in Germany CY - Online meeting DA - 12.09.2025 KW - Per- and polyfluoroalkyl substances (PFAS) KW - Incineration PY - 2025 AN - OPUS4-64081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Yi T1 - MicroPhase: An Open-Source Flexible Ultrasonic Phased Array Based on Microcontrollers N2 - The use of resonant acoustic fields has gained significant attention due to their capability for contactless manipulation of objects in the open air and other media, referred to as ultrasonic levitation. To overcome the limitations in air-coupling efficiency, Langevin-type ultrasonic transducers are often employed, as they can operate at relatively high power, ranging from several tens to thousands of watts. However, such platforms typically lack the ability to move acoustically trapped objects efficiently, often requiring additional mechanical structures for even basic motion control, such as translation. In contrast, ultrasonic phased arrays offer clear advantages by leveraging their inherent beam-forming capabilities, which allows for dynamic shaping of acoustic fields in situ. Unfortunately, phased array control systems are not readily accessible, particularly when specific geometric or performance criteria must be met. Most commercially available phased array controllers are designed to operate in the MHz range; those are suitable only for high acoustic impedance media, such as water. Conversely, platforms for open-air applications typically utilize ultrasonic speakers operating at 40 kHz. In both cases, these systems are built on field-programmable gate arrays (FPGAs). However, interfacing FPGAs with computers and developing FPGA firmware (e.g., in VHDL) can be technically demanding, and analog components such as power amplifiers further complicate the system design. These limitations severely restrained the use of flexible ultrasonic levitations in analytical chemistry. Here, we present a novel platform for controlling ultrasonic phased arrays using single modern microcontrollers. This platform leverages the connectivity features of microcontrollers, allowing straightforward interfacing with computers via common programming languages (e.g., Python). The system employs fast direct memory access (DMA) to control up-to 256 ultrasonic transducers with a resolution of 0.5 µs, which is suitable for air-based applications in the 20-50 kHz range. Additionally, the platform can interface with traditional Langevin-type transducers, enabling their conversion into phased arrays. Optical characterization of acoustic field optimization is also discussed. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Acoustic ion manipulation PY - 2025 AN - OPUS4-64112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Yi T1 - Acoustic Ion Manipulation (AIM) N2 - The precise control of gaseous ions is a cornerstone in ion-based spectrometry and other disciplines such as materials processing. Traditional high-pressure ion optics rely on electrostatic and magnetic fields that often demand the use of intense electric fields, radio frequency activation, complex geometrical arrangements, or partially transmissive grids. Consequently, the efficiencies of such devices tend to be low or they require large footprints, as ion motions under ambient conditions are governed aerodynamically by collisions and fluid dynamics. However, from a different perspective and holistic reasoning, the limitations posed by collisions, aerodynamics, and other factors that hinder ion control in the open-air suggested an innovative direction for ion manipulation. Our study introduces a novel method that employs low-power standing acoustic waves to effectively manipulate ion beams. We observe that ions distinctively prefer traveling through areas of static pressure within the acoustic field, identified as "nodes." In contrast, neutral gases are unaffected by the acoustic field structure and continue to move along a straight trajectory. We have named this method Acoustic Ion Manipulation (AIM). Initial studies demonstrated selective and efficient manipulations of ion with AIM, including gating, redirection, regional dispersion, and focusing. This technique broadens the scope of ion manipulation strategies at high pressures while enriching our fundamental understanding of ion-acoustic kinetics. The potential applications of this method are vast, promising significant advancements in the fields of analytical chemistry, environmental science, and beyond. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Acoustic ion manipulation KW - Mass spectrometry PY - 2025 AN - OPUS4-64110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blume, Simon T1 - Femtosecond Laser-induced XUV Spectroscopy (LIXS) for Elemental Analysis N2 - In a typical laser-induced breakdown spectroscopy (LIBS) setup, emissions from collisional excitation of the atoms in the later stages of the plasma are detected and provide information about the elemental fingerprint of the sample. However, precise measurements, in particular quantification efforts, suffer from fluctuations of the intensity of the detected emission lines due to matrix effects and plasma-flicker noise, as well as significant background noise. In contrast, the early stages of the plasma are dominated by electron-ion recombination and Bremsstrahlung, which lead to sharp and intense x-ray emissions with consistent intensity profiles between laser pulses and suppressed background noise, therefore improving the limit of detection, especially for lighter elements. These emissions are detected in laser-induced XUV spectroscopy (LIXS).[1] Introduction of a femtosecond laser (pulse length ~100 fs) to the LIXS setup fundamentally changes the laser energy absorption and ablation process. The laser pulse energy is absorbed and redistributed by multiphoton absorption and inverse Bremsstrahlung and operates on a time frame faster than the plasma formation. Additionally, the plasma formation itself is accelerated leading to signal generation in the XUV-range before generation of the undesired background emissions. Thus, utilization of a femtosecond laser allows for further suppression of broadband emissions from the plasma allowing for sharper separation of the emission lines and improved limit of detection. This work presents the results of the combination of a LIXS setup with a femtosecond laser and assess the capabilities of this system with a model sample of cathode material from a spent lithium-ion battery. T2 - AMACEE 2025 CY - Brno, Czech Republic DA - 26.8.2025 KW - LIXS KW - Femtosecond laser KW - Instrumentation PY - 2025 AN - OPUS4-64118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sarif, Raduan A1 - Tiebe, Carlo A1 - Herglotz, Christian T1 - Early Response Prediction for H2 Sensors N2 - Green hydrogen (H2) is essential for the global transition to clean energy; it will significantly reduce emissions from heavy industry and the long-distance transport system. H2 can be used as fuel in fuel cells, storing surplus renewable energy, and as a feedstock in industrial processes. However, H2 faces significant safety challenges during storage and transportation. Accidents due to H2 leakage and explosions raise serious concerns due to its high flammability, rapid diffusion in air, and extremely low ignition energy. To mitigate risks associated with H2 leakages, reliable and automated H2 safety systems are essential for emergency repairs or shutdown. An early response from H2 sensors is crucial for early warning in accidents. The earlier response time of H2 sensors is often constrained by their sensor principle, which is heavily influenced by the sensor material’s properties. This study explores methods for earlier sensor response through predictive algorithms. Specifically, we investigate transient response predictions using a First-Order (FO) model and propose improvements through the First-Order with early response and the First-Order with adapted early response model. Both models can predict the stable value of the H2 sensor response from a small time window, which is 70.89% and 83.72% earlier, respectively, than the time required for the sensor hardware to reach it physically. The model’s performance is evaluated by calculating the fitting error with a 2 % threshold. Our current research lays the groundwork for future advancements in real-time sensor response predictions for hydrogen leakage. T2 - IARIA Congress 2025 : The 2025 IARIA Annual Congress on Frontiers in Science, Technology, Services, and Applications CY - Venice, Italy DA - 06.07.2025 KW - H2 Safety KW - H2 leakage detection KW - First-Order (FO) model KW - H2 Sensor data analysis KW - H2 sensor response predictions PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640676 UR - https://www.thinkmind.org/articles/iaria_congress_2025_1_250_50159.pdf SN - 978-1-68558-284-5 SP - 1 EP - 8 PB - IARIA Press CY - Wilmington AN - OPUS4-64067 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Classification of mineral wool by spectroscopic methods N2 - Mineral wools from demolition projects are currently disposed of in landfills. To reintroduce them into the material cycle, it is essential (i) to distinguish between glass wool (GW) and rock wool (RW), (ii) to detect foreign substances, and (iii) to assess the period of production (before/after 2000) to identify “old”, potentially carcinogenic wool. Both X-ray and NIR spectroscopic methods are being developed for this purpose and handheld (portable) devices are being tested for field application. To this end, more than 160 mineral wool samples were collected and examined. Since no reference information on the “material” or “age” was available for many samples, we characterized the elemental composition of the mineral wool using wavelength dispersive X-ray fluorescence spectroscopy (WDXRF). For this purpose, pellets and melt tablets were evaluated using a spectrometer-integrated semi-quantitative approach (Omnian). The resulting mass fractions of SiO2, Al2O3, CaO, MgO, K2O, Na2O, Fe2O3, and TiO2 could be used to distinguish between GW and RW and, in the case of RW, also whether it was “old” or “new” wool according to VDI guideline 3492. In some cases, however, ambiguous results were obtained in the material classification. Therefore, a principal component analysis (PCA) was performed enabling the identification of possible outliers and subgroups. Since the classification of “old” and “new” rock wool based on VDI 3492 yielded many unclear results, with the help of partial least squares discriminant analysis (PLS-DA), the classification was significantly improved [1]. WDXRF spectroscopy delivers accurate results, however, the spectrometers are not mobile and require time demanding sample preparation (pellets, melt tablets). Therefore, it was examined whether useful results could be achieved with portable energy dispersive (EDXRF) spectrometers. For this purpose, a portable EDXRF spectrometer (pXRF) was calibrated based on the WDXRF results. In general, oxides of the lighter elements (MgO and Na2O) could not be analyzed with EDXRF. Although prediction of oxide contents in melt tablets was successful by this approach, no reliable results could be obtained when predicting the oxide content of natural mineral wools. Attempts to perform calibration based on natural wools also failed. However, PCA of EDXRF spectra in the “Light” range was able to distinguish between GW and RW, even with “real-world” samples from so-called Bigbags [2], in which mineral wool in Germany is collected in recycling centers. In addition to XRF, a previous study has already demonstrated that at least the distinction between GW and RW can be performed using near-infrared spectroscopy (NIR) [3]. For this reason, measurements were also carried out with a handheld NIR device (pNIR) in parallel with the pXRF investigations. Using PLS-DA, it was possible to classify RW and GW using the handheld device with a sensitivity and specificity of 95% for 38 test samples, including wool from big bags. pNIR also remains sensitive when it comes to determining non-metallic “foreign materials.” For example, materials such as brick, plaster, concrete, and organic fibers could be detected by SIMCA as “non-mineral” wool with a specificity of 92% for 19 tested interferents [2]. Questions regarding the detection of metallic impurities based on EDXRF measurements are the subject of ongoing investigations. T2 - Doctoral Seminar of the Working Group Chemometrics & Quality Assurance CY - Hamburg, Germany DA - 10.09.2025 KW - Mineral wool KW - X-ray fluorescence KW - Data analyis PY - 2025 AN - OPUS4-64077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Denißen, M. A1 - Nirmalananthan-Budau, Nithiya A1 - Behnke, Thomas A1 - Hoffmann, Katrin A1 - Resch-Genger, Ute A1 - Müller, T. J. J. T1 - 3-Piperazinyl propenylidene indolone merocyanines: consecutive three-component synthesis and electronic properties of solid-state luminophores with AIE properties N2 - A series of twelve 3-piperazinyl propenylidene indolone merocyanines was synthesized in a one-pot fashion using a consecutive three-component insertion-coupling-Michael addition sequence. Physicalorganic treatment of the absorption data of a consanguineous series of this library allows semiquantitative Linear Free Energy Relationships (LFERs) to be established and confirmation of the positive Absorption solvatochromicity. All Boc-substituted piperazinyl merocyanines display aggregation induced Emission (AIE), which was corroborated for two solvent systems. In particular, crystallization-induced Emission enhancement (CIEE) induced by ultrasonication could be shown for a model chromophore by confocal laser scanning microscopy (CLSM). KW - Indolone merocyanines KW - AIE KW - CIEE KW - CLSM PY - 2017 DO - https://doi.org/10.1039/c7qm00198c SN - 2052-1537 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. VL - 1 IS - 10 SP - 2013 EP - 2026 AN - OPUS4-43213 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ramirez, Alejandra A1 - Pauli, Jutta A1 - Crasselt, C. A1 - Simon, S. A1 - Schmidt, W. A1 - Resch-Genger, Ute T1 - The effect of a polycarboxylate ether on C3A / CaSO4.2H2O passivation monitored by optical spectroscopy N2 - Polycarboxylate ethers (PCEs) are widely used in construction, but the exact nature of their interaction with cement is still debated. Aiming at a better understanding of the role of tricalcium Aluminate (C3A) in cement hydration, we assessed the potential of optical spectroscopy in combination with a water-soluble fluorescent organic reporter dye (S0586) to monitor the early hydration of C3A in the presence of 26 wt% CaSO4.2H2O (C3A26G-S) with and without PCE. As optical methods, steady-state fluorescence and diffuse reflectance (UV–VisDR) spectroscopy were employed. Phase characterization and particle size distribution were performed with in-situ X-ray diffraction (in-situ XRD) and dynamic light scattering (DLS). Our results show that fluorescence and UV–VisDR spectroscopy can be used to monitor the formation of metastable phases by the disaggregation of the dye S0586 in a cement paste as well as changes in ettringite formation. Addition of PCE slowed down the disaggregation of the dye as reflected by the corresponding changes of the dyes absorption and fluorescence. This prolonged induction period is a well-known side effect of PCEs and agrees with previous reported calorimetric studies and the Inhibition of gypsum dissolution observed by in-situ XRD. This demonstrates that fluorescence and UV–VisDR spectroscopy together with a suitable optical probe can provide deeper insights into the influence of PCE on C3A-gypsum hydration which could be e.g., utilized as screening method for comparing the influences of different types of PCEs. KW - Fluorescence KW - Cement KW - Nano KW - Particle KW - Optical spectroscopy KW - PCE KW - XRD KW - Calorimetry KW - Monitoring KW - Diffuse KW - Reflection KW - Phase KW - Dye KW - Optical probe KW - Cyanine KW - Sensor KW - Method KW - Analysis PY - 2020 DO - https://doi.org/10.1016/j.conbuildmat.2020.121856 VL - 270 SP - 121856 PB - Elsevier Ltd. AN - OPUS4-52118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Löhr, Konrad A1 - Traub, Heike A1 - Wanka, Antje Jutta A1 - Panne, Ulrich A1 - Jakubowski, Norbert T1 - Quantification of metals in single cells by LA-ICP-MS: Comparison of single spot analysis and imaging N2 - LA-ICP-MS is increasingly used for single cell analysis in two different detection modes using either the imaging mode with subcellular resolution or alternatively single spot analysis of cells with a larger laser spot size. This study compares the analytical figures of merit of both detection modes (signal to noise, precision, accuracy, throughput), as well as ease of operation and data evaluation. Adherent 3T3 fibroblast cells were stained with two metal dyes (mDOTA-Ho, Ir-DNA-intercalator) and several dozen cells were measured using both modes. We found a ten times higher throughput for single spot analysis, which has as well a straightforward data analysis, shortening the total analysis time further. The signal to noise ratio for single spot analysis was found to be slightly better compared to the signal to noise of pixels in imaging. The mean metal intensity per single cell differed by only 10% between both modes and obtained distributions were found to show no statistically significant differences. Using matrix matched calibration based on standards spotted onto nitrocellulose membrane, we achieved detection limits (10s) of 12 fg for Ir and 30 fg for Ho and quantified 57 +/-35 fg Ir and 1192 +/- 707 fg Ho per single cell. Compared to a conventional ICP-MS measurement of a digest of about 60000 cells, 54% of Ir content and 358% Ho content was found using quantitative LA-ICP-MS. The difference might be a consequence of the two metal dyes binding to different structures of the cell and therefore might behave differently in sample preparation for conventional and LA-ICP-MS. KW - Cells KW - Laser ablation KW - ICP-MS KW - Metals KW - Quantification PY - 2018 DO - https://doi.org/10.1039/c8ja00191j SN - 0267-9477 VL - 33 IS - 9 SP - 1579 EP - 1587 PB - RSC Royal Society of Chemistry CY - London AN - OPUS4-46441 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Loehr, Konrad A1 - Jakubowski, Norbert A1 - Wanka, Antje Jutta A1 - Traub, Heike A1 - Panne, Ulrich T1 - Quantification of metals in single cells by LA-ICP-MS comparison of single spot analysis and imaging N2 - LA-ICP-MS is increasingly used for single cell analysis in two different detection modes using either the imaging mode with subcellular resolution or alternatively single spot analysis of cells with a larger laser spot size. This study compares the analytical figures of merit of both detection modes (signal to noise, precision, accuracy, throughput), as well as ease of operation and data evaluation. Adherent 3T3 fibroblast cells were stained with two metal dyes (mDOTA-Ho, Ir-DNA-intercalator) and several dozen cells were measured using both modes. We found a ten times higher throughput for single spot analysis, which has as well a straightforward data analysis, shortening the total analysis time further. The signal to noise ratio for single spot analysis was found to be slightly better compared to the signal to noise of pixels in imaging. The mean metal intensity per single cell differed by only 10% between both modes and obtained distributions were found to show no statistically significant differences. Using matrix matched calibration based on standards spotted onto nitrocellulose membrane, we achieved detection limits (10 σ) of 12 fg for Ir and 30 fg for Ho and quantified 57 ± 35 fg Ir and 1,192 ± 707 fg Ho per single cell. Compared to a conventional ICP-MS measurement of a digest of ~60,000 cells, 54 % of Ir content and 358 % Ho content was found using quantitative LA-ICP-MS. The difference might be a consequence of the two metal dyes binding to different structures of the cell and therefore might behave differently in sample preparation for conventional and LA-ICP-MS. KW - Single cell analysis KW - LA-ICP-MS PY - 2018 DO - https://doi.org/10.1039/c8ja00191j SN - 0267-9477 SN - 1364-5544 VL - 33 IS - 9 SP - 1579 EP - 1587 PB - Royal Society of Chemistry AN - OPUS4-45903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Tobias A1 - Gornushkin, Igor B. T1 - Mass and mole fractions in calibration-free LIBS N2 - This technical note highlights the fact that CF-LIBS algorithms work in mole fractions, while results of spectrochemical analysis are usually reported in mass fractions or mass percent. Ignoring this difference and not converting mole fractions to mass fractions can lead to errors in reported concentrations determined by the CF-LIBS method and inadequate comparison of these concentrations with certified concentrations. Here, the key points of the CF-LIBS algorithm are reproduced and the formulae for converting a mole fraction to a mass fraction and vice versa are given. Several numerical examples are also given, which show that the greater the difference between the molar mass of an individual element in a sample and the average molar mass, the greater the discrepancy between the mole and mass fractions. KW - Spectroscopy KW - Analytical Chemistry KW - LIBS KW - Calibration PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598611 DO - https://doi.org/10.1039/d4ja00028e SN - 0267-9477 VL - 39 IS - 4 SP - 1030 EP - 1032 PB - Royal Society of Chemistry (RSC) AN - OPUS4-59861 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roebben, G. A1 - Kestens, V. A1 - Varga, Z. A1 - Charoud-Got, J. A1 - Ramaye, Y. A1 - Gollwitzer, Christian A1 - Bartczak, D. A1 - Geißler, Daniel A1 - Noble, J.E. A1 - Mazoua, S. A1 - Meeus, N. A1 - Corbisier, P. A1 - Palmai, M. A1 - Mihály, J. A1 - Krumrey, M. A1 - Davies, J. A1 - Resch-Genger, Ute A1 - Kumarswami, N. A1 - Minelli, C. A1 - Sikora, A. A1 - Goenaga-Infante, H. T1 - Reference materials and representative test materials to develop nanoparticle characterization methods: the NanoChOp project case N2 - This paper describes the production and characteristics of the nanoparticle test materials prepared for common use in the collaborative research project NanoChOp (Chemical and optical characterization of nanomaterials in biological systems), in casu suspensions of silica nanoparticles and CdSe/CdS/ZnS quantum dots (QDs). This paper is the first to illustrate how to assess whether nanoparticle test materials meet the requirements of a "reference material" (ISO Guide 30, 2015) or rather those of the recently defined category of "representative test material (RTM)" (ISO/TS 16195, 2013). The NanoChOp test materials were investigated with small-angle X-ray scattering (SAXS), dynamic light scattering (DLS), and centrifugal liquid sedimentation (CLS) to establish whether they complied with the required monomodal particle size distribution. The presence of impurities, aggregates, agglomerates, and viable microorganisms in the suspensions was investigated with DLS, CLS, optical and electron microscopy and via plating on nutrient agar. Suitability of surface functionalization was investigated with attenuated total reflection Fourier transform infrared spectrometry (ATR-FTIR) and via the capacity of the nanoparticles to be fluorescently labeled or to bind antibodies. Between-unit homogeneity and stability were investigated in terms of particle size and zeta potential. This paper shows that only based on the outcome of a detailed characterization process one can raise the status of a test material to RTM or reference material, and how this status depends on its intended use. KW - Nanoparticle KW - Materials characterization KW - Reference material KW - Analytical quality assurance KW - Metrology PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-349644 DO - https://doi.org/10.3389/fchem.2015.00056 SN - 2296-2646 VL - 3 SP - Article 56, 1 EP - 16 PB - Frontiers Media CY - Lausanne AN - OPUS4-34964 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niederleithinger, Ernst A1 - Wolf, Julia A1 - Mielentz, Frank A1 - Wiggenhauser, Herbert A1 - Pirskawetz, Stephan T1 - Embedded ultrasonic transducers for active and passive concrete monitoring N2 - Recently developed new transducers for ultrasonic transmission, which can be embedded right into concrete, are now used for non-destructive permanent monitoring of concrete. They can be installed during construction or thereafter. Large volumes of concrete can be monitored for changes of material properties by a limited number of transducers. The transducer design, the main properties as well as installation procedures are presented. It is shown that compressional waves with a central frequency of 62 kHz are mainly generated around the transducer's axis. The transducer can be used as a transmitter or receiver. Application examples demonstrate that the transducers can be used to monitor concrete conditions parameters (stress, temperature, …) as well as damages in an early state or the detection of acoustic events (e.g., crack opening). Besides application in civil engineering our setups can also be used for model studies in geosciences. KW - Ultrasound KW - Transmission KW - Concrete KW - Damages KW - Cracks KW - Stress KW - Monitoring KW - Acoustic emission KW - Transducers KW - Coda wave interferometry PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-345632 DO - https://doi.org/10.3390/s150509756 SN - 1424-8220 VL - 15 IS - 5 SP - 9756 EP - 9772 PB - MDPI CY - Basel AN - OPUS4-34563 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grohmann, Maria A1 - Müller, Sabine A1 - Niederleithinger, Ernst T1 - Reverse time migration: Introduction of a new imaging technique for ultrasonic measurements in civil engineering N2 - Ultrasonic echo testing is widely used in non-destructive testing in civil engineering to investigate concrete structures, to measure thickness, and to locate and characterise built-in components or inhomogeneities. Currently, synthetic aperture focusing techniques are mostly used for imaging. These algorithms are highly developed but have some limitations. For example, it is not possible to image the lower boundary of built-in components like tendon ducts or vertical reflectors. We adopted reverse time migration for non-destructive testing in civil engineering in order to improve the imaging of complicated structures in concrete. By using the entire wavefield, including waves reflected more than once, there are fewer limitations compared to synthetic aperture focusing technique algorithms. As a drawback, the required computation is significantly higher than that for the techniques currently used. Simulations for polyamide and concrete structures showed the potential for non-destructive testing. The simulations were followed by experiments at a polyamide specimen. Here, having acquired almost noise-free measurement data to test the algorithm, we were able to determine the shape and size of boreholes with sufficient accuracy. After these successful tests, we performed experiments at a reinforced concrete foundation slab. We obtained information from the data by reverse time migration, which was not accessible by traditional imaging. The imaging of the location and structure of the lower boundary of the concrete foundation slab was improved. Furthermore, vertical reflectors inside the slab were imaged clearly, and more flaws were found. It has been shown that reverse time migration is a step forward in ultrasonic testing in civil engineering. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - Ultrasound KW - Imaging KW - Reverse time migration KW - Reflection seismics KW - Concrete PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-345406 SN - 1435-4934 SP - 1 EP - 10 PB - Technische Universität Berlin / Bundesanstalt für Materialforschung und -prüfung AN - OPUS4-34540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niederleithinger, Ernst A1 - Abraham, O. A1 - Mooney, M. T1 - Geophysical methods in civil engineering: Overview and new concepts N2 - Geophysical methods have been used in civil engineering for decades. The main field of application is - to no surprise – in geotechnical projects from site characterization to foundation quality assurance. For more than 25 years, ground penetrating radar (GPR) and seismic methods have found applications in structural engineering. Recently introduced geophysical methods have been adopted to ultrasonic investigations in various fields. They help to improve the quality of structural imaging and to detect small changes in concrete. An overview of the history and current use of geophysics in civil engineering is given. Selected examples of new concepts include advances in wave based imaging, quality assurance for foundations, detecting small changes in concrete as well as moisture and corrosion detection are discussed. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - Nondestructive testing KW - Civil engineering KW - Geophysics PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-344666 UR - https://www.ndt.net/?id=18260 SN - 1435-4934 VL - 20 IS - 11 SP - 1 EP - 6 PB - NDT.net CY - Kirchwald AN - OPUS4-34466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Galindo Guerreros, Julio Cesar A1 - Niederleithinger, Ernst A1 - Mackens, S. A1 - Fechner, T. T1 - Quality assurance of jet grout columns with borehole seismic measurements N2 - Sealing and strengthening of the subsoil by injection is a major issue in the field of geotechnical engineering. One commonly applied method is jet grouting, which allows creating columns of grouted soil by eroding and mixing the in-situ soil with a thin cement suspension. A general difficulty linked with this method is to predict the resulting column diameter and its material strength. In this paper we illustrate the application of a newly developed non-destructive quality assurance testing tool used to determine the diameter of jet grout columns. This approach incorporates standard crosshole and downhole seismic measurements. To demonstrate its effectiveness, we tested the new approach within two-dimensional finite-difference numerical simulations. Additional field tests showed that this tool is also applicable in real site conditions. For this purpose, three jet grout columns were produced with different process parameters in a depth between 3.0 and 10 m. The evaluated diameters were within 1.0 and 1.5 m, slightly deviating from the previously predicted range by the jet grouting contractor. Moreover, we were able to detect the base of the columns at 10 m depth with no significant difficulties. On the other hand, unsaturated, partly unconsolidated sands between ground water level and surface considerably affected the seismic data, hence complicating the detection of the top of the columns. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - Jet grout KW - Seismics KW - Crosshole KW - Downhole PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-346753 UR - https://www.ndt.net/?id=18277 SN - 1435-4934 VL - 20 IS - 11 SP - 1 EP - 7 PB - NDT.net CY - Kirchwald AN - OPUS4-34675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niederleithinger, Ernst A1 - Wolf, Julia A1 - Mielentz, Frank A1 - Wiggenhauser, Herbert T1 - Using embedded ultrasonic sensors for active and passive concrete monitoring N2 - Challenging new constructions and ageing infrastructure are increasing the demand for permanent monitoring of loads and condition. Various methods and sensors are used for this purpose. But the technologies available today have difficulties in detecting slowly progressing locally confined damages. Extensive investigations or instrumentations are required so far for this purpose. In this study we present new sensors and data processing methods for ultrasonic transmission, which can be used for non-destructive long term monitoring of concrete. They can be mounted during construction or thereafter. Larger volumes can be monitored by a limited number of sensors for changes of material properties. The principles of ultrasonic transmission and influencing factors are presented. This latter include load, damages as well as environmental parameters as temperature or moisture. Various methods for data processing, e. g. coda wave interferometry are introduced. They allow the detection of very small changes in the medium. The embedded sensors are shown including mounting and operation. Application examples so far include small scale laboratory freeze-thaw experiments, localizing loads in larger concrete models, monitoring load effects on real structures as well as detecting acoustic events. Some sensors are operating already for several years. The sensors can be used as transmitter or receivers or switched between both roles. While most of the previous experiments have been active (at least one sensor serving as transmitter), new studies show that the sensors are useful as well for passive measurements, e. g. in acoustic emission or time reversal experiments. Besides application in civil engineering our setups can also be used for model studies in geosciences. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 15.09.2015 KW - SHM KW - Monitoring KW - Ultrasound concrete KW - Embedded sensors PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-344652 UR - http://www.ndt.net/?id=18408 SN - 1435-4934 VL - 20 IS - 11 SP - 1 EP - 4 PB - NDT.net CY - Kirchwald AN - OPUS4-34465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Levchuk, I. A1 - Würth, Christian A1 - Krause, F. A1 - Osvet, A. A1 - Batentschuk, M. A1 - Resch-Genger, Ute A1 - Kolbeck, C. A1 - Herre, P. A1 - Steinrück, H.P. A1 - Peukert, W. A1 - Brabec, C. J. T1 - Industrially scalable and cost-effective Mn2+ doped ZnxCd1-xS/ZnS nanocrystals with 70% photoluminescence quantum yield, as efficient down-shifting materials in photovoltaics N2 - We present colloidally stable and highly luminescent ZnxCd1_xS:Mn/ZnS core–shell nanocrystals (NCs) synthesized via a simple non-injection one-pot, two-step synthetic route, which can be easily upscaled. A systematic variation of the reaction component, parameters and thickness of the ZnS shell yielded doped nanocrystals with a very high photoluminescence quantum yield (pl) of 70%, which is the highest value yet reported for these Mn-doped sulfide-semiconductor NCs. These materials can be synthesized with high reproducibility in large quantities of the same high quality, i.e., the same pl using accordingly optimized reaction conditions. The application of these zero-reabsorption high quality NCs in the light conversion layers, deposited on top of a commercial monocrystalline silicon (mono-Si) solar cell, led to a significant enhancement of the external quantum efficiency (EQE) of this device in the ultraviolet spectral region between 300 and 400 nm up to ca. 12%. EQE enhancement is reflected by an increase in the power conversion efficiency (PCE) by nearly 0.5 percentage points and approached the theoretical limit (0.6%) expected from down-shifting for this Si solar cell. The resulting PCE may result in a BoM (bill of materials) cost reduction of app. 3% for mono-Si photovoltaic modules. Such small but distinct improvements are expected to pave the road for an industrial application of doped semiconductor NCs as cost-effective light converters for silicon photovoltaic (PV) and other optoelectronic applications. KW - photovoltaics KW - solar cell KW - photoluminescence quantum yield KW - nanocrystals PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-358594 DO - https://doi.org/10.1039/c5ee03165f VL - 9 SP - 1083 EP - 1094 PB - The Royal Society of Chemistry CY - Cambridge, England AN - OPUS4-35859 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Büchner, T. A1 - Drescher, D. A1 - Merk, V. A1 - Traub, Heike A1 - Guttmann, P. A1 - Werner, St. A1 - Jakubowski, Norbert A1 - Schneider, G. A1 - Kneipp, J. T1 - Biomolecular environment, quantification, and intracellular interaction of multifunctional magnetic SERS nanoprobes N2 - Multifunctional composite nanoprobes consisting of iron oxide nanoparticles linked to silver and gold nanoparticles, Ag–Magnetite and Au–Magnetite, respectively, were introduced by endocytic uptake into cultured fibroblast cells. The cells containing the non-toxic nanoprobes were shown to be displaceable in an external magnetic field and can be manipulated in microfluidic channels. The distribution of the composite nanostructures that are contained in the endosomal system is discussed on the basis of surfaceenhanced Raman scattering (SERS) mapping, quantitative laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) micromapping, and cryo soft X-ray tomography (cryo soft-XRT). Cryo soft-XRT of intact, vitrified cells reveals that the composite nanoprobes form intra-endosomal aggregates. The nanoprobes provide SERS signals from the biomolecular composition of their surface in the endosomal environment. The SERS data indicate the high stability of the nanoprobes and of their plasmonic properties in the harsh environment of endosomes and lysosomes. The spectra point at the molecular composition at the surface of the Ag–Magnetite and Au–Magnetite nanostructures that is very similar to that of other Composite structures, but different from the composition of pure silver and gold SERS nanoprobes used for intracellular investigations. As shown by the LA-ICP-MS data, the uptake efficiency of the magnetite composites is approximately two to three times higher than that of the pure gold and silver nanoparticles. KW - Nanoparticles KW - SERS KW - Cell KW - LA-ICP-MS KW - X-ray tomography PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-371811 DO - https://doi.org/10.1039/c6an00890a SN - 0003-2654 VL - 141 IS - 17 SP - 5096 EP - 5106 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-37181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, Ralf A1 - Weigert, Florian A1 - Lesnyak, V. A1 - Leubner, S. A1 - Lorenz, T. A1 - Behnke, Thomas A1 - Dubavik, A. A1 - Joswig, J.-O. A1 - Resch-Genger, Ute A1 - Gaponik, N. A1 - Eychmüller, A. ED - Resch-Genger, Ute ED - Schneider, Ralf T1 - pH and concentration dependence of the optical properties of thiol-capped CdTe nanocrystals in water and D2O N2 - The optical properties of semiconductor nanocrystals (SC NCs) are largely controlled by their size and surface chemistry, i.e., the chemical composition and thickness of inorganic passivation shells and the chemical nature and number of surface ligands as well as the strength of their bonds to surface atoms. The latter is particularly important for CdTe NCs, which – together with alloyed CdₓHg₁₋ₓTe – are the only SC NCs that can be prepared in water in high quality without the need for an additional inorganic passivation shell. Aiming at a better understanding of the role of stabilizing ligands for the control of the application-relevant fluorescence features of SC NCs, we assessed the influence of two of the most commonly used monodentate thiol ligands, thioglycolic acid (TGA) and mercaptopropionic acid (MPA), on the colloidal stability, photoluminescence (PL) quantum yield (QY), and PL decay behavior of a set of CdTe NC colloids. As an indirect measure for the strength of the coordinative bond of the ligands to SC NC surface atoms, the influence of the pH (pD) and the concentration on the PL properties of these colloids was examined in water and D₂O and compared to the results from previous dilution studies with a set of thiol-capped Cd₁₋ₓHgₓTe SC NCs in D₂O. As a prerequisite for these studies, the number of surface ligands was determined photometrically at different steps of purification after SC NC synthesis with Ellman’s test. Our results demonstrate ligand control of the pH-dependent PL of these SC NCs, with MPA-stabilized CdTe NCs being less prone to luminescence quenching than TGA-capped ones. For both types of CdTe colloids, ligand desorption is more pronounced in H₂O compared to D₂O, underlining also the role of hydrogen bonding and solvent molecules. KW - Quantum dots KW - Fluorescence KW - Ligand analysis KW - Nano particles PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-371253 DO - https://doi.org/10.1039/c6cp03123d VL - 18 IS - 28 SP - 19083 EP - 19092 PB - RSC CY - Cambridge AN - OPUS4-37125 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dackermann, U. A1 - Yu, Y. A1 - Niederleithinger, Ernst A1 - Li, J. A1 - Wiggenhauser, Herbert T1 - Condition Assessment of Foundation Piles and Utility Poles Based on Guided Wave Propagation Using a Network of Tactile Transducers and Support Vector Machines N2 - This paper presents a novel non-destructive testing and health monitoring system using a network of tactile transducers and accelerometers for the condition assessment and damage classification of foundation piles and utility poles. While in traditional pile integrity testing an impact hammer with broadband frequency excitation is typically used, the proposed testing system utilizes an innovative excitation system based on a network of tactile transducers to induce controlled narrow-band frequency stress waves. Thereby, the simultaneous excitation of multiple stress wave types and modes is avoided (or at least reduced), and targeted wave forms can be generated. The new testing system enables the testing and monitoring of foundation piles and utility poles where the top is inaccessible, making the new testing system suitable, for example, for the condition assessment of pile structures with obstructed heads and of poles with live wires. For system validation, the new system was experimentally tested on nine timber and concrete poles that were inflicted with several types of damage. The tactile transducers were excited with continuous sine wave signals of 1 kHz frequency. Support vector machines were employed together with advanced signal processing algorithms to distinguish recorded stress wave signals from pole structures with different types of damage. The results show that using fast Fourier transform signals, combined with principal component analysis as the input feature vector for support vector machine (SVM) classifiers with different kernel functions, can achieve damage classification with accuracies of 92.5% ± 7.5%. KW - Structural Health Monitoring KW - Non-Destructive Testing KW - Sensor network KW - Support vector machine KW - Utility poles PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-434868 UR - http://www.mdpi.com/1424-8220/17/12/2938 DO - https://doi.org/10.3390/s17122938 SN - 1424-8220 VL - 17 IS - 12 SP - Article 2938, 1 EP - 16 PB - MDPI CY - Basel, Schweiz AN - OPUS4-43486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niederleithinger, Ernst A1 - Wang, Xin A1 - Herbrand, M. A1 - Müller, M. T1 - Processing ultrasonic data by coda wave interferometry to monitor load tests of concrete beams N2 - Ultrasonic transmission measurements have been used for decades to monitor concrete elements, mostly on a laboratory scale. Recently, coda wave interferometry (CWI), a technique adapted from seismology, was introduced to civil engineering experiments. It can be used to reveal subtle changes in concrete laboratory samples and even large structural elements without having a transducer directly at the place where the change is taking place. Here, several load tests until failure on large posttensioned concrete beams have been monitored using networks of embedded transducers. To detect subtle effects at the beginning of the experiments and cope with severe changes due to cracking close to failure, the coda wave interferometry procedures had to be modified to an adapted step-wise approach. Using this methodology, we were able to monitor stress distribution and localize large cracks by a relatively simple technique. Implementation of this approach on selected real structures might help to make decisions in infrastructure asset management. KW - Ultrasound KW - Concrete KW - Monitoring KW - Coda wave interferometry KW - Embedded transducers PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-452328 DO - https://doi.org/10.3390/s19010147 SN - 1424-8220 VL - 19 IS - 1 SP - Article 147, 1 EP - 13 PB - MDPI CY - Basel AN - OPUS4-45232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst A1 - Herbrand, Martin A1 - Müller, Matthias T1 - Codawelleninterferometrie zur Detektion von Spannungszuständen in Betonbauteilen N2 - Informationen zu in Betonbauteilen stattfindenden Umlagerungsprozessen sowie Druckspannungsverteilungen können mit konventioneller Messtechnik bislang nicht zweifelsfrei beantwortet werden. Ultraschallmessungen mit eingebetteten Sensoren könnten hier eine sinnvolle Ergänzung zur konventionellen Messtechnik sein. Durch Einsatz der Codawelleninterferometrie (CWI) sind hiermit schon sehr kleine Änderungen im Material detektierbar. Um diese neue Methodik zu evaluieren, wurde das Forschungsprojekt „Querkrafttragfähigkeit von Spannbetonbrücken – Erfassung von Spannungszuständen in den Spannbetonversuchsträgern mit Ultraschallsensoren“ durch die Bundesanstalt für Straßenwesen (BASt) initiiert. In diesem Projekt wurden durch die Bundesanstalt für Materialforschung und –prüfung (BAM) Ultraschall-Transducer in mehrere Spannbetonträger des Instituts für Massivbau der RWTH Aachen eingebettet, die anschließend bis zum Bruch belastet wurden. Der Belastungsversuch an einem der Spannbetondurchlaufträger zeigte das große Potential dieser Methodik. Die im Netzwerk erfassten Änderungen der Ultraschallwellengeschwindigkeit geben die Spannungsverhältnisse im Längsschnitt des Trägers schon bei sehr niedrigen Belastungen qualitativ richtig wieder und zeigen bei hohen Belastungen eine gute Korrelation zum Rissbild. Dabei weisen räumliche Anomalien und Änderungen in der Charakteristik der Geschwindigkeitsänderungen oft schon auf Rissbildung hin, wenn diese noch nicht an der Oberfläche sichtbar ist. Dies zeigt das Potential im Hinblick auf eine Frühwarnung. Hierfür und ebenso in Bezug auf eine Quantifizierung der Effekte ist aber noch Entwicklungsarbeit notwendig. Ein Vorteil der Methodik ist, dass die Transducer nicht direkt am Ort der Änderung platziert werden müssen und einen relativ großen Bereich um die Transducer herum erfassen. T2 - DGZfP Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Ultraschall KW - Monitoring KW - Codawelleninterferometrie KW - Brückenträger PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-448642 SP - Mo.3.A.4, 1 EP - 8 PB - DGZfP AN - OPUS4-44864 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Coelho Lima, Isabela A1 - Grohmann, Maria A1 - Niederleithinger, Ernst T1 - Advanced ultrasonic imaging for concrete: Alternative imaging conditions for reverse time migration N2 - Ultrasound echo is a widely used NDT technique for determining the internal geometry of structures. Reverse-time migration (RTM) has been recently introduced to NDT applications, as an imaging method for ultrasound data, to overcome some of the limitations (e.g. imaging steeply dipping reflector) experienced by the Synthetic Aperture Focusing Technique (SAFT), the most commonly used imaging algorithm for these measurements. The standard implementation of RTM also experiences some drawbacks caused by its imaging condition, which is based on the zero-lag of the cross-correlation between source and receiver wavefields and generates high-amplitude low-frequency artifacts. Three alternative imaging conditions, developed for seismic data applications, were tested for their ability to provide better images than the standard cross-correlation: illumination compensation, deconvolution and wavefield decomposition. A polyamide specimen was chosen for the simulation of a synthetic experiment and for real data acquisition. The migrations of both synthetic and real data were performed with the software Madagascar. The illumination imaging condition was able to reduce the low-frequency noise and had a good performance in terms of computing time. The deconvolution improved the resolution in the synthetic tests, but did not showed such benefit for the real experiments. Finally, as for the wavefield decomposition, although it presented some advantages in terms of attenuating the low-frequency noise and some unwanted reflections, it was not able to image the internal structure of the polyamide as well as the cross-correlation did. Suggestions on how to improve the cost-effectiveness of the implementation of the deconvolution and wavefield decomposition were presented, as well as possible investigations that could be carried out in the future, in order to obtain better results with those two imaging conditions. T2 - DGZfP Jahrestagung 2018 CY - Leipzig DA - 07.05.2018 KW - Ultrasound KW - Reverse time migration KW - Imaging condition KW - Concrete PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-448704 SP - Mi.3.A.4, 1 EP - 10 PB - DGZfP AN - OPUS4-44870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst A1 - Wiggenhauser, Herbert A1 - Milmann, Boris T1 - LAUS - Erste praktische Erfahrungen mit einem neuartigen Ultraschallsystem großer Eindringtiefe N2 - Konventionelle Systeme zur Ultraschall-Echo-Prüfung von Betonbauteilen sind in ihrer Eindringtiefe auf etwa einem Meter begrenzt. Zur Prüfung stärkerer Objekte war die Entwicklung eines neuartigen Prüfsystems notwendig. Das LAUS-System (Large Aperture UltraSound) besteht aus 12 einzelnen Arrays, die mit jeweils 32 Einzelprüfköpfen (Scherwellen, 25 – 50 kHz) als Sender oder Empfänger betrieben werden können. Sie werden unabhängig auf Betonoberflächen mit Unterdruck befestigt und kommunizieren drahtlos untereinander und mit der Zentraleinheit. Alle möglichen Kombinationen ergeben 132 Einzelmessungen, die zur Rekonstruktion des durchschallten Volumens genutzt werden. Mehrere dieser Datensätze lassen sich zu einer 3D-Auswertung kombinieren. Das System wurde an mehreren Testobjekten und Bauwerken erfolgreich erprobt. So konnte die fünf Meter dicke, sehr stark bewehrte Fundamentplatte des Fallturms auf dem BAM-Testgelände bei Horstwalde durchschallt werden. Ein zweites Beispiel ist die erfolgreiche Detektion von Spannkanälen in 1,8 m Tiefe in einem massiven Brückenbauwerk. T2 - Fachtagung Bauwerksdiagnose 2018 CY - Berlin DA - 15.2.2018 KW - Beton KW - Ultraschall KW - LAUS KW - Brücke KW - Fundament PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-445786 UR - https://www.bauwerksdiagnose2018.de/Portals/bauwerksdiagnose2018/BB/16.pdf SP - Paper 16, 1 EP - 8 CY - Berlin AN - OPUS4-44578 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abraham, O. A1 - Ferria, H. A1 - Niederleithinger, Ernst A1 - Brühwiler, E. A1 - Dalsgard Sörensen, J. A1 - Klikowicz, P. A1 - Kirsch, F. A1 - Niedermayer, H. A1 - Yalamas, T. T1 - INFRASTAR - Innovation and networking for fatigue and reliability analysis of structures - Training for assessment of risk - H2020 N2 - "INFRASTAR aims to develop knowledge, expertise and skills for optimal and reliable management of structures. The generic methodology is applied to bridges and wind turbines in relation to fatigue offering the opportunity to deal with complementary notions (such as old and new asset management, unique and similar structures, wind and traffic actions) while addressing 3 major challenges: 1/ advanced modelling of concrete fatigue behaviour, 2/new non destructive testing methods for early aged damage detection and 3/probabilistic approach of structure reliability under fatigue. Benefit of cross-experience and inter-disciplinary synergies creates new knowledge. INFRASTAR proposes innovative solutions for civil infrastructure asset management so that young scientists acquire a high employment profile in close dialogue between industry and academic partners. Modern engineering methods, including probabilistic approaches, risk and reliability assessment tools, will take into account the effective structural behaviour of existing bridges and wind turbines by exploiting monitored data. Existing methods and current state-of -the art is based on excessive conservatism which produces high costs and hinders sustainability. INFRASTAR improves knowledge for optimising the design of new structures, for more realistic verification of structural safety and more accurate prediction of future lifetime of the existing structures. That is a challenge for a sustainable development because it reduces building material and energy consumption as well as CO2 production. Within the global framework of optimal infrastructure asset management, INFRASTAR will result in a multi-disciplinary body of knowledge covering generic problems from the design stage process of the new civil infrastructures up to recycling after dismantlement. This approach and the proposed methods and tools are new and allow a step forward for innovative and effective process." KW - Concrete KW - Fatigue KW - Wind turbine KW - Bridge PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-447016 UR - http://www.ingentaconnect.com/content/sil/impact/2018/00002018/00000001/art00023 DO - https://doi.org/10.21820/23987073.2018.70 SN - 2398-7073 VL - 2018 IS - 1 SP - 70 EP - 72 PB - Science Impact Ltd. CY - Bristol, UK AN - OPUS4-44701 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kage, Daniel A1 - Hoffmann, Katrin A1 - Wittkamp, M. A1 - Ameskamp, J. A1 - Göhde, W. A1 - Resch-Genger, Ute T1 - Luminescence lifetime encoding in time-domain flow cytometry N2 - Time-resolved flow cytometry represents an alternative to commonly applied spectral or intensity multiplexing in bioanalytics. At present, the vast majority of the reports on this topic focuses on phase-domain techniques and specific applications. In this report, we present a flow cytometry platform with time-resolved detection based on a compact setup and straightforward time-Domain measurements utilizing lifetime-encoded beads with lifetimes in the nanosecond range. We provide general assessment of time-domain flow cytometry and discuss the concept of this platform to address achievable resolution limits, data analysis, and requirements on suitable encoding dyes. Experimental data are complemented by numerical calculations on photon count numbers and impact of noise and measurement time on the obtained lifetime values. KW - Flow cytometry KW - Fluorescence KW - Life sciences KW - Lifetime encoding KW - Polymer particles PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-465765 DO - https://doi.org/10.1038/s41598-018-35137-5 SN - 2045-2322 VL - 8 IS - 1 SP - 16715, 1 EP - 11 PB - Nature CY - London AN - OPUS4-46576 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Treiling, S. A1 - Wang, Cui A1 - Förster, C. A1 - Reichenauer, F. A1 - Kalmbach, J. A1 - Boden, P. A1 - Harris, J. P. A1 - Carrella, L. M. A1 - Rentschler, E. A1 - Resch-Genger, Ute A1 - Reber, C. A1 - Seitz, M. A1 - Gerhards, M. A1 - Heinze, K. T1 - Luminescence and Light-Driven Energy and Electron Transfer from an Exceptionally Long-Lived Excited State of a Non-Innocent Chromium(III) Complex N2 - Photoactive metal complexes employing Earth‐abundant metal ions are a key to sustainable photophysical and photochemical applications. We exploit the effects of an inversion center and ligand non‐innocence to tune the luminescence and photochemistry of the excited state of the [CrN6] chromophore [Cr(tpe)2]3+ with close to octahedral symmetry (tpe=1,1,1‐tris(pyrid‐2‐yl)ethane). [Cr(tpe)2]3+ exhibits the longest luminescence lifetime (τ=4500 μs) reported up to date for a molecular polypyridyl chromium(III) complex together with a very high luminescence quantum yield of Φ=8.2 % at room temperature in fluid solution. Furthermore, the tpe ligands in [Cr(tpe)2]3+ are redox non‐innocent, leading to reversible reductive chemistry. The excited state redox potential and lifetime of [Cr(tpe)2]3+ surpass those of the classical photosensitizer [Ru(bpy)3]2+ (bpy=2,2′‐bipyridine) enabling energy transfer (to oxygen) and photoredox processes (with azulene and tri(n‐butyl)amine). KW - Quantum yield KW - Cr(III) complex KW - Longst luminescence lifetime KW - Electron transfer PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-494870 DO - https://doi.org/10.1002/anie.201909325 VL - 58 SP - 2 EP - 13 PB - Wiley-VCH AN - OPUS4-49487 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nirmalananthan-Budau, Nithiya A1 - Rühle, Bastian A1 - Geißler, Daniel A1 - Moser, Marko A1 - Kläber, Christopher A1 - Schäfer, A. A1 - Resch-Genger, Ute T1 - Multimodal cleavable reporters for quantifying carboxy and amino groups on organic and inorganic nanoparticles N2 - Organic and inorganic nanoparticles (NPs) are increasingly used as drug carriers, fluorescent sensors, and multimodal labels in the life and material sciences. These applications require knowledge of the chemical nature, total number of surface groups, and the number of groups accessible for subsequent coupling of e.g., antifouling ligands, targeting bioligands, or sensor molecules. To establish the concept of catch-and-release assays, cleavable probes were rationally designed from a quantitatively cleavable disulfide moiety and the optically detectable reporter 2-thiopyridone (2-TP). For quantifying surface groups on nanomaterials, first, a set of monodisperse carboxy-and amino-functionalized, 100 nm-sized polymer and silica NPs with different surface group densities was synthesized. Subsequently, the accessible functional groups (FGs) were quantified via optical spectroscopy of the cleaved off reporter after its release in solution. Method validation was done with inductively coupled plasma optical emission spectroscopy (ICP-OES) utilizing the sulfur atom of the cleavable probe. This comparison underlined the reliability and versatility of our probes, which can be used for surface group quantification on all types of transparent, scattering, absorbing and/or fluorescent particles. The correlation between the total and accessible number of FGs quantified by conductometric titration, qNMR, and with our cleavable probes, together with the comparison to results of conjugation studies with differently sized biomolecules reveal the potential of catch-and-release reporters for surface analysis. Our findings also underline the importance of quantifying particularly the accessible amount of FGs for many applications of NPs in the life sciences. KW - Advanced Materials KW - Surface Chemistry KW - Organic–inorganic nanostructures KW - Funtional Groups KW - Quantitative Analysis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499081 DO - https://doi.org/10.1038/s41598-019-53773-3 VL - 9 SP - 17577-1 EP - 17577-11 PB - Springer Nature CY - London AN - OPUS4-49908 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kage, Daniel A1 - Hoffmann, Katrin A1 - Nifontova, G. A1 - Krivenkov, V. A1 - Sukhanova, A. A1 - Nabiev, I. A1 - Resch-Genger, Ute T1 - Tempo-spectral multiplexing in flow cytometry with lifetime detection using QD-encoded polymer beads N2 - Semiconductor quantum dots (QDs) embedded into polymer microbeads are known to be very attractive emitters for spectral multiplexing and colour encoding. Their luminescence lifetimes or decay kinetics have been, however, rarely exploited as encoding parameter, although they cover time ranges which are not easily accessible with other luminophores. We demonstrate here the potential of QDs made from II/VI semiconductors with luminescence lifetimes of several 10 ns to expand the lifetime range of organic encoding luminophores in multiplexing applications using time-resolved flow cytometry (LT-FCM). For this purpose, two different types of QD-loaded beads were prepared and characterized by photoluminescence measurements on the ensemble level and by single-particle confocal laser scanning microscopy. Subsequently, these lifetime-encoded microbeads were combined with dye-encoded microparticles in systematic studies to demonstrate the potential of these QDs to increase the number of lifetime codes for lifetime multiplexing and combined multiplexing in the time and colour domain (tempo-spectral multiplexing). These studies were done with a recently developed novel luminescence lifetime flow cytometer (LT-FCM setup) operating in the time-domain, that presents an alternative to reports on phase-sensitive lifetime detection in flow cytometry. KW - Fluorescence life time KW - Flow cytometry KW - Lifetime-encoded beads KW - Quantum dots KW - Multiplexing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-503316 DO - https://doi.org/10.1038/s41598-019-56938-2 VL - 10 IS - 1 SP - Article number: 653 PB - nature.com AN - OPUS4-50331 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kirilina, E. A1 - Helbling, S. A1 - Morawski, M. A1 - Pine, K. A1 - Reimann, K. A1 - Jankuhn, S. A1 - Dinse, J. A1 - Deistung, A. A1 - Reichenbach, J. R. A1 - Trampel, R. A1 - Geyer, S. A1 - Müller, Larissa A1 - Jakubowski, Norbert A1 - Arendt, T. A1 - Bazin, P.-L. A1 - Weiskopf, N. T1 - Superficial white matter imaging: Contrast mechanisms and whole-brain in vivo mapping N2 - Superficial white matter (SWM) contains the most cortico-cortical white matter connections in the human brain encompassing the short U-shaped association fibers. Despite its importance for brain connectivity, very little is known about SWM in humans, mainly due to the lack of noninvasive imaging methods. Here, we lay the groundwork for systematic in vivo SWM mapping using ultrahigh resolution 7 T magnetic resonance imaging. Using biophysical modeling informed by quantitative ion beam microscopy on postmortem brain tissue, we demonstrate that MR contrast in SWM is driven by iron and can be linked to the microscopic iron distribution. Higher SWM iron concentrations were observed in U-fiber–rich frontal, temporal, and parietal areas, potentially reflecting high fiber density or late myelination in these areas. Our SWM mapping approach provides the foundation for systematic studies of interindividual differences, plasticity, and pathologies of this crucial structure for cortico-cortical connectivity in humans. KW - Magnetic resonance imaging KW - Laser ablation KW - ICP-MS KW - Brain KW - Imaging PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514430 DO - https://doi.org/10.1126/sciadv.aaz9281 SN - 2375-2548 VL - 6 IS - 41 SP - eaaz9281 PB - American Association for the Advancement of Science (Science/AAAS) CY - Washington, DC, USA AN - OPUS4-51443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Frenzel, F. A1 - Fiedler, S. A1 - Bardan, A. A1 - Güttler, Arne A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - Influence of Measurement Geometry and Blank on Absolute Measurements of Photoluminescence Quantum Yields of Scattering Luminescent Films N2 - For a series of 500 μm-thick polyurethane films containing different concentrations of luminescent and scattering YAG:Ce microparticles, we systematically explored and quantified pitfalls of absolute measurements of photoluminescence quantum yields (Φf) for often employed integrating sphere (IS) geometries, where the sample is placed either on a sample holder at the bottom of the IS surface or mounted in the IS center. Thereby, the influence of detection and illumination geometry and sample position was examined using blanks with various scattering properties for measuring the number of photons absorbed by the sample. Our results reveal that (i) setup configurations where the scattering sample is mounted in the IS center and (ii) transparent blanks can introduce systematic errors in absolute Φf measurements. For strongly scattering, luminescent samples, this can result in either an under- or overestimation of the absorbed photon flux and hence an under- or overestimation of Φf. The size of these uncertainties depends on the scattering properties of the sample and instrument parameters, such as sample position, IS size, wavelength-dependent reflectivity of the IS surface coating, and port configuration. For accurate and reliable absolute Φf measurements, we recommend (i) a blank with scattering properties closely matching those of the sample to realize similar distributions of the diffusely scattered excitation photons within the IS, and (ii) a sufficiently high sample absorption at the excitation wavelength. For IS setups with center-mounted samples, measurement geometries should be utilized that prevent the loss of excitation photons by reflections from the sample out of the IS. KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Quantum yield KW - Characterization KW - Silica KW - Scattering KW - Uncertainty KW - Film KW - Pphosphor KW - YAG:Ce KW - LED KW - Converter material KW - Solid material KW - Polymer KW - Composite material KW - Advanced material PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638304 DO - https://doi.org/10.1021/acs.analchem.4c06726 SN - 1520-6882 SP - 1 EP - 8 PB - ACS Publications AN - OPUS4-63830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maisuls, I. A1 - Wang, Cui A1 - Gutierrez Suburu, M. E. A1 - Wilde, S. A1 - Daniliuc, C.-G. A1 - Brunink, D. A1 - Doltsinis, N. L. A1 - Ostendorp, S. A1 - Kösters, J. A1 - Resch-Genger, Ute A1 - Strassert, C. A. T1 - Ligand-controlled and nanoconfinement-boosted luminescence employing Pt(II) and Pd(II) complexes: from color-tunable aggregation-enhanced dual emitters towards self-referenced oxygen reporters N2 - In this work, we describe the synthesis, structural and photophysical characterization of four novel Pd(II) and Pt(II) complexes bearing tetradentate luminophoric ligands with high photoluminescence quantum yields (FL) and long excited state lifetimes (s) at room temperature, where the results were interpreted by means of DFT calculations. Incorporation of fluorine atoms into the tetradentate ligand favors aggregation and thereby, a shortened average distance between the metal centers, which provides accessibility to metal–metal-to-ligand charge-transfer (3MMLCT) excimers acting as red-shifted Energy traps if compared with the monomeric entities. This supramolecular approach provides an elegant way to enable room-temperature phosphorescence from Pd(II) complexes, which are otherwise quenched by a thermal population of dissociative states due to a lower ligand field splitting. Encapsulation of These complexes in 100 nm-sized aminated polystyrene nanoparticles enables concentration-controlled aggregation-enhanced dual emission. This phenomenon facilitates the tunability of the absorption and emission colors while providing a rigidified environment supporting an enhanced FL up to about 80% and extended s exceeding 100 ms. Additionally, these nanoarrays constitute rare examples for selfreferenced oxygen reporters, since the phosphorescence of the aggregates is insensitive to external influences, whereas the monomeric species drop in luminescence lifetime and intensity with increasing triplet molecular dioxygen concentrations (diffusion-controlled quenching). KW - Fluorescence KW - Multiplexing KW - Lifetime KW - Bead KW - Particle KW - Dye KW - Barcoding KW - Encoding KW - Quantum yield KW - Label KW - Reporter KW - Pd(II) KW - Pt(II) KW - Complex KW - NMR KW - X-ray KW - Sythesis KW - Aggregation KW - Monomer KW - Color PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525288 DO - https://doi.org/10.1039/d0sc06126c VL - 12 IS - 9 SP - 3270 EP - 3281 PB - Royal Society of Chemistry AN - OPUS4-52528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sun, C. A1 - Schäferling, Michael A1 - Resch-Genger, Ute A1 - Gradzielski, M. T1 - Solvothermal Synthesis of Lanthanide-doped NaYF4 Upconversion N2 - Lanthanide-doped NaYF4 upconversion nano- and microcrystals were synthesized via a facile solvothermal approach. Thereby, the influence of volume ratios of ethylene glycol (EG)/H2O, molar ratios of NH4F/RE3+ (RE3+ represents the total amount of Y3+ and rare-earth dopant ions), Gd3+ ion contents, types of activator dopant ions, and different organic co-solvents on the crystal phase, size, and morphology of the resulting particles were studied systematically. A possible formation mechanism for the growth of crystals of different morphology is discussed. Our results show that the transition from the α- to the β-phase mainly depends on the volume ratio of EG/H2O and the molar ratio of NH4F/RE3+, while the morphology and size could be controlled by the type of organic co-solvent and Gd3+ dopant ions. Furthermore, the reaction time has to be long enough to convert α-NaYF4 into β-NaYF4 during the growth process to optimize the upconversion luminescence. The formation of larger β-NaYF4 crystals, which possess a higher upconversion luminescence than smaller particles, proceeds via intermediates of smaller crystals of cubic structure. In summary, our synthetic approach presents a facile route to tailor the size, Crystal phase, morphology, and luminescence features of upconversion materials. KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Photoluminescence KW - Lanthanide KW - Quantum yield KW - Photophysics KW - Lifetime KW - Surface chemistry KW - Single particle KW - Brightness KW - NIR KW - Synthesis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520307 DO - https://doi.org/10.1002/cnma.202000564 VL - 7 IS - 2 SP - 174 EP - 183 PB - Wiley AN - OPUS4-52030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rietsch, P. A1 - Sobottka, S. A1 - Hoffmann, Katrin A1 - Hildebrandt, P. A1 - Sarkar, B. A1 - Resch-Genger, Ute A1 - Eigler, S. T1 - Identification of the Irreversible Redox Behavior of Highly Fluorescent Benzothiadiazoles N2 - Redox switches are applied in various fields of research, including molecular lifts, electronic devices and sensors. Switching the absorbance between UV and Vis/NIR by redox processes is of interest for applications in light harvesting or biomedicine. Here, we present a series of push-pull benzothiadiazole derivatives with high fluorescence quantum yields in solution and in the crystalline solid state. Spectroelectrochemical analysis reveals the switching of UV-absorption in the neutral state to Vis/NIR absorption in the reduced state. We identify the partial irreversibility of the switching process, which appears to be reversible on the cyclic voltammetry timescale. KW - Redox switch KW - Electrochemistry KW - Dye KW - Fluorescence KW - Absorption KW - Sensor KW - Benzothiadiazole PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520865 DO - https://doi.org/10.1002/cptc.202000050 SN - 2367-0932 VL - 4 IS - 9 SP - 668 EP - 673 PB - Wiley Online Library AN - OPUS4-52086 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geißler, Daniel A1 - Nirmalananthan-Budau, Nithiya A1 - Scholtz, Lena A1 - Tavernaro, Isabella A1 - Resch-Genger, Ute T1 - Analyzing the surface of functional nanomaterials — how to quantify the total and derivatizable number of functional groups and ligands N2 - Functional nanomaterials (NM) of different size, shape, chemical composition, and surface chemistry are of increasing relevance for many key technologies of the twenty-first century. This includes polymer and silica or silica-coated nanoparticles (NP) with covalently bound surface groups, semiconductor quantum dots (QD), metal and metal oxide NP, and lanthanide-based NP with coordinatively or electrostatically bound ligands, as well as surface-coated nanostructures like micellar encapsulated NP. The surface chemistry can significantly affect the physicochemical properties of NM, their charge, their processability and performance, as well as their impact on human health and the environment. Thus, analytical methods for the characterization of NM surface chemistry regarding chemical identification, quantification, and accessibility of functional groups (FG) and surface ligands bearing such FG are of increasing importance for quality control of NM synthesis up to nanosafety. Here, we provide an overview of analytical methods for FG analysis and quantification with special emphasis on bioanalytically relevant FG broadly utilized for the covalent attachment of biomolecules like proteins, peptides, and oligonucleotides and address methodand material-related challenges and limitations. Analytical techniques reviewed include electrochemical titration methods, optical assays, nuclear magnetic resonance and vibrational spectroscopy, as well as X-ray based and thermal analysis methods, covering the last 5–10 years. Criteria for method classification and evaluation include the need for a signal-generating label, provision of either the total or derivatizable number of FG, need for expensive instrumentation, and suitability for process and production control during NM synthesis and functionalization. KW - Functional group quantification KW - Surface ligand KW - Nanomaterial KW - Optical detection KW - Electrochemical titration KW - Nanosafety (Safe-by-design) PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533597 DO - https://doi.org/10.1007/s00604-021-04960-5 VL - 188 IS - 10 SP - 1 EP - 28 PB - Springer Nature AN - OPUS4-53359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grauel, Bettina A1 - Würth, Christian A1 - Homann, C. A1 - Krukewitt, Lisa A1 - Andresen, Elina A1 - Roik, Janina A1 - Recknagel, Sebastian A1 - Haase, M. A1 - Resch-Genger, Ute T1 - Volume and surface effects on two-photonic and three-photonic processes in dry co-doped upconversion nanocrystals N2 - Despite considerable advances in synthesizing high-quality core/shell upconversion (UC) nanocrystals (NC; UCNC) and UCNC photophysics, the application of near-infrared (NIR)-excitable lanthanide-doped UCNC in the life and material sciences is still hampered by the relatively low upconversion luminescence (UCL) of UCNC of small size or thin protecting shell. To obtain deeper insights into energy transfer and surface quenching processes involving Yb3+ and Er3+ ions, we examined energy loss processes in differently sized solid core NaYF4 nanocrystals doped with either Yb3+ (YbNC; 20% Yb3+) or Er3+ (ErNC; 2% Er3+) and co-doped with Yb3+ and Er3+ (YbErNC; 20% Yb3+ and 2% Er3+) without a surface protection shell and coated with a thin and a thick NaYF4 shell in comparison to single and co-doped bulk materials. Luminescence studies at 375 nm excitation demonstrate backenergy transfer (BET) from the 4G11/2 state of Er3+ to the 2F5/2 state of Yb3+, through which the red Er3+ 4F9/2 state is efficiently populated. Excitation power density (P)-dependent steady state and time-resolved photoluminescence measurements at different excitation and emission wavelengths enable to separate surface-related and volume-related effects for two-photonic and threephotonic processes involved in UCL and indicate a different influence of surface passivation on the green and red Er3+ emission. The intensity and lifetime of the latter respond particularly to an increase in volume of the active UCNC core. We provide a threedimensional random walk model to describe these effects that can be used in the future to predict the UCL behavior of UCNC. KW - Nano KW - Nanomaterial KW - Upconversion KW - Nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Pphotophysics KW - Lifetime KW - Sensor KW - Excitation KW - Power density KW - Single particle KW - Brightness KW - NIR KW - Mechanism KW - Modeling KW - Simulation KW - Energy transfer PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-535317 DO - https://doi.org/10.1007/s12274-021-3727-y SN - 1998-0124 VL - 15 IS - 3 SP - 2362 EP - 2373 PB - Springer AN - OPUS4-53531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Biesen, L. A1 - May, L. A1 - Nirmalananthan-Budau, Nithiya A1 - Hoffmann, Katrin A1 - Resch-Genger, Ute A1 - Müller, T. J. J. T1 - Communication of Bichromophore Emission upon Aggregation – Aroyl-S,N-ketene Acetals as Multifunctional Sensor Merocyanines N2 - Aroyl-S,N-ketene acetal-based bichromophores can be readily synthesized in a consecutive three-component synthesis in good to excellent yields by condensation of aroyl chlorides and an N-(p-bromobenzyl) 2-methyl benzothiazolium salt followed by a Suzuki coupling, yielding a library of 31 bichromophoric fluorophores with substitution patterntunable emission properties. Varying both chromophores enables different communication pathways between the chromophores, exploiting aggregation-induced emission (AIE) and energy transfer (ET) properties, and thus, furnishing aggregation-based fluorescence switches. Possible applications range from fluorometric analysis of alcoholic beverages to pH sensors. KW - Dye KW - Fluorescence KW - Aggregation induced emission KW - Signal enhancement KW - Energy transfer KW - Switch KW - Sensor KW - Quantum yield KW - Lifetime KW - Photophysics KW - Synthesis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531123 DO - https://doi.org/10.1002/chem.202102052 VL - 27 IS - 53 SP - 13426 EP - 13434 PB - Wiley-VCH AN - OPUS4-53112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Witte, F. A1 - Rietsch, P. A1 - Nirmalananthan-Budau, Nithiya A1 - Weigert, Florian A1 - Götze, J. P. A1 - Resch-Genger, Ute A1 - Eigler, S. A1 - Paulus, B. T1 - Aggregation-induced emission leading to two distinct emissive species in the solid-state structure of high-dipole organic chromophores N2 - The concept of aggregation-induced emission represents a means to rationalise photoluminescence of usually nonfluorescent excimers in solid-state materials. In this publication, we study the photophysical properties of selected diaminodicyanoquinone (DADQ) derivatives in the solid state using a combined approach of experiment and theory. DADQs are a class of high-dipole organic chromophores promising for applications in non-linear optics and light-harvesting devices. Among the compounds investigated, we find both aggregation-induced emission and aggregation-caused quenching effects rationalised by calculated energy transfer rates. Analysis of fluorescence spectra and lifetime measurements provide the interesting result that (at least) two emissive species seem to contribute to the photophysical properties of DADQs. The main emission peak is notably broadened in the long-wavelength limit and exhibits a blue-shifted shoulder. We employ high-level quantum-chemical methods to validate a molecular approach to a solid-state problem and show that the complex emission features of DADQs can be attributed to a combination of H-type aggregates, monomers, and crystal structure defects. KW - Fluorescence KW - Optical probe KW - Dye KW - Photophysics KW - Theory KW - Quantum yield KW - Mechanism KW - Quantum chemistry KW - Modelling KW - Aggregation KW - Lifetime KW - Single particle KW - Microscopy KW - Solid KW - Crystal PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531138 DO - https://doi.org/10.1039/d1cp02534a SP - 1 EP - 9 PB - Royal Society of Chemistry AN - OPUS4-53113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Srivastava, Priyanka A1 - Fürstenwerth, Paul Christian A1 - Witte, J. F. A1 - Resch-Genger, Ute T1 - Synthesis and spectroscopic characterization of a fluorescent phenanthrene-rhodamine dyad for ratiometric measurements of acid pH values N2 - We present the rational design, synthesis and spectroscopic characterization of a novel dual excitation, three color emitting, pH-responsive fluorescent probe consisting of two phenanthrene and one rhodamine B units linked by click chemistry. The rhodamine moiety, excitable at λEx = 315 nm and at λEx = 560 nm in its ring-opened form, provides the pH-responsive fluorophore, while the pH-insensitive phenanthrene, excited at λEx = 315 nm, serves as inert internal reference, The presence of two phenanthrene moieties enables a blue monomer and a blueish green excimer emission at 351 nm and 500 nm, respectively. Opening of the rhodamine B spirolactam ring at an acidic pH below 5.0 (pKa = 2.59 ± 0.04) switches on its emission at 580 nm. Simultaneously, the phenanthrene excimer emission decreases caused by a change in orientation of the phenanthrene units, while the monomer emission is barely affected. This sensor design enables ratiometric measurements in the low acidic pH range utilizing the intensity ratios of the rhodamine B and phenanthrene excimer emission at 580 nm and 500 nm. Alternatively, also the intensity ratios of the rhodamine B and the phenanthrene monomer emission could be exploited or the sum of the phenanthrene monomer and excimer fluorescence. To the best of our knowledge, this is the first report of ratiometric sensing utilizing such a versatile type of tricolor emissive dyad probe bearing phenanthrene moieties and showing phenanthrene monomer and excimer emission. KW - Fluorescence KW - Optical probe KW - Sensor KW - Dye KW - Rhodamine KW - Synthesis KW - Photophysics KW - PH KW - Quantum yield KW - Quality assurance KW - Mechanism KW - Chemodosimeter KW - Phenanthrene KW - Ratiometric KW - Dyad PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530554 DO - https://doi.org/10.1039/d1nj01573g SN - 1144-0546 VL - 45 IS - 31 SP - 13755 EP - 13762 PB - Royal Society of Chemistry AN - OPUS4-53055 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andresen, Elina A1 - Radunz, Sebastian A1 - Resch-Genger, Ute T1 - Novel PET-Operated Rosamine Sensor Dyes with Substitution Pattern-Tunable pKa Values and Temperature Sensitivity N2 - We present the synthesis and characterization of a family of regioisomerically pure pH-sensitive rosamine fluorophores consisting of xanthene fluorophore cores, which determine the dyes’ photophysical properties such as excitation/emission wavelength, fluorescence quantum yield, and fluorescence lifetime, and differently substituted phenol moieties. The hydroxyl substituent of the phenol moiety introduces a pH sensitivity of the dyes’ fluorescence exploiting a photoinduced electron transfer (PET), that leads to a protonation-induced switching ON of the rosamine emission. Rational tuning of the pKa value of the rosamine fluorescence between 4 to 9 is achieved by altering the substitution pattern and degree of bromination of the phenolic subunits. Additionally, a temperature sensitivity of the fluorescence quantum yield is introduced or suppressed based upon the degree of rigidity of the xanthene scaffold. KW - Fluorescence KW - Optical probe KW - Sensor KW - Dye KW - Rosamine KW - Synthesis KW - Photophysics KW - PH KW - Quantum yield KW - Quality assurancemechanism KW - temperature PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530562 DO - https://doi.org/10.1039/d1nj02505h VL - 45 IS - 31 SP - 13934 EP - 13940 PB - Royal Society of Chemistry AN - OPUS4-53056 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cruz-Alonso, M. A1 - Fernandez, B. A1 - Álvarez, L. A1 - González-Iglesias, H. A1 - Traub, Heike A1 - Jakubowski, Norbert A1 - Pereiro, R. T1 - Bioimaging of metallothioneins in ocular tissue sections by laser ablation-ICP-MS using bioconjugated gold nanoclusters as specific tags N2 - An immunohistochemical method is described to visualize the distribution of metallothioneins 1/2 (MT 1/2) and metallothionein 3 (MT 3) in human ocular tissue. It is making use of (a) antibodies conjugated to gold nanoclusters (AuNCs) acting as labels, and (b) laser ablation (LA) coupled to inductively coupled plasma – mass spectrometry (ICP-MS).Water-soluble fluorescent AuNCs (with an average size of 2.7 nm) were synthesized and then conjugated to antibody by carbodiimide coupling. The surface of the modified AuNCs was then blocked with hydroxylamine to avoid nonspecific interactions with biological tissue. Immunoassays for MT 1/2 and MT 3 in ocular tissue sections (5 μm thick) from two post mortem human donors were performed. Imaging studies were then performed by fluorescence using confocal microscopy, and LA-ICP-MS was performed in the retina to measure the signal for gold. Signal amplification by the >500 gold atoms in each nanocluster allowed the antigens (MT 1/2 and MT 3) to be imaged by LA-ICP-MS using a laser spot size as small as 4 μm. The image patterns found in retina are in good agreement with those obtained by conventional fluorescence immunohistochemistry which was used as an established reference method. KW - Metal nanoclusters KW - Fluorescence KW - Protein imaging KW - Thin tissue sections KW - Immunohistochemistry KW - Bioconjugation KW - Carbodiimide crosslinking KW - Laser ablation KW - Mass spectrometry PY - 2018 DO - https://doi.org/10.1007/s00604-017-2597-1 VL - 185 IS - 1 SP - 1 EP - 9 PB - Springer AN - OPUS4-44022 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hendriks, L. A1 - Ramkorun-Schmidt, Benita A1 - Grundlach-Graham, A. A1 - Koch, J. A1 - Grass, R. N. A1 - Jakubowski, Norbert A1 - Günther, D. T1 - Single-particle ICP-MS with online microdroplet calibration: toward matrix independent nanoparticle sizing N2 - Single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS) has become an effective tool for the detection and quantification of inorganic nanoparticles (NPs). While sizing of NPs suspended in water is relatively straightforward by sp-ICP-MS, accurate mass quantification of NPs in complex media, such as consumer products and natural systems still remains a challenge. When NPs are suspended in a complex medium, the matrix may affect the analyte sensitivity and lead to inaccurate NP sizing. Here, we investigate the use of an online microdroplet calibration system to size NPs in a single step. In this setup, microdroplets—which are used as the calibrant to determine elemental sensitivities—and nebulized NP-containing solutions are introduced concurrently into the ICP via a dual-inlet sample introduction system. Because calibrant microdroplets and analyte NPs experience the same plasma conditions, both the microdroplets and the NPs are subjected to the same matrix-related signal enhancement or suppression. In this way, the microdroplet calibration standards are automatically matrix matched with the NP-containing solution. The online microdroplet calibration system is combined with an ICP-TOFMS instrument for simultaneous measurement of multiple elements in microdroplets and NPs. We investigate the ability of online microdroplet calibration to compensate for matrix effects through a series of experiments, in which Ag and Au NPs are measured with variable plasma-sampling positions, varying concentrations of HCl and HNO3, varying concentrations of single element solutions, and high concentrations of a salt matrix, i.e. phosphate buffered saline (PBS). Through these experiments, we demonstrate that the online microdroplet calibration strategy provides a matrix-independent mass quantification of analyte NPs in the presence of several established types of matrix effects, including acid effects, space-charge effects, and ionisation suppression. In results presented here, we focus on the size determination of the NPs. KW - Nanoparticle KW - ICP-MS KW - Calibration PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-477589 DO - https://doi.org/10.1039/c8ja00397a SN - 0267-9477 VL - 34 IS - 4 SP - 716 EP - 728 PB - Royal Society of Chemistry CY - London AN - OPUS4-47758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Huang, J. A1 - Tarábek, J. A1 - Kulkarni, R. A1 - Wang, Cui A1 - Dračínský, M. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Resch-Genger, Ute A1 - Bojdys, M. J. T1 - A π-conjugated, covalent phosphinine framework N2 - Structural modularity of polymer frameworks is a key advantage of covalent organic polymers, however, only C, N, O, Si and S have found their way into their building blocks so far. Here, we expand the toolbox available to polymer and materials chemists by one additional nonmetal, phosphorus. Starting with a building block that contains a λ⁵‐phosphinine (C₅P) moiety, we evaluate a number of polymerisation protocols, finally obtaining a π‐conjugated, covalent phosphinine‐based framework (CPF‐1) via Suzuki‐Miyaura coupling. CPF‐1 is a weakly porous polymer glass (72.4 m2 g‐1 N2 BET at 77 K) with green fluorescence (λmax 546 nm) and extremely high thermal stability. The polymer catalyzes hydrogen evolution from water under UV and visible light irradiation without the need for additional co‐catalyst at a rate of 33.3 μmol h‐¹ g‐¹. Our results demonstrate for the first time the incorporation of the phosphinine motif into a complex polymer framework. Phosphinine‐based frameworks show promising electronic and optical properties that might spark future interest in their applications in light‐emitting devices and heterogeneous catalysis. KW - Phosphinine KW - Fully aromatic frameworks KW - Suzuki-Miyaura coupling KW - Polymers KW - Fluorescence KW - Small-angle scattering PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485330 DO - https://doi.org/10.1002/chem.201900281 SP - 2 EP - 10 PB - Wiley VCH-Verlag CY - Weinheim AN - OPUS4-48533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bassil, A. A1 - Wang, Xin A1 - Chapeleau, X. A1 - Niederleithinger, Ernst A1 - Abraham, O. A1 - Leduc, D. T1 - Distributed fiber optics sensing and coda wave interferometry techniques for damage monitoring in concrete structures N2 - The assessment of Coda Wave Interferometry (CWI) and Distributed Fiber Optics Sensing (DFOS) techniques for the detection of damages in a laboratory size reinforced concrete beam is presented in this paper. The sensitivity of these two novel techniques to micro cracks is discussed and compared to standard traditional sensors. Moreover, the capacity of a DFOS technique to localize cracks and quantify crack openings is also assessed. The results show that the implementation of CWI and DFOS techniques allow the detection of early subtle changes in reinforced concrete structures until crack formation. With their ability to quantify the crack opening, following early detection and localization, DFOS techniques can achieve more effective monitoring of reinforced concrete structures. Contrary to discrete sensors, CWI and DFOS techniques cover larger areas and thus provide more efficient infrastructures asset management and maintenance operations throughout the lifetime of the structure. KW - Distributed fiber optic sensors KW - Coda wave interferometry KW - Reinforced concrete KW - Cracks KW - Damage detection KW - Structural health monitoring PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472549 DO - https://doi.org/10.3390/s19020356 SN - 1424-8220 VL - 19 IS - 2 SP - 356, 1 EP - 15 PB - MDPI AN - OPUS4-47254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niederleithinger, Ernst A1 - Wang, Xin A1 - Mierschke, Vivien A1 - Bertschat, Anja Sophie T1 - Concepts from seismic interferometry transferred to sonic and ultrasonic concrete inspection and monitoring N2 - Seismic interferometry (SI) deals either with the sensible detection of changes in the subsurface or with the reconstruction of virtual signals between two receivers by crosscorrelation of signals from diffuse sources. These concepts can be applied in NDT in civil engineering for various purposes, e. g. to detect changes in bridges. Here it is demonstrated using data from a reference structure on our test site. Practical applications can be expected in the very near future. T2 - 12th European Conference on Non-Destructive Testing (ECNDT 2018) CY - Gothenburg, Sweden DA - 11.6.2018 KW - Ultrasound KW - Concrete KW - Monitoring KW - Coda KW - Interferometry PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-468465 UR - http://www.ndt.net/?id=22760 SN - 1435-4934 VL - 23 IS - 8 SP - 1 EP - 2 PB - NDT.net CY - Kirchwald AN - OPUS4-46846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moll, J. A1 - Wang, Cui A1 - Päpcke, A. A1 - Förster, C. A1 - Resch-Genger, Ute A1 - Lochbrunner, S. A1 - Heinze, K. T1 - Green Light Activation of Push-Pull Ruthenium(II) Complexes N2 - Synthesis, characterization, electrochemistry, and photophysics of novel homo- and heteroleptic ruthenium(II) complexes [Ru(cpmp)2] 2+ (22+) and [Ru(cpmp)(ddpd)]2+ (32+) bearing the tridentate ligands 6,2’’-carboxypyridyl-2,2’-methylamine-pyridylpyridine (cpmp) and N,N’-dimethyl-N,N’-dipyridin-2-ylpyridine-2,6-diamine (ddpd) are reported. The complexes possess one (32+) or two (22+) electron-deficient dipyridyl ketone fragments as electron accepting sites enabling intraligand charge transfer (ILCT), ligand-toligand charge transfer (LL’CT) and low-energy metal-to-ligand charge transfer (MLCT) absorptions. The latter peak around 544 nm (green light). 22+ shows 3MLCT phosphorescence in the red to near-infrared spectral region at room temperature in deaerated acetonitrile solution with an emission quantum yield of 1.3 % and a 3MLCT lifetime of 477 ns, while 3 2+ is much less luminescent. This different behaviour is ascribed to the energy gap law and the shape of the parasitic excited 3MC state potential energy surface. This study highlights the importance of the excited state energies and geometries for the actual excited state dynamics. Aromatic and aliphatic amines reductively quench the excited state of 22+ paving the way to photocatalytic applications using low-energy green light as exemplified with the green-light sensitized thiol-ene click reaction. KW - Green light excitation KW - Ruthenium(II) complexes KW - Phosphorescence KW - MLCT KW - Photoinduced electron transfer PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506759 DO - https://doi.org/10.1002/chem.202000871 SP - 1 EP - 13 PB - Wiley-VCH Verlag AN - OPUS4-50675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arakawa, Akihiro A1 - Jakubowski, Norbert A1 - Koellensperger, G. A1 - Theiner, S. A1 - Schweikert, A. A1 - Flemig, Sabine A1 - Iwahata, D. A1 - Traub, Heike A1 - Hirata, T. T1 - Imaging of Ag NP transport through collagen-rich microstructures in fibroblast multicellular spheroids by high-resolution laser ablation inductively coupled plasma time-of-flight mass spectrometry N2 - We investigated the penetration of silver nanoparticles (Ag NPs) into a three-dimensional in vitro tissue analog using NPs with various sizes and surface coatings, and with different incubation times. A high-Resolution laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) time-of-flight (TOF) instrument was applied for imaging the distributions of elements in thin sample sections (20 μm thick). A fibroblast multicellular spheroid (MCS) was selected as the model system and cultured for more than 8 days to produce a natural barrier formed by the extracellular matrix containing collagen. The MCS was then exposed for up to 48 h to one of four types of Ag NPs (∅ 5 nm citrate coated, ∅ 20 nm citrate coated, ∅ 20 nm polyvinylpyrrolidone coated, and ∅ 50 nm citrate coated). Imaging showed that the penetration pathway was strongly related to steric networks formed by collagen fibrils, and Ag NPs with a hydrodynamic diameter of more than 41 nm were completely trapped in an outer rim of the MCSs even after incubation for 48 h. In addition, we examined the impact of these NPs on essential elements (P, Fe, Cu, and Zn) in areas of Ag NP accumulation. We observed a linear increase at the sub-femtogram level in the total concentration of Cu (fg per pixel) in samples treated with small or large Ag NPs (∅ 5 nm or ∅ 50 nm) for 48 h. KW - Nanoparticle KW - Laser ablation KW - ICP-MS KW - Imaging KW - Cell PY - 2019 DO - https://doi.org/10.1039/c9an00856j SN - 0003-2654 VL - 144 IS - 16 SP - 4935 EP - 4942 PB - Royal Society of Chemistry RSC CY - Cambridge AN - OPUS4-48531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, Katrin A1 - Nirmalananthan-Budau, Nithiya A1 - Resch-Genger, Ute T1 - Fluorescence calibration standards made from broadband emitters encapsulated in polymer beads for fluorescence microscopy and flow cytometry N2 - We present here the design and characterization of a set of spectral calibration beads. These calibration beads are intended for the determination and regular control of the spectral characteristics of fluorescence microscopes and other fluorescence measuring devices for the readout of bead-based assays. This set consists of micrometer-sized polymer beads loaded with dyes from the liquid Calibration Kit Spectral Fluorescence Standards developed and certified by BAM for the wavelength-dependent Determination of the spectral responsivity of fluorescencemeasuring devices like spectrofluorometers. To cover the wavelength Region from 400 to 800 nm, two new near-infrared emissive dyes were included, which were spectroscopically characterized in solution and encapsulated in the beads. The resulting set of beads presents the first step towards a new platform of spectral calibration beads for the determination of the spectral characteristics of fluorescence instruments like fluorescence microscopes, FCM setups, and microtiter plate readers, thereby meeting the increasing demand for reliable and comparable fluorescence data especially in strongly regulated areas, e.g., medical diagnostics. This will eventually provide the basis for standardized calibration procedures for imaging systems as an alternative to microchannel slides containing dye solutions previously reported by us. KW - Fluorescence standard KW - Fluorescence KW - Dye KW - Microscopy KW - Bead KW - Particle KW - NIR KW - calibration KW - Quality assurance KW - Traceability PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508117 DO - https://doi.org/10.1007/s00216-020-02664-y SN - 1618-2642 VL - 412 IS - 24 SP - 6499 EP - 6507 PB - Springer AN - OPUS4-50811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalmbach, J. A1 - Wang, Cui A1 - You, Yi A1 - Förster, C. A1 - Schubert, H. A1 - Heinze, K. A1 - Resch-Genger, Ute A1 - Seitz, M. T1 - Near-IR to near-IR upconversion luminescence in molecular chromium ytterbium salts N2 - Upconversion photoluminescence in hetero-oligonuclear metal complex architectures featuring organic ligands is an interesting but still rarely observed phenomenon, despite its great potential from a basic research and application perspective. In this context, a new photonic material consisting of molecular chromium(III) and ytterbium(III) complex Ions was developed that exhibits excitation-power density-dependent cooperative sensitization of the chromium-centered 2E/2T1 phosphorescence at approximately 775 nm after excitation of the ytterbium band 2F7/2!2F5/2 at approximately 980 nm in the solid state at ambient temperature. The upconversion process is insensitive to atmospheric oxygen and can be observed in the presence of water molecules in the crystal lattice. KW - Upconversion KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - NIR KW - Cr(III) KW - Yb(III) complex KW - Crystal KW - Triplet-triplet annihilation KW - Sensitization KW - Light harvesting PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512619 DO - https://doi.org/10.1002/anie.202007200 SN - 1433-7851 SN - 1521-3773 VL - 59 IS - 42 SP - 18804 EP - 18808 PB - Wiley CY - Weinheim AN - OPUS4-51261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Biesen, L. A1 - Nirmalananthan-Budau, Nithiya A1 - Hoffmann, Katrin A1 - Resch-Genger, Ute A1 - Müller, T. J. J. T1 - Solid-State Emissive Aroyl-S,N-Ketene Acetals with Tunable N2 - N-Benzyl aroyl-S,N-ketene acetals can be readily synthesized by condensation of aroyl chlorides and N-Benzyl 2-methyl benzothiazolium salts in good to excellent yields, yielding a library of 35 chromophores with bright solid-state emission and aggregation-induced emission characteristics. Varying the substituent from electron-donating to electronwithdrawing enables the tuning of the solid-state emission Color from deep blue to red. KW - Nano KW - Nanoparticle KW - Photoluminescence KW - Fluorescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - dye KW - Enhancement KW - Particle KW - Polarity KW - AIE KW - Aggregation KW - Aggregation-induced emission KW - Solid state emission PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509072 DO - https://doi.org/10.1002/anie.201916396 VL - 59 IS - 25 SP - 10037 EP - 10041 PB - Wiley Online Libary AN - OPUS4-50907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramirez Caro, Alejandra A1 - Pauli, Jutta T1 - Study of the hydration of superplasticizer-cement pastes with optical spectroscopy N2 - Chemical admixtures like superplasticizers or stabilizing agents are of ever increasing importance for modern concrete technology. Although such admixtures have meanwhile become common practice in many applications of concrete technology, the understanding of these highly complex systems is still limited and the relevant parameters, which predominantly control the interaction between the superplasticizer and the cement components, have not been identified yet. Optical methods have been successfully used for the analysis and monitoring of the interactions between a broad variety of nanoscale and molecular systems like nanoparticles of various chemical composition and different types of organic ligands or biomolecules. This encouraged us to assess the potential of these methods, and particularly reflectance and fluorescence measurements, for the study of the interactions that occur at the interface between particle or hydrate surfaces and the fluid phase at a very early stage of concrete formation. Special emphasis is dedicated to search for and identify differences between commonly used superplasticizers. Here, we focus on hydration effects using commercial comb shape polycarboxylate ethers (PCEs) with different charge densities, which are known to allow a very low water/cement ratio (w/c of 0.20 or less) while maintaining good workability. Based upon changes of the intensity of the reflectance and fluorescence signal and spectral effects of a dye, acting as optical reporter, a model for the interactions of dye, PCE molecules and cement nanoparticles in the very first phase of cement hydration is derived T2 - Gesellschaft Deutscher Chemiker-Analytische Chemie-Anakon 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Cement hydration KW - Optical spectroscopy KW - Superplasticizers PY - 2017 AN - OPUS4-39882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weigert, Florian A1 - Müller, A. A1 - Häusler, I. A1 - Geißler, Daniel A1 - Skroblin, D. A1 - Unger, Wolfgang A1 - Radnik, Jörg A1 - Resch-Genger, Ute T1 - Combining HR‑TEM and XPS to elucidate the core–shell structure of ultrabright CdSe/CdS semiconductor quantum dots N2 - Controlling thickness and tightness of surface passivation shells is crucial for many applications of core–shell nanoparticles (NP). Usually, to determine shell thickness, core and core/shell particle are measured individually requiring the availability of both nanoobjects. This is often not fulfilled for functional nanomaterials such as many photoluminescent semiconductor quantum dots (QD) used for bioimaging, solid state lighting, and display technologies as the core does not show the applicationrelevant functionality like a high photoluminescence (PL) quantum yield, calling for a whole nanoobject approach. By combining high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS), a novel whole nanoobject approach is developed representatively for an ultrabright oleic acid-stabilized, thick shell CdSe/CdS QD with a PL quantum yield close to unity. The size of this spectroscopically assessed QD, is in the range of the information depth of usual laboratory XPS. Information on particle size and monodispersity were validated with dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) and compared to data derived from optical measurements. In addition to demonstrating the potential of this novel whole nanoobject approach for determining architectures of small nanoparticles, the presented results also highlight challenges faced by different sizing and structural analysis methods and method-inherent uncertainties. KW - Photoluminescence KW - Single particle KW - Microscopy KW - Particle architecture KW - Thickness KW - SAXS KW - Shell KW - XPS KW - TEM KW - Semiconductor KW - Quantum dot KW - Photophysics KW - Quantum yield PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517911 DO - https://doi.org/10.1038/s41598-020-77530-z VL - 10 IS - 1 SP - 20712 PB - Springer Nature AN - OPUS4-51791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Carl, F. A1 - Grauel, Bettina A1 - Pons, Monica A1 - Würth, Christian A1 - Haase, M. T1 - LiYF4:Yb/LiYF4 and LiYF4:Yb,Er/LiYF4 core/shell nanocrystals with luminescence decay times similar to YLF laser crystals and the upconversion quantum yield of the Yb,Er doped nanocrystals N2 - We developed a procedure to prepare luminescent LiYF4:Yb/LiYF4 and LiYF4:Yb,Er/LiYF4 core/shell nanocrystals with a size of approximately 40 nm revealing luminescence decay times of the dopant ions that approach those of high-quality laser crystals of LiYF4:Yb (Yb:YLF) and LiYF4:Yb,Er (Yb,Er:YLF) with identical doping concentrations. As the luminescence decay times of Yb3+ and Er3+ are known to be very sensitive to the presence of quenchers, the long decay times of the core/shell nanocrystals indicate a very low number of defects in the core particles and at the core/shell interfaces. This improvement in the performance was achieved by introducing two important modifications in the commonly used oleic acid based synthesis. First, the shell was prepared via anewly developed method characterized by a very low nucleation rate for particles of pure LiYF4 shell material. Second, anhydrous acetates were used as precursors and additional drying steps were applied to reduce the incorporation of OH− in the crystal lattice, known to quench the emission of Yb3+ ions. Excitation power density (P)-dependent absolute measurements of the upconversion luminescence quantum yield (Φ,UC) of LiYF4:Yb,Er/LiYF4 core/shell particles reveal a maximum value of 1.25% at P of 180 W·cm−2. Although lower than the values reported for NaYF4:18%Yb,2%Er core/shell nanocrystals with comparable sizes, these Φ, UC values are the highest reported so far for LiYF4:18%Yb,2%Er/LiYF4 nanocrystals without additional dopants. Further improvements May nevertheless be possible by optimizing the dopant concentrations in the LiYF4 nanocrystals. KW - Nano KW - Crystal KW - Quantum yield KW - LiYF4 KW - Synthesis KW - Lifetime KW - Fluorescence KW - NIR KW - Photoluminescence KW - Lanthanide KW - Upconversion nanoparticle KW - Nanomaterial PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515395 DO - https://doi.org/10.1007/s12274-020-3116-y SN - 1998-0124 VL - 14 IS - 3 SP - 797 EP - 806 PB - Springer AN - OPUS4-51539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saleh, Maysoon I. A1 - Rühle, Bastian A1 - Wang, Shu A1 - Radnik, Jörg A1 - You, Yi A1 - Resch-Genger, Ute T1 - Assessing the protective effects of different surface coatings on NaYF4:YB3+, Er3+, upconverting nanoparticles in buffer and DMEM N2 - We studied the dissolution behavior of β NaYF4:Yb(20%), Er(2%) UCNP of two different sizes in biologically relevant media i.e., water (neutral pH), phosphate buffered saline (PBS), and Dulbecco’s modified Eagle medium (DMEM) at different temperatures and particle concentrations. Special emphasis was dedicated to assess the influence of different surface functionalizations, particularly the potential of mesoporous and microporous silica shells of different thicknesses for UCNP stabilization and protection. Dissolution was quantified electrochemically using a fluoride ion selective electrode (ISE) and by inductively coupled plasma optical emission spectrometry (ICP OES). In addition, dissolution was monitored fluorometrically. These experiments revealed that a thick microporous silica shell drastically decreased dissolution. Our results also underline the critical influence of the chemical composition of the aqueous environment on UCNP dissolution. In DMEM, we observed the formation of a layer of adsorbed molecules on the UCNP surface that protected the UCNP from dissolution and enhanced their fluorescence. Examination of this layer by X ray photoelectron spectroscopy (XPS) and mass spectrometry (MS) suggested that mainly phenylalanine, lysine, and glucose are adsorbed from DMEM. These findings should be considered in the future for cellular toxicity studies with UCNP and other nanoparticles and the design of new biocompatible surface coatings. KW - Fluorescence KW - Lifetime KW - Method KW - Quantification KW - Stability KW - Coating KW - Surface chemistry KW - Lanthanide KW - Fluoride KW - Electrochemistry KW - ICP-OES KW - Upconversion KW - Nano KW - Particle KW - Aging KW - Quality assurance KW - Mass spectrometry KW - XPS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515984 DO - https://doi.org/10.1038/s41598-020-76116-z SN - 2045-2322 VL - 10 IS - 1 SP - 19318-1 EP - 19318-11 PB - Springer Nature CY - London AN - OPUS4-51598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kage, Daniel A1 - Hoffmann, Katrin A1 - Borcherding, H. A1 - Schedler, U. A1 - Resch-Genger, Ute T1 - Lifetime encoding in flow cytometry for bead‑based sensing of biomolecular interaction N2 - To demonstrate the potential of time-resolved flow cytometry (FCM) for bioanalysis, clinical diagnostics, and optically encoded bead-based assays, we performed a proof-of-principle study to detect biomolecular interactions utilizing fluorescence lifetime (LT)-encoded micron-sized polymer beads bearing target-specific bioligands and a recently developed prototype lifetime flow cytometer (LT-FCM setup). This instrument is equipped with a single excitation light source and different fluorescence detectors, one operated in the photon-counting mode for time-resolved measurements of fluorescence decays and three detectors for conventional intensity measurements in different spectral windows. First, discrimination of bead-bound biomolecules was demonstrated in the time domain exemplarily for two targets, Streptavidin (SAv) and the tumor marker human chorionic gonadotropin (HCG). In a second step, the determination of biomolecule concentration levels was addressed representatively for the inflammation-related biomarker tumor necrosis factor (TNF-α) utilizing fluorescence intensity measurements in a second channel of the LT-FCM instrument. Our results underline the applicability of LT-FCM in the time domain for measurements of biomolecular interactions in suspension assays. In the future, the combination of spectral and LT encoding and multiplexing and the expansion of the time scale from the lower nanosecond range to the longer nanosecond and the microsecond region is expected to provide many distinguishable codes. This enables an increasing degree of multiplexing which could be attractive for high throughput screening applications. KW - Fluorescence KW - Sensor KW - Assay KW - Protein KW - Multiplexing KW - Flow cytometry KW - Barcoding KW - Lifetime KW - Dye KW - Bead KW - Bead-based assay KW - Method KW - Quantification PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-516007 DO - https://doi.org/10.1038/s41598-020-76150-x VL - 10 IS - 1 SP - 19477 PB - Nature AN - OPUS4-51600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cruz-Alonso, M. A1 - Fernandez, B. A1 - Alvarez, L. A1 - Gonzalez-Iglesias, H. A1 - Traub, Heike A1 - Jakubowski, Norbert A1 - Pereiro, R. T1 - Bioimaging of metallothioneins in ocular tissue sections by laser ablation-ICP-MS using bioconjugated gold nanoclusters as specific tags N2 - An immunohistochemical method is described to visualize the distribution of metallothioneins 1/2 (MT 1/2) and metallothionein 3 (MT 3) in human ocular tissue. It is making use of (a) antibodies conjugated to gold nanoclusters (AuNCs) acting as labels, and (b) laser ablation (LA) coupled to inductively coupled plasma – mass spectrometry (ICP-MS). Water-soluble fluorescent AuNCs (with an average size of 2.7 nm) were synthesized and then conjugated to antibody by carbodiimide coupling. The surface of the modified AuNCs was then blocked with hydroxylamine to avoid nonspecific interactions with biological tissue. Immunoassays for MT 1/2 and MT 3 in ocular tissue sections (5 μm thick) from two post mortem human donors were performed. Imaging studies were then performed by fluorescence using confocal microscopy, and LA-ICP-MS was performed in the retina to measure the signal for gold. Signal amplification by the >500 gold atoms in each nanocluster allowed the antigens (MT 1/2 and MT 3) to be imaged by LA-ICP-MS using a laser spot size as small as 4 μm. The image patterns found in retina are in good agreement with those obtained by conventional fluorescence immunohistochemistry which was used as an established reference method. KW - Nanocluster KW - Immunohistochemistry KW - Laser ablation KW - ICP-MS KW - Fluorescence KW - Bioimaging PY - 2018 DO - https://doi.org/10.1007/s00604-017-2597-1 SN - 1436-5073 SN - 0026-3672 VL - 185 IS - 1 SP - 64 EP - 72 PB - Springer CY - Vienna AN - OPUS4-44637 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Wang, Cui A1 - You, Y. A1 - Förster, C. A1 - Schubert, H. A1 - Heinze, K. A1 - Seitz, M. T1 - NIR-NIR-Aufkonvertierung in molekularen Chrom-Ytterbium-Salzen N2 - Photonen-Aufkonvertierung in hetero-oligonuklearen, Metallkomplex-Architekturen mit organischen Liganden ist ein interessantes, aber bisher selten beobachtetes Phänomen, trotz des großen Potentials sowohl aus Sicht der Grundlagenforschung als auch aus der Anwendungsperspektive. Nun wurde ein neues photonisches Material aus molekularen Chrom(III)- und Ytterbium(III)-Komplexionen entwickelt. Dieses zeigt im Festkörper bei Raumtemperatur abhängig von der Anregungsleistungsdichte nach Anregung des 2F7/2! 2F5/2-3berganges des Ytterbiums bei ca. 980 nm eine kooperative Sensibilisierung der Chrom(III)-zentrierten 2E/2T1-Phosphoreszenz bei ca. 775 nm. Der Aufkonvertierungsprozess ist unempfindlich gegenüber Luftsauerstoff und kann in Gegenwart von Wassermolekülen im Kristallgitter beobachtet werden. KW - Crystal KW - Sensor KW - NIR KW - Yb(III) complex KW - Cr(III) KW - Upconversion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517217 DO - https://doi.org/10.1002/ange.202007200 VL - 132 IS - 42 SP - 18804 EP - 18808 PB - Angewandte Chemie AN - OPUS4-51721 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rietsch, P. A1 - Sobottka, S. A1 - Hoffmann, K. A1 - Popov, A. A. A1 - Hildebrandt, P. A1 - Sarkar, B. A1 - Resch-Genger, Ute A1 - Eigler, S. T1 - Between Aromatic and Quinoid Structure: A Symmetrical UV to Vis/NIR Benzothiadiazole Redox Switch N2 - Reversibly switching the light absorption of organic molecules by redox processes is of interest for applications in sensors, light harvesting, smart materials, and medical diagnostics. This work presents a symmetrical benzothiadiazole (BTD) derivative with a high fluorescence quantum yield in solution and in the crystalline state and shows by spectroelectrochemical analysis that reversible switching of UV absorption in the neutral state, to broadband Vis/NIR absorption in the 1st oxidized state, to sharp band Vis absorption in the 2nd oxidized state, is possible. For the one-electron oxidized species, formation of a delocalized radical is confirmed by electron paramagnetic resonance spectroelectrochemistry. Furthermore, our results reveal an increasing quinoidal distortion upon the 1st and 2nd oxidation, which can be used as the leitmotif for the development of BTD based redox switches. KW - Dye KW - Electrochemistry KW - Switch KW - Redox KW - Sensor KW - Photophysics KW - Quantum yield KW - photoluminescence PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517222 DO - https://doi.org/10.1002/chem.202004009 VL - 26 IS - 72 SP - 17361 EP - 17365 PB - Wiley-VCH GmbH AN - OPUS4-51722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reichenauer, F. A1 - Wang, Cui A1 - Förster, C. A1 - Boden, P. A1 - Ugur, N. A1 - Báez-Cruz, R. A1 - Kalmbach, J. A1 - Carrella, L. M. A1 - Rentschler, E. A1 - Ramanan, C. A1 - Niedner-Schatteburg, G. A1 - Gerhards, M. A1 - Seitz, M. A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Strongly Red-Emissive Molecular Ruby [Cr(bpmp)2]3+ Surpasses [Ru(bpy)3]2+ N2 - Gaining chemical control over the thermodynamics and kinetics of photoexcited states is paramount to an efficient and sustainable utilization of photoactive transition metal complexes in a plethora of technologies. In contrast to energies of charge Transfer states described by spatially separated orbitals, the energies of spinflip states cannot straightforwardly be predicted as Pauli Repulsion and the nephelauxetic effect play key roles. Guided by multireference quantum chemical calculations, we report a novel highly luminescent spin-flip emitter with a quantum chemically predicted blue-shifted luminescence. The spin-flip emission band of the chromium complex [Cr(bpmp)2]3+ (bpmp = 2,6-bis(2-pyridylmethyl) pyridine) shifted to higher energy from ca. 780 nm observed for known highly emissive chromium(III) complexes to 709 nm. The photoluminescence quantum yields climb to 20%, and very long excited state lifetimes in the millisecond range are achieved at room temperature in acidic D2O solution. Partial ligand deuteration increases the quantum yield to 25%. The high excited state energy of [Cr(bpmp)2]3+ and its facile reduction to [Cr(bpmp)2]2+ result in a high excited state redox potential. The ligand’s methylene bridge acts as a Brønsted acid quenching the luminescence at high pH. Combined with a pH-insensitive chromium(III) emitter, ratiometric optical pH sensing is achieved with single wavelength excitation. The photophysical and Ground state properties (quantum yield, lifetime, redox potential, and acid/base) of this spin-flip complex incorporating an earth-abundant metal surpass those of the classical precious metal [Ru(α-diimine)3]2+ charge transfer complexes, which are commonly employed in optical sensing and photo(redox) catalysis, underlining the bright future of these molecular ruby analogues. KW - Fluorescence KW - Optical probe KW - Sensor KW - PH KW - Quantum yield KW - Quality assurance KW - Complex KW - Cr(III) KW - Lifetime KW - Ligand KW - Theory PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530548 DO - https://doi.org/10.1021/jacs.1c05971 VL - 143 IS - 30 SP - 11843 EP - 11855 PB - ACS Publications AN - OPUS4-53054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kossatz, Philipp A1 - Mezhov, Alexander A1 - Andresen, Elina A1 - Prinz, Carsten A1 - Schmidt, Wolfram A1 - Resch-Genger, Ute T1 - Assessing the Applicability of Lanthanide-Based Upconverting Nanoparticles for Optically Monitoring Cement Hydration and Tagging Building Materials N2 - Chemically stable, lanthanide-based photon upconversion micro- and nanoparticles (UCNPs) with their characteristic multicolor emission bands in the ultraviolet (UV), visible (vis), near-infrared (NIR), and short-wave infrared (SWIR) arepromising optical reporters and barcoding tags. To assess the applicability of UCNPs for the monitoring of early stage cement hydration processes and as authentication tags for cementitious materials, we screened the evolution of the luminescence of Selfmade core-only NaYF4:Yb,Er UCNPs and commercial μm-sized Y2O2S:Yb,Er particles during the first stages of cement hydration, which largely determines the future properties of the hardened material. Parameters explored from the UCNP side included particle size, morphology, surface chemistry or coating, luminescence properties, and concentration in different cement mixtures. From the cement side, the influence of the mineral composition of the cement matrix was representatively examined for ordinary Portland cement (OPC) and its constituents tricalcium aluminate (C3A), tricalcium silicate (C3S), and gypsum at different water to cement ratios. Based on reflection and luminescence measurements, enabling online monitoring, which were complemented by XRD and isothermal heat-flow calorimetric measurements to determine whether the incorporation of these particles could impair cement hydration processes, well suited lanthanide particle reporters could be identified as well as application conditions. In addition, thereby the reporter influence on cement hydration kinetics could be minimized while still preserving a high level of information content. The best performance for the luminescence probing of changes during early stage cement hydration processes was observed for 25 nm-sized oleate (OA)-coated UCNPs added in a concentration of 0.1 wt %. Higher UCNP amounts of 1.0 wt % delayed cement hydration processes size- and surface coatingspecifically in the first 24 h. Subsequent luminescence stability screening studies performed over a period of about one year support the applicability of UCNPs as optical authentication tags for construction materials. KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Quantum yield KW - NIR KW - Mechanism KW - Characterization KW - XRD KW - Calorimetry KW - Advanced material KW - Cement KW - Monitoring KW - Surface KW - Size KW - Lifetime KW - Barcode KW - Lanthanide KW - Upconversion KW - Encoding KW - Method PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638318 DO - https://doi.org/10.1021/acsomega.5c02236 SN - 2470-1343 SP - 1 EP - 13 PB - ACS Publications AN - OPUS4-63831 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Xu, R. A1 - Teich, W. A1 - Frenzel, Florian A1 - Hoffmann, Katrin A1 - Radke, J. A1 - Rösler, J. A1 - Faust, K. A1 - Blank, A. A1 - Brandenburg, S. A1 - Misch, M. A1 - Vajkoczy, P. A1 - Onken, J. S. A1 - Resch-Genger, Ute T1 - Optical characterization of sodium fluorescein in vitro and ex vivo N2 - Objective: The utilization of fluorescein-guided biopsies and resection has been recently discussed as a suitable strategy to improve and expedite operative techniques for the resection of central nervous system (CNS) tumors. However, little is known about the optical properties of sodium fluorescein (NaFl) in human tumor tissue and their potential impact on ex vivo analyses involving fluorescence-based methods. Methods: Tumor tissue was obtained from a study cohort of an observational study on the utilization of fluorescein-guided biopsy and resection (n=5). The optical properties of fluorescein-stained tissue were compared to the optical features of the dye in vitro and in control samples consisting of tumor tissue of high-grade glioma patients (n=3) without intravenous (i.v.) application of NaFl. The dye-exposed tumor tissues were used for optical measurements to confirm the detectability of NaFl emission ex vivo. The tissue samples were fixed in 4%PFA, immersed in 30% sucrose, embedded in Tissue-Tek OCT compound, and cut to 10 mm cryosections. Spatially resolved emission spectra from tumor samples were recorded on representative slides with a Confocal Laser Scanning Microscope FV1000 (Olympus GmbH, Hamburg, Germany) upon excitation with lexc = 488 nm. Results: Optical measurements of fluorescein in 0.9% sodium chloride (NaCl) under in vitro conditions showed an absorption maximum of lmax abs = 479 nm as detected with spectrophotometer Specord 200 and an emission peak at lmax em = 538 nm recorded with the emCCD detection system of a custom-made microscope-based single particle setup using a 500 nm long-pass filter. Further measurements revealed pH- and concentration-dependent emission spectra of NaFl. Under ex vivo conditions, confocal laser scanning microscopy of fluorescein tumor samples revealed a slight bathochromic shift and a broadening of the emission band. Conclusion: Tumor uptake of NaFl leads to changes in the optical properties – a bathochromic shift and broadening of the emission band – possibly caused by the dye’s high pH sensitivity and concentration-dependent reabsorption acting as an innerfilter of the dye’s emission, particularly in the short wavelength region of the Emission spectrum where absorption and fluorescence overlap. Understanding the ex vivo optical properties of fluorescein is crucial for testing and validating its further applicability as an optical probe for intravital microscopy, immunofluorescence localization studies, and flow cytometry analysis. KW - Fluorescence KW - Optical probe KW - Sensor KW - Fluorescein KW - PH KW - Imaging KW - Tissue KW - Cancer KW - Medical diagnostics KW - Tumor KW - In vivo KW - Ex vivo KW - Quantum yield KW - Dye KW - Quality assurance KW - Microscopy PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527843 DO - https://doi.org/10.3389/fonc.2021.654300 SN - 2234-943X VL - 11 SP - 1 EP - 8 PB - Frontiers Media CY - Lausanne AN - OPUS4-52784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niederleithinger, Ernst A1 - Gardner, S. A1 - Kind, Thomas A1 - Kaiser, R. A1 - Grunwald, Marcel A1 - Yang, G. A1 - Redmer, Bernhard A1 - Waske, Anja A1 - Mielentz, Frank A1 - Effner, Ute A1 - Köpp, Christian A1 - Clarkson, A. A1 - Thompson, F. A1 - Ryan, M. A1 - Mahon, D. T1 - Muon Tomography of the Interior of a Reinforced Concrete Block: First Experimental Proof of Concept N2 - Quality assurance and condition assessment of concrete structures is an important topic world-wide due to the aging infrastructure and increasing traffic demands. Common topics include, but are not limited to, localisation of rebar or tendon ducts, geometrical irregularities, cracks, voids, honeycombing or other flaws. Non-destructive techniques such as ultrasound or radar have found regular, successful practical application but sometimes suffer from limited resolution and accuracy, imaging artefacts or restrictions in detecting certain features. Until the 1980s X-ray transmission was used in case of special demands and showed a much better resolution than other NDT techniques. However, due to safety concerns and cost issues, this method is almost never used anymore. Muon tomography has received much attention recently. Novel detectors for cosmic muons and tomographic imaging algorithms have opened up new fields of application, such as the investigation of freight containers. Muon imaging also has the potential to fill some of the gaps currently existing in concrete NDT. As a first step towards practical use and as a proof of concept we used an existing system to image the interior of a reference reinforced 600 kg concrete block. Even with a yet not optimized setup for this kind of investigation, the muon imaging results are at least of similar quality compared to ultrasonic and radar imaging, potentially even better. The data acquisition takes more time and signals contain more noise, but the images allowed to detect the same important features that are visible in conventional high energy X-ray tomography. In our experiment, we have shown that muon imaging has potential for concrete inspection. The next steps include the development of mobile detectors and optimising acquisition and imaging parameters. KW - Concrete KW - Muon KW - Radar KW - Ultrasound KW - X-ray PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529974 DO - https://doi.org/10.1007/s10921-021-00797-3 VL - 40 IS - 3 SP - 1 EP - 14 PB - Springer Nature AN - OPUS4-52997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauli, Jutta A1 - Ramírez, A. A1 - Crasselt, C. A1 - Schmidt, W. A1 - Resch-Genger, Ute T1 - Utilizing optical spectroscopy and 2',7'-difluorofluorescein to characterize the early stages of cement hydration N2 - The increasingly sophisticated nature of modern, more environmentally friendly cementitious binders requires a better understanding and control particularly of the complex, dynamic processes involved in the early phase of cement hydration. In-situ monitoring of properties of a constantly changing system over a defined period of time calls for simple, sensitive, fast, and preferably also non-invasive methods like optical spectroscopy KW - Flourescence KW - Optical probe KW - Sensor KW - Dye KW - Flourescin KW - Photophysics KW - PH KW - Quantum yield KW - Quality assurance KW - Mechanism KW - Cement KW - Concrete KW - Building material KW - Hydration KW - Process monitoring PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537176 DO - https://doi.org/10.1088/2050-6120/ac2da0 SN - 2050-6120 VL - 10 IS - 1 SP - 2 EP - 13 PB - IOP Science AN - OPUS4-53717 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Büttner, C. A1 - Niederleithinger, Ernst A1 - Buske, S. A1 - Friedrich, C. T1 - Ultrasonic Echo Localization Using Seismic Migration Techniques in Engineered Barriers for NuclearWaste Storage N2 - In the framework of non-destructive-testing advanced seismic imaging techniques have been applied to ultrasonic echo data in order to examine the integrity of an engineered test-barrier designed to be used for sealing an underground nuclear waste disposal site. Synthetic data as well as real multi-receiver ultrasonic data acquired at the test site were processed and imaged using Kirchhoff prestack depth migration reverse time migration (RTM). In general, both methods provide a good Image quality as demonstrated by various case studies, however deeper parts within the test barrier containing inclined reflectors were reconstructed more accurately by RTM. In particular, the image quality of a specific target reflector at a depth of 8 m in the test-barrier has been significantly improved compared to previous investigations using synthetic aperture Focusing technique, which justifies the considerable computing time of this method. KW - Radioactive waste disposal KW - Engineered barrier KW - Ultrasound KW - Imaging KW - Crack detection PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537956 DO - https://doi.org/10.1007/s10921-021-00824-3 SN - 0195-9298 VL - 40 IS - 4 SP - 1 EP - 10 PB - Springer AN - OPUS4-53795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Denißen, M. A1 - Hannen, R. A1 - Itskalov, D. A1 - Biesen, L. A1 - Nirmalananthan-Budau, Nithiya A1 - Hoffmann, Katrin A1 - Reiss, G. J. A1 - Resch-Genger, Ute A1 - Müller, T. J. J. T1 - One-pot synthesis of a white-light emissive bichromophore operated by aggregation-induced dual emission (AIDE) and partial energy transfer N2 - Merocyanine–triarylamine bichromophores are readily synthesized by sequentially Pd-catalyzed insertion alkynylation–Michael–Suzuki four-component reactions. White-light emissive systems form upon aggregation in 1 : 99 and 0.1 : 99.9 vol% CH2Cl2–cyclohexane mixtures, ascribed to aggregation-induced dual emission (AIDE) in combination with partial energy transfer between both chromophore units as supported by spectroscopic studies. KW - Energy transfer KW - Nano KW - Nanoparticle KW - Photoluminescence KW - Fluorescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - Dye KW - Enhancement KW - Particle KW - Polarity KW - AIE KW - Aggregation KW - Aggregation-induced emission KW - Solid state emission KW - Merocyanine PY - 2020 DO - https://doi.org/10.1039/d0cc03451g VL - 56 IS - 54 SP - 7407 PB - Royal Society of Chemistry AN - OPUS4-50936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nordholt, Niclas A1 - O'Hara, Kate A1 - Resch-Genger, Ute A1 - Blaskovich, M. A1 - Rühle, Bastian A1 - Schreiber, Frank T1 - A fluorescently labelled quaternary ammonium compound (NBD-DDA) to study resistance mechanisms in bacteria N2 - Quaternary ammonium compounds (QACs) are widely used as active agents in disinfectants, antiseptics, and preservatives. Despite being in use since the 1940s, there remain multiple open questions regarding their detailed mode-of-action and the mechanisms, including phenotypic heterogeneity, that can make bacteria less susceptible to QACs. To facilitate studies on resistance mechanisms towards QACs, we synthesized a fluorescent quaternary ammonium compound, namely N-dodecyl-N,N-dimethyl-[2-[(4-nitro-2,1,3-benzoxadiazol-7-yl)amino]ethyl]azanium-iodide (NBD-DDA). NBD-DDA is readily detected by flow cytometry and fluorescence microscopy with standard GFP/FITC-settings, making it suitable for molecular and single-cell studies. As a proof-of-concept, NBD-DDA was then used to investigate resistance mechanisms which can be heterogeneous among individual bacterial cells. Our results reveal that the antimicrobial activity of NBD-DDA against Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa is comparable to that of benzalkonium chloride (BAC), a widely used QAC, and benzyl-dimethyl-dodecylammonium chloride (BAC12), a mono-constituent BAC with alkyl-chain length of 12 and high structural similarity to NBD-DDA. Characteristic time-kill kinetics and increased tolerance of a BAC tolerant E. coli strain against NBD-DDA suggest that the mode of action of NBD-DDA is similar to that of BAC. As revealed by confocal laser scanning microscopy (CLSM), NBD-DDA is preferentially localized to the cell envelope of E. coli, which is a primary target of BAC and other QACs. Leveraging these findings and NBD-DDA‘s fluorescent properties, we show that reduced cellular accumulation is responsible for the evolved BAC tolerance in the BAC tolerant E. coli strain and that NBD-DDA is subject to efflux mediated by TolC. Overall, NBD-DDA’s antimicrobial activity, its fluorescent properties, and its ease of detection render it a powerful tool to study resistance mechanisms of QACs in bacteria and highlight its potential to gain detailed insights into its mode-of-action. KW - Antimicrobial resistance KW - Bacteria KW - Disinfection KW - Biocides PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563811 DO - https://doi.org/10.3389/fmicb.2022.1023326 SN - 1664-302X IS - 13 SP - 1 EP - 13 PB - Frontiers Media CY - Lausanne AN - OPUS4-56381 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Arndt, R.W. A1 - Grosse, C.U, A1 - Maehner, D. A1 - Niederleithinger, Ernst A1 - Taffe, A. A1 - Algernon, D. A1 - Berger, J. A1 - Kessler, S. A1 - Krueger, M. A1 - Kruschwitz, Sabine A1 - Ufermann-Wallmeier, D. A1 - Walther, A. T1 - Non-destructive testing in civil engineering: A memorandum for teaching at German-speaking universities N2 - This contribution summarizes actual developments and draft fundamental teaching topics in the field of nondestructive testing in civil engineering (NDT-CE). It is based on the first memorandum on teaching and research in the field of NDT-CE at German speaking universities and provides an overview of the academic education and highlights possible focuses, especially in teaching but also takes into account noteworthy developments and topics in research in the field of NDT-CE. Suggestions are given for the development and advancement of the teaching curricula in regards to a comprehensive and sound professional education of students in civil engineering and adjacent disciplines. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Curriculum KW - NDT-CE KW - University KW - Competencies PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563269 UR - https://www.ndt.net/article/ndtce2022/paper/61547_manuscript.pdf SP - 1 EP - 10 PB - NDT.net AN - OPUS4-56326 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabe, U. A1 - Pudovikov, S. A1 - Herrmann, H.-G. A1 - Wiggenhauser, H. A1 - Prabhakara, Prathik A1 - Niederleithinger, Ernst T1 - Evaluation of retroreflective corner echo for detection of surface breaking cracks in concrete by ultrasound N2 - The retroreflective corner echo is used, for example, in ultrasonic non-destructive testing of metals to find fatigue cracks in tubes or shafts. If the much weaker crack tip signal is additionally detected, the crack length can also be determined. A corner reflection occurs in cases of surface breaking cracks with predominantly perpendicular orientation to the surface. The intensity of the corner reflection depends on the angle of incidence and on the ultrasonic wave mode used. For the reliable detection of vertical surface breaking cracks in metals, transversal waves are commonly used, which propagate at an angle of 37° to 53° to the inspection surface. As shown in this contribution, the wide spread low frequency ultrasonic arrays with dry point contact sources available for ultrasonic testing of concrete also allow to receive corner echoes. These devices generate transversal waves in concrete structures with a large divergence of the sound field. A series of experiments was carried out with such dry point contact arrays on concrete specimens with artificial test defects and controlled induced cracks of different depths. The ultrasonic time-of-flight signals were recorded, exported and reconstructed utilising the SAFT (Synthetic Aperture Focusing Technique) algorithm. The SAFT reconstruction parameters were adjusted to visualize the corner echo indication. As will be shown, with this targeted processing, the reproducible detection of surface breaking cracks in concrete is possible. The retroreflective corner echo can thus be exploited in civil engineering for non-destructive inspection of concrete. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Concrete KW - Crack depth KW - Ultrasound KW - SAFT PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563365 UR - https://www.ndt.net/article/ndtce2022/paper/27256_manuscript.pdf IS - 27256 SP - 1 EP - 4 PB - NDT.net AN - OPUS4-56336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Landis, E. A1 - Hassefras, Emiel A1 - Oesch, Tyler A1 - Niederleithinger, Ernst T1 - A Microstructural Basis for Diffuse Ultrasound in Concrete N2 - Attenuation of ultrasonic signals in concrete has the potential to carry much information about the microstructure of the material. In this work a series of concrete specimens of varying porosities and pore size distributions were internally imaged with x-ray computed tomography (CT), and then subsequently examined with throughtransmission ultrasound. The CT images were used to quantify both capillary porosity of cement paste as well as internal interfaces that are likely to produce elastic wave scattering. Ultrasound signals were represented as a diffusion process such that absorption and scattering attenuation could be isolated. As implemented, the diffusion model was a poor predictor of capillary porosity, while diffusivity was a reasonable predictor of scattering interfaces. Diffusivity was found to scale extremely well with small scale porosity, which made it a good predictor of compressive strength. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Concrete KW - X-ray tomography KW - Ultrasound PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563371 UR - https://www.ndt.net/article/ndtce2022/paper/61592_manuscript.pdf SP - 1 EP - 4 PB - NDT.net AN - OPUS4-56337 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Behnke, Thomas A1 - Gienger, J. A1 - Resch-Genger, Ute T1 - Efficiency scale for scatteringluminescent particles linkedto fundamental and measurablespectroscopic properties N2 - Comparing the performance of molecular and nanoscale luminophores and luminescent microand nanoparticles and estimating achievable signal amplitudes and limits of detection requires a standardizable intensity scale. This initiated the development of the relative MESF (number of molecules of equivalent soluble fluorochromes) and ERF (equivalent reference fluorophores) scales for flow cytometry and fluorescence microscopy. Both intensity scales rely on fluorescence intensity values assigned to fluorescent calibration beads by an intensity comparison to spectrally closely matching fluorophore solutions of known concentration using a spectrofluorometer. Alternatively, the luminophore or bead brightness (B) can be determined that equals the product of the absorption cross section (σa) at the excitation wavelength (σa(λex)) and the photoluminescence quantum yield (Φpl). Thereby, an absolute scale based on fundamental and measurable spectroscopic properties can be realized which is independent of particle size, material, and luminophore staining or labeling density and considers the sensitivity of the optical properties of luminophores to their environment. Aiming for establishing such a brightness scale for light-scattering dispersions of luminescent particles with sizes exceeding a few ten nanometers, we demonstrate how the brightness of quasi-monodisperse 25 nm, 100 nm, and 1 μm sized polystyrene particles (PSP), loaded with two different dyes in varying concentrations, can be obtained with a single custom-designed integrating sphere setup that enables the absolute determination of Φpl and transmittance and diffuse reflectance measurements. The resulting Φpl, σa(λex), imaginary parts of the refractive index, and calculated B values of these samples are given in dependence of the number of incorporated dye molecule per particle. Finally, a unitless luminescence efficiency (LE) is defined allowing for the direct comparison of luminescence efficiencies of particles with different sizes. KW - Brightness KW - Quantum yield KW - Cross section KW - Lluminescence PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573680 DO - https://doi.org/10.1038/s41598-023-32933-6 VL - 13 IS - 1 SP - 14 PB - Nature AN - OPUS4-57368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grohmann, Maria A1 - Niederleithinger, Ernst A1 - Buske, S. A1 - Büttner, C. T1 - Application of Elastic P-SV Reverse Time Migration to Synthetic Ultrasonic Echo Data from Concrete Members N2 - The ultrasonic echo technique is frequently used in non-destructive testing (NDT) of concrete structures for thickness measurements, geometry determinations as well as localization of built-in components. To improve ultrasonic imaging of complex structures in concrete, we transferred a geophysical imaging technique, the reverse time migration (RTM), to NDT in civil engineering. In contrast to the conventionally used synthetic aperture focusing technique (SAFT) algorithms, RTM is a wavefield continuation method in time and uses the full wave equation. Thus, RTM can handle complicated wave propagations in any direction without dip limitation. In this paper, we focused on the application and evaluation of a two-dimensional (2D) elastic RTM algorithm considering compressional waves, vertically polarized shear waves, and Rayleigh waves. We tested the elastic RTM routine on synthetic ultrasonic echo data generated with a 2D concrete model consisting of several steps and circular air inclusions. As these complex structures can often be found in real-world NDT use cases, their imaging is especially important. By using elastic RTM, we were able to clearly reproduce vertical reflectors and lower edges of circular air voids inside our numerical concrete model. Such structures cannot be imaged with conventional SAFT algorithms. Furthermore, the used elastic RTM approach also yielded a better reconstruction of a horizontal reflector and upper boundaries of circular air inclusions. Our encouraging results demonstrate that elastic RTM has the potential to significantly improve the imaging of complex concrete structures and, thus, is a step forward for detailed, high-quality ultrasonic NDT in civil engineering. KW - Concrete KW - Ultrasound KW - Imaging KW - Reverse time migration KW - Elastic PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580680 DO - https://doi.org/10.1007/s10921-023-00962-w SN - 0195-9298 VL - 42 IS - 3 SP - 1 EP - 18 PB - Springer Nature AN - OPUS4-58068 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabe, U. A1 - Pudovikov, S. A1 - Herrmann, H.-G. A1 - Wiggenhauser, H. A1 - Prabhakara, Prathik A1 - Niederleithinger, Ernst T1 - Using the Corner Reflection for Depth Evaluation of Surface Breaking Cracks in Concrete by Ultrasound N2 - The corner echo is a well-known effect in ultrasonic testing, which allows detection of surface breaking cracks with predominantly perpendicular orientation to the surface as, for example, corrosion cracks in metal pipes or shafts. This echo is formed by two planes, the surface of the crack and the surface which the crack breaks. It can also be classified as a half-skip method, since a reflection of the pulse occurs on the backwall before the reflection at the defect takes place. In combination with the diffraction from the crack tip, the corner echo also allows crack sizing. As shown in this paper, the corner reflection can be used in civil engineering for nondestructive inspection of concrete. Commercially available low frequency ultrasonic arrays with dry point contact sources generate SH transversal waves with sufficient divergence of the sound field in order to detect corner reflections. Ultrasonic line-scans and area-scans were acquired with a linear array on flat concrete specimens, and the data were reconstructed by the Synthetic aperture focusing technique. If the angles and the area of reconstruction are chosen accordingly, the corner echo reflection can be distinguished from other ultrasonic information. The corner echo can thus be used as a method for deciding whether a crack is a partial-depth crack or a full-depth crack and thus for obtaining a statement about crack depth. This paper presents corresponding experimental results obtained on concrete specimens with artificial test defects and cracks induced under controlled conditions. KW - Ultrasound KW - Crack depth KW - Concrete KW - Corner echo PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-574631 DO - https://doi.org/10.1007/s10921-023-00956-8 SN - 0195-9298 VL - 42 IS - 2 SP - 1 EP - 19 PB - Springer Nature AN - OPUS4-57463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stein, L. A1 - Wang, Cui A1 - Förster, C. A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Bulky ligands protect molecular ruby from oxygen quenching N2 - Chromium(III) complexes can show phosphorescence from the spin-flip excited doublet states 2E/2T1 in the near-infrared with high photoluminescence quantum yields and extremely long lifetimes in the absence of dioxygen. The prototype molecular ruby, [Cr(ddpd)2]3+ (ddpd = N,N’-dimethyl-N,N’-dipyridine-2-ylpyridine-2,6-diamine), has a photoluminescence quantum yield and a luminescence lifetime of 13.7% and 1.1 ms in deaerated acetonitrile, respectively. However, its luminescence is strongly quenched by 3O2 via an efficient Dexter-type energy transfer process. To enable luminescence applications of molecular rubies in solution under aerobic conditions, we explored the potential of sterically demanding ddpd ligands to shield the chromium(III) center from O2 using steady state and time-resolved photoluminescence spectroscopy. The structures of the novel complexes with sterically demanding ligands were investigated by single crystal X-ray diffraction and quantum chemically by density functional theory calculations. The O2 sensitivity of the photoluminescence was derived from absolutely measured photoluminescence quantum yields and excited state lifetimes under inert and aerobic conditions and by Stern–Volmer analyses of these data. Optimal sterically shielded chromium(III) complexes revealed photoluminescence quantum yields of up to 5.1% and excited state lifetimes of 518 μs in air-saturated acetonitrile, underlining the large potential of this ligand design approach to broaden the applicability of highly emissive chromium(III) complexes. KW - Fluorescence KW - Synthesis KW - Production KW - Optical spectroscopy KW - Ligand KW - Photophysics KW - Cr(III) KW - Mechanism KW - NIR KW - Sensor KW - Oxygen PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570807 DO - https://doi.org/10.1039/d2dt02950b VL - 51 IS - 46 SP - 17664 EP - 17670 PB - The Royal Society of Chemistry CY - Berlin AN - OPUS4-57080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maack, Stefan A1 - Küttenbaum, Stefan A1 - Bühling, Benjamin A1 - Borchardt-Giers, Kerstin A1 - Aßmann, Norman A1 - Niederleithinger, Ernst T1 - Low frequency ultrasonic pulse-echo datasets for object detection and thickness measurement in concrete specimens as testing tasks in civil engineering N2 - The dataset contains raw data gathered with the ultrasonic pulse-echo method on concrete specimens. The surfaces of the measuring objects were automatically scanned point by point. Pulse-echo measurements were performed at each of these measuring points. The test specimens represent two typical testing tasks in construction industry: the detection of objects and the determination of dimensions to describe the geometry of components. By automating the measurement process, the different test scenarios are examined with a high repeatability, precision and measuring point density. Longitu- dinal and transversal waves were used and the geometrical aperture of the testing system was varied. The low-frequency probes operate in a range of up to approximately 150 kHz. In addition to the specification of the geometrical dimensions of the individual probes, the directivity pattern and the sound field characteristics are provided. The raw data are stored in a universally readable format. The length of each time signal (A-scan) is two milliseconds and the sampling rate is two mega-samples per second. The provided data can be used for comparative studies in signal analysis, imag- ing and interpretation as well as for evaluation pur- poses in different, practically relevant testing scenarios. KW - Validation KW - Puls-echo method KW - Ultrasonic KW - Non-destructive testing KW - SAFT KW - Reconstruction algorithm PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575185 DO - https://doi.org/10.1016/j.dib.2023.109233 SN - 2352-3409 VL - 48 SP - 1 EP - 16 PB - Elsevier Inc. AN - OPUS4-57518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Potopnyk, M. A1 - Mech-Piskorz, J. A1 - Angulo, G. A1 - Ceborska, M. A1 - Luboradzki, R. A1 - Andresen, Elina A1 - Gajek, A. A1 - Wisniewska, A. A1 - Resch-Genger, Ute T1 - Aggregation/Crystallization-Induced Emission in Naphthyridine-Based Carbazolyl-Modified Donor-Acceptor Boron Dyes Tunable by Fluorine Atoms N2 - Four donor-acceptor boron difluoride complexes based on the carbazole electron donor and the [1,3,5,2]oxadiazaborinino[3,4-a][1,8]naphthyridine acceptor were designed, synthesized, and systematically spectroscopically investigated in solutions, in the solid states, and dye-doped polymer films. The dyes exhibit an intense blue to red solid-state emission with photoluminescence quantum yields of up to 56% in pure dye samples and 86% in poly(methyl methacrylate) films. All boron complexes show aggregation-induced emission and reversible mechanofluorochromism. The optical properties of these dyes and their solid state luminescence can be tuned by substitution pattern, i.e., the substituents at the naphthyridine unit. Exchange of CH3- for CF3-groups does not only increase the intramolecular charge transfer character, but also provides a crystallization-induced emission enhancement. KW - Spectroscopy KW - Dye KW - Luminescence KW - Sensor KW - Fluorescence KW - Quantum yield KW - Lifetime KW - Quality assurance KW - Synthesis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597426 DO - https://doi.org/10.1002/chem.202400004 SN - 0947-6539 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-59742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Labrador-Paez, Lucia, L. A1 - Kankare, J. A1 - Hyppanen, I. A1 - Soukka, T. A1 - Andresen, Elina A1 - Resch-Genger, Ute A1 - Widengren, J A1 - Liu, H. T1 - Frequency-Domain Method for Characterization of Upconversion Luminescence Kinetics N2 - The frequency-domain (FD) method provides an alternative to the commonly used time-domain (TD) approach in characterizing the luminescence kinetics of luminophores, with its own strengths, e.g., the capability to decouple multiple lifetime components with higher reliability and accuracy. While extensively explored for characterizing luminophores with down-shifted emission, this method has not been investigated for studying nonlinear luminescent materials such as lanthanide-doped upconversion nanoparticles (UCNPs), featuring more complicated kinetics. In this work, employing a simplified rate-equation model representing a standard two-photon energy-transfer upconversion process, we thoroughly analyzed the response of the luminescence of UCNPs in the FD method. We found that the FD method can potentially obtain from a single experiment the effective decay rates of three critical energy states of the sensitizer/activator ions involved in the upconversion process. The validity of the FD method is demonstrated by experimental data, agreeing reasonably well with the results obtained by TD methods. KW - Quality assurance KW - Luminescence KW - Method KW - Quantitative spectroscopy KW - Nano KW - Particle KW - Lifetime KW - Method development PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597435 DO - https://doi.org/10.1021/acs.jpclett.3c00269 SP - 3436 EP - 3444 AN - OPUS4-59743 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohammad, W. A1 - Wegner, Karl David A1 - Comby-Zerbino, C. A1 - Trouillet, V. A1 - Ogayer, M. P. A1 - Coll, J.-L. A1 - Marin, R. A1 - Jaque Garcia, D. A1 - Resch-Genger, Ute A1 - Antoine, R. A1 - Le Guevel, X. T1 - Enhanced brightness of ultra-small gold nanoparticles in the second biological window through thiol ligand shell control N2 - Gold-based nanoparticles below 2 nm in size are promising as luminescent probes for in vivo bioimaging, owing to their brightness and rapid renal clearance. However, their use as contrast agents in the near-infrared II (NIR-II, 1000–1700 nm) range remains challenging due to their low photoluminescence (PL) quantum yield. To address this, PL enhancement can be achieved by either rigidifying the ligand-shell structure or increasing the size of the ligand shell. In this study, we synthesized ultra-small gold nanoparticles stabilized by co-ligands, namely monothiol and short dithiol molecules. By precisely controlling the amount of reducing agent used during particle preparation, we successfully modulated the physicochemical properties of the co-ligand shell, including its size, composition, and structure. Consequently, we achieved a remarkable 60-fold increase in the absorption cross-section at 990 nm while maintaining the small size of the 1.5-nm metal core. The analytical and optical characterization of our thiol-capped gold nanoparticles indicates that the ligand shell size is governed by the quantity of the reducing agent, which, in turn, impacts the balance between radiative and non-radiative processes, thereby influencing the PL quantum yield. KW - Gold nanocluster KW - NIR-II fluorescence KW - SWIR KW - Nanomaterial design KW - Calibrated fluorescence measurements PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588117 DO - https://doi.org/10.1039/D3TC03021K SN - 2050-7526 VL - 11 IS - 42 SP - 14714 EP - 14724 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Billimoria, K. A1 - Diaz Fernandez, Y. A. A1 - Andresen, Elina A1 - Sorzabal-Bellido, I. A1 - Huelga-Suarez, G. A1 - Bartczak, D. A1 - Ortiz de Solórzano, C. A1 - Resch-Genger, Ute A1 - Goenaga Infante, H. T1 - The potential of bioprinting for preparation of nanoparticle-based calibration standards for LA-ICP-ToF-MS quantitative imaging N2 - This paper discusses the feasibility of a novel strategy based on the combination of bioprinting nano-doping technology and laser ablation-inductively coupled plasma time-of-flight mass spectrometry analysis for the preparation and characterization of gelatin- based multi-element calibration standards suitable for quantitative imaging. To achieve this, lanthanide up-conversion nanoparticles were added to a gelatin matrix to produce the bioprinted calibration standards. The features of this bioprinting approach were com- pared with manual cryosectioning standard preparation, in terms of throughput, between batch repeatability and elemental signal homogeneity at 5 μm spatial resolution. By using bioprinting, the between batch variability for three independent standards of the same concentration of 89 Y (range 0–600 mg/kg) was reduced to 5% compared to up to 27% for cryosectioning. On this basis, the relative standard deviation ( RSD ) obtained between three independent calibration slopes measured within 1 day also reduced from 16% (using cryosectioning ) to 5% (using bioprinting), supporting the use of a single standard preparation replicate for each of the concentrations to achieve good calibration performance using bioprinting. This helped reduce the analysis time by approximately 3-fold. With cryosectioning each standard was prepared and sectioned individually, whereas using bio-printing it was possible to have up to six different standards printed simultaneously, reducing the preparation time from approximately 2 h to under 20 min (by approxi- mately 6-fold). The bio-printed calibration standards were found stable for a period of 2 months when stored at ambient temperature and in the dark. KW - Environmental analysis KW - LA-ICP-MS KW - Lanthanide KW - Tag KW - Fluorescence KW - Nanoparticles KW - Reference material KW - Quality assurance KW - 3D-printing KW - Synthesis KW - Production KW - Multimodal PY - 2022 DO - https://doi.org/10.1093/mtomcs/mfac088 SN - 1756-591X VL - 14 IS - 12 SP - 1 EP - 9 PB - Oxford University Press CY - Oxford AN - OPUS4-57018 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst A1 - Guangliang, Y. A1 - Mahon, D. A1 - Gardner, S. T1 - Muon tomography applied to assessment of concrete structures: First experiments and simulations. N2 - Non-destructive techniques for reinforced or prestressed concrete inspection such as ultrasound or radar have found regular, successful practical application but sometimes suffer from limited resolution and accuracy, imaging artefacts or restrictions in detecting certain features. Until the 1980s X-ray transmission was used in case of special demands and showed a much better resolution than other NDT techniques. However, due to safety concerns and cost issues, this method is almost never used anymore. Muon tomography has received much attention recently. Novel detectors for cosmic muons and tomographic imaging algorithms have opened new fields of application. As a first step towards practical application in civil engineering and as a proof of concept we used an existing system to image the interior of a reference reinforced 600 kg concrete block. Even with a yet not optimized setup for this kind of investigation, the muon imaging results are at least of similar quality compared to ultrasonic and radar imaging, potentially even better. In a second step, we have performed simulations to assess the potential for a set of important testing problems such as grouting defects in tendon ducts. The next steps include the development of mobile detectors and optimizing acquisition and imaging parameters. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Muon tomography KW - Concrete KW - Inspection KW - Simulation PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563224 UR - https://www.ndt.net/article/ndtce2022/paper/60943_manuscript.pdf SP - 1 EP - 8 PB - NDT.net AN - OPUS4-56322 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Srivastava, Priyanka A1 - Tavernaro, Isabella A1 - Scholtz, Lena A1 - Genger, C. A1 - Welker, P. A1 - Schreiber, Frank A1 - Meyer, Klas A1 - Resch-Genger, Ute T1 - Dual color pH probes made from silica and polystyrene nanoparticles and their performance in cell studies N2 - Ratiometric green–red fluorescent nanosensors for fluorometrically monitoring pH in the acidic range were designed from 80 nm-sized polystyrene (PS) and silica (SiO2) nanoparticles (NPs), red emissive reference dyes, and a green emissive naphthalimide pH probe, analytically and spectroscopically characterized, and compared regarding their sensing performance in aqueous dispersion and in cellular uptake studies. Preparation of these optical probes, which are excitable by 405 nm laser or LED light sources, involved the encapsulation of the pH-inert red-fuorescent dye Nile Red (NR) in the core of self-made carboxylated PSNPs by a simple swelling procedure and the fabrication of rhodamine B (RhB)-stained SiO2-NPs from a silane derivative of pH-insensitive RhB. Subsequently, the custom-made naphthalimide pH probe, that utilizes a protonation-controlled photoinduced electron transfer process, was covalently attached to the carboxylic acid groups at the surface of both types of NPs. Fluorescence microscopy studies with the molecular and nanoscale optical probes and A549 lung cancer cells confirmed the cellular uptake of all probes and their penetration into acidic cell compartments, i.e., the lysosomes, indicated by the switching ON of the green naphthalimide fluorescence. This underlines their suitability for intracellular pH sensing, with the SiO2-based nanosensor revealing the best performance regarding uptake speed and stability. KW - Sensors KW - Silica and polystyrene nanoparticles KW - pH probe KW - Fluorescence spectroscopy KW - Cell studies KW - Dye KW - Particle synthesis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569198 DO - https://doi.org/10.1038/s41598-023-28203-0 SN - 2045-2322 VL - 13 IS - 1 SP - 1321 EP - 1336 PB - Nature CY - London AN - OPUS4-56919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prabhakara, Prathik A1 - Mielentz, Frank A1 - Stolpe, Heiko A1 - Behrens, Matthias A1 - Lay, Vera A1 - Niederleithinger, Ernst T1 - Validation of novel ultrasonic phased array borehole probe by using simulation and measurement N2 - Low-frequency ultrasonic testing is a well-established non-destructive testing (NDT) method in civil engineering for material characterization and the localization of cracks, reinforcing bars and delamination. A novel ultrasonic borehole probe is developed for in situ quality assurance of sealing structures in radioactive waste repositories using existing research boreholes. The aim is to examine the sealing structures made of salt concrete for any possible cracks and delamination and to localize built-in components. A prototype has been developed using 12 individual horizontal dry point contact (DPC) shear wave transducers separated by equidistant transmitter/receiver arrays. The probe is equipped with a commercially available portable ultrasonic flaw detector used in the NDT civil engineering industry. To increase the sound pressure generated, the number of transducers in the novel probe is increased to 32 transducers. In addition, the timed excitation of each transducer directs a focused beam of sound to a specific angle and distance based on the previously calculated delay time. This narrows the sensitivity of test volume and improves the signal-to-noise ratio of the received signals. In this paper, the newly designed phased array borehole probe is validated by beam computation in the CIVA software and experimental investigations on a half-cylindrical test specimen to investigate the directional characteristics. In combination with geophysical reconstruction methods, it is expected that an optimised radiation pattern of the probe will improve the signal quality and thus increase the reliability of the imaging results. This is an important consideration for the construction of safe sealing structures for the safe disposal of radioactive or toxic waste. KW - Ultrasound KW - Phased array KW - Concrete KW - Borehole PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565722 DO - https://doi.org/10.3390/s22249823 SN - 1424-8220 VL - 22 IS - 24 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-56572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholtz, Lena A1 - Tavernaro, Isabella A1 - Eckert, J. G. A1 - Lutowski, Marc A1 - Geißler, Daniel A1 - Hertwig, Andreas A1 - Hidde, Gundula A1 - Bigall, N. C. A1 - Resch-Genger, Ute T1 - Influence of nanoparticle encapsulation and encoding on the surface chemistry of polymer carrier beads N2 - Surface-functionalized polymer beads encoded with molecular luminophores and nanocrystalline emitters such as semiconductor nanocrystals, often referred to as quantum dots (QDs), or magnetic nanoparticles are broadly used in the life sciences as reporters and carrier beads. Many of these applications require a profound knowledge of the chemical nature and total number of their surface functional groups (FGs), that control bead charge, colloidal stability, hydrophobicity, and the interaction with the environment and biological systems. For bioanalytical applications, also the number of groups accessible for the subsequent functionalization with, e.g., biomolecules or targeting ligands is relevant. In this study, we explore the influence of QD encoding on the amount of carboxylic acid (COOH) surface FGs of 2 μm polystyrene microparticles (PSMPs). This is done for frequently employed oleic acid and oleylamine stabilized, luminescent core/shell CdSe QDs and two commonly used encoding procedures. This included QD addition during bead formation by a thermally induced polymerization reaction and a post synthetic swelling procedure. The accessible number of COOH groups on the surface of QD-encoded and pristine beads was quantified by two colorimetric assays, utilizing differently sized reporters and electrostatic and covalent interactions. The results were compared to the total number of FGs obtained by a conductometric titration and Fourier transform infrared spectroscopy (FTIR). In addition, a comparison of the impact of QD and dye encoding on the bead surface chemistry was performed. Our results demonstrate the influence of QD encoding and the QD-encoding strategy on the number of surface FG that is ascribed to an interaction of the QDs with the carboxylic acid groups on the bead surface. These findings are of considerable relevance for applications of nanoparticle-encoded beads and safe-by-design concepts for nanomaterials. KW - Optical spectroscopy KW - Particle KW - Optical assay KW - IR spectroscopy KW - Fluorescence KW - Quantum yield KW - Quality assurance KW - Nano KW - Synthesis KW - Surface chemistry KW - Quantification KW - Method KW - Conductometry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581502 DO - https://doi.org/10.1038/s41598-023-38518-7 SN - 2045-2322 VL - 13 IS - 1 SP - 1 EP - 15 PB - Springer Nature CY - London AN - OPUS4-58150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholtz, Lena A1 - Eckert, J. G. A1 - Graf, Rebecca T. A1 - Kunst, A. A1 - Wegner, Karl David A1 - Bigall, N. C. A1 - Resch-Genger, Ute T1 - Correlating semiconductor nanoparticle architecture and applicability for the controlled encoding of luminescent polymer microparticles N2 - Luminophore stained micro- and nanobeads made from organic polymers like polystyrene (PS) are broadly used in the life and material sciences as luminescent reporters, for bead-based assays, sensor arrays, printable barcodes, security inks, and the calibration of fluorescence microscopes and flow cytometers. Initially mostly prepared with organic dyes, meanwhile luminescent core/shell nanoparticles (NPs) like spherical semiconductor quantum dots (QDs) are increasingly employed for bead encoding. This is related to their narrower emission spectra, tuneability of emission color, broad wavelength excitability, and better photostability. However, correlations between particle architecture, morphology, and photoluminescence (PL) of the luminescent nanocrystals used for encoding and the optical properties of the NP-stained beads have been rarely explored. This encouraged us to perform a screening study on the incorporation of different types of luminescent core/shell semiconductor nanocrystals into polymer microparticles (PMPs) by a radical-induced polymerization reaction. Nanocrystals explored include CdSe/CdS QDs of varying CdS shell thickness, a CdSe/ZnS core/shell QD, CdSe/CdS quantum rods (QRs), and CdSe/CdS nanoplatelets (NPLs). Thereby, we focused on the applicability of these NPs for the polymerization synthesis approach used and quantified the preservation of the initial NP luminescence. The spectroscopic characterization of the resulting PMPs revealed the successful staining of the PMPs with luminescent CdSe/CdS QDs and CdSe/CdS NPLs. In contrast, usage of CdSe/CdS QRs and CdSe QDs with a ZnS shell did not yield luminescent PMPs. The results of this study provide new insights into structure–property relationships between NP stained PMPs and the initial luminescent NPs applied for staining and underline the importance of such studies for the performance optimization of NP-stained beads. KW - Quantitative spectroscopy KW - Energy transfer KW - Synthesis KW - Surface chemistry KW - Semiconductor quantum dot KW - Luminescence KW - Nano KW - Particle KW - Quantum yield KW - Lifetime KW - Quality assurance KW - Polymer particle KW - Quantum rod KW - Nanoplatelet PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602206 DO - https://doi.org/10.1038/s41598-024-62591-1 SN - 2045-2322 VL - 14 SP - 1 EP - 16 AN - OPUS4-60220 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reiber, T. A1 - Hübner, Oskar A1 - Dose, C. A1 - Yushchenko, D. A. A1 - Resch-Genger, Ute T1 - Fluorophore multimerization on a PEG backbone as a concept for signal amplification and lifetime modulation N2 - Fluorescent labels have strongly contributed to many advancements in bioanalysis, molecular biology, molecular imaging, and medical diagnostics. Despite a large toolbox of molecular and nanoscale fluorophores to choose from, there is still a need for brighter labels, e.g., for flow cytometry and fluorescence microscopy, that are preferably of molecular nature. This requires versatile concepts for fluorophore multimerization, which involves the shielding of dyes from other chromophores and possible quenchers in their neighborhood. In addition, to increase the number of readout parameters for fluorescence microscopy and eventually also flow cytometry, control and tuning of the labels’ fluorescence lifetimes is desired. Searching for bright multi-chromophoric or multimeric labels, we developed PEGylated dyes bearing functional groups for their bioconjugation and explored their spectroscopic properties and photostability in comparison to those of the respective monomeric dyes for two exemplarily chosen fluorophores excitable at 488 nm. Subsequently, these dyes were conjugated with anti-CD4 and anti-CD8 immunoglobulins to obtain fluorescent conjugates suitable for the labeling of cells and beads. Finally, the suitability of these novel labels for fluorescence lifetime imaging and target discrimination based upon lifetime measurements was assessed. Based upon the results of our spectroscopic studies including measurements of fluorescence quantum yields (QY) and fluorescence decay kinetics we could demonstrate the absence of significant dye-dye interactions and self-quenching in these multimeric labels. Moreover, in a first fluorescence lifetime imaging (FLIM) study, we could show the future potential of this multimerization concept for lifetime discrimination and multiplexing. KW - Imaging KW - Quantum yield KW - Quality assurance KW - Antibody KW - Conjugate KW - Cell KW - FLIM KW - PEG KW - Flow cytometry KW - Lifetime KW - Energy transfer KW - Quantitative spectroscopy KW - Nano KW - Particle KW - Fluorescence KW - Dye KW - Amplification KW - Microscopy PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-602197 DO - https://doi.org/10.1038/s41598-024-62548-4 SN - 2045-2322 VL - 14 IS - 1 SP - 1 EP - 11 AN - OPUS4-60219 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geißler, Daniel A1 - Wegner, Karl David A1 - Fischer, C. A1 - Resch-Genger, Ute T1 - Exploring Simple Particle-Based Signal Amplification Strategies in a Heterogeneous Sandwich Immunoassay with Optical Detection N2 - Heterogeneous sandwich immunoassays are widely used for biomarker detection in bioanalysis and medical diagnostics. The high analyte sensitivity of the current “gold standard” enzyme-linked immunosorbent assay (ELISA) originates from the signal-generating enzymatic amplification step, yielding a high number of optically detectable reporter molecules. For future point-of-care testing (POCT) and point-of-need applications, there is an increasing interest in more simple detection strategies that circumvent time-consuming and temperature-dependent enzymatic reactions. A common concept to aim for detection limits comparable to those of enzymatic amplification reactions is the usage of polymer nanoparticles (NP) stained with a large number of chromophores. We explored different simple NP-based signal amplification strategies for heterogeneous sandwich immunoassays that rely on an extraction-triggered release step of different types of optically detectable reporters. Therefore, streptavidinfunctionalized polystyrene particles (PSP) are utilized as carriers for (i) the fluorescent dye coumarin 153 (C153) and (ii) hemin (hem) molecules catalyzing the luminol reaction enabling chemiluminescence (CL) detection. Additionally, (iii) NP labeling with hemin-based microperoxidase MP11 was assessed. For each amplification approach, the PSP was first systematically optimized regarding size, loading concentration, and surface chemistry. Then, for an immunoassay for the inflammation marker C- eactive protein (CRP), the analyte sensitivity achievable with optimized PSP ystems was compared with the established ELISA concept for photometric and CL detection. Careful optimization led to a limit of detection (LOD) of 0.1 ng/mL for MP11-labeled PSP and CL detection, performing similarly well to a photometric ELISA (0.13 ng/mL), which demonstrates the huge potential of our novel assay concept. KW - Nanoparticle KW - Fluorescence KW - Immunoassay KW - Quality assurance KW - Antibody KW - Polymer KW - Dye KW - Signal enhancement KW - CRP KW - Biosensing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597853 DO - https://doi.org/10.1021/acs.analchem.3c03691 SN - 1520-6882 VL - 96 IS - 13 SP - 5078 EP - 5085 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-59785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fiedler, Saskia A1 - Frenzel, Florian A1 - Würth, Christian A1 - Tavernaro, Isabella A1 - Grüne, M. A1 - Schweizer, S. A1 - Engel, A. A1 - Resch-Genger, Ute T1 - Interlaboratory Comparison on Absolute Photoluminescence Quantum Yield Measurements of Solid Light Converting Phosphors with Three Commercial Integrating Sphere Setups N2 - Scattering luminescent materials dispersed in liquid and solid matrices and luminescent powders are increasingly relevant for fundamental research and industry. Examples are luminescent nano- and microparticles and phosphors of different compositions in various matrices or incorporated into ceramics with applications in energy conversion, solid-state lighting, medical diagnostics, and security barcoding. The key parameter to characterize the performance of these materials is the photoluminescence/fluorescence quantum yield (Φf), i.e., the number of emitted photons per number of absorbed photons. To identify and quantify the sources of uncertainty of absolute measurements of Φf of scattering samples, the first interlaboratory comparison (ILC) of three laboratories from academia and industry was performed by following identical measurement protocols. Thereby, two types ofcommercial stand-alone integrating sphere setups with different illumination and detection geometries were utilized for measuring the Φf of transparent and scattering dye solutions and solid phosphors, namely, YAG:Ce optoceramics of varying surface roughness, used as converter materials for blue light emitting diodes. Special emphasis was dedicated to the influence of the measurement geometry, the optical properties of the blank utilized to determine the number of photons of the incident excitation light absorbed by the sample, and the sample-specific surface roughness. While the Φf values of the liquid samples matched between instruments, Φf measurements of the optoceramics with different blanks revealed substantial differences. The ILC results underline the importance of the measurement geometry, sample position, and blank for reliable Φf data of scattering the YAG:Ce optoceramics, with the blank’s optical properties accounting for uncertainties exceeding 20%. KW - Nano KW - Fluorescence KW - Reference material KW - Luminescence KW - Quantitative spectroscopy KW - Particle KW - Quantum yield KW - Quality assurance KW - Phosphor KW - Converter material KW - Lifetime KW - Interlaboratory comparison KW - Method KW - Uncertainty PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600945 DO - https://doi.org/10.1021/acs.analchem.4c00372 SN - 0003-2700 SP - 6730 EP - 6737 PB - ACS Publications AN - OPUS4-60094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - López-Iglesias, C. A1 - Markovina, A. A1 - Nirmalananthan-Budau, N. A1 - Resch-Genger, Ute A1 - Klinger, D. T1 - Optically monitoring the microenvironment of a hydrophobic cargo in amphiphilic nanogels: influence of network composition on loading and release N2 - Amphiphilic nanogels (ANGs) are promising carriers for hydrophobic cargos such as drugs, dyes, and catalysts. Loading content and release kinetics of these compounds are controlled by type and number of hydrophobic groups in the amphiphilic copolymer network. Thus, understanding the interactions between cargo and colloidal carrier is mandatory for a tailor-made and cargo-specific ANG design. To systematically explore the influence of the network composition on these interactions, we prepared a set of ANGs of different amphiphilicity and loaded these ANGs with varying concentrations of the solvatochromic dye Nile Red (NR). Here, NR acts as a hydrophobic model cargo to optically probe the polarity of its microenvironment. Analysis of the NR emission spectra as well as measurements of the fluorescence quantum yields and decay kinetics revealed a decrease in the polarity of the NR microenvironment with increasing hydrophobicity of the hydrophobic groups in the ANG network and dye–dye interactions at higher loading concentrations. At low NR concentrations, the hydrophobic cargo NR is encapsulated in the hydrophobic domains. Increasing NR concentrations resulted in probe molecules located in a more hydrophilic environment, i.e., at the nanodomain border, and favored dye–dye interactions and NR aggregation. These results correlate well with release experiments, indicating first NR release from more hydrophilic network locations. Overall, our findings demonstrate the importance to understand carrier–drug interactions for efficient loading and controlled release profiles in amphiphilic nanogels. KW - Particle KW - Energy transfer KW - Limit of detection KW - Polymer KW - Luminescence KW - Quantitative spectroscopy KW - Nano KW - Quantum yield KW - Lifetime KW - Quality assurance KW - Dye KW - Probe KW - Sensor KW - Nile Red PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601603 DO - https://doi.org/10.1039/d4nr00051j SN - 2040-3364 IS - 16 SP - 9525 EP - 9535 PB - The Royal Society of Chemistry AN - OPUS4-60160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Photoluminescence at BAM – Photoluminescence at BAM – Photophysical Studies, Quantum Yield Measurements, Multiplexing Strategies, and Standards N2 - Photoluminescence applications in the life and material sciences require bright molecular and nanocrystalline emitters, stimuli-responsive optical probes, signal enhancement, multiplexing, and barcoding strategies and traceable methods to quantify the signal-relevant optical properties of luminescent materials at the ensemble and single molecule/particle level. In this context, current research at Division Biophotonics of BAM is presented ranging from dye and nanocrystal photophysics, absolute measurements of photoluminescence quantum yields in the UV/vis/NIR/SWIR, lifetime multiplexing, and the development of different types of fluorescence standards for validating optical-spectroscopic measurements. T2 - Institutskolloquium IPHT CY - Jena, Germany DA - 22.10.2019 KW - Surface group analysis KW - NIR KW - SWIR KW - Quantum dot KW - Lanthanide KW - Cleavable probe KW - Lifetime KW - Multiplexing KW - Sensor KW - Assay PY - 2019 AN - OPUS4-49360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Maack, Stefan T1 - Low-frequency ultrasound data (pulse-echo technique) with shear horizontal and longitudinal waves on a reference polyamide specimen “BAM-Pk218” N2 - This dataset contains raw data observed with ultrasound measurements on a polyamide reference specimen at Bundesanstalt für Materialforschung und -prüfung (BAM), Berlin. The internal specimen identifier is „Pk218“. The measurements were conducted using the pulse-echo method. KW - Nondestructive testing KW - Ultrasound KW - Pulse-echo technique KW - Validation KW - Reference material KW - Reconstruction algorithm PY - 2022 DO - https://doi.org/10.7910/DVN/KVN7CY PB - Harvard College CY - Cambridge, MA, USA AN - OPUS4-54959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Algernon, D. A1 - Arndt, R.W. A1 - Denzel, W. A1 - Ebsen, B. A1 - Feistkorn, S. A1 - Friese, M. A1 - Große, C.U. A1 - Kathage, S. A1 - Keßler, S. A1 - Köpp, Christian A1 - Küttenbaum, Stefan A1 - Lohse, C. A1 - Maack, Stefan A1 - Niederleithinger, Ernst A1 - Schickert, M. A1 - Schröder, G. A1 - Taffe, A. A1 - Timofeev, Juri A1 - Walther, A. A1 - Wilcke, M. A1 - Wolf, J. A1 - Wöstmann, Jens T1 - Test specimen concepts in regard to quality assurance and validation of nondestructive testing in civil engineering N2 - The process of ensuring reliability of NDT applications contains various aspects, such as determining the performance and probability of success, the uncertainty in measurement, the provision of clear and functional procedures and ensuring the correct application accordingly. Test specimens have become powerful elements in supporting many of these aspects. Within the committee for NDT in Civil Engineering (NDT-CE) of the German Society for Nondestructive Testing (DGZfP), the subcommittee on Quality Assurance (UA-QS) therefore addresses the design and the integration of test specimens in the quality assurance process. Depending on the specific purpose, the requirements on test specimens can vary significantly based on the defined simulated scenario. The most prominent purposes of test specimens might be seen in providing references for inspection systems in regard to function control, calibration and validation. Further aspects can be parametric studies, basic investigation of physical principles related to NDT or a simplified and therefore comprehensive demonstration of inspection concepts (e.g. for teaching purposes). The specific purpose of a test specimen dictates the requirements regarding its conception, including the exact design, the material or the fabrication accuracy and the conditioning. In the development of a general guideline by the UA-QS for application-specific procedures and their validation, the use of test specimens is addressed and specific concepts for the design of test specimens are made. This includes the analysis of the measurement process regarding any given application, deriving an adequate calibration approach for it and designing test specimens (calibration specimens) accordingly. Furthermore, it includes the validation of the procedure taking into account all conditions related to the specific application in the field. The validation requires a statistically sufficient number of trials. Thorough evaluation of each trial can only be established if the ground-truth is known. Therefore, test specimens providing a realistic but controlled simulation of the inspection problem are valuable and indispensable elements in the validation process. The requirement of being fully realistic will often not be possible to fulfill due to practical restrictions. Any aspect that cannot be included in the simulation realistically needs to be simulated conservatively. This again, requires a sufficient understanding of the inspection principle and technique to ensure conservativeness. Among other quality-assurance-related aspects, the UA-QS establishes concepts and guidelines regarding sound and efficient approaches for the specific purposes of test specimens. This subcommittee brings together representatives of different Groups along the entire value chain of NDT-CE, including researchers, practitioners, manufacturers and clients. They all work together in establishing a common understanding and level of quality assurance in the industry. T2 - SMT and NDT-CE 2018 CY - New Brunswick, NJ, USA DA - 27.08.2018 KW - Quality assurance KW - Procedure KW - Reliability KW - Validation KW - Reference specimen PY - 2019 UR - https://asnt.org/smt18papers SN - 978-1-57117-456-7 VL - 11/19 SP - 39 EP - 48 PB - The American Society for Nondestructive Testing, Inc. CY - Columbus, OH, USA AN - OPUS4-47240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ahiboz, D. A1 - Andresen, Elina A1 - Manley, P. A1 - Resch-Genger, Ute A1 - Würth, Christian A1 - Becker, C. T1 - Metasurface-Enhanced Photon Upconversion upon 1550 nm Excitation N2 - Photon upconversion upon 1550 nm excitation is of high relevance for applications in the third biological excitation window, for photovoltaics beyond current limitations, and enables appealing options in the field of glass Fiber telecommunications. Trivalent doped erbium ions (Er3+) are the material of choice for 1550 nm excited upconversion, however, they suffer from a low absorption cross-section and a low brightness. Therefore, the ability of Silicon metasurfaces to provide greatly enhanced electrical near-fields is employed to enable efficient photon upconversion even at low external Illumination conditions. Hexagonally shaped β-NaYF4:Er3+ nanoparticles are placed on large-area silicon metasurfaces designed to convert near-infrared (1550 nm) to visible light. More than 2400-fold enhanced photon upconversion luminescence is achieved by using this metasurface instead of a planar substrate. With the aid of optical simulations based on the finite-element method, this result is attributed to the coupling of the excitation source with metasurface resonances at appropriate incident angles. Analysis of the excitation power density dependence of upconversion luminescence and red-to-green-emission ratios enables the estimation of nanoscale near-field enhancement on the metasurface. The findings permit the significant reduction of required external excitation intensities for photon upconversion of 1550 nm light, opening perspectives in biophotonics, telecommunication, and photovoltaics. KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - Excitation power density KW - Single particle KW - Brightness KW - NIR KW - Mechanism KW - Single enhancement KW - SWIR KW - Method PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-537193 DO - https://doi.org/10.1002/adom.202101285. SN - 2195-1071 VL - 9 IS - 24 SP - 2101285 PB - Wiley-VCH-GmbH AN - OPUS4-53719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Große, Christian A1 - Arndt, Ralf A1 - Mähner, Dietmar A1 - Niederleithinger, Ernst A1 - Taffe, Alexander T1 - Zerstörungsfreie Prüfung im Bauwesen: Memorandum zur Lehre an deutschsprachigen Hochschulen N2 - Dieses erste Memorandum zur Lehre und Forschung an deutschsprachigen Hochschulen auf dem Gebiet der zerstörungsfreien Prüfung im Bauwesen gibt einen Überblick hinsichtlich der akademischen Ausbildung und zeigt mögliche Schwerpunkte vor allem in der Lehre auf. Diese Schwerpunkte berücksichtigen auch aktuelle Entwicklungen und Themen auf dem Gebiet der Forschung. Es werden Anregungen zur Entwicklung bzw. Weiterentwicklung der Lehr-Curricula im Hinblick auf eine umfassende und solide fachliche Ausbildung der Studierenden des Bauwesens und angrenzender Fachrichtungen gegeben. Inhaltlich und formal lehnt sich der Beitrag an dem Memorandum der Hochschullehrer im Fachgebiet „Werkstoffe im Bauwesen“ (Breit et al., 2012) an und beruht auf einer Initiative des Unterausschusses Ausbildung – Arbeitsgruppe Ausbildung in der Hochschule – des Fachausschusses ZfP im Bauwesen der Deutschen Gesellschaft für zerstörungsfreie Prüfung (DGZfP). Die Hauptredaktion wurde übernommen von Prof. Christian U. Grosse (TU München) und Prof. Ralf W. Arndt (FH Erfurt). KW - Zerstörungsfreie Prüfung KW - Lehrplan KW - Bauwesen PY - 2019 UR - https://onlinelibrary.wiley.com/doi/epdf/10.1002/bate.201900008 DO - https://doi.org/10.1002/bate.201900008 SN - 1437-0999 SN - 0932-8351 VL - 96 IS - 4 SP - 360 EP - 368 PB - Ernst & Sohn CY - Berlin AN - OPUS4-47606 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stroyuk, O. A1 - Raievska, O. A1 - Barabash, A. A1 - Batentschuk, M. A1 - Osvet, A. A1 - Fiedler, Saskia A1 - Resch-Genger, Ute A1 - Hauch, J. A1 - Brabec, C. J. T1 - "Green" synthesis of highly luminescent lead-free Cs2AgxNa1-xBiyIn1-yCl6 perovskites N2 - A new “green” and mild synthesis of highly stable microcrystalline Cs2AgxNa1-xBiyIn1-yCl6 (CANBIC) perovskites under ambient conditions was developed that is scalable to the multi-gram production. Under UV illumination, the CANBIC perovskites emit intense broadband photoluminescence (PL) with a quantum yield (QY) of 92% observed for x = 0.35 and y = 0.01-0.02. The combination of strong UV absorbance and broadband visible emission, high PL QY, and long PL lifetimes of up to 1.4 μs, along with an outstanding stability makes these CANBICs a promising material class for many optical applications. KW - Fluorescence KW - Perovskites KW - Solar cell KW - Automated synthesis KW - Green synthesis KW - Quantum yield KW - Integrating sphere spectroscopy KW - Absolute fluorescence KW - Quality assurance KW - Nano KW - Particle KW - Application KW - Semiconductor KW - Quantum dot KW - Renewable energy PY - 2022 DO - https://doi.org/10.1039/d2tc02055f SN - 2050-7526 VL - 10 IS - 27 SP - 9938 EP - 9944 PB - Royal Society of Chemistry AN - OPUS4-55453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Auxillos, J. A1 - Crouigneau, R. A1 - Li, Y.-F. A1 - Dai, Y. A1 - Stigliani, A. A1 - Tavernaro, Isabella A1 - Resch-Genger, Ute A1 - Sandelin, A. A1 - Marie, R. A1 - Pedersen, S. F. T1 - Spatially resolved analysis of microenvironmental gradient impact on cancer cell phenotypes N2 - Despite the physiological and pathophysiological significance of microenvironmental gradients, e.g., for diseases such as cancer, tools for generating such gradients and analyzing their impact are lacking. Here, we present an integrated microfluidic-based workflow that mimics extracellular pH gradients characteristic of solid tumors while enabling high-resolution live imaging of, e.g., cell motility and chemotaxis, and preserving the capacity to capture the spatial transcriptome. Our microfluidic device generates a pH gradient that can be rapidly controlled to mimic spatiotemporal microenvironmental changes over cancer cells embedded in a 3D matrix. The device can be reopened allowing immunofluorescence analysis of selected phenotypes, as well as the transfer of cells and matrix to a Visium slide for spatially resolved analysis of transcriptional changes across the pH gradient. This workflow is easily adaptable to other gradients and multiple cell types and can therefore prove invaluable for integrated analysis of roles of microenvironmental gradients in biology. KW - Bioimaging KW - Fluorescence KW - Cell KW - Cancer KW - Method KW - Microfluids KW - Model KW - Calibration KW - Sensor KW - Ph KW - Probe KW - Workflow PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-604631 DO - https://doi.org/10.1126/sciadv.adn3448 VL - 19 IS - 18 SP - 1 EP - 17 AN - OPUS4-60463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Amouroux, B. A1 - Eftekhari, A. A1 - Roux, C. A1 - Micheau, J. A1 - Roblin, P. A1 - Pasturel, M. A1 - Gauffre, F. A1 - Würth, Christian A1 - Resch-Genger, Ute A1 - Sliwa, M. A1 - Bouchet, A. A1 - Coudret, C. T1 - Synthesis and Emission Dynamics of Sub-3 nm Upconversion Nanoparticles N2 - Reducing the size of upconversion nanoparticles (UCNPs) down to a few nm yields luminescent materials containing a very small number of emitters. Considering the bottom limit of one activator per particle ultrasmall UCNPs offer an unprecedented platform to study the contributions of the energy transfers at play in upconversion luminescence. Maintaining detectable emission despite the limited number of emitting ions and the high surface-to-volume ratio requires suitable particle architectures. Na(Gd-Yb)F4:Tm3+ emissive sub-3 nm diameter 𝜷-phase UCNPs are prepared using a gadolinium-rich composition in situ mixing of the precursors and a microwave high-temperature cycling sequence allowing precise control of the particle size and dispersity. These cores are coated with a NaGdF4 inert shell to minimize the deleterious influence of surface quenching (SQ). Time-resolved luminescence measurements combining standard NIR excitation of the Yb3+ sensitizer and direct UV excitation of the Tm3+ activator are performed to quantify cross relaxation and surface quenching processes. The fine tuning of the number of activators per particle via an optimized synthesis pathway along with the use of an appropriate excitation scheme enabled to provide an accurate analysis of the different mechanisms at play in these model nanoparticles and to characterize the structure of the core-shell architecture. KW - Lanthanide KW - Nanoparticle KW - Luminescence KW - Quantitative spectroscopy KW - Quantum yield KW - Energy transfer KW - Quality assurance KW - Synthesis KW - Surface modification KW - Photophysics PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-606877 DO - https://doi.org/10.1002/adom.202303283 SN - 2195-1071 SP - 1 EP - 13 AN - OPUS4-60687 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zheng, H. A1 - Ertel, Jens-Peter A1 - Kourmpetis, M. A1 - Kanfoud, J. A1 - Niederleithinger, Ernst A1 - Gan, T.-H. T1 - Integrity testing of cast in situ concrete piles based on an impulse response function method using sine‑sweep excitation by a shaker N2 - In this study, an Impulse Response Function analysis of pile response to sine-sweep excitation by a low cost, portable Shaker was used to identify defects in piles. In straightforward impact-echo methods, echoes from the pile toe and defects are visible in the time domain measurements. However, these echoes are not present in the time domain records of piles subjected to sine-sweep excitations, due to interactions between the input and output signals. For this reason, the impulse response function in the time domain has been calculated and is able to identify the echoes from pile impedance changes. The proposed methodology has been evaluated both numerically and experimentally. A one-dimensional pile-soil interaction system was developed, and a finite difference method used to calculate the pile response to sine-sweep excitation. The numerical simulations indicate that impulse response measurements with a synthesized logarithmic, sine-sweep excitation could be an effective tool for detecting defects in piles. The methodology was further tested with field trials on 6 cast in situ concrete test piles including 1 intact pile and 5 defective piles subjected to sine-sweep excitations by a shaker. In 5 of the 6 cases the echoes from the pile toe could be identified in the deconvoluted waveforms—the impulse Response functions. Damage detection is more difficult and dependent on the selection of the optimal regularization parameter. Further research and optimization of the deconvolution process is needed to evaluate the effectiveness compared to standard pile integrity testing methods. KW - Pile testing KW - Shaker KW - Deconvolution PY - 2019 DO - https://doi.org/10.1007/s10921-019-0595-4 SN - 0195-9298 SN - 1573-4862 VL - 38 IS - 2 SP - 55, 1 EP - 18 PB - Springer CY - Cham, Switzerland AN - OPUS4-48185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wasternack, J. A1 - Schröder, H. V. A1 - Witte, J. F. A1 - Ilisson, M. A1 - Hupatz, H. A1 - Hille, J. F. A1 - Gaedke, M. A1 - Valkonen, A. M. A1 - Sobottka, S. A1 - Krappe, A. A1 - Schubert, M. A1 - Paulus, B. A1 - Rissanen, K. A1 - Sarkar, B. A1 - Eigler, S. A1 - Resch-Genger, Ute A1 - Schalley, C. A. T1 - Switchable protection and exposure of a sensitive squaraine dye within a redox active rotaxane N2 - In nature,molecular environments in proteins can sterically protect and stabilize reactive species such as organic radicals through non-covalent interactions.Here, wereport a near-infrared fluorescent rotaxane in which the stabilization of a chemically labile squaraine fluorophore by the coordination of a tetralactam macrocycle can be controlled chemically and electrochemically. The rotaxane can be switched between two co-conformations inwhich thewheel either stabilizes or exposes the fluorophore. Coordination by the wheel affects the squaraine’s stability across four redox states and renders the radical anion significantly more stable—by a factor of 6.7—than without protection by a mechanically bonded wheel. Furthermore, the fluorescence properties can be tuned by the redox reactions in a stepwise manner. Mechanically interlockedmolecules provide an excellent scaffold to stabilize and selectively expose reactive species in a co-conformational switching process controlled by external stimuli. KW - Fluorescence KW - Dye KW - Sensor KW - Quantum yield KW - Spectroscopy KW - Photophysics KW - Synthesis KW - Squaraine KW - Switch KW - Redox-active KW - Rotaxane PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-614959 DO - https://doi.org/10.1038/s42004-024-01312-1 VL - 7 SP - 1 EP - 11 AN - OPUS4-61495 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, P. A1 - Morales-Marquez, R. A1 - Cervas, G. A1 - Hernandez Medel, A. A1 - Ogayar, M. P. A1 - Jimenez de Aberasturi, D. A1 - de Isidro-Gomez, A. I. A1 - Torres-Padro, A. A1 - Palomares, F. J. A1 - Garcia-Orrit, S. A1 - Sousa, C. T. A1 - Espinosa, A. A1 - Telle, H. H. A1 - Ortgies, D. H. A1 - Vega-Mayoral, V. A1 - Cabanillas-Gonzalez, J. A1 - Rodriguez, E. M. A1 - Resch-Genger, Ute A1 - Wegner, Karl David A1 - Juarez, B. H. T1 - The role of temperature in the photoluminescence quantum yield (PLQY) of Ag2S-based nanocrystals N2 - Highly emissive Ag2S nanocrystals (NCs) passivated with a gradated shell incorporating Se and Zn were synthesized in air, and the temperature dependence of their photoluminescence quantum yield (PLQY) was quantified in both organic and aqueous media at B1200 nm. The relevance of this parameter, measured at physiological temperatures, is highlighted for applications that rely on the near infrared (NIR) photoluminescence of NCs, such as deep NIR imaging or luminescence nanothermometry. Hyperspectral NIR imaging shows that Ag2S-based NCs with a PLQY in organic media of about 10% are inefficient for imaging at 40 8C through 20 mm thick tissue with low laser irradiation power densities. In contrast, water-transferred Ag2S-based NCs with an initial PLQY of 2% in water exhibit improved robustness against temperature changes, enabling improved imaging performance. KW - Quantum dots KW - Ag2S KW - Fluorescence KW - Nanomaterial design KW - Advanced nanomaterials KW - Shortwave infrared (SWIR) KW - Temperature sensing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613877 DO - https://doi.org/10.1039/D4MH01016G SP - 1 EP - 11 PB - Royal Society of Chemistry (RSC) AN - OPUS4-61387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deumer, J. A1 - Andresen, Elina A1 - Gollwitzer, C. A1 - Schürmann, R. A1 - Resch-Genger, Ute T1 - Adding More Shape to Nanoscale Reference Materials-LiYF4:Yb,Tm Bipyramids as Standards for Sizing Methods and Particle Number Concentration N2 - The increasing industrial use of nanomaterials calls for the reliable characterization of their physicochemical key properties like size, size distribution, shape, and surface chemistry, and test and reference materials (RMs) with sizes and shapes, closely matching real-world nonspheric nano-objects. An efficient strategy to minimize efforts in producing nanoscale RMs (nanoRMs) for establishing, validating, and standardizing methods for characterizing nanomaterials are multimethod nanoRMs. Ideal candidates are lanthanide-based, multicolor luminescent, and chemically inert nanoparticles (NPs) like upconversion nanoparticles (UCNPs), which can be prepared in different sizes, shapes, and chemical composition with various surface coatings. This makes UCNPs interesting candidates as standards not only for sizing methods, but also for element-analytical methods like laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS), quantitative bioimaging methods like X-ray fluorescence computed tomography (XFCT), and luminescence methods and correlative measurements. Here, we explore the potential of two monodisperse LiYF4:Yb,Tm bipyramids with peak-to-peak distances of (43 ± 2) nm and (29 ± 2) nm as size standards for small-angle X-ray scattering (SAXS) and tools for establishing and validating the sophisticated simulations required for the analysis of SAXS data derived from dispersions of nonspheric nano-objects. These SAXS studies are supplemented by two-dimensional (2D)-transmission electron microscopy measurements of the UCNP bipyramids. Additionally, the particle number concentration of cyclohexane dispersions of these UCNP bipyramids is determined by absolute SAXS measurements, complemented by gravimetry, thermogravimetric analysis (TGA), and inductively coupled plasma optical emission spectrometry (ICP-OES). This approach enables traceable particle number concentration measurements of ligand-capped nonspheric particles with unknown chemical composition. KW - Fluorescence KW - Upconversion nanoparticles KW - SAXS KW - Particle number concentration KW - Reference material KW - Traceability KW - Quality assurance KW - Quantum yield KW - Spectroscopy KW - Synthesis KW - Quantification KW - NanoRM KW - Nano KW - Particle KW - Bipyramid KW - Reference data KW - Simulation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-617940 DO - https://doi.org/10.1021/acs.analchem.4c03641 SP - 1 EP - 8 PB - ACS Publications AN - OPUS4-61794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stiegler, L. M. S. A1 - Wegner, Karl David A1 - Weigert, Florian A1 - Peukert, W. A1 - Resch-Genger, Ute A1 - Walter, J. T1 - Analysis of Giant-Shell CdSe/CdS Quantum Dots via Analytical Ultracentrifugation Combined with Spectrally Resolved Photoluminescence N2 - Knowledge of the structure–property relationships of functional nanomaterials, including, for example, their size- and composition-dependent photoluminescence (PL) and particle-to-particle variations, is crucial for their design and reproducibility. Herein, the Angstrom-resolution capability of an analytical ultracentrifuge combined with an in-line multiwavelength emission detection system (MWE-AUC) for measuring the sedimentation coefficient-resolved spectrally corrected PL spectra of dispersed nanoparticles is demonstrated. The capabilities of this technique are shown for giant-shell CdSe/CdS quantum dots (g-QDs) with a PL quantum yield (PL QY) close to unity capped with oleic acid and oleylamine ligands. The MWE-AUC PL measurements are calibrated and validated with certified fluorescence standards. The spectrally corrected and size-dependent PL spectra of the g-QDs derived from a single MWE-AUC experiment are then analyzed and compared with the results of single-particle spectroscopic studies, yielding the PL spectra, decay kinetics, and blinking behavior of individual g-QDs. This study underlines the vast potential of MWE-AUC with in-line optical detection for the characterization of advanced nanomaterials with a complex structure. KW - Quantum dots KW - Analytical ultracentrifugation KW - Photoluminescence KW - Advanced nanomaterial characterization KW - Calibrated fluorescence measurements KW - Reference materials PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624357 DO - https://doi.org/10.1002/smtd.202401700 SN - 2366-9608 SP - 1 EP - 7 PB - Wiley VHC-Verlag AN - OPUS4-62435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Habib, Abdel Karim A1 - Kluge, Martin A1 - van Wingerden, Kees T1 - Untersuchung der Freisetzung von Flüssigwasserstoff auf und unter Wasser N2 - In einer Reihe von Experimenten wurden die möglichen Folgen der Freisetzung von verflüssigtem Wasserstoff (LH2) auf, bzw. unter Wasser untersucht. Die Experimente zielten darauf ab, eine unbeabsichtigte Freisetzung von LH2 (z.B. durch Schlauchabriss) insbesondere bei der Betankung eines Schiffes zu simulieren. Für verflüssigtes Erdgas (LNG) wurden dabei sog. RPT’s (rapid phase transition) nachgewiesen, bei denen die spontane Verdampfung relevante Druckwellen erzeugt. Es kann nicht ausgeschlossen werden, dass RPTs auch im Falle von LH2 möglich sind. Die Versuche wurden auf dem Testareal Wasserstoffsicherheit auf dem Testgelände Technische Sicherheit der Bundesanstalt für Materialforschung und -prüfung (BAM-TTS) in Horstwalde, im Rahmen einer Forschungskooperation zwischen der BAM und Gexcon im Rahmen des SH2IFT-Programms durchgeführt. Die LH2-Freisetzungen erfolgten direkt aus einem LH2-Tanklastwagen über eine lange, flexible, vakuumisolierte Transferleitung. Während die Freisetzung oberhalb und unterhalb der Wasseroberfläche jeweils vertikal orientiert war, wurde bei der Unterwasserfreisetzung zusätzlich eine horizontale Ausströmung, parallel zur Wasseroberfläche realisiert. Zur Bestimmung des Massenstromes, wurde ein Wägesystem unter dem Tankwagen eingesetzt. Spezielle Drucksensoren wurden verwendet, um die durch die Freisetzungsvorgänge erzeugten Stoßwellen sowohl im Wasser als auch in der Luft zu messen. Die Gaskonzentrationen über dem Wasserbecken wurden an verschiedenen Positionen gemessen. Hochgeschwindigkeits-, Infrarot- (IR) und normale Kameras wurden eingesetzt, um die Phänomenologie der Freisetzung aufzuzeichnen und das Verhalten der Gaswolke im Zeitverlauf zu verfolgen. Neben den fest installierten Systemen an Land, kamen auch Unterwasserkameras sowie eine Drohne mit Normal- und IR-Kameras zum Einsatz. Zwei Wetterstationen wurden zur Messung von Windgeschwindigkeit, Windrichtung, Temperatur und Luftfeuchtigkeit während aller durchgeführten Tests eingesetzt. Des Weiteren kamen Bolometer zur Wärmestrahlungsmessung zum Einsatz. Zwar führten die Freisetzung zu einer hochturbulenten LH2/Wasser Mischzone, jedoch zu keinen nennenswerten Überdrücken durch RPT. Im Gegensatz dazu wurde unerwartet, aber reproduzierbar, eine Zündung der Gaswolke in freier Luft in einiger Entfernung von den Instrumenten und dem Ort der Freisetzung beobachtet. Die daraus resultierenden Gaswolkenexplosionen führten zu relevanten Überdrücken und zur Wärmeabstrahlung in die Umgebung. T2 - Magdeburg-Köthener Brandschutz- und Sicherheitstagung 2024 CY - Magdeburg, Germany DA - 14.03.2024 KW - Flüssigwasserstoff KW - LH2 KW - Freisetzung KW - RPT KW - Gaswolkenexplosion PY - 2024 SN - 978-3-948749-42-2 SP - 127 EP - 136 CY - Magedburg AN - OPUS4-59709 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Chemometric tools for LIBS analysis N2 - LIBS matures to a quantitative method for elemental analysis rather than a qualitative diagnostic tool. Numerous real world applications for bulk and microanalysis profit from instrumental and methodical advances in the last decade. Today, recording of numerous spectra from samples can be done with low experimental efforts and low cost per spectrum. Not surprisingly, LIBS data, with a high spectral resolution and a broad spectral range, become “big data” and can be utilized in different ways beyond elemental analysis. But, what is the generic or best approach for quantitative LIBS analysis? What techniques can be employed to gain new insights into data? Emergent information can arise through data fusion of LIBS data with other data, i.e. orthogonal spectroscopic or other information related to the sample. But are fused data better than data from a single method? This talk will provide an in-depth overview what chemometric tools can do for LIBS. For quantitative analysis, pre-processing tools are essential to improve precision, accuracy, and reproducibility but at the same time their application to data is still based on phenomenological criteria. Multivariate analysis seems to dominate LIBS, but are there drawbacks on using all information from spectra. For different data sets from real applications, the use of multivariate calibration and (un)supervised pattern recognition will be discussed in comparison with reference analytical methods and possible improvements through plasma diagnostics and modelling. T2 - 9th International Confrence on Laser-Indusced Breakdown Spectroscopy (LIBS) CY - Charmonix-Mont-Blanc, France DA - 12.09.2016 KW - Chemometrics KW - Analytical method KW - LIBS PY - 2016 AN - OPUS4-37534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Sobol, Oded T1 - Hydrogen assisted cracking and transport studied by ToF-SIMS and data fusion with HR-SEM N2 - For almost 150 years it is known that hydrogen has a deleterious effect on the mechanical properties of metallic components. Nowadays, the problem of hydrogen assisted degradation is highly relevant in energy related fields due to the massive use of steel as a structural component in these applications and its sensitivity to hydrogen. Since the discovery of hydrogen assisted cracking (HAC), researchers studied intensively and suggested possible explanations and mechanisms in order to define how hydrogen is affecting the material. In general, it is considered that hydrogen changes the mechanical properties more in terms of ductility (deformation capacities) than in strength (load capacities). Hydrogen concentration is one of three crucial factors in the degradation process, together with the microstructure of the material and the internal/external mechanical load. The relatively high concentration of hydrogen resulting in this loss of ductility can originate during production or before service (e.g. welding processes) and during service (i.e. catholically protected systems to eliminate corrosion processes in sour environments). In parallel to the theoretical work, tremendous efforts were, and are still, invested in searching for a proper method to elucidate, map and quantify the hydrogen in the microstructure, which is the basis for this work. For steels, the focus is mainly on the observations of diffusion processes and the interaction of hydrogen with the microstructure in regions with high local stresses/strains (for example around evolving cracks). The challenge for reaching this goal arises from the fact that accurate indication of hydrogen by means of position, unlike heavier atoms, can be made only by mass spectrometry or by interaction with another element (e.g. silver decoration, special coating and resonant nuclear reaction by nitrogen). In addition to this, the difficulty recording the hydrogen behavior while it rapidly diffuses through the material, leaving only the unpredicted failure, should be taken into account. Although using powerful characterization methods, models and computational simulations, the key to defining the mechanisms behind HAC is still under debate and not fully understood. The relationship between material and hydrogen is determined by three factors, i.e., the material structure and microstructure – determining the physical properties, the mechanical load applied on the material and the hydrogen concentration. It is well known that in order to have a complete definition of HAC these three factors must be examined locally with the minimal scale and the maximal resolution reachable. The major gap is the lack in such a characterization method or a technique by which one has the ability to detect and observe the hydrogen in the metallic microstructure. The commonly used techniques nowadays are capable of characterization of the microstructure without the ability to observe the hydrogen distribution. Global hydrogen concentration and localized hydrogen observation are possible by some techniques which are incapable of indicating a change in the structure or microstructure therefore a comprehensive overview can be gained only by combining several methods. In the presented research, secondary ion mass spectrometry (SIMS) was adopted as the main tool to detect and locally map the hydrogen distribution in two types of duplex stainless steel grades: EN 1.4462 (standard 2205 duplex stainless steel) and EN 1.4162 (2101 lean duplex stainless steel). The term duplex stainless steel (DSS) refers to the austenitic-ferritic microstructure of the steel where the combination of physical and mechanical properties of the two phases is achieved. The DSS was selected as a case study for this work due to the wide use of this grade in many energy and the lack of knowledge on hydrogen behavior in two-phase containing microstructures. ToFSIMS was exploited in-situ and ex-situ in three experimental approaches during or following an electrochemical charging procedure. This type of hydrogen charging was selected as it simulated a procedure of cathodic protection of most sub-water oil and gas extraction and delivery systems. The experimental procedures were: 1. Ex-situ charging followed by ToF-SIMS imaging for basic understanding of hydrogen distribution. 2. Ex-situ charging followed by in-situ mechanical loading to obtain information on hydrogen behavior around a propagating crack. 3. In-situ permeation of hydrogen through a steel membrane inside the ToF-SIMS to obtain information on diffusion behavior of hydrogen in a two-phase microstructure. The comprehensive view of the effect of hydrogen on steel was gained by using supplementary methods, such as high resolution scanning electron microscopy (HR-SEM), focused ion beam (FIB) and electron back-scattered diffraction (EBSD). The state of the art in this work lies in applying both: in-situ experimental approaches and data treatment of the ToF-SIMS raw data. The data treatment includes the combination of data from several sources (data fusion). The results for the ex-situ charging followed by static sample imaging and data fusion showed that when the analyzed surface is directly exposed to the electrolyte the degradation is pronounced differently in the ferrite, austenite and interface. The degradation mechanisms in the ferrite and austenite were reflected by the formation of cracks on the surface of both, where a high concentration of hydrogen was obtained. This result supports the assumption that hydrogen is attracted to highly deformed regions. The advantage of using in-situ charging/permeation in comparison to ex-situ charging is that the effect of hydrogen on the ferrite and austenite phases when the hydrogen is evolving from within the microstructure is realized, in comparison to when the analyzed surface is initially exposed directly to the electrolyte. In both experiments the ferrite was observed as a fast diffusion path for the hydrogen. The faster diffusion of hydrogen through the ferrite is expected due to the higher diffusion coefficient, however, a direct proof for the diffusion sequence in this scale was never shown. Most significant results were achieved by the ‘core’ experiments of this research. These experiments included the design of a novel dynamic mechanical loading device to apply an external load during SIMS imaging of a hydrogen precharged-notched sample. For the first time it was shown that plastic deformation induced by applying a mechanical load is resulting in a redistribution of hydrogen locally around the notch. T3 - BAM Dissertationsreihe - 160 KW - Duplex stainless steels KW - Hydrogen assisted cracking KW - Time-of-Flight secondary ion mass spectrometry KW - Data fusion PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-447331 SN - 1613-4249 VL - 160 SP - I EP - 180 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-44733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Garcia-Fernandez, J. A1 - Turiel, D. A1 - Bettmer, J. A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Rivas Garcia, L. A1 - Llopis, J. A1 - Sanchez-Gonzalez, C. A1 - Montes-Bayon, M. T1 - In vitro and in situ experiments to evaluate the biodistribution and cellular toxicity of ultrasmall iron oxide nanoparticles potentially used as oral iron supplements N2 - Well-absorbed iron-based nanoparticulated materials are a promise for the oral management of iron deficient anemia. In this work, a battery of in vitro and in situ experiments are combined for the evaluation of the uptake, distribution and toxicity of new synthesized ultrasmall (4 nm core) Fe2O3 nanoparticles coated with tartaric/adipic acid with potential to be used as oral Fe supplements. First, the in vitro simulated gastric acid solubility studies by TEM and HPLC-ICP-MS reveal a partial reduction of the core size of about 40% after 90 min at pH3. Such scenario confirms the arrival of the nanoparticulate material in the small intestine. In the next step, the in vivo absorption through the small intestine by intestinal perfusion experiments is conducted using the sought nanoparticles in Wistar rats. The quantification of Fe in the NPs Suspension before and after perfusion shows Fe absorption levels above 79%, never reported for other Fe treatments. Such high absorption levels do not seem to compromise cell viability, evaluated in enterocytes-like models (Caco-2 and HT-29) using cytotoxicity, ROS production, genotoxicity and lipid peroxidation tests. Moreover, regional differences in terms of Fe concentration are obtained among different parts of the small intestine as duodenum>jejunum>ileum. Complementary transmission electron microscopy (TEM) images show the presence of the intact particles around the intestinal microvilli without significant tissue damage. These studies show the high potential of these NP preparations for their use as oral management of anemia. KW - Iron nanoparticles KW - Anemia KW - ICP-MS KW - In vitro KW - In situ PY - 2020 DO - https://doi.org/10.1080/17435390.2019.1710613 VL - 14 IS - 3 SP - 388 EP - 403 PB - Taylor & Francis Online CY - London AN - OPUS4-50314 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Redefining stable isotope analysis by molecular absorption spectrometry N2 - Variations in the isotope amount composition of some elements like lithium, boron, magnesium, calcium, copper and strontium have been used as proof of provenance of a sample and to describe geological processes. Routinely, isotope compositions are determinate by mass spectrometry; the working horse of the isotope analysis. However, mass spectrometric methods are expensive, time consuming and they require a high qualified analysist. Here an alternative faster and low cost optical method for isotope ratio determination is proposed: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Stable isotope amount composition of X= Li, B, Mg, Ca, Cu and Sr have been determined by monitoring the absorption spectrum of their monohydride (XH) in graphite furnace HR-CS-MAS. For example, for the three Mg isotopes (24Mg, 25Mg and 26Mg) band (0→0) for the electronic transition X1Σ+ → A1Π was evaluated around wavelength 513.4 nm (Fig. 1). Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression were built. Results are metrological compatible with those reported by mass spectrometric methods. T2 - Adlershofer Forschungsforum 2017 CY - Berlin, Germany DA - 10.11.2017 KW - Isotopes KW - High-Resolution Continuum Source Molecular Absorption Spectrometry KW - HR-CS-MAS KW - Isotopic shift KW - Metal hydrides KW - Graphite furnace KW - Molecular absorption PY - 2017 AN - OPUS4-43342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Straub, F. A1 - Wirth, Thomas A1 - Holzlechner, G. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Real Time Imaging of Deuterium in a Duplex Stainless Steel Microstructure by Time-of-Flight SIMS N2 - For more than one century, hydrogen assisted degradation of metallic microstructures has been identified as origin for severe technical component failures but the mechanisms behind have not yet been completely understood so far. Any in-situ observation of hydrogen transport phenomena in microstructures will provide more details for further elucidation of these degradation mechanisms. A novel experiment is presented which is designed to elucidate the permeation behaviour of deuterium in a microstructure of duplex stainless steel (DSS). A hydrogen permeation cell within a TOF-SIMS instrument enables electrochemical charging with deuterium through the inner surface of the cell made from DSS. The outer surface of the DSS permeation cell exposed to the vacuum has been imaged by TOF-SIMS vs. increasing time of charging with subsequent chemometric treatment of image data. This in-situ experiment showed evidently that deuterium is permeating much faster through the ferrite phase than through the austenite phase. Moreover, a direct proof for deuterium enrichment at the austenite-ferrite interface has been found. KW - Characterization and analytical techniques KW - Corrosion KW - Imaging technique KW - Mass spectrometry PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-353872 UR - http://www.nature.com/articles/srep19929 DO - https://doi.org/10.1038/srep19929 SN - 2045-2322 VL - 6 IS - 19929 SP - 1 EP - 7 PB - nature publishing group CY - London, United Kingdom AN - OPUS4-35387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El-Dahshan, O. A1 - Deniaud, A. A1 - Ling, W. L. A1 - Wegner, Karl David A1 - Proux, O. A1 - Veronesi, G. A1 - Reiss, P. T1 - Hydrothermal microwave synthesis of water soluble NIR-II emitting Ag2S quantum dots N2 - Hydrothermal-based synthetic methods of quantum dots allow for the exploration of reaction parameters normally inaccessible to typical aqueous-based batch reactions, such as elevated reaction temperatures (>100 °C) and reaction pressures above atmospheric pressure. Coupled with microwave heating, new instantaneously bio-compatible quantum dots (QDs) with enhanced opitcal properties can be yielded. As of today, aqueous-based synthetic methods often lag behind their organic analogues in terms of the photophysical properties of the QDs obtained and the ease of modulation of both the emission wavelength and crystallite size. Using a novel microwave-assisted hydrothermal approach, the synthesis of silver sulphide (Ag2S) QDs exhibiting NIR emission spanning the biological transparency windows via modulation of the reaction parameters has been developed. The intrinsic link between their optical and structural properties is explored via laboratory and synchrotron-based structural analysis techniques. Their toxicity towards a hepatic cell line was assessed, and related back to their structure and size. Overall this work aims to not only further develop the repertoire of synthetic methods for the synthesis of Ag2S QDs, but also paves the way for the development of safer QDs suitable for future clinical applications. KW - Quantum dots KW - Microwave synthesis KW - Quality assurance KW - NIR-II emission KW - PL quantum yield KW - Ag2S PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634825 DO - https://doi.org/10.1039/d5nr00052a SN - 2040-3372 VL - 17 IS - 24 SP - 14637 EP - 14646 PB - RSC AN - OPUS4-63482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohan, M. A1 - Prochazka, D. A1 - You, Yi A1 - Riedel, Jens A1 - Gornushkin, Igor A1 - Rocnakova, I. A1 - Papula, M. A1 - Porízka, P. A1 - Kaizer, J. T1 - Investigating plasma morphology at material boundaries under varying ambient pressures N2 - Laser-Induced Breakdown Spectroscopy (LIBS) is a widely used technique for elemental analysis. The analysis of the obtained LIBS spectra generally assumes plasma homogeneity. However, using focused laser beams for interrogation, LIBS probes materials on the microscale and is, thus, prone to artefacts from sample heterogeneities on the micrometer scale. An ablation at a material boundary of two matrices may result in a significant inhomogeneity in the plasma plume, which can severely impact the accuracy of quantitative analysis. Since this propagation of the surface morphology into the plasma plume is driven by the plasma expansion, its final impact is strongly pressure dependent. This study examines the influence of varying ambient pressures (7–1000 mbar) on plasma morphology, spectral characteristics, and key plasma properties such as electron number density at a well-defined Cu–Sn boundary, in comparison with the results obtained using homogeneous alloys. Several approaches of plasma imaging with bandpass filters, spectroscopy, and Radon transform-based 3D reconstruction were employed to analyze elemental distribution, signal-to-noise (SNR) and signal-to-background (SBR) ratios, as well as electron number densities. The 3D reconstructions revealed a pronounced plasma asymmetry for the ablation at the material boundary, in contrast to the near-axial symmetry observed for the ablation of homogeneous alloys. At lower pressures, this distinct elemental separation in plasma persisted, while higher pressures led to an increased collisional mixing and homogenization. SNR and SBR were consistently lower for ablation at the boundary compared to homogeneous samples. These findings highlight how boundary ablation contributes to plasma inhomogeneities in LIBS analysis of heterogeneous materials and emphasize the need to account for these effects when using LIBS for elemental mapping of fine heterogeneous structures. KW - Laser-induced breakdown spectroscopy KW - Plasma inhomogeneity KW - Plasma tomography KW - Radon transform KW - Material boundaries KW - Ambient pressure effects PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634777 DO - https://doi.org/10.1016/j.talanta.2025.128377 SN - 1873-3573 VL - 295 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-63477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herrmann, Antje Jutta A1 - Techritz, Sandra A1 - Jakubowski, Norbert A1 - Haase, A. A1 - Luch, A. A1 - Panne, Ulrich A1 - Müller, Larissa T1 - A simple metal staining procedure for identification and visualization of single cells by LA-ICP-MS N2 - High lateral resolution of metal detection in single cells by use of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) demands powerful staining methods. In this work different staining procedures for the single cell analysis with LA-ICP-MS were optimized. An iridium intercalator was utilized to stain the cell nuclei whereas the whole cell was stained by the use of maleimido-mono-amide-DOTA (mDOTA) complexing lanthanide(III) ions. The content of the artificially introduced metals per cell was quantified using a matrix matched calibration approach based on cellulose membranes onto which standards were spotted by a microarray spotter. Absolute metal stain amounts in the range of 2.34 to 9.81 femtomole per cell were determined. The metal staining procedures allow direct identification and visualization of single cells and their cell compartments by element microscopy without the use of bright field images of the sample. KW - Single Cell Analysis KW - Bioimaging KW - LA-ICP-MS based immunoassays PY - 2017 DO - https://doi.org/10.1039/c6an02638a SN - 0003-2654 SN - 1364-5528 VL - 142 IS - 10 SP - 1703 EP - 1710 PB - The Royal Society of Chemistry AN - OPUS4-40251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Phukphatthanachai, Pranee T1 - An alternative approach of using pe frits for the quantification of sulfur in copper metals and its alloys by isotope dilution LA-ICP-MS N2 - This is the first time that PE frits were used to quantify sulfur in copper and its alloys by isotope dilution combined with LA-ICP-MS: an alternative approach for sample preparation. The following properties of the PE frit meet the requirements for isotope dilution LA-ICPMS:: porous material, thermo plastic (melting point >100oC), chemical resistance (nitric acid >70%) and high adsorption efficiency. The breakthrough, however, as a support material, especially when comparing the PE frit with other materials such gelatin or sodium silicate is the low blank, which is only two times of the gas flow blank (2.3-4.0 x 104 cps). Additionally, the porosity of the frit was considered, as it directly affects the adsorption efficiency for the sample solution, which is present in the cavities of the frit. Adsorption efficiency was studied by depositing sulfur standards with varying sulfur amounts (0, 2, 5, 10, 20, 40 and 80 µg S) on the frits. The remaining sulfur which was not absorbed by the frit was rinsed off and was measured by ICP-MS. This indirect method shows that more than 99.5 % of the loaded sulfur was absorbed by the frit. Such high absorption efficiency is completely sufficient for a support material to be used in LA-ICP-IDMS. The so prepared frits whith increasing sulfur amount were measured by LA-ICP-MS showing a good linearity between 0 µg S and 40 µg S whit a correlation coefficient r2 of 0.9987 and sensitivy of 3.4x104 cpsµg-1 for 32S. Three copper reference materials produced by BAM were selected to develop and validate the LA-ICP-IDMS procedure. The IDMS technique was applied to these samples as follows: the samples were spiked, dissolved, digested and then the digest was adsorbed on the frits. T2 - Winter Conference on Plasma Spectrochemistry CY - Amelia Island, FL, USA DA - 08.01.2018 KW - Laser ablation KW - Isotope dilution mass spectrometry KW - SI traceability KW - Measurement uncertainty PY - 2018 AN - OPUS4-44642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Müller-Vahl, H. A1 - Nayeri, C. N. A1 - Paschereit, C. O. A1 - Greenblatt, D. T1 - Airfoil in a high amplitude oscillating stream N2 - A combined theoretical and experimental investigation was carried out with the objective of evaluating theoretical predictions relating to a two-dimensional airfoil subjected to high amplitude harmonic oscillation of the free stream at constant angle of attack. Current theoretical approaches were reviewed and extended for the purposes of quantifying the bound, unsteady vortex sheet strength along the airfoil chord. This resulted in a closed form solution that is valid for arbitrary reduced frequencies and amplitudes. In the experiments, the bound, unsteady vortex strength of a symmetric 18 % thick airfoil at low angles of attack was measured in a dedicated unsteady wind tunnel at maximum reduced frequencies of 0.1 and at velocity oscillations less than or equal to 50 %. With the boundary layer tripped near the leading edge and mid-chord, the phase and amplitude variations of the lift coefficient corresponded reasonably well with the theory. Near the maximum lift coefficient overshoot, the data exhibited an additional high-frequency oscillation. Comparisons of the measured and predicted vortex sheet indicated the existence of a recirculation bubble upstream of the trailing edge which sheds into the wake and modifies the Kutta condition. Without boundary layer tripping, a mid-chord bubble is present that strengthens during flow deceleration and its shedding produces a dramatically different effect. Instead of a lift coefficient overshoot, as per the theory, the data exhibit a significant undershoot. This undershoot is also accompanied by high-frequency oscillations that are characterized by the bubble shedding. In summary, the location of bubble and ist subsequent shedding play decisive roles in the resulting temporal aerodynamic loads. KW - vortex shedding KW - aerodynamics KW - general fluid mechanics PY - 2016 DO - https://doi.org/10.1017/jfm.2016.126 SN - 0022-1120 VL - 2016 IS - 793 SP - 79 EP - 108 AN - OPUS4-35594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Multimethodische Bestimmung von Feuchtegradienten in Estrich N2 - Um den Feuchtegehalt von Fußbodenestrich vor der Verlegung von Holz- oder anderen Bodenbelägen zu bestimmen, werden zerstörende Prüfverfahren wie die Calcium-Carbid Methode (CM) oder das thermogravimetrische Darr-Verfahren eingesetzt. Diese liefern jedoch einmalig nur punktuelle Informationen und sind je nach Estrichtyp auch störanfällig. Zusammen mit Partnern aus Forschung und Industrie wurde an der BAM ein Ringversuch durchgeführt, dessen Ziel es war, verschiedene nach Möglichkeit zerstörungsfreie oder – arme Prüfverfahren hinsichtlich ihrer Genauigkeit und Sensitivität vor allem im Bereich der Belegereife zu testen. Hier dargestellt sind die Ergebnisse aufgenommen an einer Calciumsulphat-Estrich Probe vom Typ Knauf FE80 Largo mit drei Verfahren, die auch Aussagen über die Feuchtegradienten in die Tiefe zulassen. Die Proben wurden bei Konstant-Normklima mit T=23 °C und rH=50 % zur Trocknung gelagert. T2 - Bauwerksdiagnose 2016 CY - Berlin, Germany DA - 25.02.2016 KW - Feuchtemessung KW - Estrich KW - Sensorik PY - 2016 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-35478 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias T1 - Chances and limitations of RFID sensor systems – practical experiences from research projects with different application scenarios N2 - The combination of Radio-frequency identification (RFID) and low energy sensors offers promising chances to implement cost effective, easy to apply, and easy to handle sensor systems for a variety of applications. The RFID technology is already well established in logistics. Enhanced processing and interface capabilities enable the integration of various sensors for control, diagnostics, and monitoring tasks. In the scope of research projects carried out at the Federal Institute for Materials Research and Testing (BAM), RFID sensor systems were developed and validated with regard to two different application scenarios: the Identification and diagnosis of concrete components for road bridges and the monitoring of dangerous goods transportation. This contribution presents selected research results and reflects the practical experiences on future chances and limitations of RFID sensor systems. T2 - IDTechEx Show! Europe 2016 CY - Berlin, Germany DA - 27.04.2016 KW - RFID Sensors systems KW - Diagnosis of concrete components KW - Monitoring of dangerous goods PY - 2016 AN - OPUS4-36034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine A1 - Strangfeld, Christoph A1 - Wöstmann, Jens T1 - Measuring screed moisture with EM methods – a comparison of capacitive handheld and microwave resonator probes N2 - We have compared the performance of the typical Darr and CM moisture testing techniques, which are destructive with several non-destructive testing techniques on two types of floor screeds. In case of cement based screeds these destructive tests failed to deliver reliable results. Moreover, our measurements indicate significantly different drying and moisture transport behavior for the investigated cement based and calcium-sulphate based screeds. Whereas we have strong with depth decreasing moisture gradients in the CT material, we observe in the penetrated volumes of our ndt methods basically no clear moisture gradient in the CA samples. The findings with ndt methods could be supported by moisture gradient studies with nuclear magnetic resonance measurements. T2 - 11th Int. Conference on electromagnetic wave interaction with water and moist substances CY - Florenz, Italy DA - 23.5.2016 KW - Moisture KW - Screed KW - Microwave KW - Nuclear magnetic resonance PY - 2016 SP - 77 EP - 84 AN - OPUS4-36674 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Johann, Sergej A1 - Kammermeier, Michael A1 - Müller, Maximilian A1 - Strangfeld, Christoph T1 - Transmission characteristics of RFID sensor systems embedded in concrete N2 - Completely embedded sensor systems for long-term operation offer innovative possibilities for structural health monitoring of concrete structures. Measuring of relevant parameters, e.g., temperature, humidity, or indication of corrosion can be performed with low energy sensors. This allows to implement passive RFID sensor systems without cable connection and battery, which are power supplied exclusively by the electromagnetic field from the external reader device. To evaluate characteristics and conditions of this concept, a systematical investigation of the transmission characteristics with variation of relevant parameters, as communication frequency, installation depth, type of concrete, moisture content, etc. is currently carried out in an interdisciplinary research project at BAM. First results are presented in this paper. T2 - IEEE Sensors 2016 CY - Orlando, FL, USA DA - 30.10.2016 KW - Embedded sensors KW - Energy harvesting KW - Wireless sensors KW - RFID sensors KW - Transmission characteristics KW - Structural health monitoring PY - 2016 SN - 978-1-4799-8287-5 SN - 1930-0395 SP - 1541 EP - 1543 PB - IEEE AN - OPUS4-38388 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Intelligent bridge: the durabasttest bridge equipped with RFID-based sensors N2 - The duraBASt area at the highway intersection “Köln-Ost” is a large test field for road testing. It includes the duraBASt test bridge which is ca. 66 m long and 14.25m broad. This bridge is part of the “road in the 21st century” project and is equipped with several sensors for structural health monitoring. This feasibility study is realised to construct intelligent bridges in the future. Quantities like temperature, strain, moisture, corrosion, etc. are measured by embedded sensors. In the presented work, the focus lays on passive RFID-based sensors. The communication and energy supply is realised by a mobile transmitter through the concrete cover. Hence, no cables or batteries are required. The sensors are design to withstand in the alkaline environment in concrete. Thus, moisture and corrosion are detectable for several decades. T2 - Structural Materials Technology 2016 CY - Portland, ME, USA DA - 29.08.2016 KW - RFID based sensors KW - SHM in civil engineering PY - 2016 AN - OPUS4-37466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias T1 - Transmission characteristics of RFID sensor systems embedded in concrete N2 - Completely embedded sensor systems for long-term operation offer innovative possibilities for structural health monitoring of concrete structures. Measuring of relevant parameters, e.g., temperature, humidity, or indication of corrosion can be performed with low energy sensors. This allows to implement passive RFID sensor systems without cable connection and battery, which are power supplied exclusively by the electromagnetic field from the external reader device. To evaluate characteristics and conditions of this concept, a systematical investigation of the transmission characteristics with variation of relevant parameters, as communication frequency, installation depth, type of concrete, moisture content, etc. is currently carried out in an interdisciplinary Research project at BAM. First results are presented in this paper. T2 - IEEE Sensors 2016 CY - Orlando, FL, USA DA - 30.10.2016 KW - Embedded sensors KW - Energy harvesting KW - Wireless sensors KW - RFID sensors KW - Transmission characteristics KW - Structural health monitoring PY - 2016 AN - OPUS4-38387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reuter, U. A1 - Taffe, A. A1 - Maack, Stefan T1 - Messung von Bauteildicken an Brückenquerschnitten mit Ultraschallecho zur weiteren Verwendung in statischen Berechnungen zur verbesserten Ermittlung des Eigengewichts N2 - Mit zunehmenden Alter und wachsenden Verkehr treten vermehrt Verschleißerscheinungen an Brückenbauwerken auf. Um in der Zukunft dem weiter steigendem Straßenverkehr gewachsen zu sein, muss besonders der Zustand der Bestandsbrücken vor 1985 erfasst und beurteilt werden. Im Rahmen der Nachrechnungsrichtlinie von Straßenbrücken können genauere Kenntnisse über das Eigengewicht eines Brückenbauwerks dazu genutzt werden, um den entsprechenden Teilsicherheitsbeiwert auf der Einwirkungsseite der statischen Berechnung abzusenken und dadurch die Realität genauer abzubilden. Mit Hilfe des Ultraschallechoverfahrens wurden die Bauteildicken an einem Brückensegment der Spandauer-Damm-Brücke auf dem TTS der BAM ermittelt und zur Berechnung des Eigengewichtes weiter verwendet. Zeitgleich wurde dabei untersucht, wie dicht das Messraster gewählt werden muss, damit bei einem möglichst geringen Messaufwand dennoch zuverlässig Bauteildicken abgeschätzt werden können. Auf Grundlage der ausgewerteten Messdaten wurde für die verschiedenen Messpunktabstände die jeweilige Masse des Bauteils berechnet. Zur Überprüfung der Genauigkeit der Ergebnisse wurde das Brückensegment als Ganzes gewogen. Des Weiteren wurden die ermittelten Bauteildicken und Massen des Brückensegmentes nach der Methode des GUMs (Guide to the Expression of uncertainty in measurement) statistisch bewertet. Die Ergebnisse zeigen, das Bauteildicken bis auf 96 % genau mit dem Ultraschallechoverfahren ermittelt werden können. Dabei offenbarte die statistische Auswertung, dass das Eigengewicht von der Rohdichte des Betons und den mit Ultraschallechoverfahren ermittelten Bauteildicken maßgebend beeinflusst werden. Daher sollte einer genaueren Bestimmung der Rohdichte zur Abschätzung des Eigengewichts nach der vorgestellten Methode besondere Aufmerksamkeit geschenkt werden. Die Masterarbeit (Titel s.o.) entstand im Sommersemester 2015 an der HTW Berlin in Kooperation mit der BAM und ist in der Bibliothek der HTW Berlin verfügbar. T2 - Fachtagung Bauwerksdiagnose Praktische Anwendungen Zerstörungsfreier Prüfungen und Zukunftsaufgaben CY - Berlin, Germany DA - 25.02.2016 KW - Brücke KW - Nachrechnungsrichtlinie KW - Zerstörungsfreie Prüfung PY - 2016 AN - OPUS4-39297 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan A1 - Zoёga, Andreas T1 - Lösung bautechnischer Fragestellungen mit der ZfPBau-Toolbox N2 - Darstellung verschiedener praxisrelevanter zerstörungsfreier Prüfverfahren im Bauwesen. T2 - Fachtagung Bauwerksdiagnose Praktische Anwendungen Zerstörungsfreier Prüfungen und Zukunftsaufgaben CY - Berlin, Germany DA - 25.02.2016 KW - zerstörungsfreie Prüfung im Bauwesen PY - 2016 AN - OPUS4-39295 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Loehr, Konrad T1 - Quantitative LA-ICP-MS of single cells: Comparison of single spot ablation and imaging N2 - LA-ICP-MS finds widespread use in the analysis of biological samples and its importance as an analysitical method is still increasing. Often tissues or single cells are ablated in imaging mode on glass slides, but the analysis time increases by reducing the spot size of the laser. Additionally, with increased lateral resolution a loss in sensitivity is inherently connected and this holds true in particular for single cell analysis in imaging mode. However, if only the composition of elements in a single cell needs to be measured, complete ablation of cells by single shots looks promising. This approach was already discussed by Managh et al. and will be discussed in more detail in this presentation. The aim of this study is to develop a calibration strategy for single cell analysis based on the total consumption concept. It will be shown that this concept provides quantitative results at single cell level, if the target material is ablated. We compare two different laser spot sizes, 30 µm and 110 µm. The smaller spot size of 30 µm is used for imaging and the larger spot size of 110 µm is used for the targeted ablation of complete single cells. Cells were stained by two novel cell dyes, mDOTA-Tb (CheMatech, Dijon, France), which binds to free thiol groups of proteins, and Ir-DNA intercalator (Maxpar®, Fluidigm, San Francisco, USA), which stains DNA quantitatively. Finally, quantification of Ir and Tb will be performed by matrix matching calibration, following the approach of Drescher et al.[1], i.e. spotting of a dilution series of Ir and Tb standards on nitrocellulose membrane. Results obtained so far show a good correlation between imaging and single spot ablation, indicating that the total consumption concept may serve as an acceptable assumption. T2 - EWCPS CY - St. Anton am Arlberg, Austria DA - 19.02.2017 KW - Single spot ablation KW - LA-ICP-MS KW - Single cell analysis KW - Bioimaging PY - 2017 AN - OPUS4-39763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine A1 - Wöstmann, Jens A1 - Munsch, Sarah Mandy A1 - Hase, Felix T1 - Moisture in screed: a non-destructive multi-sensor approach N2 - Eight different screed types are tested including two different sample heights of 35 and 70 mm. The moisture of the four cement based and four sulphate based screeds are monitored during hydration and evaporation. All samples are stored in a climatic chamber at 23◦ C and 50 % relative humidity. Embedded sensors like temperature arrays, humidity sensor arrays, and multi-ring electrodes are embedded in the samples to yield a detailed moisture evolution with high depth resolution. Furthermore, nuclear magnetic resonance is used to quantify the water content at different depths. This multi-sensor approach allows a comprehensive monitoring of the moisture and its gradient in the different screed samples. This yields a deeper insight into the hydration, moisture convection, and diffusion processes. T2 - 8th European Workshop On Structural Health Monitoring CY - Bilbao, Spain DA - 05.07.2016 KW - NMR KW - Screed KW - Embedded sensors KW - Moisture KW - Corresponding relative humidity PY - 2016 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. SP - 1 EP - 11 AN - OPUS4-36814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture in screed: a non-destructive multi-sensor approach N2 - Eight different screed types are tested including two different sample heights of 35 and 70 mm. The moisture of the four cement based and four sulphate based screeds are monitored during hydration and evaporation. All samples are stored in a climatic chamber at 23° C and 50 % relative humidity. Embedded sensors like temperature arrays, humidity sensor arrays, and multi-ring electrodes are embedded in the samples to yield a detailed moisture evolution with high depth resolution. Furthermore, nuclear magnetic resonance is used to quantify the water content at different depths. This multi-sensor approach allows a comprehensive monitoring of the moisture and its gradient in the different screed samples. This yields a deeper insight into the hydration, moisture convection, and diffusion processes. T2 - EWSHM 2016 CY - Bilbao, Spain DA - 05.07.2016 KW - Moisture KW - Screed KW - Embedded sensors KW - Corresponding relative humidity KW - NMR PY - 2016 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-36840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture Measurements with RFID based Sensors in Screed and Concrete N2 - To quantify the moisture in concrete, RFID based humidity sensors are embedded. Passive high frequency, ultra-high frequency RFID tags as well as active Bluetooth sensors are tested. After concreting, all sensors measure the corresponding relative humidity to monitor the concrete moisture. Two case studies are performed, embedding in an existing construction, i.e. the duraBASt test bridge, and embedding in cement based mortar in the laboratory. As basis for robust and long-life sensors in alkaline concrete, different casing materials are tested. Furthermore, signal strength measurements and their sensitivity to different moisture levels are performed. T2 - EWSHM 2016 CY - Bilbao, Spain DA - 05.07.2016 KW - Moisture measurements KW - RFID based sensors KW - DuraBASt KW - Humidity sensors KW - Long-life sensor casing PY - 2016 AN - OPUS4-36834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Moisture measurement methods N2 - Moisture can cause imperfect sealings, faulty roof constructions, cracks and other kind of damages. For measuring the moisture in construction materials like concrete and screed, there are destructive(direct) and non-destructive(indirect) methods, that can be used. This presentation gives an overview and a comparison of these methods. T2 - Nondestructive Testing and Evaluation in Civil Engineering and Surveying - Advanced Training 2016 CY - Berlin, Germany DA - 14.07.2016 KW - Moisture KW - Non-destructive testing PY - 2016 AN - OPUS4-37005 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weller, Andreas A1 - Zhang, Zeyu A1 - Slater, L. A1 - Kruschwitz, Sabine A1 - Halisch, M. T1 - Induced polarization and pore radius - a discussion N2 - Permeability estimation from spectral induced polarization (SIP) measurements is based on a fundamental premise that the characteristic relaxation time (t) is related to the effective hydraulic radius (reff) controlling fluid flow. The approach requires a reliable estimate of the diffusion coefficient of the ions in the electrical double layer. Others have assumed a value for the diffusion coefficient, or postulated different values for clay versus clay-free rocks. We examine the link between t and reff for an extensive database of sandstone samples where mercury porosimetry data confirm that reff is reliably determined from a modification of the Hagen- Poiseuille equation assuming that the electrical tortuosity is equal to the hydraulic tortuosity. Our database does not support the existence of 1 or 2 distinct representative diffusion coefficients but instead demonstrates strong evidence for 6 orders of magnitude of variation in an apparent diffusion coefficient that is well correlated with both reff and the specific surface area per unit pore volume (Spor). Two scenarios can explain our findings: (1) the length-scale defined by t is not equal to reff and is likely much longer due to the control of pore surface roughness; (2) the range of diffusion coefficients is large and likely determined by the relative proportions of the different minerals (e.g. silica, clays) making up the rock. In either case, the estimation of reff (and hence permeability) is inherently uncertain from SIP relaxation time. T2 - IP Workshop 2016 CY - Aarhus, Denmark DA - 06.06.2016 KW - Pore radius KW - Mercury intrusion capillary pressure KW - Spectral induced polarization KW - Relaxation time PY - 2016 SP - 1 EP - 4 AN - OPUS4-37004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weller, Andreas T1 - Induced polarization and pore radius – a discussion N2 - Permeability estimation from spectral induced polarization (SIP) measurements is based on a fundamental premise that the characteristic relaxation time (t) is related to the effective hydraulic radius (reff) controlling fluid flow. The approach requires a reliable estimate of the diffusion coefficient of the ions in the electrical double layer. Others have assumed a value for the diffusion coefficient, or postulated different values for clay versus clay-free rocks. We examine the link between t and reff for an extensive database of sandstone samples where mercury porosimetry data confirm that reff is reliably determined from a modification of the Hagen-Poiseuille equation assuming that the electrical tortuosity is equal to the hydraulic tortuosity. Our database does not support the existence of 1 or 2 distinct representative diffusion coefficients but instead demonstrates strong evidence for 6 orders of magnitude of variation in an apparent diffusion coefficient that is well correlated with both reff and the specific surface area per unit pore volume (Spor). Two scenarios can explain our findings: (1) the length-scale defined by t is not equal to reff and is likely much longer due to the control of pore surface roughness; (2) the range of diffusion coefficients is large and likely determined by the relative proportions of the different minerals (e.g. silica, clays) making up the rock. In either case, the estimation of reff (and hence permeability) is inherently uncertain from SIP relaxation time. T2 - IP Workshop 2016 CY - Aarhus, Denmark DA - 06.06.2016 KW - Pore radius KW - Mercury intrusion capillary pressure KW - Spectral induced polarization KW - Relaxation time PY - 2016 AN - OPUS4-37003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Halisch, M. T1 - Quantification of rock structures with high resolution X-Ray μ-CT for laboratory SIP measurements N2 - Spectral Induced Polarization (SIP) measurements are used in many different ways to characterize natural rocks and soils. Main foci of interest are the enhanced characterization of the causes of IP-effects in clastic rocks (especially sandstones), the interactions between the matrix-fluid-system and within the electrical double layers as well as the correlation with “classical” petrophysical parameters, such as specific surface area, permeability, mercury intrusion capillary pressure (MICP) and others. Nevertheless, for all of these investigations, knowledge of the inner structure of the sample material is essential in order to create reliable and validated models as well as to interpret and to assess the data most completely. Unfortunately, many of the methods used, to get access to the inner structure of rocks are destructive (e.g. MICP, thin sectioning, etc.) and the valuable sample is lost. In addition, data is either of volume integrated nature or only available for the 2D case and the usage of sister cores does not necessarily lead to reliable results. In this paper, the authors showcase the possibilities of non-destructive and three dimensional X-ray computed tomography and of enhanced image analysis capabilities for the quantification of rock structures at the pore scale. T2 - IP Workshop 2016 CY - Aarhus, Denmark DA - 06.06.2016 KW - SIP KW - μ-CT imaging KW - Rock structure KW - Digital image analysis KW - Pore geometry KW - Grain geometry PY - 2016 AN - OPUS4-37000 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine T1 - Multimethodische Bestimmung von Feuchtegradienten in Estrich N2 - Um den Feuchtegehalt von Fußbodenestrich vor der Verlegung von Holz- oder anderen Bodenbelägen zu bestimmen, werden zerstörende Prüfverfahren wie die Calcium-Carbid Methode (CM) oder das thermogravimetrische Darr-Verfahren eingesetzt. Diese liefern jedoch einmalig nur punktuelle Informationen und sind je nach Estrichtyp auch störanfällig. Zusammen mit Partnern aus Forschung und Industrie wurde an der BAM ein Ringversuch durchgeführt, dessen Ziel es war, verschiedene nach Möglichkeit zerstörungsfreie oder – arme Prüfverfahren hinsichtlich ihrer Genauigkeit und Sensitivität vor allem im Bereich der Belegereife zu testen. Hier dargestellt sind die Ergebnisse aufgenommen an einer Calciumsulphat-Estrich Probe vom Typ Knauf FE80 Largo mit drei Verfahren, die auch Aussagen über die Feuchtegradienten in die Tiefe zulassen. Die Proben wurden bei Konstant-Normklima mit T=23 °C und rH=50 % zur Trocknung gelagert. T2 - Fachtagung Bauwerksdiagnose CY - Berlin, Germany DA - 25.02.2016 KW - Estrich KW - Nuklear Magnetische Resonanz KW - Elektrischer Widerstand KW - Feuchtegehalt KW - Zerstörungsfreie Prüfverfahren PY - 2016 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-36994 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Measuring screed moisture with EM methods – a comparison of capacitive Handheld and microwave resonator probes N2 - Measuring the moisture state of screeds is critical for floorers in order to prevent structural damages of bottom coverings. Typically destructive tests are carried out on small samples delivering only punctual information. We tested several non-destructive testing methods in terms of sensitivity in the critical low moisture range and observed substantially different drying behavior for the two tested cement based and calcium-sulphate based screed samples. Our findings are supported by moisture gradient measurements using the nuclear magnetic resonance technique. T2 - 11th Int. Conference on Electromagnetic Wave Interaction with Water and Moist Substances CY - Florence, Italy DA - 23.05.2016 KW - resonance KW - moisture KW - screed KW - microwave KW - nuclear magnetic PY - 2016 AN - OPUS4-36945 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Measuring moisture in building material - an overview N2 - In Germany there is an existing built infrastructure worth about 50 trillion Euros. The expected lifetimes of individual structures are up to 100 years. Considerable costs (annually about 35 billion Euros, the trend continues upwards) are involved in order to maintain and rehabilitate both residential as well as transportation infrastructure buildings. Most damages we observe on our built infrastructure are moisture-induced processes. Consequently reliable moisture measurement tools a highly needed for meaningful building diagnosis investigations. The optimal moisture measuring technique would be non-destructive, fast, repeatable, reliable, independent of steel in the vicinity, the surface condition or possible salt loads of the material under test. Since this is unfortunately not the case for any non-destructive method, it is often very difficult to decide for users which method to use for the particular testing problem. The only standardized methods in Germany are the “direct” and destructive Darr- and the CM tests. Although they can be highly accurate (when handled with care during the sampling), they deliver only punctual information and cannot be used for monitoring. The other, non-destructive methods are based on the change in humidity-dependent physical material properties. The underlying physics, their particular advantages and disadvantages are discussed in this paper. T2 - Building Safety Symposium CY - Hong Kong, China DA - 22.04.2016 KW - Non-destructive methods KW - Moisture measuring KW - Electrical methods KW - Microwave PY - 2016 AN - OPUS4-37118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Estrichfeuchteuntersuchungen mit geophysikalischen Methoden - ein Laborversuch N2 - Zur Bestimmung des Feuchtezustands und insbesondere der Belegereife von Estrichfußböden kommen in Deutschland zerstörende Prüfverfahren zum Einsatz, die eine punktuelle Probenahme erfordern. Hierbei ergeben sich immer wieder Fehlinterpretationen, da zum einen die Probenahme selbst zu einer Veränderung des Feuchtezustands führt und zum anderen, weil die Verfahren an sich mitunter ungenau sind (z.B. abhängig von der Estrichzusammensetzung). Zusammen mit vier Forschungsinstituten und dem Industriepartner Bosch wurden an der BAM zerstörungsfreie Prüfverfahren auf deren Tauglichkeit zur Estrichfeuchtemessung untersucht und mit den herkömmlichen zerstörenden Verfahren verglichen. Für diesen Versuch kamen verschiedene geophysikalische Verfahren zum Einsatz, darunter Nuklear Magnetische Resonanz (NMR), elektrische Widerstandsmessungen und Impulsradar (GPR). Es wurden neun verschiedene Estrichsorten hergestellt und während der Trocknungsphase bei Konstant-Normklima gelagert. Diese wurden sowohl zerstörend als auch zerstörungsfrei mit den o. g. Verfahren untersucht. Gleichzeitig wurden die Masseänderungen der Proben zur Bestimmung des integralen Feuchtehalts aufgezeichnet. Die Ergebnisse zeigen zum einen, dass das Abtrocknungsverhalten von zementgebundenen Estrichen grundsätzlich unterschiedlich von dem anhydritgebundener Estriche ist. Während sich bei ersteren zügig ein deutlicher Feuchtegradient über die Höhe der Proben einstellt, verläuft dieser bei der zweiten Probengruppe sehr flach. Dies lässt sich vor allem in den NMR Daten räumlich hochaufgelöst nachvollziehen - die Datenakquise erfolgte mit einer NMR MOUSE PM 25. Ein ähnliches Bild ergibt sich auch aus den elektrischen Widerstandsmessungen, die mittels sog. Multi-Ring-Elektroden (MRE) durchgeführt wurden. MRE bezeichnen als Vertikalprofil angeordnete Ringelektroden mit einem Abstand von ca. 1-2 mm, zwischen denen jeweils Zwei-Punkt Widerstandsmessungen durchgeführt werden. Bei sehr geringen Feuchtegehalten (z.T. auch um die Belegereife) waren mit dieser Methode jedoch wegen der zu hohen Übergangswiderstände nur bedingt Messungen möglich. Im Gegensatz zu NMR und MRE sind mit dem Radarverfahren (2 GHz Antenne) keine tiefenbezogenen Aussagen möglich. Jedoch lässt sich über eine Amplitudenauswertung von direkter und an der Rückwand reflektierter Welle teilweise eine Aussage über Restfeuchtigkeit im Volumen treffen. Ebenso zeigt die Laufzeitdifferenz der beiden Wellen eine starke Abhängigkeit vom Feuchtegehalt. T2 - DGG 2016 CY - Münster, Germany DA - 14.03.2016 KW - Nuklear magnetische Resonanz KW - Zerstörungsfreie Methoden KW - Estrichfeuchtemessung PY - 2016 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-37117 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Johann, Sergej A1 - Kammermeier, Michael A1 - Müller, Maximilian A1 - Strangfeld, Christoph T1 - RFID sensor systems embedded in concrete – systematical investigation of the transmission characteristics N2 - Long-term completely embedded sensor systems offer innovative possibilities for structural health monitoring of concrete structures. Measuring of relevant parameters, e.g., temperature, humidity, or indication of corrosion can be performed with low energy sensors. This allows to implement passive RFID sensor systems without cable connection and battery, which are power supplied exclusively by the electromagnetic field from the external reader device. To evaluate characteristics and conditions of this concept, a systematical investigation of the transmission characteristics with variation of relevant parameters, as communication frequency, installation depth, type of concrete, moisture content, etc. is currently carried out in an interdisciplinary research project at BAM. First results are presented in this paper. T2 - 8th European Workshop On Structural Health Monitoring CY - Bilbao, Spain DA - 05.07.2016 KW - Structural health monitoring KW - Embedded sensor KW - Energy harvesting KW - Wireless sensors KW - RFID sensors KW - Transmission characteristics PY - 2016 SP - 1 EP - 5 AN - OPUS4-37129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hauke, Max T1 - Autonomes mobiles Scanner-System zur zerstörungsfreien Prüfung von Stahlbeton N2 - Der BetoScan Light ist eine mobile autonome Messplattform zur automatisierten Ausführung von verschiedenen zerstörungsfreien Messverfahren. Das System besitzt eine kamerabasierte Navigation und ist fähig, anhand eines aufgestellten Schildes, welches als Ziel dient, eine Spur mit möglichst geringer Abweichung von der geraden Luftlinie abzufahren. Dabei wer-den in kurzen Abständen Bilder von einer, auf dem System angebrachten, Kamera aufge-nommen, welche dann einer Kantenanalyse unterzogen werden. Anhand der erkannten Kan-ten, kann ein Schild, welches ein spezielles Muster trägt, vom System geortet werden. Das System verfügt über drei Steuerungsmodi: der direkten Steuerung per Controller, der automa-tisierten Steuerung bei schrittweiser Fahrt, hierbei stoppt das System in bestimmten Abstän-den für eine bestimmte Zeit und die automatisierte Steuerung ohne Stopps. Die abschließen-den Testfahrten wurden mit einer Logitech C270 Webcam durchgeführt. Dabei ergab sich mit der C270 eine maximale Abweichung von 3,8 cm auf 10 Meter Teststrecke. Das System kann als genau und zuverlässig betrachtet werden. KW - Autonomer Messroboter KW - Zerstörungsfreie Prüfung KW - Stahlbeton PY - 2016 SP - 1 CY - Berlin AN - OPUS4-37696 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wilzeck, René T1 - Methodenentwicklung zur akustischen Detektion von Delaminationen in Stahlbeton N2 - Die vorliegende Arbeit beschäftigt sich mit der Methodenentwicklung eines automatischen Messverfahrens zur akustischen Detektion von Delaminationen in Stahlbeton. Ziel war das Konstruieren einer Messeinheit, welche mittels eines Zahnrads kontinuierlich auf eine Stahlbetonoberfläche klopft und den somit einstehenden Körperschall mit einem Richtmikrofon aufnimmt. Somit können Rückschlüsse über den Zustand des Betons getroffen werden. Das Grundkonzept bildet die Frequenzbandanalyse von Audioaufnahmen mittels einer gefensterten Schnellen Fourier Transformation. Ein auftragen des Frequenzbands über die gefahrene Strecke bietet die exakte Positionierung einer Fehlstelle. Für die Validierung der Methodengenauigkeit entstand ein Betonprobekörper mit eingebrachten Fehlstellen, welche unter mechanischer Anregung durch das Zahnrad ähnlich dumpfe Töne wie eine reale Delamination erzeugen. Die Ergebnisse der Tonanalyse zeigen eindeutige Frequenzänderungen beim Übergang von einem intakten zu einen fehlerhaften Bereich. Im Bauwesen angesiedelt, ist die vorliegende Arbeit besonders für LeserInnen aus dem Bereich der Zerstörungsfreie Schadensdiagnose interessant. KW - Resonanzverfahren KW - Stahlbeton KW - Delaminationen PY - 2016 SP - 1 CY - Berlin AN - OPUS4-37697 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Embedded RFID-sensors for concrete bridge structures N2 - In the near future, it will be important to adopt innovative approaches and technologies in order to further guarantee the reliability and availability of the highway network. New tools are therefore needed in order to obtain in-depth information about the condition of bridges and its development early enough before significant, precarious damage cases occur. In 2011, the research program “Intelligente Brücken (Smart Bridges)” was launched by the BASt together with the BMVI to evolve systems for information and holistic evaluation for Bridge structures as a supplement to the current inspection-based maintenance management. Several projects dealt with the topic in the last few years and provided guidelines and a solid basis to move towards a first implementation considering the input of all research projects carried out so far. T2 - International Symposium Non-Destructive Testing in Civil Engineering CY - Berlin, Germany DA - 15.09.2015 KW - RFID based sensors KW - Embedded sensors KW - Structural health monitoring KW - Concrete condition monitoring PY - 2015 AN - OPUS4-37626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej A1 - Strangfeld, Christoph A1 - Müller, Maximilian A1 - Bartholmai, Matthias ED - Aulova, Alexandra ED - Rogelj Ritonja, Alenka ED - Emri, Igor T1 - RFID sensor systems embedded in concrete - requirements for long-term operation N2 - One of the more difficult tasks for structural health monitoring is the continuous evaluation of the stability and load capacity of the building materials. This knowledge can be won, e.g., by taking material samples at the examining place with the drawback of partly destroying the structure. To avoid this, modern sensor and communication technologies offer promising methods for non-destructive testing. To address the tasks for monitoring of concrete structures, in the presented study, different sensors were combined with RFID transponders and embedded in concrete components. T2 - 33rd Danubia - Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Structure health monitoring KW - Concrete KW - Embedded KW - RFID sensors PY - 2016 SN - 978-961-94081-0-0 SP - 68 EP - 69 CY - Ljubljana AN - OPUS4-37535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej T1 - RFID sensor systems embedded in concrete - requirements for long-term operation N2 - One of the more difficult tasks for structural health monitoring is the continuous evaluation of the stability and load capacity of the building materials. This knowledge can be won, e.g., by taking material samples at the examining place with the drawback of partly destroying the structure. To avoid this, modern sensor and communication technologies offer promising methods for non-destructive testing. To address the tasks for monitoring of concrete structures, in the presented study, different sensors were combined with RFID transponders and embedded in concrete components. T2 - 33rd Danubia- Adria Symposium on Advances in Experimental Mechanics CY - Portorož, Slovenia DA - 20.09.2016 KW - Concrete KW - Embedded KW - RFID sensors KW - Structure health monitoring PY - 2016 AN - OPUS4-37533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Borges de Oliveira, F. A1 - Reuter, T. A1 - Plotzki, David A1 - Wohlgemuth, F. A1 - Bartscher, M. A1 - Bellon, Carsten A1 - Kasperl, S. T1 - Assessment of 2D-based tests for the qualification of simulation software for dXCT N2 - The interest in using computer simulations of dimensional x-ray computed tomography (dXCT) for various metrological purposes—such as measurement planning, performance prediction, performance optimisation and, finally, measurement uncertainty estimation—is increasing along with the ever-growing demand for more reliable measurements with dXCT. However, before a piece of simulation software can be used for tasks related to coordinate metrology, it has to be ensured that it is able to simulate physical laws, characteristic effects and basic CT system functionalities correctly and with sufficient accuracy. In short, the software must be qualified for dimensional metrology tasks. As one part of such a qualification process, a method is presented here for determining conformity intervals of 2D tests (projection-based tests) based on 3D tests (testing based on dimensional evaluations in a reconstructed volume) for the assessment of dXCT simulation software. The method consists of varying relevant parameter values in order to verify their influence on 3D measurement results. The results of the 3D tests with varied parameter values are then transferred to the quantities tested in the 2D tests and used as the basis for determining conformity intervals. Two approaches are applied for determining whether or not a variation of a parameter value is significant: (a) statistical and (b) heuristic. Two examples are presented, each based on simulated images, which show the application of the two different approaches for determining conformity intervals for the results of the 2D tests. KW - dXCT KW - X-ray computed tomography KW - Simulation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573316 DO - https://doi.org/10.1088/1361-6501/acc1f9 VL - 34 IS - 6 SP - 1 EP - 12 PB - IOP Publishing AN - OPUS4-57331 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kjaervik, Marit A1 - Ramstedt, M. A1 - Schwibbert, Karin A1 - Dietrich, P. M A1 - Unger, Wolfgang T1 - Comparative Study of NAP-XPS and Cryo-XPS for the Investigation of Surface Chemistry of the Bacterial Cell-Envelope N2 - Bacteria generally interact with the environment via processes involving their cell-envelope. Thus, techniques that may shed light on their surface chemistry are attractive tools for providing an understanding of bacterial interactions. One of these tools is Al Kα-excited photoelectron spectroscopy (XPS) with its estimated information depth of <10 nm. XPS-analyses of bacteria have been performed for several decades on freeze-dried specimens in order to be compatible with the vacuum in the analysis chamber of the spectrometer. A limitation of these studies has been that the freeze-drying method may collapse cell structure as well as introduce surface contaminants. However, recent developments in XPS allow for analysis of biological samples at near ambient pressure (NAP-XPS) or as frozen hydrated specimens (cryo-XPS) in vacuum. In this work, we have analyzed bacterial samples from a reference strain of the Gram-negative bacterium Pseudomonas fluorescens using both techniques. We compare the results obtained and, in general, observe good agreement between the two techniques. Furthermore, we discuss advantages and disadvantages with the two analysis approaches and the output data they provide. XPS reference data from the bacterial strain are provided, and we propose that planktonic cells of this strain (DSM 50090) are used as a reference material for surface chemical analysis of bacterial systems. KW - P. Fluorescens KW - Cryo XPS KW - NAP-XPS KW - DSM 5009 PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525640 DO - https://doi.org/10.3389/fchem.2021.666161 VL - 9 SP - Article 666161 PB - Frontiers CY - Switzerland AN - OPUS4-52564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Binder, F. A1 - Bellon, Carsten A1 - Wohlgemuth, F. A1 - Hausotte, T. T1 - Ein praxisnaher Leitfaden für computertomografische Untersuchungen mit der radiografischen Simulationsumgebung aRTist N2 - Radiografische Simulationswerkzeuge wie aRTist, ScorpiusXLab, SimCT oder CIVA CT verwenden analytische Methoden und physikalische Monte-Carlo-Teilchentransportsimulationen, um die Interaktionsprozesse zwischen Röntgenstrahlung und Materie zu simulieren. Die berechneten Projektionen bilden anschließend unter Berücksichtigung einer definierten Scan-Trajektorie die Basis der Simulation einer röntgencomputertomografischen Untersuchung. Für den erfolgreichen Einsatz der Computertomografie, sei es als zerstörungsfreie Prüfmethode oder beim dimensionellen Messen, ist es generell notwendig, bekannte Fehler- bzw. Abweichungsquellen des Messverfahrens auszuschließen oder zu reduzieren. Dabei hat sich gezeigt, dass die Auswahl der Messparameter und die Erfahrung des Anwenders direkten Einfluss auf das erzielbare Messergebnis einer computertomografischen Untersuchung nehmen. Es ist daher sinnvoll, die Parameterauswahl in einem virtuellen Simulationsaufbau vorher zu erproben und an die Messaufgabe anzupassen. Neben der Optimierung von Messparametern finden radiografische Simulationswerkzeuge auch Anwendung für Machbarkeitsstudien und werden zur Schulung von Anwendern im Bereich der Röntgen-Computertomografie verwendet. Radiografische Simulationswerkzeuge befinden sich in einem stetigen Wandel, beispielsweise durch die Entwicklung neuer Rekonstruktionsmethoden, durch Erweiterung von analytischen Modellen, durch Integration komplexer Trajektorien oder durch Berücksichtigung von prozessbedingten geometrischen Abweichungen. Im laufenden EMPIR-Projekt „AdvanCT“ entsteht deshalb ein „Good Practice Guide“ für die Simulationsumgebung aRTist. Ziel dieses Guides ist es, die mit steigender Komplexität verbundenen Einstiegshürden für Anwender von aRTist zu reduzieren, um damit einen praxisnahen Zugang zur virtuellen Computertomografie zu ermöglichen. Dabei werden anhand von praktisch nachvollziehbaren Beispielen die grundlegenden Mechanismen der Simulationsumgebung erklärt und ein strukturierter Leitfaden zur Simulation röntgencomputertomografischer Untersuchungen mit aRTist vermittelt. In diesem Beitrag werden erste Auszüge des Guides sowie eine Übersicht der weiteren geplanten Themen für die anschließende Diskussion vorgestellt. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Computertomografie KW - Simulation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530476 UR - https://jahrestagung.dgzfp.de/portals/jt2021/bb176/inhalt/poster.htm SN - 978-3-947971-18-3 VL - 176 SP - 1 EP - 9 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-53047 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten A1 - Jaenisch, Gerd-Rüdiger A1 - Deresch, Andreas T1 - Combining analytical and Monte Carlo modelling for industrial radiology N2 - Modelling becomes more and more important in modern NDE. It is increasingly used to optimize techniques for complex applications, to support the preparation of written procedures, and for education purposes. To describe the complete chain of RT, the model includes simulating all necessary properties of X- or Gamma-ray sources, the interaction of photons with material with special attention to scattered radiation, the detection process, and the complete geometrical RT setup handling arbitrary parts or constructions. Depending on the given inspection problem and the influencing factors that should be addressed by the simulation, an appropriate physical model has to be chosen to describe the underlying interaction mechanisms. The simulator aRTist combines analytical and Monte Carlo methods to efficiently model the radiation transport such that transmission as well as scatter techniques can be modelled. In this contribution we Focus on Monte Carlo Simulation of scatter contribution within aRTist. Examples for RT/tomographic applications and back-scatter techniques are presented to demonstrate the usability of the presented simulation tool for a broad range of radiological applications. T2 - 19th Wolrd Conference on Nondestructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Radiography KW - Computed tomography KW - Simulation KW - Monte Carlo methods PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-365856 SN - 978-3-940283-78-8 VL - 158 SP - 1 EP - 9 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung (DGZfP) CY - Berlin, Germany AN - OPUS4-36585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lukowiak, M.C. A1 - Wettmarshausen, Sascha A1 - Hidde, Gundula A1 - Landsberger, Petra A1 - Boenke, Viola A1 - Rodenacker, K. A1 - Braun, Ulrike A1 - Friedrich, Jörg Florian A1 - Gorbushina, Anna A1 - Haag, R. T1 - Polyglycerol coated polypropylene surfaces for protein and bacteria resistance N2 - Polyglycerol (PG) coated polypropylene (PP) films were synthesized in a two-step approach that involved plasma bromination and subsequently grafting hyperbranched polyglycerols with very few amino functionalities. The influence of different molecular weights and density of reactive linkers were investigated for the grafted PGs. Longer bromination times and higher amounts of linkers on the surface afforded long-term stability. The protein adsorption and bacteria attachment of the PP-PG films were studied. Their extremely low amine content proved to be beneficial for preventing bacteria attachment. PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-325406 DO - https://doi.org/10.1039/c4py01375a SN - 1759-9954 SN - 1759-9962 VL - 6 IS - 8 SP - 1350 EP - 1359 AN - OPUS4-32540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Noack-Schönmann, Steffi A1 - Bus, T. A1 - Banasiak, Ronald A1 - Knabe, Nicole A1 - Broughton, William J. A1 - Dulk-Ras, H.D. A1 - Hooykaas, P.J.J. A1 - Gorbushina, Anna T1 - Genetic transformation of Knufia petricola A95 - a model organism for biofilm-material interactions N2 - We established a protoplast-based system to transfer DNA to Knufia petricola strain A95, a melanised rock-inhabiting microcolonial fungus that is also a component of a model sub-aerial biofilm (SAB) system. To test whether the desiccation resistant, highly melanised cell walls would hinder protoplast formation, we treated a melanin-minus mutant of A95 as well as the type-strain with a variety of cell-degrading enzymes. Of the different enzymes tested, lysing enzymes from Trichoderma harzianum were most effective in producing protoplasts. This mixture was equally effective on the melanin-minus mutant and the type-strain. Protoplasts produced using lysing enzymes were mixed with polyethyleneglycol (PEG) and plasmid pCB1004 which contains the hygromycin B (HmB) phosphotransferase (hph) gene under the control of the Aspergillus nidulans trpC. Integration and expression of hph into the A95 genome conferred hygromycin resistance upon the transformants. Two weeks after plating out on selective agar containing HmB, the protoplasts developed cell-walls and formed colonies. Transformation frequencies were in the range 36 to 87 transformants per 10 µg of vector DNA and 106 protoplasts. Stability of transformation was confirmed by sub-culturing the putative transformants on selective agar containing HmB as well as by PCR-detection of the hph gene in the colonies. The hph gene was stably integrated as shown by five subsequent passages with and without selection pressure. KW - DNA transfer KW - Fungal cell-walls KW - Protoplasts KW - Hygromycin resistance KW - Black yeast KW - Sub-aerial biofilms KW - Stress-protective morphology KW - Ancestor of opportunistic pathogens & lichens PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-320840 UR - http://www.amb-express.com/content/4/1/80 DO - https://doi.org/10.1186/s13568-014-0080-5 SN - 2191-0855 VL - 4 SP - 80, 1 EP - 6 PB - Springer CY - Heidelberg AN - OPUS4-32084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silveira, A. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Longo, E. A1 - Greving, I. A1 - Lasch, P. A1 - Shahar, R A1 - Zaslansky, P. T1 - Water flow through bone: Neutron tomography reveals differences in water permeability between osteocytic and anosteocytic bone material N2 - Vertebrate bones are made of a nanocomposite consisting of water, mineral and organics. Water helps bone material withstand mechanical stress and participates in sensation of external loads. Water diffusion across vertebrae of medaka (bone material lacking osteocytes) and zebrafish (bone material containing osteocytes) was compared using neutron tomography. Samples were measured both wet and following immersion in deuterated-water (D2O). By quantifying H+ exchange and mutual alignment with X-ray lCT scans, the amount of water expelled from complete vertebra was determined. The findings revealed that anosteocytic bone material is almost twice as amenable to D2O diffusion and H2O exchange, and that unexpectedly, far more water is retained in osteocytic zebrafish bone. Diffusion in osteocytic bones (only 33 % – 39 % water expelled) is therefore restricted as compared to anosteocytic bone (~ 60 % of water expelled), presumably because water flow is confined to the lacunar-canalicular network (LCN) open-pore system. Histology and Raman spectroscopy showed that anosteocytic bone contains less proteoglycans than osteocytic bone. These findings identify a previously unknown functional difference between the two bone materials. Therefore, this study proposes that osteocytic bone retains water, aided by non-collagenous proteins, which contribute to its poroelastic mechano-transduction of water flow confined inside the LCN porosity. KW - Bone porosity KW - Anosteocytic bone KW - Water permeability KW - Neutron tomography KW - Proteoglycans PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564563 DO - https://doi.org/10.1016/j.matdes.2022.111275 VL - 224 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-56456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Strangfeld, Christoph T1 - RFID sensor systems embedded in concrete – systematical investigation of the transmission characteristics N2 - Long-term completely embedded sensor systems offer innovative possibilities for structural health Monitoring of concrete structures. Measuring of relevant parameters, e.g., temperature, humidity, or indication of corrosion can be performed with low energy sensors. This allows to implement passive RFID sensor systems without cable connection and battery, which are power supplied exclusively by the electromagnetic field from the external Reader device. To evaluate characteristics and conditions of this concept, a systematical Investigation of the transmission characteristics with variation of relevant parameters, as communication frequency, installation depth, type of concrete, moisture content, etc. is currently carried out in an interdisciplinary research project at BAM. First results are presented in this paper. T2 - 8th European Workshop On Structural Health Monitoring CY - Bilbao, Spain DA - 05.07.2016 KW - Embedded sensor KW - Energy harvesting KW - Wireless sensors KW - RFID sensors KW - Transmission characteristics KW - Structural health monitoring PY - 2016 AN - OPUS4-37130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture testing and mapping N2 - Presentation of the Non-destructive testing and evaluation advanced training workshop of division 8.2 regarding moisture measurements. T2 - NDT&E Advanced Training Workshop CY - Berlin, Germany DA - 21.06.2023 KW - Material moisture KW - Moisture transport KW - Building materials KW - Concrete KW - Moisture measurement techniques PY - 2023 AN - OPUS4-57799 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ladu, Luana T1 - Exploring the digital transformative potential of the conformity assessment industry - An international comparison N2 - First insights from a survey conducted among Conformity Assessment Bodies (CABs) accross 15 countries. It aims at exploring their status of digital transformation, incl. their digital maturity, benefits and obstacles as well as actual technology trends. T2 - EU - SPRI 2023 CY - Brighton, UK DA - 15.06.2023 KW - Digitaler Reifegrad KW - Digitalisierung KW - Zertifizierungsstellen KW - Konformitätsbewertung KW - Prüflaboratorien KW - Qualitätsinfrastruktur PY - 2023 AN - OPUS4-57780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kardjilov, N A1 - Manke, I A1 - Hilger, A A1 - Arlt, T A1 - Bradbury, R A1 - Markötter, Henning A1 - Woracek, R A1 - Strobel, M A1 - Treimer, W A1 - Banhart, J T1 - The Neutron Imaging Instrument CONRAD — Post‐Operational Review N2 - The neutron imaging instrument CONRAD was operated as a part of the user program of the research reactor BER‐II at Helmholtz‐Zentrum Berlin (HZB) from 2005 to 2020. The Instrument was designed to use the neutron flux from the cold source of the reactor, transported by a curved neutron guide. The pure cold neutron spectrum provided a great advantage in the use of different neutron optical components such as focusing lenses and guides, solid‐state polarizers, Monochromators and phase gratings. The flexible setup of the instrument allowed for implementation of new methods including wavelength‐selective, dark‐field, phase‐contrast and imaging with polarized neutrons. In summary, these developments helped to attract a large number of scientists and industrial customers, who were introduced to neutron imaging and subsequently contributed to the Expansion of the neutron imaging community. KW - Neutron imaging KW - Neutron scattering KW - Neutron instrument KW - Tomography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534190 DO - https://doi.org/10.3390/ jimaging7010011 VL - 7 IS - 11 SP - 7010011 PB - MDPI AN - OPUS4-53419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zimmek, David T1 - Entwicklung von Fluoreszenzspektroskopischer Sensorik zur pH-Wert Bestimmung in Baustoffen N2 - Das Projekt befasst sich mit einem neuen Ansatz, den pH-Wert im Beton zu bestimmen. Der pH-Wert ist vor allem für Stahlbeton-Bauwerke von Bedeutung, da dieser maßgeblich die Korrosion des Stahls beeinflusst. Im frischen Beton liegt der pH-Wert im basischen Bereich. Der Stahl ist in diesem Bereich passiviert, also vor schädlicher Korrosion geschützt. Durch die sogenannte Karbonatisierung sinkt der pH-Wert und die Korrosionswahrscheinlichkeit steigt deutlich an. Die Stabilität von Bauwerken in denen Stahlbeton verbaut ist, wird durch diese Korrosion langfristig beeinträchtigt. Allein in deutscher Infrastruktur rechnet man mit circa 5 Milliarden Euro Schaden jährlich. Die entwickelte Methode verwendet Sonden, welche die Korrosion Monitoren sollen. Im Sondeninneren befindet sich eine Schicht pH-Indikator (Thymolblau) und eine Schicht mit Quantenpunkten. Die Quantenpunkte fluoreszieren, nach Anregung durch zum Beispiel einen Laser, bei circa 440 nm (blau) beziehungsweise 610 nm (gelb-orange). Das Thymolblau ist im basischen Milieu (pH > 9,6) blau, im neutralen Milieu (um pH 7) gelb-orange. Der Indikator wirkt wie ein Farbfilter und lässt, je nach pH-Wert, unterschiedliche Wellenlängen zur Glasfaser durch. Aus der gemessenen Intensität bei 440 nm und 610 nm kann ein Verhältnis ermittelt werden. Dieses Verhältnis lässt erkennen, welchen pH-Wert das Milieu besitzt, in dem sich die Sonde befindet. Die entwickelte Methodik ist zerstörungsfrei, das heißt kein Material muss aus den Bauwerken entnommen werden. Vielmehr sollen die Sonden beim Betonieren in das Bauwerk eingebettet werden. Über Glasfasern können die Sonden jederzeit angesprochen werden. Dies ermöglicht permanentes pH-Monitoring, was die Früherkennung von Korrosionsgefahr verbessert und die Sanierungskosten verringert. T2 - Simulation in den Umwelt- und Geowissenschaften 2019 CY - Kassel, Germany DA - 08.05.2019 KW - pH-Monitoring KW - Korrosion KW - Stahlbeton KW - Quantenpunkte KW - Thymolblau PY - 2019 AN - OPUS4-47993 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brierley, N. A1 - Bellon, Carsten A1 - Lazaro Toralles, B. T1 - Optimized multi-shot imaging inspection design N2 - The inspection of complex-shaped components, such as those enabled by additive manufacturing, is a major challenge in industrial quality assurance. A frequently adopted approach to volumetric non-destructive evaluation is X-ray computed tomography, but this has major drawbacks. Two-dimensional radiography can overcome some of these problems, but does not generally provide an inspection that is as capable. Moreover, designing a detailed inspection for a complex-shaped component is a labour-intensive task, requiring significant expert input. In response, a computational framework for optimizing the data acquisition for an image-based inspection modality has been devised. The initial objective is to advance the capabilities of radiography, but the algorithm is, in principle, also applicable to alternative types of imaging. The algorithm exploits available prior information about the inspection and simulations of the inspection modality to allow the Determination of the optimal inspection configuration, including specifically component poses with respect to the imaging system. As an intermediate output, spatial maps of inspection performance are computed, for understanding spatially varying limits of detection. Key areas of innovation concern the defect detectability evaluation for arbitrarily complex indications and the creation of an application-specific optimization algorithm. Initial trials of the algorithm are presented, with good results. KW - Inspection design and planning KW - Optimization KW - Radiography KW - Simulation PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-458363 DO - https://doi.org/10.1098/rspa.2017.0319 SN - 1471-2946 SN - 1364-5021 VL - 474 IS - 2216 SP - 70319, 1 EP - 25 PB - The Royal Society CY - London AN - OPUS4-45836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illemann, J. A1 - Meinel, Dietmar A1 - Bellon, Carsten T1 - Effektive Bestimmung der Fokusparameter von Mikrofokus-Röntgenquellen N2 - Mikrofokus-Röntgenquellen werden in der industriellen CT flexibelverwendet, um mit kleiner Leistung hohe Auflösung zu erzielen oder mit verminderter Auflösung bei höherer Leistung kürzere Messzeiten zu erreichen. Insbesondere Quellen in offener Bauweise benötigen Wartung wie Filamentwechsel und Nachstellen der Fokusparameter. Ziel ist es, einen optimal kleinen Quellfleck bei bekannter Spannung einzustellen und dessen Größe zu bestimmen. Zur Überprüfung der Quellfleckgröße sind bereits Verfahren unter Verwendung lithographisch hergestellter Masken mit Strichmustern oder Siemenssternen aus Mikrometer dünnen Schichten aus stark absorbierendem Material wie z.B. Gold bekannt. Diese erfordern wegen der geringen Absorption eine lange Messzeit und sind nur kostenintensiv herzustellen. Ihre Verwendung zur regelmäßigen Qualitätsüberprüfung von CT-Anlagen ist daher nicht verbreitet. Ziel dieser Arbeit ist es, die richtungsabhängige Quellfleckgröße absolut zu bestimmen, wobei nur einfach zu beschaffende Wolframspitzen verwendet werden. Dazu werden radiographische Bilder in hoher Vergrößerung aufgenommen und die Grauwertverteilung parametrisiert. Unter Verwendung der Kenntnis von Targetmaterial und Spannung wird eine eineindeutige Zuordnung zur Quellfleckgröße vorgenommen. Dieses erfordert eine extensive Simulation für verschiedene Spannungen, Fokusgrößen und andere Einflussgrößen, sowie die experimentelle Verifikation an verschiedenen CT-Anlagen im Vergleich zu einer bekannten Methode. Erste Ergebnisse werden vorgestellt und die praktische Implementierung unter Angabe der Einschränkungen der Verwendbarkeit diskutiert. Die Autoren hoffen, damit einen wesentlichen Beitrag zur Verbesserung der Qualitätssicherung und zur Arbeitseffizienz in der Mikrocomputertomographie leisten zu können. T2 - DGZfP DACH-Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Mikro-Computertomographie KW - Röntgenröhre KW - Quellfleckgröße KW - Brennfleck PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485960 UR - https://www.ndt.net/search/docs.php3?id=24551 UR - https://www.ndt.net/article/dgzfp2019/papers/Mi.2.A.3.pdf IS - NDT.net Issue: 2019-08 SP - 1 EP - 13 AN - OPUS4-48596 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaenisch, Gerd-Rüdiger A1 - Kolkoori, Sanjeevareddy A1 - Bellon, Carsten T1 - Quantitative simulation of back scatter X-ray imaging and comparison to experiments N2 - X-ray backscatter imaging is a well established NDT technique to inspect complex objects using only a single-sided access. In difference to conventional transmission X-ray radiography, the X-ray backscatter imaging utilizes the scattered radiation caused by the Compton scattering effect. In order to achieve high backscatter intensities from a test object, it is necessary to optimize the backscatter system parameters namely the angle between source and slit camera, the slit collimator system, the shielding between source and scatter camera, and the type of detector. In addition, the scatter phenomena in to the investigated object need to be understood. In this contribution, we present a Monte Carlo model McRay which considers all relevant single and multiple interactions of photons and electrons. This model can be used to simulate back scatter techniques. It allows not only calculating the scatter image for a given experimental setup but also registering the spectrum of the detected scattered photons. Both aspects are important to understand the imaging process, to interpret the results, and to optimize the backscatter camera investigated here. Additionally experimental results will be presented and compared with simulations. T2 - 19th World Conference on Nondestructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Radiology KW - Back-scatter techniques KW - Simulation KW - Monte Carlo methods KW - Measurements PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-365897 SN - 978-3-940283-78-8 VL - 158 SP - 1 EP - 11 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung (DGZfP) CY - Berlin, Germany AN - OPUS4-36589 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Deresch, Andreas A1 - Jaenisch, Gerd-Rüdiger A1 - Bellon, Carsten T1 - A fast general spectrum model for quantitative radiography simulation N2 - One essential step on the way towards accurate quantitative simulation of radiographic testing is an accurate description of the utilized energy spectrum of X-ray photons. For use in general purpose simulation tools, the spectra of X-ray tubes have to be described by a model covering at least the intended range of applications. This range includes transmission tubes as well as direct beam tubes with varying angles of incidence and emission, for a number of typical target materials. In radiographic testing acceleration voltages frequently reach up to 450 kV for direct beam targets and up to 225 kV for transmission targets, with even higher voltages available or being developed. Currently used models are unable to cover the whole range of configurations. Here a model is presented that employs a unified approach for simulating the photon energy spectra for transmission and direct beam targets composed of arbi-trary homogeneous materials. In order to achieve this, a detailed model of electron transport within the target is employed. The validity of the developed model is shown through comparisons with Monte Carlo simulations as well as measurements for a number of different configurations. T2 - 19th World Conference on Nondestructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Measurements KW - X-ray spectra KW - Simulation KW - Electron transport PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-365959 SN - 978-3-940283-78-8 VL - 158 SP - 1 EP - 7 PB - DGZfP CY - Berlin, Germany AN - OPUS4-36595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Breitenbach, Romy A1 - Silbernagl, Dorothee A1 - Toepel, J. A1 - Sturm, Heinz A1 - Broughton, William J. A1 - Sassaki, G. L. A1 - Gorbushina, Anna T1 - Corrosive extracellular polysaccharides of the rock-inhabiting model fungus Knufia petricola N2 - Melanised cell walls and extracellular polymeric matrices protect rock-inhabiting microcolonial fungi from hostile environmental conditions. How extracellular polymeric substances (EPS) perform this protective role was investigated by following development of the model microcolonial black fungus Knufia petricola A95 grown as a sub-aerial biofilm. Extracellular substances were extracted with NaOH/formaldehyde and the structures of two excreted polymers studied by methylation as well as NMR analyses. The main polysaccharide (~ 80%) was pullulan, also known as α-1,4-; α-1,6-glucan, with different degrees of polymerisation. Αlpha-(1,4)-linked-Glcp and α-(1,6)-linked-Glcp were present in the molar ratios of 2:1. A branched galactofuromannan with an α-(1,2)-linked Manp main chain and a β-(1,6)-linked Galf side chain formed a minor fraction (~ 20%). To further understand the roles of EPS in the weathering of minerals and rocks, viscosity along with corrosive properties were studied using atomic force microscopy (AFM). The kinetic viscosity of extracellular K. petricola A95 polysaccharides (≈ 0.97 × 10-6 m2 s-1) ranged from the equivalent of 2% (w/v) to 5% glycerine, and could thus profoundly affect diffusion-dominated processes. The corrosive nature of rock-inhabiting fungal EPS was also demonstrated by its effects on the aluminium coating of the AFM cantilever and the silicon layer below. KW - Corrosion KW - EPS KW - Melanised microcolonial fungi (MCF) KW - Pullulan KW - Sub-aerial biofilms (SAB) KW - α-1,4- and α-1,6-glucans KW - AFM cantilever vibration KW - Nanoviscosity KW - Nanocorrosion of aluminium and silicon PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435910 DO - https://doi.org/10.1007/s00792-017-0984-5 SN - 1433-4909 SN - 1431-0651 VL - 22 IS - 2 SP - 165 EP - 175 PB - Springer CY - Berlin AN - OPUS4-43591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten A1 - Zhukovskiy, M. A1 - Markov, M. A1 - Podolyako, S. A1 - Uskov, R. A1 - Jaenisch, Gerd-Rüdiger T1 - Supercomputing the cascade processes of radiation transport N2 - Modeling of the photon-electron cascade progress in multicomponent objects of complex geometrical structure by use of hybrid supercomputers is considered. An approach to computing the cascade processes is developed. The approach has three key properties allowing the effective use of heterogeneous structure of computers for solving the tasks of radiation transport in complex multi-scale geometries. Firstly, two different discreet geometrical description of an object being under radiation is used: triangulated model for photon transport and voxel model for electron transport. Secondly, small parameter of the problem is explicitly taking into account for modeling surface effects (for instance, electron emission). Thirdly, the effective calculation decomposition between CPU and GPU is developed for significant increasing the speed of calculations of processes in question. Modeling of experiment on researching the bremsstrahlung generated by electron beam in Ta target is carried out. Comparison of computing and experimental results shows satisfactory consent. T2 - 19th World Conference on Nondestructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Super somputing KW - Photon-electron transport KW - Monte Carlo methods KW - Modelling PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-365932 SN - 978-3-940283-78-8 VL - 158 SP - 1 EP - 6 PB - DGZfP CY - Berlin, Germany AN - OPUS4-36593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kjaervik, Marit A1 - Schwibbert, Karin A1 - Dietrich, P. A1 - Thissen, A. A1 - Unger, Wolfgang T1 - Surface characterisation of Escherichia coli under various conditions by near-ambient pressure XPS N2 - Bacteria are inherently in a hydrated state and therefore not compatible to ultra-high vacuum techniques such as XPS without prior sample preparation involving freeze drying or fast freezing. This has changed with the development of near-ambient pressure (NAP)-XPS, which makes it possible to characterise the bacterial surface with minimal sample preparation. This paper presents NAP-XPS measurements of Escherichia coli under various NAP conditions: at 11 mbar in a humid environment, at 2 mbar after drying in the chamber, pre-dried at 4 mbar, and at 1 mbar after overnight pumping at 10^−4 mbar. The high-resolution spectra of carbon, nitrogen, and oxygen are presented and found to be in general agreement with XPS measurements from freeze-dried and fast-frozen bacteria. However, it was found that the amount of carbon components associated with polysaccharides increases relative to aliphatic carbon during drying and increases further after overnight pumping. This implies that drying has an impact on the bacterial surface. T2 - European conference on applications of surface and interface analysis (ECASIA'17) CY - Montpellier, France DA - 24.09.2018 KW - Bacteria KW - E. coli KW - NAP-XPS PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-454047 DO - https://doi.org/10.1002/sia.6480 SN - 0142-2421 SN - 1096-9918 VL - 50 IS - 11 SP - 996 EP - 1000 PB - John Wiley & Sons CY - Hoboken, New Jersey, USA AN - OPUS4-45404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tengattini, A A1 - Kardjilov, N A1 - Helfen, L A1 - Douissard, P A A1 - Lenoir, N A1 - Markötter, Henning A1 - Hilger, A A1 - Arlt, T A1 - Paulisch, M A1 - Turek, T A1 - Manke, Ingo T1 - Compact and versatile neutron imaging detector with sub-4μm spatial resolution based on a single-crystal thin-film scintillator N2 - A large and increasing number of scientific domains pushes for high neutron imaging resolution achieved in reasonable times. Here we present the principle, design and performance of a detector based on infinity corrected optics combined with a crystalline Gd3Ga5O12 : Eu scintillator, which provides an isotropic sub-4 μm true resolution. The exposure times are only of a few minutes per image. This is made possible also by the uniquely intense cold neutron flux available at the imaging beamline NeXT-Grenoble. These comparatively rapid acquisitions are compatible with multiple high quality tomographic acquisitions, opening new venues for in-operando testing, as briefly exemplified here. KW - Neutron imaging KW - Scintillator KW - Resolution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549836 DO - https://doi.org/10.1364/oe.448932 VL - 30 IS - 9 SP - 14461 EP - 14477 PB - Optica CY - Washington, DC AN - OPUS4-54983 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Binder, F. A1 - Bircher, B. A1 - Laquai, René A1 - Küng, A. A1 - Bellon, Carsten A1 - Meli, F. A1 - Deresch, A. A1 - Ulrich Neuschaefer-Rube, U. A1 - Hausotte, T. T1 - Methodologies for model parameterization of virtual CTs for measurement uncertainty estimation N2 - X-ray computed tomography (XCT) is a fast-growing technology for dimensional measurements in industrial applications. However, traceable and efficient methods to determine measurement uncertainties are not available. Guidelines like the VDI/VDE 2630 Part 2.1 suggest at least 20 repetitions of a specific measurement task, which is not feasible for industrial standards. Simulation-based approaches to determine task specific measurement uncertainties are promising, but require closely adjusted model parameters and an integration of error sources like geometrical deviations during a measurement. Unfortunately, the development of an automated process to parameterize and integrate geometrical deviations into XCT models is still an open issue. In this work, the whole processing chain of dimensional XCT measurements is taken into account with focus on the issues and requirements to determine suitable parameters of geometrical deviations. Starting off with baseline simulations of different XCT systems, two approaches are investigated to determine and integrate geometrical deviations of reference measurements. The first approach tries to iteratively estimate geometric deviation parameter values to match the characteristics of the missing error sources. The second approach estimates those values based on radiographs of a known calibrated reference object. In contrast to prior work both approaches only use a condensed set of parameters to map geometric deviations. In case of the iterative approach, some major issues regarding unhandled directional dependencies have been identified and discussed. Whereas the radiographic method resulted in task specific expanded measurements uncertainties below one micrometre even for bi-directional features, which is a step closer towards a true digital twin for uncertainty estimations in dimensional XCT. KW - Geometrical deviation KW - X-ray computed tomography KW - Uncertainty estimation KW - Virtual CT PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553263 DO - https://doi.org/10.1088/1361-6501/ac7b6a VL - 33 IS - 10 SP - 1 EP - 15 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-55326 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Falahat, A M A1 - Kardjilov, N A1 - Woracek, R A1 - Boin, M A1 - Markötter, Henning A1 - Kuhn, L T A1 - Makowska, M A1 - Strobl, M A1 - Pfretzschner, B A1 - Banhart, J A1 - Manke, I T1 - Temperature dependence in Bragg edge neutron transmission measurements N2 - A systematic study has been carried out to investigate the neutron transmission signal as a function of sample temperature. In particular, the experimentally determined wavelength-dependent neutron attenuation spectra for a martensitic steel at temperatures ranging from 21 to 700°C are compared with simulated data. A theoretical description that includes the Debye–Waller factor in order to describe the temperature influence on the neutron cross sections was implemented in the nxsPlotter software and used for the simulations. The analysis of the attenuation coefficients at varying temperatures shows that the missing contributions due to elastic and inelastic scattering can be clearly distinguished: while the elastically scattered intensities decrease with higher temperatures, the inelastically scattered intensities increase, and the two can be separated from each other by analysing unique sharp features in the form of Bragg edges. This study presents the first systematic approach to quantify this effect and can serve as a basis , for example, to correct measurements taken during in situ heat treatments, in many cases being a prerequisite for obtaining quantifiable results. KW - Neutron Bragg edge imaging KW - Debye–Waller factor KW - Temperature-dependent neutron transmission KW - Super martensitic stainless steel PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556896 DO - https://doi.org/10.1107/S1600576722006549 VL - 55 IS - Pt 4 SP - 919 EP - 928 PB - International Union of Crystallography AN - OPUS4-55689 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neuschaefer-Rube, U. A1 - Illemann, J. A1 - Sturm, M. A1 - Bircher, B. A1 - Meli, F. A1 - Bellon, Carsten A1 - Evsevleev, Sergei T1 - Validation of a fast and traceable radiographic scale calibration of dimensional computed tomography N2 - A fast and highly precise method of determining the geometrical scale factor of computed tomography (CT) measurements has been validated successfully by Bundesanstalt für Materialforschung und -prüfung (BAM), the Federal Institute of Metrology (METAS) and Physikalisch-Technische Bundesanstalt (PTB) within the scope of AdvanCT (Advanced Computed Tomography for dimensional and surface measurements in industry), a project funded in the European Metrology Programme for Innovation and Research (EMPIR). The method has been developed by PTB and requires only two radiographic images of a calibrated thin 2D standard (hole grid standard) from two opposite directions. The mean grid distance is determined from both radiographs. From this and with the help of the calibration result, the radiographic scale and therefore the voxel size is determined. The procedure takes only a few minutes and avoids a time-consuming CT scan. To validate the method, the voxel sizes determined via this method were compared with voxel sizes determined from CT scans of calibrated objects. Relative deviations between the voxel sizes in the range of 10−5 were achieved with minimal effort using cone-beam CT systems at moderate magnifications. KW - Dimensional metrology KW - Voxel size KW - Industrial CT KW - Geometrical magnification PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553271 DO - https://doi.org/10.1088/1361-6501/ac74a3 SN - 0957-0233 VL - 33 IS - 9 SP - 1 EP - 9 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-55327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bartholmai, Matthias A1 - Strangfeld, Christoph A1 - Van Bocxlaer, A. T1 - RFID-Sensor-Transponder in Beton N2 - Sensor-Transponder-Lösung der BAM ermöglicht automatisiertes Brückenmonitoring und Predictive Maintenance und detektiert Korrosion in Beton. KW - RFID-Sensorsysteme KW - Bauteilintegrierte Sensoren KW - Betonkorrosion KW - Structural health monitoring PY - 2017 SN - 1860-5907 VL - 2017 IS - 5 SP - 46 EP - 49 PB - Verlag & Freie Medien, Lüneburg CY - Lüneburg AN - OPUS4-40873 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Johann, Sergej T1 - RFID sensor systems embedded in concrete – validation experiments for long-term monitoring N2 - Structural Health Monitoring (SHM) is an important part of buildings surveillance and maintenance to detect material failure as early as possible and to contribute in protection of structures and their users. The implementation of Radio Frequency Identification (RFID) sensor systems without cable connection and battery into building components offers innovative possibilities to enable long-term in-situ SHM of addressed structures, bridges. The objectives of the presented study are complete embedding of RFID sensors systems in concrete, full passive communication with the systems, at best for the whole life span of structures. One challenge for this task is the highly alkaline environment in concrete, which requires non-degrading and robust encapsulation. Further Requirements are passive communication and energy supply, appropriate antenna design, placement and fixation in concrete, and the selection and implementation of sensors and connections. The concept is to develop and optimize a simple and robust system, which meets the requirements, as well as comprehensive validation in concrete specimen and real world applications. Two different systems were developed (HF and UHF RFID, respectively). First tasks were the implementation of analog sensors using the superposition principle for the signal adaption. Investigation of suitable materials for robust encapsulation and sensor protection against basic environments. Four materials were investigated in pH 13 solution for 14 days - 3D-Printer-Polymer was completely resolved - PVC has no noticeable decrease in weight - (VitaPro) glass filter for the sensor protector, has weight loss 2.7 % - The epoxy resin has increased by 1.8 % due to moisture expansion Different concrete samples were prepared for the validation of the systems. RFID sensors were embedded in different integration depths. Investigate the energy- and data transfer through concrete, also with varying moisture content. Additionally, signal strength data was used to optimize and validate the antenna characteristics in concrete. Next steps are to guarantee a sufficient energy supply for UHF RFID systems embedded in different concrete mixtures and further embedding the HF and UHF RFID systems in real bridges and buildings to validate the long term monitoring. T2 - DGZfP-Jahrestagung 2017 CY - Koblenz, Germany DA - 22.05.2017 KW - RFID sensors KW - Long-term requirements KW - Structural health monitoring KW - Passive RFID KW - Sensor requirements KW - Sensors in concrete KW - Smart structures PY - 2017 AN - OPUS4-40348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler T1 - In-situ analysis of water transport in concrete completed using X-ray computed tomography N2 - The water-transport characteristics of concrete have a major impact on its resistance to damaging chemical processes such as Alkali-Silica-Reaction (ASR). Water transport in samples of damaged and undamaged concrete was measured using in-situ CT. The resulting measurements of water-front movement relative to time and the change in 3D-moisture distribution within the samples, are needed for calibration and validation of water-transport numerical models. T2 - 3rd International Conference on Tomography of Materials and Structures CY - Lund, Sweden DA - 26.06.2017 KW - X-ray computed tomography (CT) KW - In situ KW - Water transport KW - Alkali-silica-reaction (ASR) PY - 2017 AN - OPUS4-40876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia ED - Jakobs, K. ED - Blind, K. T1 - Standardization in emerging technologies - The case of additive manufacturing N2 - Additive Manufacturing provides an important enabling technology for the digital transformation of the economy. As an emerging technology it has seen a remarkable development over the last three decades. Nevertheless, it is far from a broad adoption with several barriers to overcome yet. One of the major challenges is the lack of standards. The critical role of standardization for innovation is generally recognized, still the topic too often has been neglected in strategic roadmapping exercises for emerging technologies. Too little is known about the complex dynamics and interrelations of standardization and innovation. The anticipation of standardization needs and the timely and efficient implementation of standards is challenging. This paper aims at contributing to a better understanding of the role that standards play in the multi-dimensional system of innovation. It analyzes the trajectories of innovation in Additive Manufacturing in a systematic and holistic way, focusing on standardization activities with regard to coordination, stakeholders involved, the timing and types of standards developed. Putting standardization in context of the multi-dimensional innovation system of Additive Manufacturing the research shows where standards can support the diffusion of an emerging technology. T2 - 22nd EURAS Annual Standardisation Conference: Digitalisation: Challenge and Opportunity for Standardisation CY - Berlin, Germany DA - 28.06.2017 KW - Additive manufacturing KW - 3D Printing KW - Innovation KW - Emerging technologies KW - Standards PY - 2017 SN - 978-3-95886-172-5 VL - 2017 SP - T117 EP - T135 PB - Wissenschaftsverlag Mainz CY - Aachen ET - 1. AN - OPUS4-41020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture testing and mapping N2 - Eight different screed types are tested including two different sample heights of 35 and 70 mm. The moisture of the four cement based and four sulphate based screeds are monitored during hydration and evaporation. All samples are stored in a climatic chamber at 23° C and 50 % relative humidity. Embedded sensors like temperature arrays, humidity sensor arrays, and multi-ring electrodes are embedded in the samples to yield a detailed moisture evolution with high depth resolution. Furthermore, nuclear magnetic resonance is used to quantify the water content at different depths. This multi-sensor approach allows a comprehensive monitoring of the moisture and its gradient in the different screed samples. This yields a deeper insight into the hydration, moisture convection, and diffusion processes. T2 - 4. Autumn School - Moisture measurements in porous mineral materials CY - Karlsruhe, Germany DA - 18.09.2017 KW - Material moisture KW - Moisture measurements KW - Corresponding relative humidity KW - Sorption isotherme KW - Porous materials PY - 2017 AN - OPUS4-42096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Mishurova, Tatiana A1 - Khrapov, D. A1 - Paveleva, A. A1 - Meinel, Dietmar A1 - Surmenev, R. A1 - Surmeneva, M. A1 - Koptyug, A. A1 - Bruno, Giovanni T1 - X-ray Computed Tomography Procedures to Quantitatively Characterize the Morphological Features of Triply Periodic Minimal Surface Structures N2 - Additively manufactured (AM) metallic sheet-based Triply Periodic Minimal Surface Structures (TPMSS) meet several requirements in both bio-medical and engineering fields: Tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some challenges related to quality control, which can prevent their successful application. In fact, the optimization of the AM process is impossible without considering structural characteristics as manufacturing accuracy, internal defects, as well as surface topography and roughness. In this study, the quantitative non-destructive analysis of TPMSS manufactured from Ti-6Al-4V alloy by electron beam melting was performed by means of X-ray computed tomography (XCT). Several advanced image analysis workflows are presented to evaluate the effect of build orientation on wall thicknesses distribution, wall degradation, and surface roughness reduction due to the chemical etching of TPMSS. It is shown that the manufacturing accuracy differs for the structural elements printed parallel and orthogonal to the manufactured layers. Different strategies for chemical etching show different powder removal capabilities and both lead to the loss of material and hence the gradient of the wall thickness. This affects the mechanical performance under compression by reduction of the yield stress. The positive effect of the chemical etching is the reduction of the surface roughness, which can potentially improve the fatigue properties of the components. Finally, XCT was used to correlate the amount of retained powder with the pore size of the functionally graded TPMSS, which can further improve the manufacturing process. KW - Metamaterials KW - Functionally graded porous structure KW - Triply periodic minimal surface structures KW - Roughness analysis KW - Powder removal KW - Deep learning segmentation PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528142 DO - https://doi.org/10.3390/ma14113002 VL - 14 IS - 11 SP - 3002 PB - MDPI AN - OPUS4-52814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Magkos, Sotirios A1 - Kupsch, Andreas A1 - Bruno, Giovanni T1 - Suppression of Cone-Beam Artefacts with Direct Iterative Reconstruction Computed Tomography Trajectories (DIRECTT) N2 - The reconstruction of cone-beam computed tomography data using filtered back-projection algorithms unavoidably results in severe artefacts. We describe how the Direct Iterative Reconstruction of Computed Tomography Trajectories (DIRECTT) algorithm can be combined with a model of the artefacts for the reconstruction of such data. The implementation of DIRECTT results in reconstructed volumes of superior quality compared to the conventional algorithms. KW - DIRECTT KW - Iterative method KW - Signal processing KW - X-ray imaging KW - Computed tomography PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531085 DO - https://doi.org/10.3390/jimaging7080147 SN - 2313-433X) VL - 7 IS - 8 SP - 147 - 1 EP - 147 -9 PB - MDPI CY - Basel, Switzerland AN - OPUS4-53108 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruno, Giovanni T1 - Micro Non-Destructive Testing and Evaluation N2 - What is meant by ‘Micro Non-Destructive Testing and Evaluation’? This was the central subject of debate in this Special Issue. At present, sub-millimeter-size components or even assemblies are pervading the industrial and scientific world. Classic examples are electronic devices and watches (as well as parts thereof), but recent examples encompass additively manufactured lattice structures, stents, or other microparts. Moreover, most assemblies contain micro-components. Testing such components or their miniaturized parts would fit well within the topic of micro non-destructive testing and evaluation. In all cases, performance and integrity testing, quality control, and dimensional tolerances need to be measured at the sub-millimeter level (ideally with a spatial resolution of about a micron); most of the time, such features and components are embedded in much larger assemblies, which also need to be taken into account. The solution to this dilemma (i.e. measuring large parts with high resolution) depends on the part and on the problem under consideration. Another possible definition of micro non-destructive testing and evaluation can relate to the characterization of micro-features (e.g., the microstructure) in much larger specimens, such as damage in concrete cores or porosity in additively manufactured components. A further aspect is the use of microscopic probes to evaluate macroscopic properties. This is the case, for instance but not at all exclusively, in the use of diffraction techniques to determine macroscopic stress. The splits between testing and characterization at the micro-level (or of micro parts) from one side and handling of macroscopic assemblies on the other represent a great challenge for many fields of materials characterization. On top of that, including the use of microscopic methods to test integrity would add a further level of complexity. Imaging, mechanical testing, non-destructive testing, measurement of properties, structural health monitoring, and dimensional metrology all need to be re-defined if we want to cope with the multi-faceted topic of micro non-destructive testing and evaluation. The challenge has already been accepted by the scientific and engineering communities for a while but is still far from being universally tackled. This Special Issue yields an interesting answer to the questions posed above. It presents the progress made and the different aspects of the challenge as well as at indicates the paths for the future of NDT&E. KW - Ultrasound KW - Materials Characterization KW - Residual Stress KW - Thermography Computed KW - Tomography KW - Non-destructive Testing KW - Magnetic Methods PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556849 DO - https://doi.org/10.3390/ma15175923 VL - 15 IS - 17 SP - 1 EP - 3 PB - MDPI CY - Basel, Schweiz AN - OPUS4-55684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Alekseychuk, V. O. A1 - Kupsch, Andreas A1 - Plotzki, D. A1 - Bellon, Carsten A1 - Bruno, Giovanni T1 - Simulation-Assisted Augmentation of Missing Wedge and Region-of-Interest Computed Tomography Data N2 - This study reports a strategy to use sophisticated, realistic X-ray Computed Tomography (CT) simulations to reduce Missing Wedge (MW) and Region-of-Interest (RoI) artifacts in FBP (Filtered Back-Projection) reconstructions. A 3D model of the object is used to simulate the projections that include the missing information inside the MW and outside the RoI. Such information augments the experimental projections, thereby drastically improving the reconstruction results. An X-ray CT dataset of a selected object is modified to mimic various degrees of RoI and MW problems. The results are evaluated in comparison to a standard FBP reconstruction of the complete dataset. In all cases, the reconstruction quality is significantly improved. Small inclusions present in the scanned object are better localized and quantified. The proposed method has the potential to improve the results of any CT reconstruction algorithm. KW - Computed tomography KW - Missing wedge KW - Region of interest KW - Augmented data KW - CT simulation KW - aRTist PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-593799 UR - https://www.mdpi.com/2313-433X/10/1/11 DO - https://doi.org/10.3390/jimaging10010011 SN - 2313-433X VL - 10 IS - 1 SP - 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-59379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Fioresi, Rita A1 - Faglioni, Francesco A1 - Bruno, Giovanni T1 - A Complete Strategy to Achieve High Precision Automatic Segmentation of Challenging Experimental X‐Ray Computed Tomography Data Using Low‐Resemblance Synthetic Training Data N2 - It is shown that preconditioning of experimental X‐ray computed tomography (XCT) data is critical to achieve high‐precision segmentation scores. The challenging experimental XCT datasets and deep convolutional neural networks (DCNNs) are used that are trained with low‐resemblance synthetic XCT data. The material used is a 6‐phase Al–Si metal matrix composite‐reinforced with ceramic fibers and particles. To achieve generalization, in our past studies, specific data augmentation techniques were proposed for the synthetic XCT training data. In addition, two toolsets are devised: (1) special 3D DCNN architecture (3D Triple_UNet), slicing the experimental XCT data from multiple views (MultiView Forwarding), the i.S.Sy.Da.T.A. iterative segmentation algorithm, and (2) nonlocal means (NLM) conditioning (filtering) for the experimental XCT data. This results in good segmentation Dice scores across all phases compared to more standard approaches (i.e., standard UNet architecture, single view slicing, standard single training, and NLM conditioning). Herein, the NLM filter is replaced with the deep conditioning framework BAM SynthCOND introduced in a previous publication, which can be trained with synthetic XCT data. This leads to a significant segmentation precision increase for all phases. The proposed methods are potentially applicable to other materials and imaging techniques. KW - Automatic Segmentation KW - XCT KW - Artificial Intelligence KW - Synthetic Training Data KW - i.S.Sy.Da.T.A. KW - BAM SynthMAT KW - BAM SynthCOND KW - Triple UNet KW - Convolutional Neural Network (DCNN) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-590912 DO - https://doi.org/10.1002/adem.202301030 SN - 1438-1656 VL - 26 IS - 2 SP - 1 EP - 9 PB - Wiley online library AN - OPUS4-59091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oesch, Tyler A1 - Weise, Frank A1 - Bruno, Giovanni T1 - Detection and Quantification of Cracking in Concrete Aggregate through Virtual Data Fusion of X-ray Computed Tomography Images N2 - In this work, which is part of a larger research program, a framework called “virtual data fusion“ was developed to provide an automated and consistent crack detection method that allows for the cross-comparison of results from large quantities of X-ray Computed Tomography (CT) data. A partial implementation of this method in a custom program was developed for use in research focused on crack quantification in Alkali-Silica Reaction (ASR)-sensitive concrete aggregates. During the CT image processing, a series of image analyses tailored for detecting specific, individual crack-like characteristics were completed. The results of these analyses were then “fused” in order to identify crack-like objects within the images with much higher accuracy than that yielded by any individual image analysis procedure. The results of this strategy demonstrated the success of the program in effectively identifying crack-like structures and quantifying characteristics, such as surface area and volume. The results demonstrated that the source of aggregate has a very significant impact on the amount of internal cracking, even when the mineralogical characteristics remain very similar. River gravels, for instance, were found to contain significantly higher levels of internal cracking than quarried stone aggregates of the same mineralogical type. KW - X-ray Computed Tomography (CT) KW - Alkali-Silica Reaction (ASR) KW - Crack Detection KW - Damage Quantification KW - ASR-Sensitive Aggregate PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512170 DO - https://doi.org/10.3390/ma13183921 VL - 13 IS - 18 SP - Paper 3921 PB - MDPI CY - Basel, Switzerland AN - OPUS4-51217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Magkos, Sotirios A1 - Kupsch, Andreas A1 - Bruno, Giovanni T1 - Direct iterative reconstruction of computed tomography trajectories: Reconstruction from limited number of projections with DIRECTT N2 - X-ray computed tomography has many applications in materials science and non-destructive testing. While the standard filtered back-projection reconstruction of the radiographic data sets is fast and simple, it typically fails in returning accurate results from missing or inconsistent projections. Among the alternative techniques that have been proposed to handle such data is the Direct Iterative REconstruction of Computed Tomography Trajectories (DIRECTT) algorithm. We describe a new approach to the algorithm, which significantly decreases the computational time, while achieving a better reconstruction quality than that of other established algorithms. KW - Computed tomography KW - DIRECTT KW - Iterative reconstruction KW - Limited data PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514403 DO - https://doi.org/10.1063/5.0013111 SN - 0034-6748 VL - 91 IS - 10 SP - 103107-1 EP - 103107-8 PB - AIP Publishing CY - Melville, NY, USA AN - OPUS4-51440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Bruno, Giovanni T1 - Micro Non-Destructive Testing and Evaluation N2 - What is meant by ‘Micro Non-Destructive Testing and Evaluation’? This was the central subject of debate in this Special Issue. At present, sub-millimeter-size components or even assemblies are pervading the industrial and scientific world. Classic examples are electronic devices and watches (as well as parts thereof), but recent examples encompass additively manufactured lattice structures, stents, or other microparts. Moreover, most assemblies contain micro-components. Testing such components or their miniaturized parts would fit well within the topic of micro non-destructive testing and evaluation. In all cases, performance and integrity testing, quality control, and dimensional tolerances need to be measured at the sub-millimeter level (ideally with a spatial resolution of about a micron); most of the time, such features and components are embedded in much larger assemblies, which also need to be taken into account. The solution to this dilemma (i.e. measuring large parts with high resolution) depends on the part and on the problem under consideration. Another possible definition of micro non-destructive testing and evaluation can relate to the characterization of micro-features (e.g., the microstructure) in much larger specimens, such as damage in concrete cores or porosity in additively manufactured components. A further aspect is the use of microscopic probes to evaluate macroscopic properties. This is the case, for instance but not at all exclusively, in the use of diffraction techniques to determine macroscopic stress. The splits between testing and characterization at the micro-level (or of micro parts) from one side and handling of macroscopic assemblies on the other represent a great challenge for many fields of materials characterization. On top of that, including the use of microscopic methods to test integrity would add a further level of complexity. Imaging, mechanical testing, non-destructive testing, measurement of properties, structural health monitoring, and dimensional metrology all need to be re-defined if we want to cope with the multi-faceted topic of micro non-destructive testing and evaluation. The challenge has already been accepted by the scientific and engineering communities for a while but is still far from being universally tackled. This Special Issue yields an interesting answer to the questions posed above. It presents the progress made and the different aspects of the challenge as well as at indicates the paths for the future of NDT&E. KW - Neutron Diffraction KW - Ultrasound KW - Eddy Currents KW - X-ray Computed Tomography KW - Mechanical Properties KW - Residual Stress KW - Defects PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570321 SN - 978-3-0365-6180-6 DO - https://doi.org/10.3390/books978-3-0365-6180-6 SN - 1996-1944 SP - 1 EP - 304 PB - MDPI CY - Basel AN - OPUS4-57032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schalau, Sebastian A1 - Habib, Abdel Karim A1 - Michel, S. T1 - A modified k-ε turbulence model for heavy gas dispersion in built-up environment N2 - For hazard assessment purposes, the dispersion of gases in complex urban areas is often a scenario to be considered. However, predicting the dispersion of heavy gases is still a challenge. In Germany, the VDI Guideline 3783, Part 1 and 2 is widely used for gas dispersion modelling. Whilst Part 1 uses a gauss model for calculating the dispersion of light or neutrally buoyant gases, Part 2 uses wind tunnel experiments to evaluate the heavier-than-air gas dispersion in generic built up areas. In practice, with this guideline, it is often not possible to adequately represent the existing obstacle configuration. To overcome this limitation, computational fluid dynamics (CFD) methods could be used. Whilst CFD models can represent obstacles in the dispersion area correctly, actual publications show that there is still further research needed to simulate the atmospheric flow and the heavy gas dispersion. This paper presents a modified k-ε-turbulence model that was developed in OpenFOAM v5.0 (England, London, The OpenFOAM Foundation Ltd Incorporated) to enhance the simulation of the atmospheric wind field and the heavy gas dispersion in built-up areas. Wind tunnel measurements for the dispersion of neutrally buoyant and heavy gases in built-up environments were used to evaluate the model. As a result, requirements for the simulation of the gas dispersion under atmospheric conditions have been identified and the model showed an overall good performance in predicting the experimental values. KW - Atmospheric boundary layer KW - OpenFOAM KW - Heavy gas KW - CFD PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568898 DO - https://doi.org/10.3390/atmos14010161 VL - 14 IS - 1 SP - 1 EP - 21 PB - MDPI AN - OPUS4-56889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dorgerloh, Ute A1 - Becker, Roland A1 - Freeling, Finnian A1 - Scheurer, Marco A1 - Gökçe, Emine A1 - Strack, Katrin A1 - Sommerfeld, Thomas A1 - Sauer, Andreas A1 - Schneider, Jonas A1 - Härtel, Christoph A1 - Valkov, Vassil A1 - Moser, Lukas A1 - Geiß, Sabine A1 - Junginger, Sabine A1 - Schlittenbauer, Linda A1 - Suess, Elke A1 - Ruth, Katinka T1 - Standardising the quantification of trifluoroacetic acid in water: Interlaboratory validation trial using liquid chromatography-mass spectrometric detection (LC–MS/MS) N2 - The concentration of trifluoroacetic acid in surface and groundwaters and drinking water is subject of increasing concern. Since there is no standardised procedure available, German standardisation body DIN has initiated the first draft standard using liquid chromatography with tandem mass spectrometry (LC–MS/MS) after direct injection for the concentration range between ≥ 0.1 and 3 µg/L. Herein, the interlaboratory comparison as final validation step involving 12 expert laboratories from Germany and Switzerland is described. Two groundwaters, two surface waters, a drinking water, a rainwater, and two fortified groundwater samples displayed relative repeatability standard deviations between 3 and 7% and relative reproducibility standard deviation between 6 and 20% and were included in the draft standard DIN 38407-53. KW - TFA Trifluoroacetic acid KW - LC/MS-MS KW - Validation trial PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-632376 DO - https://doi.org/10.1007/s00769-025-01640-2 SN - 0949-1775 SP - 1 EP - 4 PB - Springer CY - Berlin AN - OPUS4-63237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krauss, B. A1 - Mügge, C. A1 - Ziemer, B. A1 - Zschunke, Adolf A1 - Krech, F. T1 - 1-Phosphabicyclo[3.2.1]octane N2 - 1-Phosphabicyclo[3.2.1]octan erhält man durch radikalische Ringschlußreaktion von (2-Vinyl-4-pentenyl)-phosphan in Gegenwart von AIBN. Ein weiterer Weg zu 1-Phosphabicyclo[3.2.1]octanen beruht auf der radikalischen Cyclisierung von 2-Methyl-4-allyl-phospholan, das bei der Reaktion von (2-Allyl-4-pentenyl)-phosphan mit KPH2/18-Krone-6 in THF entsteht. Die bicyclischen Phosphane werden durch Reaktionen mit CS2, Selen, Schwefel, NO, CH3I und HSO3F, Struktur- und analytische Daten sowie 1H-, 13C-, 31P- und 77Se-NMR-Spektren charakterisiert. Der Raumbedarf der Phosphane als Komplexliganden wird entsprechend dem Tolman-Modell aus den 31P–1H-Kopplungskonstanten abgeschätzt. Die Konfiguration der Methylsubstituenten sowie die Konformation des Sechsringes wird aus den NMR-Parametern (Kopplungskonstanten, NOE's) bestimmt und durch die Röntgenkristallstrukturanalyse bestätigt. KW - NMR Spektroskopie KW - Kristallstruktur PY - 2001 DO - https://doi.org/10.1002/1521-3749(200107)627:7<1542::AID-ZAAC1542>3.0.CO;2-F SN - 0044-2313 VL - 627 IS - 7 SP - 1542 EP - 1552 PB - Wiley-VCH CY - Weinheim AN - OPUS4-63393 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Fritsch, Tobias T1 - A Multiscale Analysis of Additively Manufactured Lattice Structures N2 - Additive Manufacturing (AM) in terms of laser powder-bed fusion (L-PBF) offers new prospects regarding the design of parts and enables therefore the production of lattice structures. These lattice structures shall be implemented in various industrial applications (e.g. gas turbines) for reasons of material savings or cooling channels. However, internal defects, residual stress, and structural deviations from the nominal geometry are unavoidable. In this work, the structural integrity of lattice structures manufactured by means of L-PBF was non-destructively investigated on a multiscale approach. A workflow for quantitative 3D powder analysis in terms of particle size, particle shape, particle porosity, inter-particle distance and packing density was established. Synchrotron computed tomography (CT) was used to correlate the packing density with the particle size and particle shape. It was also observed that at least about 50% of the powder porosity was released during production of the struts. Struts are the component of lattice structures and were investigated by means of laboratory CT. The focus was on the influence of the build angle on part porosity and surface quality. The surface topography analysis was advanced by the quantitative characterisation of re-entrant surface features. This characterisation was compared with conventional surface parameters showing their complementary information, but also the need for AM specific surface parameters. The mechanical behaviour of the lattice structure was investigated with in-situ CT under compression and successive digital volume correlation (DVC). The Deformation was found to be knot-dominated, and therefore the lattice folds unit cell layer wise. The residual stress was determined experimentally for the first time in such lattice structures. Neutron diffraction was used for the non-destructive 3D stress investigation. The principal stress directions and values were determined in dependence of the number of measured directions. While a significant uni-axial stress state was found in the strut, a more hydrostatic stress state was found in the knot. In both cases, strut and knot, seven directions were at least needed to find reliable principal stress directions. KW - Additive manufacturing KW - Laser powder bed fusion KW - Residual stress KW - Surface roughness analysis KW - Computed tomography PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:517-opus4-470418 DO - https://doi.org/10.25932/publishup-47041 SP - 1 EP - 97 PB - Universitätsbibliothek Potsdam CY - Potsdam AN - OPUS4-53476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Bruno, Giovanni T1 - Noise and blur removal from corrupted X-ray computed tomography scans: A multilevel and multiscale deep convolutional framework approach with synthetic training data (BAM SynthCOND) N2 - Regardless of the experimental care practiced in acquiring X-ray computed tomography (XCT) data, artifacts might still exist, such as noise and blur. This is typical for fast XCT data acquisitions (e.g., in-situ investigations), or low-dose XCT. Such artifacts can complicate subsequent analysis of the data. Digital filters can moderately cure extensive artifacts. The selection of filter type, intensity, and order of application is not always straight forward. To tackle these problems, a complete sequential multilevel, multi-scale framework: BAM SynthCOND, employing newly designed deep convolutional neural networks (DCNNs), was formulated. Although data conditioning with neural networks is not uncommon, the main complication is that completely artifact-free XCT data for training do not exist. Thus, training data were acquired from an in-house developed library (BAM SynthMAT) capable of generating synthetic XCT material microstructures. Some novel DCNN architectures were introduced (2D/3D ACEnet_Denoise, 2D/3D ACEnet_Deblur) along with the concept of Assertive Contrast Enhancement (ACE) training, which boosts the performance of neural networks trained with continuous loss functions. The proposed methodology accomplished very good generalization from low resemblance synthetic training data. Indeed, denoising, sharpening (deblurring), and even ring artifact removal performance were achieved on experimental post-CT scans of challenging multiphase Al-Si Metal Matrix Composite (MMC) microstructures. The conditioning efficiencies were: 92% for combined denoising/sharpening, 99% for standalone denoising, and 95% for standalone sharpening. The results proved to be independent of the artifact intensity. We believe that the novel concepts and methodology developed in this work can be directly applied on the CT projections prior to reconstruction, or easily be extended to other imaging techniques such as: Microscopy, Neutron Tomography, Ultrasonics, etc. KW - XCT Data Conditioning KW - Denoising Deblurring Sharpening KW - Deep Convolutional Neural Network (DCNN) KW - Synthetic Training Data KW - ACEnet KW - Metal Matrix Composite (MMC) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579129 DO - https://doi.org/10.1016/j.tmater.2023.100011 VL - 2 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-57912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bayerlein, Bernd A1 - Hanke, T. A1 - Muth, Thilo A1 - Riedel, Jens A1 - Schilling, Markus A1 - Schweizer, C. A1 - Skrotzki, Birgit A1 - Todor, A. A1 - Moreno Torres, Benjami A1 - Unger, Jörg F. A1 - Völker, Christoph A1 - Olbricht, Jürgen T1 - A Perspective on Digital Knowledge Representation in Materials Science and Engineering N2 - The amount of data generated worldwide is constantly increasing. These data come from a wide variety of sources and systems, are processed differently, have a multitude of formats, and are stored in an untraceable and unstructured manner, predominantly in natural language in data silos. This problem can be equally applied to the heterogeneous research data from materials science and engineering. In this domain, ways and solutions are increasingly being generated to smartly link material data together with their contextual information in a uniform and well-structured manner on platforms, thus making them discoverable, retrievable, and reusable for research and industry. Ontologies play a key role in this context. They enable the sustainable representation of expert knowledge and the semantically structured filling of databases with computer-processable data triples. In this perspective article, we present the project initiative Materials-open-Laboratory (Mat-o-Lab) that aims to provide a collaborative environment for domain experts to digitize their research results and processes and make them fit for data-driven materials research and development. The overarching challenge is to generate connection points to further link data from other domains to harness the promised potential of big materials data and harvest new knowledge. KW - Data infrastructures KW - Digital representations KW - Digital workflows KW - Knowledge graphs KW - Materials informatics KW - Ontologies KW - Vocabulary providers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546729 DO - https://doi.org/10.1002/adem.202101176 SN - 1438-1656 SP - 1 EP - 14 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-54672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Stegemann, R. A1 - Lyamkin, V. A1 - Cabeza, S. A1 - Evsevleev, S. A1 - Pelkner, Matthias A1 - Bruno, Giovanni T1 - Subsurface and Bulk Residual Stress Analysis of S235JRC + C Steel TIG Weld by Diffraction and Magnetic Stray Field Measurements N2 - Background Due to physical coupling between mechanical stress and magnetization in ferromagnetic materials, it is assumed in the literature that the distribution of the magnetic stray field corresponds to the internal (residual) stress of the specimen. The correlation is, however, not trivial, since the magnetic stray field is also influenced by the microstructure and the geometry of component. The understanding of the correlation between residual stress and magnetic stray field could help to evaluate the integrity of welded components. Objective This study aims at understanding the possible correlation of subsurface and bulk residual stress with magnetic stray field in a low carbon steel weld. Methods The residual stress was determined by synchrotron X-ray diffraction (SXRD, subsurface region) and by neutron diffraction (ND, bulk region). SXRD possesses a higher spatial resolution than ND. Magnetic stray fields were mapped by utilizing high-spatial-resolution giant magneto resistance (GMR) sensors. Results The subsurface residual stress overall correlates better with the magnetic stray field distribution than the bulk stress. This correlation is especially visible in the regions outside the heat affected zone, where the influence of the microstructural features is less pronounced but steep residual stress gradients are present. Conclusions It was demonstrated that the localized stray field sources without any obvious microstructural variations are associated with steep stress gradients. The good correlation between subsurface residual stress and magnetic signal indicates that the source of the magnetic stray fields is to be found in the range of the penetration depth of the SXRD measurements. KW - Residual stress KW - Magnetic stray field KW - Synchrotron X-ray diffraction KW - Neutron diffraction KW - TIG welding PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547419 DO - https://doi.org/10.1007/s11340-022-00841-x VL - 62 IS - 6 SP - 1017 EP - 1025 PB - Springer AN - OPUS4-54741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - De la Hoz Alford, L. A1 - Pecanha de Souza, C. G. A1 - Paciornik, S. A1 - d` Almeida, J. R. M. A1 - Santos Leite, B. A1 - Avila, H. C. A1 - Léonard, F. A1 - Bruno, Giovanni T1 - Three-Dimensional Characterization of Polyurethane Foams Based on Biopolyols N2 - Two biopolyol-based foams derived from banana leaves (BL) or stems (BS) were produced, and their compression mechanical behavior and 3D microstructure were characterized. Traditional compression and in situ tests were performed during 3D image acquisition using X-ray microtomography. A methodology of image acquisition, processing, and analysis was developed to discriminate the foam cells and measure their numbers, volumes, and shapes along with the compression steps. The two foams had similar compression behaviors, but the average cell volume was five times larger for the BS foam than the BL foam. It was also shown that the number of cells increased with increasing compression while the average cell volume decreased. Cell shapes were elongated and did not change with compression. A possible explanation for these characteristics was proposed based on the possibility of cell collapse. The developed methodology will facilitate a broader study of biopolyol-based foams intending to verify the possibility of using these foams as green alternatives to the typical petrol-based foams. KW - Compression mechanical KW - Biopolyol KW - Banana KW - 3D microstructure KW - X-ray microtomography PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571982 DO - https://doi.org/10.3390/ma16052118 SN - 1996-1944 VL - 16 IS - 5 SP - 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-57198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Fioresi, R. A1 - Faglioni, F. A1 - Bruno, Giovanni T1 - Synthetic Data Generation for Automatic Segmentation of X-ray Computed Tomography Reconstructions of Complex Microstructures N2 - The greatest challenge when using deep convolutional neural networks (DCNNs) for automatic segmentation of microstructural X-ray computed tomography (XCT) data is the acquisition of sufficient and relevant data to train the working network. Traditionally, these have been attained by manually annotating a few slices for 2D DCNNs. However, complex multiphase microstructures would presumably be better segmented with 3D networks. However, manual segmentation labeling for 3D problems is prohibitive. In this work, we introduce a method for generating synthetic XCT data for a challenging six-phase Al–Si alloy composite reinforced with ceramic fibers and particles. Moreover, we propose certain data augmentations (brightness, contrast, noise, and blur), a special in-house designed deep convolutional neural network (Triple UNet), and a multi-view forwarding strategy to promote generalized learning from synthetic data and therefore achieve successful segmentations. We obtain an overall Dice score of 0.77. Lastly, we prove the detrimental effects of artifacts in the XCT data on achieving accurate segmentations when synthetic data are employed for training the DCNNs. The methods presented in this work are applicable to other materials and imaging techniques as well. Successful segmentation coupled with neural networks trained with synthetic data will accelerate scientific output. KW - Automatic segmentation KW - 3D deep convolutional neural network (3D DCNN) KW - Dice score KW - Metal matrix composite (MMC) KW - Modified U-Net architectures KW - Multi-phase materials PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571243 DO - https://doi.org/10.3390/jimaging9020022 VL - 9 IS - 2 SP - 1 EP - 23 PB - MDPI AN - OPUS4-57124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wieder, Frank A1 - Ewert, Uwe A1 - Vogel, Justus A1 - Jaenisch, Gerd-Rüdiger A1 - Bellon, Carsten T1 - A Novel Multi Slit X-Ray Backscatter Camera Based on Synthetic Aperture Focusing N2 - A special slit collimator was developed earlier for fast acquisition of X-ray back scatter images. The design was based on a twisted slit design (ruled surfaces) in a Tungsten block to acquire backscatter images. The comparison with alternative techniques as flying spot and coded aperture pin hole technique could not prove the expected higher contrast sensitivity. In analogy to the coded aperture technique, a novel multi slit camera was designed and tested. Several twisted slits were parallelly arranged in a metal block. The CAD design of different multi-slit cameras was evaluated and optimized by the computer simulation packages aRTist and McRay. The camera projects a set of equal images, one per slit, to the digital detector array, which are overlaying each other. Afterwards, the aperture is corrected based on a deconvolution algorithm to focus the overlaying projections into a single representation of the object. Furthermore, a correction of the geometrical distortions due to the slit geometry is performed. The expected increase of the contrast-to-noise ratio is proportional to the square root of the number of parallel slits in the camera. However, additional noise has to be considered originating from the deconvolution operation. The slit design, functional principle, and the expected limits of this technique are discussed. T2 - 43rd Annual Review of Progress in QNDE CY - Atlanta, GA, USA DA - 17.07.2016 KW - Deconvolution KW - Back scatter imaging KW - Computer simulation KW - Aperture focusing PY - 2017 SN - 978-0-7354-1474-7 DO - https://doi.org/10.1063/1.4974711 VL - 1806 SP - 1 EP - 9 PB - AIP Publishing AN - OPUS4-42429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - A brief introduction to wind turbine aerodynamics N2 - In general, wind turbines transform the kinetic energy of the wind into electric power. Thereby, the wind turbine blades are facing unsteady loads which are transferred to the hub to generate a rotation of the turbine’s axis. This brief introduction focuses on the aerodynamics of the blades and the corresponding loads. Starting with the basic flow field and loads of an airfoil, terms like stagnation point, boundary layer, Reynolds number, transition, and separation are introduced. For different geometries, lift and drag coefficient curves are discussed. Then, full wings will be considered, including their three-dimensional flow field due to wing tip vortices and crossflows. As a main source of increased loads, unsteady effects are explained in more detail such as gusts, tower passing, earth boundary layer crossing, free stream turbulences, yaw misalignment, etc. At the end, extra loads due to an oscillating free stream are introduced. T2 - QI-Digital: KI-Machbarkeitsstudie Thermografie Rotorblätter CY - Berlin, Germany DA - 13.12.2022 KW - Wind turbine KW - Nondestructive testing KW - Aerodynamics KW - Dynamic stall PY - 2022 AN - OPUS4-56728 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bühling, Benjamin T1 - Using a spectral entropy criterion for improved onset picking in ultrasonic testing N2 - In ultrasonic testing, the time of flight (ToF) of a signal can be used to infer material and structural properties of a test item. In dispersive media, extracting the bulk wave velocity from a received signal is challenging as the waveform changes along its path of propagation. When using signal features such as the first peak or the envelope maximum, the calculated velocity changes with the propagation distance. This does not occur when picking the signal onset. Borrowing from seismology, researchers used the Akaike information criterion (AIC) picker to automatically obtain onset times. In addition to being dependent on arbitrarily set parameters, the AIC picker assumes no prior knowledge of the spectral properties of the signal. This is unnecessary in ultrasonic through-transmission testing, where the signal spectrum is known to differ significantly from noise. In this contribution, a novel parameter-free onset picker is proposed, that is based on a spectral entropy criterion (SEC) to model the signal using the AIC framework. Synthetic and experimental data are used to compare the performance of SEC and AIC pickers, showing an improved accuracy for densely sampled data. T2 - 183rd Meeting of the Acoustical Society of America CY - Nashville, TN, USA DA - 05.12.2022 KW - ToF KW - Arrival time KW - Nondestructive testing KW - Through-transmission KW - AIC picker PY - 2022 AN - OPUS4-56616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture diffusion affected by the Knudsen effect in temporal changing pore networks N2 - Almost all building materials in civil engineering have an open porosity and interact with or are affected by the environmental conditions. Structures might suffer from effects such as moisture adsorption, carbonation, corrosion, penetration of salt ions and chemical substances, etc. In the hygroscopic range, these processes are mostly driven by diffusion. Due to the confinement of small pores ( 1 m), the Knudsen effect reduces the molecular diffusion. This reduction can become more significant in case of temporal changing pore systems because of physisorption of water vapor, carbonation, or chemisorption. In this study, unstabilised earth blocks and earth masonry are investigated. In a first step, the pore size distribution of the blocks is measured and sorption isotherms are recorded in experiments. Besides the ordinary physisorption, the involved clay minerals undergo swelling or shrinking due to chemisorption. The following two effects must be considered: first, the reduction of the available pore space by the adsorbed water layer. For this, the Hillerborg sorption theory is used, which is a combination of the well-known Brunauer-Emmett-Teller sorption theory and the Kelvin equation. This allows the computation of adsorbed water layers even in curved pore geometries. Second, the variation of the initial pore size distribution due to chemisorption needs to be modelled. Based on these two models, the effective diffusion coefficient can be predicted. For validation, arrays of relative humidity sensors were embedded into a free-standing earth masonry wall. This monitoring was carried out over more than a year to have a broad variety of environmental conditions and was located in Berlin, Germany. The prediction of the effective diffusion coefficient can also be transferred to other processes and allows the investigation of materials having temporarily changing pore systems. Examples are the carbonation of cementitious materials, alkali silica reaction, calcium leaching of long-lasting structures, etc. This effect becomes most prominent in the meso-pore range and might alter the effective diffusion coefficient by more than 100 %. T2 - 4th International Congress on Materials & Structural Stability CY - Rabat, Morocco DA - 08.03.2023 KW - Earth masonry KW - Material moisture KW - Molecular diffusion KW - Chemisoprtion KW - Knudsen effect KW - Physisorption PY - 2023 AN - OPUS4-57140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Vertrauen in Qualität und Sicherheit in der Digitalisierung - Eine digital gestützte Qualitätssicherung für die additive Fertigung N2 - Der Vortrag stellt die Initiative QI-Digital vor, deren Ziel es ist, Lösungen für eine moderne, digitale Qualitätsinfrastruktur (QI) zu entwickeln. Dabei wird insbesondere auf den das praxisnahe Pilotprojekt der Qualitätssicherung in der additiven Fertigung eingegangen und aufgezeigt, wie digitale QI-Werkzeuge wie Smart Standards, digitale Zertifikate und Kalibrierscheine, eine QI-Cloud und der digitale Produktpass zu einer vernetzten und vertrauenswürdigen Qualitätssicherung beitragen. T2 - Leichtbau-Workshop Digitalisierung „Digitalisierung, Motor für nachhaltigen Leichtbau – Leichtbau, Motor für die Digitalisierung!“ CY - Online meeting DA - 24.11.2022 KW - Qualitätsinfrastruktur KW - Digitalisierung KW - Kalibrierung KW - Konformitätsbewertung KW - Prüfung KW - digitale Transformation KW - Additive Fertigung PY - 2022 AN - OPUS4-56384 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönsee, Eric T1 - Calculating rheological properties of fresh mortar for additive manufacturing based on experimental, multi sensor data N2 - Additive manufacturing of concrete structures is a novel and emerging technology. Free contouring in civil engineering, which allows for entirely new designs, is a significant advantage. In the future, lower construction costs are expected with increased construction speeds and decreasing required materials and workers. However, architects and civil engineers rely on a certain quality of execution to fulfil construction standards. Although several techniques and approaches demonstrate the advantages, quality control during printing is highly challenging and rarely applied. Due to the continuous mixing process commonly used in 3D concrete printing, it is impossible to exclude variations in the dry mixture or water content, and a test sample cannot be taken as a representative sample for the whole structure. Although mortar properties vary only locally, a defect in one layer during printing could affect the entire integrity of the whole structure . Therefore, real-time process monitoring is required to record and document the printing process. At the Bundesanstalt für Materialforschung und -prüfung (BAM) a new test rig for the additive manufacturing of concrete is built. The primary purpose is measuring and monitoring the properties of a mortar during the printing process. The following study investigates an approach for calculating yield stress and plastic viscosity based on experimentally recorded pressure data. The calculations assume that fresh mortar behaves as a Bingham fluid and that the Buckingham-Reiner-equation is applicable. A test setup consisting of rigid pipes with integrated pressure sensors at different positions is utilized. Monitoring the printing process with different sensors is crucial for the quality control of an ongoing process. T2 - Non-Tradijtional Cement and Concrete CY - Brno, Czech Republic DA - 25.06.2023 KW - 3DCP KW - Monitoring KW - Additive Manufacturing KW - Rheology KW - Bingham Fluid PY - 2023 AN - OPUS4-58144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - Current Digitalization Approaches in Quality Infrastructure -The QI-Digital Initiative N2 - The talk provides an overview on the importance and drivers of digital transformation in quality infrastructure (QI) as well as the approach the initiative QI-Digital takes to provide solutions. Special emphasis is given to the pilot projects implemented at BAM. T2 - Global Technical Regulation and Standardization Board Meeting CY - Erlangen, Germany DA - 20.07.2023 KW - Quality Infrastructure KW - Conformity Assessment KW - Quality-X KW - Smart standard KW - Additive manufacturing KW - Hydrogen fueling station KW - Digitalization PY - 2023 AN - OPUS4-58118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - A Modern Quality Infrastructure: Digital and Networked N2 - The presentation provides an overview and introduction to the need and drivers for the digital transformation of the quality infrastructure (QI). It illustrates the tools and processes that are the fundation of a digital QI and how the initiatve QI-Digital aims at developing accordant solutions. Special emphasis is given to the pilot projects at BAM. T2 - Visit of Indian delegation at BAM hosted by GIZ and BMWK CY - Berlin, Germany DA - 24.04.2023 KW - Quality Infrastructure KW - Conformity Assessment KW - Quality-X KW - Smart standard KW - Additive manufacturing KW - Hydrogen fueling station KW - Digitalization KW - Digital certificate PY - 2023 AN - OPUS4-58119 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia A1 - Hilgenberg, Kai T1 - Eine moderne Qualitätsinfrastruktur: digital und vernetzt N2 - Der Vortrag stellt die Arbeiten der BAM in der Initiative QI-Digital vor, in deren Rahmen Lösungen für eine moderne und digitale Qualitätsinfrastruktur entwickelt werden. Schwerpunkt liegt auf dem zentralen Werkzeug Quality-X sowie dem Pilotprojekt "Moderne Qualitätssicherung in der Additiven Fertigung". T2 - BAM Kuratoriumssitzung CY - Berlin, Germany DA - 22.06.2023 KW - Qualitätsinfrastruktur KW - Digitalisierung KW - Quality-X KW - Additive Fertigung PY - 2023 AN - OPUS4-58121 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Claudia T1 - A Modern Quality Infrastructure: Digital and Networked N2 - Introduction to the initiative QI-Digital and the BAM pilot projects, especially hydrogen fueling station, that seek to develop solutions for a modern and digital Quality Infrastructure (QI). T2 - Meeting mit Korea Delegation (Motie RHS Projekt) CY - Online meeting DA - 28.02.2023 KW - Quality Infrastructure KW - Conformity Assessment KW - Quality-X KW - Smart standard KW - Additive manufacturing KW - Hydrogen fueling station KW - Digitalization KW - Digital certificate PY - 2023 AN - OPUS4-58120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias T1 - Towards Autonomous NDT Inspection: Setup and Validation of an Indoor Localization System N2 - Monitoring and maintenance of civil infrastructure are of great importance, as any undetected damage can cause high repair costs, unintended deadtime, or endanger structural integrity. The inspection of large concrete structures such as bridges and parking lots is particularly challenging and time-consuming. Traditional methods are mostly manual and involve mapping a grid of measurement lines to record the position of each measurement. Current semi-automated methods, on the other hand, use GPS or tachymeters for localization but still require trained personnel to operate. An entirely automated approach using mobile robots would be more cost- and time-efficient. While there have been developments in using GPS-enabled mobile robots for bridge inspection, the weak signal strength in indoor areas poses a challenge for the automated inspection of structures such as parking lots. This paper aims to develop a solution for the automated inspection of large indoor concrete structures by addressing the problem of robot localization in indoor spaces and the automated measurement of concrete cover and rebar detection. T2 - 39th Danubia-Adria Symposium on Advances in Experimental Mechanics CY - Siófok, Hungary DA - 26.09.2023 KW - NDT Inspection KW - Mobile Robot KW - Indoor Localization KW - Setup and Validation PY - 2023 AN - OPUS4-58662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Küttenbaum, Stefan A1 - Maack, Stefan A1 - Aßmann, Norman A1 - Feistkorn, S. T1 - Ways to unlock the potential of non-destructive concrete testing for the reliability assessment of our built environment N2 - This contribution attempts to shed light on the application of POD analyses and measurement uncertainty calculations in nondestructive testing of concrete structures to provide useful and quality-assured information for reliability assessments of our built environment - with an emphasis on ground penetrating radar. It is shown that signal processing techniques affect POD analysis results to varying degrees, that measurement uncertainties are useful to validate PODs, and that the utilization of both POD analysis and measurement uncertainty calculations can pave the way to NDT-based reliability assessment, which will be exemplarily demonstrated in conclusion – generally aiming to derive those maintenance strategies and actions that are in line with actual demands. T2 - SPIE Smart Structures + Nondestructive Evaluation 2023 CY - Los Angeles, USA DA - 12.03.2023 KW - Probability of detection KW - Measurement uncertainty KW - Ground penetrating radar (GPR) KW - Existing structures PY - 2023 DO - https://doi.org/10.1117/12.2658736 VL - 12491 SP - 1 EP - 11 PB - SPIE AN - OPUS4-57393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Electrochemical immunosensing with a 3-dimensional microfluidic cell N2 - The flash presentation give a quick overview of the work performed. T2 - European Biosensor Symposium CY - Aachen, Germany DA - 28.08.2023 KW - Biosensors KW - microfluidics KW - antibodies KW - Electrochemical detection PY - 2023 AN - OPUS4-59202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Destructive and non-destructive 3D-characterization of inner metal structures in ceramic packages N2 - Ceramic multilayer packages provide successful solutions for manifold applications in telecommunication, microsystem, and sensor technology. In such packages, three-dimensional circuitry is generated by combination of structured and metallized ceramic layers by means of tape casting and multilayer technology. During development and for quality assurance in manufacturing, characterization of integrity, deformation, and positioning of the inner metal features is necessary. Visualization with high resolution and material contrast is needed. Robot-assisted 3D-materialography is a useful technique to characterize such multimaterial structures. In that, many sections of the specimen are polished and imaged automatically. A three-dimensional representation of the structure is created by digital combination of the image stack. A quasi non-destructive approach is to perform X-ray computer tomography (CT) with different beam energies. The energies are chosen to achieve a good imaging of either the metal features, or the ceramic matrix of the structure. The combination of the respective tomograms results in a high contrast representation of the entire structure. Both methods were tested to characterize Ag and Ag/Pd conductors in a ceramic multilayer package. The results were compared in terms of information content, effort, and applicability of the methods. T2 - 98th DKG Annual Meeting - CERAMICS 2023 CY - Jena, Germany DA - 27.03.2023 KW - Ceramics KW - Synchrotron CT KW - 3D materialography PY - 2023 AN - OPUS4-57268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dittrich, Maria A1 - Paulo, Carlos A1 - Knabe, Nicole A1 - Sturm, Heinz A1 - Zaitsev, Vladimir A1 - Gorbushina, Anna T1 - Microscopic Raman study of fungal pigment using the genetically amenable rock inhabitant Knufia petricola as a model organism N2 - Fungal pigments such as melanin and carotenoids are distinctive markers of animal and plant pathogenic fungi as well as their environmental relatives. These complex pigments play important roles in pathogenicity and stress tolerance while also being useful as biomarkers. Accordingly, it is important to be able to identify in situ the pigments in black fungi, a group of clinical and environmental importance. In this study, wild-type and genetically modified strains of Knufia petricola A95 and wild fungal cells attached to ancient rock were investigated for their spectroscopic and microscopic Raman features and morphological appearance. Knockout mutants of melanin synthesis genes pks1 (polyketide synthase), sdh1 (scytalone dehydratase), and both pks1 and the carotenoid synthesis gene phd1 (phytoene desaturase) were studied We applied two different Raman microscopes using two lasers, with 633 nm and 488 nm wavelengths. We analyzed and compared Raman spectra between the measured reference substances and the mutant and wild-type strains. In the wild strain WT:A95, the peaks close to melanin peals were found at 1353 cm−1 and 1611 cm−1. There are no characteristic melanin peaks at 1580–1600 cm−1 and around 1350 cm−1 at the spectrum of the Δpks1/Δphd1 mutant and the Δsdh1 mutant. The Δpks1 mutant spectrum has the peaks at the beta-carotene v2 C-C in-plane stretch at 1155 cm−1 and v3 C-CH3 deformation at 1005 cm−1. The peaks of carotenoids and melanin were found in all mutants and the wild strain, except the Δpks1/Δphd1 mutant. Raman spectra allow for discrimination between the various pigments. Hence, interactions between natural fungal melanin, as well as other protective pigments, and complex environmental matrices can be characterized on a range of spatial and temporal scales. KW - Raman Spectroscopy KW - Instrumentation KW - Analytical Chemistry KW - Knufia petricola KW - Confocal microscopy KW - Atomic and Molecular Physics and Optics PY - 2023 DO - https://doi.org/10.1016/j.saa.2023.123250 SN - 1386-1425 VL - 303 SP - 1 EP - 11 PB - Elsevier BV AN - OPUS4-58792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Okeke, Joseph T1 - In situ and operando imaging, spectroscopy and tomography of batteries N2 - The development of more powerful and more efficient lithium-ion batteries (LIBs) is a key area in battery research, aiming to support the ever-increasing demand for energy storage systems. To better understand the causes and mechanisms of degradation, and thus the diminishing cycling performance and lifetime often observed in LIBs, in operando techniques are essential, because battery chemistry can be monitored non-invasively, in real time. Moreover, there is increasing interest in developing new battery chemistries. Beyond LIBs, sodium ion batteries (NIBs) have gained increasing interest in recent years, as they are a promising candidate to complement LIBs, owing to their improved sustainability and lower cost, while still maintaining high energy density.[1] Initial phases of NIB commercialisation have occurred in the past year. However, for the widespread commercialisation of NIBs, there are still challenges that need to be overcome in developing optimized electrode materials and electrolytes. For the development of such materials and greater understanding of sodium storage mechanisms, solid electrolyte interface (SEI) formation and stability, and degradation processes, in operando methodologies are crucial. Among the techniques available for in operando analysis, nuclear magnetic resonance spectroscopy (NMR) and imaging (MRI) are becoming increasingly used to characterize the chemical composition of battery materials, study the growth and distribution of dendrites, and investigate battery storage and degradation mechanisms. In situ and in operando 1H, 7Li and 23Na NMR and MRI have recently been used to study LIBs and NIBs, identifying chemical changes in Li and Na species respectively, in metallic, quasimetallic and electrolytic environment as well as directly and indirectly studying dendrite formation in both systems.[2-4] The ability of NMR and MRI to probe battery systems across multiple environments can further be complemented by the enhanced spatial resolution of micro-computed X-ray tomography (μ-CT) which can provide insight into battery material microstructure and defect distribution. Here, we report in operando 1H and 7Li NMR and MRI experiments that investigate LIB performance, and the identification of changes in the Li signal during charge cycling, as well as the observation of signals in both 1H and 7Li NMR spectra that we attribute to diminishing battery performance, capacity loss and degradation. Additionally, recent operando methodology are adapted and implemented to study Sn based anodes in NIBs. 23Na spectroscopy is performed to monitor the formation and evolution of peaks assigned to stages of Na insertion into Sn, while 1H MRI is used to indirectly visualize the volume expansion of Sn anodes during charge cycling. Battery operation and degradation is further explored in these NIBs, using μ-CT, where the anode is directly visualized to a higher resolution and the loss of electrolyte in the cell, during cycling is observed T2 - 17th International Conference on Magnetic Resonance Microscopy CY - Singapore DA - 27.08.2023 KW - Sodium ion battery KW - Lithium ion battery KW - NMR KW - MRI KW - Tomography PY - 2023 AN - OPUS4-58421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reuter, T. T1 - Vorstellung des Projektes CTSimU2 Realistische Simulation realer Röntgencomputertomografie-Systeme mit basisqualifizierter Simulationssoftware N2 - Die Entwicklung von Werkzeugen zur realitätsnahen Nachbildung eines industriellen CT-Systems in einer Simulationssoftware ist derzeit Hauptaufgabe des WIPANO Forschungsprojektes CTSimU2 Realistische Simulation realer Röntgencomputertomografie - Systeme mit basisqualifizierter Simulationssoftware. Als Voraussetzung dienen dabei Simulationssoftwares, die durch das Testframework aus dem Vorprojekt CTSimU1 basisqualifiziert wurden. Das Testframework testet die hinreichende physikalische Korrektheit und Funktionalität einer Simulationssoftware (Basisqualifizierung der Software). Für eine realitätsnahe Nachbildung ist nicht nur die Güte der Simulationssoftware, sondern insbesondere die Güte der Parametrisierung des realen CT-Systems in der Simulationssoftware ausschlaggebend. Dabei kann das Vorgehen der Parametrisierung in vier Schritte unterteilt werden: die Datenaufnahme am realen CT-System (Schritt 1), die Auswertung der aufgenommenen Daten für die Generierung allgemeiner Parameterangaben (Schritt 2), die Übertragung der Parameter in die spezifischen Simulationssoftwares (Schritt 3) und die Validierung der resultierenden Simulationsparameter durch einen geeigneten Test (Schritt 4). Ziel des Projektes ist es daher neben der Erarbeitung eines Werkzeugkastens mit allgemeinen Methoden zur Datenaufnahme und Auswertung der Daten, die Entwicklung eines Tests, auf dessen Basis die ausreichend korrekte Simulation einer realen Anlage beurteilt werden kann. Die erarbeiteten Ergebnisse sollen wie bereits im Vorprojekt CTSimU1 in einen Richtlinienentwurf für die Richtlinienreihe VDI/VDE 2630 übertragen werden. Dieser Beitrag soll einen Überblick über das Projekt und die ersten Ergebnisse geben. T2 - DGZfP Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - XCT KW - Simulation PY - 2023 UR - https://www.ndt.net/?id=28620 AN - OPUS4-58922 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - Realistic Simulation of CT Systems - An Introduction to The CTSimU2 Project N2 - The project series CTSimU was initiated with the goal to develop a set of procedures to enable the determination of the task-specific measurement uncertainty of a CT system numerically by radiographic simulation. The first project (2019-2022) “Radiographic Computed Tomography Simulation for Measurement Uncertainty Evaluation - CTSimU” was focused on the sufficient physical correctness of the radiographic simulation and created as a result a test framework for simulation softwares and a draft of a VDI standard in the series VDI/VDE 2630 for this application. However, for the realistic simulation of a CT system in a simulation software (i.e. a digital twin), not only the correctness of the simulation software itself is crucial, but also the quality of the parameterization of the CT system in the simulation software - this represents the starting point of the 2nd project “Realistic Simulation of real CT systems with a basic-qualified Simulation Software - CTSimU2” (2022-2024). The parameterization of a CT system in a simulation software can be divided into four steps: after the data acquisition at the real CT system (step 1) follows the evaluation of the acquired data for the generation of general parameter specifications (step 2). It follows the transfer of the parameters into the specific simulation software (step 3) and the validation of the resulting simulation parameters by a suitable test (step 4). The intended result of the project CTSimU2 is a draft VDI standard (for VDI/VDE 2630) for this test, which contains an informative annex on the state of the art regarding the possibilities for parameter determination. T2 - 13th European Conference on Non-Destructive Testing (ECNDT) CY - Lisbon, Portugal DA - 03.07.2023 KW - X-ray computed tomography KW - dXCT KW - Simulation PY - 2023 AN - OPUS4-58923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning A1 - Sintschuk, Michael T1 - Work- and Dataflow for CT at BAM N2 - The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The imaging capabilities allow for in-situ and operando experiments. In this presentation the data handling pipeline is presented. T2 - Kickoff Meeting Best practices and solutions in the development of the control and data analysis system for custom designed CT setups CY - Online Meeting DA - 27.11.2023 KW - Synchrotron radiation KW - X-ray imaging KW - Double-multilayer monochromators PY - 2023 AN - OPUS4-58959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - Virtual CT with aRTist N2 - The software aRTist is a simulation tool for the generation of realistic radiographs of virtual radiographic superstructures. With radiographic simulations, virtual component models can be scanned as in a computer tomograph. Industrial X-ray computed tomography (CT) enables the non-destructive detection of internal and external surfaces as well as inhomogeneities of technical objects. Virtual CT offers new possibilities for the investigation of parameter influences of this complex testing and measuring technique. In addition to the option of switching physical effects on and off, scanning movements can also be tested before their technical realization. The virtual CT generates projection images from different directions for the subsequent reconstruction of a volume model of the examined object. The reconstruction of the simulated scans is carried out with the algorithms and programs for real scans. Tomographic scans consist of a large number of projections, which practically cannot be generated individually by the user of a simulation. The software offers various options for the automated simulation of tomographic scans. These range from standard CT to scans on free trajectories or with individual projection matrices. T2 - 12th Conference on Industrial Computed Tomography (iCT) 2023 CY - Fürth, Germany DA - 27.02.2023 KW - X-ray computed tomography KW - Simulation PY - 2023 AN - OPUS4-58919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Falahat, A.M. A1 - Kupsch, Andreas A1 - Hentschel, M.P. A1 - Lange, A. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Manke, I. T1 - Correction approach of detector backlighting in radiography N2 - In various kinds of radiography, deficient transmission imaging may occur due to backlighting inside the detector itself arising from light or radiation scattering. The related intensity mismatches barely disturb the high resolution contrast, but its long range nature results in reduced attenuation levels which are often disregarded. Based on X-ray observations and an empirical formalism, a procedure is developed for a first order correction of detector backlighting. A backlighting factor is modeled as a function of the relative detector coverage by the sample projection. Different cases of sample transmission are regarded at different backlight factors and detector coverage. The additional intensity of backlighting may strongly affect the values of materials’ attenuation up to a few 10%. The presented scenario provides a comfortable procedure for corrections of X-ray or neutron transmission imaging data. KW - X-ray imaging KW - Neutron imaging KW - Radiology KW - Backlighting KW - Digital detector array PY - 2019 DO - https://doi.org/10.1063/1.5097170 SN - 0034-6748 VL - 90 IS - 12 SP - 125108 PB - American Institute of Physics CY - Melville, NY, USA AN - OPUS4-50217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bellon, Carsten T1 - Virtuelle CT N2 - Das Computerprogramm aRTist ist ein praktisches Simulationswerkzeug zur Erzeugung realistischer Radiographien virtueller Durchstrahlungsaufbauten. Mit Durchstrahlungssimulationen können Bauteile, repräsentiert durch STL-Geometrien, wie in einem Computertomografen gescannt werden. Dabei werden verschiedenste Parameter gezielt und exakt berücksichtigt. Die Virtuelle Computertomografie bietet neue Möglichkeiten der Untersuchung von Parametereinflüssen. Neben der Möglichkeit, physikalische Effekte an- und abzuschalten, z.B. die Streustrahlung, können auch Scanbewegungen getestet werden, bevor diese technisch realisiert werden. Das für die Forschung entwickelte Simulationsprogramm aRTist bietet mit seiner intuitiven grafischen Benutzeroberfläche vielfältige Anwendungsmöglichkeiten auch in Praxis und Entwicklung, beispielsweise zur Parameteroptimierung, für Machbarkeitsstudien oder zur Abschätzung der Unsicherheit dimensioneller Messungen. KW - Vituelle Computertomographie Simulation PY - 2020 SN - 2199-8299 VL - 2020 IS - April SP - 50 EP - 51 PB - TeDo Verlag GmbH CY - Marburg AN - OPUS4-50691 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - Radiographic Simulator aRTist - Computer simulation for industrial Tomography N2 - aRTist is an easy-to-use and practical simulation tool to generate realistic radiographic images from CAD objects. A dedicated add-on module makes CT simulation easy (virtual computer tomography). Just choose the number of projections. Unlike in the practice, simulation can separately image the primary and scatter radiation. This allows studying the scattering artefacts in CT (gray-level variations in regions of homogeneous material). T2 - 5. Jenaer μCT-Workshop CY - Jena, Germany DA - 20.11.2019 KW - Vitual computer tomography simulation PY - 2019 AN - OPUS4-49826 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning T1 - Work- and Data flow for CT at BAMline I N2 - After a general presentation of the beamline, specifically the workflow for ex-situ CT at BAMline is presented. Although being used in a broad variety of research fields the usual workflow for CT experiments is in most cases similar in terms of sample mounting, tomographic scan and reconstruction. Specific scanning schemes allow for a preview reconstruction carried out during the scan. A detailed description of the used hardware as well as the self-coded programs applied in the data pipeline will be given. This will be accompanied by a practical demonstration of the software involved in the entire process. T2 - Pipeline for XCT data acquisition and reduction workshop CY - Online meeting DA - 22.02.2021 KW - BAMline KW - Synchrotron KW - Tomography PY - 2021 AN - OPUS4-52168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - AdvanCT Virtual CT N2 - Simulation becomes more and more important in modern CT imaging. It is increasingly used to optimize techniques for complex applications, and for educational purposes. Simulation can also be used for uncertainty estimation of dimensional CT measurements. The radiographic simulator aRTist is a modelling tool which simulates X-ray imaging using a hybrid analytical and Monte-Carlo method to efficiently model the radiation transport. In addition to the relevant physical effects such as absorption and scattering, simplified fast models are employed to describe the characteristics of the X-ray source and the detector. aRTist is well equipped to model realistic X-ray imaging setups due to the ability to load exported CAD object descriptions. By repetitive simulation runs aRTist can function as virtual CT device. A simple CT scan module is contained in aRTist which allows the simulation of standard (circular cone beam) scanning trajectories. AdvanCT is a module for aRTist which allows to set up more complex scanning trajectories by attaching geometrical modification functions to the objects in the radiographic scene. In this way, advanced scanning modes can be realized. In addition to deterministic motion, also random variations can be introduced. By combining random variations with deterministic motion, non-ideal (realistic) CT scan geometries can be simulated, e.g. focal spot drift and mechanical instability of the axis of rotation. The AdvanCT module conveniently allows to construct these scenarios in a graphical interface and provides a preview before starting the (potentially long running) batch job. Therefore, deviations from ideal CT scan trajectories can be easily adjusted which is a necessary step towards uncertainty determination from simulation. T2 - dXCT conference 2021 CY - Online meeting DA - 17.05.2021 KW - X-ray Virtual Computer Tomography Simulation PY - 2021 AN - OPUS4-52953 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - CTSimU — Durchstrahlungssimulation für die Messunsicherheitsbestimmung beim Messen geometrischer Merkmale mittels Röntgen- Computertomographie N2 - Die industrielle Röntgen-Computertomographie (CT) ist in der geometrischen Messtechnik die einzige Technologie, die sowohl innen- als auch außenliegende Merkmale eines Werkstücks mit einer Messung zerstörungsfrei messen kann. Die Güte der Messung kann mittels einer dem Messwert beigeordneten Messunsicherheit angegeben werden. Allerdings sind zur Ermittlung der Messunsicherheit für eine Messgröße einer CT-Messung nach Stand der Technik (VDI/VDE 2630 Blatt 2.1) zwanzig Wiederholmessungen an kalibrierten Werkstücken notwendig. Da die Messung mit realen CT-Messgeräten zeit- und kostenintensiv ist, wird analog zur taktilen Koordinatenmesstechnik eine numerische Messunsicherheitsbestimmung durch Simulation angestrebt (vgl. VDI/VDE 2617 Blatt 7, GUM Supplement 1). Die Simulation bietet den Vorteil, dass sie sowohl zeitsparend als auch kosten- und ressourceneffizient ist. Allerdings ist die Zuverlässigkeit der verschiedenen Simulationsumgebungen momentan nicht quantifizierbar. Für eine glaubwürdige Anwendung von Simulationsumgebungen für die Messunsicherheitsbestimmung benötigen Anwender eine Beurteilung derselben – auch um eine Norm- bzw. Richtliniensicherheit in der Praxis sicherzustellen. Das Ziel dieses Projekts ist es daher, einen Richtlinienentwurf VDI/VDE 2630 Blatt 2.2 „Basisqualifizierung von Softwaresystemen für die Simulation geometrischer Messungen mit Röntgen-Computertomografie“ zu erstellen. Auf dieser Basis soll es möglich sein, die Eignung von Simulationsumgebungen zur Ermittlung der aufgabenspezifischen Messunsicherheit zu bewerten. Dazu wird ein Testframework entwickelt, mit welchem Durchstrahlungssimulationssoftwares basisqualifiziert werden können. Das Projekt wird in der Förderrichtlinie WIPANO durch das Bundesministerium für Wirtschaft und Energie gefördert. T2 - DGZfP-Jahrestagung 2021 CY - Online meeting DA - 10.05.2021 KW - Computertomographie Simulation PY - 2021 AN - OPUS4-52753 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deresch, Andreas A1 - Bellon, Carsten A1 - Jaenisch, Gerd-Rüdiger T1 - A general spectrum model for X-ray generators N2 - A fast quantitative model for the energy spectra of radiation emitted by X-ray tubes is described, handling thin as well as thick plane targets of arbitrary materials. The developed model is based on fundamental interaction cross sections, describing electron and photon transport via numerical integration of discretized distributions. While the focus lies on bremsstrahlung production, modeling of characteristic radiation is fully integrated. The model does not include any free parameters. The validity of the model is shown through comparison with measurements and Monte Carlo simulations for several combinations of target material and acceleration potential between 30 kV and 450 kV. KW - Modeling KW - X-ray KW - Spectrum KW - Bremsstrahlung KW - Electron transport PY - 2016 DO - https://doi.org/10.1016/j.ndteint.2015.12.007 SN - 0963-8695 VL - 79 SP - 92 EP - 97 PB - Butterworth-Heinemann CY - Oxford AN - OPUS4-35263 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumm, A. A1 - Duvauchelle, P. A1 - Kaftandjian, V. A1 - Jaenisch, Gerd-Rüdiger A1 - Bellon, Carsten A1 - Tabary, J. A1 - Mathy, F. A1 - Legoupil, S. ED - Büyüköztürk, O. T1 - Modelling of radiographic inspections N2 - Computer modelling of non-destructive testing methods has come a long way from the beginnings in the mid 90s to today. Radiographic modelling for components with higher wall thicknesses, as they are typical for nuclear applications, must include precise predictions of scattered radiation and its impact in terms of contrast reduction. Dedicated or general purpose Monte Carlo methods with the ability to calculate higher order scattering events are the state of the art for these applications. Aerospace applications, on the other hand, have stronger requirements on the modelling code's capabilities to import complex CAD geometries, and can benefit from faster analytical scatter models, limited to first or second order scattering events. Similar distinctions can be made for the various approaches proposed to accurately model geometrical and film unsharpness, film granularity, film responses, film/foil cartridges and photon noise. This article presents a state-of-the-art review of radiographic modelling from the perspective of two important application domains with very different requirements, nuclear and aerospace. T2 - NDTMS-2011 CY - Istanbul, Turkey DA - 15.05.2011 KW - Computer modelling KW - Monte-Carlo KW - Radiography KW - Film KW - Selenium PY - 2013 SN - 978-94-007-0722-1 SN - 978-94-007-0723-8 DO - https://doi.org/10.1007/978-94-007-0723-8_99 VL - 6 SP - 697 EP - 702 PB - Springer Netherlands AN - OPUS4-36655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Christina A1 - Tillack, Gerd-Rüdiger A1 - Bellon, Carsten A1 - Scharmach, Martina T1 - Wie kann man den Einfluß der industriellen Anwendungsfaktoren innerhalb der ZfP-Zuverlaessigkeitsformel messen? N2 - Dieses Poster beschäftigt sich mit der Zuverlässigkeitsformel und der Metrik für die Messung der Zuverlässigkeit T2 - DGZfP Jahrestagung 2000 CY - Innsbruck, Austria DA - 29.05.2000 KW - Anwendungszuverlässigkeit KW - Anwendungsparameter KW - ZfP-System PY - 2000 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-35849 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - Combining analytical and Monte Carlo modelling for industrial radiology N2 - Modelling becomes more and more important in modern NDE. It is increasingly used to optimize techniques for complex applications, to support the preparation of written procedures, and for education purposes. To describe the complete chain of RT, the model includes simulating all necessary properties of X- or Gamma-ray sources, the interaction of photons with material with special attention to scattered radiation, the detection process, and the complete geometrical RT setup handling arbitrary parts or constructions. Depending on the given inspection problem and the influencing factors that should be addressed by the simulation, an appropriate physical model has to be chosen to describe the underlying interaction mechanisms. The simulator aRTist combines analytical and Monte Carlo methods to efficiently model the radiation transport such that transmission as well as scatter techniques can be modelled. In this contribution we focus on Monte Carlo simulation of scatter contribution within aRTist. Examples for RT/tomographic applications and back-scatter techniques are presented to demonstrate the usability of the presented simulation tool for a broad range of radiological applications. T2 - 19th World Conference on Non-Destructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Monte Carlo method KW - Radiography KW - Simulation PY - 2016 AN - OPUS4-36617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - A fast general spectrum model for quantitative radiography simulation N2 - A model is presented that employs a unified approach for simulating the photon energy spectra for transmission and direct beam targets composed of arbitrary homogeneous materials. In order to achieve this, a detailed model of electron transport within the target is employed. The validity of the developed model is shown through comparisons with Monte Carlo simulations as well as measurements for a number of different configurations. T2 - 19th World Conference on Non-Destructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Modelling KW - Radiography KW - Simulation KW - X-ray spectrum PY - 2016 AN - OPUS4-36628 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten A1 - Jaenisch, Gerd-Rüdiger T1 - Supercomputing the cascade processes of radiation transport N2 - Modeling of the photon-electron cascade process in multicomponent objects of complex geometrical structure by use of hybrid supercomputers is considered. An approach to computing the cascade processes is developed. The approach has three key properties allowing the effective use of heterogeneous structure of computers for solving the tasks of radiation transport in complex multi-scale geometries. Firstly, two different discreet geometrical description of an object being under radiation is used: triangulated model for photon transport and voxel model for elec-tron transport. Secondly, small parameter of the problem is explicitly taking into ac-count for modeling surface effects (for instance, electron emission). Thirdly, the ef-fective calculation decomposition between CPU and GPU is developed for signifi-cant increasing the speed of calculations of processes in question. Modeling of ex-periment on researching the bremsstrahlung generated by electron beam in Ta target is carried out. Comparison of computing and experimental results shows satisfactory consent. T2 - 19th World Conference on Non-Destructive Testing CY - Munich, Germany DA - 13.06.2016 KW - Modelling KW - Monte Carlo method KW - Photon-electron transport PY - 2016 AN - OPUS4-36608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hilpert, U. A1 - Bartscher, M. A1 - Neugebauer, M. A1 - Goebbels, Jürgen A1 - Weidemann, Gerd A1 - Bellon, Carsten T1 - Simulation-aided computed tomography (CT) for dimensional measurements N2 - Carrying out dimensional measurements by CT means assessing coordinates in space. CT must therefore be treated as a coordinate measuring technique similar to optical or tactile Coordinate Measuring Machines (CMMs). The well-established standards and guidelines for the acceptance- and verificationtesting of CMMs require the use of calibrated reference standards to achieve measurement machine characteristics. Hence, transferring these concepts from coordinate metrology to CT, a dedicated CT-specific reference standard was designed, manufactured and calibrated using a tactile CMM. For comparison purposes, a CAD model was created by reverse engineering using the calibration data. The calibrated model was fed into a virtual CT and the measurement process was simulated. The reference standard was measured by micro-CT. By comparing the characteristics of the measurement output of CT and the output gained from simulation, the influences of measurement artefacts can be judged, for the first time, in analogy to existing Guidelines of coordinate metrology. T2 - DIR 2007 - International Symposium on Digital industrial Radiology and Computed Tomography CY - Lyon, France DA - 25.06.2007 KW - Computed tomography KW - X-ray KW - Simulation KW - Coordinate metrology PY - 2007 UR - http://www.ndt.net/article/dir2007/papers/12.pdf SP - Paper 6, 1 EP - 15 AN - OPUS4-37045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaenisch, Gerd-Rüdiger T1 - Back scatter X-ray imaging with twisted slit collimator – quantitative simulation and comparison to experiments N2 - X-ray backscatter imaging is a promising NDT technique to inspect complex objects using only a single-sided access. In difference to conventional transmission X-ray radiography, the X-ray backscatter imaging utilizes the scattered radiation caused by the Compton scattering effect. In order to achieve high backscatter intensities from a test object, it is necessary to optimize the backscatter system parameters namely the angle between source and slit camera, the slit-collimator system, the shielding between the source and scatter camera, and the type of detector. Here a single-slit as well as a multi-slit camera are considered. For the multi-slit camera several twisted slits were parallel arranged in a metal block. This camera generates a set of similar projections per slit overlaying each other. Afterwards, the image is corrected based on a de-convolution algorithm to focus the overlaying projections into a single representation of the object. The scatter phenomena in the object under inspection are investigated. In this contribution, the Monte Carlo model McRay is discussed, which considers all relevant single and multiple interactions of photons and electrons. This model can be used to simulate back scatter techniques. Simulations are important to describe the imaging process, to interpret the results, and to optimize the backscatter camera investigated here. Experimental results will be presented and compared with simulations. T2 - 55th Annual British Conference of Non-Destructive Testing CY - Nottingham, UK DA - 12.09.2016 KW - Modeling KW - X-rays KW - Backscatter application KW - Synthetic aperture focusing PY - 2016 AN - OPUS4-37618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haith, M. I. A1 - Ewert, Uwe A1 - Hohendorf, Stefan A1 - Bellon, Carsten A1 - Deresch, Andreas A1 - Huthwaite, P. A1 - Lowe, M. J. S. A1 - Zscherpel, Uwe T1 - Radiographic modelling for NDE of subsea pipelines N2 - This work presents an investigation of the accuracy of a radiographic simulation model applied to subsea pipeline inspections. Experimental measurements of a sample in a water tank are used to develop a set of calibrated simulation parameters for the modelling software aRTist. Image quality parameters such as signal-tonoise ratio, contrast and basic spatial resolution are compared with the aim of matching simulated values to experimental results. With this method signal-to-noise ratio was successfully matched while differences were still found in contrast-to-noise ratio comparisons. This means that measurements depending on absolute intensity are not accurate enough, however wall thickness measurements in tangential images, which are not based on absolute intensity, were found to produce similar results in simulated and experimental cases. The differences in contrast and intensity are thought to be due to detector backscatter and additional scatter from out-of-setup objects within the exposure bay, due to a lack of source collimation. These would affect the experimental results but were not included in the simulated setup. This was investigated by including different proportions of peripheral water and other objects in the modelled setup and examining the effect on Image quality parameters. Results show that this additional scatter has a significant impact on the radiograph, particularly on image contrast, and is therefore the likely cause of differences between experimental and simulated images. This implies that it will be very difficult to completely match simulated to experimental results, as including all possible scattering objects in the model would be very complex. An improvement could be made by using real subsea data to estimate this additional scattering, which could then be used to calibrate the model. However there would still be significant uncertainty in the ability of the model to accurately produce realistic intensity and contrast. KW - Digital radiography KW - Modelling validation KW - Subsea pipeline inspection KW - Tangential radiography PY - 2017 DO - https://doi.org/10.1016/j.ndteint.2016.11.006 SN - 0963-8695 SN - 1879-1174 VL - 86 SP - 113 EP - 122 AN - OPUS4-39053 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - Computersimulation in der Durchstrahlungsprüfung N2 - Vorstellung der Software "aRTist" zur Computersimulation von Durchstrahlungsprüfungen und deren Anwendungsfelder. T2 - DGZfP-Arbeitskreis Berlin, 385. Sitzung CY - Berlin, Germany DA - 07.03.2017 KW - Radiography KW - Simulation PY - 2017 AN - OPUS4-40165 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej A1 - Mansurova, Maria A1 - Kohlhoff, Harald A1 - Gkertsos, Aris A1 - Neumann, Patrick P. A1 - Bell, Jérémy A1 - Bartholmai, Matthias T1 - Wireless Mobile Sensor Device for in-situ Measurements with Multiple Fluorescent Sensors N2 - This paper describes a wireless mobile prototype able to perform optical measurements by means of a miniatur-ized spectrometer for low light analysis, e.g. fluorescent sensors. Evaluations, calculations, calibration management and result display are performed by a computer or a standard tablet. The device was designed primarily to detect traces of oil in drinking or ground water and for the analyses of crude oils. However, it can also address a wide range of fluorescent sensors. The fast and user-friendly inspection of water quality or oil properties, as well as the adaptability and mobility, make the device attractive for a variety of users. Further application areas could be easily imple-mented by adapting the optics and the software (database, data processing and calibration plots, etc.) T2 - IEEE Sensors 2018 CY - New Delhi, India DA - 28.10.2018 KW - Wireless mobile sensor device KW - Fluorescent sensor KW - Embedded system KW - Water quality KW - Oil PY - 2018 SN - 978-1-5386-4707-3 SP - 1067 EP - 1070 PB - IEEE CY - New Delhi, India AN - OPUS4-46556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Investigations of biofilms in various conditions by near-ambient pressure XPS N2 - X-ray photoelectron spectroscopy (XPS) provides elemental and chemical information from the outermost ~10 nm of the sample surface. This is in the same order of magnitude as the thickness of the outer bacterial membrane of gram-negative bacteria, as well as outer membrane molecules as exopolysaccharides and lipopolysaccharides, commonly attached to the cell surface. With the development of near-ambient pressure (NAP)-XPS, bacteria can be analysed with minimal sample preparation. EnviroESCA is a laboratory based NAP-XPS instrument, equipped with a monochromated Al Kα radiation source and a differentially pumped energy analyser connected to an exchangeable sample environment. It allows for measurements in various gas-atmospheres, including water vapor, which makes it possible to characterise bacteria and other biological samples close to their natural, hydrated state. Artificial model-biofilms of exopolysaccharides, planktonic Pseudomonas Fluorescens and biofilms of Escherichia Coli have been characterised in hydrated and dried state. High-resolution XPS-spectra from carbon, oxygen, nitrogen and phosphorous can be assigned to carbohydrates, lipids and proteins in general agreement with literature. Especially the carbon 1s peak is of interest. A series of measurements of an E. coli biofilm from 11 mbar in humid environment to 1 mbar air reveal changes in the C1s peak, which suggests that the bacterial surface undergo substantial Change. T2 - BAM PhD-retreat CY - Warnemünde, Germany DA - 28.09.2018 KW - Biofilms KW - E. coli KW - NAP-XPS PY - 2018 AN - OPUS4-46132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian T1 - The TomoSynth module for the simulation of complex and noisy scanning trajectories in aRTist N2 - Simulation becomes more and more important in modern CT imaging. It is increasingly used to optimize techniques for complex applications, to support the preparation of written procedures, and for educational purposes. The radiographic simulator aRTist is a modelling tool which simulates X-ray imaging using a hybrid analytical and Monte Carlo method to efficiently model the radiation transport. In addition to the relevant physical effects such as absorption, scattering and fluorescence, simplified fast models are employed to describe the characteristics of the X-ray source and the detector. aRTist is well equipped to model realistic X-ray imaging setups due to the ability to load exported CAD object descriptions. A simple CT scan module is contained in aRTist which allows the simulation of standard (circular cone beam) scanning trajectories. TomoSynth is a module for aRTist which allows to set up more complex scanning trajectories by attaching geometrical modification functions to the objects in the radiographic scene. In this way, advanced scanning modes can be realized, for instance helical CT as an overlay of a rotation and a linear motion, or laminography as a motion of the source point. In addition to deterministic motion, also random variations can be introduced. By combining random variations with deterministic motion, non-ideal (realistic) CT scan geometries can be simulated, e.g. focal spot drift and mechanical instability of the axis of rotation. The TomoSynth module conveniently allows to construct these scenarios in a graphical interface and provides a preview before starting the (potentially long running) batch job. Therefore, deviations from ideal CT scan trajectories can be easily adjusted which is a necessary step towards uncertainty determination from simulation. T2 - dXCT 2018 CY - Nottingham, UK DA - 02.07.2018 KW - Simulation KW - Tomography KW - aRTist KW - X-ray PY - 2018 AN - OPUS4-46428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej T1 - Wireless Mobile Sensor Device for in-situ Measurements with Multiple Fluorescent Sensors N2 - This paper describes a wireless mobile prototype able to perform optical measurements by means of a miniaturized spectrometer for low light analysis, e.g. fluorescent sensors. Evaluations, calculations, calibration management and result display are performed by a computer or a standard tablet. The device was designed primarily to detect traces of oil in drinking or ground water and for the analyses of crude oils. However, it can also address a wide range of fluorescent sensors. The fast and user-friendly inspection of water quality or oil properties, as well as the adaptability and mobility, make the device attractive for a variety of users. Further application areas could be easily implemented by adapting the optics and the software (database, data processing and calibration plots, etc.). T2 - IEEE Sensors 2018 CY - New Delhi, India DA - 28.10.2018 KW - Wireless mobile sensor device KW - Fluorescent sensor KW - Embedded system KW - Water quality KW - Oil PY - 2018 AN - OPUS4-46554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Exploring the capabilities of NAP-XPS: Application to metal-organic frameworks, nanoparticles and biofilms N2 - Near-ambient pressure XPS makes it possible to characterise samples not compatible to ultra-high vacuum, and enables the study of liquid-solid, gas-liquid and gas-solid interfaces. NAP-XPS meas-urements of biofilms, suspended nanoparticles and metal-organic frameworks were performed with EnviroESCA developed by SPECS. An interesting application is surface characterisation of biofilms, which are bacterial communities embedded in a self-produced polysaccharide matrix. Various model systems ranging from pure polysaccharides of alginate to biofilms harvested directly from the growth medium have been char-acterised in humid conditions[1]. NAP-XPS also makes it possible to characterise nanoparticles in solution. Silver nanoparticles in aqueous solution were characterised and the Ag 3d-spectrum compared to spectra obtained of dried nanoparticles in UHV-conditions[2]. The binding energy of the Ag 3d-core level peak was shifted by 0,6 eV towards higher binding energy for suspended nanoparticles compared to the dried sample measured in UHV. This can be assigned to a change in surface potential at the water-nanoparticle interface. Metal-organic frameworks (MOFs) are suitable materials for gas storage of small molecules due to their nanoporous, crystalline structure. However, instability in humidity remains an issue for many types of MOFs. XPS-measurements of the MOF-structure HKUST-1 were performed in various NAP-conditions to assess the stability of the sample and its interaction with the gas molecules as water, methanol and pyridine. T2 - 5th AP-XPS Workshop CY - Berlin, Germany DA - 11.12.18 KW - Biofilms KW - E. coli KW - NAP-XPS KW - Metal organic frameworks KW - Nanoparticles PY - 2018 AN - OPUS4-47060 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - Virtual CT with Complex scanning trajectories in aRTist N2 - The simulator aRTist combines analytical and Monte Carlo methods to efficiently model the radiographic process of industrial radiology. In this contribution we focus on virtual computer tomography, the simulation of tomographic scans. The possibilities to simulate complex scanning trajectories are shown in combination with the tomographic reconstruction using individual projection matrices. T2 - The 4th Annual Advances in X-Ray Imaging Workshop CY - Diamond Light Source, Didcot, UK DA - 11.06.2019 KW - X-ray Computer-tomography simulation PY - 2019 AN - OPUS4-48297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Depth-dependent analysis of model biofilms by combining laboratory- and synchrotron-based X-ray photoelectron spectroscopy N2 - Synchrotron XPS in the soft-X-ray regime is suitable for the detection of light elements commonly found in biological samples. Various model systems of biofilms have been developed and characterised at synchrotron- and lab-based facilities. By obtaining the chemical composition at various information depths, the vertical distribution of iodine in an artificial biofilm have been determined. T2 - Tenth Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 05.12.2018 KW - Biofilms KW - HAXPES KW - XPS KW - Iodine KW - Synchrotron-XPS PY - 2018 AN - OPUS4-46929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bellon, Carsten T1 - Virtual CT acquisition and reconstruction of complex and noisy scanning trajectories in aRTist N2 - In modern CT imaging, simulation has become an important tool to minimize cost- and time-intensive measurements. It is increasingly used to optimize techniques for complex applications, to support the preparation of written procedures, and for educational purposes. We extended the CT simulation software ‘aRTist’ with a module to set-up arbitrary trajectories including disturbing influences during the scan. Moreover, such geometric deviations can be compensated by the internal reconstruction tool. T2 - 9th Conference on Industrial Computed Tomography (iCT) CY - Padua, Italy DA - 13.02.2019 KW - Simulation KW - Arbitrary trajectories KW - Projection matrix KW - Filtered back projection PY - 2019 AN - OPUS4-47476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaenisch, Gerd-Rüdiger A1 - Wieder, Frank A1 - Vogel, Justus A1 - Ewert, Uwe A1 - Bellon, Carsten A1 - Messerschmid, Magdalena ED - Xu, C. T1 - Scatter imaging – Simulation of aperture focusing by deconvolution N2 - X-ray scatter imaging is a well-established NDT technique to inspect complex objects using only a single-sided access. We present a specially designed multi-slit scatter camera consisting of several twisted slits which are parallelly arranged in a metal block. The camera projects one image per slit to the digital detector array, where the images are overlaying each other. The aperture is corrected based on a de-convolution algorithm to focus the overlaying projections into a single representation of the object. To achieve high scatter intensities from an object, it is necessary to optimize the parameters of the scatter system by simulation. T2 - IEEE Far East NDT New Technology & Application Forum CY - Xi'an, China DA - 22.06.2017 KW - Scatter imaging KW - Computer simulation KW - Aperture focusing KW - Deconvolution PY - 2018 SN - 978-1-5386-1615-4 DO - https://doi.org/10.1109/FENDT.2017.8584606 SP - 301 EP - 306 PB - IEEE CY - Piscataway, NJ AN - OPUS4-48395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit T1 - Model systems and sample preparation for surface characterisation of bacteria and biofilms by near-ambient pressure XPS N2 - Bacterial samples are typically freeze dried or cryo-prepared prior to XPS analysis to allow for measurements in ultra-high vacuum (UHV). The sample environment in the near-ambient pressure (NAP) XPS instrument EnviroESCA allows for measurements in up to 15 mbar water vapor, thus, sample preparation is no longer restricted to UHV-compatible techniques. For instance, biofilms grown in medium can be transferred directly from the medium to the measurements chamber, maintaining a humid environment throughout the measurements. Considering the complexity of bacterial samples, sample preparation must be carefully considered in order to obtain meaningful and reproducible results. In this talk, various strategies for sample preparation of bacteria and biofilms for NAP-XPS measurements will be discussed. Model systems of planktonic bacteria, artificial biofilms resembling the exopolysaccharide matrix and biofilms have been characterised in various conditions. The stability and homogeneity of the samples was assessed by monitoring the C1s core level peak at different sample locations. The quality of the XPS-spectra is also influenced by the gas environment, which will be exemplified by core level spectra of P. Fluorescens acquired in air, water vapor and ultra-high vacuum. T2 - 18th European conference on applications of surface and interface analysis (ECASIA) CY - Dresden, Germany DA - 15.09.2019 KW - NAP-XPS KW - Biofilms KW - Bacteria KW - E. coli KW - XPS PY - 2019 AN - OPUS4-49189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Foroutan, F. A1 - Kyffin, B. A. A1 - Nikolaou, A. A1 - Merino-Gutierrez, J. A1 - Abrahams, I. A1 - Kanwal, N. A1 - Knowles, J. C. A1 - Smith, A. J. A1 - Smales, Glen Jacob A1 - Carta, D. T1 - Highly porous phosphate-based glasses for controlled delivery of antibacterial Cu ions prepared via sol–gel chemistry N2 - Mesoporous glasses are a promising class of bioresorbable biomaterials characterized by high surface area and extended porosity in the range of 2 to 50 nm. These peculiar properties make them ideal materials for the controlled release of therapeutic ions and molecules. Whilst mesoporous silicate-based glasses (MSG) have been widely investigated, much less work has been done on mesoporous phosphate-based glasses (MPG). In the present study, MPG in the P2O5–CaO–Na2O system, undoped and doped with 1, 3, and 5 mol% of Cu ions were synthesized via a combination of the sol–gel method and supramolecular templating. The non-ionic triblock copolymer Pluronic P123 was used as a templating agent. The porous structure was studied via a combination of Scanning Electron Microscopy (SEM), Small-Angle X-ray Scattering (SAXS), and N2 adsorption–desorption analysis at 77 K. The structure of the phosphate network was investigated via solid state 31P Magic Angle Spinning Nuclear Magnetic Resonance (31P MAS-NMR) and Fourier Transform Infrared (FTIR) spectroscopy. Degradation studies, performed in water via Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES), showed that phosphates, Ca2+, Na+ and Cu ions are released in a controlled manner over a 7 days period. The controlled release of Cu, proportional to the copper loading, imbues antibacterial properties to MPG. A significant statistical reduction of Staphylococcus aureus (S. aureus) and Escherichia coli (E. coli) bacterial viability was observed over a 3 days period. E. coli appeared to be more resistant than S. aureus to the antibacterial effect of copper. This study shows that copper doped MPG have great potential as bioresorbable materials for controlled delivery of antibacterial ions. KW - Bioresorbable Biomaterials KW - Mesoporous phosphate-based glasses KW - Synthesis KW - Degradation studies KW - X-ray scattering KW - MOUSE KW - Antibacterial properties KW - Aantimicrobial PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578101 DO - https://doi.org/10.1039/D3RA02958A VL - 13 IS - 29 SP - 19662 EP - 19673 PB - Royal Society of Chemistry AN - OPUS4-57810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, W. A1 - Schweins, R. A1 - Nöcker, B. A1 - Kohlbrecher, J. A1 - Smales, Glen Jacob A1 - Huber, K. T1 - Comparative study of the co-assembly behaviour of 3-chloro-4-hydroxy-phenylazo dyes with DTAB N2 - The co-assembly of three one-fold negatively charged 3-chloro-4-hydroxy-phenylazo dyes (Yellow, Blue and Red) with the cationic surfactant dodecyltrimethylammoniumbromide (DTAB) was studied to probe dye–DTAB binding stoichiometry and assembly morphology. For each dye, phase separation was observed above a given dye : DTAB ratio with the ratio depending on the dye. While Yellow and DTAB showed liquid/liquid phase separation above Yellow : DTAB = 1 : 1.67, crystalline dye–DTAB complexes were observed for Blue–DTAB and Red–DTAB above Blue : DTAB = 1 : 2.56 and Red : DTAB = 1 : 2.94 respecively. In homogeneous solution, UV/vis spectroscopic investigations suggest stochiometries of Yellow : DTAB = 1 : 2, Blue : DTAB = 1 : 3 and Red : DTAB = 1 : 4. It was concluded, that Yellow exhibits the highest dye : DTAB binding stoichiometry in both, dye–surfactant complexes in the 2-phase region and in solution, whereas the lowest dye : DTAB binding stoichiometry was observed for Red–DTAB in both cases. The observed stoichiometries are inversely correlated to the impact dye addition has on the morphology of DTAB micelles. Generally, addition of dye to DTAB micelles leads to a reduction in spontaneous curvature of these micelles and to the formation of triaxial ellipsoidal or cylindrical micelles from oblate ellipsoidal DTAB micelles. At a DTAB concentration of 30 mM and a dye concentration of 5 mM, this effect was most pronounced for Red and least pronounced for Yellow, whilst Blue showed an intermediate effect. KW - Dye KW - DTAB KW - SAXS KW - Small-angle X-ray scattering KW - X-ray scattering KW - Data analysis KW - Micelle PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576978 DO - https://doi.org/10.1039/D3SM00501A SN - 1744-683X VL - 19 IS - 24 SP - 4588 EP - 4598 PB - Royal Society of Chemistry AN - OPUS4-57697 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Synthesizing a library of 1000+ reproducible MOFs N2 - While the synthesis of Metal-Organic Framework (MOF) particles can be as easy as adding two solutions together, reproducibly obtaining the same particles, time and time again, is a lot harder. As laboratory-independent reproducibility is a cornerstone of the scientific method, we must put effort into finding and controlling all necessary parameters to achieve this. An open-source Python/EPICS-controlled robotic platform (see picture) was adapted to systematically explore this for a 20 ml MOF synthesis of the Zeolitic Imidazole Framework-8 (ZIF-8) chemistry in methanol. Parameters that were explored included: 1) addition sequence, 2) addition speeds, 3) reaction times, 4) source chemicals, 5) stirring speeds, 6) stirring bar choice, 7) starting concentrations, and 8) workup methodologies. It was found that, by controlling these parameters, highly reproducible syntheses are obtained. Secondly, the variation of these parameters alone led to a dramatic difference in volume-weighted particle size means, which exceeds an order of magnitude as investigated by our in-house X-ray scattering instrument [1]. The syntheses are thoroughly documented in an automated fashion, and the synthesis libraries as well as analyses libraries will become available in batches soon. With this library, it will be possible to extract previously unknown correlations, and other laboratories can produce specific particles by following the exact procedures of the particles of their choice. T2 - 787. WE-Heraeus-Seminar: Accelerated Discovery of New Materials CY - Bad Honnef, Germany DA - 15.05.2023 KW - Metal organic frameworks KW - Automation KW - Lab automation KW - Robotic-supported synthesis KW - Reproducibility KW - Synthesis library KW - X-ray scattering KW - Particle size distribution PY - 2023 AN - OPUS4-57596 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - What’s that beyond the grasslands? Expanding your world view via wide-range X-ray scattering N2 - This talk introduces the expanded view that comes from wide-range X-ray scattering investigations. Compared to X-ray diffraction studies alone, the additional angular range of this technique provides information on the larger structural dimensions present in your samples. This allows for the extraction of information on the size and size distribution of nanostructural components, such as nanoparticles, nanovoids, and any other structure exhibiting an electron density contrast. The talk introduces the technique, the MOUSE instrument used for these investigations, and provides several real-world examples of its uses. The audience is invited to choose which examples captures their interest from a range of options, in the latter segment of the talk. T2 - ECS8: European Crystallography School 2023 CY - Berlin, Germany DA - 18.06.2023 KW - X-ray scattering KW - Introduction KW - Fourier transforms KW - Nanostructure investigation KW - Instrument automation KW - MOUSE PY - 2023 AN - OPUS4-57769 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard A1 - Breßler, Ingo T1 - 30.000+ datasets in an underground SciCat instance: the good, the bad, and the improvables. N2 - For the last four years, we have been running a SciCat instance to manage the projects and data in our X-ray scattering laboratory. We here report on the configuration of this SciCat instance, how it connects to the scientific workflow, and how it is integrated in the data pipeline. T2 - SciCat 2023 CY - Didcot, UK DA - 18.07.2023 KW - Scicat KW - X-ray scattering KW - Laboratory management KW - Research Data Management KW - Laboratory organization KW - RunDeck PY - 2023 AN - OPUS4-57958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - McSAS3: live demo of a Monte Carlo data analyis package for scattering studies N2 - McSAS3 is a refactored software package for fitting large batches of (X-ray or Neutron) scattering data. It uses a Monte-Carlo acceptance-rejection algorithm to optimize model parameters - ideal for analysis of size-disperse scatterers. The refactored code can exploit multiprocessing, traceably stores (multiple) results in the output file, and allows for re-histogramming of previous optimizations. Besides analysis of large batches, it can also be integrated in automated data processing pipelines. The live demonstration will show how to use the software, what its limitations are, and what outcomes can look like for batches of results. T2 - SAS Analysis Course 2023 CY - Didcot, UK DA - 05.06.2023 KW - Scattering KW - Software KW - Analysis KW - Demonstration KW - McSAS3 KW - MOUSE KW - Monte Carlo KW - Automated analysis PY - 2023 AN - OPUS4-57630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Plarre, Rüdiger A1 - Zocca, Andrea A1 - Spitzer, Andrea A1 - Benemann, Sigrid A1 - Gorbushina, Anna A1 - Li, Y. A1 - Waske, Anja A1 - Funk, Alexander A1 - Wilgig, Janka A1 - Günster, Jens T1 - Searching for biological feedstock material: 3D printing of wood particles from house borer and drywood termite frass N2 - Frass (fine powdery refuse or fragile perforated wood produced by the activity of boring insects) of larvae of the European house borer (EHB) and of drywood termites was tested as a natural and novel feedstock for 3D-printing of wood-based materials. Small particles produced by the drywood termite Incisitermes marginipennis and the EHB Hylotrupes bajulus during feeding in construction timber, were used. Frass is a powdery material of particularly consistent quality that is essentially biologically processed wood mixed with debris of wood and faeces. The filigree-like particles flow easily permitting the build-up of woodbased structures in a layer wise fashion using the Binder Jetting printing process. The Quality of powders produced by different insect species was compared along with the processing steps and properties of the printed parts. Drywood termite frass with a Hausner Ratio HR = 1.1 with ρBulk = 0.67 g/cm3 and ρTap = 0.74 g/cm3 was perfectly suited to deposition of uniformly packed layers in 3D printing. We suggest that a variety of naturally available feedstocks could be used in environmentally responsible approaches to scientific material sciences/additive manufacturing. KW - 3D printing KW - X-ray tomographic KW - SEM micrography KW - Drywood termite PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521517 DO - https://doi.org/10.1371/journal.pone.0246511 VL - 16 IS - 2 SP - e0246511 AN - OPUS4-52151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, Henning A1 - Sintschuk, Michael A1 - Britzke, Ralf A1 - Dayani, Shahabeddin A1 - Bruno, Giovanni T1 - Upgraded imaging capabilities at the BAMline (BESSY II) N2 - The BAMline at the BESSY II synchrotron X-ray source has enabled research for more than 20 years in widely spread research fields such as materials science, biology, cultural heritage and medicine. As a nondestructive characterization method, synchrotron X-ray imaging, especially tomography, plays a particularly important role in structural characterization. A recent upgrade of key equipment of the BAMline widens its imaging capabilities: shorter scan acquisition times are now possible, in situ and operando studies can now be routinely performed, and different energy spectra can easily be set up. In fact, the upgraded double-multilayer monochromator brings full flexibility by yielding different energy spectra to optimize flux and energy resolution as desired. The upgraded detector (based on an sCMOS camera) also allows exploiting the higher flux with reduced readout times. Furthermore, an installed slip ring allows the sample stage to continuously rotate. The latter feature enables tomographic observation of processes occurring in the time scale of a few seconds. KW - Synchrotron radiation KW - Computed tomography KW - Double-multilayer monochromators KW - Pink beams KW - X-ray optics PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556907 DO - https://doi.org/10.1107/S1600577522007342 SN - 1600-5775 VL - 29 IS - Pt 5 SP - 1292 EP - 1298 PB - International Union of Crystallography CY - Chester AN - OPUS4-55690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Z. A1 - Villa Santos, C. A1 - Legrand, A. A1 - Haase, F. A1 - Hara, Y. A1 - Kanamori, K. A1 - Aoyama, T. A1 - Urayama, K. A1 - Doherty, C. M. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Colon, Y. J. A1 - Furukawa, S. T1 - Multiscale structural control of linked metal–organic polyhedra gel by aging-induced linkage-reorganization N2 - Assembly of permanently porous metal–organic polyhedra/cages (MOPs) with bifunctional linkers leads to soft supramolecular networks featuring both porosity and processability. However, the amorphous nature of such soft materials complicates their characterization and thus limits rational structural control. Here we demonstrate that aging is an effective strategy to control the hierarchical network of supramolecular gels, which are assembled from organic ligands as linkers and MOPs as junctions. Normally, the initial gel formation by rapid gelation leads to a kinetically trapped structure with low controllability. Through a controlled post-synthetic aging process, we show that it is possible to tune the network of the linked MOP gel over multiple length scales. This process allows control on the molecular-scale rearrangement of interlinking MOPs, mesoscale fusion of colloidal particles and macroscale densification of the whole colloidal network. In this work we elucidate the relationships between the gel properties, such as porosity and rheology, and their hierarchical structures, which suggest that porosity measurement of the dried gels can be used as a powerful tool to characterize the microscale structural transition of their corresponding gels. This aging strategy can be applied in other supramolecular polymer systems particularly containing kinetically controlled structures and shows an opportunity to engineer the structure and the permanent porosity of amorphous materials for further applications. KW - SAXS KW - Metal-organic polyhedra KW - Structural control PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532309 DO - https://doi.org/10.1039/d1sc02883a SN - 1478-6524 SN - 1742-2183 VL - 12 IS - 38 SP - NIL_1 EP - NIL_9 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-53230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Enhancing your SAXS with interleaved USAXS for less than 50 k€ N2 - A portable, inexpensive module is presented that can enhance good existing SAXS instruments by offering an extension on the angular range to include the ultra-small-angles. The instrument has been shown to work for interleaved SAXS/USAXS experiments. T2 - XVII International Small Angle Scattering Conference - SAS2018 CY - Traverse City, Michigan, USA DA - 07.10.2018 KW - Small-angle scattering KW - USAXS KW - Bonse Hart KW - Instrumentation KW - Data analysis PY - 2018 AN - OPUS4-46519 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Marc Benjamin A1 - Smales, Glen Jacob A1 - Seitz, H. A1 - Solomun, Tihomir A1 - Sturm, Heinz T1 - Ectoine interaction with DNA: Influence on ultraviolet radiation damage N2 - Ectoine is a small zwitterionic osmolyte and compatible solute, which does not interfere with cell metabolism even at molar concentrations. Plasmid DNA (pUC19) was irradiated with ultraviolet radiation (UV-C at 266 nm) under quasi physiological conditions (PBS) and in pure water in the presence and absence of ectoine (THP(B)) and hydroxyectoine (THP(A)). Different types of UV induced DNA damage were analysed: DNA single-strand breaks (SSBs), abasic sites and cyclobutane pyrimidine dimers (CPDs). A complex interplay between these factors was observed with respect to the nature and occurrence of DNA damage with 266 nm photons. In PBS, the cosolutes showed efficient protection against base damage, whilst in pure water, a dramatic shift from SSB damage to base damage was observed when cosolutes were added. To test whether these effects are caused by ectoine binding to DNA, further experiments were conducted: small-angle X-ray scattering (SAXS), surface-plasmon resonance (SPR) measurements and Raman spectroscopy. The results show, for the first time, a close interaction between ectoine and DNA. This is in stark contrast to the assumption made by preferential exclusion models, which are often used to interpret the behaviour of compatible solutes within cells and with biomolecules. It is tentatively proposed that the alterations of UV damage to DNA are attributed to ectoine influence on nucleobases through the direct interaction between ectoine and DNA. KW - Ectoine KW - DNA KW - Radiation damage KW - Radiation protection KW - SSB KW - DNA damage KW - DNA protection KW - Compatible solute KW - Zwitterion KW - Hydroxyectoine KW - Salt KW - PBS KW - UV absorption KW - DNA strand-break KW - DNA base damage KW - Ectoine UV absorption KW - Ectoine DNA protection KW - Excited states KW - UV irradiation KW - UV-A KW - UV-B KW - UV-C KW - 266nm KW - UV photons KW - Ectoine-DNA binding KW - Raman spectroscopy KW - UV-Vis KW - Radical scavenger KW - OH scavenger KW - Hydroxyl radicals KW - CPD KW - Abasic site KW - Agarose gel electrophorese KW - SYBR gold KW - DNA melting temperature KW - Counterions KW - Preferential exclusion KW - Cancer KW - Therapy KW - UV protection KW - Sunscreen PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505772 DO - https://doi.org/10.1039/d0cp00092b SN - 1463-9076 SN - 1463-9084 VL - 22 IS - 13 SP - 6984 EP - 6992 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-50577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yildirim, Arda A1 - Sentker, K. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Huber, P. A1 - Schönhals, Andreas T1 - Collective orientational order and phase behavior of a discotic liquid crystal under nanoscale confinement N2 - The phase behavior and molecular ordering of hexakishexyloxy triphenylene (HAT6) DLC under cylindrical nanoconfinement is studied utilizing differential scanning calorimetry (DSC) and dielectric spectroscopy (DS), where cylindrical nanoconfinement is established through embedding HAT6 into the nanopores of anodic aluminum oxide membranes (AAO), and a silica membrane with pore diameters ranging from 161 nm down to 12 nm. Both unmodified and modified pore walls were considered, and in the latter case the pore walls of AAO membranes were chemical treated with n octadecylphosphonic acid (ODPA) resulting in the formation of a 2.2 nm thick layer of grafted alkyl chains. Phase transition enthalpies decrease with decreasing pore size, indicating that a large proportion of the HAT6 molecules within the pores has a disordered structure, which increases with decreasing pore size for both pore walls. In the case of the ODPA modification the amount of ordered HAT6 is increased compared to the unmodified case. The pore size dependencies of the phase transition temperatures were approximated using the Gibbs Thomson equation, where the estimated surface tension is dependent on the molecular ordering of HAT6 molecules within the pores and upon their surface. DS was employed to investigate the molecular ordering of HAT6 within the nanopores. These investigations revealed that with a pore size of around 38 nm, for the samples with the unmodified pore walls, the molecular ordering changes from planar axial to homeotropic radial. However, the planar axial configuration, which is suitable for electronic applications, can be successfully preserved through ODPA modification for most of the pore sizes. KW - Discotic Liquid Crystals KW - Nanoconfinement PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475222 DO - https://doi.org/10.1039/c8na00308d SN - 2516-0230 VL - 1 IS - 3 SP - 1104 EP - 1116 PB - RSC AN - OPUS4-47522 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Shebanova, O. A1 - Sutter, J. P. A1 - Ilavsky, J. A1 - Hermida-Merino, D. A1 - Smales, Glen Jacob A1 - Terrill, N. J. A1 - Thünemann, Andreas A1 - Bras, W. T1 - Extending SAXS instrument ranges through addition of a portable, inexpensive USAXS module N2 - Ultra-SAXS can enhance the capabilities of existing SAXS/WAXS beamlines and laboratory instruments. A compact Ultra-SAXS module has been developed, which extends the measurable q-range with 0:0015 < q 1/nm) < 0:2, allowing structural dimensions between 30 < D(nm) < 4000 to be probed in addition to the range covered by a high-end SAXS/WAXS instrument. By shifting the module components in and out on their respective motor stages, SAXS/WAXS measurements can be easily and rapidly interleaved with USAXS measurements. KW - Small-angle scattering PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504867 DO - https://doi.org/10.48550/arXiv.1904.00080 SN - 2331-8422 SP - 1 EP - 25 PB - Cornell University CY - Ithaca, NY AN - OPUS4-50486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fletcher, D. C. A1 - Hunter, R. A1 - Xia, W. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Blackburn, E. A1 - Kulak, A. A1 - Xin, H. A1 - Schnepp, Z. T1 - Scalable synthesis of dispersible iron carbide (Fe3C) nanoparticles by ‘nanocasting’ N2 - Metal carbides have shown great promise in a wide range of applications due to their unique catalytic, electrocatalytic and magnetic properties. However, the scalable production of dispersible metal carbide nanoparticles remains a challenge. Here, we report a simple and scalable route to dispersible iron carbide (Fe3C) nanoparticles. This uses MgO nanoparticles as a removable ‘cast’ to synthesize Fe3C nanoparticles from Prussian blue (KFeIII[FeII(CN)6]). Electron tomography demonstrates how nanoparticles of the MgO cast encase the Fe3C nanoparticles to prevent sintering and agglomeration during the high-temperature synthesis. The MgO cast is readily removed with ethylenediaminetetraacetic acid (EDTA) to generate Fe3C nanoparticles that can be used to produce a colloidal ferrofluid or dispersed on a support material. KW - Small-angle scattering KW - SAXS KW - Metal carbides KW - Nanoparticles KW - Nanocasting PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-486295 DO - https://doi.org/10.1039/C9TA06876G SN - 2050-7488 SN - 2050-7496 VL - 7 IS - 33 SP - 19506 EP - 19512 PB - Royal Society of Chemistry (RSC) AN - OPUS4-48629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Experimenting on MAUS N2 - Initial results, findings and experience after 1.5 years of using the Multi-scale Analyser for Ultrafine Structures (MAUS), a bespoke wide-range SAXS instrument for the nanostructure quantification of demanding materials science samples. T2 - S4SAS Conference 2019 CY - Diamond Light Source, Didcot, UK DA - 06.06.2019 KW - X-ray scattering KW - SAXS KW - Nanostructure quantification KW - Nanocharacterisation PY - 2019 AN - OPUS4-48193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Smales, Glen Jacob T1 - THE MAUS: A GI-/ULTRA-/W/SAXS Instrument of the future N2 - The Multi-scale Analyzer for Ultrafine Structures or the “MAUS” for short, is a SAXS instrument that combines a multitude of features that make it both unique, and one of the most adaptable instruments around. T2 - SAS2018 CY - Traverse City, MI, USA DA - 07.10.2018 KW - SAXS KW - MAUS KW - Small-angle scattering KW - DAWN KW - Grazing incidence PY - 2018 AN - OPUS4-46523 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friberg, I. A1 - Clark, A. H. A1 - Ho, P. A1 - Sadokhina, N. A1 - Smales, Glen Jacob A1 - Woo, J. A1 - Auray, X. A1 - Ferri, D. A1 - Nachtegaal, M. A1 - Krocher, O. A1 - Olsson, L. T1 - Structure and performance of zeolite supported Pd for complete methane oxidation N2 - The influence of zeolite support materials and their impact on CH4 oxidation activity was studied utilizing Pd supported on H-beta and H-SSZ-13. A correlation between CH4 oxidation activity, Si/Al ratio (SAR), the type of zeolite framework, reduction-oxidation behaviour, and Pd species present was found by combining catalytic activity measurements with a variety of characterization methods (operando XAS, NH3-TPD, SAXS, STEM and NaCl titration). Operando XAS analysis indicated that catalysts with high CH4 oxidation activity experienced rapid transitions between metallic- and oxidized-Pd states when switching between rich and lean conditions. This behaviour was exhibited by catalysts with dispersed Pd particles. By contrast, the formation of ion-exchanged Pd2+ and large Pd particles appeared to have a detrimental effect on the oxidation-reduction behaviour and the conversion of CH4. The formation of ion-exchanged Pd2+ and large Pd particles was limited by using a highly siliceous beta zeolite support with a low capacity for cation exchange. The same effect was also found using a small-pore SSZ-13 zeolite due to the lower mobility of Pd species. It was found that the zeolite support material should be carefully selected so that the well-dispersed Pd particles remain, and the formation of ion-exchanged Pd2+ is minimized. KW - SAXS KW - Zeolites KW - Methane Oxidation KW - XAS KW - Catalysis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529606 DO - https://doi.org/10.1016/j.cattod.2020.11.026 VL - 382 SP - 3 EP - 12 PB - Elsevier B.V. AN - OPUS4-52960 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Prause, A. A1 - Hormann, A. A1 - Cristiglio, V. A1 - Smales, Glen Jacob A1 - Thünemann, Andreas A1 - Gradzielski, M. A1 - Findenegg, G. H. T1 - Incorporation and structural arrangement of microemulsion droplets in cylindrical pores of mesoporous silica N2 - The behaviour of microemulsion (ME) droplets in mesoporous systems is highly important for understanding the immobilisation of drugs or chemical formulations, cleaning processes or enhanced oil recovery. The loading of pores as well as the structural organisation of MEs within the pores is a relevant parameter, especially for immobilisation applications. For this reason, the uptake of microemulsions in cylindrical pores of SBA-15 was investigated via adsorption and small-angle neutron scattering (SANS). Adsorption isotherms revealed an adsorption of the microemulsion droplets based on the adsorption of surfactant as a driving force. The adapted scattering model is based on the analysis of bare SBA-15 in full contrast conditions and employs microemulsions inside of SBA-15 measured at the silica contrast matching point. Accordingly, the structural arrangement of microemulsion droplets in the pores of SBA-15 was determined in good detail. Microemulsion droplets smaller than the pore size access the pores while retaining their spherical shape and become increasingly ordered for higher loading, where the droplets arrange in a dense packing of spherical droplets in a cylindrical pore. Interestingly, microemulsion droplets larger than the pore size can easily be incorporated, but become deformed upon entering and are present as elongated rod-like structures. KW - Mesoporous Silica KW - SAXS KW - Microemulsion PY - 2021 DO - https://doi.org/10.1080/00268976.2021.1913255 VL - 119 IS - 15-16 SP - 13255 PB - Taylor & Francis AN - OPUS4-52959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauw, Brian Richard A1 - Smith, A. J. A1 - Snow, T. A1 - Shebanova, O. A1 - Sutter, J. P. A1 - Ilavsky, J. A1 - Hermida-Merino, D. A1 - Smales, Glen Jacob A1 - Terrill, N. J. A1 - Thünemann, Andreas A1 - Bras, W. T1 - Extending synchrotron SAXS instrument ranges through addition of a portable, inexpensive USAXS module with vertical rotation axes N2 - Ultra-SAXS can enhance the capabilities of existing synchrotron SAXS/WAXS beamlines. A compact ultra-SAXS module has been developed, which extends the measurable q-range with 0.0015 ≤ q (nm−1) ≤ 0.2, allowing structural dimensions in the range 30 ≤ D (nm) ≤ 4000 to be probed in addition to the range covered by a high-end SAXS/WAXS instrument. By shifting the module components in and out on their respective motor stages, SAXS/WAXS measurements can be easily and rapidly interleaved with USAXS measurements. The use of vertical crystal rotation axes (horizontal diffraction) greatly simplifies the construction, at minimal cost to efficiency. In this paper, the design considerations, realization and synchrotron findings are presented. Measurements of silica spheres, an alumina membrane, and a porous carbon catalyst are provided as application examples. KW - X-ray scattering KW - Microstructure KW - Instrumentation KW - SAXS KW - USAXS KW - Nanostructure KW - Combined techniques PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524919 DO - https://doi.org/10.1107/S1600577521003313 SN - 1600-5775 VL - 28 IS - 3 SP - 824 EP - 833 PB - Wiley CY - Oxford AN - OPUS4-52491 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Saloga, Patrick E. J. A1 - Smales, Glen Jacob A1 - Clark, Adam H. A1 - Thünemann, Andreas T1 - Zinc Phosphate Nanoparticles Produced in Saliva N2 - This paper reports the formation of zinc phosphate nanoparticles from the artificial digestion of zinc chloride. Initially, the formation of amorphous primary particles with a mean radius of 1.1 nm is observed, alongside the formation of larger, protein stabilized aggregates. These aggregates, with a radius of gyration of 37 nm, are observed after 5 minutes of exposure to artificial saliva and are shown to be colloidally stable for a minimum time of two weeks. The initially formed primary particles are thought to consist of amorphous zinc phosphate, which is then transformed into crystalline Zn3(PO4)2·4H2O over the course of two weeks. Our results demonstrate that the interaction of inorganic salts with bodily fluids can induce the formation of de novo nanoparticles, which in turn, provides insights into how zinc‐enriched foods may also facilitate the formation of nanoparticles upon contact with saliva. As such, this may be considered as an undesirable (bio)mineralization. KW - SAXS KW - Digestion KW - Zinc phosphate PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514239 DO - https://doi.org/10.1002/ejic.202000521 IS - 38 SP - 3654 EP - 3661 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-51423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - How to manage a modern X-ray scattering lab – a modest example N2 - Introduction A good laboratory organization can help address the reproducibility crisis in science, and easily multiply the scientific output of a laboratory, while greatly elevating the quality of the measurements. We have demonstrated this for small- and wide-angle X-ray scattering in the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration). In the MOUSE, we have combined: a) a comprehensive laboratory workflow with b) a heavily modified, highly automated X-ray scattering instrument. This combination allows us to collect fully traceable scattering data, with a well-documented data flow (akin to what is found at the more automated beamlines). With two full-time researchers, the lab collects and interprets thousands of datasets, on hundreds of samples for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data. While these numbers do not light a candle to those achieved by our hardworking compatriots at the synchrotron beamlines, the laboratory approach does allow us to continually modify and fine-tune the integral methodology. So for the last three years, we have incorporated e.g. FAIR principles, traceability, automated processing, data curation strategies, as well as a host of good scattering practices into the MOUSE system. We have concomitantly expanded our purview as specialists to include an increased responsibility for the entire scattering aspect of the resultant publications. This ensures full exploitation of the data quality, whilst avoiding common pitfalls. Talk scope This talk will present the MOUSE project as implemented to date, and will introduce foreseeable upgrades and changes. These upgrades include better pre-experiment sample scattering predictions to filter projects on the basis of their suitability, exploitation of the measurement database for detecting long-term changes and automated flagging of datasets, extending the measurement range through an Ultra-SAXS module, and enhancing MC fitting with sample scattering simulations for better matching of odd-shaped scatterers. T2 - 2021 joint virtual meeting of the African Light Source (AfLS), the African Physical Society (AfPS), and Pan African Conference on Crystallography (ePCCr) CY - Online meeting DA - 15.11.2021 KW - X-ray scattering KW - MOUSE KW - Instrumentation KW - SAXS KW - Methodology KW - Laboratory management KW - Databases KW - Data management KW - Data catalog KW - Scicat PY - 2021 UR - https://events.saip.org.za/event/170/contributions/7619/ AN - OPUS4-53811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stawski, Tomasz A1 - Smales, Glen Jacob A1 - Scoppola, E. A1 - Jha, D. A1 - Morales, L. F. G. A1 - Moya, A. A1 - Wirth, R. A1 - Pauw, Brian Richard A1 - Emmerling, Franziska A1 - Van Driessche, A. E. S. T1 - Seeds of imperfection rule the mesocrystalline disorder in natural anhydrite single crystals N2 - In recent years, we have come to appreciate the astounding intricacies associated with the formation of minerals from ions in aqueous solutions. In this context, a number of studies have revealed that the nucleation of calcium sulfate systems occurs nonclassically, involving the aggregation and reorganization of nanosized prenucleation species. In recent work, we have shown that this particle-mediated nucleation pathway is actually imprinted in the resultant micrometer-sized CaSO4 crystals. This property of CaSO4 minerals provides us with the unique opportunity to search for evidence of nonclassical nucleation pathways in geological environments. In particular, we focused on large anhydrite Crystals extracted from the Naica Mine in Mexico. We were able to shed light on this mineral's growth history by mapping defects at different length scales. Based on this, we argue that the nanoscale misalignment of the structural subunits, observed in the initial calcium sulfate crystal seeds, propagates through different length scales both in morphological, as well as in strictly crystallographic aspects, eventually causing the formation of large mesostructured single crystals of anhydrite. Hence, the nonclassical nucleation mechanism introduces a “seed of imperfection,” which leads to a macroscopic “single” crystal whose fragments do not fit together at different length scales in a self-similar manner. Consequently, anisotropic voids of various sizes are formed with very welldefined walls/edges. However, at the same time, the material retains in part its single crystal nature. KW - Calcium sulfate KW - Anhydrite KW - Mesocrystal KW - Nucleation KW - Naica PY - 2021 DO - https://doi.org/10.1073/pnas.2111213118 SN - 0027-8424 VL - 118 IS - 48 SP - 1 EP - 11 PB - National Academy of Sciences (USA) CY - Washington AN - OPUS4-53820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Better with Scattering Part 1: Fundamentals of X-ray scattering N2 - Today's speaker is a young scientist whose research on all aspects of small-angle scattering has taken him from his birthplace in Netherlands, to Denmark, Japan and now Germany. His research has led to a new method and software for scattering pattern analysis, a comprehensive set of data corrections together with the Diamond Light Source, and a new ultra-SAXS plug-in instrument. For the last few years, he has been working on a comprehensive and universal methodology to get high-quality X-ray scattering measurements for any sample, using his new instrument at the institute. This instrument has now been heavily modified both in hardware and software, so that it can deliver better data. These developments are always driven by interesting collaborations with materials researchers and other scientists. As a joint member he has published works on a wide variety of materials, including self-assembled structures in liquids, composite materials and porous carbon catalysts. He has also been very active in outreach, for example by co-organizing an online lecture series called ‘#the Light Stuff’ on scattering and diffraction, running the ‘looking at nothing’ weblog, hosting a yearly introductory scattering course, and he has many scattering-related lectures available on YouTube. Our distinguished speaker is Dr. Brian Richard Pauw from the Federal Institute for Materials Research and Testing in Germany. I proudly invite Dr. Pauw to begin his talk T2 - The first training course on the principles & application of X-ray scattering in nanomaterials CY - Online meeting DA - 28.04.2021 KW - X-ray scattering KW - Methodology KW - MOUSE KW - Introduction KW - Theory PY - 2021 AN - OPUS4-53275 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Better with Scattering Part 2: Nanostructural investigations with X-ray scattering N2 - Today's speaker is a young scientist whose research on all aspects of small-angle scattering has taken him from his birthplace in Netherlands, to Denmark, Japan and now Germany. His research has led to a new method and software for scattering pattern analysis, a comprehensive set of data corrections together with the Diamond Light Source, and a new ultra-SAXS plug-in instrument. For the last few years, he has been working on a comprehensive and universal methodology to get high-quality X-ray scattering measurements for any sample, using his new instrument at the institute. This instrument has now been heavily modified both in hardware and software, so that it can deliver better data. These developments are always driven by interesting collaborations with materials researchers and other scientists. As a joint member he has published works on a wide variety of materials, including self-assembled structures in liquids, composite materials and porous carbon catalysts. He has also been very active in outreach, for example by co-organizing an online lecture series called ‘#the Light Stuff’ on scattering and diffraction, running the ‘looking at nothing’ weblog, hosting a yearly introductory scattering course, and he has many scattering-related lectures available on YouTube. Our distinguished speaker is Dr. Brian Richard Pauw from the Federal Institute for Materials Research and Testing in Germany. I proudly invite Dr. Pauw to begin his talk. T2 - The first training course on the principles & application of X-ray scattering in nanomaterials CY - Online meeting DA - 28.04.2021 KW - X-ray scattering KW - Methodology KW - MOUSE KW - Practical examples KW - Automation KW - Data organization PY - 2021 AN - OPUS4-53276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Smales, Glen Jacob T1 - Introduction to SAXS N2 - A simplified introductions to small-angle scattering (SAXS), to put across the main concepts and not get bogged down in equations. T2 - Better with Scattering workshop 2020 CY - BAM, Berlin, Germany DA - 16.03.2020 KW - SAXS KW - WAXS KW - MOFs KW - Data analysis KW - Nano PY - 2020 UR - https://www.youtube.com/watch?v=_YY9XtQfANk AN - OPUS4-51021 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - More of the same, please! Standardizing a perfectionist X-ray Scattering methodology for labs and synchrotrons N2 - After a colleague sent me a more useful measurement from a laboratory instrument than what I could get from the beamline, I knew it was time to reassess my life's choices. Over the course of several subsequent post-doc and permanent positions around lab instruments, I managed to refine a flexible, comprehensive methodology for data collection, correction and analysis which can be applied to many X-ray scattering investigations at the lab and at the synchrotron. With the help of friends at round places, this methodology was implemented and put into production, and has been delivering high-quality data since then. Now, we have almost all possible data corrections (for X-ray scattering) implemented, and are improving the hardware to deliver higher-quality metadata to enable the corrections to be performed to a higher accuracy. Simultaneously, we have set up a mini-large facility at BAM with the MAUS, the Multi-scale Analyzer for Ultrafine Structures. The MAUS combines the freedom of a laboratory instrument, with the spectrum of users of a beamline: besides measuring our own samples, and performing our own machine and methodology developments, we have opened this instrument for collaboration with fellow scientists from within BAM and from external institutes and universities. Here, we provide a comprehensive support for these collaborations, guiding the user from concept to sample selection, to interpretation and analysis. In 2019, we have supported over 30 different projects this way, leading to seven co-authored publications involving the MAUS in that year alone. As the MAUS uses the latest iteration of our comprehensive measurement methodology, the data quality is unmatched by any other lab instrument, and fully traceable to boot. The freedom of the laboratory allows for more proof-of-principle experimentation than what is possible at the synchrotron. Therefore, the MAUS provides a good first (and sometimes final) step towards many experimental materials science investigations, nicely complementing the capabilities of the synchrotron. If and when more flux is needed, the step to the synchrotron is now smaller than ever, in particular with the same method T2 - Symposium on large scale facilities CY - BAM, Berlin, Germany DA - 09.03.2020 KW - Small angle scattering KW - Methodology KW - X-ray scattering PY - 2020 AN - OPUS4-51014 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - The Meticulous Approach: Fully traceable X-ray scattering data via a comprehensive lab methodology N2 - To find out if experimental findings are real, you need to be able to repeat them. For a long time, however, papers and datasets could not necessarily include sufficient details to accurately repeat experiments, leading to a reproducibility crisis. It is here, that the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration) tries to implement change – at least for small- and wide-angle X-ray scattering (SAXS/WAXS). In the MOUSE project, we have combined: a) a comprehensive laboratory workflow with b) a heavily modified, highly automated Xenocs Xeuss 2.0 instrumental component. This combination allows us to collect fully traceable scattering data, with a well-documented data flow (akin to what is found at the more automated beamlines). With two full-time researchers, the lab collects and interprets thousands of datasets, on hundreds of samples for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data. While these numbers do not light a candle to those achieved by our hardworking compatriots at the synchrotron beamlines, the laboratory approach does allow us to continually modify and fine-tune the integral methodology. So for the last three years, we have incorporated e.g. FAIR principles, traceability, automated processing, data curation strategies, as well as a host of good scattering practices into the MOUSE system. We have concomitantly expanded our purview as specialists to include an increased responsibility for the entire scattering aspect of the resultant publications, to ensure full exploitation of the data quality, whilst avoiding common pitfalls. This talk will discuss the MOUSE project1 as implemented to date, and will introduce foreseeable upgrades and changes. These upgrades include better pre-experiment sample scattering predictions to filter projects on the basis of their suitability, exploitation of the measurement database for detecting long-term changes and automated flagging of datasets, and enhancing MC fitting with sample scattering simulations for better matching of odd-shaped scatterers. T2 - S4SAS CY - Online meeting DA - 01.09.2021 KW - X-ray scattering KW - Methodology KW - MOUSE KW - Data organization KW - Automation KW - Traceability PY - 2021 AN - OPUS4-53273 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Smales, Glen Jacob T1 - Structural characterization using small-angle X-ray scattering (SAXS) N2 - A short introduction to small-angle scattering, followed by a "choose your own adventure" style of talk on the characterisation of different materials using SAXS/WAXS. T2 - Operando workshop “SAXS and Ptychography” at the Paul Scherrer Institut CY - Villigen, Switzerland DA - 17.08.2021 KW - SAXS KW - Materials KW - Characterisation PY - 2021 AN - OPUS4-53188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - Complete set of raw and processed datasets, as well as associated Jupyter notebooks for analysis, associated with manuscript entitled: "The MOUSE project: a practical approach for obtaining traceable, wide-range X-ray scattering information" N2 - This dataset is a complete set of raw, processed and analyzed data, complete with Jupiter notebooks, associated with the manuscript mentioned in the title. In the manuscript, we provide a "systems architecture"-like overview and detailed discussions of the methodological and instrumental components that, together, comprise the "MOUSE" project (Methodology Optimization for Ultrafine Structure Exploration). Through this project, we aim to provide a comprehensive methodology for obtaining the highest quality X-ray scattering information (at small and wide angles) from measurements on materials science samples. KW - X-ray scattering KW - Measurement methodology KW - Traceability derivation KW - Multi-scale measurements KW - Systems architecture KW - Nanomaterials PY - 2020 DO - https://doi.org/10.5281/zenodo.4312953 PB - Zenodo CY - Geneva AN - OPUS4-51825 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - The SPONGE N2 - This software tool is intended to calculate X-ray scattering patterns from 3D objects described by an STL file. The fundamentals and use example(s) are shown. T2 - Better with Scattering workshop 2020 CY - BAM, Berlin, Germany DA - 16.03.2020 KW - Small angle scattering KW - Software KW - Simulation PY - 2020 AN - OPUS4-51020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard T1 - The MOUSE project - A meticulous approach for obtaining traceable, wide-range X-ray scattering information N2 - Herein, we provide a "systems architecture"-like overview and detailed discussions of the methodological and instrumental components that, together, comprise the "MOUSE" project (Methodology Optimization for UltrafineStructure Exploration). The MOUSE project provides scattering information on a wide variety of samples, with traceable dimensions for both the scattering vector (q) and the absolute scattering cross-section (I). The measurable scattering vector-range of 0.012≤ q (nm-1) ≤ 92, allows information across a hierarchy of structures with dimensions ranging from ca. 0.1 to 400 nm. In addition to details that comprise the MOUSE project, such as the organisation and traceable aspects, several representative examples are provided to demonstrate its flexibility. These include measurements on alumina membranes, the tobacco mosaic virus, and dual-source information that overcomes fluorescence limitations on ZIF-8 and iron-oxide-containing carbon catalyst materials. KW - X-ray scattering KW - MOUSE KW - Instrumentation KW - SAXS KW - Methodology KW - Traceability KW - Wide-range KW - Data curation KW - FAIR KW - Uncertainties KW - Nanomaterials KW - Nanometrology PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528669 DO - https://doi.org/10.1088/1748-0221/16/06/P06034 VL - 16 IS - 6 SP - 1 EP - 50 PB - IOP CY - Bristol, UK AN - OPUS4-52866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cano Murillo, Natalia A1 - Szymoniak, Paulina A1 - Smales, Glen Jacob A1 - Sturm, Heinz A1 - Schönhals, Andreas T1 - Electrospun nanocomposites fibers of polycarbonate and taurine modified boehmite nanoparticles - What can be learned from structural and thermal investigations N2 - Though the reinforcing properties of inorganic particles in thermosetting nanocomposites, has been exploited, the integration of nanoparticles continues to be challenging in terms of their homogeneous distribution and their manipulation which can contribute to occupational hazards. Due to a second encapsulations of nanoparticles, electrospun nanocomposite fibers containing nanoparticles might be an alternative for overcoming these issues, as the fiber nonwovens contains the nanoparticles allowing for safer manipulation. Here, the morphology, and the thermal properties of electrospun polycarbonate fibers containing taurine modified boehmite nanoparticles (BNP) are investigated by means of small and wide-angle X-ray scattering as well as fast scanning and temperature modulated fast scanning calorimetry for the first time. The latter techniques allow the investigation of the thermal properties of single fibers at heating rates up to 10^4 K s^-1 keeping its structure intact. A quantitative analysis of the scattering data reveals a porous structure of the fibers. The porous structure is quantified regarding the pore volume and the pore size. A constant amount of aggregation is found even for the highly BNP loaded fibers. Thermal analysis on the fibers reveals a rigid amorphous fraction (RAF) where it is known that RAF determinates the properties of a nanocomposite to a large extent. For the fibers RAF amounts up to 40 wt%, which is essential higher compared to equally formulated PC/BNP composite cast films. The RAF in the case of the fibers, is not only due to the presence of particles in the polymer but also due to orientation effects induced by the electrospinning process. KW - Nanocomposite fibers KW - Electrospinning KW - X-ray scattering KW - Fast scanning calorimetry KW - Rigid amorphous fraction PY - 2021 DO - https://doi.org/10.1021/acsapm.1c01265 VL - 3 IS - 12 SP - 6572 EP - 6585 PB - ACS AN - OPUS4-53871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - X-ray Scattering for Nanostructure Quantification, and the Quest for the Perfect Experiment N2 - Compared to the clear, real-space images you can get from electron microscopy, X-ray scattering patterns are rather featureless. These patterns, however, contain structural information from all of the material structure illuminated by the X-ray beam. With this technique, you can measure nanoparticle dispersions, catalysts, composites, MOF powders, battery materials, light metal alloys and gels to reveal information on the structural features found within these materials. We have even measured many such materials for several research groups from the University of Birmingham, revealing structure features in the sub-nm to the micrometer range. Measuring an X-ray scattering pattern is relatively easy, but measuring a high-quality, useful pattern requires significant effort and good laboratory organization. Such laboratory organization can help address the reproducibility crisis in science, and easily multiply the scientific output of a laboratory, while greatly elevating the quality of the measurements. We have demonstrated this for small- and wide-angle X-ray scattering in the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration) [1]. With the MOUSE, we have combined: a) a comprehensive and highly automated laboratory workflow with b) a heavily modified X-ray scattering instrument. This combination allows us to collect fully traceable scattering data, within a well-documented, FAIR-compliant data flow (akin to what is found at the more automated synchrotron beamlines). With two full-time researchers, our lab collects and interprets thousands of datasets, on hundreds of samples, for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data. T2 - School of Chemistry Seminars CY - Birmingham, UK DA - 10.11.2021 KW - X-ray scattering KW - MOUSE KW - Instrumentation KW - SAXS KW - Methodology KW - Nanostructure PY - 2021 UR - https://www.youtube.com/watch?v=N2kY4wbqeM4 AN - OPUS4-53810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - What is in X-ray scattering Data? An overview of features. N2 - During the Better with Scattering 2021 workshop, we discuss what information can be obtained from an X-ray scattering pattern. Examples of structural features and their physical expression in scattering patterns are demonstrated. T2 - Better with Scattering workshop 2021 CY - Online meeting DA - 29.11.2021 KW - Scattering KW - SAXS KW - X-ray scattering KW - Data analysis KW - Data interpretation KW - Fourier transforms PY - 2021 AN - OPUS4-54011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lopez-Heredia, M.A. A1 - Gildenhaar, Renate A1 - Berger, Georg A1 - Linow, Ulf A1 - Wirth, Cynthia A1 - Günster, Jens A1 - Houshmand, A. A1 - Stiller, M. A1 - Knabe-Ducheyne, C. T1 - Effect of stressed and unstressed cell culture environments on the viability of MC3T3 cells with calcium phosphates T2 - ISACB-6 - International symposium on apatite and correlative biomaterials CY - Nantes, France DA - 2013-06-05 KW - Cell culture media KW - Fetal bovine serum KW - Stressed KW - Unstressed KW - Calcium alkaline orthophosphates PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-299387 DO - https://doi.org/10.4172/2090-5025.S1-002 SN - 2090-5017 SN - 2090-5025 N1 - Geburtsname von Wirth, Cynthia: Gomes, C. M. - Birth name of Wirth, Cynthia: Gomes, C. M. SP - 1 EP - 3(?) PB - Ashdin AN - OPUS4-29938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buljak, V. A1 - Oesch, Tyler A1 - Bruno, Giovanni T1 - Simulating fiber-reinforced concrete mechanical performance using CT-based fiber orientation data N2 - The main hindrance to realistic models of fiber-reinforced concrete (FRC) is the local materials property variation, which does not yet reliably allow simulations at the structural level. The idea presented in this paper makes use of an existing constitutive model, but resolves the problem of localized material variation through X-ray computed tomography (CT)-based pre-processing. First, a three-point bending test of a notched beam is considered, where pre-test fiber orientations are measured using CT. A numerical model is then built with the zone subjected to progressive damage, modeled using an orthotropic damage model. To each of the finite elements within this zone, a local coordinate system is assigned, with its longitudinal direction defined by local fiber orientations. Second, the parameters of the constitutive damage model are determined through inverse analysis using load-displacement data obtained from the test. These parameters are considered to clearly explain the material behavior for any arbitrary external action and fiber orientation, for the same geometrical properties and volumetric ratio of fibers. Third, the effectiveness of the resulting model is demonstrated using a second, “control” experiment. The results of the “control” experiment analyzed in this research compare well with the model results. The ultimate strength was predicted with an error of about 6%, while the work-of-load was predicted within 4%. It demonstrates the potential of this method for accurately predicting the mechanical performance of FRC components. KW - Fiber-reinforced concrete KW - X-ray computed tomography (CT) KW - Anisotropic fiber orientation KW - Inverse analysis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474728 DO - https://doi.org/10.3390/ma12050717 SN - 1996-1944 VL - 12 IS - 5 SP - 717, 1 EP - 16 PB - MDPI AN - OPUS4-47472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska A1 - Baer, Wolfram A1 - Wossidlo, Peter A1 - Habib, Abdel Karim T1 - Frequenzanalyse von Schallemission an einem Stahlrohr unter Biegebeanspruchung N2 - Um ein tieferes Verständnis über die Schallemission bei der Entstehung und Ausbreitung von Rissen in Stahlrohrleitungen zu erlangen, wurde ein Stahlrohr der Güte S355J2H im Vierpunkt-Biegeversuch quasistatisch bis hin zum Wanddurchbruch (Leckage) belastet und mittels Schallemissionsmessung und Gleichstrompotentialmessung überwacht. Das Rohrsegment wurde durch einen 90°- Außenumfangskerb in der Mitte der Rohrlänge definiert vorgeschädigt, um davon ausgehend ein stabiles Risswachstum zu induzieren und die Analyse von Schallemission aus Rissereignissen, die am Kerb eintraten, sicherzustellen. Für die Schallemissionsmessung wurden vier Breitbandsensoren max. 105 mm vom Kerb entfernt montiert. Die Signalaufzeichnung erfolgte kontinuierlich und schwellwertunabhängig. Für die Gleichstrompotentialmessung wurde ein Gleichstrom von 300 A eingeleitet und der Potentialabfall über dem Kerb mit fünf Sonden entlang des Kerbs gemessen. Beide Messverfahren identifizieren die Rissinitiierung sowie Veränderungen im Risswachstum. Die detektierten Schallemissionsereignisse werden, unter Berücksichtigung spektraler Eigenschaften, mit fortschreitender Belastung und Rissentwicklung analysiert. Diese Studien wurden im Rahmen des interdisziplinären Forschungsprojekts AGIFAMOR, Aging infrastructure - Faseroptisches Monitoring von Rohrleitungen, an der BAM durchgeführt. T2 - 22. Kolloquium Schallemission und 3. Anwenderseminar Zustandsüberwachung mit geführten Wellen CY - Karlsruhe, Germany DA - 27.03.2019 KW - Schallemission KW - Frequenzanalyse KW - Rissbildung in Stahl PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476888 SN - 978-3-947971-00-8 VL - 169 SP - 1 EP - 8 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-47688 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Kohlhoff, Harald A1 - Hüllmann, Dino A1 - Krentel, Daniel A1 - Kluge, Martin A1 - Dzierliński, M. A1 - Lilienthal, A. J. A1 - Bartholmai, Matthias T1 - Aerial-based gas tomography – from single beams to complex gas distributions N2 - In this paper, we present and validate the concept of an autonomous aerial robot to reconstruct tomographic 2D slices of gas plumes in outdoor environments. Our platform, the so-called Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), combines a lightweight Tunable Diode Laser Absorption Spectroscopy (TDLAS) gas sensor with a 3-axis aerial stabilization gimbal for aiming at a versatile octocopter. While the TDLAS sensor provides integral gas concentration measurements, it does not measure the distance traveled by the laser diode’s beam nor the distribution of gas along the optical path. Thus, we complement the set-up with a laser rangefinder and apply principles of Computed Tomography (CT) to create a model of the spatial gas distribution from a set of integral concentration measurements. To allow for a fundamental ground truth evaluation of the applied gas tomography algorithm, we set up a unique outdoor test environment based on two 3D ultrasonic anemometers and a distributed array of 10 infrared gas transmitters. We present results showing its performance characteristics and 2D plume reconstruction capabilities under realistic conditions. The proposed system can be deployed in scenarios that cannot be addressed by currently available robots and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO). KW - Aerial robot olfaction KW - Mobile robot olfaction KW - Gas tomography KW - TDLAS KW - Plume PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-487843 DO - https://doi.org/10.1080/22797254.2019.1640078 SP - 1 EP - 16 PB - Taylor & Francis CY - London AN - OPUS4-48784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Léonard, Fabien A1 - Zhang, Zhen A1 - Krebs, Holger A1 - Bruno, Giovanni T1 - Structural and Morphological Quantitative 3D Characterisation of Ammonium Nitrate Prills by X-ray Computed Tomography N2 - The mixture of ammonium nitrate (AN) prills and fuel oil (FO), usually referred to as ANFO, is extensively used in the mining industry as a bulk explosive. One of the major performance predictors of ANFO mixtures is the fuel oil retention, which is itself governed by the complex pore structure of the AN prills. In this study, we present how X-ray computed tomography (XCT), and the associated advanced data processing workflow, can be used to fully characterise the structure and morphology of AN prills. We show that structural parameters such as volume fraction of the different phases and morphological parameters such as specific surface area and shape factor can be reliably extracted from the XCT data, and that there is a good agreement with the measured oil retention values. Importantly, oil retention measurements (qualifying the efficiency of ANFO as explosives) correlate well with the specific surface area determined by XCT. XCT can therefore be employed non-destructively; it can accurately evaluate and characterise porosity in ammonium nitrate prills, and even predict their efficiency. KW - ANFO KW - Explosives KW - Surface area KW - Porosity KW - XCT KW - Data processing PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505395 DO - https://doi.org/10.3390/ma13051230 VL - 13 IS - 5 (Special Issue "Micro Non-Destructive Testing and Evaluation") SP - 1230 PB - MDPI AN - OPUS4-50539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan A1 - Torrent, R. A1 - Ebell, Gino A1 - Völker, Tobias A1 - Küttenbaum, Stefan T1 - Testing to reassess – Corrosion activity assessment based on NDT using a prestressed concrete bridge as case-study N2 - Corrosion of concrete reinforcement is one of the major damage mechanisms affecting both the load-bearing capacity and the serviceability of re-inforced concrete structures significantly. When externally discernible damages are observed during visual inspections on the structure, the extent of the damage inside the concrete is often already significant. Corrosion caused by carbonation often leads to severe discoloration of the surface or even large-area spalling of the concrete cover. In contrast, chloride-induced corrosion is usually difficult to observe visually but can cause much more serious damage in less time. The effect occurs locally and can lead to weakening of the cross-section of the reinforce-ment. This, in turn, can cause sudden structural collapses without prior notice. In the meanwhile, various non-destructive and minimally invasive testing methods are available to evaluate the resistance to penetration of corrosion-pro-moting pollutants and to detect active corrosion. In this paper, a bridge crossing the river Regen is used as a case-study to demonstrate how the information ob-tained applying different testing methods can be combined and evaluated in the context of structural reassessments. Both the results of the permeability testing and the electrical resistance measurement are considered, as well as active corro-sion areas are localized using the half-cell potential mapping combined with the concrete cover measurement with the eddy current method and ground penetrat-ing radar. The results are evaluated using drill cores and in addition laser-induced breakdown spectroscopy was applied to obtain information about possible chlo-ride ion transport into the concrete. T2 - EUROSTRUCT 2021 – 1ST conference of the european association on quality control of bridges and structures - Eurostruct CY - Padova, Italy DA - 30.08.2021 KW - Nondestructive testing KW - Corrosion KW - Bridge KW - Durability assessment KW - Civil engineering PY - 2022 SN - 978-3-030-91876-7 SP - 1 EP - 9 PB - Springer International Publishing AN - OPUS4-54006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Explaining Deviatoric Residual Stresses and Load Transfer in Aluminum Alloys and Composites with Complex Microstructure N2 - The residual stresses and load transfer in multiphase metal alloys and their composites (with both random planar-oriented short fibers and particles) will be shown, as studied by neutron diffraction, by X-ray computed tomography, and by a model based on the reformulation of classic Maxwell’s homogenization method. Contrary to common understanding and state-of-the-art models, we experimentally observe that randomly oriented phases possess non-hydrostatic residual stress. Moreover, we disclose that the unreinforced matrix alloy stays under hydrostatic compression even under external uniaxial compression. The recently developed modeling approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses accounting for the interaction of random oriented phases with fibers having preferential orientation. It also allows the explanation of the unconventional in-situ behavior of the unreinforced alloy and the prediction of the micromechanical behavior of other similar alloys. T2 - MLZ Konferenz 2022 CY - Lenggries, Germany DA - 31.05.2022 KW - Residual Stresses KW - Aluminium Alloys KW - Microstructures PY - 2022 AN - OPUS4-55020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Molecular absorption spectrometry: a fast and accurate optical method for boron isotope analysis comparable to mass spectrometry N2 - Boron presents two stable isotopes, 10B and 11B and due to their relatively large mass difference (~ 10%) isotope fractionation leads to considerable isotope amount ratio variations n(10B)/n(11B) in natural occurrence. These have been used as a proof of provenance of mineral and biological samples, to estimate a contamination source and to the determination of geological processes by erosion or subduction. Additionally, boron is employed in the nuclear industry due to the capability of its isotope 10B to thermal-neutron capture and therefore 10B enriched boric acid solutions are used in the cooling system of thermonuclear facilities and in the alloying of steel and carbides for protective shielding. Usually, isotope ratio variations are determined by mass spectroscopic methods. Here an alternative faster and low cost method for isotope ratio determination is proposed: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Boron isotope amount ratios have been determined by monitoring the absorption spectrum of boron monohydride (BH) in graphite furnace HR-CS-MAS. Bands (0→0) and (1→1) for the electronic transition X1Σ+ → A1Π were evaluated around wavelengths 433.1 nm and 437.1 nm respectively. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained around the 433.1 nm and 437.1 nm spectral regions are metrologically compatible with those reported by mass spectrometric methods. Moreover, a precision and accuracy of the method of ± 0.5 ‰ for the evaluated spectral region around 437.1 nm is reported here. This accuracy and precision is comparable with those obtained by thermal ionization mass spectrometry (TIMS) and multiple collector inductively coupled plasma mass spectrometry (MC-ICP-MS) for boron isotope ratio measurements. T2 - 30. Tag der Chemie CY - Berlin, Germany DA - 05.07.2017 KW - Boron isotopes KW - High-Resolution Continuum Source Molecular Absorption Spectrometry KW - HR-CS-MAS KW - Isotopic shift KW - Boron monohydride KW - Isotope ratio KW - Molecular absorption KW - Memory effect KW - Graphite furnace PY - 2017 AN - OPUS4-41060 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Nolze, Gert A1 - Saliwan Neumann, Romeo A1 - Eliezer, D. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Novel approach to image hydrogen distribution and related phase transformation in duplex stainless steels at the sub-micron scale N2 - The effect of electrochemical charging of hydrogen on the structure of a lean duplex stainless steel LDX 2101® (EN 1.4162, UNS S32101) was examined by both Time-of-Flight secondary ion mass spectrometry and electron back-scatter diffraction. The goal is to correlate hydrogen concentration and induced structural changes. Chemical and structural characterizations were done for the same region at the sample's surface with sub-micron spatial resolution. Regions of interest were varying in size between 50 × 50 μm and 100 × 100 μm. The results show a phase transformation of austenite to mainly a defect-rich BCC and scarcely a HCP phase. The phase transformation occurred in deuterium rich regions in the austenite. KW - Time-of-flight secondary ion mass spectrometry KW - ToF-SIMS KW - Electron backscatter diffraction KW - EBSD KW - Hydrogen-assisted cracking KW - Data fusion KW - Lean duplex stainless steel PY - 2017 DO - https://doi.org/10.1016/j.ijhydene.2017.08.016 SN - 0360-3199 VL - 42 IS - 39 SP - 25114 EP - 25120 AN - OPUS4-42022 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - The quantitative elemental microscope: for what is it good for? N2 - Elemental imaging of biological samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) provides spatially resolved information on element distribution in thin sections. By rastering with a laser across the sample, a two-dimensional image of the elemental distribution can be reconstructed that shows the intensities of the respective elements. Using overlapping laser shots the area ablated from single cells or thin sections (thickness 5 to 10 µm) can be reduced significantly so that the pixel size of the intensity measurement is significantly reduced. Having in mind that a laser shot ablates thin biological samples completely, we can make use of a new concept for calibration in the laser ablation method: the concept of total consumption. This calibration strategy allows production of simple matrix matched standards and provides an internal standardisation by ink jet technology, where a metal containing inks is printed on as thin layer on top of a biological sample. Different applications will be presented where our concepts have been applied. In the first example we used nanoparticle suspension of given particle numbers to quantify the uptake of metallic nanoparticles by biological cells. In the second example antibodies have been tagged by metals to measure protein expression in prostata cancer. In this approach application of house keeping proteins are investigated additionally to compensate variations in thickness and density of the biopsy samples. In the third application different nephrotoxic behaviour of Pt containing drugs have been investigated to study the local enrichement in kidney samples of mice treated with these three different compounds. Here the internal standard is required to allow intercomparisons between different individual mouse tissues. At the end of the lecture future trends will be discussed for elemental microscopy. T2 - European Winter Conference on Plasma Spectrochemistry 2017 CY - Sankt Anton am Arlberg, Austria DA - 19.02.2017 KW - LA-ICP-MS KW - Bioimaging KW - Nanoparticles KW - Biomarker PY - 2017 AN - OPUS4-39267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Following fluorinated drugs by molecular absorption spectrometry – from cancer cells to body fluids N2 - Fluorine has been widely introduced into pharmaceutical drugs. Due to the high C-F bond strength, a single atom substitution with fluorine produces drastic desirable and tunable changes in the molecular properties. However, the clinical monitoring of these drugs is not straightforward. Organofluorine compounds are elusive for a non-targeted analysis; a significant problem in fluorine determination is the lack of suitable detection techniques. Standard atomic absorption and emission spectrometers cannot access fluorine, because their resonance lines lie in the VUV spectral range below 100 nm. In the case of conventional inductively coupled argon plasmas (ICP), the plasma energy is too low to generate a significant population of excited fluorine atoms. Recently, our group introduces high-resolution continuum source absorption spectrometry (HR-CS MAS) as a new way for the indirect monitoring of fluorinated compounds. Main benefits of HR-CS-MAS includes low limits of detection, complete analyte recovery, simple to no sample preparation, and short time analysis. T2 - 16th Annual Congress of International Drug Discovery Science and Technology 2018 CY - Cambridge, MA, USA DA - 16.08.2018 KW - Fluorine KW - Anti-cancer KW - Capecitabine KW - Fluorouracil KW - HR-CS-MAS PY - 2018 AN - OPUS4-45822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steiner, S. A1 - Heldt, J. A1 - Sobol, Oded A1 - Unger, Wolfgang A1 - Frömeling, T. T1 - Influence of oxygen vacancies on core-shell formation in solid solutions of (Na,Bi)TiO3 and SrTiO3 N2 - Solid solutions of (Na,Bi)TiO3 (NBT) and SrTiO3 (ST) are materials of interest for high-strain or high-energy density capacitor applications. Often, they exhibit chemical heterogeneity and develop core-shell structures during regular solid-state synthesis with an NBT-rich core. In this case, the NBT forms first so that the strontium needs to diffuse into the material to reach chemical homogeneity. Depending on the presence of core-shell structures, the electrical properties can vary drastically. In this work, we rationalize the effect of variations in oxygen vacancy concentration by Fe-acceptor and Nb-donor doping. It can be shown that a diffusion couple of strontium and oxygen is responsible for chemical homogenization and that the oxygen vacancy content can control the formation of a core-shell structure. KW - Lead-free ceramics KW - Bismuth titanates KW - Core-shell structures KW - Diffusion/diffusivity KW - Ferroelectricity/ferroelectric materials PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525988 DO - https://doi.org/10.1111/jace.17845 SP - 1 EP - 10 PB - Wiley Periodicals LLC, John Wiley & Sons, Inc. AN - OPUS4-52598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - On nominal-actual comparisons for additive manufacturing applications N2 - Nominal-actual comparisons are routinely performed to compare a manufactured specimen to a reference specimen. X-ray Computed Tomography (CT) has brought a profound change in the way that tolerance verifications are performed in industry, by allowing the inner and outer geometries of an object to be measured, without the need for external access or destructive testing. As a results, CT is increasingly used in additive manufacturing applications, where a nominal-actual comparison performed between the digital model (CAD file), used as an input for the 3D printer, and the CT volume from the printed part, can provide invaluable information as to the accuracy of the printing process. However, the nominal-actual comparison process is somewhat different when applied to additively manufactured specimens by comparison to conventionally manufactured specimens. T2 - 9th Conference on Industrial Computed Tomography CY - Padova, Italy DA - 14.02.2019 KW - Computed tomography KW - X-ray computed tomography PY - 2019 AN - OPUS4-47833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - Morphological characterisation of explosive powders by XCT: When grain numbers count N2 - Ammonium nitrate (AN) prills are commonly used as an ingredient in industrial explosives and in fertilisers. Conventional techniques (such as BET or mercury intrusion porosimetry) can measure the open porosity and specific surface area of AN prill, but the closed porosity is not obtainable. This work was focused on evaluating X-ray computed tomography (XCT) as a non-destructive technique for the assessment of porosity in AN prills. An advanced data processing workflow was developed so that the segmentation and quantification of the CT data could be performed on the entire 3D volume, yet allowing the measurements (e.g.; volume, area, shape factor…) to be extracted for each individual phase (prill, open porosity, closed porosity) of each individual prill, in order to obtain statistically relevant data. Clear morphological and structural differences were seen and quantified between fertiliser and explosive products. Overall, CT can provide a very wide range of parameters that are not accessible to other techniques, destructive or non-destructive, and thus offers new insights and complementary information. T2 - iCT2020 CY - Wels, Austria DA - 04.02.2020 KW - Ammonium nitrate KW - Prill KW - Non-destructive characterisation KW - Porosity KW - Specific surface area PY - 2020 AN - OPUS4-50347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Léonard, Fabien A1 - Zhang, Zhen A1 - Krebs, Holger A1 - Bruno, Giovanni T1 - Morphological characterisation of explosive powders by XCT: When grain numbers count N2 - Ammonium nitrate (AN) prills are commonly used as an ingredient in industrial explosives and in fertilisers. Conventional techniques (such as BET or mercury intrusion porosimetry) can measure the open porosity and specific surface area of AN prill, but the closed porosity is not obtainable. This work was focused on evaluating X-ray computed tomography (XCT) as a non-destructive technique for the assessment of porosity in AN prills. An advanced data processing workflow was developed so that the segmentation and quantification of the CT data could be performed on the entire 3D volume, yet allowing the measurements (e.g.; volume, area, shape factor…) to be extracted for each individual phase (prill, open porosity, closed porosity) of each individual prill, in order to obtain statistically relevant data. Clear morphological and structural differences were seen and quantified between fertiliser and explosive products. Overall, CT can provide a very wide range of parameters that are not accessible to other techniques, destructive or non-destructive, and thus offers new insights and complementary information. T2 - 10th Conference on Industrial Computed Tomography (iCT 2020) CY - Wels, Austria DA - 04.02.2020 KW - Ammonium nitrate KW - Prill KW - Non-destructive characterisation KW - Porosity KW - Specific surface area PY - 2020 UR - http://www.ndt.net/?id=25118 SN - 1435-4934 VL - 25 IS - 2 SP - 1 EP - 6 PB - NDT.net CY - Kirchwald AN - OPUS4-50348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Phukphatthanachai, Pranee T1 - How to quantify the exact amount and establish metrological traceability of sulphur in biodiesel by ICP-IDMS and in copper samples by ICP-IDMS, GDMS, LA-ICP-MS, and LA-ICP-IDMS N2 - The quantification of the exact amount of sulphur is a big challenge due to a lack of SI-traceability and inconsistent results, when different methods are compared. Therefore, a reference procedure is required which allows SI-traceable values. In this work three procedures were developed for the quantification of the total sulphur amount in biodiesel by using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS), pure copper metals and copper alloys by ICP-IDMS and external calibration for GDMS and LA-ICP-MS at low concentration levels. The most critical parts of the sulphur quantification were sulphur purification and pre-concentration. Sulphur-matrix separation procedures were developed to serve both sample types. For biodiesel samples the sulphur was purified and matrix separated by an anion exchange chromatographic procedure. The analytical procedure was fully validated by the use of a certified reference material, a step-by-step validation and an inter-laboratory comparison at CCQM key comparison level. In the case of copper samples, the copper matrix was separated from sulphur by adding ammonia which forms a complex with the copper while releasing the sulphur prior to a chromatographic separation using a weak cation resin. After that the sulphur fraction was further purified by chromatographic means using first an anion ion exchange method and second a chelating resin. The method was validated by appropriate certified reference materials. The developed procedures enable sulphur measurements at the low g·g-1 level with sufficiently low measurement uncertainties (< 2 %, Urel). The external calibration was performed to produce reliable measurement results for the routine analytical techniques GDMS and LA-ICP-MS. Matrix-matched reference materials whith exactly known amount of sulphur obtained by ICP-IDMS beforehand, were used as calibrators to quantify sulphur in copper samples. The metrological traceability to the SI for the mass fraction of sulphur is established for all presented procedures by an unbroken chain of comparisons, each accompanied by an uncertainty budget. T2 - CCQM Workshop on Advances in Metrology in Chemistry and Biology CY - Sèvres, France DA - 09.04.2019 KW - Copper KW - Sulfur KW - IDMS KW - SI traceability PY - 2019 AN - OPUS4-47931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Stable isotope amount ratio analysis by using high-resolution continuum source molecular absorption spectrometry N2 - Analysis of stable isotopes has been used as proof of provenance of mineral and biological samples, to estimate a contamination source and to determine geological processes. This kind of analysis needs high accuracy and precision for reliable conclusions. Currently, stable isotope analysis is dominated by mass spectrometric techniques that are time consuming and expensive. Here we present a fast and low cost alternative for isotope analysis of boron and magnesium: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). Two stable isotope systems were evaluated separately: boron (10B:11B) and magnesium 24Mg:25Mg:26Mg). Their isotope amount ratios were estimated by monitoring their absorption spectra in-situ generated monohydrides. The molecular absorption spectrum of a XH molecule (X= B or Mg) with n isotopes would be a linear combination of n isotopologue spectra and the amount of each component (isotope) could be calculated by a multivariate regression (n= 2 and 3 for B and Mg respectively). For the Analysis of boron certified reference materials (CRM), the band 1→1 for the electronic transition X1Σ+ → A1Π was measured around wavelength 437.1 nm. Since boron has a Memory effect in graphite furnaces, a combination of 2 % (v/v) hydrogen gas in argon, 1 % trifluoromethane in argon, an acid solution of calcium chloride and mannitol as chemical modifiers were used during the BH vaporization at 2600 °C. Partial least square regression (PLS) for analysis of samples was applied. For this, a spectral library with different isotope ratios for PLS regression was created. Magnesium does not have memory effect. Therefore, only 2 % of hydrogen in argon as gas modifier during vaporization at 2500 °C was employed for analysis of magnesium CRM. Absorption spectra of MgH for the X2Σ→A2Π electronic transition (band 0→0) were recorded around wavelength 513.45 nm. A similar PLS procedure to the BH was applied. Results for B and Mg CRM are metrologically compatible with those reported by mass spectrometric methods. An accuracy of 0.08 ‰ for B and 0.1 ‰ Mg was obtained as the average deviation from the isotope CRM. Expanded uncertainties with a coverage factor of k = 2 range between 0.10 - 0.40 ‰. T2 - SAS meeting FACSS / SciX Conference 2017 CY - Reno, NV, USA DA - 08.10.2017 KW - Boron isotopes KW - High-Resolution Continuum Source Molecular Absorption Spectrometry KW - Graphite furnace KW - Molecular absorption PY - 2017 AN - OPUS4-43528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ascher, Lena T1 - Bildgebung von Eu-dotierten sehr kleinen Eisenoxid-Nanopartikeln in atherosklerotischen Plaques mittels LA-ICP-MS N2 - Atherosklerotische Läsionen können durch Magnetresonanztomographie (MRT) unter Verwendung von sehr kleinen Eisenoxidnanopartikeln (VSOP) sichtbar gemacht werden. VSOP akkumulieren in atherosklerotischen Plaques und dienen somit als Atherosklerosesonde. Das Ziel dieses Projektes war die Abbildung der Verteilung von Europium-dotierten VSOP (Eu-VSOP) durch Laserablation ICP-MS in histologischen Dünnschnitten der Aortenwurzelregion des ApoE-Knockout-Mausmodells, das reich an atherosklerotischen Plaques ist. Darüber hinaus wurde untersucht, ob die VSOP-Akkumulation in den Plaques mit anderen Biomarkern der Entzündung wie Makrophagen und verändertem Endothel korreliert. Somit wäre eine Beurteilung, ob es sich hierbei um instabile bzw. vulnerable Plaque-Regionen handelt möglich. Zu diesem Zweck wurden Antikörper mit verschiedenen Lanthaniden markiert und mit der Eu-VSOP-Verteilung unter Verwendung von LA-ICP-MS in einem Multiplex-Messmodus korreliert. Eine mögliche Korrelation von reaktiven Stickstoffspezies (RNS) mit endogenem Eisen oder Eu-VSOP kann ebenfalls durch LA-ICP-MS nachgewiesen werden. Zu diesem Zweck wurden RNS-spezifische Antikörper auch mit Lanthaniden markiert. T2 - 26. ICPMS-Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - Bioimaging KW - LA-ICP-MS KW - Nanopartikel KW - Antikörpermarkierung PY - 2018 AN - OPUS4-45921 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, Holger A1 - Baldofski, Stefanie A1 - Hoffmann, Kristin A1 - Flemig, Sabine A1 - Silva, C. P. A1 - Esteves, V. I. A1 - Emmerling, Franziska A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - Structural considerations on the selectivity of an immunoassay for sulfamethoxazole N2 - Sulfamethoxazol (SMX),a sulfonamide, is a widely used bacteriostatic antibiotic and therefore a promising marker for the entry of anthropogenic Pollution in the environment. SMX is frequently found in wastewater and surface water. This study presents the production of high affinity and selective polyclonal antibodies for SMX and the development and Evaluation of a direct competitive enzyme-linked immunosorbent assay(ELISA)for the quantification of SMX in environmental watersamples. The crystal structures of the cross-reacting compounds sulfamethizole, N4-acetyl-SMX andsuccinimidyl-SMX were determined by x-ray diffraction aiming to explain their high cross-reactivity. These crystal structures are described for the first time. The quantification range of the ELISA is 0.82–63 µg/L. To verify our results, the SMX concentration in 20 environmental samples,including wastewater and surfacewater,was determined by ELISA and tandem mass spectrometry(MS/MS).A good Agreement of the measured SMX concentrations was found with average recoveries of 97–113%for the results of ELISA compared to LC-MS/MS. KW - X-Ray diffraction KW - ELISA KW - LC-MS/MS KW - Sulfamethoxazole PY - 2016 DO - https://doi.org/10.1016/j.talanta.2016.05.049 SN - 0039-9140 SN - 1873-3573 IS - 158 SP - 198 EP - 207 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-38530 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - von Rüden, H. T1 - Röntgen-Computertomographie (CT) für die Kulturguterhaltung N2 - Als bildgebendes und zerstörungsfreies Verfahren eignet sich die Röntgen-Computertomographie (CT) insbesondere bei der Untersuchung von Kunst- und Kulturgütern. Die für Werkstoffprüfung und Materialanalyse konzipierten CT-Anlagen bieten dank hoher Röntgenleistung die Möglichkeit zusätzlich zu Holz, Keramiken und Kunststoffen auch stark schwächende Materialien, wie bspw. Metalle, zu durchdringen. Für eine hohe räumliche Auflösung im unteren Mikrometerbereich (2-200µm) sorgen entsprechend ausgelegte CT-Anlagen. In der Bundesanstalt für Materialforschung und -prüfung (BAM) stehen mehrere solcher CT-Anlagen für unterschiedliche Fragestellungen sowie Probengrößen und - materialien zur Verfügung. Einige Beispiele aus den vergangenen Arbeiten der BAM veranschaulichen das große Potential dieser Untersuchungsmethode. Da bei einer CT-Messung in der Regel das gesamte Untersuchungsobjekt erfasst und in ein digitales Volumenmodell überführt wird, eröffnet sich für Archäologen und Restoratoren die Möglichkeit Untersuchungen hinsichtlich Materialzusammensetzung, Erhaltungszustand und Herstellungstechnik am virtuellen Objekt vorzunehmen, ohne die Originalsubstanz zu beeinträchtigen. Gegenüber der klassischen Radiografie, bei der nur eine zweidimensionale Abbildung erreicht wird, bietet die CT-Untersuchung die Möglichkeit innenliegende Strukturen dreidimensional zu erfassen. Die notwendige Bestimmung der Objektoberfläche erlaubt zudem die Erstellung eines Oberflächenmodells des untersuchten Gegenstandes. Damit lassen sich unter anderem mechanische Simulationen (Belastung, Durchbiegung, Durchströmung) durchführen. Der erzeugte Datensatz kann somit auch zur Herstellung eines Replikats im 3D-Druckverfahren genutzt werden. Anhand der Untersuchung der Mandoline von Smorsone wird gezeigt, wie eine CT-Messung durchgeführt wird und wie in dem anschließend rekonstruierten 3D-Datensatz mittels Koordinatenmesstechnik Maße (Abstände, Wandstärken, Winkel) exakt ermittelt werden können. T2 - Jahrestagung der Gesellschaft für Musikforschung CY - Berlin, Germany DA - 28.09.2022 KW - Mikro-CT KW - Bildverarbeitung KW - Holz KW - Bronze KW - ZfP PY - 2022 AN - OPUS4-56412 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ulbricht, Alexander A1 - Gollwitzer, Christian A1 - Kupsch, Andreas A1 - Léonard, Fabien A1 - Müller, Bernd R. A1 - Oesch, Tyler A1 - Onel, Yener A1 - Thiede, Tobias A1 - Zscherpel, Uwe ED - Puente León, F. ED - Zagar, B. T1 - Moderne Methoden der CT-gestützten Strukturanalyse T1 - Modern techniques of CT based structure analysis N2 - Durch den großflächigen Einsatz der Computertomographie (CT) in unterschiedlichen Industriebereichen steigen auch die Anforderungen an die quantitative Bildanalyse. Subjektive Bildwahrnehmung muss durch objektive Algorithmen ersetzt werden. In diesem Artikel stellt die Bundesanstalt für Materialforschung und -prüfung (BAM), die seit den 1980er Jahren an der Entwicklung der industriellen CT beteiligt ist, anhand ausgewählter Beispiele den aktuellen Stand ihrer Analysemethoden an verschiedenen Anwendungsbeispielen der CT vor. N2 - The increasing use of computed tomography (CT) in various industrial sectors requires more sophisticated techniques of quantitative image analysis. Subjective image perception needs to be replaced by objective algorithms. The German Federal Institute for Materials Research and Testing (BAM) has been involved in the development of industrial CT since the 1980s. This paper summarizes the current status of quantitative 3D image analysis techniques based on selected examples. KW - Computed tomography KW - Computertomographie KW - Röntgen-Refraktion KW - X-Ray refraction KW - Schadensanalyse KW - Damage analysis KW - Normung KW - standardization PY - 2020 DO - https://doi.org/10.1515/teme-2019-0125 SN - 0171-8096 SN - 2196-7113 VL - 87 IS - 2 SP - 81 EP - 91 PB - de Gruyter CY - Berlin AN - OPUS4-50337 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Method development for metal detection at cellular levels by ICP-MS N2 - An overview about different analytical approaches will be presented of how to detect metals in individual biological cells by use of ICP-MS. For this purpose, we are using different sample introduction systems for ICP-MS for detection, imaging and quantification of metals at cellular levels. By use of laser ablation, we have studied the up-take by and distribution of nanoparticles in single cells. Recently we have developed staining techniques to measure protein and DNA content of cells and identifying the cell status by immunoassays using metal-tagging of antibodies. New research based on cell arrays will be shortly discussed. Using pneumatic nebulization and microdroplet generation, we have also studied the up-take of nanoparticles and toxic metals as well as essential elements in single cells using different ICP-MS mass spectrometric concepts (sector field instrument, triple-quad instrument, time of flight (CyTOF) instrument). The different ICP-MS based methods will be compared concerning their analytical figures of merit and their strengths and weaknesses will be evaluated. T2 - ACS Annual Meeting CY - New Orleans, LA, USA DA - 18.03.2018 KW - Single cell ICP-MS KW - LA-ICP-MS with cellular resolution KW - Nanoparticles PY - 2018 AN - OPUS4-44799 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Diagnostics and modeling of laser induced plasma in relation to current needs of spectrochemical analysis N2 - The short report on computer modeling and diagnostics of laser induced plasmas T2 - Winter Plasma Conference CY - Tucson, USA DA - 08.01.2016 KW - Plasma diagnostics KW - Laser induced plasma KW - LIBS KW - Plasma modeling PY - 2016 AN - OPUS4-38773 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhou, Z. A1 - Han, Q. A1 - Wang, D. A1 - Macé, T. A1 - Kipphardt, Heinrich A1 - Maiwald, Michael A1 - Tuma, Dirk A1 - Uehara, S. A1 - Akima, D. A1 - Shimosaka, T. A1 - Jung, J. A1 - Oh, S.-H. A1 - van der Veen, A. A1 - van Wijk, J.I.T. A1 - Ziel, P. R. A1 - Konopelko, L. A1 - Valkova, M. A1 - Mogale, D.M. A1 - Botha, A. A1 - Brewer, P. A1 - Murugan, A. A1 - Minnaro, M.D. A1 - Miller, M. A1 - Guenther, F. A1 - Kelly, M.E. T1 - CCQM K101 Final report international comparison CCQM-K101:Oxygen in nitrogen-a track B comparison and that the matrix contains argon N2 - This key comparison aims to assess the capabilities of the participants to determine the amount-of-substance fraction oxygen in nitrogen. The GAWG has classified this as a track B comparison, due to the unexpected 50 μmol/mol argon mole fraction content of the transfer standards, which effects the achievable performance of some measurement techniques such a GC-TCD. The separation of oxygen and argon is challenging, and not all systems in use are equally well designed for it. As this analytical challenge due to a substantial fraction of argon in the transfer standards became a reality, the Gas Analysis Working Group (GAWG) decided to qualify this key comparison as a regular key comparison and not as a core comparison, which may be used to support calibration and measurement capabilities (CMCs) for oxygen in nitrogen, or for oxygen in nitrogen mixtures containing argon only (see also the section on support to CMCs). KW - CCQM-K101 KW - Gas analysis PY - 2016 UR - http://iopscience.iop.org/article/10.1088/0026-1394/53/1A/08013 SN - 1681-7575 SN - 0026-1394 VL - 53 IS - Techn Suppl SP - 08013, 1 EP - 71 PB - IOP publishing AN - OPUS4-40013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Larissa A1 - Herrmann, Antje Jutta A1 - Techritz, Sandra A1 - Panne, Ulrich A1 - Jakubowski, Norbert T1 - Quantitative characterization of single cells by use of immunocytochemistry combined with multiplex LA-ICP-MS N2 - Actual research demonstrates that LA-ICP-MS is capable of being used as an imaging tool with cellular resolution. The aim of this investigation was the method development for LA-ICP-MS to extend the versatility to quantitative and multiplexing imaging of single eukaryotic cells. For visualization of individual cells selected, lanthanide-labeled antibodies were optimized for immuno-imaging of single cells with LA-ICP-MS. The molar content of the artificial introduced labels per cell was quantified using self-made nitrocellulose-coated slides for matrix-matched calibration and calculated amounts were in the range of 3.1 to 17.8 atmol per cell. Furthermore, the quantification strategy allows a conversion of 2D intensity profiles based on counts per second (cps) to quantitative 2D profiles representing the molar amount of the artificial introduced elemental probes per pixel for each individual cell. KW - Single cell analysis KW - Bioimaging by LA-ICP-MS KW - Immunoassays PY - 2017 DO - https://doi.org/10.1007/s00216-017-0310-1 SN - 1618-2642 SN - 1618-2650 VL - 409 IS - 14 SP - 3667 EP - 3676 PB - Springer AN - OPUS4-40068 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donskyi, Ievgen A1 - Azab, W. A1 - Cuellar-Camach, J. L. A1 - Guday, G. A1 - Lippitz, Andreas A1 - Unger, Wolfgang A1 - Osterrieder, K. A1 - Adeli, M. A1 - Haag, R. T1 - Functionalized nanographene sheets with high antiviral activity through synergistic electrostatic and hydrophobic interactions N2 - As resistance to traditional drugs emerges for treatment of Virus infections, the need for new methods for virus inhibition increases. Graphene derivatives with large surface areas have shown strong activity against different viruses. However, the inability of current synthetic protocols to accurately manipulate the structure of graphene sheets in order to control their antiviral activity remains a major challenge. In this work, a series of graphene derivatives with defined polyglycerol sulfate and fatty amine functionalities have been synthesized and their interactions with herpes simplex Virus type 1 (HSV-1) are investigated. While electrostatic interactions between polyglycerol sulfate and virus particles trigger the binding of graphene to virus, alkyl chains induce a high antiviral activity by secondary hydrophobic interactions. Among graphene sheets with a broad range of alkyl chains, (C3–C18), the C12-functionalized sheets showed the highest antiviral activity, indicating the optimum synergistic effect between electrostatic and hydrophobic interactions, but this derivative was toxic against the Vero cell line. In contrast, sheets functionalized with C6- and C9-alkyl chains showed low toxicity against Vero cells and a synergistic Inhibition of HSV-1. This study shows that antiviral agents against HSV-1 can be obtained by controlled and stepwise functionalization of graphene sheets and may be developed into antiviral agents for future biomedical applications. KW - Functionalized nanographene KW - X-ray Photoelectron Spectroscopy (XPS) KW - NEXAFS KW - Antiviral activity PY - 2019 DO - https://doi.org/10.1039/c9nr05273a SN - 2040-3364 VL - 11 IS - 34 SP - 15804 EP - 15809 PB - The Royal Society of Chemistry AN - OPUS4-48807 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tannenberg, Robert T1 - Troponin I Assay in Wafer-Level Backside Optofluidics N2 - Cardiovascular diseases are the number one cause of death worldwide and responsible for 17.9 million casualities worldwide in 2019. Cardiac Troponin I (cTnI) is the most important biomarker for acute events such as heart attacks. The development of novel photonic integrated microchips (PIC) is a promising approach to allow the convenient detection of key biomarkers in complex matrices through multichannel real-time analysis in a highly compact package. This study presents the development and proof-of-concept of a backside released CMOS chip designed for the multichannel real-time detection of biomarkers. In this work, we introduce a Troponin I assay as well that utilizes a potential and practical approach to backside optofluidics on a wafer-level platform. T2 - Biosensors 2025 - 35th Anniversary World Congress on Biosensors CY - Lisbon, Portugal DA - 19.05.2025 KW - Ring resonator KW - Semiconductor KW - CMOS KW - cTnI KW - Heart attack KW - Biomarker KW - Sandwich immunoassay PY - 2025 AN - OPUS4-63481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Damage and stress evolution in multi-phase metal matrix composites N2 - While there is a extensive literature on the micro-mechanical behavior of metal matrix composites (MMCs) under uniaxial applied stress, very little is available on multi-phase MMCs. In order to cast light on the reinforcement and damage processes in such multi-phase composites, an Al alloy with one and two ceramic reinforcements (planar-random oriented alumina fibers and SiC particles) were studied. In-situ compression tests during neutron diffraction experiments were used to track the load transfer among phases, while X-ray computed tomography was used to investigate pre-strained samples, in order to monitor and quantify damage. We found that damage progresses differently in composites with different orientations of the fiber mat. Because of the presence of the intermetallic network, it was observed that the second ceramic reinforcement changes the load transfer scenario only at very high applied load, when also intermetallic particles break. We rationalized the experimental results by means of a micromechanical model based on Maxwell’s homogenization scheme, and we could explain why no damage is observed in the ductile matrix under compression: the matrix finds itself in hydrostatic compression, and the Poisson’s tensile strain is totally carried by the reinforcement phases T2 - CIMTEC CY - Perugia, Italy DA - 20.06.2022 KW - Load transfer KW - Neutron Diffraction KW - Michromechanical modeling KW - Computed Tomography KW - Machine Learning PY - 2022 AN - OPUS4-55404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Magkos, Sotirios T1 - Reconstruction of limited-angle projection data with DIRECTT N2 - Direct Iterative Reconstruction of Computed Tomography Trajectories is a fully three-dimensional algorithm that prioritizes the reconstruction of voxels corresponding to dominant trajectories across the projections. T2 - MUMMERING outreach conference CY - Online meeting DA - 10.06.2021 KW - Iteration method KW - X-ray imaging KW - Signal processing KW - Computed tomography PY - 2021 AN - OPUS4-53466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - In situ analysis of damage evolution in an Al/Al2O3 MMC under tensile load by synchrotron x-ray refraction imaging N2 - 3D imaging techniques have an enormous potential to understand the microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this conference paper we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. We demonstrate showcases of ceramics and composite materials, where microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. We present in situ analysis of the damage evolution in a carbon fibre reinforced polymer and a Al/Al2O3metal matrix composite during tensile load, the direct observation of damage accumulation during creep of Al-3.85Mg and the identification of void formation (different kinds of defects, particularly unsintered powder hidden in pores, and small inhomogeneity’s like cracks) in Ti64 parts produced by selective laser melting using synchrotron X-ray refraction radiography tomography. T2 - Materials Science and Engineering 2018 (MSE2018) CY - Darmstadt, Germany DA - 26.09.2018 KW - Synchrotron X-ray refraction radiography KW - In-situ tensile test KW - Damage evolution KW - Metal matrix composite PY - 2018 AN - OPUS4-46149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska T1 - Frequenzanalyse von Schallemission an einem Stahlrohr unter Biegebeanspruchung N2 - Um ein tieferes Verständnis über die Schallemission bei der Entstehung und Ausbreitung von Rissen in Stahlrohrleitungen zu erlangen, wurde ein Stahlrohr der Güte S355J2H im Vierpunkt-Biegeversuch quasistatisch bis hin zum Wanddurchbruch (Leckage) belastet und mittels Schallemissionsmessung und Gleichstrompotentialmessung überwacht. Das Rohrsegment wurde durch einen 90°- Außenumfangskerb in der Mitte der Rohrlänge definiert vorgeschädigt, um davon ausgehend ein stabiles Risswachstum zu induzieren und die Analyse von Schallemission aus Rissereignissen, die am Kerb eintraten, sicherzustellen. Für die Schallemissionsmessung wurden vier Breitbandsensoren max. 105 mm vom Kerb entfernt montiert. Die Signalaufzeichnung erfolgte kontinuierlich und schwellwertunabhängig. Für die Gleichstrompotentialmessung wurde ein Gleichstrom von 300 A eingeleitet und der Potentialabfall über dem Kerb mit fünf Sonden entlang des Kerbs gemessen. Beide Messverfahren identifizieren die Rissinitiierung sowie Veränderungen im Risswachstum. Die detektierten Schallemissionsereignisse werden, unter Berücksichtigung spektraler Eigenschaften, mit fortschreitender Belastung und Rissentwicklung analysiert. Diese Studien wurden im Rahmen des interdisziplinären Forschungsprojekts AGIFAMOR, Aging infrastructure - Faseroptisches Monitoring von Rohrleitungen, an der BAM durchgeführt. T2 - 22. Kolloquium Schallemission und 3. Anwenderseminar Zustandsüberwachung mit geführten Wellen CY - Karlsruhe, Germany DA - 27.03.2019 KW - Schallemission KW - Frequenzanalyse KW - Rissbildung in Stahl PY - 2019 AN - OPUS4-47690 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Procedures to Quantitatively Characterize Morphological Features of Triply Periodic Minimal Surface Structures (TPMSS) N2 - The residual stresses and load transfer in multiphase metal alloys and their composites (with both random planar-oriented short fibers and particles) will be shown, as studied by neutron diffraction, by X-ray computed tomography, and by a model based on the reformulation of classic Maxwell’s homogenization method. Contrary to common understanding and state-of-the-art models, we experimentally observe that randomly oriented phases possess non-hydrostatic residual stress. Moreover, we disclose that the unreinforced matrix alloy stays under hydrostatic compression even under external uniaxial compression. The recently developed modeling approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses accounting for the interaction of random oriented phases with fibers having preferential orientation. It also allows the explanation of the unconventional in-situ behavior of the unreinforced alloy and the prediction of the micromechanical behavior of other similar alloys. T2 - 5th International Conference on Tomography of Materials and Structures CY - Grenoble, France DA - 27.06.2022 KW - Load transfer KW - Neutron Diffraction KW - Micromechanical modeling KW - Computed tomography PY - 2022 AN - OPUS4-55406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saadeh, Qais T1 - In-Situ SAXS Techniques N2 - Our project's aim is to enhance the capabilities of additive manufacturing techniques, where enabling a Two-Photon-Polymerization (TPP) 3D printer of producing arrays of precisely aligned nanoparticles is of an enormous value. As heterogeneous functional nanostructures with arrays of oriented nanoparticles are very promising in many fields; electrochemistry, energy storage, nanoelectronics among other vital fields. The feasibility and the convenience of orienting nanoparticles using magnetic, electric fields and ultrasonic vibrations will be systematically investigated, using Small Angle X-ray Scattering (SAXS), since SAXS can provide detailed information about the orientation characteristics of nano-Ensembles. Corresponding to our prerequisites, a set ad hoc functional sample holders, sample stages and other In-Situ SAXS solutions were developed, and incorporated to be compatible with a state-of-the-arts SAXS machine, called Multi-scale Analyzer for Ultrafine Structures (MAUS). The MAUS has been customized and engineered to serve as a miniaturized synchrotron, and that is exactly what we need. Experiments attempting to orient superparamagnetic nanoparticles will be discussed, where the outcomes will not only help in understanding the mechanics of field-particle interactions, it will also help in further developing the adequate needed set of corrections to the SAXS data, that is especially regards oriented samples. T2 - XVII International Small Angle Scattering Conference – SAS 2018 CY - Traverse City, Michigan, USA DA - 07.10.2018 KW - In-Situ Techniques KW - SAXS KW - Magnetic nano-particles PY - 2018 AN - OPUS4-46443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hüllmann, Dino A1 - Bartholmai, Matthias A1 - Tiebe, Carlo T1 - Gas Tomography Up In The Air! N2 - In this paper, we present an autonomous aerial robot to reconstruct tomographic 2D slices of gas plumes in outdoor environments. Our platform, the so-called Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS) combines a lightweight Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile octocopter. The TDLAS sensor provides integral gas concentration measurements but no information regarding the distance traveled by the laser diode's beam or the distribution of the gas along the optical path. We complemented the set-up with a laser rangefinder and apply principles of Computed Tomography (CT) to create a model of the spatial gas distribution from these integral concentration measurements. To allow for a rudimentary ground truth evaluation of the applied gas tomography algorithm, we set up a unique outdoor test environment based on two 3D ultrasonic anemometers and a distributed array of 10 infrared gas transmitters. We present first results showing the 2D plume reconstruction capabilities of the system under realistic conditions. T2 - NetMon International training course - Low-cost Environmental Monitoring CY - BAM, Berlin, Germany DA - 09.04.2019 KW - Aerial robot KW - Gas tomography KW - Plume KW - TDLAS PY - 2019 AN - OPUS4-47800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria T1 - Synthesis of Bimetallic Nickel Nanoparticles as Catalysts for the Sabatier Reaction N2 - Nanoparticles (NP) have become important materials for a variety of chemical technologies. The enhance surface-area-to-volume ratio of NPs is very high, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles. Monodisperse monometallic Ni nanoparticles were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the catalytically active sites are accessible. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni. Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage. T2 - Joint Polish-German Crystallographic Meeting CY - Wroclaw, Poland DA - 24.02.2020 KW - Nanoparticles KW - Synthesis KW - Catalysis PY - 2020 AN - OPUS4-51663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Powierza, Bartosz A1 - Gollwitzer, C. A1 - Wolgast, D. A1 - Staude, A. A1 - Bruno, Giovanni T1 - Fully experiment-based evaluation of few digital volume correlation techniques N2 - Digital Volume Correlation (DVC) is a powerful set of techniques used to compute the local shifts of 3D images obtained, for instance, in tomographic experiments. It is utilized to analyze the geometric changes of the investigated object as well as to correct the corresponding image misalignments for further analysis. It can therefore be used to evaluate the local density changes of the same regions of the inspected specimens, which might be shifted between measurements. In recent years, various approaches and corresponding pieces of software were introduced. Accuracies for the computed shift vectors of up to about 1‰of a single voxel size have been reported. These results, however, were based either on synthetic datasets or on an unrealistic setup. In this work, we propose two simple methods to evaluate the accuracy of DVC-techniques using more realistic input data and apply them to several DVC programs. We test these methods on three materials (tuff, sandstone, and concrete) that show different contrast and structural features. KW - DVC KW - Finite-element analysis KW - Image processing KW - Stress strain relations KW - Computed tomography PY - 2019 DO - https://doi.org/10.1063/1.5099572 SN - 1089-7623 VL - 90 IS - 11 SP - 115105 PB - AIP Publishing AN - OPUS4-49671 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Michalik-Onichimowska, Aleksandra A1 - Kern, Simon A1 - Riedel, Jens A1 - Panne, Ulrich A1 - King, R. A1 - Maiwald, Michael T1 - ‘‘Click” analytics for ‘‘click” chemistry – A simple method for calibration–free evaluation of online NMR spectra N2 - Driven mostly by the search for chemical syntheses under biocompatible conditions, so called "click" chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques possessing short set-up times. Here, we report on a fast and reliable calibration-free online NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement of 1H spectra with a time interval of 20 s per spectrum, and a robust, fully automated algorithm to interpret the obtained data. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in a variety of non-deuterated solvents while its time-resolved behaviour was characterized with step tracer experiments. Overlapping signals in online spectra during thiol-ene coupling could be deconvoluted with a spectral model using indirect hard modeling and were subsequently converted to either molar ratios (using a calibrationfree approach) or absolute concentrations (using 1-point calibration). For various solvents the kinetic constant k for pseudo-first order reaction was estimated to be 3.9 h-1 at 25 °C. The obtained results were compared with direct integration of non-overlapping signals and showed good agreement with the implemented mass balance. KW - Online NMR Spectroscopy KW - Reaction Monitoring KW - Automated Data Evaluation KW - Thiol-ene click chemistry KW - Click Chemistry KW - Process Analytical Technology PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-393232 UR - http://www.sciencedirect.com/science/article/pii/S1090780717300575 DO - https://doi.org/10.1016/j.jmr.2017.02.018 VL - 277 SP - 154 EP - 161 PB - Elsevier Inc. CY - Oxford AN - OPUS4-39323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sötebier, Carina A1 - Bierkandt, Frank A1 - Rades, Steffi A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Weidner, Steffen T1 - Sample loss in asymmetric flow field-flow fractionation coupled to inductively coupled plasma-mass spectrometry of silver nanoparticles N2 - In this work, sample losses of silver nanoparticles (Ag NPs) in asymmetrical flow field-flow fractionation (AF4) have been systematically investigated with the main focus on instrumental conditions like focusing and cross-flow parameters as well as sample concentration and buffer composition. Special attention was drawn to the AF4 membrane. For monitoring possible silver depositions on the membrane, imaging laser ablation coupled to inductively coupled plasma mass spectrometry (LA-ICP-MS) was used. Our results show that the sample residue on the membrane was below 0.6% of the total injected amount and therefore could be almost completely avoided at low sample concentrations and optimized conditions. By investigation of the AF4 flows using inductively coupled plasma mass spectrometry (ICP-MS), we found the recovery rate in the detector flow under optimized conditions to be nearly 90%, while the cross-flow, slot-outlet flow and purge flow showed negligible amounts of under 0.5%. The analysis of an aqueous ionic Ag standard solution resulted in recovery rates of over 6% and the ionic Ag content in the sample was found to be nearly 8%. Therefore, we were able to indicate the ionic Ag content as the most important source of sample loss in this study. KW - Asymmetric flow filed-flow fractionation KW - ICP-MS KW - Nanoparticles KW - Sample loss KW - Quantification PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-336171 DO - https://doi.org/10.1039/c5ja00297d SN - 0267-9477 SN - 1364-5544 VL - 30 IS - 10 SP - 2214 EP - 2222 PB - Royal Society of Chemistry CY - London AN - OPUS4-33617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Walter, Astrid A1 - Panne, Ulrich A1 - Weller, Michael G. T1 - A novel immunoreagent for the specific and sensitive detection of the explosive triacetone triperoxide (TATP) N2 - Triacetone triperoxide (TATP) is a primary explosive, which was used in various terrorist attacks in the past. For the development of biosensors, immunochemical µ-TAS, electronic noses, immunological test kits, or test strips, the availability of antibodies of high quality is crucial. Recently, we presented the successful immunization of mice, based on the design, synthesis, and conjugation of a novel TATP derivative. Here, the long-term immunization of rabbits is shown, which resulted in antibodies of extreme selectivity and more than 1,000 times better affinity in relation to the antibodies from mice. Detection limits below 10 ng L-1 (water) were achieved. The working range covers more than four decades, calculated from a precision profile. The cross-reactivity tests revealed an extraordinary selectivity of the antibodies—not a single compound could be identified as a relevant cross-reactant. The presented immunoreagent might be a major step for the development of highly sensitive and selective TATP detectors particularly for security applications. KW - Organic peroxides KW - Terrorism KW - Biosensor development PY - 2011 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-240291 UR - http://www.mdpi.com/2079-6374/1/3/93 DO - https://doi.org/10.3390/bios1030093 SN - 2079-6374 VL - 1 IS - 3 SP - 93 EP - 106 PB - MDPI CY - Basel AN - OPUS4-24029 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sötebier, Carina A. A1 - Kutscher, D. J. A1 - Rottmann, L. A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Bettmer, J. T1 - Combination of single particle ICP-QMS and isotope dilution analysis for the determination of size, particle number and number size distribution of silver nanoparticles N2 - Single particle ICP-MS (spICP-MS) has gained great influence in the analysis of engineered nanoparticles (NPs) due to its simplicity, speed and ability to obtain a particle number size distribution. Despite its many advantages, the method is hampered by matrix effects affecting the sensitivity of the instruments. Consequently, over- or underestimated particle sizes might be obtained. To overcome these challenges, we present in this work the detection of both Ag isotopes with a quadrupole mass spectrometer for the application of isotopic dilution analysis (IDA) in combination with spICP-MS. Here, the isotopes are measured sequentially using the conventional spICP-MS integration time of 10 ms. Citrate stabilized Ag NPs of a spherical shape with the nominal diameters of 30, 40, 50 and 80 nm have been investigated. The experimental concept of adding ¹⁰⁹Ag+ solutions to the NP suspensions resulted in the NP Spikes being only visible in the ¹⁰⁷Ag trace. Therefore, a maximum of 45% of the particles was detected compared to that by conventional spICP-MS. A modified mass flow equation was applied to determine the particle sizes, particle size distributions and particle number concentrations of various Ag NPs. The addition of different spike concentrations between 0.5 and 4 mg L⁻¹ ¹⁰⁹Ag resulted in similar particle diameters, suggesting that the calculated diameter might be independent of the spike concentration. This would have the advantage that no size information would be needed before the analysis. By analyzing Ag NP suspensions in a simulated seawater matrix, we demonstrate its significant influence on the particle size determination using conventional spICP-MS. A lower transport efficiency of 6.1% was found in the matrix compared to 7.3% without the matrix. In our approach, the addition of the Matrix influenced the NP intensity stronger than the spike signal, resulting in slightly smaller diameters using IDA–spICP-MS with the matrix compared to the results without the matrix. On the other hand, the IDA–spICP-MS approach with the matrix can result in equivalent results for the particle sizes compared with conventional spICP-MS using suspensions without the matrix. Due to the lower instrument sensitivity in the matrix, a diameter of 30 nm was found to be close to the detection limit of the instrument. KW - Ag nanoparticles KW - Single particle ICP-MS KW - Matrix influence KW - Isotope dilution analysis PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-376490 DO - https://doi.org/10.1039/c6ja00137h SN - 0267-9477 VL - 31 IS - 10 SP - 2045 EP - 2052 AN - OPUS4-37649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Holzlechner, Gerald A1 - Holzweber, Markus A1 - Lohninger, H. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - First use of data fusion and multivariate analysis of ToF-SIMS and SEM image data for studying deuterium-assisted degradation processes in duplex steels N2 - Time-of-flight secondary ion mass spectrometry (ToF-SIMS) and high-resolution scanning electron microscopy are well-acknowledged tools in materials characterization. The ability to map chemical species on the surface of an investigated sample with often low mass detection limits makes ToF-SIMS an essential tool in fields where many question marks concerning Degradation processes and damage mechanisms exist. The aim of this paper is to describe the power of data fusion of ToF-SIMS and high-resolution scanning electron microscopy results employing computational methods for multivariate data Analysis such as principal component analysis. As a case study the investigation of hydrogen distribution in an artificially charged Duplex stainless steel microstructure is presented aiming on a better understanding of hydrogen embrittlement. T2 - 16th European Conference on Applications of Surface and Interface Analysis CY - Granada, Spain DA - 28.09.2015 KW - ToF-SIMS KW - HR-SEM KW - Data fusion KW - Duplex stainless steel KW - Hydrogen embrittlement PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/sia.6015/full DO - https://doi.org/10.1002/sia.6015 VL - 48 IS - 7 SP - 474 EP - 478 PB - John Wiley & Sons, Ltd CY - Surface and Interface Analysis AN - OPUS4-36832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Phukphatthanachai, Pranee T1 - A new approach of using polyethylene frits for the quantification of sulphur in copper metals by isotope dilution LA-ICP-MS N2 - For the first time polyethylene (PE) frits were used to quantify sulphur in copper metal and its alloys by isotope dilution combined with LA-ICP-MS: an alternative approach for sample preparation. The properties of the PE frit meet the requirements for isotope dilution LA-ICPMS which are porous material, thermal and chemical resistance and high absorption efficiency. The breakthrough, however, as a support material, is the low sulphur blank, which is only two times of the gas flow blank (2.3-4.0 x 10⁴ cps). Additionally, the porosity of the frit was considered, as it directly affects the absorption efficiency for the sample solution, which is present in the cavities of the frit. The absorption efficiency was studied by loading sulphur standards with varying sulphur amounts (0 - 80 µg S) onto the frits. The remaining sulphur which was not absorbed by the frit was rinsed off and was measured by ICP-MS. This indirect method shows that more than 99.5 % of the loaded sulphur was absorbed by the frit. The so prepared frits with increasing sulphur amount were measured by LA-ICP-MS showing a good linearity between 0 µg S and 40 µg S with a coefficient of determination, r2 of 0.9987 and a sensitivity of 3.4x10⁴ cps µgˉ¹ for 32S. Three copper reference materials produced by BAM (BAM-M376a, BAM-228 and BAM-227) were selected to develop and validate the LA-ICP-IDMS procedure. The IDMS technique was applied to these samples as follows: the samples were spiked, dissolved, digested and then the digested solution was absorbed on the frits. The dried frit samples were then analyzed by LA-ICP-IDMS and it could be demonstrated that the sample solution dispersed on the frits did not influence the 32S/34S ratio significantly even though the sulphur intensities were fluctuating along the scan lines. Relative standard deviations of the isotope ratios were below 5 % in average between 3 lines (except for the pure spike solution and procedure blank). The measurement results were validated by comparing them with the results obtained by conventional ICP-IDMS. Plotting the mass fraction of sulphur in copper obtained by LA-ICP-IDMS versus those obtained by ICP-IDMS yields a linear curve with a correlation coefficient of 0.9999 showing a strong agreement between both techniques. The metrological traceability to the SI for the mass fraction of sulphur in copper is established by an unbroken chain of comparisons, each accompanied by an uncertainty budget. Thus, the measurement results are considered reliable, acceptable and comparable within the stated measurement uncertainty. The metrological traceability chain from the kg down to the final mass fraction in the samples obtained by LA-ICP-IDMS is illustrated in this presentation. T2 - ESAS & CANAS 2018 CY - Berlin, Germany DA - 20.03.2018 KW - Laser ablation KW - Isotope dilution mass spectrometry KW - SI traceability KW - Measurement uncertainty PY - 2018 AN - OPUS4-44641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - Heinrich, Hans-Joachim A1 - Recknagel, Sebastian A1 - Vogl, Jochen A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Determination of boron isotope ratios by high-resolution continuum source molecular absorption spectrometry using graphite furnace vaporizers N2 - Boron isotope amount ratios n(10B)/n(11B) have been determined by monitoring the absorption spectrum of boron monohydride (BH) in a graphite furnace using high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Bands (0→0) and (1→1) for the electronic transition X1Σ+ → A1Π were evaluated around wavelengths 433.1 nm and 437.1 nm respectively. Clean and free of memory effect molecular spectra of BH were recorded. In order to eliminate the memory effect of boron, a combination of 2% (v/v) hydrogen gas in argon and 1% trifluoromethane in argon, an acid solution of calcium chloride and mannitol as chemical modifiers was used. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained around the 433.1 nm and 437.1 nm spectral regions are metrologically compatible with those reported by mass spectrometric methods. Moreover, for the evaluated region of 437 nm, an accuracy of 0.15‰ is obtained as the average deviation from the isotope reference materials. Expanded uncertainties with a coverage factor of k = 2 range between 0.15 and 0.44‰. This accuracy and precision are compatible with those obtained by mass spectrometry for boron isotope ratio measurements. KW - Boron isotopes KW - Isotope ratios KW - Boron monohydride KW - Molecular absorption KW - High-resolution continuum source absorption spectrometry KW - Graphite furnace KW - Memory effect KW - HR-CS-MAS PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0584854717302537 DO - https://doi.org/10.1016/j.sab.2017.08.012 SN - 0584-8547 VL - 136 SP - 116 EP - 122 PB - Elsevier CY - Amsterdam, The Netherlands AN - OPUS4-42071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosenkranz, D. A1 - Kriegel, F. L. A1 - Mavrakis, E. A1 - Pergantis, S. A. A1 - Reichardt, P. A1 - Tentschert, J. A1 - Jakubowski, N. A1 - Laux, P. A1 - Panne, Ulrich A1 - Luch, A. T1 - Versatile dual-inlet sample introduction system for multi-mode single particle inductively coupled plasma mass spectrometry N2 - Metal-containing nanoparticles (NP) can be characterized with inductively coupled plasma mass spectrometers (ICP-MS) in terms of their size and number concentration by using the single-particle mode of the instrument (spICP-MS). The accuracy of measurement depends on the setup, operational conditions of the instrument and specific parameters that are set by the user. The transport efficiency of the ICP-MS is crucial for the quantification of the NP and usually requires a reference material with homogenous size distribution and a known particle number concentration. Currently, NP reference materials are available for only a few metals and in limited sizes. If particles are characterized without a reference standard, the results of both size and particle number may be biased. Therefore, a dual-inlet Setup for characterizing nanoparticles with spICP-MS was developed to overcome this problem. This setup is based on a conventional introduction system consisting of a pneumatic nebulizer (PN) for nanoparticle solutions and a microdroplet Generator (μDG) for ionic calibration solutions. A new and flexible interface was developed to facilitate the coupling of μDG, PN and the ICP-MS system. The interface consists of available laboratory components and allows for the calibration, nanoparticle (NP) characterization and cleaning of the arrangement, while the ICP-MS instrument is still running. Three independent analysis modes are available for determining particle size and number concentration. Each mode is based on a different calibration principle. While mode I (counting) and mode III (μDG) are known from the literature, mode II (sensitivity), is used to determine the transport efficiency by inorganic ionic Standard solutions only. It is independent of NP reference materials. The μDG based inlet system described here guarantees superior analyte sensitivities and, therefore, lower detection limits (LOD). The size dependent LODs achieved are less than 15 nm for all NP (Au, Ag, CeO2) investigated. KW - Spectrometer KW - Reference KW - Calibration PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536121 DO - https://doi.org/10.3791/61653 SN - 1940-087X IS - 163 SP - 1 EP - 19 PB - MyJoVE Corporation CY - Cambridge, MA, USA AN - OPUS4-53612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Panne, Ulrich T1 - Book review: Silvio Vaz Jr.: Applications of analytical chemistry in industry N2 - The book emphasizes the practical applications of analytical chemistry to solve problems in major industrial sectors involving analytes such as pharmaceuticals and agrochemicals, metals in mining, polymers, typical analytes in biotechnology, and the oil and gas sector. Industrial analytical chemistry plays a critical role by providing the composition, concentration, and properties of materials. Applications include quality control, process monitoring, research and development, and environmental monitoring. By describing the analytical challenges from the perspective of the specifics of each industrial sector, Silvio Vaz Jr. takes a new and fresh approach to applied analytical chemistry. KW - Analytical instrumentation KW - Analytical technology KW - Chemical technology KW - Chemometrics KW - Analytical chemistry KW - Industrial chemistry PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626802 DO - https://doi.org/10.1007/s00216-024-05666-2 SN - 1618-2642 SN - 1618-2650 VL - 417 SP - 229 EP - 230 PB - Springer CY - Berlin AN - OPUS4-62680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neamtu, Mariana A1 - Nadejde, C. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Verestiuc, L. A1 - Panne, Ulrich T1 - Functionalized magnetic nanoparticles: Synthesis, characterization, catalytic application and assessment of toxicity N2 - Cost-effective water cleaning approaches using improved Treatment technologies, for instance based on catalytic processes with high activity catalysts, are urgently needed. The aim of our study was to synthesize efficient Fenton-like photo-catalysts for rapid degradation of persistent organic micropollutants in aqueous medium. Iron-based nanomaterials were chemically synthesized through simple procedures by immobilization of either iron(II) oxalate (FeO) or iron(III) citrate (FeC) on magnetite (M) nanoparticles stabilized with polyethylene glycol (PEG). Various investigation techniques were performed in order to characterize the freshly prepared catalysts. By applying advanced oxidation processes, the effect of catalyst dosage, hydrogen peroxide concentration and UV-A light exposure were examined for Bisphenol A (BPA) conversion, at laboratory scale, in mild conditions. The obtained results revealed that BPA degradation was rapidly enhanced in the presence of low-concentration H2O2, as well as under UV-A light, and is highly dependent on the surface characteristics of the catalyst. Complete photo-degradation of BPA was achieved over the M/PEG/FeO catalyst in less than 15 minutes. Based on the catalytic performance, a hierarchy of the tested catalysts was established: M/PEG/FeO > M/PEG/FeC > M/PEG. The results of cytotoxicity assay using MCF-7 cells indicated that the aqueous samples after treatment are less cytotoxic. KW - Bisphenol A KW - Magnetic nanocatalyst KW - Endocrine disruptor KW - Nanoparticle KW - Photodegradation KW - Fenton PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-448297 DO - https://doi.org/10.1038/s41598-018-24721-4 SN - 2045-2322 VL - 8 SP - Article 6278, 1 EP - 11 PB - Springer Nature CY - London AN - OPUS4-44829 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hachenberger, Y. U. A1 - Rosenkranz, D. A1 - Kriegel, Fabian L. A1 - Krause, B. A1 - Matschaß, René A1 - Reichardt, P. A1 - Tentschert, J. A1 - Laux, P. A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Luch, A. T1 - Tackling Complex Analytical Tasks: An ISO/TS-Based Validation Approach for Hydrodynamic Chromatography Single Particle Inductively Coupled Plasma Mass Spectrometry N2 - Nano-carrier systems such as liposomes have promising biomedical applications. Nevertheless, characterization of these complex samples is a challenging analytical task. In this study a coupled hydrodynamic chromatography-single particle-inductively coupled plasma mass spectrometry (HDC-spICP-MS) approach was validated based on the technical specification (TS) 19590:2017 of the international organization for standardization (ISO). The TS has been adapted to the hyphenated setup. The quality criteria (QC), e.g., linearity of the calibration, transport efficiency, were investigated. Furthermore, a cross calibration of the particle size was performed with values from dynamic light scattering (DLS) and transmission electron microscopy (TEM). Due to an additional Y-piece, an online-calibration routine was implemented. This approach allows the calibration of the ICP-MS during the dead time of the chromatography run, to reduce the required time and enhance the robustness of the results. The optimized method was tested with different gold nanoparticle (Au-NP) mixtures to investigate the characterization properties of HDC separations for samples with increasing complexity. Additionally, the technique was successfully applied to simultaneously determine both the hydrodynamic radius and the Au-NP content in liposomes. With the established hyphenated setup, it was possible to distinguish between different subpopulations with various NP loads and different hydrodynamic diameters inside the liposome carriers. KW - Single particle ICP-MS KW - Nanoparticle characterization KW - Nano-carrier KW - Iposomes KW - Hydrodynamic chromatography (HDC) KW - Validation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506609 DO - https://doi.org/10.3390/ma13061447 VL - 13 IS - 6 SP - 1 EP - 14 CY - Basel, Switzerland AN - OPUS4-50660 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Falkenhagen, Jana A1 - Panne, Ulrich A1 - Hiller, W. A1 - Gruendling, T. A1 - Staal, B. A1 - Lang, C. A1 - Lamprou, A. T1 - Simultaneous characterization of poly(acrylic acid) andpolysaccharide polymers and copolymers N2 - Copolymer products that result from grafting acrylic acid and other hydrophilicmonomers onto polysaccharides have recently gained significant interest in researchand industry. Originating from renewable sources, these biodegradable, low toxicity,and polar copolymer products exhibit potential to replace polymers from fossil sourcesin several applications and industries. The methods usually employed to character-ize these copolymers are, however, quite limited, especially for the measurement ofbulk properties. With more sophisticated applications, for example, in pharmaceu-tics requiring a more detailed analysis of the chemical structure, we describe a newapproach for this kind of complex polymers. Our approach utilizes chromatographyin combination with several detection methods to separate and characterize reactionproducts of the copolymerization of acrylic acid and chemically hydrolyzed starch.These samples consisted of a mixture of homopolymer poly (acrylic acid), homopoly-mer hydrolyzed starch, and – in a lower amount – the formed copolymers. Several chro-matographic methods exist that are capable of characterizing either poly (acrylic acid)or hydrolyzed starch. In contrast, our approach offers simultaneous characterization ofboth polymers. The combination of LC and UV/RI offered insight into the compositionand copolymer content of the samples. Size exclusion chromatography experimentsrevealed the molar mass distribution of homopolymers and copolymers. FTIR inves-tigations confirmed the formation of copolymers while ESI-MS gave more details onthe end groups of hydrolyzed starches and poly (acrylic acids). Evidence of copolymerstructures was obtained through NMR measurements. Finally, two-dimensional chro-matography led to the separation of the copolymers from both homopolymers as wellas the additional separation of sodium clusters. The methods described in this work area powerful toolset to characterize copolymerization products of hydrolyzed starch andpoly(acrylic acid). Together, our approach successfully correlates the physicochemicalproperties of such complex mixtures with their actual composition. KW - 2D chromatography KW - LC-MS KW - SEC KW - Renewable copolymers KW - Grafting PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508873 DO - https://doi.org/10.1002/ansa.202000044 SP - 1 EP - 12 PB - Wiley-VCH Verlag-GmbH&Co. KGaA CY - Weinheim AN - OPUS4-50887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emteborg, H. A1 - Florian, D. A1 - Choquette, S. A1 - Ellison, S. L. R. A1 - Fernandes-Whaley, M. A1 - Mackay, L. A1 - McCarron, P. A1 - Panne, Ulrich A1 - Sander, S. G. A1 - Kim, S.-K. A1 - Held, A. A1 - Linsinger, T. A1 - Trapmann, S. T1 - Cooperation in publicly funded reference material production N2 - The meeting was organised by the European Commission’s Joint Research Centre and held at the JRC-Geel site on 22–23 February 2018. It was a follow-up of a similar meeting held in 2009. The objective of the meeting was to exchange information about ongoing publicly funded reference material (RM) production, identify areas of interest for future specific RMs, including certified reference material (CRM) developments, investigate potential areas of collaboration, and to identify areas which may be of a lower importance in the future for a specific RM producer. The benefit of exchanging such information is to avoid duplication of efforts in RM production, make better use of public funds by potentially matching competencies, and to address problems that are common to publicly funded RM producers. T2 - Meeting regarding cooperation in publicly funded reference material production, European Commission's Joint Research Centre CY - Geel, Belgium DA - 22.02.2018 KW - Public funding KW - Reference materials PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-470206 DO - https://doi.org/10.1007/s00769-018-1349-1 SN - 0949-1775 SN - 1432-0517 VL - 23 IS - 6 SP - 371 EP - 377 PB - Springer CY - Berlin AN - OPUS4-47020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Michalik-Onichimowska, Aleksandra A1 - Riedel, Jens A1 - Panne, Ulrich A1 - King, R. A1 - Maiwald, Michael ED - Herwig, Christoph T1 - “Click” analytics for “click” chemistry – a simple method for calibration-free evaluation of online NMR spectra N2 - Currently, research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algorithm to interpret the obtained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16-inch polymer tubing working as a flow cell. Single scan 1H NMR spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in non-deuterated solvents while its time-resolved behaviour was characterised with step tracer experiments. Through the application of spectral modeling the signal area for each reactant can be deconvoluted in the online spectra and thus converted to the respective concentrations or molar ratios. The signals which were suitable for direct integration were used herein for comparison purposes of both methods. T2 - 11. Interdisziplinäres Doktorandenseminar CY - Berlin, Germany DA - 12.03.2017 KW - Process Monitoring KW - Online NMR Spectroscopy KW - Indirect Hard Modeling KW - Process Control KW - Process Analytical Technology KW - CONSENS KW - Click Chemistry PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435531 SP - 33 EP - 35 PB - Gesellschaft Deutscher Chemiker (GDCh) CY - Frankfurt a. M. AN - OPUS4-43553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Prinz, Carsten A1 - Zimathies, Annett A1 - Emmerling, Franziska T1 - Experimantal raw data sets associated with certified reference material BAM-P116 (titanium dioxide) for comparison of nitrogen and argon sorption, available in the universal adsorption information format (AIF) N2 - These data sets serve as models for calculating the specific surface area (BET method) using gas sorption in accordance with ISO 9277. The present measurements were carried out with nitrogen at 77 Kelvin and argon at 87 Kelvin. It is recommended to use the following requirements for the molecular cross-sectional area: Nitrogen: 0.1620 nm² Argon: 0.1420 nm² Titanium dioxides certified with nitrogen sorption and additionally measured with argon for research purposes were used as sample material. The resulting data sets are intended to serve as comparative data for own measurements and show the differences in sorption behaviour and evaluations between nitrogen and argon. These data are stored in the universal AIF format (adsorption information file), which allows flexible use of the data. KW - Physisorption KW - Surface area KW - AIF KW - Argon KW - Nitrogen PY - 2023 DO - https://doi.org/10.5281/zenodo.10199628 PB - Zenodo CY - Geneva AN - OPUS4-59102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Testing to reasses - Corrosion activity assessment based on NDT using a prestressed concrete bridge as case study N2 - Corrosion of concrete reinforcement is one of the major damage mechanisms affecting both the load-bearing capacity and the serviceability of reinforced concrete structures significantly. The challenge of detecting corrosion is that the corrosion process in its various forms is not immediately visible, especially in the corrosion initiation phase inside the concrete. When externally discernible damages are observed during visual inspections on the structure, the extent of the damage inside the concrete is often already significant. Corrosion caused by carbonation often leads to severe discoloration of the surface or even large-area spalling of the concrete cover. In contrast, chloride-induced corrosion is usually difficult to observe visually, but can cause much more serious damage in less time. The effect occurs locally and can lead to weakening of the cross-section of the reinforcement. This, in turn, can cause sudden structural collapses without prior notice. Therefore, it is important to investigate whether there is protection against corrosion of the reinforcement in the concrete and to detect active corrosion in the structure at an early stage. In the meanwhile, various non-destructive and minimally invasive testing methods are available to evaluate the resistance to penetration of corrosion-promoting pollutants and to detect active corrosion. In this paper, a bridge crossing the river Regen (Germany) is used as a case-study to demonstrate how the information obtained applying different testing methods can be combined and evaluated in the context of structural reassessments. Both the results of the permeability testing (Torrent tester) and the electrical resistance measurement (Wenner probe) are considered, as well as active corrosion areas are localized using the half-cell potential mapping combined with the concrete cover measurement with the eddy current method and ground penetrating radar (GPR). The results are evaluated using drill cores and in addition laser-induced breakdown spectroscopy (LIBS) was applied to obtain information about possible ion transport in the concrete. T2 - EUROSTRUCT 2021 - 1st Conference of the European Association on Quality Control of Bridges and Structures - EUROSTRUCT CY - Padova, Italy DA - 30.08.2021 KW - Nondestructive testing KW - Corrosion KW - Bridge KW - Durability assessment KW - Civil engineering PY - 2021 AN - OPUS4-53222 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Magkos, Sotirios T1 - The DIRECTT algorithm: A promising alternative for Computed Tomography reconstructions N2 - The DIRECTT (Direct Iterative REconstruction of Computed Tomography Trajectories) algorithm represents a promising alternative to conventional algorithms, such as the Filtered Backprojection (FBP) or the Algebraic Reconstruction Technique (ART), by overcoming restrictions associated with them. Such restrictions include the limited spatial resolution achieved through FBP due to Nyquist‘s sampling theorem, the inability of FBP to perform a quality reconstruction when projections are missing, and the excessive computing time needed for ART. T2 - CINEMAX IV Summer School CY - Toreby, Danmark DA - 27.08.2018 KW - Computed tomography KW - Reconstruction algorithm KW - Spatial resolution PY - 2018 AN - OPUS4-46448 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Prinz, Carsten T1 - Importance of stability studies on porous certified reference materials N2 - In the development of certified reference materials (CRM), it is necessary to examine appropriate materials in advance for homogeneity and stability to meet the criteria of a CRM. In this case, the materials properties are characterized at the actual time without being possible to give a prognosis for suitability in the following years. It is, therefore, necessary to follow the certified material parameters via a monitoring system over the years on sale. For the current development of CRMs, the gained experience from long-term stability studies about the first generation of porous CRMs is significant. This experience is useful to better assess the suitability of candidate materials and thus develop higher quality CRMs in the future. A comparison between the gas sorption CRM materials silica, activated carbons, alpha alumina and anatase titanium oxides will illustrate the importance of long-term stability studies on porous CRMs. T2 - BERM 2018 - 15th International Symposium on Biological and Environmental Reference Materials CY - Berlin, Germany DA - 23.09.2018 KW - Reference material KW - Monitoring KW - Long-term stability PY - 2018 AN - OPUS4-46257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rosenkranz, Daniel A1 - Kriegel, F. L. A1 - Mavrakis, E. A1 - Pergantis, S. A. A1 - Reichardt, Ph. A1 - Tentschert, J. A1 - Jakubowski, Norbert A1 - Laux, P. A1 - Panne, Ulrich T1 - Improved validation for single particle ICP-MS analysis using a pneumatic nebulizer / microdroplet generator sample introduction system for multi-mode nanoparticle determination N2 - This study reports on the development of a single-particle (sp) inductively coupled plasma mass spectrometry (ICP-MS) technique suitable for the multi-mode determination of nanoparticle (NP) metal mass fraction and number concentration. The described technique, which is based on a dual inlet System consisting of a pneumatic nebulizer (PN) and a microdroplet generator (MDG), allows for the sequential introduction of ionic metal calibrant solutions and nanoparticle suspensions via all combinations of the two inlets; thus allowing for a combination of three independent modes of analysis. A novel interface, assembled using standard analytical components (a demountable quartz ICP-MS torch, flexible nonconducting silicon tubing and various connectors), was used to interface the dual inlet system to an ICP-MS. The interface provided improved functionality, compared to a previous design. It is now possible to conveniently exchange and introduce standard solutions and samples via all inlet combinations, analyze them, and also wash the sample inlet systems while the whole setup is still connected to an operating ICP-MS. This setup provided seamless and robust operation in a total of three analysis modes, i.e. three ways to independently determine the metal mass fraction and NP number concentration. All three analyses modes could be carried out within a single analytical run lasting approximately 20 min. The unique feature of the described approach is that each analysis mode is based on a different. KW - Nanomaterials KW - Nanoparticles KW - Single particle ICP-MS KW - Microdroplet generator PY - 2020 DO - https://doi.org/10.1016/j.aca.2019.11.043 VL - 1099 SP - 16 EP - 25 PB - Elsevier B.V. AN - OPUS4-50361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Klas A1 - Rademann, K. A1 - Panne, Ulrich A1 - Maiwald, Michael T1 - Quantitative NMR spectroscopy for gas analysis for production of primary reference gas mixtures N2 - Due to its direct correlation to the number of spins within a sample quantitative NMR spectroscopy (qNMR) is a promising method with absolute comparison abilities in complex systems in technical, as well as metrological applications. Most of the samples studied with qNMR are in liquid state in diluted solutions, while gas-phase applications represent a rarely applied case. Commercially available NMR equipment was used for purity assessment of liquid and liquefied hydrocarbons serving as raw materials for production of primary reference gas standards. Additionally, gas-phase studies were performed within an online NMR flow probe, as well as in a high-pressure NMR setup to check feasibility as verification method for the composition of gas mixtures. KW - Quantitative NMR spectroscopy KW - Gas-phase NMR spectroscopy KW - Primary reference gas mixtures PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S1090780716302518 DO - https://doi.org/10.1016/j.jmr.2016.11.016 SN - 1090-7807 SN - 1096-0856 VL - 275 SP - 1 EP - 10 AN - OPUS4-38803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ascher, Lena T1 - Imaging of Eu doped very small iron oxide nanoparticle in atherosclerotic plaques via LA ICP-MS N2 - Atherosclerotic lesions can be visualized by magnetic resonance imaging (MRI) using very small iron oxide nanoparticles (VSOP). VSOP accumulate in atherosclerotic plaques and thus serve as an atherosclerosis probe. The aim of this project was to image the distribution of europium doped VSOP (Eu-VSOP) by laser ablation ICP-MS in histological thin cuts of the aortic root region of ApoE knockout mouse model that is rich in atherosclerotic plaques. In addition, it was investigated whether VSOP accumulation in the plaques correlates with other biomarkers of inflammation for example macrophages and altered endothelium to assess whether it correlates with instability or vulnerability of the plaque regions. For this purpose, antibodies were labeled with various lanthanide elements and correlated with the Eu-VSOP distribution using LA-ICP-MS in a multiplex measurement mode. A possible correlation of reactive oxygen species (ROS) with endogenous iron or Eu-VSOP can also be detected by LA-ICP-MS. For this purpose, ROS-specific antibodies were also labeled with lanthanides. T2 - BI(MS)2 2018 – First Workshop on Laser Bioimaging Mass Spectrometry CY - Münster, Germany DA - 23.05.2018 KW - Bioimaging KW - LA-ICP-MS KW - Immunoassay KW - Nanoparticle KW - Labeling PY - 2018 AN - OPUS4-45133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nourinejhad Zarghani, S. A1 - Monavari, Mehran A1 - Nourinejhad Zarghani, A. A1 - Nouri, S. A1 - Ehlers, J. A1 - Hamacher, J. A1 - Bandte, M. A1 - Büttner, C. T1 - Quantifying plant viruses: Evolution from bioassay to infectivity dilution curves along the model of tobamoviruses N2 - This review describes the development of the bioassay as a means of quantifying plant viruses, with particular attention to tobamovirus. It delves into various models used to establish a correlation between virus particle concentration and the number of induced local lesions (the infectivity dilution curve), including the Poisson, Furumoto and Mickey, Kleczkowski, Growth curve, and modified Poisson models. The parameters of each model are described, and their application or performance in the context of the tobacco mosaic virus is explored. This overview highlights the enduring value of the infectivity dilution curve in tobamovirus quantification, providing valuable insights for researchers or practitioners of bioassays and theoreticians of modeling. KW - Local lesion KW - qRT-PCR KW - Nicotiana KW - ToBRFV KW - TMV KW - CGMMV KW - Disinfection KW - Modeling PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-630142 DO - https://doi.org/10.3390/v16030440 SN - 1999-4915 VL - 16 IS - 3 SP - 1 EP - 14 PB - MDPI CY - Basel AN - OPUS4-63014 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - O'Connor, Daniel T1 - European Metrology Network (EMN) for Advanced Manufacturing Development of the Strategic Research Agenda (SRA) N2 - The European Commission has identified Advanced Manufacturing and Advanced Materials as two of six Key Enabling Technologies (KETs). It is considered that Metrology is a key enabler for the advancement of these KETs. Consequently, EURAMET, the association of metrology institutes in Europe, has strengthened the role of Metrology for these KETs by enabling the creation of a European Metrology Network (EMN) for Advanced Manufacturing. The EMN is comprised of National Metrology Institutes (NMIs) and Designated Institutes (DIs) from across Europe and was formally established in October 2021. The aim of the EMN is to provide a high-level coordination of European metrology activities for the Advanced Manufacturing community. The EMN itself is organized in three sections representing the major stages of the manufacturing chain: 1) Advanced Materials, 2) Smart Manufacturing Systems, and 3) Manufactured Components & Products. The EMN for Advanced Manufacturing is engaging with stakeholders in the field of Advanced Manufacturing (large companies & SMEs, industry organisations, existing networks, and academia), as well as the wider Metrology community, including Technical Committees, to provide input for the Strategic Research Agenda (SRA) on Metrology for Advanced Manufacturing. This contribution will give an overview about the first version of the SRA prepared by the EMN for Advanced Manufacturing. T2 - Euspen, 23rd International Conference & Exhibitio CY - Copenhagen, Danmark DA - 13.06.2023 KW - European Metrology Network (EMN) KW - Advanced Manufacturing KW - Metrology KW - Strategic Research Agenda (SRA) PY - 2023 AN - OPUS4-59176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Devi, Sarita T1 - Metal-Organic Magnetic Framework-Based Immunosensor for Label-free Electrochemical sensing of NeuroToxin N2 - A metal-organic framework (MOF)-integrated microfluidic flow-cell (MFC) based electrochemical immunodetection of the tetanus toxoid (TT) is presented. The magnetic property of Fe-MOF helped to hold them on the working electrode (WE) at detection zone of MFC, surpassing the requirement of additional conjugation chemistry, and the conductive property was utilized to observe the change in signal efficiency in the presence of TT. The one-pot hydrothermal synthesis of iron-based MOF (Fe-MOF) was performed using the Fe3+/Fe2+ precursors as 1.2/1 mmol and dual ligands, tetrahydroxy-1,4-benzoquinone and 2 aminobenzene-1,4-dicarboxylic acid. The human anti-TT mAb SA13 was purified in-house from the cell culture supernatant of SA13 hybridoma cells by Protein-A affinity. SDS-PAGE showed the high purity as of a band just above the 140kDa mark in the eluate lane. The hydrodynamic radius of 5.35 nm and thermal unfolding temperature of 73°C were typical for antibodies. Indirect ELISA confirmed the high binding affinity. The mAb was conjugated on the Fe-MOF/Phe surface with the help of ethylenediamine (Fe MOF/Phe/EDA/anti-TTmAb). A specifically tailored MFC, made of Poly(methyl methacrylate) substrate was crafted at the BAM workshop. The limit of detection (LOD) and analytical sensitivity of the TT biosensor was 9.4 ng/ml [y=1.93E-5 + (-1.86E-6)x] and 11.6 μA/ng ml-1cm-2, respectively. The good reproducibility, selectivity, and stability show the applicability of these Fe-MOFs for detecting various other toxins. T2 - European Materials Research Society (E-MRS) Spring Meeting CY - Strasbourg, France DA - 26.05.2025 KW - Magnetic Metal-Organic Framework KW - Tetanus toxoid KW - Antibody KW - Electrochemistry KW - Biosensor PY - 2025 AN - OPUS4-63492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chemello, Giovanni A1 - Knigge, Xenia A1 - Ciornii, Dmitri A1 - Reed, B.P. A1 - Pollard, A.J. A1 - Clifford, C.A. A1 - Howe, T. A1 - Vyas, N. A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Influence of the Morphology on the Functionalization of Graphene Nanoplatelets Analyzed by Comparative Photoelectron Spectroscopy with Soft and Hard X-Rays N2 - Since its isolation, graphene has received growing attention from academia and industry due to its unique properties. However, the “what is my material” barrier hinders further commercialization. X-ray photoelectron spectroscopy (XPS) is considered as a method of choice for the determination of the elemental and chemical composition. In this work the influence of the morphology of graphene particles on the XPS results is studied and investigated as a function of X-ray energy, using conventional XPS with Al K𝜶 radiation and hard X-ray photoemission spectroscopy (HAXPES) using Cr K𝜶 radiation. Thereby, the information depth is varied between 10 and 30 nm. For this purpose, two commercial powders containing graphene nanoplatelets with lateral dimensions of either ≈100 nm or in the micrometer range are compared. These larger ones exist as stack of graphene layers which is inspected with scanning electron microscopy. Both kinds of particles are then functionalized with either oxygen or fluorine. The size of the graphene particles is found to influence the degree of functionalization. Only the combination of XPS and HAXPES allows to detect the functionalization at the outermost surface of the particles or even of the stacks and to provide new insights into the functionalization process. KW - Functionalized graphene KW - Hard-energy X-ray photoelectron spectroscopy KW - X-ray photoelectron spectroscopy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578860 DO - https://doi.org/10.1002/admi.202300116 SN - 2196-7350 SP - 1 EP - 8 PB - Wiley VCH AN - OPUS4-57886 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Kersting, R. A1 - Hagenhoff, B. A1 - Bennet, Francesca A1 - Ciornii, Dmitri A1 - Nymark, P. A1 - Grafström, R. A1 - Hodoroaba, Vasile-Dan T1 - Reliable Surface Analysis Data of Nanomaterials in Support of Risk Assessment Based on Minimum Information Requirements N2 - The minimum information requirements needed to guarantee high-quality surface Analysis data of nanomaterials are described with the aim to provide reliable and traceable Information about size, shape, elemental composition and surface chemistry for risk assessment approaches. The widespread surface analysis methods electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS) were considered. The complete analysis sequence from sample preparation, over measurements, to data analysis and data format for reporting and archiving is outlined. All selected methods are used in surface analysis since many years so that many aspects of the analysis (including (meta)data formats) are already standardized. As a practical analysis use case, two coated TiO2 reference nanoparticulate samples, which are available on the Joint Research Centre (JRC) repository, were selected. The added value of the complementary analysis is highlighted based on the minimum information requirements, which are well-defined for the analysis methods selected. The present paper is supposed to serve primarily as a source of understanding of the high standardization level already available for the high-quality data in surface analysis of nanomaterials as reliable input for the nanosafety community. KW - Electron microscopy KW - X-ray photoelectron spectroscopy KW - Secondary ion mass spectrometry KW - Energy dispersive X-ray spectroscopy KW - Standardization PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522683 DO - https://doi.org/10.3390/nano11030639 VL - 11 IS - 3 SP - 639 PB - MDPI AN - OPUS4-52268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Radnik, Jörg A1 - Schönhals, Andreas T1 - Unraveling the Dynamics of Nanoscopically Confined PVME in Thin Films of a Miscible PVME/PS Blend N2 - Broadband dielectric spectroscopy (BDS) was employed to investigate the glassy dynamics of thin films (7−200 nm) of a poly(vinyl methyl ether) (PVME)/polystyrene (PS) blend (50:50 wt %). For BDS measurements, nanostructured capacitors (NSCs) were employed, where films are allowed a free surface. This method was applied for film thicknesses up to 36 nm. For thicker films, samples were prepared between crossed electrode capacitors (CECs). The relaxation spectra of the films showed multiple processes. The first process was assigned to the α-relaxation of a bulklike layer. For films measured by NSCs, the rates of α-relaxation were higher compared to those of the bulk blend. This behavior was related to the PVME-rich free surface layer at the polymer/air interface. The second process was observed for all films measured by CECs (process X) and the 36 nm film measured by NSCs (process X2). This process was assigned to fluctuations of constraint PVME segments by PS. Its activation energy was found to be thickness-dependent because of the evidenced thickness dependency of the compositional heterogeneity. Finally, a third process with an activated temperature dependence was observed for all films measured by NSCs (process X1). It resembled the molecular fluctuations in an adsorbed layer found for thin films of pure PVME, and thus, it is assigned accordingly. This process undergoes an extra confinement because of frozen adsorbed PS segments at the polymer/substrate interface. To our knowledge, this is the first example where confinement-induced changes were observed by BDS for blend thin films KW - Thin Films KW - Broadband Dielectric Spectroscopy PY - 2017 DO - https://doi.org/10.1021/acsami.7b10572 SN - 1944-8244 VL - 9 IS - 42 SP - 37289 EP - 37299 PB - ACS Publications AN - OPUS4-42652 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Chemello, Giovanni T1 - Characterization of Graphene using HAXPES N2 - Since its discovery, graphene has got growing attention in the industrial and application research due to its unique properties . However, graphene has not been yet implemented into the industrial market, in particularly due to the difficulty of properly characterizing this challenging material. As most of other nanomaterials, graphene’s properties are closely linked to its chemical and structural properties, such as number of layers, flake thickness, degree of functionalisation and C/O ratio. For the commercialization, suitable procedures for the measurement and characterization of the ultrathin flakes, of lateral dimensions in the range from µm to tens of µm, are essential.Surface chemical methods, especially XPS, have an outstanding role of providing chemical information on the composition. Thereby, one well-known problem for surface analytical methods is the influence of contamination on the composition as in the case of adventitious carbon. The differentiation between carbon originated from the contamination or from the graphene sample itself is often not obvious, which can lead to altered results in the determination of the composition. To overcome this problem, Hard Energy X-ray Photoelectron Spectroscopy (HAXPES) offers new possibilities due to its higher information depth. Therefore, XPS measurement obtained with Al Kα radiation (E = 1486. 6 eV) were compared with analyses performed with a Cr Kα (E = 5414. 8 eV) excitation on functionalized graphene samples. Differences are discussed in terms of potential carbon contamination, but also of oxygen on the composition of the samples. Measurements are performed on O-, N- and F-functionalized graphene. Different preparation procedures (powder, pellet, drop cast from liquid suspension) will be also discussed, correlation of the results with the flakes morphology as well as their validation with other independent methods are in progress. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Graphene KW - Functionalized graphene KW - Depth profiling PY - 2022 AN - OPUS4-56814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pu, Y. A1 - Celorrio, V. A1 - Stockmann, Jörg Manfred A1 - Sobol, Oded A1 - Sun, Z. A1 - Wang, W. A1 - Lawrence, M. J. A1 - Radnik, Jörg A1 - Russel, A. E. A1 - Hodoroaba, Vasile-Dan A1 - Huang, L. A1 - Rodriguez, P. T1 - Surface galvanic formation of Co-OH on Birnessite and its catalytic activity for the oxygen evolution reaction N2 - Low-cost, high-efficient catalysts for water splitting can be potentially fulfilled by developing earthabundant metal oxides. In this work, surface galvanic formation of Co-OH on K0.45MnO2 (KMO) was achieved via the redox reaction of hydrated Co2+ with crystalline Mn4+. The synthesis method takes place at ambient temperature without using any surfactant agent or organic solvent, providing a clean, green route for the design of highly efficient catalysts. The redox reaction resulted in the formation of ultrathin Co-OH nanoflakes with high electrochemical surface area. X-ray absorption spectroscopy (XAS) and X-ray photoelectron spectroscopy (XPS) analysis confirmed the changes in the oxidation state of the bulk and surface species on the Co-OH nanoflakes supported on the KMO. The effect of the anions, such as chloride, nitrate and sulfate, on the preparation of the catalyst was evaluated by electrochemical and spectrochemical means. XPS and Time of flight secondary ion mass spectrometry (ToF-SIMS) analysis demonstrated that the layer of CoOxHy deposited on the KMO and its electronic structure strongly depend on the anion of the precursor used during the synthesis of the catalyst. In particular, it was found that Cl- favors the formation of Co-OH, changing the rate-determining step of the reaction, which enhances the catalytic activity towards the OER, producing the most active OER catalyst in alkaline media. KW - Nanoparticles KW - Oxygen evolution reaction (OER) KW - Catalysis KW - ToF-SIMS KW - XPS KW - K-rich Birnessite (K0.45MnO2) PY - 2021 DO - https://doi.org/10.1016/j.jcat.2021.02.025 VL - 396 SP - 304 EP - 314 PB - Elsevier Inc. AN - OPUS4-52328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Energy-resolved x-ray photoelectron spectroscopy measurements on the concentration profile of thin blended poly(vinyl methyl ether)/polystyrene films N2 - The composition of thin films of polymer blends in vertical direction is still under discussion. For explaining the thickness dependence of some properties like the thermal glass transition temperature, a three-layer model has been introduced consisting of an adsorbed layer with a reduced segmental mobility at the substrate, a bulk-like layer in the middle of the film and an outermost surface layer with a higher molecular mobility. X-ray photoelectron spectroscopy (ER-XPS) measurements with a varying excitation energy from 400 eV to 1486.6 eV and, herewith, an information depth from 1.5 nm to 10 nm were performed at PVME/PS films with compositions of 25/75 wt% and 50/50 wt% and thicknesses between 15 nm and 190 nm. As expected, it was found that the PVME concentration decreases with increasing information depth. Secondly, a complex correlation between the PVME concentration at the surface and the film thickness was found. The PVME concentration increases with decreasing film thickness until a maximum at 30 nm. For thinner films, the PVME concentration decreases. These data agree with previous investigations obtained with specific heat spectroscopy. We thank BESSY II (HZB) for the allocation of beamtime at the HE-SGM beamline and for technical support. DFG (Project number 124846229) is acknowledged for financial support. T2 - German Conference for Research with Synchrotron Radiation, Neutrons and Ion Beams at Large Facilities (SNI2022) CY - Berlin, Germany DA - 05.09.2022 KW - X-ray photoelectron spectroscopy KW - Miscible polymer films KW - Depth profiling PY - 2022 AN - OPUS4-55654 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - VAMAS ILC of functionalized Graphene by XPS and Graphene Oxide by SEM N2 - The ideas of the planned VAMAS interlaboratory comparisons of functionalized graphene and graphene oxide are presented. T2 - Stakeholder Advisory Board ISO-G-Scope CY - Online meeting DA - 12.01.2022 KW - Graphene KW - XPS KW - SEM PY - 2022 AN - OPUS4-54375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - In-situ monitoring of water dependent DNA and protein radiation damage by near-ambient-pressure XPS N2 - X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. Our results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further. T2 - ICRR 2023 CY - Montreal, Canada DA - 26.08.2023 KW - DNA KW - XPS KW - Proteins KW - Protein KW - G5P KW - Base damage KW - Base loss KW - Cancer treatment KW - DEA KW - DET KW - DNA radiation damage KW - Direct damage KW - Dissociative electron attachment (DEA) KW - Dissociative electron transfer (DET) KW - Dosimetry KW - ESCA KW - Energy deposit KW - Geant4 KW - Geant4-DNA KW - Hydrated DNA KW - Hydrated electron KW - Hydrated electrons KW - Hydration shell KW - Hydroxyl radical KW - Indirect damage KW - Ionisation KW - Ionization KW - LEE KW - Low energy electrons KW - MCS KW - Microdosimetry KW - NAP-XPS KW - Near ambient pressure xray photo electron spectroscopy KW - Net-ionization reaction KW - OH radical KW - PES KW - Particle scattering KW - Prehydrated electron KW - Presolvated electron KW - Quasi-direct damage KW - ROS KW - Radiation damage KW - Radiation therapy KW - Radical KW - Radiolysis KW - Radiotherapy KW - Reactive oxygen species KW - Simulation KW - Single-strand break (SSB) KW - Single-stranded DNA-binding proteins KW - TOPAS KW - TOPAS-nbio KW - TopasMC KW - Xray photo electron spectrocopy PY - 2023 AN - OPUS4-58214 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Page, T.M. A1 - Nie, C. A1 - Neander, L. A1 - Povolotsky, T.L. A1 - Sahoo, A.K. A1 - Nickl, Philip A1 - Adler, J.M. A1 - Bawadkji, O. A1 - Radnik, Jörg A1 - Achazi, K. A1 - Ludwig, K. A1 - Lauster, D. A1 - Netz, R.R. A1 - Trimpert, J. A1 - Kaufer, B. A1 - Haag, R. A1 - Donskyi, Ievgen T1 - Functionalized Fullerene for Inhibition of SARS-CoV-2 Variants N2 - As virus outbreaks continue to pose a challenge, a nonspecific viral inhibitor can provide significant benefits, especially against respiratory viruses. Polyglycerol sulfates recently emerge as promising agents that mediate interactions between cells and viruses through electrostatics, leading to virus inhibition. Similarly, hydrophobic C60 fullerene can prevent virus infection via interactions with hydrophobic cavities of surface proteins. Here, two strategies are combined to inhibit infection of SARS-CoV-2 variants in vitro. Effective inhibitory concentrations in the millimolar range highlight the significance of bare fullerene’s hydrophobic moiety and electrostatic interactions of polysulfates with surface proteins of SARS-CoV-2. Furthermore, microscale thermophoresis measurements support that fullerene linear polyglycerol sulfates interact with the SARS-CoV-2 virus via its spike protein, and highlight importance of electrostatic interactions within it. All-atom molecular dynamics simulations reveal that the fullerene binding site is situated close to the receptor binding domain, within 4 nm of polyglycerol sulfate binding sites, feasibly allowing both portions of the material to interact simultaneously. KW - Covalent functionalization KW - Fullerene KW - SARS-CoV 2 KW - Sulfated materials KW - Virus inhibition PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568672 DO - https://doi.org/10.1002/smll.202206154 SN - 1613-6810 SP - 1 EP - 8 PB - Wiley VCH AN - OPUS4-56867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Czeskleba, Denis A1 - Nietzke, Jonathan A1 - Rhode, Michael A1 - Kannengießer, Thomas T1 - Investigation of stress relief crack susceptibility of CrMoV steels coarse grain HAZ via simulation of uniaxial stress conditions during PWHT N2 - Creep-resistant steels such as the 13CrMoV9-10, used in the construction of thick-walled pressure vessels, are most commonly submerged arc welded (SAW). These steels can develop stress relief cracks (SRC) if the mandatory post weld heat treatment (PWHT) is performed improperly. Current PWHT parameters, such as heating rate and holding time at a specific holding temperature, are based on both empirical experience and conventional free shrinking welding experiments to characterize the SRC-susceptibility of the weld. These cannot adequately depict the higher residual stresses caused by the structurally induced stiffness of the surrounding construction. This study discusses the development of a repeatable, precise, and time-efficient methodology to study the effects of different stress levels and heating rates on the SRC susceptibility of the coarse grain heat-affected zone (CGHAZ). For that purpose, samples were thermically treated to simulate a coarse grain heat-affected zone (CGHAZ) and subsequently exposed to representative levels of stress during the heating phase of a PWHT. The recorded stress and heating rate–dependent strains were mathematically analyzed via curve tracing/calculus to identify interdependent effects. This procedure facilitates the measurement of material characteristics such as carbide growth on grain boundaries at the µm-scale via an integrated value over the entire sample volume. The first and second derivatives show a slight, precipitate-dependent, increase in hardness of the sample, depending on the heating rate and applied stress. This new methodology generates an improved assessment of the SRC susceptibility of SAW microstructures of creep-resistant CrMoV steels. KW - Submerged arc welding KW - Creep-resistant steel KW - Stress relief cracking KW - Component-like test KW - Post weld heat treatment PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576007 DO - https://doi.org/10.1007/s40194-023-01539-x SN - 0043-2288 SP - 1 EP - 9 PB - Springer Nature CY - Basel (CH) AN - OPUS4-57600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jungnickel, R. A1 - Mirabella, Francesca A1 - Stockmann, Jörg Manfred A1 - Radnik, Jörg A1 - Balasubramanian, K. T1 - Graphene‑on‑gold surface plasmon resonance sensors resilient to high‑temperature annealing N2 - Gold films coated with a graphene sheet are being widely used as sensors for the detection of label-free binding interactions using surface plasmon resonance (SPR). During the preparation of such sensors, it is often essential to subject the sensor chips to a high-temperature treatment in order to ensure a clean graphene surface. However, sensor chips used currently, which often use chromium as an adhesion promoter, cannot be subjected to temperatures above 250 °C, because under such conditions, chromium is found to reorganize and diffuse to the surface, where it is easily oxidized, impairing the quality of SPR spectra. Here we present an optimized preparation strategy involving a three-cycle tempering coupled with chromium (oxide) etching, which allows the graphene-coated SPR chips to be annealed up to 500 °C with little deterioration of the surface morphology. In addition, the treatment delivers a surface that shows a clear enhancement in spectral response together with a good refractive index sensitivity. We demonstrate the applicability of our sensors by studying the kinetics of avidin–biotin binding at different pH repeatedly on the same chip. The possibility to anneal can be exploited to recover the original surface after sensing trials, which allowed us to reuse the sensor for at least six cycles of biomolecule adsorption. KW - Surface plasmon resonance KW - Graphene KW - Sensing KW - Surface regeneration PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564585 DO - https://doi.org/10.1007/s00216-022-04450-4 SN - 1618-2642 SP - 1 EP - 7 PB - Springer AN - OPUS4-56458 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Quackatz, Lukas A1 - Gornushkin, Igor B. A1 - Griesche, Axel A1 - Kannengießer, Thomas A1 - Treutler, Kai A1 - Wesling, Volker T1 - In situ chemical analysis of duplex stainless steel weld by laser induced breakdown spectroscopy N2 - The high corrosion resistance and good mechanical properties of duplex stainless steel (DSS) are due to its special chemical composition, which is a balanced phase ratio of ferrite (α) and austenite (γ). Many industrial applications require the integration of DSS components. For this, Gas tungsten arc welding (GTAW) is an excellent choice, as it allows an automated operation with high reproducibility. However, when the weld pool solidifies, critical ratios of α- and γ- phases can occur, which lead to solidification cracking, increased susceptibility to corrosion, and a decrease in ductility and critical strength. Previous studies have shown that these defects can be caused by the accumulation of manganese and chromium in the heat affected zone (HAZ), requiring ongoing monitoring of this accumulation. A suitable method for such monitoring is laser-induced breakdown spectroscopy (LIBS), which can be used in two operating modes: calibration using standard reference samples and calibration-free. Unlike conventional quantitative LIBS measurements, which require reference samples to generate a calibration curve, calibration-free LIBS (CF-LIBS) allows chemical compositions to be determined solely from the emission spectrum of the plasma. Numerous publications show that CF-LIBS is a fast and efficient analytical method for the quantitative analysis of metal samples. In this work, CF-LIBS is applied to spectra obtained during GTAW DSS welding and the result is compared with those obtained by PLS analysis. A good correlation was found between both types of analysis, demonstrating the suitability of the CF-LIBS method for this application. The CF-LIBS method has a significant advantage over conventional LIBS due to the rapid in situ measurement of concentrations of major alloying elements without calibration procedure. This, combined with fast feedback and appropriate adjustment of welding parameters, helps prevent welding defects. KW - Duplex stainless steels KW - In situ measurement KW - LIBS KW - GMAW PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-597940 DO - https://doi.org/10.1016/j.sab.2024.106899 SN - 0584-8547 VL - 214 SP - 1 EP - 7 PB - Elsevier B.V. AN - OPUS4-59794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reed, B. P. A1 - Cant, D.J.H. A1 - Spencer, S.J. A1 - Carmona-Carmona, A. J. A1 - Bushell, A. A1 - Herrara-Gómez, A. A1 - Kurokawa, A. A1 - Thissen, A. A1 - Thomas, A.G. A1 - Britton, A.J. A1 - Bernasik, A. A1 - Fuchs, A. A1 - Baddorf, A.P. A1 - Bock, B. A1 - Thellacker, B. A1 - Cheng, B. A1 - Castner, D.G. A1 - Morgan, D.J. A1 - Valley, D. A1 - Willneff, E.A. A1 - Smith, E.P. A1 - Nolot, E. A1 - Xie, F. A1 - Zorn, G. A1 - Smith, G.C. A1 - Yasukufu, H. A1 - Fenton, J.L. A1 - Chen, J. A1 - Counsell, J.D.P. A1 - Radnik, Jörg A1 - Gaskell, K.J. A1 - Artyushkova, K. A1 - Yang, L. A1 - Zhang, L. A1 - Eguchi, M. A1 - Walker, M. A1 - Hajdyla, M. A1 - Marzec, M.M. A1 - Linford, M.R. A1 - Kubota, N. A1 - Cortazar-Martinez, O. A1 - Dietrich, P. A1 - Satoh, R. A1 - Schroeder, S.L.M. A1 - Avval, T.G. A1 - Nagatomi, T. A1 - Fernandez, V. A1 - Lake, W. A1 - Azuma, Y. A1 - Yoshikawa, Y. A1 - Compean-Gonzalez, C.L. A1 - Ceccone, G. A1 - Shard, A.G. T1 - ERRATUM: “Versailles project on advanced materials and standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene” [J. Vac. Sci. Technol. A 38, 063208 (2020)] N2 - The lead authors failed to name two collaborators as co-authors. The authors listed should include: Miss Claudia L. Compean-Gonzalez (ORCID: 0000-0002-2367-8450) and Dr. Giacomo Ceccone (ORCID: 0000-0003-4637-0771). These co-authors participated in VAMAS project A27, provided data that were analyzed and presented in this publication (and supporting information), and reviewed the manuscript before submission. KW - X-ray photoelectron spectroscopy KW - Transmission function KW - Low-density polyethylene PY - 2021 DO - https://doi.org/10.1116/6.0000907 VL - 39 IS - 2 SP - 027001 PB - American Vacuum Society AN - OPUS4-52380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reed, B. P. A1 - Cant, D.J.H. A1 - Spencer, J. A1 - Carmona-Carmona, A. J. A1 - Bushell, A. A1 - Herrara-Gómez, A. A1 - Kurokawa, A. A1 - Thissen, A. A1 - Thomas, A.G. A1 - Britton, A.J. A1 - Bernasik, A. A1 - Fuchs, A. A1 - Baddorf, A. P. A1 - Bock, B. A1 - Thellacker, B. A1 - Cheng, B. A1 - Castner, D.G. A1 - Morgan, D.J. A1 - Valley, D. A1 - Willneff, E.A. A1 - Smith, E.F. A1 - Nolot, E. A1 - Xie, F. A1 - Zorn, G. A1 - Smith, G.C. A1 - Yasukufu, H. A1 - Fenton, J. L. A1 - Chen, J. A1 - Counsell, J..D.P. A1 - Radnik, Jörg A1 - Gaskell, K.J. A1 - Artyushkova, K. A1 - Yang, L. A1 - Zhang, L. A1 - Eguchi, M. A1 - Walker, M. A1 - Hajdyla, M. A1 - Marzec, M.M. A1 - Linford, M.R. A1 - Kubota, N. A1 - Cartazar-Martínez, O. A1 - Dietrich, P. A1 - Satoh, R. A1 - Schroeder, S.L.M. A1 - Avval, T.G. A1 - Nagatomi, T. A1 - Fernandez, V. A1 - Lake, W. A1 - Azuma, Y. A1 - Yoshikawa, Y. A1 - Shard, A.G. T1 - Versailles Project on Advanced Materials and Standards interlaboratory study on intensity calibration for x-ray photoelectron spectroscopy instruments using low-density polyethylene N2 - We report the results of a Versailles Project on Advanced Materials and Standards interlaboratory study on the intensity scale calibration of x-ray photoelectron spectrometers using low-density polyethylene (LDPE) as an alternative material to gold, silver, and copper. An improved set of LDPE reference spectra, corrected for different instrument geometries using a quartz-monochromated Al Kα x-ray source, was developed using data provided by participants in this study. Using these new reference spectra, a transmission function was calculated for each dataset that participants provided. When compared to a similar calibration procedure using the NPL reference spectra for gold, the LDPE intensity calibration method achieves an absolute offset of ∼3.0% and a systematic deviation of ±6.5% on average across all participants. For spectra recorded at high pass energies (≥90 eV), values of absolute offset and systematic deviation are ∼5.8% and ±5.7%, respectively, whereas for spectra collected at lower pass energies (<90 eV), values of absolute offset and systematic deviation are ∼4.9% and ±8.8%, respectively; low pass energy spectra perform worse than the global average, in terms of systematic deviations, due to diminished count rates and signal-to-noise ratio. Differences in absolute offset are attributed to the surface roughness of the LDPE induced by sample preparation. We further assess the usability of LDPE as a secondary reference material and comment on its performance in the presence of issues such as variable dark noise, x-ray warm up times, inaccuracy at low count rates, and underlying spectrometer problems. In response to participant feedback and the results of the study, we provide an updated LDPE intensity calibration protocol to address the issues highlighted in the interlaboratory study. We also comment on the lack of implementation of a consistent and traceable intensity calibration method across the community of x-ray photoelectron spectroscopy (XPS) users and, therefore, propose a route to achieving this with the assistance of instrument manufacturers, metrology laboratories, and experts leading to an international standard for XPS intensity scale calibration. KW - X-ray photoelectron spectroscopy KW - Transmission function KW - Intensity scale calibration KW - Reference spectra KW - Low-density polyethylene (LDPE) PY - 2020 DO - https://doi.org/10.1116/6.0000577 VL - 38 IS - 6 SP - 063208 AN - OPUS4-51655 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Reliable Chemical Characterization Protocols for Industrial Graphene-Related Materials N2 - Since its isolation, graphene has received growing attention from academia and industry due to its unique properties. Promising opportunities for applications are discussed in different field like electronics and optoelectronics, detection, and sensing devices, biosystems or chemical and environmental corrosion inhibition. Here, functionalization with elements like oxygen, nitrogen or fluorine can broaden the application, for example in composite materials. However, lack of generally accepted operation procedures hinders the commercialization, the so-called “what is my material” barrier. Therefore, first efforts were done to develop common, reliable, and reproducible ways to characterize the morphological and chemical properties of the industrially produced material. In this contribution, our efforts in the development of reliable chemical characterizations protocols for functionalized graphene are presented. An ISO standard for the chemical characterization of graphene-related (GRM) is under development with X-ray photoelectron spectroscopy (XPS) having a prominent role. With its information depth of around 10 nm, which is the similar length scale as the thickness of particles of 2D materials consisting of a few monolayers, XPS seems to be highly suitable for the quantitative analysis of (functionalized) GRM. Thereby, different sample preparation methods like pressing the powders onto adhesive tapes, into recesses, or into solid pellets result in inconsistencies in the quantification. Furthermore, different morphologies like stacks of graphene layers (left figure) or irregular particles (right figure) lead to different analysis results for the chemical composition. For the validation of the quantification with XPS and the further development of standards an international interlaboratory comparison was initiated under the head of the “Versailles Project on Advanced Materials and Standards” (VAMAS). First results are reported showing the suitability of the protocols. Finally, the XPS results are compared with the elemental composition results obtained after quantification with energy-dispersive X-ray spectroscopy (EDS) as a fast analytical method which is usually combined with electron microscopy. T2 - nanoSAFE 2023 CY - Grenoble, France DA - 05.06.2023 KW - X-ray photoelectron spectroscopy KW - Functionalized graphene KW - Interlaboratory comparison KW - VAMAS PY - 2023 AN - OPUS4-57652 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sötebier, Carina A1 - Weidner, Steffen A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Bettmer, J. T1 - Separation and quantification of silver nanoparticles and silver ions using reversed phase high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry in combination with isotope dilution analysis N2 - A reversed phase high performance liquid chromatography coupled to an inductively coupled plasma mass spectrometer (HPLC-ICP-MS) approach in combination with isotope dilution analysis (IDA) for the separation and parallel quantification of nanostructured and ionic silver (Ag) is presented. The main focus of this work was the determination of the ionic Ag concentration. For a sufficient stabilization of the ions without dissolving the nanoparticles (NPs), the eluent had to be initially optimized. The determined Ag ion concentration was in a good agreement with results obtained using ultrafiltration. Further, the mechanism of the NP separation in the HPLC column was investigated. Typical size exclusion effects were found by comparing results from columns with different pore sizes. Since the recovery rates decreased with increasing Ag NP size and large Ag NPs did not elute from the column, additional interactions of the particles with the stationary phase were assumed. Our results reveal that the presented method is not only applicable to Ag NPs, but also to gold and polystyrene NPs. Finally, IDA-HPLC-ICP-MS experiments in single particle mode were performed to determine the particle cut-off size. The comparison with conventional spICP-MS experiments resulted in a similar diameter and particle size distribution. KW - ICP-MS KW - Silver nanoparticles KW - HPLC KW - Isotope dilution analysis KW - Field flow fractionation KW - Toxicology PY - 2016 DO - https://doi.org/10.1016/j.chroma.2016.09.028 SN - 0021-9673 VL - 1468 SP - 102 EP - 108 PB - Elsevier B.V. AN - OPUS4-38642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Greiser, Sebastian A1 - Hunger, M. A1 - Jäger, Christian T1 - 29Si{27Al} TRAPDOR MAS NMR to distinguish Qn(mAl) sites in aluminosilicates. Test case: Faujasite-type zeolites N2 - 29Si{27Al} TRAPDOR MAS NMR was applied to two faujasite-type zeolites with Si/Al ratios of 1.3 (Na-X) and 2.7 (Na-Y). The aim of this test study is to show that different Q4(mAl) sites (m=4,3,2,1) can be distinguished by differently strong TRAPDOR effects (ΔS/S0). Indeed, it was found that the TRAPDOR effect depends on the number m of AlO4 units connected to the Q4 silicon tetrahedrons. For Na-X, the measured ΔS/S0 values are 1:0.81:0.56 for Q4(4Al), Q4(3Al) and Q4(2Al), respectively (normalized to Q4(4Al)). The corresponding ΔS/S0 values are the same for Na-Y within the error bars, although the silicon sites are different: Q4(3Al), Q4(2Al) and Q4(1Al) and now normalized to Q4(3Al) as no Q4(4Al) is present. Nevertheless, the proposed method opens up the possibility to distinguish overlapping 29Si NMR signals of the Qn(mAl) sites in amorphous materials as the main goal of these investigations. KW - Solid-state NMR KW - 29Si{27Al} TRAPDOR MAS NMR KW - Q4(mAl) sites KW - Faujasite-type zeolites KW - Aluminosilicates PY - 2016 DO - https://doi.org/10.1016/j.ssnmr.2016.10.004 SN - 0926-2040 SN - 1527-3326 VL - 80 SP - 6 EP - 10 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-38718 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - De Souza, C.M.G. A1 - Greiser, Sebastian A1 - Garcia, E. A1 - Quarcioni, V.A. A1 - Jäger, Christian T1 - Evaluation of pozzolanic reactivity of calcined kaolinite N2 - The need to improve the sustainability and the need for innovation in the cement industry has brought to light the practice of using additives to the cement in order to decrease CO2 emissions in industrial plants and increase the quality of cement in terms of durability and performance. Currently some additives have been employed as granulated blast furnace slag, limestone and pozzolan. The additives give mortar and concrete larger energy efficiency, gain in durability and resistance, contributing to buildings with slender structures and cheaper and durable maintenance. Besides natural pozzolan can be used artificial ones, as calcined clays, and over a range of amorphous aluminates and silicates waste, with highly reactive function as a binder material in the presence of water and calcium hydroxide. Calcined kaolinite clays were characterized using various techniques such as XRD, thermal analysis, and NMR observing 27Al and 29Si nuclei. The results showed that there is a structural modification of the samples, from crystalline to amorphous phases with the increasing of temperature in the calcination process. There is an improving in the reactivity of calcined clays by the range of 600ºC to 750ºC temperature in the reaction with calcium oxide, according to data from Chapelle test, indicating the possibility of using them as additives for cement and confirming their pozzolanic potential. KW - Kaolin KW - Pozzolan KW - Calcined clays KW - Cement additive PY - 2014 DO - https://doi.org/10.15623/ijret.2014.0325033 SN - 2321-7308 SN - 2319-1163 VL - 3 IS - Special Issue 13 SP - 209 EP - 213 PB - eSAT Publishing House CY - Kothapatnam AN - OPUS4-38719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - “Click” analytics for “click” chemistry – a simple method for calibration-free evaluation of online NMR spectra N2 - Currently research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual cam-paigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The re-sulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via compara-bly straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algo-rithm to interpret the ob-tained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16 inch polymer tubing working as a flow cell. Single scan 1H spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. T2 - 12. Kolloquium des Arbeitskreises Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Online NMR KW - Online monitoring KW - “Click” chemistry PY - 2016 AN - OPUS4-38585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abdelshafi, Nahla A. T1 - Electrochemical immunosensor for screening using voltammetry N2 - Immunoassays based on the detection of the antibody -Antigen interaction belong to the most important analytical techniques. Electrochemical methods in immunoassays are increasingly used as they offer some advantages as being fast, simple, portable and cheap detection methods. Cocaine is a highly addictive stimulant that occurs naturally as an Alkaloid of the Coca plants. It is frequently detected on bank notes and in wastewater. T2 - 67th Annual Meeting of the International Socieity of Electrochemistry CY - The Hague, The Netherlands DA - 21.08.2016 KW - Cocain PY - 2016 AN - OPUS4-38551 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abdelshafi, Nahla A. T1 - Microfluidic electrochemical immunosensor for cocaine monitoring N2 - Immunoassays based on the detection of the antibody-antigen interaction belong to the most important analytical techniques. Electrochemical methods in immunoassays are increasingly used as they offer some Advantages as being fast, simple, portable and cheap detection methods. Cocaine is a highly addictive stimulant that occurs naturally as an Alkaloid of the Coca plants. It is frequently detected on bank notes and in wastewater. T2 - Biosensors 2016 CY - Gothenburg, Sweden DA - 25.05.2016 KW - Cocain PY - 2016 AN - OPUS4-38552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Loehr, Konrad T1 - Towards quantitative high throughput single cell LA-ICP-MS: microarraying of single cells and calibration standards via piezo based non-contact dispensing N2 - Analysis of single cells via LA-ICP-MS is a technique with great potential, however manual targeting of single cells is laborious and therefore microarraying of cells looks promising. In this work, we investigate the potential of a commercial non-contact piezo dispenser arraying system (S3, Scienion AG, Berlin), equipped with a novel technology for single-cell Isolation called CellenONE™ (Cellenion, Lyon). Usually if one aims to create a microarray of single cells via spotting a suitably diluted cell suspension, one will observe a Poisson-distributed cell number per spot. CellenONE™ overcomes this problem by controlling the number of cells optically in the piezo dispense capillary (PDC) via image recognition to obtain true single cell arrays. We will present the figures of merit of the customized and optimized setup. As a model system we use THP-1 cells stained with two dyes, mDOTAHo(CheMatech, Dijon), and Ir-DNA intercalator (Fluidigm, San Francisco) and used LA-ICP-MS (NWR213, ESI, Portland; ElementXR, ThermoScientific, Bremen) to measure Ho and Ir signals from single cells. Both metallo-dyes will be quantified by matrix matched calibration at single cell resolution after Wang et al. (Anal. Chem. 2014, 86, 10252−10256). We believe that this novel approach opens new ways for automated quantitative single cell LA-ICP-MS. T2 - Metallomics 2017 CY - Vienna, Austria DA - 13.08.2017 KW - Single cell arraying PY - 2017 AN - OPUS4-41873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Molecular absorption spectrometry: a fast and accurate optical method for boron isotope analysis comparable to mass spectrometry N2 - Boron presents two stable isotopes, 10B and 11B and due to their relatively large mass difference (~ 10%) isotope fractionation leads to considerable isotope amount ratio variations n(10B)/n(11B) in natural occurrence. These have been used as a proof of provenance of mineral and biological samples, to estimate a contamination source and to the determination of geological processes by erosion or subduction. Additionally, boron is employed in the nuclear industry due to the capability of its isotope 10B to thermal-neutron capture and therefore 10B enriched boric acid solutions are used in the cooling system of thermonuclear facilities and in the alloying of steel and carbides for protective shielding. Usually, isotope ratio variations are determined by mass spectroscopic methods. Here an alternative faster and low cost method for isotope ratio determination is proposed: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Boron isotope amount ratios have been determined by monitoring the absorption spectrum of boron monohydride (BH) in graphite furnace HR-CS-MAS. Bands (0→0) and (1→1) for the electronic transition X1Σ+ → A1Π were evaluated around wavelengths 433.1 nm and 437.1 nm respectively. Partial least square regression (PLS) for analysis of samples and reference materials were applied. For this, a spectral library with different isotopes ratios for PLS regression was built. Results obtained around the 433.1 nm and 437.1 nm spectral regions are metrologically compatible with those reported by mass spectrometric methods. Moreover, a precision and accuracy of the method of ± 0.5 ‰ for the evaluated spectral region around 437.1 nm is reported here. This accuracy and precision is comparable with those obtained by thermal ionization mass spectrometry (TIMS) and multiple collector inductively coupled plasma mass spectrometry (MC-ICP-MS) for boron isotope ratio measurements. T2 - 30. Tag der Chemie CY - Berlin, Germany DA - 05.07.2017 KW - Boron isotopes KW - High-Resolution Continuum Source Molecular Absorption Spectrometry KW - HR-CS-MAS KW - Isotopic shift KW - Boron monohydride KW - Isotope ratio KW - Molecular absorption KW - Memory effect KW - Graphite furnace PY - 2017 AN - OPUS4-41059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Calibration-free Monte Carlo method for laser induced breakdown spectroscopy N2 - Calibration-free LIBS via Monte Carlo approach T2 - 8-14.10.2017 SciX, Reno, NV, USA CY - Reno, NV, USA DA - 7.10.2016 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics KW - Lasers PY - 2017 AN - OPUS4-42298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Calibration-free Monte Carlo method for laser induced breakdown spectroscopy N2 - Calibration-free LIBS by Monte Carlo simulation of plasma spectra T2 - April 26 2017, Johannes Kepler University, Linz, Austria CY - Johannes Kepler University, Linz, Austria DA - 26.04.2017 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2017 AN - OPUS4-42288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Model of stimulated emission in aluminium laser-induced plasma produced by resonance pumping N2 - Model of lasing effect in resonantly pumped aluminum laser induced plasma T2 - EMS LIBS CY - Pisa, Italy DA - 11.06.2017 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2017 AN - OPUS4-42292 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Demidov, Alexandr A1 - Eschlböck-Fuchs, S. A1 - Kazakov, Alexander Ya. A1 - Gornushkin, Igor B. A1 - Kolmhofer, P. J. A1 - Pedarnig, J. D. A1 - Huber, N. A1 - Heitz, J. A1 - Schmid, Thomas A1 - Rössler, R. A1 - Panne, Ulrich T1 - Monte Carlo standardless approach for laser induced breakdown spectroscopy based on massive parallel graphic processing unit computing N2 - The improved Monte-Carlo (MC) method for standard-less analysis in laser induced breakdown spectroscopy (LIBS) is presented. Concentrations in MC LIBS are found by fitting model-generated synthetic spectra to experimental spectra. The current version of MC LIBS is based on the graphic processing unit (GPU) computation and reduces the analysis time down to several seconds per spectrum/sample. The previous version of MC LIBS which was based on the central processing unit (CPU) computation requested unacceptably long analysis times of 10's minutes per spectrum/sample. The reduction of the computational time is achieved through the massively parallel computing on the GPU which embeds thousands of co-processors. It is shown that the number of iterations on the GPU exceeds that on the CPU by a factor > 1000 for the 5-dimentional parameter space and yet requires > 10-fold shorter computational time. The improved GPU-MC LIBS outperforms the CPU-MS LIBS in terms of accuracy, precision, and analysis time. The performance is tested on LIBS-spectra obtained from pelletized powders of metal oxides consisting of CaO, Fe2O3, MgO, and TiO2 that simulated by-products of steel industry, steel slags. It is demonstrated that GPU-based MC LIBS is capable of rapid multi-element analysis with relative error between 1 and 10's percent that is sufficient for industrial applications (e.g. steel slag analysis). The results of the improved GPU-based MC LIBS are positively compared to that of the CPU-based MC LIBS as well as to the results of the standard calibration-free (CF) LIBS based on the Boltzmann plot method. KW - Monte Carlo simulation KW - Parallel computing KW - Calibration-free laser-induced breakdown spectroscopy KW - Post-breakdown laser induced plasma KW - Quaternary oxides PY - 2016 DO - https://doi.org/10.1016/j.sab.2016.09.016 VL - 125 SP - 97 EP - 102 PB - Elsevier B.V. AN - OPUS4-38489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Franziska A1 - Lubjuhn, Dominik A1 - Greiser, Sebastian A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Supply and demand in the ball mill: competitive cocrystal reactions N2 - The stability of different theophylline cocrystals under milling conditions was investigated by competitive cocrystal reactions. To determine the most stable cocrystal form under milling conditions, the active pharmaceutical ingredient theophylline was either ground with two similar coformers (benzoic acid, benzamide, or isonicotinamide), or the existing theophylline cocrystals were ground together with a competitive coformer. All competitive reactions were investigated by in situ powder X-ray diffraction disclosing the formation pathway of the milling processes. On the basis of these milling reactions, a stability order (least to most stable) was derived: tp/bs < tp/ba < tp/ina < bs/ina. KW - Mechanochemistry KW - Cocrystal KW - Milling PY - 2016 DO - https://doi.org/10.1021/acs.cgd.6b00928 SN - 1528-7483 SN - 1528-7505 VL - 16 IS - 10 SP - 5843 EP - 5851 AN - OPUS4-38097 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Franziska A1 - Greiser, Sebastian A1 - Peifer, Dietmar A1 - Jäger, Christian A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Mechanochemically Induced Conversion of Crystalline Benzamide Polymorphs by Seeding N2 - Benzamide has been known for its polymorphism for almost 200 years.Three polymorphic forms are described. To date,itwas only possible to crystallizeametastable form in amixture together with the thermodynamically most stable form I. Acomplete transformation of form Iinto the metastable form III by mechanochemical treatment has been achieved. Catalytic amounts of nicotinamide seeds were used to activate the conversion by mechanochemical seeding. NMR experiments indicated that the nicotinamide molecules were incorporated statistically in the crystal lattice of benzamide form III during the conversion. The transformation pathway was evaluated using in situ powder X-ray diffraction. KW - Nicotinamide KW - Benzamide KW - In situ reactions KW - Mechanochemistry KW - Polymorphs PY - 2016 DO - https://doi.org/10.1002/anie.201607358 VL - 128 IS - 46 SP - 14493 EP - 14497 PB - WILEY-VCH CY - Weinheim AN - OPUS4-38472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Herrmann, Antje Jutta T1 - Simple and fast metal staining procedures for identification and characterization of single cells via laser ablation ICP-MS N2 - Biological systems exhibit a very high complexity, because they consist of various cell populations showing heterogenic characteristics. Therefore the individual analysis of single cells is important to understand cellular processes as well as their function in a cell system. Especially investigation in the question about what is biological variability and what is a substantial difference between two cells of the same type (which might lead to dysfunction or disease) is of high interest. Today improved spatial and temporal resolution enable the use of laser ablation inductively coupled mass spectrometry (LA-ICP-MS) for element microscopy of single cells. Next to the characterization of natural trace elements the introduction of artificial metal labels into cells is of high interest. Element labeling of cell compartments and/or proteins allows its simultaneous analysis and localization within a cell via element microscopy. Two fast and simple metal staining procedures of adherent cells for identification of single cells via LA-ICP-MS at sub micrometer resolution are presented. Two labeling reagents were selected which were already described in literature for applications around protein and cell analysis. An Iridium-intercalator is utilized to stain the cell nuclei whereas the whole cell is stained by maleimido-mono-amide-DOTA-complexes (mDOTA) loaded with lanthanide(III) isotope ions. The metal staining procedures allow the visualization of single cells by element microscopy independent of a superposition of analyte’s 2D element intensity profile with a prior taken bright field image of the sample. The applicability was shown on an actual question in nano-toxicology (the cellular uptake of nanoparticles). T2 - 25. ICP-MS Anwendertreffen CY - Siegen, Germany DA - 12.09.2016 KW - Metal staining procedures KW - Single cell analysis KW - Bioimaging PY - 2016 AN - OPUS4-37979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Comparison of the separation performance of a conventional and a miniaturized AF4 channel N2 - A miniaturized AF4 channel was introduced for the rapid analysis of different nanoparticle samples. UV-Vis-MALS provides the possibility to measure the particle size and molar mass and offers a powerful tool for the investigation of separation performances of different AF4 channels. T2 - BfR Retreat 2016 CY - Berlin, Germany DA - 23.09.2016 KW - Field-flow fractionation KW - Miniaturized AF4 channel PY - 2016 AN - OPUS4-38255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Michalik-Onichimowska, Aleksandra A1 - Riedel, Jens A1 - Panne, Ulrich A1 - King, Rudibert A1 - Maiwald, Michael ED - Maiwald, Michael T1 - “Click” analytics for “click” chemistry – a simple method for calibration-free evaluation of online NMR spectra N2 - Currently research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual cam-paigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The re-sulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via compara-bly straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algo-rithm to interpret the ob-tained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16 inch polymer tubing working as a flow cell. Single scan 1H spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. T2 - 12. Kolloquium des Arbeitskreises Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - “Click” chemistry KW - Online NMR KW - Online monitoring PY - 2016 SP - 72 EP - 74 AN - OPUS4-38385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Phukphatthanachai, Pranee A1 - Panne, Ulrich A1 - Jakubowski, Norbert A1 - Vogl, Jochen T1 - SI-traceable quantification of sulphur in copper metal and its alloys by ICP-IDMS N2 - Previously applied methods for the quantification of sulphur in copper and other pure metals revealed a lack of SI-traceability and additionally showed inconsistent results, when different methods were compared. Therefore, a reference procedure is required which allows SI-traceable values accompanied by a Sound uncertainty budget. In this study a procedure was developed for the quantification of total sulphur in copper at low concentration levels using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS). The major part of the copper matrix was separated by adding ammonia which forms a complex with the copper while releasing the sulphur followed by chromatographic separation using a weak cation resin. After that the sulphur fraction was further purified by chromatographic means using first an anion exchange method and second a chelating resin. The developed procedure shows high performance, especially concerning high efficiency in matrix removal (>99.999%) while keeping the recovery of sulphur above 80%. Procedure blanks are in the order of 3–53 ng resulting in LOD and LOQ values of 0.2 mg g1 and 0.54 mg g1, respectively. The procedure is sufficient to facilitate value assignment of the total sulphur mass fraction in reference materials. Additionally, relative measurement uncertainties were calculated to be below 1% and the measurement results were traceable to the SI. The procedure reported in this study is a new reference procedure for sulphur measurement in copper, being fit for two major purposes, certification of reference materials and assignment of reference values for inter-laboratory comparison. KW - Traceability KW - Measuremment uncertainty KW - Isotope dilution mass spectrometry KW - Reference measurements PY - 2018 DO - https://doi.org/10.1039/c7ja00338b SN - 0267-9477 SN - 1364-5544 VL - 33 IS - 1 SP - 90 EP - 101 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-43614 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - García-Fernández, J. A1 - Bettmer, J. A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Añón, E. A1 - Montes-Bayón, M. A1 - Sanz-Medel, A. T1 - The fate of iron nanoparticles used for treatment of iron deficiency in blood using mass-spectrometry based strategies N2 - The release of iron from iron nanoparticles (NPs) used as parenteral formulations appears to be influenced by the size and surface properties of the colloidal iron complex and the matrix. A clinically applied product Venofer® has been used as a model formulation to establish adequate analytical strategies to evaluate the fate of iron nanoparticles (NPs) in blood. First, the preparation was characterized by high resolution transmission electron microscopy (HRTEM), dynamic light scattering (DLS) and UV-vis absorption spectroscopy. This revealed the presence of monodisperse iron NPs with a hydrodynamic diameter of ∼15 nm and an iron core of ∼4 nm. Venofer® was then incubated with serum and whole blood in a quantitative study on the iron bioavailability from these NPs. Iron was speciated and quantified by using inductively coupled plasma mass spectrometry (ICP-MS). Iron solubilization levels of up to 42% were found in both fluids using isotope dilution of iron for quantification within the first hour of incubation even in the absence of the reticuloendothelial system. The monitoring of the iron-containing proteins present in serum was conducted by highperformance liquid chromatography with ICP-MS detection. It indicated that the dissolved iron ions are bound to transferrin. Quantitative speciation studies using isotope pattern deconvolution experiments concluded that the released iron saturated almost completely (up to 90%) the metal binding sites of transferrin. The remaining iron appeared also associated to albumin and, to a lesser extent, forming smaller sized particles. Thus, the methods presented here provide new insights into the fate of Venofer® nanoparticles and may be applied to other formulations. KW - Iron-sucrose nanoparticles KW - Serum KW - Bioavailability KW - Speciation KW - HPLC KW - ICP-MS PY - 2017 DO - https://doi.org/10.1007/s00604-017-2388-8 SN - 0026-3672 SN - 1436-5073 VL - 184 IS - 10 SP - 3673 EP - 3680 AN - OPUS4-43128 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bierstedt, Andreas A1 - Panne, Ulrich A1 - Riedel, Jens T1 - Confinement and enhancement of an airborne atmospheric laser-induced plasma using an ultrasonic acoustic resonator N2 - Optical elemental analysis in the gas phase typically relies on electrically driven plasmas. As an alternative approach, laser-induced plasmas (LIPs) have been suggested but have so far been only scarcely used. Here, a novel signal enhancement strategy for laser-based airborne plasma optical Emission spectroscopy for gas phase analytics is presented. In contrast to an electrically driven plasma, in the laser-induced analogue dynamic matter transport equilibrium builds up. The latter results in a rarefied density regime in the plasma core itself, surrounded by an area of compressed matter. The central rarefaction leads to a decrease in plasma intensity and analyte number density, both of which are detrimental for analytical purposes. Since the repetitive ignition of LIPs is a transient process, a restoration of the former gaseous medium by other dynamically equilibrated diffusion processes would be favourable. The presented combination of an airborne LIP and an ultrasonic acoustic resonator yields a fourfold signal enhancement while the Background contribution of ubiquitous air is at the same time effectively suppressed. Since the entire enhancement effect occurs without contact, no additional sources for abrasive sample contamination are introduced. KW - DPSS laser KW - Laser-induced plasma KW - High repetition rate KW - Ultrasonic acoustic resonator KW - Optical emission spectroscopy PY - 2018 DO - https://doi.org/10.1039/C7JA00297A SN - 0267-9477 SN - 1364-5544 VL - 33 IS - 1 SP - 135 EP - 140 PB - Royal Society of Chemistry CY - London AN - OPUS4-43619 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Priebe, Nsesheye Susan T1 - Evaluation of brick clays from various deposits in central Germany for use as SCMs N2 - The development of low carbon cements has gained great importance over the last decades. In the effort to limit the carbon content related to its production, cement is often replaced with supplementary cementitious materials (SCMs). Commonly used SCMs such as fly ash and slag have undergone extensive research, but are currently limited in supply and availability. Among the researched SCMs, calcined clays have proven to be a suitable alternative pozzolan due to their worldwide availability and extremely low calcination temperatures when compared to clinker. This poster presents the results from an ongoing project, aimed at obtaining pozzolans, available in sufficient quantities for Portland-pozzolana cement production in Germany. The poster shows the analyses of seven brick clays from various deposits in central Germany. The chemical and mineral composition of the brick clays was evaluated through inductively coupled plasma – optical emission spectroscopy (ICP-OES), X-ray diffraction (XRD), and thermogravimetric analysis (TG/DTG). The particle size distribution (PSD) was also evaluated by laser granulometry. The results show that the brick clays contain a substantial amount of kaolinite, illite and smectite minerals, the relative proportions differing significantly between deposits. The suitable calcination temperature range of the clays is also evaluated through TG/DTG analysis to obtain the optimum degree of dehydroxylation from which the bricks clays can be suitable for use as a pozzolan. T2 - 2nd International Conference on Calcined Clays for Sustainable Concrete CY - Havana City, Cuba DA - 04.12.2017 KW - Cement KW - CO2 reduction KW - Supplementary cementitious materials KW - Calcined clay KW - Kaolinite KW - Illite KW - Smectite PY - 2017 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. AN - OPUS4-43719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mundra, Shishir A1 - Samson, G. A1 - Masi, G. A1 - Achenbach, R. A1 - Bastidas, D. M. A1 - Bernal, S. A. A1 - Bignozzi, M. C. A1 - Criado, M. A1 - Cyr, M. A1 - Gartner, N. A1 - von Greve-Dierfeld, S. A1 - Legat, A. A1 - Nikoonasab, Ali A1 - Provis, J. L. A1 - Raupach, M. A1 - Gluth, Gregor T1 - Stahlkorrosion in alkalisch aktivierten Bindemitteln und Betonen: Anwendung elektrochemischer Methoden N2 - Alkalisch aktivierte Bindemittel (AAB) und Betone können herkömmliche Zemente beziehungsweise Betone potentiell in vielen Anwendungen ersetzen und dadurch den CO2-Fußabdruck der Bauindustrie wesentlich verkleinern. Zur Untersuchung der Stahlkorrosion in bewehrten („armierten“) Betonbauteilen werden elektrochemische Methoden wie Messungen des Freien Korrosionspotentials, des Polarisationswiderstands oder von Stromdichte-Potential-Kurven eingesetzt. Diese Methoden und die etablierten Grenzwerte zur Detektion von Korrosion sind für die Anwendung bei herkömmlichen Zementen beziehungsweise Betonen entwickelt und erprobt worden. Neue Forschungsergebnisse demonstrieren, dass Unterschiede zwischen den Porenlösungszusammensetzungen von herkömmlichen Zementen und bestimmten AAB sowie anderen schlackehaltigen Zementen erhebliche Unterschiede bei den Ergebnissen der elektrochemischen Messungen bewirken und damit zur fehlerhaften Detektion von Stahlkorrosion führen können. Ursache hierfür sind vor allem reduzierte Schwefelspezies in den Porenlösungen von AAB und anderen schlackehaltigen Zementen. KW - Zement KW - Hüttensandmehl KW - Schlacke KW - Sulfid KW - Korrosion PY - 2023 UR - https://bit.ly/GIT-Gluth UR - https://analyticalscience.wiley.com/content/magazine-do/git-labor-fachzeitschrift-10-2023 SN - 0016-3538 VL - 67 IS - 10 SP - 28 EP - 31 PB - Wiley-VCH AN - OPUS4-58573 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ascher, Lena T1 - Imaging of Eu doped very small iron oxide nanoparticle in atherosclerotic plaques via LA-ICP-MS N2 - Atherosclerotic lesions can be visualized by magnetic resonance imaging (MRI) using very small iron oxide nanoparticles (VSOP). VSOP accumulate in atherosclerotic plaques and thus serve as an atherosclerosis probe. The aim of this project was to image the distribution of europium doped VSOP (Eu-VSOP) by laser ablation ICP-MS in histological thin cuts of the aortic root region of ApoE knockout mouse model that is rich in atherosclerotic plaques. In addition, it was investigated whether VSOP accumulation in the plaques correlates with other biomarkers of inflammation for example macrophages and altered endothelium to assess whether it correlates with instability or vulnerability of the plaque regions. For this purpose, antibodies were labeled with various lanthanide elements and correlated with the Eu-VSOP distribution using LA-ICP-MS in a multiplex measurement mode. A possible correlation of reactive nitrogen species (RNS) with endogenous iron or Eu-VSOP can also be detected by LA-ICP-MS. For this purpose, RNS-specific antibodies were also labeled with lanthanides. T2 - 26. ICPMS-Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - Bioimaging KW - LA-ICP-MS KW - Immunoassay KW - Nanoparticle KW - Labeling PY - 2018 AN - OPUS4-45920 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nietzold, Carolin A1 - Dietrich, Paul A1 - Holzweber, M. A1 - Lippitz, Andreas A1 - Kamalakumar, A. A1 - Blanchard, V. A1 - Ivanov-Pankov, S. A1 - Weigel, W. A1 - Panne, Ulrich A1 - Unger, Wolfgang T1 - Surface chemical characterization of model glycan surfaces and shelf life studies of glycan microarrays using XPS, NEXAFS spectroscopy, ToF-SIMS and fluorescence scanning N2 - Biomedical applications, including functional biomaterials, carbohydrate-arrays, and glycan-based biosensors. The chemistry of glycan immobilization plays an essential role in the bioavailability and function of surface bound carbohydrate moieties. For biomedical applications the stability over time (shelf life) of glycan arrays is a crucial factor. Herein we report on approaches for surface and interface characterization relevant to the needs of production of glycan microarrays which were tested using model carbohydrate surfaces. For detailed characterization of glycan model surfaces we used a combination of X-ray photoelectron spectroscopy (XPS), near edge X-ray absorption fine structure spectroscopy (NEXAFS) and ToF SIMS which are complementary techniques of surface chemical analysis. Links to fluorescence spectroscopy often used for characterization in the microarray community were established as well. In detail, amine-reactive silicon oxide and glass surfaces were used for anchoring oligosaccharides with an amino linker. The amount of surface bound carbohydrates was estimated by X-ray photoelectron spectroscopy (XPS). Glycan immobilization was investigated using lectins, which are glycan-binding molecules. A shelf life study of model glycan microarrays on epoxy-coated glass surfaces was done over a period of 160 days under different storage conditions utilizing fluorescence, ToF-SIMS and XPS analysis. It was shown that glycan activity of the models used can be maintained at least for half a year of storage at 4 °C. KW - Glycan microarray KW - XPS KW - NEXAFS KW - ToF-SIMS KW - Fluorescence PY - 2018 UR - https://www.sciencedirect.com/science/article/pii/S0169433218320300?via%3Dihub DO - https://doi.org/10.1016/j.apsusc.2018.07.133 SN - 0169-4332 SN - 1873-5584 VL - 459 SP - 860 EP - 873 PB - Elsevier B.V. AN - OPUS4-46212 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Hüllmann, Dino A1 - Krentel, Daniel A1 - Kluge, Martin A1 - Kohlhoff, Harald A1 - Lilienthal, A. J. T1 - Gas Tomography Up In The Air! N2 - In this paper, we present an autonomous aerial robot to reconstruct tomographic 2D slices of gas plumes in outdoor environments. Our platform, the so-called Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS) combines a lightweight Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile octocopter. The TDLAS sensor provides integral gas concentration measurements but no information regarding the distance traveled by the laser diode's beam or the distribution of the gas along the optical path. We complemented the set-up with a laser rangefinder and apply principles of Computed Tomography (CT) to create a model of the spatial gas distribution from these integral concentration measurements. To allow for a rudimentary ground truth evaluation of the applied gas tomography algorithm, we set up a unique outdoor test environment based on two 3D ultrasonic anemometers and a distributed array of 10 infrared gas transmitters. We present first results showing the 2D plume reconstruction capabilities of the system under realistic conditions. T2 - IEEE Sensors 2018 CY - New Delhi, India DA - 28.10.2018 KW - Aerial robot KW - TDLAS KW - Gas tomography KW - Plume PY - 2018 SN - 978-1-5386-4707-3 SP - 396 EP - 398 PB - IEEE AN - OPUS4-46477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - 2D and 3D imaging characterization techniques for porous ceramics N2 - The combination of microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on porous material properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of porosity in ceramics. Moreover, I will show how not-so-novel 2D characterization techniques, based X-ray refraction, can allow a great deal of insights in the damage evolution in microcracked (and porous) ceramics. I will show how X-ray refraction can detect objects (e.g. microcracks) below its own spatial resolution. Finally, I will discuss the link between the microstructural findings and the mechanical properties of porous microcracked ceramics. T2 - Colloques de l"universite' de Limoges, France CY - Limoges, France DA - 17.10.2018 KW - Tomography KW - X-ray refraction KW - Porous ceramics KW - Microcracking PY - 2018 AN - OPUS4-46350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Enhanced characterization of pore systems by simultaneous use of SIP, µ-CT and NMR N2 - Other than commonly assumed the relaxation times observed in the electrical low-frequency range (1 mHz – 40 kHz) of natural porous media like sandstones and tuff stones cannot be directly related to the dominant (modal) pore throat sizes, measured (e.g.) with mercury intrusion porosimetry (MIP). Working with a great variety of sandstones from very different origins and featuring great variations in textural and chemical compositions as well as in geometrical pore space properties, we observed that particularly samples with narrow pore throats were characterized by long (low-frequency) relaxations. These, however, can (following the current theories) be rather explained by long “characteristic length scales” in these media or low diffusion coefficients along the electrical double layer. However, there is no straightforward way (or single approved method) of getting reliable numbers for properties such as the lengths of pore throats, the diameter and length of the wide pores and their respective distributions. Consequently we follow a multi-methodical approach and combine the benefits of MIP, micro-computed tomography (µ-CT) and nuclear magnetic resonance (NMR) to achieve much deeper insight due to the different resolutions and sensitivities to either pore constrictions (throats) or wide pores. This helps us to understand, whether the observed electrical relaxation phenomena actually depend on geometric length scales or rather on other properties such as chemical composition, clay content, clay type or cation exchange capacity. Our poster showcases selected results of a systematic study on texturally and petrophysically very different sandstones. T2 - 5th Int. Workshop on Induced Polarization CY - Rutgers, The State University of New Jersey, Newark, NJ, USA DA - 03.10.2018 KW - µ-CT KW - Pore size distribution KW - Spectral induced polarzation KW - NMR PY - 2018 AN - OPUS4-46335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abram, Sarah-Luise T1 - Iron oxide nanoparticles as a reference material candidate for particle size measurements N2 - This poster presentation covers the development of iron oxide nanoparticles as reference material candidate in the context of the project "Nanoplattform". T2 - EMRS Spring Meeting CY - Online meeting DA - 31.05.2021 KW - Iron oxide nanoparticles KW - Reference material KW - Particle size KW - Transmission electron microscopy KW - Small angle x-ray scattering PY - 2021 AN - OPUS4-52773 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon T1 - A complementary spectroscopic approach for the non invasive in situ identification of synthetic organic pigments in modern reverse paintings on glass N2 - This work addresses the identification of synthetic organic pigments (SOP) in ten modern reverse paintings on glass (1912-1946) by means of an in-situ multi-analytical approach. The combination of the complimentary properties of mobile Raman spectroscopy and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) enabled the detection of sixteen SOP even in complex mixtures with inorganic compounds and binders. For the β-naphthol pigments, both Raman and DRIFTS yield appropriate results. DRIFTS was the preferred method for the detection of synthetic alizarin (PR83). Its diagnostic band pattern even allows its detection in complex mixtures with mineral pigments, binders and fillers. Raman spectroscopy yielded distinctive spectra for the triaryl carbonium pigments (PG1, PV2, PR81) and the two-yellow azo SOP (PY3, PY12), whereas DRIFT spectra were affected by extensive band overlapping. This may also occur in Raman spectra, but in less problematic amounts. Fluorescence is the major problem with Raman and it significantly hampers the SOP spectra even with the 785 nm laser. On the one hand the big spot size of DRIFTS (10 mm) limits the technique to rather large sampling areas, whereas the use of a 50× objective for in-situ Raman measurements permits a focus on small spots and aggregated SOP flakes. Moreover, “environmental” factors like temperature changes, artificial light, limited space and vibrations when people pass by need to be considered for in-situ measurements in museums. Finally, the results show the experimental use of SOP in modern reverse glass paintings. Among several rare SOP (e.g. PB52, PR81), two of them (PG1, PV2) have never been reported before in any artwork. T2 - Technart2019 CY - Bruges, Belgium DA - 07.05.2019 KW - Synthetic organic pigments KW - Reverse glass painting KW - DRIFTS KW - Raman spectroscopy PY - 2019 AN - OPUS4-48009 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Wolfram A1 - Mota, Berta A1 - Ramirez Caro, Alejandra T1 - The action of aggregates on concrete rheology N2 - Most factors acting on concrete rheology work at an extremely small-scale level. Influencing factors in the millimetre or centimetre area are essentially restricted to sand and aggregates. The latter, however, make up 50 to 70% of the total volume of most concretes – a fact often ignored in research on controlling concrete processing properties. Whereas suitably chosen concrete admixtures and additives can influence rheology in a very targeted manner, sand and aggregates are less suitable for controlling rheology but nonetheless contribute to the rheology of the Overall system. The actions of sand and aggregate can impose themselves upon the actions of admixtures and additives and, in unfavourable circumstances, even render them redundant. For this reason, any results concerning the processability of binding agent systems can only be transferred to concrete with great care. It is important to better understand the action of sand and aggregates in order to be able to harmonise them in such a way that they complement the action of superplasticisers positively, instead of working against them. Savings on costs can also be made by this targeted fine-tuning. KW - Rheology KW - Aggregates KW - Viscosity KW - Yield stress KW - Concrete PY - 2018 VL - 3 SP - 42 EP - 49 PB - ad-media GmbH CY - Cologne AN - OPUS4-47045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gawek, Marcel A1 - Madkour, Sherif A1 - Szymoniak, Paulina A1 - Radnik, Jörg A1 - Schönhals, Andreas T1 - Energy Dependent XPS Measurements on Thin Films of a Poly(vinyl methyl ether)/Polystyrene Blend in Dependence on Film Thickness – Concentration Profile on a Nanometer Resolution to Understand the Behavior of Nanofilms N2 - The composition of the surface layer in dependence from the distance of the polymer/air interface in thin films with thicknesses below 100 nm of miscible polymer blends in a spatial region of a few nanometers is not investigated completely. Here, thin films of the blend poly vinyl methyl ether) (PVME)/polystyrene (PS) with a composition of 25/75 wt% are investigated by Energy Resolved X-ray Photoelectron Spectroscopy (ER-XPS) at a synchrotron storage ring using excitation energies lower than 1 keV. By changing the energy of the photons the information depth is varied in the range from ca. 1 nm to 10 nm. Therefore, the PVME concentration could be estimated in dependence from the distance of the polymer/air interface for film thicknesses below 100 nm. Firstly, as expected for increasing information depth the PVME concentration decreases. Secondly, it was found that the PVME concentration at the surface has a complicated dependence on the film thickness. It increases with decreasing film thickness until 30 nm where a maximum is reached. For smaller film thicknesses the PVME concentration decreases. A simplified layer model is used to calculate the effective PVME concentration in the different spatial regions of the surface layer. KW - Energy dependent XPS KW - Soft X-ray KW - Thin films PY - 2021 DO - https://doi.org/10.1039/d1sm00656h VL - 17 IS - 29 SP - 6985 EP - 6994 PB - The Royal Chemical Society AN - OPUS4-53039 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nehring, Grzegorz A1 - Bonnerot, Olivier A1 - Gerhardt, M. A1 - Krutzsch, M. A1 - Rabin, Ira T1 - Looking for the missing link in the evolution of black inks N2 - In the transition from carbon to iron-gall inks, the two documents from the Egyptian Museum and Papyrus Collection in Berlin with shelfmarks P 13500 and P 13501 discussed in this work present an important case. Their inks appear brownish, although they date back to the fourth and third century BCE, when carbon inks are believed to have been commonly if not exclusively used. Using imaging micro-X-ray fluorescence and infrared reflectography, we discovered that the inks in both documents contain a significant amount of copper in addition to carbon. Comparing the extant recipes for black writing inks and the experimental evidence, we suggest that these inks are a transition between the pure carbon and the iron-gall inks. Such inks may have been quite common before the production of iron-gall ink was clearly understood and established. KW - Black writing ink KW - Hellenistic KW - Papyrus KW - XRF imaging KW - NIR imaging PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-523708 DO - https://doi.org/10.1007/s12520-021-01320-5 VL - 13 IS - 4 SP - Article 71 PB - Springer AN - OPUS4-52370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steinborn, Gabriele A1 - Gemeinert, Marion A1 - Schmidt, Wolfram T1 - Vergleich verschiedener Messverfahren zur Partikelgrößenanalyse am Beispiel von nanodispersem ZrO2-Pulver N2 - Fünf verschiedene Messverfahren wurden zur Partikelgrößenanalyse von nanodispersen ZrO₂-Pulver verglichen. Mit der Laserstreulichtanalyse, der dynamischen Lichtstreuung (heterodyne DLS und homodyne DLS-PCS), der Sedimentationsanalyse im Zentrifugalfeld und der Ultraschallspektrometrie wurden wässrige ZrO₂-Suspensionen mit verschiedenen Feststoffkonzentrationen hinsichtlich ihrer Partikelgrößenverteilung analysiert. Als Referenz diente die REM-Analyse zur Ermittlung der Primärpartikelgröße (ca. 40 nm). Mit den hier vorgestellten Messverfahren konnten in den entsprechenden Suspensionen nur Sekundärpartikel im Bereich von 105 nm bis 224 nm detektiert werden, die somit auf das Vorhandensein von Aggregaten bzw. harten Agglomeraten hinweisen. T2 - Tagung, Produktgestaltung in der Partikeltechnologie CY - Berlin, Germany DA - 23.04.2015 KW - Agglomeration KW - Nanopulver KW - Partikelgröße KW - Suspension PY - 2016 DO - https://doi.org/10.1002/cite.201500164 SN - 0009-286 X VL - 88 IS - 7 SP - 984 EP - 994 PB - WILEY-VCH CY - Weinheim AN - OPUS4-36960 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rabin, Ira ED - Raggetti, L. T1 - Material Studies of Historic Inks: Transition from Carbon to Iron-Gall Inks N2 - This chapter offers observations and considerations concerning black writing inks encountered in writing supports transmitting documentary and literary texts of the late Antiquity and early Middle Ages. It discusses different types of inks, the Methods of their detection and their use in different times and geographical areas. KW - Material analysis KW - Writing inks KW - Ink fingerprint PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528057 DO - https://doi.org/10.1163/9789004444805_006 SP - 70 EP - 78 PB - Brill CY - Leiden AN - OPUS4-52805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Rabin, Ira A1 - Hahn, Oliver ED - Michel, C. ED - Friedrich, M. T1 - Detection of Fakes: The Merits and Limits of Non-Invasive Materials Analysis N2 - This paper addresses the sensitive issue of authenticating unprovenanced manuscripts of high monetary value to certify they are genuine. Over the last decade, the popularity of material studies of manuscripts using non-destructive testing (NDT) has increased enormously. These studies are held in especially high esteem in the case of suspicious writings due to the methodological rigour they are reputed to contribute to debate. We would like to stress that materials analysis alone cannot prove that an object is genuine. Unfortunately, audiences with a humanities background often tend to disregard the technical details and treat any published interpretation of instrumental analysis as an objective finding. Four examples are outlined here to illustrate what questionable contributions the natural sciences can make in describing manuscripts that have actually been forged. KW - Fakes KW - Non-invasive analysis KW - Limitations PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517202 SN - 978-3-11-071422-7 DO - https://doi.org/10.1515/9783110714333 SN - 2365-9696 VL - 20 SP - 281 EP - 290 PB - Walter de Gruyter GmbH CY - Berlin/Boston AN - OPUS4-51720 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - The contribution of material analysis to the identification of forged writing materials N2 - This paper addresses the role of material analysis in the current discussion on the authenticity of unprovenanced fragments. It will show that material analysis alone, especially its non-destructive variety, cannot prove that the object is genuine. The best material analysis can do, after all appropriate tests have been conducted, is to announce that nothing has been found that contradicts the assumption of genuineness. Moreover, the results of the material analysis can never be used as the only justification of authentication in cases of composite objects such as manuscripts or epigraphs. The most effective approach for testing suspicious artifacts has been established by forensic science. Not limited to non-invasive analysis, this approach relies on validated techniques that usually require the extraction of samples and comparison with reference materials and are capable of delivering unambiguous results. In contrast, the analysis of suspicious manuscripts has to overcome additional obstacles such as the heterogeneity of historical material, the scarcity of suitable reference standards, and restriction to strictly non-invasive techniques. We discuss the reliability of the testing protocol based on the non-destructive multi-instrumental approach developed by the BAM for the investigation of writing materials. In the case of the DSS, it relies on comparison with the genuine DSS fragments studied over the last 10 years. T2 - SBL Interenational 2017 CY - Berlin, Germany DA - 07.08.2017 KW - Cultural assets KW - Forgery PY - 2017 AN - OPUS4-43481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Hahn, Oliver ED - Breiding, Sonja ED - Doil, Thorsten T1 - Materialität - Das Objektverständnis der vielfältigen Disziplinen im Bereich von Kunst- und Kulturgut N2 - Naturwissenschaftliche Verfahren gewinnen zunehmend an Bedeutung bei der Untersuchung von Kunst- und Kulturgut und bei der Entwicklung von Konservierungskonzepten zum Erhalt des kulturellen Erbes. Neben bildgebenden Verfahren wie beispielsweise der Computertomographie oder der Radiographie sind materialanalytische Verfahren von großer Wichtigkeit. Durch die Miniaturisierung elektronischer Bauteile kommen immer mehr mobile Untersuchungstechniken auf den Markt, so dass die Objekte vor Ort im musealen Kontext untersucht werden können. Zudem erfüllen viele Verfahren die Bedingung der zerstörungsfreien Analyse, so dass Untersuchungen ohne Probenentnahmen durchgeführt werden können. Im Jahre 2006 wurde das Netzwerk zur interdisziplinären Kulturguterhaltung in Deutschland (N.i.Ke.) gegründet. Dieses Netzwerk soll den Austausch zwischen Natur- und Geisteswissenschaften fördern und versteht sich daher als Kommunikations- und Kooperationsplattform der Disziplinen Archäologie und Kunstgeschichte, Restaurierung und Konservierung sowie Natur- und Ingenieurswissenschaften. In loser Abfolge veranstaltet N.i.Ke. seit 2006 Workshops zu aktuellen Themen aus dem Bereich der Kunst- und Kulturgutanalyse. Durch eine intensive fachübergreifende Zusammenarbeit der verschiedenen Disziplinen werden hier neue naturwissenschaftliche Untersuchungsmethoden für restauratorisch-konservatorische oder kulturhistorische und archäologische Fragestellungen etabliert oder bestehende Verfahren weiterentwickelt. Hier kann das Netzwerk wesentliche Beiträge zum Erhalt unseres kulturellen Erbes leisten. Was zunächst als kleine Zusammenkunft begonnen hat, entwickelte sich im Laufe der letzten 10 Jahre zu einer Veranstaltung, welche sich immer größerer Beliebtheit erfreute, gerade weil grundsätzlich unterschiedliche Themen aus dem Bereich der präventiven Konservierung, der Restaurierung oder Archäometrie in den Fokus gestellt wurden und werden. Der erste vorliegende Band widmet sich dem Thema „Materialität“ und enthält Beiträge, die auf dem letzten Workshop „Der Exzellenzcluster Bild Wissen Gestaltung. Ein interdisziplinäres Labor zu Gast in der Bundesanstalt der Bundesanstalt für Materialforschung und –prüfung (BAM)“ präsentiert wurden. T2 - 8. N.i.Ke.-Workshop: Materialität - Das Objektverständnis der vielfältigen Disziplinen im Bereich von Kunst- und Kulturgut CY - Berlin, Germany DA - 26.11.2015 KW - Netzwerk zur interdisziplinären Kulturguterhaltung PY - 2017 SN - 2567-1251 VL - 1 SP - 1 EP - 121 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-43477 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Priebe, Nsesheye Susan A1 - Schmidt, Wolfram A1 - Mota, Berta A1 - Leinitz, Sarah A1 - Kühne, Hans-Carsten A1 - Rogge, Andreas T1 - The effect of superplasticizers on rheology and early hydration kinetics of rice husk ash-blended cementitious systems N2 - Superplasticizers (SPs) have been employed in concrete technology for decades to improve the workability of concrete in its fresh state. The addition of SPs in cement-based systems affects the early properties. Although the interaction of the cement particles with various SPs has been extensively researched, there still exists limited research on the interaction of SPs with supplementary cementitious materials such as rice husk ash (RHA). This paper investigates the rheological properties and early hydration kinetics of RHA-blended systems with three types of SPs, a polycarboxylate ether (PCE) and two lignosulphonates (LS-acc and LS-ret). In rheological properties, the addition of SP causes an initial improvement of workability as the yield stress is significantly reduced. The pastes with PCE and LS-acc show a slight increase of yield stress over time whereas pastes with LS-ret tend to lower the yield stress slightly over time, further improving the workability. Without SP, pastes with RHA show a lower yield stress but an increase in plastic viscosity as cement is further replaced with RHA. The addition of the LS SPs is observed to lower the plastic viscosity but remains constant with further replacement of cement with RHA. This indicates that LS SPs further adsorbs on RHA particles and hydration products produced causing dispersion of the particles within the system. In early hydration kinetics, pastes with PCE retard hydration and the degree of retardation is further increased with LS SPs. In the presence of RHA, the retardation of LS SP systems is significantly reduced. The pastes with PCE show more ettringite in the SEM micrographs, but is observed to be shorter needles. This indicates an initial good workability for PCE. However, C-S-H and CH were observed to be low in quantity, whereby the pastes with LS show more nucleation sites for C-S-H and CH. The ettringite needles in the LS systems were similar in quantity and more elongated in some cases but not abundant as in the PCE systems. KW - Plastic viscosity KW - Cement KW - CO2 reduction KW - Supplementary cementitious materials KW - Rice husk ash KW - Superplasticizers KW - Hydration KW - Rheology KW - Yield stress KW - Slump flow PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0950061817310978?via%3Dihub DO - https://doi.org/10.1016/j.conbuildmat.2017.05.197 SN - 0950-0618 SN - 1879-0526 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. VL - 150 SP - 511 EP - 519 PB - Elsevier Ltd. AN - OPUS4-41036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Priebe, Nsesheye Susan A1 - Schmidt, Wolfram A1 - Rogge, Andreas A1 - Kühne, Hans-Carsten T1 - Performance of rice husk ash as an alternative binder in a modified cementitious system with added superplasticizers N2 - Rice husk as (RHA) is an eco-friendly material, which can be used as a supplementary cementitious material (SCM) in cement and concrete. Due to the high water demand for the material, superplasticizers (SPs) are essential to improve the performance. However, the interaction between the SPs and RHA systems is limited. This paper investigates the interaction of the binders with three SPs, i.e. two polycarboxylate ethers (PCEs) and one lignosulphonate (LS). The investigations are performed on blended systems of mortar containing various percentages of RHA and limestone powder (LSP). LSP is used in this research to improve the workability of the mortar. The results from the zeta potential (ZP) shows that the SPs are extremely dependent on the pH of the suspension. At higher pH values such as in a cementitious system, the ZP becomes less negative indicating that the ions in the suspension interact with the carboxyl groups in the backbone of the polymers thus reducing the surface charges of the SP. The mini-slump flow shows that the workability of the blended mortar systems is significantly improved with the addition of SPs. LS systems with increasing RHA is observed to have similar workability as the control mix over time. The compressive strength test results show increased strength for all mortar specimens with added RHA and LSP at later ages. KW - Compressive strength KW - Rice husk ash KW - Superplasticizers KW - Zeta potential KW - Workability PY - 2017 DO - https://doi.org/10.1016/j.cemconcomp.2017.07.014 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. VL - 83 SP - 202 EP - 208 PB - Elsevier Ltd. AN - OPUS4-42602 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon T1 - Non-invasive, spectroscopic study of a modern reverse glass painting N2 - We present the first spectroscopic study on a reverse glass painting form the classic modern period (1905-1955). Marianne Uhlenhuth’s painting “Ohne Titel, 1954” shows characteristics like experimental use of colorants and abstract compositions, which are well-established in classic modern art. Compared to stained glass, reverse glass paintings are viewed in reflected light, hence they reveal strong and intense colors. New inorganic pigments, development of synthetic organic pigments and the simultaneous supersession of well-known ancient colorants result in experimental works and remarkable pigment mixtures in this period of time. An in-situ, non-invasive approach was used to study the pigments and binding media. In-situ measurements were carried out using Raman spectroscopy (i-Raman®Plus, Bwtek Inc., 785 nm, 20× objective, resolution 4 cm-1), X-ray fluorescence (Tracer III-SD, Bruker AXS Microanalysis GmbH, 40 kV, 15 μA), VIS spectroscopy (SPM 100, Gretag-Imaging AG) and DRIFTS: Diffuse Reflection-Infrared-Fourier-Transform Spectroscopy (ExoScan, Agilent GmbH, 4000-650 cm-1, 256 scans, resolution 4cm-1). The pigments consist of inorganic as well as organic materials. Phthalocyanin green (PG7, colour index No. 74260), viridian and emerald green were used for the green areas. The yellow parts consist of chrome yellow and cadmium yellow. Pigment Yellow 1 (C.I. 11680) was used for the dark yellow/orange part. Red areas were characterized by the presence of cadmium and selenium (cadmium red) in the XRF spectrum. Ultramarine was detected in the blue parts. Concerning the violet color PR81 (bluish red, C.I. 45160:1) in mixture with PG7 (bluish green) were identified as main components. We want to outline that PR81 was rarely found in paintings. It was only recorded in the palettes of Lucio Fontana and Mary Cassatt before. The dark violet areas consist of Prussian blue and an unknown red (organic) colorant. Brown iron oxide was identified as the brown pigment. Bone black in mixture with black iron oxide were used as black materials and zinc white and titanium white as white pigments. XRF analysis of the metal color yields intense copper, zinc and nickel peaks (intensity ratio 3:3:1), which corresponds to “new silver” alloy. Barite and chalk are the fillers in this painting. Results of DRIFTS spectra show gum sometimes mixed with protein or oil (metal soaps) as binding media. The results point out that reverse glass paintings from the classic modern period are excellent examples to study the evolution of new pigments and their acceptance in artist’s palettes. T2 - CSI-XL CY - Pisa, Italy DA - 11.06.2017 KW - Pigments KW - Reverse glass painting KW - Spectroscopy PY - 2017 AN - OPUS4-42336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Priebe, Nsesheye Susan T1 - Effect of rheological parameters on rice husk ash blended pastes with various superplasticizers N2 - Rice husk ash (RHA) is a low-energy efficient material with high pozzolanic characteristics compared to other supplementary cementitious materials (SCMs). The replacement of cement with RHA has extensive improvement on the mechanical properties of concrete. However due to the porous nature of the RHA particles, it requires a higher water demand when replaced with Portland cement. Therefore, superplasticizers (SPs) are essential to reduce the water demand and improve the workability of the mixes. There is very little information about the effect of RHA with added SPs in its fresh state. Hence, this paper investigates the interaction of RHA pastes with three types of SPs, i.e. one polycarboxylate-based SP and two different types of lignosulphonates. This paper presents results of the investigation related to the flow behaviour of blended mixes with increasing percentage of RHA. The yield stress for the pastes with and without the addition of SPs is investigated over time as well as the plastic viscosity. T2 - 1st International Conference on Construction Materials for Sustainable Future CY - Zadar, Croatia DA - 19.04.2017 KW - Yield stress KW - Cement KW - Workability KW - Superplasticizers KW - Rice husk ash KW - Plastic viscosity PY - 2017 UR - http://www.grad.hr/coms/ocs/public/coms2017/Proceedings_of_the_CoMS_2017.pdf N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. AN - OPUS4-41035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon T1 - Study of modern reverse paintings on glass with Raman Spectroscopy N2 - The technique of painting on the reverse side of glass was rediscovered by artists in the 20th and gained especially in Germany strong popularity. Compared to other techniques (e.g. canvas, mural paintings), the paint layers are applied in reverse succession. The paintings are viewed in reflected light, thus revealing an impressive gloss, luminosity, and depth of color. Reverse glass paintings comprise a non-porous glass substrate and multi-layered paint system, hence delamination of the paint layer is the most common disfigurement. Scientific investigation of the material provides important information for appropriate conservation concepts. Transport of the precious and fragile objects to the lab is often not feasible. Therefore, in-situ, non-invasive analysis is necessary to analyze colorants and binders. Based on modern reverse glass paintings, we clarify advantages and limitations of mobile Raman spectroscopy for the identification of colorants. We compare the use of mobile Raman spectroscopy with other methods of our mobile lab (i.e. X-ray fluorescence (XRF), Diffuse Reflectance Fourier Transform Infrared Spectroscopy (DRIFTS). T2 - 9th International Congress on the Application of Raman Spectroscopy in Art and Archaeology (RAA2017) CY - Évora, Portugal DA - 24.10.2017 KW - Reverse glass painting KW - Raman spectroscopy KW - Synthetic organic pigments PY - 2017 AN - OPUS4-42825 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier T1 - A non-invasive study of the illuminated manuscript MS. Fr. 9084: one or two palettes? N2 - The manuscript of the History of Outremer by William of Tyre stored at the BNF (ms. fr. 9084) is believed to have been illustrated by two different hands. Indeed, the first five miniatures of this manuscript appear to be very different from the last seventeen, which were supposedly painted by an artist known as the "Hospitaller Master". This painter worked on at least two manuscripts in Paris between 1276 and 1280, and eight more in Saint Jean d'Acre before 1291. During his stay in the Latin Kingdom of Jerusalem, his palette changed and reached its most important development in the Manuscript of the History of Outremer, maybe influenced by the colourful crusader style of the first five miniatures. The present work aims at identifying the pigments used on both parts of the manuscripts and see whether they are the same for both artists or not. For that, portable XRF analysis was used directly at the Bibliothèque National de France in Paris, where the manuscript is stored. This allowed a quick, non destructive and non invasive study of the manuscript. Significant differences were observed in the compositions of some pigments indeed, in particular for the red and green, showing the use of different palettes. This could indicate that the Hospitaller Master not only brought his knowledge and style, but also probably part of his palette of pigments with him when moving to Saint Jean d'Acre. T2 - MANUSCRIPTS in the MAKING: Art and Science CY - Cambridge, UK DA - 08.12.2016 KW - Miniature KW - Pigment KW - XRF PY - 2016 AN - OPUS4-41529 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wintermann, C. T1 - Die Farbe als Hilfsmittel N2 - In vielen Zeichnungen lassen sich farbige Elemente feststellen, deren Funktion und Bedeutung Fragen aufwerfen. So diente die Farbe weder der Nachahmung naturalistischer Gegebenheiten, noch wurde sie für eine nachträgliche Wertsteigerung eingesetzt. Vielmehr scheint Farbe als Hilfsmittel verwendet worden zu sein, um Kopien oder Vervielfältigungen mittels Abklatsch, Durchzeichnung oder Durchgriffelung herzustellen. Darüber hinaus können entsprechende farbige Elemente auch als Hinweise auf eine Übertragung der Zeichnung in andere Medien gewertet werden, wie beispielsweise auf Druckplatten oder Malgründe. An zahlreichen Zeichnungen der frühen Neuzeit soll nachgewiesen werden, dass Farbe per se nicht nur eigenständiges künstlerisches Ausdrucksmittel ist. Basierend auf dieser Erkenntnis dürfen die betreffenden Zeichnungen nicht als sofort abgeschlossene, von der Hand eines Künstlers geschaffene Werke besprochen werden; vielmehr dokumentieren sie unterschiedliche Stadien eines Gestaltungsprozesses, die den Gebrauch und die Evidenz der Zeichnung reflektieren. T2 - Farbe auf Zeichnungen der frühen Neuzeit - Symbiose und Antagonismus. Gernsheim-Studientage CY - Rom, Italy DA - 25.10.2017 KW - Archäometrie KW - Farbe KW - ZfP PY - 2017 AN - OPUS4-42714 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niemeyer, B. A1 - Schwarzmaier, A. A1 - Radtke, Martin A1 - Hahn, Oliver T1 - Archaische Goldarbeiten aus Kleinasien in der Berliner Antikensammlung – Herstellungstechnik, Materialanalytik und der Fundkomplex »aus Ephesos« N2 - Ein Konvolut einzelner Schmuckstücke und die Goldbeigaben eines angeblichen Grabfundes wurden technologisch und analytisch untersucht. Die meisten Objekte sind Blecharbeiten, die aus einer Vielzahl von Einzelteilen mit metallischem Goldlot zusammengefügt und mit Granulation oder granulations-imitierendem Perl- oder Kerbdraht verziert wurden. Nur vier kleine Ohrringe sind massiv gegossen. Zwei Zierbleche dürften über Patrizen (Positivmodeln), die Deckel der Astragale in Matrizen (Negativmodeln) geformt worden sein. Alle Objekte wurden mit Synchrotron- und atmosphärischer Röntgenfluoreszenz analysiert. Die Daten zeigen das breite Spektrum an Goldlegierungen, die im 7./6. Jahrhundert v. Chr. in Kleinasien verarbeitet wurden: vom natürlichen Seifengold (Elektrum) bis zu geläutertem, fast reinem Gold. Eine Korrelation zwischen Goldqualität und Verarbeitungsmethode konnte nicht festgestellt werden. Sowohl hochreines als auch mit viel Silber und Kupfer legiertes Gold wurde zum Schmieden von Blecharbeiten, aber auch zum Massivguss verwendet. Aus der Goldfarbe kann wegen des Phänomens der oberflächlichen Goldanreicherung nicht auf eine Legierungszusammensetzung geschlossen werden. Der 1963 angekaufte Fundkomplex aus lydischen Metallarbeiten und ostionischen Salbgefäßen aus Ton dürfte einen Grabfund des frühen 6. Jahrhunderts v. Chr. darstellen, dessen Herkunft aus Ephesos jedoch nicht zu sichern ist. KW - Gold KW - Synchrotron KW - XRF PY - 2017 SN - 1866-7007 VL - 9 SP - 57 EP - 83 PB - RGZM. Archäologische Staatssammmlung München CY - München AN - OPUS4-42986 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Davis, K. A1 - Rabin, Ira A1 - Feldman, Ines A1 - Krutzsch, M. A1 - Rimon, H. A1 - Justnes, Å. A1 - Elgvin, T. A1 - Langlois, M. ED - Hempel, C. ED - Zahn, M. ED - Jokiranta, J. T1 - Nine dubious “Dead Sea Scrolls” fragments from the twenty-first century N2 - In 2002 new “Dead Sea Scrolls” fragments began to appear on the antiquities market, most of them through the Kando family. In this article is presented evidence that nine of these Dead Sea Scrolls-like fragments are modern forgeries. KW - Dead Sea Scrolls KW - NDT KW - Forgery KW - Papyrology PY - 2017 DO - https://doi.org/10.1163/15685179-12341428 SN - 0929-0761 SN - 1568-5179 VL - 24 IS - 2 SP - 189 EP - 228 PB - Brill CY - Leiden AN - OPUS4-42869 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver T1 - Zerstörungsfreie Materialanalyse an Kunst- und Kulturgut – Möglichkeiten und Grenzen N2 - Naturwissenschaftliche Verfahren sind zunehmend von Bedeutung bei der Untersuchung von Kunst- und Kulturgut und der Entwicklung von Konservierungskonzepten. Neben bildgebenden Verfahren sind materialanalytische Methoden von großer Wichtigkeit. Mobilen, zerstörungsfreien Verfahren ist grundsätzlich den Vorzug zu geben. Es ist jedoch zu konstatieren, dass Probenentnahmen unumgänglich sind, wenn spezielle Fragen an die Materialanalyse gestellt werden. T2 - Ringvorlesung Materialkunde, Technologie, Denkmalpflege und Kulturwissenschaften CY - Cologne Institute of Conservation Sciences, TH Köln DA - 06.11.2017 KW - Zerstörungsfreie Prüfung KW - Archäometrie KW - Kunst- und Kulturgut PY - 2017 AN - OPUS4-43424 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier T1 - What information can Raman spectroscopy provide about pure and mixed carbon inks? N2 - Two main types of inks coexisted in Early Medieval times: carbon inks and iron-gall inks. Many variations within these types existed, depending on the source of raw materials and their proportion. In addition to these, an intermediate mixed type of ink, with both iron and carbon as colouring agents, was sometimes used, especially in early Arab manuscripts. Two projects are being conducted currently at the Bundesanstalt für Materialforschung und -prüfung (BAM) concerning the analysis of inks with Raman spectroscopy. The first one aims at comparing the spectra of different carbon inks from Antiquity to the Middle Ages with Raman spectroscopy, while the second one focuses on the identification and comparison of mixed inks. For the first project, several carbon inks were made using different sources of carbon (pine soot, olive oil soot, date seeds charcoal etc.) and various binders (fish glue, gum Arabic, proteinic binder etc.), following antique recipes. These inks were then analysed with Raman spectroscopy and fitted with the “two-peaks” and the “three-peaks” models following the procedure described by Goler et al., to help spotting differences between the spectra, depending on the recipe. Some samples were then disposed in an ageing chamber at 80°C and 60% RH and analysed again in order to determine whether changed in the spectra are observable. The procedure proposed by Goler et al. to date inks with Raman spectroscopy was also evaluated during this process. Although several carbon inks could be distinguished from their spectra, no differences were seen between aged and fresh samples. Furthermore, experimental conditions were found to have such a significant influence that reliable dating of inks through Raman spectroscopy seems dubious. T2 - 9th International Congress on the Application of Raman Spectroscopy in Art and Archaeology CY - Évora, Portugal DA - 24.10.2017 KW - Carbon ink KW - Mixed ink KW - Dating KW - Raman PY - 2017 AN - OPUS4-42942 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Unveiling secrets of the Dead Sea scrolls N2 - The first manuscripts from the Qumran caves were found in 1947. Within the following 10 years, clandestine and legal excavations revealed some 900 highly fragmented manuscripts from the late Second Temple period. This collection is generally known as Scrolls of the Judea Desert or Dead Sea Scrolls (DSS). For many years after their discovery, text analysis and fragments attribution were the main concern of the scholars dealing with the scrolls. The uncertain archaeological provenance of the larger part of the collection added an additional difficulty to the formidable task of sorting some 19000 fragments. After 60 years of scholar research the questions of origin, archaeological provenance and correct attribution of the fragments are still hotly debated. In many cases material characterization of the scroll writing media deliver answers to the questions stated above. Furthermore, issues concerning corrosion pathways, ancient technologies and contemporary conservation activities demand in depth material studies. To obtain a comprehensive picture we use optical and electron microscopy, various X-ray based techniques as well as vibrational spectroscopy. We validated our approach with SY- based studies using the advantages of the synchrotron radiation source with respect to the bench-top devices. Our laboratory studies showed that often production and storage locality could be distinguished thanks to the specific residues (“fingerprint”) they left on the material. Moreover, we have discovered that different parchment production processes coexisted in the antiquity, and the resulting writing materials can readily be distinguished. Within our recent studies we tentatively reconstructed the history of the Genesis Apocryphon. Written with a corrosive ink on a tanned parchment, it was found rolled together with an additional layer of non-inscribed non-tanned parchment. Chemical composition of the ink is in agreement with a 1st century AD ink recipe recorded in Materia Medica by a Greek physician, Pedanius Dioscorides. Study of the scroll deterioration as a function of time and exposition to light during the post-discovery period allows us to speculate that the scroll was rather “archived” than hidden in Cave 1. These results confirm the theory of Eliezer Sukenik who believed Cave 1 to be a “geniza”. A similar study of the Temple Scroll, discovered in the cave 11 indicates that the scroll was rather hidden than “archived”. T2 - 2nd International Conference on Patristic Studies CY - San Juan, Argentina DA - 28.03.2017 KW - Dead Sea scrolls PY - 2017 AN - OPUS4-43442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Instrumental studies of writing inks: from typology to composition N2 - The course presents panorama of historic writing inks, their use the methods of their identification. First, we discuss the possible types of the inks and show how one can determine these types using very simple instrumentation. The change of the inks from those based on soot to the iron-gall inks commonly used in the Middle Age constitutes the second half of the course. T2 - Workshop CY - Buenos Aires, Argentina DA - 23.03.2017 KW - Ink KW - Carbon ink KW - Iron-gall ink PY - 2017 AN - OPUS4-43445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Material studies of inks N2 - The course presents panorama of historic writing inks, their use the methods of their identification. First, we discuss the possible types of the inks and show how one can determine these types using very simple instrumentation. The change of the inks from those based on soot to the iron-gall inks commonly used in the Middle Age constitutes the second half of the course. T2 - Summer School Hebrew Codicology and Palaeography Based on the Collection of the State and University Library Hamburg CY - Hamburg, Germany DA - 07.09.2017 KW - Iron-gall ink KW - Carbon ink KW - Mixed ink PY - 2017 AN - OPUS4-43448 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Schmidt, Wolfram A1 - Tchetgnia Ngassam, Ines Leana ED - Schmidt, Wolfram ED - Tchetgnia Ngassam, Ines Leana T1 - Cement proficiency testing scheme 2016/2017 - Final report N2 - The cement proficiency testing (PT) scheme was set up by the German Metrology Institute (PTB) and the Federal Institute for Materials Research and Testing (BAM) in 2012. The PT scheme was a spin-off from a European Commission and African, Caribbean and Pacific-Group of States funded project entitled SPIN – Spearhead Network for Innovative, Clean and Safe Cement and Concrete Technologies (www.spin.bam.de). The SPIN project aimed at crosslinking experts in industry and policy making bodies, with the prospect of establishing a sustainable cement and concrete construction capacity in Africa. After a successful first pan-African proficiency testing scheme in 2012/2013, it was decided to establish the scheme permanently and independent of the SPIN project. The main focus of setting up a testing scheme was to enable all cement testing laboratories in Africa to evaluate their competence and efficiency in cement testing and further enhance their capacity to obtain better quality products according to their environment. The acronym developed for the PT scheme is PACE-PTS (Pan-African Cement Proficiency Testing Scheme). The framework for the PT scheme was set up jointly among the organisers and the first participants. The first PT scheme was initiated in Dar Es Salaam in 2012 followed by a final workshop in Berlin in 2013. The second PT scheme began in 2014. A final workshop was organised in Dar es Salaam in 2015. The third and current scheme was started in 2016 and the final workshop is held in Yaoundé. KW - PACE-PTS KW - Round Robin KW - Proficiency testing KW - Cement KW - Quality infrastructure PY - 2017 VL - 3 SP - 1 EP - 74 PB - BAM CY - Berlin AN - OPUS4-43546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira A1 - Hahn, Oliver ED - Hahn, Oliver ED - Breiding, Sonja ED - Doil, Thorsten T1 - Röntgenfluoreszenzanalyse als bildgebendes Verfahren - Die Visualisierung von Materialität N2 - Naturwissenschaftliche Verfahren sind inzwischen fester Bestandteil bei der materialwissenschaftlichen Untersuchung von Kunst- und Kulturgut und bei der Entwicklung von Konservierungskonzepten zum Erhalt des kulturellen Erbes. Insbesondere werden zunehmend bildgebenden Verfahren wie die Computertomographie, die Radiographie oder die Multispektralanalyse verwendet, um die für das menschliche Auge nicht sichtbare Inhalte wie Vorzeichnungen, Pentimenti oder innere Strukturen zu visualisieren. Die entstehenden „neuen Bilder“ verändern jedoch die Sichtweise auf das kulturelle Artefakt, da sie tiefere Einblicke in den Herstellungsprozess, den Aufbau oder den Erhaltungszustand geben können. Weiterhin dokumentieren sie Veränderungen, denen ein Objekt unterworfen wurde. Anhand der Untersuchung von zwei Objekten mit dem Röntgenfluoreszenzportalscanner Jet Stream soll das Verhältnis Original – Digitalisat – Rekonstruktion diskutiert werden. T2 - 8. N.i.Ke.-Workshop: Materialität - Das Objektverständnis der vielfältigen Disziplinen im Bereich von Kunst- und Kulturgut CY - Berlin, Germany DA - 26.11.2015 KW - Röntgenfluoreszenzanalyse KW - Zerstörungsfreie Prüfung KW - Archäometrie PY - 2017 SN - 2567-1251 SP - 68 EP - 73 PB - Druckerei G. Bohm CY - Berlin AN - OPUS4-43484 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram T1 - Concrete casting robustness improvement due to active rheology control N2 - With ongoing innovation in process technology, the challenges of concrete technology are more and more focused on the rheological optimisation for these processes, since improper mixture stability or poor compaction ability negatively affect the concrete homogeneity and quality. However, along with the increasing complexity of today’s concrete mixture compositions, concrete becomes more prone to failure regarding the casting process. Variable properties of the raw materials typically cause changing workability. The reasons can be found among others in scattering water contents, physical or chemical properties of the cement or varying environmental temperatures. Robustness in the delicately adjusted rheology, however, is of utmost importance for modern and future process technology, from sprayed concrete over pumpable concrete towards 3D-printing, with regard to the long-term strength, the function and the durability. Typically, material induced changes cannot be identified easily due to the complex interactions of concrete constituents. Therefore, a precise and prompt counteraction is impossible. However, it is known that the yield stress can be controlled by addition of supplementary superplasticizer or stabilising agent. In combination with computerized process observation tools that can rapidly interpret and react on changes in the rheology, it is therefore thinkable, that only these two admixture types can adjust the rheology steadily and permanently, regardless of the actual root cause for observed macroscopic rheology change. The presentation will firstly give a comprehensive overview of effects at the interface between pore solution, particles and hydrates, which affect the rheology of fresh concrete. Secondly, ways are recommended how the rheology can be actively manipulated before eventually computerized methods are demonstrated that help to actively and rapidly assess and counteract performance scatter during steady casting processes. T2 - 2nd International Congress on Materials & Structural Stability CY - Rabat, Morocco DA - 21.11.2017 KW - Rheology KW - Control charts KW - Cusum KW - Additive manufacturing KW - Online quality control PY - 2017 AN - OPUS4-43542 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Parchment N2 - This lecture will present history of parchment based on written sources and chemical examination of antique, medieval and modern parchment. Our studies of the Dead Sea Scrolls writing surfaces show that they can be divided roughly into three groups: leather, parchments of a light tint, and those of various shades of brown. The latter ones are invariably tanned, whereas the middle group is characterized by the presence of various inorganic salts. Some of the pale parchments, among them the Temple Scroll (11Q19), are remarkably similar to medieval European parchment. Therefore we have formulated the working theory that in the Judaea of the Hellenistic period two different parchment-making traditions existed side by side: an ‘eastern’ one (represented by the tanned parchments of Qumran, closely resembling Aramaic documents from the fifth century BC, and a ‘western’ one (represented by the untanned/lightly tanned ones similar to early Christian Greek parchments). This division has found support during our studies of the Geniza fragments, in which Babylonian and Palestinian traditions seem to follow the “eastern” and “western” technologies, respectively. T2 - Manusciences 17 CY - Frejus, France DA - 10.09.2017 KW - Parchment KW - Leather PY - 2017 AN - OPUS4-43478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Material analysis: authentication or forgery detection? N2 - This paper addresses the sensitive issue of authentication of the un-provenanced manuscripts of high monetary value if certified to be genuine. Over the last decade the popularity of material studies of manuscripts using non-destructive technologies (NDT) has increased enormously. In the case of suspicious writings these studies are held in especially high esteem due to the methodological rigor they are reputed to contribute to debate. Moreover, audiences from a humanities background often tend to disregard the technical details and treat any published interpretation of instrumental analysis as an objective finding. The paper will discuss the currently available methods and testing protocols for writing materials stressing the advantages and limitations of the non-invasive analysis. As an example we will consider the recent announcement of the possibility of non-invasive dating of carbon inks focusing on the validation required for a testing method. We will make clear that material analysis alone cannot prove that the object is genuine. We should rather adopt the effective approach for testing suspicious artifacts that has been established by the forensic science. Here, not the authentication, but the determination of the forgery stands in the focus of the work. T2 - SBL Annual Meeting 2017 CY - Boston, MA, USA DA - 18.11.2017 KW - Cultural assets KW - Forgery PY - 2017 AN - OPUS4-43483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Durkin-Meisterernst, D. A1 - Friedrich, M. A1 - Helman-Wazny, A. A1 - Nöller, R. A1 - Raschmann, S.-Ch. A1 - Hahn, Oliver T1 - Scientific methods for philological scholarship: Pigment and paper analyses in the field of manuscriptology N2 - In this paper, members of three research teams, namely the Turfan Project of the Berlin BrandenburgAcademy of Sciences and Humanities, the Berlin-based research project on pigments in Central Asianpaper manuscripts, and the Hamburg-based project on the history and typology of Central Asian papermanuscripts, present some of the results of their cooperation. The investigated manuscripts belong tothe Berlin Turfan Collection. On the basis of different examples the contribution of scientific methods tophilological scholarship within a multidisciplinary approach is demonstrated. KW - Turfan manuscripts KW - Material analysis KW - Paper KW - Ink KW - Turfan Manuskripte KW - Materialanalyse KW - Papier KW - Tinte PY - 2016 DO - https://doi.org/http://dx.doi.org/10.1016/j.culher.2015.06.004 SN - 1296-2074 VL - 17 SP - 7 EP - 13 PB - Elsevier, München AN - OPUS4-35551 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stroh, Julia A1 - Schlegel, Moritz-Caspar A1 - Schmidt, Wolfram A1 - Nguyen, Thi Yen A1 - Meng, Birgit A1 - Emmerling, Franziska T1 - Time-resolved in situ investigation of Portland cement hydration influenced by chemical admixtures N2 - Numerous admixtures are used in the building practice to customize the properties of the cement paste during application. The influences of admixtures on the course of cement hydration and formation of hydrate phases have to be considered. Polycarboxylate ether (PCE) based polymeric superplasticizers (SPs) are known to retard the setting of the cement paste. The extent of the retardation differs depending on the molecular structure of the SP. Additionally, the presence of a stabilizing agent (SA) in the cement paste has a retarding side effect on the setting. The initial cement hydration processes and the detailed mechanisms of the retardation influenced by PCEs, as well as their interactions with particular SAs, are insufficiently understood. Up to now, only the results of phenomenological studies were taken into account to describe this retardation process. A detailed structure analysis monitoring the change of the phase composition during the hydration was never applied. Both SP and SA affect the adsorption of the sulphate ions on the clinker particles, causing changes in the formation of ettringite during the initial hydration, and are therefore a crucial part of the setting process itself. Here, the initial hydration of cement influenced by the interaction of SP and SA was monitored in situ by synchrotron X-ray diffraction. The high time resolution of the measurements allowed a continuous detection of the hydrates formed. The hydration was followed from the starting point of water addition and for couple of hours afterwards. The hydration of the levitated cement pellets containing starch as SA was initialized by adding aqueous solutions of different commercial SPs. Changes in the ettringite formation were detected in comparison to the reference hydration of pure cement. KW - Synchrotron KW - Portland cement Initial hydration KW - Superplasticizer KW - Stabilizer KW - XRD PY - 2016 DO - https://doi.org/http://dx.doi.org/10.1016/j.conbuildmat.2015.12.097 IS - 106 SP - 18 EP - 26 PB - Elsevier AN - OPUS4-35467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver T1 - Farbe auf Papier - Materialwissenschaftliche Aspekte des Buchdrucks N2 - Der Vortrag beschäftigt sich mit den materialwissenschaftlichen Aspekten des Buchdrucks. Hierbei geht es weniger um die Darstellung und Erklärung der unterschiedlichen Druckverfahren (Hochdruck, Tiefdruck, Flachdruck und Durchdruck), diese werden nur am Rande gestreift, um die Vielfalt der unterschiedlichen Drucktechniken darzulegen. Vielmehr beschäftigt sich der Vortrag mit den Materialien, d.h. Druckfarben, die sich dann tatsächlich auf dem Schriftträger analysieren lassen. Unterschiedliche Drucktechniken (und Effekte) erfordern unterschiedliche Materialzusammensetzungen - diese werden innerhalb des Vortrags diskutiert. T2 - Transformationen des Buchdrucks, Konferenz des Basisprojekts "Matter of Typography" CY - Berlin, Germany DA - 09.06.2016 KW - Buchdruck KW - Material KW - Farbmittel PY - 2016 AN - OPUS4-36565 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gemeinert, Marion A1 - Steinborn, Gabriele T1 - Stabilized dielectric barium titanate dispersions for sensor filling N2 - Resolution of special capacitive sensors can be improved enormously by replacement of the gaseous material between the capacitor plates by a ceramic dispersion with high permittivity. High dielectric liquid dispersions of ceramic submicron and nano barium titanate powders should be qualified as dielectric fluid with long-term shelf life for this use. Investigations for the production of stabilized barium titanate dispersions in aqueous and organic liquids by use of different dispersant aids were performed. Characterization of dispersed particles and agglomerates was done by use of zeta potential measurements for aqueous dispersions as well as particle sizing by laser diffraction, ultrasound spectroscopy and dynamic light scattering for aqueous and organic dispersions. Optimization of stability was evaluated by accelerated sedimentation measurements with an optical centrifuge. Best results were achieved for barium titanate dispersions in silicone oil. T2 - 91. Jahrestagung der deutschen keramischen Gesellschaft CY - Freiberg, Germany DA - 07.03.2016 KW - Stabilized dispersions KW - Barium titanate nanopowder KW - Particle size analysis PY - 2016 AN - OPUS4-35635 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Weimann, Christiane A1 - Chaves Weba, Luciana ED - Schmidt, Wolfram ED - Priebe, Nsesheye Susan T1 - Influences of hydration effects on the flow phenomena of concrete with admixtures N2 - Chemical admixtures like superplasticisers or stabilising agents are of ever increasing importance for modern concrete technology. They liberate the workability of concrete from its dependency on water content, and thus, open the gate towards innovative and future oriented concrete technologies such as self-compacting concrete. Today, admixture addition has become common practice in concrete technology, but the understanding of their highly complex mode of operation is extremely difficult and demands for understanding of processes within the range between nanometres and centimetres. Due to its complex time-dependent, multi-phase and multi-scale behaviour, flowable concrete systems are highly complicated and cannot be described comprehensively by simple models. It is therefore extremely challenging to identify the relevant parameters that predominantly control flow phenomena on different size scales, since these may occur on any scale between the nano scale (e.g. superplasticizer adsorption) and macro scale (e.g. grading of the aggregates). The present study discusses fundamental mechanisms at the interface between particle or hydrate surfaces and the fluid phase at a very early stage of concrete formation, and links these effects to macroscopic flow phenomena. Methods are discussed that appear promising interdisciplinary tools for enhancement of the understanding of the relevant interactions that are responsible for the macroscopic flow of flowable concrete. T2 - 2nd International Conference on Advances in Cement and Concrete Technology in Africa CY - Dar es Salaam, Tanzania DA - 27.01.2016 KW - Cement hydration KW - Polymer adsorption KW - Rheology KW - Superplasticizer KW - Self-compacting concrete PY - 2016 SN - 978-3-9817502-3-2 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. SP - 79 EP - 88 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-36875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Umeche, E. L. A1 - Schmidt, Wolfram A1 - Uzoegbo, H. Ch. ED - Schmidt, Wolfram ED - Priebe, Nsesheye Susan T1 - A survey and analysis of locally available cements in South Africa N2 - South Africa and recently Nigeria are the only net exporter of cement in Africa, yet cements are imported into the country mainly on the basis of price competitiveness. This poses potential for scatter in the properties of the cements in the South African market as pricing seems to be the only determining factor that affects Portland cements imported. A survey of cements of grade 42.5N in the South African cement market was carried out to identify major players in the industry. The identified cements, which included four locally produced and one imported cement were then analysed for both chemical composition and physical properties in line with the Eurocode EN 196. Tests carried out include loss on ignition, chloride content, sulphate content, specific surface (Blaine), standard consistence, initial setting time, final setting time, soundness and flexural and compressive strength at 2, 7 and 28 days. The testing program was initiated as part of on-going Africa-wide cement testing competency program in partnership with BAM and PTB in Germany. The performance of the identified cements from the different local manufacturers and the imported cement were analysed and are presented in this paper. These results reveal some similarities and differences in the properties. Particularly of interest is the marked difference in the 28 days compressive strength of the cements. This paper shows that there is need for further tests across the cement industry as some of the cements failed to meet certain requirement as set by EN 196. The paper also recommends the use of proficiency testing schemes in the cement industry of the country to ensure the cement laboratories are providing results of high quality and at the same time act as a check to make sure these laboratories are not failing to meet standard requirements. T2 - 2nd International Conference on Advances in Cement and Concrete Technology in Africa CY - Dar es Salaam, Tanzania DA - 27.01.2016 KW - Cement KW - Proficiency testing KW - EN 196 KW - Standards KW - South Africa PY - 2016 SN - 978-3-9817502-3-2 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. SP - 91 EP - 98 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-36876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Mota Gassó, Berta A1 - Sturm, Heinz A1 - Pauli, Jutta ED - Greim, M. ED - Kusterle, W. ED - Teubert, O. T1 - Influence of effects on nano and micro scale on the rheological performance of cement paste, mortar and concrete N2 - Chemical admixtures like superplasticisers or stabilising agents are of ever increasing importance for modern concrete technology. They liberate the workability of concrete from its dependency on water content, and thus, open the gate towards innovative and future oriented concrete technologies such as self-compacting concrete. Today, admixture addition has become common practice in concrete technology, but the understanding of their highly complex mode of operation is extremely difficult and demands for understanding of processes within the range between nanometres and centimetres. Due to its complex time-dependent, multi-phase and multi-scale behaviour, flowable concrete systems are highly complicated and cannot be described comprehensively by simple models. It is therefore extremely challenging to identify the relevant parameters that predominantly control flow phenomena on different size scales, since these may occur on any scale between the nano scale (e.g. superplasticizer adsorption) and macro scale (e.g. grading of the aggregates). The present study discusses fundamental mechanisms at the interface between particle or hydrate surfaces and the fluid phase at a very early stage of concrete formation, and links these effects to macroscopic flow phenomena. Methods are discussed that appear promising interdisciplinary tools for enhancement of the understanding of the relevant interactions that are responsible for the macroscopic flow of flowable concrete. T2 - 25. Workshop und Kolloquium Rheologische Messsungen an Baustoffen CY - Regensburg, Germany DA - 02.03.2016 KW - Rheology KW - Cement KW - Concrete KW - Superplasticizer KW - Nano scale PY - 2016 SN - 978-3-7345-1313-8 SP - 294 EP - 307 PB - tredition CY - Hamburg AN - OPUS4-36862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Kühne, Hans-Carsten ED - Khayat, Kamal Henry T1 - Cusum charts for the control of the slump flow of self-compacting concrete in a steady production process N2 - Control chart systems are commonly used in quality management systems to keep production processes stable. The most efficient control chart systems are cumulated sums (cusum), which look at the deviations from a target value. Cusum charts react more rapidly on systematic changes in processes than other charts such as Shewhart charts, which look at the process values. The cusum method is often applied for compressive strength but it is particularly suitable if counteractions be taken immediately, like in the case of fresh concrete properties. The present study shows that regardless of the manipulation, a steady slump flow can be achieved only by adding supplementary superplasticizer in case of loss of flow and adding stabilising agent (ST) in case of increased flow if the V-mask indicates a systematic change. A reference SCC was artificially manipulated in order to achieve either increased or reduced flowability. Arithmetic mean values and standard deviations were determined experimentally without and after taking counteractions. These parameters were used for case studies of steady SCC productions based on normally distributed random values. For the indication of a systematic change, a standard V-mask was used. The results point out that productions with applied cusum methods were capable of keeping the slump flow deviation from the target in the order of magnitude of about 1% despite drastic manipulations, while productions without applied cusum method deviated up to 14% and more from the target slump flow value. T2 - 8th RILEM Symposium on Self-Compacting Concrete CY - Washington, USA DA - 15.05.2016 KW - Control charts KW - Cusum KW - Quality control KW - Rheology KW - Self-compacting concrete PY - 2016 SN - 978-2-35158-157-5 SP - 283 EP - 294 PB - RILEM Publications S.A.R.L. CY - Paris, France AN - OPUS4-36874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Leinitz, Sarah A1 - Kühne, Hans-Carsten ED - Malhotra, V. M. ED - Gupta, P. R. ED - Holland, T. C. T1 - Effects of particle volume fraction and size on polysaccharide stabilizing agents N2 - Polysaccharides modify the rheological properties of cement based systems. Depending upon their chemistry, molecular architecture, and adsorption tendency, they have different modes of action. Some polysaccharides like diutan gum have strong effect on the fluid phase; others like starch strongly interact with particles. This paper presents effects of diutan gum and starches in presence of polycarboxylates. Rheometric investigations with varied particle volume fractions and increasing coarse aggregate diameters were conducted. The results show that starches have stronger influence on the rheology at high particle volume fractions than diutan gum. At lower particle volume fractions this trend is inverted. Experiments with aggregates sizes up to 16 mm (0.63 in.) indicate that stabilizing agent influences on the effects of aggregates on yield stress were small; however up to 1.0 mm (0.04 in.), a significant effect on the plastic viscosity could be observed, which levelled off at larger diameters. T2 - 11th International Conference on Superplasticizers and Other Chemical Admixtures in Concrete CY - Ottawa, Canada DA - 12.07.2015 KW - Diutan gum KW - Starch KW - Polysaccharides KW - Polycarboxylate ether KW - Volume fraction PY - 2015 SN - 9781942727224 SP - SP-302-03, 39 EP - 52 AN - OPUS4-36861 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vasilic, Ksenija A1 - Schmidt, Wolfram A1 - Kühne, Hans-Carsten A1 - Haamkens, Frank A1 - Mechtcherine, V. A1 - Roussel, N. T1 - Flow of fresh concrete through reinforced elements: Experimental validation of the porous analogy numerical method N2 - Numerical simulations of concrete castings are complex and time consuming. In order to decrease simulation time and to simplify simulation procedure, an innovative modelling approach, which treats reinforced sections in a formwork as porous media, was proposed. In the previous studies, this numerical model was proved suitable to simulate casting of model yield-stress fluids through reinforced elements. This article focuses on the experimental validation of the proposed model at the concrete scale. For this purpose, a large-scale laboratory casting of a highly reinforced beam is performed. The casting process is numerically simulated and the numerical results are compared to the experimental measurements. KW - Porous medium KW - Self-compacting concrete KW - Casting KW - CFD simulation KW - Reinforcement PY - 2016 UR - http://www.sciencedirect.com/science/article/pii/S0008884616301880 DO - https://doi.org/10.1016/j.cemconres.2016.06.003 SN - 0008-8846 VL - 2016/88 SP - 1 EP - 6 PB - Elsevier Ltd. AN - OPUS4-37441 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vasilic, Ksenija A1 - Schmidt, Wolfram A1 - Kühne, Hans-Carsten A1 - Roussel, N. T1 - Model of SCC flow through reinforced sections: experimental validation N2 - This study focuses on concrete flow in presence of obstacles and develops a mathematical model and a computational approach for SCC flow through reinforced formworks. In order to decrease high computational times needed to simulate castings through reinforced elements, an innovative approach to model the reinforced sections as porous media is proposed here. In the previous work, this numerical model is proved able to simulate the free-surface flow of non-Newtonian fluids through the reinforcement networks. In the present study, the applicability of the model on the concrete flow will finally be proved. The large-scale form-filling experiments with SCC will be conducted and the experiments will be simulated using the proposed numerical model. The numerical model will then be validated through the comparison of the experimental results and the results of the numerical simulations. T2 - 7th RILEM International Conference on Self-Compacting Concrete and 1st RILEM International Conference on Rheology and Processing of Construction Materials CY - Paris, France DA - 02.09.2013 KW - Porous medium KW - Rheology KW - Numerical modelling KW - Reinforcement PY - 2013 SN - 978-2-35158-137-7 SN - 978-2-35158-138-4 SP - 229 EP - 236 PB - RILEM Publishing S.A.R.L CY - Paris, France AN - OPUS4-37442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Barthel, Maria A1 - Schmidt, Wolfram A1 - Kühne, Hans-Carsten A1 - Rübner, Katrin ED - Schmidt, Wolfram ED - Priebe, Nsesheye Susan T1 - Interactions between waste paper sludge ashes and superplasticizers based on polycarboxylates N2 - In many industrial nations, about two third of the paper demand is covered by recovered paper. A major process step within the treatment of waste paper is the de-inking. It is a floating process yielding paper sludge as a waste product. About 50 % of this residue is used as a fuel. In several cases it is burnt at temperature of about 850 °C and thereafter the accrued ashes are collected in the flue gas filter. During the combustion, kaolinite and calcium oxide generate gehlenite and larnite. Calcite is the main component of waste paper sludge ash (PA).The chemical and mineralogical composition of PA suggests using it as a supplementary cementitious material. In modern construction materials technology, workability aspects gain importance, since for most modern materials the rheology and compaction ability are relevant for the operation at a hardened state. It was observed that PA significantly increases the water demand of powder systems, which can cause serious problems during the casting of mineral binder systems containing PA. It is therefore obvious that binder systems containing PA might demand for the use of superplasticizers. Superplasticizers are polymers with anionic backbone that cause electrostatic and steric repulsion effects upon adsorption on surfaces of particles and hydration phases. In this paper interactions between superplasticizers and waste paper sludge ashes are discussed and analysed. Based on observations of changes in the zeta potential and the dispersion of the particle system, the influence of the charge density of superplasticizers is observed and time dependent effects are demonstrated. T2 - 2nd International Conference on Advances in Cement and Concrete Technology in Africa CY - Dar es Salaam, Tanzania DA - 27.01.2016 KW - Waste paper sludge KW - Rheology KW - Cement KW - Concrete KW - Polycarboxylate ether PY - 2016 SN - 978-3-9817502-3-2 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. SP - 181 EP - 186 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-36877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vasilic, Ksenija A1 - Kühne, Hans-Carsten A1 - Schmidt, Wolfram A1 - Roussel, N. T1 - Numerical simulations of scc casting: parameter determination N2 - The paper addresses numerical modelling of fresh self-compacting concrete. In the previous studies, a numerical tool for casting prediction is built based on the assumption that fresh concrete behaves as a yield-stress fluid and treating zones with rebars as porous media. The present contribution discusses the determination of material parameters, which are required as an input for numerical simulations of casting processes. T2 - International RILEM Conference on Materials, Systems and Structures in Civil Engineering 2016, Segment on Fresh Concrete CY - Lyngby, Denmark DA - 22.08.2016 KW - Fresh concrete KW - Simulation KW - CFD KW - Rheology PY - 2016 SN - 978-2-35158-184-1 SP - 163 EP - 172 PB - RILEM Publications S.A.R.L. CY - Paris, France AN - OPUS4-37446 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steger, Simon A1 - Stege, H. A1 - Bretz, S. A1 - Hahn, Oliver T1 - Capabilities and limitations of handheld Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) for the analysis of colourants and binders in 20th-century reverse paintings on glass N2 - A non-invasivemethod has been carried out to show the capabilities and limitations of Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS) for identifying of colourants and binders in modern reverse glass paintings. For this purpose, the reverse glass paintings “Zwei Frauen am Tisch” (1920–22), “Bäume” (1946) (both by Heinrich Campendonk), “Lofoten” (1933) (Edith Campendonk-van Leckwyck) and “Ohne Titel” (1954) (Marianne Uhlenhuth), were measured. In contrast to other techniques (e.g. panel and mural painting), the paint layers are applied in reverse succession. In multi-layered paint systems, the front paint layer may no longer be accessible. The work points out the different spectral appearance of a given substance (gypsum, basic lead white) in reverse glass paintings. However, inverted bands, band overlapping and derivative-shaped spectral features can be interpreted by comparing the spectra fromthe paintingswith spectra frompure powders and pigment/linseed oil mock-ups. Moreover, the work focuses on this method's capabilities in identifying synthetic organic pigments (SOP). Reference spectra of three common SOP (PG7, PY1, PR83) were obtained from powders and historical colour charts.We identified PR83 and PY1 in two reverse glass paintings, using the measured reference spectra. The recorded DRIFTS spectra of pure linseed oil, gum Arabic, mastic, polyvinyl acetate resin and bees wax can be used to classify the binding media of the measured paintings. KW - DRIFTS KW - Painting KW - Non-invasive KW - Pigment PY - 2018 DO - https://doi.org/10.1016/j.saa.2018.01.057 SN - 1873-3557 VL - 195 SP - 103 EP - 112 PB - Elsevier B.V. AN - OPUS4-44023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Brüning, Gerrit A1 - Hahn, Oliver ED - Nutt-Kofoth, Rüdiger ED - Plachta, Bodo T1 - Goethes Helena-Dichtung in ursprünglicher Gestalt. Zum methodischen Verhältnis von Materialanalyse und Textkritik N2 - Seit 2009 entsteht die historisch-kritische Hybridediton von Goethes „Faust“. Im Januar 2013 ist im Rahmen dieses editorischen Unternehmens die Röntgenfluoreszenzanalyse (RFA) zum Einsatz gekommen, um auf der Grundlage der Zusammensetzung der verwendeten Eisengallustinten entstehungsgeschichtliche Erkenntnisse über das handschriftliche Material zu gewinnen. Im Mittelpunkt stand neben der zeitlichen Einordnung von Handschriften vor allem die Identifikation von unterscheidbaren Bearbeitungsschichten innerhalb der jeweiligen Handschrift. Besonderes Interesse kommt dabei denjenigen Handschriften zu, von denen sicher ist oder angenommen wird, dass Goethe sie über längere Zeit hinweg oder sogar in sehr großen Abständen bearbeitet hat. Die von der traditionellen Philologie in Anschlag gebrachten äußeren und inneren Gründe und die darauf gestützten Hypothesen haben nicht ausgedient. Hypothesen zur Datierung von Handschriften Goethes lassen sich in der Regel gut anhand bestehender materieller Zusammenhänge (wie der Zuordnung des Papiers in Kombination mit der Bestimmung der Schreiberhand) verifizieren. Dagegen ermöglicht materialwissenschaftliche Charakterisierung der Eisengallustinten alleine zunächst noch keine vergleichbar genauen Datierungen. Eine Kombination der beiden Zugänge und Verfahren kann jedoch dort Erkenntnisse zutage fördern, wo die traditionellen philologischen Mittel ausgeschöpft sind. Dies wird exemplarisch innerhalb der Publikation gezeigt werden. KW - Materialanalyse KW - Eisengallustinten KW - Germanistik PY - 2017 DO - https://doi.org/10.1515/editio-2017-0009 SN - 0931-3079 SN - 1865-9446 VL - 31 SP - 145 EP - 172 PB - Walter de Gruyter GmbH CY - Berlin AN - OPUS4-43849 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver T1 - Inks and Pigments N2 - The writing materials used in various cultures and epochs can be divided into two groups. The first comprises materials that write themselves, producing script by rubbing their own material off onto the writing surface. It includes charcoal, graphite, chalk, raddle, and metal styluses. Depending on the material and consistency, these are cut or pressed to make styluses and then used for writing. The second group comprises all coloring liquids that are applied to the writing surface with a quill, pen, or printing block. It includes inks made from dye solutions (for example, tannin inks) and those made from pigment dispersions (for example, sepia, soot, and bister inks). The latter are sometimes also rubbed as pastes into letters incised into the writing surface, where they increase visual contrast. Due to the variety of recipes and the natural origin of raw materials, there is a wide range of different components and impurities in writing materials. Soluble inks (Tinten) Soluble inks are based mainly on dyes forming a water solution. Colored inks were manufactured with different plant or insect dyes (e.g. Brazil wood, kermes). To stabilize the volatile material, the dyes were mixed with a mordant (e.g., alum). Brown plant inks – best-known as blackthorn or Theophilus’ inks – are usually produced from the blackthorn bark and wine. In the early European Middle Ages, inks of this kind were widely used in the production of manuscripts in monasteries. Usually, they are light brown, so sometimes small amounts of iron sulfate were added, which led to what was called an “imperfect” iron gall ink. The difference between “classic” iron gall ink and such imperfect ink is therefore not clear: the distinction is not possible, especially with the naked eye. Dispersion inks (Tuschen) According to its generic recipe, one of the oldest black writing materials is produced by mixing soot with a binder dissolved in a small amount of water. Thus, along with soot, binders such as gum arabic (ancient Egypt) or animal glue (China) are among the main components of soot inks. From Pliny’s detailed account of the manufacture of various soot-based inks, we learn that, despite its seeming simplicity, producing pure soot of high quality was not an easy task in Antiquity. Therefore, we expect to find various detectable additives that might be indicative of the time and place of production. One such carbon ink requires the addition of copper sulfate . The experimental discovery of this ink in 1990 led to a misleading expression “metal ink” that is sometimes found in the literature. Colored dispersion inks based on pigments such as orpiment, cinnabar, or azurite have been known since Antiquity. Natural or artificially produced minerals are finely ground and dispersed in a binding medium. As in soot inks, water-soluble binders such as gum arabic or egg white were used. Iron gall ink (Eisengallustinten) Iron gall inks are a borderline case between these two groups. They are produced from four basic ingredients: galls, vitriol as the main source of iron, gum arabic as a binding media, and an aqueous medium such as wine, beer, or vinegar. By mixing gallic acid with iron sulfate, a water-soluble ferrous gallate complex is formed; this product belongs to the type “soluble inks”. Due to its solubility, the ink penetrates the writing support’s surface, making it difficult to erase. Exposure to oxygen leads to the formation of insoluble black ferric gallate pigment, i.e., “dispersion ink”. Natural vitriol consists of a varying mixture of metal sulfates. Since for ink making it was obtained from different mines and by various techniques, inks contain many other metals, like copper, aluminum, zinc, and manganese, in addition to the iron sulfate. These metals do not contribute to color formation in the ink solution, but possibly change the chemical properties of the inks. T2 - Manusciences 17 CY - Frejus, France DA - 10.9.2017 KW - Medieval ink KW - Medieval pigment KW - Material analysis PY - 2017 AN - OPUS4-43556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Rabin, Ira ED - Elgvin, T. T1 - The Temple Scroll: Wrapper and fragment. MS 5095/2, MS 5095/4 N2 - The following specification of experimental methods refers to tests performed in 2009–10 on vellum,textile, ink, pottery, leather, and palm-fibre tool, as described in the chapter written by me and Roman Schütz. KW - Dead Sea Scrolls KW - The Temple Scroll PY - 2016 SN - 978-0-5672-8571-3 SN - 978-0-5671-1300-9 VL - 71 SP - 327 EP - 338 PB - Bloomsbury T&T Clark AN - OPUS4-43949 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Characterization of the Dead Sea Scrolls by advanced analytical techniques. N2 - For many years after the discovery of the Dead Sea Scrolls, text analysis and fragment attribution were the main concern of the scholars dealing with them. The uncertain archaeological provenance of a large part of the collection added difficulties to the already formidable task of sorting thousands of fragments. After 60 years of scholarly research the questions of origin, archaeological provenance and correct attribution of the fragments are still debated. To help address these questions we have developed a methodology suitable to the material studies of the scrolls using combinations of X-ray, FTIR and Raman techniques. On the one hand, an accurate characterization of the highly heterogeneous writing media of the Dead Sea Scrolls leads to a reliable reconstruction of their history and, thus, contributes significantly to the current debate. On the other hand, it provides new information on the production of ancient parchment towards the end of the Second Temple period, opening a new page in the historical study of technology. T2 - Civil and Environmental Engineering Special Seminar CY - Cambridge, UK DA - 17.11.2017 KW - Dead Sea Scrolls PY - 2017 AN - OPUS4-43557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Rabin, Ira ED - Elgvin, T. T1 - Palm fibre tool from cave 11Q. MS 5095/3 N2 - The Schøyen Collection includes a palm fibre object claimed to have come from Cave 11. According to Kando, it was found by the Bedouin together with the Temple Scroll, the Temple Scroll wrapper and minor fragments from 11QTᵃ (MS 5095/1) in the scroll jar that is still the property of William Kando. KW - Dead Sea Scrolls KW - Qumran archaeology PY - 2016 SN - 978-0-5672-8571-3 SN - 978-0-5671-1300-9 VL - 71 SP - 357 EP - 359 PB - Bloomsbury T&T Clark AN - OPUS4-43951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bosch, S. A1 - Colini, C. A1 - Hahn, Oliver A1 - Janke, A. A1 - Shevchuk, I. ED - Friedrich, M. ED - Quenzer, J. ED - Wandrey, I. T1 - The Atri fragment revisited I: Multispectral imaging and ink identification N2 - This paper reports the outcome of an interdisciplinary team’s application of multispectral imaging techniques and material analysis to a music fragment from the first decades of the fifteenth century: Atri, Archivio Capitolare, Museo della Basilica Cattedrale, Biblioteca del Capitolo della Cattedrale, Frammento 17. This important parchment leaf has rarely been investigated since its discovery 45 years ago. Thanks to the applied techniques and methods (such as the evaluation of the data using the fingerprint model), it is now possible to discuss new evidence supporting conclusions regarding the fragment’s origin and afterlife. KW - Archaeometry KW - Cultural heritage KW - Non-destructiv testing PY - 2018 SN - 1867-9617 VL - 2018 IS - 11 SP - 141 EP - 156 PB - Universität Hamburg CY - Hamburg AN - OPUS4-45741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Colini, C. A1 - Hahn, Oliver A1 - Bonnerot, Olivier A1 - Steger, Simon A1 - Cohen, Zina A1 - Ghigo, Tea A1 - Christiansen, T. A1 - Bicchieri, M. A1 - Biocca, P. A1 - Krutzsch, M. A1 - Rabin, Ira ED - Friedrich, M. ED - Quenzer, J. ED - Wandrey, I. T1 - The quest for the mixed inks N2 - In this article, we would like to share our observations concerning the inks produced by intentionally mixing soot or charcoal with tannin extracts or iron-gall ink. Aside from Zerdoun’s mention in her outstanding review of written sources, “Les encres noires au Moyen-Âge”, this ink category has received little if any attention from scholars and scientists. And yet, if analytically attested, the use of such inks could serve as an additional category to classify and distinguish the writing inks on the historical socio-geographic map of the writing inks we are trying to build. KW - Archaeometry KW - Non-destructive testing KW - Inks PY - 2018 SN - 1867-9617 VL - 2018 IS - 11 SP - 41 EP - 48 PB - Universität Hamburg CY - Hamburg AN - OPUS4-45784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nöller, Renate T1 - Untersuchungen der Humboldt Codices "Fragmens de peinture hiéroglyphique Aztèques, deposés à la bibliotheque royale de Berlin" N2 - In der Berliner Sammlung "Manuscripta Americana" befinden sich Fragmente von Bilderhandschriften, die Alexander von Humboldt 1804 in Mexiko erwarb und der Königlichen Bibliothek schenkte. Die in der frühen Kolonialzeit hergestellten verschiedenartigen Codices waren damals schon nicht mehr an den Orten ihrer ursprünglichen Verwendung. Entsprechend ihres Seltenheitswertes gelangten einzelne Schriftstücke seit der Conquista in die Bestände bedeutender Persönlichkeiten. Hierzu fertigte man auch Abschriften oder Kopien an, oder zerstückelte sogar einzelne Blätter, so dass die Darstellungen auf den abgetrennten Fragmenten oft nur zum Teil abgebildet vorliegen. Um herauszufinden, ob einige Schriftstücke der "Humboldt Codices" in Bezug zu einander stehen, werden die Dokumente, ihre Symbole und Schriftzeichen und das zur Herstellung verwendete Material miteinander verglichen. Mit den für die Analyse von Manuskripten bewährten Untersuchungsmethoden werden Papier und Farbmittel identifiziert. Hierzu zählen Raman-, FTIR-, Röntgenfluoreszenz- und VIS- Spektroskopie. Charakteristisch für die Herstellung von schriftlichen Dokumenten in der Kolonialzeit von Amerika ist die Verwendung von indigenem Material wie Papier aus Baumrinde und Pflanzenfarben zusammen mit den aus Europa bekannten Materialien. Geklärt wird, inwieweit neben den bekanntesten Farbstoffen wie Cochenille, Mayablau oder Mischungen mit Tonmineralen auch mineralische Pigmente zum Einsatz kamen. Vorgestellt werden die auf Tafel 36 in den "Vues des Cordillères et Monuments des Peuples Indigènes de l`Amerique, Voyage de Humboldt et Bonpland" abgebildeten Fragmente. Die hier von Humboldt vorgenommene Zusammenstellung wird mit der Farbpalette der in Berlin archivierten originalen Schriftstücke verglichen. Die Interpretation der Ergebnisse gibt einen Hinweis auf die Zuordnung oder auch Zusammengehörigkeit dieser einzigartigen Dokumente amerikanischer Geschichte. Hierbei wird die Frage aufgeworfen, inwiefern davon auszugehen ist, dass diese mit weiteren Fragmenten in Verbindung gebracht werden können, was für die Beleuchtung der kulturhistorischen Zusammenhänge von großer Bedeutung ist. T2 - Archäometrie und Denkmalpflege 2018 CY - Hamburg, Germany DA - 20.03.2018 KW - FTIR KW - Humboldt Codices KW - XRF KW - VIS KW - RAMAN PY - 2018 AN - OPUS4-44746 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier T1 - Scientific service project Z02 at the CSMC: Material-science methods of reconstructing the history of manuscripts N2 - Z02 is one of the three technically supporting projects at the CSMC. In collaboration with Z01 and Z03, it aims at bridging the gap between humanities and natural sciences and technology. To that purpose, we set up a laboratory with a range of high-end instruments, most of them mobile, allowing thorough non-destructive analysis of manuscripts. In addition to working on constantly improving the laboratory and the methods of analysis, a substantial part of our activities is dedicated to service, by supporting different research projects conducted at the center. In this talk, we will present our equipment and the possibilities offered by the different techniques available regarding the different kinds of missions: typology and classification of inks, provenance studies, recovery of faded inscriptions and palimpsests, reconstruction of the history of manuscripts, authentication and dating. We will give a brief overview of our past and ongoing activities in the frame of the second phase of the CSMC. Finally, a selection of three projects will be presented in greater detail to highlight the possibilities of our laboratory and the diversity of missions which can be carried out: - Support of project C08 on East Frankish manuscripts containing collections of formulae - Identifying color materials applied in Muhammad Juki's Shahnamah with non-invasive combined methods - Checking for the presence of metals in the Herculaneum papyri T2 - 3rd International Conference on Natural Sciences and Technology in Manuscript Analysis CY - Hamburg, Germany DA - 13.06.2018 KW - CSMC KW - Manuscript KW - Ink KW - Pigment PY - 2018 AN - OPUS4-45504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon T1 - Development of a methodical approach for in-situ analysis of modern reverse paintings on glass N2 - The technique of painting on the reverse side of glass was rediscovered by artists in the early 20th century and gained great popularity, especially in Germany. In contrast to other paint techniques (e.g. panel and mural painting), the paint layers are applied in reverse succession starting with the foremost paint layer and ending with the primer (backmost layer). The paintings are viewed in reflected light, thus revealing an impressive gloss, luminosity and depth of colour. Scientific investigation of the material provides important information for appropriate conservation concepts. Transport of the precious and fragile objects to the lab is often not feasible. Therefore, in-situ, non-invasive analysis is necessary to analyse colorants and binders. However, some analytical problems need to be considered: due to the reverse paint stratigraphy in reverse paintings on glass, the measured layer is always the backmost one. The analytical possibilities are extremely reduced, when the back is covered by a metal foil (or by paper, carton etc.). However, measurements through the glass (using Raman and VIS) can still yield information on the colourants of the front layer. When the paint layer is accessible, we start our procedure using X-ray fluorescence (Tracer III-SD, Bruker AXS Microanalysis GmbH, 40 kV, 15 μA) and VIS reflectance spectroscopy (SPM 100, Gretag-Imaging AG). Both techniques provide first information on the inorganic colourants. Raman measurements (i-Raman®Plus, Bwtek inc., 785 nm, 50× objective, resolution 4 cm-1) are then carried out to clarify uncertain XRF measurements and to identify synthetic organic pigments (SOP). Diffuse Reflection-Infrared-Fourier-Transform Spectroscopy (DRIFTS; ExoScan, Agilent GmbH, 4000–650 cm-1, 500 scans, spectral resolution 4 cm-1) is used for the classification of the binders. Moreover, it may help to identify SOP, when fluorescence dominates the Raman signal. This analytical sequence yields the best results, when time is the limiting factor. We present two in-situ studies of the paintings “Kreuzabnahme” (1914-15) by Carlo Mense and “Stadt am Morgen” (1921) by Walter Dexel. The painting “Kreuzabnahme” is an outstanding piece in Mense’s ɶuvre, because the glass plate was painted on both sides (Fig. 1). The results of the back-side show mainly inorganic pigments: basic lead white, talc, red and brown ochre, cinnabar, chrome yellow, viridian, ultramarine blue, Prussian blue and bone black. The classification of binding media using DRIFTS yields positive results for drying oil. Acrylic resin could be identified in two areas, resulting from a previous restauration treatment. For the front side painting, Mense used basic lead white, cinnabar, chrome yellow and umbra as pigments and oil as binder. Measurements of the abstract painting “Stadt am Morgen” by Walter Dexel show zinc white, basic lead white, chalk, cinnabar, red lead, strontium yellow, cadmium yellow, cobalt blue, Prussian blue, ultramarine blue, brown ochre and bone black as pigments. Moreover, synthetic alizarin (PR83) was identified as dark red colorant. The results of DRIFTS classify oil as binding media. We conclude that, the use of complementary spectroscopic methods yields the best results for in-situ analysis of reverse paintings on glass. T2 - 3rd International Conference on Innovation in Art Research and Technology CY - Parma, Italy DA - 26.03.2018 KW - Modern painting KW - Non invasive analysis KW - Raman spectroscopy PY - 2018 AN - OPUS4-44780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon T1 - In-situ Raman spectroscopic study of pigments used in modern reverse paintings on glass N2 - The technique of painting on the reverse side of glass was rediscovered by artists in the early 20th century. The artist group “Der Blaue Reiter” around Wassily Kandinsky and Franz Marc got in touch with this technique in 1908 and 1909. In the following years it gained great popularity, especially in Germany. Nevertheless, the technique has not received its due appreciation in art history. It was considered as stained glass. However, the paint layers are applied cold, hence this artistic technique doesn’t involve a firing step. Our multidisciplinary project investigates the art historic backgrounds, the painting techniques and materials of modern reverse paintings on glass. More than 1000 paintings from ~100 artists were discovered in the framework of our project. A selection of 60 paintings could be analyzed using non-invasive, in-situ methods such as Raman and VIS spectroscopy, Diffuse Reflectance Fourier Transform Infrared Spectroscopy (DRIFTS) and X-ray fluorescence (XRF). In this paper we want to point out the key role of Raman spectroscopy for our research. It offers the unique opportunity to measure paint layers from both sides. (front = through the glass; reverse = directly on the paint layer). T2 - XIII International GeoRaman Conference CY - Catania, Italy DA - 10.06.2018 KW - Raman spectroscopy KW - Reverse painting on glass KW - Non-invasive analysis PY - 2018 AN - OPUS4-45400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nöller, Renate T1 - Analyses of pigments, paints and inks from silk road sites N2 - One of the most important collections of manuscripts and wall paintings from sites of the northern Silk Road, discovered at the beginning of the 20thC, are deposited in Berlin. The fragments represent a broad spectrum of scripts, languages, and painting styles depending on the region of origin and purpose of dissemination. The manufacturing material reflects the various influences in the oasis sites. Based on analyses of some pigments, examples are posed. T2 - TechnArt 2015 CY - Catania, Italy DA - 27.04.2015 KW - Pigments KW - Analyses of inks KW - Silk Roas Sites KW - Wall paint PY - 2015 AN - OPUS4-44793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nöller, Renate T1 - The writing materials of the Silk Road book cultures in Turfan – Analysis of inks and pigments N2 - Manuscript fragments discovered in the oasis of Turfan and in other sites of present-day China in the beginning of the 20th century by A. Grünwedel and A. von Le Coq, represent one of the most fascinating cultural testimonies of people who both lived there and travelled along the trade routes between East and West. To determine the different materials used for writing and painting the Chinese, Sanskrit, Manichaean, Syrian, Sogdian, Tocharian and Uighur fragments of the Berlin collection, analysis of inks and pigments were conducted using non-destructive methods. The research was funded by the German Research Foundation DFG for a period of three years. The identification of specific techniques of preparation allows manuscript groups and sub-groups to be specified, aiding their cultural assignment. This is important for further cultural studies, for the development of conservation strategies and the identification of forgeries. T2 - European Cultural Heritage Research and Innovation “Zukunftsort EUROPA” CY - British Embassy in Berlin, Germany DA - 15.09.2014 KW - XRF-analyses KW - Ink analyses KW - Turfan manuscripts PY - 2014 AN - OPUS4-44787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heiles, M. A1 - Rabin, Ira A1 - Hahn, Oliver ED - Friedrich, M. ED - Quenzer, J. ED - Wandrey, I. T1 - Palaeography and X-ray fluorescence spectroscopy: Manuscript production and censorship of the fifteenth century German manuscript Cod. germ. 1 of the Staats- und Universitätsbibliothek Hamburg N2 - The manuscript Codex germanicus 1 (Cod. germ. 1) of the Staats- und Universitätsbibliothek Hamburg is a fifteenth-century German-language manuscript. It comprises two codicological units and has an especially complex developmental history. To trace this developmental history, neglected until now in the research literature, the manuscript was investigated, for the first time not solely with classical codicological and palaeographical methods, but also with the aid of X-ray fluorescence spectroscopy, in order to determine the composition of the writing materials. These methods made it possible, first, to support and check palaeographic findings and, second, to gain information about the stratigraphy of the manuscript where palaeographic methods find their limits – in regard to short entries, rubrications, and non-alphabetical signs. KW - Archaeometry KW - Non-destructive testing KW - Inks PY - 2018 SN - 1867-9617 VL - 2018 IS - 11 SP - 109 EP - 132 PB - Universität Hamburg CY - Hamburg AN - OPUS4-45818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geissbühler, M. A1 - Dietz, G. A1 - Hahn, Oliver A1 - Rabin, Ira ED - Friedrich, M. ED - Quenzer, J. ED - Wandrey, I. T1 - Advanced codicological studies of Cod. germ. 6 (Hamburg, Staats- und Universitätsbibliothek): Part 2 N2 - The work presented here follows the article Combining Codicology and X-Ray Spectrometry to Unveil the History of Production of Codex germanicus 6 (Staats- und Universitätsbibliothek Hamburg), published in 2014.1 It confirms the main result of the previous article: the Artusnotiz, the fourth text in the bound manuscript, must have been introduced as the last one. This paper offers further details of the codex production, based on the composition of the black and red inks collected in four measurement campaigns. Furthermore, using imaging μ-XRF, we succeeded in understanding the strong variation of the composition of the red inks in the initials of all the texts except for Parzival and Jeanne d’Arc. KW - Archaeometry KW - Non-destructive testing KW - Inks PY - 2018 SN - 1867-9617 VL - 2018 IS - 11 SP - 133 EP - 139 PB - Universität Hamburg CY - Hamburg AN - OPUS4-45816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghigo, Tea A1 - Bonnerot, Olivier A1 - Buzi, P. A1 - Krutzsch, M. A1 - Hahn, Oliver A1 - Rabin, Ira ED - Friedrich, M. ED - Quenzer, J. ED - Wandrey, I. T1 - An Attempt at a Systematic study of inks from Coptic manuscripts N2 - It is well documented that throughout Antiquity, ancient Egyptians used mostly carbon inks as a writing material. In Late Antiquity, some metals started to be added to carbon based inks. We have records of five manuscripts from the Dead Sea Scrolls collection whose carbon inks were found to contain copper Also, lead was recently found as an additive in carbon inks on a charred fragment from Herculaneum. Furthermore, the earliest evidence of iron-gall ink was found in the Book of Proverbs (Codex Ms. Berol. orient. oct. 987) dating to the third fourth centuries ce. It has been suggested that along with carbon and iron-gall inks, there is no reason to think that purely tannin inks were not also in use in Egypt. However, so far, we just have evidence of a copper-tannin ink identified in a number of documents from Egypt in the first third centuries bce. In an attempt to fill this gap in this extremely fragmented scenario during our studies of the socio-geographic history of inks, we arrived at the conclusion that the continuous production of Coptic manuscripts from Late Antiquity to the Middle Ages offers a unique opportunity for the historical study of inks across a large geographic area. KW - Archaeometry KW - Non-destructive testing KW - Inks PY - 2018 SN - 1867-9617 VL - 2018 IS - 11 SP - 157 EP - 163 PB - Universität Hamburg CY - Hamburg AN - OPUS4-45817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghigo, Tea T1 - Understanding the technological evolution of writing materials. Scientific systematic study of inks from Coptic manuscripts N2 - While studying the socio-geographic history of inks, division 4.5 of the BAM (Bundesanstalt für Materialforschung und Prüfung) together with the Centre for the Study of Manuscript Cultures in Hamburg has developed a protocol for ink analysis. It consists of a primary screening to determine the type of the ink and a subsequent in-depth analysis using several spectroscopic techniques: XRF, FTIR, and Raman. In most cases, we can obtain satisfactory results using a non-invasive protocol. However, mixed inks that contain no metals evade such a protocol. These inks constitute a heterogeneous group of media used especially in the Middle East and the Islamicate world since at least the 10th century; they are characterized by blending carbon ink and tannins, with or without the addition of vitriol. Our own research aims primarily at recreating a socio-geographic history of inks, parchment, and papyrus and includes the comparative analysis of the writing materials of the Dead Sea Scrolls, ink and papyrus in Ancient and Hellenistic Egypt, and inks in documents from various contemporary medieval communities in Fustat (first nucleus of Cairo). During many years of study, we concluded that the continuous production of Coptic manuscripts from late Antiquity to the Middle Ages offers a unique opportunity for historical study of the ink in a large geographic area. Thanks to the collaboration with the ERC project “PAThs” (www.paths.uniroma1.it), based at the University of Rome La Sapienza, and within the activities of a PhD research dedicated to this topic, we therefore created a new branch of our project focused entirely on the analysis of Coptic inks, pigments, and dyes. This pioneering systematic study of writing materials coming from a specific area and time frame (5th-10th century) aims not only at a better understanding of the complex Coptic multicultural and plurilingual society, but also and mainly at clarifying the links among the Coptic and other societies between the ancient and medieval eras. Finally, it will cast light on the history of the technological development of inks in the eastern world, from Antiquity to the middle ages. T2 - Konferenz: Scientific Methods in Cultural Heritage Research, Gordon Research Conference CY - Castelldefels, Spain DA - 22.07.2018 KW - Coptic KW - Ink KW - Manuscript PY - 2018 AN - OPUS4-46024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ghigo, Tea T1 - Comprehensive analysis of manuscripts. Systematic study of Coptik inks N2 - While studying the socio-geographic history of inks, division 4.5 of the BAM (Bundesanstalt für Materialforschung und Prüfung) together with the Centre for the Study of Manuscript Cultures in Hamburg has developed a protocol for ink analysis. It consists of a primary screening to determine the type of the ink, and a subsequent in-depth analysis using several spectroscopic techniques. The XRF elemental analysis aims primarily at understanding the fingerprints of inks containing metals, making it possible to distinguish among different inks. Our own research aims primarily at recreating a socio-geographic history of inks, parchment, and papyrus and includes the comparative analysis of the writing materials of the Dead Sea Scrolls, ink and papyrus in Ancient and Hellenistic Egypt, and inks in documents from various contemporary medieval communities in Fustat (first nucleus of Cairo). During many years of study, we concluded that the continuous production of Coptic manuscripts from late Antiquity to the Middle Ages offers a unique opportunity for historical study of the ink in a large geographic area. Thanks to the collaboration with the ERC project “PAThs” (www.paths.uniroma1.it), based at the University of Rome La Sapienza, and within the activities of a PhD research dedicated to this topic, we therefore created a new branch of our project focused entirely on the analysis of Coptic inks, pigments, and dyes. This pioneering systematic study of writing materials coming from a specific area and time frame (5th-10th century) aims not only at a better understanding of the complex Coptic multicultural and plurilingual society, but also and mainly at clarifying the links among the Coptic and other societies between the ancient and medieval eras. Finally, it will cast light on the history of the technological development of inks in the eastern world, from Antiquity to the middle ages. T2 - 7th Meeting 'X-ray and other techniques in investigations of the objects of cultural heritage' CY - Cracow, Poland DA - 17.05.2018 KW - Coptic KW - Ink KW - Manuscript PY - 2018 AN - OPUS4-46025 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cohen, Zina A1 - Kindzorra, Emmanuel A1 - Hahn, Oliver A1 - Glaser, L. A1 - Łojewski, T. A1 - Rabin, Ira T1 - Composition of the primary inks in medieval palimpsests – effects of ink removal N2 - The qualitative and quantitative investigations of historical iron-gall inks by use of μ-XRF spectrometry is a common method for analyzing the diff erences in their composition. When a fingerprint is established, it is possible to characterize the distinguishable inks used in the production of medieval manuscripts, and, in turn assist in the reconstruction of the manuscript’s history.The characterization of the primary inks in palimpsests, i.e. manuscripts written on re-used parchment, presents a serious problem as the effect of the partial removal on the inks fi ngerprint is yet known. In this paper we explore our preliminary results concerning the effects of two removal techniques on the fingerprint of iron-gall inks on parchment. KW - Palimpsests KW - Iron-gall ink KW - XRF PY - 2015 DO - https://doi.org/10.4467/20843852.OM.15.007.5385 SN - 0239-9989 VL - 23 SP - 75 EP - 82 AN - OPUS4-46130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cohen, Zina T1 - Composition analysis of writing materials in Geniza fragments N2 - The Cairo Geniza is an “archive” discovered in the 19th century in Ben Ezra Synagogue in Fustat, a district in Old Cairo (Egypt), located south of the center of modern Cairo. The giant collection of mostly Jewish documents that vary in genres, languages and writing supports contains a large number of early medieval Hebrew manuscripts, mostly in fragmentary form. The larger part of the Cairo Geniza is stored today in the Cambridge University Library (CUL). The Geniza provides sources for the literary, linguistic, historical studies of the various aspects Jewish life. As the documents attest, at least two Jewish communities co-existed in Fustat up to 11th century: a so-called Babylonian and Palestinian. These communities had different leaders, different traditions and lived independently. The differences seem to manifest themselves also in the paleographical, codicological and some material properties of the manuscripts produced by each community. The aim of this project is to compare the inks used in the Jewish documents depending on different variables: support (paper, parchment), purpose of the manuscript (legal, private, religious), provenance of the scribe. For the determination of the inks type and composition we had to choose non-invasive, non-destructive and portable techniques to analyse the corpus directly in the CUL. The analyses were carried out with a mobile energy dispersive micro-X-ray spectrometer ArtTAX® (Bruker GmbH, Berlin, Germany), which consists of an air-cooled, low-power molybdenum tube, polycapillary X-ray optics (measuring spot size 70 µm in diameter), an electrothermally cooled Xflash detector, and a CCD camera for sample positioning (Bronk et al 2001, Hahn et al. 2010). All measurements are executed using a 30 W low-power Mo tube, 50 kV, 600 µA Mo tube, and with an acquisition time of 15 s (live time) to minimize the risk of damage (Fig. 1, 2). Fig. 1: XRF spectrometer probe above a manuscript fragment Fig. 2: Typical element profile of a XRF linescan The Dino Lite digital stereomicroscope (Fig. 3) features built-in LED illumination at 395 nm and 940 nm and a customized external white light source. During use, the microscope is fastened to a small tripod or mounted on a Plexiglas ring holder that incorporates a white light source. Fig. 3: Dino Lite digital stereomicroscope Fig. 4: Details of one fragment (T-S 16.124) observed with the Dino microscope (x20). On the left, when illuminated with NIR (Near-Infrared, 940 nm) light, the ink fades, indicating iron-gall ink. On the right, the image under NIR light does not change. It is carbon ink. On example of these studies is the manuscript T-S 16.124 (Cambridge University Library, Fig. 5) whom belongs to the third corpus. It is a deed, written in Hebrew, dated from 1328 (= 1017 CE) and witnessed by a very high number of people (6) comparing to the standard of similar documents (between 2 and 3), from at least two different Jewish communities in Fustat (trans congregational). The verso is written in Arabic (Bareket 1999). Fig. 5: Manuscript T-S 16.124 (Cambridge University Library) To compare the inks, we used the fingerprint model. This method relies on the determination of characteristic elemental compositions and represents the amount of a minor constituent relative to the main component, iron in iron gall ink (Malzer et al. 2004, Hahn et al. 2004, Rabin et al 2014). However, a calculation of a fingerprint based on XRF measurements is not possible in the case of carbon ink since carbon, its main component, cannot be detected with this technique. Fig. 6: Ink fingerprint T-S 16-124 (recto) normalized to iron (Fe) Conclusion We show that using reflectography and XRF analysis it is possible to sort the inks according to their type. In the case of the iron-gall inks, use of the ink fingerprint, i.e. amount of the vitriol components normalized to iron we can make direct comparisons of the ink composition. We would like also to stress that though the methods of material analysis listed above have been successfully employed in the field of cultural heritage and conservation including ancient and medieval manuscripts they have not yet been used to study fragments from the Cairo Genizah. Therefore, we believe that this research project is a pioneering study that will provide new insights into the history of Hebrew writing materials, their production techniques and materials and, thus, contribute new data to the field of Hebrew paleography. T2 - Konferenz DESY “Archäometrie und Denkmalpflege 2018” CY - Hamburg, Germany DA - 20.03.2018 KW - Ink KW - XRF Analysis KW - Manuscript PY - 2018 AN - OPUS4-46042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon T1 - In-situ spectroscopic analysis of modern reverse paintings on glass (1905-1955) N2 - The technique of painting on the reverse side of a glass panel was rediscovered by German artists at the beginning of the 20th century. In contrast to other paint techniques (e.g. panel and mural painting), the paint layers are applied in reverse succession starting with the foremost paint layer and ending with the primer (backmost layer). The paintings are viewed in reflected light, thus revealing an impressive gloss, luminosity and depth of colour. The artist group “Der Blaue Reiter” (the Blue Rider) around W. Kandinsky and F. Marc got in touch with this technique in the summers of 1908 and 1909 and spread their knowledge in different regions. Our pioneering project is tracing this transfer of knowledge by a multidisciplinary approach in terms of art history, painting technology and material science. More than 100 artists and >1000 reverse paintings on glass (1905-1955) were identified during the project. This numbers clearly point out that this technique was by far more important for modern art than previously assumed. In-situ, non-invasive measurements (XRF, Raman, VIS, DRIFTS) on a well-considered selection of 67 paintings reveal the broad palette of colorants ranging from traditional to experimental materials. Special attention is paid on artists who are strongly connected to Berlin. Demonstrative examples by W. Dexel, G. Muche and L. Hildebrandt are used to discuss analytical challenges and highlights. T2 - Young Researchers in Archaeometry (YRA) 2nd Workshop CY - Berlin, Germany DA - 23.09.2018 KW - Raman spectroscopy KW - DRIFTS KW - Reverse glass painting PY - 2018 AN - OPUS4-46066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cohen, Zina T1 - Ink analysis in Cairo Geniza fragments N2 - The Cairo Geniza is an “archive” discovered in the 19th century in Ben Ezra Synagogue in Fustat, a district in Old Cairo (Egypt), located south of the center of modern Cairo. The giant collection of mostly Jewish documents that vary in genres, languages and writing supports contains a large number of early medieval Hebrew manuscripts, mostly in fragmentary form. The larger part of the Cairo Geniza is stored today in the Cambridge University Library. The Geniza provides sources for the literary, linguistic, historical studies of the various aspects Jewish life. As the documents attest, at least two Jewish communities co-existed in Fustat up to 11th century: a so-called Babylonian and Palestinian. These communities had different leaders, different traditions and lived independently. The differences seem to manifest themselves also in the paleographical, codicological and some material properties of the manuscripts produced by each community. My work addresses the ink composition in the documents attributed to the members of these communities. For the determination of the inks type and composition I employ reflectography and µ-XRF spectrometry, respectively. The preliminary typological studies indicate that iron-gall inks were found predominantly in the manuscripts attributed to the Palestinian community. T2 - Konferenz WCJS CY - Jerusalem, Israel DA - 06.08.2017 KW - Ink KW - Manuscript KW - XRF analysis PY - 2017 AN - OPUS4-46041 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cohen, Zina T1 - Analysis of writing materials in Genizah fragments written during the first half of the XIth century N2 - My doctoral dissertation in progress focuses on ink composition on some fragments found in the Cairo Genizah and written by the leaders of the Jewish communities in Fustat during the first half of the XIth century. This is a project at the intersection of historical (Hebrew paleography) and scientific (physics, chemistry and materials science) disciplines. Indeed, I’m analyzing the corpus I constituted (written by Ephraim ben Shemarya and Yephet ben David from the Palestinian congregation and Elhanan ben Shemarya, Abraham ben Sahlan and Sahlan ben Abraham from the Babylonian community). The interests of such a study are numerous: provide insights on trade, local technologies, and social structures. If sufficient data is collected, the tabulated results have the potential for use as an indirect geochronological marker, in particular in the case of iron-gall ink. The composition of the vitriol used for the iron-gall ink preparation depends on the place of extraction. While attributing the vitriol used to a specific source of extraction is seldom possible, a number of origins can be excluded thanks to such analysis. Though ink composition alone cannot be used as a direct geochronological marker, superposition of chemical, palaeographical, codicological, and textual data would help to date and localize and serve as an additional argument for a typology and dating of other Hebrew scripts. T2 - Konferenz EAJS Summer Laboratory for Young Genizah Researchers and those Interested in the Field CY - Munich, Germany DA - 06.09.2017 KW - XRF Analysis KW - Archaeometry KW - Medieval Jewish manuscripts KW - Cairo Genizah PY - 2017 AN - OPUS4-46128 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bhatia, S. A1 - Donskyi, Ievgen A1 - Block, S. A1 - Nie, C. A1 - Burdinski, A. A1 - Lauster, D. A1 - Radnik, Jörg A1 - Herrmann, A. A1 - Haag, R. A1 - Ludwig, K. A1 - Adeli, M. T1 - Wrapping and Blocking of Influenza A Viruses by Sialylated 2D Nanoplatforms N2 - Inhibition of respiratory viruses is one of the most urgent topics as underlined by different pandemics in the last two decades. This impels the development of new materials for binding and incapacitation of the viruses. In this work, we have demonstrated that an optimal deployment of influenza A virus (IAV) targeting ligand sialic acid (SA) on a flexible 2D platform enables its binding and wrapping around IAV particles. A series of 2D sialylated platforms consisting graphene and polyglycerol are prepared with different degrees of SA functionalization around 10%, 30%, and 90% named as G-PG-SAL, G-PG-SAM, and G-PG-SAH, respectively. The cryo-electron tomography (Cryo-ET) analysis has proved wrapping of IAV particles by G-PG-SAM. A confocal-based colocalization assay established for these materials has offered the comparison of binding potential of sialylated and non-sialylated nanoplatforms for IAV. With this method, we have estimated the binding potential of the G-PG-SAM and G-PG-SAH sheets for IAV particles around 50 and 20 times higher than the control sheets, respectively, whereas the low functionalized G-PG-SAL have not shown any significant colocalization value. Moreover, optimized G-PG-SAM exhibits high potency to block IAV from binding with the MDCK cells. KW - 2D Materials KW - Graphhene KW - Influenza A virus KW - Sialic acid KW - wrapping PY - 2021 DO - https://doi.org/10.1002/admi.202100285 VL - 8 IS - 12 SP - 285 PB - Wiley VCH AN - OPUS4-52715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hülagü, Deniz A1 - Ermilova, Elena A1 - Weise, Matthias A1 - de Préville, Sophie A1 - Hoffmann, Johannes A1 - Morán-Meza, José A1 - Piquemal, Francois A1 - Hertwig, Andreas T1 - Characterization of electrical properties in microstructured ITO layers using spectroscopic ellipsometry N2 - Thin indium tin oxide (ITO) layers are essential in optoelectronics due to their good electrical conductivity, optical transparency in the visible and near infrared regions, substrate adherence and chemical stability. They are widely used in photovoltaic cells, displays, and organic LEDs, and as low emissivity coatings in smart windows and energy-efficient buildings. For nanophotonic devices, understanding the interplay of ITO’s optical and electrical properties is crucial. Electrical resistivity can be tuned by modifying deposition conditions and layer thickness. However, measuring these properties, especially on microstructured surfaces, remains challenging due to the issues like homogeneity and instability during etching. Spectroscopic ellipsometry (SE), a non-destructive and phase-sensitive optical technique, offers precise measurement of thin film thickness and dielectric properties. In this study, we investigated the layer thickness, optical constants, and sheet resistance of unstructured and microstructured ITO thin layers using SE. Unstructured layers were deposited via DC-magnetron sputtering on silicon (Si) substrates in argon (Ar) atmospheres with varying oxygen (O2) flows. This multi-technique approach enhances the understanding of ITO layer structuring and provides robust methodologies for correlating optical and electrical properties, advancing metrology for nanotechnology applications and material science. It also opens the pathway to new reference samples and calibration methods for electrical properties involving device-like structured samples. T2 - ICSE10 - 10th International Conference on Spectroscopic Ellipsometry CY - Boulder, CO, USA DA - 08.06.2025 KW - Ellipsometry KW - Indium tin oxide (ITO) KW - Scanning microwave microscopy (SMM) KW - Sheet resistance calibration standards KW - ITO wet etching PY - 2025 AN - OPUS4-63631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hülagü, Deniz A1 - Hirahara, Kenta A1 - Fischer, Daniel A1 - Florian, Camilo A1 - Schusterbauer, Robert A1 - Ermilova, Elena A1 - Krüger, Jörg A1 - Unterreiner, Andreas-Neil A1 - Bonse, Jörn A1 - Hertwig, Andreas T1 - Using imaging ellipsometry to understand femtosecond laser materials processing of group IV materials N2 - Laser materials processing is an important tool for creating and shaping new materials. Laser machining, especially with ultrashort pulses offers the modification of surfaces, thin coatings, and bulk materials with an unprecedented precision and control. The most desired feature of pulsed laser processing in the femtosecond range is that the heat-affected zone in the irradiated material will be extremely small. To better understand the mechanisms involved during laser irradiation, it is important to analyse the outcome of light-matter interaction with spectroscopic methods. Ellipsometry, especially spectroscopic imaging ellipsometry (SIE), has become an important tool for this in recent times, as it gives access to local layer thicknesses, materials dielectric functions, and features like changes in surface roughness. This work includes an overview over our recent studies examining near-infrared fs-laser surface processing of different group IV materials. The superficial phase change of silicon from crystalline to amorphous has been investigated in the past as the result of laser processing strongly depends on the crystal orientation. Moreover, SIE is capable of determining the properties of buried a-Si interfaces with micrometer lateral and sub-nanoneter vertical precision. Additionally, the growth of native and laser-induced oxides can be revealed. T2 - ICSE10 - 10th International Conference on Spectroscopic Ellipsometry CY - Boulder, CO, USA DA - 08.06.2025 KW - Laser surface ablation KW - Amorphous Carbon KW - Silicon KW - Correlative Imaging Ellipsometry PY - 2025 AN - OPUS4-63633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hajhariri, Aliasghar ED - Eberwein, Robert ED - Perrone, Luca pakj ED - Cozzani, Valerio ED - Otremba, Frank ED - Seidlitz, Holger T1 - Study the Impact of Spacer at Thermal Degradation Process of MLI-based Insulation in Fire Condition N2 - To reduce carbon dioxide emissions, energy carries such as hydrogen consider to be a solution. Consumption of hydrogen as a fuel meets several restrictions such as its low volumetric energy density in gas phase. To tackle this problem, storage as well as transportation in liquid phase is recommended. To be able to handle this component in liquid phase, an efficient thermal insulation e.g., MLI insulation is required. Some studies have been revealed vulnerability of this type of insulation against high heat flux, for instance a fire accident. Some investigations have been depicted the importance of consideration of the MLI thermal degradation in terms of its reflective layer. However, limited number of studies have been focused on the thermal degradation of spacer material and its effect on the overall heat flux. In this study, through systematic experimental measurements, the effect of thermal loads on glass fleece, glass paper as well as polyester spacers are investigated. The results are reported in various temperature and heat flux profiles. Interpreting the temperature profiles revealed as the number of spacers in the medium increases, the peak temperature detectable by the temperature sensor on the measurement plate decreases. Moreover, the contribution of each individual spacer in all cases regarding the experimental temperature range is assessed to be around 8%. This value may increase to around 50% for glass paper and polyester spacers, and to around 25% for glass fleece spacers as the number of spacer layers increases up to six layers. To utilize the outcomes of the experiment later and integrate the results into numerical and CFD simulations, a model is proposed for the mentioned experimental temperature range up to 300°C to predict a heat flux attenuation factor. The model proposes a fitting factor that can reproduce the least square fitted line to the experimental data. T2 - 15th International Symposium on Hazards, Prevention, and Mitigation of Industrial Explosions Naples (ISHPMIE) CY - Naples, Italy DA - 10.06.2024 KW - Multi-Layer Insulation KW - Cryogenics KW - Liquid Hydrogen KW - Heat Transfer KW - Hydrogen Storage PY - 2024 SP - 744 EP - 755 AN - OPUS4-60461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hajhariri, Aliasghar T1 - Experimental and Numerical Investigation on Multi-layer Insulation Thermal Deterioration N2 - To reduce carbon dioxide emissions, energy carries such as hydrogen consider to be a solution. Consumption of hydrogen as a fuel meets several restrictions such as its low volumetric energy density in gas phase. To tackle this problem, storage as well as transportation in liquid phase is recommended. To be able to handle this component in liquid phase, an efficient thermal insulation e.g., MLI insulation is required. Some studies have been revealed vulnerability of this type of insulation against high heat flux, for instance a fire accident. Some investigations have been depicted the importance of consideration of the MLI thermal degradation in terms of its reflective layer. However, limited number of studies have been focused on the thermal degradation of spacer material and its effect on the overall heat flux. In this study, through systematic experimental measurements, the effect of thermal loads on glass fleece, glass paper as well as polyester spacers are investigated. The results are reported in various temperature and heat flux profiles. Interpreting the temperature profiles revealed as the number of spacers in the medium increases, the peak temperature detectable by the temperature sensor on the measurement plate decreases. Moreover, the contribution of each individual spacer in all cases regarding the experimental temperature range is assessed to be around 8%. This value may increase to around 50% for glass paper and polyester spacers, and to around 25% for glass fleece spacers as the number of spacer layers increases up to six layers. To utilize the outcomes of the experiment later and integrate the results into numerical and CFD simulations, a model is proposed for the mentioned experimental temperature range up to 300°C to predict a heat flux attenuation factor. The model proposes a fitting factor that can reproduce the least square fitted line to the experimental data. T2 - 15th International Symposium on Hazards, Prevention, and Mitigation of Industrial Explosions Naples (ISHPMIE) CY - Naples, Italy DA - 10.06.2024 KW - Multi-Layer Insulation KW - Cryogenic KW - Liquid Hydrogen KW - Heat Transfer KW - Hydrogen Storage PY - 2024 AN - OPUS4-60457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Konthur, Zoltán T1 - Enzyme-Based Electrochemical Detection of Fumonisins Applying Amperometric Sensing N2 - Fumonisins represent a class of toxic secondary metabolites produced primarily by Fusarium species, notably F. verticillioides and F. proliferatum, though Aspergillus niger can also produce these mycotoxins. They are most commonly found contaminating maize, but other grains are also at risk. Dietary exposure to fumonisins poses serious health risks to both humans and livestock, prompting the European Commission to set regulatory limits on their presence in food and animal feed. Traditional detection methods, such as chromatography, are often costly, are laboratory based and require specialized expertise. To address the need for simpler, more accessible detection methods, portable electrochemical biosensors present a promising solution. In this study, we introduce a novel enzymatic approach for fumonisin detection using amperometric sensing. Here, a recently discovered fumonisin amine oxidase (AnFAO) from Aspergillus niger, which catalyses the oxidative deamination of fumonisins and generates hydrogen peroxide, was produced recombinantly in Escherichia coli. In our hands, the enzyme exhibited higher specific activity toward Fumonisin B1 compared to Fumonisin B2 at the same substrate concentration (0.0037 U/mg and 0.0014 U/mg at 25 µM substrate, respectively). We demonstrated that enzyme activity correlates with both enzyme and substrate concentrations. To detect Fumonisin B1, the enzyme was covalently attached to magnetic particles, and hydrogen peroxide production was measured amperometrically in a flow injection system with Prussian blue carbon electrodes. This method enabled the quantification of Fumonisin B1 concentrations as low as 1.5 µM and proved that recombinant AnFAO effectively deaminated fumonisins even in its immobilized form. These results highlight AnFAO’s potential for developing an enzyme-based electrochemical biosensor to detect fumonisin contamination in food and feed products. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Immunoassay KW - Mycotoxin KW - Electrochemistry KW - Antibody KW - Biosensor PY - 2025 AN - OPUS4-63496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel T1 - Imaging of Hydrogen in Steels with Neutrons N2 - Cold neutrons are predominantly scattered at hydrogen when penetrating hydrogen-charged samples, resulting in a high image contrast between hydrogen and e.g. iron. The used radiographic set-ups consist of a neutron source, state-of-the-art scintillator screens and digital cameras. This allows monitoring diffusive hydrogen fluxes two-dimensionally with 20s temporal resolution. Such hydrogen fluxes can be quantified by using standards with known hydrogen content and similar sample thickness. Neutron tomography generates three-dimensional models of the hydrogen distribution in steel. Such models gain new insight for damage analysis by showing the hydrogen accumulations around cracks and by enabling the hydrogen gas pressure estimation inside cracks. The capabilities and limitations, as well as perspectives of this method will be discussed and illustrated with help of selected examples. T2 - MS&T 2016 CY - Salt Lake City, Utah, USA DA - 23.10.2016 KW - Hydrogen embrittlement KW - Neutron imaging KW - Neutron radiography KW - Neutron tomography PY - 2016 AN - OPUS4-38066 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Quantitative chemichal depth-profiling by synchrotron-radiation-XPS N2 - Synchrotron-radiation enables the adjustment of the XPS information depth and, thus, the visualization of depth profiles of the elemental composition within the first 10 nm of a surface. This project deals with the analysis of core-shell nanoparticles. It constitutes first steps towards a valid methodology for studying the surface chemistry of nanoparticles in a quantitative and accurate manner. T2 - Eighth Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 07.12.2016 KW - XPS KW - Synchrotron KW - Depth-profiling KW - Core@Shell Nanoparticles PY - 2016 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-38782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Griesche, Axel T1 - Real-time X-ray Radiography for Hot Crack Detection during Welding N2 - Fast digital radiography was used to observe the crack development during single pass bead-on-plate gas tungsten arc welding with a minifocus X-ray source and a digital detector array with 75-micrometer pixel size. The sample material were 5 mm thick AlMgSi plates. An acquisition rate of 12 frames per second and an exposure time of 40 ms per frame were used for real-time observation of the hot crack propagation during welding. The basic spatial resolution of the images is about 80 µm. A 3D laminographic reconstruction of the acquired 2D radiographic images gives access to the volumetric extent of the cracks in the welded sample. The parallel use of a high-speed camera during welding allows the real-time inspection of surface cracks. The development of surface cracks was compared with the crack’s distribution in the sample volume and these results were correlated to the used welding parameters. T2 - MS&T 2016 CY - Salt Lake City, Utah, USA DA - 23.10.2016 KW - X-ray radiography KW - Welding KW - Hot crack KW - X-ray imaging KW - Laminography PY - 2016 AN - OPUS4-38069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gatla, S. A1 - Mathon, O. A1 - Rogalev, A. A1 - Pascarelli, S. A1 - Radnik, Jörg A1 - Pohl, M.-M. A1 - Brückner, A. T1 - Influence of Sb on the structure and performance of Pd-based catalysts: An X-ray spectroscopic study N2 - Combined X-ray photoelectron and absorption fine spectroscopy (XAFS) investigations on 10 wt % Pd–16 wt % Sb/TiO2 catalyst allow new insight into the impact of the co-component Sb on the active Pd species, which catalyzes the gas-phase acetoxylation of toluene to benzyl acetate. Ex situ Pd 3d XPS and Pd L-edge XANES studies indicate the presence of an excess electron charge on metallic Pd species (more 4d electrons than in Pd metal) formed after several hours of stream. This observation was explained by the electron transfer from metallic Sb incorporated into the Pd bulk to the neighboring Pd atoms. TEM-EDX analysis confirms the presence of intermixed Pd–Sb particles with an atomic ratio of between 5 and 6 in the most active catalysts and of 3 in deactivated samples. In situ Sb-K-edge XAFS investigations provide evidence that the Pd–Sb interaction is more pronounced under reaction feed than in the ex situ samples. KW - X-ray spectroscopy KW - Catalysis KW - Alloying / Intermixing PY - 2017 DO - https://doi.org/10.1021/acs.jpcc.6b10932 SN - 1932-7447 VL - 121 IS - 7 SP - 3854 EP - 3861 PB - American Chemical Society AN - OPUS4-39231 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Synchrotron radiation as a tool in applied catalytic research N2 - Synchrotron Radiation with its high intensity and the opportunity to tune the wavelength offers unique possibilities to investigate real catalysts, even under industry-like conditions. A good example is a XAFS study performed at supported Ni catalysts used for the dimerization of butene at elevated temperature and pressure. Another example are investigations at titania supported Pd based catalyst elucidating the role of co-components (e.g. Sb, Co, Mn and Au) which are necessary to get the desired promising performance in the gas phase acetoxylation of toluene to benzyl acetate, an environmentally benign alternative for the conventional process using chlorine. Furthermore, investigations about the redox properties of different Cu catalysts will be presented. It could be shown that the redox properties of Cu have a great impact on the performance of such catalysts, not only in some gas phase reactions, but also in photocatalytic applications, e.g. water splitting. T2 - EMIL Seminar CY - Berlin, Germany DA - 23.01.2017 KW - Catalysis KW - Synchrotron radiation KW - Nanochemistriy PY - 2017 AN - OPUS4-39026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernegger, Raphael A1 - Altenburg, Simon A1 - Roellig, Mathias A1 - Maierhofer, Christiane T1 - Applicability of a 1D analytical model for pulse thermography of laterally heterogeneous semitransparent materials N2 - Pulse thermography (PT) has proven to be a valuable non-destructive testing method to identify and quantify defects in fiber-reinforced polymers. To perform a quantitative defect characterization, the heat diffusion within the material as well as the material parameters must be known. The heterogeneous material structure of glass fiber-reinforced polymers (GFRP) as well as the semitransparency of the material for optical excitation sources of PT is still challenging. For homogeneous semitransparent materials, 1D analytical models describing the temperature distribution are available. Here, we present an analytical approach to model PT for laterally inhomogeneous semitransparent materials.We show the validity of the model by considering different configurations of the optical heating source, the IR camera, and the differently coated GFRP sample. The model considers the lateral inhomogeneity of the semitransparency by an additional absorption coefficient. It includes additional effects such as thermal losses at the samples surfaces, multilayer systems with thermal contact resistance, and a finite duration of the heating pulse. By using a sufficient complexity of the analytical model, similar values of the material parameters were found for all six investigated configurations by numerical fitting. KW - Absorption coefficient KW - Analytical model KW - GFRP KW - Heterogeneous KW - Pulse thermography KW - Semitransparent PY - 2018 DO - https://doi.org/10.1007/s10765-018-2362-7 SN - 0195-928X SN - 1572-9567 VL - 39 IS - 3 SP - Article 39, ICPPP 19, 1 EP - 17 PB - Springer International Publishing AG AN - OPUS4-44003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Taparli, Ugur Alp T1 - In situ laser-induced breakdown spectroscopy measurements in stainless steels during TIG welding N2 - Chemical composition of the welding seam and HAZ has significant effect on weld quality. Current inspection methods for weld seams measure and investigate post factum and cannot prevent weld defects. Element burn-off may significantly affect solidification leading to embrittlement or cracking Control of weld chemical compositions insures a controlled solidification and resistance to related weld defects. A prototype of a LIBS controlled welding process is presented. T2 - Forschungsseminar Universität Magdeburg CY - Magdeburg, Germany DA - 17.01.2018 KW - LIBS KW - TIG-Welding KW - Chemical compositions KW - In situ measurements PY - 2018 AN - OPUS4-43830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernegger, Raphael A1 - Maierhofer, Christiane A1 - Altenburg, Simon T1 - Quantification of delaminations in semitransparent solids using pulsed thermography and mathematical 1D models N2 - Material defects in fiber reinforced polymers such as delaminations can rapidly degrade the material properties or can lead to the failure of a component. Pulse thermography (PT) has proven to be a valuable tool to identify and quantify such defects in opaque materials. However, quantification of delaminations within semitransparent materials is extremely challenging. We present an approach to quantify delaminations within materials being semitransparent within the wavelength ranges of the optical excitation sources as well as of the infrared (IR) camera. PT experimental data of a glass fiber reinforced polymer with a real delamination within the material were reconstructed by one dimensional (1D) mathematical models. These models describe the heat diffusion within the material and consider semitransparency to the excitation source as well to the IR camera, thermal losses at the samples surfaces and a thermal contact resistance between the two layers describing the delamination. By fitting the models to the PT data, we were able to determine the depth of the delamination very accurately. Additionally, we analyzed synthetic PT data from a 2D simulation with our 1D-models to show how the thermal contact resistance is influenced by lateral heat flow within the material. KW - Pulsed thermography KW - Quantification KW - Numerical simulation KW - Analytical model KW - Semitransparent KW - GFRP KW - Delamination PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505766 DO - https://doi.org/10.1007/s10765-020-02642-7 VL - 41 IS - 5 SP - Article number: 67 PB - Springer AN - OPUS4-50576 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krankenhagen, Rainer A1 - Altenburg, Simon T1 - Transient behaviour of the energy release after the discharge of flash lamps – A consideration of the afterglow N2 - The knowledge about energy release and transient behaviour of flash lamps, used as short-term energy source in flash thermography investigations, is essential for a quantitative analysis of the results as well as for simulations regarding such experiments. Usually, only a rectangular pulse shape of a typical duration of a few milliseconds is regarded when flash lamps pulses are described. This note considers the afterglow period of a flash lamp explicitly and shows that negligence of this afterglow effect leads to a systematic underestimation of the pulse length and the related total energy release. In the reported case, the intensity transient recorded by a Silicon photo diode was transformed into a temperature transient, allowing the study of the real energy release. It turns out that approximately only 50% of the entire pulse energy were released during the usually regarded period of 2.8 ms, while the other half was released within a period of 20 ms with an exponential decay. KW - Flash thermography KW - Flash lamp KW - Afterglow KW - Discharge arc KW - Pulse energy PY - 2021 DO - https://doi.org/10.1016/j.infrared.2021.103951 SN - 1350-4495 VL - 119 IS - 103951 SP - 1 EP - 4 PB - Elsevier B.V. AN - OPUS4-53642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breese, Philipp Peter A1 - Becker, Tina A1 - Oster, Simon A1 - Altenburg, Simon A1 - Metz, C. A1 - Maierhofer, Christiane T1 - Aktive Laserthermografie im L-PBF-Prozess zur in-situ Detektion von Defekten N2 - Die zerstörungsfreie Prüfung von metallischen Bauteilen hergestellt mit additiver Fertigung (Additive Manufacturing - AM) gewinnt zunehmend an industrieller Bedeutung. Grund dafür ist die Feststellung von Qualität, Reproduzierbarkeit und damit auch Sicherheit für Bauteile, die mittels AM gefertigt wurden. Jedoch wird noch immer ex-situ geprüft, wobei Defekte (z.B. Poren, Risse etc.) erst nach Prozessabschluss entdeckt werden. Übersteigen Anzahl und/oder Abmessung die vorgegebenen Grenzwerte für diese Defekte, so kommt es zu Ausschuss, was angesichts sehr langer Bauprozessdauern äußerst unrentabel ist. Eine Schwierigkeit ist dabei, dass manche Defekte sich erst zeitverzögert zum eigentlichen Materialauftrag bilden, z.B. durch thermische Spannungen oder Schmelzbadaktivitäten. Dementsprechend sind reine Monitoringansätze zur Detektion ggf. nicht ausreichend. Daher wird in dieser Arbeit ein Verfahren zur aktiven Thermografie an dem AM-Prozess Laser Powder Bed Fusion (L-PBF) untersucht. Das Bauteil wird mit Hilfe des defokussierten Prozesslasers bei geringer Laserleistung zwischen den einzelnen gefertigten Lagen unabhängig vom eigentlichen Bauprozess erwärmt. Die entstehende Wärmesignatur wird ort- und zeitaufgelöst durch eine Infrarotkamera erfasst. Durch diese der Lagenfertigung nachgelagerte Prüfung werden auch zum Bauprozess zeitversetzte Defektbildungen nachweisbar. In dieser Arbeit finden die Untersuchungen als Proof-of-Concept, losgelöst vom AM-Prozess, an einem typischen metallischen Testkörper statt. Dieser besitzt eine Nut als oberflächlichen Defekt. Die durchgeführten Messungen finden an einer eigens entwickelten L-PBF-Forschungsanlage innerhalb der Prozesskammer statt. Damit wird ein neuartiger Ansatz zur aktiven Thermografie für L-PBF erforscht, der eine größere Bandbreite an Defektarten auffindbar macht. Der Ansatz wird validiert und Genauigkeit sowie Auflösungsvermögen geprüft. Eine Anwendung am AM-Prozess wird damit direkt forciert und die dafür benötigten Zusammenhänge werden präsentiert. T2 - DGZfP-Jahrestagung 2022 CY - Kassel, Germany DA - 23.05.2022 KW - Additive Manufacturing KW - Laser Powder Bed Fusion KW - Thermografie KW - Zerstörungsfreie Prüfung KW - Aktive Laserthermografie PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550353 SN - 978-3-947971-25-1 VL - 177 SP - 1 EP - 9 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung e.V. AN - OPUS4-55035 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breese, Philipp Peter T1 - Aktive Laserthermografie im L-PBF-Prozess zur in-situ Detektion von Defekten N2 - Die zerstörungsfreie Prüfung von metallischen Bauteilen hergestellt mit additiver Fertigung (Additive Manufacturing - AM) gewinnt zunehmend an industrieller Bedeutung. Grund dafür ist die Feststellung von Qualität, Reproduzierbarkeit und damit auch Sicherheit für Bauteile, die mittels AM gefertigt wurden. Jedoch wird noch immer ex-situ geprüft, wobei Defekte (z.B. Poren, Risse etc.) erst nach Prozessabschluss entdeckt werden. Übersteigen Anzahl und/oder Abmessung die vorgegebenen Grenzwerte für diese Defekte, so kommt es zu Ausschuss, was angesichts sehr langer Bauprozessdauern äußerst unrentabel ist. Eine Schwierigkeit ist dabei, dass manche Defekte sich erst zeitverzögert zum eigentlichen Materialauftrag bilden, z.B. durch thermische Spannungen oder Schmelzbadaktivitäten. Dementsprechend sind reine Monitoringansätze zur Detektion ggf. nicht ausreichend. Daher wird in dieser Arbeit ein Verfahren zur aktiven Thermografie an dem AM-Prozess Laser Powder Bed Fusion (L-PBF) untersucht. Das Bauteil wird mit Hilfe des defokussierten Prozesslasers bei geringer Laserleistung zwischen den einzelnen gefertigten Lagen unabhängig vom eigentlichen Bauprozess erwärmt. Die entstehende Wärmesignatur wird ort- und zeitaufgelöst durch eine Infrarotkamera erfasst. Durch diese der Lagenfertigung nachgelagerte Prüfung werden auch zum Bauprozess zeitversetzte Defektbildungen nachweisbar. In dieser Arbeit finden die Untersuchungen als Proof-of-Concept, losgelöst vom AM-Prozess, an einem typischen metallischen Testkörper statt. Dieser besitzt eine Nut als oberflächlichen Defekt. Die durchgeführten Messungen finden an einer eigens entwickelten L-PBF-Forschungsanlage innerhalb der Prozesskammer statt. Damit wird ein neuartiger Ansatz zur aktiven Thermografie für L-PBF erforscht, der eine größere Bandbreite an Defektarten auffindbar macht. Der Ansatz wird validiert und Genauigkeit sowie Auflösungsvermögen geprüft. Eine Anwendung am AM-Prozess wird damit direkt forciert und die dafür benötigten Zusammenhänge werden präsentiert. T2 - DGZfP-Jahrestagung 2022 CY - Kassel, Germany DA - 23.05.2022 KW - Additive Manufacturing KW - Laser Powder Bed Fusion KW - Thermografie KW - Zerstörungsfreie Prüfung KW - Aktive Laserthermografie PY - 2022 AN - OPUS4-55040 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oster, Simon T1 - Porosity prediction in metal based additive manufacturing utilizing in situ thermography N2 - Quality assessment of components produced by metal based additive manufacturing (AM) technologies such as laser powder bed fusion is rising in importance due to the increased use of AM in industrial production. Here, the presence of internal porosity was identified as a limiting factor for the final component quality. The utilization of thermography as an in-situ monitoring technique allows the determination of the part’s thermal history which was found to be connected to the porosity formation [1]. Combining the local thermal information derived from thermography with the porosity information obtained by x-ray micro computed tomography, machine learning algorithms can be utilized to predict the porosity distribution in the part. In this study, a first approach for the prediction of keyhole porosity in a cylindric specimen from AISI 316L stainless steel is presented. It is based on data augmentation using the “SmoteR” algorithm [2] to cure the dataset imbalance and a 1-dimensional convolutional neural network. [1] C.S. Lough et al., Local prediction of Laser Powder Bed Fusion porosity by short-wave infrared thermal feature porosity probability maps. Journal of Materials Processing Technology, 302, p. 117473 (2022) https://dx.doi.org/10.1016/j.imatprotec.2021.117473 [2] L. Torgo et al., SMOTE for Regression. Progress in Artificial Intelligence, Chapter 33, p. 378-289 (2013) https://dx.doi.org/10.1007/978-3-642-40669-0_33 T2 - KI-Tag Arbeitskreis Chemometrik & Qualitätssicherung - Chemometrics meets Artificial Intelligence CY - Berlin, Germany DA - 01.04.2022 KW - Laser Powder Bed Fusion KW - Thermography KW - Defect Prediction KW - Convolutional Neural Networks PY - 2022 AN - OPUS4-54621 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oster, Simon A1 - Scheuschner, Nils A1 - Chand, Keerthana A1 - Breese, Philipp Peter A1 - Becker, Tina A1 - Heinrichsdorff, F. A1 - Altenburg, Simon T1 - From Thermographic In-situ Monitoring to Porosity Detection – A Deep Learning Framework for Quality Control in Laser Powder Bed Fusion N2 - In this study, we present an enhanced deep learning framework for the prediction of porosity based on thermographic in-situ monitoring data of laser powder bed fusion processes. The manufacturing of two cuboid specimens from Haynes 282 (Ni-based alloy) powder was monitored by a short-wave infrared camera. We use thermogram feature data and x-ray computed tomography data to train a convolutional neural network classifier. The classifier is used to perform a multi-class prediction of the spatially resolved porosity level in small sub-volumes of the specimen bulk. T2 - SMSI - Sensor and Measurement Science International 2023 CY - Nürnberg, Germany DA - 08.05.2023 KW - Porosity KW - Laser powder bed fusion KW - In-situ monitoring KW - Thermography KW - Machine Learning PY - 2023 UR - https://www.ama-science.org/proceedings/details/4404 DO - https://doi.org/10.5162/SMSI2023/C5.4 SP - 179 EP - 180 AN - OPUS4-57616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oster, Simon T1 - From Thermographic In-situ Monitoring to Porosity Detection – A Deep Learning Framework for Quality Control in Laser Powder Bed Fusion N2 - In this study, we present an enhanced deep learning framework for the prediction of porosity based on thermographic in-situ monitoring data of laser powder bed fusion processes. The manufacturing of two cuboid specimens from Haynes 282 (Ni-based alloy) powder was monitored by a short-wave infrared camera. We use thermogram feature data and x-ray computed tomography data to train a convolutional neural network classifier. The classifier is used to perform a multi-class prediction of the spatially resolved porosity level in small sub-volumes of the specimen bulk. T2 - Sensor and Measurement Science International CY - Nurnberg, Germany DA - 08.05.2023 KW - Laser powder bed fusion KW - In-situ monitoring KW - Thermography KW - Machine Learning KW - Porosity PY - 2023 AN - OPUS4-57614 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - MinimUm Information Requirements for Electron Microscopy and Surface analysis Data For Risk Assessment of Nanoforms N2 - The European legislation has responded to the wide use of nanomaterials in our daily life and defined the term “nanoform” in the Annexes to the REACH (Registration, Evaluation, Authorization of Chemicals) Regulation. Now specific information of the nanomaterials is required from the companies when registering the appropriate materials in a dossier. In the context of REACH eleven physicochemical properties were considered as relevant, of which the following six are essential for registration of nanoforms (priority properties): chemical composition, crystallinity, particle size, particle shape, chemical nature of the surface (“surface chemistry”), and specific surface area (SSA). A key role is the reliable, reproduceable and traceable character of the data of these priority properties. In this context, we want to discuss which ‘analytical’ information is exactly required to fulfill these conditions. Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and X-ray Photoelectron Spectroscopy (XPS) were chosen as the most popular surface analytical methods. Both methods allow a detailed understanding of the surface chemistry with an information depth below ten nanometers. As a rather bulk method for the analysis of nanoforms, Electron Probe Microanalysis (EPMA) in the version with energy dispersive X-ray spectroscopy (EDS) is considered for the quick identification of the main chemical elements present in the sample. Furthermore, Scanning Electron Microscopy (SEM) results are discussed which provide results on particle size and shape. Thus, four of the six priority properties can be obtained with these methods. T2 - Nanosafe 2020 CY - Online meeting DA - 17.11.2020 KW - Risk assessment KW - Nanomaterials KW - Standardization KW - Regulation PY - 2020 AN - OPUS4-51612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Characterization of functionalized graphene particles with comparative XPS/HAXPES investigations N2 - The different chmemistry of graphitic nanoplatelets between the outermost surface and the bulk of the samples was investigated with comparative XPS/HAXPES measurements. T2 - PHI User Meeting CY - Grenoble, France DA - 18.04.2023 KW - X-ray photoelectron spectroscopy KW - Hard-energy X-ray photoelectron spectroscopy KW - graphene related 2D materials PY - 2023 AN - OPUS4-57649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Chemical characterization of nanoparticles by PCA-assisted ToF-SIMS: a) Core-shell character, b) transformation and c) grouping studies N2 - This talk was given within the scope of the SIMS-22 conference in October 2019 in Kyoto (Japan). It deals with the surface analytical investigation of nanoparticles by PCS-assisted ToF-SIMS. This technique is applicable to core-shell nanoparticles, in order to distinguish a complete encapsulation from an incomplete encapsulation of the core by the shell material. Furthermore, the depletion process of organic nanoparticle coatings caused by UV-weathering is investigated. Finally, the significance of grouping studies for nanomaterials research and risk assessment is demonstrated. T2 - The 22nd International Conference on Secondary Ion Mass Spectrometry (SIMS-22) CY - Kyoto, Japan DA - 20.10.2019 KW - Nanoparticles KW - ToF-SIMS KW - Principal component analysis (PCA) PY - 2019 AN - OPUS4-50075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altenburg, Simon T1 - Analytical modelling of semitransparent solids for flash thermography with absorption coefficient dispersion N2 - Pulse and flash thermography are experimental techniques which are widely used in the field of non-destructive evaluation for materials characterization and defect detection. We recently showed that it is possible to quantitatively determine the thickness of semitransparent polymeric solids by fitting of results of an analytical model to experimental flash thermography data, for both transmission and reflection geometry. However, depending on the chosen experimental geometry, different effective optical absorption coefficients (i.e., penetration depths of the heating light) had to be utilized in the model in order to properly fit the experimental data. Here we show that this effect is caused by the wavelength dependency of the absorption coefficient of the sample material. We present an extension of the analytical model to incorporate this dispersion. Even accounting for only two different values of the absorption coefficient, the experimental results from both measurement geometries can be fitted by a single set of absorption coefficients. Additionally, the deviations between experimental data and fit are reduced compared to a single optimized effective absorption coefficient. This work is part of the ZIM-project KF2201089AT4 and is funded by the German Federal Ministry for Economic Affairs and Energy due to an order of the German Bundestag. T2 - 19th International Conference on Photoacoustic and Photothermal Phenomena CY - Bilbao, Spain DA - 16.07.2017 KW - Analytical model KW - Semitransparency KW - Thermography PY - 2017 AN - OPUS4-41084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Singh, Chandan A1 - Riedel, Soraya A1 - Konthur, Zoltán A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg A1 - Schenk, J. A. A1 - Schneider, Rudolf T1 - Functionalized Ti3C2Tx nanosheets based biosensor for point-of-care detection of SARS-CoV‑2 antigen N2 - MXenes are considered a promising class of two-dimensional materials with extraordinary physical and electrochemical properties. Distinguished features like high specific surface area and outstanding electrical conductivity make them suitable for electrochemical biosensing applications. Here, we report the development of a biosensor involving the functionalized MXene−titanium carbide nanosheets (Ti3C2Tx-NS) and monoclonal antibodies against the SARS-CoV-2 nucleocapsid protein (anti-SARS-CoV-2 mAb) to design a point-of-care device for detection of the SARS-CoV-2 nucleocapsid protein (SARS-CoV-2 NP) antigen. Few-layered titanium carbide nanosheets (denoted as FL-Ti3C2Tx-NS) have been synthesized using a single-step etching and delamination method and characterized using optical and electron microscopy techniques revealing the suitability for immunosensing applications. Binding studies revealed the excellent affinity between the biosensor and the SARS-CoV-2 NP. Electrochemical detection of SARS-CoV-2 NP is performed using differential pulse voltammetry and read by a smartphone-based user interface. The proposed FL-Ti3C2Tx-NS based biosensor offers the detection of SARS-CoV-2 NP with a limit of detection of 0.91 nM in a wide detection range in spiked saliva samples. Additionally, there is no cross-reactivity in the presence of potential interferants like SARS-CoV-2 spike glycoprotein and bovine serum albumin. These findings demonstrate the potential of MXenes in developing a rapid and reliable tool for SARS-CoV-2 NP detection. While we report the biosensing of SARS-CoV-2 NP, our system also paves the way for the detection of other SARS-CoV-2 antigens like spike protein or other biomolecules based on antigen−antibody interactions. KW - Antigen testing KW - Few-layered titanium carbide nanosheets KW - SARS-CoV-2 nucleocapsid protein KW - Label-free detection KW - Electrochemical immunosensor PY - 2023 DO - https://doi.org/10.1021/acsaenm.2c00118 SN - 2771-9545 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. VL - 1 IS - 1 SP - 495 EP - 507 PB - American Chemical Society CY - Washington, DC AN - OPUS4-56931 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kjaervik, Marit A1 - Dietrich, P. M. A1 - Thissen, A. A1 - Radnik, Jörg A1 - Nefedov, A. A1 - Natzeck, C. A1 - Wöll, C. A1 - Unger, Wolfgang T1 - Application of near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS) in an in-situ analysis of the stability of the surface-supported metal-organic framework HKUST-1 in water, methanol and pyridine atmospheres N2 - Surface-supported metal-organic frameworks HKUST-1 (Hong Kong University of Science and Technology) were used as a model system for a development of a near ambient pressure (NAP) XPS based approach to investigate interaction with atmospheres of water, methanol or pyridine at pressures ranging from 1 to 4 mbar. The films were grown on a gold substrate functionalized with a COOH-terminated self-assembled monolayer using liquidphase epitaxy in a step-by-step fashion. Measurement protocols were developed and optimised for different gases in order to obtain spectra of similar quality in terms of signal intensity, noise and shape. Peak shapes were found to depend on the efficiency of charge compensation. Reference measurements in argon proved to be a useful strategy not only for the evaluation of the Cu(II)-fraction in pristine samples, but also to identify the contributions by the respective gas atmosphere to the C 1s and O 1s photoelectron spectra. Reduced copper was found during the exposition of HKUST-1 to water vapour and pyridine, but this effect was not observed in case of methanol. Additionally, it was established that there are no changes in relative Cu(II) percentage with increasing exposure time. This indicates that saturation was reached already at the lowest time of gas exposure. A detailed elucidation of the mechanism of Cu(II) reduction to Cu(I) in HKUST-1 mediated by water and pyridine is part of ongoing work and not in the scope of the present paper. KW - HKUST-1 KW - Near-ambient pressure X-ray photoelectron spectroscopy KW - Metal-organic frameworks KW - Interaction with atmospheres KW - Water PY - 2021 DO - https://doi.org/10.1016/j.elspec.2020.147042 SN - 0368-2048 IS - 247 SP - 147042 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-52098 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Taparli, Ugur Alp T1 - Development of a LIBS analysis system for time- and spaceresolved in situ measurement of chemical compositions during GTA-Welding N2 - A laser induced breakdown spectroscopy (LIBS) system was combined with the Gas Tungsten Arc (GTA) Welding process for the in situ measurement of chemical compositions in austenitic stainless steels during welding. The purpose of this project is to develop a prototype of an online chemical composition control system for welding applications. One of the use cases of this new LIBS-based measurement system can be the controlling of potentially dangerous emissions during the welding process in order to improve the working safety conditions. Further, the control of the weld pool composition allows governing the weld pool solidification behavior and thus allows reducing the resultant susceptibility for solidification cracking. The composition of the weld seam is from the metallurgical point of view the most critical parameter for the occurrence of weld defects1. Conventional inspection methods for weld seams as e.g. ultrasonic inspection are ex situ and cannot prevent the defects. For that reason automated in situ analysis systems for weld defect detection are much more efficient2. Beyond that, the proposed LIBS-based analysis system allows to study the correlation between the occurrence of weld defects and the chemical composition of the weld pool or the region where solid and liquid phase coexist. T2 - The 9th International Conference on Laser-Induced Breakdown Spectroscopy (LIBS 2016) CY - Charmonix, France DA - 12.09.2016 KW - In situ measurement KW - GTA-Welding KW - LIBS PY - 2016 AN - OPUS4-37417 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Schaupp, Thomas A1 - Münster, C. A1 - Mente, Tobias A1 - Kannengießer, Thomas A1 - Böllinghaus, Thomas T1 - Hydrogen determination in welded specimens by carrier gas hot extraction - a review on the main parameters and their effects on hydrogen measurement N2 - Carrier gas hot extraction (CGHE) is a commonly applied technique for determination of hydrogen in weld joints using a thermal conductivity detector (TCD) for hydrogen measurement. The CGHE is based on the accelerated hydrogen effusion due to thermal activation at elevated temperatures. The ISO 3690 standard suggests different specimen geometries as well as necessary minimum extraction time vs. temperature. They have the biggest influence on precise hydrogen determination. The present study summarizes the results and experience of numerous test runs with different specimen temperatures, geometries (ISO 3690 type B and small cylindrical samples), and factors that additionally influence hydrogen determination. They are namely specimen surface (polished/as-welded), limited TCD sensitivity vs. specimen volume, temperature measurement vs. effects of PI-furnace controller, as well as errors due to insufficient data assessment. Summarized, the temperature is the driving force of the CGHE. Two different methods are suggested to increase the heating rate up to the desired extraction temperature without changing the experimental equipment. Suggestions are made to improve the reliability of hydrogen determination depended on the hydrogen signal stability during extraction accompanied by Evaluation of the recorded data. Generally, independent temperature measurement with dummy specimens is useful for further data analysis, especially if this data is used for calculation of trapping kinetics by thermal desorption analysis (TDA). KW - Hydrogen KW - Carrier gas hot extraction KW - Experimental design KW - Thermal conductivity device PY - 2019 DO - https://doi.org/10.1007/s40194-018-0664-9 SN - 0043-2288 VL - 63 IS - 2 SP - 511 EP - 526 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-47603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Reliable, and reproducible physico-chemical data of nanomaterials for risk assessment N2 - Nanoforms with at least one dimension below 100 nm have an important part to play in more and more areas of our daily life. Therefore, risk assessment of these materials is becoming increasingly important. In this context, the European Chemical Agency (ECHA) considered eleven physico-chemical properties as relevant, of which the following six are essential for the registration: chemical composition, crystallinity, particle size, particle shape, surface chemistry and specific surface area. Four of these priority properties can be obtained with electron microscopy and surface analytics like XPS and ToF-SIMS. The reliability of this data must be ensured, especially for their use for grouping and read across approaches. On the other hand, the “reproducibility” crisis has revealed major shortcomings in the reliability of published data. In a case study, we show how the quality of the data can be ensured by using existing standards and protocols of each step in the workflow of sample characterization. As exemplary samples, two Al-coated TiO2 samples as nanopowders were selected from the JRC repository, capped either with a hydrophilic or a hydrophobic organic ultrathin shell. SEM results provided the size and shape of the nanoparticles, a first overview about the composition was obtained with EDS. XPS and ToF-SIMS supplied the surface chemistry, especially information about the shell and the coating of the particles. Standards and protocols of all steps of the analytical workflow including preparation and data reduction are discussed regarding reliable and reproducible data. Additionally, uncertainties for the different steps are specified. Only such a detailed description of all these factors allows a comprehensive physico-chemical characterization of the nanoparticles with understanding of their potential risk assessment. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Reference data KW - Risk assessment KW - Nanomaterials KW - Titania PY - 2022 AN - OPUS4-54961 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pignatelli, Giuseppe T1 - Optical emission spectroscopy as monitoring tool for ded N2 - This presentstion explains how optical emission spectroscopy can be exploited to on line monitor a DED printing production. This technique is tested printing on a substrate with artificial defects. T2 - 1st Workshop on In-situ Monitoring and Microstructure Development in Additive Manufacturing CY - Online meeting DA - 10.12.2020 KW - Monitoring KW - Spectroscopy KW - Analytical chemistry KW - Additive manufacturing PY - 2020 AN - OPUS4-51877 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lu, Z. A1 - Haist, M. A1 - Ivanov, D. A1 - Jakob, C. A1 - Jansen, D. A1 - Leinitz, Sarah A1 - Link, J. A1 - Mechtcherine, V. A1 - Neubauer, J. A1 - Plank, J. A1 - Schmidt, Wolfram A1 - Schilde, C. A1 - Schröfl, C. A1 - Sowoidnich, T. A1 - Stephan, D. T1 - Characterization data of reference cement CEM I 42.5 R used for Priority Program DFG SPP 2005 “Opus Fluidum Futurum - Rheology of reactive, multiscale, multiphase construction materials” N2 - A thorough characterization of starting materials is the precondition for further research, especially for cement, which contains various phases and presents quite a complex material for fundamental scientific investigation. In the paper at hand, the characterization data of the reference cement CEM I 42.5 R used within the priority program 2005 of the German Research Foundation (DFG SPP 2005) are presented from the aspects of chemical and mineralogical compositions as well as physical and chemical properties. The data were collected based on tests conducted by nine research groups involved in this cooperative program. For all data received, the mean values and the corresponding errors were calculated. The results shall be used for the ongoing research within the priority program. KW - Portland cement KW - Characterization KW - DFG SPP 2005 PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500849 DO - https://doi.org/10.1016/j.dib.2019.104699 SN - 2352-3409 VL - 27 SP - 104699 PB - Elsevier Inc. AN - OPUS4-50084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram ED - Schmidt, Wolfram T1 - Engineering skill requirements to cope with the local and global challenges of the future N2 - In the 21st century, adequate habitat and functioning infrastructure are critical for global societal and economic stability. In addition, growing urbanisation and environmental pollution cause challenges to societies. With increasing velocity, humanity faces that the current way of living is not sustainable. Thus, habitat,infrastructure, urbanisation, environment and sustainability are definitively among the most striking challenges of the 21st century. By consulting, planning, building, maintaining, exploiting and processing of global resources, civil engineers contribute significantly to the existence of these challenges. This is a high responsibility, but due to the heavy involvement, together with adjacent disciplines such as architecture, geosciences, chemistry, physics, environmental sciences and economics, civil engineers also hold the key to mitigate these challenges and provide a brighter global future. Solutions towards greener, more sustainable and economically viable materials do exist, and there is ongoing research on how greener technologies can contribute to better livelihood and economic growth, but their level of implementation is limited, a major reason for which is that these approaches require more fundamental understanding rather than standard application. T2 - ISEE Africa - Innovation, Science, Engineering, Education CY - Nairobi, Kenya DA - 30.01.2019 KW - Civil Engineering KW - Education KW - Sustainability KW - Materials KW - Sciences PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-484895 UR - http://isee-africa.com/wp-content/uploads/2019/07/Innovation-Science-Engineering-Education_High-Quality.pdf SN - 978-3-9818564-2-2 SP - 16 EP - 19 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-48489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Radebe, N. ED - Schmidt, Wolfram T1 - Biased by analytical equipment N2 - Today, in scientific events often a certain separation between researchers from laboratories with highly sophisticated equipment and those from less privileged laboratories can be observed. It is not an uncommon situation that results presented at conferences are rubbished or ridiculed because the investigator only used low-end analytical methods. The assessment of the study is then biased based on the equipment, regardless of the actual quality of the study. T2 - ISEE Africa - Innovation, Science, Engineering, Education CY - Nairobi, Kenya DA - 30.01.2019 KW - Analytics KW - Africa KW - Bias KW - Science KW - Research PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-484877 UR - http://isee-africa.com/wp-content/uploads/2019/07/Innovation-Science-Engineering-Education_High-Quality.pdf SN - 978-3-9818564-2-2 SP - 203 EP - 204 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-48487 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Ecke, Alexander A1 - Bell, Jérémy A1 - Schneider, Rudolf T1 - From Laboratory Immunoassays to Immunosensors with an Integrated Microfluidic Flow System N2 - This research summary describe efforts to the development of a three-dimensional microfluidic flow cell for improved electrochemical substrate detection in HRP/TMB-based immunoassays. This work provides a valuable advancement in the sensitivity and integration of immunoassay technologies, aiding in the refinement of diagnostic tools. KW - Antikörper KW - Immunoassay KW - Microfluidics KW - Electrochemical detection KW - Biosensor PY - 2025 UR - https://www.elveflow.com/microfluidics-research-summaries/from-laboratory-immunoassays-to-immunosensors-with-an-integrated-microfluidic-flow-system/ SP - 1 EP - 4 CY - Paris AN - OPUS4-62674 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Trapping in T24 steel weld joints – Effects on activation energy for hydrogen diffusion during TDA N2 - Failure cases in the past decade exhibited severe cracking in T24 welds and showed that generally hydrogen-assisted cracking (HAC) occurring up to 200°C cannot be excluded. A basic understanding is necessary on how hydrogen diffusion is influenced by the weld process. In this regard, both weld microstructures HAZ and weld metal have particular influence on hydrogen diffusion compared to the base material. In general, hydrogen diffusion at a certain temperature is described by diffusion coefficients representing an effective value of combined lattice diffusion and effects of reversible hydrogen traps. Those traps are typically precipitates, interstitials, grain boundaries and so on. A common approach to describe the trap character and its effect on diffusion is the determination of so-called activation energy. This can be done by respective thermal desorption analysis (TDA) with linear heating. In the present study, different T24 as-welded microstructures (BM, HAZ, WM) were investigated. For that purpose, electrochemically hydrogen charged specimens were analyzed by TDA with linear heating using a mass spectrometer for detection of ultra-low hydrogen amounts. The results showed that typically the as-welded HAZ had higher energy traps than the tempered base material. Nonetheless two important effects were ascertained: (1) it is strictly necessary to monitor the sample temperature due to its great impact on the hydrogen desorption peak temperature and (2) the real heating rate in the specimen vs. the applied heating rate has to be considered. Both influence the calculated activation energy, i.e. the assigned hydrogen trap character (moderate or strong trap), which changed up to a factor of two in terms of the calculated activation energy. This effect can be much more important compared to the microstructure effect itself. Hence, suitable experimental boundary conditions should be mandatory for the determination of hydrogen trap kinetics. T2 - Intermediate Meeting of IIW Commission C-II-A "Metallurgy of Weld Metal" CY - Trollhättan, Sweden DA - 06.03.2017 KW - Hydrogen KW - Trapping and diffusion KW - Thermal desorption analysis KW - Microstructure KW - Activation energy PY - 2017 AN - OPUS4-39401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Stege, Heike A1 - Hahn, Oliver ED - Geiger, Gisela ED - Bretz, Simone T1 - Möglichkeiten moderner Materialanalytik für die Untersuchung von Hinterglasbildern N2 - Materialanalytische Verfahren gewinnen zunehmend an Bedeutung bei der Beantwortung kulturhistorischer Fragestellungen, etwa nach Werkstatt, Alter, Künstler oder Provenienz eines Artefakts. Auch die Entwicklung geeigneter Restaurierungs- und Konservierungskonzepte bedarf dieser Grundlage ebenso wie die Beurteilung hinsichtlich der Frage nach Fälschung oder Kopie. Dem kunsttechnologisch orientierten Analytiker steht heute eine eindrucksvolle Bandbreite instrumenteller Methoden zur Verfügung, um die beiden Hauptkomponenten verwendeter Malfarben zu identifizieren, d.h. Farb- und Bindemittel. Der nachfolgende Aufsatz enthält eine kurze Zusammenstellung geeigneter Analyseverfahren, die üblicherweise bei der Untersuchung von Gemälden Verwendung finden. KW - Hinterglasmalerei KW - Kunsttechnologie KW - Kunst- und Kulturgut PY - 2017 SN - 978-3-86832-320-7 SP - 74 EP - 77 PB - Wienand Verlag CY - Köln AN - OPUS4-39324 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Time dependent Analysis of Morphology, Elemental and Chemical Composition of CH3NH3PbI3/TiO2 Solar Cell Layered System N2 - The motivation of this work is to produce thin films perovskite solar cells with constant high light conversion efficiency over time. Loss of efficiency may be caused by structural and/or chemical alterations of the complex layered system. As these changes might take place either in the bulk and/or on the surface of the stratified material, analytical tools addressing both key issues are selected and combined. SEM/EDS combined with XPS were chosen as appropriate methodical approach to characterise perovskite laboratory cells in depth and complementary on top, before and after light exposure. The layered perovskite system investigated here is based on glass covered with fluorine doped tin oxide (FTO), followed by three porous thin films of TiO2, ZrO2 and a thick monolithic carbon. The TiO2 film is subdivided into a dense layer covered by a porous one constituted of nanoparticles with a truncated bipyramidal shape. This layered system serves as the matrix for the perovskite. After infiltration of perovskite solution and annealing, EDS spectral maps on cross-sections of the specimen have been measured. The distribution of relevant elements – Si, Sn, Ti, Zr and C – correlates conclusively with layers visible in the acquired SEM images. Lead and iodine are distributed throughout the porous layers C, ZrO2 and TiO2. Specimens were exposed to ambient daylight for 7 weeks. In a SEM micrograph taken of the cross-section of a sample after illumination, the glass substrate and all layers FTO, TiO2, ZrO2 as well as C are clearly identified. EDS data have been acquired under the same measurement conditions as before the illumination. It was found that several weeks of ambient daylight did not change significantly the qualitative elemental composition of lead and iodine throughout the solar cell system. It was confirmed with EDS that nanoparticles identified in high-resolution SEM micrographs contain mainly Pb and I, indicating these to be the perovskite crystals. However, a time-dependent compositional and chemical altering was observed with XPS for the near-surface region of the outermost ~10 nm after 2 months of illumination. T2 - EMAS 2017 - 15th European Workshop on MODERN DEVELOPMENTS AND APPLICATIONS IN MICROBEAM ANALYSIS and IUMAS-7 Meeting CY - Konstanz, Germany DA - 07.05.2017 KW - Perovskite KW - Layer analytics KW - SEM/EDX KW - XPS KW - Solar cells PY - 2017 AN - OPUS4-40253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altenburg, Simon A1 - Krankenhagen, Rainer T1 - Continuous and Laplace transformable approximation for the temporal pulse shape of Xe-flash lamps for flash thermography N2 - Flash thermography is widely used in non-destructive testing and materials characterisation. The use of analytical modelling utilizing the Laplace transform allows one to calculate the temperature transients of flash-heated samples and therefore characterize them by fitting of the results of model calculations to experimental data. However, for samples with high thermal diffusivity or very thin samples, the temperature transient is strongly influenced by the temporal shape of the heating pulse, especially in reflection configuration. To incorporate this into the model, the temporal shape of the heating pulse and its Laplace transform have to be known. Here we present a close phenomenological approximation of the temporal shape of pulses of Xe-flash lamps. It is a non-stitched solution, has a simple Laplace transform and is suitable for different lamps and energy settings. As an example for a practical application of the pulse shape approximation, we use it to determine the thickness of polymer samples with thicknesses down to 80 µm by means of flash thermography, both in transmission and reflection configuration. Using a rectangular pulse shape or a delayed Dirac pulse shape, the thickness results are very sensitive to the start time of the fit and an additional calibration is needed. KW - Flash thermography KW - Pulse shape KW - Finite pulse length KW - Laplace transform KW - Thickness determination KW - NDT PY - 2017 DO - https://doi.org/10.1080/17686733.2017.1383765 SN - 1768-6733 SN - 2116-7176 VL - 15 IS - 1 SP - 121 EP - 131 PB - Taylor and Francis CY - Abingdon, UK AN - OPUS4-42405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Hydrogen trapping in T24 steel weld joints - microstructure influence vs. experimental design effect on activation energy for diffusion N2 - In general, hydrogen assisted cracking is a result of a critical combination of local microstructure, mechanical load and hydrogen concentration. In that connection, welded microstructures of low-alloyed creep-resistant steels can show different hydrogen trapping kinetics. That influences the adsorbed hydrogen concentration as well as the diffusion itself in terms of moderate or strong trapping. A common approach to describe trapping is by the activation energy that is necessary to release hydrogen from a specific trap site. In the present study, T24 base material and weld metal were investigated. For that purpose, electrochemically hydrogen charged specimens were analyzed by thermal desorption analysis(TDA) with linear heating using a mass spectrometer. The results showed a microstructure effect on hydrogen trapping kinetics at elevated temperatures. Additionally, it is necessary to monitor the specimen temperature. A comparison between idealized temperature profile and real specimen temperature showed that the calculated activation energy varied up to a factor of two. Thus, the assigned trap character(moderate or strong) changed. In case of high temperature peaks, this effect could be more important compared to the microstructure effect itself. T2 - 70th IIW Annual Assembly, Commission II-A CY - Shanghai, People's Republic of China DA - 25.06.2017 KW - Creep resisting materials KW - Welding KW - Hydrogen diffusion KW - Thermal desorption analysis KW - Microstructure KW - Experimental design PY - 2017 AN - OPUS4-40954 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Redox properties of Cu ions in molecular sieves N2 - Molecular sieves as materials with defined pores offer new opportunities in the preparation of nanostructured materials for different applications in chemistry, medicine and biology. Typical examples for such materials are zeolites, porous glass, different silicas and active carbon. Introducing transition metal ions in such materials can widen the possibilities of these materials in terms of chemical activity. Especially, the opportunity to tailor the redox properties of the transition metal ions by varying the location of the ion in the sieves is a promising way to obtain catalysts with the desired properties. For this purpose, Cu2+ ions were introduced into a SAPO-5 (silicoaluminaphosphate) by a hydrothermal method and by impregnation. As expected, the different preparation methods led to different locations of the Cu2+ ions: by the hydrothermal method the ions were incorporated in the SAPO-5 framework, by impregnation mononuclear Cu species randomly distributed in the pores of the support or CuO particles were formed depending on the Cu amount. These locations could be determined by Extended X-ray Absorption Fine Structure and Anomalous Small-Angle X-ray Scattering investigations. For investigating the redox properties of the Cu2+ ions the differently prepared sample were treated in Ar and H2 atmosphere until 550°C. X-ray Photoelectron Spectroscopy was performed to study the valence states of Cu after each of such treatment. For a definite determination of the valence states, both Cu 2p and Cu LMM spectra must be recorded. Cu2+ exhibits a clear chemical shift and a typical satellite structure in Cu2p spectra, but between mono- and zerovalent Cu a differentiation is not possible. On the other hand, these two species show a clear shift in the Auger spectra. Whereas in H2 atmosphere in any case metallic Cu was formed, the treatment in Ar showed significant differences between the samples. Cu2+ incorporated in the framework could not be reduced by this treatment. In contrast, the mononuclear Cu2+ species were reduced to stable Cu+. Likewise, the CuO nanoparticles were reduced to the monovalent Cu, but this species can be much more easily reoxidized in air. The consequences for the catalytic properties will be discussed. T2 - ECASIA 2017 CY - Montpellier, France DA - 24.09.2017 KW - Catalysis KW - X-ray photoelectron spectroscopy KW - Nanostructured materials PY - 2017 AN - OPUS4-42323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altenburg, Simon T1 - Energy density detector for optical heat sources in step-heating thermography N2 - In this work, we describe the extension of the applicability of a point-shaped energy density detector formerly only applicable for flash lamp excitation to optical heat sources for step-heating thermography, such as IR lamps or halogen lamps. Such continuous heat sources are often used in active thermography testing, when materials with low thermal diffusivity and specimens with large heat capacity are examined and large amounts of energy have to be deposited. Here, the temperature transient at the sensor surface is recorded by the infrared camera that is already present. The energy (power) input into the investigated specimen can be determined during the following data evaluation by fitting the results of an analytical model to the experimental data. T2 - IRS² 2017 CY - Nürnberg, Germany DA - 30.05.2017 KW - Analytical model KW - Energy detector KW - Thermography PY - 2017 AN - OPUS4-40470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Morphological and Chemical Composition of a CH3NH3PbI3/TiO2 Solar Cell Layered System N2 - Manufacturing of new perovskite layered solar cells with constant high light conversion efficiency over time may be hampered by the loss of efficiency caused by structural and/or chemical alterations of the complex layered system. SEM/EDX combined with XPS were chosen as an appropriate methodical approach to characterize perovskite laboratory cells in depth and at surface, before and after light exposure. The layered perovskite system investigated here is based on glass covered with fluorine doped tin oxide (FTO), followed by thin films of TiO2, ZrO2 and a thick monolithic carbon. TiO2 film is subdivided into a dense layer covered by porous one constituted of nanoparticles (NPs) of truncated bipyramidal shape. This layered system serves as the matrix for the perovskite. EDX spectral maps on cross-sections of specimen have shown that Pb and I are distributed homogeneously throughout the porous layers C, ZrO2 and TiO2. SEM/EDX data show that 20 weeks of ambient daylight did not change significantly the indepth distribution of the elemental composition of Pb and I throughout the entire solar cell system. It was confirmed with EDX that NPs identified in high-resolution SEM micrographs contain mainly Pb and I, indicating these to be the perovskite crystals. However, a compositional and chemical altering began in the near-surface region of the outermost ~10 nm after 2 months of illumination which was observed with XPS. T2 - 17th European Conference on Applications of Surface and Interface Analysis ECASIA 2017 CY - Montpellier, France DA - 24.09.2017 KW - Perovskite KW - Solar cells KW - SEM/EDX KW - XPS KW - Layer analysis PY - 2017 AN - OPUS4-42657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altenburg, Simon T1 - Thickness determination of polymeric multilayer surface protection systems for concrete by means of pulse thermography N2 - So far, only destructive measurement techniques are available for thickness determination of polymer based surface protection systems for concrete surfaces. Pulse thermography appears to be well suited for non-destructive thickness evaluation in these systems. Here, we present first results of the development of a respective measurement and analysis procedure. Since surface protection systems consist of a number of layers, a model for the calculation of the surface temperature of a multi-layer structure on an infinite (concrete) substrate in pulse thermography setup was developed. It considers semitransparency of the upmost layer and thermal losses at the surface. It also supports the use of an arbitrary temporal shape of the heating pulse to properly describe the measurement conditions for different heat sources. First experimental results regarding the verification of the model are presented. Funding by the Federal Ministry for Economic Affairs and Energy is gratefully acknowledged. T2 - QNDE 2016 CY - Atlanta, GA, USA DA - 17.07.2016 KW - Thermography KW - Analytical model KW - Surface protection KW - Concrete KW - Semitransparency KW - Thickness PY - 2016 AN - OPUS4-36984 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmitt, Johannes T1 - Data acquisition system for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution N2 - This study presents our data acquisition system prototype for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution (nanoDAQ) and a matching data processing approach for time-resolved data in the nanosecond range. The system continuously samples the secondary electron multiplier (SEM) detector signal with a dwell time of approximately 2 ns and enables detection of gold nanoparticles (AuNP) as small as 7.5 nm with a commercial single quadrupole ICP-MS instrument. [1] Analysis of acquired transient data is based on the temporal distance between detector events and a derived ion event density. It was shown that the inverse logarithm of the distance between detector events is proportional to particle size. Also, the number of detector events per particle can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. Particle-by-particle-based analysis of ion event density and other parameters derived from nanosecond time resolution show promising results. High data acquisition frequency of the systems allows recording of a statistically significant number of data points in 60 s or less, which leaves only the sample uptake and rinsing steps as remaining factors for limiting the total measurement time. T2 - 20th European Winter Conference on Plasma Spectrochemistry CY - Berlin, Germany DA - 02.03.2025 KW - ICP-MS KW - Instrumentation KW - Nano KW - Nanoparticle Characterization PY - 2025 AN - OPUS4-63599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Bretz, S. ED - Hagnau, C. ED - Hahn, Oliver ED - Ranz, H.-J. T1 - Deutsche und niederländische Hinterglasmalerei vom Mittelalter bis zur Renaissance N2 - Die Hinterglasmalerei fand als Zwischengattung der Glas- und Tafelmalerei eher wenig Beachtung, war sie doch lange mit dem Begriff der Glasmalerei belegt. Dieses geschah jedoch zu Unrecht, wie die Auswahl an Hinterglasbildern, die in dieser Publikation vorgestellt wird, eindrucksvoll belegt. Auch wenn Glas in beiden Fällen das Trägermaterial darstellt, wird in der Hinterglasmalerei die Rückseite der Glastafel mit organisch gebundenen Malfarben verziert, während aufzubrennende Schmelzfarben das Glas in der Glasmalerei schmücken. Der wesentliche Unterschied offenbart sich in der Lichtführung: Hinterglasbilder werden ausschließlich bei auffallendem Licht betrachtet. Der Malvorgang bei hintermalten Gläsern verläuft grundsätzlich von vorne nach hinten, da der Malgrund zugleich die Schauseite darstellt. Dieser Band, dessen Grundlage ein von der DFG gefördertes Forschungsvorhaben „Die Hinterglasmalerei in Flandern, Burgund und am Niederrhein von 1330 bis 1550. Ursprünge der ›kalten Malerei‹ auf Glas unter Berücksichtigung der Einflüsse durch die Glas- und Tafelmalerei“ ist, möchte einen Beitrag dazu leisten, die Kunstform der Hinterglasmalerei als eigenständige Kunstgattung zu etablieren. KW - Archäometrie KW - Kunst- und Kulturgut KW - ZfP PY - 2016 SN - 978-3-422-07262-6 SP - 1 EP - 340 PB - Deutscher Kunstverlag CY - Berlin AN - OPUS4-39222 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Farke, M. A1 - Binetti, M. A1 - Hahn, Oliver T1 - Light damage to selected organic materials in display cases: A study of different light sources N2 - The protection of works of art and cultural assets against light-induced aging is vital when planning exhibitions. Newly developed lighting systems render the selection of suitable light sources more difficult, not least in the context of energy–economical systems. This study accordingly examines different lighting systems (fluorescent tubes, halogen lamps, low-voltage metal halide lamps, and LED lamps) in terms of the damage potential they hold for the materials concerned. The changes in color were evaluated using the CIEDE2000 color-difference formula. This study focuses on selected organic materials and shows that changes in color already occur after only a brief exposure time. The color changes induced by the fluorescent tubes were consistently more intense than those induced by the other light sources. The results obtained with the remaining lamps show that the color changes depend more on the material under investigation than on the source used. The changes determined after a relatively short exposure period (five months) vividly demonstrate that exposing sensitive materials to light for longer terms (as is the case during a permanent exhibition) is most definitely a non-viable option. KW - Light damage KW - Non-destructive testing KW - Cultural heritage KW - Preventive conservation PY - 2016 DO - https://doi.org/10.1179/2047058414Y.0000000148 SN - 0039-3630 VL - 61 IS - Supplement 1 SP - S83 EP - S93 AN - OPUS4-39099 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Hahn, Oliver ED - Russel-Smith, Lilla ED - Konczak-Nagel, Ines T1 - Scientific investigation in arts and and culture N2 - The investigation of cultural assets often deals with the question of provenance, dating, or attribution to artists or workshops. The analysis of physical properties and chemical composition generates important data for answering cultural-historical questions that cannot be solved by stylistic and art-historical methods alone. Starting from some wooden painted architectural elements from Kocho and one from Bezeklik (III 8592), this paper aims to give some insights into the multi-instrumental approach to the analysis of cultural artefacts. KW - Archaeometry KW - X-ray fluorescence spectroscopy KW - Raman-spectroscopy KW - VIS-spectrophotometry KW - Scanning electron microscopy PY - 2016 SN - 978-3-88609-786-9 SP - 135 EP - 142 AN - OPUS4-38817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Hahn, Oliver ED - Gonella, Julia ED - Weis, Friederike ED - Rauch, Christoph T1 - Scientific investigation of carbon inks – an analytical challenge N2 - The investigation of physical properties and chemical composition generates data important for answering art-historical questions. Due to technological developments, technical diagnostics in art and culture are in ever-greater demand in such fields of transdisciplinary research. Based on one example, a collar drawing from the Berlin Diez albums, the present paper aims to give some insights into the multi-instrumental approach in the material analysis of cultural artefacts. The same methods were also applied to other drawings from the Diez Albums. KW - Archaeometry KW - X-ray fluorescence KW - Visible spectrophotometry KW - Non-destructive analysis PY - 2017 SN - 9789004323483 DO - https://doi.org/10.1163/9789004323483_016 VL - 11 SP - 427 EP - 438 PB - Brill CY - Leiden AN - OPUS4-38818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Material analysis: authentication or forgery detection? N2 - The lecture will discuss the sensitive issue of authentication of the objects of cultural heritage of immense cultural and monetary value if certified to be genuine. It will be made clear that material analysis alone, especially its non-destructive variety conducted by specialists in a single technique, can not prove that the object is genuine. The best material analysis can do, after all appropriate tests have been conducted, is to announce that nothing has been found that contradicts the assumption of genuineness. Moreover, the results of the natural analysis can never be used as the only justification of the authentication in the cases of composite objects such as manuscripts or epigraphs. A certification always requires the expertise of the specialist in the field (be it a historian, paleographer, epigrapher, etc.), whose judgment can be at the most supported by appropriate material analysis. The most effective approach for testing suspicious artifacts has been established by the forensic science. Here, not the authentication, but the determination of the forgery stands in the focus of the work. Investigation protocols developed within 150 years and constantly improved include a clear statement of the analysis purpose and the definition of plausibility criteria for the possible outcome. The younger sister of the forensics, archaeometry has to overcome additional obstacles such as the heterogeneity of historic material coupled with the scarcity of suitable reference material. Over the last two decades the popularity of archaeometric studies has increased enormously, with the industry-driven development of so-called non-destructive technologies (NDT) that do not require sampling. Further technological developments led to the appearance of NDT methods with extremely small interaction windows (µm range). Each of these methods has limitations that have to be carefully considered when planning the tests of a heterogeneous and often partially degraded historical material. This approach is inherently multi-instrumental, therefore archaeometric and forensic departments unite a number of specialists who work together defining the tasks and the methods involved for their successful completion. T2 - 2nd International Conference on Art & Archaeology CY - Jerusalem, Israel DA - 11.12.2016 KW - Archaeometry KW - Forgery KW - Cultural heritage PY - 2016 AN - OPUS4-39188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mota Gassó, Berta A1 - Schmidt, Wolfram A1 - Pauli, Jutta A1 - Sturm, Heinz T1 - Influences of hydration effects on the flow phenomena of concrete with admixtures N2 - Today, chemical admixtures like superplasticisers and stabilising agents are extremely important for modern concrete technology. These agents have meanwhile become common practice in concrete technology, but the understanding within the entire system lags far behind their application. The macroscopic rheology of concrete in the presence of superplasticizers strongly depends upon effects on a much smaller scale such as the hydration of the cement, the adsorption of superplasticizers, and the pore solution chemistry. T2 - 2nd International Conference on the Chemistry of Construction Materials CY - München, Germany DA - 10.10.2016 KW - Rheology KW - Cement KW - Superplasticiser PY - 2016 SN - 978-3-936028-96-6 VL - 50 SP - 276 EP - 279 PB - Gesellschaft Deutscher Chemiker e.V. CY - Frankfurt am Main AN - OPUS4-38849 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver T1 - Tinten und Tuschen – Die Schreib- und Zeichenmaterialien Adelbert Chamissos N2 - Im Nachlass Adelbert Chamissos, der in der Staatsbibliothek zu Berlin aufbewahrt wird, finden sich einige Zeichnungen – Lineamente – deren Inhalt rätselhaft ist. So ist nicht klar, was diese Zeichnungen darstellen und in welchem Zusammenhang sie entstanden sind. Die wenigen Aufschriften lassen weder eine eindeutige Identifizierung noch Datierung zu. Erste naturwissenschaftliche Untersuchungen widmen sich der Entstehungsgeschichte dieser Zeichnungen, der verwendeten Materialien und dem Auffinden möglicher Referenzen, um die Objekte in das Werk Chamissos einzuordnen. T2 - Öffentlicher Workshop des Internationalen Kollegs für Kulturtechnikforschung und Medienphilosophie in Kooperation mit dem Goethe-und Schiller-Archiv Weimar, Konzeption: Hanns Zischler CY - Weimar, Germany DA - 11.11.2016 KW - Archäometrie KW - Zerstörungsfreie Prüfung KW - Röntgenfluoreszenzanalyse KW - Reflektographie KW - Autograph KW - Graphik PY - 2016 AN - OPUS4-38819 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver A1 - Krug, Sonja T1 - Mobile Röntgenfluoreszenzanalyse und begleitende Methoden zur Bestimmung von Bioziden in Artefakten N2 - Der Schädlingsbefall durch Insekten stellt eines der großen Probleme in vielen Museen und historischen Bauten dar. Daher wird seit dem 18. Jahrhundert durch Einbringung von toxischen Wirkstoffen versucht, den Schädlingsbefall zu verhindern. Die verwendeten Wirkstoffe umfassen ein weites Spektrum unterschiedlicher Substanzen: Dazu gehören Arsen-, Quecksilber- und Bleiverbindungen; jedoch auch chlororganische Verbindungen, wie DDT, PCP, Lindan, Eulan , Methoxychlor sowie Triphenylmethan, Permethrin, Sulfonamid-Derivate, Diphenyl-Harnstoff-Derivate und Phosphoniumsalze. Wann und welche Mengen tatsächlich eingesetzt wurden, ist selten dokumentiert und daher die Risiken für die Gesundheit der Beschäftigten bzw. eventuelle Beeinträchtigungen für die Kunstwerke nach bisherigem Kenntnisstand nicht abzuschätzen. Zur Ermittlung des Gefahrenpotentials der Biozide und zur Einschätzung der Wirksamkeit von Auswaschverfahren sind schnelle, effiziente und kostengünstige Methoden notwendig. Da es in vielen Sammlungen nicht möglich ist, Objektproben zu entnehmen, sollen die Nachweisverfahren zudem zerstörungsfrei sein. Aufgrund der der verwendeten unterschiedlichen Biozide und der Vielfältigkeit der damit kontaminierten Objekte existiert bislang keine universelle Methode, die dieses leisten kann. Da viele Biozide entweder anorganischer Natur sind oder charakteristische Markerelemente wie Brom oder Chlor aufweisen, bietet sich die Röntgenfluoreszenzanalyse (RFA) als Nachweismethode an. Allerdings ergeben sich einige Probleme, welche die Aussagekraft des analytischen Verfahrens beeinflussen. Zunächst einmal handelt es sich um eine reine Elementanalyse, d. h. aus dem Vorhandensein eines bestimmten Elementes lässt sich nicht von vorne herein auf ein bestimmtes Biozid zurückschließen. Eine weitere Schwierigkeit liegt in der exakten Quantifizierung des jeweiligen Elementes. Die zu untersuchenden Objekte sind u. U. sehr heterogen zusammengesetzt; es ist nicht bekannt, ob das Biozid nur auf der Oberfläche aufliegt oder ob es tiefer in die Matrix eingedrungen ist und inwieweit es gleichmäßig auf das Objekt aufgetragen wurde. Diese Schwierigkeiten sind bereits in einigen Publikationen allgemein thematisiert worden und sollen anhand eines Fallbeispiels konkreter ausgeführt werden. In dieser Feldstudie soll weiterhin deutlich gemacht werden, dass zusätzliche analytische Verfahren notwendig sind, um exakte Angaben über die Art und die Konzentration der verwendeten Biozide zu machen. T2 - Kontaminiert - Dekontaminiert CY - Munich, Germany DA - 16.10.2014 KW - Biozide KW - Zerstörungsfreie Prüfung KW - Röntgenfluoreszenzanalyse KW - Arbeitsschutz PY - 2016 SN - 978-3-86222-225-4 VL - 13 SP - 66 EP - 74 PB - Volk Verlag CY - München AN - OPUS4-38923 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram T1 - Potentials for savings in the production of self-compacting and high strength concrete for precast concrete elements N2 - Over the course of the last decades, concrete construction has significantly changed from mass application towards sophisticated more innovative, future oriented, and performance based materials technology. Today concrete no longer consists of cement, water, and aggregates, but can be enhanced significantly by using supplementary additions and chemical admixtures. Advancements in admixtures eventually facilitated the development of new concrete types such as self-compacting concrete (SCC) and high performance concrete (HPC) by uncoupling the workability from the water-cement ratio (w/c). While for traditional concrete types the major mixture parameter for the workability and strength were the w/c and the grading of the aggregates, for SCC and HPC the performance parameters are more complicated and the performance depends highly on the powder components. This makes the system more sophisticated and in parallel more prone to scatter during the production. The complexity and difficulty to predict the effects of changes in the process and mixture makes it very difficult to identify the right potentials for savings. T2 - ICCX Central Europe CY - Ossa, Poland DA - 11.02.2016 KW - Rheology KW - Self-compacting concrete KW - High strength concrete KW - Packing density KW - Superplasticizers PY - 2016 SP - 18 EP - 20 AN - OPUS4-36883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Baumer, Ursula A1 - Dietemann, Patrick A1 - Hahn, Oliver A1 - Obermeier, Andrea A1 - Stege, Heike A1 - Steger, Simon A1 - Steuer, Christoph A1 - Walcher, Jeanine ED - Geiger, Gisela ED - Bretz, Simone T1 - Die Malmaterialien der Hinterglasbilder Heinrich Campendonks N2 - Die Zusammensetzung der Malfarben Heinrich Campendonks in ihrer Kombination aus Farbpigmenten, Bindemitteln und Metallpulvern ist bislang nahezu unerforscht. Lediglich für wenige Leinwandgemälde des Künstlers liegen publizierte Untersuchungen zu den Farbmitteln vor. Materialanalysen zu den Hinterglasarbeiten des Malers fehlten bisher. Im Rahmen eines Forschungs- und Restaurierungsprojektes im Zeitraum von 2014 bis 2016 wurden naturwissenschaftliche Untersuchungen an ausgewählten Hinterglasbildern durchgeführt, deren Ergebnisse in diesem Aufsatz vorgestellten werden. Die Untersuchungen erfolgten zunächst nicht-invasiv mit VIS-Spektroskopie, Röntgenfluoreszenzanalyse sowie Ramanspektroskopie, weiterhin mit Licht- und Fluoreszenzmikroskopie, Rasterelektronenmikroskopie mit energiedispersiver Röntgenmikroanalyse, Fourier-Transformations-Infrarotspektroskopie, Raman-Mikroskopie und Gas-Chromatografie/Massenspektrometrie. KW - Hinterglasmalerei KW - Kunsttechnologie KW - Kunst- und Kulturgut PY - 2017 SN - 978-3-86832-320-7 SP - 78 EP - 89 PB - Wienand Verlag CY - Köln AN - OPUS4-39325 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Rabin, Ira A1 - Schütz, Roman ED - Elgvin, Torleif ED - Langlois, Michael ED - Davis, Kipp T1 - Samples from the cylindrical jar MS 1655/1 N2 - The aim of our work was to check whether the assumption that the jar was discovered in Qumran can be substantiated. In order to establish the archaeological provenance of the jar we conducted a series of analytical tests on samples of material collected from the jar in April and June 2009. The samples were either found loose within the jar, these being probably constituted by remnants of its original contents, or were clay detached from the inner and outer surface of the jar. In addition, a portion of sand deposit coating the inside of the jar handles was analysed. KW - Archaeometry KW - Cultural heritage KW - Dead Sea scrolls PY - 2016 SN - 978-0-5671-1300-9 SN - 978-0-5672-8571-3 VL - 71 SP - 377 EP - 392 PB - Bloomsbury T&T Clark Series CY - New York, NY 10018 USA AN - OPUS4-39229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bretz, Simone A1 - Walcher, Jeanine A1 - Hahn, Oliver A1 - Stege, Heike ED - Geiger, Gisela ED - Bretz, Simone T1 - Bronzen, Brokatbronzen, Metall- oder Brokatfarben. Metalleffektpigmente in der Hinterglasmalerei Heinrich Campendonks N2 - Eine maltechnische Eigenart der Hinterglasbilder Heinrich Campendonks liegt in der Verwendung von fein gemahlenen unedlen Metallen wie Kupfer, Zinn, Zink, Aluminium sowie Metalllegierungen wie Messing. Sie waren seinerzeit entweder in Pulverform oder als gebrauchsfertige Malfarben im Handel erhältlich und wurden meist Bronzen, vereinzelt auch Brokatbronzen, Metall- oder Brokatfarben genannt. Der Aufsatz stellt die wesentlichen Aspekte der Metalleffektpigmente in Campendonks Werk vor. KW - Hinterglasmalerei KW - Kunsttechnologie KW - Kunst- und Kulturgut PY - 2017 SN - 978-3-86832-320-7 SP - 90 EP - 95 PB - Wienand Verlag CY - Köln AN - OPUS4-39326 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Observations on writing materials of the DSS N2 - The experimental knowledge about the inks of antiquity and late antiquity rarely goes beyond their visual description. In rare cases, inks typology has been determined by means of microscopy and reflectography, i.e. using their physical and optical properties, respectively. Soot, plant, and iron gall inks form different typological classes of historical black writing materials. Soot ink is a fine dispersion of carbon pigments in a water-soluble binding agent; plant-based ink consists of tannin solution; iron gall-ink presents a boundary case between soot and plant ink— a water soluble preliminary stage (similar to inks from the second group) oxidizes and evolves into a black, insoluble material (similar to the carbon pigments of the first group) when the writing is exposed to air. Each ink class has distinct properties that would readily permit their easy differentiation, if only these historical inks always belonged to just one of the classes above. In reality, inks may contain additives that obscure a clear picture. All the black inks of the DSS have been hitherto identified as soot inks. Yet some manuscripts, with 1QapGen ar among them, display ink corrosion that is incompatible with the pure soot ink. This type of corrosion commonly observed in medieval manuscripts written with iron gall inks, results from the catalytic action of metallic component in the ink. Early analysis of this ink conducted by Nir El and Broshi in 1996 found copper in the corrosive inks and attributed its presence to the use of bronze inkwells. Re-investigation of the 1QapGen ar ink suggests, however, that the ink composition, soot + copper, agrees well with the ink recipe recorded in the 1st century CE by Dioscorides. Similar inks have been already attested on contemporary Egyptian papyri. The first part of the paper is dedicated to the new results on the inks and corrosion pattern of the 1QapGen ar. In the second part of the presentation I will focus on the luxury scrolls, a distinct codicological type introduced by E. Tov. Our studies show that the preparation of the writing materials cannot supplement the list of codicological criteria offered by Tov. Therefore, one can divorce the writing material production from its inscription in contrast with the medieval scriptoria practices that included parchment production and copying of the manuscripts. T2 - Society of Biblical Literature (SBL) Annual Meeting 2016 CY - San Antonio, TX, USA DA - 19.11.2016 KW - Archaeometry KW - Dead Sea Scrolls KW - Cultural heritage KW - Manuscripts PY - 2016 AN - OPUS4-39189 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Continuities in writing material from the Dead Sea scrolls to medieval hebrew manuscripts N2 - The international Qumran project coordinated at the BAM, Berlin, resulted in an integrated methodology for determining the original and acquired properties of the skin-based writing surfaces of the Dead Sea Scrolls. This methodology offers a powerful tool for addressing such questions as the provenance, sorting and comparison of manuscripts. In addition, we have developed specific protocols for on-site studies, which were successfully applied to the fragments from the Schøyen collection in Norway. Our studies show that the Dead Sea Scrolls writing surfaces can be divided roughly into three groups: leather, parchments of a light tint, and those of various shades of brown. The latter ones are invariably tanned, whereas the middle group is characterized by the presence of various inorganic salts. Some of the pale parchments, among them the Temple Scroll (11Q19), are remarkably similar to medieval European parchment. Therefore we have formulated the working theory that in the Judaea of the Hellenistic period two different parchment-making traditions existed side by side: an ‘eastern’ one (represented by the tanned parchments of Qumran, closely resembling Aramaic documents from the fifth century BC, and a ‘western’ one (represented by the untanned/lightly tanned ones similar to early Christian Greek parchments). This division has found support during our first pilot study of the Geniza fragments, in which Babylonian and Palestinian traditions seem to follow the “eastern” and “western” technologies, respectively. The evolution and socio-geographic distribution of writing inks in late Antiquity and the early Middle Ages build the second focus of the BAM group. We use X-ray fluorescence analysis (XRF) to determine the chemical composition of the inks and NIR-reflectography for their typology. Here the early appearance of the metal containing inks clearly belongs to the western tradition as opposed to the continuous use of soot inks in the East. T2 - The Texts of the Bible from the Dead Sea Scrolls to the Biblical Manuscripts of the Vienna Papyrus Collection CY - Jerusalem, Israel DA - 10.04.2016 KW - Archaeometry KW - Non-destructive testing KW - Cultural heritage KW - Manuscripts PY - 2016 AN - OPUS4-39191 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Material study of inks N2 - Our experimental knowledge about the inks of antiquity and late antiquity rarely goes beyond their visual description. In rare cases, inks typology has been determined by means of microscopy and reflectography, i.e. using their physical and optical properties, respectively. Soot, plant, and iron gall inks form different typological classes of historical black writing materials. Soot ink is a fine dispersion of carbon pigments in a water-soluble binding agent; plant-based ink consists of tannin solution; iron gall-ink presents a boundary case between soot and plant ink— a water soluble preliminary stage (similar to inks from the second group) oxidizes and evolves into a black, insoluble material (similar to the carbon pigments of the first group) when the writing is exposed to air. Each ink class has distinct properties that would readily permit their easy differentiation, if only these historical inks always belonged to just one of the classes above. In reality, inks may contain additives that obscure a clear picture. Even crude observations suggest that the inks of antiquity differed greatly in their composition. We believe, that reconstructing the ink recipes with the help of advanced non-destructive analytical techniques could serve as a powerful accessory in the studies of ancient papyri. The proposed paper will present a short survey of the methods of material analysis and the challenges offered by ancient inks. (Two) examples of ink studies from the collections of the Israel Museum in Jerusalem and Egyptian Museum in Berlin will conclude the paper. T2 - 28th international congress of papyrology CY - Barcelona, Spain DA - 01.08.2016 KW - Archaeometry KW - Writing inks KW - Cultural heritage KW - Non-destructive testing PY - 2016 AN - OPUS4-39190 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram ED - Beushausen, Hans T1 - Application of a cusum control system for enhanced robustness of the flow properties of self-compacting concrete N2 - Control chart systems are used in quality management systems to keep production processes stable. In concrete production they are often applied for the control of the compressive strength. The most efficient control chart systems are cumulated sums (cusum), which help to observe deviations from a targeted value. Unlike alternative observation chart systems that focus on process data evaluation, cusum observations react very rapidly on systematic process changes in processes. Therefore, the cusum method is particularly suitable if immediate counteractions have to be taken, like in the case of fresh concrete properties of self-compacting concrete (SCC), which can have severe influences on the durability and mechanical strength of concrete. The rheology of SCC can be affected by an enormous variety of influencing factors, from raw material properties to handling or environmental temperature. The present study shows that regardless of the material based influencing parameter for a rheology change, a steady slump flow can be achieved only by adding supplementary superplasticizer in case of loss of flow and adding stabilising agent (ST) in case of increased flow if the respective V-mask indicates a systematic change. A reference SCC was artificially manipulated in order to achieve realistic experimental data for flowability and flowability changes due to changes in the raw material properties. The results point out that productions with applied cusum methods were capable of keeping the target slump flow deviation within approximately 1% only, while productions without applied cusum method deviated up to 14% and more from the target. T2 - fib Symposium 2016. Performance-Based Approaches for Concrete Structures. CY - Cape Town, South Africa DA - 21.11.2016 KW - Concrete KW - Self-compacting concrete KW - cusum KW - control chart KW - quality control KW - robustness PY - 2016 SN - 978-2-88394-121-2 SP - 106-1 EP - 106-10 PB - Fédération internationale du béton ( fib) CY - Lausanne, Switzerland AN - OPUS4-40976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram T1 - Influence of nano scale effects on the macroscopic rheology N2 - Chemical admixtures like superplasticisers or stabilising agents are of ever increasing importance for modern concrete technology. They liberate the workability of concrete from its dependency on water content, and thus, open the gate towards innovative and future oriented concrete technologies. Meanwhile admixtures have become common practice in concrete technology, but the understanding of these highly complex polymers in the entire concrete system lags far behind their application. Due to its complex time-dependent, multi-phase and multi-scale behaviour, flowable concrete systems are highly complicated and cannot be described comprehensively by simple models. It is therefore extremely challenging to identify the relevant parameters that predominantly control flow phenomena on different size scales, since these may occur on any scale between the nano scale (e.g. superplasticizer adsorption) and macro scale (e.g. grading of the aggregates). The present study discusses fundamental mechanisms at the interface between particle or hydrate surfaces and the fluid phase at a very early stage of concrete formation, and links these effects to macroscopic flow phenomena. Based on the observations of the nano scale effects, it seems that higher sensitivity against variations in the constituents, the handling, or the boundary condition are the inevitable price for higher performances. However, eventually a very effective method is introduced that helps to maintain stable processes regardless of the root cause for performance changes based on an efficient in-situ process control scheme and superplasticizer and stabilising agents as counter actions. T2 - International Workshop on Nano-Engineered Meta-materials for Civil Infrastructures CY - Jinan, China DA - 20.5.2017 KW - Rheology KW - Meta materials KW - Nano engineering KW - Admixtures KW - Cement KW - Ettringite PY - 2017 AN - OPUS4-41032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Priebe, Nsesheye Susan T1 - Obtaining optimum workability using RHA in a modified cementitious system N2 - In order to reduce CO2 emission in concrete and minimize the environmental impact, majority of research focuses on using supplementary cementitious materials (SCMs) such as Fly Ash (FA), blast furnace slag (GGBS) and Silica Fume (SF) or Microsilica as a replacement for ordinary Portland cement in concrete. However, in terms of sustainability, it is not economically feasible to use the above mentioned SCMs in countries where these materials are not readily available. In addition, when dealing with the carbon footprint of concrete, despite their positive influence in concrete, such SCMs cannot be said to be eco-friendly materials due to their high energy production process. In many developing countries in sub-Saharan Africa (SSA), agriculture is the leading economic sector. Generally, agricultural by-products are eco-friendly in terms of low energy in production, and they often have no further use for the environment. These by-products (baggase, cassava peels and rice husks) are mainly not the materials of discussion in this current day and age and especially in the northern hemisphere, where the majority of concrete technology originates. Hence, it is inevitable to consider other more sustainable resources in concrete for SSA. Nevertheless, optimization of these resources in concrete can only function with a clear understanding of the reactivity of the materials and its interaction and mechanism to adopt similar and workable properties as a normal performance cementitious system. This paper addresses rice husk ash (RHA) as a main SCM in various cementitious systems with added limestone filler (LSF) and observes its performance in mortar. Superplasticizers such as polycarboxylate-ethers (PCEs) and lignosulphonates (LS) are incorporated in the cementitious systems to improve workability. The interaction of RHA with the superplasticizers was investigated by means of zeta potential (ZP). According to the results presented, it is shown that RHA powder has a positive compatibility with the chosen superplasticizers and its performance in mortar with LSF also shows increase in strength and workability. T2 - International Concrete Sustainability Conference CY - Washington DC, USA DA - 15.05.2016 KW - Superplaticizers KW - Supplementary cementitious materials; KW - Sub-Saharan Africa KW - Rice husk ash KW - Cement KW - Concrete PY - 2016 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. AN - OPUS4-41033 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Priebe, Nsesheye Susan T1 - Optimising available resources for good concrete properties N2 - There is a wide range of research worldwide on supplementary cementitious materials (SCMs) such as fly ash and slag for substituting Portland cement. Such materials are suitable to be considered in a cementitious system with ordinary Portland cement (OPC) due to their high pozzolanic properties. In addition, many of the SCMs are said to significantly improve concrete properties especially in terms of strength and durability. Unfortunately, the production of such SCMs is not entirely eco-friendly and also limited to certain parts of the world, hence one has to look at alternative options. The issue of availability of resources is a strong concept that is ever-increasing, and the use of more eco-friendly SCMs in a cementitious system is furthermore attractive. Hence this paper addresses the use of eco-friendly SCMs in concrete such as rice husk ash (RHA). Despite the fact that extensive research has been done on this material, its application in a cementitious system to obtain sufficient concrete properties is still rather limited. In a country like Tanzania, high strength concrete construction is applicable in special construction cases but certainly not a high priority. Majority of construction is still undertaken using normal strength concrete. In a ternary cementitious system consisting of OPC, RHA and other readily available resources such as limestone filler (LSF), normal strength concrete can still be produced having good performance and suitable for regular on-site construction. This paper explains a possible application of obtaining sufficient concrete properties from the available resources. T2 - 2nd Conference in Advances in Cement and Concrete Technology in Africa CY - Dar es Salaam, Tanzania DA - 27.01.2016 KW - Sub-Saharan Africa KW - Rice husk ash KW - Admixtures KW - Strength KW - Workability PY - 2016 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. AN - OPUS4-41030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Łojewska, J. A1 - Rabin, Ira A1 - Pawcenis, D. A1 - Bagniuk, J. A1 - Aksamit-Koperska, M.-A. A1 - Sitarz, M. A1 - Missori, M. A1 - Krutzsch, M. T1 - Recognizing ancient papyri by a combination of spectroscopic, diffractional and chromatographic analytical tools N2 - Ancient papyri are a written heritage of culture that flourished more than 3000 years ago in Egypt. One of the most significant collections in the world is housed in the Egyptian Museum and Papyrus Collection in Berlin, from where the samples for our investigation come. The papyrologists, curators and conservators of such collections search intensely for the analytical detail that would allow ancient papyri to be distinguished from modern fabrications, in order to detect possible forgeries, assess papyrus deterioration state, and improve the design of storage conditions and conservation methods. This has become the aim of our investigation. The samples were studied by a number of methods, including spectroscopic (FTIR, fluorescent-FS, Raman) diffractional (XRD) and chromatographic (size exclusion chromatography-SEC), selected in order to determine degradation parameters: overall oxidation of lignocellulosic material, degree of polymerization and crystallinity of cellulose. The results were correlated with those obtained from carefully selected model samples including modern papyri and paper of different composition aged at elevated temperature in humid air. The methods were classified in the order SEC > FS > FTIR > XRD, based on their effectiveness in discriminating the state of papyri degradation. However, the most trustworthy evaluation of the age of papyri samples should rely on several methods. KW - Archaeometry KW - FTIR KW - XRD KW - Raman KW - Chromatography KW - Papyrology PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-428704 DO - https://doi.org/10.1038/srep46236 SN - 2045-2322 VL - 7 SP - 46236, 1 EP - 46236, 12 AN - OPUS4-42870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schütz, Roman A1 - Bertinetti, L. A1 - Rabin, Ira A1 - Fratzl, P. A1 - Masic, A. T1 - Quantifying degradation of collagen in ancient manuscripts: the case of the Dead Sea Temple Scroll N2 - Since their discovery in the late 1940s, the Dead Sea Scrolls, some 900 ancient Jewish texts, have never stopped attracting the attention of scholars and the broad public alike, because they were created towards the end of the Second Temple period and the 'time of Christ'. Most of the work on them has been dedicated to the information contained in the scrolls' text, leaving physical aspects of the writing materials unexamined. They are, however, crucial for both historical insight and preservation of the scrolls. Although scientific analysis requires handling, it is essential to establish the state of degradation of these valued documents. Polarized Raman Spectroscopy (PRS) is a powerful tool for obtaining information on both the composition and the level of disorder of molecular units. In this study, we developed a non-invasive and non-destructive methodology that allows a quantification of the disorder (that can be related to the degradation) of protein molecular units in collagen fibers. Not restricted to collagen, this method can be applied also to other protein-based fibrous materials such as ancient silk, wool or hair. We used PRS to quantify the degradation of the collagen fibers in a number of fragments of the Temple Scroll (11Q19a). We found that collagen fibers degrade heterogeneously, with the ones on the surface more degraded than those in the core. KW - Dead Sea Scrolls KW - Collagen KW - Raman spectroscopy PY - 2013 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-331769 DO - https://doi.org/10.1039/c3an00609c SN - 0003-2654 SN - 1364-5528 VL - 138 IS - 19 SP - 5594 EP - 5599 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-33176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Cohen, Zina A1 - Olszowy-Schlanger, Judith A1 - Hahn, Oliver A1 - Rabin, Ira ED - Wandrey, T1 - Composition analysis of writing materials in Geniza fragments N2 - Our current projects focus on the material analysis of the writing materials kept in the Taylor-Schechter Collection at Cambridge University Library, which houses the largest collection of Cairo Geniza fragments, about 190,000. Although Geniza manuscripts have attracted a great deal of scholarly attention, the material aspects of these documents seem to have been largely neglected. The current study aims to obtain information on the composition of the writing supports and the inks that were used, the production of the original manuscripts and the history of their degradation. The collected data should supplement the description based on Hebrew palaeography and codicology. Moreover, a characterisation of the writing materials would provide insights on trade, local production techniques and social structures. The tabulated results have the potential to be used as geo-chronological markers if sufficient data is collected. For our study, we chose Hebrew legal documents and letters from three communities that co-existed in Fustat (today Cairo) in the 11th century: the Jerusalemite (or ‘Palestinian’) community, the Babylonian community and the Karaites, three different communities with different scribal traditions. In addition to this, we studied non-biblical scrolls attributed to the Palestinian and Babylonian communities. The question we addressed was whether we can correlate the use of a specific type of ink to an objective criterion. For our analysis at Cambridge University Library, we used a number of protocols developed at BAM (Bundesanstalt für Materialforschung und -prüfung) in Berlin and at the Centre for Study of Manuscript Cultures, University of Hamburg (CSMC). These include reflectographic examination followed by non-destructive X-ray fluorescence (XRF) analysis using transportable instruments so that the analysis can be carried out in situ. We have illustrated our approach here by providing two examples. The first one describes our investigation of the leather fragment containing a portion of the Babylonian Talmud on its hair side (TS Misc.26.53.17). The second example illustrates our ability to compare iron-gall inks using the XRF method. In this case, we explored the question of the codicological attribution of three fragments (TS F17.4, TS 12.755 and TS 12.756) to the same Talmud manuscript. KW - Cairo Genizah PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-435590 DO - https://doi.org/10.1515/9783110546422-013 VL - 13 SP - 323 PB - de Gruyter CY - Berlin AN - OPUS4-43559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabin, Ira A1 - Gordon, Nehemia A1 - Calvillo, Nelson T1 - Coloured Ruling Lines in a Fourteenth-Century Ashkenazi Torah Scroll N2 - Rabbinic halakhah required that Torah scrolls be written with relief ruling, horizontal and vertical lines scored into the writing surface. Coloured ruling with plummet or ink would make a Torah scroll invalid for liturgical use. Ruling lines on some leather fragments of early Oriental Torah scrolls give the impression of being produced with plummet or ink but may be the result of dust in the furrows of relief ruling. Erfurt 9, a fourteenth-century Ashkenazi Torah scroll, has coloured ruling, which is partial secondary re-ruling, on 13 of the 34 surviving sheets, perhaps added when the original relief ruling was difficult to see. The coloured ruling in Erfurt 9 is brown, giving it the visual appearance of iron-gall ink. However, XRF tests showed that the only meaningful metallic component in the coloured ruling was lead (Pb). Lead plummet ruling tends to have a greyish appearance. Black specks under near infrared light are consistent with minium, a lead-based red ink that can turn brown when it degrades. Partial secondary re-ruling added with minium to the original relief ruling comes as a surprise as it would have rendered Erfurt 9 unfit for liturgical use. KW - Hebrew Manuscripts KW - Ruling Lines KW - Coloured Ink PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-628531 DO - https://doi.org/10.25592/uhhfdm.17169 SN - 2410-0951 VL - 10 SP - 9 EP - 32 AN - OPUS4-62853 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver T1 - Kunsttechnologie, Terminologie und Vergänglichkeit von farbigen Zeichenmitteln N2 - Eine Vielzahl unterschiedlicher Materialien findet für die farbliche Gestaltung von Zeichnungen Verwendung. Einige Pigmente und Farbstoffe, d.h. Tinten, Stifte oder Kreiden, waren nur für den Gebrauch als Zeichenmittel vorgesehen – andere wiederum finden sich auch in der Tafel- oder Fassmalerei. Der Vortrag möchte zunächst einen kurzen Überblick über die Terminologie und die Kunsttechnologie farbiger Zeichenmittel geben, um den Kosmos dieser Vielfältigkeit zu illustrieren. Im zweiten Teil des Vortrags rücken dann solche „farbige“ Elemente in den Fokus, deren Konnotation sich aus den Zeichnungen nicht erschließen lassen und die daher zunächst irritieren. Die Farbigkeit war aber ursprünglich vielleicht gar nicht intendiert, sondern ist vielmehr auf Alterungs- und Korrosionsprozesse zurückzuführen. So steht eine braune Eisengallustinte nicht für die bewusste Verwendung eines braunen Zeichenmaterials, vielmehr dokumentiert sie das Vorhandensein brauner Korrosionsprodukte, die ein völlig anderes Erscheinungsbild ergeben. Die Alterungsprozesse betreffen aber nicht nur die Zeichenmaterialien, sondern auch das jeweilige Trägermaterial. Je nach Materialzusammensetzung verbräunen oder verdunkeln Papiere sehr stark, organische Farbstoffe – insbesondere gelbe Farben – bleichen sehr schnell aus, so dass kolorierte Partien nicht mehr lesbar sind. Die Charakterisierung bzw. Bestimmung des Materials ist mit dem bloßen Auge nicht immer möglich. Erst durch entsprechende naturwissenschaftliche Verfahren lässt sich eine Typologie der Zeichenmaterialien erstellen, Farbveränderungen erklären und der ursprüngliche Erscheinungszustand dieser Zeichnungen annähernd „rekonstruieren“. Es wird aufgezeigt, dass liebgewonnene Sicht- und Ausdrucksweisen, wie beispielsweise „Pinsel und Feder in Braun“ oder „Tinte in Sepiamanier“ heute so nicht mehr aufrechtzuerhalten sind. T2 - Farbe auf Zeichnungen der frühen Neuzeit - Symbiose und Antagonismus. Gernsheim-Studientage CY - Rom, Italy DA - 25.10.2017 KW - Archäometrie KW - Alterung KW - Farbe PY - 2017 AN - OPUS4-42713 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Golle, U. A1 - Hahn, Oliver A1 - Wintermann, C. ED - Knebel, K. ED - Ortlieb, C. ED - Püschel, G. T1 - Kunsttechnologische und materialwissenschaftliche Zugänge in der Restaurierung zu Parerga in Goethes naturwissenschaftlichen Sammlungen N2 - In Goethes naturwissenschaftlichen Sammlungen, die als Arbeits- und Studiensammlungen, zum Teil aber auch als Lehrsammlung für den Sohn August angelegt sind, haben sich sowohl die eigentlichen Sammlungsobjekte als auch deren vermeintlich ursprünglichen Kontexte durch Beschriftungen, Etiketten und in Teilen noch existierende Präsentationsmedien erhalten. Es stellt sich jedoch die grundsätzliche Frage nach deren Ursprünglichkeit. Präsentieren sich die Objekte noch so wie zur Goethezeit oder erfuhren die historischen Dichotomien im Laufe der Zeit Veränderungen, sodass die zeitgenössischen Präsentationsformen und die damit verbundenen didaktischen Funktionen heute nicht mehr lesbar sind? KW - Parerga KW - Paratext KW - ZfP KW - Archäometrie PY - 2018 SN - 978-3-95498-415-2 VL - 1 SP - 235 EP - 282 PB - Sandstein Verlag CY - Dresden AN - OPUS4-47043 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steger, Simon A1 - Oesterle, D. A1 - Mayer, R. A1 - Hahn, Oliver A1 - Bretz, S. A1 - Geiger, G. T1 - First insights into Chinese reverse glass paintings gained by non-invasive spectroscopic analysis-tracing a cultural dialogue N2 - This work presents a technical investigation of two Chinese reverse glass paintings from the late 19th and early 20th centuries. A multi-analytical, non-invasive approach (X-ray fluorescence (XRF), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), Raman spectroscopy) was used to identify the pigments and classify the binding media. The results reveal a combined use of traditional Chinese and imported European materials. Several pigments like cinnabar, lead white, orpiment, carbon black and copper-arsenic green (probably emerald green) were found in both paintings; red lead, artificial ultramarine blue, Prussian blue and ochre appear in at least one of the paintings. The proof of limewash (calcite and small amounts of portlandite) as a backing layer in Yingying and Hongniang indicates that clamshell white was also used for reverse glass paintings. Drying oil was classified as a binding media in most areas of both paintings. However, the orange background of The Archer yielded prominent bands of both proteinaceous and fatty binder. KW - Non-invasive analysis KW - Reverse glass painting KW - Pigment identification KW - DRIFTS KW - Raman spectroscopy PY - 2019 DO - https://doi.org/10.1007/s12520-019-00799-3 SN - 1866-9557 SN - 1866-9565 VL - 11 IS - 8 SP - 4025 EP - 4034 PB - Springer AN - OPUS4-47364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Schmidt, Wolfram A1 - Leinitz, Sarah A1 - Mota, Berta A1 - Crasselt, Claudia ED - Liu, Jiaping ED - Wang, Ziming ED - Holland, Terence ED - Huang, Jing ED - Plank, Johann T1 - Influence of the aqueous phase of cement paste on the rheology in the presence of PCE N2 - The paper presents rheometric results and hydration curves for cementitious systems based on cement mixed with different aqueous phases at solid volume fraction of  = 0.45. The varied aqueous phases were deionized water, limewater, the filter residue of a cement paste mixed at w/c = 2.0, and the filtrate of cement paste at solid volume fraction of 0.45. Each cementitious system provided different amounts and sizes of particles formed in the aqueous phase. The pastes were observed with and without polycarboxylate ether based superplasticizer. It was observed that the presence of particles causes higher PCE saturation dosages to achieve a minimum value, but the minimum value is only affected in the case of large particles. In all cases with and without PCE, the presence of small particles causes increased plastic viscosity. In addition, with decreased number and size of hydrates in the aqueous phase the hydration was retarded, which was specifically pronounced in the presence of PCE KW - Aqueous phase of cement paste KW - Polycarboxylate ether KW - Rheology KW - Yield stress KW - Plastic viscosity KW - Heat of hydration KW - Syngenite KW - Solid volume fraction PY - 2018 SN - 978-1-64195-029-9 SP - SP-329-34, 428 EP - 443 PB - American Concrete Institute CY - Farmington Hill, Michigan AN - OPUS4-47107 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steger, Simon A1 - Bretz, Simone A1 - Stege, Heike A1 - Hahn, Oliver T1 - Methodological approach for in situ spectroscopic analysis of modern reverse paintings on glass: A case study of Kreuzabnahme (1914/15) - an outstanding example by Carlo Mense N2 - A non-invasive methodological approach has been carried out to identify the pigments and classify the binding media of the reverse painting on glass Kreuzabnahme (1914/15) by Carlo Mense. Mense was a member of the group Rhenish Expressionists around August Macke and got interested in the technique of painting on the reverse side of a glass panel. The studied painting indicates a remarkably painted reverse and front side, which creates a unique visual appearance of the glass. The applied noninvasive, spectroscopic approach includes X-ray fluorescence, VIS spectroscopy, Raman spectroscopy and diffuse reflectance infrared Fourier transform spectroscopy. The measurements revealed inorganic Pigments mixed with drying oil as binder. Together with common pigments, such as lead white, barium sulphate, bone black, cinnabar, chrome yellow, ochre, and viridian, an unusual additional material was found, Strontium white. KW - Reverse glass painting KW - Non-invasive analysis KW - DRIFTS KW - Pigment identification PY - 2019 DO - https://doi.org/10.1140/epjp/i2019-12549-6 SN - 2190-5444 VL - 134 IS - 2 SP - 64, 1 EP - 8 PB - Springer CY - Berlin AN - OPUS4-47365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Noeller, Renate T1 - Análisis del material de los Códices Humboldt N2 - Los Códices Humboldt, que proceden de la época colonial de Mexico, muestran: 1. colores indígenas típicos y sus mezclas: cochinilla (rojo), índigo/ Azul Maya (azul y verde), carbón (negro), zacatlaxcalli, mangle, colores orgánicos (amarillo) 2. influencia colonial: tinta hierro- gálico para escribir 3. fragmentos distribuidos y cortados: partes singulares forman parte de otros fragmentos dentro de la colección (y en otras colecciones?) T2 - Seminario: Estudio comparativo de los manuscritos de la colección Manuscripta Americana (Berlín y Cracovia) con los manuscritos del Archivo General de la Nación y Museo Nacional de Antropología (México); Instituto de Investigaciones Estéticas; Universidad Nacional Autónoma de México (UNAM) CY - Mexico City, Mexico DA - 05.11.2018 KW - Humboldt Codices KW - XRF-, FTIR-, VIS-espectroscopía PY - 2018 AN - OPUS4-47560 LA - spa AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Noeller, Renate T1 - Análisis de los Códices HUMBOLDT Relacionado con fragmentos en méxico: de Mizquiahualla N2 - Los códices de Mizquiahualla MsAmer1 frag VII, XIII (XIV, XV) muestran: - colores indigenes: cochinilla (rojo), indigo (verde, azul), carbón (negro), zacatlaxcalli (amarillo) - papel indigen (amate) - pintura con líneas perfil en negro, pintado antes y después de la coloración - influencía colonial: escritura en tinta hierro- gálica (1571, 1569) T2 - Seminario: Estudio comparativo de los manuscritos de la colección Manuscripta Americana (Berlín y Cracovia) con los manuscritos del Archivo General de la Nación y Museo Nacional de Antropología (México) CY - INSTITUTO DE INVESTIGACIONES ESTÉTICAS, UNAM, Mexico DA - 05.11.2018 KW - Humboldt Codices KW - FTIR-, XRF-, VIS- espectroscopia PY - 2018 AN - OPUS4-47561 LA - spa AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Noeller, Renate T1 - Analysis of `Manuscripta Americana´ related to fragments in Mexico: Codex Techialoyan N2 - Techialoyan/ Central Mexico MsAmer7 shows limited colors: ochre (yellow, brown red, rose) indigo (blue, green, greyblue+?) cerussite + chalk (white) organic ink for writing (brown) T2 - Seminario: Estudio comparativo de los manuscritos de la colección Manuscripta Americana (Berlín y Cracovia) con los manuscritos del Archivo General de la Nación y Museo Nacional de Antropología (México) CY - INSTITUTO DE INVESTIGACIONES ESTÉTICAS, UNAM, Mexico DF DA - 05.11.2018 KW - XRF-, VIS- spectroscopy KW - Manuscripta Americana, Techialoyan PY - 2018 AN - OPUS4-47562 LA - spa AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cohen, Zina A1 - Schlanger, J. A1 - Hahn, Oliver A1 - Rabin, Ira T1 - Cairo Genizah documents of the 11th century: analysis of writing materials N2 - The Cairo Geniza is an “archive” discovered in the 19th century in Ben Ezra Synagogue in Fustat, a district in Old Cairo (Egypt). The collection of mostly Jewish documents that vary in genres, languages and writing supports contains a large number of early medieval Hebrew manuscripts. The Geniza provides sources for the literary, linguistic, historical studies of the various aspects Jewish life. As the documents attest, at least two Jewish communities co-existed in Fustat up to 11th century: a so-called Babylonian and Palestinian. These communities had different leaders, different traditions and lived independently. The differences seem to manifest themselves also in the paleographical, codicological and some material properties of the manuscripts produced by each community. The aim of this project is to compare the inks used in the Jewish documents depending on different variables: support (paper, parchment), purpose of the manuscript (legal, private, religious), provenance of the scribe. For the determination of the inks type and composition we had to choose non-invasive, non-destructive and portable techniques to analyze the corpus directly on-situ. The analyses were carried out with a micro-X-ray spectrometer ArtTAX® (Bruker GmbH) and a digital stereomicroscope features built-in LED illumination at 395 nm and 940nm, Dino Lite. We would like to stress that though the methods of material analysis listed above have been successfully employed in the field of cultural heritage and conservation including ancient and medieval manuscripts they have not yet been used to study fragments from the Cairo Genizah. Therefore, we believe that this research project is a pioneering study that will provide new insights into the history of Hebrew writing materials, their production techniques and materials and, thus, contribute new data to the field of Hebrew paleography. T2 - Konferenz Art&Archaeology2018 – 3rd International Conference CY - Jerusalem, Israel DA - 09.12.2018 KW - XRF KW - Ink KW - Manuscripts KW - Cairo Genizah KW - Reflectography PY - 2018 AN - OPUS4-47100 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cohen, Zina A1 - Rabin, Ira A1 - Schlanger, Judith T1 - Quelles informations une approche archéométrique peut-elle nous apporter pour enrichir notre connaissance des manuscrits hébreux et du monde de la Génizah du Caire ? N2 - L'archéométrie est une discipline riche qui peut nous apporter beaucoup d'informations sur l'étude des manuscrits et qui, conjuguée à la paléographie et la codicologie, peut s'apporter un outil précieux pour mieux appréhender les sociétés qui ont produits ces manuscrits. Nous verrons ici quelques exemples de techniques scientifiques non destructives, principalement appliqués à la Génizah du Caire, appliquées à l'étude des manuscrits. T2 - Tagung CY - Paris, France DA - 10.12.2018 KW - XRF KW - Ink KW - Archaeometry KW - Manuscripts KW - Non destructive PY - 2018 AN - OPUS4-47098 LA - fra AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Material analysis of manuscripts: methodological introduction N2 - Natural sciences play auxiliary role in the studies of manuscripts. The success of their contribution depends strongly on the formulation of the question and the choice of the methods to obtain the requested answer. Therefore, one should try to go beyond the understanding of the basic principles of the scientific analysis. We will start with a glance at the basic principles of the techniques used in the material science for determination of the elemental composition (X-ray emission) and molecular composition (FTIR & Raman). We will move then to the bench and mobile equipment commonly used in the field of cultural heritage. At the end we will choose a question to be answered and design an ideal experiment that will be modified according to the limitations dictated by on-site conditions. In the ateliers in the afternoon we will a) compare two XRF devices that differ in their spatial resolution; b) use a high resolution microscope (Keyence) to obtain a close look at writing surfaces and materials; c) we will learn to determine the type of the inks with the help of another microscope (DinoLite AD413T-12V), a usb microscope with visible, UV and NIR illumination; d) we will learn to use FTIR-ATR device for determination of the type of the writing surface; e) We will use mobile Raman device for identification of pigments. T2 - Summer School: Manusciences19 CY - Frejus, France DA - 10.03.2019 KW - Material science KW - Cultural heritage PY - 2019 AN - OPUS4-48137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier T1 - Scientific service project z02 at the CSMC: material science methods of reconstructing the history of manuscripts N2 - Z02 is one of the three technically supporting projects at the Centre for the Study of Manuscript Cultures (CSMC). In collaboration with the other two service projects, Z01 and Z03, it aims at bridging the gap between humanities and natural sciences and technology. To that purpose, we set up a laboratory with a range of high-end instruments, most of them mobile, allowing thorough non-destructive analysis of manuscripts. In addition to working on constantly improving the laboratory and the methods of analysis, a substantial part of our activities is dedicated to service, by supporting different research projects conducted at the centre. In this talk, we will present our equipment and the possibilities offered by the different techniques available regarding the different kinds of missions: typology and classification of inks, provenance studies, recovery of faded inscriptions and palimpsests, reconstruction of the history of manuscripts, authentication and dating. We will give a brief overview of our past and ongoing activities in the frame of the second phase of the CSMC. Finally, a selection of three projects will be presented in greater detail to highlight the possibilities of our laboratory and the diversity of missions which can be carried out. T2 - International Medieval Conference CY - Leeds, United Kingdom DA - 01.07.2019 KW - Manuscript KW - Ink KW - Pigment PY - 2019 AN - OPUS4-48465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Crasselt, Claudia T1 - Influence of rheology modifying admixtures on early hydration of cementitious suspensions N2 - The presence of polycarboxylate ether (PCE) based superplasticizers (SPs) has enormous influence on the early hydration of cement. C3A as the most reactive phase of Portland cement plays a significant role in early hydration reactions and affects the rheological performance. Therefore, this talk presents experimental results about the influence of delayed addition of PCEs on the Hydration of alite and C3A-gypsum pastes investigated by isothermal heat flow calorimetry. Complementary in-situ XRD was carried out on C3S and C3A-gypsum pastes to analyze hydration and phase changes related to the addition of PCE. Cement pastes with a delayed addition of PCE showed less retardation compared to simultaneous addition. The alteration caused by PCE is much more pronounced for C3A-gypsum mixes. With a delayed addition of SP, the hydration of C3A is less retarded or even accelerated. It is obvious that there is less retardation the later the addition of SP. Furthermore, the PCE alter the hydration of C3A when added delayed and exhibit changes in kinetics and Hydration rates. XRD results showed that more C3A is dissolved in the presence of PCE. Also, the gypsum depletion occurs earlier in the presence of PCE and even faster with delayed addition. Without PCE AFm starts to form just after the gypsum depletion. However, in the presence of PCE AFm already starts to form at the beginning of the hydration. Due to the faster gypsum depletion in the presence of PCE, also the transformation from ettringite into AFm begins earlier, but takes longer as without SP. T2 - 15th International Congress on the Chemistry of Cement CY - Prague, Czech Republic DA - 16.09.2019 KW - Cement KW - Alite KW - C3S KW - C3A KW - Early hydration KW - Polycarboxylate ether (PCE) KW - Delayed addition PY - 2019 AN - OPUS4-49103 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Analyzing historic inks: From antiquity to the Middle Ages. N2 - While studying the socio-geographic history of inks, division 4.5 of the Bundesanstalt für Materialforschung und Prüfung (BAM) together with the Centre for the Study of Manuscript Cultures (CSMC) in Hamburg has developed a non-invasive protocol for ink analysis. It consists of a primary reflectographic screening to determine the type of the ink (soot, tannin or iron-gall) and a subsequent in-depth analysis using several spectroscopic techniques: X-ray fluorescence (XRF), Infrared and Raman spectroscopies. The first of them, XRF elemental analysis aims at establishing the unique fingerprints of inks containing metals or trace elements in carbon inks. In addition, we use Raman analysis to identify so-called mixed inks, an ink category that received little attention so far. Finally, with the help of IR spectroscopy we obtain information about the ink binders. T2 - Coptic Literature in Context. The Contexts of Coptic Literature Late Antique Egypt in a dialogue between literature, archaeology and digital humanities CY - Rom, Italy DA - 25.02.2019 KW - Ink PY - 2019 AN - OPUS4-48135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier T1 - XRF ink analysis of selected fragments from the Herculaneum collection N2 - Hundreds of papyrus rolls, carbonized during the 79CE eruption of Mount Vesuvius, were discovered in 1754 at Herculaneum. Sophisticated mechanical methods for unrolling the best-preserved scrolls have been applied, with varying success. However, such processes have been abandoned, to prevent risk from irremediable damage or loss and to preserve the integrity of the extremely fragile rolls. Following the development of X-ray based non-invasive techniques, attempts to virtually unroll the scrolls were made. The most common ink in Antiquity was carbon-based, and the main element of carbonized papyrus is carbon, making these investigations difficult. However, some attempts with synchrotron X-ray phase-contrast tomography (XPCT) were successful. Recently, the identification of antique inks containing metals raised hope that if some of the inks contain metal the rolls can be virtually unrolled using conventional CT- technique. We are presenting here the first results of a preliminary analysis, which aimed at identifying scrolls whose ink contains metals. T2 - Konferenz: 29th International Congress of Papyrology CY - Lecce, Italy DA - 28.07.2019 KW - Herculaneum KW - Papyrus KW - Tomography KW - XRF KW - Ink PY - 2019 AN - OPUS4-48615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Evolution of writing black inks N2 - The evolution and socio-geographic distribution of writing inks from Late Antiquity to the Middle Ages are one of the foci of our investigative work at the Bundesanstalt für Materialforschung und -prüfung (BAM) in Berlin and the Centre for the Study of Manuscript Cultures, Hamburg University. This presentation will examine the inks used by Jews in the in different geographical zones try to correlate the results of the material analysis with written records and existing traditions. We will compare the inks proposed by Maimonides, who lived in 12th-century Egypt, with the considerations of Rashi, who lived in 11th-century northern France, and see that they both advocated use of the inks commonly known and produced in their respective regions. It is Maimonides who proposes to add tannins to the soot inks, but rejects the metallic salt, both of which were practices that were well attested in contemporary Arabic recipes for making ink. In contrast, Rashi was favourable to employing the plant inks in use in contemporary Northern Europe. T2 - Jewish-Christian Relations from the Mediterranean to the Indian Ocean: Evidence from Material Culture CY - Bochum, Germany DA - 26.03.2019 KW - Ink KW - Jewish cultures PY - 2019 AN - OPUS4-48136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Zorn, Sabine A1 - Bosch, S. A1 - Hahn, Oliver ED - Klemm, D. ED - Stolzenburg, A. T1 - Materialtechnologische Untersuchungen an vier Zeichnungen Leonardo da Vincis aus dem Kupferstichkabinett N2 - Das Kupferstichkabinett der Hamburger Kunsthalle besitzt seit seiner Gründung vier Zeichnungen von Leonardo da Vinci (1452–1519). Sie sind Teil eines umfangreichen Legats des Hamburger Kunsthändlers Georg Ernst Harzen, das der Stadt Hamburg für die 1869 eröffnete Kunsthalle als Besitz übereignet wurde. Die Zeichnungen gelten aufgrund ihrer Provenienzen und stilistischen Verankerung im Werk Leonardos als gesichert. Weiterführende materialtechnologische Untersuchungen wurden nun erstmals anlässlich der Ausstellung »Leonardo da Vinci – Die Zeichnungen im Hamburger Kupferstichkabinett« durchgeführt. KW - Zerstörungsfreie Prüfung KW - Zeichnung KW - Leonardo da Vinci PY - 2019 SN - 978-3-938002-56-8 SP - 128 EP - 135 PB - Druckhaus Köthen CY - Köthen AN - OPUS4-49667 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver T1 - Zerstörungsfreie Prüfverfahren zur Authentifizierung von Manuskripten und Zeichnungen – Möglichkeiten und Grenzen N2 - Untersuchungen von Zeichnungen und Manuskripten mit zerstörungsfreien Methoden haben in den letzten Jahren enorm zugenommen. Die nicht-invasiven Analysen ermöglichen Informationen zur Herkunft, zum Herstellungsprozess und möglicherweise zum Alter (direkte Dating nicht möglich, Ausnahme: Papierstruktur, Wasserzeichen). Die zerstörungsfreien Analysen können Rückschlüsse auf mögliche Fälschungen geben, sind neben den offensichtlichen Vorteilen jedoch auch mit einzelnen Limitierungen behaftet. Der Vortrag soll anhand einiger Fallbeispiele die Möglichkeiten aber auch Grenzen bei der zerstörungsfreien (mobilen) Auffindung von Fälschungen aufzeigen. T2 - PTS Workshop"Materialwissenschaftliche Untersuchungsmethodenzur Charakterisierung und Authentifizierung von Dokumenten und Kunstwerken auf Papier" CY - Heidenau, Germany DA - 07.11.2019 KW - ZfP KW - Authentifizierung KW - Papier PY - 2019 AN - OPUS4-49666 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver A1 - Wintermann, C. T1 - Braune Tinten – Geschichte und Materialität N2 - Eine Vielzahl unterschiedlicher Materialien findet für die Gestaltung von Zeichnungen Verwendung. So sind es insbesondere „braune Tinten“, welche die Zeichnungen dominieren. Der Vortrag möchte zunächst einen kurzen Überblick über die Terminologie und die Kunsttechnologie farbiger Tinten geben, um den Kosmos dieser Vielfältigkeit und auch deren Vergänglichkeit zu illustrieren. Der zweite Teil des Vortrags ist dann den sogenannten Bistertinten und deren analytischen Nachweisen gewidmet. Es handelt sich um Zeichentinten, die aus den wasserlöslichen Bestandteilen von Kaminruß gewonnen werden. Die farbliche Bandbreite reicht von gelb-orange bis braun. Zuweilen wurden diese Tinten mit weiteren Pigmenten versetzt, um eine bestimmte Farbtiefe zu erzielen. T2 - 29. Treffen der Grafikrestauratoren CY - Weimar, Germany DA - 25.10.2019 KW - Zerstörungsfreie Prüfung KW - Zeichenmaterialien KW - Archäometrie PY - 2019 AN - OPUS4-49731 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Hahn, Oliver A1 - Golle, U. A1 - Wintermann, C. ED - Knebel, K. ED - Maul, G. ED - Schmuck, T. T1 - Schwarz auf Weiß N2 - In der Sammlung des Naturwissenschaftlichen Kabinetts Johann Wolfgang von Goethes wird ein eher unscheinbares Stück Papier aufbewahrt, welches einen grauschwarzen Aufstrich aufweist. Bei genauerer Betrachtung glaubt man, drei Querstreifen mit rötlicher, weißlicher und bläulicher Farbe innerhalb des grauschwarzen Aufstrichs zu erkennen. Das Papier weist oben die Skizze eines Prismas, im mittleren Bereich am rechten Rand die Beschriftungen „violett/blau“, „weiß“ sowie „gelb/roth“ auf. Interessanterweise ist die Aufschrift „violett/blau“ dem eher rötlichen, die Aufschrift „gelb/roth“ dem eher bläulichen Querstreifen zugeordnet. Die rechte untere Ecke ist mit „Sk“ (Seebeck?) gekennzeichnet. Sowohl die Beschriftungen als auch die Skizze wurden mit einem Graphitstift ausgeführt. Das Papier ist auf eine Pappe mit Papprahmen geklebt und mit schwarzem Papier umwickelt. Es ist unumstritten, dass es sich bei diesem Objekt um das Ergebnis eines naturwissenschaftlichen Experiments handelt, doch was stellt es dar und lässt sich die ursprüngliche Versuchsanordnung aus dem vorliegenden Befund und weiterer, heute zugänglicher naturwissenschaftlichen Untersuchungen rekonstruieren? KW - Zerstörungsfreie Prüfung KW - Farbenlehre KW - Papier KW - Johann Wolfgang von Goethe PY - 2019 SN - 978-3-95498-486-2 SP - 354 EP - 357 PB - Sandstein Verlag CY - Dresden AN - OPUS4-49668 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Wolfram A1 - Mota, Berta A1 - Ramirez Caro, Alejandra T1 - Einfluss der gesteinskörnung auf die Rheologie von Beton N2 - Die meisten Einflüsse auf die Rheologie von Beton wirken auf sehr kleinen Skalenebenen. Einflussgrößen im Millimeter oder Zentimeterbereich sind im Wesentlichen auf den Sand und die Gesteinskörnung beschränkt. Letztere machen aber in den meisten Betonen 50 %-70 % des Gesamtvolumens aus, was bei Untersuchungen zur Steuerung der Verarbeitungseigenschaften von Beton häufig vernachlässigt wird. Während Betonzusatzmittel und Zusatzstoffe bei geeigneter Wahl die Rheologie sehr gezielt beeinflussen können, eignen sich Sand und Gesteinskörnung weniger gut zur Steuerung der Rheologie, aber sie tragen zur Rheologie des Gesamtsystems bei. Hierbei können Effekte aus Sand und Gesteinskörnung die Effekte von Zusatzmitteln und Zusatzstoffen überlagern und im ungünstigsten Falle sogar nahezu unwirksam machen. Deshalb sollten Ergebnisse zur Verarbeitbarkeit von Bindemittelsystemen nur mit großer Sorgfalt auf Beton übertragen werden. Es ist wichtig, den Einfluss des Sandes und der Gesteinskörnung besser zu verstehen, um diese so abzustimmen, dass sie Effekte aus Fließmitteln positiv ergänzen anstatt diesen entgegenzuwirken. Durch eine gezielte Abstimmung lassen sich Kosten wirksam sparen. KW - Gesteinskörnung KW - Rheologie KW - Fließgrenze KW - Viskosität KW - Beton PY - 2018 VL - 3 SP - 42 EP - 51 PB - ad-media GmbH CY - Köln AN - OPUS4-47044 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon T1 - Disclosing a new aspect in modern European art: multidisciplinary analysis of modern reverse paintings on glass (1905-1955) N2 - The technique of painting on the reverse side of a glass panel was rediscovered by German artists at the beginning of the 20th century. They appreciated the impressive gloss, luminosity, and depth of colours in this genre. Compared to stained glass, the distinctive properties of this technique are: (1) the paint is applied “cold”, hence, it doesn’t involve a firing step, (2) reverse paintings on glass are framed and always viewed in reflected light and (3) the reverse paint stratigraphy is different from canvas paintings, starting with the front most layer and ending with the backing layer. In 1908 several artists, including Gabriele Münter, Wassily Kandinsky, Heinrich Campendonk, August Macke and Franz Marc of the “Der Blaue Reiter” (the Blue Rider) collective took an interest in this technique and started to share their interest with other colleagues in Europe. Our pioneering project is tracing this transfer of knowledge by a multidisciplinary approach in terms of art history, paint technology and material science. More than 100 artists and >1000 reverse paintings on glass were identified during the project. This high number of objects clearly points out that this technique was by far more important for modern art than previously assumed. In-situ, non-invasive measurements (XRF, Raman, VIS, DRIFTS) on a well-considered selection of 67 paintings reveal the broad palette of colorants ranging from traditional to experimental. Special attention is paid to the impact of synthetic organic pigments (SOP) in artists palette. Demonstrative examples by W. Kandinsky, L. G. Buchheim and F. Jespers are used to discuss analytical challenges and highlights. T2 - Art & Archaeology 2018 CY - Jerusalem, Israel DA - 09.12.2018 KW - Reverse glass painting KW - Spectroscopy KW - In-situ analysis PY - 2018 AN - OPUS4-47042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier T1 - Scientific service project z02 at the csmc: material-science methods of reconstructing the history of manuscripts N2 - Z02 is one of the three technically supporting projects at the Centre for the Study of Manuscript Cultures (CSMC). In collaboration with the other two service projects, Z01 and Z03, it aims at bridging the gap between humanities and natural sciences and technology. To that purpose, we set up a laboratory with a range of high-end instruments, most of them mobile, allowing thorough non-destructive analysis of manuscripts. In addition to working on constantly improving the laboratory and the methods of analysis, a substantial part of our activities is dedicated to service, by supporting different research projects conducted at the centre. In this talk, we will present our equipment and the possibilities offered by the different techniques available regarding the different kinds of missions: typology and classification of inks, provenance studies, recovery of faded inscriptions and palimpsests, reconstruction of the history of manuscripts, authentication and dating. We will give a brief overview of our past and ongoing activities in the frame of the second phase of the CSMC. Finally, a selection of projects will be presented in greater detail to highlight the possibilities of our laboratory and the diversity of missions which can be carried out. T2 - Konferenz: Art & Archaeology 2018 CY - Jerusalem, Israel DA - 09.12.2018 KW - Manuscripts KW - Inks KW - CSMC KW - Pigments PY - 2018 AN - OPUS4-47039 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Crasselt, Claudia T1 - Influence of rheology modifying admixtures on hydration of cementitious suspensions N2 - The state of fresh concrete is predominantly determined by the rheological properties of the cement paste. In order to control performance spectra and requirements of novel concretes and to better understand macroscopic phenomena, comprehensive knowledge of the material behavior of fresh cement suspensions as well as of the complex relationships of mechanisms at the nano and micro scale are necessary. This work focuses on micro and nano rheology of suspensions of cementitious model systems and the influence of polycarboxylate-based admixtures on the rheology. The phenomena are driven by multiple parameters such as adsorption and particle interactions. Hence, the first part examines the interaction between polycarboxylate ether (PCE) and synthesized clinker phases and hydration products as model systems with regard to early hydration products. T2 - 6th International Symposium on Nanotechnology in Construction CY - Hong Kong, China DA - 02.12.2018 KW - Cement KW - Early hydration KW - Polycarboxylate ether (PCE), PY - 2018 AN - OPUS4-46980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cohen, Zina T1 - Writing materials analysis of 11th century Cairo Genizah's fragments N2 - This study focuses on the analysis of a corpus of manuscripts found in Fustat (medieval Cairo, Egypt) in the biggest medieval “archive” found until now: the Cairo Geniza. The giant collection of mostly Jewish documents has been attracting scholars’ attention a lot but so far, the material aspects of these documents seem to have been mainly neglected. Application of scientific methods of analysis, especially X-Ray fluorescence characterization, contributes to our understanding of the materials used for production of manuscripts during the Middle ages. Our corpus of the 11th century manuscripts comprises manuscripts written by scribes belonging to three Jewish communities that co-existed in Cairo during this period: the Karaites, the so-called Jerusalemites (or Palestinian) and the so-called Babylonians (or Iraqi), three different communities with different traditions and different leaders. The differences manifest themselves also in the paleographical properties of the manuscripts produced within each community. Can we extend the differences detected by the paleographical analysis to differences in composition of the writing materials and especially the composition of the inks? Or can we relate the differences in the composition to the manuscript type (legal, private...), or to another criterion. In this presentation, we offer answers to some of the questions using statistical analysis of the measurements results. T2 - Konferenz 6th Meeting “X-ray and other techniques in investigations of the objects of cultural heritage” CY - Cracow, Poland DA - 17.05.2018 KW - Ink KW - Manuscript KW - XRF analysis PY - 2018 AN - OPUS4-46045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cohen, Zina T1 - Comment l'archéométrie et une approche matérielle de manuscrits du XIe siècle de la Genizah du Caire peuvent-elles nous aider à mieux comprendre le monde juif médiéval ? N2 - Le monde de la Génizah du Caire et plus particulièrement la collection de Cambridge (CUL) a recu l’attention des chercheurs depuis le XIXe siècle mais peu de recherches ont été faites à ce jour sur l’aspect matériel des manuscrits. Pourtant l’archéométrie est un outil précieux pour mieux comprendre les sociétés qui ont créés ces documents. T2 - Konferenz IXe journée d’études doctorale et postdoctorales en paléographie et diplomatique hébraïque CY - Paris, France DA - 05.12.2017 KW - XRF Analysis KW - Archaeometry KW - Medieval Jewish manuscripts KW - Cairo Genizah PY - 2017 AN - OPUS4-46124 LA - fra AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steger, Simon A1 - Stege, H. A1 - Bretz, S. A1 - Hahn, Oliver T1 - A complementary spectroscopic approach for the non-invasive in-situ identification of synthetic organic pigments in modern reverse paintings on glass (1913–1946) N2 - This work addresses the identification of synthetic organic pigments (SOP) in eight modern reverse paintings on glass (1913–1946) by means of an in-situ multi-analytical approach. We combined the complementary properties of mobile Raman spectroscopy and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) to overcome the main disadvantages of each method: extensive band overlapping in DRIFT spectra and fluorescence problems in Raman spectra. A collection of DRIFTS reference spectra enables a precise pigment identification by DRIFTS and establishes this method as a serious non-destructive alternative for the identification of SOP. The group of β-naphthol pigments yielded valuable results for both methods, whereas synthetic alizarin (PR83) was preferentially detected by DRIFTS. Finally, uncommon triaryl carbonium pigments and two azo group-based yellows were identified in the paintings by means of Raman spectroscopy. KW - Synthetic organic pigments KW - DRIFTS KW - Raman spectroscopy KW - Reverse glass painting PY - 2019 DO - https://doi.org/10.1016/j.culher.2019.01.011 SN - 1296-2074 SN - 1778-3674 VL - 38 SP - 20 EP - 28 PB - Elsevier Masson SAS. AN - OPUS4-48008 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram T1 - Effects and potentials of plant based chemical admixtures on the performance of cementitious construction materials N2 - While today, engineers can choose from a wide range of rheology modifying admixtures, in some parts of the world, these are difficult to access, due to their complex processing. However, alternatives can be bio-based polymers such as polysaccharides from various sources. These are easily accessible all over the world, do not demand for complicated processing, and typically they are more sustainable than many established materials, which are crude oil-based. The paper presents the effects of acacia gum, cassava starch and the gum of triumfetta pendrata A. Rich on the rheological performance of cementitious systems. It is shown that acacia gum can be as efficient as polycarboxylate based superplasticisers, cassava starch can reduce the yield stress slightly with little effect on the plastic viscosity, and the gum of triumfetta pendrata A. Rich increases the thixotropy of cement pastes with plasticizing polymers significantly. T2 - International Conference on Sustainable Materials, Systems and Structures (SMSS 2019) CY - Rovinj, Croatia DA - 20.03.2019 KW - Polysaccharides KW - Rheology KW - Cement KW - Chemical admixtures KW - Bio-based concrete PY - 2019 AN - OPUS4-47675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Material studies of historic inks: From antiquity to the Middle Ages N2 - While studying the history of inks, division 4.5 of the BAM (Bundesanstalt für Materialforschung und Prüfung) together with the Centre for the Study of Manuscript Cultures in Hamburg has developed a protocol for ink analysis. It consists of a primary screening to determine the type of the ink, and a subsequent in-depth analysis using several spectroscopic techniques. One of them, X-ray Fluorescence (XRF) aims primarily at establishing the fingerprints of inks containing metals, making it possible to distinguish among different inks. Our research aims primarily at recreating a socio-geographic history of inks, parchment, and papyrus and includes the comparative analysis of the writing materials of the Dead Sea Scrolls, ink and papyrus in Ancient and Hellenistic Egypt, and inks in documents from various contemporary medieval communities in Fustat (first nucleus of Cairo) as well as other medieval Jewish and Armenian communities. The presentation shows the panorama of historic inks and our attempt to follow up the transition of the inks from those based on soot to the iron-gall inks commonly used in the Middle Age. T2 - Kolloqium CY - KIT, Germany DA - 17.05.2019 KW - historic inks PY - 2019 AN - OPUS4-48131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Evolution of writing black inks N2 - Our research aims primarily at recreating a socio-geographic history of inks, parchment, and papyrus and includes the comparative analysis of the writing materials of the Dead Sea Scrolls, ink and papyrus in Ancient and Hellenistic Egypt, and inks in documents from various contemporary medieval communities in Fustat (first nucleus of Cairo) as well as other medieval Jewish and Armenian communities. The presentation shows the panorama of historic inks and our attempt to follow up the transition of the inks from those based on soot to the iron-gall inks commonly used in the Middle Age. T2 - Elephantine Salon CY - Ägyptisches Museum Berlin, Germany DA - 22.03.2019 KW - Carbon ink KW - Iron-gall ink KW - Historic ink PY - 2019 AN - OPUS4-48134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon T1 - First insights into Chinese reverse glass paintings gained by non invasive spectroscopic analysis N2 - A non-invasive methodological approach (X-ray fluorescence (XRF), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), Raman spectroscopy) has been carried out to identify the pigments and classify the binding media in two Chinese reverse glass paintings (The Archer, Yingying and Hongniang) from the late 19th and early 20th centuries. The results reveal a combined use of traditional Chinese and imported European materials. Several pigments like cinnabar, lead white, orpiment, carbon black and copper-arsenic green (probably emerald green) were found in both paintings; red lead, artificial ultramarine blue, Prussian blue and ochre appear in at least one of the paintings. The presence of portlandite (Ca(OH)2) along calcite (CaCO3) in the fine-grained, white backing layer of Yingying and Hongniang indicates the presence of limewash. In Chinese tradition, limewash was produced from clamshells, and was then sold as clamshell white. In contrast to the Japanese pigment, Chinese clamshell white was made of finely grounded shells, which were heated over a low fire. The residue (CaO) forms portlandite (Ca(OH)2) when water is continuously added. This water-rich mixture is applied on the painting. Portlandite reacts with atmospheric CO2 during drying and forms fine-grained calcite (CaCO3) [1,2]. The identification of emerald green (The Archer) suggests an earliest manufacturing date in the 1830s [3] and promotes the sinological dating of the painting. Drying oil was classified as a binding media in most areas of both paintings. However, the orange background of The Archer yielded prominent bands of both proteinaceous and fatty binder. T2 - Technart2019 CY - Bruges, Belgium DA - 07.05.2019 KW - Reverse glass painting KW - Raman spectroscopy KW - Non-invasive analysis PY - 2019 AN - OPUS4-48010 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Material studies of the Dead Sea Scrolls N2 - Our study is dedicated to non-destructive characterization of the support and the inks of the DSS. To that aim we use micro-XRF, 3D- SY-XRF, different IR methods including synchrotron radiation based reflectance spectroscopy, optical and electron microscopy. The lecture discusses advantages and the shortcomings of the non-destructive testing approach. T2 - Seminar CY - Freie Universität Berlin, Germany DA - 04.02.2019 KW - Dead Sea Scrolls PY - 2019 AN - OPUS4-48132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Materialwissenschaftliche Untersuchungen an Qumranrollen N2 - Heute stimmen die meisten Gelehrten und Historiker darin überein, dass die Höhlen von Qumran eine Essener-Bibliothek beherberg-ten. Über ihren Ursprung, sowie die Herkunft der einzelnen Schriften, wird noch immer rege debattiert. Der aktuelle Beitrag präsentiert detaillierte Lösungsansätze zu Klärung der Provenienzfrage der Schriftrollen von Qumran. T2 - Vorlesungsreihe CY - Freie Universität Berlin, Germany DA - 14.01.2019 KW - Qumranrollen PY - 2019 AN - OPUS4-48133 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon T1 - Non-invasive Identifizierung von Pigmenten in modernen Hinterglasbildern (1905-1955) - Highlights aus der Hinterglasforschung N2 - Im Rahmen des Projektes „Hinterglasmalerei als Technik der Klassischen Moderne von 1905 – 1955“, welches vom Museum Penzberg – Sammlung Campendonk, Penzberg (Gisela Geiger und Diana Oesterle) geleitet wurde und in Zusammenarbeit mit der freischaffenden Restauratorin Simone Bretz, der Bundesanstalt für Materialforschung und -prüfung (BAM) und dem Doerner Institut erfolgte, konnte im Rahmen einer Promotion erstmals ein Konvolut von mehr als 60 Hinterglasbildern mit nicht-invasiven Analysemethoden untersucht werden. Die eingesetzten Verfahren ermöglichten die Identifizierung der Pigmente und eine Klassifizierung der verwendeten Bindemittel. Die materialwissenschaftliche Beschäftigung mit der Hinterglaskunst in ihrer Vielfalt ist ein relativ junges Forschungsfeld. Lange wurde ihr mit Unkenntnis, Missverständnis und sogar Geringschätzung begegnet. Im kunsthistorischen Kontext wurde diese Art der Kaltmalerei zumeist mit dem Begriff der Glasmalerei belegt und nicht als eigenständige Kunstform anerkannt, da in beiden Fällen Glas als Bildträger seinen Einsatz findet. In der Hinterglasmalerei wird die Tafelrückseite mit organisch gebundenen Malfarben verziert und das Werk ausschließlich bei auffallendem Licht betrachtet. Die künstlerische Herausforderung liegt immer in der technischen Notwendigkeit eines umgekehrten Malvorganges: die oberste, durch das Glas sichtbare Schicht muss zuerst auf den Bildträger Glas aufgetragen werden, der optische Hintergrund wird zuletzt aufgebracht. Im Vergleich zum Tafelbild, bei dem die Malerei erst durch den Firnisauftrag Tiefenlicht erhält, entfalten die Farben in der Hinterglasmalerei bereits beim Malen ihre Intensität und erhalten gleichzeitig Schutz durch den gläsernen Bildträger (Bretz et al. 2016). Neben der kunstgeschichtlichen und kunsttechnologischen Bearbeitung der Hinterglasbilder spielten materialwissenschaftliche Untersuchungen an einer Auswahl von 66 Bildern im Rahmen des von der VolkswagenStiftung finanzierten Forschungsprojektes eine zentrale Rolle. Grundsätzlich wurde ein nicht-invasiver Ansatz gewählt, um die fragilen Kunstwerke in-situ zu messen und somit einen Transport zu vermeiden. Die Methodik umfasst neben VIS-Spektrometrie in Reflexion und energiedispersiver Röntgenfluoreszenzanalyse (RFA) auch Infrarotspektroskopie in diffuser Reflexion (DRIFTS) und Raman-Spektroskopie. Mit Hilfe des gewählten methodischen Ansatzes lassen sich sowohl anorganische als auch organische Pigmente identifizieren und die Zusammensetzung von Metallfarben und Folien sowie die Glaszusammensetzung qualitativ bestimmen. Ferner ermöglicht die DRIFT-Spektroskopie eine Klassifizierung der Bindemittel. Die im Rahmen des Forschungsprojektes analysierten Hinterglasbilder können folgendermaßen chronologisch gruppiert werden: 1910-1919 (17 Bilder), 1920-1929 (18 Bilder), 1930-1939 (6 Bilder), 1940-1949 (7 Bilder), 1950-1955 (13 Bilder) und >1955 (5 Bilder). Die Auswertung der Ergebnisse ermöglicht grundsätzliche Aussagen über die verwendeten Malmaterialien in Hinterglasbildern in der ersten Hälfte des 20. Jahrhunderts und zeigt Änderungen der verwendeten Pigmente im zeitlichen Kontext auf. Während der ersten Hälfte des 20. Jahrhunderts kamen viele neue Pigmente und Malmaterialien auf den Markt, wobei speziell die synthetischen organischen Pigmente (SOP) zu nennen sind. Eine Vielzahl an SOP konnte in Hinterglasbildern aus allen Zeitgruppen identifiziert werden, wobei hier vor allem Farblacke aus synthetischem Alizarin (PR83), Vertreter der roten und orangen β-Naphthol Pigmente [(z.B. PR3, PR4, PO5 (in Nächtliche Fahrt, 1921 von L. Hildebrandt nachgewiesen)], die blauen und grünen Kupferphthalocyanine [z.B. PG7, PB15 (taucht ab 1949 in Hinterglasbildern auf)] und einige gelbe Azopigmente [z.B. PY1, PY3, PY12 (in Geneigter Mädchenkopf, 1941 von Oskar Schlemmer gefunden)] aufzuführen sind (Steger et al. 2018; Steger et al. 2019a). Einige seltene SOP der Triarylcarboniumgruppe konnten ebenso nachgewiesen werden. Darunter fallen neben der Identifizierung von PR81 (Ohne Titel, 1954, M. Uhlenhuth) auch die erstmaligen Nachweise von PV2 (Hahn, um 1945, L.-G. Buchheim) und PG1 (Exzellente und einmalige Dressuren, 1945/46, L.-G. Buchheim) in Kunstwerken überhaupt (Steger et al. 2018; Steger et al. 2019a). Ferner konnten mit PB52 aus der Gruppe der Anthrachinone und PR60 aus der Gruppe der verlackten Naphthalin-Sulfonsäure-Pigmente weitere seltene SOP in den Bildern Rudern (um 1912) beziehungsweise Apokalyptischer Reiter II (1914) von Wassily Kandinsky nachgewiesen werden (Steger et al. 2019b). Neben den Entwicklungen der SOP können auch eindeutige Trends in den anorganischen Pigmenten veranschaulicht werden. Seltene anorganische Pigmente wie zum Beispiel Strontiumweiß (SrSO4) in der Kreuzabnahme (1914/15) von Carlo Mense (Steger et al. 2019c) wurden identifiziert. Neu entwickelte anorganische Pigmente wie zum Beispiel Cadmiumrot (Cd(S,Se); ab 1928 in 11 Hinterglasbildern nachgewiesen) oder Titanweiß (TiO2; Anatas kommt ab 1922 vor, Rutil konnte nur in Kissen der Träume, 1976 von Werner Schriefers identifiziert werden) tauchen in einigen Hinterglasbildern auf. Schweinfurter Grün (3Cu(AsO2)2·Cu(CH3COO)2) oder Strontiumgelb (SrCrO4) wurden in einigen Bildern bis etwa um 1925 gefunden; diese Pigmente konnten dagegen in späteren Bildern nicht mehr nachgewiesen werden. Als Beispiel sind hier vier frühe Hinterglasbilder (1909–1914) von Wassily Kandinsky zu nennen, wobei Strontiumgelb in vielen Bildpartien zu finden war (Steger et al. 2019b). Publizierte materialwissenschaftliche Ergebnisse von Kandinskys Leinwandgemälden aus späteren Werksperioden zeigen, dass Strontiumgelb zu dieser Zeit vollkommen aus seiner Palette verschwunden ist und vor allem durch ein anderes Gelbpigment, nämlich Cadmiumgelb, ersetzt wurde (McMillan et al. 2013). Eine materialtechnische Besonderheit in der Hinterglaskunst ist die Verwendung von Metallfolien und Metalleffektpigmenten. Metallfolien aus Silber, Zinn, Aluminium oder Messing wurden vielfach als künstlerisches Element in die Komposition integriert, wobei sie als finale Schicht auf, die bereits gestaltete, leicht transparente Malerei geklebt wurden. Durch die Betrachtung im auffallenden Licht erzeugten die Folien bemerkenswerte Glitzereffekte. Zinn- und Aluminiumfolien wurden zum Beispiel in Rudern (um 1912, W. Kandinsky) nachgewiesen, während Messingfolien häufig in Bildern von L.-G. Buchheim gefunden wurden. Die Zinnfolien wurden im 19. und frühen 20. Jahrhundert für Verpackungszwecke (z.B. Zigaretten, Schokolade) verwendet. Aluminiumfolie wurde erst ab 1910 industriell in der Schweiz hergestellt und zu Beginn vor allem für Schokoladenverpackungen eingesetzt (Skrabec 2016). Die frühe Verwendung solche Folien in Hinterglasbildern (z.B. Rudern, um 1912) zeigen eine rasche Verbreitung dieses Materials bei den Künstlern an. Unter Metalleffektpigmenten versteht man feingemahlene Pulver aus Metall (z.B. Zinn, Nickel, Kupfer) und Legierungen (z.B. Messing, Neusilber) mit unterschiedlichen Tönungen, welche bei seitlichem Lichteinfall auf Hinterglasbildern ein merkbares Funkeln erzeugen. Solche Metalleffektpigmente wurden vielfach bei Werken von Heinrich Campendonk nachgewiesen (Geiger und Bretz 2017) und konnten in allen chronologischen Gruppen gefunden werden. Grundsätzlich ermöglichen die Ergebnisse ein besseres Verständnis für die Technik der Hinterglasmalerei und helfen insbesondere, diese eigenständige Kunst im Hinblick auf die „klassische“ Tafel- bzw. Leinwandmalerei abzugrenzen. So zeigen Vergleiche mit Gemälden auf Leinwand von Wassily Kandinsky deutliche Unterschiede in den verwendeten Farbmitteln für beide Techniken. Die Anzahl von 66 gemessenen Hinterglasbildern von 39 Künstlern erscheint im Kontext von über 1200 Arbeiten, welche im Rahmen des Projektes lokalisiert werden konnten, gering. Allerdings können die durchgeführten Untersuchungen als Startpunkt für zukünftige Projekte in diesem Forschungsfeld, beispielsweise für einzelne Werkkomplexe verstanden werden. Die Forschungsergebnisse werden auf die Webseite www.hinterglas-klassischemoderne.de eingestellt. Im Sommer 2020 präsentiert das Museum Penzberg – Sammlung Campendonk Hinterglasbilder von 1910 bis 1960 als Abschlussausstellung des Forschungsprojektes. Die Ausstellung wird von einem ausführlichen Katalog über die fächerübergreifende Forschung begleitet. Für Herbst 2020 ist ein Hinterglas-Symposium an der Bundesanstalt für Materialforschung und -prüfung (BAM) Berlin im Rahmen eines N.i.Ke. Workshops geplant. T2 - Jahrestagung Archäometrie und Denkmalpflege 2019 CY - Vienna, Austria DA - 11.09.2019 KW - Reverse glass painting KW - Raman spectroscopy KW - DRIFTS PY - 2019 AN - OPUS4-49259 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Crasselt, Claudia A1 - Schmidt, Wolfram A1 - Sturm, Heinz T1 - Influence of rheology modifying admixtures on early hydration of cementitious suspensions N2 - The presence of polycarboxylate ether (PCE) based superplasticizers (SPs) has enormous influence on the early hydration of cement. C3A as the most reactive phase of Portland cement plays a significant role in early hydration reactions and affects the rheological performance. Therefore, this paper presents experimental results about the influence of delayed addition of PCEs on the Hydration of cement and C3A-gypsum pastes investigated by isothermal heat flow calorimetry. Complementary in-situ XRD was carried out on C3A pastes to analyze hydration and phase changes related to the addition of PCE. Cement pastes with a delayed addition of PCE showed less Retardation compared to simultaneous addition. The alteration caused by PCE is much more pronounced for C3A-gypsum mixes. With a delayed addition of SP, the hydration of C3A is less retarded or even accelerated. It is obvious that there is less retardation the later the addition of SP. Furthermore, the PCE alter the hydration of C3A when added delayed and exhibit changes in kinetics and hydration rates. XRD results showed that more C3A is dissolved in the presence of PCE. Also, the gypsum depletion occurs earlier in the presence of PCE and even faster with delayed addition. Without PCE AFm starts to form just after the gypsum depletion. However, in the presence of PCE AFm already starts to form at the beginning of the hydration. Due to the faster gypsum depletion in the presence of PCE, also the transformation from ettringite into AFm begins earlier, but takes longer as without SP. T2 - 15th International Congress on the Chemistry of Cement CY - Prague, Czech Republic DA - 16.09.2019 KW - Cement KW - C3A KW - Early hydration KW - Polycarboxylate ether (PCE) KW - Delayed addition PY - 2019 SP - 1 EP - 8 AN - OPUS4-49104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehring, Grzegorz T1 - Can an inkwell leak into ink? N2 - X-ray fluorescence analysis, due to its non-destructive nature and ist suitability to work with historic objects in situ, quickly became one of the most important methods for the evaluation of iron-gall ink. The main advantage of this qualitative and semi-quantitative method is that it makes it easy to differentiate between inks, based on the assumption that the differences result from the manufacture of the ink. This work explores the question whether the ink ‘fingerprint’ results strictly from the elemental composition of the basic ink ingredients even if it is stored in vessels made of metals or metal alloys. In addition, we tested and compared the performance of three different XRF spectrometers. We prepared various lab-grade inks according to historical ink recipes and measured the metal content of the ink deposited on sized cotton Linters paper with three types of XRF spectrometers: a simple hand-held device with an interaction spot of 4 mm and two devices equipped with poly-capillary Xray optics for line scanning and imaging. Since the exact elemental mass composition of the non-aged ink samples was known, we were able to evaluate the accuracy of the research procedure. Lab-grade inks were then aged in the metal jars imitating inkwells. The aging of the inks in the metal containers resulted in the significant change of the primary inks fingerprint as opposed to that of the control inks stored in glass containers. This effect was independently confirmed by the measurements conducted with every instrument we used. We will present a brief comparison of the results 43 achieved when using different spectrometers and a possible hypothesis explaining the processes that occurred. T2 - Konferenz -7th Meeting X-ray and other techniques in investigations of the objects of cultural heritage CY - Krakow, Poland DA - 17.05.2018 KW - Iron-gall ink KW - XRF KW - Inkwells KW - Ink composition KW - Performance comparison PY - 2018 AN - OPUS4-49157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nehring, Grzegorz T1 - What should we take into an account in the characterization of iron-gall ink by means of X-ray fluorescence? N2 - The earliest known recipes for iron gall inks include four basic ingredients: oak galls – pathological growths of oak leaves; metal salts – usually referred to as vitriol; a binder such as gum Arabic; and water. The final product differs in the elemental composition due to the multitude of recipes as well as differences within the composition of the ink’s ingredients. Nowadays, based on the qualitative and semi-quantitative evaluation of X-ray fluorescence data, it is possible to distinguish inks on the basis of the so-called fingerprint model. The first goal of our study was to determine to what extent the type of XRF spectrometer affects the quality of the ink evaluation. We tested two types of spectrometers, semi-stationary machines equipped with polycapillary focusing optics and a handheld spectrometer with a diaphragm collimator and a relatively big interaction spot. The second goal was to address the issue of whether the ink composition might be affected by storage in a metal container. The presentation will discuss the role of the spectrometer type in the evaluation of a thin layer material such as ink. We have also learned that the iron-gall ink composition might depend on the type of vessel in which ink was being stored. T2 - Konferenz - XIV IADA Congress - Warsaw 2019 CY - Warsaw, Poland DA - 23.09.2019 KW - Iron-gall ink KW - XRF KW - Inkwells KW - Ink composition PY - 2019 AN - OPUS4-49149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Glaser, L. A1 - Shevchuk, I. A1 - Tolkiehn, M. A1 - Rabin, Ira A1 - Hahn, Oliver T1 - Improving Iron Gall Ink Palimpsest X-ray Fluorescence Element Mapping Analysis N2 - In the recent years multispectral imaging and X-ray Fluorescence element mapping have established themselves as a well working two step approach, when dealing with faded, erased or overwritten text in iron gall ink. During the last years a lot was done to improve the mere technical side of the techniques. Especially in the case of XRF mapping experiments the acquisition speed needed to be increased to allow mapping in the high resolution demanded by the challenges at hand. High resolution in moderate times can now be achieved, but with the price of proportionally increased amount of data that needs to be processed ideally in parallel to the measurement. The classical approach in XRF spectroscopy of elemental fitting of the spectral data does not even come close to fulfill any on the fly processing time constraints and will consume too much processing time in the foreseeable future. In this paper we will discuss the applicability of modern statistical data processing methods to XRF mapping of iron gall ink palimpsests. We will present a comparison of a new approach based on principle and independent component analysis (PCA and ICA) and the standard element mapping method. We will show that a reduction in processing time of almost two orders of magnitude can easily be achieved. T2 - Kongress Visual Heritage, CHNT 23 CY - Vienna, Austria DA - 15.11.2018 KW - Palimpsest KW - Iron-gall ink PY - 2020 SP - 1.1 EP - 1.9 AN - OPUS4-50243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira A1 - Hahn, Oliver A1 - Kaska, K. ED - Uhlirz, T1 - Why Do We Need to Study Inks? N2 - While studying the socio-geographic history of inks, division 4.5 (Analysis of cultural artefacts and assets) of the BAM (Bundesanstalt für Materialforschung und -prüfung) in Berlin together with the Centre for the Study of Manuscript Cultures in Hamburg has developed a protocol for ink analysis. It consists of a primary screening to determine the type of the ink, and a subsequent in-depth analysis using several spectroscopic techniques. Using this protocol, scientists can assist scholars in addressing a rather broad range of historical questions that cannot be answered unequivocally through scholarly research alone. Among these are investigations on collaboration between scribes and scriptoria, on the usage and annotation of manuscripts and on their path through time and space in general. This research can thus help to reconstruct the circumstances of the production of written heritage as well as their history and transmission. To facilitate the dialogue between the scholars and the scientists a simple optical tool was developed to allow the scholars to perform preliminary ink analysis required for formulation of the question that in turn can be answered by scientific in-depth investigations. In this paper, ink types and their identification method is accompanied by examples of the recent work conducted on parchment manuscripts in the Austrian National Library. T2 - Congress Visual Heritage, CHNT 23 CY - Vienna, Austria DA - 15.12.2018 KW - Ink KW - Parchment PY - 2020 SP - 1.1 EP - 1.9 CY - Wien AN - OPUS4-50242 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Melzer, C. T1 - Red chalk as a medium of transfer in dutch and flemish drawings N2 - The Weimar research project has set the goal of placing style-critical research on Old Master drawings on a new, methodologically proven foundation. The starting point is the stock of Dutch drawings possessed by the Klassik Stiftung Weimar, whose extent (ca. 1,400 items) and character make it one of the most significant outside the Netherlands. The focus here is on drawings that were executed with red chalk. This drawing material has different functions - one of which is the use as a transmission material. The methodological approach is double: first, the scientific indexing of this stock. The foundations for this, along with classic analysis of style, are innovative material-scientific methods of investigation. T2 - Red Chalk Drawings. Sources, Techniques and Styles c. 1500-1800 CY - Florence, Italy DA - 18.09.2019 KW - Drawing KW - Red chalk KW - Non-destructiv testing PY - 2019 AN - OPUS4-50240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Colini, Claudia T1 - A black ink by any other name...: Typologies of Arabic inks and their detection limits N2 - In this poster we will present some results of a research projects dealing with Arabic recipes of black inks. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed. First, we will provide an overview of the sources [1-2] employed in the study – dating from 9th to 14th century, although the manuscripts in which they can be found dates up to the 20th century – with an eye on the ink typologies (real and perceived by the compilers). Then we will show how, by reproducing the recipes, it was possible to shed light on some oddities in the procedures and the choice of ingredients. In the end we will discuss problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect [3]. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol and the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts. [1] A. Schopen, Tinten und Tuschen des arabisch-islamischen Mittelalters, Göttingen: Vandenhoeck & Ruprecht, 2004 [2] S. Fani, Le arti del libro secondo le fonti arabe originali. I ricettari arabi per la fabbricazione degli inchiostri (sec. IX-XIII): loro importanza per una corretta valutazione e conservazione del patrimonio manoscritto, PhD thesis, Napoli: Università L’Orientale, 2013 [3] C. Colini et. al, Manuscript cultures, 11 (2018) 43-50 T2 - Technart 2019 CY - Bruges, Belgium DA - 07.05.2019 KW - Inks KW - Reflectography KW - XRF KW - Raman Spectroscopy KW - ATR PY - 2019 AN - OPUS4-50112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Colini, Claudia T1 - A black ink by any other name...: Typologies of arabic inks and their detection limits N2 - In this poster we will present some results of a research projects dealing with Arabic recipes of black inks [1-2]. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed. We will show procedures and problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on squid ink [3] and mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect [4]. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol, the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts. [1] A. Schopen, Tinten und Tuschen des arabisch-islamischen Mittelalters, Göttingen: Vandenhoeck & Ruprecht, 2004 [2] S. Fani, Le arti del libro secondo le fonti arabe originali. I ricettari arabi per la fabbricazione degli inchiostri (sec. IX-XIII): loro importanza per una corretta valutazione e conservazione del patrimonio manoscritto, PhD thesis, Napoli: Università L’Orientale, 2013 [3] S. Centeno, J. Shamir Journal of Molecular Structure, 873 (2008), 149-159 [4] C. Colini et. al, Manuscript cultures, 11 (2018) 43-50 T2 - Jahrestagung „Archäometrie und Denkmalpflege 2019“ CY - Vienna, Austria DA - 11.09.2019 KW - Inks KW - Reflectography KW - XRF KW - Raman Spectroscopy KW - ATR PY - 2019 AN - OPUS4-50162 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Colini, Claudia ED - Hahn, Oliver ED - Rabin, Ira T1 - A black ink by any other name... Typologies of Arabic inks and their detection limits N2 - In this poster we will present some results of a research projects dealing with Arabic recipes of black inks. To improve conservation practices of Arabic manuscripts we have assessed the feasibility of the recipes collected from many Arabic sources on bookmaking and reproduced the most common inks. Ink samples were then artificially aged and analysed using an array of analytical techniques, mostly non-invasive, in order to build a database of Arabic inks and their ingredients and also to verify the detection limits of the portable equipment employed. We will show procedures and problems concerning the identification of ink types and ingredients using reflectography (in Vis, IR and UV), X-Ray Fluorescence, Infrared and Raman spectroscopy. The focus will be in particular on squid ink and mixed inks – both in the form of carbon inks with the addition of tannins and of a mixture of carbon and iron gall inks – which are particularly difficult to detect. We will also examine the results of iron gall inks made with iron filings or nails instead of vitriol, the various precursor used to extract gallic acid that are mentioned in the sources as surrogates of gall nuts. T2 - Jahrestagung „Archäometrie und Denkmalpflege 2019“ CY - Vienna, Austria DA - 11.09.2019 KW - Inks KW - Reflectography KW - XRF KW - Raman Spectroscopy KW - ATR PY - 2019 SN - 0947-6229 VL - Sonderheft 9 SP - 93 EP - 96 PB - Deutsches Bergbau-Museum Bochum CY - Bochum AN - OPUS4-50163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Steger, Simon T1 - Non-invasive spectroscopic investigation of cultural artefacts: shedding light on modern reverse glass paintings N2 - This thesis addresses the development of a methodological approach for the non-invasive identification of colourants and for the classification of binding media in reverse glass paintings from the early 20th century. For this purpose, mobile and miniaturized devices were used to measure the paintings in situ. The methodology includes X-ray fluorescence (XRF), VIS spectroscopy (VIS), Raman spectroscopy and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). In a first step the capabilities of DRIFTS for binding media classification and pigment identification were tested. DRIFTS enables, besides Raman spectroscopy, the collection of molecular information of a substance that can be used as characteristic fingerprint spectrum. However, the simultaneous collection of both specular (surface) and diffuse (volume) reflection leads to complicated mixed DRIFT spectra, that can vary strongly for one substance depending on the dominant fraction of reflected light. Specular reflection causes several spectral distortions like inverted bands, band shifts and derivative-like features whereas pure diffuse reflections leads to an intensity enhancement of combination bands and overtones. Both specular and diffuse reflection cannot be optically separated, and their proportion depends on material properties like the absorption coefficient and the refractive index as well as on Parameters like surface roughness, porosity, grain size and angle of incidence and detection. A direct comparison of DRIFT spectra with IR spectra of other methods (e.g. transmission, ATR) is not possible, hence the creation of DRIFTS databases was needed. The next step was the complimentary utilization of Raman spectroscopy and DRIFTS for the dentification of synthetic organic colourants. Such colourants are in the further chapters called synthetic organic pigments (SOP) even when it’s not always entirely clear if they are soluble dyes or pigments that are practically insoluble in the medium in which they are incorporated. Raman spectroscopy is generally the method of choice when dealing with SOP, but fluorescence can hamper the Raman spectrum severely, inhibiting the proper identification of the pigment. DRIFTS was successfully applied and several SOP like synthetic alizarin (PR83), the yellow azo pigments (e.g. PY1) or the red and orange β-naphthol pigments (e.g. PR3) could be identified in the paintings solely by means of DRIFTS. The holistic methodological sequence was defined after the successful establishment of DRIFTS as serious analytical alternative. As the time is always the most limiting factor for in situ measurement campaigns in museums, the 9 sequence needs to be time saving but also efficient. The methodology starts with quick measurements by XRF and VIS to get a first idea of the pigment composition, followed by the validation of the results with the vibrational spectroscopies for selected points. Measurements of reverse glass paintings by Carlo Mense and Wassily Kandinsky were conducted to test the entire procedure. A high number of pigments could be identified, including several rare ones like strontium white (SrSO4), PR60 and PB52. The binding media were classified using the previously recorded references. The results were set in the art historian context and were discussed in a multidisciplinary way. The influence of Asian art, especially of Chinese reverse glass paintings as source of inspiration for artists of the “Blauer Reiter” collective (e.g. Wassily Kandinsky, Gabriele Münter, Franz Marc und Heinrich Campendonk) is shown. Non-invasive measurements of two Chinese reverse glass paintings from the late 19th and early 20th century were conducted, enabling a comparison of the palettes of Chinese and European painters. The Chinese palette includes heavy use of red lead and orpiment, pigments that were hardly sed in Europe anymore. More modern pigments like zinc white, cadmium yellow, viridian, chromates, cobalt blues or SOP were not found at all in the Chinese paintings. KW - Reverse glass painting KW - Raman spectroscopy KW - DRIFTS KW - Non invasive analysis PY - 2020 SP - 12 EP - 104 CY - Hamburg AN - OPUS4-51160 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonnerot, Olivier A1 - Del Mastro, G. A1 - Hammerstaedt, J. A1 - Mocella, V. A1 - Rabin, Ira T1 - XRF ink Analysis of some Herculaneum papyri N2 - Recent research has suggested that some of the inks used in Herculaneum papyri do not consist of pure carbon. Starting from this finding, in June 2018 a preliminary campaign of analysis by means of X-Ray fluorescence (XRF) of external portions removed mechanically from their original rolls in the eighteenth century (the so-called scorze) took place at the Biblioteca Nazionale at Naples. Also in this case, the aim of the survey was to investigate the ink composition in order to detect possible traces of metal. This article sums up the results of this survey. KW - Herculaneum papyri KW - Ink KW - XRF PY - 2020 SP - 50 EP - 52 AN - OPUS4-51193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietz, Georg T1 - Wasserzeichen- und Papierstrukturanalysen für die kunstgeschichtliche Forschung N2 - Wasserzeichen und Papierstrukturen können einen wesentlichen Beitrag bei der Analyse von Kunstobjekten auf Papier darstellen. Ausgangspunkt hierfür bildet die korrekte Dokumentation mit entsprechender Bildaufnahme und der richtigen Erfassung und Interpretation der Phänomene. An Fallbeispielen aus Forschungsprojekten zu niederländischen Zeichnungen am Kupferstich-Kabinett Dresden und der Grafischen Sammlung Weimar sollen die Möglichkeiten der Papier- und Wasserzeichenforschung als historische Hilfswissenschaft demonstriert werden. Dieser Abendvortrag dient zugleich als Einführung in die Technologie der (Hand-)Papierherstellung, Wasserzeichenerfassung und –recherche. T2 - Papier - unde venis? Hochschule der Künste Bern CY - Bern, Switzerland DA - 16.01.2020 KW - Papier KW - Wasserzeichen KW - ZfP PY - 2020 AN - OPUS4-50617 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietz, Georg T1 - Sieb und Filz - Entwicklungsgeschichtliche Meilensteine des Papiermaschinenbaus / der Papiermaschinenbespannungen N2 - Im Jahr 2019 jährt sich die Inbetriebnahme der ersten Papiermaschine in Deutschland zum 200. Male. Mit dem Vortrag wird eine Einführung in die Technologie der Maschinenpapierherstellung, samt entwicklungsgeschichtlicher Meilensteine gegeben. Es gilt die Produktvielfalt von Papier und die Gründe für die enormen Produktionssteigerungen bei der Papierherstellung aufzuzeigen. T2 - 27. Tagung des Deutschen Arbeitskreises für Papiergeschichte CY - Düren, Germany DA - 24.10.2019 KW - Papier KW - ZfP KW - Archäometrie PY - 2019 AN - OPUS4-50633 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier T1 - Are X-rays safe for manuscripts’ materials? N2 - In the last decade, applications of X-rays to the study of manuscripts significantly spread in both diversity and extent. They range from writing material analysis, mostly with X-ray fluorescence (XRF), permitting non-invasive characterization of inks and pigments used, to the investigation of the origin of writing supports. In addition, XRF mapping has proved to be an invaluable tool for recovering erased text. Finally, computed-tomography (CT) has shown potential in virtually unrolling rolls, making text readable without using-damaging mechanical methods. Despite their growing use, little attention has been paid to the side effects of such analytical tools. We observed irreversible parchment colour changes during some experiments on dead-sea scrolls with synchrotron radiation sources. Furthermore, partial photo-reduction of iron under high intensity beam during X-ray absorption near edge structure spectroscopy (XANES) measurements of iron-gall ink on paper has been reported several times [5,6]. Such phenomena have mostly been overlooked so far, although there is an increasing awareness of the necessity to study them. We conducted experiments at the Deutsches Elektronen-Synchrotron (DESY) facilities to investigate X-ray induced structural alteration of paper and parchment to see whether the presence of absorption centres (ink and pigments) has an impact. In addition to better understanding degradation processes, we are aiming to define an appropriate methodology of analysis of manuscripts with a tolerable risk of damage. The first results concerning X-ray induced damage of cellulose materials have already been presented at the Synchrotron Radiation and Neutrons in Art and Archaeology (SR2A). We are focusing here on the results on parchment materials. T2 - Cultural and Natural Heritage Workshop CY - Grenoble, France DA - 22.01.2020 KW - X-rays KW - Manuscripts KW - Parchment KW - Synchrotron PY - 2020 AN - OPUS4-50305 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietz, Georg T1 - Papieranalysen für die kunstgeschichtliche Forschung N2 - Wasserzeichen und Papierstrukturen können einen wesentlichen Beitrag bei der Analyse von Kunstobjekten auf Papier darstellen. An Fallbeispielen aus der gutachterlichen Praxis und Forschungsprojekten der Vergangenheit sollen die Möglichkeiten der Papier- und Wasserzeichenforschung bei Datierungen und Authentizitätsprüfungen demonstriert werden. T2 - PTS-Workshop in Heidenau zu Thema: Materialwissenschaftliche Untersuchungsmethoden zur Charakterisierung und Authentifizierung von Dokumenten und Kunstwerken auf Papier CY - Dreden-Heidenau, Germany DA - 07.11.2019 KW - Papier KW - Fälschungserkennung KW - ZfP PY - 2019 AN - OPUS4-50634 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ketelsen, T. A1 - Hahn, Oliver A1 - Golle, U. T1 - Blindness and Insight. The Rhetoric of Connoisseurship and the Investigation of Materiality. N2 - The aim of the lecture is to present the productive interplay of connoisseurs and material analysis using the example of selected drawings from the Rembrandt collection of the Klassik Stiftung Weimar. We try to determine the point at which the question of the materiality of the drawings makes sense in the traditional discourse of connoisseurship. On the one hand, this involves the question of authorship – Rembrandt – or not? – and the locating of attributed drawings in the context of the work. On the other hand, it is about making drawing processes visible, characterizing ways of drawing and workshop practices as well as distinguishing different forms of reworking and copying within the Rembrandt workshop. The material analyses culminate in the question of whether Rembrandt’s inks can be distinguished at all. It becomes apparent that the newly gained knowledge about the materiality of the drawing no longer reveals itself to the “mere” view of the connoisseur. Rather, it is only generated by the digital image. The rhetoric of connoisseurs must therefore be contrasted with the necessity of a hermeneutics of the digital image. The envisaged “material turn” of drawing science is thus simultaneously able to take up the critique of the question of authorship, which has been growing ever more recently, and to transfer it to a more comprehensive perspective of aesthetics of production. T2 - Drawings by Rembrandt. Connecting art history, science and conservation CY - Amsterdam, Rijksmuseum, The Netherlands DA - 06.02.2020 KW - Rembrandt KW - Drawings KW - Non-destructive testing KW - Inks KW - Paper PY - 2020 AN - OPUS4-50384 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bintz, Thilo A1 - Munsch, Sarah Mandy A1 - Stelzner, Ludwig A1 - Lauinger, Robert A1 - Schmidt, Wolfram A1 - Kruschwitz, Sabine T1 - An NMR tomograph for building materials - applications, experimental studies and limitations - N2 - A summary of the possibilities, technical limitations and application examples for a unique NMR tomograph at BAM. T2 - 13th International Conference on Electromagnetic Wave Interaction with Water and Moist Substances (ISEMA), 2021 CY - Kiel, Germany DA - 27.06.2021 KW - Relaxation time distribution KW - NMR imaging KW - Capillary suction PY - 2021 SN - 978-1-7281-8738-9 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. SP - 106 EP - 110 PB - IEEE AN - OPUS4-53116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Beyond Chocolate and Apricot Using Scientific Techniques to Determine the Relationship of the Inks of Codex Vaticanus N2 - Codex Vaticanus was written by multiple scribes and annotated by over thirty different hands. In the past, scholars have speculated about the relationship between the inks using highly subjective observations. For example, The scholars spoke about “apricot” and “chocolate” distigmai, arguing for their respective origins based on their visual similarity to the original ink and that of the medieval reinker, respectively. In recent decades, micro X-ray fluorescence (µXRF) has revolutionized the study of ancient and medieval cultural artifacts, making it possible to examine them using objective criteria. The application of such objective scientific measurements to ancient and medieval manuscripts will be explained with examples of how color, hue, and appearance of ink can be highly misleading. T2 - Annual Meeting of the Siciety of Biblical Literature CY - San Antonio, TX, USA DA - 18.11.2023 KW - Codex B KW - Codex Vaticanus KW - Historic ink KW - Micro-XRF PY - 2023 AN - OPUS4-61200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Hahn, Oliver A1 - Oesterle, D. A1 - Bretz, S. A1 - Steger, Simon A1 - Stege, H. A1 - Dietemann, P. A1 - Baumer, U. ED - Hahn, Oliver ED - Oesterle, D. ED - Bretz, S. ED - Doil, Thorsten T1 - Hinter Glas gemalt - Geheimnisse einer Technik - Eine Ausstellung im Museum Penzberg – Sammlung Campendonk im Rahmen des Forschungsprojektes "Hinterglasmalerei als Technik der Klassischen Moderne 1905-1955" N2 - Mit der Bezeichnung Hinterglasmalerei wird allgemein der Begriff der Glasmalerei assoziiert. Auch wenn in beiden Fällen Glas das Trägermaterial ist, bezeichnet Hinterglasmalerei jedoch eine völlig andere Technik. Während bei der Glasmalerei die Farben auf den Bildträger eingebrannt werden, handelt es sich bei der Hinterglasmalerei um eine Kaltmalerei. Selbsttrocknende Farben werden auf die Rückseite der Glastafel aufgetragen, zuweilen wird die Malweise durch aufwendige Veredelungstechniken ergänzt. Mehr und mehr rückt diese Technik, die materialtechnologisch zwischen Tafelmalerei und Glasmalerei zu verorten ist, in den Blickwinkel einer interessierten Öffentlichkeit, wie dies eine zunehmende Anzahl verschiedener Ausstellungen zur Hinterglasmalerei belegen. Die vorliegende Publikation beschäftigt sich in erster Linie mit kunsttechnologischen und materialanalytischen Aspekten der Hinterglasmalerei und ermöglicht tiefe Einblicke in die künstlerische Arbeitsweise und in die Verwendung unterschiedlichster Materialien. T2 - Ausstellung Hinterglasmalerei CY - Penzberg, Germany DA - 19.12.2020 KW - Archäometrie KW - Hinterglasmalerei KW - Kunsttechnologie KW - Zerstörungsfreie Prüfung PY - 2021 SN - 2567-1251 VL - 2 SP - VII EP - 103 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-55155 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gordon, N. A1 - Bonnerot, Olivier A1 - Rabin, Ira ED - Friedrich, M. ED - Quenzer, J. T1 - Inks Used to Write the Divine Name in a Thirteenth-Century Ashkenazic Torah Scroll: Erfurt 7 (Staatsbibliothek zu Berlin, Ms. or. fol. 1216) N2 - The scribe of ‘Erfurt 7’, a thirteenth-century Torah scroll now kept in Berlin, initially left blank spaces for the divine appellations Elohim ( אלהים ) and YHWH Elohim ( ,(יהוה אלהים which were filled in during a second stage of writing. The appearance of the ink employed to write the appellations was significantly darker than that of the surrounding ink. X-ray fluorescence analysis (XRF) has shown that the light and dark brown inks had similar elemental compositions, but contained different ratios of iron to potassium, which could be explained by the use of different batches of ink. According to some medieval sources, the divine appellations were sometimes filled in during a second stage of writing in the presence of ten men from the Jewish community. In Erfurt 7, the two-stage procedure was only performed in the first 1.5 columns of the original sheets, suggesting it may have been part of a public ceremony inaugurating the writing of the divine names in the scroll. Erfurt 7 emerges from this study not only as a ritual object used for liturgy, but as a rallying point for the Jews of Erfurt to come together as a community to express their reverence for the written form of God’s name. The divine name YHWH ( יהוה ) was written in a smaller script than the surrounding text on three replacement sheets using the same two-stage procedure. The ink used on the replacement sheets contained zinc, which is characteristic of other Erfurt manuscripts as well. This suggests that Erfurt was the place where the scroll was used, cherished and eventually repaired. KW - Torah KW - Ink KW - Erfurt KW - 13th century PY - 2020 SN - 1867–9617 VL - 15 SP - 163 EP - 184 AN - OPUS4-52965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nöller, Renate A1 - Hahn, Oliver ED - Dora, C. ED - Fabian, C. ED - Knoche, M. ED - Linder, M. ED - Mittler, E. ED - Schmitz, W. T1 - VIS-Spectroscopy of Aztec colors. Possible application of a non-destructive analytical method N2 - VIS-spectrometry is a rapid, non- invasive, mobile method that offers a first overview of possible colorants used for painting. This is worked out in detail for European paintings and applied for artefacts and illuminated manuscripts. Manuscripts from Asia for example show colorful decoration identified to be mostly prepared with mineral pigments such as cinnabar, azurite, malachite or orpiment, which can be well confirmed by elemental analyses due to their color-giving metal ions. This is not the case for the colorants used in pictorial manuscripts from pre-Hispanic America, painted mainly with organic dyes from plants. The palette of colors used by the Aztecs is very rich due to their extensive empire and long- distance communication with vassal states liable to tributes including dyes of high quality. These include for example red cochineal, yellow zacatlaxcalli, tagetes, safflower, and achiotl, as well as blue indigo, or matlalli. T2 - Manuscripta Americana: Aufarbeitung einer Sammlung CY - Ibero-Amerikanisches-Institut, SPK DA - 14.02.2019 KW - Pigments KW - Dyes KW - Humboldt Codices KW - Non-destructive test PY - 2020 SN - 978-3-447-11511-7 SN - 0067-8236 VL - 53 SP - 35 EP - 57 PB - Harrassowitz Verlag CY - Wiesbaden AN - OPUS4-51934 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Golle, U. A1 - Hahn, Oliver A1 - Wintermann, C. ED - Brahms, I. T1 - Rötel und Eisengallustinte als Farbeffekte in der Zeichnung N2 - Eine Vielzahl unterschiedlicher Materialien findet für die farbliche Gestaltung von Zeichnungen Verwendung. Einige Pigmente und Farbstoffe, d.h. Tinten, Stifte oder Kreiden, waren nur für den Gebrauch als Zeichenmittel vorgesehen – andere wiederum finden sich auch in der Tafel- oder Fassmalerei. Ausgehend von schwarzen Zeichenmaterialien soll zunächst eine allgemeine Typologie der Farbmittel entwickelt werden, um den Kosmos dieser Vielfältigkeit zu illustrieren. In einem zweiten Teil werden farbige Elemente am Beispiel von Rötel in Zeichnungen hinterfragt, deren Funktion und Bedeutung sich aus der Betrachtung heraus nicht unbedingt sofort erschließt. So diente die Farbe hier weder der naturgetreuen Nachahmung, noch wurde sie für eine nachträgliche Wertsteigerung eingesetzt. Der dritte Teil dieses Exkurses widmet sich schließlich solchen „farbigen“ Elementen, deren Konnotationen sich aus den Zeichnungen nicht ermitteln lassen und die daher zunächst irritieren. Diese vermeintliche Farbigkeit war aber ursprünglich vielleicht gar nicht intendiert, sondern ist vielmehr auf Alterungs- und Korrosionsprozesse zurückzuführen. KW - Zeichenmaterialien KW - Eisengallustinte KW - Rötel KW - Zerstörungsfreie Prüfung PY - 2020 SN - 978-3-7319-0772-5 SP - 152 EP - 159 PB - Michael Imhof Verlag CY - Petersberg AN - OPUS4-51404 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Danielewski, A. A1 - Nöller, Renate ED - Collatz, C.-F. ED - Hansen, S. ED - Witte, R. T1 - Zerfallen, zerteilt, zerschnitten: die Humboldt Fragmente IX-XII und ihre Rekonstruktion N2 - In Berlin befinden sich Fragmente indigener Bilderhandschriften, die Alexander von Humboldt aus Mexiko mitbrachte. Fast alle stammen sie aus der ehemaligen Sammlung des Italieners Lorenzo Boturini, deren Reste heute über mehrere Länder verstreut sind. Der hohe Fragmentierungsgrad sowie ungeklärte Fragen zur Provenienz und Genese der Bruchstücke machen es schwierig, sie zu rekontextualisieren. Um dies dennoch zu erreichen, kommen einander ergänzende moderne natur- und kulturwissenschaftliche Methoden zum Einsatz. Als Beispiel einer Neuzuordnung werden die Humboldt-Fragmente IX-XII vorgestellt. Dass die vier Bruchstücke verwandt sind, wurde schon lange vermutet, nicht jedoch, dass sie zusammen mit einem nicht mehr vorhandenen Mittelteil ein einziges Dokument gebildet haben. Die Gründe für eine derartige Rekonstruktion werden als Ergebnis der Forschungsarbeiten diskutiert. KW - Zeichenmaterialien KW - Zerstörungsfreie Prüfung KW - Farbmittel PY - 2019 SN - 0002-6646 VL - 64 SP - 99 EP - 116 PB - ISENSEE VERLAG CY - Oldenburg AN - OPUS4-51929 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver A1 - Nöller, Renate ED - Dora, C. ED - Fabian, C. ED - Knoche, M. ED - Linder, M. ED - Mittler, E. ED - Schmitz, W. T1 - Writing inks in the Manuscripta Americana – a pilot study N2 - The manuscripts – which have been inventoried as Manuscripta Americana in the State Library of Berlin and the Biblioteka Jagellońska in Krakow with the signatures Ms. Americ. 1-15 – are codices mainly from the colonial times of the 16th to 18th centuries. They uniquely reflect the relationships between indigenous culture and Spanish colonial masters. This study focusses on the scientific investigation of three manuscripts (Manuscripta Americana 3, 8, and 10) that are kept today in Krakow. It is assumed that these three parts belong together in a certain way, so various material analyses were carried out to prove this assumption. The scientific investigation focusses on the different black and brown writing inks. T2 - Manuscripta Americana: Aufarbeitung einer Sammlung CY - Ibero-Amerikanisches-Institut, SPK DA - 14.02.2019 KW - Humboldt Codices KW - Writing inks KW - Non-destructive testing PY - 2020 SN - 978-3-447-11511-7 SN - 0067-8236 VL - 53 SP - 21 EP - 32 PB - Harrassowitz Verlag CY - Wiesbaden AN - OPUS4-51935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hahn, Marc Benjamin T1 - Behind the paper: Radiation, DNA and water: New techniques for deeper insights N2 - To gain deeper insights into the old questions about the influence of water on radiation interaction with DNA, new spectroscopic techniques had to be applied. KW - DNA KW - DNA radiation damage KW - XPS KW - Geant4 KW - Low energy electrons KW - OH radical KW - Hydrated DNA KW - Hydration shell KW - Double-strand break (DSB) KW - Dissociative electron attachment (DEA) KW - Single-strand break (SSB) KW - LEE KW - PES KW - Ionization KW - Reactive oxygen species KW - ROS KW - Base damage KW - Base loss KW - Cancer therapy KW - TOPAS KW - TOPAS-nbio PY - 2021 UR - https://go.nature.com/3gjZVWG SP - 1 EP - 3 PB - Springer Nature CY - London AN - OPUS4-52461 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Nanocarriers – Challenges Imposed by Material Characterization N2 - A brief perspective of BAM on nanocarriers is presented including examples with special emphasis on the characterization of such materials and underlying challenges. In this respect, also ongoing activities at BAM on different types of core/shell nanomaterials and related systems are briefly summarized. T2 - Kolloquium BfR CY - Online meeting DA - 18.03.2021 KW - Nanomaterial KW - Nanocarrier KW - Size KW - Surface chemistry KW - Release kinetics KW - Chemical composition KW - Core/shell nanoparticle KW - Quantum dot KW - Spectroscopy KW - Fluorescence PY - 2021 AN - OPUS4-52412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Martin T1 - Real time multichannel biomarker detection using photonic integrated circuits on ultra compact CMOS chips N2 - This work presents the real-time, multichannel detection of the biomolecule Neutravidine using photonic integrated circuits on ultra-compact monolithic CMOS chips. The development focuses on implementing bioassays directly on CMOS platforms, enabling highly integrated and scalable biosensing. The presentation will cover key aspects including microfluidic integration, data analysis, surface functionalization, and chip packaging. T2 - World Biosensor Congress CY - Lisbon, Portugal DA - 18.05.2025 KW - Chips KW - Photonics KW - Biosensor KW - Realtime PY - 2025 AN - OPUS4-63777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fink, Friedrich A1 - Stawski, Tomasz M. A1 - Emmerling, Franziska A1 - Falkenhagen, Jana T1 - A novel machine-learning approach to unlock technical lignin classification by NIR spectroscopy - bench to handheld N2 - In this research, the utilization of near-infrared (NIR) spectroscopy in conjunction with advanced machine learning methods is investigated for categorizing technical lignins obtained from different biomass sources and industrial procedures. Technical lignins, such as kraft, organosolv and lignosulfonates, have different chemical compositions, which continue to make uniform characterization and application in sustainable sectors extremely difficult. Fast, universally accessible analytics combined with data analysis is still an open question. For the first time three distinct NIR spectrometers—a high-performance benchtop system, a mid-priced compact device, and an economical handheld unit—were utilized to record NIR spectra of 31 unique lignin samples. The spectra underwent pre-processing through standard normal variate (SNV) transformation and Savitzky-Golay derivatives to amplify spectral features and decrease noise. Principal component analysis (PCA) was employed to reduce data complexity and extract crucial characteristics for classification purposes. Subsequently, four machine learning algorithms—Support Vector Machines (SVM), Gaussian Naive Bayes (GNB), Gaussian Process Classification (GPC), and Decision Tree Classification (DTC)—were implemented for the classification of the lignin samples. The DTC model exhibited the highest accuracy among them across different spectrometers. Although the benchtop spectrometer produced the most precise outcomes, the compact NeoSpectra system also displayed potential as a cost-efficient option. Nonetheless, the restricted spectral coverage of the handheld NIRONE spectrometer resulted in reduced classification accuracy. Our discoveries highlight the capability of NIR spectroscopy, combined with robust data analysis techniques, for the swift and non-destructive classification of technical lignins, facilitating their improved utilization in sustainable fields. KW - Technical lignins KW - NIR spectroscopy KW - Classification KW - Machine-learning KW - PCA PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634518 DO - https://doi.org/10.1016/j.chemolab.2025.105467 SN - 0169-7439 VL - 264 SP - 1 EP - 10 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-63451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Andresen, Elina T1 - Optical Stability Studies of Hexagonal Upconverting Nanocrystals and Development of Monitoring Tools N2 - We demonstrate the potential of time-resolved luminesence spectroscopy for the straightforward assessment and in situ monitoring of the stabilty of UCNPs. Different analytical methods were used to assess the dissolution behaviour of UCNPs in varuous media. Potentiometric and optical data were correlated to develop a new non-invasive monitoring tool for particle dissolution T2 - UPCONline CY - Online meeting DA - 06.04.2021 KW - Dissolution KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence PY - 2021 AN - OPUS4-56230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Skłodowska, Anna A1 - Parolai, S. A1 - Petrovic, B. A1 - Romanelli, F. T1 - Soil-structure interaction assessment combining deconvolution of building and field recordings with polarization analysis: application to the Matera (Italy) experiment N2 - In this study, the wavefield radiated from a building to its surroundings is identified and extracted from M4.6 earthquake recordings collected by sensors installed in a building and on the nearby athletic field in Matera (Italy) using a new approach for soil-structure interaction assessment. The proposed approach for earthquake data analysis combines in an innovative way two methods already used in seismology and engineering seismology: deconvolution and polarization analysis. The approach enables the identification, reconstruction, and characterization of the wavefield radiated from a vibrating building into its surroundings, and the estimation of the amount of energy associated with it. The approach consists of four steps: estimation of the resonant frequencies of the building, deconvolution of the earthquake recordings from a building and its surroundings, identification of the seismic phases, reconstruction of the signal transmitted from the building to its surroundings, and estimation of its energy, and polarization analysis. Analysis of recordings of the M4.6 event highlighted that the motion related to the wavefield radiated from the building to the ground was mostly linearly polarized in the radial and transverse planes, while a clear ellipticity was observed only in the horizontal plane. The wavefield radiated from the building might be dominated by unconventionally polarized surface waves, i.e., quasi-Rayleigh waves or a combination of quasi-Rayleigh and quasi-Love waves. The results indicated that the energy transmitted from the analyzed vibrating building to its surroundings was significant and decreased the ground motion shaking due to the out-of-phase motion. KW - Radiated wavefield KW - Earthquake data KW - Seismic signal reconstruction KW - Particle motion trajectory KW - Wave propagation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582931 DO - https://doi.org/10.1007/s10518-023-01750-7 SN - 1570-761X SP - 1 EP - 25 PB - Springer Science and Business Media LLC AN - OPUS4-58293 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Laquai, René A1 - Wieder, Frank A1 - Kupsch, Andreas A1 - Müller, Bernd R. T1 - The combined use of X-ray refraction and transmission radiography and computed tomography N2 - Alternative to conventional transmission-based radiography and computed tomography, X-ray refraction techniques are being increasingly used to detect damage in light materials. In fact, their range of application has been recently extended even to metals. The big advantage of X-ray refraction techniques is that they are able to detect nanometric defects, whose size would lie below the resolution of even state-of-the-art synchrotron-based X-ray computed tomography (SXCT). The superiority of synchrotron X-ray refraction radiography and tomography (SXRR and SXRCT) has been shown in the case of light materials, in particular composites. X-ray refraction techniques also yield a quantitifaction of the amount of damage (the so-called relative internal specific surface) and can well be compared with damage models. At the same time, it is impossible for SXRR and SXRCT to image single defects. We show that the combination of refraction- and transmission-based imaging techniques yields an impressive amount of additional information about the type and amount of defects in microstructured materials such as additively manufactured metals or metal matrix composites. We also show that the use of data fusion techniques allows the classification of defects in statistically significant representative volume elements. T2 - 11th Conference on Industrial Computed Tomography CY - Online meeting DA - 08.02.2022 KW - X-ray refraction radiography KW - Computed Tomography KW - Synchrotron radiation KW - Additive manufacturing KW - Damage evolution PY - 2022 UR - https://www.ndt.net/article/ctc2022/papers/ICT2022_paper_id268.pdf SP - 1 EP - 7 AN - OPUS4-54324 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Labor und Synchrotron-Röntgenrefraktionstechniken: Neu? Interessant? Nützlich? N2 - Wir präsentieren Labor- und Synchrotron-Röntgenrefraktionstechniken, wie sie an der BAM implementiert sind. Wir zeigen, dass die Labor-Röntgenrefraktionstopographie (XRRT) und die Synchrotron-Röntgenrefraktionsradiographie (SRRR) außergewöhnliche Werkzeuge zur Untersuchung von Schädigungen und inneren Defekten (Poren, Mikrorisse) in leichten Materialien sind. Tatsächlich nutzen diese Techniken den an Grenzflächen auftretenden Röntgenbrechungseffekt aus, um den Kontrast zwischen dem (schwach absorbierenden) Objekt und dem Hintergrund zu erhöhen. Dies ermöglicht die Erkennung sehr kleiner Objekte (z. B. bis zu 1 nm Rissöffnung) und die Quantifizierung ihrer spezifischen Oberfläche, die mit ihrem Einfluss auf die Materialeigenschaften korreliert. Wir zeigen die folgenden Anwendungen: a) Quantifizierung der Faserentbindung in laminaten Epoxid-Kohlenstoff-Verbundwerkstoffen; b) Mapping der Porengröße in gesinterten Keramiken; c) Klassifizierung von Defekttypen in additiv gefertigter Ti6Al4V-Legierung; d) Früherkennung des Versagens in Aluminium-Keramik-Verbundwerkstoffen (unter Verwendung von In-situ-Experimenten); e) 3D-Darstellung von Makrorissen und Faserentbindung in Verbundwerkstoffen auf Ti-Basis für Anwendungen in der Luft- und Raumfahrt (unter Verwendung von Röntgenbeugungstomographie). T2 - DGM AK Röntgentomographie CY - Online meeting DA - 26.05.2021 KW - Rissen KW - Röntgenrefraktion KW - Leichtbau KW - Additive Fertigung KW - Keramiken KW - Poren PY - 2021 AN - OPUS4-52694 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Y. T1 - Fluid inclusion microthermometry in stalagmites: The next stage of development N2 - Fluid inclusion microthermometry is one of the analytical approaches that has been proposed for speleothem-based temperature reconstructions. The proxy of this paleothermometer is the density of drip water relicts that have been enclosed in microscopic fluid inclusions during speleothem growth. Prior to microthermometric analyses, the monophase liquid inclusions need to be transferred from a metastable liquid into a stable liquid-vapour two-phase state by stimulating vapour bubble nucleation by means of single ultra-short laser pulses. Subsequent microthermometric analyses determine the temperature at which the vapour bubble disappears again, the so-called liquid-vapour homogenisation temperature (Th(obs) ). The observed homogenisation temperature depends not only on the water density but also on the inclusion volume. In order to determine the water density, a thermodynamic model is used that takes account of the effect of surface tension on Th(obs) to calculate Th∞. This is the corresponding homogenisation temperature at saturation pressure that determines the water density and defines the formation temperature of the fluid inclusion. The analytical precision of the method ranges between 0.1 and 0.3 °C depending on the size of the inclusions. T2 - Climate Change: The Karst Record IX (KR9) CY - Innsbruck, Austria DA - 17.07.2022 KW - Fluid inclusion microthermometry KW - Stalagmites KW - Synchrotron radiation KW - X-ray imaging KW - X-ray diffraction PY - 2022 AN - OPUS4-55344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - Untersuchung der Integrität von glasfaserverstärkten Zahnstiften mittels Synchrotron-Röntgenrefraktion N2 - Die Integrität der Verstärkungsfasern in Komposit-Zahnstiften ist entscheidend für die Biegefestigkeit und die langfristige Haftung am Zement in den Wurzelkanälen. Es wurde vermutet, dass die Integrität von glasfaserverstärkten Zahnstiften durch das Beschleifen während der zahnmedizinischen Behandlung beeinträchtigt wird. Eine Beschädigung der Fasern führt zu einer erheblichen strukturellen Schwächung über den gesamten Stiftdurchmesser. Glasfragmente, die durch den Kontakt mit dem Zahnbohrer entstehen, können sich vom Stift lösen und die Haftfähigkeit erheblich verringern. Mit Hilfe hochauflösender Synchrotron-Röntgen-Refraktions-Radiographie (SXRR) konnte das Ausmaß der Schäden zuverlässig identifiziert und charakterisiert werden. Dazu wurden die Glasfaserstifte sowohl im Herstellungszustand als auch nach der Bearbeitung mit einem Diamantbohrer untersucht. Die Datensätze wurden zur Visualisierung und Quantifizierung der morphologischen Charakteristika intakter und durch das Beschleifen beschädigter Regionen analysiert. Sie zeigen Schäden im bearbeiteten Bereich (z. B. Brüche, Splitter und Risse) sowie herstellungsbedingte Inhomogenitäten der Fasern mit einer signifikanten Zunahme der inneren Oberflächen in Probenregionen, die durch das Beschleifen beschädigt wurden. T2 - DGZfP Jahrestagung 2022 CY - Kassel, Germany DA - 23.05.2022 KW - Röntgen-Refraktion KW - Verbundwerkstoffe KW - Zahnstifte PY - 2022 AN - OPUS4-54924 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Kai T1 - ToF-SIMS as a new tool for nano-scale investigation of ps-laser generated surface structures on Titanium substrates N2 - The fabrication of laser-generated surface structures on titanium and titanium alloys has recently gained remarkable interests, being technologically relevant for applications in optics, medicine, fluid transport, tribology, and wetting of surfaces. The morphology of these structures, and so their chemistry, is influenced by the different laser processing parameters such as the laser fluence, wavelength, pulse repetition rate, the effective number of laser pulses per beam spot area, etc. A simple way to characterize laser-generated surface structures is by means of optical microscopy (OM) or white light interference microscopy (WLIM). The latter can address the surface topography, while having a lateral resolution limit of ~(lambda)/2 (lambda = illumination wavelength). To resolve morphologies with spatial periods significantly smaller than (lambda)/2, scanning electron microscopy (SEM) is often used, taking benefit of the reduced de Broglie wavelength associated to the electrons of several keV energy. However, all the above-mentioned techniques lack the necessary depth-resolution to reveal and quantify sub-surface material modifications of these laser-generated structures. Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) represents a promising surface analytical technique for studying laser-induced chemical surface alterations since the method combines a high surface sensitivity with the capability to perform a depth-profiling of the laser-affected surface zone. In this study we combine WLIM and high-resolution SEM with ToF-SIMS to fully characterize the evolution of various types of laser-generated micro- and nanostructures formed on Ti-6Al-4V alloys upon irradiation by near infrared ultrashort laser pulses (1030 nm, 925 fs) at different laser fluence levels, effective number of pulses, and at different pulse repetition rates (1 – 400 kHz). We show how this combined surface analytical approach allows to evaluate alterations in the surface chemistry and topography of the laser-generated surface structures depending on the laser processing parameters T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Laser-induced periodic surface structures KW - Time of Flight - Secondary ion mass spectrometry KW - White light interferometric microscopy KW - Titanium alloy PY - 2022 AN - OPUS4-54992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - Microstructure characterization of materials using X-ray refraction techniques N2 - X-ray refraction is an excellent tool for the characterization of the microstructure of materials. However, there are only a few (synchrotron) laboratories in the world that use this technique for material characterisation. Therefore, the seminar will first explain the basic principles of X-ray refraction and the measurement techniques installed at the hard X-ray beamline BAMline at BESSY II (Berlin, Germany). This is followed by examples of investigations on fibre-reinforced plastic composites (CFRP) as well as ceramic (Cordierite, ZrO2-SiO2) and metallic materials (Ti-6Al-4V, Inconel). Some of the investigations were carried out both ex-situ and in-situ under mechanical and thermal load. The results are correlated with the mechanical properties of the materials. T2 - LNLS Users Group Seminar Series CY - Campinas, Brasil DA - 25.10.2022 KW - X-ray refraction KW - Analyzer-Based Imaging KW - BAMline PY - 2022 AN - OPUS4-56117 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Müller, Bernd R. A1 - Laquai, René A1 - Kupsch, Andreas A1 - Wieder, Frank A1 - Benemann, Sigrid A1 - Wilbig, Janka A1 - Günster, Jens A1 - Bruno, Giovanni T1 - Microstructural characterization of AP40 apatite-wollastonite glass-ceramic N2 - The microstructure of an apatite-wollastonite (code name AP40) glass-ceramic is analyzed in this study by combining 2D microscopy, phase analysis, X-ray absorption and synchrotron X-ray refraction computed tomography (XCT and SXRCT, respectively). It is shown that this combination provides a useful toolbox to characterize the global microstructure in a wide scale range, from sub-micrometer to millimeter. The material displays a complex microstructure comprising a glassy matrix with embedded fluorapatite and wollastonite small crystals. In this matrix, large (up to 200 μm) spike-shaped structures are distributed. Such microstructural features are oriented around a central sphere, thereby forming a structure resembling a sea urchin. A unique feature of SXRCT, in contrast to XCT, is that internal interfaces are visualized; this allows one to show the 3D distribution of these urchins with exceptionally good contrast. Furthermore, it is revealed that the spike-shaped structures are not single crystals, but rather composed of sub-micrometric crystals, which are identified as fluorapatite and diopside phases by SEM-EDX analysis. KW - Glass-ceramic KW - X-ray refraction KW - Computed tomography KW - Microstructure PY - 2023 DO - https://doi.org/10.1016/j.ceramint.2022.12.130 SN - 0272-8842 VL - 49 IS - 8 SP - 12672 EP - 12679 PB - Elsevier Science CY - Amsterdam AN - OPUS4-57452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - El-Athman, Rukeia A1 - Rädler, Jörg A1 - Löhmann, Oliver A1 - Ariza de Schellenberger, Angela A1 - Muth, Thilo T1 - The BAM Data Store N2 - As a partner in several NFDI consortia, the Bundesanstalt für Materialforschung und -prüfung (BAM, German federal institute for materials science and testing) contributes to research data standardization efforts in various domains of materials science and engineering (MSE). To implement a central research data management (RDM) infrastructure that meets the requirements of MSE groups at BAM, we initiated the Data Store pilot project in 2021. The resulting infrastructure should enable researchers to digitally document research processes and store related data in a standardized and interoperable manner. As a software solution, we chose openBIS, an open-source framework that is increasingly being used for RDM in MSE communities. The pilot project was conducted for one year with five research groups across different organizational units and MSE disciplines. The main results are presented for the use case “nanoPlattform”. The group registered experimental steps and linked associated instruments and chemicals in the Data Store to ensure full traceability of data related to the synthesis of ~400 nanomaterials. The system also supported researchers in implementing RDM practices in their workflows, e.g., by automating data import and documentation and by integrating infrastructure for data analysis. Based on the promising results of the pilot phase, we will roll out the Data Store as the central RDM infrastructure of BAM starting in 2023. We further aim to develop openBIS plugins, metadata standards, and RDM workflows to contribute to the openBIS community and to foster RDM in MSE. T2 - 1st Conference on Research Data Infrastructure DA - 12.09.2023 KW - Research Data Infrastructure KW - Electronic Lab Notebook (ELN) KW - openBIS KW - Research Data Management PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596032 DO - https://doi.org/10.52825/CoRDI.v1i.229 VL - 1 SP - 1 EP - 5 AN - OPUS4-59603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leidigkeit, Carolin A1 - Shokr, Mohammad A1 - Tosson, Amir A1 - Cakir, Cafer Tufan A1 - Radtke, Martin A1 - Pietsch, Ullrich A1 - Christ, Hans-Jürgen T1 - Using Energy-Dispersive Laue Diffraction to Study Dislocation Arrangements in Materials Showing Wavy and Planar Slip Behavior N2 - The present work shows an approach to monitor the evolution of the dislocation arrangement of a metallic material caused by cyclic plastic strain using white X-ray radiation in combination with an energy-dispersive detector. The method is demonstrated by single-shot experiments performed on polycrystalline nickel and α-brass, representing the pure wavy and the pure planar dislocation slip behavior. To correlate the resulting diffraction patterns with various dislocation arrangements of both metals, fatigue tests were carried out up to certain numbers of cycles and at predetermined plastic strain amplitudes. The differences in dislocation microstructure and internal stress distributions give rise to an appreciable change in the peak shape of Laue reflections, leading to unique characteristics in the respective diffraction patterns. Nickel reflections are elongated due to the high amount of cell structures leading to bending and misorientation of the lattice, whereas the present stacking faults in α-brass result in powder-like diffraction. KW - Slip behavior KW - Energy-Dispersive KW - Laue Diffraction KW - Dislocation PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-637964 DO - https://doi.org/10.1111/ffe.14535 SN - 1460-2695 VL - 48 IS - 3 SP - 1341 EP - 1351 PB - Wiley AN - OPUS4-63796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cakir, Cafer Tufan A1 - Guilherme Buzanich, Ana A1 - Radtke, Martin T1 - Digital Twin for Multimodal Synchrotron Experiments N2 - In this contribution, I present a digital twin-based workflow designed to optimize experimental parameters in X-ray emission spectroscopy (XES), with a focus on reproducibility, data integration, and alignment with FAIR (Findable, Accessible, Interoperable, Reusable) principles in materials science and engineering (MSE). The developed pipeline begins with automated retrieval of crystallographic information from the Materials Project database based on a given sample composition. This structural data is then used to simulate the corresponding XES spectra using FDMNES, allowing for accurate prediction of element-specific emission lines. The simulated emission lines are fed into an X-ray tracing (XRT) module, which builds a virtual replica of the experimental setup. This digital twin environment enables predictive modeling of spectrometer performance based on geometric configurations. The optimization focuses on two key parameters: the choice of the analyzing crystal and the distance between the sample and crystal (which also defines the crystal–detector distance due to Bragg condition constraints). An active learning algorithm is employed to iteratively adjust these parameters in order to achieve a desired energy-per-pixel (E/pixel) resolution with minimal intensity loss, enabling efficient, data-driven experimental planning. By integrating data-driven simulations with real-time optimization strategies, this workflow supports efficient experiment planning while minimizing resource consumption and human error. Furthermore, all stages of the process—from data collection and simulation to optimization and visualization—are structured to ensure traceability and interoperability, facilitating future reuse and collaborative research. I hope this contribution aligns well with the topic “Workflows for FAIR MSE Data” and offers a concrete example of how digital twins can be harnessed to improve the design, execution, and documentation of spectroscopy experiments in the MSE domain. T2 - MSE Research Data Forum 2025 CY - Siegburg, Germany DA - 08.07.2025 KW - Multi Modal KW - XRD KW - XRF KW - Optimization PY - 2025 AN - OPUS4-63794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Sensoren und Analytik für Sicherheit und Prozesskontrolle in Wasserstofftechnologien N2 - Der Beitrag beinhaltet Themen vom H2Safety@BAM-Kompetenzfeld Sensorik, Analytik und zertifizierte Referenzmaterialien (SensRef) mit Fokus auf Mess- und Prüfverfahren mit verschiedenen Sensortechnologien und Ultraschallwellen: Metrologie zur Wasserstoffspeicherung - Euramet-Vorhaben "MefHySto", Erkennung von freigesetztem Wasserstoff sowie die Bestimmung des Wasserstoff-Luftverhälntisses mit Gassensoren, zerstörungsfreie Fehlstellenerkennung mit integriertem Zustandsüberwachungssystem basierend auf geführten Ultraschallwellen zur Lebensdauerüberwachung von Composite-Behältern (Wasserstoffspeicher) sowie faseroptische Sensorik zur Schadenfrüherkennung von Wasserstoffspeichern aufgrund erkennbarer Dehnungsänderungen an Druckbehältern. T2 - DVGW Kongress H2 Sicherheit CY - Online meeting DA - 23.11.2022 KW - H2Safety@BAM KW - SensRef KW - Faseroptische Sensorik KW - Gassensorik KW - Geführte Ultraschallwellen KW - Leckdetektion KW - Metrologie zur Wasserstoffspeicherung KW - Zerstörungsfreie Prüfung KW - Structural Health Monitoring (SHM) PY - 2022 AN - OPUS4-56683 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Fernerkundung von Gaswolken und Leckageortung mittels UAV N2 - - Auswirkungen des unfallbedingten Versagens von Gasbehältern für alternative Kraftstoffe - Kurzvorstellung des Projekts „CoFi-ABV“ - UAV-REGAS Plattform (Unmanned Aerial Vehicle for Remote Gas Sensing): Kombination von Open-Path-Gassensorik mit einem 3-Achs-Gimbalsystem - Ergebnisse erster experimenteller Untersuchungen - Möglichkeiten und Herausforderungen der Lokalisierung von Gasquellen und Erstellung von Gasverteilungskarten mittels UAV - Ausblick für die Weiterentwicklung in Zukunft T2 - 2. VDI-Fachkonferenz Zivile Drohnen im Industrieeinsatz 2017 CY - Frankfurt (Main), Germany DA - 04.07.2017 KW - CoFi-ABV KW - UAV-REGAS KW - Lokalisierung von Gasquellen KW - Fernerkundung von Gaswolken PY - 2017 AN - OPUS4-40927 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haroun, A. A. A. A1 - Derbala, H. A. A1 - Bassioni, G. A1 - Resch-Genger, Ute A1 - Shafik, E. S. A1 - Hassan, A. M. A. T1 - N-aminophthalimide as a novel UV-stabilizer to promote physico-mechanical properties of highdensity polyethylene (HDPE) N2 - This study aimed to evaluate the efficacy of Naminophthalimide (NAP) as a novel UV-stabilizer for highdensity polyethylene (HDPE) in improving its physicomechanical properties under UV exposure. NAP was synthesized by interaction between phthalimide and hydrazine hydrate. It was incorporated into HDPE with different weight ratios (1, 1.5, 2, and 3%), and its performancewas compared with Hostavin as a traditional UV stabilizer. The HDPE composites were exposed to UV irradiation for different periods (7 and 14 days) to evaluate their photodegradation behavior. Tensile strength, elongation at break were assessed before and after UV exposure. Also, oxidation induction time (OIT), melt flow rate (MFR), Vicat softening temperature were evaluated. Hostavin incorporation reduced tensile strength from 22.36 to 20.62MPa at higher concentrations. It has been found that 3% Hostavin, significantly improved elongation at break, increasing from 423% to 1,170%, suggesting enhanced flexibility. In contrast, NAP increased tensile strength to 22.9MPa and moderately enhanced elongation but slightly declined at 3%due to potential over-stabilization. Under UV exposure, retained tensile strength and elongation was improved with stabilizer content, which increasing tensile strength retention. The HDPE that containing NAP showed enhanced UV resistance and superior retention of mechanical properties compared to Hostavin. KW - Polymer KW - Advanced materials KW - Quality assurance KW - Stabilizer KW - Synthesis KW - Physico-mechanical properties PY - 2025 DO - https://doi.org/10.1515/polyeng-2024-0262 SN - 2191-0340 SP - 1 EP - 8 PB - De Gruyter CY - Berlin AN - OPUS4-63534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Algernon, D. A1 - Arndt, R.W. A1 - Denzel, W. A1 - Ebsen, B. A1 - Feistkorn, S. A1 - Friese, M. A1 - Große, C.U. A1 - Kathage, S. A1 - Keßler, S. A1 - Köpp, Christian A1 - Küttenbaum, Stefan A1 - Lohse, C. A1 - Maack, Stefan A1 - Niederleithinger, Ernst A1 - Schickert, M. A1 - Schröder, G. A1 - Taffe, A. A1 - Timofeev, Juri A1 - Walther, A. A1 - Wilcke, M. A1 - Wolf, J. A1 - Wöstmann, Jens T1 - NDT procedures in relation to quality assurance and validation of nondestructive testing in civil engineering N2 - The field of non-destructive testing of civil structures (NDT-CE) has been continuously growing. Due to the complexity and diversity of civil constructions as well as the heterogeneity of concrete, specific standards or guidelines for the application of modern NDT-CE are still missing. The development of individual solutions is the current approach, which is just as challenging as it is common for NDT-CE. With the increasing development and commercialization of NDT-CE technology, the group of practitioners is growing. To ensure a good level of quality in the industry, it appears necessary to establish adequate means. Naturally, the performance of NDT-CE methods regarding a specific application is strongly dependent on choosing the most suitable inspection technique and applying it correctly, generally referred to as the inspection procedure in the field of NDT. There are well-defined guidelines regarding procedure documentation and handling in many fields of NDT (e.g. nuclear, aerospace or automotive) according to the high importance of procedures in assuring a successful and reliable application. For a long time, this has not always been the case with NDT-CE, which is still considered a unique discipline of NDT. Part of the reason for that might be the young development state of NDTCE, the heterogeneity of building materials like concrete, timber or masonry as a material and the diversity of civil structures. In consequence, NDT-CE procedure development is considered challenging. Among other aspects, addressed in the subcommittee on Quality Assurance (UA-QS) within the committee for NDT-CE of the German Society for Nondestructive Testing (DGZfP), part of its work aims at establishing an adequate basis for NDT-CE procedure development. While some of the highly developed approaches from other industries are taken into consideration, they need to be analyzed regarding their suitability for NDT-CE and adapted accordingly. For a procedure to be as defined as possible, it needs to contain sufficient information, such as the scope and limitations regarding material, geometry and condition of the test object, inspection parameters, calibration, data acquisition, analysis criteria as well as requirements regarding the inspection personnel. For a successful implementation in the field, it is important to define the specific procedure as precisely as possible. Despite the necessity of a great amount of information to be included, the procedure needs to be suitable for efficient field application. The UA-QS is developing a guideline for NDT-CE procedures suitable for application in this field of NDT to ensure correct and reproducible application. To demonstrate and evaluate this concept, specific examples of procedures are also produced. In particular, the UA-QS has developed a procedure for the detection and positioning of tendon ducts using Ground Penetrating Radar (GPR). This procedure is tested regarding the practical applicability in a roundrobin on a defined type of reference test block. T2 - SMT and NDT-CE 2018 CY - New Brunswick, NJ, USA DA - 27.08.2018 KW - Quality assurance KW - Procedure KW - Reliability KW - Validation KW - Reference specimen PY - 2019 UR - https://asnt.org/smt18papers SN - 978-1-57117-456-7 VL - 11/19 SP - 31 EP - 38 PB - The American Society for Nondestructive Testing, Inc. CY - Columbus, OH, USA AN - OPUS4-47239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ahiboz, D. A1 - Andresen, Elina A1 - Manley, P. A1 - Resch-Genger, Ute A1 - Würth, Christian A1 - Becker, C. T1 - Enhanced photon upconversion using erbium-doped nanoparticles interacting with silicon metasurfaces N2 - Photon upconversion (UC) using trivalent erbium (Er+3) doped crystals is a promising concept to harness near infrared photons of the solar spectrum which cannot be directly absorbed by silicon solar cells. However, their UC efficiency at low-intensity 1 sun illumination is not relevant on device level so far. Exploiting giant near-field enhancement effects on metasurfaces is an appealing approach to enable efficient UC at low irradiance conditions. Here, we report on more than 1000-fold enhanced photon UC of NaYF4:Er+3 nanoparticles interacting with the near-fields supported by a silicon metasurface under 1550 nm excitation. T2 - 48th Photovoltaic Specialists Conference (PVSC) CY - Online meeting DA - 20.06.2021 KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - Excitation power density KW - Brightness KW - NIR KW - Mechanism KW - Modeling KW - Simulation KW - Energy transfer KW - Photonic crystal KW - Enhancement strategy PY - 2021 DO - https://doi.org/10.1109/pvsc43889.2021.9518495 SP - 1 EP - 3 PB - IEEE CY - Berlin AN - OPUS4-53786 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Wegner, Karl David A1 - Kalot, G. A1 - Busser, B. A1 - Pliquett, J. A1 - Köster, U. A1 - Koll, J. C. A1 - Denat, F. A1 - Bodio, E. A1 - Goze, C. A1 - Sacey, L. T1 - NIR aza-BODIPY: a new vector for boron neutron capture therapy (BNCT) N2 - Boron neutron capture therapy (BNCT) relies on the activation of 10B by thermal neutrons, which results in small highly energetic particle emission inducing cancer cells damage. However, in order to overcome the limits of the currently used BNCT agents, it is necessary to design new systems, which can specifically accumulate and deliver a sufficient amount of 10B in tumors. In this study, we designed a 10B-BSH-containing aza-BODIPY (aza-SWIR-BSH). It enabled the efficient vectorization of clinically used 10B-BSH to the tumor, resulting in higher therapeutic activity than the 10B-BSH alone. T2 - EMIM 2021 CY - Göttingen, Germany DA - 24.08.2021 KW - Flourescence KW - Optical probe KW - Dye KW - Photophysics KW - Quantum yield KW - Mechanism KW - NIR KW - SWIR KW - Imaging KW - Method KW - Quality assurance KW - BODIPY KW - Boron Neutron Capture Therapy (BNCT) KW - Medicine KW - Life sciences PY - 2021 AN - OPUS4-53731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Choi, Youngeun ED - Choi, Youngeun ED - Kotthoff, L. ED - Olejko, L. ED - Resch-Genger, Ute ED - Bald, Ilko T1 - DNA origami-based Förster resonance energy-transfer nanoarrays and their application as ratiometric sensors N2 - DNA origami nanostructures provide a platform where dye molecules can be arranged with nanoscale accuracy allowing to assemble multiple fluorophores without dye−dye aggregation. Aiming to develop a bright and sensitive ratiometric sensor system, we systematically studied the optical properties of nanoarrays of dyes built on DNA Origami platforms using a DNA template that provides a high versatility of label choice at minimum cost. The dyes are arranged at distances, at which they efficiently interact by Förster resonance energy transfer (FRET). To optimize array brightness, the FRET efficiencies between the donor fluorescein (FAM) and the acceptor cyanine 3 were determined for different sizes of the array and for different arrangements of the dye molecules within the array. By utilizing nanoarrays providing optimum FRET efficiency and brightness, we subsequently designed a ratiometric pH nanosensor using coumarin 343 as a pH-inert FRET donor and FAM as a pHresponsive acceptor. Our results indicate that the sensitivity of a ratiometric sensor can be improved simply by arranging the dyes into a well-defined array. The dyes used here can be easily replaced by other analyte-responsive dyes, demonstrating the huge potential of DNA nanotechnology for light harvesting, signal enhancement, and sensing schemes in life sciences. KW - DNA KW - Nanoparticle KW - DNA Origami KW - Array KW - FRET KW - Dye KW - pH KW - Nanosensor KW - Fluorescence PY - 2018 DO - https://doi.org/10.1021/acsami.8b03585 SN - 1944-8244 SN - 1944-8252 VL - 10 IS - 27 SP - 23295 EP - 23302 PB - American Chemical Society CY - Washington, DC AN - OPUS4-45798 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Cui A1 - Otto, S. A1 - Dorn, M. A1 - Kreidt, E. A1 - Lebon, J. A1 - Sršan, L. A1 - Di Martino-Fumo, P. A1 - Gerhards, M. A1 - Resch-Genger, Ute A1 - Seitz, M. A1 - Heinze, K. T1 - Deuterated molecular ruby with record luminescence quantum yield N2 - The recently reported luminescent chromium(III) complex 13+ ([Cr(ddpd)2]3+; ddpd=N,N’-dimethyl-N,N’-dipyridine-2-yl-pyridine-2,6-diamine) shows exceptionally strong near-IR emission at 775 nm in water under ambient conditions (F=11%) with a microsecond lifetime as the ligand design in 13+ effectively eliminates non-radiative decay pathways, such as photosubstitution, back-intersystem crossing, and trigonal twists. In the absence of energy acceptors, such as dioxygen, the remaining decay pathways are energy transfer to high energy solvent and ligand oscillators, namely OH and CH stretching vibrations. Selective deuteration of the solvents and the ddpd ligands probes the efficiency of these oscillators in the excited state deactivation. Addressing these energytransfer pathways in the first and second coordination sphere furnishes a record 30% quantum yield and a 2.3 millisecond lifetime for a metal complex with an earth-abundant metal ion in solution at room temperature. The combined fundamental insights will pave the way for selective design strategies in the field of luminescent complexes with earth-abundant metal ions. KW - Record luminescence quantum yield KW - Phorsphorescence KW - Cr-complex KW - Lifetime PY - 2018 DO - https://doi.org/10.1002/ange.201711350 DO - https://doi.org/10.1002/anie.201711350 SN - 1521-3773 VL - 57 IS - 4 SP - 1112 EP - 1116 PB - Wiley-VCH Verlag & Co. KGaA CY - Weinheim AN - OPUS4-45085 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - New project on the quantification of functional groups (FGS) on nanomaterials N2 - The surface chemistry of nanomaterials controls their interaction with the environment and biological species and their fate and is hence also relevant for their potential toxicity. This has meanwhile led to an increasing interest in validated and preferably standardized methods for the determination and quantification of surface functionalities on nanomaterials and initiated different standardization projects within ISO/TC 229 and IEC/TC 113 as well as interlaboratory comparisons (ILCs) of different analytical methods for the quantification of surface coatings by OECD. Here we present the results of a first ILC on the quantification of the amount of amino functionalities on differently sized inorganic nanoparticles done by division Biophotonics and the National Research Council of Canada (NRC) and the PWI 19257 on the Characterization and Quantification of Surface Functional Groups and Coatings on Nanoobjects approved by ISO/TC 229 (WG2) in fall 2022 that will result in a VAMAS study on this topic organized by division Biophotonics. Key words: nanoparticles, surface analysis, surface functional groups, quantification, optical assay, qNMR, VAMAS, standardization, ICL, quality assurance, reference material. T2 - Eingeladener Vortrag Universität Erlangen CY - Erlangen, Germany DA - 18.01.2023 KW - Quality assurance KW - Nano KW - Particle KW - Standard KW - Reference material KW - Surface analysis KW - Quantification KW - Interlaboratory comparison KW - Standardization KW - VAMAS PY - 2023 AN - OPUS4-57044 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Osiopova, Viktoriia A1 - Tavernaro, Isabella A1 - Ge, L. A1 - Kitzmann, W. R. A1 - Heinze, K. A1 - Reithofer, M. R. A1 - Resch-Genger, Ute T1 - Complete protection of NIR-luminescent molecular rubies from oxygen quenching in air by L-arginine-mediated silica nanoparticles N2 - The application of emerging luminophores such as near-infrared (NIR) emissive complexes based on earth-abundant chromium as central ion and triplet-triplet annihilation upconversion (TTA-UC) systems in air as optical reporters for bioimaging or photonic materials for energy conversion requires simple and efficient strategies for their complete protection from uminescence quenching by oxygen. Therefore, we explored the influence of sol–gel synthesis routes on the oxygen protection efficiency of the resulting core and core/shell silica nanoparticles (SiO2 NPs), utilizing the molecular ruby-type luminophores CrPF6 ([Cr(ddpd)2](PF6)3; ddpd = N,N'-dimethyl-N,N'-dipyridin-2-ylpyridin-2,6-diamine) and CrBF4 ([Cr(ddpd)2](BF4)3) with their oxygendependent, but polarity-, proticity-, viscosity-, and concentration-independent luminescence as optical probes for oxygen permeability. The sol–gel chemistry routes we assessed include the classical Stöber method and the underexplored Larginine approach, which relies on the controlled hydrolysis of tetraethoxysilane (TEOS) in a biphasic cyclohexane/water system with the catalyst L-arginine. As demonstrated by luminescence measurements of air- and argon-saturated dispersions of CrPF6- and CrBF4-stained SiO2 NPs of different size and particle architecture, utilizing the luminescence decay kinetics of argon-saturated solutions of CrPF6 and CrBF4 in acetonitrile (ACN) as benchmarks, only SiO2 NPs or shells synthesized by the L-arginine approach provided complete oxygen protection of the CrIII complexes under ambient conditions. We ascribe the different oxygen shielding efficiencies of the silica networks explored to differences in density and surface chemistry of the resulting nanomaterials and coatings, leading to different oxygen permeabilities. Our Larginine based silica encapsulation strategy can open the door for the efficient usage of oxygen-sensitive luminophores and TTA-UC systems as optical reporters and spectral shifters in air in the future. KW - Quality assurance KW - Fluorescence KW - Quantification KW - Advanced materials KW - Nano KW - Quantum yield KW - NIR KW - Characterization KW - Electron microscopy KW - Silica KW - Synthesis KW - Oxygen sensing KW - Surface KW - Doping KW - Lifetime KW - Cr(III) complex KW - Shielding KW - Sensing PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638271 DO - https://doi.org/10.26599/NR.2025.94907241 SN - 1998-0000 VL - 18 IS - 3 SP - 1 EP - 13 PB - SciOpen AN - OPUS4-63827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Potapkin, D. V. A1 - Geißler, Daniel A1 - Resch-Genger, Ute A1 - Goryacheva, I. Y. T1 - Fluorescent quantum dot hydrophilization with PAMAM dendrimer N2 - Polyamidoamine (PAMAM) dendrimers were used to produce CdSe core/multi-shell fluorescent quantum dots (QDs) which are colloidally stable in aqueous solutions. The size, charge, and optical properties of QDs functionalized with the 4th (G4) and 5th (G5) generation of PAMAM were compared with amphiphilic polymer-covered QDs and used as criteria for the evaluation of the suitability of both water solubilization methods. As revealed by dynamic and electrophoretic light scattering (DLS and ELS), the hydrodynamic sizes of the QDs varied from 30 to 65 nm depending on QD type and dendrimer generation, with all QDs displaying highly positive surface charges, i.e., zeta potentials of around +50 mV in water. PAMAM functionalization yielded stable core/multi-shell QDs with photoluminescence quantum yields (Φ) of up to 45%. These dendrimer-covered QDs showed a smaller decrease in their Φ upon phase transfer compared with QDs made water soluble via encapsulation with amphiphilic brush polymer bearing polyoxyethylene/ polyoxypropylene chains. KW - Photoluminescence quantum yield KW - Quantum dots KW - PAMAM dendrimers KW - Phase transfer KW - Fluorescence PY - 2016 DO - https://doi.org/10.1007/s11051-016-3411-4 VL - 18 IS - 108 SP - 1 EP - 9 PB - Springer Science + Business Media B.V. CY - Dordrecht, Netherlands AN - OPUS4-35857 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Resch-Genger, Ute A1 - Richter, Maria A1 - Güttler, Arne A1 - Pauli, Jutta A1 - Vogel, K. A1 - Homann, Christian A1 - Würth, Christian T1 - Extending Certified Spectral Fluorescence Standards for the Calibration and Performance Validation of Fluorescence Instruments to the NIR – Closing the Gap from 750 nm to 940 nm with Two Novel NIR Dyes N2 - Fluorescence methods provide spectral, intensity, polarization, and lifetime information, which contain sample- and instrument-specific contributions. Fluorescence data, comparable across instruments and laboratories, require validated calibration procedures and certified fluorescence standards. KW - Quality assurance KW - Reference material KW - Fluorescence KW - Dye KW - Traceability KW - Metrology KW - Calibration KW - Reference data KW - Reference product KW - Digital certificate KW - NIR KW - Instrument performance validation PY - 2025 SP - 1 EP - 4 PB - Springer Nature CY - London AN - OPUS4-62739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arakawa, Akihiro A1 - Jakubowski, Norbert A1 - Flemig, Sabine A1 - Koellensperger, G. A1 - Rusz, M. A1 - Iwahata, D. A1 - Traub, Heike A1 - Hirata, T. T1 - High-resolution laser ablation inductively coupled plasma mass spectrometry used to study transport of metallic nanoparticles through collagen-rich microstructures in fibroblast multicellular spheroids N2 - We have efficiently produced collagen-rich microstructures in fibroblast multicellular spheroids (MCSs) as a three-dimensional in vitro tissue analog to investigate silver (Ag) nanoparticle (NP) penetration. The MCS production was examined by changing the seeding cell number (500 to 40,000 cells) and the growth period (1 to 10 days). MCSs were incubated with Ag NP suspensions with a concentration of 5 μg/mL for 24 h. For this study, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was used to visualize Ag NP localization quantitatively. Thin sections of MCSs were analyzed by LA-ICP-MS with a laser spot size of 8 μm to image distributions of 109Ag, 31P, 63Cu, 66Zn, and 79Br. A calibration using a NP suspension was applied to convert the measured Ag intensity into the number of NPs present. The determined numbers of NPs ranged from 30 to 7200 particles in an outer rim of MCS. The particle distribution was clearly correlated with the presence of 31P and 66Zn and was localized in the outer rim of proliferating cells with a width that was equal to about twice the diameter of single cells. Moreover, abundant collagens were found in the outer rim of MCSs. For only the highest seeding cell number, NPs were completely captured at the outer rim, in a natural barrier reducing particle transport, whereas Eosin (79Br) used as a probe of small molecules penetrated into the core of MCSs already after 1 min of exposure. KW - Laser ablation KW - ICP-MS KW - Nanoparticle KW - Cell KW - Speroid PY - 2019 DO - https://doi.org/10.1007/s00216-019-01827-w SN - 1618-2642 SN - 1618-2650 VL - 411 IS - 16 SP - 3497 EP - 3506 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-47900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, M. A1 - Zhang, R. A1 - Zhenlong, F. A1 - Yang, J. A1 - Ansari, A. A1 - Ou, Jun A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - Retracted article: Effect of Ca2+ doping on the upconversion luminescence properties of NaYF4:Yb3+/Tm3+ nanoparticles and study of its temperature measurement performance N2 - A solvothermal method was used to prepare a series of Yb3+/Tm3+/Ca2+ co-doped NaYF4 nanoparticles with different Ca2+ contents. Strong upconversion blue fluorescence could be observed under 980 nm laser excitation of the samples. The effect of different Ca2+ contents on the luminescence intensity was investigated, and it was found that the UV-vis upconversion luminescence increased and then decreased with an increasing Ca2+ concentration during the increase of the Ca2+ content from 0 mol% to 25 mol%, reaching the strongest fluorescence at 15 mol%, which was up to about 28 times stronger than that without Ca2+ doping. Furthermore, the mechanism was investigated, and it was found that the doping of Ca2+ disrupted the symmetry of the crystal field, resulting in a significant enhancement of the overall fluorescence. Applied to fluorescence intensity ratio thermometry, the absolute and relative sensitivities are as high as 0.0418 K−1 and 2.31% K−1, respectively, with a minimum temperature resolution of 0.0129 K. KW - Sensor KW - Temperature KW - Lanthanide KW - Luminescence KW - Nanoparticles KW - Upconversion KW - Advanced materials PY - 2022 DO - https://doi.org/10.1039/D2CE00562J SN - 1466-8033 VL - 24 IS - 27 SP - 4887 EP - 4898 PB - Royal Society of Chemistry CY - London AN - OPUS4-56952 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Portesi, C. T1 - qNMR for standardised measurements of surface functionalities on nanoparticles N2 - Engineered nanoparticles have a large application potential in fields such as medicine, sensing, catalysis, energy storage, and opto-electronics [1]. The applicability and performance of engineered nanoparticles is largely determined by their surface chemistry, i.e. functional groups and ligands on the particle surface. However, documented standards to quantify functional groups and ligands currently do not exist. Such standards are required to support quality control of nanomaterial production and surface modification processes, and safe-by-design concepts and to meet regulatory requirements. Here, this issue is addressed by developing and standardizing quantitative Nuclear Magnetic Resonance (qNMR) methods for the characterization of surface functionalized nanoparticles which specifically address the determination of the amount and chemical composition of surface functionalities and coatings. This work is being developed under the EMP project 23NRM02 SMURFnano - Standardised measurements of surface functionalities on nanoparticles. qNMR competence of 7 qNMR laboratories involved in the project was first tested with a molecular model sample i.e. citrate, to be assessed in terms of purity. Citrate is often used as hydrophilic surface ligand for different nanoparticles. Then, the first nanoparticle samples, here a set of aminated SiO2 NPs [1] with a particle size of 100 nm and two amino group densities, prepared and characterized by BAM regarding size and surface charge as well as stability over 21 months with an optical assay and qNMR, were assessed in an international interlaboratory comparison (ILC) on qNMR. Thereby, the amount of surface amino groups introduced by grafting of the silica cores with different amounts of 3-aminopropyl)triethoxysilane (APTES) was quantified by each participant following a sample preparation protocol previously developed by BAM and NRC.The results of the ILC were then used to refine the protocol for sample preparation and to identify critical points for qNMR measurement and data analysis. This work will contribute to the development of a Preliminary Work Item (PWI) 19257 (ISO/TC 229) on surface functional groups and coatings on nano-objects. Also, it will lay the groundwork to perform ILCs on the quantification and determination of the amount of surface functional groups under the roof of VAMAS TWA2 (Surface Chemical Analysis) for different types of nanomaterials possessing industry-relevant surface functionalities using qNMR. These ILCs will be complemented by other techniques like X-Ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). T2 - BERM CY - Halifax, Canada DA - 01.06.2025 KW - Quality assurance KW - Nano KW - Particle KW - Synthesis KW - Advanced materials KW - Characterization KW - Electron microscopy KW - Silica KW - Surface KW - qNMR KW - Optical assay KW - Interlaboratory comparison KW - Metrology KW - Validation KW - Standardization PY - 2025 AN - OPUS4-63443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Monks, M.-J. A1 - Würth, Christian A1 - Kemnitz, Erhard A1 - Resch-Genger, Ute T1 - Dopant ion concentration-dependent upconversion luminescence of cubic SrF2:Yb3+, Er3+ nanocrystals prepared by a fluorolytic sol–gel method N2 - A fluorolytic sol–gel method was used for the fast and simple synthesis of small cubic-phase SrF2:Yb3+, Er3+ upconversion (UC) nanocrystals (UCNC) of different composition at room temperature. Systematic studies of the crystal phase and particle size of this Yb3+,Er3+-concentration series as well as excitation power density (P)-dependent UC luminescence (UCL) spectra, UCL quantum yields (ΦUCL), and UCL decay kinetics yielded maximum UCL performance for doping amounts of Yb3+ of 13.5% and Er3+ of 1.3% in the studied doping and P-range (30–400 W cm−2). Furthermore, ΦUCL were determined to be similar to popular β-NaYF4:Yb3+,Er3+. The relative spectral UCL distributions revealed that all UCNC show a strong red emission in the studied doping and P-range (30–400 W cm−2) and suggest that the UCL quenching pathway for unshelled cubic-phase SrF2:Yb3+,Er3+ UCNC differs from the commonly accepted population and depopulation pathways of β-NaYF4:Yb3+,Er3+ UCNC. In SrF2:Yb3+,Er3+ UCNC the 4S3/2 → 4I13/2 transition exhibits a notably stronger sensitivity towards P and reveals increasing values for decreasing Yb3+–Yb3+ distances while the 4I9/2 → 4I15/2 transition is significantly less affected by P and energy migration facilitated UCL quenching. These results emphasize the complexity of the UC processes and the decisive role of the crystal phase and symmetry of the host lattice on the operative UCL quenching mechanism in addition to surface effects. Moreover, the room temperature UCNC synthesis enabled a systematic investigation of the influence of the calcination temperature on the crystal phase of powder-UCNC and the associated UCL properties. Calcination studies of solid UCNC of optimized doping concentration in the temperature range of 175 °C and 800 °C showed the beneficial influence of temperature- induced healing of crystal defects on UCL and the onset of a phase separation connected with the oxygenation of the lanthanide ions at elevated temperature. This further emphasizes the sensitivity of the UC process to the crystal phase and quality of the host matrix. KW - Upconversion nanoparticle KW - Lanthanide KW - Photophysics KW - Synthesis PY - 2022 DO - https://doi.org/10.1039/d2nr02337g SP - 1 EP - 10 PB - Royal Society of Chemistry AN - OPUS4-55364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Boehm, U. A1 - Nelson, G. A1 - Brown, C. M. A1 - Bagley, S. A1 - Bajcsy, P. A1 - Bischof, J. A1 - Dauphin, A. A1 - Dobbie, I. M. A1 - Eriksson, J. E. A1 - Faklaris, O. A1 - Fernandez-Rodriguez, J. A1 - Ferrand, A. A1 - Gelman, L. A1 - Gheisari, A. A1 - Hartmann, H. A1 - Kukat, C. A1 - Laude, A. A1 - Mitkovski, M. A1 - Munck, S. A1 - North, A. J. A1 - Rasse, T. M. A1 - Resch-Genger, Ute A1 - Schuetz, L. C. A1 - Seitz, A. A1 - Strambio-De-Castillia, C. A1 - Swedlow, J. R. A1 - Nitschke, R. T1 - Author correction: QUAREP-LiMi: a community endeavor to advance quality assessment and reproducibility in light microscopy N2 - This is a corrigendum to the original article "QUAREP-LiMi: a community endeavor to advance quality assessment and reproducibility in light microscopy" that was published in the journal "Nature methods", vol. 18 (2021), pp. 1424-1427. PY - 2022 DO - https://doi.org/10.1038/s41592-021-01387-x SN - 1548-7105 SP - 1 PB - Nature Publishing Group CY - London AN - OPUS4-54270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Fallisch, A. A1 - Petrov, E. P. A1 - Salhany, R. A1 - Forthman, C. A1 - Guttenberg, Z. A1 - Nitschke, R. T1 - Spectral fluorescence standards for the calibration and performance validation of fluorescence microscopes N2 - The standardization and calibration of fluorescence microscopy have become increasingly vital due to the wide-spread use of in life and materials sciences. As the demand for reliable and user-friendly methods to assess micro-scope performance grows, universal calibration tools accessible to both researchers and vendors are needed. To support the standardization of characterization methods in microscopy, it is crucial to provide calibration tools together with standardized operating procedures for their effective implementation. The public-funded project "FluMiKal"* develops calibration tools in the shape of typical microscopic slides to assess key parameters such as spatial resolution, point spread function, spectral sensitivity, linearity and sensitivity of the detection system. The focus is on creating calibration tools that are user-friendly, robust, and versatile in their application. This work addresses the critical parameter of wavelength-dependent spectral sensitivity, which affects the meas-ured signals from the instrument side, yielding instrument-specific data and instrument aging-induced changes over time. For this purpose, μ-slides from ibidi with six channels are used, allowing them to be filled with different solutions containing molecular or nanoscale fluorophores with well-characterized absorption and fluorescence properties. The certified spectral fluorescence standards BAM-F003, F004, F005, and F007 assessed provided as ethanolic solutions by the Federal Institute for Materials Research and Testing (BAM), cover a broad spectral range from the blue to the near-infrared [1], [2]. Dye-based slide prototypes have been used to determine the spectral sensitivity of confocal microscopes from different vendors with various detector types by acquiring the spectral data of the BAM dyes under standardized measurement conditions, demonstrating the applicability of this concept. Proof-of-concept experiments could demonstrate the proper sealing of the slides. Further experiments will explore long-term stability and their potential as standards for relative intensity calibrations. * FluMiKal is funded by the Federal Ministry for Economic Affairs and Climate Action, Germany (WIPANO FKZ 03TN0047B) [1] doi: 10.1007/4243_2008_028. [2] doi: 10.1007/s00216-024-05723-w. T2 - European Light Microscopy Initiative - ELMI 2025 CY - Heidelberg, Germany DA - 03.06.2025 KW - Fluorescence KW - Advanced material KW - Validation KW - Calibration KW - Method comparison KW - Reference material KW - Dye KW - Fluorescence standard KW - Microscopy KW - CLSM KW - Imaging PY - 2025 AN - OPUS4-64206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Muhr, V. T1 - Effect of nanoparticle size on time-resolved upconversion resonance energy transfer N2 - Upconversion nanoparticles (UCNPs) offer new strategies for luminescence-based sensing. The potential of UCNPs to serve as donors in Förster resonance energy transfer (FRET) applications is intensely discussed, owing to their anti-Stokes shifted narrow emission bands, chemical inertness, photostability, and long luminescence lifetimes (> 100 μs). Since FRET is distance dependent, the diameter of the particles is expected to affect the FRET efficiency. In order to identify the ideal particle architecture for FRET-based applications, we performed a systematic spectroscopic study of the influence of the UCNP size on the energy transfer using the organic dyes rose bengal and sulforhodamine B acting as model FRET acceptors for the green upconversion emission. High-quality Yb,Er-doped UCNPs with precisely controlled diameters between 10 and 43 nm were prepared using a high temperature synthesis. The monodisperse, oleate-capped particles were directly modified with the organic dyes by a two-step ligand exchange procedure, resulting in the shortest possible donor-acceptor distance. Successful FRET was demonstrated through the simultaneous drastic reduction of the luminescence intensity and the lifetime of the respective upconversion emission. In contrast to intensity measurements, time-resolved studies on both donor and acceptor luminescence allowed for the elimination of dependencies on excitation power density and particle concentration and for the discrimination between inner filter effects and FRET. The maximum FRET efficiency was observed at a particle diameter around 21 nm, which was attributed to an increasing fraction of the total amount of Er3+ donors inside the UCNPs being within Förster distance. Smaller UCNP diameters did not further improve the FRET efficiency, demonstrating the growing contribution of opposing effects, like the competition of non-radiative surface deactivation, at larger surface-to-volume ratios. This comprehensive understanding of energy transfer processes at the surface of UCNPs is essential for the rational design of upconversion FRET platforms for applications in sensing, imaging, and theranostics with improved sensitivity, reliability and comparability. The energy transfer can also be utilized to shift the luminescence emission by the choice of the organic dye in order to explore applications that require specific emission wavelengths due to interfering substances, while still making use of the advantages of near-infrared excitation. T2 - Material Research Society - Spring Meeting CY - Phoenix, Arizona, USA DA - 17.04.2017 KW - Upconversion KW - FRET KW - Organic dyes PY - 2017 AN - OPUS4-40096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Bridge monitoring using embedded ultrasonics First results from the BLEIB reference structure N2 - The BLEIB reference structure The structure is a two-span, 24 m long inverse u-shaped post-tensioned concrete beam. Fibre optic sensing cables, RFID sensors and ultrasonic transducers are permanently embedded. Other sensing techniques (vibrational, optical, ultrasonic, mechanical) are applied externally. Tension can be adjusted. Loads can be placed at arbitrary locations. Limited damage is introduced to one span. The BLEIB reference structure is located at BAM‘s test site in Horstwalde, south of Berlin. Ultrasonic transducer before concreting. Embedded ultrasonic transducers 14 piezo transducers have been embedded before concreting. They are located in five sections, two close to the centers of both spans respectively and one above the central bearing. Load experiment and data evaluation In a first experiment load 2 (weight 2 t) was moved three times along the southern (right) span. The tension forces were modified as well. Ultrasonic transmission measurements were repeated over time and evaluated using Coda Wave Interferomerry (CWI), which determines correlation coefficients and relative velocity changes as subtle indicators for loads and other changes in the material. T2 - New mathematics for a safer world: wave propagation in heterogeneous materials CY - Edinburgh, UK DA - 12.06.2017 KW - Bridge monitoring KW - Ultrasound KW - Embedded transducers KW - Coda wave interferometry PY - 2017 AN - OPUS4-40578 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Güttler, Arne T1 - Certified Reference Materials for the Quantification and Standardization of Fluorescence-based Measurements N2 - The size and shape of photoluminescence signals is affected by wavelength-, polarization-, and time-dependent instrumentspecific contributions and the compound- and environment-specific photoluminescence quantum yield. The former hamper the comparability of fluorescence measurements performed on different measuring devices. The commonly relatively done determination of the performance parameter requires suitable quantum yield standards with well-known. The performance of such measurements is, e.g., described in the written standard IEC 62607 currently revised. T2 - Colloquium für Optische Spektrometrie 2025 CY - Jena, Germany DA - 24.09.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Advanced material KW - Calibration KW - Characterization KW - Fluorescence quantum yield KW - Phosphor KW - Absolute KW - Integrating sphere spectroscopy KW - Dye KW - Standardization KW - Reference material KW - Interlaboratory comparison KW - Uncertainty PY - 2025 AN - OPUS4-64213 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bergstrand, J. A1 - Li, Q. A1 - Huang, B. A1 - Peng, X. A1 - Würth, Christian A1 - Resch-Genger, Ute A1 - Zhan, Q. A1 - Widengren, J. A1 - Agren, H. A1 - Liu, H. T1 - On the decay time of upconversion luminescence N2 - In this study, we systematically investigate the decay characteristics of upconversion luminescence (UCL) under anti-Stokes excitation through numerical simulations based on rate-equation models. We find that a UCL decay profile generally involves contributions from the sensitizer’s excited-state lifetime, energy transfer and cross-relaxation processes. It should thus be regarded as the overall temporal response of the whole upconversion system to the excitation function rather than the intrinsic lifetime of the luminescence emitting state. Only under certain conditions, such as when the effective lifetime of the sensitizer’s excited state is significantly shorter than that of the UCL emitting state and of the absence of cross-relaxation processes involving the emitting energy level, the UCL decay time approaches the intrinsic lifetime of the emitting state. Subsequently, Stokes excitation is generally preferred in order to accurately quantify the intrinsic lifetime of the emitting state. However, possible cross-relaxation between doped ions at high doping levels can complicate the decay characteristics of the luminescence and even make the Stokesexcitation approach fail. A strong cross-relaxation process can also account for the power dependence of the decay characteristics of UCL. KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Mechanism KW - Quantum yield KW - Photophysics KW - Lifetime KW - Modeling PY - 2019 DO - https://doi.org/10.1039/c8nr10332a VL - 11 IS - 11 SP - 4959 EP - 4969 PB - RSC Royal Society of Chemistry AN - OPUS4-47888 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niederleithinger, Ernst A1 - Katzenbach, R. A1 - Klingmüller, O. A1 - Hillmann, S. A1 - Willmes, Michael T1 - REFUND: Untersuchung von Bestandsgründungen für eine Entscheidung zur Wiedernutzung T1 - REFUND: Investigation of existing foundations and decision making before re-use N2 - Vor einer geplanten Weiter- oder Wiedernutzung von Bestandsgründungen stellt sich die Frage nach deren Lage, Geometrie und Zustand im Untergrund. Hierfür gibt es verschiedene Prüfverfahren. Die Abläufe bei Planung und Prüfung sind jedoch bisher nicht standardisiert und die Möglichkeiten bzw. Grenzen der Prüfverfahren den Planern wenig bekannt. Im Forschungsprojekt REFUND (2014–2016) wurden unter Berücksichtigung der aktuellen Normen und des Stands der Technik Ablaufdiagramme für die Planung der Wiedernutzung sowie die Untersuchung des Bestands entwickelt. Dies geschah getrennt für Einzel- und Streifenfundamente, Platten und Pfähle. An zwei Praxisbeispielen wurden die Abläufe getestet und optimiert. Die Ergebnisse wurden in einem Handbuch zusammengefasst. Es soll Planer und andere Verantwortliche bei der wirtschaftlich und technisch optimierten Durchführung von Wiedernutzungsprojekten unterstützen. N2 - Before re-using existing foundations they have to be investigated for position, geometry and condition in the subsurface. The procedures and protocols haven't been standardized yet. Capabilities and limitations of appropriate testing methods are not known to all stakeholders. In the frame of the research project REFUND (2014-2016) we have developed decision trees for the planning and the investigation process, separately for single and strip foundations, slabs and piles. The protocols were tested in line with two actual projects. The results have been compiled in a handbook, which will support planners and other participants in a technical and economical optimized way to perform re-use of foundations. KW - Fundament KW - Wiedernutzung KW - Entscheidung KW - Zerstörungsfrei PY - 2017 DO - https://doi.org/10.1002/bate.201700038 SN - 1437-0999 VL - 94 IS - 10 SP - 676 EP - 681 PB - Ernst & Sohn CY - Berlin AN - OPUS4-42615 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Quantifying functional groups and coatings on nanoobjects N2 - Engineered nanomaterials (NM) of different size, shape, chemical composition, and surface chemistry are increasingly used for many key technologies of the 21st century and consumer products. This includes polymer and silica or silica-coated nanoparticles (NP) with covalently bound surface groups, semiconductor quantum dots (QD), metal and metal oxide NP, and lanthanide NP with coordinatively or electrostatically bound ligands, as well as surface-coated nanostructures like micellar encapsulated NP. Decisive for most applications of NMs are their specific surface properties, which are largely determined by the chemical nature and amounts of ligands and functional groups (FGs) on the NM surface. The surface chemistry can strongly affect the physicochemical properties of NM, their charge, hydrophilicity/hydrophobicity, reactivity, function, stability, and processability and thereby their impact on human health and environment. Knowledge of NM surface chemistry plays an important role for NM functionality and performance in (bio)applications and the fate, exposure, dissolution, transformation, and accumulation of NM, and thus, the potential risks for human health and the environment. This highlights the importance of reliable, validated, and eventually standardized analytical methods for analyzing and quantifying NM surface chemistry for process and quality control of NM production, safe use of NMs, design of novel NM, and sustainable concepts for NM fabrication.[1-3] In this context, interlaboratory comparisons (ILCs) are needed to assess method reliability and reference materials with known surface chemistries for establishing surface analytical methods and their performance validation.[2,4] Also, to respond to the increasing number of samples to be analyzed, cost-efficient automation concepts for surface analysis are needed that can be realized with affordable and preferably commercial instrumentation.[5] Here, we provide an overview of analytical methods for FG analysis and quantification used by us for quantifying broadly utilized FGs and ligands on different types of NMs with electrochemical titration methods, optical assays, nuclear magnetic resonance (NMR) and vibrational (IR) spectroscopy, and X-ray based and thermal analysis methods.[1,2] Thereby, method- and material-related challenges are addressed, and the importance of multi-method characterization approaches easing method validation by method cross-validation. Special emphasis is dedicated to simple, versatile, and cost-efficient methods such as optical assays and electrochemical titration methods. T2 - eMRS Fall Meeting 2025 CY - Warsaw, Poland DA - 15.09.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Characterization KW - Advanced material KW - Surface KW - Standardization KW - Reference material KW - Functional group KW - Quantification KW - Coating KW - Interlaboratory comparison KW - Uncertainty PY - 2025 AN - OPUS4-64183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - Multicolored sensors based on silica and polymeric particles for ratiometric monitoring of pH, oxygen and saccharides N2 - In recent years, the use of functionalized micro- and nanomaterials has increased rapidly for a wide range of applications in the life and material sciences, due to their unique properties in combination with their high surface-to-volume ratio and stability. For instance, functionalized micro- and nanomaterials, that are labeled or stained with a multitude of sensor dyes can be used for monitoring, and quantification of neutral and ionic analytes. These materials have several advantages as compared to conventional molecular probes like enhanced brightness, ease of designing ratiometric systems by combining analyte-sensitive and inert reference dyes, and increased photostability. Moreover, stained nanoparticles can enable the use of hydrophobic dyes in aqueous environments. Versatile templates and carriers for the fabrication of nanosensors by staining and/or labeling with different fluorophores and sensor molecules are biocompatible silica and polymeric particles, because they can be synthesized in large scales at low costs with different surface chemistries. Here we present our work on multicolored sensors for the measurement of pH, oxygen and saccharides utilizing commercially available or in-house synthesized silica and polymeric particles. T2 - 4th European Biosensor Symposium 2023 CY - Aachen, Deutschland DA - 27.08.2023 KW - Nano- and microsensors KW - Silica and polystyrene nanoparticles KW - PH probe KW - Ratiometric sensors KW - Optical spectroscopy KW - Dye KW - Saccharide sensing KW - Multicolored PY - 2023 AN - OPUS4-59125 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella A1 - Sander, P. A1 - Andresen, E. A1 - Schedler, U. A1 - Resch-Genger, Ute T1 - Potentiometric and Optical Titration for Cost- Efficient Quantification of Surface Functional Groups on Silica Nanoparticles N2 - Surface chemistry of engineered nanomaterials (NMs) plays a critical role not only in determining their interactions with the environment but also in their stability, safety, and functionality across diverse applications ranging from catalysis to biomedicine. Accurate quantification of surface functional groups (FGs) is therefore essential for quality control, risk assessment, and performance optimization.[1] However, many existing analytical techniques are either cost-intensive, require specialized instrumentation, or lack scalability for routine use. In this study, we present a comparative evaluation of potentiometric and optical titration as two simple, cost-efficient, and automatable methods for quantifying surface functional groups on a variety of surface-modified silica nanoparticles (SiO₂ NPs). These NPs were chosen as they are among the most frequently utilized engineered NMs in the life and material sciences. Potentiometric titration, based on pH monitoring during acid-base neutralization, offers a direct and label-free approach to determine the total amount of FGs. Optical titration provides a complementary method with potential for high-throughput screening. To examine the accuracy and robustness of our stepwise-optimized workflows and the achievable relative standard deviations (RSDs), measurements were performed by multiple operators in two laboratories. Method validation was conducted through cross-comparison with traceable, chemo-selective quantitative nuclear magnetic resonance spectroscopy (qNMR) and thermogravimetric analysis (TGA). A comparison with optical assays highlights the importance of measuring both quantities for comprehensive characterization of surface-modified NMs.[2] A combined NM surface analysis using optical assays and pH titration will simplify quality control of NM production processes and stability studies, and can yield large datasets for NM grouping in sustainable and safe(r)-by-design studies. T2 - eMRS Fall Meeting 2025 CY - Warsaw, Poland DA - 15.09.2025 KW - Fluorescence KW - Advanced material KW - Synthesis KW - Characterization KW - Nano KW - Particle KW - Silica KW - Surface analysis KW - Validation KW - qNMR KW - Fluram assay KW - Functional group KW - Quantification KW - Potentiometry KW - Amino groups KW - Fluorescamine KW - Calibration KW - Method comparison PY - 2025 AN - OPUS4-64205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - Multivalent presentation of phenylpropenic acid amide inspired ligands by various nanoparticles and their potential use in anti-inflammatory therapy N2 - Over the years, inflammation has become one of the most rapidly developing areas in medical research, due to new studies indicating its important role in chronical diseases, thrombosis and cancer. A promising target for anti-inflammatory therapy are the multistep adhesion process of leukocytes from the blood vessels into the inflamed tissue. and the numerous involved receptors and ligands. In particular, selectins and their respective carbohydrate ligands can inhibit this key step of the inflammation cascade. In previous work, it was shown that the multivalent presentation of highly negatively charged sulfated and carboxylated ligands on the particle surface can mimic natural selectin binders and increase the inhibition significantly. Recent studies of the antioxidant and health promoting properties of cocoa, dark chocolate and red clover indicating potential anti-inflammatory properties of their clovamide-type phenylpropenoic acid amides, which are able to inhibit p-selectin expression and platelet-leukocyte interactions. Following the idea of small-molecule targeting drugs, we selected different epitopes and immobilized their sulfated derivatives onto different types nanoparticles, followed by a screening of their performance. T2 - SALSA Make and Measure 2024: Interfaces CY - Berlin, Germany DA - 11.09.2024 KW - Gold colloids KW - Surface group analysis KW - Method KW - Quantification KW - Screening KW - Nano KW - Particle KW - Synthesis KW - Quality assurance KW - Surface ligands PY - 2024 AN - OPUS4-62159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Hoffmann, Katrin A1 - Abbandonato, Gerardo T1 - Determination of quantum yields of semiconductor nanocrystals at the single emitter level via fluorescence correlation spectroscopy N2 - Comparing the photoluminescence (PL) properties of ensembles of nanocrystals like semiconductor quantum dots (QDs) with single particle studies is of increasing interest for many applications of These materials as reporters in bioimaging studies performed under very dilute conditions or even at the single particle level. Particularly relevant is here the PL quantum yield (ΦF), which determines the signal size together with the reporter’s molar extinction coefficient and is a direct measure for nanocrystal quality, especially for the inorganic surface passivation shell and its tightness, which can be correlated also with nanocrystal stability and the possible release of heavy metal ions. Exemplarily for red and green emitting CdTe nanocrystals, we present a method for the determination of ΦF of nanoparticle dispersions at ultralow concentration compared to cuvette measurements using fluorescence correlation spectroscopy (FCS), a single molecule method, and compared to molecular dyes with closely matching spectral properties and known ΦF. Our results underline the potential of this approach, provided that material-inherent limitations like ligand- and QD-specific aggregation affecting particle diffusion and QD drawbacks such as their complex and power-dependent blinking behavior are properly considered as shown here. KW - Semiconductor nanocrystal KW - Quantum dot KW - Quantum yield KW - Fluorescence correlation spectroscopy FCS KW - Single molecule PY - 2018 DO - https://doi.org/10.1039/c7nr09332b SN - 2040-3364 SN - 2040-3372 VL - 10 IS - 15 SP - 7147 EP - 7154 PB - Royal Society of Chemistry AN - OPUS4-44894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Homann, C. A1 - Krukewitt, Lisa A1 - Frenzel, Florian A1 - Grauel, Bettina A1 - Würth, Christian A1 - Resch-Genger, Ute A1 - Haase, M. T1 - NaYF4:Yb,Er/NaYF4 Core/Shell Nanocrystals with High Upconversion Luminescence Quantum Yield N2 - Upconversion core/shell nanocrystals with different mean sizes ranging from 15 to 45 nm were prepared via a modified synthesis procedure based on anhydrous rare‐earth acetates. All particles consist of a core of NaYF4:Yb,Er, doped with 18 % Yb3+ and 2 % Er3+, and an inert shell of NaYF4, with the shell thickness being equal to the radius of the core particle. Absolute measurements of the photoluminescence quantum yield at a series of different excitation power densities show that the quantum yield of 45 nm core/shell particles is already very close to the quantum yield of microcrystalline upconversion phosphor powder. Smaller core/shell particles prepared by the same method show only a moderate decrease in quantum yield. The quantum yield of 15 nm core/shell particles, for instance, is reduced by a factor of three compared to the bulk upconversion phosphor at high power densities (100 W cm−2) and by approximately a factor of 10 at low power densities (1 W cm−2). KW - Core shell structure KW - Upconversion KW - Non lienear processes KW - Nanoparticle KW - Quantum yield PY - 2018 DO - https://doi.org/10.1002/anie.201803083 VL - 57 IS - 28 SP - 8765 EP - 8769 PB - Wiley-VCH AN - OPUS4-45574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meijer, M. S. A1 - Rojas-Gutierrez, P. A. A1 - Busko, D. A1 - Howard, I. A. A1 - Frenzel, Florian A1 - Würth, Christian A1 - Resch-Genger, Ute A1 - Richards, B. S. A1 - Turshatov, A. A1 - Capobianco, J. A. A1 - Bonnet, S. T1 - Absolute upconversion quantum yields of blue-emitting LiYF4:Yb3+,Tm3+ upconverting nanoparticles N2 - The upconversion quantum yield (QY) is an essential parameter for the characterization of the optical performance of lanthanoid-doped upconverting nanoparticles (UCNPs). Despite its nonlinear dependence on excitation power density, it is typically reported only as a single number. Here, we present the first measurement of absolute upconversion quantum yields of the individual emission bands of blue light-emitting LiYF4:Yb3+,Tm3+ UCNPs in toluene. Reporting the quantum yields for the individual emission bands is required for assessing the usability of UCNPs in various applications that require upconverted light of different wavelengths, such as bioimaging, photocatalysis and phototherapy. Here, the reliability of the QY measurements is demonstrated by studying the same batch of UCNPs in three different research groups. The results show that whereas the total upconversion quantum yield of these UCNPs is quite high - typically 0.02 at a power density of 5 W/cm2 — most of the upconverted photon flux is emitted in the 794 nm upconversion band, while the blue emission band at 480 nm is very weak, with a much lower quantum yield of 6 times 10^5 at 5 W/cm2. Overall, although the total upconversion quantum yield of LiYF4:Yb3+,Tm3+ UCNPs seems satisfying, notably for NIR bioimaging, blue-light demanding phototherapy applications will require better-performing UCNPs with higher blue light upconversion quantum yields. KW - Core-shell nanoparticles KW - Lanthanide-doped nayf-4 KW - Near-infrared light KW - Upconverting nanoparticles KW - Photocatalytic activity KW - Nanocrystals KW - Photosensitizer PY - 2018 DO - https://doi.org/10.1039/c8cp03935f VL - 20 IS - 35 SP - 22556 EP - 22562 PB - Royal Society of Chemistry AN - OPUS4-46370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jakubowski, Norbert A1 - Müller, L. A1 - Traub, Heike A1 - Esteban-Fernández, D. A1 - Panne, Ulrich A1 - Herrmann, Antje A1 - Schellenberger, E. A1 - Theuring, F. A1 - Kneipp, Janina T1 - Imaging by laser ablation ICP-MS N2 - ICP-MS is a well-established analytical method which excels by high accuracy, high dynamic range and extremely low limits of detection for most metals. Furthermore ICP-MS offers a very high multi-element coverage so that many elements of the periodic table can be detected simultaneously. In this series of lectures, we want to focus on the historical developments, fundamentals, instrumentation and novel applications of ICP-MS in the life and material sciences. T2 - Ringvorlesung Analytik CY - Humboldt-Universität zu Berlin DA - 23.06.2017 KW - Laser ablation ICP-MS KW - Bio-Imaging PY - 2017 AN - OPUS4-40757 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Meng, M. A1 - Zhang, R. A1 - Cheng, Z. A1 - Fa, X. A1 - Yang, J. A1 - Ansari, A. A. A1 - Ou, Jun A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - Retraction: Effect of Ca2+ doping on the upconversion luminescence properties of NaYF4:Yb3+/Tm3+ nanoparticles and study of its temperature measurement performance N2 - Retraction of "Effect of Ca2+ doping on the upconversion luminescence properties of NaYF4:Yb3+/Tm3+ nanoparticles and study of its temperature measurement performance" by Mingzhou Meng et al., CrystEngComm, 2022, 24, 4887–4898, https://doi.org/10.1039/D2CE00562J. The Royal Society of Chemistry, with the agreement of the authors, hereby wholly retracts this CrystEngComm article due to concerns with the reliability of the data. PY - 2023 DO - https://doi.org/10.1039/d3ce90111d SN - 1466-8033 VL - 25 IS - 33 SP - 4768 PB - Royal Society of Chemistry CY - London AN - OPUS4-58494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abram, Sarah-Luise A1 - Tavernaro, Isabella A1 - Resch-Genger, Ute A1 - Johnston, L. J. A1 - Zou, S. T1 - Nanoscale reference and test materials for the validation of characterization methods for engineered nanomaterials — current state, limitations, and needs N2 - The rational design of engineered nanomaterials (NMs) with improved functionality and their increasing industrial application requires reliable, validated, and ultimately standardized characterization methods for their application-relevant, physicochemical key properties such as size, size distribution, shape, or surface chemistry. This calls for nanoscale (certified) reference materials (CRMs; RMs) and well-characterized reference test materials (RTMs) termed also quality control (QC) samples, assessed, e.g., in interlaboratory comparisons, for the validation and standardization of commonly used characterization methods. Thereby, increasing concerns regarding potential risks of NMs are also addressed and the road for safe and sustainable-by-design concepts for the development of new functional NMs and their use as nanomedicines is paved. With this respect, we will provide an overview of relevant international standardization and regulatory activities, definitions, and recommendations on characterization methods and review currently available organic or inorganic nanoscale CRMs, RMs, and RTMs, including their characterization or certification. In addition, we will highlight typical applications to streamline the regulatory approval process and improve manufacturability including the special challenges imposed by the colloidal nature and sometimes limited stability of NMs. Subsequently, we will critically assess the limitations of currently available nanoscale RMs and RTMs and address the gaps to be filled in the future such as the availability of NMs that come with reference data on properties other than commonly addressed particle size, such as surface chemistry or particle number concentration, or more closely resemble commercially available formulations or address application-relevant matrices. KW - Nano KW - Particle KW - Silica KW - Quality assurance KW - Reference material KW - Review KW - Surface chemistry KW - Size KW - Shape KW - Particle number concentration KW - Lipid nanoparticles KW - Metal nanoparticles KW - Liposomes PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625746 DO - https://doi.org/10.1007/s00216-024-05719-6 SN - 1618-2650 SP - 1 EP - 21 PB - Springer AN - OPUS4-62574 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Pilch, A. A1 - Würth, Christian A1 - Kaiser, Martin A1 - Wawrzynczyk, D. A1 - Kurnatowska, M. A1 - Arabasz, S. A1 - Prorok, K. A1 - Samoc, M. A1 - Strek, W. A1 - Bednarkiewicz, A. T1 - Shaping luminescent properties of Yb3+ and Ho3+ co-doped upconverting core-shell ß-NaYF4 nanoparticles by dopant distribution and spacing N2 - At the core of luminescence color and lifetime Tuning of rare earth doped upconverting nanoparticles (UCNPs), is the understanding of the Impact of the particle architecture for commonly used sensitizer (S) and activator (A) Ions. In this respect, a series of core@Shell NaYF4 UCNPs doped with Yb3+ and Ho3+ ions are presented here, where the same dopant concentrations are distributed in different particle architectures following the scheme: YbHo core and YbHo@..., ...@YbHo, Yb@Ho, Ho@Yb, YbHo@Yb, and Yb@YbHo core-Shell NPs. As refealed by quantitative steady-state and time-resolved luminescence studies, the relative spatial Distribution of the A and S ions in the UCNPs and their protection from surface quenching has a critical Impact on ther luminescence characteristics. Although the increased amount of Yb3+ Ions boosts UCNP Performance by amplifying the Absorption, the Yb3+ ions can also efficiently dissipate the energy stored in the material through energy Migration to the surface, thereby reducing the Overall energy Transfer Efficiency to the activator ions. The results provide yet another proof that UC Phosphor chemistry combined with materials Engineering through intentional core@shell structures may help to fine-tune the luminescence Features of UCNPs for their specific future applications in biosensing, bioimaging, photovoltaics, and Display technologies. KW - Fluorescence KW - Upconversion KW - NIR KW - Nonlinear KW - Nanoparticle KW - Surface chemistry KW - Quantum yield KW - Liftetime KW - Nanocrystal KW - Lanthanide KW - Ho(III) KW - Yb(III) KW - Mechanism KW - Absolute flourescence KW - Excitation power density dependence PY - 2017 DO - https://doi.org/10.1002/smll.201701635 SN - 1613-6810 VL - 13 IS - 47 SP - 1701635, 1 EP - 13 PB - WILEY-VCH Verlag GmbH & co. KGaA CY - Weinheim AN - OPUS4-43629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stroyuk, O. A1 - Weigert, Florian A1 - Raevskaya, A. A1 - Spranger, F. A1 - Würth, Christian A1 - Resch-Genger, Ute A1 - Gaponik, N. A1 - Zahn, D. R. T. T1 - Inherently broadband photoluminescence in Ag−In−S/ZnS quantum dots observed in ensemble and single-particle studies N2 - We present a series of results that demonstrate that the broadband photoluminescence (PL) of aqueous glutathione-capped Ag−In−S (AIS) nanocrystals (NCs) is an inherent property of each NC, rather than a collective characteristic of an NC ensemble. By analyzing parameters affecting the PL features such as the postsynthesis annealing and the deposition of a passivating ZnS shell, we found no correlation between the spectral width of the PL band of AIS (AIS/ZnS) NCs and the density of the lattice defects. Analysis of the PL spectra of a series of size-selected AIS/ZnS NCs revealed that the PL width of fractionated NCs does not depend on the NC size and size distribution. The PL measurements in a broad temperature window from 320 to 10 K demonstrated that the PL width does not decrease with decreasing temperature as expected for an emission arising from thermally activated detrapping processes. Also, we show that the model of the self-trapped exciton can be versatilely applied to reconstruct the PL spectra of different AIS NCs and can account for the effects typically attributed to variations in defect state energy. Measurements of the PL properties of single AIS/ZnS NCs highlighted the broadband nature of the emission of individual NCs. The presented results show that the broadband PL of ternary NCs most probably does not originate from lattice defects but involves the NC lattice as a whole, and, therefore, by tailoring the NC structure, PL efficiencies as high as those reported for binary cadmium or lead chalcogenide NCs can be potentially reached. KW - Nano KW - Nanomaterial KW - Ternary quantum dots KW - AIS KW - Semiconductor nanocrystal KW - Photoluminescence KW - Mechanism KW - Single particle spectroscopy KW - Quantum yield KW - Photophysics PY - 2019 DO - https://doi.org/10.1021/acs.jpcc.8b11835 SN - 1932-7447 VL - 123 IS - 4 SP - 2632 EP - 2641 PB - ACS AN - OPUS4-47419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, M. A1 - Zhang, T. A1 - Wang, J. A1 - Cheng, Z. A1 - Li, Z. A1 - Qiao, X. A1 - Wen, J. A1 - Resch-Genger, Ute A1 - Long, W. A1 - Ou, Jun T1 - Preparation of NaYF4: Yb3+/Tm3+@NaYF4@β-CD upconversion nanoparticles and application of their fluorescence temperature sensing properties N2 - The NaYF4: Yb3+/Tm3+@NaYF4@β-CD upconversion nanoparticles were successfully prepared by the solvothermal method, and the samples were pure hexagonal phase with good crystallinity and homogeneous size, asevidenced by XRD and TEM analysis. The FT-IR analysis shows that β-CD is successfully encapsulated on the surface of NaYF4: Yb3+/Tm3+@NaYF4 nanoparticles. The fluorescence intensity 3and lifetime were significantly increased after coating the inert layer on the surface of core nanoparticles. After further surface modification of β-CD, the fluorescence intensity and fluorescence lifetime were reduced, but the overall fluorescence was stronger. Temperature measurements using the fluorescence intensity ratio technique were found to have relatively low reliability and absolute sensitivity for temperature measurements using thermally coupled energy levels. However, the reliability of temperature measurements using non-thermally coupled energy levels is significantly higher and the absolute sensitivity is much higher than for measurements at thermally coupled levels. Since the maximum absolute sensitivity, maximum relative sensitivity and minimum temperature resolution are determined to be 0.1179 K-1, 2.19 %K􀀀 1 and 0.00019 K, respectively, NaYF4: Yb3+/Tm3+@NaYF4@β-CD upconversion nanoparticles are expected to be widely used in the biomedical field due to their feasibility, reliability, non-toxicity and harmlessness. KW - Upconversion KW - Surface modification KW - Fluorescence intensity ratio KW - Thermally coupled levels KW - Non-thermally coupled levels PY - 2023 DO - https://doi.org/10.1016/j.optmat.2022.113389 SN - 0925-3467 VL - 136 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-57105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya T1 - New pyrrolidinylvinylquinoxaline derivatives with aggregation-induced emission as possible fluorescent nanoreporters N2 - Background: Fluorescent amplification strategies with nanomaterials are of increasing importance for a wide range of applications in material and life sciences. This includes their use as reporters for optical assays, targeted probes in bioimaging studies and as sensor materials. Some organic dyes with twisted skeleton conformation show enhanced emission upon aggregation (AIE)in contrast to the majority of dyes which reveal aggregation-caused fluorescence quenching (ACQ). Such dyes could be candidates for amplification strategies. Here we present a series of new hydrophobic pyrrolidinylvinylquinoxaline (PVQ) dyes with different substituents, which are supposed to show AIE. This group of twisted skeleton conformed dyes are emissive in the solid state, as aggregates, and encapsulated in hydrophobic polymer materials. Results: The PVQ derivatives show strong AIE in ethanol-water-mixtures containing more than 80% water as indicated by the strong increase in fluorescence quantum yields and lifetimes upon dye aggregation and nanoparticle formation. The size of the AIE effect and the observed fluorescence enhancement are in good agreement with DFT- and XRD calculations of the torsion angle between the four different substituents and the planar backbone of the dye. In all cases, particles with diameters smaller than 450 nm were formed. The hydrodynamic diameter of the aggregates was controlled by the water content, with an increasing water content causing a decrease of the hydrodynamic diameter. In the presence of polyelectrolytes or surfactants, μm-sized crystals were obtained. Encapsulation of the dyes in preformed polymer particles provides stabil and strongly emissive nanoparticles. Conclusion: Based on new PVQ, we yielded highly emissive nanoparticles. The correlation between the torsion angle and the AIE effect underlines structural control of AIE by substitution pattern in this dye class. The loading of a polymer matrix with PVQ resulted in stable nanoparticles with varied surface modification. Applications of these effects in fluorescence assays are currently studied. T2 - Innovation Forum Senftenberg 2016 CY - Senftenberg, Germany DA - 01.06.2016 KW - Aggregation-induced emission KW - Fluorescent nanoreporters KW - Fluorescent amplification strategies PY - 2016 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-38287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kraft, Marco T1 - Particle Size Dependent Absolute Photoluminescence Quantum Yields and Lifetimes of Hexagonal beta-NaYF4: 2 % Er3+, 20 % Yb3+ Upconversion Nanoparticles in Cyclohexane and Water N2 - Hexagonal beta-NaYF₄ doped with 20 % Yb and 2 % Er is an efficient upconversion (UC) phosphor for the conversion of 976 nm to 845 nm, 655 nm and 540 nm light. The emission behavior of this material is strongly influenced by the particle size, surface chemistry, and microenvironment. Especially the design of nm-sized UC particles for bioanalytical applications requires reliable spectroscopic tools for the characterization of the optical properties of these materials like the UC quantum yield (QYUC) in aqueous media. The UC emission originates from multiphotonic absorption processes, rendering the QYUC excitation power density (P) dependent. The P-dependent absolute measurement of QYUC in aqueous media with an excitation wavelength of 976 nm presents a considerable challenge due to the low absorption coefficients of the UC materials and the absorption of water at this wavelength. Here, we present the P-dependent QYUC of 21 nm, 26 nm and 31 nm-sized NaYF₄ UC particles dispersed in cyclohexane and aqueous solutions, in view of bioanalytical applications. To gain a better insight of the photonic nature of the upconversion mechanism and the quenching processes involved, the luminescence decay behavior as well as the P-dependent red-to-green luminescence intensity ratios and slope factors of the different emission bands are studied in both solvents. These results present an important step to the rational design of brighter upconversion nanoparticles. T2 - UPCON conference 2016 CY - Wroclaw, Poland DA - 23.05.2016 KW - Water KW - Upconversion KW - Quantum Yield KW - Lifetime KW - Cyclohexane PY - 2016 AN - OPUS4-38131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kage, Daniel T1 - FLiMFlow – Recent achievements in flow cytometry with lifetime detection and lifetime-encoded beads N2 - Flow cytometry is a widespread technique in biological research and clinical applications. Two different directions are currently of importance in development of new methods in this field. Whereas analyses in research become increasingly complex and require a growing number of simultaneously detectable codes and fluorescent labels, also low-cost methods and portable devices are needed in routine application. Lifetime encoding could present an alternative to common spectral multiplexing. On the one hand, it addresses the need for additional codes by combining spectral and lifetime multiplexing. On the other hand, using only lifetime encoding could help to reduce instrument costs by keeping the number of excitation sources and detectors low. Here, we report on our recent progress in employing dye-stained lifetime-encoded polymer microparticles as a model system for lifetime encoding in flow cytometry. The discrimination of two lifetime codes was achieved with two bead sets. Moreover, the simultaneous detection of a spectrally different ligand fluorescence signal could be demonstrated. T2 - FLiMFlow meeting CY - Pisa, Italy DA - 28.09.2016 KW - Flow cytometry KW - Fluorescence KW - Life sciences KW - Lifetime encoding KW - Polymer particles PY - 2016 AN - OPUS4-38239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kage, Daniel T1 - Fluorescence lifetime multiplex flow cytometry system (FliMFlow-MultiLife) N2 - Flow cytometry is a common tool in biological research and clinical analyses. In current developments, there are two different tendencies of interest. Firstly, we face the need for analysis methods that are capable of addressing more and more involved analysis tasks, i.e., an increasing number of fluorescent codes and markers is required. Secondly, low-cost diagnostic tests, e.g. in disease recognition, are needed in routine application. Lifetime encoding could be an attractive alternative to commonly applied color (spectral) encoding. By combining spectral and lifetime multiplexing, the number of simultaneously detectable codes might be increased by adding lifetime codes to the parameter space. Otherwise, instrumentation costs could be lowered using only lifetime encoding and thus avoiding costly excitation light sources and detectors. Here, we report on our recent progress in time-resolved flow cytometry using dye-stained lifetime-encoded polymer microparticles as a model system. We could show that the discrimination of two lifetime codes is feasible. Moreover, the simultaneous detection of a spectrally different ligand fluorescence signal excited at the same wavelength as the lifetime code fluorescence could be demonstrated. T2 - Photonik in den Lebenswissenschaften CY - Berlin, Germany DA - 09.11.2016 KW - Flow cytometry KW - Fluorescence KW - Life sciences KW - Lifetime encoding KW - Polymer particles PY - 2016 AN - OPUS4-38249 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Inspection and monitoring of massive concrete structures by innovative ultrasonic methods N2 - Presentation on recent progress in ultrasinic testing and monitoring of concrete for massive structures. First, a new instrument (LAUS) for ultrasonic echo testing of thicknesses up to 5 m is shown. A new method to provide better images of the concrete interior, Reverse Mitem Migration (RTM)is presented. Second, the use of embedded ultrasonic transducers and data processing methods borrowed from seismology to detect subtle changes in concrete are documented. T2 - NUCCON 2016 CY - Helsinki, Finland DA - 31.10.2016 KW - Ultrasound KW - Concrete KW - Imaging KW - Monitoring KW - Nuclear PY - 2016 AN - OPUS4-38181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramirez Caro, Alejandra A1 - Pauli, Jutta T1 - Study of the superplasticizer-cement hydration interaction by optical spectroscopy N2 - Chemical admixtures like superplasticizers or stabilizing agents are of ever increasing importance for modern concrete technology. Although such admixtures have meanwhile become common practice in many applications of concrete technology, the understanding of these highly complex systems is still limited and the relevant parameters, which predominantly control the interaction between the superplasticizer and the cement components, have not been identified yet. Optical methods have been successfully used for the analysis and monitoring of the interactions between a broad variety of nanoscale and molecular systems like nanoparticles of various chemical composition and different types of organic ligands or biomolecules. This encouraged to assess the potential of these methods for the investigation of the interactions that occur at the interface between particle or hydrate surfaces and the fluid phase at a very early stage of concrete formation and to differentiate between different superplasticizer. T2 - 2. ICCCM CY - Munich, Germany DA - 10.10.2016 KW - Optical spectroscopy KW - Cement hydration PY - 2016 AN - OPUS4-38474 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wang, X. T1 - Gold nanoparticle-catalyzed uranine reduction N2 - Gold nanoparticles (AuNPs) can catalyze the decolorization of organic dyes in the presence of sodium borohydride (NaBH4), which can be utilized for sensitive optical signaling. Here, we monitor the catalytic reduction of a fluorescent substrate, exemplarily chosen uranine, by AuNPs serving as nanocatalysts by absorption and fluorescence spectroscopy. Dye reduction is accompanied by dramatic changes in the absorption and fluorescence properties of uranine. As proposed reaction mechanism, we assume electron transfer between uranine and NaBH4 through the AuNPs nanocatalysts which is currently investigated also by time-resolved fluorescence and detailed spectroscopic studies of the influence of pH, NaBH4, and AuNPs on these effects. As ultimate goal, a model reporter platform with colorimetric andfluorometric signaling is anticipated for the detection of different analytes by coating AuNPs with affinity ligands such as antibodies and aptamers and and special separation methods. T2 - Anakon 2015 CY - Graz, Austria DA - 23.03.2015 KW - Fluorescence lifetime KW - Uranine KW - Nanoparticle KW - Surfactant PY - 2015 AN - OPUS4-38957 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Galindo Guerreros, Julio Cesar A1 - Niederleithinger, Ernst A1 - Mackens, S. A1 - Fechner, Th. T1 - Crosshole and downhole seismics: a new quality assurance tool for jet grout columns N2 - Sealing and strengthening of the subsoil by grout injection is a major issue in the field of geotechnical engineering. One commonly applied method is jet grouting, which allows creating columns of grouted soil by eroding and mixing the in-situ soil with a thin cement suspension. A general difficulty linked with this method is in predicting the resulting column diameter and its material strength. In this paper, we illustrate the application of a newly developed non-destructive quality assurance tool used to determine the diameter of jet grout columns. This approach incorporates standard crosshole and downhole seismic measurements. To demonstrate its effectiveness, we tested the new approach within two-dimensional finite-difference numerical simulations. Additional field tests showed that this tool is also applicable in real site conditions. For this purpose, three jet grout columns were produced with different process parameters in a depth between 3 and 10 m. The evaluated diameters were within 1 and 1.5 m, slightly deviating from the previously predicted range by the jet grouting contractor. Moreover, we were able to detect the base of the columns at a 10-m depth with no significant difficulties. On the other hand, unsaturated, less compacted sands between the groundwater level and surface considerably affected the seismic data, hence complicating the detection of the top of the columns. KW - Jet grouting KW - Quality assurance PY - 2016 DO - https://doi.org/10.3997/1873-0604.2016042 SN - 1569-4445 IS - 14 SP - 493 EP - 501 PB - EAGE CY - Houton, NL AN - OPUS4-38977 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramirez Caro, Alejandra A1 - Pauli, Jutta A1 - Schmidt, Wolfram A1 - Resch-Genger, Ute T1 - Study of the superplasticizer-cement hydration interaction by optical spectroscopy N2 - Nowadays, superplasticizers (SPs) are widely used to increase fluidity and reduce water content in concrete; thus, allowing better workability for final applications. The present study will focus on the hydration effect using comb shape polycarboxylates (PCEs), which are known to allow a very low water/cement ratio (w/c of 0.20) or less.Optical methods have been successfully used for the analysis and monitoring of the interactions between a broad variety of nanoscale and molecular systems like nanoparticles of various chemical composition and different types of organic ligands or biomolecules.This encouraged us to assess the potential of these methods, and particularly fluorescence, for the investigation of the interactions that occur at the interface between hydrate surfaces of cement particles and PCE at a very early stage of concrete formation and to differentiate between the impact of PCE’s molecular structures on such interactions. T2 - 2nd International Conference on the Chemistry of Construction Materials CY - Munich, Germany DA - 10.10.2016 KW - Cement KW - Dye KW - Superplasticizers KW - Fluorescence PY - 2016 SN - 978-3-936028-96-6 VL - 50 SP - 260 EP - 263 PB - Gesellschaft Deutscher Chemiker e.V. CY - Frankfurth am Main AN - OPUS4-38881 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, Katrin T1 - Reference Materials for Standardization of Fluorescence-based Measurements N2 - Here, we summerize our efforts concerning new design concepts and examples for fluorescence standards that can provide traceability to radiometric units and present a first step towards a toolbox of fluorescence standards, currently consisting of: i) A first set of liquid fluorescence standards enables the determination of a broad variety of fluorescence parameters was developed and certified by BAM and is distributed by Sigma-Aldrich. ii) Ready-to-use, glass-based fluorescence standards for instrument performance validation (IPV) and determination instrument-to-instrument variations can also be used as wavelength standard for fluorescence instruments with low requirements on spectral resolution and allow monitoring of temporal changes of the wavelength-dependent spectral responsivity. iii) Novel calibration tools and validation concepts for microarray-based platforms used in molecular diagnostics and food safety control. iv) We currently develop reference materials, which can be used as reliable quantum yield standards for relative methods for the determination of QY and can be valuable in the evaluation of the performance and sources of uncertainty of absolute, standard-free methods using e.g. integrating spheres. T2 - 14th Conference on Methods and Applications in Fluorescence CY - Würzburg, Germany DA - 13.09.2015 KW - Fluorescence KW - Standards KW - Quantum yield KW - Microarray PY - 2015 AN - OPUS4-38882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Progress in non-destructive testing and monitoring of concrete N2 - The presentation will give an overview on non-destructive testing techniques being developed at the Federal Institute for Materials Research and Testing, Germany (BAM). This includes ultrasonic methods, ground penetration radar, Laser-Induced Breakdown Spectroscopy (LIBS), infrared thermography, pile testing, sensor technology and building scanner. A focus of the talk will be ultrasonic methods, which are well established in various aspects of concrete testing. They are used for imaging the interior geometry of constructions, estimation of concrete strength or monitoring lab investigations. However, so far the detection of distributed damages, especially in an early stage, has been almost impossible. The arrival of new technologies as embedded transducers and sensitive data processing techniques adopted from seismology has opened new field of work. Recent research has been focused to detect changes in concrete elements induced by stress, temperature, moisture or chemical attacks by permanent monitoring. Techniques as Coda Wave Interferometry can resolve changes in ultrasonic velocity in the order of 1*10-5. In addition, many researchers believe that the investigation of nonlinear effects can be used to characterize damages. The presentation will give a wrap up of ultrasonic techniques currently used in practice. This will include echo based methods as multi-channel/multi-offset imaging of structural elements using commercial and prototype devices. Imaging methods as SAFT and RTM will be shortly discussed. The focus will be on the emerging techniques used for monitoring. New types of sensors will be presented as well as the devices used in laboratory and field applications. Insight will be given on the various influence factors on ultrasonic signals and various ways of feature extraction and data processing. The results of lab experiments will be shown to demonstrate the detection of various kind of damages from mechanical load, ASR, corrosion to fatigue. The experiences with our first installations in real constructions (bridges, tunnel) will also be presented. T2 - CIES Research Seminar, University of New South Wales CY - Sydney, Australia DA - 13.12.2016 KW - Ultrasound KW - Concrete KW - Monitoring KW - Imaging PY - 2016 AN - OPUS4-38731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - State-of-the-art of ultrasonic monitoring of concrete N2 - Ultrasonic methods are well established in various aspects of concrete testing. They are used for imaging the interior geometry of constructions, estimation of concrete strength or monitoring lab investigations. However, so far the detection of distributed damages, especially in an early stage, has been almost impossible. The arrival of new technologies as embedded transducers and sensitive data processing techniques adopted from seismology has opened new field of work. Recent research has been focused to detect changes in concrete elements induced by stress, temperature, moisture or chemical attacks by permanent monitoring. Techniques as Coda Wave Interferometry can resolve changes in ultrasonic velocity in the order of 1*10-5. In addition, many researchers believe that the investigation of nonlinear effects can be used to characterize damages. The workshop will give a wrap up of ultrasonic techniques currently used in practice. This will include echo based methods as multi-channel/multi-offset imaging of structural elements using commercial and prototype devices. Imaging methods as SAFT and RTM will be shortly discussed. The focus will be on the emerging techniques used for monitoring. New types of sensors will be presented as well as the devices used in laboratory and field applications. Insight will be given on the various influence factors on ultrasonic signals and various ways of feature extraction and data processing. The results of lab experiments will be shown to demonstrate the detection of various kind of damages from mechanical load, ASR, corrosion to fatigue. The experiences with or first installations in real constructions (bridges, tunnel) will also be presented. T2 - The 8th Australian Network of Structural Monitoring Annual Workshop CY - Melbourne, Australia DA - 29.11.2016 KW - Ultrasound KW - Concrete KW - Monitoring KW - Imaging PY - 2016 AN - OPUS4-38727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fidan, Z. A1 - Wende, A. A1 - Resch-Genger, Ute T1 - Visible and red emissive molecular beacons for optical temperature measurements and quality control in diagnostic assays utilizing temperature-dependent amplification reactions N2 - Quality control requirements imposed on assays used in clinical diagnostics and point-of-care-diagnostic testing (POCT), utilizing amplification reactions performed at elevated temperatures of 35 to 95 °C are very stringent. As the temperature of a reaction vessel has a large impact on the specificity and sensitivity of the amplification reaction, simple tools for local in situ temperature sensing and monitoring are required for reaction and assay control. We describe here a platform of stem-and-loop structured DNA hairpins (molecular beacons, MBs), absorbing and emitting in the visible and red spectral region, rationally designed for precise temperature measurements in microfluidic assays for POCT, and their ap-plication for temperature measurements in a common DNA-based molecular biological assay utilizing thermophilic helicase-dependent amplification (tHDA). Spectroscopic studies of these MBs, rationally designed from DNA se-quences of different thermal stabilities, chosen not to interact with the DNA probes applied in the nucleic acid amplification assay, and temperature-dependent fluorescence measurements of MB-assay mixtures revealed the suitability of these MBs for temperature measurements directly in such an assay with a temperature resolution of about 0.5 °C without interferences from assay components. Combining two spectrally distinguishable MBs provides a broader response range and an increase in temperature sensitivity up to 0.1 °C. This approach will find future application for temperature monitoring and quality control in commercialized diagnostics assays using dried reagents and microfluidic chips as well as assays read out with tube and microplate readers and PCR detection systems for temperature measurements in the range of 35 to 95 °C. KW - Miniaturization KW - Fluorescence KW - Temperature KW - Sensor KW - Assay KW - Microfluidics KW - DNA KW - Dye KW - Molecular beacon KW - Molecular diagnostics PY - 2016 DO - https://doi.org/10.1007/s00216-016-0088-6 SN - 1618-2642 VL - 409 IS - 6 SP - 1519 EP - 1529 PB - Springer CY - Heidelberg AN - OPUS4-39589 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niederleithinger, Ernst A1 - Abraham, O. A1 - Mooney, M. T1 - Special Issue on Geophysics for Non-destructive Testing in Civil Engineering Foreword N2 - Foreword to a special issue of "Near Surface Geophysics" on the application of geophysical techniques to non-destructive testing in civil engineering KW - geophysics non-destructive testing PY - 2016 DO - https://doi.org/10.3997/1873-0604.2016043 SN - 1569-4445 VL - 14 IS - 6 SP - 479 EP - 480 PB - EAGE CY - Houton, NL AN - OPUS4-38984 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Recent insights in the spectroscopic properties of upconversion nanoparticles N2 - Lanthanide-doped up-converting nanoparticles (UCNPs) are promising reporters for medical diagnostics and bioimaging, which are excited in the near infrared (NIR) by multiphoton absorption processes, and show multiple narrow emission bands in the visible (vis) and NIR, long luminescence lifetimes in the μs range, and excellent photostability. Current limitations present their relative low absorption cross sections and low fluorescence efficiencies, with the latter being affected by particle size, surface chemistry, and microenvironment, particularly water. Here, we present results from systematic studies of the excitation power density dependent upconversion luminescence spectra, intensities/intensity ratios of the individual emission bands, slope factors, and quantum yields of UCNPs of varying size, dopant concentration, and surface chemistry in different microenvironments as well as the up- and downconversion luminescence decay kinetics of the different emission bands. Moreover, first studies of the energy transfer from UCNPs to surface-bound organic dyes acting as fluorescence acceptors are shown. Based upon these measurements, fluorescence deactivation channels are identified and spectroscopic parameters for the screening of material performance are derived. T2 - Spie Photonics west 2017 CY - San Francisco, USA DA - 28.01.2017 KW - Upconverting nanoparticles KW - Size KW - FRET KW - Fluorescence KW - Absolute fluorescence quantum yield KW - Fluorescence decay kinetics KW - Power density dependence PY - 2017 AN - OPUS4-39075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cruz Alonso, M. T1 - Bioimaging of metallothioneins in ocular tissue sections by LA-ICP-MS using bioconjugated gold nanoclusters N2 - Oxidative stress is produced by an imbalance between free radical production and biological system's ability to detoxify the reactive intermediates and repair the resulting damage. In the human eye the main causes of oxidative stress are the daily exposure to sunlight, chemical insults and the special microenvironment with abundant photo-sensitizers. For this reason, oxidative stress has been associated several ocular diseases, like aged-related macular degeneration (AMD). On the other hand, Metallothioneins (MTs) are a family of low molecular weight (6–7 kDa), cysteine-rich (30%) and metal-binding proteins. The cysteine residues can bind metal atoms such as zinc, copper, and cadmium via thiolate bonds. These proteins have a wide range of functions including defense against oxidative damage, intracellular storage and transport and metabolism of metal ions. The antioxidant properties of MTs reside in their capacity to capture and neutralize free radicals by binding and transferring zinc ions in a redox-dependent fashion, forming the antioxidant system Zinc-Metalothionein (Zn-MT). Highly sensitive analytical tools are required to study the relationship between Zn and MTs in sections from ocular tissues. These methodologies should permit the simultaneous localization (bioimaging) of metals and proteins. Laser ablation (LA) coupled to ICP-MS has shown a huge potential for bioimaging studies in biological tissues. In addition, the use of metal nanoclusters (NCs) as elemental tags will provide signal amplification, compared with other tags traditionally employed (e.g. polymeric tags). To this end, antibodies with gold nanoclusters (AuNCs) will be used in combination with LA-ICP-MS for the detection of different metallothioneins (MT 1/2 and 3) directly into the ocular tissue sections. - Methods: The AuNCs synthesized were bioconjugated with an Anti-MT 1/2 antibody and with Anti-MT 3 antibody. Next, using ocular tissue sections (5 microns thick) from different donors the immunoassays were performed. After the immunoassay protocol, imaging studies were carried out by LA-ICP-MS as well as by fluorescence (confocal microscope) in order to compare both methodologies. - Results: The MTs (measuring the Au signal) and the coordinated metals distribution (Zn and Cu) were successfully carried out in human ocular tissues, including sclera, choroid, retina and retinal pigment epithelium regions. The image patterns found in ocular tissues were in agreement with those reported by conventional immunohistochemistry. - Conclusions: It is possible to know the distribution of MT proteins and different coordinated metals using bioconjugated AuNCs and LA-ICP-MS. Proposed analytical tools could help to better understand the roles of the antioxidant system Zinc-Metalothionein in the eye. T2 - European Winter Conference on Plasma Spectrochemistry EWCPS-2017 CY - St. Anton, Austria DA - 19.02.2017 KW - Bioimaging KW - LA-ICP-MS KW - Nanocluster PY - 2017 AN - OPUS4-39293 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Ralf T1 - Investigation and control of protein adsorption for fluorescent nanosilver reference material N2 - Upon interaction of nanomaterials like noble metal nanoparticles (NPs) with biological systems like body fluids such as serum, a protein corona is formed.[1] This reversibly bound layer of proteins controls the transport of the NPs and their subsequent interaction with biological components.[2] The plasmonic properties of nobel metal NPs like Au and Ag can considerably affect the fluorescence properties of fluorophores in their vicinity, i.e., within a near field distance. Depending on the chemical composition, size and shape of these noble metal NPs, the spectral properties of the dye, and the particle-fluorophore distance, the fluorescence is quenched or in some cases enhanced.[3,4,5] This can be monitored by fluorescence intensity and lifetime measurements, with the latter effect being accompanied by an increase in fluorescence intensity and reduction in fluorescence lifetime due to an increase in radaiative rate constant. We utilized these effects to study and manipulate noble metal NP-protein interaction exemplarily for fluorophore-labeled bovine serum albumin (BSA) modified e.g. by succinylation, amination and the introduction of thiol groups, resulting in different binding affinities of the proteins.[6] Our results show that the fluorescent corona allows monitoring of the interaction of our accordingly protein-functionalized particles with biological model systems like solutions containing different amounts of various proteins. This can be eventually used for further in vitro and in vivo studies to assess the uptake, digestion, and excretion of surface functionalized noble metal NPs. T2 - EBS 2017 CY - Potsdam, Germany DA - 20.03.2017 KW - Nanoparticles KW - Reference material KW - Fluorescence probes KW - Plasmonics PY - 2017 AN - OPUS4-39552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weigert, Florian T1 - Recent Advancements of Novel core-shell CdSe Nanocrystals and their Characterization with Single Particle Spectroscopy N2 - Here, we report on the recent advancements in the synthesis and optical properties of novel core-shell CdSe semiconductor nanocrystals (SCNC) with either a thick monolithic shell of CdS or thin multi-shells of succeeding CdS and ZnS monolayers, characterized by steady state and time-resolved fluorescence spectroscopy at the ensemble level. SCNC samples, chosen upon the size of their photoluminescence quantum yield (PL QY), were subsequently investigated at the single particle level using a custom build confocal laser scanning microscope to obtain information on brightness, blinking behavior, and decay kinetics of single SCNCs and correlate these properties with their surface morphology. The results of this study can help to identify new synthetic routes and surface modifications to colloidally and photochemically stable SCNCs with a PL QY of close to unity. T2 - Quantum Dot Workshop, Technical University of Dresden CY - Dresden, Germany DA - 06.02.2017 KW - Quantum Dots KW - Colloidal KW - Single Particle KW - Specctroscopy KW - Quantum Yield KW - Bioapplication KW - CdSe PY - 2017 AN - OPUS4-39205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - König, Markus A1 - Grohmann, Maria A1 - Niederleithinger, Ernst T1 - Anwendung der Reverse-Time Migration auf Ultraschall-Echo-Daten zur Detektion von verdeckten Rissen in Betonkörpern N2 - Das Ultraschall-Echo-Verfahren ist eine wichtige Methode der zerstörungsfreien Prüfung (ZfP). Prüfaufgaben im Bauwesen beinhalten unter anderem die korrekte Dickenbestimmung von Konstruktionen, sowie die Lokalisierung von Einbauteilen und Fehlstellen. Das Abbildungsverfahren RTM (Reverse Time Migration) liefert oft bessere Bilder als konventionelle Verfahren. Die Datenaufnahme am Betonprobekörper erfolgte mit einem Scannersystem der BAM, bei dem jeweils ein Ultraschall-Prüfkopf als Sender bzw. Empfänger diente. Es wurden senkrecht zur Profilrichtung horizontal polarisierte Scherwellen genutzt. Die RTM wurde mit dem Softwarepaket Madagascar gerechnet. Die Ergebnis zeigt das Potential dieser Methode im Bezug auf komplexe Strukturen. Die lateralen Positionen der Risse im RTM-Bild sowie deren Höhe innerhalb des Probekörpers, entsprechen recht genau dem visuellen Befund. T2 - 77. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Potsdam, Germany DA - 27.03.2017 KW - Ultraschall KW - Beton KW - Riss KW - Reverse Time Migration PY - 2017 AN - OPUS4-39662 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radunz, Sebastian T1 - Simple approach to pKa tunable BOIDPY-based fluorescent pH sensors N2 - Successfull synthesis of pH-responsive fluorescence ON/OFF sensor dyes with tunable pK values covering the pH range of 5 to 12 Immobilizing of multiple dyes with different pK values into a polymer host matrix provides a pH sensor with a dynamic range. T2 - First European/ 10th German BioSensor Symposium CY - Potsdam, Germany DA - 20.03.2017 KW - Fluorescence KW - Sensing KW - pH PY - 2017 AN - OPUS4-39683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, L. A1 - Traub, Heike A1 - Jakubowski, Norbert T1 - Novel applications of lanthanoides as analytical or diagnostic tools in the life sciences by ICP-MS-based techniques N2 - Inductively coupled plasma mass spectrometry (ICP-MS) is a well-established analytical method for multi-elemental analysis in particular for elements at trace and ultra-trace levels. It has found acceptance in various application areas during the last decade. ICP-MS is also more and more applied for detection in the life sciences. For these applications, ICP-MS excels by a high sensitivity, which is independent of the molecular structure of the analyte, a wide linear dynamic range and by excellent multi-element capabilities. Furthermore, methods based on ICP-MS offer simple quantification concepts, for which usually (liquid) standards are applied, low matrix effects compared to other conventional bioanalytical techniques, and relative limits of detection (LODs) in the low pg g−1 range and absolute LODs down to the attomol range. In this chapter, we focus on new applications where the multi-element capability of ICP-MS is used for detection of lanthanoides or rare earth elements, which are applied as elemental stains or tags of biomolecules and in particular of antibodies. KW - ICP-MS KW - Life sciences KW - Mass cytometry KW - Laser ablation (LA)-ICP-MS KW - Bioimaging PY - 2016 DO - https://doi.org/10.1515/psr-2016-0064 SN - 2365-659X SN - 2365-6581 VL - 1 IS - 11 SP - 1 EP - 19 AN - OPUS4-40234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Muhr, V. A1 - Würth, Christian A1 - Kraft, Marco A1 - Buchner, M. A1 - Baeumner, A. J. A1 - Resch-Genger, Ute A1 - Hirsch, T. T1 - Particle-size-dependent Förster resonance energy transfer from upconversion nanoparticles to organic dyes N2 - Upconversion nanoparticles (UCNPs) are attractive candidates for energy transfer-based analytical applications. In contrast to classical donor−acceptor pairs, these particles contain many emitting lanthanide ions together with numerous acceptor dye molecules at different distances to each other, strongly depending on the particle diameter. UCNPs with precisely controlled sizes between 10 and 43 nm were prepared and functionalized with rose bengal and sulforhodamine B by a ligand-exchange procedure. Timeresolved studies of the upconversion luminescence of the UCNP donor revealed a considerable shortening of the donor lifetime as a clear hint for Förster resonance energy transfer (FRET). FRET was most pronounced for 21 nm-sized UCNPs, yielding a FRET efficiency of 60%. At larger surface-to-volume ratios, the FRET efficiency decreased by an increasing competition of nonradiative surface deactivation. Such dye-UCNP architectures can also provide an elegant way to shift the UCNP emission color, since the fluorescence intensity of the organic dyes excited by FRET was comparable to that of the upconversion emission of smaller particles. KW - Upconversion KW - FRET KW - Organic dyes PY - 2017 DO - https://doi.org/10.1021/acs.analchem.6b04662 SN - 0003-2700 SN - 1520-6882 VL - 89 IS - 9 SP - 4868 EP - 4874 PB - ACS AN - OPUS4-40092 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya T1 - New Approaches for the Quantification of Functional Groups on Micro- and Nanoparticle Surfaces N2 - Nanometer- and micrometer-sized particles are increasingly used as tolls in (bio)analytics with typical applications being carriers for e.g., drugs or dye molecules for use as multichromophoric reporters for signal amplification in optical assays, platforms for DNA sequencing as well as nanosensors and targeted probes for bioimaging studies. The application of such particles in the material and life sciences is closely linked to their size (and size distribution), shape, colloidal stability, biocompatibility, and ease of subsequent functionalization, e.g., with linkers, targeting ligands, and sensor molecules. The latter requires knowledge of the number of groups effectively accessible for subsequent coupling reactions and hence, selective and sensitive methods of analysis. Ideally, these methods are be robust, reliable, fast, performable with inexpensive equipment, and can be employed for the characterization of a broad variety of particle systems independent of their optical properties, i.e., scattering or the presence of encoding dyes. In this respect, we studied a variety of conventional and newly developed labels for optical readout on self-made particles with varying surface group density, utilizing e.g., changes in intensity and/or color of absorption and/or emission. We focus here on the development of a platform of cleavable and multimodal labels for optical assays which consist of a cleavable linker and an optically active reporter moiety. In contrast to conventional reporters measured directly at the particle surface, which are prone to signal distortions by scattering and encoding dyes, these cleavable labels can be detected colorimetrically or fluorometrically both bound at the particle surface and after quantitative cleavage of the linker in the transparent supernatant. Moreover, for heteroatom-containing reporters, they enable straightforward validation by method comparison with elemental analysis, ICP-OES or ICP-MS. Here, we present representative examples of our newly synthesized cleavable and multimodal labels and their application as reporters for the quantification of amino, thiol and carboxy surface groups on different nanomaterials and compare these results with measurements using conventional optical labels and results from measurements providing the total number of surface groups. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Optical quantification KW - Nanoparticle KW - Surface functional groups PY - 2017 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-39787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kage, Daniel T1 - Stained microparticles for lifetime encoding - Flow cytometry application & photophysics N2 - Multiparametric analyses involving optical techniques like flow cytometry are at the core of studying complex systems in biological research and diagnostic applications. However, for fluorescence-based techniques, the number of reporters distinguishable in spectral multiplexing is limited by spectral overlap and requires a multitude of excitation light sources and detection Systems. Intensity encoding often used for bead assays suffers from problems regarding dye concentration control and excitation light intensity fluctuations. An alternative is luminescence lifetime encoding, particularly to minimize instrument costs. Here, we report on dye-stained polymer microparticles for lifetime encoding in flow cytometry with different organic dyes. This ranges from studies of the impact of parameters like dye loading concentration and particle diameter on fluorescence decay behavior to the demonstration of lifetime code reading and simultaneous ligand fluorescence signal detection with single-wavelength excitation in a flow. T2 - DPG Spring Meeting 2017 CY - Dresden, Germany DA - 19.03.2017 KW - Flow cytometry KW - Fluorescence KW - Life sciences KW - Lifetime encoding KW - Polymer particles PY - 2017 AN - OPUS4-40056 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kage, Daniel T1 - Time domain flow cytometry utilizing lifetime-encoded polymer microparticles N2 - Flow cytometry is a widely used method in biological research and medical diagnostics. Depending on the respective application, two opposing directions of development are currently of interest. On the one hand, there is a need for analyses of growing complexity employing more and more fluorescent labels and codes. On the other hand, cost-effective methods and portable, miniaturized, and robust instruments are desired. Commonly performed spectral multiplexing utilizing a color code suffers from several problems, such as the sensitivity of fluorescence intensity measurements to fluctuations in excitation light intensity and dye concentration and hence, photobleaching, dye leaking for certain encoding procedures, and spectral crosstalk, limiting the achievable number of detection channels. Moreover, it typically requires several costly excitation light sources. An innovative alternative can be lifetime multiplexing and the discrimination between different encoding fluorophores and carrier beads based on their fluorescence decay kinetics. In order to examine the potential of this approach, dye encoded beads (lifetime encoded surface chemistry) were prepared using several fluorophores from different dye classes and their suitability for lifetime discrimination in a flow was tested in conjunction with a custom designed flow cytometer equipped with a pulsed light source and a fast detector. In a first step, the spectroscopic properties of micrometer-sized dye-stained PMMA beads were studied by means of steady state and time-resolved photoluminescence measurements. For the performance of studies on the practical use of these microbeads in flow cytometry applications, a custom-built demonstrator model for a flow system was employed. Our results demonstrated that lifetime discrimination and simultaneous readout of a ligand fluorescence signal for analyte quantification with a set of dye-stained polymer microbeads at single wavelength excitation is feasible. These studies are expected to pave the road for new applications of fluorescence lifetime multiplexing within the framework of time-domain flow cytometry and bead-based assays. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Flow cytometry KW - Fluorescence KW - Life sciences KW - Lifetime encoding KW - Polymer particles PY - 2017 AN - OPUS4-39995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kraft, Marco T1 - Particle size dependent optical properties of hexagonal β-NaYF4: 2 % Er3+, 20 % Yb3+ upconversion nanoparticles in cyclohexane and water N2 - Hexagonal NaYF4 doped with 20 % Yb3+ and 2 % Er3+ is an efficient upconversion (UC) phosphor for the conversion of 976 nm excitation light to emission at 845 nm, 800 nm, 655 nm, 540 nm and 410 nm light. The emission behavior of nanoparticles made from this material is strongly influenced by particle size, surface chemistry, and microenvironment. Furthermore their UC emission originates from multiphotonic absorption processes, rendering the resulting luminescence spectra and intensities excitation power density (P) dependent. Therefore the rational design of efficient nm-sized UC particles e.g., for applications in the material and life sciences requires reliable spectroscopic tools for the characterization of the optical properties of these materials like the excitation power density (P)-dependent UC quantum yield (QYUC) in dispersion, which presents a measure for the efficiency of the conversion of absorbed into emitted photons. Up to date the P-dependent absolute measurement of QYUC in aqueous media with an excitation wavelength of 976 nm presents a considerable challenge due to the low absorption coefficients of the UC materials and the absorption of water at this wavelength. T2 - International Conference on Advanced Materials and Nanotechnology CY - Queenstown, New Zealand DA - 12.02.2017 KW - Upconversion KW - Quantum yield KW - Lifetime KW - Water KW - Cyclohexane PY - 2017 AN - OPUS4-40093 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Maria A1 - Güttler, Arne A1 - Pauli, Jutta A1 - Vogel, K. A1 - Homann, Christian A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - Extending certified spectral fluorescence standards for the calibration and performance validation of fluorescence instruments to the NIR—closing the gap from 750 to 940 nm with two novel NIR dyes N2 - Fluorescence techniques such as fluorescence spectroscopy, microfluorometry, and fluorescence microscopy, providing spectral, intensity, polarization, and lifetime information, are amongst the most broadly utilized analytical methods in the life and materials sciences. However, the measured fluorescence data contain sample- and instrument-specific contributions, which hamper their comparability across instruments and laboratories. Comparable, instrument-independent fluorescence data require the determination of the fluorescence instrument’s wavelength-dependent spectral responsivity, also termed emission correction curve, for the same instrument settings as those used for the fluorescence measurements as a prerequisite for the subsequent correction of the measured instrument-specific data. Such a spectral correction is essential for the performance comparison of different fluorescent labels and reporters, quantitative fluorescence measurements, the determination of the fluorescence quantum yield, and the spectroscopic measure for the fluorescence efficiency of a fluorophore. Simple-to-use tools for obtaining emission correction curves are chromophore-based reference materials (RMs), referred to as fluorescence standards, with precisely known, preferably certified instrument-independent fluorescence spectra. However, for the increasingly used near-infrared (NIR) wavelength region >700 nm, at present, no spectral fluorescence standards are available. To close this gap, we developed two novel spectral fluorescence standards, BAM F007 and BAM-F009, with broad emission bands from about 580 to 940 nm in ethanolic solution. These liquid fluorescence standards currently under certification, which will be released in 2025, will expand the wavelength range of the already available certified Calibration Kit BAM F001b-F005b from about 300–730 to 940 nm. In this research article, we will detail the criteria utilized for dye and matrix selection and the homogeneity and stability tests accompanying dye certification as well as the calculation of the wavelength-dependent uncertainty budgets of the emission spectra BAM F007 and BAM-F009, determined with the traceably calibrated BAM reference spectrofluorometer. These fluorescence standards can provide the basis for comparable fluorescence measurements in the ultraviolet, visible, and NIR for the fluorescence community. KW - Quality assurance KW - Reference material KW - Fluorescence KW - Dye KW - Traceability KW - Metrology KW - Calibration KW - Reference data KW - Reference product KW - Digital certificate KW - NIR KW - Instrument performance validation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626317 DO - https://doi.org/10.1007/s00216-024-05723-w SN - 1618-2650 SP - 1 EP - 15 PB - Springer AN - OPUS4-62631 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ertel, Jens-Peter A1 - Niederleithinger, Ernst A1 - Grohmann, Maria T1 - Advances in pile integrity testing N2 - For decades, the low-strain impact integrity testing using a hammer blow is well established as a method of quality assurance for various pile types. However, this method has its limitations. Our research and development focuses on improving the excitation signal using a shaker system in contrast to the standard hammer method. Another approach is to increase the amount of sensors used during testing. The purpose is to identify the direction of wave propagation which gives advantages under difficult conditions, such as piles below structures. Pile integrity testing (PIT) using a shaker system was performed on two 11 m long piles of 90 cm in diameter. While one pile was intact, the other one showed a flaw at approx. 3.5 m below pile top, which was confirmed by standard PIT in 2012. A logarithmic sweep between 500 Hz and 1 KHz of 0.1 s was used as the input signal, being vertically injected into the pile. Prior to that, simulations on similar pile geometries showed that the depth of the pile toe as well as flaws within the pile can be extracted by applying regularized deconvolution. The result is the impulse response in the time domain. The application of deconvolution on the measured signals shows that it is possible to identify the pile length but it is more difficult to clearly extract the flaw’s position in the pile. Additional digital signal processing techniques and the improvement of the regularized deconvolution method as well as the experimental setup need to be investigated. Another way to improve the PIT method is to use a multichannel sensor arrangement. By arranging several accelerometers vertically along the accessible part of the pile shaft, it is possible to distinguish between downward and upward traveling waves. Furthermore, it is possible to estimate the unknown wave speed, which gives the possibility of more accurate pile length calculations. The method was evaluated successfully during a measurement campaign of a slab foundation with subjacent piles. In 20 of 28 cases the pile length could be detected accurately. KW - Pile integrity testing KW - Pile length KW - CEFIT KW - Deconvolution KW - Simulation PY - 2016 UR - http://nsg.eage.org/publication/publicationdetails/?publication=86879 SN - 1569-4445 SN - 1873-0604 VL - 14 IS - 6 SP - 503 EP - 512 PB - EAGE Publications AN - OPUS4-37837 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Influence of Surface Chemistry and Size on the Stability of β-NaYF4:Yb,Er Nanocrystals in Various Environments N2 - The use of inorganic lanthanide-doped upconversion nanoparticles (UCNP) in bioimaging and cellular studies requires biocompatible particles. One possible cause of UCNP toxicity is the release of potentially harmful fluoride and lanthanide ions as revealed by dilution studies in aqueous environments, particularly under high dilution conditions. To address this issue, suitable surface coatings preventing such effects in combination with fast screening methods suited for online monitoring and in situ analyses are desired. Here we present systematic studies of differently sized β-NaYF4:Yb,Er UCNP stabilized with different surface coatings and hydrophilic ligands varying in binding strength to the particle surface in various aqueous environments at different temperatures and UCNP concentrations. The concentration of the fluoride and lanthanide ions released upon particle dissolution was quantified electrochemically with a fluoride ion-sensitive electrode and inductively coupled plasma optical emission spectrometry (ICP-OES) and monitored fluorometrically, thereby exploiting the sensitivity of the upconversion luminescence to changes in size and surface chemistry. Moreover, changes in surface chemistry were determined with X-Ray photoelectron spectroscopy (XPS). Based upon our results, we could derive optimum screening parameters for UCNP stability studies and determine conditions and coating procedures and ligands for enhancing UCNP stability in aqueous environments. T2 - UPCON2021 CY - Online meeting DA - 06.04.2021 KW - Fluorescence KW - Lifetime KW - Method KW - Quantification KW - Stability KW - Coating KW - Surface chemistry KW - Lanthanide KW - Fluoride KW - Electrochemistry KW - ICP-OES KW - Upconversion KW - Nano KW - Particle KW - Aging KW - Quality assurance KW - Mass spectrometry KW - XPS PY - 2021 AN - OPUS4-52411 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Characterization of dye-protein conjugates with optical methods N2 - Fluorophore labeled proteins and antibodies, referred to also as targeted optical probes, present a promising strategy for a variety of applications from fundamental cell-based biological studies to in vivo diagnostics and image guided surgeries in humans. In this respect, design strategies for the preparation of such conjugates from different dyes including analyte-responsive fluorophores are presented as well as their analytical and spectroscopic characterization employing Absorption spectroscopy and steady state and time-resolved fluorometry. Special emphasis is dedicated to the influence of dye hydrophilicity and labeling density on the optical properties and binding behavior of these dye-bioconjugates including their performance in in vitro and in vivo bioimaging studies. T2 - International Workshop “Affinity - Mass spectrometry – New Methods and Application to Protein Therapeutics Development” CY - Rüsselsheim am Main, Germany DA - 14.11.2016 KW - Fluorescence KW - Dye bioconjugates KW - Protein KW - Immunoassay KW - Quality assurance KW - Optical characterization KW - Dye KW - NIR KW - Imaging PY - 2016 AN - OPUS4-38504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ertel, Jens-Peter T1 - Das PileInspect-Projekt: Pfahlintegritätsprüfung durch Schwinganregung mittels eines elektrodynamischen Shakers N2 - Pfahlintegritätsprüfung durch Schwinganregung und regularisierte Dekonvolution zur Messung der Impulsantwort eines Bohrpfahls. Dadurch ergeben sich Möglichkeiten zur Längenbestimmung und Schadensdiagnose T2 - Pfahlsymposium 2017 CY - Braunschweig, Germany DA - 23.02.2017 KW - Pfahlintegritätsprüfung KW - Tikhonov KW - Dekonvolution KW - PileInspect PY - 2017 AN - OPUS4-39263 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drescher, D. A1 - Büchner, T. A1 - Schrade, P. A1 - Traub, Heike A1 - Werner, S. A1 - Guttmann, P. A1 - Bachmann, S. A1 - Kneipp, J. T1 - Influence of Nuclear Localization Sequences on the Intracellular Fate of Gold Nanoparticles N2 - Directing nanoparticles to the nucleus by attachment of nuclear localization sequences (NLS) is an aim in many applications. Gold nanoparticles modified with two different NLS were studied while crossing barriers of intact cells, including uptake, endosomal escape, and nuclear translocation. By imaging of the nanoparticles and by characterization of their molecular interactions with surface-enhanced Raman scattering (SERS), it is shown that nuclear translocation strongly depends on the particular incubation conditions. After an 1 h of incubation followed by a 24 h chase time, 14 nm gold particles carrying an adenoviral NLS are localized in endosomes, in the cytoplasm, and in the nucleus of fibroblast cells. In contrast, the cells display no nanoparticles in the cytoplasm or nucleus when continuously incubated with the nanoparticles for 24 h. The ultrastructural and spectroscopic data indicate different processing of NLS-functionalized particles in endosomes compared to unmodified particles. NLS functionalized nanoparticles form larger intraendosomal aggregates than unmodified gold nanoparticles. SERS spectra of cells with NLS-functionalized gold nanoparticles contain bands assigned to DNA and were clearly different from those with unmodified gold nanoparticles. The different processing in the presence of an NLS is influenced by a continuous exposure of the cells to nanoparticles and an ongoing nanoparticle uptake. This is supported by mass-spectrometry-based quantification that indicates enhanced uptake of NLS-functionalized nanoparticles compared to unmodified particles under the same conditions. The results contribute to the optimization of nanoparticle analysis in cells in a variety of applications, e.g., in theranostics, biotechnology, and bioanalytics. KW - Nanoparticle KW - Laser ablation KW - SERS KW - ICP-MS PY - 2021 DO - https://doi.org/10.1021/acsnano.1c04925 SN - 1936-086X VL - 15 IS - 9 SP - 14838 EP - 14849 PB - American Chemical Society AN - OPUS4-54047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nirmalananthan-Budau, Nithiya A1 - Behnke, Thomas A1 - Hoffmann, Katrin A1 - Kage, Daniel A1 - Gers-Panther, Charlotte F. A1 - Frank, Walter A1 - Müller, Thomas J. J. A1 - Resch-Genger, Ute T1 - Crystallization and Aggregation-Induced Emission in a Series of Pyrrolidinylvinylquinoxaline Derivatives N2 - Aggregation-induced emission (AIE) has been meanwhile observed for many dye classes and particularly for fluorophores containing propeller-like groups. Herein, we report on the AIE characteristics of a series of four hydrophobic pyrrolidinylvinylquinoxaline (PVQ) derivatives with phenyl, pyrrolyl, indolyl, and methoxythienyl substituents used to systematically vary the torsion angle between this substituent at the quinoxaline C2 position and the planar PVQ moiety. These molecules, which are accessible via four- or five-component one-pot syntheses, were spectroscopically studied in organic solvents and solvent−water mixtures, as dye aggregates, solids, and entrapped in polystyrene particles (PSP). Steady-state and time-resolved fluorescence measurements revealed a strong fluorescence enhancement for all dyes in ethanol−water mixtures of high water content, accompanying the formation of dye aggregates with sizes of a few hundred nm, overcoming polarity and H-bonding-induced fluorescence quenching of the chargetransfer-type emission of these PVQ dyes. The size and shape of these dye aggregates and the size of the AIE effect are controlled by the water content and the substituent-dependent torsion angle that influences the nucleation process and the packing of the molecules during aggregation. Staining of 1 μm-sized carboxy-functionalized PSP with the PVQ dyes resulted also in a considerable increase in the fluorescence quantum yield and lifetime, reflecting the combined influence of the restricted molecular motion and the reduced polarity of the dye microenvironment. KW - Spectroscopy KW - AIE KW - Aggregates KW - Nanoparticle PY - 2018 DO - https://doi.org/10.1021/acs.jpcc.8b01425 SN - 1932-7447 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. VL - 122 IS - 20 SP - 11119 EP - 11127 PB - ACS Publications AN - OPUS4-45176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rietsch, P. A1 - Zeyat, M. A1 - Hübner, Oskar A1 - Hoffmann, Katrin A1 - Resch-Genger, Ute A1 - Kutter, M. A1 - Paskin, A. A1 - Uhlig, J. A1 - Lentz, D. A1 - Eigler, S. T1 - Substitution Pattern-Controlled Fluorescence Lifetimes of Fluoranthene Dyes N2 - The absorption and emission properties of organic dyes are generally tuned by altering the substitution pattern. However, tuning the fluorescence lifetimes over a range of several 10 ns while barely affecting the spectral features and maintaining a moderate fluorescence quantum yield is challenging. Such properties are required for lifetime multiplexing and barcoding applications. Here, we show how this can be achieved for the class of fluoranthene dyes, which have substitution-dependent lifetimes between 6 and 33 ns for single wavelength excitation and emission. We explore the substitution-dependent emissive properties in the crystalline solid state that would prevent applications. Furthermore, by analyzing dye mixtures and embedding the dyes in carboxyfunctionalized 8 μm-sized polystyrene particles, the unprecedented potential of these dyes as labels and encoding fluorophores for time-resolved fluorescence detection techniques is demonstrated. KW - Fluorescence KW - Label KW - Fluoranthene KW - Quantum yield KW - Reporter KW - Crystal KW - Encoding KW - Multiplexing KW - Particle KW - Bead KW - Lifetime KW - Dye KW - Barcoding PY - 2021 DO - https://doi.org/10.1021/acs.jpcb.0c08851 SN - 1520-5207 VL - 125 IS - 4 SP - 1207 EP - 1213 PB - American Chemical Society AN - OPUS4-52087 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schoder, S. A1 - Schröder, H. V. A1 - Cera, L. A1 - Puttreddy, R. A1 - Güttler, Arne A1 - Resch-Genger, Ute A1 - Rissanen, K. A1 - Schalley, C. A. T1 - Strong Emission Enhancement in pH-Responsive 2:2 Cucurbit[8]uril Complexes N2 - Organic fluorophores, particularly stimuli-responsive molecules, are very interesting for biological and material sciences applications, but frequently limited by aggregation- and rotation-caused photoluminescence quenching. A series of easily accessible bipyridinium fluorophores, whose emission is quenched by a twisted intramolecular charge-transfer (TICT) mechanism, is reported. Encapsulation in a cucurbit[7]uril host gave a 1:1 complex exhibiting a moderate emission increase due to destabilization of the TICT state inside the apolar cucurbituril cavity. A much stronger fluorescence enhancement is observed in 2:2 complexes with the larger cucurbit[8]uril, which is caused by additional conformational restriction of rotations around the aryl/aryl bonds. Because the cucurbituril complexes are pH switchable, this system represents an efficient supramolecular ON/OFF fluorescence switch. KW - Sensor KW - pH KW - Dye KW - Supramolecular chemistry KW - Synthesis KW - Host-guest interaction KW - Fluorescence KW - Enhancement KW - Curcubituril KW - Macrocyclus KW - Solid state PY - 2019 DO - https://doi.org/10.1002/chem.201806337 SN - 0947-6539 VL - 25 IS - 13 SP - 3257 EP - 3261 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-47599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Boehm, U. A1 - Nelson, G. A1 - Brown, C. M. A1 - Bagley, S. A1 - Bajcsy, P. A1 - Bischof, J. A1 - Dauphin, A. A1 - Dobbie, I. M. A1 - Eriksson, J. E. A1 - Faklaris, O. A1 - Fernandez-Rodriguez, J. A1 - Ferrand, A. A1 - Gelman, L. A1 - Gheisari, A. A1 - Hartmann, H. A1 - Kukat, C. A1 - Laude, A. A1 - Mitkovski, M. A1 - Munck, S. A1 - North, A. J. A1 - Rasse, T. M. A1 - Resch-Genger, Ute A1 - Schuetz, L. C. A1 - Seitz, A. A1 - Strambio-De-Castillia, C. A1 - Swedlow, J. R. A1 - Nitschke, R. T1 - QUAREP-LiMi: A community endeavor to advance quality assessment and reproducibility in light microscopy N2 - The community-driven initiative Quality Assessment and Reproducibility for Instruments & Images in Light Microscopy (QUAREP-LiMi) wants to improve reproducibility for light microscopy image data through Quality control (QC) management of instruments and images. It aims for a common set of QC guidelines for Hardware calibration and image acquisition, management and analysis. KW - Fluorescence KW - Microscopy KW - Quality assurance KW - Comparability KW - Imaging KW - Standards KW - Reference materials KW - Reliability KW - Data KW - Reference data KW - Biology KW - Medicine KW - Life science PY - 2021 DO - https://doi.org/10.1038/s41592-021-01162-y SN - 1548-7105 VL - 18 SP - 1424 EP - 1427 PB - Nature Publishing Group CY - London AN - OPUS4-52722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Goryacheva, O. A. A1 - Wegner, Karl David A1 - Sobolev, A. M. A1 - Häusler, I. A1 - Gaponik, N. A1 - Gorycheva, I. Y. A1 - Resch-Genger, Ute T1 - Influence of particle architecture on the photoluminescence properties of silica‑coated CdSe core/shell quantum dots N2 - Light-emitting nanoparticles like semiconductor nanocrystals (termed quantum dots, QDs) are promising candidates for biosensing and bioimaging applications based on their bright and stable photoluminescent properties. As high-quality QDs are often synthesized in organic solvents, strategies needed to be developed to render them water-dispersible without affecting their optical properties and prevent changes in postmodification steps like the biofunctionalization with antibodies or DNA. Despite a large number of studies on suitable surface modification procedures, the preparation of water-soluble QDs for nanobiotechnology applications still presents a challenge. To highlight the advantages of surface silanization, we systematically explored the influence of the core/multishell architecture of CdSe/CdS/ZnS QDs and the silanization conditions on the optical properties of the resulting silanized QDs. Our results show that the optical properties of silica-coated CdSe/CdS/ZnS QDs are best preserved in the presence of a thick CdS (6 monolayers (ML)) intermediate shell, providing a high photoluminescence quantum yield (PL QY), and a relatively thick ZnS (4.5 ML) external shell, effectively shielding the QDs from the chemical changes during silica coating. In addition to the QD core/shell architecture, other critical parameters of the silica-coating process, that can have an influence on the optical properties of the QD, include the choice of the surfactant and its concentration used for silica coating. The highest PL QY of about 46% was obtained by a microemulsion silica-coating procedure with the surfactant Brij L4, making these water-dispersible QDs to wellsuited optical reporters in future applications like fluorescence immunoassays, biomedicine, and bioimaging. KW - Nano KW - Nanomaterial KW - Particle KW - Semiconductor KW - Quantum do KW - Photoluminescence KW - Photophysics KW - Lifetime KW - Sensor KW - Mechanism KW - Surface KW - Shell KW - Silica KW - Silanization KW - Synthesis PY - 2022 DO - https://doi.org/10.1007/s00216-022-04005-7 SP - 1 EP - 13 PB - Springer AN - OPUS4-54546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, M. A1 - Zhang, R. A1 - Fa, X. A1 - Yang, J. A1 - Cheng, Z. A1 - Ansari, A. A. A1 - Ou, Jun A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - Preparation of core–shell structured NaYF4:Yb3+/ Tm3+@NaYF4:Yb3+/Er3+ nanoparticles with high sensitivity, low resolution and good reliability and application of their fluorescence temperature properties N2 - A series of NaYF4:Yb3+/Tm3+@NaYF4:Yb3+/Er3+ nanoparticles doped with Tm3+ and Er3+ were successfully prepared by the solvothermal method. Under 980 nm laser excitation, intense upconversion emission peaks of Tm3+ and Er3+ were observed for all samples. By doping Tm3+ and Er3+ with core–shell partitioning, not only a significant increase in fluorescence intensity could be achieved, but also simultaneous temperature measurements on multiple thermocouple energy levels could be realised. In addition, the temperature sensing performance of different thermocouple energy levels was also investigated, and it was found that the 3 F3 → 3 H6 and 1 G4 → 3 F4 thermocouple energy level pairs of Tm3+ were the best, with maximum absolute sensitivity and maximum relative sensitivity of up to 0.0250 K−1 and 2.155% K−1 respectively, higher than the sensitivity of other thermocouple energy levels. It has a temperature resolution of less than 0.0139 K, which is lower than that of most materials available today. By using this material as a probe to build a fiber optic temperature sensor platform, it was found to have reliable temperature measurement performance. KW - Flourescence KW - Optical probe KW - Sensor KW - Dye KW - Temperature KW - Nano KW - Particle KW - Upconversion KW - Lanthanide KW - Qantum yield KW - Quality assurance KW - Monitoring KW - Infrastructure PY - 2022 DO - https://doi.org/10.1039/d1ce01729b VL - 24 IS - 9 SP - 1752 EP - 1763 PB - RSC Publishing AN - OPUS4-54416 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hirsch, A. A1 - Lohmann, S.-H. A1 - Strelow, C. A1 - Kipp, T. A1 - Würth, Christian A1 - Geißler, Daniel A1 - Komoski, A. A1 - Wolter, C. A1 - Weller, H. A1 - Resch-Genger, Ute A1 - Mews, A. T1 - Fluorescence Quantum Yield and Single-Particle Emission of CdSe N2 - The fluorescence quantum yield (QY) of CdSe dot/CdS rod (DR) nanoparticle ensembles is dependent on the Shell growth and excitation wavelength. We analyze the origin of this dependency by comparing the optical properties of DR ensembles to the results obtained in single-particle experiments. On the Ensemble level, we find that the QY of DRs with shell lengths shorter than 40 nm exhibits no dependence on the excitation wavelength, whereas for DRs with shell lengths longer than 50 nm, the QY significantly decreases for excitation above the CdS band gap. Upon excitation in the CdSe core, the ensemble QY, the fluorescence wavelength, and the fluorescence blinking behavior of individual particles are only dependent on the radial CdS shell thickness and not on the CDs shell length. If the photogenerated excitons can reach the CdSe core region, the fluorescence properties will be dependent only on the surface passivation in close vicinity to the CdSe core. The change in QY upon excitation above the band gap of CdS for longer DRs cannot be explained by nonradiative particles because the ratio of emitting DRs is found to be independent of the DR length. We propose a model after which the decrease in QY for longer CdS shells is due to an increasing fraction of nonradiative exciton recombination within the elongated shell. This is supported by an effective-mass-approximation-based calculation, which suggests an optimum length of DRs of about 40 nm, to combine the benefit of high CdS absorption cross section with a high fluorescence QY. KW - Fluorescence KW - Quantum dot KW - Photophysics KW - Single particle spectroscopy KW - Mechanism KW - Theory KW - Ensemble measurements KW - Quantum yield KW - CdSe KW - CdS shell PY - 2019 DO - https://doi.org/10.1021/acs.jpcc.9b07957 VL - 123 IS - 39 SP - 24338 EP - 24346 PB - ACS Publications AN - OPUS4-49556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühle, Bastian T1 - Perspektive der BAM auf neuartige Materialien N2 - Neuartige Materialien, die bekannte (Werk-)Stoffe mit neuen Funktionalitäten ausstatten, spielen eine zunehmend wichtige Rolle im Bereich der Materialforschung und -prüfung. Das Spektrum neuartiger Materialien reicht von der gezielten Oberflächenfunktionalisierung und -strukturierung makroskopischer Materialien, dünnen Beschichtungen bis hin zu mikro- und nanoskaligen Kompositmaterialien und funktionalen Materialien an der Schnittstelle zur Biologie, Biotechnologie, nachhaltige Energiespeicherung und Sensorik. Dabei bieten neuartige Materialien die Chance, Werkstoffe und Produkte mit erweiterter oder verbesserter Funktionalität zu erhalten und Sicherheit bereits im Designprozess zu berücksichtigen. Durch dieses breite Anwendungsspektrum und die Herausforderungen, die solche Materialien für die Sicherheit in Chemie und Technik mit sich bringen, sind diese in allen Themenfeldern der BAM repräsentiert (Material, Analytical Sciences, Energie, Infrastruktur und Umwelt). Die Aufgaben der BAM erstrecken sich dabei von der Herstellung von Referenzmaterialien für Industrie, Forschung und Regulation, über die Erstellung von standardisierten Referenzverfahren für nachhaltige Messungen im Umwelt- und Lebenswissenschaftsbereich bis hin zur Bereitstellung von belastbaren und zitierbaren Referenzdaten. Durch die genaue Charakterisierung neuartiger Materialien können potentiell problematische Substanzen identifiziert und deren Risiken besser abgeschätzt werden. In diesem Beitrag werden einige aktuelle Beispiele aus diesen Bereichen vorgestellt. T2 - NanoDialog der Bundesregierung - Chancen und Risiken von Neuartigen Materialien CY - Berlin, Germany DA - 22.05.2019 KW - Advanced Materials KW - Nanomaterialien KW - Neuartige Materialien PY - 2019 AN - OPUS4-49594 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, Katrin T1 - Calibration Beads for the Characterization of the Performance of Fluorescence-based High- Throughput and Imaging devices N2 - In all fluorescence-based techniques, the measured signals contain not only sample-related but also instrument-specific contributions, which limit the direct comparison of fluorescence data obtained e.g. on different devices or at different times and often hamper quantification. To rule out instrumentation as major source of variability of emission data, accepted fluorescence standards and procedures for the control of instrument specifications and long-term performance are required. For flow cytometry (FCM), a broad variety of fluorophore-stained polymer beads differing in emission wavelength and intensity is available for the testing of the alignment, sensitivity, and other parameters of FCM. These calibration tools are intended to facilitate the assessment of instrument performance to ensure reliable measurements and to improve the comparability of FCM experiments. As a step towards an improved comparability of fluorescence data, with special emphasis on spectroscopic methods measuring nano- and micrometer-sized fluorescent objects, we are currently developing a set of fluorescent polystyrene (PS) beads loaded with luminophores from the certified BAM-Kit “Spectral fluorescent standards”, initially developed for the calibration of fluorescence spectrometers. Here, we present first results from studies of these fluorophore-loaded polymer beads. Moreover, new beads are made to supplement this kit by encapsulating near-infrared (NIR)-emissive luminophores in PS beads to cover the UV/VIS, and NIR wavelength range. These beads are designed for calibration of flow cytometers and other fluorescence imaging systems to meet the increasing demand for reliable and comparable fluorescence data especially in strongly regulated areas like e.g. medical diagnostics. T2 - 29th Annual Conference of the German Society for Cytometry CY - Berlin, Germany DA - 25.09.2019 KW - Calibration beads KW - Fluorescence KW - Performance validation KW - imaging KW - FCM PY - 2019 AN - OPUS4-49422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hübner, Oskar T1 - Luminescence lifetime encoding for flow cytometry with quantum-dot-encoded beads N2 - Spectral encoding of cells or particles and the discrimination of multiple spectral codes are a critical process in flow cytometry (FCM). Typical issues in spectral encoding are, e.g., the spectral overlap of codes, or the increasing complexity of instruments . The exploitation of the photoluminescence lifetime (LT) as an encoding parameter could be used to circumvent both of these issues, as it adds another dimension to the parameter space, or, when used as a stand-alone parameter, requiring only one excitation light source and one detector. While LT encoding was considered already decades ago it is still not implemented as a routine technique in FCM yet, mainly due to the challenge of very few photons being available within the limited transition time of a cell or particle through the laser spot. Recently, we demonstrated LT-FCM based on luminophores with ns LTs in a compact and low-cost flow cytometer. Measurements on polymer microbeads containing luminophores with distinctly different excited state LTs enabled the complete discrimination of three LT codes and five codes in total could be identified. Now, we have extended our approach towards considerably longer LTs by custom-made polymer microbeads loaded with different ratios of InP/ZnS and AgInS2 quantum dots. The use of these materials significantly expands the usable time range for LT encoding to up to several hundred ns. Our studies demonstrate the possibility to further increase the number of viable LT codes for multiplexing in LT-FCM without the need for extensive hardware modifications. T2 - Visions in Cytometry - 29th Annual Conference of the German Society for Cytometry CY - Berlin, Germany DA - 25.07.2019 KW - Multiplexing KW - Lifetime KW - Bead KW - Flow cytometry KW - Fluorescence KW - Quantum dot KW - InP KW - AIS KW - Dye KW - Encoding KW - Barcoding KW - Assay KW - Method PY - 2019 AN - OPUS4-49390 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühle, Bastian T1 - Surface Functional Group Quantification on Micro- and Nanoparticles N2 - Organic and inorganic micro- and nanoparticles are increasingly used as drug carriers, fluorescent sensors, and multimodal labels in the life and material sciences. Typically, these applications require further functionalization of the particles with, e.g., antifouling ligands, targeting bioligands, stimuli-responjsive caps, or sensor molecules. Besides serving as an anchor point for subsequent functionalization, the surface chemistry of these particles also fundamentally influences their interaction with the surrounding medium and can have a significant effect on colloidal stability, particle uptake, biodistribution, and particle toxicity in biological systems. Moreover, functional groups enable size control and tuning of the surface during the synthesis of particle systems. For these reasons, a precise knowledge of the chemical nature, the total number of surface groups, and the number of groups on the particle surface that are accessible for further functionalization is highly important. In this contribution, we will will discuss the advantages and limitiations of different approaches to quantify the amount of commonly used surface functional groups such as amino,[1,2] carboxy,[1,2] and aldehyde groups.[3] Preferably, the quantification is carried out using sensitive and fast photometric or fluorometric assays, which can be read out with simple, inexpensive instrumentation and can be validated by complimentary analytic techniques such as ICP-OES and quantitative NMR. T2 - NANAX Hamburg CY - Hamburg, Germany DA - 16.09.2019 KW - Microparticles KW - Nanoparticles KW - Quantitative Analysis KW - Surface KW - Funtional Groups PY - 2019 AN - OPUS4-49616 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Imaging of biological samples by LA-ICP-MS N2 - In recent years, elemental imaging of biological samples like tissue thin sections using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining more and more importance. Improvements concerning spatial resolution as well as signal-to-background ratio due to low-dispersion sample chambers make LA-ICP-MS also interesting for single cell analysis. To evaluate the interaction of nanoparticles (NPs) with cells LA-ICP-MS was applied for the imaging of individual cells. Our findings show, that NP aggregates can be localized within cellular compartments. The uptake efficiency depends strongly on the physico-chemical properties of the nanostructures (size, chemical composition, surface modification), as well as on the incubation conditions (concentration, time). Moreover, LA-ICP-MS is increasingly becoming an important complementary technique in bioanalysis by using element-tagging strategies to determine biomolecules indirectly. Based on the specific binding between antibodies and their corresponding antigens, proteins and peptides can be detected in tissue or cells using tagged antibodies. As artificial tags metal chelates loaded with lanthanides, polymer-based elemental tags or metal-containing nanoparticles can be used. Thereby LA-ICP-MS is a sensitive detection tool for multiplexed immuno-histochemistry of tissue and cell samples. Our results demonstrate the potential of LA-ICP-MS to investigate the distribution of naturally occurring elements, administered agents as well as biomolecules by using metal-tagged antibodies. T2 - Workshop on tandem LIBS/LA-ICP-MS 2019 CY - Berlin, Germany DA - 18.11.2019 KW - Laser ablation KW - ICP-MS KW - Nanoparticles KW - Imaging PY - 2019 AN - OPUS4-49704 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wang, Cui T1 - Ratiometric Nanosensors for Simultaneously “TOP” Measuring Temperature, Oxygen and pH at a Single Excitation Wavelength N2 - In summary, by combining the NIR-emissive [Cr(ddpd)2][BPh4]3 complex CrBPh4 with its extremely large energy gap between the longest wavelength absorption and emission maxima with a pH-responsive fluorescein derivative (FITC) and an inert reference dye like Nile Red (NR) and 5,10,15,20tetrakis(pentafluorophenyl) porphyrin (TFPP), we developed nanosensors for simultaneously sensing temperature, O2 partial pressure, and pH. These novel TOP nanosensors (temperature, oxygen, pH) cover the biologically and physiologically relevant concentration ranges of these parameters/analytes with single wavelength excitation in PBS buffer and in a cell culture medium containing bovine serum albumin (BSA). The response of both nanosensors to all parameters is fully reversible and only minimally affected by the presence of BSA, the most common serum albumin. Moreover, comparative studies with nanosensors containing only a single type of stimuli-responsive molecule and with the respective molecular systems revealed that the different sensor components do not interfere with each other. Future research will include the testing of these nanosensors in cellular uptake studies and, after surface modification with targeted bioligands, eventually in in vivo experiments as previously done by some of us with other polystyrene nanoparticle reporters and nanosensors.46,47 Moreover, this concept of multianalyte sensing will be expanded to nanosensors derived from differently sized premanufactured biocompatible polymer particles and different stimuli-responsive dyes like fluorescent indicators for biologically and bioanalytically relevant metal ions. T2 - ISPPCC 2019 CY - Hong Kong, China DA - 14.07.2019 KW - Medical diagnostics KW - Sensor KW - Nnanoparticle KW - Nanosensor KW - Fluorescence KW - Oxygen KW - Temperature KW - Ratiometric KW - PH KW - Lifetime KW - NIR KW - Cr(III) complex KW - FITC KW - Dye KW - Environment PY - 2019 AN - OPUS4-49698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hübner, Oskar T1 - Spectral and Lifetime Encoding of Polymer Particles with Cd-free Ternary Semiconductor Nanocrystals for Flow Cytometry with Time Resolved Fluorescence Detection N2 - Multiplexed encoding schemes of nano- and micrometer sized particles with fluorescent dyes or quantum dots (QDs) and their optical detection, are of increasing interest for applications in the life sciences, for example in flow cytometry. Almost all strategies utilizing fluorescence focus on spectrally distinguishable emission bands or colors and different intensity levels as fluorescence codes. The fluorescence parameter lifetime has been, however, barely exploited. In this work the goal is to perform multiplexing with encoding fluorophores with different fluorescence lifetimes (LTs). In comparison to the spectral multiplexing strategies this has the advantage, that the different fluorescence LT codes can be measured with the excitation and emission wavelength, thus reducing instrument costs. Moreover, LTs should not depend on emitter concentration. Unlike organic dyes, the LTs of which are typically < 10 ns, the fluorescence LTs of ternary semiconductor QDs that represent a “green” alternative to conventional Cd-containing QDs are in the range of several hundred ns, independent of oxygen concentration, and can be tuned to a certain extent by chemical composition and surface chemistry. This present a time region that can be barely covered by other emitters that have either much shorter or longer lifetimes. In this project, different encoding strategies will be assessed and the encoded particles will be then used for fluorescence assays for the analysis of several targets in parallel. Therefor the encoded particles will be functionalized with different target-specific bioligands and read out with a specifically designed flow cytometer enabling time-resolved fluorescence detection. With this instrument, the particles will be discriminated by their fluorescence LTs In one detection channel while the analytes will be quantified by fluorescence labels in a second channel in the intensity domain. T2 - Bad Honnef Physics School Exciting nanostructures: Characterizing advanced confined systems CY - Bad Honnef, Germany DA - 21.07.2019 KW - Multiplexing KW - Lifetime KW - Bead KW - Flow cytometry KW - Fluorescence KW - Quantum dot KW - InP KW - AIS KW - Dye KW - Encoding KW - Barcoding KW - Assay KW - Method PY - 2019 AN - OPUS4-49723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hübner, Oskar T1 - Lifetime Barcoding of Polystyrene Beads with Fluorescent Nanocrystals for Fluorescent Lifetime Detection in Flow Cytometry N2 - Multiplexed encoding schemes of nano- and micrometer sized polymer particles with fluorescent dyes or quantum dots (QDs) and their optical detection, are of increasing interest for applications in the life sciences, for example in flow cytometry. Almost all strategies utilizing fluorescence focus on spectrally distinguishable emission bands or colors and different intensity levels as fluorescence codes. In this work the goal is to perform multiplexing with encoding fluorophores with different fluorescence lifetimes (LTs). In comparison to the spectral multiplexing strategies this has the advantage, that the different fluorescence LT codes can be measured with the same excitation and emission wavelength, thus reducing instrumental costs. Moreover, LTs should not depend on emitter concentration. Unlike organic dyes, the LTs of which are typically <10ns, the fluorescence LTs of ternary semiconductor QDs which represent a “green” alternative to conventional Cd-containing QDs are in the range of several hundred ns, independent of oxygen concentration, and can be tuned to a certain extent by chemical composition and surface chemistry. This presents a time region that can barely be covered by other emitters that have either much shorter or longer lifetimes. In this project, different encoding strategies will be assessed, and the encoded particles will then be used for fluorescence assays for the analysis of several targets in parallel. Therefore, the encoded particles will be functionalized with different target-specific bioligands and read out with a specifically designed flow cytometer enabling time-resolved fluorescence detection. With this instrument, the particles will be discriminated by their fluorescence LTs in one detection channel while the analytes will be quantified by fluorescence labels in a second channel in the intensity domain. T2 - Tag der Chemie 2019 CY - Berlin, Germany DA - 11.07.2019 KW - Multiplexing KW - Lifetime KW - Bead KW - Flow cytometry KW - Fluorescence KW - Quantum dot KW - InP KW - AIS KW - Dye KW - Encoding KW - Barcoding KW - Assay KW - Method PY - 2019 AN - OPUS4-49722 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauli, Jutta T1 - Determination of the Uncertainty Budgets of the Fluorescence Quantum Yield Values of Certified Standards as New Optical Reference Materials N2 - Luminescence techniques are amongst the most commonly used analytical methods in the life and material sciences due to their high sensitivity and their nondestructive and multiparametric character. Photoluminescence signals are, however, affected by wavelength-, polarization- and time-dependent instrument specific effects. This hampers the comparability of fluorescence measurements and calls for simple tools for instrument characterization and the quantification of measured fluorescence intensities. Well characterized fluorescence standards for instrument calibration and performance validation (IPV) can be used also to reference fluorescence signals. Of special importance is the reliable and accurate determination of photoluminescence quantum yields (Ф f), that equals the number of emitted per absorbed photons and presents the key performance parameter for emitter efficiency and the comparison of different luminophores. The determination of Ф f is typically done with the aid of so-called quantum yield standards with well-known Ф f values. These standards can also be applied to evaluate integrating sphere setups, which are increasingly being used for absolute measurements of Ф f values. In this respect, division biophotonics of BAM has certificated a set of Ф f standards, which absorb and fluorescence in the wavelength range from 350 to 1100 nm. In the following, the route to Ф f standards with reliable and traceable Ф f values with a complete uncertainty budget will be presented. T2 - Eurachem-Workshop „Uncertainty from sampling and analysis for accredited laboratories CY - Berlin, Germany DA - 19.11.2019 KW - Uncertainty KW - Fluorescence KW - Quantum yield standard KW - Reference Material PY - 2019 AN - OPUS4-49661 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Changes in polymer surface morphology and leaching of brominated flame retardants induced by different weathering scenarios N2 - In addition to previously reported results on the accelerated weathering of polystyrene samples (PS) containing 1 wt.% hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene samples (PP) containing 0.1 wt.% BDE-209. All studied polymer samples were exposed to a defined weathering schedule in a climate chamber in accordance to regulation EN ISO 4892-3:2006. For the determination of BDE-209 in the collected raining water the samples were prepared in accordance to a validated protocol. Before the analyses each sample was spiked with isotopically labeled BDE-209. Subsequently the samples were extracted with isooctane. The obtained extracts were concentrated, and the resulting solutions were analyzed by GC/MS. Additionally, the total bromine content was monitored for the weathered and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and X-ray fluorescence analysis (XRF) as a non-destructive and rapid method. In general, the resulting data from the accelerated weathering will be compared to those from the natural weathering experiments. Here, the surfaces of the test pieces were analyzed by LA-ICP-MS and XRF as well. Moreover, soil bed tests were conducted in a well characterized model soil. This soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining basin inside of an air-conditioned cellar. In this manner, TOC, water capacity and humidity are recorded parameters. To induce a leaching process from the samples by the raining water, the target water content is calculated to 8%. The actual humidity is measured by a tensiometer, assuring the duration of the raining period. A defined humidity is a fundamental parameter for a biological activity in the soil. The test polymers were placed up to the half in the soil. Microbial activity of the soil is monitored by a reference polymer (polyurethane) and should induce the release of HBCD and BDE-209 out of the test materials. These released analytes will be captured by passive samplers (silicone tubes) placed in a distinct distance to the polymer samples in the soil. The soil bed experiments are complementary to the weathering experiments due to the biological activity in the soil. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - BFR KW - LA-ICP-MS KW - XRF KW - Polymer PY - 2019 N1 - Folien in deutscher Sprache, Votrag, Titel und Abtract in englischer Sprache AN - OPUS4-49796 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya T1 - Quantification of Aldehydes via Catch and Release of Reporter Chromophores on Polymeric Microbeads N2 - Aldehyde-functionalized materials have found widespread use in bioconjugation applications. For example, coupling of aldehyde surface groups with proteins, peptides or amine-functionalized oligonucleotides can readily produce biomolecule-decorated chip and bead surfaces for multiplex analyses. Furthermore, aldehyde-modified nanoparticles can possess bioadhesive properties that can prolong their retention time in biological compartments. These emerging novel bioanalytical and biomedical applications call for reliable tools and methods to detect and quantify accessible aldehyde functionalities on the surface of 2D- and 3D-supports. We present here a versatile concept to quantify the amount of accessible aldehyde moieties on the surface of PMMA particles through the specific binding and subsequent release of small reporter molecules such as absorbing and fluorescent dyes utilizing acylhydrazone formation as a reversible covalent labeling strategy. Unbound reporter molecules can be easily removed by washing steps, eliminating inaccuracies caused by unspecific adsorption to hydrophobic surfaces. Cleavage of the hydrazones at acidic pH assisted by a carbonyl trap releases the optical reporters rapidly and quantitatively and allows for their optical detection at low concentration. Importantly, this strategy separates the signal-generating molecules from the bead surface, thereby circumventing common pitfalls of optical assays associated with light scattering and signal distortions due to binding-induced changes in reporter fluorescence and quenching dye-dye interactions on crowded material surfaces. The potential of this catch-and-release strategy for surface group quantification is representatively demonstrated for a set of microparticles functionalized with different aldehyde densities. This concept is validated by a colorimetric assay with a different optical probe, which contains a reductively cleavable disulfide bond and a reporter that can be quantified photometrically in solution after its release. The excellent match of the results of both optical assays confirms their suitability for the rapid and sensitive quantification of aldehydes on microbead surfaces. These simple catch-and-release assays are excellent tools for process control during bead fabrication and the comparison of different bead batches. Their potential for predicting biomolecule coupling efficiencies in bioconjugation reactions is currently assessed in reductive amination reactions with streptavidin. T2 - Tag der Chemie CY - Berlin, Germany DA - 11.07.2019 KW - Optical quantification KW - Catch and release assay KW - CHO functions KW - Polymer particles PY - 2019 AN - OPUS4-49783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya T1 - Quantification of Aldehyde Functional Groups on Polymeric Microbeads via Catch and Release of Reporters N2 - Aldehyde-functionalized materials have found broad use in bioconjugation applications. For example, coupling of aldehyde surface groups with to proteins or amine-functionalized oligonucleotides can readily produce biomolecule-covered chip microarray and bead surfaces for multiplex analyses. Additionally, aldehyde-modified nanoparticles can possess bioadhesive properties that can extend their retention time in biological compartments. These emerging novel bioanalytical applications call for reliable tools and methods to detect and quantify accessible aldehyde functionalities. We present here a straightforward concept to quantify the amount of accessible aldehyde moieties on the surface of polymethylmethacrylate (PMMA) particles through the specific binding and subsequent release of small reporter molecules such as absorbing and fluorescent dyes utilizing hydrazone formation as a reversible covalent labeling strategy. Unbound reporter molecules can be easily removed by washing steps, eliminating inaccuracies caused by unspecific adsorption to hydrophobic surfaces. Cleavage of the hydrazones at acidic pH assisted by a carbonyl trap releases the optical reporters rapidly and quantitatively and allows for their optical detection at low concentration. Importantly, this strategy separates the signal-generating molecules from the bead surface, thereby circumventing light scattering and signal distortions due to binding-induced changes in reporter fluorescence and quenching dye-dye interactions on crowded material surfaces. The potential of this catch-and-release strategy for surface group quantification is representatively demonstrated for a set of microparticles functionalized with different aldehyde densities. This concept is validated by a colorimetric assay with a different optical probe, which contains a reductively cleavable disulfide bond and a reporter that can be quantified photometrically in solution after its cleavage. The excellent match of the results of both optical assays confirms their suitability for the rapid and sensitive quantification of aldehydes on microbead surfaces. These simple catch-and-release assays are excellent tools for process control during bead fabrication and the comparison of different bead batches. T2 - 29th Annual Conference of the German Society for Cytometry CY - Berlin, Germany DA - 25.09.2019 KW - Optical quantification KW - Catch and release assay KW - CHO functions KW - Polymer particles PY - 2019 AN - OPUS4-49784 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühle, Bastian T1 - Quantification of Aldehydes on Polymeric Microbead Surfaces via Catch and Release of Reporter Chromophores N2 - Aldehyde-functionalized materials have found widespread use in bioconjugation applications. For example, coupling of aldehyde surface groups with proteins, peptides or amine-functionalized oligonucleotides can readily produce biomolecule-decorated chip and bead surfaces for multiplex analyses. Furthermore, aldehyde-modified nanoparticles can possess bioadhesive properties that can prolong their retention time in biological compartments. These emerging novel bioanalytical and biomedical applications call for reliable tools and methods to detect and quantify accessible aldehyde functionalities on material surfaces. We report on a versatile concept to quantify the accessible aldehyde moieties on particle surfaces through the specific binding and subsequent release of small reporter molecules such as fluorescent dyes and non-fluorescent chromophores utilizing acylhydrazone formation as a reversible covalent labeling strategy. This is representatively demonstrated for a set of polymer microparticles with different aldehyde labeling densities. Excess reporter molecules can be easily removed by washing, eliminating inaccuracies caused by unspecific adsorption to hydrophobic surfaces. Cleavage of hydrazones at acidic pH assisted by a carbonyl trap releases the fluorescent reporters rapidly and quantitatively and allows for their fluorometric detection at low concentration. Importantly, this strategy separates the signal-generating molecule from the bead surface, thereby circumventing common issues associated with light scattering and signal distortions due to binding-induced changes in reporter fluorescence as well as quenching dye-dye interactions on crowded material surfaces. In addition, we demonstrate that the release of a non-fluorescent chromophore via disulfide cleavage and subsequent quantification by absorption spectroscopy gives comparable results, verifying that both assays are capable of rapid and sensitive quantification of aldehydes on microbead surfaces. These strategies enable a quantitative comparison of bead batches with different functionalization densities, and a qualitative prediction of their coupling efficiencies in bioconjugations, as demonstrated in reductive amination reactions with Streptavidin. T2 - Anakon CY - Münster, Germany DA - 25.04.2019 KW - Optical quantification KW - Polymer particles KW - CHO functions KW - Catch and release assay PY - 2019 AN - OPUS4-49781 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dhamo, Lorena T1 - Synthesis And Optical Properties Of AgInS2/ZnS QDs In Solution And In PLMA N2 - Ternary semiconductors quantum dots (t-QD) are Cd-free core-only or core-shell semiconductor nanocrystals with a core made from I-III-VI group elements like Cu-In-S (CIS) or Ag-In-S (AIS). To enhance the PL quantum yield (PL QY) and prevent material deterioration and oxidation, these QDs are commonly surface-passivated with ay ZnS shell. CIS and AIS QDs exhibit broad photoluminescence (PL) bands that cover visible spectrum up to the near infrared (NIR), the spectral position of which being tunable by size, chemical composition of the core (ratio of the components), and surface ligand. They show high absorption coefficients, high PL quantum yields (PL QY of up to 70%), and long luminescence lifetimes in the order of a few hundred nanoseconds that make them promising materials for a broad variety of applications. This makes them interesting alternatives for Cd-based QDs for applications as optically active components in solar concentrators or solar cells, light emitting diodes (LED) or as reporter in the life sciences. Here we present a systematic spectroscopic study of a set of AIS/ZnS QDs synthesized in water, size selected by fractioned precipitation, and after ligand exchange in an apolar organic solvent as well as embedded in a polymer. The latter was achieved by a photochemically initiated polymerization. The PL properties of these AIS/ZnS including PL QY and the PL decay kinetics assessed in different matrices/environments are shown and discussed as well as possible applications in energy conversion. T2 - Tag der Chemie CY - Berlin, Germany DA - 11.07.2019 KW - Water synthesis KW - Quantum dots KW - Nanomaterial PY - 2019 AN - OPUS4-49785 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dhamo, Lorena T1 - Synthesis and characterization of AgInS2 /ZnS Quantum Dots in solution and polymer N2 - Ternary semiconductors Quantum Dots (t-QD) are Cd-free semiconductors nanocrystals made from I-III-VI group elements like CIS or AIS. They are interesting alternatives for Cd-based QDs for applications as optically active components in solar concentrators or solar cells, light emitting diodes (LED) or in the life sciences. To enhance the PL quantum yield (PL QY) and prevent material deterioration and oxidation, these QDs are commonly surface-passivated with by ZnS shell. AIS QDs exhibit broad photoluminescence (PL) spectra in the visible and near infrared, which are tunable by size, chemical composition (ratio of components or doping), and surface ligand. They show a relatively high absorption coefficient, high PL QY (up to 70%), and long luminescence lifetimes in the order of a few hundred nanoseconds that make them promising materials for a broad variety of applications. Moreover, they can be simply prepared even in water in high quality which avoids further ligand exchange steps for all water-based applications know to decrease QY. Here we present a systematic spectroscopic study of differently colored AIS/ZnS QDs synthesized in water, size selected by precipitation, transferred to organic solvents via ligand exchange, and embedded in different polymers by a photochemically initiated polymerization. The PL properties including PL QY and the PL decay kinetics measured in different matrices are shown and discussed. T2 - Bunsentagung CY - Jena, Germany DA - 29.05.2019 KW - Water synthesis KW - Quantum dots KW - Nanomaterial KW - Energy PY - 2019 AN - OPUS4-49787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian A1 - Iznaguen, Hassan A1 - Traub, Heike A1 - Feldmann, Ines A1 - Köppen, Robert A1 - Witt, Angelika A1 - Jung, Christian A1 - Becker, Roland A1 - Oleszak, Katrin A1 - Bücker, Michael A1 - Urban, Klaus A1 - Reger, Christian A1 - Ostermann, Markus T1 - Bewitterungsszenarien im Vergleich – Veränderungen in der Oberflächenmorphologie von Polypropylen (PP) und Polystyrol (PS) unter dem Aspekt des Austrags von polybromierten Flammschutzmitteln N2 - Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umwelt-beständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polystyrol (PS) und Polypropylen (PP) zum Einsatz. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden. T2 - 47. Jahrestagung der GUS CY - Blankenloch-Stutensee, Germany DA - 21.03.2018 KW - Schadstoffaustrag KW - Umweltsimulation KW - Bewitterung PY - 2018 SN - 978-981-18507-2-7 VL - 47 SP - 115 EP - 128 AN - OPUS4-49802 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - LA-ICP-MS- und RFA-Messungen für die Bestimmung von polybromierten Flammschutzmitteln(PBFSM) in Polystyrol- und Polypropylenproben N2 - Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umwelt-beständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polystyrol (PS) und Polypropylen (PP) zum Einsatz. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe (polybromierte Flammschutzmittel) in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden. T2 - Kolloquium "Aquatische Ökologie" CY - Essen, Germany DA - 27.11.2019 KW - Umweltsimulation KW - PBFSM KW - LA-ICP-MS KW - RFA PY - 2019 AN - OPUS4-49975 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Weathering of flame-protected polymers and monitoring of the release of brominated flame retardants under different scenarios N2 - In addition to previously reported results on the accelerated weathering of polystyrene samples (PS) containing 1 wt.% hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene samples (PP) containing 0.1 wt.% BDE-209. All studied polymer samples were exposed to a defined weathering schedule in a climate chamber in accordance to regulation EN ISO 4892-3:2006. For the determination of BDE-209 in the collected raining water the samples were prepared in accordance to a validated protocol. Before the analyses each sample was spiked with isotopically labeled BDE-209. Subsequently the samples were extracted with isooctane. The obtained extracts were concentrated, and the resulting solutions were analyzed by GC/MS. Additionally, the total bromine content was monitored for the weathered and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and X-ray fluorescence analysis (XRF) as a non-destructive and rapid method. In general, the resulting data from the accelerated weathering will be compared to those from the natural weathering experiments. Here, the surfaces of the test pieces were analyzed by LA-ICP-MS and XRF as well. Moreover, soil bed tests were conducted in a well characterized model soil. This soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining basin inside of an air-conditioned cellar. In this manner, TOC, water capacity and humidity are recorded parameters. To induce a leaching process from the samples by the raining water, the target water content is calculated to 8%. The actual humidity is measured by a tensiometer, assuring the duration of the raining period. A defined humidity is a fundamental parameter for a biological activity in the soil. The test polymers were placed up to the half in the soil. Microbial activity of the soil is monitored by a reference polymer (polyurethane) and should induce the release of HBCD and BDE-209 out of the test materials. These released analytes will be captured by passive samplers (silicone tubes) placed in a distinct distance to the polymer samples in the soil. The soil bed experiments are complementary to the weathering experiments due to the biological activity in the soil. T2 - SETAC Glb 2019 CY - Landau, Germany DA - 04.09.2019 KW - Polymer KW - XRF KW - LA-ICP-MS KW - BFR PY - 2019 AN - OPUS4-49797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica T1 - Imaging mass cytometry for visualisation of neuroinflammation induced changes N2 - Multiple sclerosis (MS) is the most common acquired neurological disease affecting Young adults. It leads to myelin destruction and formation of lesions in the brain and permeabilization of the blood-brain barrier (BBB). Gadolinium based contrast agents (GBCA), used for diagnosis and monitoring by MRI, might accumulate in tissue, including brain. Using an animal model, application of linear and macrocyclic GBCA was investigated. Analysis was performed by laser ablation inductively coupled plasma (LA-ICP) MS. This method works as a bioimaging tool for sample thin sections and allows to identify regions of accumulated Gd in the samples. In healthy and diseased mice, inflammationmediated changes in the brain were investigated by application of GBCA. The mean objective is to understand the changes in inflamed tissue and correlate alterations of the BBB by LA-ICP-MS (Imaging Mass Cytometry). T2 - Colloquium Analytische Atomspektroskopie 2019 CY - Freiberg, Germany DA - 23.09.2019 KW - Bioimaging KW - LA-ICP-MS KW - Imaging Mass Cytometry KW - Gadolinium PY - 2019 AN - OPUS4-49853 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heckel, Thomas T1 - Zerstörungsfreie Prüfung @ BAM N2 - Die Schwerpunktthemen für die Forschung der BAM im Bereich der zerstörungsfreien Prüfung werden vorgestellt. Es stehen die aktuellen Forschungsprojekte der Fachbereiche 8.1 bis 8.7 der Abteilung 8 und des Arbeitsgebietes Probabilistische Sicherheits- und Zuverlässigkeitsanalysen von Frau Dr. Bertovic sowie der Nachwuchsgruppe von Frau JProf. Dr. Kruschwitz im Vordergrund. T2 - Young Professionals Aerospace 2019 CY - Wildau, Germany DA - 25.11.2019 KW - Zerstörungsfreie Prüfung KW - Sensorik KW - Bauwesen KW - Radiografie KW - Ultraschall KW - Wirbelstrom KW - Computertomografie KW - Faseropische Sensorik KW - Thermografie KW - Human Factors PY - 2019 AN - OPUS4-50013 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraft, Marco A1 - Würth, Christian A1 - Muhr, V. A1 - Hirsch, T. A1 - Resch-Genger, Ute T1 - Explaining the influence of dopant concentration and excitation power density on the luminescence and brightness of beta-NaYF_4:Yb~(3+),Er~(3+) nanoparticles: Measurements and simulations N2 - A systematic study of the luminescence properties of monodisperse β-NaYF4: 20% Yb3+, 2% Er3+ upconversion nanoparticles (UCNPs) with sizes ranging from 12–43 nm is presented utilizing steady-state and time-resolved fluorometry. Special emphasis was dedicated to the absolute quantification of size- and environment-induced quenching of upconversion luminescence (UCL) by highenergy O–H and C–H vibrations from solvent and ligand molecules at different excitation power densities (P). In this context, the still-debated Population pathways of the 4F9/2 energy level of Er3+ were examined. Our results highlight the potential of particle size and P value for color tuning based on the pronounced near-infrared emission of 12 nm UCNPs, which outweighs the red Er3+ emission under “strongly quenched” conditions and accounts for over 50% of total UCL in water. Because current rate equation models do not include such emissions, the suitability of these models for accurately simulating all (de)population pathways of small UCNPs must be critically assessed. Furthermore, we postulate population pathways for the 4F9/2 energy level of Er3+, which correlate with the size-, environment-, and P-dependent quenching states of the higher Er3+ energy levels. KW - Nanoparticle KW - Nanosensor KW - Fluorescence KW - Upconversion KW - Upconversion nanoparticle KW - NIR KW - Photophysics KW - Lanthanide KW - Size KW - Surface chemistry KW - Quantum yield KW - Mechanism KW - Lifetime KW - Decay kinetics KW - Quenching KW - Diameter KW - Cyclohexane KW - Water PY - 2018 DO - https://doi.org/10.1007/s12274-018-2159-9 VL - 11/12 SP - 6360 EP - 6374 PB - Springer Nature AN - OPUS4-50307 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vössing, Konrad A1 - Gaal, Mate A1 - Niederleithinger, Ernst T1 - Imaging wood defects using air coupled ferroelectret ultrasonic transducers in reflection mode N2 - Air-coupled ultrasound (ACU) is used to detect defects in wood panels without physically contacting the sample and with a quick scanning rate. Transducers made of cellular polypropylene (PP) with a high signal-to-noise ratio are quite suitable for ACU testing of wood. The extremely low modulus of elasticity and low density of PP transducers results in a small difference in acoustic impedance for the Transmission of ultrasonic waves between the transducer and air, allowing new areas of application to become possible. To demonstrate the suitability of the reflection technique, measurements are shown on the three samples Multiplex, LVL, and MDF and compared with transmission measurements. Due to this acoustic barrier and the use of cellular PP transducers, an exact detection of delamination and cavities is possible in wood panels up to 40 mm thick. If only one side of an object is accessible and the depth of the defect is of interest, the reflection technique is preferred at the expense of a reduced measuring accuracy and Penetration depth. KW - Wood KW - Ultrasound KW - Air coupled KW - Defects PY - 2020 DO - https://doi.org/10.1016/j.conbuildmat.2020.118032 VL - 241 SP - 118032, 1 EP - 8 PB - Elsevier Ltd. AN - OPUS4-50235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - NDE of foundations N2 - This talk teaches the basic princioles and applications of NDT methods for deep foundations, sprecifically piles. A variety of testing methods are discussed (integrity testing, ultrasonic crosshole logging, parallel seismic and others). Capabilities and limitations are given as well as specific hints for practical use. T2 - NDE 2019 Pre-Conference Tutorial PCT 4 CY - Bangalore, India DA - 03.12.2019 KW - NDT KW - Foundation KW - Pile KW - Integrity testing PY - 2019 AN - OPUS4-50169 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Standardization of Flourescence Measurements in the UV/VIS/NIR/IR at BAM N2 - Photoluminescence techniques are amongst the most widely used tools in the life sciences, with new and exciting applications in medical diagnostics and molecular imaging continuously emerging. Advantages include their comparative ease of use, unique sensitivity, non-invasive character, and potential for multiplexing, remote sensing, and miniaturization. General drawbacks are, however, signals, that contain unwanted wavelength- and polarization contributions from instrument-dependent effects, which are also time-dependent due to aging of instrument-components, and difficulties to measure absolute fluorescence intensities. Moreover, scattering systems require special measurement geometries and the interest in new optical reporters with emission > 1000 nm strategies for reliable measurements in the second diagnostic for the comparison of material performance and the rational design of new fluorophores with improved properties. Here, we present strategies to versatile method-adaptable liquid and solid fluorescence standards for different fluorescence parameters. Examples are multi-emitter glasses, spectral fluorescence standards, and quantum yield standards for the UV/vis/NIR. T2 - Konsortiumtreffen Mikroskopie CY - Universität Münster, Germany DA - 20.01.2020 KW - Fluorescence standard KW - Instrument calibration KW - Integrating sphere spectroscopy KW - Fluorescence quantum yield KW - Fluorescent glasses KW - Fluorescence microscopy KW - Particle, imaging PY - 2020 AN - OPUS4-50308 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Recent advances in NDE of concrete structures at BAM N2 - This talk gives an introduction to BAM and its NDT-CE division. Specific challenges in NDT-CE are discussed as well as recent research results. T2 - NDE 2019 Pre-Conference Tutorial PCT 4 CY - Bangalore, India DA - 03.12.2019 KW - NDT KW - Civil engineering PY - 2019 AN - OPUS4-50168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cheng, Z. A1 - Meng, M. A1 - Qiao, X. A1 - Liu, Y. A1 - Resch-Genger, Ute A1 - Ou, J. T1 - The synthesis of Er3+/Yb3+/K+ triple-doped NaYF4 phosphors and its high sensitivity optical thermometers at low power N2 - Optical Thermometry is popular among researchers because of its non-contact, high sensitivity, and fast measurement properties. In the present experiment, Er3+/Yb3+/K+ co-doped NaYF4 nanoparticles with different K+ concentrations were synthesized by solvothermal method, and the samples showed bright upconversion green emission under the excitation of a 980 nm laser. The powder X-ray diffractometer and transmission electron microscope were used to characterize the crystal structure and its surface morphology, respectively. The spectral characteristics of nanoparticles with K+ doping concentration from 10% to 30% (Molar ratio) were investigated by fluorescence spectroscopy, and it was observed that the fluorescence intensity reached the maximum at the K+ concentration of 20%, after which the intensity weakened when the K+ content continued to increase. According to the dependence between the luminescence intensity of the sample and the laser power density and fluorescence lifetime, the intrinsic mechanism was carefully investigated. Temperature-dependent spectra of the samples were recorded in the temperature range of 315–495 K, and the maximum values of absolute sensitivity (Sa) and relative sensitivity (Sr) were measured at 0.0041 K−1 (455 K) and 0.9220%K−1 (315 K). The experimental results show that K+/Er3+/Yb3+ triple-doped NaYF4 green fluorescent nanoparticles (GFNs) have good prospects for applications in display devices, temperature sensing, and other fields. KW - K+ doped KW - Upconversion luminescence KW - Optical temperature sensing KW - Thermal coupling energy level PY - 2023 DO - https://doi.org/10.1016/j.jallcom.2022.168299 VL - 937 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-57106 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Tavernaro, Isabella A1 - Abram, Sarah-Luise A1 - Homann, Christian A1 - Scholtz, Lena A1 - Radnik, Jörg T1 - Validated and standardized measurements and quantification of surface functionalities on nanoparticles N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, opto-electronics, and information storage which improve the quality of life and European prosperity. Nanoparticle function, interaction with biological species, and environmental fate are largely determined by surface functionalities. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, and mandatory to meet increasing concerns regarding their safety. Also, industry, regulatory agencies, and policymakers need validated traceable measurement methods and reference materials. Industry, e.g., must comply with various regulations, including the chemicals´ regulation REACH (2006/1907) and cosmetic products regulation (2009/1223), depending on the use. Therefore, standardization organizations such as the European Committee for Standardization (CEN), the International Organization for Standardization (ISO), and the International Electrotechnical Commission (IEC) as well as industrial stakeholders, European Medicine Agency (EMA), and the nanosafety community responsible for guidelines for nanomaterial (NM) regulation like the Organisation for Economic Co-operation and Development (OECD) have expressed needs for standardized methodologies to measure NP surface chemical properties. Despite these needs, methodologies for determining NP surface properties, including the amount, chemical composition, and homogeneity of surface functionalities and coatings are largely non-standardized. Specifically, validated quantitative procedures for the measurement of thickness and composition of nanoparticle coatings and other surface functionalities are needed. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR) as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. The latter less costly methods are often used by SMEs, e.g., for quality control. To validate methods, establish measurement uncertainties, test reference materials, and produce reference data, international interlaboratory comparisons (ILC) on NP surface functionalization measurements are required. These needs have been addressed by us in two interlaboratory comparisons, that will be presented. In addition, the European metrology project SMURFnano will be briefly presented involving 12 partners from different National Metrology Institutes, designated institutes, and research institutes, two university groups as well as one large company and one SME producing NPs. T2 - NanoCarbon Annual Conference 2025 CY - Würzburg, Germany DA - 18.03.2025 KW - Nano KW - Particle KW - Silica KW - Quality assurance KW - Reference material KW - Surface chemistry KW - Size KW - Shape KW - Particle number concentration KW - Method KW - Optical assay KW - QNMR KW - Validation KW - Potentiometry KW - XPS PY - 2025 AN - OPUS4-62790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geißler, Daniel T1 - Preparation and characterization of reference particles for the calibration of flow cytometry for the detection of extracellular vesicles within the EMPIR project MetVes II N2 - Extracellular vesicles (EV) are cell-derived particles in body fluids, which have excellent potential as next-generation biomarkers. The exploitation of EV requires reliable measurements, which is currently very difficult, as most EV are smaller than 200 nm. At present, flow cytometry (FCM) is the most appropriate technique for EV analysis in biological samples, as FCM is readily available in many clinical laboratories and allows to identify cell-specific EV at high throughput. However, due to technical variations between different FCM instruments, EV concentration measurements are currently not well comparable between most laboratories. Therefore, EV reference materials and standardized reference methods are urgently needed to calibrate flow rate, light scattering intensity, and fluorescence intensity of FCM in the sub-micrometer size range. This requires a better matching of the optical properties of calibration beads and EV as can be realized with current polystyrene calibration beads. The EMPIR project 18HLT01 “MetVes II” aims to develop synthetic reference materials and traceable measurement methods to standardize EV measurements. The reference materials should resemble EV properties, so that calibrations are reliable and do not require a change of acquisition settings. Hence, the reference materials should contain particles with a traceable number concentration in the range of 109–1012 particles/mL to calibrate flow rate, a traceable size with discrete diameters between 50–1000 nm and a refractive index (RI) in the range of 1.37–1.42 to calibrate scattering intensity, and a traceable fluorescence intensity between 100–100,000 molecules of equivalent soluble fluorochromes (MESF). At BAM, various approaches to prepare such low-RI nanometer-sized reference materials will be studied, preliminary results of the primary characterization of these candidate reference particles will be presented, and possible applications besides FCM-based EV detection will be outlined. T2 - 29th Meeting of the German Society for Cytometry (DGfZ) CY - Berlin, Germany DA - 25.09.2019 KW - Extracellular vesicles (EV) KW - Flow cytometry KW - Reference particles KW - EMPIR project KW - 18HLT01 MetVes II PY - 2019 AN - OPUS4-50394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abram, Sarah-Luise T1 - Monodisperse iron oxide nanoparticles as reference material candidate for particle size measurements N2 - In order to utilize and rationally design materials at the nanoscale the reliable characterization of their physico-chemical properties is highly important, especially with respect to the assessment of their environmental or biological impact. Furthermore, the European Commission’s REACH Regulations require the registration of nanomaterials traded in quantities of at least 1 ton. Powders or dispersions where 50% (number distribution) of the constituent particles have sizes ≤ 100 nm in at least one dimension are defined as nanomaterials. This creates a need for industrial manufacturers and research or analytical service facilities to reliably characterize potential nanomaterials. Currently, BAM is developing reference nanoparticles, which shall expand the scarce list of worldwide available nano reference materials certified for particle size distribution and will also target other key parameters like shape, structure, porosity or functional properties. In this respect, materials like iron oxide or titanium dioxide are considered as candidates to complement the already available silica, Au, Ag, and polystyrene reference nanoparticles. The thermal decomposition of iron oleate precursors in high boiling organic solvents can provide large quantities of iron oxide nanoparticles that can be varied in size and shape.[1, 2] The presence of oleic acid or other hydrophobic ligands as capping agents ensures stable dispersion in nonpolar solvents. Such monodisperse, spherical particles were synthesized at BAM and pre-characterized by electron microscopy (TEM, SEM including the transmission mode STEM-in-SEM) and dynamic light scattering comparing cumulants analysis and frequency power spectrum. 1. REACH regulations and nanosafety concerns create a strong need for nano reference materials with diverse properties. 2. Iron oxide nanoparticles are under development as new candidate reference material at BAM. 3. Narrow particle size distribution confirmed by light scattering and electron microscopy. T2 - Nanosafety 2020 CY - Online meeting DA - 05.10.2020 KW - Iron oxide nanoparticles KW - Reference material KW - Particle size KW - Electron microscopy KW - Nanoplattform PY - 2020 AN - OPUS4-52774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - Development of multimodal methods to quantify the total and accessible number of functional groups and ligands on nanomaterials N2 - Engineered and tailored nanomaterials (NM) are of great interest in the life and material sciences, as they can be used, e.g., as drug carriers, barcodes, fluorescent sensors, and multimodal labels in bioanalytical assays and imaging applications. Their performance and safety depend not only on their particle size, size distribution, and morphology, but also on their surface chemistry, i.e., the total number of surface functional groups (FG) and the number of FG accessible for subsequent functionalization with ligands or biomolecules, which in turn determines surface charge, colloidal stability, biocompatibility, and toxicity. It also underlines the importance of validated analytical methods that provide accurate information on these application-relevant physicochemical properties with a known uncertainty. In the case of FG quantification, this calls for robust, fast, inexpensive, and reliable methods which allow for the characterization of a broad variety of NM differing in size, chemical composition, and optical properties. Methods Aiming at the development of simple, versatile, and multimodal tools for the quantification of bioanalytically relevant FG such as amine, carboxy, thiol, and aldehyde functionalities, we investigated and compared various analytical methods commonly used for FG quantification. This includes electrochemical titration methods, dye-based optical assays, and other instrumental analytical techniques such as nuclear magnetic resonance (NMR), mass spectrometry (MS), and thermal analysis methods. Results Here, we will present examples for different types of NMs and FGs including results from a currently running interlaboratory comparison (ILC) with the National Research Council of Canada (NRC) to pave the road for method standardization. Innovative aspects • Surface analysis • Performance and safety of nanomaterials • Standardization T2 - ANAKON 2023 CY - Vienna, Austria DA - 11.04.2023 KW - Engineered Nanomaterials KW - Surface group analysis KW - Optical spectroscopy KW - Quantitative NMR KW - Ligands KW - Dye KW - Particle synthesis KW - Optical Assays KW - Titration KW - Safe-by-Design KW - Nano KW - Nanosafety KW - Silica- and Polystyrene Particles PY - 2023 AN - OPUS4-59127 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Ultrasonic methods for concrete: To boldly see, what we have not seen before N2 - This keynote talk at NDE 2019 discusses specific progress in ultrasonic testing of concrete structures. A deep penetration instrument (LAUS) is introduced as well as advanced imaging methods adopted from geophysics and new approaches to ultrasonic monitoring. T2 - NDE 2019 CY - Bangalore, India DA - 05.12.2019 KW - NDT KW - Concrete KW - Ultrasound KW - Imaging KW - Monitoring PY - 2019 AN - OPUS4-50170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Andresen, Elina A1 - Resch-Genger, Ute A1 - Michaelis, Matthias A1 - Prinz, Carsten A1 - Würth, Christian T1 - Time-resolved luminescence spectroscopy for monitoring the stability and dissolution behaviour of upconverting nanocrystals with different surface coatings† N2 - We demonstrate the potential of time-resolved luminescence spectroscopy for the straightforward assessment and in situ monitoring of the stability of upconversion nanocrystals (UCNPs). Therefore, we prepared hexagonal NaYF4:Yb3+,Er3+ UCNPs with various coatings with a focus on phosphonate ligands of different valency, using different ligand exchange procedures, and studied their dissolution behaviour in phosphate-buffered saline (PBS) dispersions at 20 °C and 37 °C with various analytical methods. The amount of the released UCNPs constituting fluoride ions was quantified by potentiometry using a Fluoride ion-sensitive electrode and particle disintegration was confirmed by transmission electron microscopy studies of the differently aged UCNPs. In parallel, the luminescence features of the UCNPs were measured with special emphasis on the lifetime of the sensitizer emission to demonstrate its suitability as Screening parameter for UCNP stability and changes in particle composition. The excellent correlation between the changes in luminescence lifetime and fluoride concentration highlights the potential of our luminescence lifetime method for UCNP stability screening and thereby indirect monitoring of the release of potentially hazardous fluoride ions during uptake and dissolution in biological systems. Additionally, the developed in situ optical method was used to distinguish the dissolution dynamics of differently sized and differently coated UCNPs. KW - Fluorescence KW - Lifetime KW - Method KW - Quantification KW - Stability KW - Coating KW - Surface chemistry KW - Lanthanide KW - Fluoride KW - Electrochemistry KW - ICP-OES KW - Upconversion KW - Nano KW - Particle KW - Aging KW - Quality assurance KW - TEM PY - 2020 DO - https://doi.org/10.1039/d0nr02931a VL - 12 IS - 23 SP - 12589 EP - 12601 PB - Royal Society od Chemistry AN - OPUS4-52088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geißler, Daniel T1 - Development of reference materials for flow cytometric analysis of extracellular vesicles N2 - The aim of task 1.4 within the EMPIR project 18HLT01 MetVesII is to produce low-RI solid particles with an effective RI between 1.37 and 1.42. To prepare these low-RI solid particles, polymer cores will be coated with a silica shell. Although the bulk RI of polymers, such as polystyrene (RI = 1.59) and PMMA (RI = 1.49), and fused silica (RI = 1.46) are higher than desired, an effective RI below 1.42 will be achieved by using a mesoporous silica shell with tuneable shell-thickness and a polymer core with sufficiently small size. This approach has four advantages: (1) monodisperse commercial polymer particles and silica shell chemistry are available, (2) low-RI solid particles will have a tuneable size and RI, (3) fluorescence can be added by incorporating fluorescent dyes into the polymer cores via an established staining procedure, and (4) fluorescent dyes within the polymer cores are shielded against influences from the sample matrix, e.g. fluorescence quenching effects altering the emission properties of the reference materials. T2 - MetVesII M9 Progress Meeting CY - Budapest, Hungary DA - 12.02.2020 KW - EMPIR 18HLT01 MetVesII KW - Extracellular vesicles (EV) KW - Flow cytometry (FCM) KW - Reference materials KW - Fluorescent particles PY - 2020 AN - OPUS4-50451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Optical-Spectroscopic Studies of Soot Particles N2 - Aiming at the development of a non-destructive optical measurement methods for the characterization of nano-sized airborne particulate pollutants we performed fluorescence spectroscopic investigations of their relevant emission properties. Here, we present first results from studies of soot particles from synthetic aerosols deposited on PTFE membranes. T2 - EMPIR 18HLT02 AeroTox M9 meeting CY - London, UK DA - 29.01.2020 KW - Aaerosol particles KW - Airborne particulate pollutants KW - Fluorescence spectroscopy PY - 2020 AN - OPUS4-50511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radunz, Sebastian A1 - Wedepohl, S. A1 - Röhr, Mathilde A1 - Calderón, M. A1 - Tschiche, H. R. A1 - Resch-Genger, Ute T1 - pH-Activatable Singlet Oxygen-Generating Boron-dipyrromethenes N2 - Singlet oxygen can severely damage biological tissue, which is exploited in photodynamic therapy (PDT). In PDT, the effective range is limited by the distribution of the photosensitizer (PS) and the illuminated area. However, no distinction is made between healthy and pathological tissue, which can cause undesired damage. This encouraged us to exploit the more acidic pH of cancerous tissue and design pH-controllable singlet oxygen-generating boron-dipyrromethene (BODIPY) dyes. A pH sensitivity of the dyes is achieved by the introduction of an electronically decoupled, photoinduced electron transfer (PET)-capable subunit in meso-position of the BODIPY core. To favor triplet-state formation as required for singlet Oxygen generation, iodine substituents were introduced at the chromophore core. The resulting pH-controlled singlet oxygen-generating dyes with pKa values in the physiological range were subsequently assessed regarding their potential as pH-controlled PS for PDT. Using HeLa cells, we could successfully demonstrate markedly different pH-dependent cytotoxicities upon illumination. KW - Fluorescence KW - Sensor KW - Switch KW - pH KW - Singlet oxygen KW - PDT KW - Cell KW - BODIPY KW - Dye KW - Probe KW - Synthesis PY - 2019 DO - https://doi.org/10.1021/acs.jmedchem.9b01873 VL - 63 IS - 4 SP - 1699 EP - 1708 PB - ACS Publications AN - OPUS4-50554 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radunz, Sebastian A1 - Kraus, Werner A1 - Bischoff, F. A. A1 - Emmerling, Franziska A1 - Resch-Genger, Ute A1 - Tschiche, Harald T1 - Temperature- and Structure-Dependent Optical Properties and Photophysics of BODIPY Dyes N2 - We report on the temperature- and structural-dependent optical properties and photophysics of a set of boron dipyrromethene (BODIPY) dyes with different substitution patterns of their meso-aryl subunit. Single-crystal Xray diffraction analysis of the compounds enabled a classification of the dyes into a sterically hindered and a unhindered group. The steric hindrance refers to a blocked rotational motion of the aryl subunit around the bond connecting this moiety to the meso-position of the BODIPY core. The energy barriers related to this rotation were simulated by DFT calculations. As follows from the relatively low rotational barrier calculated to about 17 kcal/mol, a free rotation is only possible for sterically unhindered compounds. Rotational barriers of more than 40 kcal/mol determined for the sterically hindered compounds suggest an effective freezing of the rotational motion in These molecules. With the aid of temperature-dependent spectroscopic measurements, we could show that the ability to rotate directly affects the optical properties of our set of BODIPY dyes. This accounts for the strong temperature dependence of the fluorescence of the sterically unhindered compounds which show a drastic decrease in fluorescence quantum yield and a significant shortening in fluorescence lifetime upon heating. The optical properties of the sterically hindered compounds, however, are barely affected by temperature. Our results suggest a nonradiative deactivation of the first excited singlet state of the sterically unhindered compounds caused by a conical intersection of the potential energy surfaces of the Ground and first excited state which is accessible by rotation of the meso-subunit. This is in good agreement with previously reported deactivation mechanisms. In addition, our results suggest the presence of a second nonradiative depopulation pathway of the first excited singlet state which is particularly relevant for the sterically hindered compounds. KW - Fluorescence KW - Sensor KW - Switch KW - pH KW - BODIPY KW - Dye KW - Probe KW - Synthesis KW - Photophysics KW - Mechanism PY - 2020 DO - https://doi.org/10.1021/acs.jpca.9b11859 SN - 1089-5639 VL - 124 IS - 9 SP - 1787 EP - 1797 PB - American Chemical Society AN - OPUS4-50639 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Qualitätssicherung von Verschlussbauwerken in Endlagern mit Ultraschall N2 - Zur Versiegelung von Endlagern für radioaktive oder chemische Abfälle in ehemaligen Salzbergwerken werden Verschlussbauwerke aus Salzbeton auf ihre Eignung geprüft. Seit einigen Jahren werden durch die Bundesgesellschaft Endlagerung (BGE) und der Bundesanstalt für Materialforschung und -prüfung (BAM) an Versuchsbauwerken Erfahrungen mit der Ultraschalltechnik zur Qualitätssicherung unter Tage gesammelt. Hierbei kommen sowohl kommerzielle und experimentelle Geräte zur Echoprüfung als auch eigens entwickelte Bohrlochsonden zum Einsatz. Alle Geräte basieren auf niederfrequenten s-Wellen-Punktkontaktprüfköpfen (25 kHz– 50 kHz), die in unterschiedlichen Arrays kombiniert werden. In mehreren Versuchsreihen gelang es, unverfüllte und teilverfüllte Risse über mehrere Meter zu verfolgen und in ihrer Lage abzubilden. Technische Einbauten konnten bis in ca. 8 m Tiefe im Bauwerk detektiert werden. Mit Hilfe aus der Geophysik adaptierte Abbildungsverfahren gelang es, einige bisher nicht detektierbare Features sichtbar zu machen. Die Ergebnisse dienen sowohl der Analyse des Versuchsbauwerks als auch der Entwicklung eines Qualitätssicherungssystems für zukünftige reale Verschlussbauwerke. T2 - DACH-Jahrestagung 2019 CY - Friedrichshafen, Germany DA - 27.05.2019 KW - Ultraschall KW - Verschlussbauwerk KW - Endlager KW - Salzbeton PY - 2019 AN - OPUS4-50568 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Zengchao A1 - Nirmalananthan-Budau, Nithiya A1 - Resch-Genger, Ute A1 - Panne, Ulrich A1 - Weidner, Steffen T1 - Separation of polystyrene nanoparticles bearing different carboxyl group densities and functional groups quantification with capillary electrophoresis and asymmetrical flow field flow fractionation N2 - Two sets of polystyrene nanoparticles (PSNPs) with comparable core sizes but different carboxyl group densities were made and separated using asymmetric flow field flow fractionation (AF4), capillary electrophoresis (CE), and the off-line hyphenation of both methods. Our results revealed the significant potential of two-dimensional off-line AF4-CE hyphenation to improve the separation and demonstrated for the first time, the applicability of CE to determine the functional group density of nanoparticles (NPs). Compared to the result acquired with conductometric titration, the result obtained with synthesized 100 nm sized PSNPs revealed only a slight deviation of 1.7%. Commercial 100 nm sized PSNPs yielded a deviation of 4.6 %. For 60 nm sized PSNPs, a larger deviation of 10.6 % between both methods was observed, which is attributed to the lower separation resolution. KW - Nanoparticle KW - A4F KW - Capillary electrophoresis KW - Carboxyl group PY - 2020 DO - https://doi.org/10.1016/j.chroma.2020.461392 VL - 1626 SP - 461392 PB - Elsevier B.V. AN - OPUS4-51080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tan, M. A1 - Monks, Melissa-Jane A1 - Huang, D. A1 - Meng, Y. A1 - Chen, X. A1 - Zhou, Y A1 - Lom, S.-F. A1 - Würth, Christian A1 - Resch-Genger, Ute A1 - Chen, G. T1 - Efficient sub-15 nm cubic-phase core/Shell upconversion nanoparticles as reporters for ensemble and single particle studies† N2 - Single particle imaging of upconversion nanoparticles (UCNPs) has typically been realized using hexagonal (β) phase lanthanide-doped sodium yttrium fluoride (NaYF4) materials, the upconversion luminescence (UCL) of which saturates at power densities (P) of several hundred W cm−2 under 980 nm nearinfrared (NIR) excitation. Cubic (α) phase UCNPs have been mostly neglected because of their commonly observed lower UCL efficiency at comparable P in ensemble level studies. Here, we describe a set of sub-15 nm ytterbium-enriched α-NaYbF4:Er3+@CaF2 core/shell UCNPs doped with varying Er3+ concentrations (5–25%), studied over a wide P range of ∼8–105 W cm−2, which emit intense UCL even at a low P of 10 W cm−2 and also saturate at relatively low P. The highest upconversion quantum yield (ΦUC) and the highest particle brightness were obtained for an Er3+ dopant concentration of 12%, reaching the highest ΦUC of 0.77% at a saturation power density (Psat) of 110 W cm−2. These 12%Er3+-doped core/shell UCNPs were also the brightest UCNPs among this series under microscopic conditions at high P of ∼102–105 W cm−2 as demonstrated by imaging studies at the single particle level. Our results underline the potential applicability of the described sub-15 nm cubic-phase core/shell UCNPs for ensemble- and single particle- level bioimaging. KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - Surface chemistry KW - Single particle KW - Brightness PY - 2020 DO - https://doi.org/10.1039/d0nr02172e VL - 12 IS - 19 SP - 10592 EP - 10599 PB - Nanoscale AN - OPUS4-50908 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ramirez Caro, Alejandra A1 - Pauli, Jutta A1 - Mota, Berta A1 - Simon, Sebastian A1 - Schmidt, Wolfram A1 - Resch-Genger, Ute T1 - C⁠3A passivation with gypsum and hemihydrate monitored by optical spectroscopy N2 - Tricalcium aluminate (C⁠3A) is found with less than 10% wt. of the total composition; however, during hydration, C⁠3A plays an important role in the early hydration of cement in the presence of gypsum as a set retarder. The aim of this investigation is to assess the suitability of optical spectroscopy and a dye-based optical probe to monitor early hydration of C⁠3A in the presence of gypsum and hemihydrate. Optical evaluation was performed using steady-state fluorescence and diffuses reflectance spectroscopy (UV-VisDR). Phase characterization during hydration was done with in-situ X-ray diffraction. UV-VisDR with a cyanine dye probe was used to monitor the formation of metastable phases and was employed together with fluorescence spectroscopy, to follow the Aggregation and disaggregation of the dye during hydration. In conclusion, for the first time, a cyanine dye was identified as a feasible and stable probe to monitor C⁠3A hydration changes in the presence of calcium sulfate. KW - Dye KW - Photoluminescence KW - Fluorescence KW - Reflection spectroscopy KW - Cement KW - Hydration KW - Method development PY - 2020 DO - https://doi.org/10.1016/j.cemconres.2020.106082 VL - 133 SP - 106082 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-50952 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhao, J. A1 - Hu, Y. A1 - wei Lin, S. A1 - Resch-Genger, Ute A1 - Zhang, R. A1 - Wen, J. A1 - Kong, X. A1 - Qin, A. A1 - Ou, J. T1 - Enhanced luminescence intensity of near-infraredsensitized sensitized upconversion nanoparticles via Ca²+ doping for a nitric oxide release platform N2 - Light-induced NO release based on exogenous NO donors has attracted substantial attention in clinical applications; the induction light source usually converts near-infrared light to blue or ultraviolet light. However, the low efficiency of near-infrared light-assisted chemical light energy conversion remains a challenge, especially for NaYF4:Yb3+/Tm3+ photoconverting near-infrared light to ultraviolet (UV) and blue light. In this paper, a luminescence-enhanced strategy is reported by doping Ca2+ into NaYF4:Yb3+/Tm3+ and coating it with NaGdF4 through a two-step solvothermal method. Then, UCNPs modified with methyl-b-cyclodextrin (M-b-CD) are loaded on a ruthenium nitrosyl complex [(3)Ru(NO)(Cl)] as nitric oxide release-molecules (NORMs). X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS) data demonstrated that Ca2+ was successfully doped into NaYF4:Yb3+/Tm3+ nanoparticles as the core, and a pure hexagonal phase, NaYF4, was obtained from the doping of Ca2+. TEM revealed that the crystallinity was significantly improved after Ca2+ doping, and the core–shell structure was successfully synthesized, with NaGdF4 directionally grown on the NaYF4:Ca/Yb/Tm core. Fluorescence tests showed that, especially in the ultraviolet and blue light excitation wavelength regions, the UC emission intensity of the Ca-doped NaYF4:Yb3+/Tm3+@NaGdF4 core–shell UCNPs increased by 302.95 times vs. NaYF4:Yb3+/Tm3+ UCNPs. Finally, the release of NO was tested by the Griess method. Under 980 nm irradiation, the cell viability distinctly decreased with increasing UCNPs@M-b-CD-NORMs concentration. This study Shows that NORM release of NO is triggered by enhanced up-converted UV and blue light, which can be used for the development of UV photo-sensitive drugs. KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - Surface chemistry KW - Single particle KW - Brightness KW - NIR KW - PDT PY - 2020 DO - https://doi.org/10.1039/d0tb00088d VL - 8 IS - 30 SP - 6481 EP - 6489 PB - Journal of Materials Chemistry B AN - OPUS4-51262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Theiner, S. A1 - Löhr, Konrad A1 - Köllensperger, G. A1 - Müller, L. A1 - Jakubowski, Norbert T1 - Single-cell analysis by use of ICP-MS N2 - This tutorial review article is highlighting the fundamentals, instrumentation, and most recent trends of single-cell analysis by use of inductively coupled plasma-mass spectrometry (ICP-MS). It is shown that metals and hetero-elements being intrinsically present in cells, taken up by cells (for instance engineered metallic nanoparticles) or binding to a cell can be detected qualitatively by existing ICP-MS Technologies on a single cell level. Adding a quantitative dimension to single-cell analysis by (laser ablation-) ICP-MS requires dedicated calibration and validation strategies, which are currently being established and are being critically discussed. In a tutorial part, the ICP-MS instruments, the measurement conditions, and the sample introduction and preparation techniques are introduced. The application section focuses on the state-of-the-art of single-cell analysis in suspension, using laser ablation or (imaging) mass cytometry. Finally, future trends are critically assessed. KW - Cell KW - ICP KW - ICP-MS KW - Laser ablation PY - 2020 DO - https://doi.org/10.1039/d0ja00194e SN - 0267-9477 VL - 35 IS - 9 SP - 1784 EP - 1813 PB - The Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-51448 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Perspective of BAM on Advanced Materials N2 - A brief perspective of BAM on advanced materials is presented including examples for nanomaterials and other systems presenting advanced materials with special emphasis on characterization methods used in different division of BAM for the determination of functional or safety parameters of such materials. In this respect, also ongoing activities of the capacity building project nanoplatform of BAM aiming at the development of nanometer-sized reference materials are briefly summarized. T2 - BfR Workshop zu Advanced Materials CY - Online meeting DA - 04.11.2020 KW - Quality assurance KW - Risk assessment KW - Safety KW - Core/shell particle KW - Characterization KW - Measurement uncertainty KW - Method KW - Nano particle PY - 2020 AN - OPUS4-51620 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geißler, Daniel T1 - Standardisation of concentration measurements of extracellular vesicles for medical diagnoses N2 - Extracellular vesicles (EVs) are cell-derived particles in body fluids, which have excellent potential as next generation biomarkers for the early diagnosis of common diseases, such as cancer and thrombosis. This project aims to tap into the clinical potential of EVs by developing traceable measurements of number concentration, size distribution, refractive index (RI) and fluorescence intensity of cell-specific EVs in human blood and urine. To realise our aims, we will develop synthetic reference materials with physical properties resembling EVs (WP1), instrumentation and procedures to standardise EV measurements in clinical laboratories (WP2), and ready-to-use biological test samples (WP3). These will then be evaluated in an inter-laboratory comparison study across a range (>20) of standard flow cytometers in clinical labs (WP4). T2 - MetVesII M18 Interim Meeting CY - Berlin, Germany DA - 20.10.2020 KW - EMPIR 18HLT01 MetVesII KW - Extracellular vesicles (EV) KW - Flow cytometry (FCM) KW - Reference materials KW - Fluorescent particles KW - Integrating sphere spectroscopy PY - 2020 AN - OPUS4-51653 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - López de Ipina, J.-M. A1 - Arevalillo, A. A1 - Martín, A. A1 - Caillard, B. A1 - Marcoulaki, E. A1 - Aguerre- Charol, O. A1 - van Duuren-Stuurman, B. A1 - Hodoroaba, Vasile-Dan A1 - Viitanen, A.-K. A1 - Witters, H. A1 - Vercauteren, S. A1 - Persson, K. A1 - Bard, D. A1 - Evans, G. A1 - Jensen, K.A. A1 - Himly, M. A1 - Scalbi, S. A1 - Papin, A. A1 - Le Bihan, O. A1 - Kanerva, T. A1 - Tirez, K. A1 - Frijns, E. A1 - Niga, P. A1 - Eleftheriadis, K. A1 - Travlos, A. A1 - Geppert, M. A1 - Himly, M. A1 - Radnik, Jörg A1 - Kuchenbecker, Petra A1 - Resch-Genger, Ute A1 - Fraboulet, I. A1 - Bressot, C. A1 - Rissler, J. A1 - Gaucher, R. A1 - Binotto, G. A1 - Krietsch, Arne A1 - Braun, A. A1 - Abenet, S. A1 - Catalan, J. A1 - Verstraelen, S. A1 - Manier, N. A1 - Manzo, S. A1 - Fransman, S. A1 - Queron, J. A1 - Charpentier, D. A1 - Taxell, D. A1 - Säämänen, A. A1 - Brignon, J.-M. A1 - Jovanovic, A. A1 - Bisson, M A1 - Neofytou, P. T1 - EC4Safenano - Catalogue of Services N2 - The publicly available document encapsulates the first version of the Catalogue of Services of the future EC4Safenano Centre (CoS 2019). The CoS 2019 is structured in 12 Service Categories and 27 Service Topics, for each of the 12 categories considered. This architecture configures a 12 x 27 matrix that allows ordering the potential EC4Safenano offer in 324 types of services/groups of services. Each type of service/group of services is described, in a simple and friendly way, by means of a specific service sheet: the EC4Safenano - Service Data Sheet (EC4-SDS). These EC4-SDSs allow structuring and summarizing the information of each service, providing the customer with a concise view of characteristics of the service and also the contact details with the service provider. The CoS 2019 deploys a map of services consisting of a set of 100 EC4-SDSs, covering 7 of the 12 Service Categories and 17 of the 27 Service Topics. The harmonization of services is visualized as a future necessary step in EC4Safenano, in order to strengthen the offer and provide added value to customers with a growing offer of harmonized services in future versions of the CoS. The information contained in this document is structured in 3 main sections, as follows: • Catalogue structure. This section describes in short the main characteristics of the CoS 2019. • Catalogue content. This section represents the core part of the document and encapsulates the set of 100 SDSs displaying the offer proposed by the CoS 2019. • Online Catalogue. This section describes the resources implemented by EC4Safenano to facilitate the on-line consultation of the CoS 2019 by customers and other interested parties. KW - Nano-safety KW - Analytical services KW - Nanomaterials KW - Catalogue of services KW - EC4SafeNano KW - European Centre PY - 2021 UR - https://ec4safenano.eu-vri.eu/Public/Guidance SP - 1 EP - 72 PB - EU-VRi – European Virtual Institute for Integrated Risk Management CY - Stuttgart, Germany AN - OPUS4-52943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiggenhauser, Herbert A1 - Niederleithinger, Ernst A1 - Milmann, Boris T1 - Zerstörungsfreie Ultraschallprüfung dicker und hochbewehrter Betonbauteile T1 - Nondestructive testing of thick and highly reinforced concrete structures with ultrasound N2 - Ein Ultraschallsystem mit großer Apertur, genannt LAUS – Large Aperture UltraSound, wird vorgestellt und die technischen Eigenschaften erläutert. Es besteht aus zwölf Prüfköpfen, die beliebig auf Betonoberflächen mit Unterdruck befestigt und jeweils als Sender oder Empfänger genutzt werden. Alle möglichen Kombinationen ergeben 132 Einzelmessungen, die zur Rekonstruktion des durchschallten Volumens genutzt werden. Das System wurde an zwei Bauwerken erfolgreich erprobt. Die Dicke einer sehr stark bewehrten Fundamentplatte eines Fallturms wurde bestimmt. Die Messungen erfolgten in einem Raster auf einer Fläche von 2,0 × 1,8 m2 und die Rückseite konnte eindeutig abgebildet werden. Weitere Anzeigen aus dem Inneren der Platte zeigen das Potenzial des Systems. An einem Brückenbauwerk wurden indirekt Verdichtungsmängel lokalisiert. Dazu wurden mit dem LAUS-System die im Brückenträger verlaufenden Spannkanäle durch fast 2 m Beton abgebildet. N2 - An ultrasound system with a large aperture, called LAUS - Large Aperture UltraSound, is presented and the technical characteristics are explained. It consists of twelve sensor units which can be attached independently on concrete surfaces with vacuum and which are used as transmitters or receivers respectively. All possible combinations result in 132 individual measurements which are used to reconstruct the insonificated volume. The system has been successfully tested on two structures. The thickness of a very heavily reinforced foundation slab of a drop tower was determined. The measurements were carried out in a grid on a surface of 2.0 x 1.8 m(2) and the back side could be clearly imaged. Further indications from inside the foundation show the potential of the system. Voids in concrete were indirectly located in a bridge structure. For this purpose, the LAUS system was used to image the tendon ducts running in the bridge beam through almost 2 m of concrete. KW - Ultraschall KW - Beton KW - Brücke KW - Fundament KW - LAUS PY - 2017 DO - https://doi.org/10.1002/bate.201700040 SN - 0932-8351 VL - 94 IS - 10 SP - 682 EP - 688 PB - Ernst & Sohn CY - Berlin AN - OPUS4-42614 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Algernon, D. A1 - Arndt, R. A1 - Ebsen, B. A1 - Feistkorn, S. A1 - Friese, M. A1 - Große, C. A1 - Kathage, S. A1 - Keßler, S. A1 - Kurz, J. A1 - Küttenbaum, Stefan A1 - Lohse, C. A1 - Maack, Stefan A1 - Niederleithinger, Ernst A1 - Schickert, M. A1 - Schröder, G. A1 - Taffe, A. A1 - Walther, A. A1 - Wilcke, M. A1 - Wolf, J. A1 - Wöstmann, Jens T1 - Leitfaden zur Erstellung von Prüfanweisungen für die Zerstörungsfreie Prüfung im Bauwesen (ZfP Bau) N2 - Der vorliegende Leitfaden dient zur Unterstützung der Entwicklung und Umsetzung von Prüfanweisungen für ZfP-Verfahren im Bauwesen. Er gibt einen Überblick über Verwendungszweck, Erstellung und Inhalte von Prüfanweisungen unter Berücksichtigung einheitlicher Standardisierungsziele. KW - Prüfanweisung KW - Beton KW - Leitfaden PY - 2022 SN - 978-3-947971-23-7 VL - Richtlinie B-LF 01 SP - 1 EP - 9 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin ET - Ausgabe April 2022 AN - OPUS4-54985 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Der Blick in die Brücke N2 - Populärwissenschaftlicher Vortrag zu jüngeren Entwicklungen beim Ultraschall für das Bauwesen. T2 - Berliner Industriegespräch der DPG CY - Berlin, Germany DA - 7.3.2018 KW - Beton KW - Ultraschall KW - Brücke PY - 2018 AN - OPUS4-44574 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Felbeck, T. A1 - Lezhnina, M.M. A1 - Resch-Genger, Ute A1 - Kynast, U.H. T1 - Red emissive nanoclay hybrids in transparent aqueous dispersion-towards optical applications in biophotonics N2 - Hydrophobic guest molecules like organic dyes and metal–ion complexes can be introduced into aqueous media via adsorption onto inorganic nanoclay host materials such as nm-sized laponite. Dispersions of these organic–inorganic hybrid materials show several advantageous properties like minimum light scattering due to their small size in the nanometer regime, ease of modification, low cost, low toxicity, and long-term stability, making them perfect candidates as signaling units and optically active materials in photonics and biotechnology. In this study, we summarize first findings on the easy-to-make, but chemically and optically fairly complex behavior of nanoclay hybrids for biotechnological applications. The latter includes the preparation of nanomaterials, which are colloidally stable in buffers and in the presence of biomolecules like proteins, and methods to control their surface chemistry. For this purpose, we used two red emitting fluorophores, the small organic dye Nile Red and the rare earth complex Eu(ttfa)3(topo)2, and evaluated the interaction of the red nanoclay hybrids with two model proteins, bovine serum albumin and β-lactoglobulin. We were able to monitor the formation of the protein corona around these hybrids using absorption and luminescence spectroscopy. KW - Nile Red KW - Europium complex KW - Protein corona KW - Nanoclay hybrids KW - Polarity probe PY - 2016 DO - https://doi.org/10.1016/j.jlumin.2014.11.039 SN - 0022-2313 SN - 1872-7883 VL - 169 SP - 728 EP - 732 PB - North-Holland Publ. Co. CY - Amsterdam AN - OPUS4-33817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brömme, T. A1 - Schmitz, C. A1 - Oprych, D. A1 - Wenda, A. A1 - Strehmel, V. A1 - Grabolle, Markus A1 - Resch-Genger, Ute A1 - Ernst, S. A1 - Reiner, K. A1 - Keil, D. A1 - Lüs, P. A1 - Baumann, H. A1 - Strehmel, B. T1 - Digital imaging of lithographic materials by radical photopolymerization and photonic baking with NIR diode lasers N2 - Photo-initiated cross-linking of multifunctional acrylic esters in polymeric binders was investigated based on digital imaging using the Computer-to-Plate (CtP) technology applying laser exposure in the near-infrared (NIR). Generation of initiating radicals occurs by electron transfer from the excited state of the NIR-sensitizer to the radical generator, an onium salt. Iodonium salts derived from several borates and those with the bis(trifluoromethylsulfonyl)imide anion resulted in lithographic materials with high sensitivity. Photo-induced electron transfer plays a major function to generate initiating radicals by a sensitized mechanism but thermal events also influence sensitivity of the coating. Internal conversion was the major deactivation pathway while a certain fraction of NIR-dye fluorescence was also available. A line shape focused laser system with emission in the NIR was successfully used to bake the materials. KW - Iodonium KW - Near-infrared laser KW - Photonic baking KW - Photophysics KW - Photopolymer PY - 2016 DO - https://doi.org/10.1002/ceat.201500453 SN - 0930-7516 SN - 1521-4125 VL - 39 IS - 1 SP - 13 EP - 25 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-35303 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Progress in using geophysical methods in foundation quality assurance and inspection N2 - Modern geophysical methods might be either directly applied to foundations or integrated into existing testing schemes to assist in quality assurance and inspections. This paper gives an overview on available ideas and some more detailed examples from the author `s work including: - Vibrator technologies to improve pile integrity testing. - Ideas from vertical seismic profiling used in multichannel pile inspection - Cross- and downhole seismics to check the diameter of jet grouting columns - Improving the parallel seismic methods for precise length measurement of piles and foundation walls - Seismic migration methods to improve ultrasonic imaging of foundation slabs - Seismological tools to monitor subtle changes in concrete constructions The author strongly believes that the cooperation between geophysics and civil engineering, which is obviously becoming stronger and stronger, will lead to a large number of innovative approaches for investigations tasks currently still unresolved. A lot of challenges and chances for science and technology are right here. T2 - SAGEEP CY - Denver, CO, USA DA - 20.03.2016 KW - Non-destructive testing KW - Piles KW - Foundations KW - Slabs KW - Parallel seismic KW - Vibrator KW - Integrity PY - 2016 SP - paper 45, 1 EP - 7 AN - OPUS4-35704 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martynenko, Irina V. A1 - Kusic, Dragana A1 - Weigert, Florian A1 - Stafford, S. A1 - Donnelly, F. C. A1 - Evstigneev, R. A1 - Gromova, Y. A1 - Baranov, A. V. A1 - Rühl, Bastian A1 - Kunte, Hans-Jörg A1 - Gun'ko, Y. K. A1 - Resch-Genger, Ute T1 - Magneto-fluorescent microbeads for bacteria detection constructed from superparamagnetic Fe3O4 nanoparticles and AIS/ZnS quantum dots N2 - The efficient and sensitive detection of pathogenic microorganisms in aqueous environments, such as water used in medical applications, drinking water, and cooling water of industrial plants, requires simple and fast methods suitable for multiplexed detection such as flow cytometry (FCM) with optically encoded carrier beads. For this purpose, we combine fluorescent Cd-free Ag−In−S ternary quantum dots (t-QDs) with fluorescence Lifetimes (LTs) of several hundred nanoseconds and superparamagnetic Fe3O4 nanoparticles (SPIONs) with mesoporous CaCO3 microbeads to a magneto-fluorescent bead platform that can be surface-functionalized with bioligands, such as antibodies. This inorganic bead platform enables immuno-magnetic separation, target enrichment, and target quantification with optical readout. The beads can be detected with steady-state and time-resolved fluorescence microscopy and flow cytometry (FCM). Moreover, they are suited for readout by time gated emission. In the following, the preparation of these magneto-fluorescent CaCO3 beads, their spectroscopic and analytic characterization, and their conjugation with bacteria-specific antibodies are presented as well as proof-of-concept measurements with Legionella pneumophila including cell cultivation and plating experiments for bacteria quantification. Additionally, the possibility to discriminate between the long-lived emission of the LT-encoded capture and carrier CaCO3 beads and the short-lived Emission of the dye-stained bacteria with time-resolved fluorescence techniques and single wavelength excitation is demonstrated. KW - Fluorescence KW - method KW - lifetime KW - quantum yield KW - particle KW - magnetic nanoparticle KW - immunoseparation KW - flow cytometry KW - fluorescence microscopy KW - nanoparticle KW - quantum dot KW - AIS QD KW - fluorescence KW - bacteria detection KW - bacteria KW - antibody KW - Legionella KW - screening tes KW - FLIM PY - 2019 DO - https://doi.org/10.1021/acs.analchem.9b01812 SN - 0003-2700 SN - 1520-6882 VL - 91 SP - 12661 EP - 12669 PB - American Chemical Society CY - Washington, DC AN - OPUS4-50117 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Maiwald, Michael T1 - Analytical Sciences an der BAM N2 - Die Bundesanstalt für Materialforschung und -prüfung (BAM) ist eine wissenschaftlich technische Bundesoberbehörde im Geschäftsbereich des Bundesministeriums für Wirtschaft und Energie (BMWi), die über einen gesetzlichen Auftrag für die Sicherheit in Technik und Chemie verfügt und auf nahezu 150 Jahre zurückblicken kann. Vor diesem Hintergrund forscht, entwickelt, und prüft die BAM in den fünf Themenfeldern Energie, Infrastruktur, Umwelt, Material und Analytical Sciences mit einer unikalen Vielfalt an analytischen Methoden. KW - BAM KW - Analytik KW - Analytical Sciences PY - 2016 SN - 0939-0065 IS - 2 SP - 6 EP - 8 AN - OPUS4-36508 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Levee inspection - geophysics between science, standards, reliability and budgets N2 - Numerous case histories show evidence that geophysical methods are valuable tools for levee inspection and monitoring. National and international standards and recommendations recommend the use of geophysics for a variety of tasks. However, in some cases reported have been flaws missed or false indications given. Due to the larger variety in type, size and construction of levees and the even larger variety of potential tasks and targets the success of geophysical surveys still pretty much depends on the available budget and the experience and capabilities of the clients and contractors involved. It is strongly recommended that all relevant parties agree on the detailed objectives of the survey, required accuracy and reliability of the results and any follow up measures. For the most common tasks more research and practical work using techniques as POD (probability of detection), which are well established in other fields of non-destructive testing, would be of benefit. T2 - SAGEEP 2016 CY - Denver, CO, USA DA - 20.03.2016 KW - Levee KW - Inspection KW - Geophysics PY - 2016 AN - OPUS4-35707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Coda wave interferometry used for monitoring of concrete constructions N2 - Concrete is known to be a very useful, flexible and durable construction material. However, due to excess load, fatigue, chemical processes, freeze-thaw or reinforcement corrosion concrete may suffer from degradation. If detected too late, repair is difficult and expensive. The propagation of ultrasonic waves is influenced by changes in the properties and structure of the material, including, but not limited to, stress, temperature, moisture content and microcracking. Ultrasonic velocieties thus may serve as indicators for structural health. Traditional ultrasonic methods as transmission time of flight measurements are used since decades, but are not sensible enough to show subtle changes. Coda Wave Interferometry (CWI), originally developed in seismology to detect stress changes in the earth's crust uses the information in the late part of ultrasonic signals originating from multiple reflections and scattering. Since a few years it is used by several researchers for lab experiments on concrete. Meanwhile specialized sensors to be embedded in concrete have been developed. We have conducted several lab and a few field experiments, which will be reported here. The capabilities and limitations of CWI are summarized. T2 - Jahrestagung der DGG CY - Münster DA - 14.03.2016 KW - Coda wave interferometry KW - Concrete KW - Monitoring KW - Ultrasound PY - 2016 AN - OPUS4-35710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Bio- and immuno-imaging by use of laser ablation ICP-MS N2 - Imuno-histochemical staining (IHC) of cancer biomarker on tissue sections is one of the most important analytical techniques for cancer diagnosis although standardization and quality management is tedious and differ significantly from clinic to clinic. Combining established IHC staining strategies with modern quantitative methods would increase it`s potential. We used element mass spectrometry (ICP-MS) and a new ink-jet printed internal standardization approach in combination with IHC staining. The printing strategy was utilized to improve elemental image resolution and reproducibility of paraffin embedded breast cancer tissue sections in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) after conventional IHC staining as a model system to investigate the new capabilities of this technique. T2 - European Winter Conference on Plasma Spectrochemistry 2016 CY - Tucson, Arizona, USA DA - 10.01.2016 KW - Laser Ablation KW - ICP-MS KW - Bio-Imaging PY - 2016 AN - OPUS4-36492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine A1 - Niederleithinger, Ernst T1 - ERT Measurements on tailings dams using multi-channel spectral induced polarization (SIP) N2 - The often poor construction and low maintenance level of tailings dams has caused serious accidents. The EC funded Project TAILSAFE is aimed at the non-destructive assessment of tailings facilities for stabilization analyses and the development of better management methods. The focus of geophysical field studies was on the discrimination of different layering and construction steps as well as the determination of the spatial (relative) water content in the dams. SIP measurements at three tailings facilities different in their geological backgrounds, composition and age have been conducted. T2 - 11th European Meeting of Environmental and Engineering Geophysics CY - Palermo, Italy DA - 04.09.2005 KW - TAILSAFE KW - Non-destructive assessment KW - Stabilization analyses PY - 2005 AN - OPUS4-36560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Weba, Luciana A1 - Silbernagl, Dorothee A1 - Mota Gassó, Berta A1 - Höhne, Patrick A1 - Sturm, Heinz A1 - Pauli, Jutta A1 - Resch-Genger, Ute A1 - Steinborn, Gabriele ED - Khayat, Kamal Henry T1 - Influences of nano effects on the flow phenomena of self-compacting concrete N2 - Chemical admixtures like superplasticisers or stabilising agents are of ever increasing importance for modern concrete technology. They liberate the workability of concrete from its dependency on water content, and thus, open the gate towards innovative and future oriented concrete technologies such as selfcompacting concrete. Meanwhile admixtures have become common practice in concrete technology, but the understanding of these highly complex polymers in the entire concrete system lags far behind their application. Due to its complex time-dependent, multi-phase and multi-scale behaviour, flowable concrete systems are highly complicated and cannot be described comprehensively by simple models. It is therefore extremely challenging to identify the relevant parameters that predominantly control flow phenomena on different size scales, since these may occur on any scale between the nano scale (e.g. superplasticizer adsorption) and macro scale (e.g. grading of the aggregates). The present study discusses fundamental mechanisms at the interface between particle or hydrate surfaces and the fluid phase at a very early stage of concrete formation, and links these effects to macroscopic flow phenomena. Methods are discussed that appear promising interdisciplinary tools for enhancement of the understanding of the relevant interactions that are responsible for the macroscopic flow of flowable concrete. T2 - 8th International RILEM Symposium on Self-Compacting Concrete CY - Washington, D.C., USA DA - 15.05.2016 KW - Adsorption KW - Analytics KW - Hydration KW - Polycarboxylate ether KW - Rheology PY - 2016 SP - 245 EP - 254 AN - OPUS4-36882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Studying cellular uptake and processing of nanoparticles by LA-ICP-MS N2 - In recent years, elemental imaging of biological samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining in importance. Recent improvements regarding spatial resolution (down to 1 µm) and washout time make LA-ICP-MS particularly interesting for single cell analysis. Many current nanomaterials can serve as contrast agents in cellular or tissue imaging, drug delivery vehicles or therapeutics, whereas others can cause toxic effects. In order to evaluate nano-bio interactions, the number of nanoparticles (NPs) inside cells as well as their localisation within cellular substructures is of particular interest. LA-ICP-MS was used to study the NP pathway from uptake, via intracellular processing up to cell division. Fibroblast cells were incubated with different metallic NPs under varying experimental conditions. For LA analysis the cells were fixed with formaldehyde and dried. Our results show that LA-ICP-MS is able to localise NP aggregates within cellular substructures. The NPs accumulate in the perinuclear region in the course of intracellular processing, e.g. multivesicular fusion and endosomal maturation, but do not enter the nucleus [1, 2]. A strong dependence of NP uptake on concentration and incubation time was found. Additionally, the number of NPs internalized by individual cells was determined and variations within the cell population became visible. A new laser ablation system providing a short washout time (50 ms) together with small spot sizes (< 4 µm) and high repetition rates allows high spatial resolution applications. First results of cell imaging will be shown. The findings demonstrate the potential of LA-ICP-MS providing insight into NP uptake and intracellular distribution dependent on experimental parameters. T2 - 13th European Workshop on Laser Ablation CY - Ljubljana, Slovenia DA - 12.07.2016 KW - LA-ICP-MS KW - Nanoparticle KW - Bio-imaging KW - Cell PY - 2016 AN - OPUS4-36891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Design, characterization and application of molecular and nanoscale optical reporters and probes and method standardization N2 - Here, we present an overview of the research activities of division Biophotonics concerning the design and (bio)analytical application of molecular and nanoscale functional chromophores for e.g., biomarker analysis including methods for the reliable determination of their application relevant properties. This includes the absolute determination of their brightness and photoluminescemce quantum yield, determining the signal size from the material side, as well as the development of fluorescence standards for such measurements and instrument calibration strategies, thereby providing important prerequisites for the comparison of material performance, the mechanistic understanding of nonradiative decay channels, and the rational design of new optical reporters. Moreover, for particle-based systems, ranging from nm-sized semiconductor quantum dots to m-sized polymeric and silica beads, simple optical methods and assays for the assessment of their surface chemistry are presented, which enable the quantification of the number of total and derivatizable surface functionalities, ligands per particle and particle-bound biomolecules. In addition, validation concepts for such methods are introduced utilizing method comparisons, multimodal and cleavable probes. T2 - Seminar Microbiology of Interfaces CY - Magdeburg, Germany DA - 16.06.2016 KW - Biomarker PY - 2016 AN - OPUS4-36997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hutchinson, R. T1 - Performance and data from an elemental microscope - The NWR image N2 - The NWRimage system is the first elemental imaging-specific laser ablation instrument, offering breakthrough sub-micron spatial resolution and ultra-fast signal response for high throughput rates. Laser ablation (LA) systems are used in conjunction with Inductively Coupled Plasma Mass Spectrometry (ICP-MS) systems to detect and analyze tiny amounts of material. As ICP-MS systems have become more sensitive, a need has emerged for LA imaging tools with < 1 micron spatial resolution - a capability not previously available on the market. The NWRimage is provided with a carefully designed aerosol path from point of ablation to injection into the ICP itself. This aerosol path combined with a novel Dual Concentric Injector (DCI) ICP torch, yields < 50ms signal response to accelerate the speed of analysis and enabling enhanced sample throughput. The LA system is used for bio imaging of single cells and medical tissue samples. T2 - Winter Conference on Plasma Spectrochemistry 2016 CY - Tucson, Arizona, USA DA - 11.01.2016 KW - Laser ablation KW - Bio imaging PY - 2016 AN - OPUS4-36513 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hutchinson, R. T1 - The NWRiMAGE - an elemental microscope N2 - The NWRiMAGE provides unique technologies for high-speed imaging with genuine sub-micron ablation. In March 2015 ESI installed the first NWR iMAGE at the Bundesanstalt für Materialforschung und –prüfung (BAM) in Berlin, and since then it has undergone extensive use in bio-imaging. The Dual Concentric Injector (DCI), a new interface between laser and plasma, has been integrated into ESI´s TwoVol2 ablation cell. This technology was developed in collaboration with the University of Loughborough, and provides single shot transition at the ICP-MS of < 20 ms with high sample transport efficiency, giving superior signals above background and improve spatial resolution capability. Here we describe some data showing ultra-fast transitions of single shot ablation, sub-micron ablation experiments and rapid acquired imaging. T2 - 13th European Workshop on Laser Ablation CY - Ljubljana, Slovenia DA - 12.07.2016 KW - Laser ablation KW - Trace element KW - Imaging PY - 2016 AN - OPUS4-36999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Bio- and immuno-imaging by use of laser ablation ICP-MS N2 - Imuno-histochemical staining (IHC) of cancer biomarker on tissue sections is one of the most important analytical techniques for cancer diagnosis although standardization and quality management is tedious and differ significantly from clinic to clinic. Combining established IHC staining strategies with modern quantitative methods would increase it`s potential. We used element mass spectrometry (ICP-MS) and a new ink-jet printed internal standardization approach in combination with IHC staining. The printing strategy was utilized to improve elemental image resolution and reproducibility of paraffin embedded breast cancer tissue sections in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) after conventional IHC staining as a model system to investigate the new capabilities of this technique. T2 - Ringvorlesung Analytik, Humboldt Universität zu Berlin CY - Berlin, Germany DA - 10.06.2016 KW - Laser ablation KW - Bio-imaging KW - Immuno-assays PY - 2016 AN - OPUS4-36476 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Deiting, D. A1 - Börno, Fabian A1 - Hanning, S. A1 - Kreyenschmidt, M. A1 - Seidl, T. A1 - Otto, M. T1 - Investigation on the suitability of ablated carbon as an internal standard in laser ablation ICP-MS of polymers N2 - The conventional quantitative method for the analysis of inorganic elements in polymer matrices is a complex and time consuming process that presents a significant risk for error. Typically, polymers are digested in a microwave oven or other devices under high temperature and pressure for several hours while employing different mixtures of high purity acids. In many cases, particularly when high concentrations of doped elements are present, the digestion is often incomplete and therefore the reproducibility depends strongly on the type of polymer and additives used. A promising alternative technology that allows for the direct analysis of these polymers without digestion is laser ablation ICP-MS. Due to a lack of available reference materials and the presence of matrix dependent effects, a precise calibration cannot be obtained. In order to compensate for the matrix dependent effects the use of internal standardization is necessary. In this study the correlation between the carbon released during the ablation process and the 13C signal detected by ICP-MS and its use as an internal standard are investigated. For this purpose, twenty-one virgin polymer materials are ablated; the released carbon is determined and correlated with the corresponding integrated 13C signal. The correlation resulted in a direct relationship between the ablated carbon and 13C signal demonstrating the potential ability to neglect at least some of the matrix dependent and transport effects which occur during the laser ablation of virgin polymers. KW - Laser ablation KW - ICP-MS KW - Polymer PY - 2016 DO - https://doi.org/10.1039/C6JA00020G SN - 0267-9477 VL - 31 IS - 8 SP - 1605 EP - 1611 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-37092 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Simple methods, validation concepts, and reference materials for the characterization of functional nanomaterials and microparticles N2 - The surface chemistry / functionalization of nanomaterials and microparticles largely controls the stability of these materials as well as their solubility and subsequent biofunctionalization and their interactions with biological systems. Moreover, in the case of some nanomaterials like semiconductor quantum dots or lanthanide-based upconversion nanocrystals, the ligand shell strongly affects their optical properties, e.g., via passivation of surface states and traps that favor luminescence quenching or the protection of surface atoms from quenching water molecules. This renders analytical methods for the quantification of surface groups like functionalities very important. Targets of broad interest are here amino, carboxyl, alkine and maleimide groups used for common bioconjugation reactions and typical ligands like thiols and polyethylene glycol (PEG) molecules of varying length, used for the tuning of material hydrophilicity and biocompatibility, minimization of unspecific interactions, prevention of biofouling, and enhancement of blood circulation times as well as surface-bound biomolecules like streptavidin or other biomolecules relevant e.g., for diagnostic assays. Here, we focus on simple optical methods relying on standard laboratory instrumentation, validated by method comparison and/or mass balances and present examples for their use for the characterization of different types of nanomaterials and microparticles. T2 - Innovationsforum Senftenberg CY - Senftenberg, Germany DA - 01.06.2016 KW - Surface chemistry KW - Functional group analysis KW - Thiol assay KW - Fluorescence KW - Nanomaterial KW - Nanoparticle KW - PEG KW - Ligand KW - Semiconductor quantum dot KW - Quantum yield KW - Quantification KW - Method validation KW - Integrating sphere spectroscopy KW - Fluorescence standard PY - 2016 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-37111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Applications and challenges of luminescence-based detection methods in the life and material sciences N2 - Luminescence-based detection methods, ranging from fluorescence spectroscopy for photophysical and mechanistic studies over sensing applications, chromatographic separation techniques and the microarray technology with fluorescence detection to fluorescence microscopy, flow cytometry, single molecule spectroscopy, and molecular imaging to integrating sphere spectroscopy, are among the most widely used methods in the life and material sciences. This is due to e.g., their unique sensitivity enabling the detection of single molecules, potential for multiplexing, ease of combination with spatial resolution, and suitability for remote sensing. Many of these advantages are closely linked to the choice of suitable molecular and nanoscale fluorescent reporters, typically required for signal generation. This includes organic dyes without and with sensor function, fluorophore-encoded polymeric and silica nanoparticles as well as nanocrystalline systems like semiconductor quantum dots and upconversion phosphors, emitting in the visible (vis), near-infrared (NIR), and IR (infrared). Current challenges present the environment sensitivity of most fluorophores, rendering fluorescence spectra, measured intensities/fluorescence quantum yields, and fluorescence decay kinetics matrix-dependent, and instrument-specific distortions of measured fluorescence signals that need to be considered for quantification and comparability of data, particularly fluorescence spectra. Here, current applications of luminescence-based methods and different types of reporters will be presented. In this context, suitable spectroscopic tools for the characteri-zation of the optical properties of fluorescent reporters and fluorophore-encoded microparticles, analytical tools for the determination of the surface chemistry of different types of particles, and different multiplexing strategies will be discussed. T2 - 9th Meeting of Engineering of Functional Interfaces CY - Wildau,Germany DA - 03.07.2016 KW - Fluorescence KW - Multiplexing KW - Lifetime KW - Nanomaterial KW - Nanoparticle KW - PEG KW - Ligand KW - Semiconductor quantum dot KW - Quantum yield KW - Quantification KW - Upconversion nanoparticle KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Fluorescence standard KW - Calibration PY - 2016 AN - OPUS4-37112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Novel strategies for standardization and calibration in Laser Ablation ICP-MS N2 - Elemental imaging of biological samples (bio-imaging) using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) provides spatially resolved information on element distribution (qualitative and quantitative) in thin sections of biological samples. By rastering with a laser across the sample, a two-dimensional image of the elemental distribution can be reconstructed that shows the relative intensities of the respective elements. However the method is hampered by a lack of internal standards and quantification concepts, which will be discussed in this lecture in more detail. In liquid analysis the internal standard is used for drift correction and calibration and thus it is required that the standard should have similar physical and chemical properties similar to the analyte element during the pneumatic nebulization process, the transport, ionization and transmission into the ICP-MS. In laser ablation it should correct additionally for differences in the ablation process by laser instabilities or changes of sample properties to compensate variations or drift effects during the LA process. T2 - SALSA Lecture CY - Berlin, Germany DA - 14.06.2016 KW - Standardization KW - Calibration KW - LA-ICP-MS PY - 2016 AN - OPUS4-37164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kage, Daniel T1 - Lifetime-encoded microparticles for application in flow cytometry N2 - The steadily increasing number of analytes, especially in bioanalytics and environmental contexts, requires the development of efficient and versatile methods for the simultaneous determination of different parameters within a single run. Additionally, these methods should be applicable in conjunction with established platform technologies like flow cytometry. Fluorescence techniques have proven to fulfill these requirements. Commonly performed spectral multiplexing utilizing a color code suffers from several problems, such as the sensitivity of fluorescence intensity measurements to fluctuations in excitation light intensity and dye concentration and hence, photobleaching and spectral crosstalk limiting the achievable number of detection channels. Moreover, it typically requires different costly excitation light sources. T2 - Innovation Forum Senftenberg 2016 CY - Senftenberg, Germany DA - 01.06.2016 KW - flow cytometry KW - lifetime encoding KW - life sciences KW - fluorescence KW - polymer particles PY - 2016 AN - OPUS4-37154 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Moser, Marko T1 - Quantification of PEG-Maleimide Ligands and Coupling Efficiencies on Nanoparticles with Ellman’s Reagent N2 - Emissive nanoparticles (NP) are of ever increasing importance in nanotechnology, optical industries, and life sciences. Applicationrelevant properties determining particle performance and biocompatibility depend mainly on surface functional groups or ligands. Coating with polyethylene glycol (PEG) ligands enhances hydrophilicity and biocompatibility of nanomaterials, and enables subsequent binding of biomolecules. Hence, PEGylated particles must be carefully engineered and monitored with simple and fast methods. T2 - 9th Meeting of Engineering of Functional Interfaces CY - Wildau, Germany DA - 03.07.2016 KW - PEG-Maleimide KW - Ellman PY - 2016 AN - OPUS4-37244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Nachbestimmung von Pfahllängen am Beispiel von Masten. N2 - Im Rahmen der Lebensdauerverlängerung oder der Umnutzung von Bauwerken (z. B. Brücken, Bürogebäude oder Maste) müssen diese zum Teil neu bewertet werden. Dafür ist eine Nachrechnung für statische und dynamische Lastfälle erforderlich. Dies betrifft zum einen die Struktur selbst, die gegebenenfalls verstärkt werden muss. Aber auch die Gründung (oft Pfähle verschiedenster Typen) muss neu beurteilt werden. Nach mehreren Jahrzehnten sind jedoch für einige Bauwerke keine zuverlässigen Bestandsunterlagen verfügbar. Eine vollständige Freilegung der Pfähle verbietet sich aus Kostengründen sowie Verlust an Widerstand gegen Zug. Lediglich der Pfahlanschluss kann visuell begutachtet werden, um Pfahlzahl, -typ und Durchmesser zu bestimmen. Für die Bestimmung der Pfahllänge müssen zerstörungsfreie Verfahren eingesetzt werden. In einer Machbarkeitsstudie wurden von den Autoren teils im Blindversuch drei Verfahren evaluiert: die klassische Pfahlintegritätsprüfung nach der Hammerschlagmethode, eine mehrkanalige Variante hierzu und das Parallel-Seismik-Verfahren. Die ersten beiden Methoden lieferten an den untersuchten Pfählen nur in Einzelfällen verwertbare Ergebnisse. Die Parallel-Seismik-Methode lieferte auch im Blindversuch an Fundamenten, bei denen die Pfahllänge dem Eigentümer bekannt war, Ergebnisse mit einer Abweichung von max. 0,5 m. Diese Toleranz lässt sich bei der Standfestigkeitsbeurteilung berücksichtigen. Die Mehrkosten des Verfahrens (anders als bei den anderen Verfahren wird ein verrohrtes Bohrloch im Boden nahe dem Pfahl benötigt) halten sich in Grenzen, wenn man es in die geotechnische Untersuchung integriert. Daher wurde es inzwischen auch in der Praxis eingesetzt. Auch liegen die Gesamtkosten für die Untersuchung deutlich unter denen für eventuell notwendigen Ersatz – oder Verstärkungsmaßnahmen, die notwendig werden, wenn keine Daten zur Pfahllänge verfügbar sind. Der Vortrag erläutert die Ergebnisse der Machbarkeitsstudie, zeigt erste Praxisfälle und weist auf Möglichkeiten hin, das Parallel-Seismik Verfahren in Zukunft noch genauer und effizienter einzusetzen. T2 - Workshop Geophysikalische Untersuchungen an Bauwerken CY - Neustadt/W., Germany DA - 05.10.2016 KW - Parallel-Seismik KW - Mast KW - Pfahl KW - Länge PY - 2016 AN - OPUS4-37720 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Nachbestimmung von Pfahllängen am Beispiel von Masten N2 - Im Rahmen der Lebensdauerverlängerung oder der Umnutzung von Bauwerken (z. B. Brücken, Bürogebäude oder Maste) müssen diese zum Teil neu bewertet werden. Dafür ist eine Nachrechnung für statische und dynamische Lastfälle erforderlich. Dies betrifft zum einen die Struktur selbst, die gegebenenfalls verstärkt werden muss. Aber auch die Gründung (oft Pfähle verschiedenster Typen) muss neu beurteilt werden. Nach mehreren Jahrzehnten sind jedoch für einige Bauwerke keine zuverlässigen Bestandsunterlagen verfügbar. Eine vollständige Freilegung der Pfähle verbietet sich aus Kostengründen sowie Verlust an Widerstand gegen Zug. Lediglich der Pfahlanschluss kann visuell begutachtet werden, um Pfahlzahl, -typ und Durchmesser zu bestimmen. Für die Bestimmung der Pfahllänge müssen zerstörungsfreie Verfahren eingesetzt werden. In einer Machbarkeitsstudie wurden von den Autoren teils im Blindversuch drei Verfahren evaluiert: die klassische Pfahlintegritätsprüfung nach der Hammerschlagmethode, eine mehrkanalige Variante hierzu und das Parallel-Seismik-Verfahren. Die ersten beiden Methoden lieferten an den untersuchten Pfählen nur in Einzelfällen verwertbare Ergebnisse. Die Parallel-Seismik-Methode lieferte auch im Blindversuch an Fundamenten, bei denen die Pfahllänge dem Eigentümer bekannt war, Ergebnisse mit einer Abweichung von max. 0,5 m. Diese Toleranz lässt sich bei der Standfestigkeitsbeurteilung berücksichtigen. Die Mehrkosten des Verfahrens (anders als bei den anderen Verfahren wird ein verrohrtes Bohrloch im Boden nahe dem Pfahl benötigt) halten sich in Grenzen, wenn man es in die geotechnische Untersuchung integriert. Daher wurde es inzwischen auch in der Praxis eingesetzt. Auch liegen die Gesamtkosten für die Untersuchung deutlich unter denen für eventuell notwendigen Ersatz – oder Verstärkungsmaßnahmen, die notwendig werden, wenn keine Daten zur Pfahllänge verfügbar sind. Der Vortrag erläutert die Ergebnisse der Machbarkeitsstudie, zeigt erste Praxisfälle und weist auf Möglichkeiten hin, das Parallel-Seismik Verfahren in Zukunft noch genauer und effizienter einzusetzen. T2 - Baugrundtagung 2016 CY - Bielefeld, Germany DA - 15.09.2016 KW - Mast KW - Pile KW - Pfahl KW - Länge KW - Parallel-Seismik KW - Integritätsprüfung KW - Tower KW - Length KW - Parallel-seismic KW - Integrity-testing PY - 2016 AN - OPUS4-37647 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Geophysik im Bauwesen - ein Überblick N2 - Überblick über den Einsatz verschiedener geophysikalischer Verfahren in der zerstörungsfreien Prüfung im Bauwesen T2 - Workshop Geophysikalische Untersuchungen an Bauwerken CY - Neustadt/W., Germany DA - 05.10.2016 KW - Geophysik KW - ZfP KW - Bauwesen PY - 2016 AN - OPUS4-37719 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Progress in non-destructive testing and monitoring of concrete N2 - Überblicksvortrag zu Aktivitäten von BAM-8.2 T2 - Seminar der Universität Lund, Fakultät, Technische Geologie und NDT CY - Lund, Sweden DA - 8.3.2018 KW - Concrete KW - Non-Destructive Testing PY - 2018 AN - OPUS4-44575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst A1 - Wiggenhauser, Herbert A1 - Milmann, Boris T1 - LAUS - Erste praktische Erfahrungen mit einem neuartigen Ultraschallsystem großer Eindringtiefe N2 - Konventionelle Systeme zur Ultraschall-Echo-Prüfung von Betonbauteilen sind in ihrer Eindringtiefe auf etwa einem Meter begrenzt. Zur Prüfung stärkerer Objekte war die Entwicklung eines neuartigen Prüfsystems notwendig. Das LAUS-System (Large Aperture UltraSound) besteht aus 12 einzelnen Arrays, die mit jeweils 32 Einzelprüfköpfen (Scherwellen, 25 – 50 kHz) als Sender oder Empfänger betrieben werden können. Sie werden unabhängig auf Betonoberflächen mit Unterdruck befestigt und kommunizieren drahtlos untereinander und mit der Zentraleinheit. Alle möglichen Kombinationen ergeben 132 Einzelmessungen, die zur Rekonstruktion des durchschallten Volumens genutzt werden. Mehrere dieser Datensätze lassen sich zu einer 3D-Auswertung kombinieren. Das System wurde an mehreren Testobjekten und Bauwerken erfolgreich erprobt. So konnte die fünf Meter dicke, sehr stark bewehrte Fundamentplatte des Fallturms auf dem BAM-Testgelände bei Horstwalde durchschallt werden. Ein zweites Beispiel ist die erfolgreiche Detektion von Spannkanälen in 1,8 m Tiefe in einem massiven Brückenbauwerk. T2 - Bauwerksdiagnose 2018 CY - Berlin, Germany DA - 15.2.2018 KW - Ultraschall KW - Beton KW - LAUS KW - Brücke KW - Fundament PY - 2018 AN - OPUS4-44577 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Method development for metal detection at cellular levels by ICP-MS N2 - An overview about different analytical approaches will be presented of how to detect metals in individual biological cells by use of ICP-MS. For this purpose, we are using different sample introduction systems for ICP-MS for detection, imaging and quantification of metals at cellular levels. By use of laser ablation, we have studied the up-take by and distribution of nanoparticles in single cells. Recently we have developed staining techniques to measure protein and DNA content of cells and identifying the cell status by immunoassays using metal-tagging of antibodies. New research based on cell arrays will be shortly discussed. Using pneumatic nebulization and microdroplet generation, we have also studied the up-take of nanoparticles and toxic metals as well as essential elements in single cells using different ICP-MS mass spectrometric concepts (sector field instrument, triple-quad instrument, time of flight (CyTOF) instrument). The different ICP-MS based methods will be compared concerning their analytical figures of merit and their strengths and weaknesses will be evaluated. T2 - Projektmeeting CY - Bremen, Germany DA - 18.04.2018 KW - Single cell ICP-MS KW - LA-ICP-MS with cellular resolution KW - Nanoparticles PY - 2018 AN - OPUS4-44851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Studying nanoparticle-cell interaction by LA ICP-MS N2 - The interaction of nanoparticles (NPs) with cells has become a major field of interest, ranging from medical applications to nanotoxicology. Size, shape and surface modification of the NPs determine the uptake rate and pathway into the cells, and therefore impact specific cell components and processes. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is an established quantitative multi-elemental analysis and mapping technique. In recent years, it was shown that LA-ICP-MS can provide quantitative as well as distribution information of NPs in cell samples. Here LA-ICP-MS was applied for the imaging of individual cells to study the uptake and intracellular processing of metal-containing nanostructures. Additionally, the local distribution of naturally occurring elements in cells like P was measured to indicate cell morphology. The cells were incubated with different types of NPs under varying experimental conditions. For LA analysis, the cells were fixed and dried. Our findings show, that LA-ICP-MS is suitable for the localisation of nanoparticle aggregates within cellular compartments. The studied NPs accumulate in the perinuclear region in the course of intracellular processing, but do not enter the cell nucleus. The uptake efficiency depends strongly on the physicochemical properties of the nanostructures as well as on the incubation conditions like concentration and incubation time. The results demonstrate the potential of LA-ICP-MS providing insight into NP uptake, intracellular distribution and cell-to-cell variation dependent on experimental parameters. T2 - Workshop on Laser Bioimaging Mass Spectrometry CY - Münster, Germany DA - 24.05.2018 KW - Imaging KW - Laser ablation KW - ICP-MS KW - Nanoparticle KW - Cell PY - 2018 AN - OPUS4-45071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Ultrasound: From Imaging to Monitoring N2 - Review of ultrasonic echo imaging and ultrasonic monitoring techniques applied to concrete structures, especially bridges. Includes newest research results from BAM. T2 - Transport Research Board Annual Meeting, Workshop 1647 CY - Washington, DC, USA DA - 6.1.2018 KW - Ultrasound KW - Imaging KW - Monitoring KW - Concrete KW - Bridges PY - 2018 AN - OPUS4-44587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wang, Xin T1 - Advanced ultrasonic instrumentation for interferometric monitoring N2 - Main aim is to improve ultrasonic sensor networks to monitor concrete structures under dynamic loads. Novel algorithms have to be developed and tested to separate the influence of various effects for field data. Ways to quantify the interpretation of ultrasonic data e.g. in terms of degree of damage or capacity, have to be found. Improve and simplify imaging techniques, extend them to arbitrary structures, to foster field applications. T2 - Implementation day of INFRASTAR CY - BASt, Bergisch Gladbach, Germany DA - 20.03.2018 KW - CODA wave interferometry KW - NDT KW - Sensor KW - Cracks KW - Embedded ultrasonic sensor PY - 2018 AN - OPUS4-44585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saleh, Maysoon I. A1 - Kembuan, C A1 - Rühle, Bastian A1 - Graf, C A1 - Resch-Genger, Ute T1 - Gold-shell coated NaYF4:Er3+, Yb3+ nanoparticles for the enhancement of fluorescence emission N2 - In the present work, we aim to explore how far the UCNP emission intensity can be enhanced by the aid of plasmonic interactions using a gold shell. The distance between the UCNP core and the gold shell is varied by adding a silica spacer of different thicknesses. The synthetic conditions for obtaining UCNP@SiO2@Au core-shell nanoparticles with precisely tuneable silica shell thicknesses were investigated. A gold shell on the UCNP@SiO2 nanoparticles is expected to give rise to a noticeable enhancement of particle brightness and fluorescence, given that the thicknesses of the silica shell and the gold coating can be controlled and fine-tuned. First single particle studies revealing shortening of the Er3+ lifetimes suggest that plasmonic enhancement occurs. T2 - 2nd Conference and Spring School on Properties, Design and Applications of Upconversion Nanomaterials CY - Valencia, Spain DA - 02.04.2018 KW - Upconversion nanoparticles KW - Silica coating KW - Plasmonic enhancement PY - 2018 AN - OPUS4-44969 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Kembuan, C A1 - Graf, C T1 - Gold-shell coated NaYF4:Er3+, Yb3+ nanoparticles for the enhancement of fluorescence emission N2 - In the present work, we aim to explore how far the UCNP emission intensity can be enhanced by the aid of plasmonic interactions using a gold shell. The distance between the UCNP core and the gold shell is varied by adding a silica spacer of different thicknesses. The synthetic conditions for obtaining UCNP@SiO2@Au core-shell nanoparticles with precisely tuneable silica shell thicknesses were investigated. A gold shell on the UCNP@SiO2 nanoparticles is expected to give rise to a noticeable enhancement of particle brightness and fluorescence, given that the thicknesses of the silica shell and the gold coating can be controlled and fine-tuned. First single particle studies revealing shortening of the Er3+ lifetimes suggest that plasmonic enhancement occurs. T2 - 2nd Conference and Spring School on Properties, Design and Applications of Upconversion Nanomaterials CY - Valencia, Spain DA - 02.04.2018 KW - Upconversion nanoparticles KW - Silica coating KW - Plasmonic enhancement PY - 2018 AN - OPUS4-44958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Homann, C. A1 - Krukewitt, Lisa A1 - Frenzel, Florian A1 - Grauel, Bettina A1 - Würth, Christian A1 - Resch-Genger, Ute A1 - Haase, M. T1 - Aufwärtskonvertierende NaYF4:Yb,Er/NaYF4‐Kern/Schale‐Nanokristalle mit hoher Lumineszenzquantenausbeute N2 - Eine modifizierte Syntheseroute auf der Basis wasserfreier Seltenerdacetate wurde zur Synthese aufwärtskonvertierender Kern/Schale‐Nanokristalle mit mittleren Größen zwischen 15 bis 45 nm eingesetzt. Die nahezu monodispersen Partikel bestehen aus einem NaYF4:Yb,Er‐Kern, dotiert mit 18 % Yb3+ und 2 % Er3+, und einer inerten Schale aus NaYF4, wobei die Dicke der Schale dem jeweiligen Radius des Kernpartikels entspricht. Absolutmessungen der Photolumineszenz‐Quantenausbeuten bei verschiedenen Anregungsleistungsdichten zeigen, dass die Quantenausbeuten von 45 nm Kern/Schale‐Partikeln schon fast an die Quantenausbeute des mikrokristallinen aufwärtskonvertierenden Leuchtstoffs heranreichen. Kleinere Kern/Schale‐Partikel, die nach der gleichen Methode hergestellt wurden, zeigen nur eine moderate Abnahme der Quantenausbeute. Beispielsweise ist die Quantenausbeute von 15 nm großen Kern/Schale‐Partikeln bei hohen Leistungsdichten (100 W cm−2) nur um einen Faktor drei kleiner als die des mikrokristallinen Leuchtstoffpulvers und um ungefähr einen Faktor 10 kleiner bei niedrigen Leistungsdichten (1 W cm−2). KW - Nicht lineare Prozesse KW - Nanopartikel KW - Quantenausbeute PY - 2018 DO - https://doi.org/10.1002/ange.201803083 VL - 130 IS - 28 SP - 8901 EP - 8905 PB - Wiley VCH Verlag AN - OPUS4-45573 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Buildings: Seismology and Strctural Health Monitoring N2 - Overview of seismological concepts unsed in nondestructive testing in civil engineering T2 - Fourth TIDES Advanced Training School CY - Prague, Czech Repubilc DA - 01.07.2018 KW - Geophysics KW - Seismology KW - Interferometry KW - Structural health monitoring KW - Nondestructive testing PY - 2018 AN - OPUS4-45361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Method development for metal detection at cellular levels by ICP-MS N2 - An overview about different analytical approaches will be presented of how to detect metals in individual biological cells by use of ICP-MS. For this purpose, we are using different sample introduction systems for ICP-MS for detection, imaging and quantification of metals at cellular levels. By use of laser ablation, we have studied the up-take by and distribution of nanoparticles in single cells. Recently we have developed staining techniques to measure protein and DNA content of cells and identifying the cell status by immunoassays using metal-tagging of antibodies. New research based on cell arrays will be shortly discussed. Using pneumatic nebulization and microdroplet generation, we have also studied the up-take of nanoparticles and toxic metals as well as essential elements in single cells using different ICP-MS mass spectrometric concepts (sector field instrument, triple-quad instrument, time of flight (CyTOF) instrument). The different ICP-MS based methods will be compared concerning their analytical figures of merit and their strengths and weaknesses will be evaluated. T2 - 16th Czech-Slovak Spectroscopic Conference CY - Luhacovice, Czech Republic DA - 27.05.2018 KW - Single cell analysis KW - ICP-MS KW - Nanoparticles PY - 2018 AN - OPUS4-45161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - LA-ICP-MS to study nanoparticle-cell interaction N2 - Nanoparticles (NPs) have found a wide range of applications in research and industry. Thereby the interaction of NPs with biological systems like cells has become a major field of interest, ranging from medical applications to nanotoxicology. Size, shape and surface modification of the nanomaterials determine the uptake rate and pathway into the cells, and therefore impact specific cell components and processes. In recent years, elemental imaging of biological samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is gaining more and more importance. Improvements concerning both spatial resolution (down to 1 µm) and signal-to-background ratio due to low-dispersion LA chambers make LA-ICP-MS particularly interesting for single cell analysis. Here LA-ICP-MS was applied for the imaging of individual cells to study the uptake and intracellular processing of metal-containing nanostructures. The cells were incubated with different NPs under varying experimental conditions and afterwards fixed with para-formaldehyde and dried for LA analysis. High-spatial resolution LA-ICP-MS was achieved by careful optimisation of the laser ablation parameters. Our findings show, that LA-ICP-MS is applicable to localize NP aggregates within cellular compartments. The uptake efficiency depends strongly on the physicochemical properties of the nanostructures as well as on the incubation conditions like concentration and incubation time. The results demonstrate the potential of LA-ICP-MS providing insight into nanoparticle-cell interaction dependent on experimental parameters. T2 - 14th European Workshop on Laser Ablation (EWLA) CY - Pau, France DA - 26.06.2018 KW - Laser ablation KW - ICP-MS KW - Imaging KW - Nanoparticle KW - Cell PY - 2018 AN - OPUS4-45570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, Katrin T1 - NanoGenotox - Automatable determination of genotoxicity of nanoparticles with DNA-based optical assays N2 - The overall interest in nanotoxicity, triggered by the increasing use of nanomaterials in the material and life sciences, and the synthesis of an ever increasing number of new functional nanoparticles calls for standardized test procedures and for efficient approaches to screen the potential genotoxicity of these materials. Aiming at the development of fast and easy to use, automated microscopic methods for the determination of the genotoxicity of different types of nanoparticles, we assess the potential of the fluorometric γH2AX assay for this purpose. This assay, which can be run on an automated microscopic detection system, relies on the detection of DNA double strand breaks (DSB) as a sign for genotoxicity. Here, we provide first results obtained with broadly used nanomaterials like CdSe/CdS and InP/ZnS quantum dots as well as iron oxide, gold, and polymer particles of different surface chemistry with previously tested colloidal stability and different cell lines like Hep-2 and 8E11 cells, which reveal a dependence of the genotoxicity on the chemical composition as well as the surface chemistry of these nanomaterials. These studies will be also used to establish nanomaterials as positive and negative genotoxicity controls or standards for assay performance validation for users of this fluorometric genotoxicity assay. In the future, after proper validation, this microscopic platform technology will be expanded to other typical toxicity assays. T2 - Nanoworkshop 2018 CY - PTB Berlin-Adlershof, Germany DA - 14.05.2018 KW - Qdots KW - Surface functions KW - Quantification KW - Nanogenotoxicity PY - 2018 AN - OPUS4-45126 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike A1 - Phukphatthanachai, Pranee T1 - Quantification of sulphur in copper metals by isotope dilution LA-ICP-MS using polyethylene frits N2 - Sulphur is one of the relevant impurities in copper and its alloys affecting their material properties. To ensure the quality of copper products, fast direct solid sampling techniques are very attractive. However, for the calibration suitable matrix reference materials are required. For the certification of such reference materials appropriate, SI-traceable analytical methods are essential. Therefore, a procedure was developed to quantify total sulphur in copper by combining the classical isotope dilution (ID) technique and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Here, for the first time, polyethylene (PE) frits were used to prepare appropriate solid samples for the sulphur quantification in copper metals (alloyed/unalloyed) by isotope dilution LA-ICP-MS. The properties of the PE frit meet the requirements as porous material with high absorption efficiency, thermal and chemical resistance as well as low sulphur blank. Different copper reference materials were used to develop and validate the procedure. The copper samples were spiked with 34S, digested with nitric acid and then the digests were absorbed on PE frits. After drying, the frits were analysed by LA-ICP-IDMS using a Nd:YAG laser at 213 nm coupled to an ICP sector field mass spectrometer. It could be demonstrated, that the sample solution dispersed on the frits did not influence the 32S/34S ratio significantly even though the sulphur intensities were fluctuating along the scanned lines. Relative standard deviations of the isotope ratios were below 5 % in average between three line scans (except for the pure spike solution and procedure blank). The measurement results were validated by comparing them with the results obtained by conventional ICP-IDMS after analyte-matrix separation. Plotting the mass fraction of sulphur in copper obtained by LA-ICP-IDMS versus those obtained by ICP-IDMS yields a linear curve with a correlation coefficient of 0.9999 showing a strong agreement between both techniques. The metrological traceability to the SI from the kg down to the sulphur mass fraction in copper is established by an unbroken chain of comparisons, each accompanied by an uncertainty budget. Thus, the measurement results are considered reliable, acceptable and comparable within the stated measurement uncertainty. T2 - 14th European Workshop on Laser Ablation (EWLA) CY - Pau, France DA - 26.06.2018 KW - ICP-MS KW - Laser ablation KW - Isotope dilution KW - Copper PY - 2018 AN - OPUS4-45569 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drescher, D. A1 - Traub, Heike A1 - Büchner, T. A1 - Jakubowski, Norbert A1 - Kneipp, J. T1 - Properties of in situ generated gold nanoparticles in the cellular context N2 - Gold nanostructures that serve as probes for nanospectroscopic analysis of eukaryotic cell cultures can be obtained by the in situ reduction of tetrachloroauric acid (HAuCl4). To understand the formation process of such intracellularly grown particles depending on the incubation medium, the reaction was carried out with 3T3 fibroblast cells in three different incubation media, phosphate buffer, Dulbecco's Modified Eagle Medium (DMEM), and standard cell culture medium (DMEM with fetal calf serum). The size, the optical properties, the biomolecular corona, and the localization of the gold nanoparticles formed in situ vary for the different conditions. The combination of surface-enhanced Raman scattering (SERS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) microscopic mapping and transmission electron microscopy (TEM) provides complementary perspectives on plasmonic nanoparticles and non-plasmonic gold compounds inside the cells. While for the incubation with HAuCl4 in PBS, gold particles provide optical signals from the nucleus, the incubation in standard cell culture medium leads to scavenging of the toxic molecules and the formation of spots of high gold concentration in the cytoplasm without formation of SERS-active particles inside the cells. The biomolecular corona of nanoparticles formed in situ after incubation in buffer and DMEM differs, suggesting that different intracellular molecular species serve for reduction and stabilization. Comparison with data obtained from ready-made gold nanoparticles suggests complementary application of in situ and ex situ generated nanostructures for optical probing. KW - Nanoparticles KW - Laser ablation KW - ICP-MS KW - SERS KW - Cell PY - 2017 DO - https://doi.org/10.1039/C7NR04620K SN - 2040-3372 VL - 9 IS - 32 SP - 11647 EP - 11656 PB - The Royal Society of Chemistry RSC CY - Cambridge, UK AN - OPUS4-41871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Von der Ölsuche zum Beton - Geophysikalische Methoden für die ZfP im Bauwesen N2 - Nutzung geophysikalischer Methoden für die zerstörungsfrei Prüfung von Betonbauwerken; Beispiel 1: Reverse Time Migration zur Verbesserung der Abbildungsqualität von Ultraschall-Echo-Prüfungen; Beispiel 2: Eingebettete Transducer und Codawelleninterferometrie für die Bauwerksüberwachung. T2 - DGZfP Arbeitskreis Berlin, 389. Sitzung CY - Berlin, Germany DA - 05.09.2017 KW - Geophysik KW - Zerstörungsfreie Prüfung KW - Monitoring KW - Beton KW - Ultraschall PY - 2017 AN - OPUS4-41849 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Studying cellular uptake of metal-containing nanoparticles by LA-ICP-MS N2 - Nanoparticles (NPs) have potential applications in medical diagnostics, imaging, drug delivery and other kinds of therapy. Furthermore, studies concerning nanoparticle uptake by cells are important for risk assessment. Size, shape and surface modification of the NPs determine the uptake rate and pathway into the cells, and therefore impact specific cell components and processes. Understanding the different uptake mechanisms and involved processes require sub-cellular resolution to determine, for example, whether the nanoparticles are reaching the nucleus. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is an established quantitative multi-elemental analysis and mapping technique. However, sub-cellular imaging has traditionally been challenging to achieve due to a lack of sensitivity at small laser spots. But now novel laser ablation systems with improved sensitivity and washout time allow imaging at high lateral resolution with spot sizes down to 1 µm. Here LA-ICP-MS was applied for the imaging of individual fibroblast cells to study the uptake and intracellular processing of metal-containing NPs. To indicate cell morphology the local distribution of naturally occurring elements in cells like P and Zn was measured, too. Our results show that LA-ICP-MS can be used to localise nanoparticle aggregates within cellular compartments. The studied NPs accumulate in the perinuclear region in the course of intracellular processing, but do not enter the cell nucleus. The uptake efficiency depends strongly on the physico-chemical properties of the nanostructures as well as on the incubation conditions like concentration and incubation time. The potential of LA-ICP-MS for analysis at single cell level will be demonstrated. T2 - Euroanalysis 2017 CY - Stockholm, Sweden DA - 28.08.2017 KW - Laser ablation KW - ICP-MS KW - Nanoparticle KW - Cell PY - 2017 AN - OPUS4-41883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Functional Nanomaterials with VIS/NIR Emission-Spectroscopic Properties And Surface Group Analysis N2 - Optical-spectroscopic methods for the quantitative characterization of the optical properties of different types of vis/NIR-emissive nanomaterials like semiconductor quantum dots and upconversion nanocrystals will be presented and their relevance for the mechanistic understanding of nonradiative decay channels and the rational design of new nanomaterials will be underpinned. In this respect, also validation concepts for such measurements and absolute fluorometry will be introduced. In addition, the potential of optical spectroscopy for surface group and ligand analysis surface chemistry will be demonstrated exemplarily for semiconductor quantum dots. T2 - Universität Mainz, AK Professor K. Heinze CY - Mainz, Germany DA - 24.07.2017 KW - Upconversion KW - Nanoparticle KW - Flourescence KW - Surface group analysis KW - NIR KW - Absolute flourometry KW - Integrating sphere spectroscopy KW - Optical probe KW - Assay KW - Thiol ligand PY - 2017 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-41115 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Frenzel, Florian T1 - Power dependent optical properties of hexagonal β-NaYF4: x % Er3+, 20 % Yb3+ core/ core-shell upconversion nanoparticles in cyclohexane and water N2 - Lanthanide doped photon upconverting nanophosphors (UCNPs) have the unique capability to produce narrow band, multi-color emission in the UV/vis/NIR upon multiphotonic absorption of infrared light, which makes them promising reporters for diagnostic, bioanalytical, and biological applications. This minimizes background signals, which normally occur due to autofluorescence from auxochromes, in biological matrices and enables deep penetration depths in biological applications. Moreover, UCNPs show long luminescence lifetimes in the μs range favorable for time gated emission in conjunction with a high photostability and chemical inertness and they do not blink. One of the most efficient upconversion (UC) phosphors for conversion of 976 nm to 655 nm and 545 nm light presents the hexagonal NaYF4-host crystal doped with 20 % Yb3+ used as sensitizer to absorb infrared light and 2 % Er3+ acting as activator mainly responsible for light emission. The high transparency in the relevant spectral windows of this host together with its low phonon frequencies ensure relatively high luminescence efficiencies. Although UCNPs are ideal candidates for many chemical and biological sensing and imaging applications, compared to other well-known chromophores like organic dyes or QDs, they suffer from a comparatively low brightness due to the low absorption cross sections of the parity forbidden f-f-transitions and low photoluminescence quantum yields (QYUC) particularly in the case of small nanoparticles with sizes of < 50 nm. The rational design of more efficient UCNPs requires an improved understanding of the nonradiative decay pathways in these materials that are influenced by particle architecture including dopant ion concentration and homogeneity of dopant distribution within UCNPs, size/surface-to-volume ratio, surface chemistry, and microenvironment. A promising approach to overcome the low efficiency of UCNPs is to use plasmonic interactions between a noble metal (Ag or Au) structure in the proximity of UCNPs and the incident light. This interaction leads to a modification of the spectroscopic properties due to local field enhancements and can involve an increase of the photoluminescence. In this respect, we study the interactions of UCNPs with metal structures (clusters and shells) by varying shape and size. Here, first results derived from integrating sphere spectroscopy and time-resolved fluorescence measurements are presented. T2 - Summer School "EXCITING NANOSTRUCTURES" CY - Bad Honnef, Germany DA - 17.07.2017 KW - Upconversion KW - Nanoparticle KW - Flourescence KW - Core-shell architecture KW - NIR KW - Absolute flourometry KW - Integrating sphere spectroscopy KW - Er(III) KW - Yb(III) KW - Single particle spectroscopy PY - 2017 AN - OPUS4-41172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jakubowski, Norbert A1 - Müller, Larissa A1 - Traub, Heike A1 - Esteban-Fernandez, Diego A1 - Panne, Ulrich A1 - Herrmann, Antje A1 - Schellenberger, E. A1 - Kneipp, Janina T1 - Lecture 5 Bio- and immuno-imaging by use of laser ablation ICP-MS N2 - ICP-MS is a well-established analytical method which excels by high accuracy, high dynamic range and extremely low limits of detection for most metals. Furthermore ICP-MS offers a very high multi-element coverage so that many elements of the periodic table can be detected simultaneously. In this series of lectures, we want to focus on the historical developments, fundamentals, instrumentation and novel applications of ICP-MS in the life and material sciences. KW - Imaging KW - Laser ablation ICP-MS PY - 2017 AN - OPUS4-40943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Detecting subtle changes in concrete with coda wave interferometry N2 - Subtle changes in concrete, caused by stress, temperature or deterioration can be detected by ultrasonic transmission measurements evaluated by coda wave interferometry. Background and examples are presented as well as possibilities to locate damages. T2 - New mathematics for a safer world: wave propagation in heterogeneous materials CY - Edinburgh, UK DA - 12.06.2017 KW - Concrete KW - Ultrasound KW - Coda wave interferometry KW - Monitoring PY - 2017 AN - OPUS4-40580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Bridge Monitoring by Passive Seismic Data, First tests at the BLEIB reference structure N2 - Seismic wave velocities are related to elastic moduli and other properties and can serve as indicators for changes in the material. They are conventionally determined by active measurements. Using ideas from seismic interferometry Determination from stacked cross-correlations of registrations of man- made and natural noise (“passive seimics“) is an effective alternative, as these data might be available from vibration monitoring anyway. The validity of this approach is demonstrated by a simple experiment based on recordings of man made noise using accelerometers at the reference structure. The s-wave (or more probable. guided wave) velocity was determined to be 2100 m/s in both active and passive experiments. T2 - Passive Imaging and monitoring in wave physics: from seismology to ultrasound CY - Cargese, France DA - 05.06.2017 KW - Passive Seismics KW - Bridge monitoring KW - Elastic wave velocity PY - 2017 AN - OPUS4-40575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Müller, L. A1 - Traub, Heike A1 - Jakubowski, Norbert ED - Prof. Dr. Golloch, Alfred T1 - Novel applications of lanthanoides as analytical or diagnostic tools in the life sciences by ICP-MS-based techniques N2 - Inductively coupled plasma mass spectrometry (ICP-MS) is a well-established analytical method for multi-elemental analysis in particular for elements at trace and ultra-trace levels. It has found acceptance in various application areas during the last decade. ICP-MS is also more and more applied for detection in the life sciences. For these applications, ICP-MS excels by a high sensitivity, which is independent of the molecular structure of the analyte, a wide linear dynamic range and by excellent multi-element capabilities. Furthermore, methods based on ICP-MS offer simple quantification concepts, for which usually (liquid) standards are applied, low matrix effects compared to other conventional bioanalytical techniques, and relative limits of detection (LODs) in the low pg g−1 range and absolute LODs down to the attomol range. In this chapter, we focus on new applications where the multi-element capability of ICP-MS is used for detection of lanthanoides or rare earth elements, which are applied as elemental stains or tags of biomolecules and in particular of antibodies. KW - ICP-MS KW - Life sciences KW - Mass cytometry KW - Laser ablation (LA)-ICP-MS KW - Bioimaging PY - 2017 SN - 978-3-11-036523-8 SP - Chapter 11, 301 EP - 320 PB - De Gruyter AN - OPUS4-40244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Quantitative Characterization of Functional Nanomaterials with vis/NIR Emission N2 - The rational design of functional nanomaterials for optical applications in the material and life sciences requires optical-spectroscopic methods for the quantitative characterization of their signal-relevant optical properties. Additionally, methods for the simple and quantitative analysis of the surface chemistry are desired as the chemical nature and number of the surface groups and ligands can affect the optical features and controls the interaction of these nanomaterials with their environment. Here, we present quantitative photoluminescenvce studies of different types of vis/NIR-emissive nanomaterials like semiconductor quantum dots and upconversion nanocrystals will be presented and their relevance for the mechanistic understanding of nonradiative decay channels and the rational design of new nanomaterials will be underpinned. In this respect, also validation concepts for such measurements and absolute fluorometry will be introduced. In addition, the potential of optical spectroscopy for surface group and ligand analysis surface chemistry will be demonstrated exemplarily for semiconductor quantum dots T2 - AK Prof. Voss CY - Uni Brunswick, Germany DA - 03.08.2017 KW - Semiconductor KW - Upconversion KW - Nanoparticle KW - Fluorescence KW - Surface group analysis KW - NIR KW - Absolute fluoreometry KW - Integrating sphare spectroscopy KW - Optical probe KW - Assay KW - Thiol ligand PY - 2017 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-41366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - The European Upconversion Network: From the Design of Photon-upconverting Nanomaterials to (Biomedical) Applications (CM1403) WG1 Materials Research & Photophysical Characterization N2 - Lanthanide-doped photon-upconversion nanoparticles (UCNPs) have been in the focus of many research activities in the material and life sciences over the last 15 years because of their potential to convert light between different spectral regions and their unique photophysical properties. In order to fully exploit the application potential of these fascinating nanomaterials, a number of challenges has to be overcome such as the low brightness particularly of small UCNPs and the reliable quantification of the excitation power density (P)-dependent upconversion luminescence (UCL). Here, the need and requirements on the characterization of the optical properties of UCNPs are discussed with special focus on the reliabiliy and comparability of relative and quantitative luminescence measurements and prerequisites for their standardization. T2 - COST Treffen CY - Aveiro, Portugal DA - 26.06.2017 KW - Upconversion KW - Nanoparticle KW - Fluorescence KW - NIR KW - Absolute fluorometry KW - Integrating sphere spectroscopy KW - Reference maerial KW - Standardization KW - Quantum yield PY - 2017 AN - OPUS4-41367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weigert, Florian T1 - Probing the bright and dark fraction of core-shell CdSe nanocrystals with single particle spectroscopy N2 - "The optical properties of semiconductor nanocrystals (SCNC) are controlled by constituent material, particle size, and surface chemistry, specifically the number of dangling bonds favoring nonradiative deactivation. This can lead to a distribution of photoluminescence Quantum yields (PL QY) amongst the SCNC particles, i.e., mixtures of “bright” and “grey” or “dark” SCNCs. Particularly the number of absorbing, yet not emitting particles can have a significant effect on the PL quantum yield obtained in ensemble measurements, leading to ist underestimation. The “dark fraction” is not assessable in common ensemble measurements; it can be probed only on a single particle level using a confocal laser scanning microscope coupled with an AFM. Such a setup was used to study core‐shell CdSe SCNCs with different shells and surface chemistries. Special emphasis was dedicated to correlate brightness, blinking, dark fraction, and decay kinetics of the single SCNCs with the ensemble PL QY and the PL decay kinetics. The results of this study can help to identify new synthetic routes and surface modifications to colloidally and photochemically stable SCNCs with a PL QY of close to unity." T2 - Summer School "EXCITING NANOSTRUCTURES" CY - Bad Honnef, Germany DA - 17.07.2017 KW - Semiconductor KW - Nanoparticle KW - Quantum dot KW - Flourescence KW - CdSe KW - Shell KW - Surface chemistry KW - Single particle spectroscopy PY - 2017 AN - OPUS4-41192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dhamo, Lorena T1 - Syntheses and characterization of 2-4nm AgInS2/ZnS quantum dots N2 - Ternary semiconductors Quantum Dots (t-QDs) like AgInS (AIS) QDs are interesting alternatives to Cd-based QDs for applications as optical active materials in light-emitting diodes (LEDs), solar concentrators and solar cells as well as as biodiagnostic tools, respectively. AIS QDs exhibit broad photoluminescence (PL) spectra in the visible and near infrared, which are tunable by size and chemical composition (ratio of components or doping). In order to enhance the PL quantum yield (PL QY or Fpl) and prevent material deterioration and oxidation, these QDs are covered by ZnS shell. Here we show a spectroscopic study of differently colored AIS QDs synthesized in water, evaluating their PL properties, their PL QY and their PL decay. The simple aqueous synthesis that avoids further ligand exchange steps for bioanalytical applications, the tunable emission color, the high PL QY, the high absorption coefficients and the long lifetime make these t-QDs promising Cd-free materials as biodiagnostic tools or optical active materials. T2 - Summer School "EXCITING NANOSTRUCTURES" CY - Bad Honnef, Germany DA - 17.07.2017 KW - Semiconductor KW - Nanoparticle KW - Quantum dot KW - Flourescence KW - Synthesis KW - Spectral multiplexing KW - Ternary quantum dot PY - 2017 AN - OPUS4-41173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Method development for metal detection at cellular levels N2 - An overview about different analytical approaches will be presented of how to detect metals in individual biological cells by use of ICP-MS. For this purpose, we are using different sample introduction systems for ICP-MS for detection, imaging and quantification of metals at cellular levels. By use of laser ablation, we have studied the up-take by and distribution of nanoparticles in single cells. Recently we have developed staining techniques to measure protein and DNA content of cells and identifying the cell status by immunoassays using metal-tagging of antibodies. New research based on cell arrays will be shortly discussed. Using pneumatic nebulization and microdroplet generation, we have also studied the up-take of nanoparticles and toxic metals as well as essential elements in single cells using different ICP-MS mass spectrometric concepts (sector field instrument, triple-quad instrument, time of flight (CyTOF) instrument). The different ICP-MS based methods will be compared concerning their analytical figures of merit and their strengths and weaknesses will be evaluated. T2 - Metallomics 2017 CY - Vienna, Austria DA - 14.08.2017 KW - Single cell analysis KW - Laser ablation KW - Nanoparticles KW - ICP-MS PY - 2017 AN - OPUS4-41690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Gorris, H.H. T1 - Perspectives and challenges of photon-upconversion nanoparticles - Part I: routes to brighter particles and quantitative spectroscopic studies N2 - Lanthanide-doped photon-upconversion nanoparticles (UCNPs) have been the Focus of many Research activities in materials and life sciences in the last 15 years because of their potential to convert light between different spectral regions and their unique photophysical properties. To fully exploit the application potential of These facinating nanomaterials, a number of challenges have to be overcome, such as the low brightness, particularly of small UCNPs, and the reliable quantification of the excitation-power-density-dependent upconversion luminescence. In this series of critical Reviews, recent developments in the design, Synthesis, optical-spectroscopic characterization, and application of UCNPs are presented with Special Focus on bioanalysis and the life sciences. Here we guide the reader from the Synthesis of UCNPs to different concepts to enhance their luminescence, including the required optical-spectroscopic assessment to quantify material Performance; surface modification strategies and bioanalytical applications as well as selected examples of the use of UCNPs as reporters in different Assay formats are addressed in part II. Future Trends and challenges in the field of upconversion are discussed with Special emphasis on UCNP Synthesis and material characterization, particularly quantitative luminescence studies. KW - Fluorescence KW - Lanthanide KW - Upconversion KW - Brightness KW - Quantification KW - Nanoparticle KW - Absolute fluorometry KW - NIR KW - IR KW - Quantum yield PY - 2017 DO - https://doi.org/10.1007/s00216-017-0499-z SN - 1618-2650 SN - 1618-2642 VL - 409 IS - 25 SP - 5855 EP - 5874 PB - Springer AN - OPUS4-41665 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Mousavi, M. ED - Thomasson, B. ED - Li, M. ED - Kraft, Marco ED - Würth, Christian ED - Andersson-Engels, S. T1 - Beam-profile-compensated quantum yield measurements of upconverting nanoparticles N2 - The quantum yield is a critically important parameter in the development of lanthanide-based upconverting nanoparticles (UCNPs) for use as novel contrast agents in biological imaging and optical reporters in assays. The present work focuses on the influence of the beam Profile in measuring the quantum yield (f) of nonscattering dispersions of nonlinear upconverting probes, by establishing a relation between f and excitation light power density from a rate equation analysis. A resulting 60% correction in the measured f due to the beam profile utilized for excitation underlines the significance of the beam profile in such measurements, and its impact when comparing results from different Setups and groups across the world. KW - Fluorescence KW - Lanthanide KW - Upconversion KW - Brithtness KW - Quantification KW - Nanoparticle KW - Absolute fluoreometry KW - NIR KW - IR KW - Quantum yield KW - Integrating sphere spectroscopy KW - Method PY - 2017 DO - https://doi.org/10.1039/c7cp03785f SN - 1463-9076 SN - 1463-9084 VL - 19 IS - 33 SP - 22016 EP - 22022 PB - Royal Society of Chemistry AN - OPUS4-42583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Otto, S. ED - Scholz, Norman ED - Behnke, Thomas ED - Heinze, K. T1 - Thermo-Chromium: A Contactless Optical Molecular Thermometer N2 - The unparalleled excited-state potential-energy landscape of the chromium(III)-based dye [1]3+ ([Cr(ddpd)2]3+; ddpd=N,N’-dimethyl-N,N’-dipyridin-2-ylpyridin-2,6-diamine) enables a strong dual emission in the near infrared region. The temperature dependence of this dual emission allows the use of [1]3+ as an unprecedented molecular ratiometric thermometer in the 210–373 K temperature range in organic and in aqueous media. Incorporation of [1]3+ in biocompatible nanocarriers, such as 100 nm-sized polystyrene nanoparticles and solutol micelles, provides nanodimensional thermometers operating under physiological conditions. KW - Temperature KW - Sensor KW - Dual emission KW - Fluorescence KW - Cr complex KW - Nano KW - Particle KW - Micelle KW - Probe KW - Environment PY - 2017 DO - https://doi.org/10.1002/chem.201701726 SN - 0947-6539 VL - 23 IS - 50 SP - 12131 EP - 12135 PB - Wiley-VCH AN - OPUS4-42539 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauli, Jutta A1 - Hoffmann, Katrin A1 - Würth, Christian A1 - Behnke, Thomas A1 - Resch-Genger, Ute T1 - Standardization of fluorescence measurements in the UV/vis/NIR/IR N2 - Photoluminescence techniques are amongst the most widely used Tools in the life sciences, with new and exciting applications in medical diagnostics and molecular Imaging continuously emerging. Advantages include their comparative ease of use, unique sensitivity, non-invasive character, and potential for Multiplexing, remote sensing, and miniaturization. General drawbacks are, however, signals, that contain unwanted wavelength- and polarization contributions from Instrument-dependent effects, which are also time-dependent due to aging of Instrument-components, and difficulties to measure absolute flourescence entensities. Moreover, scattering Systems require Special measurement geometries and the interest in new optical Reporters with Emission > 1000 nm strategies for reliable measurements in the second diagnostic for the comparison of material Performance and the rational designg of new flourophores with improved properties. Here, we present strategies to versatile method-adaptable liquid and solid flourescence Standards for different flourescence paramters including traceable Instrument calibration procedures and the design of integrating spere setups for the absolute measurements of emission spectra and Quantum yields in the wavelength Region of 350 to 1600 nm. Examples are multi-Emitter glasses, spectral flourescence Standards, and quantum yield Standards for the UV/vis/NIR. T2 - Conference on Molecular-Guided Surgery - Molecules, Devices, and Applications III CY - San Francisco, CA, USA DA - 28.01.2017 KW - Fluorescence KW - Reference material KW - Standard KW - Calibration KW - Nanoparticle KW - Absolute flourometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Quantum yield standard KW - Emission standards PY - 2017 SN - 978-1-5106-0539-8 DO - https://doi.org/10.1117/12.2255728 SN - 0277-786X VL - 10049 SP - 1 PB - Proceedings of SPIE AN - OPUS4-41783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radunz, Sebastian A1 - Tschiche, Harald Rune A1 - Moldenhauer, Daniel A1 - Resch-Genger, Ute T1 - Broad range ON/OFF pH sensors based on pKa tunable fluorescent BODIPYs N2 - A set of highly fluorescent, pH-responsive boron dipyrromethene dyes covering the pH range of 5-12 is presented for broad range pH measurements in mixed aqueous-organic median and polymer matrices. Readout in the intensity Domain with low cost and miniaturized Instrumentation utilizes reversible protonation induced switching ON of their initially completely quenched flourescence mediated by photoinduced electron Transfer. All dyes, rationally designed to reveal closely matching Absorption and Emission properties, are accessible via facile two-step reactions in Overall yields of up to 20%. By modifying the Substitution pattern of the meso-Aryl substiuent, the pKa values could be fine-tuned from 6 to 11. Integration of these molecules into polymeric films by a simple mixing procedure yielded reversible and longterm stable pH sensors for naked eye detection. KW - Fluorescence KW - Sensor KW - PH KW - Dye KW - BODIPY KW - Synthesis KW - Quantification KW - Film KW - Quantum yield KW - Lifetime KW - PET PY - 2017 DO - https://doi.org/10.1016/j.snb.2017.05.080 SN - 0925-4005 VL - 251 SP - 490 EP - 494 PB - Elsevier AN - OPUS4-41782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Method development for metal detection at cellular levels N2 - An overview about different analytical approaches will be presented of how to detect metals in individual biological cells by use of ICP-MS. For this purpose, we are using different sample introduction systems for ICP-MS for detection, imaging and quantification of metals at cellular levels. By use of laser ablation, we have studied the up-take by and distribution of metallic nanoparticles (Ag, Au) in single adherent cells (fibroblast cell line). Recently, we have developed staining techniques to image the protein (by a lanthanide containing chelate) and DNA (by an Ir-containing intercalator) distribution in single cells which can be combined with the nanoparticle studies. Additionally, we have developed an immunoassay by use of metal-tagged antibodies to identify the cell status of individual cells. Using pneumatic nebulization or microdroplet generation, we have also studied the up-take of nanoparticles and toxic metals as well as essential elements in single suspension cells using different ICP-MS mass spectrometric concepts (sector field instrument, triple-quad instrument, time of flight (CyTOF) instrument). For this purpose, the ICP-MS was operated in the single particle mode. First results of single cell ICP-MS (scICP-MS) will be presented for up-take of metallic (Ag) nanoparticles by THP 1 and macrophage cells and the strength of the different instruments will be discussed. T2 - 10th International Conference on Instrumental Methods of Analysis - IMA-2017 CY - Heraklion, Greece DA - 17.09.2017 KW - Imaging by LA-ICP-MS KW - Immunoassay KW - Metal-tagged antibodies PY - 2017 AN - OPUS4-42187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiggenhauser, Herbert T1 - Bauwerksdiagnostik – Indikatoren für die Zukunft T1 - Building Diagnostics - Indicators for the Future N2 - Vor dem Hintergrund der alternden Verkehrsinfrastruktur und des großen Bauwerksbestands allgemein gewinnt deren Zustandserfassung an Bedeutung. Durch die Einführung von Bauwerksmanagementsystemen und die Digitalisierung der Wirtschaft im Rahmen von Industrie 4.0 wird diese Entwicklung noch mehr Dynamik entfalten. Die Vernetzung von Zustandsdaten mit der Belastung, Wartung und Instandsetzung sowie der politischen Planung, wird eine hohe Bedeutung bekommen. Angesichts der Altersstruktur der Verkehrsinfrastruktur und begrenzter öffentlicher Gelder wird zukünftig eine selektive Instandsetzung von Bauwerken nach deren Zustandsnoten notwendig sein. Zerstörungsfreie Untersuchungsverfahren für Bauwerke nehmen in diesem Kontext eine wichtige Rolle ein, sie sollen die quantitativen Zustandsdaten erbringen und in die Datenbanken für Managementsysteme mit zuverlässigen und objektiven Messdaten füllen. KW - Bauwerksdiagnostik KW - Zerstörungsfreie Prüfung KW - Infrastruktur PY - 2017 DO - https://doi.org/10.1002/bate.201771003 SN - 1437-0999 VL - 94 IS - 10 SP - 675 EP - 675 PB - Ernst & Sohn CY - Berlin AN - OPUS4-42618 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niederleithinger, Ernst A1 - Herbrand, M. A1 - Müller, M. T1 - Monitoring von Querkraftversuchen an Spannbetondurchlaufträgern mit Ultraschall und Codawelleninterferometrie T1 - Monitoring of shear tests on prestressed concrete continuous beams using ultrasound and coda wave interferometry N2 - Zusammenfassung Im Rahmen eines Forschungsvorhabens an der RWTH Aachen wurden mehrere Spannbetondurchlaufträger bis zum Versagen belastetet. Neben umfangreicher konventioneller Messtechnik wurden zusätzlich innovative Messmethoden durch die Bundesanstalt für Materialforschung und –prüfung (BAM) getestet. Darunter waren eingebettete Ultraschall-Transducer, deren Daten mit einer neuartigen Methode, der Codawelleninterferometrie (CWI), ausgewertet wurden. Dieses Verfahren detektiert auch kleinste Änderungen im Signal und in der Wellengeschwindigkeit gegenüber einer Referenzmessung. Hiermit können Belastungs- und Strukturänderungen sowie Schäden sehr viel sensibler angezeigt werden als bei konventionellen Ultraschallmessungen. Durch eine Modifikation des Verfahrens mit gleitender Referenz können aber auch starke Veränderungen im Material, wie sie bei Bruchversuchen auftreten, erfasst werden. In den Versuchen gelang es mit Netzwerken aus bis zu 20 Ultraschall-Transducern, Spannungskonzentrationen und Rissbildungen qualitativ zu detektieren und zu verfolgen, ohne dass die Sensoren direkt am Ort der Änderung angebracht sein müssen. N2 - Abstract In the framework of a research project at RWTH Aachen University, a set of large scale post-tensioned concrete continuous beams has been loaded until failure. In addition to conventional measurement techniques, innovative methods like embedded ultrasonic transducers have been applied by the Bundesanstalt für Materialforschung und -prüfung (BAM). The data acquired with theses transducers has been processed with a novel method called coda wave interferometry (CWI). This technique is able to detect even very small changes in the ultrasonic signal and in wave velocity. Loads or structural changes as well as damages can be detected with a much higher sensitivity compared to conventional measurements. Using a modification of the technique with step-wise referencing larger changes in the material can be followed as well. In the experiments, networks of up to 20 ultrasonic transducers have been used. Stress concentrations and crack formation have been detected and monitored qualitatively, without having to place the transducers directly at the place of interest. KW - Ultraschall KW - Codawelleninterferometrie KW - Brücken KW - Belastung KW - Monitoring PY - 2017 SN - 0005-6650 SN - 1436-4867 VL - 92 IS - November SP - 474 EP - 481 PB - Springer CY - Düsseldorf AN - OPUS4-42677 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Challenges and examples for quantitative fluorescence measurements > 800 nm with semiconductor and lanthanide-doped nanocrystals N2 - There is an increasing interest in molecular and nanoscale with emission > 800 nm and recently also > 1000 nm for bioanalysis, medical diagnostics, bioimaging, and safety barcodes. Mandatory for the comparison of different emitter classes and the rational design of the next generation of reporters for the short wavelength infrared (SWIR) Region are reliable and quantitative photoluminescence measurements in this challenging wavelength region. This is of special relevance for nanocrystalline emitters like semiconductor quantum dots and rods as well as lanthanide-based upconversion and downconversion nanocrystals, where surface states and the accessibility of emissive states by quenchers largely control accomplishable photoluminescence quantum yields and hence, signal sizes and detection sensitivities from the reporter side. Such measurements are currently hampered by the lack of suitable methods and standards for instrument calibration and validation and quantum yield standards with emission > 800 nm and especially > 1000 nm. In this respect, we present the design of integrating sphere setups for absolute and excitation power density-dependent measurements of emission spectra and photoluminescence quantum yields in the wavelength Region of 650 to 1650 nm including calibration strategies and first candidates for potential fluorescence standards. Subsequently, the photoluminescence properties of different types of nanocrystals are presented including the upconversion and downconversion emission of differently sized and surface functionalized lanthanide-doped nanoparticles and photoluminescence quenching effects are quantified. T2 - SHIFT 2017 CY - Teneriffa, Spain DA - 13.11.2017 KW - Upconversion KW - Nanoparticle KW - Absolute fluorometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Fluorescence KW - Surface chemistry KW - Deactivation pathways KW - Semiconductor quantum dot KW - SWIR KW - Quantum yield PY - 2017 AN - OPUS4-43203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Instrument Calibration and Standardization of Fluorescence Measurements in the UV/vis/NIR/IR N2 - Comparison of fluorescence measurements performed on different fluorescence instruments, analyte quantification from fluorescence intensities as well as the determination of fluorescence quantum yields require instrument calibration and consideration of the wavelength-dependent instrument-specific quantities spectral photon flux reaching the sample and spectral responsivity. Here, we present guidelines and recommendations for the qualification of fluorescence instruments and introduce suitable chromophore-based reference materials. Moreover, the design concepts of the different BAM fluorescence standards are discussed. T2 - COST 2017 CY - Turku, Finland DA - 03.04.2017 KW - Fluorescence KW - Dye KW - Glass KW - Calibration KW - Fluorescence standard KW - Integrating sphere spectroscopy KW - Fluorescence quantum yield KW - Instrument qualification KW - Quality assurance KW - NIR KW - IR PY - 2017 AN - OPUS4-43174 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Foundations N2 - NDT-CE methods for foundations. T2 - NDT&E Advanced Training Workshop CY - Berlin, Germany DA - 05.07.2017 KW - NDT KW - Foundations KW - Pile integrity testing KW - Parallel seismic KW - Crosshole sonic logging PY - 2017 AN - OPUS4-42663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya T1 - Quantification of surface groups on core-shell polymer particles with optical spectroscopy N2 - Polymer nanoparticles (NPs) are of increasing importance for a wide range of applications in the material and life sciences. This includes their use as carriers for dye molecules and drugs, multichromophoric reporters for signal enhancement strategies in optical assays, targeted probes in bioimaging studies, and nanosensors.[1] Application-relevant properties of such NPs include their size, morphology, colloidal stability, and ease of surface functionalization with e.g., sensor molecules and targeting ligands. Many of these features as well as the interaction of NPs with their microenvironment are closely linked to the knowledge of the chemical nature and total number of surface groups as well as the number of surface functionalities accessible for subsequent coupling reactions of differently sized ligands, biomolecules or reporter molecules. This underlines the importance of simple, robust, reliable, and validated methods, which can be employed for the characterization of a broad variety of particle systems independent of their optical properties, i.e., scattering or the presence of encoding dyes.[2] In this respect, we assessed a variety of conventional and newly developed colorimetric or fluorometric labels for the optical surface group analysis, utilizing e.g., changes in intensity and/or color for signal generation.[3] Moreover, novel cleavable and multimodal reporters were developed which consist of a reactive group, a cleavable linker, and an optically active moiety, chosen to contain also heteroatoms for straightforward method validation by elemental analysis, ICP-OES, ICP-MS or NMR. In contrast to conventional labels measured bound at the particle surface, which can favor signal distortions by scattering and encoding dyes, cleavable reporters can be detected colorimetrically or fluorometrically both attached at the particle surface and after quantitative cleavage of the linker in the transparent supernatant after particle removal e.g., by centrifugation. Here, we present first results obtained for the optical quantification of carboxylic and amino groups on a series of self-made NPs with different types of labels and compare their potential and drawbacks for surface group analysis. T2 - Jubiläumskongress "Chemie bewegt" 2017 CY - Berlin, Germany DA - 10.09.2017 KW - Nanoparticle KW - Surface groups KW - Optical assays KW - Carboxy and amin PY - 2017 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-43212 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zavoiura, Oleksandr T1 - RNA detection by FRET systems based on peptide nucleic acid-QD conjugates N2 - Today, 40 % of the world’s population live in areas with a significant risk of dengue infection. Early and reliable diagnosis of dengue virus (DENV) is essential to provide the patients with the required medical care and prevent spreading of the disease. Conventional methods for DENV diagnosis like PCR and virus isolation can be used in laboratory settings, yet are difficult to implement in point-of-care diagnostics, requiring simple, selective, fast, and sensitive detection schemes. We present here a novel approach for the detection of DENV, via its RNA, with optical read-out that relies on RNA-catalyzed fluorophore transfer onto a semiconductor quantum dot (QD) and Förster resonance energy transfer (FRET). For this RNA assay, peptide nucleic acid (PNA) oligomers were used as highly specific capture and reporter probes. PNA exhibits remarkable affinity towards RNA as well as extremely high chemical and enzymatic stability. The capture probe, which is immobilized on a QD acting as FRET donor, bears a nucleophile at the N-terminus and the reporter probe is modified with an organic dye acting as FRET acceptor. The presence of DENV genomic RNA in the sample triggers a transfer of the dye onto the QD, signaled by FRET between the QD and the dye. A unique advantage of this system is the ability of one RNA molecule to trigger multiple transfer reactions, thereby amplifying the fluorescence signal. This assay together with the exceptional brightness of QDs and outstanding hybridization properties of PNA allows for highly specific and sensitive detection of DENV RNA in the sub-nM range. T2 - MAF 2017 CY - Brügge, Belgium DA - 10.09.2017 KW - QD KW - RNA detection KW - PNA KW - Click chemistry PY - 2017 AN - OPUS4-43230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Guhrenz, C. ED - Sayevich, V. ED - Weigert, Florian ED - Hollinger, E. ED - Reichhelm, A. ED - Gaponik, N. ED - Eychmüller, A. T1 - Transfer of Inorganic-Capped Nanocrystals into Aqueous Media N2 - We report on a novel and simple approach to surface ligand design of CdSe-based nanocrystals (NCs) with biocompatible, heterobifunctional polyethylene glycol (PEG) molecules. This method provides high transfer yields of the NCs into aqueous media with preservation of the narrow and symmetric emission bands of the initial organic-capped NCs regardless of their interior crystal structure and surface chemistry. The PEG-functionalized NCs show small sizes, high photoluminescence quantum yields of up to 75%, as well as impressive optical and colloidal stability. This universal approach is applied to different fluorescent nanomaterials (CdSe/CdS, CdSe/CdSCdxZn1-xS, and CdSe/CdS/ZnS), extending the great potential of organic-capped NCs for biological applications. KW - Fluorescence KW - Ligand exchange KW - Quantum dot KW - Surface chemistry KW - Semiconductor nanocrystal KW - Quantum yield KW - Lifetime KW - Dispersibillity KW - Colloid PY - 2017 DO - https://doi.org/10.1021/acs.jpclett.7b02319 VL - 8 IS - 22 SP - 5573 EP - 5578 PB - The Journal of Physical Chemistry Letters AN - OPUS4-43377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Effect of surface chemistry on optical, chemical and electronic properties of blue luminescent graphene quantum dots N2 - Due to their unique physical properties, particularly their electronic and luminescent properties, graphene quantum dots (GQDs) are expected to be suitable for a wide range of applications in bioimaging, electro-optical and photonic materials or energy harvesting among others.1 Tuning the surface chemistry provides an efficient approach to modulate the fluorescence and distinct electronic properties of GQDs.2 Nevertheless, the role of surface chemistry on the electronic structure of GQDs remains poorly understood. In this presentation, we will compare systematically the electronic and chemical structures of GQDs functionalized with carboxylic and aminated groups to those of non-functionalized GQDs, combining theoretical and experimental approaches, here various photon-based spectroscopies. First, the electronic structure of GQDs was characterized by soft X-ray absorption (XA) and X-ray emission (XE) spectroscopies, probing unoccupied and occupied electronic states, respectively, at the carbon K edge for the first time. The interpretation of the XA/XE spectra was done based on theoretical calculations. Then, the chemical structure of the GQDs was characterized in situ by ATR-FTIR in water, thereby accounting for the importance of the interface between GQDs and water believed to play a central role in the chemical reactivity and the optical properties. We previously demonstrated that monitoring the OH vibrations of water molecules during exposure to humid air was a powerful method to probe H-bonding environment around carbon nanomaterials.3 For GQDs, clear surface-dependent water adsorption profiles are observed and discussed. Finally, UV/Vis absorption and photoluminescence measurements were done to characterize the optical properties of these GQDs. Our results suggest that the surface chemistry of the GQDs affects significantly their electronic structure and optical properties. These findings will contribute to an improved understanding of the structure–activity relationship of GQDs and other carbon nanomaterials with surface modifications. T2 - MRS Fall Meeting 2017 CY - Boston, USA DA - 26.11.2017 KW - Carbon KW - Nanoparticle KW - Fluorescence KW - NIR KW - IR KW - Surface chemistry KW - Deactivation pathways KW - Lifetime KW - Size KW - Giant carbon dot KW - Quantum yield PY - 2017 AN - OPUS4-43494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Iznaguen, Hassan T1 - Homogeneity of dispersed brominated flame retardants (HBCD) in polystyrene by LA-ICP-MS and XRF N2 - To investigate the release or migration of flame retardants from polypropylene (PP) and polysytrene (PS) samples with a defined content of flame retardants as additives were prepared and used. Therefore a distinct 1,2,5,6,9,10-hexabromocyclododecane HBCD concentration of 1 wt.% in PS resp. a specified bromodiphenylether (BDE-209) of 0.1 wt.% in PP is defined. For the preparation of the samples granular PP or PS are extruded together with the BFR additives. Even the result of this process may lead to homogenous partitions of the BFR additives. So, the distribution of these additives must be proven before using the samples in an experimental setup for weathering studies. In accordance to the regulation of RoHS (2011/65/EU) , where the use of XRF is recommended for the proof of flame retardants in electronic consumer products, we use this method as a reference to the laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Therefore we present the correlation of these experiments. The experimental setup for the XRF experiment is like a standard addition: in cavities, which are introduced in the sample plates subsequently, solutions of defined concentration of flame retardants are put in there. According to the idea of standard addition, we get an information of the originating mass fraction of flame retardant in each sample and we can monitor the release and migration of these additives during/after the weathering experiments with high precision. An internal standard of HBCD is added as a marker and can be analyzed after the weathering experiment. T2 - 8th European Weathering Symposium EWS CY - Wien, Austria DA - 20.09.2017 KW - LA-ICP-MS KW - XRF KW - BFR PY - 2017 AN - OPUS4-43313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramirez Caro, Alejandra T1 - A spectroscopic study of the superplasticizer effect on early cement hydration N2 - Besides their plasticizing effect, superplasticizers (SPs) are known to retard the hydration of inorganic systems such as cement. Despite their frequent use, the understanding of these highly complex systems is still limited and the relevant parameters, which control the interaction between SPs, and cement components and reaction products are in the focus of ongoing research activities.[1] Optical methods have been successfully used for the analysis and monitoring of the interactions between a broad variety of nanoscale and molecular systems like nanoparticles of various chemical composition and different types of organic ligands or biomolecules. The potential of these methods to study processes at the interface between (hydrated) particles and the fluid phase at a very early stage of concrete formation could reveal possible mechanisms of interaction. This investigation focuses on the study of organic/inorganic mixtures consisting of cement (CEM) and cement phases (C3S and C3A) in the presence of polycarboxylate ether and organic dyes in aqueous solution (particularly alkali resistant dyes) at a water to powder ratio of 1. Diffuse reflectance as well as steady state and time resolved fluorescence spectroscopy of the above mentioned mixtures were evaluated. Based upon changes of the intensity of the reflectance and fluorescence signal and spectral changes of the dye, acting as optical reporter, a model for the interactions of dye, PCE and cement (including different cement phases) was derived which describes the very first stage of cement hydration. T2 - 2nd International Conference on Polycarboxylate Superplasticizers CY - München, Germany DA - 27.09.2017 KW - Cement KW - Superplasticizers KW - Dyes KW - Spectroscopy PY - 2017 AN - OPUS4-43365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Resch-Genger, Ute ED - Schäferling, Michael T1 - Luminescent nanoparticles for chemical sensing and imaging N2 - The implementation of fluorescent methods is of outstanding importance in the field of optical chemical sensor Technology and biosciences. Their bioanalytical applications are manifold including fluorescence microscopy, fluorescence in situ hybridization, DNA sequencing, fluorescence-activated cell sorting, immunoassays, analysis of DNA and Protein microarrays, and quantitative PCR, just to name a few examples. Particularly, fluorescence microscopy is a valuable method in the versatile field of biomedical imaging methods which nowadays utilizes different fluorescence Parameters like emission wavelength/Color and lifetime for the discrimination between different targets. Sectional Images are available with confocal microscopes. Tissue, cells or single cellular compartments can be stained and visualized with fluorescent dyes and biomolecules can be selectively labeled with fluorescent dyes to Monitor biomolecular interactions inside cells or at Membrane bound receptors. On the other hand , fluorophores can act as indicator (or "molecular probe") to visualize intrinsically colorless and non-fluorescent ionic and neutral analytes such as pH, Oxygen (pO2), metal ions, anions, hydrogen peroxide or bioactive small organic molecules such as Sugars or nucleotides. Thereby, their photoluminescent properties (fluorescence or phoporescence intensity, exitation and/or Emission wavelength, emission lifetime or anisotropy) respond to the presence of these species in their immediate Environment. In general, the use of luminescent probes has the advantage that they can be delivered directly into the sample, and detected in a contactless remote mode. By now, these probes are often encapsulated in different types of nanoparticles (NPs) made from (biodegradable) organic polymers, biopolymers or inorganic materials like silica or bound to their surface. KW - Fluorescence KW - Upconversion KW - NIR KW - Sensor KW - Nanoparticle KW - Surface chemistry KW - Quantum yield KW - Liftetime KW - Nanocrystal KW - Lanthanide KW - Semiconductor KW - Polymer KW - Silica KW - Imaging KW - Application KW - Dye KW - Quantum dot PY - 2017 SN - 978-3-319-48260-6 SN - 978-3-319-48259-0 DO - https://doi.org/10.1007/978-3-319-48260-6_5 SN - 1573-8086 SP - 71 EP - 109 PB - SPRINGER INTERNATIONAL PUBLISHING AG CY - Cham, Schweiz AN - OPUS4-44011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Scholz, Norman ED - Behnke, Thomas T1 - Determination of the critical micelle concentration of neutral and ionic surfactants with fluorometry, conductometry, and surface tension - a method comparison N2 - Micelles are of increasing importance as versatile carriers for hydrophobic substances and nanoprobes for a wide range of pharmaceutical, diagnostic, medical, and therapeutic applications. A key Parameter indicating the Formation and stability of micelles is the critical micelle concentration (CMC). In this respect, we determined the CMC of common anionic, cationic, and non-ionic surfactants fluorometrically using different fluorescent probes and fluorescence Parameters for Signal detection and ompared the results with conductometric and surface Tension measurements. Based upon These results, requirements, Advantages, and pitfalls of each methods are discussed. Our study underlines the versatility of fluorometric methods that do not impose specific requirements on surfactants and are especially suited for the quantification of very low CMC values. Conductivity and surface Tension measurements yield smaller uncertainties particularly for high CMC values, yet are more time- and substance consuming and not suitable for every surfactant. KW - Fluorescence KW - Methods KW - Critical micelle concentration (CMC) KW - Conductometry KW - Fluorescence probe KW - Dye KW - Nile Red KW - Pitfalls KW - Method evaluation KW - Uncertainty PY - 2017 DO - https://doi.org/10.1007/s10895-018-2209-4 SN - 1053-0509 SN - 1573-4994 VL - 28 IS - 1 SP - 465 EP - 476 AN - OPUS4-43905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Huang, K. A1 - Liu, H. A1 - Kraft, Marco A1 - Shikha, S. A1 - Zheng, X. A1 - Agren, H. A1 - Würth, Christian A1 - Resch-Genger, Ute A1 - Zhang, Y. T1 - A protected excitation-energy reservoir for efficient upconversion luminescence N2 - Lanthanide-doped upconversion nanoparticles (UCNPs) are of great interest for biomedical applications. Currently, the applicability of UCNP bionanotechnology is hampered by the generally low luminescence intensity of UCNPs and inefficient energy Transfer from UCNPs to surface-bound chromophores used e.g. for photodynamic therapy or analyte sensing. In this work, we address the low-Efficiency issue by developing versatile core-Shell nanostructures, where high-concentration sensitizers and activators are confined in the core and Shell Region of representative hexagonal NaYF2:Yb,Er UCNPs. After Doping concentration optimization, the sensitizer-rich core is able to harvest/accumulate more excitation energy and generate almost one order of Magnitude higher luminescence intesity than conventional homogeneously doped nanostructures. At the same time, the activator Ions located in the Shell enable a ~6 times more efficient resonant energy Transfer from UCNPs to surface-bound acceptor dye molecules due to the short distance between donor-acceptor pairs. Our work provides new insights into the rational design of UCNPs and will greatly encrease the General applicability of upconversion nanotechnologies. KW - Fluorescence KW - Lanthanide KW - Upconversion KW - Brightness KW - Quantification KW - Nanoparticle KW - Absolute fluorometry KW - NIR KW - IR KW - Quantum yield KW - Integrating sphere spectroscopy KW - Method KW - Energy transfer KW - Shell KW - Particle architecture PY - 2017 DO - https://doi.org/10.1039/c7nr06900f SN - 2040-3372 SN - 2040-3364 VL - 10 IS - 1 SP - 250 EP - 259 PB - The Royal Society of Chemistry AN - OPUS4-43893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Phukphatthanachai, Pranee T1 - An alternative approach of using PE frits for the quantification of sulfur in copper metals and its alloys by isotope dilution LA-ICP-MS N2 - This is the first time that PE frits were used to quantify sulfur in copper and its alloys by isotope dilution combined with LA-ICP-MS: an alternative approach for sample preparation. The following properties of the PE frit meet the requirements for isotope dilution LA-ICPMS: porous material, thermo plastic (melting point >100°C), chemical resistance (nitric acid >70%) and high adsorption efficiency. The breakthrough, however, as a support material, especially when comparing the PE frit with other materials such gelatin or sodium silicate is the low blank, which is only two times of the gas flow blank (2.3-4.0 x 10⁴ cps). Additionally, the porosity of the frit was considered, as it directly affects the adsorption efficiency for the sample solution, which is present in the cavities of the frit. Adsorption efficiency was studied by depositing sulfur standards with varying sulfur amounts (0, 2, 5, 10, 20, 40 and 80 µg S) on the frits. The remaining sulfur which was not absorbed by the frit was rinsed off and was measured by ICP-MS. This indirect method shows that more than 99.5 % of the loaded sulfur was absorbed by the frit. Such high absorption efficiency is completely sufficient for a support material to be used in LA-ICP-IDMS. The so prepared frits with increasing sulfur amount were measured by LA-ICP-MS showing a good linearity between 0 µg S and 40 µg S with a correlation coefficient r2 of 0.9987 and sensitivity of 3.4x10⁴ cps µgˉ¹ for 32S. Three copper reference materials produced by BAM were selected to develop and validate the LA-ICP-IDMS procedure. The IDMS technique was applied to these samples as follows: the samples were spiked, dissolved, digested and then the digest was adsorbed on the frits. T2 - Winter Conference on Plasma Spectrochemistry 2018 CY - Amelia Islands, FL, USA DA - 08.01.2018 KW - Laser ablation KW - Isotope dilution mass spectrometry KW - Sulfur quantification PY - 2018 AN - OPUS4-43996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Wang, Cui ED - Otto, S. ED - Dorn, M. ED - Kreidt, E. ED - Lebon, J. ED - Srsan, L. ED - di Martino-Fumo, P. ED - Gerhards, M. ED - Seitz, M. ED - Heinze, K. T1 - Deuterierter molekularer Rubin mit Rekord-Lumineszenzquantenausbeute N2 - Der kürzlich publizierte Chrom(III)-Komplex 13+([Cr(ddpd)2]3+) zeigt in wässriger Lösung unter Umgebungsbedingungen eine bemerkenswert starke Emission im nahen Infrarot-Bereich mit einer Emissionswellenlänge von 775 nm. Geschicktes Ligandendesign verhindert strahlungslose Desaktivierungsprozesse wie Photosubstitution, Rück-Intersystem-Crossing und trigonale Verzerrungen und führt damit zu einer Phosphoreszenzlebensdauer im Bereich von Mikrosekunden. In Abwesenheit von Energieakzeptoren wie molekularem Sauerstoff verbleibt nur Energietransfer zu hochenergetischen Oszillatoren der Liganden und Lösungsmittelmoleküle wie beispielsweise OH- und CH-Streckschwingungen als Desaktivierungspfad. Selektive Deuterierung der ddpd-Liganden und der Lösungsmittel l-sst die Effizienz dieser Oszillatoren bei der Desaktivierung angeregter Zustände erkennbar werden. Gezieltes Ausschalten dieser Relaxationspfade führt zu einer Quantenausbeute von 30% und einer Lebensdauer von 2.3 Millisekunden bei Raumtemperatur in Lösung – Rekordwerte für einen Komplex, der auf dem Element Chrom basiert. Diese fundamentalen Erkenntnisse ebnen den Weg für gezieltes Ligandendesign zur Synthese lumineszierender Komplexe mit gut verfügbaren Übergangsmetallen. KW - Fluorescence KW - Quantum yield KW - Ligand design KW - Cr(III) KW - Complex KW - Oxygen sensor KW - NIR KW - Fluorescence lifetime PY - 2018 DO - https://doi.org/10.1002/ange.201711350 SN - 1521-3757 VL - 130 IS - 4 SP - 1125 EP - 1130 PB - Wiley-VCH Verlag & Co. KGaA CY - Weinheim AN - OPUS4-44043 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Martynenko, Irina ED - Baimuratov, A. S. ED - Osipova, V. A. ED - Kuznetsova, V. A. ED - Purcell-Milton, F. ED - Rukhlenko, I. D. ED - Fedorov, A. V. ED - Gun'ko, Y. K. ED - Baranov, A. V. T1 - Excitation energy dependence of the photoluminescence quantum yield of core/shell CdSe/CdS quantum dots and correlation with circular dichroism N2 - Quantum dot (QD) based nanomaterials are very promising materials for the fabrication of optoelectronic devices like solar cells, light emitting diodes (LEDs), and photodetectors as well as as reporters for chemo- and biosensing and bioimaging. Many of These applications involve the monitoring of changes in photoluminescence intensity and energy transfer processes which can strongly depend on excitation wavelength or energy. In this work, we analyzed the excitation energy dependence (EED) of the photoluminescence quantum yields (PL QYs) and decay kinetics and the circular dichroism (CD) spectra of CdSe/CdS core/shell QDs with different thicknesses of the surface passivation shell. Our results demonstrate a strong correlation between the spectral position of local maxima observed in the EED of PL QY and the zero-crossing points of the CD profiles. Theoretical analysis of the energy band structure of the QDs with effective mass approximation suggests that these structures could correspond to exciton energy levels. This underlines the potential of CD spectroscopy for the study of electronic energy structure of chiroptically active nanocrystals which reveal quantum confinement effects. KW - Fluorescence KW - Semiconductor KW - Nanoparticle KW - Surface chemistry KW - Quantum yield KW - Lifetime KW - Nanocrystal KW - Cysteine KW - Thiol KW - Ligand KW - Quantum dot KW - CdSe KW - Exciton KW - Circular dichroism KW - Theory KW - Excitation spectra KW - Excitation energy dependence PY - 2017 DO - https://doi.org/10.1021/acs.chemmater.7b04478 SN - 0897-4756 SN - 1520-5002 VL - 30 IS - 2 SP - 465 EP - 471 PB - ACS Publications AN - OPUS4-44034 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Wang, Cui ED - Otto, S. ED - Dorn, M. ED - Kreidt, E. ED - Lebon, J. ED - Srsan, L. ED - di Martino-Fumo, P. ED - Gerhards, M. ED - Seitz, M. ED - Heinze, K. T1 - Deuterated Molecular Ruby with Record Luminescence Quantum Yield N2 - The recently reported luminescent chromium(III) complex 13+ ([Cr(ddpd)2]3+; ddpd=N,N’-dimethyl-N,N’-dipyridine-2-yl-pyridine-2,6-diamine) shows exceptionally strong near-IR emission at 775 nm in water under ambient conditions (F=11%) with a microsecond lifetime as the ligand design in 13+ effectively eliminates non-radiative decay pathways, such as photosubstitution, back-intersystem crossing, and trigonal twists. In the absence of energy acceptors, such as dioxygen, the remaining decay pathways are energy transfer to high energy solvent and ligand oscillators, namely OH and CH stretching vibrations. Selective deuteration of the solvents and the ddpd ligands probes the efficiency of these oscillators in the excited state deactivation. Addressing these energytransfer pathways in the first and second coordination sphere furnishes a record 30% quantum yield and a 2.3 millisecond lifetime for a metal complex with an earth-abundant metal ion in solution at room temperature. KW - Fluorescence KW - Quantum yield KW - Ligand design KW - Cr(III) KW - Complex KW - Oxygen sensor KW - NIR KW - Fluorescence lifetime PY - 2018 DO - https://doi.org/10.1002/ange.201711350 SN - 1521-3773 VL - 57 IS - 4 SP - 1112 EP - 1116 PB - Wiley-VCH Verlag & Co. KGaA CY - Weinheim AN - OPUS4-44045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Automated determination of genotoxicity of nanoparticles with DNA-based optical assays - The NANOGENOTOX project N2 - The overall interest in nanotoxicity, triggered by the increasing use of nanomaterials in the material and life sciences, and the synthesis of an ever increasing number of new functional nanoparticles calls for standardized test procedures1,2 and for efficient approaches to screen the potential genotoxicity of these materials. Aiming at the development of fast and easy to use, automated microscopic methods for the determination of the genotoxicity of different types of nanoparticles, we assess the potential of the fluorometric γH2AX assay for this purpose. This assay, which can be run on an automated microscopic detection system, relies on the detection of DNA double strand breaks as a sign for genotoxicity3. Here, we provide first results obtained with broadly used nanomaterials like CdSe/CdS and InP/ZnS quantum dots as well as iron oxide, gold, and polymer particles of different surface chemistry with previously tested colloidal stability and different cell lines like Hep-2 and 8E11 cells, which reveal a dependence of the genotoxicity on the chemical composition as well as the surface chemistry of these nanomaterials. These studies will be also used to establish nanomaterials as positive and negative genotoxicity controls or standards for assay performance validation for users of this fluorometric genotoxicity assay. In the future, after proper validation, this microscopic platform technology will be expanded to other typical toxicity assays. T2 - SPIE 2018 CY - San Francisco, USA DA - 27.01.2018 KW - Nanoparticle KW - Fluorescence KW - Surface chemistry KW - Size KW - Assay KW - Microscopy KW - Nanotoxicity KW - Toxicity KW - Automation KW - Calibration KW - Standard PY - 2018 AN - OPUS4-44186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, Katrin T1 - Time-resolved flow cytometry N2 - The fast identification of a large number of analytes or events is increasingly required in bioanalytical, diagnostic, and security applications. The versatility and straightforward use make multiparametric fluorescence techniques particularly interesting as detection techniques. An established method for high-throughput single-cell and single-particle measurements is flow cytometry (FCM). Using only spectral encoding without further intensity information, state-of-the-art instruments equipped with several light sources and detectors can resolve almost 20 different color codes. However, this is not sufficient to answer complex research questions, e.g. in cell biology and immunology. In contrast, routine applications demand low-cost and sometimes even portable instruments and thus a minimum number of instrument components. Thus, there are currently two main research directions in FCM: the development of methods that can either address increasingly complex analytical challenges or provide low-cost and robust approaches for routine multiplex analyses. Common spectral multiplexing approaches face limitations in both directions. On the one hand, spectral overlap of labels restricts the number of codes and makes elaborate correction schemes necessary. On the other hand, even for lower degrees of multiplexing often a sophisticated optical setup is needed. An alternative to spectral multiplexing and intensity encoding is to exploit the luminescence lifetime (LT) as an encoding parameter. This can allow for extending the parameter space in combination with spectral encoding or result in more simple and compact devices due to fewer optical components. The availability of fast electronics enables miniaturized and portable lifetime measurement setups at relatively low cost. LT-FCM requires to master LT determination with a limited number of detected photons due to the short interaction time of the encoded objects with the laser spot. In this study, we address this issue for time-domain cytometry and present a novel lifetime flow cytometry (LT-FCM) platform based on a compact setup and straightforward time-domain measurements utilizing LT-encoded luminescent beads. Moreover, we present the realization of a first bioanalytical assay with LT-encoded beads. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Fluorescence KW - Time-resolved KW - Flow cytometry KW - Lifetime-encoding KW - Bead-based assays PY - 2019 AN - OPUS4-47708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Büttner, C. T1 - Anwendung seismischer Abbildungsverfahren auf Ultraschallecho-Daten von Verschlussbauwerken unter Tage N2 - Ein Endlager für radioaktive Abfälle muss auf Dauer vor dem Eindringen von Wasser geschützt werden. Aus diesem Grund errichtete die Bundesgesellschaft für Endlagerung (BGE) ein Verschlussbauwerk als InSitu Versuch im Endlager Morsleben. Hierfür wurde eine bergmännische Auffahrung mit Salzbeton verfüllt. Zusätzliche in regelmäßigen Abständen eingebaute Trennbleche sollen der Ausbreitung eventueller Risse entgegenwirken. Das Versuchsobjekt wurde mit Ultraschallmessungen bezüglich der Lage und Orientierung möglicher Risse untersucht. Diese Messungen wurden an der Stirnfläche des Salzbetonkörpers durchgeführt. Für die Datenakquisition fand ein neuartiges Messsystem Anwendung, mit welchem ein seismisches Akquisitionsschema realisiert werden kann. Dieses setzt sich aus mehreren Prüfköpfen zusammen, welche sowohl als Sender als auch als Empfänger fungieren. Somit lassen sich auch größere Sender-Empfänger-Abstände realisieren. Vor der Bearbeitung der realen Messdaten wurde ein realitätsnahes synthetisches Modell erstellt, mit welchem die Abbildung eines Risses, eines eingebauten Monitoring-Instruments sowie des ersten Trennbleches in einer Tiefe von 8 m untersucht wurden. Die generierten synthetischen Daten wurden nach minimaler Preprozessierung mittels Kirchhoff-Prestack-Tiefenmigration sowie Reverse Time Migration (RTM) in Tiefensektionen umgewandelt. Insbesondere bei der Abbildung steilstehender Reflektoren lieferte die RTM hier ein besseres Ergebnis. Im Anschluss wurden reale Messdaten in der gleichen Weise bearbeitet. Zusätzlich wurden die Ergebnisse mit denen der Synthetic-Aperture-Focusing-Technique (SAFT) verglichen. Dieses Verfahren ist der Kirchhoff-Migration sehr ähnlich und findet in der zerstörungsfreien Werkstoffprüfung routinemäßig Anwendung. Es stellte sich heraus, dass der RTM Algorithmus in einigen Fällen ein realitätsnäheres Abbild liefert. Die Resultate von Kirchhoff-Migrationund SAFT-Rekonstruktion sind hingegen sehr ähnlich. Alle Verfahren lokalisierten in gleicher Weise Risse in verschiedenen Tiefenlagen, welche hauptsächlich oberflächenparallel orientiert sind. Diese werden auch von Bohrungen bestätigt. Besonders herauszustellen ist die deutliche Abbildung des Trennbleches in großer Tiefe, was bisher noch nicht eindeutig gelungen war. T2 - Jahrestagung der Deutschen geophysikalischen Gesellschaft CY - Brunswick, Germany DA - 03.03.2019 KW - Ultraschall KW - Verschlussbauwerk KW - Endlagerung KW - RTM KW - Kirchhoff PY - 2019 AN - OPUS4-47705 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wang, Cui A1 - Resch-Genger, Ute T1 - Luminescent TOP nanosensors for simultaneously measuring temperature, oxygen, and pH at a single excitation wavelength N2 - Two nanosensors for simultaneous optical measurements of temperature (“T”), oxygen (“O”), and pH (“P”) have been designed. These “TOP” nanosensors are based on 100 nm-sized silica-coated polystyrene nanoparticles (PS-NPs) doped with the near infrared emissive oxygen- and temperature-sensitive chromium(III) complex ([Cr(ddpd)2][BPh4]3 CrBPh4)[1][2] and an inert reference fluorescence dye (Nile Red NR or 5,10,15,20tetrakis-(pentafluorophenyl) porphyrin TFPP) and are covalently labeled with the pHsensitive fluorophore fluorescein isothiocyanate (FITC). These emitters can be excited at the same wavelength and reveal distinguishable emission spectra suitable for ratiometric intensity-based and time-resolved studies in the visible and near infrared spectral region. The core-shell nanostructure of these sensors reveals high colloidal stability in various aqueous media. Studies in PBS buffer solutions and in a model body liquid demonstrate the applicability of the TOP nanosensors for optically detecting the three bioanalytically and biologically relevant analytes temperature, oxygen and pH simultaneously at the same position. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Sensor KW - Nanoparticle KW - Nanosensor KW - Fluorescence KW - Oxygen KW - Temperature KW - pH KW - Ratiometric KW - Lifetime KW - NIR KW - Cr(III) complex KW - FITC KW - Dye KW - Environment KW - Medical diagnostics PY - 2019 AN - OPUS4-47698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wang, Cui T1 - Ratiometric luminescent TOP nanosensors for simultaneously measuring temperature, oxygen, and pH at a single excitation wavelength N2 - Two nanosensors for simultaneous optical measurements of temperature (“T”), oxygen (“O”), and pH (“P”) have been designed. These “TOP” nanosensors are based on 100 nm-sized silica-coated polystyrene nanoparticles (PS-NPs) doped with the near infrared emissive oxygen- and temperature-sensitive chromium(III) complex ([Cr(ddpd)2][BPh4]3 CrBPh4)[1][2] and an inert reference fluorescence dye (Nile Red NR or 5,10,15,20-tetrakis-(pentafluorophenyl) porphyrin TFPP) and are covalently labeled with the pH-sensitive fluorophore fluorescein isothiocyanate (FITC). These emitters can be excited at the same wavelength and reveal distinguishable emission spectra suitable for ratiometric intensity-based and time-resolved studies in the visible and near infrared spectral region. The core-shell nanostructure of these sensors reveals high colloidal stability in various aqueous media. Studies in PBS buffer solutions and in a model body liquid demonstrate the applicability of the TOP nanosensors for optically detecting the three bioanalytically and biologically relevant analytes temperature, oxygen and pH simultaneously at the same position. T2 - 2nd European Biosensor Symposium CY - Florenz, Italy DA - 18.02.2019 KW - Sensor KW - Nanoparticle KW - Nanosensor KW - Fluorescence KW - Oxygen KW - Temperature KW - pH KW - Ratiometric KW - Lifetime KW - NIR KW - Cr(III) complex KW - FITC KW - Dye KW - Environment KW - Medical diagnostics PY - 2019 AN - OPUS4-47700 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vössing, Konrad T1 - Air-coupled ferroelectret ultrasonic transducers for nondestructive testing of wood in through transmission and reflection mode N2 - The necessity and demand for nondestructive testing of wood-based materials which can automatically scan huge areas of wood is increasing. Air-coupled ultrasound (ACU) is used to detect defects and damage without altering the structure permanently. Using through transmission it is possible to detect even small holes and missing adhesive. If only one side of an object is accessible the reflection mode is preferred at the expense of a reduced resolution and penetration depth. Novel ferroelectret transducers with a high signal-to-noise ratio (SNR) enable a high-precision structure recognition. The transducers made of cellular polypropylene (PP) are quite suitable for ACU testing due to their extremely low Young’s modulus and low density which result in a favorable acoustic impedance for the transmission of ultrasonic waves between the transducer and air. Thus, defects such as delamination, rot, and cracks can be detected. Promising results were obtained under laboratory conditions with frequencies from 90 kHz to 200 kHz. The advantage of these ACU transducers is that they do not require contact to the sample, are accurate, and cost effective. Ultrasonic quality assurance for wood is an important attempt to increase the acceptance of wooden structures and towards sustainability in civil engineering in general. T2 - International Conference on Sustainable Materials, Systems and Structures CY - Rovinj, Croatia DA - 20.03.2019 KW - Air-coupled ultrasound KW - Cellular polypropylene KW - Wood KW - Nondestructive Testing KW - Defect detection PY - 2019 AN - OPUS4-47683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vössing, Konrad A1 - Gaal, Mate A1 - Niederleithinger, Ernst T1 - Air-coupled ferroelectret ultrasonic transducers for nondestructive testing of wood in through transmission and reflection mode N2 - The necessity and demand for nondestructive testing of wood-based materials which can automatically scan huge areas of wood is increasing. Air-coupled ultrasound (ACU) is used to detect defects and damage without altering the structure permanently. Using through transmission it is possible to detect even small holes and missing adhesive. If only one side of an object is accessible the reflection mode is preferred at the expense of a reduced resolution and penetration depth. Novel ferroelectret transducers with a high signal-to-noise ratio (SNR) enable a high-precision structure recognition. The transducers made of cellular polypropylene (PP) are quite suitable for ACU testing due to their extremely low Young’s modulus and low density which result in a favorable acoustic impedance for the transmission of ultrasonic waves between the transducer and air. Thus, defects such as delamination, rot, and cracks can be detected. Promising results were obtained under laboratory conditions with frequencies from 90 kHz to 200 kHz. The advantage of these ACU transducers is that they do not require contact to the sample, are accurate, and cost effective. Ultrasonic quality assurance for Wood is an important attempt to increase the acceptance of wooden structures and towards sustainability in civil engineering in general. T2 - International Conference on Sustainable Materials, Systems and Structures CY - Rovinj, Croatia DA - 20.03.2019 KW - Air-coupled ultrasound KW - Cellular polypropylene KW - Wood KW - Nondestructive Testing KW - Defect detection PY - 2019 SP - 28 EP - 33 AN - OPUS4-47682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst ED - Gabrijel, Ivan ED - Grosse, Christian ED - Skazlić, Marijan T1 - Ultrasonic monitoring of structural concrete elements N2 - Ultrasonic transmission measurements are used to monitor concrete elements mostly on a laboratory scale since decades. Recently, coda wave interferometry, a technique adapted from seismology, has been introduced to civil engineering experiments. It can be used to reveal subtle changes in concrete samples and even large construction elements without having a transducer directly at the location where the change is taking place. The methodology works best with embedded transducers to avoid coupling issues or excessive environmental influence. These transducers can be used for newly built and existing structures. Recently, large concrete beams have been equipped with a network of transducers and loaded until failure. Using code wave interferometry, it was possible to visualize stress fields and damaged areas. This paper gives an overview of the state of the art, recent results achieved at BAM and a task list for further results and development. T2 - International Conference on Sustainable Materials, Systems and Structures (SMSS 2019) CY - Rovinj, Croatia DA - 20.3.2019 KW - Concrete KW - Ultrasound KW - Monitoring KW - coda wave interferometry PY - 2019 SN - 978-2-35158-227-5 SP - 1 EP - 11 PB - RILEM Publications S.A.R.L. CY - Paris, France AN - OPUS4-47677 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arakawa, Akihiro A1 - Jakubowski, Norbert A1 - Koellensperger, G. A1 - Theiner, S. A1 - Schweikert, A. A1 - Flemig, Sabine A1 - Iwahata, D. A1 - Traub, Heike A1 - Hirata, T. T1 - Quantitative Imaging of Silver Nanoparticles and Essential Elements in Thin Sections of Fibroblast Multicellular Spheroids by High Resolution Laser Ablation Inductively Coupled Plasma Time-of-Flight Mass Spectrometry N2 - We applied high resolution laser ablation inductively coupled plasma time-of-flight mass spectrometry (LA-ICP-TOF-MS) with cellular spatial resolution for bioimaging of nanoparticles uptaken by fibroblast multicellular spheroids (MCS). This was used to quantitatively investigate interactions of silver nanoparticles (Ag NPs) and the distributions of intrinsic minerals and biologically relevant elements within thin sections of a fibroblast MCS as a three-dimensional in vitro tissue model. We designed matrix-matched calibration standards for this purpose and printed them using a noncontact piezo-driven array spotter with a Ag NP suspension and multielement standards. The limits of detection for Ag, Mg, P, K, Mn, Fe, Co, Cu, and Zn were at the femtogram (fg) level, which is sufficient to investigate intrinsic minerals in thin MCS sections (20 μm thick). After incubation for 48 h, Ag NPs were enriched in the outer rim of the MCS but not detected in the core. The localization of Ag NPs was inhomogeneous in the outer rim, and they were colocalized with a single-cell-like structure visualized by Fe distribution (pixel size of elemental images: 5 × 0.5 μm). The quantitative value for the total mass of Ag NPs in a thin section by the present method agreed with that obtained by ICP-sector field (SF)-MS with a liquid mode after acid digestion. KW - Laser ablation KW - ICP-MS KW - Imaging KW - Nanoparticle KW - Cell KW - Spheroid PY - 2019 UR - https://pubs.acs.org/doi/10.1021/acs.analchem.9b02239 DO - https://doi.org/10.1021/acs.analchem.9b02239 SN - 0003-2700 VL - 91 IS - 15 SP - 10197 EP - 10203 PB - American Chemical Society, ACS Publications CY - Washington D.C. AN - OPUS4-48719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauli, Jutta T1 - Certified Fluorescence Quantum Yield Standards as New Optical Reference Materials N2 - Luminescence techniques are amongst the most commonly used analytical methods in life and material sciences due to their sensitivity and their nondestructive and multiparametric character. Photoluminescence signals are, however, affected by wavelength, polarization and time dependent instrument specific effects, and provide only relative intensities. This hampers the comparability of fluorescence measure-ments and calls for simple tools for instrument characterization and the quantification of measured fluorescence intensities. Well characterized fluorescence standards for instrument calibration and performance validation (IPV) can be used as references for fluorescence signals. Of special importance is the correct determination of photoluminescence quantum yields (QF) (number of emitted per absorbed photons) that provides a direct comparison of the fluorescence efficiency of emitters. Such well characterized standards have been successfully developed by BAM for the relative determination of f values of transparent solutions of molecular and nanoscale emitters in the wavelength range from 350 and 1100 nm and will be soon certified. These standards can also be used to evaluate integrating sphere setups, which are increasingly being used for absolute measurements of QF values. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2091 KW - Fluoreszenz KW - Referenzmaterial PY - 2019 AN - OPUS4-47795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Arakawa, Akihiro T1 - Localization of cells and exposed nanoparticles in three-dimensional in vitro tissue analog measured by means of an elemental microscopy based on LA-ICP-TOF-MS N2 - Metallic nanoparticles (NPs) are currently applied in a variety of consumer products and are also attractive for medical applications. With their widespread use, the potential for human exposure to NPs — either intended or unintended — is increasing. Therefore, many studies have evaluated the toxicity and transport mechanism of NPs. In comparison with two-dimensional cultured cells, multicellular spheroids (MCS) look promising to be used as a three-dimensional cellular model, having unique advantages in nanoparticle studies due to the fact that interactions with excreted extracellular matrix can be investigated. Fibroblast cells are one of the most important cell systems to express a microenvironment by excreting an abundant extracellular matrix. For bioimaging laser ablation inductively coupled-plasma mass spectrometry (LA-ICP-MS) is used in this investigation to study the interaction of metallic NPs with MCS for multi-element detection offering a wide dynamic range. As a mass spectrometer we have applied a time-of-flight (TOF) instrument for (quasi-) simultaneous detection of all isotopes of elements of interest. The aim of this study is to investigate the localization of silver (Ag) NPs exposed to fibroblast MCSs by means of LA-ICP-TOF-MS. In addition, for demonstrating elemental microscopy we chose phosphorous (31P) and iron (56Fe) to visualize regions of enriched extracellular matrix and single cells, respectively. In this presentation, we show that exposed Ag NPs are highly accumulated at the same position of single cells in an outer rim of fibroblast MCSs. T2 - 7th International Symposium on Metallomics CY - Warsaw, Poland DA - 30.06.2019 KW - Nanoparticle KW - Laser ablation KW - ICP-MS KW - Multicellular spheroid PY - 2019 AN - OPUS4-48425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Musnier, B. A1 - Wegner, Karl David A1 - Comby-Zerbino, C. A1 - Trouillet, V. A1 - Jourdan, M. A1 - Häusler, I. A1 - Antoine, R. A1 - Coll, J.-L. A1 - Resch-Genger, Ute A1 - Le Guevel, X. T1 - High photoluminescence of shortwave infrared-emitting anisotropic surface charged gold nanoclusters N2 - Incorporating anisotropic surface charges on atomically precise gold nanoclusters (Au NCs) led to a strong absorption in the nearinfrared region and could enable the formation of self-assembled Au NCs xhibiting an intense absorption band at ∼1000 nm. This surface modification showed a striking enhancement of the photoluminescence in the Shortwave Infrared (SWIR) region with a quantum yield as high as 6.1% in water. KW - Gold nanoclusters KW - SWIR photoluminescence KW - Self-assembly PY - 2019 DO - https://doi.org/10.1039/C9NR04120F VL - 11 IS - 25 SP - 12092 EP - 12096 PB - Royal Society of Chemistry AN - OPUS4-48305 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - A review on ultrasonic monitoring of concrete: coda wave interferometry and beyond N2 - The propagation of ultrasonic waves in concrete is affected by its micro- and macro-structure, geometry and properties as well as external influences as stress, temperature or moisture. In addition, age and degradation have a strong influence. Therefore, Ultrasound has been used to monitor concrete samples and structures since decades. However, early applications using conventional techniques as time-of flight or changes in amplitudes have been limited to detect changes in a late stage close to serviceability or ultimate load states. Around 2000, several new, more sensitive techniques adopted from geophysics or other field of material sciences have been introduced to research in ultrasonic monitoring of concrete. The most discussed methodologies are coda wave interferometry, a technique which allows to detect very subtle changes from repeated ultrasonic measurements. Nonlinear acoustic techniques help to identify e. g. cracks even in an inhomogeneous background. Both techniques can be combined. This paper reviews methods and results achieved so far on the laboratory scale and with full scale models the directions for future research and application is given as well. T2 - QNDE 2019 CY - Portland, OR, USA DA - 14.07.2019 KW - Ultrasound KW - Coda wave interferometry KW - Concrete KW - Nonlinear KW - Monitoring PY - 2019 AN - OPUS4-48688 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Kaiser, Martin ED - Würth, Christian ED - Kraft, Marco ED - Soukka, T. T1 - Explaining the influence of dopant concentration and excitation power density on the luminescence and brightness of β-NaYF4:Yb3+,Er3+ nanoparticles: Measurements and simulations N2 - We assessed the influence of Yb3+ and Er3+ dopant concentration on the relative spectral distribution, quantum yield (  UC), and decay kinetics of the upconversion luminescence (UCL) and particle brightness (BUC) for similarly sized (33 nm) oleate-capped -NaYF4:Yb3+,Er3+ upconversion (UC) nanoparticles (UCNPs) in toluene at broadly varied excitation power densities (P). This included an Yb3+ series where the Yb3+ concentration was varied between 11%–21% for a constant Er3+ concentration of 3%, and an Er3+ series, where the Er3+ concentration was varied between 1%–4% for a constant Yb3+ concentration of 14%. The results were fitted with a coupled rate equation model utilizing the UCL data and decay kinetics of the green and red Er3+ emission and the Yb3+ luminescence at 980 nm. An increasing Yb3+ concentration favors a pronounced triphotonic population of 4F9/2 at high P by an enhanced back energy transfer (BET) from the 4G11/2 level. Simultaneously, the Yb3+-controlled UCNPs absorption cross section overcompensates for the reduction in  UC with increasing Yb3+ concentration at high P, resulting in an increase in BUC. Additionally, our results show that an increase in Yb3+ and a decrease in Er3+ concentration enhance the color tuning range by P. These findings will pave the road to a deeper understanding of the energy transfer processes and their contribution to efficient UCL, as well as still debated trends in green-to-red intensity ratios of UCNPs at different P. KW - Nanoparticle KW - Lanthanide KW - Upconversion nanoparticle KW - Fluorescence KW - Integration sphere spectroscopy KW - Mechanism KW - Lifetime, synthesis KW - Surface chemistry KW - Yb(III) KW - Er(III) KW - Energy transfer KW - Absolute measurement KW - Quantum yield PY - 2019 DO - https://doi.org/10.1007/s12274-019-2450-4 SN - 1998-0124 SN - 1998-0000 VL - 12 IS - 8 SP - 1871 EP - 1879 PB - Springer AN - OPUS4-48880 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rietsch, P. A1 - Soyka, J. A1 - Brülls, S. A1 - Er, J. A1 - Hoffmann, Katrin A1 - Beerhues, J. A1 - Sakar, B. A1 - Resch-Genger, Ute A1 - Eigler, S. T1 - Fluorescence of a chiral pentaphene derivative derived from the hexabenzocoronene Motif N2 - A new fluorescent pentaphene derivative is presented that differs from hexabenzocoronene (HBC) by one carbon atom in the basal plane skeleton. A 500% increased fluorescence quantum yield is measured compared to the HBC derivative. The pentaphene compound, obtained by a modified Scholl oxidation, is also emissive in the solid-state, due to the packing motif in the crystal. KW - Hexabenzocoronenes KW - Pentaphenes KW - Solid-state fluorescence PY - 2019 DO - https://doi.org/10.1039/c9cc05451k SN - 1364-548X N1 - Corrigendum: Chemical Communications 55 (2019) 12879 VL - 55 IS - 71 SP - 10515 EP - 10518 PB - The Royal Society of Chemistry AN - OPUS4-48908 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Löhr, Konrad A1 - Borovinskaya, O. A1 - Tourniaire, G. A1 - Panne, Ulrich A1 - Jakubowski, Norbert T1 - Arraying of single cells for quantitative high throughput laser ablation ICP-TOF-MS N2 - Arraying of single cells for mass spectrometric analysis is a considerable bioanalytical challenge. In this study, we employ a novel single cell arraying technology for quantitative analysis and isotopic fingerprinting by laser ablation inductively coupled plasma time-of-flight mass spectrometry (LA-ICP-TOF-MS). The single cell arraying approach is based on a piezo-acoustic microarrayer with software for automated optical detection of cells within the piezo dispense capillary (PDC) prior to arraying. Using optimized parameters, single cell occupancy of >99%, high throughput (up to 550 cells per hour), and a high cell recovery of >66% is achieved. LA-ICP-TOF-MS is employed to detect naturally occurring isotopes in the whole mass range as fingerprints of individual cells. Moreover, precise quantitative determination of metal-containing cell dyes is possible down to contents of ∼100 ag using calibration standards which were produced using the same arrayer. KW - Laser ablation KW - Cell KW - Array KW - ICP-MS PY - 2019 DO - https://doi.org/10.1021/acs.analchem.9b00198 SN - 0003-2700 SN - 1520-6882 VL - 91 IS - 18 SP - 11520 EP - 11528 PB - American Chemical Society (ACS Publications) CY - Washington AN - OPUS4-48985 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geißler, Daniel T1 - Development of reference materials (WP1) and reference methods (WP2) for the standardisation of concentration measurements of extracellular vesicles N2 - BAM provides leading expertise in preparation, characterisation and application of fluorescent reference standards and biomedical relevant nanomaterials, as well as in traceable, absolute, and quantitative fluorometric measurements of transparent and scattering systems in the ultraviolet, visible, and near infrared spectral region. BAM will prepare solid low-RI particles in WP1, will develop reference methods to determine the fluorescence intensity and RI of reference materials in WP2, and will measure the fluorescence intensity of EVs in biological test samples of WP3. T2 - EMPIR 18HLT01 "MetVesII" Kick-off meeting CY - Delft, The Netherlands DA - 17.06.2019 KW - Reference materials KW - Reference methods KW - Extracellualr vesicles PY - 2019 AN - OPUS4-48813 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lopez-Serrano Oliver, Ana A1 - Haase, A. A1 - Peddinghaus, A. A1 - Wittke, D. A1 - Jakubowski, Norbert A1 - Luch, A. A1 - Grützkau, A. A1 - Baumgart, S. T1 - Mass cytometry enabling absolute and fast quantification of silver nanoparticle uptake at the single cell level N2 - In the last decades, significant efforts have been made to investigate possible cytotoxic effects of metallic nanoparticles (NPs). Methodologies enabling precise information regarding uptake and intracellular distribution of NPs at the single cell level remain to be established. Mass cytometry (MC) has been developed for high-dimensional single cell analyses and is a promising tool to quantify NP−cell interactions. Here, we aim to establish a new MC-based quantification procedure to receive absolute numbers of NPs per single cell by using a calibration that considers the specific transmission efficiency (TE) of suspended NPs. The current MC-quantification strategy accept TE values of complementary metal solutions. In this study, we demonstrate the different transmission behavior of 50 nm silver NPs (AgNP) and silver nitrate solution. We have used identical AgNPs for calibration as for in vitro-differentiated macrophages (THP-1 cell line) in a time- and dose-dependent manner. Our quantification relies on silver intensities measuring AgNPs in the same detection mode as the cells. Results were comparable with the TE quantification strategy using AgNPs but differed when using ionic silver. Furthermore, intact and digested cell aliquots were measured to investigate the impact of MC sample processing on the amount of AgNPs/cell. Taken together, we have provided a MC-specific calibration procedure to precisely calculate absolute numbers of NPs per single cell. Combined with its unique feature of multiplexing up to 50 parameters, MC provides much more information on the single cell level than single cell-inductively coupled plasma mass spectrometry (SC-ICP-MS) and, therefore, offers new opportunities in nanotoxicology. KW - ICP-MS KW - Nanoparticle KW - Cell KW - SC-ICP-MS KW - Mass cytometry PY - 2019 DO - https://doi.org/10.1021/acs.analchem.9b01870 SN - 0003-2700 SN - 1520-6882 VL - 91 IS - 18 SP - 11514 EP - 11519 PB - American Chemical Society (ACS Publications) CY - Washington AN - OPUS4-48986 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Environmental sustainability and –stability of materials concerning the migration of pollutants N2 - In addition to previously reported results on the accelerated weathering of polystyrene samples (PS) containing 1 wt. % hexabromocyclododecane (HBCD), we present the first results of our investigations of polypropylene samples (PP) containing 0.1 wt. % BDE-209. All studied polymer samples were exposed to a defined weathering schedule in a climate chamber in accordance to regulation EN ISO 4892-3:2006. For the determination of BDE-209 in the collected raining water the samples were prepared in accordance to a validated protocol. Before the analyses each sample was spiked with isotopically labeled BDE-209. Subsequently the samples were extracted with isooctane. The obtained extracts were concentrated, and the resulting solutions were analyzed by GC/MS. Additionally, the total bromine content was monitored for the weathered and untreated samples using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and X-ray fluorescence analysis (XRF) as a non-destructive and rapid method. In general, the resulting data from the accelerated weathering will be compared to those from the natural weathering experiments. Here, the surfaces of the test pieces were analyzed by LA-ICP-MS and XRF as well. Moreover, soil bed tests were conducted in a well characterized model soil. This soil (boulder-clay, sand with 12 % loam, particle size in total 0.2-4 mm) is filled in a free-draining basin inside of an air-conditioned cellar. In this manner, TOC, water capacity and humidity are recorded parameters. To induce a leaching process from the samples by the raining water, the target water content is calculated to 8%. The actual humidity is measured by a tensiometer, assuring the duration of the raining period. A defined humidity is a fundamental parameter for a biological activity in the soil. The test polymers were placed up to the half in the soil. Microbial activity of the soil is monitored by a reference polymer (polyurethane) and should induce the release of HBCD and BDE-209 out of the test materials. These released analytes will be captured by passive samplers (silicone tubes) placed in a distinct distance to the polymer samples in the soil. The soil bed experiments are complementary to the weathering experiments due to the biological activity in the soil. T2 - Goldschmidt 2019 CY - Barcelona, Spain DA - 18.08.2019 KW - Pollutants KW - Environmental simulation KW - Migration PY - 2019 AN - OPUS4-49803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Luminescent nanocrystals – Photophysics and applications for lifetime multiplexing N2 - Bioanalytical, diagnostic, and security applications require the fast and sensitive determination of a steadily increasing number of analytes or events in parallel in a broad variety of detection formats.[1,2] Ideal candidates for spectral encoding and multiplexing schemes are luminescent nanocrystals like semiconductor quantum dots (QDs), particularly Cd-containing II/VI QDs with their narrow and symmetric emission bands. With the availability of relatively simple and inexpensive instrumentation for time-resolved fluorescence measurements, similar strategies utilizing the compound-specific parameter fluorescence lifetime or fluorescence decay kinetics become increasingly attractive.[3-5] The potential of different types of QDs like II/VI, III/V and Cd-free ternary QDs such as AgInS (AIS) QDs for lifetime-based encoding and multiplexing has been, however, barely utilized, although the lifetimes of these nanocrystals cover a time windows which is barely accessible with other fluorophores. Here we present a brief insight into the photophysics of AIS QDs and show the potential of dye- and QD-encoded beads for lifetime-based encoding and detection schemes in conjunction with flow cytometry and fluorescence lifetime imaging microscopy T2 - Nanax 2019 CY - Hamburg, Germany DA - 16.09.2019 KW - Nano KW - Microparticle KW - Bead KW - Encoding KW - Lifetime KW - Multiplexing KW - Flow cytometry KW - Bead-based assay KW - Fluorescence KW - Dye KW - LT-FCM KW - Time-resolved flow cytometry KW - Method PY - 2019 AN - OPUS4-49039 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramirez Caro, Alejandra T1 - The Effect of Low Charge Polycarboxylate on C3A Passivation Monitored by Optical Spectroscopy N2 - Tricalcium aluminate (C3A) is less than 10 wt.% of the total cement composition; however, during hydration, the soluble C3A plays an important role in cement setting when mixed with the appropriate amount of sulfate.1 A good understanding about the balance of these components is therefore crucial to follow with the rapid growth of substitution materials and the rising levels of aluminate clinker. The aim of this investigation is the use of optical spectroscopy and in-situ X-ray diffraction utilizing a water-soluble organic dye (dye-S) to monitor early hydration of calcium aluminate (C3A) in the presence of 26 wt.% CaS04.2H2O (G) and PCE polymers with different charge densities (PCE-LC and PCE-HC). Phase characterization and optical evaluation were performed using in-situ X-ray diffraction and steady-state fluorescence and diffuse reflectance spectroscopy. Fluorescence spectroscopy of the reference C3A + dye-S revealed a fast decay in fluorescence intensity. However, in the presence of 26 wt.% G (C3A + dye-S + 26 wt.% G), a gradual increase in fluorescence intensity was observed in the first hours of reaction followed by a plateau that subsequently dropped in intensity after eight hours. The addition of PCE-LC and PCE HC to the mixture exhibited changes in the intensity threshold and overall a higher fluorescence intensity. Dye changes during hydration and structural changes will be further discussed. T2 - 3rd International Conference on Polycarboxylate Superplasticizers (PCE 2019) CY - Munich, Germany DA - 23.10.2019 KW - Dye KW - C3A KW - Optical Spectroscopy KW - Gypsum PY - 2019 AN - OPUS4-49343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramirez Caro, Alejandra T1 - Use of Optical Spectroscopy to Monitor Cement Hydration and Additive Effect N2 - Use of optical spectroscopy and fluorescence reporter (DFFL and dye-S) to visualize the effects of additives on the hydration of cement pastes as a fast, sensitive and monitoring method. T2 - Beirat Tagung CY - Berlin, Germany DA - 26.04.2019 KW - Cement KW - Optical Spectroscopy KW - Dye KW - Hydration KW - Superplasticizer PY - 2019 AN - OPUS4-49349 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Determining Photoluminescence Quantum Yields of Molecular and Nanocrystal Emitters in the UV/vis/NIR/SWIR N2 - The comparison of different emitter classes and the rational design of the next generation of molecular and nanoscale reporters require accurate and quantitative photo-luminescence measurements. This is of special importance for all photoluminescence applications in the life and material sciences and nanobiophotonics. In the following, procedures for the determination of the spectroscopic key parameter photoluminescence quantum yield, i.e., the number of emitted per absorbed photons, in the UV/vis/NIR/SWIR are presented including pitfalls and achievable uncertainties and material-specific effects related to certain emitter classes are addressed. T2 - Kolloqium National Center for Nanoscience and Technology CY - Peking, People's Republic of China DA - 18.10.2019 KW - Fluorescence KW - Quantum yield KW - Integrating sphere spectroscopy KW - Dye KW - Nanocrystal KW - NIR KW - SWIR KW - Quantum dot KW - Fluorescence standard KW - Uncertainty KW - Calibration PY - 2019 AN - OPUS4-49362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramirez Caro, Alejandra A1 - Pauli, Jutta A1 - Mota, Berta A1 - Crasselt, Claudia A1 - Artemeva, Elena A1 - Schmidt, Wolfram A1 - Resch-Genger, Ute T1 - A Spectroscopic Study of the Superplasticizer Effect on Early Cement Hydration N2 - Organic/inorganic mixtures were prepared from ordinary Portland cement (OPC), water (w/c 0.22), a fluorescent dye in aqueous solution (stable at alkaline pH; BAM-I), and two different comb shape polycarboxylates (PCEs), i.e., high charge (PCE-HC) and low charge (PCE-LC), respectively. Rheological and calorimetric measurements were performed prior to optical studies in order to select PCE concentrations. Absorption and fluorescence spectroscopy of the system OPC + BAM-I (CBAM-I) revealed maxima of dye BAM-I located at 645 nm and 663 nm, respectively. In presence of PCE-HC and PCE-LC, these mixtures displayed a small red shift in reflectance and a faster decrease in intensity compared to studies with CBAM-I; however, only slight differences were observed between the different PCEs. With time, all systems exhibited a decrease in intensity of BAM-I in absorption/reflectance and emission. This could be caused by dye adsorption and possibly decomposition when in contact with cement particles or hydration products. T2 - The Sixth International Symposium on Nanotechnology in Construction (NICOM6) CY - Hong Kong, China DA - 02.12.2018 KW - Cement KW - Optical Spectroscopy KW - Dye KW - Hydration PY - 2018 SP - 1 EP - 9 AN - OPUS4-49378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Nanocrystals with Luminescence in the vis, NIR and SWIR – Photophysics and Applications N2 - Luminescent nanocrystals like core/shell semiconductor quantum dots and lanthanide doped nanophosphors as well as gold nanoclusters with emission in the visible (vis) and particularly in the near infrared (NIR) and short wavelength infrared (SWIR) region have been increasingly used as reporters in the life sciences and for bioimaging studies in the last years. This has led to sophisticated core-shell particle architectures of different chemical composition utilizing semiconductor quantum dots and lanthanide-based nanocrystals and initiated the design of gold nanoclusters with different ligands. In addition, this led to an increasing number of quantitative spectroscopic studies focusing on the key performance parameter photoluminescence quantum yield to identify optimum particle structures. In the following, an overview of different classes of nanocrystalline emitters and their photophysics is provided and examples for the absolute characterization of the photoluminescence properties of these different vis/NIR/SWIR emitters are shown including excitation power density-dependent studies on the ensemble and single particle level. Also, the impact of such measurements on a profound mechanistic understanding of the underlying nonradiative deactivation pathways is highlighted as required for reporter design. T2 - MIMIT 2019 CY - Peking, People's Republic of China DA - 18.10.2019 KW - Fluorescence KW - Quantum yield KW - Integrating sphere spectroscopy KW - Dye KW - Nanocrystal KW - NIR KW - SWIR KW - Quantum dot KW - Lanthanide nanoparticle KW - Old nanocrystal KW - Imaging KW - Lifetime KW - Nanoparticle PY - 2019 AN - OPUS4-49361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zou, Q. A1 - Marcelot, C. A1 - Ratel-Ramond, N. A1 - Yi, X. A1 - Roblin, P. A1 - Frenzel, Florian A1 - Resch-Genger, Ute A1 - Eftekhari, A. A1 - Bouchet, A. A1 - Coudret, C. A1 - Verelst, M. A1 - Chen, X. A1 - Mauricot, R. A1 - Roux, C. T1 - Heterogeneous Oxysulfide@Fluoride Core/ Shell Nanocrystals for Upconversion-Based Nanothermometry N2 - Lanthanide (Ln3+)-doped upconversion nanoparticles (UCNPs) often suffer from weak luminescence, especially when their sizes are ultrasmall (less than 10 nm). Enhancing the upconversion luminescence (UCL) efficiency of ultrasmall UCNPs has remained a challenge that must be undertaken if any practical applications are to be envisaged. Herein, we present a Ln3+-doped oxysulfide@fluoride core/shell heterostructure which shows efficient UCL properties under 980nm excitation and good stability in solution. Through epitaxial heterogeneous growth, a ∼4 nm optically inert β-NaYF4 shell was coated onto ∼5 nm ultrasmall Gd2O2S:20%Yb,1%Tm. These Gd2O2S:20%Yb,1%Tm@NaYF4 core/shell UCNPs exhibit a more than 800-fold increase in UCL intensity compared to the unprotected core, a 180-fold increase in luminescence decay time of the 3H4 → 3H6 Tm3+ transition from 5 to 900 μs, and an upconversion quantum yield (UCQY) of 0.76% at an excitation power density of 155 W/cm2. Likewise, Gd2O2S:20%Yb,2%Er@NaYF4 core/shell UCNPs show a nearly 5000-fold increase of their UCL intensity compared to the Gd2O2S:20%Yb,2%Er core and a maximum UCQY of 0.61%. In the Yb/Er core−shell UCNP system, the observed variation of luminescence intensity ratio seems to originate from a change in lattice strain as the temperature is elevated. For nanothermometry applications, the thermal sensitivities based on thermally coupled levels are estimated for both Yb/Tm and Yb/Er doped Gd2O2S@NaYF4 core/shell UCNPs. KW - Upconversion nanoparticle KW - Nanosensor KW - Lanthanide KW - Surface coating KW - Quantum yield KW - Photophysic PY - 2022 DO - https://doi.org/10.1021/acsnano.2c02423 SN - 1936-0851 SP - 1 EP - 11 PB - ACS Publications AN - OPUS4-55440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Preiss, J. A1 - Kage, Daniel A1 - Hoffmann, Katrin A1 - Martínez, T. J. A1 - Resch-Genger, Ute A1 - Presselt, M. T1 - Ab initio prediction of fluorescence lifetimes involving solvent environments by means of COSMO and vibrational broadening N2 - The fluorescence lifetime is a key property of fluorophores that can be utilized for microenvironment probing, analyte sensing, and multiplexing as well as barcoding applications. For the rational design of lifetime probes and barcodes, theoretical methods have been developed to enable the ab initio prediction of this parameter, which depends strongly on interactions with solvent molecules and other chemical species in the emitters' immediate environment. In this work, we investigate how a conductor-like screening model (COSMO) can account for variations in fluorescence lifetimes that are caused by such fluorophore−solvent interactions. Therefore, we calculate vibrationally broadened fluorescence spectra using the nuclear ensemble method to obtain distorted molecular geometries to sample the electronic transitions with time-dependent density functional theory (TDDFT). The influence of the solvent on fluorescence lifetimes is accounted for with COSMO. For example, for 4-hydroxythiazole fluorophore containing different heteroatoms and acidic and basic moieties in aprotic and protic solvents of varying polarity, this approach was compared to experimentally determined lifetimes in the same solvents. Our results demonstrate a good correlation between theoretically predicted and experimentally measured fluorescence lifetimes except for the polar solvents Ethanol and acetonitrile that can specifically interact with the heteroatoms and the carboxylic acid of the thiazole derivative. KW - Fluorescence lifetime KW - Ab initio calculation KW - COSMO KW - Conductor-like screening model PY - 2018 DO - https://doi.org/10.1021/acs.jpca.8b08886 SN - 1089-5639 SN - 1520-5215 VL - 122 IS - 51 SP - 9813 EP - 9820 PB - American Chemical Society CY - Washington, DC AN - OPUS4-47177 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Billimoria, K. A1 - Andresen, Elina A1 - Resch-Genger, Ute A1 - Goenaga-Infante, H. T1 - A Strategy for Quantitative Imaging of Lanthanide Tags in A549 Cells Using the Ratio of Internal Standard Elements N2 - One remaining handicap for spatially resolved elemental quantification in biological samples is the lack of a suitable internal standard (IS) that can be reliably measured across both calibration standards and samples. In this work, multielement quantitative intracellular imaging of cells tagged with lanthanide nanoparticles containing key lanthanides, e.g., Eu and Ho, is described using a novel strategy that uses the ratio of IS elements and LA-ICP-TOFMS analysis. To achieve this, an internal standard layer is deposited onto microscope slides containing either gelatin calibration standards or Euand Ho-tagged cell samples. This IS layer contains both gallium (Ga) and indium (In). Monitoring either element as an IS individually showed significant variability in intensity signal between sample or standards prepared across multiple microscope slides, which is indicative of the difficulties in producing a homogeneous film at intracellular resolution. However, normalization of the lanthanide signal to the ratio of the IS elements improved the calibration correlation coefficients from 0.9885 to 0.9971 and 0.9805 to 0.9980 for Eu and Ho, respectively, while providing a consistent signal to monitor the ablation behavior between standards and samples. By analyzing an independent quality control (QC) gelatin sample spiked with Eu and Ho, it was observed that without normalization to the IS ratio the concentrations of Eu and Ho were highly biased by approximately 20% in comparison to the expected values. Similarly, this overestimation was also observed in the lanthanide concentration distribution of the cell samples in comparison with the normalized data. KW - Nanoparticle KW - Nano KW - Luminescence KW - Quality assurance KW - Synthesis KW - Standardization KW - Reference material KW - ICP-MS KW - LA-ICP-MS KW - Quantification KW - Bioimaging PY - 2024 DO - https://doi.org/10.1021/acs.analchem.4c02763 SN - 0003-2700 VL - 96 IS - 30 SP - 12570 EP - 12576 AN - OPUS4-60768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meierhofer, F. T1 - Citric-Acid-Based Carbon Dots with Luminescence Quantum Yields > 50%: spectral tuning of the luminescence by ligand exchange and pH adjustment N2 - We report the synthesis and characterization of carbon nanodots (CDs) with high quantum yield (>50%) and tailored optical absorption as well as emission properties. A well-described protocol with polyethyleneimine (PEI) as amine precursor is used as a reference to a new CD system which is stabilized by aromatic 2,3-diaminopyridine (DAP) molecules instead. The DAP stabilizer is installed in order to red-shift the absorption peak of the n-π* electron transition allowing efficient radiative recombination and light emission. Size, shape, and chemical composition of the samples are determined by (HR)TEM, EDX and FTIR-spectroscopy. Optical parameters are investigated using UV-VIS, PL and QY measurements. Several parameters such as concentration, excitation wavelength and pH are studied. Zeta-potential analysis indicate that pH-induced (de-)protonation processes of functional moieties directly affect the n-π* energy bands. This results in unique pH-dependent absorption and emission characteristics which are discussed on the specific chemical composition of each CD system. T2 - MRS 2019 CY - Boston, MA, USA DA - 03.12.2019 KW - Nanoparticle KW - Carbon dot KW - Surface chemistry KW - Fluorescence KW - PH KW - Ligand KW - FTIR KW - Synthesis KW - Characterization PY - 2019 AN - OPUS4-49968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pohl, O. A1 - Kraft, Marco A1 - Kovac, J. A1 - Belec, B. A1 - Ponikvar-Svet, M. A1 - Würth, Christian A1 - Lisjak, D. A1 - Resch-Genger, Ute T1 - Optically detected degradation of NaYF4:Yb,Tm-based upconversion nanoparticles in phosphate buffered saline solution N2 - In a proof-of-concept study, we assessed different analytical and spectroscopic parameters for stability screening of differently sized β-NaYF4:20 mol % Yb3+, 2 mol % Tm3+ upconversion nanoparticles (UCNPs) exemplarily in the bioanalytically relevant buffer phosphate buffered saline (PBS; pH 7.4) at 37 and 50 °C. This included the potentiometric determination of the amount of released fluoride ions, surface analysis with X-ray photoelectron spectroscopy (XPS), and steady-state and time-resolved fluorescence measurements. Based on these results, the luminescence lifetime of the 800 nm upconversion emission was identified as an Optimum parameter for stability screening of UCNPs and changes in particle surface chemistry. KW - Upconverion KW - Nanoparticle KW - Dissolution PY - 2017 DO - https://doi.org/10.1021/acs.langmuir.6b03907 SN - 0743-7463 VL - 33 IS - 2 SP - 553 EP - 560 PB - ACS AN - OPUS4-39212 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Quantifying the total and accessible amount of surface functionalities and ligands on nanomaterials N2 - Engineered nanomaterials (NMs) of various chemical composition and surface functionalization are routinely fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, opto-electronics, and information storage. NM dispersibility, stability, processability, and function as well as the interaction with biological species and environmental fate are largely determined by NM surface functionalities, i.e., functional groups (FGs) and ligands. Therefore, reliable, reproducible, and eventually standardized surface characterization methods are vital for quality control of NMs, and mandatory to meet increasing concerns regarding their safety. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR) as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods.[1] The latter less costly and fast methods, which can be automated, are often used by NM producers for process and quality control.[1,2] To validate methods, establish measurement uncertain-ties, test reference materials, and produce reference data, multi-method characterization studies are needed.[3,4] as well as interlaboratory comparisons (ILC) on determining NM surface chemistry and well characterized test and reference NMs providing benchmark values.[5,6] Here, we present examples for quantifying common surface FGs such as amino and carboxyl groups on functional NMs of different chemical composition such as silica, polymer, iron oxide, and lanthanide-based upconversion nanoparticles with optical assays, electrochemical titration methods, qNMR, and chromatographic separation techniques. In addition, ongoing interlaboratory comparisons will be presented. T2 - Yucomat 2025 CY - Herec Novi, Montenegro DA - 01.09.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Characterization KW - Advanced material KW - Surface KW - Standardization KW - Reference material KW - Functional group KW - Quantification KW - Coating KW - Interlaboratory comparison KW - Uncertainty PY - 2025 AN - OPUS4-64182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, Katrin T1 - Fluorescence intensity and quantum yield reference materials for standardization of fluorescence-based measurements N2 - Luminescence techniques are amongst the most commonly used analytical methods in life and material sciences due to their high sensitivity, nondestructive character, and easy instrumentation suitable for miniaturization. Photoluminescence signals are, however, affected by wavelength-, polarization-, and time-dependent instrument-related effects. Thus, at the core of standardization approaches for all fluorescence-based techniques are evaluated fluorescence standards for the consideration of instrument-specific spectral and intensity distortions of measured signals and for instrument performance validation (IPV). Here, we summarize the research of BAM division 1.2 on development of liquid and solid fluorescence standards for various application-relevant fluorescence parameters and techniques. The portfolio of BAM fluorescence reference materials presently consists of: i) a Spectral Fluorescence Standard Kit, i.e., a set of liquid fluorescence standards with certified normalized corrected emission spectra, for the determination of a broad variety of fluorescence parameters ii) a ready-to-use, glass-based multi-emitter fluorescence standard for IPV and the determination of instrument-to-instrument variations iii) specially adapted calibration tools and validation concepts for microarray-based platforms used in molecular diagnostics and food safety control iv) quantum yield (Φf) standards for relative determination of the key performance parameter Φf of fluorescent materials, which can be also used for the evaluation of the performance of absolute, standard-free methods utilizing integrating sphere setups or spectrometer accessories. These materials, that will eventually cover the ultraviolet, visible, and near infrared spectral region, are currently under certification. This toolbox of method-adapted reference materials can perfectly complement existing fluorescence standards. These easy-to-use, reference materials can pave the way to traceable fluorescence measurements to a radiometric scale like the spectral radiance or spectral photon radiance for all users of fluorescence techniques in material sciences and analysis, as well as environmental monitoring and biotechnology. They are particularly useful for customers working in strongly regulated areas like medical diagnostics or pharmaceutical research, where certified standards in conjunction with validated standard operating procedures are mandatory. T2 - International Symposium on Biological and Environmental Reference Materials BERM-15 CY - Berlin, Germany DA - 23.09.2018 KW - Reference materials KW - Fluorescence standards PY - 2018 AN - OPUS4-47140 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Arakawa, Akihiro T1 - LA-ICP-MS study of Ag nanoparticle transport in a three-dimensional in vitro model N2 - We have applied laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) with subcellular resolution as an elemental mass microscope to investigate the distributions of Ag nanoparticles (NP) in a 3-dimentional multicellular spheroid (MCS) model. The production of MCS has been optimized by changing the seeding cell number (500 to 40,000 cells) and the growth period (1 to 10 days). Incubations of MCS with Ag nanoparticle suspensions were performed with a concentration of 5 µg mL-1 for 24 hours. Thin-sections of the Eosin stained MCS were analysed by elemental mass microscopy using LA-ICP-MS to image distributions of 109Ag, 31P, 63Cu, 66Zn and 79Br. A calibration using NP suspensions was applied to convert the measured Ag intensity into the number of particles being present in each measurement pixel. The numbers of NP determined ranged from 30 up to 4,000 particles in an enrichment zone. The particle distribution was clearly correlated to 31P, 66Zn and 79Br and was localized in an outer rim of proliferating cells (confirmed by DAPI) with a width of about two-single cell diameters. For the highest seeding cell number NPs were only detected in this outer rim, whereas small molecules as for instance 79Br and 109Ag ions were detected in the core of the MCS as well. Aniline blue staining demonstrated that this outer rim was rich in collagen structures in which fibroblast cells were embedded and a thin-membrane was visible which separated the core from the biological active cell layer functioning as biological barriers for NP transport. In this presentation, we will show the possibility using this 3-dimensional model for toxicological and medical applications. T2 - European Winter Conference on Plasma Spectrochemistry EWCPS-2019 CY - Pau, France DA - 03.02.2019 KW - Laser ablation KW - ICP-MS KW - Nanoparticles KW - Cell KW - Multicellular spheroid PY - 2019 AN - OPUS4-47374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schannor, Mathias A1 - Oelze, Marcus A1 - Traub, Heike A1 - He, Yubei A1 - Schmidt, Robin A1 - Heidemann, Luisa A1 - Savic, Lynn Jeanette A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Advancing Biomarker Research: In Situ Cu Isotope Analysis in Liver Tumors by LA-MC-ICP-MS N2 - Stable metal isotopes have received increasing attention as medical biomarkers due to their potential to detect changes in metal metabolism related to diseases. In particular, copper stable isotopes are a powerful tool to identify isotopic variation between tumors and healthy tissue, suggesting application in cancer diagnosis. However, potential mechanisms causing isotope fractionation, such as redox- or bond-forming reactions and interactions of metals during transmembrane import and export, are less well understood. Here, we established an in situ method using laser ablation-multicollector-inductively coupled plasma-mass spectrometry (LA-MC-ICP-MS) to advance our understanding of the underlying processes responsible for isotope fractionation between normal and diseased tissues. Gelatin-based bracketing standards and quality control reference materials, crucial for laser ablation analysis, were developed to allow correction for instrumentally induced isotope fractionation during LA-MC-ICP-MS analysis. Using such matrix-matched standards, the method achieved intermediate precisions for delta values of better than 0.15 ‰ (2 s) for inorganic reference materials and of better than 0.17 ‰ (2 s) for biological reference materials. The developed routine was tested on rabbit VX2 liver tumor samples, a model system resembling human hepatocellular carcinoma (HCC) used to study liver cancer. In situ Cu isotope compositions between healthy (𝛿65/63NIST976(Cu) = −1.5 ‰ to 0.2 ‰) and tumorous (𝛿65/63NIST976(Cu) = 0.0 ‰ to 1.3 ‰) liver tissue show distinct differences in their isotope ratios. The observed isotopic dichotomy is consistent with previous solution-based MC-ICP-MS work, showing enrichment of heavy 65Cu in cancer biopsies relative to healthy tissue. KW - Biomarker KW - Laser Ablation KW - Reference Material PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626865 DO - https://doi.org/10.1021/acs.analchem.4c05626 SN - 1520-6882 VL - 97 IS - 8 SP - 4425 EP - 4432 PB - American Chemical Society (ACS) AN - OPUS4-62686 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Srivastava, Priyanka A1 - Tavernaro, Isabella A1 - Genger, C. A1 - Welker, P. A1 - Huebner, Oskar A1 - Resch-Genger, Ute T1 - Multicolor Polystyrene Nanosensors for the Monitoring of Acidic, Neutral, and Basic pH Values and Cellular Uptake Studies N2 - A first tricolor fluorescent pH nanosensor is presented, which was rationally designed from biocompatible carboxylated polystyrene nanoparticles and two analyte-responsive molecular fluorophores. Its fabrication involved particle staining with a blue-red-emissive dyad, consisting of a rhodamine moiety responsive to acidic pH values and a pH-inert quinoline fluorophore, followed by the covalent attachment of a fluorescein dye to the particle surface that signals neutral and basic pH values with a green fluorescence. These sensor particles change their fluorescence from blue to red and green, depending on the pH and excitation wavelength, and enable ratiometric pH measurements in the pH range of 3.0−9.0. The localization of the different sensor dyes in the particle core and at the particle surface was confirmed with fluorescence microscopy utilizing analogously prepared polystyrene microparticles. To show the application potential of these polystyrene-based multicolor sensor particles, fluorescence microscopy studies with a human A549 cell line were performed, which revealed the cellular uptake of the pH nanosensor and the differently colored emissions in different cell organelles, that is, compartments of the endosomal-lysosomal pathway. Our results demonstrate the underexplored potential of biocompatible polystyrene particles for multicolor and multianalyte sensing and bioimaging utilizing hydrophobic and/or hydrophilic stimuli-responsive luminophores. KW - Microparticle KW - Fluorescence KW - Sensor KW - pH KW - Quantum yield KW - Multiplexing KW - Imaging KW - Cell KW - Quality assurance KW - Nano KW - Polymer KW - Bioimaging KW - Particle KW - Application PY - 2022 DO - https://doi.org/10.1021/acs.analchem.2c00944 VL - 94 IS - 27 SP - 9656 EP - 9664 PB - ACS AN - OPUS4-55365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matiushkina, Anna T1 - Synthesis and physical properties studies of bifunctional nanocomposites N2 - At present, the field of research on nanostructures is actively developing, which is due to their unique physico-chemical properties compared to bulk materials. Many research activities are focused on obtaining nanocomposites, which combine various types of nanostructures with different properties and function. For example, the development of magneto-luminescent nanocomposites makes it possible to use their luminescence for optical imaging, and their magnetic properties for magnetic targeted delivery and as agents of hyperthermia and magnetic resonance imaging. My master studies as part of the project Goszadanie 2019-1080 at ITMO were focused on the investigation of nanocomposites, consisting of semiconductor quantum dots (QDs) as luminescent component and superparamagnetic iron oxide nanoparticles (SPIONs) as magnetic one, in solution and during their incubation with HeLa cells. The spectrally resolved analysis of the QD photoluminescence (PL) kinetics of the free QDs and the QDs incorporated in these nanocomposites undergoing energy transfer processes allowed for (1) understanding the reasons for the quenching of QD luminescence in cells, (2) evaluating the average distance between the QDs and, based on this, concluding the degree of QD aggregation in cells, and (3) drawing conclusions about the QD-quencher composites integrity in cells. Overall, the analysis of the PL kinetics confirmed that QDs and SPIONs remain bound in the obtained nanocomposites during incubation with cells. To ensure the successful advancement of nanomaterials in biomedicine and the transition from their laboratory preparation and studies to their use in different applications and in industry, it is crucial to develop reliable measurement methods and reference materials candidates for the characterization of functional nanomaterials and assessing the quality of the obtained nanostructures. My recently started project at BAM, which is part of the EU metrology project MeTrINo, will be devoted to this topic. There we will focus on the development of methodologies for the synthesis and characterization of iron oxide nanoparticles, already used in biomedicine, and multi-element lanthanide-based nanoparticles with attractive upconversion luminescence, as reference materials with high monodispersity and reproducibility. Also, these nanoparticles will be functionalized with organic dyes for optical imaging and, probably, the study of the energy transfer phenomena. T2 - Bad Honnef Summer School CY - Bad Honnef, Germany DA - 30.07.2023 KW - Quantum dots KW - Iron oxide nanoparticles KW - Upconversion nanoparticles PY - 2023 AN - OPUS4-58075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Ultraschallprüfung von Verschlussbauwerken im Salinar N2 - Zu jedem Endlager gehört die Entwicklung eines Verschlusskonzept. Im Endlager Morsleben und an anderer Stelle werden in Abhängigkeit vom Wirtsgestein verschiedene Materialien und Bauweisen für Streckenverschlüsse entwickelt und in großem Maßstab erprobt. Hierzu gehören auch Maßnahmen der Qualitätssicherung, die Informationen über Ausführung und Zustand der Versuchsbauwerke liefern. Hierzu werden von der Bundesanstalt für Materialforschung und -prüfung (BAM) für verschiedene Forschungsvorhaben und Prüfaufträge Methoden und Geräte getestet, verbessert und vor Ort unter Tage eingesetzt Die hier beschriebenen Verfahren lassen sich auch zu Untersuchungen im Wirtsgestein anwenden. T2 - Tage der Standortauswahl CY - Freiberg/S., Germany DA - 11.02.2021 KW - Endlager KW - Verschlussbauwerke KW - Qualitätssicherung KW - Ultraschall PY - 2021 AN - OPUS4-54166 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Measuring the Upconversion Luminescence of Ensemble and Single Particle Lanthanide-Based Upconversion Nanocrystals N2 - Lanthanide-based upconversion nanoparticles (UCNPs) like hexagonal 𝛽-NaYF4 UCNPs doped with Yb3+ and Er3+, which efficiently convert 976 nm light to ultraviolet, visible, and near infrared photons, offer new strategies for luminescence-based sensing, barcoding, and Imaging. Their upconversion (UC) luminescence (UCL) features like UCL intensity, quantum yield, relative spectral distribution / UCL luminescence color, and luminescence decay kinetics are, however, strongly influenced by particle size, dopant ion concentration, particle architecture, surface chemistry including presence and thickness of surface passivation and shielding shells, microenvironment/presence of quenchers with high energy vibrations, and excitation power density (P). We present here a comprehensive study of the influence of excitation power density on the UCL features of different types of UCNPs, focusing on Yb3+ and Er3+ co-doped NaYF4 core-only and core-shell nanostructures with different sizes and doping ion concentration, which underlines the importance of P-dependent optimum dopant concentrations for UCNP performance and the potential of P-tuning of UCL. T2 - Materials Challenges in Alternative & Renewable Energy 2021 (MCARE 2021) CY - Online meeting DA - 19.07.2021 KW - Fluorescence KW - Lifetime KW - Method KW - Stability KW - Coating KW - Surface chemistry KW - Lanthanide KW - Upconversion KW - Nano KW - Particle KW - Single particle spectroscopy KW - Quantum yield KW - Microscopy KW - Photophysics PY - 2021 AN - OPUS4-53111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - Project Status report IEC TS 62607-3-1 ED2 N2 - Project Status report IEC TS 62607-3-1 ED2 reklative and absolute quantum yield determinations T2 - IEC TC 113 Plenary Meeting CY - Online meeting DA - 17.04.2023 KW - Quantum yield KW - Standardization KW - Nanomaterials KW - Nanomanufacturing KW - IEC PY - 2023 AN - OPUS4-57477 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Phukphatthanachai, Pranee A1 - Vogl, Jochen A1 - Traub, Heike A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - A new approach of using polyethylene frits for the quantification of sulphur in copper metals by isotope dilution LA-ICP-MS and comparison with conventional IDMS techniques N2 - Polyethylene (PE) frits were used to quantify sulphur in copper and its alloys by isotope dilution combined with LA-ICP-MS as an alternative approach to conventional sample preparation: the copper samples were spiked, the spiked samples were dissolved, the resulting solutions were absorbed in the PE frits and finally the PE frits were analysed by LA-ICP-MS. A prerequisite for such a support material is a low sulphur blank and thus PE was selected for this purpose. The absorption efficiency of the PE frits was studied for varying sulphur amounts ranging from 2 mg S to 80 mg S showing that more than 99.5% of the loaded sulphur was absorbed by the frit. The so prepared PE frits were measured by LA-ICP-MS and yielded a good linearity (R2 ¼ 0.999) for the sulphur ion intensities corresponding to sulphur amounts up to 40 mg S; the associated sensitivity is approximately 3.4 x 10⁴ cps μg⁻¹ for ³²S. For the validation of the developed procedure the reference materials BAM-M376a, BAM-228 and BAM-227 were applied such that 2 μg S, 5 μg S and 11 μg S were absorbed in the PE frits, respectively. These samples were pre-quantified for the adsorbed sulphur amount by external calibration LA-ICP-MS yielding sulphur amounts of 0.9 μg, 5.1 μg and 8.5 μg (quantified for ³²S only), respectively. Relative Standard deviations of the isotope ratios were below 5% in average (n ¼ 3 lines) in all cases (except for the pure spike solution). These samples were then analysed by LA-ICP-IDMS and the measurement results were validated by comparing them with the results obtained by conventional ICP-IDMS. The obtained relative expanded measurement uncertainties ranged between 10% and 26%. Pearson's coefficient was used to express the correlation between both techniques; the obtained value was 0.999 demonstrating a strong correlation. Contrary to most published LA-ICP-IDMS procedures, the developed procedure enables SI-traceability for the measurement results. The metrological traceability to the SI for the sulphur mass fractions in copper was established by an unbroken chain of comparisons, each accompanied by an uncertainty budget. Thus, the measurement results are considered reliable, acceptable and comparable within the stated measurement uncertainty. The metrological traceability chain from the kg down to mass fraction in the samples obtained by LA-ICP-IDMS is presented as well. KW - Laser ablation KW - IDMS KW - Traceability KW - Uncertainty KW - Purity PY - 2018 DO - https://doi.org/10.1039/c8ja00116b SN - 0267-9477 SN - 1364-5544 VL - 33 IS - 9 SP - 1506 EP - 1517 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-45899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica T1 - Tagging reagents for imaging mass cytometry N2 - In der klinischen Diagnostik werden für zytometrische Messverfahren bereits eine Reihe von Reagenzien eingesetzt zur Markierung von Antikörper eingesetzt, um die Detektion von Biomarkern mittels Fluoreszenz- oder Flugzeitmassenspektrometrie zu ermöglichen. Seit kurzem ist auch eine Imaging Mass Cytometry Kombination direkt erhältlich, wodurch der Nachweis von Biomarkern in Gewebeschnitten erreicht werden kann. Dazu wird eine Kopplung von Laser Ablation und induktiv gekoppeltem Plasma Massenspektrometrie eingesetzt, wobei ähnlich der Massenzytometrie, zuvor Antikörper mit Metallen markiert, und im Anschluss mit dem Gewebeschnitt inkubiert werden. Durch die hohe Ortsauflösung können die Biomarker lokalisiert, und zukünftig vielleicht auch quantifiziert werden. Insbesondere Lanthanide eignen sich als Markierungsmetalle, da sie einen niedrigen Untergrund und chemisch ähnliches Verhalten zueinander aufweisen. Allein durch diese Elemente können bereits etwa 15 Parameter unterschieden werden, was durch isotopenreine Standards weiter gesteigert werden kann. Vom Markierungsgrad abhängig werden unterschiedlich viele Metalle am Antikörper gebunden, und beeinflussen so die Sichtbarkeit im ICP-MS. Nanopartikel könnten daher eine deutliche Steigerung der Sensitivität bewirken. GdVO4 Nanokristalle scheinen bisher sehr vielversprechend und bieten neben multiparametrischen Anwendungen auch Multimodalität. Die Synthese der Nanokristalle zeigte hohe Homogenität und Reproduzierbarkeit in Partikelgröße in der Zusammensetzung. Ein erstes Experiment mit einer Zellkultur konnte bereits die effiziente Markierung der Zellen unter Beweis stellen, wobei durch hohe Signalstärke auch subzelluläre Auflösung in der LA-ICP-MS erreicht werden konnte. T2 - ICPMS Anwendertreffen 2018 CY - Berlin, Germany DA - 03.09.2018 KW - LA-ICP-MS KW - Immuno assay KW - Bioimaging KW - Nanocrystal KW - Lanthanide KW - Metal-tag PY - 2018 AN - OPUS4-45866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Studying nanoparticle-cell interaction by ICP-MS based techniques N2 - Nanoparticles (NPs) have found a wide range of applications in research and industry. Thereby the interaction of NPs with biological systems like cells has become a major field of interest, ranging from medical applications to nanotoxicology. Size, shape and surface modification of the nanomaterials determine the uptake rate and pathway into the cells, and therefore impact specific cell components and processes. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is an established quantitative multi-elemental analysis and mapping technique. In recent years, it was shown that LA-ICP-MS can provide quantitative as well as distribution information of metal containing nanoparticles (NPs) in cell samples. Here LA-ICP-MS was applied for the imaging of individual fibroblast cells to study the uptake and intracellular processing of NPs. Our results show that LA-ICP-MS can be used to localize nanoparticle aggregates within cellular compartments. The studied NPs accumulate in the perinuclear region in the course of intracellular processing, but do not enter the cell nucleus. The uptake efficiency depends strongly on the physico-chemical properties of the nanostructures as well as on the incubation conditions like concentration and incubation time. ICP-MS was used to determine the composition of the nanomaterials as well as the number of NPs in cells after acid digestion of the samples. T2 - 13. Symposium „Massenspektrometrische Verfahren der Element­spurenanalyse“ & 26. ICP-MS-Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - ICP-MS KW - Nanoparticle KW - Cell KW - Laser ablation PY - 2018 AN - OPUS4-45860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Ultrasonic monitoring of full-scale load experiments N2 - Previous work has shown that ultrasonic monitoring using externally applied or embedded transducers and imaging methods based on coda wave interferometry are able to detect subtle changes in concrete elements. In this study, a limited number of embedded transducers has been used to monitor changes in several 12 m long two-span concrete beams subjected to point or linear loads until failure. The ultrasonic results showed the high sensitivity to stress changes and the nonlinear character of the associated effects. However, the ultrasonic features showed a very good correlation to several conventional monitoring parameters. For higher loads (significant amount of cracking), the technique had to be modified to cope with large wave velocity variations and high decorrelation compared to the reference signal. Using a very simple imaging procedure, the 2D stress field inside the beam has been visualized including inhomogeneities and artifact at places where cracking occurred at higher loads. The technique has the potential to be included in real time monitoring systems. T2 - ASNT SMT/NDT-CE 2018 CY - New Brunswick, NJ, USA DA - 27.8.2018 KW - Concrete KW - Monitoring KW - Ultrasound KW - Coda wave interferometry PY - 2018 AN - OPUS4-45827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Otto, S. A1 - Förster, C. A1 - Wang, Cui A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - A Strongly Luminescent Chromium(III) ComplexAcid N2 - The synthesis, structure, reactivity,and photophysical properties of anovel acidic,luminescentchromium(III) complex [Cr(H2tpda)2]3+ (23+ +)bearing the tridentate H2tpda (2,6-bis(2-pyridylamino)pyridine) ligand are presented. Excitation of 23+ + at 442 nm results in strong, long-lived NIR luminescence at 782 nm in water and in acetonitrile. X-ray diffraction analysis and IR spectroscopy revealhydrogen-bonding interactions of the counter ions to the NH groups of 23+ + in the solidstate. Deprotonation of the NH groups of 23+ + by using anon-nucleophilic Schwesinger base in CH3CN switches off the luminescence. Re-protonation by using HClO4 restores the emission. In water,the pKa value of 23+ + amountsto8 .8, yet deprotonation is not reversible in the presence of hydroxide ions. Dioxygen quenches the emission of 23+ +,but to aweaker extent than expected. This is possibly due to the strong ion-pairing properties of 23+ + even in solution, reducing the energy transfer efficiency to O2.Deuteration of the NH groups of 23+ + approximately doubles the quantum yield and lifetime in water,demonstrating the importance of multiphoton relaxation in these NIR emitters. KW - Cr(III) complex KW - Oxygen sensor KW - pH sensor KW - Luminescence KW - Luminescence lifetime KW - Quantum yield KW - NIR emitter PY - 2018 DO - https://doi.org/10.1002/chem.201802797 SN - 0947-6539 VL - 24 IS - 48 SP - 12555 EP - 12563 PB - Wiley‐VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-45929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grunert, B. A1 - Saatz, Jessica A1 - Hoffmann, Katrin A1 - Appler, F. A1 - Lubjuhn, Dominik A1 - Jakubowski, Norbert A1 - Resch-Genger, Ute A1 - Emmerling, Franziska A1 - Briel, A. T1 - Multifunctional rare-earth element nanocrystals for cell labeling and multimodal imaging N2 - In this work, we describe a simple solvothermal route for the synthesis of Eu3+-doped gadolinium orthovanadate nanocrystals (Eu:GdVO4−PAA) functionalized with poly(acrylic)acid (PAA), that are applicable as cell labeling probes for multimodal cellular imaging. The Eu3+ doping of the vanadate matrix provides optical functionality, due to red photoluminescence after illumination with UV light. The Gd3+ ions of the nanocrystals reduce the T1 relaxation time of surrounding water protons, allowing these nanocrystals to act as a positive MRI contrast agent with a r1 relaxivity of 1.97 mM−1 s−1. Low background levels of Eu3+, Gd3+, and V5+ in biological systems make them an excellent label for elemental microscopy by Laser Ablation (LA)-ICP-MS. Synthesis resulted in polycrystalline nanocrystals with a hydrodynamic diameter of 55 nm and a crystal size of 36.7 nm, which were further characterized by X-ray diffraction (XRD), photoluminescence spectroscopy (PL) and transmission electron microscopy (TEM). The multifunctional nanocrystals were subsequently used for intracellular labeling of both human adipose-derived stem cells (MSCs) and A549 (adenocarcinomic human alveolar basal epithelial) cells. KW - Bioimaging KW - Nanoparticle KW - Multimodal KW - Lanthanide PY - 2018 DO - https://doi.org/10.1021/acsbiomaterials.8b00495 SN - 2373-9878 VL - 4 IS - 10 SP - 3578 EP - 3587 PB - ACS Publications CY - Washington, USA AN - OPUS4-46244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ramirez Caro, Alejandra A1 - Mota, Berta A1 - Artemeva, E. A1 - Pauli, Jutta A1 - Schmidt, Wolfram A1 - Resch-Genger, Ute T1 - A spectroscopic study of the superplasticizer effect on early cement hydration N2 - Organic/inorganic mixtures were prepared from ordinary Portland cement (OPC), water (w/c 0.22), a fluorescent dye in aqueous solution (stable at alkaline pH; BAM-I), and two different comb shape polycarboxylates (PCEs), i.e., high charge (PCE-HC) and low charge (PCE-LC), respectively. Rheological and calorimetric measurements were performed prior to optical studies in order to select PCE concentrations. Absorption and fluorescence spectroscopy of the system OPC + BAM-I (CBAM-I) revealed maxima of dye BAM-I located at 645 nm and 663 nm, respectively. In presence of PCE-HC and PCE-LC, these mixtures displayed a small red shift in reflectance and a faster decrease in intensity compared to studies with CBAM-I; however, only slight differences were observed between the different PCEs. With time, all systems exhibited a decrease in intensity of BAM-I in absorption/reflectance and emission. This could be caused by dye adsorption and possibly decomposition when in contact with cement particles or hydration products. T2 - 20. Internationale Baustofftagung CY - Weimar, Germany DA - 12.09.2018 KW - Optical spectroscopie KW - Cement hydration KW - Dyes PY - 2018 SN - 978-3-00-059950-7 VL - 20 SP - 1 EP - 6 PB - F.A. Finger-Institut für Baustoffkunde CY - Weimar AN - OPUS4-46277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Quantification of Parameters Affecting the Upconversion Luminescence of Lanthanide-Based Upconversion Nanocrystals N2 - Lanthanide-based upconversion nanoparticles (UCNPs) like hexagonal Beta-NaYF4 UCNPs doped with Yb3+ and Er3+, which efficiently convert 976 nm light to ultraviolet, visible, and near infrared photons, offer new strategies for luminescence-based sensing, barcoding, and imaging. The properties of their upconversion (UC) luminescence (UCL) are, however, strongly influenced by particle size, the concentration and spatial arrangement of the dopant ions, surface chemistry including presence and thickness of surface passivation and shielding shells, microenvironment/presence of quenchers with high energy vibrations, and excitation power density (P). We present here a comprehensive study of the influence of UCNP size and particle architecture for Yb3+ and Er3+ co-doped NaYF4 core-only and core-shell nanostructures in the size range of about 5 nm to 50 nm, which underlines the importance of particle synthesis, surface chemistry, and quantitative luminescence measurements for mechanistic insights and the determination of application-relevant matrix- and P-dependent optimum dopand concentrations. T2 - Materials Challenges in Alternative and Renewable Energy (MCARE) 2018 CY - Vancouver, BC, Canada DA - 20.08.2018 KW - Upconverting nanoparticles KW - Size KW - Energy transfer KW - Fluorescence KW - Absolute fluorescence quantum yield KW - Fluorescence decay kinetics KW - Power density dependence PY - 2018 AN - OPUS4-46393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Non-destructive Evaluation for Nuclear Power Plant concrete infrastructure N2 - The ageing and decommissioning of nuclear concrete infrastructure (e. g. safety containments) as well as the building and closure of waste repositories gives new challenges to non-destructive testing. For example, the quality assurance of very thick concrete structures is beyond the limitations of commercial ultrasonic instrumentation. The presentation introduces typical testing tasks and the application of state of the art NDT techniques. In addition, it describes some new developments in ultrasonic testing and monitoring. Specifically, the application of the unique deep penetration system LAUS is shown. Ultrasonic monitoring using embedded transducers to check for subtle and sudden changes in the material is introduced as well. T2 - Aalto University Special Guest Seminar CY - Espoo, Finland DA - 25.10.2018 KW - Ultrasound KW - Concrete KW - Nuclear PY - 2018 AN - OPUS4-46425 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Biophotonics and analytics – Quantum Yields of Single Emitters and Lifetime Multiplexing N2 - An increasing number of (bio)analytical techniques rely on multiparametric analyses and the measurement of a very small number of emitters. While the former implies encoding or labeling by means of easily distinguishable properties like luminescence color or lifetime in conjunction with high-throughput optical-spectroscopic methods such as flow cytometry, the latter requires methods suitable for the characterization of the optical properties of single emitters. Here, we present the use of fluorescence correlation spectroscopy (FCS) for the relative determination of the key parameter photoluminescence quantum yield [5] and first results from flow cytometry measurements in the time-domain with a custom-designed instrument with luminescence lifetime analysis capability. T2 - ICENAP-Projekttreffens CY - Reims, Italy DA - 20.09.2018 KW - Single emitter KW - Semiconductor quantum dot KW - Lifetime KW - Multiplexing KW - Single particle spectroscopy KW - Photoluminescence quantum yield PY - 2018 AN - OPUS4-46385 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Biophotonics and analytics - Photoluminescence properties of nanocrystals and surface group analysis N2 - Correlating the photoluminescence (PL) properties of nanomaterials like semiconductor nanocrystals (QDs) and upconversion nanocrystals (UCNPs) assessed in ensemble studies and at the single particle level and studying their surface chemistry is increasingly relevant for applications of these nanomaterials in the life and material sciences. Here we present a comparison of the spectroscopic properties of ensembles and single nanocrystalline emitters and simple methods for the quantification of functional groups and ligands on particle surfaces. The overall goal of this study was to derive particle architectures and surface chemistries well suited for spectroscopic and microscopic applications. T2 - Institutskolloqium Jozef Stefan Institute CY - Ljubljana, Slovenia DA - 07.11.20218 KW - Lanthanide KW - Nanoparticle KW - Nanocrystal KW - Upconversion KW - Absolute fluorometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Fluorescence KW - Surface chemistry KW - Deactivation pathways KW - Modeling KW - Photophysics KW - Size KW - Cleavable probe PY - 2018 AN - OPUS4-46578 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - LA-ICP-MS for the analysis of nanoparticles in cells N2 - Many current nanomaterials can serve as contrast agents in cellular or tissue imaging, drug delivery vehicles or therapeutics, whereas others can cause toxic effects. In order to evaluate nano-bio interactions, the number of nanoparticles (NPs) inside cells as well as their localisation within cellular substructures is of particular interest. The cellular uptake depends on the primary characteristics of the NPs (e.g. size, shape, surface coating) and on the cell type. Laser ablation inductively coupled plasma mass spectrometry (LA‑ICP‑MS) is more and more used to study the NP pathway from uptake, via intracellular processing up to cell division. High-spatial resolution laser ablation at single cell level is achieved using novel low-dispersion LA chambers and by careful optimisation of laser energy, ablation frequency and scan speed at small laser spot sizes down to 1 µm. Different examples from BAM, Division 1.1 and cooperation partners using LA-ICP-MS to localize and quantify metal-containing nanoparticles are shown. The results demonstrate the potential of LA-ICP-MS providing insight into NP uptake, intracellular distribution and cell-to-cell variation. T2 - 13. Symposium "Massensprektrometrische Verfahren der Elementspurenanalyse" + 26. ICP-MS Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - Laser ablation KW - Cells KW - Nanoparticles KW - Imaging PY - 2018 AN - OPUS4-46440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vössing, Konrad A1 - Gaal, Mate A1 - Niederleithinger, Ernst T1 - Air‑coupled ferroelectret ultrasonic transducers for nondestructive testing of wood‑based materials N2 - Air-coupled ultrasound (ACU) is used in through transmission to detect delamination, rot, and cracks in wood without altering the structure permanently. Novel ferroelectret transducers with a high signal-to-noise ratio enable high-precision structure recognition. Transducers made of cellular polypropylene are quite suitable for ACU testing due to their extremely low Young’s modulus and low density resulting in a favorable acoustic impedance for the transmission of ultrasonic waves between the transducer and air. Thus, structures with great dimensions, with a thickness of up to 300 mm and material densities below 500 kg/m3, can be inspected. Promising results were obtained under laboratory conditions with frequencies ranging from 90 to 200 kHz. The advantage of ACU transducers is that they do not equire contact to the sample; they are accurate and cost-effective. Ultrasonic quality assurance for wood is an important avenue to increase the acceptance of wooden structures and toward sustainability in civil engineering in general. KW - Ultrasound KW - Wood KW - Defect KW - Air-coupled PY - 2018 DO - https://doi.org/10.1007/s00226-018-1052-8 VL - 52 IS - 6 SP - 1527 EP - 1538 PB - Springer AN - OPUS4-46653 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - TF-Projekt MaUS: Material und Umweltsimulation N2 - Gegenstand des Projekts ist die Prüfung der Umweltbeständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polycarbonat, Polytetrafluorethylen, Polystyrol und Polypropylen zum Einsatz. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden, die es gestatten, Schnellprüfverfahren zu etablieren, die die Simulation der realen Beanspruchungen im Zeitraffermodell anwendbar machen. Somit sollen standardisierbare Schnellbeanspruchungs-verfahren erarbeitet werden, die als Prüfeinrichtungen etabliert werden und von externen Auftraggebern zur Prüfung der Umweltbeständigkeit und -verträglichkeit von neuen Materialien genutzt werden können. Die Umweltwirkungen (chemisch-physikalisch und mikrobiologisch) sollen so definiert eingesetzt werden, dass eine reproduzierbare Prüfung möglich wird. Aus diesen Verfahren und Methoden sollen Normen abgeleitet werden, die eine standardisierte Materialprüfung ermöglichen. T2 - Projektmeeting BAM - Covestro CY - Leverkusen, Germany DA - 29.05.2018 KW - Umweltsimulation KW - Schadstoffaustrag PY - 2018 AN - OPUS4-47025 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niederleithinger, Ernst T1 - Ultrasonic monitoring of concrete constructions using embedded transducers N2 - Ultrasonic transmission measurements are used to monitor concrete elements mostly on a laboratory scale since decades. Recently, coda wave interferometry, a technique adapted from seismology, has been introduced to civil Engineering experiments. It can be used to reveal subtle changes in concrete samples and even large construction elements without having a transducer directly at the location where the change is taking place. The methodology works best with embedded transducers to avoid coupling issues or excessive environmental influence. These transducers can be used for newly built and existing structures. Recently, large concrete beams have been equipped with a network of transducers and loaded until failure. Using code wave interferometry, it was possible to visualize stress fields and damaged areas. T2 - International Symposium on Structural Health Monitoring and Nondestructive Testing CY - Saarbrücken, Germany DA - 4.10.2018 KW - Ultrasound KW - Monitoring KW - Concrete PY - 2018 UR - http://www.ndt.net/?id=23542 SN - 1435-4934 VL - 23 IS - 12 SP - 1 EP - 6 PB - NDT.net CY - Kirchwald AN - OPUS4-46842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Quantification of Surface Groups on Nanomaterials with Simple Optical Methods N2 - Surface functionalization of nanomaterials is nowadays at the core of many applications of functional materials in the life and material sciences. Examples range from membranes and microarrays over bead-based assays, and next generation sequencing to nanometer-sized optical reporters, nanosensors, and magnetic and optical contrast agents. Typical function-nalization steps include silanization and grafting reactions with reactive monomers to introduce functional groups like amino or carboxylic acid groups or the attachment of ligands like polyethylene glycol (PEG) molecules and biomolecules. [1-3] This enables to tune e.g., dis-persibility, hydrophilicity and biocompatibility, minimize unspecific interactions, improve biofunctionalization efficiencies, and enhance blood circulation times and allows for the use of nanomaterials as reporters in assays or the design of targeted probes for bioimaging. At the core of all functionalization strategies are reliable and validated methods for surface group and ligand quantification that can be preferably performed with routine laboratory instrumentation, require only small amounts of substances, and are suitable for many different types of nanomaterials. [3] There is meanwhile a considerable need to make these methods traceable. We present here versatile and simple concepts for the quantification of common functional groups, ligands, and biomolecules on different types of organic and inorganic nanomaterials, using conventional and newly developed cleavable and multimodal reporters, that can be detected with optical spectroscopy. [4-7] These reporters are chosen to enable method validation with the aid of method comparisons and mass balances. Also, strategies how to make these simple assays traceable to SI units using quantitative nuclear resonance spectroscopy (qNMR) and X-ray photoelectron spectroscopy (XPS) are derived. T2 - JRC-NIST Workshop CY - Ispra, Italy DA - 04.12.2018 KW - Nanoparticle KW - Nanocrystal KW - Absolute fluorometry KW - Fluorescence KW - Surface chemistry KW - Assay KW - Cleavable probe KW - Conductometry KW - Quantification KW - Functional group PY - 2018 AN - OPUS4-46950 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oesch, Tyler T1 - Quality assurance of engineered barriers in underground waste disposals N2 - This poster provides an overview of ultrasonic investigations of an engineered test barrier at ERAM Morsleben, which were completed as part of contractual work with the Bundesgesellschaft für Endlagerung mbH (BGE). This includes both experiments with the Large Aperture Ultrasound System (LAUS) and the ultrasonic borehole array. Also included in the poster is a description of the planned BAM thematic project “SealWasteSafe”. In particular, the proposed geopolymer materials are described and future research requirements are detailed. T2 - 1. Statuskonferenz Endlagerung von hochradioaktiven Abfällen CY - Berlin, Germany DA - 08.11.2018 KW - Large Aperture Ultrasound System (LAUS) KW - Ultrasonic Borehole Array KW - SealWasteSafe KW - Geopolymer KW - Crack Detection PY - 2018 AN - OPUS4-47021 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraft, Marco A1 - Würth, Christian A1 - Muhr, Verena A1 - Hirsch, Thomas A1 - Resch-Genger, Ute T1 - Particle-size-dependent upconversion luminescence of NaYF4: Yb, Er nanoparticles in organic solvents and water at different excitation power densities N2 - A systematic study of the luminescence properties of monodisperse β-NaYF4: 20% Yb3+, 2% Er3+ upconversion nanoparticles (UCNPs) with sizes ranging from 12–43 nm is presented utilizing steady-state and time-resolved fluorometry. Special emphasis was dedicated to the absolute quantification of size- and environment-induced quenching of upconversion luminescence (UCL) by highenergy O–H and C–H vibrations from solvent and ligand molecules at different excitation power densities (P). In this context, the still-debated Population pathways of the 4F9/2 energy level of Er3+ were examined. Our results Highlight the potential of particle size and P value for color tuning based on the pronounced near-infrared emission of 12 nm UCNPs, which outweighs the red Er3+ emission under “strongly quenched” conditions and accounts for over 50% of total UCL in water. Because current rate equation models do not include such emissions, the suitability of these models for accurately simulating all (de)population pathways of small UCNPs must be critically assessed. Furthermore, we postulate population pathways for the 4F9/2 energy level of Er3+, which correlate with the size-, environment-, and P-dependent quenching states of the higher Er3+ energy levels. KW - Quantum Yield KW - Nanoparticle KW - Quenching KW - Upconversion PY - 2018 DO - https://doi.org/10.1007/s12274-018-2159-9 VL - 11 IS - 12 SP - 6360 EP - 6374 PB - Tsinghua Univ. Press CY - Beijing AN - OPUS4-47172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Relative and Absolute Methods for Measuring Photoluminescence Quantum Yields of UV/vis/NIR Emitters N2 - One of the key spectroscopic performance parameters of molecular and particulate emitters is the photoluminescence quantum yield (PL QY) that provides a direct measure for the number of emitted per absorbed photons. This triggered the interest in methods suitable for measuring this property for emitters in various environments in the UV/vis/NIR and above 1000 nm as well as on the ensemble and single emitter level. Moreover, for nonlinear emitters like lanthanide-based upconversion nanocrystals methods including instrumentation for power density-dependent PL QY studies are required. An overview of the research activities in Division Biophotonics of BAM is given and suitable relative and absolute methods for the deter-mination of PL QY of organic dyes and different types of application-relevant nanomaterials in dispersion and in the solid state are presen-ted. This covers also the design and calibration of integrating sphere setups, achievable uncertainties, and candidates for PL QY reference materials. T2 - OSRAM Veranstaltung CY - Regensburg, Germany DA - 09.01.2019 KW - Quantum yield KW - Calibration KW - Reference material KW - Uncertainty KW - Absolute fluorometry KW - Integrating sphere spectroscopy KW - NIR KW - IR KW - Fluorescence KW - Nanoparticle KW - Dye PY - 2019 AN - OPUS4-47263 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - LA-ICP-MS- und RFA-Messungen für die Bestimmung von polybromierten Flammschutzmitteln (PBFSM) in Polystyrol- und Polypropylenproben N2 - To investigate the release and migration of flame retardants from polypropylene (PP) and polysytrene (PS) we use samples of with defined content of flame retardants as additives. Therefore we use HBCD in the concentration of 1% wt. resp. BDE-209 in the concentration of 0.1% wt. For the preparation of the samples granular of PP resp. PS are extruded together with the BFRs additives. Even the result of this process may lead to homogenous partition of the BFRs additives, this has to be proven before using the samples in the experimental setup for weathering studies. In accordance to the regulation of RoHS, where the use of XRF is recommended for the proof of flame retardants in electronic consumer products, we use this method as a reference to the laser ablation ICP/MS. Therefore we present the correlation of these experiments. The experimental setup for the XRF experiment is like a standard addition: in cavities, which are introduced in the sample plates subsequently, solutions of defi ned concentration of flame retardants are put in these cavities. According to the idea of standard addition, we get an information of the originating concentration of flame retardant in each sample and we can monitor the release and migration of these additives during/after the weathering experiment with high precision. Therefore to the designated plates an internal standard is added as a marker and can be analyzed after the weathering experiment. As awaited, the light exposed site, shows a deviating content in flame retardants compared to the sheltered site. N2 - Gegenstand der vorzustellenden Arbeiten ist die Prüfung der Umweltbeständigkeit und -verträglichkeit von Materialien und Produkten hinsichtlich der Emission von potenziellen Schadstoffen in die Umwelt. Hierzu werden chemisch-physikalische Einflüsse (Bewitterung) und mikrobielle Beanspruchungen an Modellmaterialien evaluiert. So werden die Freisetzungsraten von Schadstoffen in Abhängigkeit der Beanspruchung beschrieben. Als Modellmaterialien kommen die Polymere Polystyrol (PS) und Polypropylen (PP) zum Einsatz, die jeweils mit polybromierten Flammschutzmitteln (PBFSM) versehen sind. Synergistische Effekte der Bewitterungsparameter und der mikrobiologischen Beanspruchung sollen dabei ebenso betrachtet werden, wie die gezielte Alterung. Auch findet eine Beschreibung des Verhaltens der ausgetragenen Schadstoffe in den Umweltkompartimenten Boden oder Wasser statt. Hier sind mit Hilfe der zu entwickelnden Screening- und non-Target-Analyseverfahren die Transformation und der Metabolismus durch Mikroorganismen zu beschreiben. Auch soll mit Hilfe der RFA und der LA-ICP-MS die Abreicherung der PBFSM in den Modellmaterialien beschrieben werden. Aus den Ergebnissen sollen Korrelationen zwischen den künstlichen Alterungsverfahren und realen Szenarien abgeleitet werden. T2 - Umwelt 2018 CY - Münster, Germany DA - 09.09.2018 KW - PBFSM KW - RFA KW - LA-ICP-MS KW - Polypropylen KW - Polystyrol PY - 2018 AN - OPUS4-47028 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Piechotta, Christian T1 - Environmental sustainability and –stability of Materials concerning the Migration of pollutants N2 - MaUS is an acronym for ”Material und Umweltsimulationen“. Plastics are in the focus of environmental politics due to their long-term behaviour and therefore to their persistence. Not only that they appear as visible contaminants in the sea and on the beach, but their unknown behaviour concerning their additives as well as the related transformation products are anxious. Therefore, we wish to establish a certified reference method to provide a method for testing plastics. Aim of this project is the development of fast motion standard reference methods for testing plastics regarding to their environmental compatibility. To establish these testing methods, we use polystyrene (PS) and polypropylene (PP) with environmental relevant brominated flame retardants, known for their persistent bioaccumulative and toxic (PBT) properties. In case of PS the material contains 1 wt% of 1,2,5,6,9,10-hexabromocyclododecan (HBCD) and in case of PP 0.1 wt% bromodiphenylether (BDE-209), which is known as a substance of very high concern (SVHC). Furthermore, we use polycarbonate (PC), which is still used as material in baby flasks and releases Bisphenol A (BPA), an estrogenic active substance. As an additional material PTFE is used for its importance as a source for two ubiquitous environmental substances (PFOS and PFOA), whose toxicological effects are still incompletely known. The focus in this current work is set on the transfer of potential pollutants out of applied materials mentioned above into environmental compartments like water or soil. Here an accelerated aging concept should be developed to shortened time consuming natural processes. For these resulting simulations we use a programmable weathering chamber with dry and wet periods and with high and low temperatures. These programmes run for several weeks and according to a defined sampling schedule we take water samples, run a clean-up procedure by SPE (Molecular imprinted polymers (MiPs) resp. polymer-based cartridges (Waters Oasis HLB)) and analyse them by HPLC-UV resp. LC-MS/MS. Of most interest in case of flame retardants are photocatalytic transformation products. Therefore, we conduct a non-target-screening resp. a suspected target-screening by LC-MS/MS and HRMS. T2 - Project meeting PlasticsEurope - BAM CY - Leverkusen, Germany DA - 06.11.2018 KW - Environmental simulation KW - Pollutants PY - 2018 AN - OPUS4-47026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Cui A1 - Otto, S. A1 - Dorn, M. A1 - Heinze, K. A1 - Resch-Genger, Ute T1 - Luminescent TOP nanosensors for simultaneously measuring temperature, oxygen, and pH at a single excitation wavelength N2 - Two nanosensors for simultaneous optical measurements of the bioanalytically and biologically relevant analytes temperature (“T”), oxygen (“O”), and pH (“P”) have been designed. These “TOP” nanosensors are based on 100 nmsized silica-coated polystyrene nanoparticles (PS-NPs) doped with a near-infrared emissive oxygen- and temperature-sensitive chromium(III) complex ([Cr(ddpd)2][BPh4]3, CrBPh4) and an inert reference dye (Nile Red, NR or 5,10,15,20tetrakis(pentafluorophenyl) porphyrin, TFPP) and are covalently labeled with pHsensitive fluorescein isothiocyanate (FITC). These emitters can be excited at the same wavelength and reveal spectrally distinguishable emission bands, allowing for ratiometric intensity-based and time-resolved studies in the visible and near-infrared wavelength region. Studies in PBS buffer solutions and in a model body liquid demonstrate the applicability of these nanosensors for the sensitive luminescence readout of TOP simultaneously at the same spatialposition. KW - Medical diagnostics KW - Sensor KW - Nanoparticle KW - Fluorescence KW - Nanosensor KW - Oxygen KW - Temperature KW - pH KW - Ratiometric KW - Lifetime KW - NIR KW - Cr(III) complex KW - Dye KW - FITC KW - Environment PY - 2019 DO - https://doi.org/10.1021/acs.analchem.8b05060 SN - 0003-2700 VL - 91 IS - 3 SP - 2337 EP - 2344 PB - ACS AN - OPUS4-47455 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraft, Marco A1 - Würth, Christian A1 - Palo, Emilia A1 - Soukka, Tero A1 - Resch-Genger, Ute T1 - Colour-optimized quantum yields of Yb, Tm Co-doped upconversion nanocrystals N2 - Wepresent here a systematic analysis of the influence of Tm3+ Doping concentrations (xTm) on the excitation power (P)-dependent upconversion luminescence and -performance of hexagonal-Phase NaYF4: 20% Yb3+, xTm%Tm3+ upconversion nanoparticles (UCNPs) for xTm of 0.2, 0.5, 0.8, 1.2, and 2.0, respectively. Our results reveal the influence of these differentTm3+ doping concentrations with respect to optimized upconversion quantum yield (ΦUC) values of the variousTm3+ upconversion emission bands, with the highestΦUC values of theTm3+ emission bands above 700 nmresulting for different xTm values as theTm3+ emission bands below 700 nm. This underlines the potential ofTm3+ dopant concentration for colour tuning. Special emphasis was dedicated to the spectroscopic parameters that can be linked to the (de)population pathways of the variousTm3+ energy levels, like the P- and xTm-dependent slope factors and the intensity ratios of selected emission bands. The evaluation of all parameters indicates that not only energy transfer upconversion-, but also crossrelaxation processes between neighbouringTm3+ ions play a vital role in the (de)population of the excited energy levels of Yb3+, Tm3+ codoped nanocrystals. KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Mechanism KW - Quantum yield KW - Photophysics KW - Lifetime PY - 2019 DO - https://doi.org/10.1088/2050-6120/ab023b SN - 2050-6120 VL - 7 IS - 2 SP - 024001, 1 EP - 6 PB - IOP AN - OPUS4-47420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - EvstigneevT, Roman V. A1 - Parfenov, Peter S. A1 - Dubavik, Aliaksei A1 - Cherevkov, Sergei A A1 - Fedorov, Anatoly V A1 - Martynenko, Irina V. A1 - Resch-Genger, Ute A1 - Ushakova, Elena V. A1 - Baranov, Alexander V. T1 - Time-resolved FRET in AgInS2/ZnS-CdSe/ZnS quantum dot systems N2 - The fast and accurate detection of disease-related biomarkers and potentially harmful analytes in different matrices is one of the main challenges in the life sciences. In order to achieve high signal-to-background ratios with frequently used photoluminescence techniques, luminescent reporters are required that are either excitable in the first diagnostic window or reveal luminescence lifetimes exceeding that of autofluorescent matrix components. Here, we demonstrate a reporter concept relying on broad band emissive ternary quantum dots (QDs) with luminescence lifetimes of a few hundred nanoseconds utilized for prolongating the lifetimes of organic or inorganic emitters with lifetimes in the order of a very few 10 ns or less through fluorescence resonant energy transfer. Using spectrally resolved and time-resolved measurements of the system optical response we demonstrate the potential of lifetime multiplexing with such systems exemplarily for AgInS2/ZnS and CdSe/ZnS QDs. KW - Nano KW - Nanomaterial KW - Ternary quantum dots KW - AIS KW - Semiconductor nanocrystal KW - Photoluminescence KW - Mechanism KW - Quantum yield KW - Photophysics KW - Energy transfer KW - Lifetime KW - Time-gated emission PY - 2019 DO - https://doi.org/10.1088/1361-6528/ab0136 SN - 0957-4484 SN - 1361-6528 VL - 30 IS - 19 SP - 195501, 1 EP - 7 PB - IOP Publishing Ltd AN - OPUS4-47434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Measuring photoluminescence quantum yields of molecular and nanocrystal emitters N2 - Mandatory for the comparison of different emitter classes and the rational design of the next generation of molecular and nanoscale reporters are reliable and quantitative photoluminescence measurements. This is of special relevance for all fluorescence applications in the life and material sciences. In the following, procedures for the determination of this spectroscopic key parameter are presented including pitfalls and achievable uncertainties and material-specific effects related to certain emitter classes are addressed. T2 - National Research Council Canada (NRC) CY - Ottawa, Canada DA - 11.12.2018 KW - Photoluminescence KW - Quantum yield KW - Instrument calibration KW - Quality assurance KW - Measurement uncertainty KW - Dye KW - Nanocrystal KW - Integrating sphere spectroscopy KW - Absolute measurement PY - 2018 AN - OPUS4-47550 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Biophotonics at BAM – From photophysics of fluorescent nanocrystals to surface group analysis with optical methods N2 - Optical spectroscopic studies of the influence of size, particle architecture, and surface chemistry of different types of photoluminescent nanocrystals with emission in the vis/NIR will be presented including semiconductor quantum dots and lanthanide-based upconversion nanoparticles. This will include the photophysics of these materials assessed with steady state and time-resolved fluorometry on the ensemble and single particle level and concepts for the quantification of surface groups at nanomaterials with optical methods using cleavable probes and catch-and-release assays. T2 - Fakultät der University of Ottawa CY - Ottawa, Canada DA - 10.12.18 KW - Photoluminescence KW - Quantum yield KW - Nanocrystal KW - Semiconductor quantum dot KW - Upconversion nanoparticle KW - Integrating sphere spectroscopy KW - Cleavable probe KW - Surface analysis KW - Ligand quantification PY - 2018 AN - OPUS4-47551 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Photoluminescence Properties of Different Types of Nanocrystals at the Ensemble and Single Emitter Level N2 - Correlating the photoluminescence (PL) properties of nanomaterials like semiconductor nanocrystals (QDs) and upconversion nanocrystals (UCNPs) assessed in ensemble studies and at the single particle level is increasingly relevant for applications of these nanomaterials in the life sciences like bioimaging studies or their use as reporters in microfluidic assays. Here we present a comparison of the spectroscopic properties of ensembles and single emitters for QDs like II/VI QDs and cadmium-free AIS/ZnS QDs as well as different UCNPs. The overall goal of this study was to derive particle architectures well suited for spectroscopic and microscopic applications. T2 - BIOSSPIE CY - San Francisco, CA, USA DA - 02.02.2019 KW - Quantum yield KW - Nanomaterial KW - Photoluminescence KW - Absolute fluorometry KW - Integrating sphere spectroscopy, KW - NIR KW - IR KW - Fluorescence KW - Nanoparticle KW - Semiconductor KW - Quantum dot KW - Single particle spectroscopy KW - Surface chemistry PY - 2019 AN - OPUS4-47358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Seismic methods to test concrete strcutures N2 - Seismic methods are increasingly used to improve ultrasonic imaging and monitoring of concrete. At BAM, we are research mainly the use of Reverse Time Migration to get better images from ultrasonic echo data of thick, complex concrete structures. Coda wave interferometry is used to detect subtle changes in concrete constructions, e. g. using embedded ultasonic transducers. T2 - Geophysikalisches Seminar der Universität Potsdam CY - Potsdam,. Germany DA - 25.01.2019 KW - Concrete KW - Ultrasound KW - Monitoring KW - Imaging PY - 2019 AN - OPUS4-47302 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geißler, Daniel T1 - NanoGenotox - Automatable Determination of the Genotoxicity of Nanoparticles with DNA-based Optical Assays N2 - Nanomaterials are used in many different applications in the material and life sciences. Examples are optical reporters, barcodes, and nanosensors, magnetic and optical contrast agents, and catalysts. Due to their small size and large surface area, there are also concerns about their interaction with and uptake by biological systems. This has initiated an ever increasing number of cyctoxicity studies of nanomaterials of different chemical composition and surface chemistry, but until now, the toxicological results presented by different research groups often do not address or differ regarding a potential genotoxicity of these nanomaterials. This underlines the need for a standardized test procedure to detect genotoxicity.1,2 Aiming at the development of fast, easy to use, and automatable microscopic methods for the determination of the genotoxicity of different types of nanoparticles, we assess the potential of the fluorometric γH2AX assay for this purpose. This assay, which can be run on an automated microscopic detection system, relies on the determination of DNA double strand breaks as a sign for genotoxicity.3 Here, we present first results obtained with broadly used nanomaterials like CdSe/CdS and InP/ZnS quantum dots as well as iron oxide, gold, and polymer particles of different surface chemistry with previously tested colloidal stability. These studies will be also used to establish nanomaterials as positive and negative genotoxicity controls or standards for assay performance validation for users of this fluorometric genotoxicity assay. In the future, after proper validation, this microscopic platform technology will be expanded to other typical toxicity assays. References. (1) Landsiedel, R.; Kapp, M. D.; Schulz, M.; Wiench, K.; Oesch, F., Reviews in Mutation Research 2009, 681, 241-258. (2) Henriksen-Lacey, M.; Carregal-Romero, S.; Liz-Marzán, L. M., Bioconjugate Chem. 2016, 28, 212-221. (3) Willitzki, A.; Lorenz, S.; Hiemann, R.; Guttek, K.; Goihl, A.; Hartig, R.; Conrad, K.; Feist, E.; Sack, U.; Schierack, P., Cytometry Part A 2013, 83, 1017-1026. T2 - 9th International Conference on Nanotoxicology - New tools in risk assessment of nanomaterials CY - Dusseldorf/Neuss, Germany DA - 18.09.2018 KW - Nano KW - Nanotoxicity KW - Fluorescence KW - Quantum dot KW - Surface KW - Passivation shell KW - Automated assay KW - Nanoparticle PY - 2018 AN - OPUS4-47540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, Katrin T1 - Determination of Photoluminescence Quantum Yields of Semiconductor Quantum Dots with Fluorescence Correlation Spectroscopy N2 - There is an increasing interest in bridging the gap between the photoluminescence (PL) properties of nanomaterials like semiconductor nanocrystals (QDs) commonly assessed in ensemble studies and the PL features of single QDs for life sciences applications such as bioimaging studies or use in microfluidic assays. The fluorescence quantum yield (ΦF) is a key performance parameter for all molecular and nanoscale emitters, increasingly employed in nanoscience, nanotechnology, and medical diagnostics. ΦF determines not only the signal size together with the reporter´s molar extinction coefficient, yet it is particularly relevant for nanocrystals like QDs with coordinatively bound surface ligands and size- and surface chemistry-dependent PL characteristics. The importance of ΦF measurements at ultralow concentration encouraged us to explore the potential of fluorescence correlation spectroscopy (FCS) for the relative determination of ΦF of ligand-stabilized CdTe nanocrystals in comparison to molecular dyes with closely matching spectral properties and known ΦF. We describe a FCS-based method for the relative determination of ΦF of dispersed QDs at ultralow concentrations, and procedures to overcome QD-inherent challenges like complex and power-dependent blinking behavior as well as ligand- and QD-specific aggregation. We could demonstrate the potential of this approach by comparison with steady state ensemble measurements. T2 - BIOS SPIE 2019 CY - San Francisco, CA, USA DA - 02.02.2019 KW - Quantum yield KW - Quantum dots KW - FCM PY - 2019 AN - OPUS4-47427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Luminescence measurements, calibration strategies and photoluminescence quantum yields N2 - Different types of optical spectroscopies are introduced with special emphasis on method-inherent limitations and reliable instrument calibration and performance validation. In addition, procedures for the determination of spectroscopic key parameters like the photoluminescence quantum yield are presented including required instrument calibrations and material-specific effects related to certain emitters. T2 - Fakultät der University of Ottawa CY - Ottawa, Canada DA - 11.12.2018 KW - Quality assurcance KW - Optical spectroscopy KW - Method comparison KW - Photoluminescence KW - Calibration KW - Performance validation KW - Dye KW - Nanoparticle KW - Quantum dots KW - Quantum yields KW - Uncertainty KW - Method validation PY - 2019 AN - OPUS4-47630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Optical spectroscopy – Techniques, instrumentation, and typical molecular and nanoscale reporters N2 - Different types of optical spectroscopies are introduced with special emphasis on method-inherent limitations and reliable instrument calibration and performance validation. In addition, different classes of molecular and nanocrystalline emitters are presented and the underlying photophysical processes are briefly described. T2 - Fakultät der University of Ottawa CY - Ottawa, Canada DA - 11.12.2018 KW - quality assurcance KW - Optical spectroscopy KW - Method comparison KW - Photoluminescence KW - Calibration KW - Performance validation KW - Dye KW - Nanoparticle KW - Quantum dots KW - Quantum yields KW - Uncertainty KW - Method validation PY - 2018 AN - OPUS4-47631 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Ultrasonic monitoring of structural concrete elements N2 - Ultrasonic transmission measurements are used to monitor concrete elements mostly on a laboratory scale since decades. Recently, coda wave interferometry, a technique adapted from seismology, has been introduced to civil engineering experiments. It can be used to reveal subtle changes in concrete samples and even large construction elements without having a transducer directly at the location where the change is taking place. The methodology works best with embedded transducers to avoid coupling issues or excessive environmental influence. These transducers can be used for newly built and existing structures. Recently, large concrete beams have been equipped with a network of transducers and loaded until failure. Using code wave interferometry, it was possible to visualize stress fields and damaged areas. This paper gives an overview of the state of the art, recent results achieved at BAM and a task list for further results and development. T2 - International Conference on Sustainable Materials, Systems and Structures (SMSS 2019) CY - Rovinj, Croatia DA - 20.03.2019 KW - Concrete KW - Ultrasound KW - Monitoring KW - coda wave interferometry PY - 2019 AN - OPUS4-47676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rezvani, A. A1 - Wang, Z. A1 - Wegner, Karl David A1 - Soltanmoradi, H. A1 - Kichigin, A. A1 - Zhou, X. A1 - Gantenberg, T. A1 - Schram, J. A1 - Zubiri, B. A. A1 - Spiecker, E. A1 - Walter, J. A1 - Resch-Genger, Ute A1 - Segets, D. T1 - Separation of Indium Phosphide/Zinc Sulfide Core−Shell Quantum Dots from Shelling Byproducts through Multistep Agglomeration N2 - Semiconductor quantum dots (QDs) possess unique electronic and optical properties, making them promising candidates for applications in lightemitting diodes, solar cells, bioimaging, and photocatalysis. Precise control over their size, shape, and chemical and electronic structure is crucial to ensure the desired functional properties and optimize device performance. However, challenges in QD synthesis and post-synthesis modification persist, especially in large-scale production. This study addresses the classification of QDs synthesized in a tubular flow reactor consisting of a mixture of the desired InP/ZnS core−shell QDs and QDs made from the shell material, i.e., here ZnS QDs formed as a byproduct during the formation step of the ZnS shell. The homogeneous nucleation of ZnS nanoparticles from the shelling material introduces a heterogeneity in size and composition and affects the optical properties of the resulting QDs. To address this issue, we developed a size-selective agglomeration (SSA) technique by incrementally introducing ethanol as a poor solvent and classified the synthesized QDs into 13 distinct fractions. These 13 fractions are sorted into three distinct groups: (i) larger InP/ZnS QDs, (ii) a combination of smaller InP/ZnS QDs and larger ZnS QDs, and (iii) predominant ZnS QDs with some very tiny InP/ZnS QDs. The comprehensive characterization of the fractions was conducted using UV−visible absorption spectroscopy, photoluminescence spectroscopy, high-resolution scanning transmission electron microscopy, energy-dispersive X-ray spectroscopy, total reflection X-ray fluorescence, and analytical ultracentrifugation. We could demonstrate that our method effectively separated unwanted ZnS QDs from the target InP/ZnS QDs. In addition, the fractions enriched in smaller InP/ZnS QDs exhibited a higher photoluminescence quantum yield compared to the fractions with larger QDs. This demonstrates the efficacy of SSA in finetuning the composition of QD mixtures produced on a larger scale to improve their functional properties. This approach provides fundamental understanding toward the development of a scalable two-dimensional classification process for such ultrasmall nanoparticles by particle size and composition. KW - Quality assurance KW - Reference material KW - Nano KW - Particle KW - Quantum dot KW - Synthesis KW - Flow reactor KW - InP KW - Shell KW - ZnS KW - Surface chemistry KW - Method KW - Fluorescence KW - Quantum yield KW - TEM PY - 2025 DO - https://doi.org/10.1021/acsnano.4c18530 SN - 1936-086X VL - 19 IS - 20 SP - 19080 EP - 19094 PB - ACS Publications AN - OPUS4-63215 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kothavale, S. A1 - Jadhav, A. G. A1 - Scholz, Norman A1 - Nirmalananthan-Budau, Nithiya A1 - Behnke, Thomas A1 - Resch-Genger, Ute A1 - Sekar, N. T1 - Corrigendum to "Deep red emitting triphenylamine based coumarin-rhodamine hybrids with large stokes shift and viscosity sensing: Synthesis, photophysical properties and DFT studies of their spirocyclic and open forms" [Dyes Pigments 137 (2017) 329-341] N2 - We designed and synthesized triphenylamine based and coumarin fused rhodamine hybrid dyes and characterized using 1H, 13C NMR and HR-LCMS analysis. Both the newly synthesized hybrid dyes were found to show red shifted absorption as well as emissions and large Stokes shift (40e68 nm) as compared to the small Stokes shift (25e30 nm) of reported dyes Rhodamine B and 101. Photophysical properties of these dyes were studied in different solvents and according to the solvents acidity or basicity they preferred to remain in their spirocyclic or open form in different ratio. We studied the spirocyclic as well as open form derivatives of these dyes for their viscosity sensitivity in three different mixture of solvents i.e. polar-protic [EtOH-PEG 400], polar-aprotic [toluene-PEG 400] and non-polaraprotic [toluene-paraffin]. They are found to show very high viscosity sensitivity in polar-protic mixture of solvents [EtOH-PEG 400] and hence concluded that both polarity as well as viscosity factor worked together for the higher emission enhancement rather than only viscosity factor. As these dyes showed very high viscosity sensitivity in their spirocyclic as well as open form, they can be utilized as viscosity sensors in visible as well as deep red region. We also correlated our experimental finding theoretically by using Density Functional theory computations. KW - Dye KW - Fluorescence KW - Synthesis KW - Quantum yield KW - Lifetime KW - Coumarin KW - Rhodamine KW - Probe KW - Viscosity PY - 2018 DO - https://doi.org/10.1016/j.dyepig.2017.06.021 SN - 0143-7208 SN - 1873-3743 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. VL - 149 SP - 929 PB - Elsevier CY - Amsterdam AN - OPUS4-44038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abraham, O. A1 - Niederleithinger, Ernst A1 - Chapeleau, X. A1 - Klikowicz, P. A1 - Brühwiler, E. A1 - Bassil, A. A1 - Wang, Xin A1 - Chakraborty, J. A1 - Bayane, I. A1 - Leduc, D. A1 - Salamak, M. A1 - Katunin, A. A1 - Sørensen, J.D. T1 - Addressing the need to monitor concrete fatigue with nondestructive testing: Results of infrastar European project N2 - Fatigue is one of the most prevalent issues, which directly influences the service life expectancy of concrete structures. Fatigue has been investigated for years for steel structures. However, recent findings suggest that concrete structures may also be significantly subjected to fatigue phenomena that could lead to premature failure of certain structural elements. To date, fatigue of reinforced concrete has been given little focus. Knowledge on the influence factors and durability/capacity effects on this material should be improved. Current technological means to measure fatigue in civil structures like bridges and wind turbines (both onshore and offshore) are outdated, imprecise and inappropriate. Meanwhile, this topic has got much more attention as time-variant loading on concrete structures plays an increasing role, e.g. in bridges with increasing traffic and heavier trucks, and for wind turbines for renewable energy production, e.g. for offshore wind turbine support structures affected by wind and waves. The European Innovative Training Networks (ITN) Marie Skłodowska-Curie Actions project INFRASTAR (Innovation and Networking for Fatigue and Reliability Analysis of Structures - Training for Assessment of Risk) provides research training for 12 PhD students. The project aims to improve knowledge for optimizing the design of new structures as well as for more realistic verification of structural safety and more accurate prediction of the remaining fatigue lifetime of existing concrete structures. First, the INFRASTAR research framework is detailed. Then it will be exemplified through the presentation of the major results of the four PhD students involved in the work package dealing with auscultation and monitoring. This includes the development and improvement of Fiber Optics (FO) and Coda Wave Interferometry (CWI) for crack sizing and imagery, new sensor technologies and integration, information management, monitoring strategy for fatigue damage investigation and lifetime prediction. T2 - SMT and NDT-CE 2018 CY - New Brunswick, NJ, USA DA - 27.08.2018 KW - Concrete KW - Fatigue KW - Crack KW - Monitoring KW - Non-destructive testing PY - 2019 UR - https://asnt.org/smt18papers SN - 978-1-57117-456-7 VL - 11/19 SP - 2 EP - 13 PB - The American Society for Nondestructive Testing, Inc. CY - Columbus, OH, USA AN - OPUS4-47237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst A1 - Wiggenhauser, Herbert A1 - Mielentz, Frank A1 - Bertschat, Anja-Sophie A1 - Mierschke, Vivien A1 - Werner, Andreas T1 - Untersuchung von Veränderungen in Beton mit Ultraschall-Codawelleninterferometrie N2 - Die Coda transmittierter Ultraschallsignale in Beton enthält Informationen zu Struktur und Zustand des Materials bzw. deren Änderung. Relevant sind u. a. Temperatur, Stress, Feuchtigkeit und verschiedene Schädigungsmechanismen. Die zahlreichen Einflussfaktoren sind nur schwer zu trennen und die Messeffekte oft zu Beginn sehr klein.Die CWI ermöglicht die Detektion kleinster Geschwindigkeitsveränderungen durch den Vergleich, der in kleinen Schritten gestauchten oder gestreckten Signalen mit eine Referenzmessung. Andere Indikatoren für Änderungen im Material sind: • Kreuzkorrelation • Laufzeit direkte Welle • Energie/Amplitude • Änderungen im Frequenzspektrum Die beschriebene Technik wird von uns bisher primär in klein- und großskaligen Laborversuchen genutzt. Die Forschung konzentriert sich auf die Untersuchung und Trennung verschiedener Einflusseffekte. Aber auch erste reale Bauwerke wurden schon instrumentiert, z. B. Brücken und eine Tunneldecke. T2 - 77. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Potsdam, Germany DA - 27.03.2017 KW - Beton Ultraschall Monitoring PY - 2017 AN - OPUS4-39661 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauli, J. A1 - Güttler, Arne A1 - Schneider, T. A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - Fluorescence Quantum Yield Standards for the UV/Visible/NIR: Development, Traceable Characterization, and Certification N2 - The rational design of next generation molecular and nanoscale reporters and the comparison of different emitter classes require the determination of the fluorometric key performance parameter fluorescence quantum yield (Φf), i.e., the number of emitted photons per number of absorbed photons. Main prerequisites for reliable Φf measurements, which are for transparent luminophore solutions commonly done relative to a reference, i.e., a fluorescence quantum yield standard of known Φf, are reliable and validated instrument calibration procedures to consider wavelength-, polarization-, and time-dependent instrument specific signal contributions, and sufficiently well characterized fluorescence quantum yield standards. As the standard’s Φf value directly contributes to the calculation of the sample’s Φf, its accuracy presents one of the main sources of uncertainty of relative Φf measurements. To close this gap, we developed a first set of 12 fluorescence quantum yield standards, which absorb and emit in the wavelength region of 330−1000 nm and absolutely determined their Φf values with two independently calibrated integrating sphere setups. Criteria for standard selection and the configuration of these novel fluorescence reference materials are given, and the certification procedure is presented including homogeneity and stability studies and the calculation of complete uncertainty budgets for the certified Φf values. The ultimate goal is to provide the community of fluorescence users with available reference materials as a basis for an improved comparability and reliability of quantum yield data since the measurement of this spectroscopic key property is an essential part of the characterization of any new emitter. KW - Optical spectroscopy KW - Traceability KW - Reference product KW - Dye KW - Fluorescence KW - Quantum yield KW - Reference material KW - Reference data KW - Certification KW - Quality assurance PY - 2023 DO - https://doi.org/10.1021/acs.analchem.2c05530 VL - 95 SP - 5671 EP - 5677 PB - American Chemical Society AN - OPUS4-58151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Cui A1 - Otto, S. A1 - Dorn, M. A1 - Kreidt, E. A1 - Lebon, J. A1 - Sršan, L. A1 - Di Martino-Fumo, P. A1 - Gerhards, M. A1 - Seitz, M. A1 - Resch-Genger, Ute A1 - Heinze, K. T1 - Deuterierter molekularer Rubin mit Rekord-Lumineszenzquantenausbeute N2 - Der kürzlich publizierte Chrom(III)-Komplex 13+([Cr(ddpd)2]3+) zeigt in wässriger Lösung unter Umgebungsbedingungen eine bemerkenswert starke Emission im nahen Infrarot-Bereich mit einer Emissionswellenlänge von 775 nm. Geschicktes Ligandendesign verhindert strahlungslose Desaktivierungsprozesse wie Photosubstitution, Rück-Intersystem-Crossing und trigonale Verzerrungen und führt damit zu einer Phosphoreszenzlebensdauer im Bereich von Mikrosekunden. In Abwesenheit von Energieakzeptoren wie molekularem Sauerstoff verbleibt nur Energietransfer zu hochenergetischen Oszillatoren der Liganden und Lösungsmittelmoleküle wie beispielsweise OH- und CH-Streckschwingungen als Desaktivierungspfad. Selektive Deuterierung der ddpd-Liganden und der Lösungsmittel l-sst die Effizienz dieser Oszillatoren bei der Desaktivierung angeregter Zustände erkennbar werden. Gezieltes Ausschalten dieser Relaxationspfade führt zu einer Quantenausbeute von 30% und einer Lebensdauer von 2.3 Millisekunden bei Raumtemperatur in Lösung – Rekordwerte für einen Komplex, der auf dem Element Chrom basiert. Diese fundamentalen Erkenntnisse ebnen den Weg für gezieltes Ligandendesign zur Synthese lumineszierender Komplexe mit gut verfügbaren Übergangsmetallen. KW - Cr(III)-Komplex KW - Rekord Luminescence Quantum Ausbeute KW - Abklingzeit PY - 2018 DO - https://doi.org/10.1002/ange.201711350 SN - 1521-3757 VL - 130 IS - 4 SP - 1125 EP - 1130 PB - Wiley-VCH Verlag & Co. KGaA CY - Weinheim AN - OPUS4-45086 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vössing, Konrad A1 - Niederleithinger, Ernst ED - Faix, O. T1 - Nondestructive assessment and imaging methods for internal inspection of timber. A review. N2 - This paper reviews state-of-the-art in nondestructive testing (NDT) and semidestructive testing (SDT) methods applicable for imaging the condition of structural timber. Both NDT and SDT imaging reveal defects, damages, and decay, while the extent of wood decay can also be quantified. Combined with an appropriate data interpretation concerning the internal defects, the mechanical properties of the material can also be assessed. The possibilities and limitations of the most relevant individual NDT and SDT methods, also in combination with each other, are outlined and compared. To facilitate comparison, many observations are reported based on the same test specimen. KW - Drilling resistance KW - Electrical resistivity KW - Radar KW - Radiography KW - Sonic stress wave KW - Ultrasound KW - Non destructive testing KW - Timber structure PY - 2018 DO - https://doi.org/10.1515/hf-2017-0122 SN - 0018-3830 SN - 1437-434X VL - 72 IS - 6 SP - 467 EP - 476 PB - De Gruyter CY - Berlin AN - OPUS4-44445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Resch-Genger, Ute A1 - Abram, Sarah-Luise A1 - Tavernaro, Isabella A1 - Zou, Shan A1 - Johnston, Linda T1 - Behind the Paper: Nanoscale Reference and Test Materials for the Validation of Characterization Methods for Engineered Nanomaterials – Current State, Limitations and Needs N2 - Engineered nanomaterials (NMs) of different material composition, morphology, and surface chemistry are widely used in material and life sciences. For NM quality control and risk assessment, NM key properties must be characterized with validated methods, requiring reference materials (RMs). KW - Engineered Nanomaterials KW - Nanoscale reference materials KW - Interlaboratory comparisons KW - Traceability KW - Standardization and Regulation KW - Nano KW - Particle KW - Quality assurance KW - Surface chemistry PY - 2025 UR - https://communities.springernature.com/posts/nanoscale-reference-and-test-materials-for-the-validation-of-characterization-methods-for-engineered-nanomaterials-current-state-limitations-and-needs SP - 1 EP - 3 PB - Springer Nature CY - Online AN - OPUS4-62572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nirmalananthan-Budau, Nithiya A1 - Budau, J. H. A1 - Moldenhauer, Daniel A1 - Hermann, G. A1 - Kraus, Werner A1 - Hoffmann, Katrin A1 - Paulus, Beate A1 - Resch-Genger, Ute T1 - Substitution pattern controlled aggregation-induced emission in donor-acceptor-donor dyes with one and two propeller-like triphenylamine donors N2 - We present a comparative study of the spectroscopic properties of the donor–acceptor–donor substituted dyes triphenylamine-allylidenemalononitrile-julolidine (TMJ) and triphenylamine-allylidenemalononitriletriphenylamine (TMT), bearing one and two propeller-like triphenylamine donor moieties, in solvents of varying polarity and viscosity and in the aggregated and solid state. Our results reveal control of the aggregation-induced spectroscopic changes and the packing motifs of the dye molecules in the solid state by the chemical nature and structure of the second nitrogen-containing donor, i.e., a planar and a rigid julolidine or a twisted triphenyl group. Assuming that the TMT and TMJ aggregates show a comparable arrangement of the molecules to the respective crystals, these different molecular interactions in the solid state are responsible for aggregation induced emission (AIE) in the case of TMT and its absence for TMJ. Moreover, a versatile strategy for the fluorescence enhancement of only weakly emissive AIE dyes is shown, turning these dyes into bright nanoscale fluorescent reporters by using them as stains for preformed polymer particles. KW - Nano KW - Nanoparticle KW - Photoluminescence KW - Fluorescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - Dye KW - Enhancement KW - Particle KW - Polarity KW - AIE KW - Aggregation KW - Aggregation-induced emission KW - Solid state emission PY - 2020 DO - https://doi.org/10.1039/d0cp00413h VL - 22 IS - 25 SP - 14142 EP - 14154 AN - OPUS4-50967 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moser, Marko A1 - Schneider, Ralf A1 - Behnke, Thomas A1 - Schneider, Thomas A1 - Falkenhagen, Jana A1 - Resch-Genger, Ute T1 - Ellman’s and aldrithiol assay as versatile and complementary tools for the quantification of thiol groups and ligands on nanomaterials N2 - Simple, fast, and versatile methods for the quantification of thiol groups are of considerable interest not only for protein analysis but also for the characterization of the surface chemistry of nanomaterials stabilized with thiol ligands or bearing thiol groups for the subsequent (bio-) functionalization via maleimide−thiol chemistry. Here, we compare two simple colorimetric assays, the widely used Ellman’s assay performed at alkaline pH and the aldrithiol assay executed at acidic and neutral pH, with respect to their potential for the quantification of thiol groups and thiol ligands on different types of nanoparticles like polystyrene nanoparticles, semiconductor nanocrystals (SC NC), and noble metal particles, and we derive criteria for their use. In order to assess the underlying reaction mechanisms and to obtain stoichiometry factors mandatory for reliable thiol quantification, both methods were studied photometrically and with electrospray ionization time-of-flight mass spectrometry (ESI-TOF-MS), thereby demonstrating the influence of different thiols on the reaction mechanism. Our results underline the suitability of both methods for the quantification of directly accessible thiol groups or ligands on the surface of 2D- and 3D-supports, here exemplarily polystyrene nanoparticles. Moreover, we could derive strategies for the use of these simple assays for the determination of masked (i.e., not directly accessible) thiol groups like disulfides such as lipoic acid and thiol stabilizing ligands coordinatively bound to Cd and/or Hg surface atoms of II/VI and ternary SC NC and to gold and silver nanoparticles. KW - Nanoparticles KW - Ligands KW - Ellman KW - Aldrithiol KW - Quantification PY - 2016 DO - https://doi.org/10.1021/acs.analchem.6b01798 SN - 0003-2700 SN - 1520-6882 VL - 88 IS - 17 SP - 8624 EP - 8631 PB - ACS Publications CY - Washington AN - OPUS4-37561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Landis, E. A1 - Hassfras, Emiel A1 - Oesch, Tyler A1 - Niederleithinger, Ernst T1 - Relating ultrasonic signals to concrete microstructure using X-ray computed tomography N2 - With a goal to improve our understanding of the relationships between microstructural features and ultrasonic signal behavior, concrete specimens of varying water-to-cement ratio were imaged using X-ray computed tomography (CT), and subsequently subjected to ultrasonic testing. From the CT scans, measurements were made of cement paste density and number of interfaces. Ultrasonic signals produced using a through-transmission configuration were analyzed and fit to a diffusion model to separate absorption from scattering attenuation. The results showed that at the frequencies tested, ultrasonic dissipation rate correlated weakly with paste density, while diffusivity correlated well with number of interfaces, but only if entrained air is considered separately. Cement paste density was found to be very well predicted by diffusivity, leading to a clear power-law relationship between diffusivity and compressive strength. KW - Concrete KW - Ultrasound KW - Strength KW - CT PY - 2021 DO - https://doi.org/10.1016/j.conbuildmat.2020.121124 SN - 0950-0618 VL - 268 SP - Paper 121124, 1 EP - 12 PB - Elsevier Ltd. AN - OPUS4-52073 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Xin A1 - Chakraborty, J. A1 - Niederleithinger, Ernst T1 - Noise Reduction for Improvement of Ultrasonic Monitoring Using Coda Wave Interferometry on a Real Bridge N2 - Reinforced concrete bridges are iconic parts of modern infrastructure. They are designed for a minimum service life of 100 years. However, environmental factors and/or inappropriate use might cause overload and accelerate the deterioration of bridges. In extreme cases, bridges could collapse when necessary maintenance lacks. Thus, the permanent monitoring for structure health assessment has been proposed, which is the aim of structural health monitoring (SHM). Studies in laboratories have shown that ultrasonic (US) coda wave interferometry (CWI) using diffuse waves has high sensitivity and reliability to detect subtle changes in concrete structures. The creation of micro-cracks might be recognized at an early stage. Moreover, large-volume structures can be monitored with a relatively small number of US transducers. However, it is still a challenge to implement the CWI method in real SHM practical applications in an outdoor environment because of the complex external factors, such as various noise sources that interfere with the recorded signals. In this paper, monitoring data from a 36-m long bridge girder in Gliwice, Poland, instrumented with embedded US transducers, thermistors, and vibrating wire strain gauges, is presented. Noise estimation and reductionmethods are discussed, and the influence of traffic, as well as temperature variation, are studied. As a result, the relative velocity variation of US waves following the temperature change with a very high precision of 10−4% is shown, and a good bridge health condition is inferred. The influence of lightweight real traffic is negligible. The study verified the feasibility of the implementation of the CWI method on real bridge structures. KW - Ultrasound KW - Coda Wave Interferometry KW - Noise KW - Concrete KW - Bridge PY - 2021 DO - https://doi.org/10.1007/s10921-020-00743-9 VL - 40 IS - 1 SP - Article number: 14 PB - Springer Nature AN - OPUS4-52052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - News from NDT@BAM N2 - The presentation summarizes some recent research at BAM in the field of NDT in civil engineering. the firste xample decribes lab experiments on the degardation of concrete during tunnel fires. Radar measuremenst were sucessfully used to detect interior damage. The second example decribes the first ever experiment on using muon imaging to evaluate concrete constructions. T2 - TRB 100th Annual Meeting, Subcommittee AKB40(1) CY - Online meeting DA - 05.01.2021 KW - Non-destructive testing KW - Civil engineering KW - Tunnel fire KW - Radar KW - Muon imaging PY - 2021 AN - OPUS4-52053 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Traub, Heike ED - Milacic, R. ED - Scancar, J. ED - Goenaga-Infante, H. ED - Vidmar, J. T1 - Imaging of metal-based nanoparticles in tissue and cell samples by laser ablation inductively coupled plasma mass spectrometry N2 - Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is nowadays a versatile and powerful analytical method for direct solid sample analysis. The applicability has been demonstrated for a wide variety of samples covering hard and soft materials. In an imaging mode the technique provides quantitative information on the elemental distribution within a sample. LA-ICP-MS imaging is of particular interest in biomedical research as the distribution of an element gives valuable insight on uptake and distribution of essential and toxic trace elements, administered contrast agents as well es nanoparticles. LA-ICP-MS is therefore a powerful complement to other imaging techniques. Recent instrumental improvements, especially in sample chamber design, have contributed to better sensitivity and spatial resolution enabling subcellular imaging. The book chapter provides a comprehensive overview about spatially resolved localisation and quantification of various nanoparticles in cells and tissue thin sections by LA-ICP-MS. Furthermore, different sample preparation strategies and internal standardisation and calibration approaches for bioimaging by LA-ICP-MS are summarized and discussed. Metal-containing nanomaterials are used in numerous fields ranging from industrial applications to nanomedicine. Several studies have demonstrated that the physicochemical properties of nanoparticles have an impact on their pharmacokinetics, transfer and clearance. The high sensitivity and multielement capability of LA-ICP-MS enables the elucidation of interactions between tissue components and nanomaterials used as imaging probes or drug carriers. Potential toxic effects are investigated as well. Thus, LA imaging significantly supports the clinical translation of safe and efficient nanoparticles for diagnostic and therapeutic purposes. KW - Laser ablation KW - ICP-MS KW - Imaging KW - Nanoparticle KW - Nanomaterial KW - Tissue KW - Cell PY - 2021 SN - 978-0-323-85305-7 SN - 0166-526X VL - 93 SP - 173 EP - 240 PB - Elsevier CY - Amsterdam ET - 1 AN - OPUS4-52775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Witte, F. A1 - Rietsch, P. A1 - Sinha, S. A1 - Krappe, A. A1 - Joswig, J.-O. A1 - Götze, J. P. A1 - Nirmalananthan-Budau, Nithiya A1 - Resch-Genger, Ute A1 - Eigler, S. A1 - Paulus, B. T1 - Fluorescence Quenching in J‑Aggregates through the Formation of Unusual Metastable Dimers N2 - Molecular aggregation alters the optical properties of a system as fluorescence may be activated or quenched. This is usually described within the well-established framework of H- and J-aggregates. While H-aggregates show nonfluorescent blueshifted absorption bands with respect to the isolated monomer, Jaggregates are fluorescent displaying a redshifted peak. In this publication, we employ a combined approach of experiment and theory to study the complex aggregation features and photophysical properties of diaminodicyanoquinone derivatives, which show unusual and puzzling nonfluorescent redshifted Absorption bands upon aggregation. Our theoretical analysis demonstrates that stable aggregates do not account for the experimental observations. Instead, we propose an unprecedented mechanism involving metastable dimeric species formed from stable dimers to generate nonfluorescent J-aggregates. These results represent a novel kind of aggregation-induced optical effect and may have Broad implications for the photophysics of dye aggregates. KW - Fluorescence KW - Llifetime KW - Dye KW - Quantum yield KW - Label KW - Reporter KW - Aggregation KW - Monomer KW - Heory KW - Mechanism KW - photophysics PY - 2021 DO - https://doi.org/10.1021/acs.jpcb.1c01600 SN - 1520-5207 VL - 125 IS - 17 SP - 4438 EP - 4446 PB - ACS Publikations AN - OPUS4-52619 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - ZfPBau 4.0 - Herausforderungen an die ZfP im Bauwesen im Rahmen der Digitalisierung N2 - Die ZfP ist im Bauwesen bisher deutlich weniger reguliert (und auch akzeptiert) als in anderen Industriebereichen. Zum Beispiel gibt für die meisten Prüfverfahren weder Normen noch ein allgemein akzeptiertes Ausbildungs- und Zertifizierungssystem. Dies hat auch Konsequenzen für die Digitalisierung. Im Gegensatz dazu wird im Bauwesen derzeit für viele Bereiche verbindlich ein neues Verfahren zur Unterstützung von Design, Planung, Herstellung und Betrieb eingeführt: BIM (Building Information Modeling). Der Vortrag beleuchtet das Spannungsfeld zwischen dem geringen Organisations- und Standardisierungsgrad und den neuen digitalen Möglichkeiten und stellt den neuen Arbeitskreis zur ZfP 4.0 im Bauwesen vor. Er beleuchtet auch, in welchen Bereichen die ZfP im Bauwesen von Entwicklungen aus „Industrie 4.0“ und der zerstörungsfreien Prüfung in anderen Anwendungsbereichen profitieren kann - z. B. bei Datenformaten, Datenarchivierung und Schnittstellen. T2 - TAE Fachkongress Digitale Transformation im Lebenszyklus der Verkehrsinfrastruktur CY - Esslingen, Germany DA - 29.06.2021 KW - ZfPBau KW - SHM KW - Industrie 4.0 KW - BIM KW - Datenbank PY - 2021 AN - OPUS4-52914 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blanchard, V. A1 - Traub, Heike T1 - Central project for biochemical analysis of proteoglycans and glycosaminoglycans and for element-specific microscopy N2 - Nearly all disease processes are associated with variations of components of the extracellular matrix (ECM) that are typically observed during the development of inflammation. This concerns for example proteoglycans and their associated glycosaminoglycans (GAG), which have been shown to bind to cationic metal imaging probes due to their strong complexing activity. The complexing activity largely depends on the degree of GAG sulfation and/or carboxylation as well as on the GAG isomericity. In this central project, we investigate GAG structures from inflammatory disorders (namely cardiovascular diseases, inflammatory intestinal diseases and neuroinflammation) provided by researchers of the Collaborative Research Center at the molecular disaccharidic level using chromatographic and mass spectrometric methods. In parallel, the spatial localization and quantification of metal-based imaging probes are evaluated by LA-ICP-MS imaging. T2 - 1st International Symposium In vivo Visualization of Extracellular Matrix Pathology CY - Online Meeting DA - 27.05.2021 KW - Laser ablation KW - ICP-MS KW - MALDI PY - 2021 AN - OPUS4-52716 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Mess- und Prüfverfahren mit Sensorik N2 - Mess- und prüftechnische Verfahren sind zur Prozesskontrolle und Sicherheitsüberwachung in Wasserstofftechnologien von hoher Bedeutung. Typische Anwendungsgebiete von Sensoren sind Sicherheitsüberwachung, Leckdetektion und Prozesskontrolle. In diesem Beitrag werden Themen zur Erkennung von freigesetztem Wasserstoff sowie die Bestimmung des Wasserstoff-Luftverhältnisses mit Gassensoren, Fehlstellenerkennung mit geführten Ultraschallwellen zur Lebensdauerüberwachung (Structural Health Monitoring) von Wasserstoffspeichern sowie der Einsatz faseroptischer Sensoren zur Überwachung des Dehnungs- und Alterungsverhaltens sowie zur Schadensfrüherkennung von Wasserstoffspeichern vorgestellt. T2 - DVGW Kongress H2 Sicherheit CY - Online meeting DA - 27.01.2021 KW - Metrologie KW - Gassensoren KW - Structural Health Monitoring KW - Faseroptische Sensoren KW - Wasserstoff PY - 2021 AN - OPUS4-52141 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neumann, Patrick P. A1 - Kohlhoff, Harald A1 - Hüllmann, Dino A1 - Kluge, Martin A1 - Askar, Enis A1 - Habib, Abdel Karim A1 - Krentel, Daniel A1 - Mair, Georg W. A1 - Rudolph, Michael A1 - Schoppa, André A1 - Szczepaniak, Mariusz A1 - Storm, Sven-Uwe A1 - Tschirschwitz, Rico T1 - Auswirkungen von Behälterversagen bei alternativen PKW-Antrieben - Teil 2: UAV-basierte Fernerkundung von Gaswolken N2 - Verkehrsunfälle unter Beteiligung von Fahrzeugen mit alternativen Kraftstoffen wie LPG („Autogas“, Liquefied Petroleum Gas), CNG (Compressed Natural Gas, komprimiertes Erdgas) oder CGH2 (Compressed Gas Hydrogen, komprimierter Wasserstoff), bergen neue, komplexe Risiken für Passagiere, Einsatzkräfte und deren Umfeld. Im Rahmen des Projektes „CoFi-ABV“ beschäftigt sich die Bundesanstalt für Materialforschung und -prüfung (BAM) unter Berücksichtigung komplexer Brand- und Explosionsszenarien mit einer ganzheitlichen Betrachtung der Auswirkungen des unfallbedingten Versagens von Gasbehältern für alternative Kraftstoffe. Ein wichtiger Teil des Forschungsvorhabens umfasst Entwicklung, Aufbau und Validierung einer unbemannten Flugplattform (Unmanned Aerial Vehicle, UAV) zur Ferndetektion von Gaswolken. Für das sogenannte gassensitive Mini-UAV wird ein robuster Open-Path-Gasdetektor auf einer Sensorbewegungsplattform in Form eines modifizierten Kamera-Gimbals, integriert. Ziel ist es, ein leistungsfähiges und robustes Werkzeug zu entwickeln, welches Einsatzkräften im Falle eines Unfalls als Hilfe zur Abschätzung der Gefahr durch Gaswolken, ihrer Ausbreitung und der notwendigen Absperrbereiche zur Verfügung steht. Dieser Artikel ist der zweite der Reihe und legt, nach Projektvorstellung im ersten Teil, nun den Schwerpunkt auf das gassensitive Mini-UAV. KW - UAV KW - Fernerkundung KW - Open-Path-Gasdetektor KW - Alternative Antriebe/Kraftstoffe KW - Behälterversagen PY - 2016 SN - 2191-0073 VL - 6 IS - 11/12 SP - 23 EP - 28 PB - Springer-VDI-Verlag CY - Düsseldorf AN - OPUS4-38517 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fogang, S. G. A1 - Temgoua, Ranil C. T. A1 - Deussi Ngaha, M. C. A1 - Kougoum Thieda, V. A1 - Fotsop, C. G. A1 - Averie Vomo, L. A1 - Teikam Kenda, G. A1 - Ngueko Makengue, Y. P. A1 - Deffo, G. A1 - Njanja, E. ED - Teamgoua, Ranil C. T. T1 - Room-Temperature Co-Precipitation Synthesis of Magnetite Nanoparticles and Application as Electrocatalytic Platform for Agricultural Pesticides Sensing in Water N2 - This work presents a straightforward room-temperature co-precipitation method for the synthesis of magnetite nanoparticles (Fe3O4NPs) and application as electrocatalytic material for the simultaneous determination of diuron (DR) and thiabendazole (TBZ) pesticides in water for the first time. The Fe3O4NPs were synthesized using an aqueous-based approach and immobilized onto a glassy carbon electrode (GCE) surface. Comprehensive characterization using Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, energy dispersive X-ray, cyclic voltammetry (CV), and electrochemical impedance spectroscopy have confirmed the successful formation of well-crystallized Fe3O4NPs with an average crystallinity size of 61.62 nm. Electrochemical studies demonstrated strong electrostatic interactions between GCE/Fe3O4NPs and [Ru(NH3)6]3+. The electrochemical behavior of both pesticides were established by CV, while sensing parameters were optimized through differential pulse voltammetry. Under optimal conditions, the sensor achieved detection limits of 0.398 and 0.480 μM for DR and TBZ, respectively, with good selectivity and reproducibility. The practical utility of the sensor was successfully demonstrated through analysis of real water samples, offering a cost-effective solution for environmental monitoring applications. KW - Nanoparticles KW - Electrochemical sensors KW - Environmental analysis KW - Quality assurance PY - 2025 DO - https://doi.org/10.1002/elan.70022 SN - 1521-4109 VL - 37 IS - 7 SP - 1 EP - 11 PB - Wiley VHC-Verlag AN - OPUS4-63942 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Serrano-Munoz, Itziar A1 - Laquai, René A1 - Bruno, Giovanni T1 - Anwendungen der Röntgenrefraktionstechnik zur zerstörungsfreien Charakterisierung von Keramiken und Verbundwerkstoffen N2 - Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenk-ung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede: a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1); Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für: a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung. Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie: a) Sintern von SiC-Grünkörpern b) Porositätsanalyse in Dieselpartikelfiltersilikaten c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen d) Mikrorissbildung in Glaskeramik. Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Röntgen-Refraktion KW - Verbundwerkstoffe KW - Keramik PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576171 UR - https://jahrestagung.dgzfp.de/Portals/jt2023/BB180/Inhalt/p9.pdf UR - https://jahrestagung.dgzfp.de/Portals/jt2023/BB180/Inhalt/default.htm SN - 978-3-947971-29-9 SP - 1 EP - 16 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-57617 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fritsch, Tobias A1 - Farahbod-Sternahl, L. A1 - Serrano-Munoz, Itziar A1 - Léonard, F. A1 - Haberland, C. A1 - Bruno, Giovanni T1 - 3D Computed Tomography Quantifies the Dependence of Bulk Porosity, Surface Roughness, and Re-Entrant Features on Build Angle in Additively Manufactured IN625 Lattice Struts N2 - Layer-by-layer additive manufacturing (AM) by means of laser-powder bed Fusion (L-PBF) offers many prospects regarding the design of lattice structures used, for example, in gas turbines. However, defects such as bulk porosity, Surface roughness, and re-entrant features are exacerbated in nonvertical structures, such as tilted struts. The characterization and quantification of these kinds of defects are essential for the correct estimation of fracture and fatigue properties. Herein, cylindrical struts fabricated by L-PBF are investigated by means of X-ray computed tomography (XCT), with the aim of casting light on the dependence of the three kinds of defects (bulk porosity, surface roughness, and re-entrant features) on the build angle. Innovative analysis methods are proposed to correlate shape and position of pores, to determine the angular-resolved Surface roughness, and to quantify the amount of re-entrant surface features, q. A meshing of the XCT surface enables the correlation of q with the classical Surface roughness Pa. This analysis leads to the conclusion that there is a linear correlation between q and Pa. However, it is conjectured that there must be a threshold of surface roughness, below which no re-entrant features can be build. KW - Additive manufacturing KW - Laser powder bed fusion KW - Computed tomography KW - Surface roughness analysis KW - Re-entrant surface feature PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534728 DO - https://doi.org/10.1002/adem.202100689 IS - 2100689 SP - 1 EP - 8 PB - Wiley-VCH Verlag AN - OPUS4-53472 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Döring, Sarah T1 - Sequence of Mus Musculus monoclonal IgG2c anti-CCMV Immunoglobulin N2 - We report the full-length nucleotide and amino acid sequences of the light (κ) and heavy chain of the IgG2c anti-CCMV monoclonal antibody (hybridoma clone BAM-CCMV-29-81), generated against Cowpea Chlorotic Mottle Virus (CCMV). Sequencing of hybridoma clone was performed using a cost-effective Sanger-based workflow that includes DNA-level subclass determination and peptide mass fingerprint confirmation. The κ-chain sequence was assigned to IGKV4-6101 / IGKJ101, while the heavy chain was assigned to IGHV2-601 / IGHD1-101 / IGHJ3*01 with IgG2c constant regions from the NOD strain. Both chains were validated against RNA Illumina sequencing, confirming 100% identity. The sequences are available in GenBank under accession numbers PX123807 (κ-chain) and PX123808 (heavy chain). KW - Antibody Sequencing KW - BAM-CCMV-29-81 KW - anti-CCMV-antibody PY - 2025 UR - https://www.ncbi.nlm.nih.gov/nuccore/PX123807 UR - https://www.ncbi.nlm.nih.gov/nuccore/PX123808 PB - National Library of Medicine CY - Bethesda AN - OPUS4-63968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guilherme Buzanich, Ana T1 - Bridging Structure and Electronic State: Real-time XES–XRD Fusion for Functional Alloys N2 - We present a unified X-ray Emission Spectroscopy (XES) and X-ray Diffraction (XRD) approach for real-time, in situ characterization of materials, demonstrated on Co₂FeSi Heusler alloys under varied heat treatments. The combination of XES and XRD is particularly well-suited to Heusler alloys, where subtle changes in atomic ordering and electronic structure (e.g. site occupancy, hybridization, and spin state) are tightly interdependent and critical for their magnetic and transport properties. In addition, this method enables more efficient materials design by reducing experimental iterations through comprehensive structural and electronic analysis. Developed at the mySpot beamline at BESSY-II, the platform integrates (a) digital twin-based experiment planning, (b) open-source XES spectral simulations, (c) an optimized single-shot, two-element XES setup with sub-pixel resolution for enhanced energy precision, and (d) result-driven beamtime utilization. With an unprecedented synchronized XES-XRD platform, we aim to shed light on how diffusion-controlled processes in Heusler alloys and double perovskites at elevated temperatures establish the formation of specific phases with distinct structure types in real time. This, in turn, strongly impacts the functional properties of the materials under scrutiny. T2 - XLIV Colloquium Spectroscopicum Internationale CY - Ulm, Germany DA - 27.07.2025 KW - Multimodal KW - X-ray spectroscopy KW - X-ray diffraction KW - Functional alloys PY - 2025 AN - OPUS4-63991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, Hans R. A1 - Weidner, Steffen. M. T1 - Zwitterionic polymerization of glycolide catalyzed by pyridine N2 - The usefulness of various N- and P-based catalysts for syntheses of cyclic polyglycolide via zwitterionic polymerization of glycolide was examined. Most catalysts produced discolored, largely insoluble polyglycolides consisting of cycles and unidentified byproducts. Soluble, cyclic polyglycolides were obtained using neat pyridine as catalyst at 120 °C, 100 °C, 80 °C, and even at 60 °C. The number-average molecular weights were extremely low and depended slightly on the glycolide-to-pyridine ratio. Three different mass distributions of the cycles were detected by mass spectrometry, depending on the reaction conditions. The cyclic polyglycolides were also characterized by differential scanning calorimetry (DSC) and small-angle X-ray scattering (SAXS) measurements. The SAXS data in combination with the mass spectra indicate that the majority of the cycles form extended-ring crystallites KW - MALDI-TOF MS KW - Polylactide KW - Polymerization KW - Zitterions PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639748 DO - https://doi.org/10.1039/d5py00762c SN - 1759-9954 SP - 1 EP - 9 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63974 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Online NMR spectroscopy for process analytical applications and aspects on automation and digitization of process industry N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts while being based on “chemical” information. As an example, a fully automated NMR sensor is introduced, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. Therefore, a commercially available benchtop NMR spectrometer was adapted to the full requirements of an automated chemical production environment such as, e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. A full integration and intelligent interconnection of such systems and processes progresses only hesitantly. The talk should encourage to re-think digitization of process industry based on smart sensors, actuators, and communication more comprehensively and informs about current technical perspectives such as the “one-network paradigm”, edge computing, or virtual machines. These give smart sensors, actuators, and communication a new perspective. T2 - Advances in Process Analytics and Control Technology 2019 Conference (APACT) CY - Chester, United Kingdom DA - 30.04.2019 KW - Process Analytical Technology KW - Reaction Monitoring KW - Online NMR Spectroscopy KW - Process Industry KW - Distributed Networks KW - Digital Twin PY - 2019 AN - OPUS4-47907 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Jacobasch, Stefan A1 - Duffner, Eric A1 - Goedecke, Thomas A1 - Portella, Pedro Dolabella A1 - Mair, Georg W. A1 - Schendler, Thomas A1 - Gradt, Thomas A1 - Askar, Enis A1 - Bartholmai, Matthias A1 - Schröder, Volkmar A1 - Maiwald, Michael A1 - Holtappels, Kai A1 - Tschirschwitz, Rico A1 - Neumann, Patrick P. T1 - Unser Beitrag zum Thema Wasserstoff N2 - Die BAM ist nahezu über die gesamte Wertschöpfungskette hinweg wissenschaftlich tätig. Von der sicheren und effizienten Wasserstofferzeugung (POWER-to-GAS), über die (Zwischen-)Speicherung von Wasserstoff in Druckgasspeichern bis hin zum Transport bspw. mittels Trailerfahrzeug zum Endverbraucher. Komplettiert werden die Aktivitäten der BAM durch die sicherheitstechnische Beurteilung von wasserstoffhaltigen Gasgemischen, die Verträglichkeitsbewertung von Werkstoffen bis hin zur Detektion von Wasserstoffkonzentrationen über geeignete Sensorik, auch mittels ferngesteuerter Messdrohnen (sog. UAV-Drohnen). Zudem untersucht die BAM proaktiv Schadensrisiken und Unfallszenarien für die Sicherheitsbetrachtung, um mögliche Schwachstellen aufzeigen und potenzielle Gefährdungen erkennen zu können. KW - Wasserstoff KW - Wasserstofferzeugung KW - Energiespeicherung KW - Gasdetektion KW - Risikoanalyse KW - Power-to-Gas KW - Explosionsschutz KW - Tribologie KW - Druckgasspeicher KW - Glasspeicher KW - Gassensorik KW - Mini-UAV PY - 2019 SP - 1 CY - Berlin AN - OPUS4-47960 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Schnelle Identifizierung von Mineralwolle mittels Nah-Infrarot-Spektroskopie N2 - Künstliche Mineralfasern (KMF) werden weltweit in vielfältiger Weise als Dämmstoffe verwendet. Jährlich fallen in Deutschland ungefähr 20 Millionen Tonnen KMF an, die nach dem Abriss auf Deponien entsorgt werden müssen. Grundsätzlich besteht jedoch die Möglichkeit der Rückführung dieser Materialien in den Produktionsprozess. Dafür ist es notwendig, anfallende KMF sowohl nach Material (Glaswolle, Steinwolle) als auch nach Alter zu sortieren. Auf der Suche nach einer Methode, die es grundsätzlich gestattet eine schnelle Untersuchung vor Ort auf einer Baustelle durchzuführen, wurde die Nah-Infrarot (NIR) Spektroskopie unter Verwendung eines Prozessspektrometers mit Reflexionssonde getestet. Anhand von Laboruntersuchungen an 70 KMF Proben, die entweder betriebsneu waren oder bundesweit auf Baustellen gesammelt wurden, konnte eine NIR-basierte Methode zur Unterscheidung in Glas- und Steinwolle entwickelt werden. Mittels Partial Least Square Diskriminanzanalyse (PLS-DA) der NIR Spektren wurde basierend auf 40 zufällig ausgewählten Proben ein chemometrisches Modell kalibriert, das erfolgreich zur Klassifizierung der verbleibenden 30 Proben eingesetzt werden konnte. Unabhängig von Farbe, Dichte oder Alter der untersuchten KMF Proben war es möglich, eine 100% korrekte Zuordnung des Materials zu erzielen. Die nötigen Referenzwerte wurden unter Nutzung eines Röntgenfluoreszenzspektroskopischen Verfahrens über den Elementgehalt nach VDI 3492 ermittelt. Insgesamt ist der experimentelle Aufwand für die Durchführung und Auswertung der NIR Messungen gering und manifestiert sich vor allem in der Kalibrierphase, die in diesem Fall die Untersuchung von 8-fach aliquotierten Probestücken der 70 KMF umfasste. Nur bei deutlich feuchtem Material muss ein zusätzlicher Trocknungs-schritt berücksichtigt werden. Das vorgestellte Verfahren wurde nachfolgend zu einem Patent angemeldet. Untersuchungen zu einer weiteren Unterscheidung der KMF nach Alter sind geplant. T2 - 16. Kolloquium Prozessanalytik der GDCh & Dechema CY - Online meeting DA - 23.11.2020 KW - Mineralwolle KW - NIR KW - Chemometrie PY - 2020 AN - OPUS4-51731 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Certified reference material for the determination of hydrolytic resistance of borosilicate glass N2 - The preparation of certified reference material for the determination of hydrolytic resistance of borosilicate glass is described. Certified properties are the acid consumption according to the relevant standard procedures described in ISO 720, USP<660> and Ph.Eur. 3.2.1. T2 - PharmaGlass Workshop CY - Sheffield, UK DA - 09.10.2019 KW - CRM KW - Hydrolytic resistance KW - Borosilicate glass PY - 2019 AN - OPUS4-49466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Industrielle Anwendungen der Niederfeld-NMR-Spektroskopie für die Prozess- und Qualitätskontrolle von Silanen N2 - Aus der Kombination verschiedener Silane als Ausgangsstoffe und als Produkt der Hydrolyse durch eine Reihe von Alkoholen oder Wasser ergibt sich eine Palette von hunderten technischen Produkten für verschiedenste Anwendungen. Funktionelle Trialkoxysilane haben sich in den vergangenen Jahren als vielseitig einsetzbare Organosilane erwiesen. Die Einsatzgebiete erstrecken sich vom Witterungsschutz von Bauwerken über haftvermittelnde Eigenschaften in der Glasfaserindustrie, bei Dicht- und Klebstoffen, in Farben und Lacken bis hin zur Modifizierung von polymeren Werkstoffen. Kommerzielle Benchtop-NMR-Spektrometer haben das Potential auch im Bereich der Silanchemie als Online-Methode zur Reaktionsüberwachung und für die Qualitätskontrolle eingesetzt zu werden. Interessante NMR-Kerne für die oben genanntem Produkte sind 1H und 29Si. In einer gemeinsamen Forschungs-kooperation zwischen EVONIK und BAM wurde anhand verschiedener Fallstudien die Anwendbarkeit der Niederfeld-NMR-Spektroskopie zur chemischen Analyse von Silanen evaluiert. Die Möglichkeiten der Konzentrationsbestimmung erweitern die Anwendungsgebiete, in denen bestehende Technologien wie z. B. NIR, Raman, UV/VIS, etc. mangels Referenzdaten nicht quantitativ eingesetzt werden können. Eine Fallstudie setzte dazu an, den Hydrolyse- und Kondensationsverlauf mit geeigneter Online-NMR-Analytik zu beobachten, den Reaktionsfortschritt der Hydrolyse und Kondensation auf dieser Basis besser zu verstehen und zu optimieren. Zu diesem Zweck werden durch Zugabe von Wasser zunächst die Alkoxysubstituenten eines Trialkoxysilans hydrolysiert und entsprechende Silanole gebildet. Diese können dann über eine SiOH-Funktion an den zu modifizierenden Werkstoff anbinden und über weitere Silanolgruppen unter Ausbildung von Siloxaneinheiten vernetzen. In einer weiteren Fallstudie wurde die Kinetik der Aufspaltungen einer cyclischen Silanverbindung untersucht. Die Online-NMR-Analytik kam hierbei sowohl im Labor als auch in der industriellen Produktionsanlage zum Einsatz. Hierfür wurde eine automatisierte Einhausung verwendet, welche den Einsatz eines kommerziellen NMR-Spektrometers in explosionsgeschützten Bereichen ermöglicht. T2 - 10. ProcessNet-Jahrestagung CY - Online meeting DA - 21.09.2020 KW - NMR-Spektroskopie KW - Benchtop-NMR KW - Silane PY - 2020 AN - OPUS4-51350 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Industrial applications of low-field NMR spectroscopy for process and quality control of silanes N2 - The combination of different silanes as starting materials and as a product of hydrolysis by several alcohols or water creates a range of hundreds of technical products for a wide range of applications. In recent years, functional trialkoxysilanes have proven to be multi-purpose organosilanes. Applications range from weather protection of buildings to additives for glass fiber industry, sealants, adhesives, coatings and paints to the modification of polymers. Commercial benchtop NMR spectrometers have the potential to be used in silane chemistry as an online method for reaction monitoring and quality control. NMR nuclei of interest for silane products are 1H and 29Si. In a joint research cooperation between EVONIK and BAM, the applicability of low-field NMR spectroscopy for the chemical analysis of silanes was evaluated. It was shown how it can extend the application range where existing technologies like NIR, Raman, UV/VIS, etc. cannot be used quantitatively due to a lack of reference data. In a first case study the process of hydrolysis and condensation was observed using online NMR analysis. For this purpose, the substituents of a trialkoxysilane are first hydrolyzed by adding water and corresponding silanols are formed, which can then bind to materials via SiOH functions and crosslink to form siloxane units. Another case study was dealing with the kinetics of the cleavage of a cyclic silane compound. Online NMR analysis was used both in the laboratory and in the manufacturing plant. For this purpose, a fully automated containment system was used, which enables the use of a commercial NMR spectrometer in ATEX-environments. In the third case study presented, quantitative 1H-NMR spectra were acquired on product mixtures of a trialkoxysilane and other components such as organic stabilizers, organotin compounds, an aromatic amine and organic peroxides. An automatic evaluation method based on Indirect Hard Modeling (IHM) was developed. T2 - Practical Applications of NMR in Industry Conference (PANIC) CY - Online meeting DA - 19.10.2020 KW - Process Analytical Technology KW - NMR spectroscopy KW - Benchtop-NMR KW - Process-NMR PY - 2020 AN - OPUS4-51465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Martos, G. A1 - Josephs, R. A1 - Choteau, T. A1 - Wielgosz, R. A1 - Davies, S. A1 - Moawad, M. A1 - Tarrant, G. A1 - Chan, B. A1 - Alamgir, M. A1 - de Rego, E. A1 - Wollinger, W. A1 - Garrido, B. A1 - Fernandes, J. A1 - de Sena, R. A1 - Oliveira, R. A1 - Melanson, J. A1 - Bates, J. A1 - Mai Le, P. A1 - Meija, J. A1 - Quan, C. A1 - Huang, T. A1 - Zhang, W. A1 - Ma, R. A1 - Zhang, S. A1 - Hao, Y. A1 - He, Y. A1 - Song, S. A1 - Wang, H. A1 - Su, F. A1 - Zhang, T. A1 - Li, H. A1 - Lam, W. A1 - Wong, W. A1 - Fung, W. A1 - Philipp, Rosemarie A1 - Dorgerloh, Ute A1 - Meyer, Klas A1 - Piechotta, Christian A1 - Riedel, Juliane A1 - Westphalen, Tanja A1 - Giannikopoulou, P. A1 - Alexopoulos, Ch. A1 - Kakoulides, E. A1 - Kitamaki, Y. A1 - Yamazaki, T. A1 - Shimizu, Y. A1 - Kuroe, M. A1 - Numata, M. A1 - Pérez-Castorena, A. A1 - Balderas-Escamilla, M. A1 - Garcia-Escalante, J. A1 - Krylov, A. A1 - Mikheeva, A. A1 - Beliakov, M. A1 - Palagina, M. A1 - Tkachenko, I. A1 - Spirin, S. A1 - Smirnov, V. A1 - Tang Lin, T. A1 - Pui Sze, C. A1 - Juan, W. A1 - Lingkai, W. A1 - Ting, L. A1 - Quinde, L. A1 - Yizhao, C. A1 - Lay Peng, S. A1 - Fernandes-Whaley, M. A1 - Prevoo-Franzsen, D. A1 - Quinn, L. A1 - Nhlapo, N. A1 - Mkhize, D. A1 - Marajh, D. A1 - Chamane, S. A1 - Ahn, S. A1 - Choi, K. A1 - Lee, S. A1 - Han, J. A1 - Baek, S. A1 - Kim, B. A1 - Marbumrung, S. A1 - Jongmesuk, P. A1 - Shearman, K. A1 - Boonyakong, C. A1 - Bilsel, M. A1 - Gündüz, S. A1 - Ün, I. A1 - Yilmaz, H. A1 - Bilsel, G. A1 - Gökçen, T. A1 - Clarkson, C. A1 - Warren, J. A1 - Achtar, E. T1 - Mass fraction assignment of Bisphenol-A high purity material N2 - The CCQM-K148.a comparison was coordinated by the BIPM on behalf of the CCQM Organic Analysis Working Group for NMIs and DIs which provide measurement services in organic analysis under the CIPM MRA. It was undertaken as a "Track A" comparison within the OAWG strategic plan. CCQM-K148.a demonstrates capabilities for assigning the mass fraction content of a solid organic compound having moderate molecular complexity, where the compound has a molar mass in the range (75 - 500) g/mol and is non-polar (pKow < −2), when present as the primary organic component in a neat organic solid and where the mass fraction content of the primary component in the material is in excess of 950 mg/g. Participants were required to report the mass fraction of Bisphenol A present in one supplied unit of the comparison material. Participants using a mass balance method for the assignment were also required to report their assignments of the impurity components present in the material. Methods used by the seventeen participating NMIs or DIs were predominantly based on either stand-alone mass balance (summation of impurities) or qNMR approaches, or the combination of data obtained using both methods. The results obtained using thermal methods based on freezing-point depression methods were also reported by a limited number of participants. There was excellent agreement between assignments obtained using all three approaches to assign the BPA content. The assignment of the values for the mass fraction content of BPA consistent with the KCRV was achieved by most of the comparison participants with an associated relative standard uncertainty in the assigned value in the range (0.1 - 0.5)%. KW - Bisphenol-A KW - Purity assessment KW - Interlaboratory key comparison KW - Metrology PY - 2021 DO - https://doi.org/10.1088/0026-1394/58/1A/08015 VL - 58 IS - 1A SP - 08015 PB - IOP Publishing AN - OPUS4-54188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Metrology for Advanced Hydrogen Storage Solutions (MefHySto) – Overviewand Tangible Results N2 - The European project MefHySto addresses the need of large-scale energy storage, which is required for a shift to renewable energy supply. The project is funded by the European Metrology Programme on Innovation and Research (EMPIR) and consists of 14 consortium partners from all over Europe (www.mefhysto.eu). It is demonstrated, how MefHySto is contributing to the EMN for Energy Gases aiming at prioritisation of the measurement gaps and challenges interacting with the EMN stakeholders. T2 - European Metrology Network Energy Gases “Measurement Solutions for Energy Gases” Workshop CY - Lisbon, Portugal DA - 21.03.2023 KW - MefHySto KW - EMPIR KW - Hydrogen Storage KW - Hydrogen Metrology KW - Hydrogen Purity KW - Geological Storage PY - 2023 AN - OPUS4-57193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online-NMR Spektroskopie in der PAT - Entwicklungen zwischen Labor- und Feldeinsatz N2 - Die NMR-Spektroskopie ist eine der zentralen nicht-invasiven Analysenmethoden in der organischen Chemie und aus dem Laboralltag nicht mehr wegzudenken. Die direkte Proportionalität zwischen der Anzahl der Atomkerne im Messvolumen und der Signalfläche im Spektrum ist vergleichbar mit einem „Zählen der Kernspins“. Der Kalibrieraufwand für die Quantifizierung ist minimal und aus dem NMR-Spektrum sind Informationen zu Struktur und Identität zugänglich. Online-NMR-Spektroskopie wird unter Zuhilfenahme von speziellen Durchflussproben-köpfen und Messzellen bereits seit Jahrzehnten erforscht und eingesetzt. Durch die hohen Anforderungen an die Aufstellung und den Betrieb von klassischen Hochfeld-NMR-Spektrometern konnte sie allerdings nie den Sprung vom Labor in den Prozess schaffen. Dies hat sich durch die Entwicklungen im Bereich mobil einsetzbarer Benchtop-NMR-Spektrometer grundlegend verändert. Geringere Investitions- und Betriebskosten, sowie die Robustheit und einfache Bedienbarkeit dieser Systeme sind entscheidende Faktoren. Damit rückt eine Anwendung als Online-PAT-Methode technisch in greifbare Nähe. Designierte Prozess-NMR-Spektrometer sucht man heutzutage allerdings auf dem Markt meist noch vergebens. Die Reaktionsverfolgung im Labormaßstab konnte an unterschiedlichen Systemen erfolgreich demonstriert werden. Dabei zeigten sich allerdings Limitierungen in Hinblick auf einen möglichen Prozesseinsatz. Insbesondere die Temperaturempfindlichkeit der Magnetsysteme ist hier zu nennen. Anhand eines Prototyps wurde eine aktive Temperaturisolation mittels temperierter Luftströmungen entwickelt und erprobt. Eine Feldintegration von Laborsystemen geht sowohl technisch als auch regulatorisch mit zahlreichen Herausforderungen einher. Das raue Umfeld von Produktionsanlagen, sowie die Anforderungen an Explosionsschutz erfordern eine zugelassene Einhausung. Auf Basis von Erfahrungen mit einem ersten Prototyp erfolgte die gemeinsame Entwicklung eines möglichst flexibel einsetzbaren Analysenschranks. Neben der Hardware-Integration sind die automatisierte modellbasierte Auswertung der NMR-Spektren, sowie die Einbindung in die Prozessleittechnik essenziell für einen zuverlässigen Betrieb als PAT-Analysengerät. T2 - 18. Kolloquium AK Prozessanalytik CY - Krefeld, Germany DA - 27.11.2023 KW - Prozessanalytik KW - Online-NMR-Spektroskopie KW - NMR-Spektroskopie KW - Benchtop-NMR KW - Feldintegration PY - 2023 AN - OPUS4-58969 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - How does solid microanalysis profit from innovations in EUV research N2 - Research into new sources for EUV lithography is driving advancements in experimental methods tailored for this short wavelength range. This progress enables the exploration of spectroscopic techniques aimed at monitoring electronic transitions within this energy spectrum. Laser-induced breakdown spectroscopy (LIBS) serves as a rapid tool for elemental analysis, primarily established in the UV-vis range. However, LIBS encounters challenges such as limited repeatability precision and elevated background noise resulting from continuum radiation. In parallel, laser-induced extreme UV spectroscopy (LIXS) delves into the initial stages of plasma evolution, characterized by the emergence of soft X-ray and extreme UV radiation. The method benefits from a fast timeframe and constrained plasma confinement, leading to better precision. Nevertheless, LIXS encounters convoluted spectra arising from unresolved transition arrays (UTA), particularly pronounced for heavier elements. This complexity renders conventional univariate data analysis impractical, demanding the adoption of a multivariate data analysis approach. Multiple cathode samples, each coated with varying stoichiometries of lithium nickel manganese cobalt oxide (NMC), were prepared and used for calibration purposes. Through the application of Partial Least Squares (PLS) regression, a robust correlation with an R2 value exceeding 0.97 was achieved. The LIXS technique underwent a comparative evaluation against UV-vis LIBS. Furthermore, a comparison between univariate and multivariate analysis approaches was conducted, incorporating validation through y-randomization to mitigate overfitting risks. The viability of this approach was confirmed through the testing of an NMC reference material. The results showed metrological compatibility with reference values, underscoring the potential capability of the proposed methodology. T2 - 322. PTB Seminar 2023 - VUV and EUV Metrology CY - Berlin, Germany DA - 14.11.2023 KW - Laser induced XUV spectroscopy KW - Lithium-ion batteries KW - Solid microanalysis PY - 2023 UR - https://www.euv2023.ptb.de/ AN - OPUS4-58834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian A1 - Vogel, Kristin T1 - Berechnung und Nutzung von Unsicherheiten zertifizierter Werte von Referenzmaterialien N2 - Referenzmaterialien sind unter anderem ein wichtiges Werkzeug zur Qualitätskontrolle von Messungen bestimmter Merkmalswerte. Dabei ist zu berücksichtigen, dass zertifizierte Merkmalswerte immer eine gewisse Unsicherheit haben. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Vortrags. Referenzmaterialien sind gleichzeitig ein wertvolles Werkzeug zur Ermittlung der Unsicherheit von Messverfahren und -Analysen unbekannter Proben. Die Vorgehensweise bei der Ermittlung der Messunsicherheit mit Hilfe eines Referenzmaterials wird beschrieben. T2 - 11. VDI-Fachtagung Messunsicherheit und Prüfprozesse CY - Erfurt, Germany DA - 14.11.2023 KW - Referenzmaterial KW - Messunsicherheit KW - ISO Guide 35 PY - 2023 AN - OPUS4-58946 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Study of lithium-ion battery aging using laser-induced XUV spectroscopy (LIXS) N2 - Laser-induced XUV spectroscopy (LIXS) is an emerging technique for elemental mapping. In comparison to conventional laser-induced breakdown spectroscopy in UV-vis (LIBS), it has a higher precision and wider dynamic range, and it is well suited for the quantification light elements like lithium and fluorine. Further it can spot oxidation states. The XUV spectra are produced at a very early stage of the plasma formation. Therefore, effects from plasma evolution on the reproducibility can be neglected. It has been shown, that high-precision elemental quantification in precursor materials for lithium-ion batteries (LIBs) can be performed using LIXS. Based on these results, LIXS mapping was used to investigate aging processes in LIBs. Different cathode materials with varying compositions of fluorine containing polymer binders were compared at different stages of aging. Due to effects comparable to X-ray photoelectron spectroscopy but in reverse, monitoring of changes in the oxidation state is envisioned, which makes information about the chemical environment of the observed elements accessible. The combination of elemental distribution and structural information leads to a better understanding of aging processes in LIBs, and the development of more sustainable and safe batteries. T2 - Conference on Applied Surface and Solid Material Analysis - AOFKA 2023 CY - Zurich, Switzerland DA - 11.09.2023 KW - Lithium Ion Batteries KW - Laser-induced XUV spectroscopy KW - Multivariate data analysis PY - 2023 AN - OPUS4-58587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Benchtop-NMR-Spektroskopie – Praktische Probleme in Labor- und Prozessanwendungen N2 - In den letzten Jahren erfreut sich die Benchtop-NMR-Spektroskopie steigender Beliebtheit. Zusätzlich zu Anwendungen im Labor werden die kompakten Geräte auch zunehmend in industriellen Bereichen eingesetzt. Neben geringeren Investitions- und Betriebskosten sind insbesondere die Robustheit und einfache Bedienbarkeit dieser Systeme entscheidende Faktoren. Ein prozessnaher Einsatz kann sowohl nach Probenahme im Rahmen der Betriebsanalytik erfolgen als auch als Online-Analytik mit direkter Ankopplung an Prozesse. Insbesondere bei der direkten Kopplung mittels Durchflusszellen spielt der Probentransfer eine entscheidende Rolle. Dies zeigt sich auch am Beispiel eines Extraktionsprozesses im Labormaßstab. Das in einem Bioprozess aus tierischen Altfetten hergestellte Copolymer PHB(Co-HHX) wurde in einem Batch-Prozess mit organischen Lösungsmitteln aus gefrier-getrockneten Zellen extrahiert. Unter Variation der Parameter wurde der Prozess direkt in der mehrphasigen Suspension mittels Benchtop-NMR-Spektroskopie verfolgt. Eine große Limitierung für den Einsatz als Online-Methode ist die Temperaturempfindlichkeit der Magnetsysteme. Während die Umgebungstemperatur gut kontrollierbar ist, stellt sich die Thematik der Probentemperatur komplexer dar. Bei größeren Abweichungen von der Magnettemperatur kommt es bereits nach kurzer Zeit zu Drift-Effekten, die die Lock-Systeme nur begrenzt kompensieren können. Ein Ansatz ist die Nutzung temperierter Luftströme, ähnlich bekannter VT-Einheiten ergänzt um eine aktive Isolierung zum Magneten. An einem Modellaufbau wurden dazu verschiedene Konstruktionen zunächst mittels Thermographie charakterisiert und anschließend die Anwendbarkeit in einem Prototyp-Gerät überprüft. In der rauen industriellen Umgebung von Produktionsanlagen sind weitere Maßnahmen zum Betrieb eines Laborgerätes nötig (z.B. Temperierung, Witterungsschutz). Zusätzlich bestehen häufig strikte Anforderungen an den Explosionsschutz. Zu diesem Zweck wurde gemeinsam mit der Evonik Rheinfelden eine Einhausung entwickelt, die es ermöglicht neben der NMR-Spektroskopie auch eine weitere analytische Methode möglichst flexibel direkt an großtechnische Anlagen anzubinden. T2 - 44. Tagung Praktische Probleme der Kernresonanzspektroskopie 2023 CY - Berlin, Germany DA - 21.03.2023 KW - Benchtop-NMR KW - Prozessanalytik KW - Extraktion PY - 2023 AN - OPUS4-57202 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Multivariate data analysis for laser-induced XUV spectroscopy (LIXS) N2 - The application of multivariate data analysis is essential in extracting the full potential of laser-induced XUV spectroscopy (LIXS) for high-precision elemental mapping. LIXS offers significant advantages over traditional laser-induced breakdown spectroscopy in UV-vis (LIBS), including higher precision and a wider dynamic range,[1,2] while making it possible to determine light elements like lithium and fluorine. However, it is challenged by the presence of unresolved transition arrays (UTAs) for heavier elements. These UTAs add considerable complexity to the spectral data, often concealing crucial information. In this study, we employ well-established multivariate data analysis techniques and intensive data preprocessing to unravel this contained information. The refined analysis reveals a high level of detail, enabling the precise identification of inhomogeneities within material samples. Our approach has particular relevance for studying aging processes in lithium-ion batteries (LIBs), specifically in relation to varying cathode materials and fluorine-containing polymer binder content. By combining elemental distribution with structural information, this improved method can offer a more comprehensive understanding of sample inhomogeneities and aging processes in LIBs, contributing to the development of more reliable and sustainable battery technologies. T2 - Berliner Chemie in Praxis Symposium - BCPS 2023 CY - Berlin, Germany DA - 06.10.2023 KW - Lithium Ion Batteries KW - Laser-induced XUV spectroscopy KW - Multivariate data analysis PY - 2023 AN - OPUS4-58588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Meyer, Klas T1 - NMR Spectroscopy for Online Monitoring and Process Control N2 - The departure from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. The talk introduces a smart online NMR sensor module provided in an explosion proof housing as example. This sensor was developed for an intensified industrial process (pharmaceutical lithiation reaction step) funded by the EU’s Horizon 2020 research and innovation programme (www.consens-spire.eu). Due to NMR spectroscopy as an “absolute analytical comparison method”, independent of the matrix, it runs with extremely short set-up times in combination with “modular” spectral models. Such models can simply be built upon pure component NMR spectra within a few hours (i.e., assignment of the NMR signals to the components) instead of tedious calibrations runs. The talk also generally covers current aspects of high-field and low-field online NMR spectroscopy for reaction monitoring and process control. T2 - Lonza Shared Best Practice Seminar CY - Visp, Switzerland DA - 26.02.2019 KW - Process Analytical Technology KW - Reaction Monitoring KW - Online NMR Spectroscopy KW - Compact NMR Spectroscopy KW - Quantitative NMR Spectroscopy PY - 2019 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-47453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - ISO-Guide 35 in der Praxis eines RM-Herstellers N2 - Der ISO-Guide 35 beschreibt die notwendigen Schritte zur Herstellung von zertifizierten Referenzmaterialien. Anhand praktischer Beispiele wird die Umsetzung des Guide 35 in der BAM dokumentiert. T2 - DAkkS-Informationsveranstaltung - Akkreditierung von Referenzmaterialherstellern; Fachbereich Ringversuche / Referenzmaterialien CY - Berlin, Germany DA - 14.02.2019 KW - ZRM KW - ISO-Guide 35 KW - Referenzmaterial-Herstellung PY - 2019 AN - OPUS4-47395 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Modular process control with compact NMR spectroscopy – From Field Integration to Automated Data Analysis N2 - Chemical and pharmaceutical companies have to find new paths to survive successfully in a changing environment, while also finding more flexible ways of product and process development to bring their products to market more quickly – especially high-quality high-end products like fine chemicals or pharmaceuticals. A current approach uses flexible and modular chemical production units, which can produce different high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce the time to market of new products. NMR spectroscopy appeared as excellent online analytical tool and allowed a modular data analysis approach, which even served as reliable reference method for further Process Analytical Technology (PAT) applications. Using the available datasets, a second data analysis approach based on artificial neural networks (ANN) was evaluated. Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously. In future, such fully integrated and interconnecting “smart” systems and processes can increase the efficiency of the production of specialty chemicals and pharmaceuticals. At the end of the article, ideas for solutions are discussed in order to speed up the implementation of new special products from the point of view of process analytics and to network the existing process chains more closely. T2 - PATriCK 2022 – Merck conference on PAT technology CY - Darmstadt, Germany DA - 19.10.2022 KW - Process Analytical Technology KW - Digitalisation KW - Process Industry KW - Online NMR Spectroscopy KW - Modular Production PY - 2022 AN - OPUS4-56089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Integrierte und vernetzte Systeme und Prozesse – Eine Perspektive für die smarte Laborinfrastruktur N2 - Chemie- und Pharmaunternehmen müssen neue Wege gehen, um in einem sich wandelnden Umfeld erfolgreich zu überleben, und gleichzeitig flexiblere Wege der Produkt- und Prozessentwicklung finden, um ihre Produkte schneller auf den Markt zu bringen - vor allem hochwertige High-End-Produkte wie Feinchemikalien oder Arzneimittel. Dazu gehört auch das Potenzial der digitalen Technologien, um ein umfassenderes Wissensmanagement zu ermöglichen. Eine wichtige Wissensquelle sind analytische Labors, die Unternehmensweit aktiv sind – von F&E bis zur Produktion. Die ganzheitliche Einbindung von analytischen Labors und ein unternehmensweites Daten- und Wissensmanagement sind wichtige Bausteine zur Integration und Vernetzung aller Systeme und Prozesse. Das Potenzial von Daten aus der Produktion mit ihren Kontextinformationen wird heute oft noch nicht konsequent für ein umfassendes Verständnis der Produktion genutzt. Dieser Beitrag skizziert anhand von Beispielen einen möglichen ganzheitlicheren Ansatz zur Digitalisierung und zum Einsatz maschineller Verfahren in der Produktion von Spezialchemikalien und Pharmazeutika durch die Einführung integrierter und vernetzter Systeme und Prozesse. T2 - 6. Analytik-Tag des Institut für Energie- und Umwelttechnik e.V. (IUTA) CY - Duisburg, Germany DA - 10.11.2022 KW - Prozessindustrie KW - Online-NMR-Spektroskopie KW - Prozessanalytik KW - Digitalisierung KW - Datenauswertung KW - IUTA PY - 2022 AN - OPUS4-56226 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Integrierte und vernetzte Systeme und Prozesse – Prozessnahe Sensorik für die digital transformierte Prozessindustrie N2 - Unternehmen der Prozessindustrie müssen neue Wege finden, um in einem sich wandelnden Umfeld erfolgreich zu überleben, und gleichzeitig flexiblere Wege der Produkt- und Prozessentwicklung finden, um ihre Produkte schneller auf den Markt zu bringen – insbesondere hochwertige, hochwertige Produkte wie Feinchemikalien oder Arzneimittel. Dies wird zukünftig durch Veränderungen in den Wertschöpfungsketten entlang einer potenziellen Kreislaufwirtschaft erschwert. Anhand von Beispielen wird in diesem Vortrag ein möglicher ganzheitlicher Ansatz zur Digitalisierung und zum Einsatz maschineller Verfahren in der Produktion von Spezialchemikalien durch die Einführung integrierter und vernetzter Systeme und Prozesse skizziert. Es wird auch auf die aktuelle Technologie-Roadmap „Prozess-Sensoren 2027+“ eingegangen, die Ende 2021 erschienen ist. Im Zentrum dieser Roadmaps stehen Sensoren zur Erfassung von physikalischen und chemischen Messgrößen mittels spezifischer und unspezifischer Messverfahren, die zur Steuerung und dem besseren Verständnis von Prozessen dienen. Die Roadmap fasst die gemeinsame Technologie- und Marktsicht von Anwendern, Herstellern und Forschungs¬einrichtungen im Bereich Prozess-Sensorik in der verfahrenstechnischen Industrie zusammen. Digitalisierung und Nachhaltigkeit sind übergreifende Kernthemen der künftigen Entwicklung. T2 - 11. Fachtagung Prozessnahe Röntgenanalytik PRORA CY - Berlin, Germany DA - 24.11.2022 KW - Digital Transformatioin KW - Prozessindustrie KW - Sensorik KW - Prozessanalytik KW - Industrie 4.0 KW - PRORA PY - 2022 AN - OPUS4-56391 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Prozessindustrie Gemeinsam Digital – Forschungsbedarf für die Digitalisierung der Prozessindustrie N2 - Die Digitale Transformation durchdringt weite Teile der Industrie mit einer zunehmenden Vernetzung und Digitalisierung entlang der Wertschöpfungskette. Basierend auf dem Whitepaper der DECHEMA „Digitalisierung in der Chemieindustrie“ entsteht die Vision eines gläsernen Apparates mit einem zeitlich, räumlich und methodisch dichtem Monitoring der Betriebszustände, das eine daten- und modellbasierte Optimierung transienter oder instationärer Prozesse (das heißt An-/Abfahren, Laständerungen, etc.) erlaubt. Auch der nicht bestimmungsmäßige Betrieb von Apparaten oder Modulen wird zuverlässig erkannt. Basis ist hier die Implementierung von innovativer Messtechnik und neuartigen Sensoren in Kombination mit der Anwendung datengetriebener oder rigoroser Modelle zur Prozesssimulation und -kontrolle. Anlagen, die auf diesem Konzept basieren, lassen sich sicher an Stabilitäts- bzw. Kapazitätsgrenzen und mit höherem Durchsatz betreiben. Trotz schwankender Rohstoffqualitäten kann eine gleichbleibende Zielqualität der Produkte mit rentablen Qualitätssicherungskosten garantiert werden. Dazu ist eine Vernetzung über weitere Branchen (Softwareingenieure, MSR-Technik, Betreiber, Hersteller) notwendig. Sie ergänzt komplementär die ENPRO-Initiative mit Themen der modularen Anlagenplanung und -konstruktion und modular verteilter Intelligenz. Ein Digitalisierungsbedarf besteht auch für bereits vorhandenen Anlagenbestand bzw. zukünftig nicht modular gestalteter Produktionsapparate der chemischen Industrie, um auch dort einen wesentlichen Beitrag zur Ressourcen- und Energieeffizienz zu leisten. T2 - DECHEMA-Workshop "Impulse für die Forschungsförderung - Digitalisierung" CY - Frankfurt am Main, Germany DA - 14.02.2019 KW - Pozessindustrie KW - Digitalisierung KW - Industrie 4.0 KW - Digitale Transformation KW - Forschungsbedarf PY - 2019 AN - OPUS4-47385 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Determination of calcium, iron, and selenium in human serum by isotope dilution analysis using MICAP-MS N2 - Trace elemental analysis in human serum is integral in both clinical and research settings. Analyzing the level of some specific elements like Se and Zn helps indicate the nutritional and health status. Furthermore, elucidating the roles of trace elements in various physiological and pathological conditions can shed light on disease mechanisms and potential treatments. Inductively coupled plasma mass spectrometry (ICP-MS) stands out as a preeminent method for trace elemental analysis, given its exceptional sensitivity and minimal sample requirements. However, ICP-MS has challenges, such as argon-related interferences that hinder the accurate quantification of elements like Ca, Fe, and Se. The naturally most abundant isotopes of Ca (40Ca), Fe (56Fe), and Se (80Se) are subject to isobaric interference from 40Ar+, 40Ar16O+, and 40Ar2+, thereby complicating their direct measurement and preventing isotope dilution analysis. In response to these challenges, nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) emerges as a viable alternative to ICP-MS, eliminating argon consumption and associated interferences. This study employed MICAP-MS to quantify Ca, Fe, and Se in 11 certified reference human serums using matrix-matched calibration and isotope dilution with the isotopes 40Ca, 56Fe, and 80Se. The results obtained with both methods were validated against certified values, and the suitability of MICAP-MS for isotope dilution was evaluated. Additionally, the performance of MICAP-MS in the Na matrix was investigated and discussed alongside the impact of organic species. T2 - Winter Conference on Plasma Spectrochemistry 2024 CY - Tucson, AZ, USA DA - 15.01.2024 KW - MICAP-MS KW - Isotope-dilution KW - Human serum PY - 2024 AN - OPUS4-60210 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Erfahrungsaustausch Labor-Robotik N2 - Die BAM setzt in ihren analytischen Labors zunehmend Labor-Robotik ein, um gefähliche oder zeitraubende Routineaufgaben zu automatisieren. Durch Automation kann auch die Reproduzierbarkeit solcher Anwendungen erhöht werden. Im Beitrag werden einige aktuelle Beispiele aus den Analytiklabors diskutiert, wie z. B. die Anwendung für die Herstellung und RFA-Analytik von Gläsern, eine Feinwäge-Robotik für 10-L-Gaszylinder im Rahmen der Herstellung von Primärnormalen oder die Automatisierung von Probenpräsentationen für optische Spektroskopie und chemical Imaging. Auch wird kurz auf den Einsatz von Speicherprogrammierbaren Steuerungen in der modularen Laborautomation und die Virtualisierung von analytischen Laborrechnern eingengangen. T2 - Industrienetzwerk Smartes Labor am Institut für Energie- und Umwelttechnik e.V. (IUTA) CY - Duisburg, Germany DA - 09.11.2022 KW - Laborautomation KW - Labor-Robotik KW - Automatisierung KW - Smartes Labor PY - 2022 AN - OPUS4-56227 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Taking Chances – Cheese, Chocolate and Laser Spectroscopy N2 - Science Café Adlershof is having its next edition in 2024 on February 20th '24! We will have one speaker next week: Alexander Winckelmann is a PhD student at Bundesanstalt für Materialforschung und -Prüfung and will give a talk about his stay abroad in Switzerland - there will be free chocolates! There will be enough time to ask questions or simply chat with the guests and participants. T2 - Science Café Adlershof CY - Berlin, Germany DA - 20.02.2024 KW - Laser-induced XUV Spectroscopy KW - Multivariate Data Analysis KW - Science Communication PY - 2024 AN - OPUS4-60197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - QM Summer School – teaching living quality management to our young generation N2 - In 2018, BAM (Federal Institute for Materials Research and Testing) and the young analysts of the department Analytical Chemistry at the Gesellschaft Deutscher Chemiker (German Chemical Society, GDCh) jointly organized the second summer school on quality assurance in analytical chemistry in Berlin, Germany. Over fifty doctoral students that are still in the initial stages of work participated in the week-long event and the participants were confronted with the most important basic concepts of internal and external systems of quality assurance in analytical chemistry. Especially young scientists and scholars deal with the development of analysis methods and often generate an increasingly growing wealth of data. Results are mostly evaluated under quantitative aspects and need to be assessed subject-specifically. In addition to the purely scientific requirements these results also should meet the requirements of analytical quality assurance. For this purpose, the development of analytical methods is accompanied by a process of validation – the documented proof that a method is suitable for the intended purpose and the defined requirements. This talk summarizes the didactic concept, which was used by the organizers to span an arc from the handling of process characteristics, such as accuracy, precision, linearity, recovery, up to measurement uncertainty and modern multivariate analysis techniques. In an open space workshop, the participants discussed their idea of quality management and worked out requirements after common sense. Interestingly, many participants had already implemented important quality assurance without professionally knowing it. T2 - Euroanalysis XX 2019 CY - Istanbul, Turkey DA - 01.09.2019 KW - Quality Management KW - Summer School KW - GDCh KW - Joung Analysts KW - Chemometrics KW - Education PY - 2019 UR - http://euroanalysis2019.com/ AN - OPUS4-48834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian T1 - Certified reference material for the determination of hydrolytic resistance of borosilicate glass N2 - The preparation, analysis and certification of a new certified glass reference material (CRM) for the determination of hydrolytic resistance of borosilicate glass with the glass grains test is described. The CRM BAM-S053 is available in the form of glass rods (length: 185 mm, diameter: 9 mm, weight: 27·5 g). Certified properties are the acid consumption determined according to the procedures described in ISO 720, USP<660>, Ph.Eur. 3.2.1, data obtained following the procedure of ISO 719 was scattering too widely. The certified values are based on the results of 15 laboratories which participated in the certification interlaboratory comparison. The CRM is intended for the quality control when applying ISO 720, USP<660>, Ph.Eur. 3.2.1 and with limitations ISO 719. KW - CRM KW - Hydrolytic resistance KW - Borosilicate glass PY - 2021 DO - https://doi.org/10.13036/17533562.62.1.001 VL - 62 IS - 1 SP - 25 EP - 27 AN - OPUS4-52195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fricke, F. A1 - Meyer, Klas T1 - Artificial Intelligence for Mass Spectrometry and Nuclear Magnetic Resonance Spectroscopy N2 - Mass Spectrometry (MS) and Nuclear Magnetic Resonance Spectroscopy (NMR) are critical components of every industrial chemical process as they provide information on the concentrations of individual compounds and by-products. These processes are carried out manually and by a specialist, which takes a substantial amount of time and prevents their utilization for real-time closed-loop process control. This paper presents recent advances from two projects that use Artificial Neural Networks (ANNs) to address the challenges of automation and performance-efficient realizations of MS and NMR. In the first part, a complete toolchain has been developed to develop simulated spectra and train ANNs to identify compounds in MS. In the second part, a limited number of experimental NMR spectra have been augmented by simulated spectra to train an ANN with better prediction performance and speed than state-of-theart analysis. These results suggest that, in the context of the digital transformation of the process industry, we are now on the threshold of a possible strongly simplified use of MS and MRS and the accompanying data evaluation by machine-supported procedures, and can utilize both methods much wider for reaction and process monitoring or quality control. T2 - 2021 Design, Automation & Test in Europe Conference & Exhibition (DATE) CY - Online meeting DA - 01.02.2021 KW - Industry 4.0 KW - Cyber-Physical Systems KW - Artificial Neural Networks KW - Mass Spectrometry KW - Nuclear Magnetic Resonance Spectroscopy PY - 2021 UR - www.date-conference.com AN - OPUS4-52181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Industrielle Anwendungen der Niederfeld-NMR-Spektroskopie für die Qualitätskontrolle von Silanen N2 - Aus der Kombination verschiedener Silane als Ausgangsstoffe und als Produkt der Hydrolyse durch eine Reihe von Alkoholen oder Wasser ergibt sich eine Palette von hunderten technischen Produkten für verschiedenste Anwendungen. Funktionelle Trialkoxysilane haben sich in den vergangenen Jahren als vielseitig einsetzbare Organosilane erwiesen. Die Einsatzgebiete erstrecken sich vom Witterungsschutz von Bauwerken über haftvermittelnde Eigenschaften in der Glasfaserindustrie, bei Dicht- und Klebstoffen, in Farben und Lacken bis hin zur Modifizierung von polymeren Werkstoffen. Kommerzielle Benchtop-NMR-Spektrometer haben das Potential auch im Bereich der Silanchemie als Online-Methode zur Reaktionsüberwachung und für die Qualitätskontrolle eingesetzt zu werden. Interessante NMR-Kerne für die oben genanntem Produkte sind 1H und 29Si. In einer gemeinsamen Forschungskooperation zwischen EVONIK und BAM wurde anhand verschiedener Fallstudien die Anwendbarkeit der Niederfeld-NMR-Spektroskopie zur chemischen Analyse von Silanen evaluiert. Die Möglichkeiten der Konzentrationsbestimmung erweitern die Anwendungsgebiete, in denen bestehende Technologien wie z. B. NIR, Raman, UV/VIS, etc. mangels Referenzdaten nicht quantitativ eingesetzt werden können. Eine Fallstudie setzte dazu an, den Hydrolyse- und Kondensationsverlauf mit geeigneter Online-NMR-Analytik zu beobachten, den Reaktionsfortschritt der Hydrolyse und Kondensation auf dieser Basis besser zu verstehen und zu optimieren. Zu diesem Zweck werden durch Zugabe von Wasser zunächst die Alkoxysubstituenten eines Trialkoxysilans hydrolysiert und entsprechende Silanole gebildet. Diese können dann über eine SiOH-Funktion an den zu modifizierenden Werkstoff anbinden und über weitere Silanolgruppen unter Ausbildung von Siloxaneinheiten vernetzen. In einer weiteren Fallstudie wurde die Kinetik der Aufspaltungen einer cyclischen Silanverbindung untersucht. Die Online-NMR-Analytik kam hierbei sowohl im Labor als auch in der industriellen Produktionsanlage zum Einsatz. Hierfür wurde eine automatisierte Einhausung verwendet, welche den Einsatz eines kommerziellen NMR-Spektrometers in explosionsgeschützten Bereichen ermöglicht. T2 - Praktische Probleme der Kernresonanzspektroskopie CY - Online meeting DA - 16.03.2021 KW - NMR-Spektroskopie KW - Benchtop-NMR KW - Silane KW - Prozessanalytik PY - 2021 AN - OPUS4-52298 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Industrial Applications of benchtop NMR Spectroscopy for Quality Control of Silanes N2 - The combination of different silanes as starting materials and as a product of hydrolysis by several alcohols or water creates a range of hundreds of technical products for a wide range of applications. In recent years, functional trialkoxysilanes have proven to be multi-purpose organosilanes. Applications range from weather protection of buildings to additives for glass fiber industry, sealants, adhesives, coatings and paints to the modification of polymers. Commercial benchtop NMR spectrometers have the potential to be used in silane chemistry as an online method for reaction monitoring and quality control. NMR nuclei of interest for silane products are 1H and 29Si. In a joint research cooperation between EVONIK and BAM, the applicability of low-field NMR spectroscopy for the chemical analysis of silanes was evaluated. It was shown how it can extend the application range where existing technologies like NIR, Raman, UV/VIS, etc. cannot be used quantitatively due to a lack of reference data. In a first case study the process of hydrolysis and condensation was observed using online NMR analysis. For this purpose, the substituents of a trialkoxysilane are first hydrolyzed by adding water and corresponding silanols are formed, which can then bind to materials via SiOH functions and crosslink to form siloxane units. Another case study was dealing with the kinetics of the cleavage of a cyclic silane compound. Online NMR analysis was used both in the laboratory and in the manufacturing plant. For this purpose, a fully automated containment system was used, which enables the use of a commercial NMR spectrometer in ATEX-environments. In the third case study presented, quantitative 1H-NMR spectra were acquired on product mixtures of a trialkoxysilane and other components such as organic stabilizers, organotin compounds, an aromatic amine and organic peroxides. An automatic evaluation method based on Indirect Hard Modeling (IHM) was developed. T2 - Magritek's Spinsolve NMR Users Meeting 2021 CY - Online meeting DA - 20.04.2021 KW - NMR spectroscopy KW - Silanes KW - Process Analytical Technology KW - Quality Control PY - 2021 AN - OPUS4-52557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gojani, Ardian T1 - Application of spatial heterodyne spectroscopy for chemical analysis based on Raman and laser-induced breakdown spectroscopy N2 - Spatial Heterodyne Spectroscopy (SHS) is a spectrometric technique that combines both dispersive and interferometric features into a customizable instrument. The Basis of SHS is a Michelson interferometer with its mirrors replaced by diffraction gratings and with no moving parts. The output signal from SHS is the interferogram, which is recorded with a 1D or 2D pixel array detector. The spatial periodicity of the fringes on the interferogram is a function of the wavelength of the diffracted light. Using the Fast Fourier Transform, the original optical spectrum that enters SHS is retrieved. The light that is analyzed by SHS can come from a variety of sources. In our work, we used Raman scattering and Laser-Induced Plasma to perform quantitative and qualitative analyses. Figure 1 compares the performance of the SHS with that of high Resolution echelle and portable low-resolution asymmetrically crossed Czerny-Turner spectrometers (OO in Fig.1). The analyzed light came from the plasma induced on a stainless-steel reference material. The SHS exhibits the resolution comparable to that of the echelle spectrometer used, about 8000. Due to a high throughput of the SHS (theoretically, ~200 times higher than that of grating instruments), the number of spectra needed to be accumulated for comparable signal-to-noise ratios is much smaller than in the case of the echelle and comparable to OO spectrometers. Examples of Raman SHS applied to several pure liquids are given in Fig. 2. Raman SHS was used in three different settings: (i) for classification of six types of oils, (ii) for univariate/multivariate analysis of binary mixture cyclohexane-isopropanol, and (iii) for multivariate analysis of glycerol solution in water. For the last two settings, chemometric analysis of the spectra yielded linear calibration plots over the range 1-90% of concentrations of isopropanol in cyclohexane, and 0.5-10% of glycerol in water. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Spatial heterodyne spectroscopy KW - Raman spectroscopy KW - Laser-Induced Background Spectroscopy PY - 2019 AN - OPUS4-49176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas T1 - Multivariate analysis of large µ-FTIR datasets in search of microplastics N2 - µ-FTIR spectroscopy is a widely used technique in microplastics research. It allows to simultaneously characterize the material of the small particles, fibers or fragments, and to specify their size distribution and shape. Modern detectors offer the possibility to perform two-dimensional imaging of the sample providing detailed information. However, datasets are often too large for manual evaluation calling for automated microplastic identification. Library search based on the comparison with known reference spectra has been proposed to solve this problem. To supplement this ‘targeted analysis’, an exploratory approach was tested. Principal component analysis (PCA) was used to drastically reduce the size of the data set while maintaining the significant information. Groups of similar spectra in the prepared data set were identified with cluster analysis. Members of different clusters could be assigned to different polymer types whereas the variation observed within a cluster gives a hint on the chemical variability of microplastics of the same type. Spectra labeled according to the respective cluster can be used for supervised learning. The obtained classification was tested on an independent data set and results were compared to the spectral library search approach. T2 - CEST 2019 CY - Rhodes, Greece DA - 04.09.2019 KW - FTIR KW - Microplastics KW - Multivariate data analysis PY - 2019 AN - OPUS4-48889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Aus dem Labor in den Prozess: Anforderungen an Smarte Laborgeräte vor dem Hintergrund der Digitalisierung N2 - Im Vortrag werden Anforderungen und Lösungsvorschläge für das Labor der Zukunft diskutiert. Industrie 4.0 bzw. das Labor 4.0 hilft uns, komplexere Prozesse schneller umzusetzen. Entwicklung von Anlagen und Prozessen beginnt im Labor 4.0. Dazu werden offene, nicht proprietäre Schnittstellen und Standards bei Laborgeräten und Feldgeräten dringend benötigt. T2 - Branchentreff Chromatografie: Analytik gestern, heute – morgen? CY - Berlin, Germany DA - 30.09.2019 KW - Smarte Laborgeräte KW - Digitalisierung KW - Prozessanalytik KW - Labor 4.0 KW - Prozesslabor PY - 2019 UR - https://www.healthcapital.de/termine/termin/branchentreff-chromatografie-analytik-gestern-heute-morgen/ AN - OPUS4-49186 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Editorial: Es ist Arznei, nicht Gift, was ich dir reiche N2 - Der Artikel ist ein Editorial, der für die Herstellung eines grundlegenden Vertrauens in medizinische Produkte - insbesondere Impfstoffe - wirbt, um Skeptiker zu Unterstützern zu machen. Er wirbt nicht nur für die Impfstoffe, sondern auch für die Kultur der Pharmazie und Chemie und die Wissenschaft ganz allgemein und regt an, mehr erklärende Formate wie z. B. im Stil der Sendung mit der Maus für diese Dinge zu werben. Der Artikel geht auch auf den ungeheuren Reiz der seit gut zwanzig Jahren diskutierten risikobasierten Ansätze für pharmazeutische Entwicklung und Herstellung von Arzneimitteln auf Basis der Quality Guidelines ein. KW - Impfstoffe KW - Pharmazeutische Produktion KW - Qualitätssicherung KW - Wissenschaftskultur KW - Prozessanalytik KW - Quality by Design PY - 2021 SN - 2625-4212 SN - 2364-3137 VL - 63 IS - 3 SP - 1 PB - Vulkan Verlag CY - Essen AN - OPUS4-52264 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Maiwald, Michael A1 - Bassler, M. A1 - Deilmann, M. A1 - Ens, W. A1 - Frenzel, F. A1 - Gerlach, M. A1 - Großmann, J. A1 - Grümbel, F. A1 - Heisterkamp, M. A1 - Kaiser, U. A1 - Lambrecht, A. A1 - Ohlenkamp, R. A1 - Pötter, T. A1 - Pyka, P. A1 - Roos, E. A1 - Schmidt, A. A1 - Schünemann, U. A1 - Theuer, M. A1 - Tukle, A. A1 - Weber, N. T1 - Technologie-Roadmap „Prozess-Sensoren 2027+“ N2 - Die Technologie-Roadmap „Prozess-Sensoren 2027+“ ist eine Weiterentwicklung vorgängiger Technologie-Roadmaps. Im Zentrum dieser Roadmaps stehen Sensoren zur Erfassung von physikalischen und chemischen Messgrößen mittels spezifischer und unspezifischer Messverfahren, die zur Steuerung und dem besseren Verständnis von Prozessen dienen. Die Roadmap fasst die gemeinsame Technologie- und Marktsicht von Anwendern, Herstellern und Forschungseinrichtungen im Bereich Prozess-Sensorik in der verfahrenstechnischen Industrie zusammen. Sie beschreibt die wesentlichen Trends im Bereich Prozess-Sensorik und künftige Handlungsbedarfe für Hersteller, Anwender sowie für Einrichtungen der Forschung und Lehre. Für die aktuellen und zukünftigen Anforderungen an Prozess-Sensoren werden 19 Thesen formuliert. Die Thesen basieren auf den Thesen der vorangegangenen Roadmaps, wobei die aus heutiger Sicht erforderlichen Anpassungen, Ergänzungen und teilweise auch Streichungen vorgenommen wurden. Die Thesen sind in 5 Themencluster eingeordnet. Digitalisierung und Nachhaltigkeit sind übergreifende Kernthemen der künftigen Entwicklung. KW - Technologie-Roadmap Prozess-Sensoren KW - Prozessindustrie KW - Prozessanalytik KW - Sensorik KW - Digitalisierung KW - NAMUR PY - 2021 SP - 1 EP - 63 AN - OPUS4-53741 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Quantitative NMR Spectroscopy (qNMR) as an Indispensable Instrumental Analytical Method and its Metrological Application N2 - Introduction NMR spectroscopy is one of the most important analytical methods in organic chemistry. While most analyses are carried out qualitatively with the aim of substance identification and structure elucidation, quantitative NMR spectroscopy (qNMR) is increasingly gaining importance in research and industry. qNMR provides the most universally applicable form of direct purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. Methods One of the most attractive features of quantitative NMR spectroscopy is that the NMR peak areas can be used directly for concentration quantification without further calibration. Another advantage of NMR spectroscopy is that the method has a high linearity between absolute signal area and sample concentration, which makes it an absolute analytical comparison method that is independent of the matrix. This enables automated robust data evaluation strategies that can be used for online applications of qNMR spectroscopy. Jancke et al. proposed NMR spectroscopy as a relative primary analytical method because it can be fully described by mathematical equations from which a complete uncertainty budget can be derived, allowing it to be used at the highest metrological level. Weber et al. discussed in detail important aspects of the procedure that enable the realisation of low measurement uncertainties in qNMR measurements. Since certification of CRM requires expanded mea¬sure¬ment uncertainties of less than 0.5 % (relative), the work of Weber et al. demonstrated for the first time that qNMR can fulfil this criterion. Results To date, further comparative studies have been carried out in metrology and industry, demonstrating the performance of quantitative NMR spectroscopy and further reducing measurement uncertainties. The development of validation concepts and the commercial availability of suitable certified reference materials facilitate the application, especially in the usually highly regulated industrial environment. Users can thus accelerate the development of analytical methods. The talk will cover a wide range of topics from current metrological activities to new challenges for qNMR spectroscopy and also deals with aspects such as validation and accreditation. Innovative aspects • qNMR provides the most universally applicable form of direct purity determination • Expanded measurement uncertainties lower than 0.15 % (relative) possible • Benchtop NMR instruments increasingly used for qNMR spectroscopy T2 - ANAKON 2023 CY - Vienna, Austria DA - 11.04.2023 KW - Quantitative NMR Spectroscopy KW - qNMR KW - Process Analytical Technology KW - NMR Validation KW - NMR Accreditation KW - Purity KW - ANAKON PY - 2023 AN - OPUS4-57304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Online NMR spectroscopy paves the way for short development times in industrial reaction and process monitoring N2 - Modular chemical production is a tangible implementation of the digital transformation of the specialty chemicals process industry. In particular, it enables acceleration of process development and thus faster time to market by flexibly interconnecting and orchestrating standardized physical modules and bringing them to life. For this purpose, specific (chemical) sensors of process analytics are needed, preferably without lengthy calibration or spectroscopic model development. An excellent example of a "direct" analytical method is online nuclear magnetic resonance (NMR) spectroscopy. NMR spectroscopy meets the requirements of a direct analytical method because of the direct correlation between the signal area in the spectrum ("counting" the nuclear spins) and the analyte amount of substance concentrations. It is also extremely linear over the concentration range. With the availability of compact benchtop NMR instruments, it is now possible to bring NMR spectroscopy directly into the field, in close proximity to specialized laboratory facilities, pilot plants, and even industrial-scale production facilities. The first systems are in TRL 8 (Qualified System with Proof of Functionality in the Field). The presentation will discuss the many building blocks of online nuclear magnetic resonance spectroscopy, from flow cells to automated data analysis. T2 - SFB 1527 HyPERiON “High Performance Compact Magnetic Resonance“ Online Seminar CY - Karlsruhe, Germany DA - 06.07.2023 KW - Online NMR Spectroscopy KW - Process Monitoring KW - Reaction Monitoring KW - Industry 4.0 KW - Automation KW - Modular Production PY - 2023 AN - OPUS4-57862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Optical spectrometry for isotope analysis N2 - Isotope analysis plays a critical role in various disciplines, including environmental science, archaeology, and forensic investigations. Traditional methods such as mass spectrometry provide precise isotopic data but often require complex, costly setups and extensive sample preparation. As an alternative, optical spectrometry has emerged as a versatile and less invasive technique. This presentation explores the advancements and applications of optical spectrometry methods in isotope analysis, emphasizing their benefits and challenges. T2 - University of Calgary PHYS 561 - Stable And Radioactive Isotope - Winter 2024 CY - Online meeting DA - 07.03.2024 KW - Isotopes KW - HR-CS-MAS KW - Chemometrics KW - Laser Ablation Molecular Absorption spectrometry KW - LAMIS PY - 2024 AN - OPUS4-59948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Isotope analysis through the integration of chemometrics into optical spectroscopy N2 - Lithium (Li), Boron (B), Nitrogen (N), Magnesium (Mg), and Calcium (Ca) are pivotal elements across various spheres such as the hydrosphere, biosphere, and lithosphere, significantly impacting (bio-) geochemical and physiological processes. These elements exhibit stable isotopes with substantial roles in geological, environmental, and biological studies. The traditional method for measuring isotope amount ratios has been through mass spectrometry, which, despite its accuracy, comes with high operational costs, the need for skilled operators, and time-consuming sample preparation processes. Combining optical spectroscopy with chemometrics introduces an innovative, cost-effective approach by the hand of high-resolution continuum source atomic and molecular absorption spectrometry (HR-CS-AAS and HR-CS-MAS) for the analysis of isotope ratios in Li, B, N, Mg, and Ca. By analyzing the atomic or molecular absorption spectrum of the in-situ generated cloud of atoms of diatomic molecules (e.g., Li, BH, NO, MgF, CaF) during the electronic transition from the fundamental state, this method allows for the rapid determination of isotope ratios directly from sample solutions without the need for complex sample preparation. For each element, the respective atomic or molecule's absorption spectrum was deconvoluted into its isotopic components using partial least squares regression or machine learning algorithms. Robust calibration models were developed, calibrated with enriched isotope, and validated against certified reference materials. Spectral data underwent preprocessing to optimize the modeling to determine the optimal number of latent variables. The findings showcase that this optical spectrometric method yields results that agree with those obtained via inductively coupled plasma mass spectrometry (ICP-MS), offering a promising, cost-effective, and rapid alternative for isotope analysis with precisions as low as ± 0.2‰. This approach is a significant advancement in analytical chemistry, providing a new way to study isotope variations in biological, environmental, and geological samples. T2 - Analytica Conference CY - Munich, Germany DA - 09.04.2024 KW - Isotopes KW - HR-CS-MAS KW - Chemometrics KW - Lithium KW - Boron KW - Magnesium KW - Nitrogen PY - 2024 AN - OPUS4-59946 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian A1 - Vogel, Kristin T1 - Berechnung und Nutzung von Unsicherheiten zertifizierter Werte von Referenzmaterialien N2 - Referenzmaterialien sind unter anderem ein wichtiges Werkzeug zur Qualitätskontrolle von Messungen bestimmter Merkmalswerte. Dabei ist zu berücksichtigen, dass zertifizierte Merkmalswerte immer eine gewisse Unsicherheit haben. Die Ermittlung dieser Unsicherheitsbeiträge ist Gegenstand des Vortrags. Referenzmaterialien sind gleichzeitig ein wertvolles Werkzeug zur Ermittlung der Unsicherheit von Messverfahren und -Analysen unbekannter Proben. Die Vorgehensweise bei der Ermittlung der Messunsicherheit mit Hilfe eines Referenzmaterials wird beschrieben. T2 - Jahrestagung des GDMB-Chemiker-Ausschusses CY - Kassel, Germany DA - 07.11.2023 KW - Referenzmaterial KW - Messunsicherheit KW - ISO Guide 35 PY - 2023 AN - OPUS4-58929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Remelting Miwo - Methoden für die Vor-Ort Analytik N2 - In Deutschland werden jährlich rund 20 Millionen Tonnen künstliche Mineralwolle für die Dämmung von Dächern und Fassaden sowie für Brandschutzprodukte verwendet. Um künstliche Mineralwolle aus Rückbaumaßnahmen in den Produktionsprozess zurückführen zu können, ist eine Trennung in Glas- und Steinwolle erforderlich, um eine Vermischung der beiden Produkte, die unterschiedliche Schmelztemperaturen aufweisen, zu vermeiden. Anstatt die Mineralwolle in spezielle Labors zu schicken, was zeitaufwendig und teuer ist, wurde das Potenzial eines tragbaren Nahinfrarot-Spektrometers (NIR) für den Einsatz vor Ort getestet. 140 verschiedene Mineralwolleproben wurden untersucht, um eine NIR-basierte Methode für die Vor-Ort-Unterscheidung zwischen Glas- und Steinwolle zu etablieren. Die Validierung der Methode mit Testproben und die Anwendung auf Materialien, die aus BigBags für Deponien entnommen wurden, haben gezeigt, dass die Methode präzise und robust ist. Als Referenzmethode wurde die Röntgenfluoreszenzspektroskopie (RFA) mit einer Kalibrierung auf der Grundlage der VDI 3492 verwendet. T2 - 23. Projektetage der Bauforschung CY - Online meeting DA - 14.03.2023 KW - NIR KW - RFA KW - Mineralwolle PY - 2023 AN - OPUS4-57372 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Sensors, Analytics and Certified Reference Materials safeguarding the quality infrastructure in the hydrogen economy N2 - The prerequisites for a successful energy transition and the economic use of hydrogen as a clean green energy carrier and for H2 readiness are a rapid market ramp-up and the establishment of the required value chains. Reliable quality and safety standards for innovative technologies are the prerequisite for ensuring supply security, for environmental compatibility and sustainable climate protection, for building trust in these technologies and thus enable product and process innovations. With the Competence Centre "H2Safety@BAM", BAM is creating the safety-related prere-quisites for the successful implementation of hydrogen technologies at national as well as European level. BAM uses decades of experience in dealing with hydrogen technologies to develop the necessary quality and safety standards. The presentation will draw a bow from the typical basic tasks of BAM in the field of competence "Sensors, analytics and certified reference materials", such as maintenance and dissemination of the national gas composition standards for calorific value determination as Designated Institute for Metrology in Chemistry within the framework of the Metre Convention, to the further development of measurement and sensor technology for these tasks. For the certification of reference materials, a mostly slow and time-consuming but solid reference analysis is common. With hydrogen and its special properties, completely new requirements are added. In addition, fast and simple online analysis is required for process control, for example to register quality changes, e.g., during load changes or refuelling processes. T2 - Indo-German International Conference on Metrology for the Deployment of Green Hydrogen and Renewable Fuels in India CY - Online meeting DA - 04.04.2022 KW - Quality Infrastructure KW - Gas Reference Material KW - Hydrogen KW - Energy Gases KW - Sensors KW - Hydrogen Storage Materials PY - 2022 UR - https://www.imeko-gh2fuels.ptb.de/ AN - OPUS4-54596 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Integrated and networked systems and processes – A perspective for digital transformation of our chemical and pharmaceutical production N2 - Chemical and pharmaceutical companies have to find new paths to survive successfully in a changing environment, while also finding more flexible ways of product and process development to bring their products to market more quickly – especially high-quality high-end products like fine chemicals or pharmaceuticals. The potential of digital technologies belongs to these. A current approach uses flexible and modular chemical production units, which can produce different high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce the time to market of new products. At the same time, we need to move towards knowledge-based production that takes into account all essential equipment, process and control data from plants and laboratories and makes valuable expertise available and transferable. The potential of data from production together with its contextual information is often not yet consistently used today for a comprehensive understanding of production. By giving examples this paper outlines a possible more holistic approach to digitalisation and the use of machine-based methods in the production of specialty chemicals and pharmaceuticals through the introduction of integrated and networked systems and processes. T2 - GDCh Science Forum 2021 - GDCh Wissenschaftsforum 2021 CY - Online meeting DA - 29.08.2021 KW - Process analytical technology KW - Online NMR spectroscopy KW - Process industry KW - Industry 4.0 KW - Digital transformation KW - Autonomous chemistry PY - 2021 AN - OPUS4-53171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - A comparative analysis of optical spectrometry methods and MC-ICP-MS for stable isotope analysis of magnesium in geological samples N2 - Society for Applied Spectroscopy (SAS) Atomic Section Student Award. Magnesium is a major element in the hydrosphere and biosphere and plays important roles in (bio-) geochemical and physiological cycles. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg. It is due to their relatively large mass difference (~8% between) that isotope fractionation leads to slight variations of isotope amount ratios in biological, environmental and geological samples. Traditionally, isotope ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation. Recently, optical spectrometric methods have been proposed as faster and low-cost alternative for the analysis of isotope ratios of selected elements by means of high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS), and laser ablation molecular isotopic spectrometry (LAMIS). For the determination of Mg isotope ratios in selected rock reference materials, the molecular spectrum of the in-situ generated MgF and MgO molecules were studied and their results compared with MC-ICP-MS. By HR-CS-MAS, samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix. The absorption spectrum was recorded for MgF for the electronic transitions X 2Σ → A 2 Πi, and X 2Σ → B 2Σ+. In the case of LAMIS, we investigated the MgF molecule for the electronic transition A 2Πi → X 2Σ, as well as direct analysis by the MgO molecule for the electronic transition A 1Π+ → X 1Σ. The MgF and MgO spectra are described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF for the MgF and 24MgO, 25MgO, and 26MgO for the MgO. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS) calibrated with enriched isotope spikes. Results were accurate with precisions ranging between 0.2 ‰ and 0.8 ‰ (2 SD, n= 10) for HR-CS-GFMAS. No statistically significant differences were observed for samples w/o matrix extraction. On the other hand, LAMIS allows the direct analysis of solid samples with the extended possibility of direct analysis, however the precision is lower due the lack of solid isotopic calibration standards. T2 - SciX 2019. 46th Annual North American Meeting of the Federation of Analytical Chemistry and Spectroscopy Societies (FACSS) CY - Palm Springs, CA, USA DA - 13.10.2019 KW - Isotope analysis KW - Diatomic molecule KW - Magnesium KW - MC-ICP-MS KW - HR-CS-MAS KW - LIBS PY - 2019 AN - OPUS4-49883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Schmid, Thomas ED - Dariz, P. T1 - Special issue: Modern Raman spectroscopy of minerals N2 - Dear Colleagues, Raman spectroscopy provides vibrational fingerprints of chemical compounds, enabling their identification via a comparison with reference spectra. This analytical tool has high potential not only in the identification of minerals from natural sources but also for studying the complex microstructure and mineral distribution of both ancient and modern man-made materials, ranging from, e.g., historical ceramics and mortars to modern solar cell materials. In addition to the chemical identity of minerals, Raman spectra are affected by crystal orientations, substoichiometric to stoichiometric compositional changes (e.g., in solid solution series), traces of foreign ions, stress, strain, and crystallinity, enabling a comprehensive physicochemical characterisation of minerals. This Special Issue includes method developments and applications in the field of modern Raman spectroscopy of minerals in a broad sense, from natural mineral deposits to inorganic phases in materials; covers both spectroscopic and imaging studies; and provides a platform for discussing the possibilities and limits of the technique in the context of the existing analytical arsenal. Thomas Schmid Petra Dariz KW - Analytical sciences KW - Raman spectroscopy KW - Raman microspectroscopy KW - Mineral identification KW - Mineral paragenesis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519117 UR - https://www.mdpi.com/journal/minerals/special_issues/Raman_Spectroscopy_Minerals VL - 10 SP - 1 EP - 156 PB - MDPI CY - Basel AN - OPUS4-51911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Chao, Madlen T1 - Entwicklung und Validierung eines Online-LIBS-Verfahrens für die Bestimmung von Nährelementen in Böden N2 - In den letzten Jahrzehnten ist die Nachfrage nach kostengünstigen und flächendeckenden Kartierungsmöglichkeiten im Hinblick auf eine ertragssteigernde und umweltfreundlichere Bewirtschaftung von landwirtschaftlichen Nutzflächen stark gestiegen. Hierfür eignen sich spektroskopische Methoden wie die Röntgenfluoreszenzanalyse (RFA), Raman- und Gammaspektroskopie sowie die laserinduzierte Plasmaspektroskopie (LIBS). In Abhängigkeit von der Funktionsweise der jeweiligen Methoden werden Informationen zu verschiedensten Bodeneigenschaften wie Nährelementgehalt, Textur und pH-Wert erhalten. Ziel dieser Arbeit ist die Entwicklung eines Online-LIBS-Verfahrens zur Nährelementbestimmmung und Kartierung von Ackerflächen. Die LIBS ist eine schnelle und simultane Multielementanalyse bei der durch das Fokussieren eines hochenergetischen Laserpulses Probenmaterial von der Probenoberfläche ablatiert wird und in ein Plasma überführt wird. Beim Abkühlen des Plasmas wird Strahlung emittiert, welche Rückschlüsse über die elementare Zusammensetzung der Probe gibt. Diese Arbeit ist im Teilprojekt I4S (Intelligenz für Böden) im Forschungsprogramm BonaRes (Boden als nachhaltige Ressource für die Bioökonomie) des Bundesministerium für Bildung und Forschung (BMBF) entstanden. Es wurden insgesamt 651 Bodenproben von verschiedenen Test-Agrarflächen unterschiedlichster Standorte Deutschlands gemessen, ausgewertet und zu Validierungszwecken mit entsprechender Referenzanalytik wie die Optische Emissionsspektroskopie mittels induktiv gekoppeltem Plasma (ICP-OES) und die wellenlängendispersive Röntgenfluoreszenzanalyse (WDRFA) charakterisiert. Für die Quantifizierung wurden zunächst die Messparameter des LIBS-Systems auf die Bodenmatrix optimiert und für die Elemente geeignete Linien ausgewählt sowie deren Nachweisgrenzen bestimmt. Es hat sich gezeigt, dass eine absolute Quantifizierung basierend auf einem univariaten Ansatz aufgrund der starken Matrixeffekte und der schlechten Reproduzierbarkeit des Plasmas nur eingeschränkt möglich ist. Bei Verwendung eines multivariaten Ansatz wie der Partial Least Squares Regression (PLSR) für die Kalibrierung konnten für die Nährelemente im Vergleich zur univariaten Variante Analyseergebnisse mit höherer Güte und geringeren Messunsicherheiten ermittelt werden. Die Untersuchungen haben gezeigt, dass das multivariate Modell weiter verbessert werden kann, indem mit einer Vielzahl von gut analysierten Böden verschiedener Standorte, Bodenarten und einem breiten Gehaltsbereich kalibriert wird. Mithilfe der Hauptkomponentenanalyse (PCA) wurde eine Klassifizierung der Böden nach der Textur realisiert. Weiterhin wurde auch eine Kalibrierung mit losem Bodenmaterial erstellt. Trotz der Signalabnahme konnten für die verschiedenen Nährelemente Kalibriergeraden mit ausreichender, analytischer Güte erstellt werden. Für den Einsatz auf dem Acker wurde außerdem der Einfluss von Korngröße und Feuchtigkeit auf das LIBS-Signal untersucht. Die unterschiedlichen Korngrößen haben nur einen geringen Einfluss auf das LIBS-Signal und das Kalibriermodell lässt sich durch entsprechende Proben leicht anpassen. Dagegen ist der Einfluss der Feuchtigkeit deutlich stärker und hängt stark von der Bodenart ab, sodass für jede Bodenart ein separates Kalibriermodell für verschiedene Feuchtigkeitsgehalte erstellt werden muss. Mithilfe der PCA kann der Feuchtigkeitsgehalt im Boden grob abgeschätzt werden und die entsprechende Kalibrierung ausgewählt werden. Diese Arbeit liefert essentielle Informationen für eine Echtzeit-Analyse von Nährelementen auf dem Acker mittels LIBS und leistet einen wichtigen Beitrag zu einer fortschrittlichen und zukunftsfähigen Nutzung von Ackerflächen. KW - Boden KW - Chemometrie KW - LIBS KW - Nährelemente KW - Düngeempfehlung KW - Precision Agriculture KW - Prozessanalytik PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:517-opus4-476772 DO - https://doi.org/https://doi.org/10.25932/publishup-47677 SP - 1 EP - 130 PB - Universität Potsdam CY - Potsdam AN - OPUS4-52183 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmid, Thomas A1 - Jungnickel, R. A1 - Dariz, P. T1 - Raman band widths of anhydrite II reveal the burning history of high‐fired medieval gypsum mortars N2 - When used as a mineral binder, gypsum is thermally dehydrated and mixed with water, resulting in a paste hardening in the backreaction to calcium sulphate dihydrate (CaSO4 · 2 H2O). Although nowadays mainly hemihydratebased (CaSO4 · ½ H2O) binders are employed, higher firing temperatures in medieval kilns yielded anhydrite II (CaSO4). Except for the discrimination of the metastable phases anhydrite III and I due to different crystal structures, variations within the production temperature range of anhydrite II (approximately 300 to 1180°C) were not analytically accessible until recently. This study describes the development of an analytical technique, which is based on steady changes of band widths in room‐temperature Raman spectra of anhydrite II as a function of burning temperature. Raman microspectroscopic mapping experiments enable to pinpoint individual unreacted grains of thermal anhydrite in mortars and to discriminate them from natural anhydrites originating from the raw gypsum. The determination of band full widths at half maximum of down to 3 cm−1 and differences between them of a few tenths of wavenumbers is not a trivial task. Thus, a focus of this work is on peak fitting and strategies for correction of instrument‐dependent band broadening, which is often neglected also beyond the field of mortar analysis. Including other potential influences on band widths, burning temperatures of 400 to 900°C can be retraced in high‐fired medieval gypsum mortars with an uncertainty of approximately ± 50 K, as demonstrated with sample material of a stucco sculpture dated around 1400. KW - Analytical methods KW - Gypsum dehydration KW - High-fired gypsum mortar KW - Raman band width determination KW - Thermal anhydrite PY - 2019 DO - https://doi.org/10.1002/jrs.5632 SN - 1097-4555 VL - 50 IS - 8 SP - 1154 EP - 1168 PB - Wiley AN - OPUS4-48757 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hommel, C. A1 - Hassler, J. A1 - Matschat, Ralf A1 - Vogt, T. A1 - Detcheva, A. K. A1 - Recknagel, Sebastian T1 - A fast and robust direct solid sampling method for the determination of 27 trace, main and minor elements in soda-lime glass based on ETV-ICP OES and using a gaseous halogenating modifier N2 - A method, based on electrothermal vaporization (ETV) coupled to inductively coupled plasma optical emission spectrometry (ICP OES), has been optimized for direct solid sampling analysis of soda-lime glass - the most common type of industrially manufactured glass. This method allows fast and reliable quantification of the main elements - Al, Ca, K, Mg, Na, and Si - and trace elements - As, Ba, Cd, Ce, Co, Cr, Cu, Fe, Mn, Mo, Ni, (P), Pb, Sb, (Se), Sn, Sr, Ti, V, Zn, and Zr. In the presented ETV-ICP OES method, calibration is performed predominantly with matrix-free synthetic samples. This metrological advantage is normally not achieved with direct solid sampling methods and is one of the goals of the present study. In a certification interlaboratory comparison for the soda-lime glass CRM BAM-S005c, 2 out of 16 laboratories employed the ETV-ICP OES method. An improved analytical performance was obtained compared with the results of laboratories that used conventional liquid ICP OES. For both methods, the average relative deviations between the laboratory results and certified values as well as the average values of relative standard deviation were with a few exceptions <10%, in most cases even <5%, which indicated high trueness and precision. KW - ICP-OES KW - ETV KW - Soda-lime glass KW - Reference material PY - 2021 DO - https://doi.org/10.1039/d1ja00081k SN - 0267-9477 SN - 1364-5544 VL - 36 IS - 8 SP - 1683 EP - 1693 PB - Royal Society of Chemistry CY - London AN - OPUS4-53181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fernandez-Menendez, L. J. A1 - Mendez-Lopez, C. A1 - Abad Andrade, Carlos Enrique A1 - Fandino, J. A1 - Gonzalez-Gago, C. A1 - Pisonero, J. A1 - Bordel, N. T1 - A critical evaluation of the chlorine quantification method based on molecular emission detection in LIBS N2 - The entire process involving the determination of Cl by molecular emission detection in Laser-Induced Breakdown Spectroscopy (LIBS) is thoroughly studied in this paper. This critical evaluation considers how spectra are normalized, how interferences from other molecular species signals are removed, and how signal integration is applied. Moreover, a data treatment protocol is proposed to achieve reliable and accurate Cl determination from the CaCl molecular spectral signal, not requiring the use of more complex numerical approaches. Calcium chloride dihydrate (CaCl2⋅2H2O) and high purity anhydrite samples (CaSO4) are used to optimize the acquisition conditions and data treatment of CaCl emission signal. Using the developed protocol, calibration curves for Cl, covering the concentration range from 0 μg/g to 60,000 μg/g of Cl, are successfully achieved. Finally, the suitability of the proposed methodology for Cl determination is successfully applied in industrial gypsum waste samples, where the results obtained by LIBS are validated using high-resolution molecular absorption spectroscopy (HR-CS-MAS) and potentiometric titration. KW - Laser induced breakdown Spectrocopy (LIBS) KW - Molecular spectra KW - Chlorine determination KW - CaCl emission bands KW - Industrial gypsum PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544292 DO - https://doi.org/10.1016/j.sab.2022.106390 SN - 0584-8547 VL - 190 SP - 1 EP - 9 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-54429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Klas T1 - Flexible Prozessanalytik für die pharmazeutische Produktion - Benchtop-NMR-Spektroskopie im industriellen Einsatz N2 - Im Rahmen des EU-Projekts „CONSENS – Integrated Control and Sensing“ wurde ein vollautomatisiertes, gemäß Atmosphère-Explosibles(ATEX)-Regeln zertifiziertes Analysatormodul auf Basis eines kommerziellen Benchtop-Kernspinresonanzspektrometers (Engl. nuclear magnetic resonance, NMR) entwickelt und im Umfeld einer modularen containerbasierten Produktionsanlage validiert. Auf Basis der gewonnenen Daten konnten sowohl eine iterative Optimierung der Prozessparameter erfolgen als auch Referenzdaten für die Kalibrierung eines Nahinfrarot-Spektrometers gewonnen werden. KW - Prozessanalytik KW - NMR-Spektroskopie KW - Modulare Produktion KW - Kalibriertransfer PY - 2022 VL - 12 IS - 3 SP - 122 EP - 129 PB - Editio Cantor Verlag CY - Aulendorf AN - OPUS4-55402 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Integrated and Networked Systems and Processes - How NMR Spectroscopy Can Transform our Chemical and Pharmaceutical Production N2 - Chemical and pharmaceutical companies need to find new ways to survive successfully in a changing environment, while finding more flexible ways of product and process development to bring their products to market faster - especially high-value, high-end products such as fine chemicals or pharmaceuticals. This is complicated by changes in value chains along a potential circular economy. One current approach is flexible and modular chemical production units that use multi-purpose equipment to produce various high-value products with short downtimes between campaigns and can shorten time-to-market for new products. Online NMR spectroscopy will play an important role for plant automation and quality control, as the method brings very high linearity, matrix independence and thus works almost calibration-free. Moreover, these properties ideally enable automated and machine-aided data analysis for the above-mentioned applications. Using examples, this presentation will outline a possible more holistic approach to digitalization and the use of machine-based processes in the production of specialty chemicals and pharmaceuticals through the introduction of integrated and networked systems and processes. T2 - 43rd FGMR Annual Discussion Meeting CY - Karlsruhe, Germany DA - 12.09.2022 KW - Digital Transformatioin KW - Process Industry KW - Pharmaceuticals KW - Specialty Chemicals KW - Automation KW - Online NMR Spectroscopy KW - Industry 4.0 PY - 2022 AN - OPUS4-55715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Modular process control with compact NMR spectroscopy - From field integration to automated data analysis N2 - Chemical companies must find new paths to stay productive in a rapidly changing environment. One of these is the potential of digital technologies. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market. Process safety is improved due to smaller amounts processed and the abilities of efficient heat-transfer allow for otherwise difficult-to-produce compounds. To exploit these advantages, a fully automated process control along with real-time quality control is mandatory and should be based on “chemical” information. The advances of a fully automated NMR analyzer were demonstrated, using a given pharmaceutical reaction step operated within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the requirements of an automated chemical production environment such as explosion safety, field communication, and robust data evaluation. Obtained results were used for direct loop advanced process control and real-time optimization of the process. NMR spectroscopy appeared as excellent online analytical tool and allowed a modular data analysis approach, which even served as reliable reference method for further PAT applications. Using the available datasets, a second data analysis approach based on artificial neural networks (ANN) was evaluated.Therefore, amount of data was augmented to be sufficient for training. The results show comparable performance, while improving the calculation time tremendously. In future, such fully integrated and interconnecting “smart” systems and processes can increase the efficiency of the production of specialty chemicals and pharmaceuticals. T2 - 5th European Conference on Process Analytics and Control Technology (EuroPACT) CY - Online meeting DA - 15.11.2021 KW - NMR spectroscopy KW - Benchtop-NMR KW - Modular production KW - Process Analytical Technology PY - 2021 AN - OPUS4-53776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Multi element analysis in soil using nitrogen microwave inductively coupled plasma mass spectrometry (MICAP MS) N2 - Due to the fast growth of industry and the use of metal-containing compounds such as sewage sludge in agricultural fields, soil pollution associated with heavy metals presents a terrifying threat to the environment. Throughout the world, there are already 5 million sites of soil contaminated by heavy metals1. Some heavy metals pollutants can influence food chain safety and food quality, which in turn affects human health. According to the German Federal Soil Protection and Contaminated Site Ordinance (BBodSchV) 13 heavy metals such as arsenic (As), lead (Pb) and cadmium (Cd) are classified as heavily toxic to human health2. Therefore, elemental analysis and precise quantification of the heavy metals in soil are of great importance. Inductively coupled plasma mass spectrometry (ICP-MS) emerged as a powerful technique for trace analysis of soil due to its multi-element capability, high sensitivity and low sample consumption. However, despite its success and widespread use, ICP-MS has several persistent drawbacks, such as high argon gas consumption, argon-based polyatomic interferences and the need for complicated RF-power generators. Unlike argon-based ICP, the nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) uses nitrogen as plasma gas, which eliminates high operating costs associated with argon-gas consumption as well as the argon-based interferences3. For the first time, the applicability of MICAP-MS for elemental analysis of environmental soils is investigated in this work. For this purpose, 7 reference- and 3 random soil samples containing vanadium (V), cobalt (Co), zink (Zn), copper (Cu), chrome (Cr), mercury (Hg), As, Pb and Cd are digested with aqua regia and used for analysis. Concentrations of selected elements are determined using MICAP-MS and validated using ICP-MS. Sensitivities, limits of detection and gas consumption for both methods are compared and discussed in detail. Moreover, the performance of MICAP-MS under different nitrogen plasma gas concentrations is investigated and compared. T2 - BAM Adlershofer Kolloquium CY - Online meeting DA - 21.06.2022 KW - Microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) KW - Multi-element analysis KW - Soil KW - Nitrogen plasma PY - 2022 AN - OPUS4-55182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Multi element analysis in soil using nitrogen microwave inductively coupled plasma mass spectrometry (MICAP MS) N2 - Due to the fast growth of industry and the use of metal-containing compounds such as sewage sludge in agricultural fields, soil pollution associated with heavy metals presents a terrifying threat to the environment. Throughout the world, there are already 5 million sites of soil contaminated by heavy metals1. Some heavy metals pollutants can influence food chain safety and food quality, which in turn affects human health. According to the German Federal Soil Protection and Contaminated Site Ordinance (BBodSchV) 13 heavy metals such as arsenic (As), lead (Pb) and cadmium (Cd) are classified as heavily toxic to human health2. Therefore, elemental analysis and precise quantification of the heavy metals in soil are of great importance. Inductively coupled plasma mass spectrometry (ICP-MS) emerged as a powerful technique for trace analysis of soil due to its multi-element capability, high sensitivity and low sample consumption. However, despite its success and widespread use, ICP-MS has several persistent drawbacks, such as high argon gas consumption, argon-based polyatomic interferences and the need for complicated RF-power generators. Unlike argon-based ICP, the nitrogen microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) uses nitrogen as plasma gas, which eliminates high operating costs associated with argon-gas consumption as well as the argon-based interferences3. For the first time, the applicability of MICAP-MS for elemental analysis of environmental soils is investigated in this work. For this purpose, 7 reference- and 3 random soil samples containing vanadium (V), cobalt (Co), zink (Zn), copper (Cu), chrome (Cr), mercury (Hg), As, Pb and Cd are digested with aqua regia and used for analysis. Concentrations of selected elements are determined using MICAP-MS and validated using ICP-MS. Sensitivities, limits of detection and gas consumption for both methods are compared and discussed in detail. Moreover, the performance of MICAP-MS under different nitrogen plasma gas concentrations is investigated and compared T2 - Spectroscopium Colloquium CY - Gijon, Spain DA - 30.05.2022 KW - Microwave inductively coupled atmospheric pressure mass spectrometry (MICAP-MS) KW - Multi-element analysis KW - Soil KW - Nitrogen plasma PY - 2022 AN - OPUS4-55181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Next Generation Automation - Arbeitskreis 3.7: Smarte Sensorik, Aktorik und Kommunikation N2 - Der AK 3.7 ist ein "erweiterter" AK und je zur Hälfte mit NAMUR-Vertretern und Vertretern der Geräte- und Softwarehersteller besetzt. Er wurde ins Leben gerufen, um Begrifflichkeiten der digitalen Transformation aufzugreifen, wie etwa Smarte Sensorik, Sensordatenfusion, Schwarmsensorik oder Softsensorik. Eine erste Aufgabe bestand darin, einige exemplarische Anwendungsfälle der Nutzung smarter Eigenschaften von Feldgeräten sowie deren zukünftige Kommunikationsmöglichkeiten sowohl mit Bezug auf Bestandsanlagen als auch mit Blick auf einen potentiellen Technologiewechsel zu betrachten. Neuer Scope des AK 3.7 ist eine "Next Generation Automation" um einen potentiellen Technologiewechsel rechtzeitig vorauszudenken. Dieses erfolgt unter vollständiger gedanklicher Trennung von heutiger Automatisierung und auch vom NOA-Konzept. Ebenso wird ein Technologiewechsel in der Produktion der Prozessindustrie (wahrscheinlich modulbasiert) postuliert. Ziel des AK 3.7 wird es in Zukunft sein, diese Anforderungen an smarte Feldgeräte aufzugreifen und gemeinsam mit den thematisch überlappenden Interessenskreisen in Standards zu übersetzen. KW - Prozessindustrie KW - Automation KW - NAMUR KW - Sensorik KW - Aktorik KW - Kommunikation PY - 2021 SN - 2190-4111 SN - 2364-3137 IS - 9 SP - 73 PB - Vulkan Verlag CY - Essen AN - OPUS4-54336 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dariz, P. A1 - Schmid, Thomas T1 - Phase composition and burning history of high-fired medieval gypsum mortars studied by Raman microspectroscopy N2 - The use of high-fired gypsum as binder for masonry and joint mortars or stuccowork in Central Europe in the Early and High Middle Ages was a regional specific as it depended on local gypsum deposits. The calcination technology possible at the time resulted in an assemblage of calcium sulphate phases dehydrated to different degrees and partly thermally damaged accessory minerals of the raw gypsum. Not hydrated clusters of firing products preserved in the binder matrix are a typical feature of such mortars. A novel Raman microspectroscopic approach, providing access to the burning history of individual anhydrite grains, was applied to samples from medieval South Tyrolean stucco decorations and sculptures. Beyond that, Raman microspectroscopy was employed for tracing and visualising pyrometamorphic reactions in natural impurities of the kiln run. In the discussed examples mineral thermometry indicates process temperatures above 800°C: the breakdown of magnesium-rich chlorite led to the formation of forsterite Mg2SiO4, while the thermal decomposition of dolomite CaMg(CO3)2 to periclase MgO and lime CaO yielded – after hydration and carbonation – magnesite MgCO3, CaCO3 polymorphs and magnesian calcite. Hydration of periclase in the mixed gypsum paste containing sulphate ions also resulted in magnesium sulphate hydrates, here identified in the form of hexahydrite MgSO4·6H2O. Lower burning temperatures left the accessory minerals in their pristine form, but can be traced by measuring the spectra of individual anhydrite crystals in grains of firing products and evaluating Raman band widths. Throughout the present study, calcination temperatures ranging from approx. 600°C to 900°C were determined. KW - High-fired gypsum mortar KW - Anhydrite KW - Dolomite KW - Forsterite KW - Raman microspectroscopy PY - 2019 DO - https://doi.org/10.1016/j.matchar.2019.03.013 VL - 151 SP - 292 EP - 301 PB - Elsevier Inc. AN - OPUS4-48102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Potential of multivariate data analysis (MVA) in X-ray fluorescence analysis N2 - X-ray fluorescence spectrometry (XRF) is used, for example, in geochemistry, archaeology, materials science and agriculture to analyze the elemental composition of various samples [1]. Quantitative spectrum analysis typically applies methods such as fundamental parameters or intensity correction [1, 2]. However, there are also approaches to analyze XRF spectra using data-driven MVA approaches that are not based on a physical model. Principal component analysis (PCA) enables the visualization of data and the discovery of hidden relationships between analytical signals and sample parameters [1, 3]. Classification methods, e.g. PCA, cluster or discriminant analysis, can help to distinguish samples based on various complex integral features such as authenticity or origin of the sample [3]. MVA can also be used to correlate various external factors with elemental composition. In addition to classifying mineral wool into different material types based on characteristic oxides, PCA also enables the visualization of problem cases and supports the detection of possible outliers [4]. Multivariate regression methods such as partial least squares regression (PLSR) are a powerful tool for the quantitative analysis of spectra. In contrast to univariate analysis, in which only one characteristic is used as the basis for the regression, entire spectra or spectral ranges are analyzed here. It has been shown that the quantitative determination of C, H, N and O in polymers based on WDXRF spectra can be achieved by PLSR [5]. However, in the presence of complex matrix effects, the limitations of PLSR become clear, as was shown in a reference case (EDXRF spectra of steel and ore samples) [2]. Here, PLSR still outperformed the fundamental parameter approach, but proved to be less accurate than an intensity correction approach. Neural networks, which are better able to deal with nonlinear effects, are only an alternative if both a large number of calibration samples are available for adequate network training and a lot of time is available for network optimization. Despite limitations, it can be summarized that MVA, if used correctly, can contribute to increasing the informative value of XRF and to opening up new fields of application in areas of growing economic importance [1-5]. T2 - 12. PRORA Fachtagung Prozessnahe Röntgenanalytik CY - Berlin, Germany DA - 28.11.2024 KW - Chemometrics KW - Mineral wool KW - Data analysis KW - X-ray fluorescence PY - 2024 AN - OPUS4-62032 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Deconvolution in High-Field- and Benchtop-NMR applications N2 - Numerical "sum integration" is the typical way to extract signal area from NMR spectra for quantitative evaluation, however, in complex situations of peak overlaps or crowded spectra this can be impractical. Deconvolution methods based on linefitting and optimization allow for a more accurate extraction of signal features from the spectrum in these cases. The increasing number of benchtop NMR applications showing lower signal dispersion and therefore more often complex spectral patterns foster the development and application of model-based spectra evaluation methods. This includes techniques like Indirect Hard Modeling (IHM), Quantum-Mechanical Spectra Analysis (QMSA), Chemometric modeling like PLS-R or MCR, as well as Machine-learning approaches using Neural Networks. This presentation gives an overview and introduction into deconvolution methods in the context of high-field and benchtop-NMR applications in complex spectra and process monitoring. T2 - CCQM OAWG/PAWG Advances in qNMR Workshop CY - Sèvres, France DA - 08.04.2025 KW - NMR Spectroscopy KW - Process Analytical Technology KW - Deconvolution KW - Benchtop-NMR PY - 2025 AN - OPUS4-62956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Process Monitoring with Compact NMR spectroscopy: Applications from Lab to Field N2 - The use of compact NMR instruments based on permanent magnets has been increasing in recent years. Their affordability, portability, and ease of operation without the need for trained staff make them particularly interesting for quality control application in industrial production. Recent developments by instrument manufacturers, such as multi-nuclei options or extended interfacing, have made these systems even more versatile. However, the application of NMR spectroscopy as an online PAT tool remains rare, despite its significant potential for process optimization and control. A key challenge in exploiting this potential is the integration of lab instruments into the harsh environment of a chemical plant. Additionally, advancements in automation and data evaluation are key tasks to ensure robust, unattended operation with minimal maintenance requirements. In this presentation, we showcase examples of using NMR spectroscopy for process monitoring at the lab scale, the development of open-source software tools for NMR data evaluation (PyIHM, within the Python package KLASSEZ), and a successful example of field integration, running an automated laboratory instrument in the environment of a industrial production plant. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 31.03.2025 KW - Compact NMR spectroscopy KW - Process Monitoring KW - Downstream processing KW - Indirect Hard Modeling KW - Field integration PY - 2025 AN - OPUS4-62850 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Kombinierte Bestimmung von Wasserstoff in Gasgemischen mittels Raman- und NMR-Spektroskopie N2 - Vorgestellt wird die Nutzung von Online tauglichen Raman- und NMR-Spektrometern zur Quantifizierung des Wasserstoffmolanteils in gravimetrisch hergestellten Primärgasstandards unter Labor-Bedingungen. Es zeigte sich, dass Matrixeffekte insbesondere bei der Raman-Spektroskopie vernachlässigbar sind für die Quantifizierung von H2. Aufgrund der leichten Handhabbarkeit und der geringen Messunsicherheiten ergibt sich eine potenzielle Anwendung von Raman- und NMR-Spektroskopie unter Feldbedingungen als Online-Messeinheit im Bereich 5-100 cmol/mol Wasserstoff. T2 - 19. PAT Erfahrungsaustauschtreffen CY - Basel, Switzerland DA - 17.09.2024 KW - Raman KW - NMR KW - Wasserstoff PY - 2024 AN - OPUS4-62035 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhuang, Yiling A1 - Haderlein, Stefan B. A1 - Hagemann, Nikolas A1 - Grafmüller, Jannis A1 - Gogler, Karolin A1 - Paul, Andrea A1 - Fink, Friedrich A1 - Spahr, Stephanie T1 - Activation of persulfate by biochar and iron: role of biochar pyrolysis conditions and ash amendments N2 - Redox-active biochars can enhance contaminant transformation in persulfate-based Fenton-like water treatment by facilitating Fe(III) reduction to Fe(II). However, biochar properties vary greatly depending on both feedstock selection and pyrolysis conditions. Best suited biochars for Fe(III) reduction and persulfate activation have yet to be identified. Here, we investigated eight biochars for their ability to activate persulfate with Fe(III) to transform N,N-diethyl-m-toluamide (DEET) in water. Four of the biochars were produced from beech wood under different pyrolysis conditions (450–750 °C, high and low nitrogen flow rate in the reactor) and four biochars were produced from softwood amended with 0 – 43 weight percent (wt%) wood ash prior to pyrolysis at 500 °C. Beech wood biochar produced at 450 °C transformed DEET most efficiently with a half-life time of 39 ± 4 min, likely due to the high concentration of surface oxygen functional groups and persistent free radicals that accelerated Fe(III) reduction and formation of reactive species. Among the ash-amended biochars, biochar with 16 wt% ash amendment showed the most efficient DEET transformation with a half-life time of 27 ± 0.6 min, which is 10-times faster compared to a non-ash-amended biochar produced from the same biomass under similar pyrolysis conditions. Ash amendment led to the formation of crystalline iron minerals in biochars, which likely promoted Fe(III) reduction and persulfate activation. Our results highlight the potential for fine-tuning the redox properties of biochar, e.g., by ash amendment to a woody feedstock, enabling tailored performance for specific water treatment applications. KW - Persistent free radicals KW - Redox-active moieties KW - Fenton-like systems PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634504 DO - https://doi.org/10.1016/j.seppur.2025.133634 SN - 1383-5866 VL - 374 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-63450 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sowoidnich, Kay A1 - Pätzold, Stefan A1 - Ostermann, Markus A1 - Sumpf, Bernd A1 - Maiwald, Martin T1 - Qualitative and quantitative soil characterization on an agricultural field using a portable shifted excitation Raman difference spectroscopy instrument N2 - Site-specific farmland management requires comprehensive information about the soil status to derive informed treatment decisions, e.g. for liming or fertilizer recommendations. Standard laboratory methods relying on sample collection have only limited ability to adequately capture the spatial variability of typical agricultural fields. Here, on-site analytical techniques with the potential to measure the soil properties on a substance-specific level and at the required spatial resolution could be very beneficial. Raman spectroscopy is a very promising technique for this purpose as it provides a molecular fingerprint of soil constituents. However, intrinsic soil fluorescence and daylight interference can be major issues masking characteristic Raman signals. Here, we apply an in-house developed portable shifted excitation Raman difference spectroscopy (SERDS) instrument based on a dual-wavelength diode laser emitting around 785 nm to effectively separate the Raman signals of soil from such interferences. SERDS investigations on a selected agricultural field in Germany demonstrate that the Raman spectroscopic signature of 9 soil minerals and organic carbon could successfully be separated from intense backgrounds. Using partial least squares regression against reference analyses, a successful prediction of the soil carbonate (R2 = 0.86, root mean squared error of cross validation RMSECV = 2.49%) and soil organic carbon content (R2 = 0.89, RMSECV = 0.32%) as important soil parameters is realized. The results obtained on-site with the portable instrument were confirmed by SERDS laboratory experiments of collected soil samples thus highlighting the capability and reliability of portable SERDS as promising and complementary tool for precision agriculture KW - XRF KW - Raman spectroscopy KW - Soil KW - SERDS KW - Precision agriculture PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634597 DO - https://doi.org/10.1039/d5an00178a SN - 0003-2654 VL - 150 IS - 13 SP - 2934 EP - 2944 PB - Royal Society of Chemistry (RSC) AN - OPUS4-63459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Golub, Tino Petar A1 - Meyer, Klas A1 - Paul, Andrea A1 - Kipphardt, Heinrich A1 - Tuma, Dirk T1 - Exploring the potential of a setup for combined quantification of hydrogen in natural gas – Raman and NMR spectroscopy N2 - An accurate measurement of the amount fraction of hydrogen in gas mixtures is mandatory for practical applications, requiring methods that are fast, continuous, robust, and cost-effective. This study compares the performance of Raman and benchtop NMR process spectroscopy for determining the hydrogen amount fraction in gas mixtures. A setup was designed to integrate both techniques, enabling measurements of the same sample. Tests were conducted with gravimetrically prepared gas mixtures of reference quality ranging from 1.20 cmol/mol to 85.83 cmol/mol of hydrogen. The results demonstrate that Raman spectroscopy provides superior performance, with a minimal root mean square error (RMSE) of 0.22 cmol/mol and excellent linearity. In contrast, benchtop NMR spectroscopy faced challenges, such as overlapping peaks and longer measurement times, resulting in a higher RMSE of 0.71 cmol/mol. Raman spectroscopy proves to be particularly well-suited for practical applications due to its high accuracy and linearity. Meanwhile, benchtop NMR spectroscopy holds potential for future enhancements through ongoing technological advances, such as higher magnetic field strengths. In summary, the results from our study indicate that Raman spectroscopy is already a serviceable method for precise hydrogen quantification, whereas benchtop NMR spectroscopy can be attributed potential for future applications. KW - Hydrogen amount fraction KW - Raman spectroscopy KW - NMR spectroscopy KW - Field applicability PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610093 DO - https://doi.org/10.1016/j.saa.2024.125087 SN - 1386-1425 VL - 325 SP - 1 EP - 9 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-61009 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abad Andrade, Carlos Enrique A1 - Mimus, S. A1 - Recknagel, Sebastian A1 - Jakubowski, N. A1 - Panne, Ulrich A1 - Becker-Ross, H. A1 - Huang, M.-D. T1 - Determination of organic chlorine in water via AlCl derivatization and detection by high-resolution continuum source graphite furnace molecular absorption spectrometry N2 - High-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GF-MAS) was employed for determining adsorbable organic chlorine (AOCl) in water. Organic chlorine was indirectly quantified by monitoring the molecular absorption of the transient aluminum monochloride molecule (AlCl) around a wavelength of 261.42 nm in a graphite furnace. An aluminum solution was used as the molecularforming modifier. A zirconium coated graphite furnace, as well as Sr and Ag solutions were applied as modifiers for a maximal enhancement of the absorption signal. The pyrolysis and vaporization temperatures were 600 °C and 2300 °C, respectively. Non-spectral interferences were observed with F, Br, and I at concentrations higher than 6 mg L-1, 50 mg L-1, and 100 mg L-1, respectively. Calibration curves with NaCl, 4-chlorophenol, and trichlorophenol present the same slope and dynamic range, which indicates the chlorine atom specificity of the method. This method was evaluated and validated using synthetic water samples, following the current standard DIN EN ISO 9562:2004 for the determination of the sum parameter adsorbable organic halides (AOX) for water quality. These samples contain 4-chlorophenol as the chlorinated organic standard in an inorganic chloride matrix. Prior to analysis, organic chlorine was extracted from the inorganic matrix via solid-phase extraction with a recovery rate >95%. There were no statistically significant differences observed between measured and known values and for a t-test a confidence level of 95% was achieved. The limits of detection and characteristic mass were found to be 48 and 22 pg, respectively. The calibration curve was linear in the range 0.1–2.5 ng with a correlation coefficient R2 = 0.9986. KW - Chlorides KW - Chlorine KW - Graphite furnace KW - Spectrometry KW - Diatomic molecule KW - Water KW - AlCl PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-534426 DO - https://doi.org/10.1039/D1AY00430A SN - 1759-9660 VL - 13 IS - 33 SP - 3724 EP - 3730 PB - The Royal Society of Chemistry CY - London, UK AN - OPUS4-53442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bashiri, Termeh A1 - Yu, Phelan A1 - Hutzler, Nicholas R. A1 - Steimle, Timothy C. A1 - Abad Andrade, Carlos Enrique A1 - Okumura, Mitchio T1 - A Molecular Beam Spectroscopic Study of the A2Π − X2Σ + Band of CaF Isotopologues N2 - This study presents an experimental determination of spectroscopic parameters for the less-abundant isotopologues 42CaF and 44CaF, alongside 40CaF, by high resolution laser-induced fluorescence spectroscopy in a skimmed free jet expansion. We recorded spectra near the natural linewidth limit and derived spectroscopic constants for both 𝑋2𝛴+ and 𝐴2𝛱 states, including the fine and 19F magnetic hyperfine parameters. We also estimated the r(44Ca/40Ca) isotope amount ratio, demonstrating the potential use of optical spectroscopy for isotope analysis. KW - High-resolution spectroscopy KW - Molecular beam spectrometer KW - Isotope ratios KW - Isotopologues KW - Calcium KW - CaF KW - Calcium fluoride PY - 2025 DO - https://doi.org/10.1016/j.jms.2025.112023 SN - 1096-083X VL - 410 SP - 1 EP - 6 PB - Elsevier Inc. AN - OPUS4-63506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Prüf- und Messverfahren mit verschiedenen Sensortechnologien und Ultraschallwellen N2 - Der Vortrag zum Mess- und Prüfverfahren mit verschiedenen Sensortechnologien und Ultraschallwellen beinhaltet die Themen: Metrologie zur Wasserstoffspeicherung - Euramet-Vorhaben "MefHySto", Erkennung von freigesetztem Wasserstoff sowie die Bestimmung des Wasserstoff-Luftverhälntisses mit Gassensoren, zerstörungsfreie Fehlstellenerkennung mit integriertem Zustandsüberwachungssystem basierend auf geführten Ultraschallwellen zur Lebensdauerüberwachung von Composite-Behältern (Wasserstoffspeicher) sowie faseroptische Sensorik zur Schadenfrüherkennung von Wasserstoffspeichern aufgrund erkennbarer Dehnungsänderungen an Druckbehältern. T2 - DVGW Kongress H2 Sicherheit CY - Online meeting DA - 28.09.2021 KW - Leckdetektion KW - Metrologie zur Wasserstoffspeicherung KW - Gassensorik KW - Structural Health Monitoring (SHM) KW - Geführte Ultraschallwellen KW - Faseroptische Sensorik KW - Zerstörungsfreie Prüfung PY - 2021 AN - OPUS4-54136 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Versatility of nitrogen microwave-induced plasma mass spectrometry in elemental and isotopic analysis N2 - The introduction of Nitrogen-based Microwave Inductively Coupled Atmospheric-Pressure Plasma Mass Spectrometry (MICAP-MS) addresses the necessity for a plasma source that matches the capabilities of traditional argon-based Inductively Coupled Plasma Mass Spectrometry (ICP-MS) while exploiting the availability and cost-effectiveness of nitrogen gas. MICAP-MS uses nitrogen plasma, offering significant advantages such as reduced operational costs and eliminating specific isobaric interferences common in argon plasma systems [1]. This presentation explores the principles of MICAP-MS, highlighting its similarities to conventional ICP-MS in terms of analytical performance while emphasizing unique benefits like eliminating interferences from argon-based polyatomic species. MICAP-MS exhibits robust performance using nitrogen gas of varying purities—including ultra-high purity and industrial-grade nitrogen—without compromising analytical results [2]. We have applied MICAP-MS for multielement analysis in soil samples, serving as a proof of concept for environmental monitoring applications. The technique achieved figures of merit comparable to traditional ICP-MS, even when analyzing real-world samples with complex matrices [2]. MICAP-MS demonstrated high tolerance to high-concentration matrices, maintaining accuracy and precision without extensive sample preparation or matrix separation [3]. In clinical diagnostics, MICAP-MS was employed for the precise and traceable quantification of calcium, iron, and selenium in human serum using isotope dilution analysis [4]. These elements often face interferences in argon-based ICP-MS due to argon-associated isobaric interferences (40Ca+, 56Fe+, and 80Se+); however, MICAP-MS effectively overcomes these challenges, providing traceable and accurate determinations. The stability of the microwave plasma in MICAP-MS facilitates precise isotopic analysis. This capability investigated age-induced lithium isotope fractionation in lithium-ion batteries, offering critical insights into battery aging mechanisms and performance degradation [5]. MICAP-MS is a versatile analytical tool that combines the operational benefits of nitrogen plasma with the strengths of traditional ICP-MS. Its ability to handle complex matrices, reduce interferences, and perform precise elemental and isotopic analyses across various applications makes it a valuable instrument. T2 - European Winter Conference on Plasma Spectrochemistry CY - Berlin, Germany DA - 02.03.2025 KW - MICAP-MS KW - Nitrogen plasma KW - Isotope dilution analysis KW - Matrix tolerance KW - Argon interference elimination KW - Trace analysis PY - 2025 AN - OPUS4-63485 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Maiwald, Michael A1 - Schukar, Marcus T1 - Beiträge der Prozessanalytik und Sensorik zur Sicherheit in Wasserstofftechnologien N2 - Intelligent sensor systems, certified reference materials and instrumental analytical-chemical methods contribute to safety and functionality in hydrogen technologies. This article gives a brief overview of SensRef activities in the Competence Centre H2Safety@BAM on the issues: Analytical methods for the determination of hydrogen purity, certified reference materials as measurement standards with regard to gas quality (primary calibrators) of BAM, test methods for gas sensor systems to detect hydrogen in air as well as the application of fibre-optic sensor systems to monitor the expansion and ageing behaviour of composite containers in hydrogen technologies. T2 - Berlin Brandenburger Optik-Tag "Einsatz von Sensorik und Mikroelektronik in der Wasserstoffwirtschaft" CY - Online meeting DA - 29.11.2021 KW - H2Safety@BAM KW - SensRef KW - Gas analysis KW - Gas purity KW - Fibre-optic sensors KW - Sensor response KW - Certified reference materials PY - 2021 AN - OPUS4-54138 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Erler, A. A1 - Riebe, D. A1 - Beitz, T. A1 - Löhmannsröben, H.-G. A1 - Leenen, M. A1 - Pätzold, S. A1 - Ostermann, Markus A1 - Wójcik, M. T1 - Mobile Laser-Induced Breakdown Spectroscopy for Future Application in Precision Agriculture—A Case Study N2 - In precision agriculture, the estimation of soil parameters via sensors and the creation of nutrient maps are a prerequisite for farmers to take targeted measures such as spatially resolved fertilization. In this work, 68 soil samples uniformly distributed over a field near Bonn are investigated using laser-induced breakdown spectroscopy (LIBS). These investigations include the determination of the total contents of macro- and micronutrients as well as further soil parameters such as soil pH, soil organic matter (SOM) content, and soil texture. The applied LIBS instruments are a handheld and a platform spectrometer, which potentially allows for the single-point measurement and scanning of whole fields, respectively. Their results are compared with a high-resolution lab spectrometer. The prediction of soil parameters was based on multivariate methods. Different feature selection methods and regression methods like PLS, PCR, SVM, Lasso, and Gaussian processes were tested and compared. While good predictions were obtained for Ca, Mg, P, Mn, Cu, and silt content, excellent predictions were obtained for K, Fe, and clay content. The comparison of the three different spectrometers showed that although the lab spectrometer gives the best results, measurements with both field spectrometers also yield good results. This allows for a method transfer to the in-field measurements KW - LIBS KW - Precision agriculture KW - Soil KW - Multivariate methods KW - Feature selection PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580777 DO - https://doi.org/10.3390/s23167178 VL - 23 IS - 16 SP - 1 EP - 17 PB - MDPI AG CY - Basel, Schweiz AN - OPUS4-58077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wander, Lukas A1 - Lommel, Lukas A1 - Meyer, Klas A1 - Braun, Ulrike A1 - Paul, Andrea T1 - Development of a low-cost method for quantifying microplastics in soils and compost using near-infrared spectroscopy N2 - Near-infrared (NIR) spectroscopy is a promising candidate for low-cost, nondestructive, and high-throughput mass quantification of micro¬plastics in environmental samples. Widespread application of the technique is currently hampered mainly by the low sensitivity of NIR spectroscopy compared to thermo-analytical approaches commonly used for this type of analysis. This study shows how the application of NIR spectroscopy for mass quantification of microplastics can be extended to smaller analyte levels by combining it with a simple and rapid microplastic enrichment protocol. For this purpose, the widely used flotation of microplastics in a NaCl solution, accelerated by centrifugation, was chosen which allowed to remove up to 99 % of the matrix at recovery rates of 83–104 %. The spectroscopic measurements took place directly on the stainless-steel filters used to collect the extracted particles to reduce sample handling to a minimum. Partial least squares regression (PLSR) models were used to identify and quantify the extracted microplastics in the mass range of 1–10 mg. The simple and fast extraction procedure was systematically optimized to meet the requirements for the quantification of microplastics from common PE-, PP-, and PS-based packaging materials with a particle size < 1 mm found in compost or soils with high natural organic matter content (> 10 % determined by loss on ignition). Microplastics could be detected in model samples at a mass fraction of 1 mg g-1. The detectable microplastic mass fraction is about an order of magnitude lower compared to previous studies using NIR spectroscopy without additional enrichment. To emphasize the cost-effectiveness of the method, it was implemented using some of the cheapest and most compact NIR spectrometers available. KW - NIR KW - Soil KW - compost KW - PLSR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546405 DO - https://doi.org/10.1088/1361-6501/ac5e5f SN - 0957-0233 VL - 33 IS - 7 SP - 075801 EP - 075814 PB - IOP Publishing Ltd. CY - UK AN - OPUS4-54640 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wander, Lukas A1 - Lommel, Lukas A1 - Braun, Ulrike A1 - Meyer, Klas A1 - Paul, Andrea T1 - Development of a Low-Cost Method for Quantifying Microplastics in Soils and Compost Using Near-Infrared Spectroscopy N2 - Near-infrared (NIR) spectroscopy is a promising candidate for low-cost, nondestructive, and highthroughput mass quantification of microplastics in environmental samples. Widespread application of the technique is currently hampered mainly by the low sensitivity of NIR spectroscopy compared to thermoanalytical approaches commonly used for this type of analysis. This study shows how the application of NIR spectroscopy for mass quantification of microplastics can be extended to smaller analyte levels by combining it with a simple and rapid microplastic enrichment protocol. For this purpose, the widely used flotation of microplastics in a NaCl solution, accelerated by centrifugation, was chosen which allowed to remove up to 99 % of the matrix at recovery rates of 83–104 %. The spectroscopic measurements took place directly on the stainless-steel filters used to collect the extracted particles to reduce sample handling to a minimum. Partial least squares regression (PLSR) models were used to identify and quantify the extracted microplastics in the mass range of 1–10 mg. The simple and fast extraction procedure was systematically optimized to meet the requirements for the quantification of microplastics from common PE-, PP-, and PS-based packaging materials with a particle size < 1 mm found in compost or soils with high natural organic matter content (> 10 % determined by loss on ignition). Microplastics could be detected in model samples at a mass fraction of 1 mg g-1. The detectable microplastic mass fraction is about an order of magnitude lower compared to previous studies using NIR spectroscopy without additional enrichment. To emphasize the cost-effectiveness of the method, it was implemented using some of the cheapest and most compact NIR spectrometers available. KW - Mikroplastik KW - NIR KW - Sensor KW - Kompost KW - Multivariat PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552605 DO - https://doi.org/10.1088/1361-6501/ac5e5f VL - 33 IS - 7 SP - 1 EP - 13 PB - IOP Publishing Ltd. CY - Bristol AN - OPUS4-55260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winckelmann, Alexander A1 - Roik, Janina A1 - Recknagel, Sebastian A1 - Abad Andrade, Carlos Enrique A1 - You, Zengchao T1 - Investigation of matrix effects in nitrogen microwave inductively coupled atmospheric-pressure plasma mass spectrometry (MICAP-MS) for trace element analysis in steels N2 - We investigated the performance of nitrogen microwave inductively coupled atmospheric-pressure plasma mass spectrometry (MICAP-MS) under matrix effects and its applicability to trace element analysis in steels. Influences of different gas flows and ion optics on the matrix tolerance are studied, indicating that nebulizer gas flow has the most significant impact. Optimization of ion optics improves matrix tolerance for light elements due to the reduction of the inelastic collisional scattering effect. With optimized operating conditions, MICAP-MS achieves an internal standard intensity recovery of over 90% at an Fe concentration of 500 mg L−1. Even at an Fe concentration of 1 g L−1, the recovery remains above 80%. Three certified reference materials – non-alloy, low-alloy and high-alloy steel – were analyzed using MICAP-MS. The determined mass concentrations of the trace and minor components show metrological compatibility to the reference values. No significant differences are observed between the results obtained with aqueous and matrix-matched calibration, demonstrating the strong matrix tolerance of MICAP-MS, and its promising applicability to steel analysis. KW - MICAP-MS KW - Trace Analysis KW - Steel PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576323 DO - https://doi.org/10.1039/d3ja00088e SN - 0267-9477 VL - 38 IS - 6 SP - 1253 EP - 1260 PB - Royal Society of Chemistry AN - OPUS4-57632 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Metrologie für fortschrittliche Wasserstoffspeicherlösungen – Das EU-Projekt MefHySto T1 - Metrology for advanced hydrogen storage solutions – The EU project MefHySto N2 - Das europäische Projekt MefHySto befasst sich mit dem Bedarf an großmaßstäblichen Energiespeichern, die für eine Umstellung der Energieversorgung auf erneuerbare Energien erforderlich sind. Eine solche Speicherung ist entscheidend, um Energie zu Spitzenzeiten zu liefern, wenn die erneuerbaren Energiequellen schwanken. Eine mögliche Lösung für die Energiespeicherung ist der großtechnische Einsatz von Wasserstoff. Die messtechnische Rückführbarkeit in der Energieinfrastruktur für die Wasserstoffspeicherung ist dann von entscheidender Bedeutung und eine bessere Kenntnis der chemischen und physikalischen Eigenschaften von Wasserstoff sowie rückführbare Messungen und validierte Techniken unverzichtbar. N2 - The European project MefHySto addresses the need of large-scale energy storage, which is required for a shift to renewable energy supply. Such storage is mandatory to supply energy at peak times when renewable sources fluctuate. A possible solution for energy storage is large-scale use of hydrogen. Metrological traceability in the energy infrastructure for hydrogen storage is then crucial and a better knowledge of the chemical and physical properties of hydrogen as well as traceable measurements and validated techniques are indispensable. KW - Wasserstoff KW - Wasserstoffspeicher KW - Infrastruktur KW - Metrologie KW - PEM-Wasserelektrolyse KW - Rückverstromung KW - Lastwechsel KW - Wasserstoff-Qualität PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-556451 UR - https://gwf-gas.de/forschung-entwicklung/metrologie-fuer-fortschrittliche-wasserstoffspeicherloesungen-das-eu-projekt-mefhysto/ SN - 2366-9594 VL - 163 IS - 9 SP - 38 EP - 45 PB - Vulkan Verlag CY - Essen AN - OPUS4-55645 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bornemann-Pfeiffer, Martin A1 - Meyer, Klas A1 - Lademann, J. A1 - Kraume, M. A1 - Maiwald, Michael T1 - Contributions towards variable temperature shielding for compact NMR instruments N2 - The application of compact NMR instruments to hot flowing samples or exothermically reacting mixtures is limited by the temperature sensitivity of permanent magnets. Typically, such temperature effects directly influence the achievable magnetic field homogeneity and hence measurement quality. The internal-temperature control loop of the magnet and instruments is not designed for such temperature compensation. Passive insulation is restricted by the small dimensions within the magnet borehole. Here, we present a design approach for active heat shielding with the aim of variable temperature control of NMR samples for benchtop NMR instruments using a compressed airstream which is variable in flow and temperature. Based on the system identification and surface temperature measurements through thermography, a model predictive control was set up to minimise any disturbance effect on the permanent magnet from the probe or sample temperature. This methodology will facilitate the application of variable-temperature shielding and, therefore, extend the application of compact NMR instruments to flowing sample temperatures that differ from the magnet temperature. KW - Benchtop NMR KW - Continuous Processes KW - Inline Analytics KW - Model Predictive Control KW - Process Analytical Tecnology KW - Temperature Control PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579219 DO - https://doi.org/10.1002/mrc.5379 SN - 1097-458X SP - 1 EP - 10 PB - John Wiley & Sons Ltd. AN - OPUS4-57921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Büchele, Dominique T1 - Entwicklung einer robusten Online-Methode zur Bestimmung von Nährelementen in Ackerböden mit einem Energie-dispersiven RFA-Sensor N2 - Im Rahmen der vom Bundesministerium für Bildung und -forschung geförderten Forschungsinitiative „BonaRes – Boden als nachhaltige Ressource der Bioökonomie“ soll sich das Teilprojekt „I4S – integrated system for site-specific soil fertility management“ der Entwicklung eines integrierten Systems zum ortsspezifischen Management der Bodenfruchtbarkeit widmen. Hierfür ist eine Messplattform zur Bestimmung relevanter Bodeneigenschaften und der quantitativen Analyse ausgewählter Makro- und Mikronährstoffe geplant. In der ersten Phase dieses Projekts liegt das Hauptaugenmerk auf der Kalibrierung und Validierung der verschiedenen Sensoren auf die Matrix Boden, der Probennahme auf dem Acker und der Planung sowie dem Aufbau der Messplattform. Auf dieser Plattform sollen in der zweiten Phase des Projektes die verschiedenen Bodensensoren installiert, sowie Modelle und Entscheidungsalgorithmen zur Steuerung der Düngung und dementsprechend Verbesserung der Bodenfunktionen erstellt werden. Ziel der vorliegenden Arbeit ist die Grundlagenuntersuchung und Entwicklung einer robusten Online-Analyse mittels Energie-dispersiver Röntgenfluoreszenzspektroskopie (EDRFA) zur Quantifizierung ausgewählter Makro- und Mikronährstoffe in Böden für eine kostengünstige und flächendeckende Kartierung von Ackerflächen. Für die Entwicklung eines Online-Verfahrens wurde ein dem Stand der Technik entsprechender Röntgenfluoreszenzmesskopf in Betrieb genommen und die dazugehörigen Geräteparameter auf die Matrix Boden optimiert. Die Bestimmung der analytischen Qualitäts-merkmale wie Präzision und Nachweisgrenzen fand für eine Auswahl an Nährelementen von Aluminium bis Zink statt. Um eine möglichst Matrix-angepasste Kalibrierung zu erhalten, wurde sowohl mit zertifizierten Referenzmaterialien (CRM), als auch mit Ackerböden kalibriert. Da einer der größten Nachteile der Röntgenfluoreszenzanalyse die Beeinflussung durch Matrixeffekte ist, wurde neben der klassischen univariaten Datenauswertung auch die chemometrische multivariate Methode der Partial Least Squares Regression (PLSR) eingesetzt. Die PLSR bietet dabei den Vorteil, Matrixeffekte auszugleichen, wodurch robustere Kalibriermodelle erhalten werden können. Zusätzlich wurde eine Hauptkomponentenanalyse (PCA) durchgeführt, um Gemeinsamkeiten und Ausreißer innerhalb des Probensets zu identifizieren. Es zeigte sich, dass eine Klassifizierung der Böden anhand ihrer Textur Sand, Schluff, Lehm und Ton möglich ist. Aufbauend auf den Ergebnissen idealer Bodenproben (zu Tabletten gepresste luftgetrocknete Proben mit Korngrößen < 0,5 mm) wurde im Verlauf dieser Arbeit die Probenvorbereitung immer weiter reduziert und der Einfluss verschiedener Kenngrößen untersucht. Diese Einflussfaktoren können die Dichte und die Homogenität der Probe, sowie Korngrößeneffekte und die Feuchtigkeit sein. Anhand des RMSE (Wurzel der mittleren Fehlerquadratsumme) und unter Berücksichtigung der Residuen werden die jeweils erstellten Kalibriermodelle miteinander verglichen. Um die Güte der Modelle zu bewerten, wurden diese mit einem Testset validiert. Hierfür standen 662 Bodenproben von 15 verschiedenen Standorten in Deutschland zur Verfügung. Da die Ergebnisse an gepressten Tabletten für die Elemente Al, Si, K, Ca, Ti, Mn, Fe und Zn den Anforderungen für eine spätere Online-Analyse entsprechen, wurden im weiteren Verlauf dieser Arbeit Kalibriermodelle mit losen Bodenproben erstellt. Auch hier konnten gute Ergebnisse durch ausreichende Nachweisgrenzen und eine niedrige gemittelte Messabweichung bei der Vorhersage unbekannter Testproben erzielt werden. Es zeigte sich, dass die Vorhersagefähigkeit mit der multivariaten PLSR besser ist als mit der univariaten Datenauswertung, insbesondere für die Elemente Mn und Zn. Der untersuchte Einfluss der Feuchtigkeit und der Korngrößen auf die Quantifizierung der Elementgehalte war vor allem bei leichteren Elementen deutlich zu sehen. Es konnte schließlich eine multivariate Kalibrierung unter Berücksichtigung dieser Faktoren für die Elemente Al bis Zn erstellt werden, so dass ein Einsatz an Böden auf dem Acker möglich sein sollte. Eine höhere Messunsicherheit muss dabei einkalkuliert werden. Für eine spätere Probennahme auf dem Feld wurde zudem der Unterschied zwischen statischen und dynamischen Messungen betrachtet, wobei sich zeigte, dass beide Varianten genutzt werden können. Zum Abschluss wurde der hier eingesetzte Sensor mit einem kommerziell erhältlichen Hand-Gerät auf sein Quantifizierungspotential hin verglichen. Der Sensor weist anhand seiner Ergebnisse ein großes Potential als Online-Sensor für die Messplattform auf. Die Ergebnisse unter Laborbedingungen zeigen, dass eine robuste Analyse Ackerböden unter Berücksichtigung der Einflussfaktoren möglich ist. KW - Boden KW - Chemometrie KW - ICP-OES KW - Nährelemente KW - PLS-R KW - Röntgenfluoreszenz KW - Prozessanalytik PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:517-opus4-483735 DO - https://doi.org/https://doi.org/10.25932/publishup-48373 SP - 1 EP - 106 PB - Universität Potsdam CY - Potsdam AN - OPUS4-52182 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Musyanovych, A. A1 - Grimmer, Christoph A1 - Sadak, A. E. A1 - Heßling, L. A1 - Lüdicke, M. A1 - Bilsel, M. A1 - Horn, Wolfgang A1 - Richter, Matthias T1 - Polymer Capsules with Volatile Organic Compounds as Reference Materials for Controlled Emission N2 - Encapsulation of volatile organic compounds (VOCs) that could evaporate at a defined rate is of immense interest for application in emission reference materials (ERMs). Polyurethane/polyurea microcapsules with various VOC active ingredients (limonene, pinene, and toluene) were successfully produced by interfacial polymerization with Shirasu porous glass membrane emulsification in a size range between 10 and 50 μm. The effect of surfactant, VOC, monomer(s) type, and ratio has a great effect on the formulation process and morphology of capsules. The type of VOC played a significant role in the encapsulation efficiency. Due to the difference in vapor pressure and VOC/water interfacial tension, the formulation for encapsulation was optimized for each individual VOC. Furthermore, to achieve effective stability of the large droplets/capsules, a combination of ionic and nonionic surfactants was used. Optical and scanning electron microscopy, Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA), were used to characterize the optimized microcapsules. The results showed that the obtained microcapsules exhibited a spherical shape and core–shell morphology and featured characteristic urethane-urea bonds. The amount of encapsulated VOC ranges between 54 and 7 wt %. The emission tests were performed with the help of the emission test chamber procedure (EN 16516). The limonene-loaded polyurethane/polyurea microcapsules show a change in emission rate of less than 10% within 14 days and can be considered as a potential candidate for use as an ERM. KW - Polymer microcapsules KW - Membrane emulsification KW - Polyaddition KW - Volatile organic compound (VOC) KW - Emission testing PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-619227 DO - https://doi.org/10.1021/acsami.4c12826 SN - 1944-8252 VL - 16 IS - 50 SP - 69999 EP - 70009 PB - ACS AN - OPUS4-61922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grimmer, Christoph A1 - Richter, Matthias A1 - Neuhaus, T. A1 - Prinz, Carsten A1 - Strzelczyk, Rebecca Skadi A1 - Colakoglu, Irem A1 - Horn, Wolfgang T1 - Towards a multi-VOC emission reference material with temporally constant emission profile for QA/QC of materials emission testing procedures N2 - Emission reference materials (ERMs) are sought after to further control and improve indoor air quality. The impregnation of porous materials with volatile organic compounds (VOCs) is a promising approach to produce ERMs. Different VOCs were used to impregnate various porous materials (mainly zeolites, activated carbons and a metal organic framework). The influence of different methodological parameters and material properties were studied to optimize the impregnation procedure and to find the best material/VOC combination. The impregnation procedure remains quite irreproducible, nevertheless, very good ERM candidates were identified. Two materials (zeolite 4 and AC 1 impregnated with n-hexadecane) showed a very stable emission over 14 days (<10 % change). Another material (AC 1 impregnated with toluene) showed a declining emission profile but with a very good in-batch reproducibility and a storage stability of up to 12 months. KW - Emission reference material KW - Porous materials KW - Indoor air quality KW - Emission test chamber KW - CO2 assisted impregnation KW - EN 16516 PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-612238 DO - https://doi.org/10.1016/j.chemosphere.2024.143437 SN - 1879-1298 VL - 366 SP - 1 EP - 8 PB - Elsevier AN - OPUS4-61223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thiele, Isabel A1 - Weiske, Björn A1 - Riedel, Sebastian L. A1 - Meyer, Klas T1 - On-line monitoring of polyhydroxyalkanoate extraction by low-field nuclear magnetic resonance spectroscopy N2 - The use of low-field nuclear magnetic resonance (NMR) spectroscopy enables real-time reaction monitoring in contrast to time-consuming gas chromatography or off-line high-field NMR measurements. In this study, NMR spectroscopy is demonstrated as a novel process analytical technology (PAT) tool in the downstream processing of polyhydroxyalkanoate (PHA) biopolymers. On-line NMR spectroscopy measurements were performed using a Spinsolve 43 Carbon Ultra instrument in a fully automated mode with a flow-assembly based on PTFE tubing. Single-scan NMR spectra were acquired for real-time monitoring of the extraction process of the PHA copolymer poly(hydroxybutyrate-co-hydroxyhexanoate) with 13.5 mol.% hydroxyhexanoate [P(HB-co-13.5 mol.%HHx)] from Ralstonia eutropha biomass using chloroform or acetone as PHA solvents at lyophilized cell loadings of 20–120 g L􀀀 1. The reproducibility and reliability of low-field NMR spectroscopy was comparable to high-field NMR spectroscopy, with superior performance in terms of time. The correlation between the results of on-line monitoring using low-field NMR spectroscopy and off-line analysis using gas chromatography (GC) showed a correlation coefficient of >94 %. The versatility of low-field NMR spectroscopy for elucidating reaction kinetics, facilitating endpoint determination and accelerating extraction processes by maximizing solubility is highlighted as plateau values were reached within 6–10 min for chloroform and acetone, respectively. This novel low-field NMR spectroscopy application promotes a new monitoring approach for downstream PHA processing and supports process development and optimization. KW - Polyhydroxyalkanoate KW - Extraction KW - NMR KW - Ralstonia eutropha KW - Downstream processing PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624215 DO - https://doi.org/10.1016/j.polymdegradstab.2025.111188 SN - 1873-2321 VL - 233 SP - 1 EP - 10 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-62421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Krom, I. A1 - Heikens, D. A1 - Horn, Wolfgang A1 - Wilke, Olaf A1 - Richter, Matthias A1 - Baldan, A. T1 - Metrological generation of SI-traceable gas-phase standards and reference materials for (semi-) volatile organic compounds N2 - EN 16516 sets specifications for the determination of emissions into indoor air from construction products. Reliable, accurate and International System of Unit (SI)-traceable measurement results of the emissions are the key to consumer protection. Such measurement results can be obtained by using metrologically traceable reference materials. Gas-phase standards of volatile organic compounds (VOCs) in air can be prepared by a variety of dynamic methods according to the ISO 6145 series. However, these methods are not always applicable for semi-VOCs (SVOCs) due to their high boiling point and low vapour pressure. Therefore, a novel dynamic gas mixture generation system has been developed. With this system gas-phase standards with trace level VOCs and SVOCs in air can be prepared between 10 nmol mol−1 and 1000 nmol mol−1. The VOCs and SVOCs in this study have normal boiling points ranging from 146 °C to 343 °C. Metrologically traceable reference materials of the gas-phase standard were obtained by sampling of the VOC gas-phase standard into Tenax TA® sorbent material in SilcoNert® coated stainless steel tubes. Accurately known masses between 10 ng and 1000 ng per VOC were sampled. These reference materials were used to validate the dynamic system. Furthermore, the storage and stability periods of the VOCs in the reference materials were determined as these are crucial characteristics to obtain accurate and SI-traceable reference materials. In a round robin test (RRT), the reference materials were used with the aim of demonstrating the feasibility of providing SI-traceable standard reference values for SVOCs for interlaboratory comparison purposes. Based on the results from the validation, the storage and stability studies and the RRT, gas-phase standards and reference materials of VOCs and SVOCs with relative expanded uncertainties between 5% and 12% (k = 2) have been developed. These reference standards can be used as calibrants, reference materials or quality control materials for the analysis of VOC emissions. KW - SVOC KW - Dynamic calibration gas mixtures KW - Reference materials KW - Indoor air KW - Thermal desorption PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-565978 DO - https://doi.org/10.1088/1361-6501/aca704 VL - 34 IS - 3 SP - 1 EP - 13 PB - IOP Publishing AN - OPUS4-56597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Kern, Simon T1 - Prozessüberwachung mittels Niederfeld-NMR-Spektroskopie als Online-Methode N2 - Die Geräteentwicklungen im Bereich der Niederfeld-NMR-Spektroskopie im vergangenen Jahrzehnt ermöglichen den Einsatz kompakter, portabler Magnete mit geringen Streufeldern in Laborumgebungen und industriellen Produktionsanlagen. Somit werden neue Möglichkeiten für hochauflösende NMR-Experimente zur Reaktionsüberwachung eröffnet. Im Rahmen des EU-Projekts CONSENS wurden die Möglichkeiten dieser Methode umfassend anhand einer technisch bedeutenden Reaktion (elektrophile aromatische Substitutionsreaktionen) evaluiert. Um die Flexibilität einer kontinuierlichen und modularen Pilotanlage durch Echtzeit- Qualitätskontrolle zu fördern, wurde ein vollständig automatisiertes Online- NMR-Modul entwickelt. Der Einsatz eines kommerziellen Niederfeld-NMR-Geräts im industriellen Umfeld wurde durch die entwickelten Lösungen der automatisierten Datenanlyse sowie durch ein zertifiziertes Sicherheitskonzept für den Betrieb in explosionsgefährdeten Zonen ermöglicht. Neben der Überwachung der Produktqualität wurden Online-NMR-Daten in einem neuen iterativen Optimierungsansatz zur Maximierung des Anlagenertrags eingesetzt und dienten als zuverlässige Referenz für die Kalibrierung eines Nahinfrarot-Spektrometers. Für die Entwicklung einer robusten Datenauswertung der NMR-Spektren, die dem Anspruch der Flexibilität bei Produktwechseln genügt, wurden zunächst Versuche im Labormaßstab durchgeführt, um eine Datenbasis zu schaffen. In diesen Versuchen wurden die aromatischen Amine Anilin, p-Toluidin und p-Fluoranilin mit o-Fluornitrobenzol gekoppelt. Durch Zugabe einer Organolithium-Verbindung (Li- HMDS) findet ein Protonenaustausch zwischen dem primären Amin und Li-HMDS statt. Dies führt zu einer hohen Reaktionsenthalpie und instabilen Aryllithium-Verbindungen. Die Reaktionen wurden hinsichtlich anfallender Zwischenprodukte mittels Hochfeld-NMR-Spektroskopie analysiert. Nachfolgend wurden die Reaktionen sowohl im Semi-Batch-Verfahren als auch im kontinuierlichen Laborbetrieb mit Online-Niederfeld-NMR-Spektroskopie und Online- Hochfeld-NMR-Spektroskopie untersucht. Da die gemessenen NMR-Spektren besonders im aromatischen Spektralbereich hohe Signalüberlappungen der Reaktanden aufweisen, wurden chemometrische Modelle entwickelt und anhand der Hochfeld-NMR-Methode validiert. Die verwendeten Durchflusszellen für die Niederfeld-NMR-Spektroskopie wurden hinsichtlich ihrer Anwendbarkeit für quantitative Messungen im kontinuierlichen Durchfluss untersucht. Es konnte gezeigt werden, dass Messungen mit einer additiv gefertigten Keramikdurchflusszelle prinzipiell möglich sind. KW - NMR-Spektroskopie KW - Niederfeld-NMR-Spektroskopie KW - Prozessanalytik KW - Industrie 4.0 KW - Indirect Hard Modeling KW - CONSENS PY - 2019 UR - https://nbn-resolving.org/10.14279/depositonce-9404 DO - https://doi.org/10.14279/depositonce-9404 SP - 1 EP - 112 CY - Berlin AN - OPUS4-50196 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Algernon, Daniel T1 - Impact echo data analysis based on duration and bandwidth of signal components N2 - Impact echo (IE) is successfully applied for the nondestructive evaluation of concrete structures. Its principle is based on the use of longitudinal waves generated by the elastic impact of a steel sphere. However, this impact creates other wave types such as Rayleigh and shear waves. Especially when IE is applied on structures with compact dimensions, the effects of these waves become crucial. The separation of the different signal components and the definition of effective criteria to distinguish between them are therefore highly relevant. In this study, the duration and attenuation of the different signal components are explained and used to distinguish between the actual measurement information and interfering effects caused by reflections at the boundaries. An explanation is offered for why the different components of an IE signal have different characteristics in regard to their duration over time. Furthermore, a procedure is introduced that makes use of the relation between the signal duration in the time domain and the bandwidth in the frequency domain. It therefore avoids the application of a rather complex time– frequency analysis. This characteristic is demonstrated on simple sinusoidal signals in a first step and then applied to data collected from IE measurements. Because of the low computation effort and the fact that only few input parameters have to be chosen, this method is also applicable to whole scan lines composed of a large number of measurement points and the imaging of the results. KW - Impact echo KW - Data analysis KW - Signal component PY - 2008 DO - https://doi.org/10.3141/2050-13 SN - 0361-1981 VL - 2050 IS - 1 SP - 127 EP - 133 PB - Sage Publishing CY - Thousand Oaks, CA AN - OPUS4-64012 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - "Ultima Ratio": Multi-scale, high-resolution 3D-FFT scattering pattern simulations N2 - This talk highlights a proof-of-concept that demonstrates the ability to calculate high-resolution Fourier transforms. These can be combined with multi-scale modeling to simulate scattering over a wide range, from small-angle scattering to XRD and PDF. T2 - Shapespyer/MuSSIC Launch Workshop CY - Didcot, UK DA - 20.02.2023 KW - X-ray scattering KW - Simulation KW - Fourier Transform KW - 3D KW - High resolution KW - Multi-scale PY - 2023 AN - OPUS4-57031 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Laskina, Sofya A1 - Naik, Aakash A1 - Smales, Glen Jacob A1 - George, Janine A1 - Breßler, Ingo A1 - Benner, Philipp T1 - Jupyter notebook and VASP calculation details accompanying the manuscript: "Ultima Ratio: Simulating wide-range X-ray scattering and diffraction" N2 - Summary: This notebook and associated datasets (including VASP details) accompany a manuscript available on the ArXiv (https://doi.org/10.48550/arXiv.2303.13435) and hopefully soon in a journal as short communication as well. Most of the details needed to understand this notebook are explained in that paper with the same title as above. For convenience, the abstract is repeated here: Paper abstract: We demonstrate a strategy for simulating wide-range X-ray scattering patterns, which spans the small- and wide scattering angles as well as the scattering angles typically used for Pair Distribution Function (PDF) analysis. Such simulated patterns can be used to test holistic analysis models, and, since the diffraction intensity is presented coupled to the scattering intensity, may offer a novel pathway for determining the degree of crystallinity. The "Ultima Ratio" strategy is demonstrated on a 64-nm Metal Organic Framework (MOF) particle, calculated from $Q<0.01$\,$\mathrm{nm}^{-1}$ up to $Q\approx150$\,$\mathrm{nm}^{-1}$, with a resolution of 0.16\,\AA. The computations exploit a modified 3D Fast Fourier Transform (3D-FFT), whose modifications enable the transformations of matrices at least up to $8000^3$ voxels in size. Multiple of these modified 3D-FFTs are combined to improve the low-$Q$ behaviour. The resulting curve is compared to a wide-range scattering pattern measured on a polydisperse MOF powder. While computationally intensive, the approach is expected to be useful for simulating scattering from a wide range of realistic, complex structures, from (poly-)crystalline particles to hierarchical, multicomponent structures such as viruses and catalysts. KW - X-ray KW - Simulation KW - Scattering KW - MOUSE KW - Nanomaterials KW - XRD KW - SAXS KW - PDF KW - Total scattering KW - 3D Fourier transform KW - High resolution KW - FFT PY - 2023 DO - https://doi.org/10.5281/zenodo.7764044 PB - Zenodo CY - Geneva AN - OPUS4-57207 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, Hans R. A1 - Weidner, Steffen M. T1 - Polymerization of l‐Lactide Catalyzed by Metal Acetylacetonate Complexes N2 - ABSTRACTRing‐opening polymerizations (ROPs) of l‐lactide (LA) were performed at 120°C, 140°C, 150°C, and 180°C in bulk catalyzed by acetylacetonate (acac) complexes of manganese(II), nickel(II), copper(II), zirconium(IV), dibutyltin(IV), and vanadyl(V). These experiments revealed that only the acac complexes of Zr and Bu2Sn were reactive enough to enable quantitative polymerization within a few hours. Further ROPs with Bu2Sn(acac)2 and Zr(acac)4 showed that Bu2Sn(acac)2 had a slightly lower reactivity than the Zr complex. The ROPs catalyzed with Zr(acac)4 yielded number average molecular weights (Mn) up to 70,000 g mol−1. The matrix‐assisted laser desorption/ionization time‐of‐flight (MALDI‐TOF) mass spectra indicated an exclusive formation of cycles in the mass range of up to m/z 13,000 for Zr(acac)4 and up to m/z 18,000 for Bu2Sn(acac)2. Unusually high melting temperatures (187°C–192°C) were also achieved along with high crystallinities. Furthermore, four lactide/glycolide copolymerizations catalyzed by Zr(acac)4 were performed, and the topology and the extent of transesterification were characterized by MALDI‐TOF mass spectrometry and 13C NMR spectroscopy. KW - MALDI-TOF MS KW - Polycondensation KW - Acetylacetonate PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639754 DO - https://doi.org/10.1002/pol.20250788 SN - 2642-4150 SP - 1 EP - 9 PB - Wiley Periodicals LLC. AN - OPUS4-63975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Winkler, Nicolas P. A1 - Nerger, Tino A1 - Lohrke, Heiko A1 - Stanisavljevi, Mila T1 - DLR Research Seminar - ARO Lab@BAM – Current Research Topics N2 - This seminar presents the key research activities of ARO Lab@BAM, focusing on five main areas: • Learning-based Gas Distribution Mapping utilizes machine learning to accurately model and predict spatial gas concentrations, enhancing environmental monitoring and safety. • Mimose-A develops autonomous systems using artificial intelligence to enable the early detection of leaks in industrial environments. • AGATO (Gastomography) introduces a novel robotic system for high-resolution gas distribution mapping. • Passive Smart Dust detects chemically hazardous substances using drones equipped to distribute and detect particles carrying selective dyes, enabling rapid and reliable monitoring without complex components. • HyAirLogic Lab advances hydrogen (H₂) research by testing the entire value chain in various Berlin-Brandenburg quarters, addressing technological challenges, public acceptance, and sustainable energy solutions for H₂-cargo drones. T2 - DLR Research Seminar CY - Weßling, Germany DA - 04.11.2024 KW - Aerial robot KW - Learning Based Gas Distribution Mapping KW - Mobile Robotic Olfaction KW - Aerial-based Gas Tomography KW - Passive Smart Dust PY - 2024 AN - OPUS4-61611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Devi, Sarita A1 - Riedel, Soraya A1 - Döring, Sarah A1 - Hiller, Lukas A1 - Kaliyaraj Selva Kumar, Archana A1 - Flemig, Sabine A1 - Singh, Chandan A1 - Konthur, Zoltán A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf T1 - Antibodies Functionalized Magnetic Fe-Metal-Organic Framework Based Biosensor for Electrochemical Detection of Tetanus Neurotoxin N2 - This work presents a metal-organic framework (MOF)-integrated microfluidic flow-cell (MFC) based immunodetection of the tetanus toxoid (TT) using electrochemical technique for the first time. The magnetic property of Fe-MOF helped to hold them on the working electrode at detection zone of MFC surpassing the requirement of additional conjugation chemistry, whereas the conductive property was utilized to observe the change in signal efficiency in the presence of TT. The one-pot hydrothermal synthesis of a magnetic and conductive iron-based MOF (Fe-MOF) was performed using the Fe3 +/Fe2+ precursors as 1.2/1 mmol and dual ligands, i.e., tetrahydroxy-1,4-benzoquinone and 2-aminobenzene-1,4-dicarboxylic acid. The Fe-MOF was conjugated with L-phenylalanine (Fe-MOF/Phe) to increase its electric conductivity owing to the enhanced electron flow rate. The human monoclonal antibody SA13 against TT (anti-TT mAb) was conjugated on the Fe-MOF/Phe surface with the help of ethylenediamine (Fe-MOF/Phe/EDA/anti-TT mAb). The binding affinity of Fe-MOF/Phe/EDA/anti-TT mAb for the TT antigen was evaluated using cyclic voltammetry technique. The limit of detection of the Fe-MOF/Phe/EDA/anti-TT mAb-based biosensor for TT was 9.4 ng/ml in spiked buffer. This study shows the applicability of these Fe-MOFs in the detection of various other microbial toxins or other biomolecules. KW - Antikörper KW - Elektrochemischer Immunoassay KW - Molecular Organic Framework (MOF) KW - Microfluidics KW - Rekombinant PY - 2025 DO - https://doi.org/10.1016/j.snb.2025.137381 SN - 0925-4005 VL - 431 SP - 1 EP - 12 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-62673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Cakir, Cafer Tufan T1 - Optimization of depth resolved X-ray absorption spectroscopy in grazing emission mode for characterizing compositionally complex alloys N2 - Layered materials are fundamental to technological advancements, offering distinct properties that differentiate them from bulk materials. In electronics, for instance, thin-film transistors (TFTs) are used to enhance charge transport and flexibility, thereby improving device performance. In the same way, thin-film photovoltaic devices used in renewable energy use strategic layering to absorb light more efficiently and separate electron-hole pairs more effectively, which leads to higher energy conversion efficiency. In recent decades, the development of new alloys has highlighted the importance of layered materials in another context. Compositionally complex alloys, for example, form multiple oxide layers on their surfaces when they oxidize. Studying these corrosion layers is crucial for understanding material-environment interactions. Typical surface analysis techniques, including X-ray photoelectron spectroscopy (XPS), secondary ion mass spectrometry (SIMS), and Meitner-Auger electron spectroscopy (MAES), provide valuable insights but are constrained by their requirements for high Vacuum conditions and their limited depth analysis. In contrast, X-ray absorption near-edge structure (XANES) spectroscopy presents a versatile and advantageous alternative. It operates effectively under ambient conditions and allows time-resolved measurements, enhancing the analysis of materials in real-time as they undergo structural and compositional changes. This adaptability broadens the scope for material analysis, allowing for a more comprehensive understanding of dynamic processes. Grazing Emission X-ray Fluorescence (GEXRF) spectroscopy stands out as a nondestructive, depth-resolved, element-specific characterization technique important for collecting depth-resolved information at the nanometer scale. Its ability to collect in-Depth resolved information based on the grazing emission angle of the fluorescence Radiation makes it ideal for investigating thin films, corrosion layers, and interfaces within layered materials. The integration of XANES in emission mode with GEXRF enables detailed exploration of the chemical states of the analyzed atom and provides depth-resolved information. This study discusses grazing emission X-ray absorption near-edge structure spectroscopy (GEXANES), a novel layer analysis technique that is created by integrating these two methods. This study also innovatively combines machine learning with GEXANES spectroscopy to reduce experimental times. By using active learning, a subset of machine learning, it refines the data acquisition process, enabling more efficient and streamlined methods. The application of active learning in this context illustrates the potential of data-driven approaches to transform experimental methodologies, particularly in resource-limited environments such as synchrotron facilities, thereby accelerating scientific research and discovery. KW - Angle resolved XRF KW - GEXRF KW - BO KW - Active Learning KW - XRF PY - 2025 DO - https://doi.org/10.34726/hss.2025.101302 SP - 1 EP - 129 CY - Technische Univeristät Wien AN - OPUS4-63793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Szymoniak, Paulina A1 - Smales, Glen Jacob A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Molecular Dynamics of Janus Polynorbornenes: Glass Transitions and Nanophase Separation N2 - For the first time, dielectric and calorimetric investigations of an homologous series of Janus polynorbornenes with rigid main backbones and flexible -Si(OR)3 side groups, of differing length alkyl chains (R = Propyl, Butyl, Hexyl, Octyl, Decyl) is reported. Generally, this class of polymers has some potential for applications in the field of gas separation membranes. Two dielectrically active processes are observed at low temperatures, denoted as β- and α- relaxation. The former can be assigned to localized fluctuations, whilst the latter is related to the glassy dynamics of the flexible -Si(OR)3 side groups, creating a nanophase separation in both the alkyl chain rich and backbone rich domains. This is confirmed through temperature modulated DSC measurements and X-ray scattering experiments. The glass transition temperatures of the backbone rich domains, which are beyond or near to their degradation temperatures in terms of conventional DSC, are determined for the first time using Fast Scanning Calorimetry employing both fast heating and cooling rates. This is complimented with scattering experiments that show how the size of the alkyl chain rich domains increases with chain length. Alongside these results, a significant conductivity contribution was observed for all poly(tricyclononenes) with -Si(OR)3 side groups, which is interpreted in terms of a percolation model. KW - Polynorbornenes KW - Broadband Dielectric Spectrscopy KW - Advanced calorimetry PY - 2020 DO - https://doi.org/10.1021/acs.macromol.0c01450 VL - 53 IS - 17 SP - 7410 EP - 7419 PB - ACS AN - OPUS4-51196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schönhals, Andreas A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Böhning, Martin A1 - Zamponi, M. A1 - Frick, B. A1 - Appel, M. A1 - Günther, G. A1 - Russina, M. A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Zorn, R. T1 - Microscopic dynamics of highly permeable super glassy polynorbornenes revealed by quasielastic neutron scattering N2 - The molecular dynamics of addition-type poly(tricyclononenes) with Si-substituted bulky side groups has been investigated by a combination of neutron time-of-flight and neutron backscattering spectroscopy methods on a time scale from 0.1 ps to ca. 3 ns. The investigated poly(tricyclononenes) PTCNSi1 and PTCNSi2g both bear a high microporosity which makes them promising candidates for active separation layers for gas separation membranes. At least for larger gas molecules it is assumed that the pathways for diffusion require an enlargement of pre-existing micropores in terms of an activated zone. A low temperature relaxation process was found for both polymers by the performed neutron scattering experiments. This process was assigned to the methyl group rotation. It was analysed in terms of a jump diffusion in a three-fold potential. The analysis of the dependence of the elastic incoherent structure factor on the scattering vector yields the number of methyl groups which might be immobilized. For PTCNSi1 (3 methyl groups in the monomeric unit) it was found that all methyl groups take part in the methyl group rotation whereas for PTCNSi2g (6 methyl groups in monomeric unit) a considerable number of methyl groups are blocked in their rotation. This immobilization of methyl groups is due to the sterically demanding arrangement of the methyl groups in PTCNSi2g. This conclusion is further supported by the result that the activation energy for the methyl group rotation is three times higher for PTCNSi2g than that of PTCNSi1. KW - Highly permeably polynorbornenes KW - Polymers of intrinsic microporosity KW - Gas separation membranes KW - Quasielastic neutron scattering PY - 2021 DO - https://doi.org/10.1016/j.memsci.2021.119972 SN - 0376-7388 VL - 642 PB - Elesevier B.V. AN - OPUS4-53508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Szymoniak, Paulina A1 - Smales, Glen Jacob A1 - Bermeshev, M. A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Molecular mobility of polynorbornenes with trimethylsiloxysilyl side groups: Influence of the polymerization mechanism N2 - We report dielectric and calorimetric studies on metathesis and addition-type polytricyclononenes, both based on the same monomer bearing three pendant OSiMe3 groups. For the addition-type polymer, dielectric spectroscopy reveals a β*-process related to the microporosity, whereas for its metathesis counterpart, the segmental dynamics manifests as an α-process related to a glass transition. Besides active dielectric processes, a significant conductivity contribution is detected for both samples which for the microporous additiontype polymer is three orders of magnitude greater than for the metathesis polymer. The broadband dielectric spectroscopy is complemented by detailed calorimetric investigations, comprising DSC, FSC, and TMDSC. The calorimetric methods detected the glass transition for the metathesis polymer in agreement with the observed dielectric α-process. Furthermore, the already reported gas transport properties for both polymers are compared, setting them in correlation with the observed molecular mobility and conductivity behavior. The discussed results reflect significant differences in molecular mobility of the two polymers affecting the appearance of microporosity which strongly determines the gas transport properties. KW - Microporous polymers KW - Molecular mobility KW - Electrical conductivity KW - Membrane polymers KW - Gas separation PY - 2022 DO - https://doi.org/10.22079/JMSR.2021.538060.1495 SN - 2476-5406 VL - 8 IS - 3 SP - 1 EP - 9 PB - Membrane Processes Research Laboratory (MPRL) CY - Tehran AN - OPUS4-54303 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Wolf, M. A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Low frequency vibrational density of state of highly permeable super glassy polynorbornenes – The Boson peak N2 - Inelastic incoherent neutron time-of flight scattering was employed to measure the low frequency density of states for a series of addition polynorbornenes with bulky side groups. The rigid main chain in combination with the bulky side groups give rise to a microporosity of these polymers in the solid state. The microporosity characterized by the BET surfaces area varies systematically in the considered series. Such materials have some possible application as active separation layer in gas separation membranes. All investigated materials show excess contributions to the Debye type density of states characteristic for glasses known as Boson peak. The maximum position of the Boson peak shifts to lower frequency values with increasing microporosity. Data for PIM-1 and Matrimid included for comparison are in good agreement to this dependency. This result supports the sound wave interpretation of the Boson peak. KW - Polynorbornes KW - Neutron Scattering PY - 2020 DO - https://doi.org/10.1039/d0cp03360j SN - 1463-9076 VL - 22 IS - 33 SP - 18381 EP - 18387 PB - Royal Chemical Society AN - OPUS4-51165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schönhals, Andreas T1 - Vibrational density of states and molecular mobility in a polymer with intrinsic microporosity PIM-1 as revealed by inelastic neutron scattering N2 - Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. Here, by means of inelastic neutron scattering, the vibrational density of states (VDOS) and the molecular mobility were investigated for PIM-1, the prototypical polymer with intrinsic microporosity. The results are compared to data measured for a more conventional high-performance polyimide used in gas separation membranes (Matrimid). The measured data show the characteristic low frequency excess contribution to the VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. In comparison to the Boson peak of Matrimid, that of PIM-1 is shifted to lower frequencies. This shift is discussed considering the microporous, sponge-like structure of PIM-1 as providing a higher compressibility at the molecular scale than for conventional polymers. Elastic fixed window scans were measured on a neutron backscattering spectrometer to have an overview about the molecular dynamics at a time scale of ca. 1 ns. The temperature dependence of the estimated mean squared displacement shows a step-like increase in the temperature range from 100 K to 250 K indicating the onset of some molecular mobility. The nature of this motional process was analyzed in detail by quasielastic neutron scattering combining Time-of-Flight and backscattering where the data are discussed with regard to both the q- and the temperature dependence. T2 - 7. European Conference on Neutron Scattering 2019 CY - Saint Petersburg, Russia DA - 30.06.2019 KW - Neutron Scattering KW - Polymer of intrinsic microporosity PY - 2019 AN - OPUS4-48421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning T1 - Hard X-Ray Imaging Capabilities at BAMline (BESSY II) N2 - The BAMline at the 3rd generation synchrotron X-ray source BESSY II has been supporting researchers in a wide range of research areas for over 20 years. In addition to materials science, these fields also include biology, cultural heritage, and medicine. Being a non-destructive characterization method, synchrotron X-ray imaging, in particular tomography (SXCT), plays a particularly important role in structural characterization. A recent upgrade of key BAMline equipment expands the imaging capabilities: The upgraded dual multilayer monochromator offers flexibility by providing different energy spectra to optimize flux and energy resolution as desired. Different spectra (8 – 60 keV with ΔE/E 0.01%, 1.5%, 4% and pink beam) can be selected. The upgraded detector (in white beam configuration, equipped with an sCMOS camera) allows the higher flux to be exploited with reduced readout times. Shorter tomographic acquisition times in the range of seconds are now possible. Hence, in-situ and operando examinations are routinely available. An integrated slip ring allows continuous rotation of the sample stage for ease of wiring. The pink beam option allows tomographic observation of processes occurring in the time domain of a few seconds with a resolution down to ~ 1 µm. Different scan methods, optimized for quality and speed are available and discussed. Examples of energy related materials from fuel cell and battery research are shown. An optional end station allows refraction enhanced imaging (synchrotron X-Ray refraction radiography (SXRR) and tomography (SXRCT)). That includes an analyzer Si-crystal in Bragg alignment between sample and detector. This technique obtains sensitivity to smaller structures (cracks, pores) down to a few wavelengths, while obtaining field of view sizes in the range of several mm. Besides medicine (e.g., teeth explants), several applications are found in material science, like studies on diesel particulate filters, ceramics, additively manufactured (AM) alloys and metal matrix composites (MMC). The in-situ capabilities include mechanical load (tension and compression) and heating up to 1100°C. A case study, the microstructural evolution during heat treatment of an AM AlSi10Mg, will be shown. T2 - 15th International Conference on X-Ray Microscopy (XRM 2022) CY - Online meeting DA - 19.06.2022 KW - BAMline KW - X-ray imaging KW - Tomography PY - 2022 AN - OPUS4-55691 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana A1 - Serrano-Munoz, Itziar T1 - Multiscale residual stress analysis and synchrotron X-ray refraction of additively manufactured parts N2 - The overview of the activity of group 8.5 Micro-NDT (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The challenges in the residual stress analysis of AM components are discussed on the basis on the show studies performed in BAM. Also, the synchrotron X-ray refraction technique, available in BAM, is presented, showing example of in-situ heating test of Al10SiMg AM material. T2 - Seminar at Grenoble INP, Science et Ingénierie des Matériaux et Procédés (SIMaP) CY - Grenoble, France DA - 01.07.2022 KW - Additive manufacturing KW - Residual stress KW - X-ray refraction KW - Computed tomography PY - 2022 AN - OPUS4-55232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - Röntgenrefraktionstechnik - Charakterisierung von Keramiken und Verbundwerkstoffen N2 - Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenkung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede: a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1); Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für: a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung. Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie: a) Sintern von SiC-Grünkörpern b) Porositätsanalyse in Dieselpartikelfiltersilikaten c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen d) Mikrorissbildung in Glaskeramik. Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Röntgen-Refraktion KW - Verbundwerkstoffe KW - Keramik PY - 2023 AN - OPUS4-57615 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Synchrotron X-Ray Refraction during in-situ heat treatments N2 - In this work, synchrotron X-ray refraction radiography (SXRR) was combined with in-situ heat treatment to monitor microstructure and porosity evolution as a function of temperature. The investigated material was a laser powder bed fusion (LPBF) manufactured AlSi10Mg, where the initial eutectic Si network is known to break down into larger particles with increasing temperature. Such alloy is also prone to thermally induced porosity (TIP). We show that SXRR allows detecting the changes in the Si-phase morphology upon heating, while this is currently possible only using scanning electron microscopy. SXRR also allows observing the growth of pores, usually studied via X-ray computed tomography, but on much smaller fields-of-view. Our results show the great potential of in-situ SXRR as a tool to gain in-depth knowledge of the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes. T2 - MSE 2022 CY - Darmstadt, Germany DA - 27.09.2022 KW - Si network KW - Al alloys KW - PBF-LB KW - X-ray refraction radiography KW - Pore nucleation PY - 2022 AN - OPUS4-56161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning T1 - Tomographic Imaging Capabilities with hard X-Rays at BAMline (Bessy II) N2 - The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers in a wide range of research areas since more than 20 years. These fields include biology, cultural heritage, medicine, and also materials science. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. A recent upgrade of key equipment at the BAMline expands the imaging capabilities towards shorter acquisition times. Therefore, in-situ and operando experiments can now be routinely conducted. Also, different energy resolutions can be set up to optimize flux and energy resolution as desired. This requires an adaptation of the used reconstruction methods in order to perform necessary analyses also during the experiment. In this presentation the equipment, data handling pipeline as well as various examples from material science are presented. T2 - 5th Conference for Research with Synchrotron Radiation, Neutrons and Ion Beams at Large Facilities (SNI 2022) CY - Berlin, Germany DA - 05.09.2022 KW - BAMline KW - X-ray imaging KW - Tomography PY - 2022 AN - OPUS4-55692 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning T1 - Synchrotron X-Ray Tomography Techniques at BAMline N2 - Synchrotron X-Ray computed tomography at the BAMline is constantly evolving. During monochromatic tomographic scans a preview reconstruction is offered. Newly introduced scanning schemes suppress certain types of reconstruction artifacts. Additionally, the application of a pink beam enables for faster tomographic scans even within seconds. T2 - HZB User Meeting CY - Online meeting DA - 09.12.2021 KW - BAMline KW - X-ray imaging KW - Tomography PY - 2021 AN - OPUS4-54075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - X-ray refraction techniques non-destructively quantify and classify defects in am materials N2 - X-ray refraction is analogous to visible light deflection by matter; it occurs at boundaries between different media. The main difference between visible light and X-rays is that in the latter case deflection angles are very small, from a few seconds to a few minutes of arc (i.e., the refraction index n is near to 1). Importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks and quantify their densities in bulk (not too heavy) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, they can detect objects with size above a few wavelengths of the radiation. Such techniques, especially at the Synchrotron BESSY II, Berlin, Germany, can be used in-situ, i.e. when the specimen is subjected to temperatures or external loads. The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models. We hereby show the application of non-destructive X-ray refraction radiography (SXRR, 2D mapping also called topography) to problems in additive manufacturing: 1) Porosity analysis in PBF-LM-Ti64. Through the use of SXRR, we could not only map the (very sparse) porosity distribution between the layers and quantify it, but also classify, and thereby separate, the filled porosity (unmolten powder) from the keyhole and gas pores (Figure 1). 2) In-situ heat treatment of laser powder bed fusion PBF-LM-AlSi10Mg to monitor microstructure and porosity evolution as a function of temperature (Figure 2). By means of SXRR we indirectly observed the initial eutectic Si network break down into larger particles as a function of increasing temperature. We also could detect the thermally induced porosity (TIP). Such changes in the Si-phase morphology upon heating is currently only possible using scanning electron microscopy, but with a much smaller field-of-view. SXRR also allows observing the growth of some individual pores, usually studied via X-ray computed tomography, but again on much smaller fields-of-view. Our results show the great potential of in-situ SXRR as a tool to gain in-depth knowledge of the defect distribution and the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes. T2 - AAMS 2023 CY - Madrid, Spain DA - 27.09.2023 KW - X-ray refraction radiography KW - Defects KW - Large scale facilities KW - Computed tomography PY - 2023 AN - OPUS4-58508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vermeeren, Sarah A1 - Witzler, Markus A1 - Makarow, Ramona A1 - Engelhard, Carsten A1 - Kaul, Peter T1 - Multivariate evaluation method for the detection of pest infestations on plants via VOC analysis using gas chromatography mass spectrometry N2 - Volatile organic compounds (VOCs) play an important role in the defense against pest infestations on plants. The analysis of these VOCs using gas chromatography mass spectrometry (GC-MS) enables the detection of pests by analyzing the VOC composition (VOC profiles) for specific patterns and markers. The analysis of such complex datasets with high biovariability poses a particular challenge. For this reason, a multivariate evaluation method based on a self-written Python script, using principal component analysis (PCA) and linear discriminant analysis (LDA), was developed and tested for functionality using a dataset, which has been evaluated manually and has identified five specific markers (2,4-dimethyl-1-heptene, 3-carene, alpha-longipinene, cyclosativene, and copaene) for Anoplophora glabripennis (ALB) infestation on Acer trees. The results obtained in the present study did not only match the manually evaluated results, but lead to further insight into the dataset. Another sesquiterpene which is assumed to be alpha-zingiberene was identified as an ALB specific marker in addition to 2,4-dimethyl-1-heptene and 3-carene. Furthermore, the European native beetle species goat moth Cossus cossus (CC) and poplar long-horned beetle Saperda carcharias (SC) were also analyzed for their VOCs to differentiate ALB specific VOC from other pest infestations. This comparison lead to the conclusion that the compounds alpha-longipinene, cyclosativene, and copaene are not specific for ALB but for pest infestation in general. It was possible to identify not only specifically produced VOCs, but also differences in concentrations that arise specifically during ALB infestation. Therefore, the evaluation method for the detection of plant pests presented in this study represents a time-saving alternative to conventional non computing methods, which in addition provides more detailed results. KW - Mass Spectrometry KW - Gas Chromatography KW - Volatile organic compounds KW - Pest infestation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639526 DO - https://doi.org/10.1038/s41598-025-11607-5 SN - 2045-2322 VL - 15 IS - 1 SP - 1 EP - 10 PB - Springer Science and Business Media LLC AN - OPUS4-63952 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Serrano-Munoz, Itziar A1 - Kupsch, Andreas A1 - Müller, Bernd R. T1 - X-Ray-Refraction-Imaging-Techniques high-resolution microstructural characterization N2 - X-ray refraction is analogous to visible light deflection by matter; it occurs at boundaries between different media. The main difference between visible light and X-rays is that in the latter case deflection angles are very small, from a few seconds to a few minutes of arc (i.e., the refraction index n is near to 1). Trivially but importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks and quantify their densities in bulk (not too heavy) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, their detectability is simply limited by the wavelength of the radiation. We thereby show the application of X-ray refraction 2D mapping (topography) and tomography to different sorts of problems in materials science and technology: 1) Sintering of SiC green bodies; 2) Porosity analysis in additively manufactured alloys; 3) Fiber de-bonding in metal and polymer matrix composites. Such techniques, especially at the Synchrotron BESSY II, Berlin, Germany, can be used in-situ, i.e. when the specimen is subjected to temperatures or external loads. Applications of in-situ X-ray refraction radiography on aluminum alloys and composites are also shown. The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models. T2 - ICT 2023 CY - Fürth, Germany DA - 27.02.2023 KW - X-ray refraction KW - Composites KW - In-situ KW - Additive Manufacturing KW - Sintering KW - Ceramics PY - 2023 AN - OPUS4-57200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Jennifer A1 - Engelhard, Carsten A1 - Kaul, Peter T1 - Optimized fast gas chromatography coupled with proton-transfer-reaction time-of-flight mass spectrometry for the selective near real-time analysis of herbivore-induced plant volatiles N2 - The analysis of herbivore-induced plant volatiles (HIPVs) is essential for understanding plant-environment interactions and defense strategies against herbivores. Proton transfer reaction time-of-flight mass spectrometry (PTR–TOF–MS) is a powerful analytical tool that enables real-time monitoring and quantification of diverse groups of HIPVs. However, the PTR–TOF–MS technique is constrained in its ability to effectively differentiate between isomers. When analyzing complex mixtures of HIPVs, the separation of isomers becomes crucial as major compound classes such as terpenes comprise thousands of isomers. In this study, we present an optimized fast gas chromatography (fastGC) based on a modified version of the commercially available fastGC add-on integrated into a mobile PTR–TOF. The system was optimized for the analysis of emissions from enclosed trunks of Acer platanoides infested by Anoplophora glabripennis (Motschulsky), commonly known as Asian longhorned beetle (ALB). The development of fastGC was primarily focused on the sesquiterpenes α-longipinene, cyclosativene and α-copaene, which serve as strong indicators of ALB infestation. These sesquiterpenes were separated in less than three minutes, with intra-day retention time RSD < 0.6 % and resolutions of 2.6 ± 0.3 and 1.3 ± 0.2. In comparison to the original system, the optimized fastGC demonstrates more than tripled sesquiterpene resolution, twice the sensitivity relative to direct inlet mode, and an approximately 10 % reduction in total analysis time. The optimized fastGC–PTR–TOF allows for near real-time analysis of complex mixtures of biogenic VOCs, making it a powerful tool for environmental monitoring, integrated pest management, and forest protection. KW - Mass Spectrometry KW - PTR-TOF-MS KW - Gas Chromatography KW - Herbivore-induced plant volatiles KW - Sesquiterpenes PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639513 DO - https://doi.org/10.1016/j.chroma.2025.466236 SN - 0021-9673 VL - 1759 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-63951 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Serrano-Munoz, Itziar A1 - Evsevleev, Sergei T1 - Damage characterization via 2D and 3D X-ray refraction techniques N2 - We present two examples of the potential of synchrotron X-ray refraction techniques. First, we focus on the 3D imaging of hydrogen assisted cracks in an EN AW – 6060 aluminium alloy which are otherwise undetected by absorption-based CT. The second work is a quantitative analysis of the damage evolution in an Al/Al2O3 Metal Matrix Composite during interrupted in-situ tensile load. T2 - International Conference on Tomography of Materials & Structures CY - Cairns, Australia DA - 22.07.2019 KW - X-ray refraction KW - Analyzer-based imaging KW - Aluminum alloy KW - Metal matrix composite KW - Damage characterization PY - 2019 AN - OPUS4-48604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fritsch, Tobias T1 - 3D Analysis of Powder for Laser Beam Melting by Synchrotron X-ray CT N2 - Additive Manufacturing (AM) in terms of laser powder-bed fusion (L-PBF) offers new prospects regarding the design of parts and enables therefore the production of complex structures. The quality of the feedstock material receives increasing attention, as it depicts the first part of the L-PBF process chain. The powder quality control in terms of flowability and powder bed packing density is therefore mandatory. In this work, a workflow for quantitative 3D powder analysis in terms of particle size, particle shape, particle porosity, inter-particle distance and packing density was established. Synchrotron computed tomography (CT) was used to correlate the packing density with the particle size and particle shape for three different powder batches. The polydisperse particle size distribution (PSD) was transformed into a statistically equivalent bidisperse PSD. The ratio of the small and large particles helped to understand the powder particle packing density. While the particle shape had a neglectable influence, the particle size distribution was identified as major contributor for the packing density. T2 - AM- Workshop BAM CY - Online meeting DA - 20.04.2021 KW - Additive manufacturing KW - Laser powder bed fusion KW - Powder KW - Particle size distribution KW - Packing density PY - 2021 AN - OPUS4-53477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Redefining residual stress analysis to tackle the challenges posed by additively manufactured materials and structures N2 - Additively manufactured (and in particular laser powder bed fused) materials represent a manyfold challenge for the materials scientist and engineer because of their distinctive microstructure. If laser powder bed fusion is used to produce components, the complexity level increases because meso-structures (e.g., overhanging features, surface and internal defects) gain importance. Furthermore, if the main advantage of additive manufacturing, i.e., the freedom of design, is to be fully exploited, and geometrically complex structures, such as lattices, are manufactured, then such structures become meta-materials. This means that the geometry and the materials properties become equally important. This matryoshka-like (more literary than the dry “multi-scale”) complexity makes the characterization of the residual stress fields by means of diffraction methods so difficult with the current means, that new paradigms are necessary to tackle the challenge. Indeed, classic open problems acquire an extra layer of difficulty, such that new solutions need to be found and the sometimes-dormant debate needs to be re-opened. Examples include the determination of: a- the unstrained reference: this reference can become location-dependent and needs to be carefully determined; b- the so-called diffraction elastic constants, which becomes immensely challenging since even the single-crystal elastic constants are not known for additively manufactured materials. On top of this, other problems arise. The determination of the principal axes of stress becomes non-trivial because the hatching strategy sometimes dominates over the sample geometry. Even further, in complex structures, such as lattices, the textbook statement that the strain measurement in six independent directions uniquely identifies the strain tensor becomes simply invalid. The peculiar surface features of additively manufactured materials transform trivial tasks into formidable challenges: the precise alignment of a specimen in a beam or the determination of surface stresses with laboratory X-rays need to be thoroughly re-discussed and lay far from being routine tasks. In this paper, we will show a few examples of the cases mentioned above. We will demonstrate that sometimes the classic approach works very well, but other times surprising conclusions can be drawn from in-depth studies of the residual stress in additively manufactured materials. In short, we predicate that classic methods cannot be used on additively manufactured materials and structures without a critical evaluation of their validity and application range. T2 - ICRS11 CY - Nancy, France DA - 28.03.2022 KW - Neutron diffraction KW - Laser powder bed fusion KW - Diffraction elastic constants KW - Unstrained reference KW - Surface roughness KW - Porosity PY - 2022 AN - OPUS4-54642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - The combined use of X-ray refraction and trans-mission radiography and computed tomography N2 - Alternative to conventional transmission-based radiography and computed tomography, X-ray refraction techniques are being increasingly used to detect damage in light materials. In fact, their range of application has been recently extended even to metals. The big advantage of X-ray refraction techniques is that they are able to detect nanometric defects, whose size would lie below the resolution of even state-of-the-art synchrotron-based X-ray computed tomography (SXCT). The superiority of synchrotron X-ray refraction radiography and tomography (SXRR and SXRCT) has been shown in the case of light materials, in particular composites. X-ray refraction techniques also yield a quantitifaction of the amount of damage (the so-called relative internal specific surface) and can well be compared with damage models. At the same time, it is impossible for SXRR and SXRCT to image single defects. We show that the combination of refraction- and transmission-based imaging techniques yields an impressive amount of additional information about the type and amount of defects in microstructured materials such as additively manufactured metals or metal matrix composites. We also show that the use of data fusion techniques allows the classification of defects in statistically significant representative volume elements. T2 - 11th Conference on Industrial Computed Tomography CY - Online meeting DA - 08.02.2022 KW - X-ray refraction radiography KW - Computed Tomography KW - Synchrotron radiation KW - Additive manufacturing KW - Damage evolution PY - 2022 AN - OPUS4-54327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana T1 - In-situ imaging of additively manufactured alloys at the BAMline N2 - In this work, we present the recent in-situ imaging developments at the BAMline (of synchrotron BESSY II, HZB), focused on the in-situ characterization and understanding of microstructural evolution of additively manufactured materials subjected to different environments. Two show cases are presented. In the first, X-ray refraction radiography (SXRR) was combined with in-situ heat treatment to monitor the microstructural evolution as a function of temperature in a laser powder bed fusion (LPBF) manufactured AlSi10Mg alloy. We show that SXRR allows detecting the changes in the Si-phase morphology upon heating using statistically relevant volumes. SXRR also allows observing the growth of pores (i.e., thermally induced porosity), usually studied via X-ray computed tomography (XCT), but using much smaller fields-of-view. In the second case study, XCT was combined with in-situ tensile test to investigate the damage mechanism in a LPBF Aluminum Metal Matrix Composite (MMC). In-situ SXCT test disclosed the critical role of the defects in the failure mechanism along with pre-cracks in the reinforcement phase of MMC. We found that cracks were initiated from lack-of-fusion defects and propagated through coalescence with other defects. T2 - New Frontiers in Materials Design for Laser Additive Manufacturing CY - Montabaur, Germany DA - 22.05.22 KW - Additive manufacturing KW - Laser powder bed fusion KW - Synchrotron X-ray computed tomography KW - Synchrotron X-ray Refraction PY - 2022 AN - OPUS4-54900 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Konnertz, Nora A1 - Ding, Yi A1 - Harrison, W.J. A1 - Budd, P.M. A1 - Schönhals, Andreas A1 - Böhning, Martin T1 - Molecular mobility of the high performance membrane polymer PIM-1 as investigated by dielectric spectroscopy N2 - The increasing demand for energy efficient separation processes fosters the development of new high performance polymers as selective separation layers for membranes. PIM-1 is the archetypal representative of the class of polymers of intrinsic microporosity (PIM) which are considered most promising in this sector, especially for gas separations. Since their introduction, PIMs stimulated a vast amount of research in this field and meanwhile evolved to the state of the art in membrane technology for gas separation. The major obstacle for extending the practical membrane application is their strong tendency to physical aging. For the first time, investigations by broadband dielectric spectroscopy (BDS) addressing molecular dynamics and conductivity in PIM 1 are presented. As chain packing during film formation from the casting solution and physical aging are key factors determining the separation performance of PIMs as membrane materials, characterization of the molecular mobility in such materials as revealed by BDS will provide valuable information for further development and optimization. KW - PIM-1 KW - BDS broadband dielectric spectroscopy KW - Relaxation KW - Membrane PY - 2016 DO - https://doi.org/10.1021/acsmacrolett.6b00209 SN - 2161-1653 VL - 5 IS - 4 SP - 528 EP - 532 PB - ACS American Chemical Society CY - Washington, DC, USA AN - OPUS4-35798 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Yin, Huajie A1 - Lohstroh, W. A1 - Harrison, W. A1 - Budd, P.M. A1 - Pauw, Brian Richard A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Anomalies in the low frequency vibrational density of states for a polymer with intrinsic microporosity - the Boson peak of PIM-1 N2 - Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. Here, the vibrational density of states (VDOS) for PIM-1, the prototypical polymer with intrinsic microporosity, is investigated by means of inelastic neutron scattering. The results are compared to data measured for a more conventional high-performance polyimide used in gas separation membranes (Matrimid). The measured data show the characteristic low frequency excess contribution to VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. In comparison to the Boson peak of Matrimid, that of PIM-1 is shifted to lower frequencies. This shift is discussed considering the microporous, sponge-like structure of PIM-1 as providing a higher compressibility at the molecular scale than for conventional polymers. For an annealed PIM-1 sample, the Boson peak shifts to higher frequencies in comparison to the un-annealed sample. These changes in the VDOS of the annealed PIM-1 sample are related to changes in the microporous structure as confirmed by X-ray scattering. KW - Polymers KW - Boson peak KW - Neutron scattering KW - Physical aging KW - Polymer of intrinsic microporosity PY - 2018 DO - https://doi.org/10.1039/C7CP07141H SN - 1463-9076 SN - 1463-9084 VL - 20 IS - 3 SP - 1355 EP - 1363 PB - The Royal Society of Chemistry AN - OPUS4-43808 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kern, Simon A1 - Liehr, Sascha A1 - Wander, Lukas A1 - Bornemann-Pfeiffer, Martin A1 - Müller, S. A1 - Maiwald, Michael A1 - Kowarik, Stefan T1 - Artificial neural networks for quantitative online NMR spectroscopy N2 - Industry 4.0 is all about interconnectivity, sensor-enhanced process control, and data-driven systems. Process analytical technology (PAT) such as online nuclear magnetic resonance (NMR) spectroscopy is gaining in importance, as it increasingly contributes to automation and digitalization in production. In many cases up to now, however, a classical evaluation of process data and their transformation into knowledge is not possible or not economical due to the insufficiently large datasets available. When developing an automated method applicable in process control, sometimes only the basic data of a limited number of batch tests from typical product and process development campaigns are available. However, these datasets are not large enough for training machine-supported procedures. In this work, to overcome this limitation, a new procedure was developed, which allows physically motivated multiplication of the available reference data in order to obtain a sufficiently large dataset for training machine learning algorithms. The underlying example chemical synthesis was measured and analyzed with both application-relevant low-field NMR and high-field NMR spectroscopy as reference method. Artificial neural networks (ANNs) have the potential to infer valuable process information already from relatively limited input data. However, in order to predict the concentration at complex conditions (many reactants and wide concentration ranges), larger ANNs and, therefore, a larger Training dataset are required. We demonstrate that a moderately complex problem with four reactants can be addressed using ANNs in combination with the presented PAT method (low-field NMR) and with the proposed approach to generate meaningful training data. KW - Online NMR spectroscopy KW - Real-time process monitoring KW - Artificial neural networks KW - Automation KW - Process industry PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507508 DO - https://doi.org/10.1007/s00216-020-02687-5 SN - 1618-2642 VL - 412 IS - 18 SP - 4447 EP - 4459 PB - Springer CY - Berlin AN - OPUS4-50750 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Garde, Raul T1 - Simultaneous determination of halogens by high resolution absortion spectrometry N2 - The high ionization potentials and low wavelength emission lines of halogens difficult the analysis of their organohalogen compounds by ICP-based methods [1]. Other techniques, such as combustion ion chromatography (CIC) or ion-selective electrodes have proven to be more reliable to determine these elements. However, these techniques are more time-consuming and/or have lower precision and accuracy. High resolution continuum source graphite furnace molecular absorption spectrometry (HR CS GFMAS) allows the determination of solid and liquid samples by monitoring a molecule formed with the analyte and a molecule forming reagent. In the case of F, Cl and Br, several molecule forming agents have been studied for their determination. Among all of them, calcium can form a stable bond with the three elements and provides optimal analytical properties for trace analysis [2]. However, the spectral window of commercially available continuum source AAS instruments is not broad enough to cover the wavelength range necessary for a simultaneous determination. Thus, coupling it with a modular simultaneous echelle spectrograph (MOSES), which can register around 200 nm in a single measure, allows the simultaneous study of the three analytes [3]. This instrumentation is capable of register more than 200 nm of the spectra per measure keeping a high resolution. This spectral window is suitable for the monitorization of a variety of transitions of the three molecules. However, some of them are overlapped and the competitive mechanism of formation of the three molecules modify their sensitivity depending on the proportions in the sample. In this study, a compromise in the conditions and modifiers were selected in order to maximize the sensitivity and signal to noise ratio for the three molecules. The determination was carried out by standard addition of CaF and Cl and Br were obtained from the PLS model. References: [1] X. Bu, T. Wang, G. Hall, J. Anal. At. Spectrom., 18, 1443–1451 (2003) [2] M. Resano, E. García-Ruiz, M. Aramendía, M. A. Belarra, J. Anal. At. Spectrom., 34, 59–80 (2019) [3] S. Geisler, M. Okruss, H. Becker-Ross, M. Dong Huang, N. Esser, S. Florek, Spectrochimica Acta PartB, 107, 11–16 (2015) T2 - Adlershofer Forschungsforum CY - Berlin, Germany DA - 11.11.2019 KW - Halogens KW - Fluorine KW - Simultaneous determination KW - MOSES KW - Chemometry KW - Interferences PY - 2019 AN - OPUS4-51998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Compact NMR Spectroscopy in the field: A Versatile Tool for Automated Continuous-Flow Production N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as, e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. Field studies in modular and conventional production plant setups show promising results gaining process knowledge for further optimization. NMR appeared as preeminent online analytical method and allow using a modular data analysis tool, which even served as reliable reference method for further PAT applications (e.g. NIR spectroscopy). In the future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - DECHEMA Workshop "Sensorik für die Digitalisierung chemischer Produktionsanlagen" CY - Frankfurt am Main, Germany DA - 13.06.2022 KW - Compact NMR KW - Process Control KW - Modular Production KW - Process Analytical Technology PY - 2022 AN - OPUS4-55037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Compact NMR Spectroscopy in the field: A Versatile Tool for Automated Continuous- Flow Production N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as, e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. Field studies in modular and conventional production plant setups show promising results gaining process knowledge for further optimization. NMR appeared as preeminent online analytical method and allow using a modular data analysis tool, which even served as reliable reference method for further PAT applications (e.g. NIR spectroscopy). In the future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - 9th Annual Practical Applications of NMR in Industry Conference (PANIC) CY - Nashville, Tennessee, USA DA - 17.10.2021 KW - Process Analytical Technology KW - Benchtop-NMR KW - NMR spectroscopy PY - 2021 AN - OPUS4-53585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online-NMR- und -Raman-Spektroskopie – Kombination von PAT-Methoden für mehr Prozessverständnis N2 - Die Verbesserung des Prozessverständnisses ist eine notwendige Voraussetzung für die Anwendung von Konzepten wie „Industrial Internet of Things (IIoT)“ oder „Industrie 4.0“. Online-Methoden der Prozessanalytik (PAT) ermöglichen die direkte Verfolgung der ablaufenden Reaktionen innerhalb chemischer und pharmazeutischer Produktionsschritte und können somit einen wichtigen Beitrag für die Entwicklung von neuen, innovativen Prozessführungsstrategien liefern. Während die Online-Raman-Spektroskopie bereits erfolgreich im industriellen Umfeld zum Einsatz kommt, ist der Entwicklungsstand für die Online-Niederfeld-NMR-Spektroskopie bislang noch nicht ausreichend für einen routinemäßigen Einsatz innerhalb industrieller Produktionsumgebungen. Der hohe Informationsgehalt der NMR-Daten in Verbindung mit einem geringen Kalibrieraufwand macht die Methode sehr interessant für moderne Konzepte flexibler Produktionsanlagen für die Herstellung vieler unterschiedlicher Produkte in wechselnden Kampagnen. Speziell in modularen Produktionskonzepten kann so die Rüstzeit der Prozessanalytik deutlich verkürzt werden. Am Beispiel der heterogen katalysierten Hydrogenierung von 2-Butin-1,4-diol wird der Einsatz der Kombination von Online-NMR und -Raman-Spektroskopie demonstriert. Dieser Prozessschritt aus der industriellen Synthese des Lösungsmittels Tetrahydrofuran verläuft über ein Zwischenprodukt, welches konkurrierende Reaktionspfade aufweist. Die Kombination von Informationen aus der PAT, sowie von klassischen Prozessgrößen, wie Druck, Temperatur und Durchfluss in einem hoch automatisierten Aufbau erleichtert die Entwicklung und Erprobung von neuen Konzepten für die Prozessführung. T2 - 10. ProcessNet-Jahrestagung CY - Online meeting DA - 21.09.2020 KW - Hydrogenierung KW - Benchtop-NMR KW - Raman-Spektroskopie KW - Prozessanalytik PY - 2020 AN - OPUS4-51363 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Industrial Applications of Low-Field NMR Spectroscopy for Process and Quality Control of Silanes N2 - The combination of different silanes as starting materials and as a product of hydrolysis by several alcohols or water creates a range of hundreds of technical products for a wide range of applications. In recent years, functional trialkoxysilanes have proven to be multi-purpose organosilanes. Applications range from weather protection of buildings to bonding-imparting properties in the glass fiber industry, for sealants and adhesives, for coatings and paints to the modification of polymer materials. Commercial benchtop NMR spectrometers have the potential to be used in silane chemistry as an online method for reaction monitoring and quality control [1]. Interesting NMR nuclei for the above-mentioned products are 1H and 29Si. In a joint research cooperation between EVONIK and BAM, the applicability of low-field NMR spectroscopy for the chemical analysis of silanes was evaluated based on various case studies. In the course of the case studies it was shown how low-field NMR spectroscopy extends the application range of chemical analysis to new applications where existing technologies such as NIR, Raman, UV/VIS, etc. cannot be used quantitatively due to lack of reference data. T2 - 5th European Conference on Process Analytics and Control Technology (EuroPACT) CY - Online meeting DA - 15.11.2021 KW - NMR spectroscopy KW - Benchtop-NMR KW - Silanes KW - Quality Control PY - 2021 AN - OPUS4-53777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Certified reference material for the determination of hydrolytic resistance of borosilicate glass N2 - The preparation of certified reference material for the determination of hydrolytic resistance of borosilicate glass is described. Certified properties are the acid consumption according to the relevant standard procedures described in ISO 720, USP<660> and Ph.Eur. 3.2.1. T2 - 26. International Congress on Glass CY - Berlin, Germany DA - 03.07.2022 KW - Borosilicate glass KW - CRM KW - Hydrolytic resistance PY - 2022 AN - OPUS4-55521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kern, Simon A1 - Liehr, Sascha A1 - Wander, Lukas A1 - Bornemann-Pfeiffer, Martin A1 - Müller, S. A1 - Maiwald, Michael A1 - Kowarik, Stefan T1 - Training data of quantitative online NMR spectroscopy for artificial neural networks N2 - Data set of low-field NMR spectra of continuous synthesis of nitro-4’-methyldiphenylamine (MNDPA). 1H spectra (43 MHz) were recorded as single scans. Two different approaches for the generation of artificial neural networks training data for the prediction of reactant concentrations were used: (i) Training data based on combinations of measured pure component spectra and (ii) Training data based on a spectral model. Synthetic low-field NMR spectra First 4 columns in MAT-files represent component areas of each reactant within the synthetic mixture spectrum. Xi (“pure component spectra dataset”) Xii (“spectral model dataset”) Experimental low-field NMR spectra from MNDPA-Synthesis This data set represents low-field NMR-spectra recorded during continuous synthesis of nitro-4’-methyldiphenylamine (MNDPA). Reference values from high-field NMR results are included. KW - NMR spectroscopy KW - Real-time process monitoring KW - Artificial neural networks KW - Online NMR spectroscopy KW - Automation KW - Process industry PY - 2020 DO - https://doi.org/10.5281/zenodo.3677139 PB - Zenodo CY - Geneva AN - OPUS4-50456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Chemische Prozesskontrolle für modulare Produktionskonzepte mit direkten analytischen Methoden N2 - Flexible Produktionskonzepte werden oft mit modularen, schnell rekonfigurierbaren Einheiten verbunden. Um die Vorteile dieser flexiblen Produktion tatsächlich nutzen zu können ist neben einer geeigneten Infrastruktur auch eine ebenso anpassungsfähige Qualitätskontrolle unverzichtbar. Analysengeräte und Sensoren werden heutzutage immer kompakter und kostengünstiger in ihrer Anschaffung. Dadurch wird es möglich eine große Anzahl von Messstellen innerhalb einer Anlage zu realisieren. Die erfassten Datenmengen erfordern zuverlässige und robuste Auswerteverfahren, die sich in das Gesamtkonzept der Automatisierung einer derart flexiblen Produktion nahtlos integrieren. Referenzdaten aus direkten Methoden wie der NMR-Spektroskopie können hier einen wertvollen Beitrag zur Generierung von Prozesswissen für die Entwicklung neuer Modelle für kostengünstigere Analysenverfahren leisten. T2 - 16. Kolloquium des AK Prozessanalytik CY - Online meeting DA - 23.11.2020 KW - NMR-Spektroskopie KW - Prozessanalytik KW - Modulare Produktion KW - Chemische Prozesskontrolle PY - 2020 AN - OPUS4-51658 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bornemann-Pfeiffer, Martin A1 - Kern, Simon A1 - Jurtz, N. A1 - Thiede, Tobias A1 - Kraume, M. A1 - Maiwald, Michael T1 - Design and validation of an additively manufactured flowCell–static mixer combination for inline NMR spectroscopy N2 - There have been an increasing number of publications on flow chemistry applications of compact NMR. Despite this, there is so far no comprehensive workflow for the technical design of flow cells. Here, we present an approach that is suitable for the design of an NMR flow cell with an integrated static mixing unit. This design moves the mixing of reactants to the active NMR detection region within the NMR instrument, presenting a feature that analyses chemical reactions faster (5–120 s region) than other common setups. During the design phase, the targeted mixing homogeneity of the components was evaluated for different types of mixing units based on CFD simulation. Subsequently, the flow cell was additively manufactured from ceramic material and metal tubing. Within the targeted working mass flow range, excellent mixing properties as well as narrow line widths were confirmed in validation experiments, comparable to common glass tubes. KW - Inline NMR Spectroscopy KW - Integrated Processes KW - Reaction Monitoring KW - Process Analytical Technology KW - Flow Chemistry KW - Static Mixing KW - Modular Production PY - 2019 UR - https://pubs.acs.org/doi/abs/10.1021/acs.iecr.9b03746 DO - https://doi.org/10.1021/acs.iecr.9b03746 SN - 0888-5885 SN - 1520-5045 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. VL - 58 IS - 42 SP - 19562 EP - 19570 PB - American Chemical Society CY - Washington AN - OPUS4-49041 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin T1 - Modular production involving Benchtop NMR: Current application examples driven by digitalization N2 - The demand for increasing product diversity in the chemical and pharmaceutical industry calls for new production processes that enable greater flexibility. Therefore, plants are needed which can be adapted to new processes in a fast manner and be scaled up and down easily to volatile market demands. Modular production techniques in combination with advanced process analytical technology (PAT) are considered as a promising solution able to fulfil these requirements. The success and acceptance of modular concepts in both new and existing plants is dependent of its reliability, easy applicability, and standardization. In recent past, enormous efforts were made to overcome existing barriers in a superordinate level, e.g. DEXPI [1], ENPRO [2], or MTP [3] naming just a few. Here, we’d like to present a few, more hands-on, application examples which are shown in Figure 1 aiming to increase process flexibility and applicability. This includes: a) The development of an additively manufactured mixer—flow reactor combination for the application inside of NMR instruments. [4] b) The application of automated, model-based approaches for model development and spectra evaluation. c) The application of machine-assisted spectral model building as a genuine alternative to classical model-based approaches [5] d) Improvement of NIR calibration through online available NMR reference data. [6] These examples represent miscellaneous use cases but result of the same fact: the increased use and availability of data through advanced PAT and therefore new opportunities utilizing them. T2 - SMASH - Small Molecule NMR Conference CY - Online meeting DA - 30.08.2021 KW - Process analytical technology KW - NMR spectroscopy KW - Automation PY - 2021 AN - OPUS4-53803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Low-Field NMR Spectroscopy on Solid Dispersions A Flow Injection Method for End-Point Control of Azo Couplings for Industrial Pigment Production N2 - Global demand for pigments is expected to increase to around 13.4 million tons per year by 2030, representing approximately $22 billion – 5% of which will be azo pigments as the main organic pigments. Azo pigments, i.e., especially the azo bridge required for them, are almost exclusively produced in technology by the so-called azo coupling reaction in large-scale approaches on the scale of 50–100 cubic meters. Among other things, one of the reasons why large-scale production itself is still essentially discontinuous is the lack of analytical methods for a continuous azo pigment synthesis. In an azo coupling process, an aromatic amine is diazotized to form the diazonium compound (diazo compound), which then reacts with a coupling component, i.e., "couples". A slight excess of the coupler is desired for the end of the reaction, which stoichiometrically consumes the remaining (harmful) diazo compound, i.e., below 500 ppm. This is carried out with a manual spotting reaction of a fast-binding coupler. To carry out continuous azo coupling, care must be taken to ensure that the actual coupling reaction proceeds as rapidly as possible, i.e., preferentially, compared with possible side reactions. Reliable measuring methods are thus a decisive criterion for the useful performance of a continuous azo pigment synthesis. An analytical online procedure is difficult due to several limitations at once: solid dispersions extremely limit the range of reproducible analytical procedures. In addition, the appearance of a signal (e.g., excess of a starting material) in the ppm range must be reliably detected against the matrix background. The back-titration method and benchtop NMR spectroscopy were used to overcome these problems. We present a feasibility study for a suitable process analysis with benchtop NMR spectroscopy on disperse systems for equimolar dosing of the "diazotization" or "coupling" sub-step in azo coupling, which was carried out in cooperation with a chemical company. This could replace tedious manual spotting T2 - SMASH Small molecule NMR conference 2023 CY - Baveno, Italy DA - 17.09.2023 KW - Benchtop NMR KW - Dispersions KW - Process Analytical Technology KW - Process monitoring PY - 2023 AN - OPUS4-58399 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Compact NMR Spectroscopy in the field: A Versatile PAT Tool for Production of Specialty Chemicals N2 - Companies of chemical industry find themselves more often in a rapidly changing environment, e.g., due to variability of raw material quality or energy costs and efficiency. Process optimization and new process concepts become more and more important. For example, flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds like exothermic reactions with high heat dissipation. Highly automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. Field studies in modular and conventional production plant setups show promising results gaining process knowledge for further optimization. NMR appeared as preeminent online analytical method and allow using a modular data analysis approach, which can even serve as reliable reference method for further calibration-dependent PAT applications (e.g., NIR or Raman spectroscopy). Based on experiences from earlier field studies an improved NMR analyzer enclosure setup was developed and built, including the option of a secondary method (e.g., optical spectroscopy). Integrated control systems allow for a flexible implementation based on the available automation infrastructure at the chemical plant or pilot plant setup. In the future, fully integrated and intelligently interconnecting “smart” PAT systems and processes have the potential speed up the setup of production equipment for chemicals and pharmaceuticals and therefore help to reduce the time-to-market. T2 - SMASH Small molecule NMR conference 2023 CY - Baveno, Italy DA - 17.09.2023 KW - Benchtop-NMR KW - Process Analytical Technology KW - Chemical Production KW - NMR spetroscopy PY - 2023 AN - OPUS4-58398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - High-resolution optical spectrometry for lithium isotope ratio analysis N2 - An alternative method for lithium isotope amount ratio analysis is proposed by combining atomic absorption spectrometry with spectra data analysis by machine leaning. It is based on the well-known isotope shift of around 15 pm for the electronic transition at wavelength 670.7845 nm which can be measured by a high-resolution continuum source atomic absorption spectrometer (HR-CS-AAS). For isotope amount ratio analysis, a scalable three boosting machine learning algorithm (XGBoost) was employed and calibrated with a set of samples with a 6Li isotope amount fraction ranging from 99% to 6%. The absolute Li isotope amount fractions of these calibration samples were previously measured by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) and used as ab-initio data for the machine learning algorithm. Validation of the machine leaning model was performed with two standard reference materials (LSVEC and IRMM-016). The procedure was employed for the isotope amount ratio determination of a set of stock chemicals (Li2CO3, LiNO3, LiCl, LiOH, and LiF) as well as a BAM candidate LiMNC cathode reference material. Achieved uncertainties are one order of magnitude higher than those obtained by MC-ICP-MS. This precision and accuracy is nonetheless sufficient to resolve natural occurring variations in Lithium isotope ratios. Also, the LiMNC material was analyzed by HR-CS-AAS with and without matrix purification. The results are comparable within statistical error. T2 - Groupseminar - GFZ Potsdam CY - Online Meeting DA - 27.10.2020 KW - Lithium batteries KW - HR-CS-AAS KW - Machine learning KW - Isotope analysis PY - 2020 AN - OPUS4-51572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Contributions Towards Variable Temperature Shielding for Compact NMR Instruments N2 - The application of compact NMR instruments to hot flowing samples or exothermically reacting mixtures is limited by the temperature sensitivity of permanent magnets. Typically, such temperature effects directly influence the achievable magnetic field homogeneity and hence measurement quality. The internal-temperature control loop of the magnet and instruments is not designed for such temperature compensation. Passive insulation is restricted by the small dimensions within the magnet borehole. Here, we present a design approach for active heat shielding with the aim of variable temperature control of NMR samples for benchtop NMR instruments using a compressed airstream which is variable in flow and temperature. Based on the system identification and surface temperature measurements through thermography, a model predictive control was set up to minimise any disturbance effect on the permanent magnet from the probe or sample temperature. This methodology will facilitate the application of variable-temperature shielding and, therefore, extend the application of compact NMR instruments to flowing sample temperatures that differ from the magnet temperature. T2 - SMASH Small molecule NMR conference 2023 CY - Baveno, Italy DA - 17.09.2023 KW - Benchtop NMR KW - Temperature Control KW - Process Analytical Technology KW - Flow NMR PY - 2023 AN - OPUS4-58400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Already Producing or Still Calibrating? – Advances of Model-Based Automation for Online NMR Spectroscopy N2 - The transition from the current automation landscape to next generation automation concepts for the process industry has already begun. Smart functions of sensors simplify their use and enable plug-and-play integration, even though they may appear to be more complex at first sight. Monitoring specific information (i.e., “chemical” such as physico-chemical properties, chemical reactions, etc.) is the key to “chemical” process control. Here we introduce our smart online NMR sensor module provided in an explosion proof housing as example. Due to NMR spectroscopy as an “absolute comparison method”, independent of the matrix, it runs with very short set-up times in combination with “modular” spectral models. These are based on pure component NMR spectra without the need for tedious calibrations runs. We present approaches from statistical, (i.e., Partial Least Squares Regression) to physically motivated models (i.e., Indirect Hard Modelling). Based on concentration measurements of reagents and products by the NMR analyser a continuous production and direct loop process control were successfully realized for several validation runs in a modular industrial pilot plant and compared to conventional analytical methods (HPLC, near infrared spectroscopy). The NMR analyser was developed for an intensified industrial process funded by the EU’s Horizon 2020 research and innovation programme (“Integrated CONtrol and SENsing”, www.consens-spire.eu). T2 - 2nd Reaction Monitoring Symposium CY - Bath, UK DA - 28.01.2019 KW - Process Analytical Technology KW - NMR Spectroscopy KW - Modular Production PY - 2019 AN - OPUS4-47309 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Low-Field NMR Spectroscopy on Solid Dispersions – A Flow Injection Method for End-Point Control of Azo Couplings for Industrial Pigment Production N2 - Global demand for pigments is expected to increase to around 13.4 million tons per year by 2030, representing approximately $22 billion – 5 % of which will be azo pigments as the main organic pigments. Azo pigments, i.e., especially the azo bridge required for them, are almost exclusively produced in technology by azo coupling reactions in large-scale approaches on the scale of 50–100 cubic meters. Among other things, one of the reasons why large-scale production itself is still essentially discontinuous is the lack of analytical methods for a continuous process control. In an azo coupling process, an aromatic amine is diazotized to form the diazonium compound (diazo compound), which reacts with a coupling component, i.e., "couples". A slight excess of the coupler is desired for the end of the reaction, which stoichiometrically consumes the remaining (harmful) diazo compound, i.e., below 500 ppm. This is carried out with a manual spotting reaction of a fast-binding reagent. To carry out continuous azo coupling, care must be taken to ensure that the actual coupling reaction proceeds as rapidly as possible, i.e., preferentially, compared with possible side reactions. Reliable measuring methods are thus a decisive criterion for the useful performance of a continuous azo pigment synthesis. An analytical online procedure is difficult due to several limitations at once: solid dispersions extremely limit the range of reproducible analytical procedures. In addition, the appearance of a signal (e.g., excess of a starting material) in the ppm range must be reliably detected within the matrix background. A proposal based on a back-titration method and benchtop NMR spectroscopy were used to overcome these problems. We present a feasibility study for a suitable process analysis with benchtop NMR spectroscopy on disperse systems for equimolar dosing of the "diazotization" or "coupling" sub-step in azo coupling. This could potentially replace tedious manual spotting reactions in conventional discontinuous production and paves the way for continuous production. T2 - 19. Kolloquium AK Prozessanalytik CY - Darmstadt, Germany DA - 04.12.2024 KW - NMR Spectroscopy KW - Process Analytical Technology KW - Azo-Pigments KW - Benchtop-NMR PY - 2024 AN - OPUS4-62176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Interlaboratory Comparison of Low-Field NMR Spectrometers – Purities at 200 and 10 mmol/L N2 - Due to its advantages of being a direct comparison method, quantitative NMR spectroscopy (qNMR) becomes more and more popular in industry. While conventional high-field NMR systems are often associated with high investment and operational costs, the upcoming market of permanent-magnet based benchtop NMR systems show a considerable option for a lot of applications. The mobility of these systems allows to bring them more closely to the real production environment, e.g. for at-line quality control. In this work we present an interlaboratory comparison study investigating the qNMR performance of state-of-the-art benchtop NMR spectrometers. Therefore, BAM prepared two samples of a mixture of NMR reference standards tetramethylbenzene (TMB) and tetrachloronitrobenzene (TCNB) at concentration levels of 200 mM and 10 mM. These “ready-to-use” samples were sent to participant laboratories, which performed analysis on their benchtop NMR equipment of different vendors and fields from 43 to 80 MHz. Raw data was reported back and further investigated by using different data analysis methods at BAM. After this very first qNMR comparison study of benchtop NMR spectrometers show promising results, following studies are planned to cover more parts of the qNMR process, e.g. sample preparation and weighing, but also data analysis, as commonly done in similar studies for high-field NMR spectroscopy in industry and metrology. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 31.01.2019 KW - qNMR KW - Compact NMR spectroscopy KW - Interlaboratory Comparison PY - 2019 AN - OPUS4-47311 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Online NMR and Raman Spectroscopy – Combination of PAT tools for Process Monitoring N2 - Improvement in deep process understanding is a mandatory prerequisite for the application of modern concepts like Industrial Internet of Things (IIoT) or “Industrie 4.0”. The direct hyphenation with online methods of process analytical technology (PAT) allows profound insights into the actual reactions within chemical and pharmaceutical production steps and provides necessary information for associated advanced control strategies. While the industrial application of online Raman spectroscopy has already been successfully demonstrated, low-field NMR spectroscopy is not yet adequately developed as a robust online method for use in process industry. The high information content combined with the low calibration effort makes NMR spectroscopy a highly promising method for modern process automation with a high flexibility due to short set-up times and novel calibration concepts. This is a major advantage compared to other analytical methods, especially regarding multi-purpose plant strategies, as well as processes suffering from fluctuating quality of raw materials. The work presented here focusses on the heterogeneous catalyzed hydrogenation of 2-butyne-1,4-diol, as a step of the synthesis of industrially important solvent tetrahydrofuran. This reaction is proceeding via an intermediate product and suffers from competitive reaction paths. In this application, online NMR and Raman spectroscopy were combined with data from classical process sensors, e.g., pressure, temperature, and flow transducers in a highly automated setup for the development of innovative control concepts. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 31.01.2019 KW - Process Analytical Technology KW - Hydrogenation KW - Compact NMR Spectroscopy KW - Online-NMR spectroscopy PY - 2019 AN - OPUS4-47310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Maiwald, Michael A1 - Villajos Collado, José Antonio T1 - Metal-organic framework compounds as hydrogen storage materials to enhance the safety, capacity, and efficiency of hydrogen refueling stations N2 - Gas adsorption is based on physical properties between gases and solid materials, enriching the surface with packed gas molecules with a higher density than in the bulk phase. For using this mechanism as a gas storage strategy, highly porous materials are necessary since large surfaces in small volumes can provide the storage system with a higher density than the gas phase. In the case of hydrogen gas, the interaction forces with solid surfaces are generally low at room temperature but can increase considerably at low operating temperatures. As a counterpart, the storage pressure is considerably lower than that necessary by traditional gas compression. Amongst ultra-porous adsorbent materials for hydrogen cryoadsorption, metal-organic frameworks (MOFs) are a group of remarkable solids made from metallic nodes linked by organic molecules exhibiting a wide variety of composition, geometry, porous properties, and chemical functionality. The scientific community focused in the last years on enhancing both the specific area of materials and the interaction energy to extend the storage properties of cryoadsorption to ambient-temperature and use it as hydrogen storage mechanisms in vehicles. However, the found difficulty in achieving ultra-porous structures with high-enough interaction energies decreased this research interest in the last years. However, for a stationary application like hydrogen refueling stations, where space and weight are not such limits as in vehicles, cryoadsorption can still be considered a feasible candidate for hydrogen storage. Cryoadsorption is the only fast and fully reversible approach to store hydrogen at similar density values as compressed gas. Cryogenic operation is a technological challenge, but first, liquid nitrogen is cheap, and second, it is less energy-demanding than hydrogen liquefaction, which is indeed considered as feasible for transportation and storage. Cryoadsorption involves lower pressure than compressed gas, increasing safety in the storage facilities, but additional research on the construction materials properties is necessary to better understand their behavior in contact with hydrogen at cryogenic temperatures. However, the knowledge of all these mechanisms is important to identify the improvement opportunities based on, probably, the interphase between different solutions. To achieve the set project goals, this internal research report describes the work packages realised within the framework of the project. KW - Metal-organic frameworks (MOFs) KW - Hydrogen Storage KW - Reversible Hydrogen Storage KW - Hydrogen Fuelling Stations KW - Croyo-starage KW - High-pressure volumetric analyzer (HPVA) PY - 2021 SP - 1 EP - 48 CY - Berlin AN - OPUS4-53582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kazlagić, Anera A1 - Stephan, D. A1 - Ostermann, Markus A1 - Possolo, A. A1 - Vogl, Jochen T1 - Fingerprinting Portland cements by means of 87Sr/86Sr and 143Nd/144Nd isotope ratios and geochemical profiles N2 - This study uses conventional 87Sr/86Sr and 143Nd/144Nd isotope and interelement ratios of Ca, Sr, K, Mn, Mg and Ti as fingerprints for provenancing ordinary Portland cements (OPC). Herein, the first database of Sr and Nd isotope ratios investigated in OPCs, stemming from 29 cement plants located worldwide, was created. The results show that the Sr isotope ratios of OPCs are higher than those of seawater from the observed geological period. The spread of 143Nd/144Nd in OPCs is not as large as the spread for 87Sr/86Sr isotope ratios. However, the combination of both Sr and Nd isotope ratios provides the potential for distinguishing between cements of different production sites. Most of the OPCs investigated have measurable differences in their 87Sr/86Sr and 143Nd/144Nd isotope ratios, which can be employed as a valuable analytical fingerprinting tool. In the case of equivocal results, divisive hierarchical clustering was employed to help overcome this issue. The construction of geochemical profiles allowed the computing of suitably defined distances between cements and clustering them according to their chemical similarity. By applying this methodology, successful fingerprinting was achieved in 27 out of the 29 ordinary Portland cements that were analysed. KW - Elemental fingerprints KW - Geochemistry KW - Portland cement KW - Sr and Nd isotope analysis KW - Statistical analysis PY - 2023 DO - https://doi.org/10.1680/jadcr.23.00018 SN - 0951-7197 VL - 36 IS - 6 SP - 260 EP - 271 PB - Emerald Publishing Limited AN - OPUS4-57979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gugin, Nikita A1 - Villajos Collado, José Antonio A1 - Dautain, O. A1 - Maiwald, Michael A1 - Emmerling, Franziska T1 - Optimizing the Green Synthesis of ZIF-8 by Reactive Extrusion Using In Situ Raman Spectroscopy N2 - We report the scale-up of a batch solid synthesis of zeolitic imidazolate framework-8 (ZIF-8) for reactive extrusion. The crystalline product forms in the extruder directly under the mixture of solid 2-methylimidazole and basic zinc carbonate in the presence of a catalytic amount of liquid. The process parameters such as temperature, liquid type, feeding rate, and linker excess were optimized using the setup specifically designed for in situ Raman spectroscopy. Highly crystalline ZIF-8 with a Brunauer–Emmett–Teller (BET) surface area of 1816 m2 g–1 was quantitatively prepared at mild temperature using a catalytic amount of ethanol and a small excess of the linker. Finally, we developed a simple and comprehensive approach to evaluating the environmental friendliness and scalability of metal–organic framework (MOF) syntheses in view of their large-scale production. KW - Mechanochemistry KW - In situ Raman KW - Large-scale processing KW - Metal−organic frameworks KW - Twin-screw extrusion (TSE) PY - 2023 DO - https://doi.org/10.1021/acssuschemeng.2c07509 SN - 2168-0485 VL - 11 IS - 13 SP - 5175 EP - 5183 PB - ACS Publications AN - OPUS4-57366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martins, Ines A1 - Al-Sabbagh, Dominik A1 - Bentrup, U. A1 - Marquardt, Julien A1 - Schmid, Thomas A1 - Scoppola, E. A1 - Kraus, Werner A1 - Stawski, Tomasz A1 - de Oliveira Guilherme Buzanich, Ana A1 - Yusenko, Kirill A1 - Weidner, Steffen A1 - Emmerling, Franziska T1 - Formation Mechanism of a Nano-Ring of Bismuth Cations and Mono-Lacunary Keggin-Type Phosphomolybdate N2 - A new hetero-bimetallic polyoxometalate (POM) nano-ring was synthesized in a one-pot procedure. The structure consists of tetrameric units containing four bismuth-substituted monolacunary Keggin anions including distorted [BiO8] cubes. The nano-ring is formed via self-assembly from metal precursors in aqueous acidic medium. The compound (NH4)16[(BiPMo11O39)4] ⋅ 22 H2O; (P4Bi4Mo44) was characterized by single-crystal X-ray diffraction, extended X-ray absorption fine structure spectroscopy (EXAFS), Raman spectroscopy, matrix-assisted laser desorption/ionisation-time of flight mass spectrometry (MALDI-TOF), and thermogravimetry/differential scanning calorimetry mass spectrometry (TG-DSC-MS). The formation of the nano-ring in solution was studied by time-resolved in situ small- and wide-angle X-ray scattering (SAXS/WAXS) and in situ EXAFS measurements at the Mo−K and the Bi−L3 edge indicating a two-step process consisting of condensation of Mo-anions and formation of Bi−Mo-units followed by a rapid self-assembly to yield the final tetrameric ring structure. KW - Bismuth KW - In situ EXAFS KW - In situ SAXS/WAXS KW - Lacunary Keggin ion KW - Polyoxometalates KW - Self-assembly PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546823 DO - https://doi.org/10.1002/chem.202200079 SN - 0947-6539 VL - 28 IS - 27 SP - 1 EP - 7 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54682 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Compact NMR Spectroscopy in the field: A Versatile PAT Tool for Production of Specialty Chemicals N2 - Companies of chemical industry find themselves more often in a rapidly changing environment, e.g., due to variability of raw material quality or energy costs and efficiency. Process optimization and new process concepts become more and more important. For example, flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds like exothermic reactions with high heat dissipation. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. Field studies in modular and conventional production plant setups show promising results gaining process knowledge for further optimization. NMR appeared as preeminent online analytical method and allow using a modular data analysis approach, which can even serve as reliable reference method for further calibration-dependent PAT applications (e.g., NIR spectroscopy). Based on experiences from these field studies an improved analyzer enclosure setup was developed and built, including the option of a secondary method besides NMR spectroscopy. Integrated control systems allow for a flexible implementation based on the available automation infrastructure at the chemical plant or pilot plant setup. In the future, fully integrated and intelligently interconnecting “smart” PAT systems and processes have the potential speed up the setup of production equipment for chemicals and pharmaceuticals and therefore help to reduce the time-to-market. T2 - Practical Applications of NMR in Industry Conference (PANIC) 2022 CY - La Jolla, CA, USA DA - 16.10.2022 KW - Process Analytical Technology KW - Benchtop NMR KW - Modular production PY - 2022 AN - OPUS4-56090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Compact NMR Spectroscopy in the field: A Versatile PAT Tool for Production of Specialty Chemicals N2 - Chemical companies must find new paths to successfully survive in a changing environment, especially by utilizing the potential of digital technologies. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Therefore, fully automated process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. It was used for direct loop advanced process control and real-time optimization of the process. Field studies in modular and conventional production plants show promising results gaining process knowledge. NMR appeared as preeminent online analytical method and allow using a modular data analysis tool, which even served as reliable reference method for further PAT applications (e.g. NIR spectroscopy). In the future, fully integrated and interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - ProcessNet and DECHEMA-BioTechNet Jahrestagungen 2022 with 13th ESBES Symposium CY - Aachen, Germany DA - 12.09.2022 KW - Process Analytical Technology KW - Benchtop NMR KW - Modular production PY - 2022 AN - OPUS4-55918 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Compact NMR Spectroscopy in the field: A Versatile PAT Tool for Production of Specialty Chemicals N2 - Chemical companies must find new paths to successfully survive in a changing environment, especially by utilizing the potential of digital technologies. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Therefore, fully automated process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. It was used for direct loop advanced process control and real-time optimization of the process. Field studies in modular and conventional production plants show promising results gaining process knowledge. NMR appeared as preeminent online analytical method and allow using a modular data analysis tool, which even served as reliable reference method for further PAT applications (e.g. NIR spectroscopy). In the future, fully integrated and interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - 17. AKPAT Kolloquium 2022 CY - Amersfoort, Netherlands DA - 19.09.2022 KW - Process Analytical Technology KW - Benchtop NMR KW - Modular production PY - 2022 AN - OPUS4-55919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin T1 - Accelerating chemical process development and manufacturing – Design and validation of an integrated NMR micro mixer N2 - The future competitiveness of the process industry and their providers depends on its ability to deliver high quality and high value products at competitive prices in a sustain-able fashion, and to adapt quickly to changing customer needs. The transition of pro-cess industry due to the mounting digitalization of technical devices and their provided data used in chemical plants proceeds. Though, the detailed characteristics and con-sequences for the whole chemical and pharmaceutical industry are still unforeseeable, new potentials arise as well as questions regarding the implementation. As the digitali-zation gains pace fundamental subjects like the standardization of device interfaces or organization of automation systems must be answered. Still, process industry lack of sufficient system and development concepts with commercial advantage from this trend. Compared to traditional batch processes, intensified continuous production allows new and difficult to produce compounds with better product uniformity and reduced con-sumption of raw materials and energy. Flexible (modular) chemical plants can produce various products using the same equipment with short down-times between cam-paigns, and quick introduction of new products to the market. Full automation is a prerequisite to realize such benefits of intensified continuous plants. In continuous flow processes, continuous, automated measurements and closed-loop control of the product quality are required. Consequently, the demand for smart sensors, which can monitor key variables like component concentrations in real-time, is increasing. Low-Field NMR spectroscopy presents itself as such an upcoming smart sensor1,2 (as addressed, e.g., in the CONSENS project3). Systems utilizing such an online NMR analyzer benefits through short development and set-up times when applied to modular production plants starting from a desired chemi-cal reaction3. As an example for such a modular process unit, we present the design and validation of an integrated NMR micro mixer based on computational modelling suited for a desired chemical reaction. This method includes a proper design of a con-tinuous reactor, which is optimized through computational fluid dynamics (CFD) for the demands of the NMR sensor as well as for the given reaction conditions. The system was validated with a chemical reaction process. T2 - Practical Application of NMR in Industry Conference CY - HIlton Head Island, SC, USA DA - 04.03.2019 KW - NMR KW - Benchtop KW - Flow Cell KW - Inline PY - 2019 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-47568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Interlaboratory comparison of low-field NMR spectrometers – Purities at 200 and 10 mmol/L - Preliminary results N2 - Due to its advantages of being a direct comparison method, quantitative NMR spectroscopy (qNMR) becomes more and more popular in industry. While conventional high-field NMR systems are often associated with high investment and operational costs, the upcoming market of permanent-magnet based benchtop NMR systems show a considerable option for a lot of applications. The mobility of these systems allows to bring them more closely to the real production environment, e.g. for at-line quality control. In this work we present an interlaboratory comparison study investigating the qNMR performance of state-of-the-art benchtop NMR spectrometers. Therefore, BAM prepared two samples of a mixture of NMR reference standards tetramethylbenzene (TMB) and tetrachloronitrobenzene (TCNB) at concentration levels of 200 mM and 10 mM. These “ready-to-use” samples were sent to participant laboratories, which performed analysis on their benchtop NMR equipment of different vendors and fields from 43 to 80 MHz. Raw data was reported back and further investigated by using different data analysis methods at BAM. After this very first qNMR comparison study of benchtop NMR spectrometers show promising results, following studies are planned to cover more parts of the qNMR process, e.g. sample preparation and weighing, but also data analysis, as commonly done in similar studies for high-field NMR spectroscopy in industry and metrology. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - qNMR KW - Benchtop NMR KW - Interlaboratory Comparison PY - 2019 AN - OPUS4-47662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tuma, Dirk T1 - Comparison of multi-parameter Helmholtz and molecular-based EoS for the description of the density of a gravimetrically prepared LNG-type mixture N2 - The composition of liquefied natural gas (LNG) depends on the original gas composition and on the process of liquefaction and regasification. Regasified LNG typically has a lower percentage content of N2 and CH4 and a slightly higher percentage of higher alkanes than the original natural gas. The densities of this mixture, at four different temperatures, from 250 to 350 K and pressures up to 20 MPa, were determined using a high-accuracy single-sinker magnetic suspension densimeter at the UVa. The experimental densities were compared to those calculated by different multi-parameter equation of state (EoS) in terms of the reduced Helmholtz energy (AGA8-DC92, GERG-2008 and EoS-LNG), by a truncated virial EoS (SGERG-88), and by other EoS based on the perturbed-chain statistical associating fluid theory (PC-SAFT) and CP-PC-SAFT. T2 - 17th PPEPPD International Conference on Properties and Phase Equilibria for Product and Process Design CY - Bad Gögging, Germany DA - 11.05.2025 KW - LNG KW - High-pressure density KW - Reference equation of state PY - 2025 AN - OPUS4-63524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - NMR Spectroscopy as a PAT tool: Field integration of a laboratory instrument N2 - Companies of chemical industry find themselves more often in a rapidly changing environment, e.g., due to variability of raw material quality or energy costs and efficiency. Process optimization and new process concepts become more and more important. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds like exothermic reactions with high heat dissipation. Highly automated chemical process monitoring along with real-time quality control are prerequisites to such concepts and, thus, should be based on chemical information. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as explosion safety, field communication, and robust evaluation of sensor data. Field studies in modular and conventional production plant setups show promising results gaining process knowledge for further optimization. NMR spectroscopy appeared as preeminent online analytical method and allows using a modular data analysis approach, which can even serve as reliable reference method for further calibration-dependent PAT applications (e.g., NIR or Raman spectroscopy). Based on experiences from earlier field studies an improved field enclosure setup was developed and built, including the option of a secondary analytical method (e.g., optical spectroscopy). Integrated control systems allow for a flexible implementation based on the available automation infrastructure at the chemical plant or pilot plant setup. In the future, modular interconnecting “smart” PAT systems and process equipment have the potential speed up the setup of production equipment for chemicals and pharmaceuticals and therefore help to reduce the time-to-market. T2 - Practical Applications of NMR in Industry Conference (PANIC) CY - Rockville, MD, USA DA - 19.05.2025 KW - Compact NMR spectroscopy KW - Process Analytical Technology KW - Field Integration KW - qNMR PY - 2025 AN - OPUS4-63193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Poelke, B. A1 - Klein, Luise A1 - Hoffmann, H. A1 - Wilke, Olaf A1 - Roloff, A. T1 - Bestimmung von VOC-Emissionen aus Verbraucherprodukten in mikroskaligen Emissionsprüfkammern: Ergebnisse eines Rundversuchs N2 - Die Bestimmung der Anfangskonzentrationen flüchtiger organischer Verbindungen, die innerhalb der ersten Stunden des Gebrauchs aus Verbraucherprodukten emittiert werden, wurde in einem Ringversuch getestet, bei dem Mikro-Kammern verwendet wurden. Neun Labore nahmen an dem Ringversuch teil, der sich aus zwei Teilen zusammensetzte: Im ersten Teil wurde die analytische Leistungsfähigkeit beurteilt. Jedes beteiligte Labor erhielt zwei mit Analyten dotierte Tenax® TA Desorptionsröhrchen zur Qualitätskontrolle (QC). Im zweiten Teil führte jedes Labor Emissionsmessungen über einen Zeitraum von 48 Stunden in Mikro-Kammern mit Volumina von 44 oder 114 ml durch. Als Probenmaterial dienten Stücke eines Regenponchos, der Cyclohexanon, Phenol, 2-Ethylhexanol, Naphthalin und Isophoron in signifikanten Konzentrationen emittierte. Für den QC-Test wurden sehr geringe relative Standardabweichungen (9 14 %) erhalten. Die Ergebnisse der Emissionsmessungen waren ebenfalls sehr gut. In der frühen Phase (0,5 4 Stunden) wurden akzeptable z-Scores (|z| ≤ 2,00) von mindestens sieben Laboren erhalten, nach 24 und 48 Stunden erhielten alle Labore akzeptable z-Scores. KW - Emissionsprüfkammer KW - Ringversuch KW - Verbraucherprodukt KW - VOC-Emission PY - 2025 DO - https://doi.org/10.37544/0949-8036-2025-03-04-71 VL - 85 IS - 03-04 SP - 71 EP - 76 AN - OPUS4-63561 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Soraya A1 - Hülagü, Deniz A1 - Bennet, Francesca A1 - Carl, Peter A1 - Flemig, Sabine A1 - Schmid, Thomas A1 - Schenk, J. A. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf T1 - Electrochemical Immunomagnetic Ochratoxin A Sensing: Steps Forward in the Application of 3,3’,5,5’- Tetramethylbenzidine in Amperometric Assays N2 - Electrochemical methods offer great promise in meeting the demand for user-friendly on-site devices for Monitoring important parameters. The food industry often runs own lab procedures, for example, for mycotoxin analysis, but it is a major goal to simplify analysis, linking analytical methods with smart technologies. Enzyme-linked immunosorbent assays, with photometric detection of 3,3’,5,5’-tetramethylbenzidine (TMB),form a good basis for sensitive detection. To provide a straightforward approach for the miniaturization of the detectionstep, we have studied the pitfalls of the electrochemical TMB detection. By cyclic voltammetry it was found that the TMB electrochemistry is strongly dependent on the pH and the electrode material. A stable electrode response to TMB could be achieved at pH 1 on gold electrodes. We created a smartphonebased, electrochemical, immunomagnetic assay for the detection of ochratoxin A in real samples, providing a solid basis forsensing of further analytes. KW - Ochratoxin A KW - Amperometry KW - Cyclic voltammetry KW - Electrochemistry KW - Immunoassay PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-530421 DO - https://doi.org/10.1002/celc.202100446 N1 - Geburtsname von Riedel, Soraya: Höfs, S. - Birth name of Riedel, Soraya: Höfs, S. VL - 8 IS - 13 SP - 2597 EP - 2606 AN - OPUS4-53042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bornemann-Pfeiffer, Martin A1 - Wolf, Jakob A1 - Meyer, Klas A1 - Kern, S. A1 - Angelone, D. A1 - Leonov, A. A1 - Cronin, L. A1 - Emmerling, Franziska T1 - Standardization and control of Grignard reactions in a universal chemical synthesis machine using online NMR T1 - Standardisierung und Kontrolle von Grignard-Reaktionen mittels Online-NMR in einer universellen chemischen Syntheseplattform N2 - A big problem with the chemistry literature is that it is not standardized with respect to precise operational parameters, and real time corrections are hard to make without expert knowledge. This lack of context means difficult reproducibility because many steps are ambiguous, and hence depend on tacit knowledge. Here we present the integration of online NMR into an automated chemical synthesis machine (CSM aka. “Chemputer” which is capable of small-molecule synthesis using a universal programming language) to allow automated analysis and adjustment of reactions on the fly. The system was validated and benchmarked by using Grignard reactions which were chosen due to their importance in synthesis. The system was monitored in real time using online-NMR, and spectra were measured continuously during the reactions. This shows that the synthesis being done in the Chemputer can be dynamically controlled in response to feedback optimizing the reaction conditions according to the user requirements. N2 - Ein Problem der chemischen Literatur ist die fehlende Standardisierung bezüglich genauer Bedingungen, auch Echtzeit-Korrekturen sind ohne Expertenwissen nur schwer möglich. Dieser Mangel an Details erschwert experimentelle Reproduzierbarkeit, da Schritte oft mehrdeutig sind und daher von implizitem Wissen abhängen. Hier präsentieren wir die Integration von Online-NMR Spektroskopie in eine automatisierte chemische Syntheseplattform (CSM aka. “Chemputer”, unter Verwendung einer universellen Programmiersprache zur Synthese kleiner Moleküle fähig), um eine automatisierte Analyse und Anpassung von Reaktionen im laufenden Betrieb zu ermöglichen. Das System wurde anhand von Grignard-Reaktionen, die aufgrund ihrer Bedeutung für die Synthese ausgewählt wurden, validiert und einem Härtetest unterzogen. Synthesen wurden in Echtzeit mit Online-NMR überwacht, und die Spektren wurden während der Reaktionen kontinuierlich aufgenommen und analysiert. Dies zeigt, dass der Chemputer dynamisch mittels einer Regelung kontrolliert werden kann, um die Reaktionsbedingungen entsprechend den Anforderungen des Benutzers zu optimieren. KW - Grignard reaction KW - NMR spectroscopy KW - Process analytical technology KW - Process control KW - Grignard-Reaktion KW - NMR-Spektroskopie KW - Prozessanalytik KW - Prozesskontrolle PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531260 DO - https://doi.org/10.1002/anie.202106323 SN - 1521-3773 SN - 1433-7851 N1 - Bibliografische Angaben für die deutsche Version: Angewandte Chemie 2021, Jg. 133, S. 1–7, ISSN 0044-8249, ISSN 1521-3757, https://doi.org/10.1002/ange.202106323 - Bibliographic information for the German version: Angewandte Chemie 2021, vol. 133, p. 1–7, ISSN 0044-8249, ISSN 1521-3757, https://doi.org/10.1002/ange.202106323 VL - 60 IS - 43 SP - 1 EP - 6 PB - Wiley-VCH CY - Weinheim AN - OPUS4-53126 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, G. A1 - Marquardt, Julien A1 - Emmerling, Franziska T1 - Structural changes in Ba-compounds of different hardness induced by high-energy ball milling – evidenced by 137Ba NMR and X-ray powder diffraction N2 - Changes in the global bulk and local structures, of three different barium compounds (BaZrO3, BaF2, and BaFCl),were induced by mechanical milling and followed using X-ray powder diffraction (PXRD), subsequent microstructure analysis, and 137Ba solid state NMR spectroscopy. Harder materials like BaZrO3 experience significantly higher structural changes upon milling than softer materials like BaF2. Moreover, soft materials with layered structures, like BaFCl, show a pronounced structural change during the milling process. By combining PXRD and solid state NMR, detailed information on the changes to the global and local structures were obtained, which are of interest for mechanochemical synthesis, mechanically treated catalysts or ionic conductors. KW - Mechanochemistry KW - X-ray diffraction KW - Solid state NMR PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547397 DO - https://doi.org/10.1002/zaac.202200026 SN - 0044-2313 VL - 648 IS - 10 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Contributions Towards Variable Temperature Shielding for Compact NMR Instruments N2 - The application of compact NMR instruments to continuously flowing samples at higher temperatures or exothermically reacting mixtures is limited by the temperature sensitivity of permanent magnets. Typically, such temperature effects directly influence the achievable magnetic field homogeneity and hence measurement quality. The internal-temperature control loop of the magnet and instruments is typically not designed for compensation of such effects. Passive insulation is restricted by the small dimensions within the magnet borehole. Here, we present a design approach for active heat shielding with the aim of variable temperature control of NMR samples for benchtop NMR instruments using a compressed airstream which is variable in flow and temperature. Based on the system identification and surface temperature measurements using an optical thermo-graphy setup, a model predictive control was set up to minimize any disturbance effect on the permanent magnet from the probe or sample temperature. This methodology will facilitate the application of variable-temperature shielding and, therefore, potentially extend the application of compact NMR instruments to flowing samples at higher temperature than the permanent magnet. T2 - 18. Kolloquium AK Prozessanalytik CY - Krefeld, Germany DA - 27.11.2023 KW - Thermostating KW - Benchtop-NMR KW - NMR spectroscopy KW - Process Analytical Technology PY - 2023 AN - OPUS4-58970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Advantages of N2-MICAP-MS for Trace Metal Analysis in Steel N2 - The climate and energy crisis are extreme challenges. One possible solution could be hydrogen technology. Safety is a big concern. Steel used for pipelines and storage is under permanent stress from low temperatures and high pressures. The content of different alloyed metals determines the performance of the steel. Nitrogen microwave inductively coupled atmosphere pressure plasma mass spectrometry (N2-MICAP-MS) is a promising method for trace metal analysis in steel. Nitrogen is cheap and can be generated on site. It has fewer interferences than argon. Additionally, MICAP-MS is very matrix tolerant, proving the matrix-matched calibration expendable. Safety in technology and chemistry is the mission of BAM. Providing reference methods and materials can create trust in future technologies like hydrogen. T2 - SALSA Make and Measure 2022 CY - Berlin, Germany DA - 15.09.2022 KW - Trace analysis KW - Steel KW - Microwave plasma KW - Mass spectrometry KW - Safety PY - 2022 AN - OPUS4-55792 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Olaf T1 - PTR-MS as a tool for the determination of formaldehyde, ammonia and volatile organic sulfur compounds together with VOC N2 - The use of proton-transfer-reaction mass spectrometry (PTR-MS) for the determination of formaldehyde, ammonia and volatile sulfur organic compounds is described and suggestions are made for the application of stationary PTR-MS in a test laboratory. One advantage of PTR-MS compared to TD-GC-MS (thermal desorption gas chromatography mass spectrome-try) is the faster online measurement. Another advantage is the simultaneous determination of formaldehyde, ammonia, very volatile organic compounds (VVOC) and volatile organic com-pounds (VOC) which normally needs four different kinds of sampling. Coupling the PTR-MS with (multiple) air sample canisters or (multiple) emission test chambers would enable a quick analysis of indoor air and material emissions. T2 - Indoor Air Conference 2024 CY - Honolulu, HI, USA DA - 07.07.2024 KW - Proton-transfer-reaction mass spectrometry PY - 2024 AN - OPUS4-60746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Liehr, Sascha T1 - ANNforPAT - Artificial Neural Networks for Process Analytical Technology N2 - This code accompanies the paper "Artificial neural networks for quantitative online NMR spectroscopy" published in Analytical and Bioanalytical Chemistry (2020). KW - Artificial neural networks KW - Automation KW - Online NMR spectroscopy KW - Process industry KW - Real-time process monitoring PY - 2020 UR - https://github.com/BAMresearch/ANNforPAT PB - GitHub CY - San Francisco AN - OPUS4-54481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balderas-Xicohtencatl, R. A1 - Villajos Collado, José Antonio A1 - Casabán, J. A1 - Wong, D. A1 - Maiwald, Michael A1 - Hirscher, M. T1 - ZIF‑8 Pellets as a Robust Material for Hydrogen Cryo-Adsorption Tanks N2 - Cryoadsorption on the inner surface of porous materials is a promising solution for safe, fast, and reversible hydrogen storage. Within the class of highly porous metal−organic frameworks, zeolitic imidazolate frameworks (ZIFs) show high thermal, chemical, and mechanical stability. In this study, we selected ZIF-8 synthesized mechanochemically by twin-screw extrusion as powder and pellets. The hydrogen storage capacity at 77 K and up to 100 bar has been analyzed in two laboratories applying three different measurement setups showing a high reproducibility. Pelletizing ZIF-8 increases the packing density close to the corresponding value for a single crystal without loss of porosity, resulting in an improved volumetric hydrogen storage capacity close to the upper limit for a single crystal. The high volumetric uptake combined with a low and constant heat of adsorption provides ca. 31 g of usable hydrogen per liter of pellet assuming a temperature−pressure swing adsorption process between 77 K − 100 bar and 117 K − 5 bar. Cycling experiments do not indicate any degradation in storage capacity. The excellent stability during preparation, handling, and operation of ZIF-8 pellets demonstrates its potential as a robust adsorbent material for technical application in pilot- and full-scale adsorption vessel prototypes. KW - Hydrogen adsorption storage KW - Metal−organic frameworks KW - ZIF-8 KW - Cryoadsorption KW - Hydrogen Storage KW - MefHySto PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569473 DO - https://doi.org/10.1021/acsaem.2c03719 SN - 2574-0962 SP - 1 EP - 8 PB - ACS Publications CY - Washington DC AN - OPUS4-56947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin T1 - Design and validation of an integrated NMR micro mixer N2 - Intensified continuous processes are in focus of current research. Compared to traditional batch processes, intensified continuous production allows the synthesis of new and difficult producible compounds with better product uniformity and reduced consumption of raw materials and energy. Flexible (modular) chemical plants can produce various products using the same equipment with short down-times between campaigns, and quick introduction of new products to the market. Full automation is a prerequisite to realize such benefits of intensified continuous plants. In continuous flow processes, continuous, automated measurements and closed-loop control of the product quality are required. Consequently, the demand for smart sensors, which can monitor key variables like component concentrations in real-time, is increasing. Low-Field NMR spectroscopy presents itself as such an upcoming smart sensor (as addressed, e.g., in the CONSENS project1,2). Systems utilizing such an online NMR analyzer benefits through short development and set-up times when applied to modular production plants starting from a desired chemical reaction. As an example for such a modular process unit, we present the design and validation of an integrated NMR micro mixer based on computational modelling suited for a desired chemical reaction. This method includes a proper design of a continuous reactor, which is optimized through computational fluid dynamics (CFD) for the demands of the NMR sensor as well as for the given reaction conditions. The system was validated with a chemical reaction process. T2 - NMRPM Konferenz 2019 CY - Kaiserslautern, Germany DA - 31.01.2019 KW - NMR KW - Mikromischer KW - Flow Chemie KW - Reaktionsmonitoring PY - 2019 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-47334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT ED - Tuma, Dirk ED - Weide, T. ED - Rasmusson, H. T1 - MefHySto - Metrology for advanced hydrogen storage solutions N2 - The “Metrology for Advanced Hydrogen Storage Solutions” (MefHySto) project is a European initiative addressing the need for large-scale energy storage solutions, that is crucial for the successful transition to renewable energy sources. The main objective of this project was to develop and provide metrological standards and validated techniques for the storage and utilization of hydrogen. Hydrogen is increasingly recognized as an important component in the future energy system due to its ability to store and supply energy during peak demand periods when renewable sources, such as solar and wind, are not generating power. KW - Water electrolysis KW - Thermophysical properties KW - Fuel cell KW - Hydrogen storage PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-625952 DO - https://doi.org/10.5281/zenodo.12684898 SP - 1 EP - 40 PB - ERIG European Research Institute for Gas and Energy Innovation a.i.s.b.l. CY - Bruxelles AN - OPUS4-62595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Haferkamp, Sebastian A1 - Paul, Andrea A1 - Michalchuk, Adam A1 - Emmerling, Franziska T1 - Unexpected polymorphism during a catalyzed mechanochemical Knoevenagel condensation N2 - The transformation of a base-catalyzed, mechano-assisted Knoevenagel condensation of mono-fluorinated benzaldehyde derivatives (p-, m-, o-benzaldehyde) with malonodinitrile was investigated in situ and in real time. Upon milling, the para-substituted product was found to crystallize initially into two different polymorphic forms, depending on the quantity of catalyst used. For low catalyst concentrations, a mechanically metastable phase (monoclinic) was initially formed, converting to the mechanically stable phase (triclinic) upon further grinding. Instead, higher catalyst concentrations crystallize directly as the triclinic product. Inclusion of catalyst in the final product, as evidenced by mass spectrometric analysis, suggests this complex polymorphic pathway may be due to seeding effects. Multivariate analysis for the in situ Raman spectra supports this complex formation pathway, and offers a new approach to monitoring multi-phase reactions during ball milling. KW - Ball milling KW - C-C coupling KW - In situ KW - Mechanochemistry KW - Multivariate data analysis PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-481872 DO - https://doi.org/10.3762/bjoc.15.110 SN - 1860-5397 VL - 15 SP - 1141 EP - 1148 PB - Beilstein Insitut CY - Frankfurt am Main AN - OPUS4-48187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas T1 - Analyzing large μ-FTIR data sets in search of microplastics N2 - Working towards a comprehensive understanding of introduction pathways, number, and fate of micro¬plastics in the environment, suitable analytical methods are a precondition. Micro-spectroscopic methods are probably the most widely used techniques. Besides their ability to measure single spectra of a particle or fiber, most modern FTIR- and Raman microscopes are also capable of two-dimensional imaging. This is very appealing to microplastics research because it allows to simultaneously characterize the analytes chemically as well as their size (distribution) and shape. Two-dimensional imaging on extensive sample areas with FTIR-micros¬copes is facilitated by focal plane array (FPA) detectors resulting in large data sets comprised of up to several million spectra. With numbers too large for manual inspection of each individual spectrum, automated data evaluation is inevitable. Identifying different polymers based on the comparison with known reference spectra (library search) has proven to be a suitable approach. For that purpose, FTIR-spectra of common plastics can be collected to create an individual reference library. To Supplement this ‘targeted analysis’, looking for known substances via library search, an exploratory approach was tested. Principal component analysis (PCA) proved to be a helpful tool to drastically reduce the size of the data set while maintaining the significant information. Subsequently, cluster analysis was used to find groups of similar spectra. Spectra found in different clusters could be assigned to different polymer types. The variation observed within clusters gives a hint on chemical variability of microplastics of the same polymer found in the sample. Spectra labeled according to the respective cluster/polymer type were used to build a classification model which allowed to quickly predict the polymer type based on the FTIR spectrum. Classification was tested on a second, independent data set and results were compared to the spectral library search procedure. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Microplastics KW - FTIR KW - Principal component analysis (PCA) PY - 2019 AN - OPUS4-47658 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Advanced spectroscopic methods for fluorine microanalysis in lithium-ion batteries N2 - To address the challenges of the climate crisis, multiple solutions for sustainable energy sources and storage systems are needed. One such solution is lithium-ion batteries (LIBs). Currently, 5 to 30 % of LIBs are discarded immediately after manufacturing. The homogeneous distribution of all materials used in the coating of cathodes and anodes is critical for the quality of LIBs. Furthermore, during formation i.e., the first steps of the charge/discharge cycling, the solid-electrolyte interphase forms on the anode particles, which has a huge impact on the performance. The same happens to some extent on the cathode, forming the cathode-electrolyte interphase. Fluorinated polymers and electrolytes are used in the manufacturing of LIBs. The electrolyte in particular is prone to degradation during formation and aging of the batteries. The interface of the cathode material with the aluminum current collector is also a critical point where degraded fluorine components cause pitting corrosion and at the same time promote passivation of the metal foil. Monitoring the spatial distribution of fluorine on these surfaces and interfaces is essential for sustainable LIB production. T2 - SALSA Kick-Off Meeting CY - Berlin, Germany DA - 11.04.2024 KW - Lithium Ion Batteries KW - solid microanalysis KW - depth-profiling KW - fluorine PY - 2024 AN - OPUS4-60199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Abad Andrade, Carlos Enrique T1 - Advances and Applications of Molecular Absorption Spectrometry: from Non-Metals to Isotope Analysis N2 - The present work covers two main aspects of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS), an analytical technique for elemental trace analysis. First, a comprehensive mechanistic study of molecule formation in graphite furnaces is presented, which is a key step into the recovery of analytical signals. For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in HR-CS-GFMAS. A zirconium coating catalyzes the CaF formation, and its structure was investigated. The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. Here a mechanism is proposed, where ZrO2 works as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. Second, analytical methods were developed by using HR-CS-MAS as detector for non-metals and isotope analysis. Therefore, the determination of organic absorbable chlorine in water, the quantification of fluorine in consume care products with declared perfluorinated ingredients, and the determination of sulfur content in crude oils were investigated. Finally, the high resolution of the instrumentation allows to measure isotopic shifts with high precision in some observed molecular spectra. Consequently, the molecular spectra of enriched isotopes of boron and magnesium were investigated, establishing so the potential of HR-CS-MAS for the accurate and precise determination of isotopic amount ratios. Zusammenfassung Die vorliegende Arbeit befasst sich mit zwei zentralen Aspekten der High-Resolution-Continuum-Source-Molekülabsorptionsspektrometrie mit Graphitrohrtechnik (HR-CS-GFMAS), einer Analysetechnik für elementare Spurenanalyse. Der erste Teil der Arbeit umfasst eine mechanistische Studie zur Molekülbildung auf Graphitoberflächen. Dies ist ein wichtiger Schritt, um analytische Signale zu entdecken. Dazu wurde die Molekülbildung von CaF analysiert, welches für die indirekte, analytische Bestimmung von Fluor in HR-CS-GFMAS genutzt wird. Die CaF Bildung wurde mittels einer Beschichtung aus Zirconium katalysiert und deren Struktur analysiert. Die Kinetik dieser Reaktion wurde durch Beobachtung des jeweiligen Molekülspektrums bei verschiedenen Atomisierungstemperaturen beobachtet. Ein Arrheniusplot zeigte für Fluor (n = 1) eine Reaktion Pseudo-erster Ordnung. Ein Übergangszustand wurde über die mit Zirconium überzogene Grafitoberfläche isoliert und seine Struktur mittels spektroskopischer Methoden Energiedispersive Rasterelektronenmikroskopie / Röntgenspektroskopie (REM-EDX), Röntgenphoto¬elektronenspektroskopie (XPS), Röntgenabsorptionsspektroskopie (XAS) und Raman Spektroskopie untersucht. Auf Grundlage dieser Ergebnisse wird ein Mechanismus vorgeschlagen, bei dem ZrO2 als heterogener Katalysator fungiert; in Folge einer Pyrolysestufe wird ein Übergangszustand des ZrO(OCaF) aktiviert, welcher bei höheren Temperaturen CaF(g) an der Zirconium-Graphitoberfläche freisetzt. Im zweiten Teil der Arbeit werden Analysemethoden entwickelt, in dem HR-CS-MAS als Detektor für Nichtmetalle und Isotopanalyse angewandt wird. Hierfür wurde organisch gebundenes Chlor im Wasser bestimmt, der Fluorgehalt in Pflegeprodukten mit perfluorierten Inhaltsstoffen quantifiziert und der Schwefelgehalt in Erdöl untersucht. Weiterhin ermöglicht die hohe Auflösung der Messgeräte eine präzise Bestimmung der Isotopenverschiebung einiger untersuchter Molekülspektren. Daher wurden die Molekülspektren angereicherter Bor- und Magnesiumisotope untersucht. Auf diese Weise wurde das Potential von HR-CS-MAS für die akkurate und präzise Bestimmung von Isotop-Mengenverhältnissen nachgewiesen. KW - Isotope analysis KW - Non-metals analysis KW - Molecular absorption spectrometry KW - Boron KW - Fluorine KW - Graphite furnace KW - HR-CS-MAS KW - Applied optical spectroscopy PY - 2019 UR - https://hu-berlin.hosted.exlibrisgroup.com/permalink/f/jl2ii5/HUB_UB_ALMA_DS21669801300002882 SP - X EP - 118 CY - Berlin, Germany AN - OPUS4-49891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Horn, Wolfgang A1 - Wilke, Olaf A1 - Richter, Matthias T1 - Round robin tests of odour and VOC emissions from building products – What have we learned so far? N2 - Emission testing of volatile organic compounds (VOC) and odour from materials and products is commonly based on emission test chamber measurements. These measurements are often the basis of mandatory or voluntary labelling procedures. To ensure the comparability of results from different testing laboratories their performance must be verified. For this purpose, round robin tests (RRTs) are conducted. Bundesanstalt für Materialforschung und - prüfung (BAM) offers such a RRT every two years using well characterised test materials with defined VOC emissions. In addition to the VOC quantification, the evaluation of odour is also implemented in the round robin tests. At the beginning, only perceived intensity (PI) was tested but over the years also the acceptance evaluation was considered. In principle, the results of PI and acceptance evaluation are comparable. The advantage of PI is the lower number of panel members necessary for one evaluation. T2 - Healthy Buildings 2023 Europe CY - Aachen, Germany DA - 11.06.2023 KW - Perceived intensity KW - VOC-emission KW - Poficiency test KW - Chamber test KW - Odour PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580001 SP - 434 EP - 436 PB - ISIAQ (International Society of Indoor Air Quality and Climate) CY - Herndon, VA, USA AN - OPUS4-58000 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Compact NMR spectroscopy: A versatile tool for automated continuous-flow production of chemicals and pharmaceuticals N2 - Um in einem veränderten Umfeld erfolgreich bestehen zu können, müssen Chemieunternehmen neue Pfade beschreiten. Dazu gehört insbesondere das Potential digitaler Technologien. Mit flexiblen, modularen chemischen Vielzweck-Produktionsanlagen lassen sich häufig wechselnde Produkte mit kürzeren Vorlauf- und Stillstandzeiten zwischen den Kampagnen und dennoch hoher Qualität realisieren. Intensivierte, kontinuierliche Produktionsanlagen erlauben auch den Umgang mit schwierig zu handhabenden Substanzen. Grundvoraussetzung für solche Konzepte ist eine hochautomatisierte "chemische" Prozesskontrolle zusammen mit Echtzeit-Qualitätskotrolle, die "chemische" Informationen über den Prozess bereitstellt. In einem Anwendungsbeispiel wurde eine pharmazeutische Lithiierungsreaktion aus einer modularen Pilot-Anlage betrachtet und dabei die Vorzüge eines vollautomatischen NMR-Sensors untersucht. Dazu wurde ein kommerziell erhältliches Benchtop-NMR-Spektrometer mit Permanentmagnet auf die industriellen Anforderungen, wie Explosionsschutz, Feldkommunikation und vollautomatischer, robuster Datenauswertung angepasst. Der NMR-Sensor konnte schließlich erfolgreich im vollautomatischen Betrieb nach fortschrittlichen Regelkonzepten und für die Echtzeitoptimierung der Anlage getestet werden. Die NMR-Spektroskopie erwies sich als hervorragende Online-Methode und konnte zusammen mit einer modularen Datenauswertung sehr flexibel genutzt werden. Die Methode konnte überdies als zuverlässige Referenzmethode zur Kalibrierung konventioneller Online-Analytik eingesetzt werden. Zukünftig werden voll integrierte und intelligent vernetzte "smarte" Sensoren und Prozesse eine kontinuierliche Produktion von Chemikalien und Pharmazeutika mit vertretbaren Qualitätskosten möglich machen. T2 - Niederfeld-NMR-Spektroskopie: Ein universelles Werkzeug für automatisierte, kontinuierliche Produktion von Chemikalien und Pharmazeutika T2 - Fresenius-Lecture Hochschule Reutlingen CY - Reutlingen, Germany DA - 18.12.2019 KW - Prozessindustrie KW - Smarte Sensoren KW - Online-NMR-Spektroskopie KW - Digitalisierung KW - Datenanalyse PY - 2019 AN - OPUS4-50111 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Compact NMR Spectroscopy: A Versatile Tool for Automated Continuous-Flow Production of Chemicals and Pharmaceuticals N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - GDCh-Kolloquium der Universität Ulm CY - Ulm, Germany DA - 28.11.2019 KW - Process Analytical Technology KW - Reaction Monitoring KW - Online NMR Spectroscopy KW - Process Industry KW - Automation PY - 2019 AN - OPUS4-49855 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Compact NMR Spectroscopy: A Versatile Tool for Automated Continuous-Flow Production of Chemicals and Pharmaceuticals N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - Global PAT Meeting Bayer AG CY - Berlin, Germany DA - 12.11.2019 KW - Process Analytical Technology KW - Reaction Monitoring KW - Online NMR Spectroscopy KW - CONSENS PY - 2019 AN - OPUS4-49602 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abele, M. A1 - Kern, Simon T1 - Industrielle Anwendungen der Niederfeld-NMR-Spektroskopie für die Prozess- und Qualitätskontrolle von Silanen N2 - Trialkoxysilane haben sich in den vergangenen Jahren als vielseitig einsetzbare Organosilane erwiesen. Die Einsatzgebiete erstrecken sich vom Witterungsschutz von Bauwerken über haftvermittelnde Eigenschaften in der Glasfaserindustrie, bei Dicht- und Klebstoffen, in Farben und Lacken bis hin zur Modifizierung von polymeren Werkstoffen. Kommerzielle Benchtop-NMR-Spektrometer haben das Potential auch im Bereich der Silanchemie als Online-Methode zur Reaktionsüberwachung und für die Qualitätskontrolle eingesetzt zu werden. Interessante NMR-Kerne für die oben genanntem Produkte sind 1H und 29Si. In einer gemeinsamen Forschungskooperation zwischen EVONIK und BAM wurde anhand verschiedener Fallstudien die Anwendbarkeit der Niederfeld-NMR-Spektroskopie zur chemischen Analyse von Silanen evaluiert. Im Zuge der Fallstudien wurde gezeigt, wie Niederfeld-NMR-Spektroskopie die Möglichkeiten der Konzentrationsmessung auf neue Anwendungsgebiete erweitert, in denen bestehende Technologien wie z. B. NIR, Raman, UV/VIS, etc. mangels Referenzdaten nicht quantitativ eingesetzt werden können. Fallstudie 1: Oligomerisierung Eine Fallstudie setzte dazu an, den Hydrolyse- und Kondensationsverlauf mit einer geeigneten Online-NMR-Analytik zu beobachten, den Reaktionsfortschritt der Hydrolyse und Kondensation auf dieser Basis besser zu verstehen und zu optimieren. Zu diesem Zweck werden durch Zugabe von Wasser zunächst die Alkoxysubstituenten eines Trialkoxysilans hydrolysiert und entsprechende Silanole gebildet. Diese können dann über eine SiOH-Funktion an den zu modifizierenden Werkstoff anbinden und über weitere Silanolgruppen unter Ausbildung von Siloxaneinheiten vernetzen. Fallstudie 2: Spaltung von cyclischen Silanverbindungen In einer weiteren Fallstudie wurde die Kinetik der Aufspaltungen einer cyclischen Silanverbindung untersucht. Die Online-NMR-Analytik kam hierbei sowohl im Labor als auch in der industriellen Produktionsanlage zum Einsatz. Hierfür wurde eine vollständig automatisierte Einhausung verwendet, welche den Einsatz eines kommerziellen NMR-Spektrometers in explosionsgeschützten Bereichen ermöglicht. Fallstudie 3: Qualitätskontrolle für Produktmischungen von Trialkoxysilanen Für Produktmischungen eines Trialkoxysilans und weiteren Bestandteilen wie u. a. org. Stabilisatoren, Organozinnverbindungen, eines aromatischen Amins und org. Peroxide wurden quantitative 1H-Spektren akquiriert und eine automatische Auswertungsmethode basierend auf Indirect Hard Modeling (IHM) entwickelt. Für die Nebenkomponenten, deren Stoffmengenanteile bis zu 3 Mol-% betragen, wurden durch die zugrunde gelegte Methode typischerweise korrekte experimentelle Stoffmengenanteile gefunden, die weniger als 0,2 Mol-% vom Referenzwert abweichen. T2 - 15. Kolloquium Arbeitskreis Prozessanalytik CY - Marl, Germany DA - 25.11.2019 KW - Prozessanalytik KW - Qualitätskontrolle KW - Silane KW - Online-NMR-Spektroskopie KW - Trialkoxysilane PY - 2019 AN - OPUS4-49825 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wander, Lukas A1 - Vianello, A. A1 - Vollertsen, J. A1 - Westad, F. A1 - Braun, Ulrike A1 - Paul, Andrea T1 - Exploratory analysis of hyperspectral FTIR data obtained from environmental microplastics samples N2 - Hyperspectral imaging of environmental samples with infrared microscopes is one of the preferred methods to find and characterize microplastics. Particles can be quantified in terms of number, size and size distribution. Their shape can be studied and the substances can be identified. Interpretation of the collected spectra is a typical problem encountered during the analysis. The image datasets are large and contain spectra of countless particles of natural and synthetic origin. To supplement existing Analysis pipelines, exploratory multivariate data analysis was tested on two independent datasets. Dimensionality reduction with principal component analysis (PCA) and uniform manifold approximation and projection (UMAP) was used as a core concept. It allowed for improved visual accessibility of the data and created a chemical two-dimensional image of the sample. Spectra belonging to particles could be separated from blank spectra, reducing the amount of data significantly. Selected spectra were further studied, also applying PCA and UMAP. Groups of similar spectra were identified by cluster analysis using k-means, density based, and interactive manual clustering. Most clusters could be assigned to chemical species based on reference spectra. While the results support findings obtained with a ‘targeted analysis’ based on automated library search, exploratory analysis points the attention towards the group of unidientified spectra that remained and are otherwise easily overlooked. KW - Microplastics KW - FTIR KW - Exploratory analysis PY - 2020 DO - https://doi.org/10.1039/c9ay02483b VL - 12 IS - 6 SP - 781 EP - 791 PB - Royal Society of Chemistry AN - OPUS4-50396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maiwald, Michael T1 - Impulse zur Nutzung smarter Sensoren und Aktoren - Aktuelle Aktivitäten und Anwendungsbeispiele N2 - Eine der vielen Vorzüge smarter Sensoren und Aktoren ist die Bereitstellung zusätzlicher Informationen, auf die zukünftig neben bereits verwendeten Signalen zugegriffen werden kann. In verschiedenen Arbeitskreisen wird dieser Themenbereich im wechselseitigen Austausch mit Geräte- und Softwareherstellern und Forschungseinrichtungen vorangetrieben. In diesem Beitrag wird der aktuelle Stand der Diskussionen anhand von Beispielen erläutert. KW - Smarter Sensor KW - Smarter Aktor KW - Digitale Transformation KW - Prozessindustrie KW - NAMUR PY - 2020 DO - https://doi.org/10.17560/atp.v62i1-2.2468 SN - 2364-3137 VL - 62 IS - 1-2 SP - 72 EP - 79 PB - Vulkan-Verlag GmbH (Verlag) CY - Essen AN - OPUS4-50443 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Informationsmanagement in der Prozessindustrie auf Basis von Labor- und Produktionsdaten N2 - Die Wettbewerbsfähigkeit der Prozessindustrie basiert auf der Sicherung der geforderten Produktqualität bei einer optimalen Nutzung von Anlagen, Rohstoffen und Energie. Ein Weg zur wissensbasierten Produktion führt über die Betrachtung der wesentlichen Apparate-, Prozess- und Freigabedaten aus Betrieben und Labors. Das Potenzial dieser Daten wird heute vielfach noch nicht konsequent für ein umfassendes Verständnis der Produktion genutzt. Neben Fragen zur Datenerfassung, Datenkonnektivität und Datenintegrität müssen solche Daten für eine ganzheitliche Prozessanalyse zunächst mit Kontextinformationen zusammengebracht werden. Datenquellen enthalten Zeitwertpaare, aber auch diskrete Daten aus LIMS (Laboratory Information Management Systems) oder ELN (Electronic Laboratory Notebooks) und werden zunehmend durch 2D- und 3D-Daten aus der Chromatographie-Massenspektrometrie oder bildbasierter Analytik ergänzt. Für die automatisierte Merkmalsextraktion, etwa zur Extraktion chemischer Informationen aus den oben genannten Datenquellen werden multivariate Werkzeuge und Algorithmen genutzt. Multivariate Statistiken wie PCA (Principle Component Analysis), PLS (Partial Least Squares) und LDA (Latent Discriminant Analysis) bilden die erste Grundlage für die Datenanalyse. Für diese Verfahren sind heute Datenvorbehandlungsschritte nötig. Die Modellbildung geschieht manuell und ist sehr aufwendig. Können diese Daten im Zeitalter von ML (Machine Learning) und KI (Artificial Intelligence) anderweitig sinnvoll genutzt werden und ohne klassische Modellbildung? Die Bezeichnung „Big Data“ als Voraussetzung für datengetriebene Auswerteverfahren ist für die Prozessindustrie allerdings unpassend, denn auch bei mengenmäßig großen Datensätzen liegen für Kampagnen typischerweise nur Informationen über einige Batches mit einer Serie von Messdaten vor, die genügend Varianz für eine datengetriebene Auswertung aufweisen – nicht vergleichbar mit den Datenmengen im WWW oder von großen Internet-Konzernen. T2 - Bio-PAT-Workshop, Aktuelle Entwicklungen im Bereich PAT & Softsensortechnologien CY - Berlin, Germany DA - 04.12.2019 KW - Prozessindustrie KW - Digitalisierung KW - Datenanalyse KW - Datenvorbehandlung KW - Multivariate Datenanalyse PY - 2019 AN - OPUS4-49942 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas T1 - Prozess-Spektroskopie: Analytik für die kontinuierliche Produktion N2 - Der Vortrag zeigt aktuelle Entwicklungen und Betätigungsfelder des Fachbereichs Prozessanalytik zum Thema Automation in der Analytik. Dies Umfasst die Laborautomation am Beispiel der Probenpräparation für die Röntgenfluoreszenzanalyse und moderne Synthesekonzepte in der organischen Chemie. Außerdem wird die Rolle der Prozessanalytik in der kontinuierlichen Produktion thematisier. Als Anschauungsgegenstand dienen die Überwachung einer Hydroformylierung mittels Raman- und NMR-Spektroskopie und der Einsatz eines NMR-Sensors in einer modularen Produktionsanlage im Pilotmaßstab. T2 - 4. Analytiktag CY - Duisburg, Germany DA - 07.11.2019 KW - NMR-Spektroskopie KW - Raman-Spektroskopie PY - 2019 N1 - Geburtsname von Bornemann-Pfeiffer, Martin: Bornemann, M. - Birth name of Bornemann-Pfeiffer, Martin: Bornemann, M. AN - OPUS4-49579 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Informationsmanagement in der Prozessindustrie auf Basis von Labor- und Produktionsdaten N2 - Ein Weg zur wissensbasierten Produktion führt über die Betrachtung der wesentlichen Apparate-, Prozess- und Freigabedaten aus Betrieben und Labors. Das Potenzial dieser Daten wird heute vielfach noch nicht konsequent für ein umfassendes Verständnis der Produktion genutzt. Neben Fragen zur Datenerfassung, Datenkonnektivität und Datenintegrität müssen solche Daten für eine ganzheitliche Prozessanalyse zunächst mit Kontextinformationen zusammengebracht werden. Datenquellen enthalten vor allem Zeitwertpaare, die numerisch vorbehandelt und möglichst vollautomatisch ausgewertet werden müssen. Am Beispiel NMR-spektroskopischer Daten wird der Stand der Auswertung mit physikalisch motivierten Modellen, wie z. B. dem IHM erläutert. T2 - Mathematisches Forschungskolloquium, Institut für Mathematik, Universität Rostock CY - Rostock, Germany DA - 02.12.2019 KW - Prozessindustrie KW - Prozesskontrolle KW - Datenanalyse KW - Datenvorbehandlung KW - Chemometrics PY - 2019 UR - https://www.mathematik.uni-rostock.de/veranstaltungen/regelmaessige-veranstaltungen/forschungskolloquium/2019/ AN - OPUS4-49939 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Grümbel, F. T1 - Aktuelle Aktivitäten und Anwendungsbeispiele zur Nutzung Smarter Sensoren N2 - Eine der vielen Vorzüge Smarter Sensoren und Aktoren ist Bereitstellung zusätzlicher Informationen, auf die zukünftig neben den Hauptsignalen zugegriffen werden kann. In den Arbeitskreisen 3.6 und 3.7 wird dieses im wechselseitigen Austausch mit Geräte- und Softwareherstellern und Forschungseinrichtungen vorangetrieben. Wir berichten kurz über den Stand der Diskussionen anhand von Beispielen und möchten in einem Open Space Workshop Meinungen und Ideen aufgreifen. T2 - NAMUR Hauptsitzung 2019 CY - Bad Neuenahr, Germany DA - 07.11.2019 KW - Prozessindustrie KW - Prozesskontrolle KW - Prozessanalytik KW - Smarte Sensoren KW - Industrie 4.0 KW - Digitalisierung PY - 2019 AN - OPUS4-49550 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas T1 - Research in the SALSA Application Lab – Shedding light onto high-fired medieval gypsum mortars N2 - After an introduction into the SALSA lab building and the ideas and sources of inspiration for building up the Application Lab as a spectroscopy lab with a strong focus on imaging and microspectroscopy, a very successful example of an interdisciplinary collaboration between the fields of art technology and analytical sciences is presented. T2 - Make and Measure 2019 CY - Berlin, Germany DA - 25.10.2019 KW - Interdisciplinary research KW - Teaching KW - High-fired medieval gypsum mortars KW - Raman spectroscopy PY - 2019 AN - OPUS4-49623 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmid, Thomas T1 - Raman band widths of anhydrite II reveal the burning history of high‐fired medieval gypsum mortars N2 - An interdisciplinary collaboration between art technology and analytical sciences yielded an approach based on Raman microspectroscopy for the determination of the burning temperatures applied during the production process of high-fired medieval gypsum mortars. Analytical challenges and applications of the approach to examples from the cultural heritage of South Tyrol are presented. T2 - 10th International Congress on the Application of Raman Spectroscopy in Art and Archaeology CY - Potsdam, Germany DA - 03.09.2019 KW - Raman microspectroscopy KW - High-fired medieval gypsum mortars KW - Thermal anhydrite PY - 2019 AN - OPUS4-49624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Maiwald, Michael ED - Meyer, Simon T1 - Voll integrierte und vernetzte Systeme und Prozesse - Perspektive: Smarte Sensorik, Aktorik und Kommunikation N2 - Unternehmen der chemischen Industrie müssen neuen Pfade beschreiten, um in einem veränderten Umfeld erfolgreich bestehen zu können. Dazu gehört insbesondere, das Potenzial digitaler Technologien zu nutzen. Die volle Integration und intelligente Vernetzung von Systemen und Prozessen kommt allerdings nur zögerlich voran. Dieser Beitrag ist ein Loblied auf die Feldebene. Er möchte dazu ermutigen, die Digitalisierung der Prozessindustrie auf Basis smarter Sensorik, Aktorik und Kommunikation ganzheitlicher zu denken und informiert über aktuelle technische Perspektiven, wie das Ein-Netzwerk-Paradigma, Ad-hoc-Vernetzungen, Edge-Computing, FPGAs, virtuelle Maschinen oder Blockchain. Diese geben smarter Sensorik, Aktorik und Kommunikation eine völlig neue Perspektive. KW - Smarte Sensoren KW - Smarte Aktoren KW - Digitalisierung KW - Prozessindustrie KW - Prozess-Sensoren 4.0 PY - 2019 SN - 978-3-8356-7436-3 SP - 28 EP - 40 PB - Vulkan-Verlag GmbH CY - Essen AN - OPUS4-50035 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Compact NMR Spectroscopy: A Versatile Tool for Automated Continuous-Flow Production of Chemicals and Pharmaceuticals N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short down-times between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as , e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. Recently, AI procedures have also been successfully used for NMR data evaluation. In order to overcome the typical limitation of too small data sets from process developments, a new method was tested, which allows a physically motivated multiplication of the available reference data together with context information in order to obtain a sufficiently large data set for the training of machine learning algorithms. In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - Compact NMR: Perspectives for (Bio)process Monitoring CY - Online meeting DA - 14.10.2020 KW - Process Industry KW - Real-time Process Monitoring KW - NMR Spectroscopy KW - Indirect Hard Modelling KW - Modular Production PY - 2020 AN - OPUS4-51430 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Aktuelles zur Technologie-Roadmap "Prozess-Sensoren 4.0" N2 - Die auf der NAMUR Hauptsitzung 2015 vorgestellte Technologie-Roadmap „Prozess-Sensoren 4.0“ zeigt die damaligen Anforderungen an Prozess-Sensoren sowie an deren Kommunikations-fähigkeiten auf. Wir berichten über die Umsetzungen der damaligen Ideen/Thesen aus heutiger Sicht und blicken nach vorn. T2 - Workshop NAMUR-Hauptsitzung 2020 CY - Online meeting DA - 05.11.2020 KW - Prozessindustrie KW - Technologie-Roadmap "Prozess-Sensoren 4.0" KW - NAMUR KW - Automation KW - Prozessanalytik KW - Sensoren PY - 2020 AN - OPUS4-51523 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Paul, Andrea T1 - Multivariate approaches in the evaluation of (hyper)spectral data for microplastics analysis - options and limitations N2 - Die zunehmende Anreicherung von Gewässern und Böden mit Plastikmüll führt zur Anhäufung von mikroskopisch kleinen Plastikpartikeln, sogenannter Mikroplastik (MP). Es werden dringend analytische Methoden benötigt, die helfen MP zu identifizieren und zu quantifizieren. Gegenwärtig kommen dafür hauptsächlich thermoanalytische und mikro¬skopische Verfahren, wie Mikro-Infrarotspektroskopie oder Mikro-Raman zum Einsatz. Letztere sind in der Regel an zeitaufwendige Probenanreicherungen und -aufbereitungen gebunden, es können nur kleine Probenmengen (Mikrogramm) untersucht werden und die Auswertung der erzielten Spektren kann anspruchsvoll sein. Im Rahmen dieser Präsentation werden zwei Ansätze vorgestellt, die über die multi-variate Analyse spektroskopischer Daten i) einen neuen methodischen Ansatz zum Screening von MP in belasteten Böden sowie ii) eine alternative Auswertung großer (Mikro)-spektroskopischer Datensätze ermöglichen. Zunächst wird ein NIR-spektroskopisches Verfahrens vorgestellt, das es gestattet MP bestehend aus Polyethylen, Polyethylenterephthalat, Polypropylen und Polystyrol im Bereich bis zu 0,5 Massenprozent zu detektieren. Aufgrund kurzer Messzeiten und robuster Technik besitzt dieser Ansatz das Potenzial, im Gegensatz zu den thermoanalytischen und mikrospektroskopischen Methoden, größere Probenmengen mit minimaler Vor¬behandlung zu untersuchen. Der zweite Ansatz befasst sich mit der Auswertung großen Datensätze, wie sie typischerweise als Resultat der Mikro-FTIR unter Nutzung moderner FPA-Detektoren erhalten werden. Die Mikro-FTIR-Technik beruht auf der spektralen Aufnahme, Abbildung und an¬schließenden Identifizierung von Schwingungsbanden, die für synthetische Polymere typisch sind. Die Bilddatensätze sind groß und enthalten Spektren von unzähligen Partikeln natürlichen und synthetischen Ursprungs. Zur Ergänzung bestehender Ansätze, die z.B. auf Recherchen von Spektren¬bibliotheken basieren, wurde die explorative multivariate Datenanalyse getestet. Als Kernkonzept wurde hierbei die Dimensionalitäts¬reduktion verwendet. Die Ergebnisse stellen nicht nur eine orthogonale Methode zur Kontrolle der Ergebnisse dar, die auf Grundlage einer automatisierten Bibliothekssuche erzielt wurden, sondern ergaben darüber hinaus eine Gruppe von Spektren, die nicht in den vorhandenen Spektrenbibliotheken erfasst wurden. N2 - The increasing enrichment of water bodies and soils with plastic waste leads to the accumulation of microscopic plastic particles, so-called microplastics (MP). There is an urgent need for analytical methods that help to identify and quantify MP. At present, mainly thermo-analytical and microscopic methods such as micro-infrared spectroscopy or micro-Raman are used for this purpose. The latter are usually tied to time-consuming sample enrichment and preparation, only small sample quantities (micrograms) can be examined and the evaluation of the obtained spectra can be demanding. In the context of this presentation, two approaches are presented which, via the multi-variate analysis of spectroscopic data, allow i) a new methodological approach to screening MP in contaminated soils and ii) an alternative evaluation of large (micro)-spectroscopic data sets. First, a NIR spectroscopic method is presented which allows MP consisting of polyethylene, polyethylene terephthalate, polypropylene and polystyrene to be detected in the range of up to 0.5 mass percent. Due to short measurement times and robust technology, this approach has the potential, in contrast to thermo-analytical and micro-spectroscopic methods, to examine larger sample quantities with minimal pre-treatment. The second approach deals with the evaluation of large data sets, as typically obtained as a result of micro-FTIR using modern FPA detectors. The micro-FTIR technique is based on the spectral recording, imaging and subsequent identification of vibration bands typical of synthetic polymers. The image data sets are large and contain spectra of numerous particles of natural and synthetic origin. Exploratory multivariate data analysis has been tested to complement existing approaches based on e.g. spectrum library searches. The core concept used was dimensionality reduction. The results not only represent an orthogonal method for checking the results obtained by an automated library search, but also revealed a group of spectra that were not recorded in the existing spectrum libraries. T2 - analytica conference 2020 CY - Online meeting DA - 19.10.2020 KW - Microplastics KW - Multivariate Datenanalyse KW - NIR KW - Hyperspectral data PY - 2020 AN - OPUS4-51516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Interlaboratory comparison of benchtop NMR spectrometers – Purities at 200 and 10 mmol/L N2 - Due to its advantages of being a direct comparison method, quantitative NMR spectroscopy (qNMR) becomes more and more popular in industry. While conventional high-field NMR systems are often associated with high investment and operational costs, the upcoming market of permanent-magnet based benchtop NMR systems show a considerable option for a lot of applications. The mobility of these systems allows to bring them more closely to the real production environment, e.g. for at-line quality control. In this work we present an interlaboratory comparison study investigating the qNMR performance of state-of-the-art benchtop NMR spectrometers. Therefore, BAM prepared two samples of a mixture of NMR reference standards tetramethylbenzene (TMB) and tetrachloronitrobenzene (TCNB) at concentration levels of 200 mM and 10 mM. These “ready-to-use” samples were sent to participant laboratories, which performed analysis on their benchtop NMR equipment of different vendors and fields from 43 to 80 MHz. Raw data was reported back and further investigated by using different data analysis methods at BAM. After this very first qNMR comparison study of benchtop NMR spectrometers show promising results, following studies are planned to cover more parts of the qNMR process, e.g. sample preparation and weighing, but also data analysis, as commonly done in similar studies for high-field NMR spectroscopy in industry and metrology. T2 - The United States Pharmacopeial Convention (USP) Emerging Technologies Workshop & Roundtable CY - Online meeting DA - 17.11.2020 KW - Quantitative NMR Spectroscopy KW - QNMR KW - Purity KW - Interlaboratory Comparison KW - Low-field NMR Spectroscopy PY - 2020 UR - https://www.cvent.com/events/emerging-technologies-workshop-roundtable-quantitative-nmr-and-digital-data-applications-overview-an/event-summary-f128e4bfbedc48d6946f554ea719d6b1.aspx?dvce=1 AN - OPUS4-51526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Simultaneous multielemental analysis of crude oils by high-resolutions absorption spectrometry N2 - When crude oil arrives at a refinery it needs a lot of processing before it is suitable for cracking into lighter fractions. Sulfur has to be extracted to meet ultra-low sulfur legislation for most of the fuel grades, and desalination is a crucial process as chlorine within salts is corrosive to refinery equipment. Measuring the amounts of sulfur and chlorine within crude oil is the first step in a complex clean-up process. Heavy metals, such as vanadium, nickel and iron need to be removed too. These metals can poison the catalyst used to crack the oil into lighter fractions. This is costly as it reduces the useful life of the catalyst. Like chlorine, heavy metals also have a corrosive effect on the plant. There is some evidence that the presence of some metals in the final product can reduce performance. A fast determination of elements and size of suspended particles is vital for diagnosis and safeguard of refinery equipment. However, sample preparation for current analytical methods consumes precious time and lost particle size information. High-resolution continuum source graphite furnace absorption spectrometry (HR-CS-GFAS) is proposed as a fast analytical method for elemental determination in crude oils and potentially for simultaneous multielement and particle size analysis. This HR-CS-GFAS instrumentation is coupled to a modular simultaneous echelle spectrometer (MOSES) and provides a full optical window with high resolution (from 180 to 900 nm with bandwidth λ/170,000). By using this set-up, it is possible to generate a multiparameter 3D spectral image (atomic and molecular lines, isotopic shift, atomization delay, and intensities). The generated spectral images can be analyzed by multivariate regressions for the elemental and particle size analysis. Additionally, if several atomic and molecular lines are simultaneously measured, they may be used in multi-energy calibration (MEC), a method based on the use of many wavelengths of the same absorbing/emitting entity to improve the accuracy in analytical atomic spectrometry. This MEC approach combined with multivariate image analysis allows the quantification of selected elements (Si, Al, Ni, Fe, V, S, and Cl) and overcomes matrix effects. T2 - Chevron Seminar- Group Chemical Characterization and Atomic Spectroscopy CY - Richmond, CA, USA DA - 22.10.2019 KW - Crude oil KW - Multielemental analysis KW - HR-CS-AAS KW - Optical spectroscopy KW - MOSES PY - 2019 AN - OPUS4-49885 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Origin, Provenance, and Isotope analysis N2 - Is it a parmesan cheese from Italy? Who painted the Mona Lisa? The determination of the place of origin is essential for consumer protection, detection of falsifications, and also to bring justice. All the tangible possess an isotopic fingerprint. However, current technologies are too expensive. We work on the development of fast and low-cost optical instruments and methods for isotope analysis. T2 - Berlin Sciendce Week – Zukunftsorte – Innovation Made in Berlin CY - Berlin, Germany DA - 07.11.2019 KW - Isotope analysis KW - Optical spectroscopy KW - Provenance KW - Iisotopic signature KW - Isotopic fingerprints PY - 2019 AN - OPUS4-49889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Breaking the wall of uncertain origin N2 - Is it a parmesan cheese from Italy? Who painted the Mona Lisa? The determination of the place of origin is essential for consumer protection, detection of falsifications, and also to bring justice. All the tangible possess an isotopic fingerprint. However, current technologies are too expensive. We work on the development of fast and low-cost optical instruments and methods for isotope analysis. T2 - Falling Walls Lab Adlershof CY - Berlin, Germany DA - 27.09.2019 KW - Isotope analysis KW - Optical spectroscopy KW - Provenance PY - 2019 AN - OPUS4-49882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Künstliche Neuronale Netze für quantitative Online-Spektroskopie in der Prozessindustrie – Lästige Modellbildung ade? N2 - Bei Industry 4.0 dreht sich alles um Interkonnektivität, sensorgestützte Prozesssteuerung und datengesteuerte Systeme. Prozessanalysentechnik (PAT) wie die Online-Kernresonanzspektroskopie (NMR) gewinnt zunehmend an Bedeutung, da sie zur Automatisierung und Digitalisierung in der Produktion beiträgt. Eine klassische Auswertung von Prozessdaten und deren Umsetzung in Wissen ist jedoch bisher in vielen Fällen aufgrund der unzureichend großen verfügbaren Datensätze nicht möglich oder nicht wirtschaftlich. Bei der Entwicklung eines automatisierten Verfahrens für die Prozesskontrolle stehen manchmal nur die Basisdaten einer begrenzten Anzahl von Batch-Versuchen aus typischen Produkt- und Prozessentwicklungskampagnen zur Verfügung. Diese Datensätze sind jedoch nicht groß genug, um maschinengestützte Verfahren zu trainieren. Um diese Einschränkung zu überwinden, wurde ein neues Verfahren entwickelt, das eine physikalisch motivierte Multiplikation der verfügbaren Referenzdaten erlaubt, um einen ausreichend großen Datensatz für das Training von maschinellen Lernalgorithmen zu erhalten. Das zugrundeliegende Beispiel einer chemischen Synthese wurde spektroskopisch verfolgt und mit der neuen Methode sowie mit einem physikalisch basierten Modell analysiert, wobei sowohl eine anwendungsrelevante Niederfeld-NMR als auch eine Hochfeld-NMR-Spektroskopie als Referenzmethode verwendet wurde. Künstliche neuronale Netze (ANNs) haben das Potenzial, bereits aus relativ begrenzten Eingabedaten wertvolle Prozessinformationen abzuleiten. Um jedoch die Konzentration unter komplexen Bedingungen (viele Edukte und weite Konzentrationsbereiche) vorherzusagen, sind größere ANNs und damit ein größerer Trainingsdatensatz erforderlich. Wir zeigen, dass ein mäßig komplexes Problem mit vier Edukten unter Verwendung von ANNs in Kombination mit der vorgestellten PAT-Methode (Niederfeld-NMR-Spektroskopie) und mit dem vorgeschlagenen Ansatz zur Erzeugung aussagekräftiger Trainingsdaten bewältigt werden kann. T2 - 16. Kolloquium Arbeitskreis Prozessanalytik CY - Online meeting DA - 23.11.2020 KW - Prozessindustrie KW - Online-NMR-Spektroskopie KW - Industrie 4.0 KW - Künstliche Neuronale Netze KW - Prozessanalytik KW - Digitale Transformation PY - 2020 AN - OPUS4-51647 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian T1 - Analytische Chemie Gusseisen, Gummi, Bodenproben N2 - Die BAM stellt seit über 100 Jahren Referenzmaterialien (RM) her. Seit damals haben sich die Anforderungen an RM stark verändert. Der Artikel gibt einen Einblick in Anforderungen und die Herstellungsweise von Referenzmaterialien. KW - Referenzmaterialien KW - ISO-Guide 35 KW - Boden PY - 2021 SP - 51 EP - 53 AN - OPUS4-53695 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Compact NMR Spectroscopy: A Versatile Tool for Automated Continuous-Flow Production of Chemicals and Pharmaceuticals N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as, e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - USP qNMR Emerging Technologies Workshop & Roundtable CY - Online meeting DA - 17.11.2020 KW - Quantitative NMR spectroscopy KW - Benchtop-NMR KW - Process Analytical Technology PY - 2020 AN - OPUS4-51595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - BAM quality toolbox framework for qNMR N2 - Accreditation of analytical methods, either according to GxP or ISO regulations, requires a comprehensive quality management system. General quality documents are often already in place, which need to be extended by method-specific documentation. In this presentation we like to show an idea of a modular set of standard operating procedures (SOP) specifically developed meeting the requirements for quantitative NMR. The future goal is to collaborate with different accreditated NMR laboratories to compile a universal set of SOP and other quality documents that can be modified and used as a starting point for developing your own quality system for applications of qNMR in a regulated environment. T2 - ValidNMR Workshop at Practical Applications of NMR in Industry Conference (PANIC) CY - Online meeting DA - 22.10.2020 KW - ValidNMR KW - Validation KW - NMR spectroscopy KW - ISO 17025 KW - GxP PY - 2020 AN - OPUS4-51466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Recknagel, Sebastian T1 - Certified reference materials for the determination of cadmium (Cd) in cocoa N2 - BAM has produced three cocoa CRMs certified for cadmium (ERM-BD513 – 515) as tools for checking analytical methods for Cd-determination. KW - Certified reference material KW - Cocoa KW - Cadmium PY - 2021 SP - 4 EP - 4 AN - OPUS4-53694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Klas T1 - Atomkerne zählen - Quantitative NMR-Spektroskopie als vielseitige Methode in Labor und Prozess N2 - Meist präsentieren sich Laboratorien für NMR-Spektroskopie auf den ersten Blick von außen nur wenig einladend. Es lohnt sich aber einen Blick hinein zu riskieren, denn die Methode ist heute unverzichtbar für die analytische Chemie. Die quantitativen Möglichkeiten werden häufig unterschätzt, erfahren allerdings durch den aufstrebenden Markt kompakter Benchtop-NMR-Spektrometer verstärktes Interesse für Anwendungen von der Laborbank bis hin zum Industrieprozess. KW - NMR-Spektroskopie KW - Benchtop-NMR KW - qNMR PY - 2020 UR - https://analyticalscience.wiley.com/do/10.1002/was.000600052 SN - 0016-3538 VL - 64 IS - 10 SP - 28 EP - 30 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-51464 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Tanz der Moleküle: Herkunftsbestimmung mittels optischer Spektroskopie N2 - Wie lässt sich die Herkunft von Rohstoffen, Lebensmitteln oder Umweltschadstoffen einfacher, schneller und kostengünstiger als mit bisherigen Methoden bestimmen? Die Dissertation zeigt auf, dass man das grundlegende physikalische Prinzip einer Isotopverschiebung mit in Adlershof entwickelten Optik-Instrumenten für die Herkunftsbestimmung nutzen kann. Die entwickelte Methode ermöglicht es in Zukunft den Ursprung von Rohstoffen, Lebensmitteln oder Umweltschadstoffen kostengünstiger und wesentlich schneller bestimmen, als dies mit bisherigen Methoden möglich ist. Kann man das grundlegende physikalische Prinzip einer Isotopieverschiebung mit einem Optik-Instrument für die Herkunftsbestimmung nutzen? Carlos Abad hat eine wegweisende Methode entwickelt, die es in Zukunft ermöglicht den Ursprung von Rohstoffen, Lebensmitteln oder Umweltschadstoffen kostengünstiger und wesentlich schneller bestimmen, als dies mit bisherigen Techniken möglich ist. T2 - Dissertationspreis Adlershof 2019 CY - Berlin, Germany DA - 12.02.2020 KW - Herkunftsbestimmung KW - Isotopenanalyse KW - Isotope KW - Optischer Spektroskopie KW - Coltan PY - 2020 AN - OPUS4-51993 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Isotopic analysis by high-resolution optical spectroscopy N2 - Isotope analysis can be used to determine the age and provenance of geological samples or to study dynamic systems like Li-ion batteries. Modern techniques in optical spectrometry allow us a fast and slow-cost isotope analysis. These techniques include high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS) and laser ablation molecular isotopic spectrometry. This seminar will discuss our recent work on precise and accurate isotope analysis of boron, magnesium, and lithium with geology, climate, and energy research applications. T2 - Recent Trends in Chemical Science and Technology, Christian College Chengannur, India CY - Online meeting DA - 29.09.2020 KW - Isotopes KW - Optical spectrometry KW - Machine learning PY - 2020 AN - OPUS4-51997 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Meyer, Klas T1 - Laboratory accreditation as a reliable indicator of technical competence for testing, calibration and measurement organizations – An introduction to ISO/IEC 17025 using the example of qNMR spectroscopy N2 - ISO/IEC 17025 is the worldwide quality standard for testing and calibration laboratories. It is the basis for accreditation by an accreditation body. The current version was published in 2018. Implementing ISO/IEC 17025 as part of laboratory quality initiatives offers both laboratory and business benefits, such as expanding the potential customer base for testing and/or calibration, increasing the reputation and image of the laboratory at national and international level, continuous improvement of the data quality and the effectiveness of the laboratory or creation of a good basis for most other quality systems in the laboratory sector, such as GxP. The main difference between a proper approach to analysis and a formal accreditation is shown in a targeted documentation, especially on the qualification of the personnel, the test equipment and the validation of the analytical methods. Using quantitative NMR spectroscopy as an example, it is shown how accreditation can be carried out and what documentation is required. In our case, we have described the procedure in an SOP ("Determination of the quantitative composition of simple mixtures of structurally known compounds with 1H-NMR spectroscopy") and supported it with a modular system of organizational and equipment SOPs. The special feature is that the accredited method is independent for the choice of the analyte and the matrix and therefore it is possible to operate with a single validated method. In our case, we have proposed three quality levels ("leagues") with different levels of analytical effort, which differ in their measurement uncertainty, in order to simplify the workflow and analysis design. T2 - 9th Annual Practical Applications of NMR in Industry Conference (PANIC) CY - Online meeting DA - 17.10.2021 KW - Quantitative NMR Spectroscopy KW - qNMR KW - Accreditation KW - ISO 17025 KW - ISO/IEC 17025 KW - PANIC PY - 2021 AN - OPUS4-53564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Compact NMR Spectroscopy: A Versatile Tool for Automated Continuous-Flow Production of Chemicals and Pharmaceuticals N2 - Chemical companies must find new paths to successfully survive in a changing environment. The potential of digital technologies belongs to these. Flexible and modular chemical plants can produce various high-quality products using multi-purpose equipment with short downtimes between campaigns and reduce time to market for new products. Intensified continuous production plants allow for difficult to produce compounds. Therefore, fully automated “chemical” process control along with real-time quality control are prerequisites to such concepts and thus should be based on “chemical” information. The advances of a fully automated NMR sensor were exploited, using a given pharmaceutical lithiation reaction as an example process within a modular pilot plant. A commercially available benchtop NMR spectrometer was integrated to the full requirements of an automated chemical production environment such as, e.g., explosion safety, field communication, and robust evaluation of sensor data. It was thereof used for direct loop advanced process control and real-time optimization of the process. NMR appeared as preeminent online analytical tool and allowed using a modular data analysis tool, which even served as reliable reference method for further PAT applications. In future, such fully integrated and intelligently interconnecting “smart” systems and processes can speed up the high-quality production of specialty chemicals and pharmaceuticals. T2 - ACHEMA Pulse 2021 CY - Online meeting DA - 15.06.2021 KW - Process Analytical Technology KW - NMR spectroscopy KW - Benchtop-NMR PY - 2021 AN - OPUS4-52822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bornemann-Pfeiffer, Martin T1 - Additively manufactured Flow Cells for Inline Mixing and Reaction Monitoring with Low-Field NMR Spectroscopy N2 - The demand for increasing product diversity in the chemical process industry calls for new production processes that enable greater flexibility. Therefore, plants are needed that produce significant quantities for market supply that can be scaled up to several tons per year. Compared to traditional batch processes, intensified continuous production enables not only flexibility but also the production of compounds that are difficult to produce. Custom-designed small-scale reactors significantly improve heat and mass transfer through micro mixing and can improve safety, e.g. in the case of high grade exothermic or high-pressure reactions, and might play an important role for customized, modular production facilities.1 Combined with optimally designed flow cells, compact NMR instruments currently present promising analytical tools for use in flow chemistry applications.2,3 In recent process monitoring applications, the flow cell and the mixing unit are usually separated parts leading to a severe time delay between mixing and first data acquisition. In this work, we present a comprehensive workflow for the design of a flow cell−mixer combination based on CFD simulation and other design principles.4 Due to the increasing opportunities in additive manufacturing of ceramics, it was possible to realize an optimized SMX-type mixer with a fully integrated NMR flow cell (cf. Fig. 1). Validation studies exhibited 1H NMR spectra with a quality comparable to common NMR glass tubes. So far, the mixing performance of the system has been evaluated for different mass flow rates within the intended working range of 5–120 seconds region and compared to ideally mixed samples. Thus, the integrated flow cell−static mixer combination can be used for different purposes such as evaluation of fluid properties, equilibration studies, or reaction monitoring of two instantaneously mixed samples. The ceramic flow cell was additively manufactured and analyzed through x-ray microtomography revealing surface characteristics due to the manufacturing process (cf. Fig. 2). Furthermore, the working range of the whole system was characterized leading to an operational specification for further applications. In summary, the role of custom-designed components for modular, chemical production, amongst other essential factors like fast development of reliable evaluation models is discussed. References [1] Bornemann-Pfeiffer et al., Chem. Ing. Tech. (2021), 93: 1–10 [2] Kern et al., Anal. Bioanal. Chem. (2018) 410: 3349–3360 [3] Kern et al., Anal. Bioanal. Chem. (2019) 411: 3037–3046 [4] Bornemann et al., Ind. Eng. Chem. Res. (2019), 58: 19562−19570 T2 - EUROPACT - European Conference on Process Analytics and Control Technology CY - Online meeting DA - 15.11.2021 KW - Process analytical technology KW - NMR spectroscopy KW - Additive manufacturing KW - Computational fluid dynamics PY - 2021 AN - OPUS4-53804 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Isotope analysis by high-resolution optical spectroscopy: a tool for planetary science N2 - Isotope analysis can be used to determine the age and provenance of geological samples. Modern techniques in optical spectrometry allow us a stand-off isotope analysis. This seminar will discuss how planetary science with the next Moon and Mars missions drive optical spectrometry into precise and accurate isotope analysis and how BAM will contribute. T2 - Adlershofer Kolloquium CY - Online meeting DA - 19.05.2020 KW - Provenance KW - Dating KW - Isotopes KW - Optical spectroscopy KW - Isotopic shift KW - Planetary science PY - 2020 AN - OPUS4-51995 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Broszies, T. T1 - Remelting Miwo - Recycling von Mineralwolldämmstoffen, die im Schmelzwannenverfahren hergestellt werden N2 - Rückgebaute Mineralwolledämmstoffe und Baustellenverschnitte werden in der Regel deponiert und damit als Rohstoffe dem Markt entzogen. Ziel dieses Projektes ist es darzulegen, dass das Recycling von Glas- und Steinwolle im großmaßstäblich volumenrelevanten Umfang für das Schmelzwannenverfahren technisch umsetzbar und ökonomisch und ökologisch vorteilhaft ist. Neben verfahrenstechnischen Herausforderungen, gilt es die wirtschaftliche in-situ-Identifikation unbekannter Mineralwolle zu ermöglichen. Dazu wird auf erste erfolgversprechende Tastversuche mit spektroskopischen Methoden weiter aufgebaut. T2 - 18. Projektetage der Bauforschung CY - Online meeting DA - 09.11.2021 KW - Mineralwolle KW - Circular Economy KW - NIR KW - RFA PY - 2021 UR - https://www.zukunftbau.de/veranstaltungen/projektetage-der-bauforschung/rueckblicke#c8553 AN - OPUS4-53982 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Advances and Applications of Molecular Absorption Spectrometry: from Non-Metals to Isotope Analysis N2 - Wie kann Nicht-Messbares messbar gemacht werden? Die Antwort der Dissertation auf diese zentrale Frage der analytischen Chemie lautet: die Anwendung der hochauflösenden optischen Spektroskopie der diatomischen Moleküle. In der Arbeit wird in einem ersten Schritt in Grafitöfen, die wie Chemiereaktoren funktionieren, und durch die Anwendung verschiedener analytischer Methoden die diatomische Molekülbildung nachvollzogen. In einem zweiten Schritt werden die aufgedeckten Mechanismen auf die Bestimmung von Nichtmetallen und die Analyse von Isotopen angewendet. Die Isotopenanalytik ist das zukunftsweisendes Herzstück der Dissertation und von alltäglicher und politischer Relevanz: Mittels dieser Technik lässt sich die Herkunft von Lebensmitteln aber auch Chemiewaffen kostengünstiger und wesentlich schneller bestimmen als mit bisherigen Methoden der Massenspektrometrie. Möglich ist die Bestimmung, da alles um uns herum aus Atomen verschiedener Elemente besteht und die meisten Elemente mehrere Isotope haben. Isotope unterscheiden sich hinsichtlich ihres Gewichts, da sie über eine unterschiedliche Anzahl an Neutronen verfügen. Die Informationen über das Verhältnis von schweren und leichten Isotopen lässt sich nutzen, um zu bestimmen wo etwas entstanden ist. Jeder Ort auf unserem Planeten hat seinen persönlichen Element- und Isotopenanteil (Isotopenfingerabdruck). Das in der Arbeit angewandte Instrument misst das Verhältnis indirekt und nutzt hierzu die Interaktion zwischen Licht und Materie. Für das schwerere Isotop wird mehr Licht/Energie benötigt, um es in Bewegung zu bringen, als für das leichtere. Diese kleinen Unterschiede an Energie, die wir dafür aufwenden müssen, werden gemessen und ermöglichen die Herkunftsbestimmung. Damit leistet die Arbeit nicht nur einen wichtigen Beitrag zur Grundlagenforschung in der analytischen Chemie, sondern kann mit den aufgezeigten Ergebnissen auch Anwendung in den Bereichen Verbraucherschutz, Umweltforschung und Waffenkontrolle finden. N2 - The present work covers two main aspects of high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS), an analytical technique for elemental trace analysis. First, a comprehensive mechanistic study of molecule formation in graphite furnaces is presented, which is a key step into the recovery of analytical signals. For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in HR-CS-GFMAS. A zirconium coating catalyzes the CaF formation, and its structure was investigated. The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. Here a mechanism is proposed, where ZrO2 works as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. Second, analytical methods were developed by using HR-CS-MAS as detector for non-metals and isotope analysis. Therefore, the determination of organic absorbable chlorine in water, the quantification of fluorine in consume care products with declared perfluorinated ingredients, and the determination of sulfur content in crude oils were investigated. Finally, the high resolution of the instrumentation allows to measure isotopic shifts with high precision in some observed molecular spectra. Consequently, the molecular spectra of enriched isotopes of boron and magnesium were investigated, establishing so the potential of HR-CS-MAS for the accurate and precise determination of isotopic amount ratios. T2 - Applied Photonics Award 2020 CY - Jena, Germany DA - 22.09.2020 KW - Herkunftsbestimmung KW - Isotopenanalyse KW - Isotope KW - Optischer Spektroskopie PY - 2020 AN - OPUS4-51996 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - Recent Trends in Inexpensive Lithium Isotopic Analysis N2 - Lithium exists in two stable isotopes, 6Li and 7Li. The ratio of these in every ore varies depending on the geological history of the sample, thus providing a tool for fingerprinting the distinct origin of Li containing samples. Determination of the exact isotope ratio for e.g. designation of provenance today relies on expensive and bulky instrumentation such as multi `collector inductively coupled plasma mass spectrometry` (MC-ICP-MS). These instruments, however, are known to bear pitfalls in the characterization of particular elements including Lithium. BAM recently developed two alternative analytical devices for this task, solely relying on inexpensive optical spectroscopy in combination with state-of-the-art multivariate data analysis such as Machine learning algorithms. Both techniques have been comprehensively studied using certified reference materials and comparing the results to MC-ICP-MS results and could be shown to result in comparable figures of merit, paving the way for a more general accessibility to provenance determination instrumentation. The results also pave the way towards even further simplification of the laboratory infrastructure demands and to further include additional elements into the isotopic fingerprinting methodology. T2 - Lithium-Days CY - Halle, Germany DA - 06.12.2021 KW - Lithium KW - Isotopes KW - Optical Spectroscopy PY - 2021 AN - OPUS4-53966 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fricke, F. A1 - Mahmood, S. A1 - Hoffmann, J. A1 - Brandalero, M. A1 - Liehr, Sascha A1 - Kern, Simon A1 - Meyer, Klas A1 - Kowarik, Stefan A1 - Westerdicky, S. A1 - Maiwald, Michael A1 - Hübner, M. T1 - Artificial Intelligence for Mass Spectrometry and Nuclear Magnetic Resonance Spectroscopy N2 - Mass Spectrometry (MS) and Nuclear Magnetic Resonance Spectroscopy (NMR) are critical components of every industrial chemical process as they provide information on the concentrations of individual compounds and by-products. These processes are carried out manually and by a specialist, which takes a substantial amount of time and prevents their utilization for real-time closed-loop process control. This paper presents recent advances from two projects that use Artificial Neural Networks (ANNs) to address the challenges of automation and performance-efficient realizations of MS and NMR. In the first part, a complete toolchain has been developed to develop simulated spectra and train ANNs to identify compounds in MS. In the second part, a limited number of experimental NMR spectra have been augmented by simulated spectra to train an ANN with better prediction performance and speed than state-of-theart analysis. These results suggest that, in the context of the digital transformation of the process industry, we are now on the threshold of a possible strongly simplified use of MS and MRS and the accompanying data evaluation by machine-supported procedures, and can utilize both methods much wider for reaction and process monitoring or quality control. T2 - 2021 Design, Automation & Test in Europe Conference & Exhibition (DATE) CY - Online meeting DA - 01.02.2021 KW - Industry 4.0 KW - Cyber-Physical Systems KW - Artificial Neural Networks KW - Mass Spectrometry KW - Nuclear Magnetic Resonance Spectroscopy PY - 2021 UR - www.date-conference.com SN - 978-3-9819263-5-4 SP - 615 EP - 620 PB - Research Publishing AN - OPUS4-52180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - How Online NMR Spectroscopy Accelerates Chemical Process Development and Manufacturing – From Automated Spectral Analysis to Integrated NMR Micro Reactors N2 - Accelerating chemical process development and manufacturing along with quick adaption to changing customer needs means consequent transformation of former batch to continuous (modular) manufacturing processes. These are justified by an improved process control through smaller volumes, better heat transfer, and faster dynamics of the examined reaction systems. As an example, for such modular process units we present the design and validation of an integrated nuclear magnetic resonance (NMR) micro mixer tailor‐made for a desired chemical reaction based on computational modelling. The micro mixer represents an integrated modular production unit as an example for the most important class of continuous reactors. The quantitative online NMR sensor represents a smart process analytical field device providing rapid and non‐invasive chemical composition information without need for calibration. We describe the custom design through computational fluid dynamics (CFD) for the demands of the NMR sensor as well as for the given reaction conditions. The system was validated with an esterification reaction as an example for a chemical reaction process. Systems utilizing such an online NMR analyser benefits through short development and set‐up times based on “modular” spectral models. Such models can simply be built upon pure component NMR spectra within minutes to a few hours (i.e., assignment of the NMR signals to the components) instead of tedious DoE calibrations runs. We present a range of approaches for the automated spectra analysis moving from statistical approach, (i.e., Partial Least Squares Regression) to physically motivated spectral models (i.e., Indirect Hard Modelling and Quantum Mechanical calculations). The approach was validated for typical industrial reactions, such as hydrogenations or lithiations. T2 - Wissenschaftliches Kolloquium des Leibniz-Institut für Katalyse e. V. an der Universität Rostock CY - Rostock, Germany DA - 09.10.2019 KW - Process Analytical Technology KW - Reaction Monitoring KW - Online NMR Spectroscopy KW - Data Analysis KW - Digitization KW - Catalysis PY - 2019 AN - OPUS4-49238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - ISO-Guide 35 in der Praxis eines RM-Herstellers N2 - Der ISO-Guide 35 beschreibt die notwendigen Schritte zur Herstellung von zertifizierten Referenzmaterialien. Anhand praktischer Beispiele wird die Umsetzung des Guide 35 in der BAM dokumentiert. T2 - DAkkS-Begutachterschulung Modul E zur Akkreditierung von Eignungsprüfungsanbietern und Referenzmaterialherstellern CY - Online meeting DA - 04.02.2021 KW - ISO-Guide 35 KW - Referenzmaterial-Herstellung KW - ZRM PY - 2021 AN - OPUS4-52099 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Phukphatthanachai, P. A1 - Panne, Ulrich A1 - Traub, Heike A1 - Pfeifer, Jens A1 - Vogl, Jochen T1 - Quantification of sulphur in copper and copper alloys by GDMS and LA-ICP-MS, demonstrating metrological traceability to the international system of units N2 - The quantification of the sulphur mass fraction in pure copper and copper alloys by GDMS and LA-ICP-MS revealed a lack of traceability mainly due to a lack of suitable certified reference materials for calibrating the instruments. Within this study GDMS and LA-ICP-MS were applied as routine analytical tools to quantify sulphur in copper samples by applying reference materials as calibrators, which were characterized for their sulphur mass fraction by IDMS beforehand. Different external calibration strategies were applied including a matrix cross type calibration. Both techniques with all calibration strategies were validated by using certified reference materials (others than those used for calibration) and good agreement with the reference values was achieved except for the matrix cross type calibration, for which the agreement was slightly worse. All measurement results were accompanied by an uncertainty statement. For GDMS, the relative expanded (k = 2) measurement uncertainty ranged from 3% to 7%, while for LA-ICP-MS it ranged from 11% to 33% when applying matrix-matched calibration in the sulphur mass fraction range between 25 mg kg-1 and 1300 mg kg-1. For cross-type calibration the relative expanded (k = 2) measurement uncertainty need to be increased to at least 12% for GDMS and to at least 54% for LA-ICP-MS to yield metrological compatibility with the reference values. The so obtained measurement results are traceable to the international system of units (SI) via IDMS reference values, which is clearly illustrated by the unbroken chain of calibrations in the metrological traceability scheme. KW - Sulfur KW - Copper KW - GDMS KW - LA-ICP-MS KW - Uncertainty KW - Traceability KW - SI PY - 2021 DO - https://doi.org/10.1039/d1ja00137j SN - 0267-9477 VL - 36 IS - 11 SP - 2404 EP - 2414 PB - Royal Society of Chemistry AN - OPUS4-53412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Ultrasonic coda wave monitoring of concrete structures: First experiences with large-scale experiments and real structures N2 - Ultrasonic monitoring, making use of the sensitivity of the coda of repeated transmission meas-urements to changes in stress, temperature, moisture, as well as localized or distributed damage, has gotten at-tention in structural health monitoring (SHM) research recently. Analysis methods such as coda wave inter-ferometry (CWI), including its nonlinear extension, have been shown to be able to measure ultrasonic wave velocity changes with a 1∙10-5 resolution, while indicators such as cross-correlation or cross-coherence have been used to distinguish between reversible and irreversible changes. Several small- and large-scale laboratory experiments have demonstrated that stress changes in structures can be captured or damage detected in a very early stage. The use of this technique for pre-warning before failure are currently under investigation, as well as detailed research on the physical causes and the connection between ultrasonic wave properties and materi-al/structural behavior. Recently, several of large-scale laboratory and real structures have been instrumented with embedded ultrasonic transducers to gather experience and evidence on how to use this technology in re-al-world applications. Preliminary results from installations on a new bridge, an existing bridge, a tunnel, a la-boratory earthquake test as well as a historic stadium in Germany, Poland, and the United States, respectively, are presented. Environmental influences (mainly temperature) and validation by load tests are discussed. T2 - IABMAS 2020 CY - Online meeting DA - 11.04.2021 KW - Ultrasound KW - Monitoring KW - Coda wave interferometry KW - Concrete KW - Bridges PY - 2021 AN - OPUS4-54167 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Practical procedure for the precise measurement of geometrical tendon positions in concrete with ultrasonic echo N2 - Existing concrete structures were usually designed for lifetimes of several decades. The current and urgently required efforts to increase sustainability and protect the environment will likely result in extended service lives up to 100 years. To achieve such objectives, it is required to assess structures over their entire lifecycles. Non-destructive testing (NDT) methods can reliably support the assessment of existing structures during the construction, operational, and decommissioning phases. One of the most important and safety-relevant components of a prestressed concrete structure are the tendons. NDT methods such as the ultrasonic echo method are suitable for both the detection and the localization of the tendons, i.e., the measurement of their geometrical position inside the component. The uniqueness of structures, concrete heterogeneity, and varying amounts of secondary components such as the reinforcement represent obstacles in the application of these methods in practice. The aim of this contribution is to demonstrate a practicable procedure, that can be used in the field to determine the parameters required for the measuring data analysis without extensive knowledge about the investigated components. For this purpose, a polyamide reference specimen is used to show which steps are required to obtain reliable imaging information on the position of tendons from the measurement data. The procedure is then demonstrated on a concrete test specimen that covers various relevant and practice-oriented test scenarios, such as varying tendon depths and component thicknesses. T2 - International Conference on Concrete Repair, Rehabilitation and Retrofitting (ICCRRR 2022) CY - Cape Town, South Africa DA - 03.10.2022 KW - Validation KW - Non-destructive testing KW - Ultrasonic KW - Reconstruction KW - Concrete KW - Tendon duct PY - 2022 AN - OPUS4-55999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Niederleithinger, Ernst A1 - Wang, Xin A1 - Epple, Niklas A1 - Schumacher, T. A1 - Ahmend, S. A1 - Klikowicz, P. ED - Yokota, H. ED - Frangopol, D. W. T1 - Ultrasonic coda wave monitoring of concrete structures: First experiences with large-scale experiments and real structures N2 - Ultrasonic monitoring, making use of the sensitivity of the coda of repeated transmission meas-urements to changes in stress, temperature, moisture, as well as localized or distributed damage, has gotten at-tention in structural health monitoring (SHM) research recently. Analysis methods such as coda wave inter-ferometry (CWI), including its nonlinear extension, have been shown to be able to measure ultrasonic wave velocity changes with a 1∙10-5 resolution, while indicators such as cross-correlation or cross-coherence have been used to distinguish between reversible and irreversible changes. Several small- and large-scale laboratory experiments have demonstrated that stress changes in structures can be captured or damage detected in a very early stage. The use of this technique for pre-warning before failure are currently under investigation, as well as detailed research on the physical causes and the connection between ultrasonic wave properties and materi-al/structural behavior. Recently, several of large-scale laboratory and real structures have been instrumented with embedded ultrasonic transducers to gather experience and evidence on how to use this technology in re-al-world applications. Preliminary results from installations on a new bridge, an existing bridge, a tunnel, a la-boratory earthquake test as well as a historic stadium in Germany, Poland, and the United States, respectively, are presented. Environmental influences (mainly temperature) and validation by load tests are discussed. KW - Coda wave interferometry KW - Structural health monitoring KW - Ultrasound KW - Concrete KW - Bridges PY - 2021 SN - 978-0-367-23278-8 DO - https://doi.org/10.1201/9780429279119-345 SP - 2525 EP - 2531 PB - Taylor & Francis CY - London, UK AN - OPUS4-54168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Ultraschallprüfung von Verschlussbauwerken im Salinar N2 - Zu jedem Endlager gehört die Entwicklung eines Verschlusskonzept. Im Endlager Morsleben und an anderer Stelle werden in Abhängigkeit vom Wirtsgestein verschiedene Materialien und Bauweisen für Streckenverschlüsse entwickelt und in großem Maßstab erprobt. Hierzu gehören auch Maßnahmen der Qualitätssicherung, die Informationen über Ausführung und Zustand der Versuchsbauwerke liefern. Hierzu werden von der Bundesanstalt für Materialforschung und -prüfung (BAM) für verschiedene Forschungsvorhaben und Prüfaufträge Methoden und Geräte getestet, verbessert und vor Ort unter Tage eingesetzt. Die hier beschriebenen Verfahren lassen sich auch zu Untersuchungen im Wirtsgestein anwenden. T2 - Tage der Standortauswahl CY - Freiberg/S., Germany DA - 11.02.2021 KW - Endlager KW - Verschlussbauwerke KW - Qualitätssicherung KW - Ultraschall PY - 2021 AN - OPUS4-54165 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Geophysical methods delivering input to geostatistical methods for geotechnical site characterization N2 - Geophysical methods are able to contribute significantly to geotechnical site characterization. In-situ parameters are collected and gaps between boreholes or other direct tests are filled with information. However the limited resolution has to be considered and the indirect geophysical parameters have to be translated into something geotechnically useful. Moreover, the limitations have to be evaluated when including geophysical data into geostatistical models. If done properly, the use of geophysics will help in an efficient and effective site characterization. A comprehensive overview on existing geophysical (mostly seismic) methods is given as well as information on the calibration of geophysical against geotechnical parameters, pitfalls and limitations and some hints how to include these data into geostatistical/geotechnical models. T2 - ICGoES International Conference on Geologicalk Engineering and Geosciences CY - Yogyakarta, Indonesia DA - 21.09.2022 KW - Geophysics KW - Geostatistics KW - Geotechnics PY - 2022 AN - OPUS4-55806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Würth, Christian A1 - Frenzel, Florian A1 - Weigert, Florian A1 - Andresen, Elina A1 - Grauel, Bettina A1 - Wegner, Karl David T1 - Semiconductor (SCNC) & Upconversion Nanocrystals (UCNC) – Optical Properties, Applications & Challenges N2 - Inorganic nanocrystals with linear and nonlinear luminescence in the ultraviolet, visible, near infrared and shortwave infrared like semiconductor quantum dots and spectrally shifting lanthanide-based nanophosphors have meanwhile found applications in the life and material sciences ranging from optical reporters for bioimaging and sensing over security barcodes to solid state lighting and photovoltaics. These nanomaterials commonly have increasingly sophisticated core/shell particle architectures with shells of different chemical composition and thickness to minimize radiationless deactivation at the particle surface that is usually the main energy loss mechanism [1]. For lanthanide-based spectral shifters, particularly for very small nanoparticles, also surface coatings are needed which protect near-surface lanthanide ions from luminescence quenching by high energy vibrators like O-H groups and prevent the disintegration of these nanoparticles under high dilution conditions. [2,3,4]. The identification of optimum particle structures requires quantitative spectroscopic studies focusing on the key performance parameter photoluminescence quantum yield [5,6], ideally flanked by single particle studies to assess spectroscopic inhomogeneities on a particle-to-particle level for typical preparation methods [7], Moreover, in the case of upconversion nanoparticles with a multi-photonic and hence, excitation power density (P)-dependent luminescence, quantitative luminescence studies over a broad P range are required to identify particle architectures that are best suited for applications in fluorescence assays up to fluorescence microscopy. Here, we present methods to quantify the photoluminescence of these different types of emitters in the vis/NIR/SWIR and as function of Pand demonstrate the importance of such measurements for a profound mechanistic understanding of the nonradiative deactivation pathways in semiconductor and upconversion nanocrystals of different size and particle architecture in different environments. T2 - 27th Annual Meeting of the Slovenian Chemical Society CY - Portoroz-Portorose, Slovenia DA - 21.09.2021 KW - Nano KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Surface chemistry KW - Single particle KW - Brightness KW - NIR KW - Synthesis KW - Semiconductur KW - Quantum dot KW - Nanocrystal KW - SWIR PY - 2021 AN - OPUS4-53723 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph A1 - Hindersmann, I. A1 - Niederleithinger, Ernst T1 - Smart Bridge The duraBASt test bridge equipped with RFID-based sensors N2 - The duraBASt area at the highway intersection “Köln-Ost” is a large test field for road testing. It includes the duraBASt test bridge which is approximately 66 m long and 14.25 m broad. This bridge is part of the “road in the 21st Century” project and is equipped with several sensors for structural health monitoring. This feasibility study is carried out to investigate the prerequisites necessary for the constraction of intelligent bridges in the foture. Embedded sensors are able to measure quantities such as temperature, strain, moisture, corrosion, etc. In the presented work, the focus is set on passive RFID-based sensors. The communication and energy supply are realised by a mobile transmitter through the concrete cover. Hence, no cables or batteries are required. The sensors are designed to withstand the alkaline environment in concrete. Thus, moisture and corrosion values are measurable for several decades. T2 - 10th International Conference on Bridge Maintenance, Safety and Management CY - Online meeting DA - 11.04.2021 KW - RFID based sensors KW - Embedded sensors KW - Bridge Monitoring PY - 2021 DO - https://doi.org/10.1201/9780429279119-321 VL - 2021 SP - 2353 EP - 2358 PB - Taylor & Francis Group CY - London AN - OPUS4-53816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hu, Y. A1 - Neumann, C. A1 - Scholtz, Lena A1 - Turchanin, A. A1 - Resch-Genger, Ute A1 - Eigler, S. T1 - Polarity, intramolecular charge transfer, and hydrogen bond comediated solvent effects on the optical properties of graphene quantum dots N2 - Graphene quantum dots (GQDs) have attracted increasing attention due to their favorable optical properties and have been widely used, e.g., in the biomedical field. However, the properties related to the chemical structure of GQDs, resulting in solventdependent optical properties, still remain unclear. Herein, we present the synthesis of long-wavelength emitting GQDs with a size of about 3.6 nm via a solvothermal method using oxo-functionalized graphene (oxo-G) and p-phenylenediamine as precursors and their structural and surface chemical analysis by transmission electron and atomic force microscopy (TEM; AFM) as well as Fourier-transform infrared, Raman, and X-ray photoelectron spectroscopy (FTIR; Raman; XPS). Subsequently, the influence of solvent polarity and proticity on the optical properties of the as-prepared GQDs bearing –OH, –NH2, –COOH and pyridine surface groups was investigated. Based on the results of the absorption and fluorescence (FL) studies, a possible luminescence mechanism is proposed. The observed solvent-induced changes in the spectral position of the FL maximum, FL quantum yield, and FL decay kinetics in protic and aprotic solvents of low and high polarity are ascribed to a combination of polarity effects, intramolecular charge transfer (ICT) processes, and hydrogen bonding. Moreover, the potential of GQDs for the optical sensing of trace amount of water was assessed. The results of our systematic spectroscopic study will promote the rational design of GQDs and shed more light on the FL mechanism of carbon based fluorescent nanomaterials. KW - Graphene quantum dots KW - Solvent polarity KW - solvent-induced changes KW - Charge transfer PY - 2022 DO - https://doi.org/10.1007/s12274-022-4752-1 SN - 1998-0124 SP - 1 EP - 8 PB - Springer AN - OPUS4-56030 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Recent advances in (ultra)sonic active and passive monitoring of reinforced and prestressed concrete structures N2 - In addition to already established structural monitoring methods such as deformation, inclination or strain gauges or acoustic emission sensors, sonic or ultrasonic monitoring might provide valuable information about the condition or alteration of a structure. Sensors such as geophones, recording ambient noise in the sonic and subsonic frequency range can provide information beyond modal analysis by using interferometric methods. Wave velocities determined by this method are related to the elastic properties and stiffness of material and structure and can be converted into damage indicators. Embedded active ultrasonic transducer networks can provide more detailed insight about deterioration or damages again, using interferometric technologies. This approach is extremely sensible, detecting relative change in velocity on down to 10-5. These methods, including benefits and remaining challenges, are demonstrated using data from a test structure at BAM’s test site demonstrating the case of prestress loss, and data from an actual bridge still under traffic. T2 - International Conference on Concrete Repair, Rehabilitation and Retrofitting (ICCRRR 2022) CY - Cape Town, South Africa DA - 03.10.2022 KW - Monitoring KW - Ultrasonic KW - Non-destructive testing KW - Coda wave KW - Bridge PY - 2022 AN - OPUS4-56000 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Andresen, Elina T1 - Assessing dissolution of upconverting nanoparticles by TEM, EDXS, potentiometry and fluorometry N2 - Inorganic lanthanide-doped upconversion nanoparticles (UCNP) constitute an emerging class of near-infrared (NIR)-excitable luminescent reporters for bioimaging, fluorescence assays, sensors in bioanalysis, and optical thermometry as well as phosphors for photovoltaic and security applications.1 However, the use of UCNPs in bioimaging and cellular studies requires biocompatible particles. One possible cause of UCNP toxicity is the release of potentially harmful fluoride fluoride and lanthanide ions as revealed by dilution studies in aqueous environments, particularly under high dilution conditions.2-5 To address this issue, suitable surface coatings preventing such effects in combination with fast screening methods suited for online in situ analysis are desired. Here we present a systematic study of differently sized β-NaYF4:Yb,Er nanocrystals stabilized with different surface coatings and different hydrophilic ligands varying in binding strength to the surface atoms in various aqueous environments at different temperatures. T2 - E-MRS Fall Meeting 2021 CY - Online meeting DA - 20.09.2021 KW - Dissolution KW - Nanomaterial KW - Upconversion nanoparticle KW - Lanthanide KW - Photoluminescence PY - 2021 AN - OPUS4-56231 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholtz, Lena T1 - Luminescence encoding of polymer microbeads with nanocrystals during polymerization N2 - The Goal & Motivation - Spherical polymer beads - Controlled size in the low µm range - Narrow size distribution - Homogeneous encoding with molecular and nanoscale luminophores (dyes , QDs, platelets etc.) - Sufficient fluorescence - Easy, accessible procedure T2 - GrK Nanohybrid Conference CY - Hamburg, Germany DA - 04.10.2022 KW - Polymerization KW - Nanocrystals KW - Fluorescence KW - Microbeads PY - 2022 AN - OPUS4-56028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Güttler, Arne A1 - Richter, Maria A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - New Reference Materials for the Quantification and Standardization of Fluorescence-based Measurements N2 - Luminescence techniques are amongst the most commonly used analytical methods in the life and material sciences due to their high sensitivity and non-destructive and multiparametric character. Photoluminescence signals are, however, affected by wavelength-, polarization-, and time-dependent instrument specific effect and the compound-specific photoluminescence quantum yield. The former hamper the comparability of fluorescence measurements, while the relative determination of the latter requires suitable quantum yield standards with well-known photoluminescence quantum yields (QY). For the simple correction of instrument specific effects in the wavelength region of 300 nm to 950 nm, the set of the five certified spectral fluorescence standards BAM-F001 – BAM-F005, has been extended to the NIR range by including two new fluorescence standards currently under certification. For the reliable and accurate determination of QY which is the key performance parameter for the comparison of different luminophores, we certified a set of 12 quantum yield standards, which absorb and emit in the wavelength range from 300 nm to 1000 nm. T2 - Methods and Applications in Fluorescence CY - Gothenburg, Sweden DA - 11.09.2022 KW - Luminescence KW - Photoluminescence KW - Fluorescence KW - Quantum yield KW - Certified reference material KW - Standard PY - 2022 AN - OPUS4-55914 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Wegner, Karl David T1 - Luminescent Nanoparticles – From Photophysics to the Measurement of Photoluminescence Quantum Yields N2 - Inorganic nanocrystals with linear and nonlinear photoluminescence in the ultraviolet, visible, near infrared and short-wave infrared like spectrally shifting lanthanide-based nanoparticles (LnNCs) like NaYF4: Yb, Er and semiconductor quantum dots have meanwhile found applications in the life and material sciences ranging from optical reporters for bioimaging and sensing over security barcodes to solid state lighting and photovoltaics. The identification of optimum particle architectures for photonic applications requires quantitative spectroscopic studies, ideally flanked by single particle studies to assess spectroscopic inhomogeneities on a particle-to-particle level for typical preparation methods. In the following, photoluminescence studies of LnNCs are presented, addressing parameters such as particle size, surface coating, and dopant ion concentration as well as excitation power density mandatory for a profound mechanistic understanding of the nonradiative deactivation pathways in these nanocrystals. In addition, methods for the determination of particle brightness and photoluminescence quantum yield in different spectral windows are presented. T2 - Phoenix Colloquium CY - Hannover, Germany DA - 22.06.2023 KW - Semiconductor quantum dot KW - Upconversation nanocrystal KW - Luminescence KW - Quantitative spectroscopy KW - Photophysics KW - Quality assurance KW - Nano KW - Particle KW - Quantum yield KW - Lifetime KW - Standard KW - Reference material KW - Surface analysis KW - Quantification PY - 2023 AN - OPUS4-57797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Luminescent Nanoparticles – Photophysics, Mechanistic Studies, and Applications N2 - Inorganic nanocrystals with linear and nonlinear luminescence in the ultraviolet, visible, near infrared and short-wave infrared like semiconductor quantum dots and spectrally shifting lanthanide-based nanophosphors have meanwhile found many applications in the life and material sciences. This includes optical reporters for bioimaging and sensing, security and authentication barcodes, solid state lighting, converter materials, and photovoltaics. The identification of optimum particle structures requires quantitative spectroscopic studies under application-relevant conditions, focusing on the key performance parameter photoluminescence quantum yield, ideally flanked by single particle studies to assess spectroscopic inhomogeneities on a particle-to-particle level for typical preparation methods. In this context, methods to quantify the photoluminescence of these different nanoscale emitters are shown and utilized as a basis for a profound mechanistic understanding of the nonradiative deactivation pathways in semiconductor and upconversion nanocrystals of different size and particle architecture in different environments. Exemplary for the application potential of such nanomaterials, in addition, the design of optical sensors from different nanomaterials and functional organic dyes is briefly summarized. T2 - CRC 1411 Symposium CY - Nürnberg, Germany DA - 20.03.2023 KW - Semiconductor quantum dot KW - Upconversion nanocrystal KW - Luminescence KW - Quantitative spectroscopy KW - Photophysics PY - 2023 AN - OPUS4-57364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholtz, Lena T1 - Luminescent polymer microbeads - Why and how? N2 - Pitch Talk about the synthesis and applications of polymer microbeads encoded with (luminescent) nanoparticles. T2 - JCF Frühjahrssymposium 2023 CY - Gießen, Germany DA - 21.03.2023 KW - Fluorescence KW - Microbeads KW - Nanocrystals KW - Polymerization PY - 2023 AN - OPUS4-57260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kimani, Martha Wamaitha A1 - Kislenko, Evgeniia A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Fluorescent molecularly imprinted polymer particles for glyphosate detection using phase transfer agents N2 - In this work, molecular imprinting was combined with direct fluorescence detection of the pesticide Glyphosate (GPS). Firstly, the solubility of highly polar GPS in organic solvents was improved by using lipophilic tetrabutylammonium (TBA+) and tetrahexylammonium (THA+) counterions. Secondly, to achieve fluorescence detection, a fluorescent crosslinker containing urea-binding motifs was used as a probe for GPS-TBA and GPS-THA salts in chloroform, generating stable complexes through hydrogen bond formation. The GPS/fluorescent dye complexes were imprinted into 2–3 nm fluorescent molecularly imprinted polymer (MIP) shells on the surface of sub-micron silica particles using chloroform as porogen. Thus, the MIP binding behavior could be easily evaluated by fluorescence titrations in suspension to monitor the spectral changes upon addition of the GPS analytes. While MIPs prepared with GPS-TBA and GPS-THA both displayed satisfactory imprinting following titration with the corresponding analytes in chloroform, GPS-THA MIPs displayed better selectivity against competing molecules. Moreover, the THA+ counterion was found to be a more powerful phase transfer agent than TBA+ in a biphasic assay, enabling the direct fluorescence detection and quantification of GPS in water. A limit of detection of 1.45 μM and a linear range of 5–55 μM were obtained, which match well with WHO guidelines for the acceptable daily intake of GPS in water (5.32 μM). KW - Glyphosate KW - Molecular imprinting KW - Core-shell particles KW - Fluorescent sensors PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555281 DO - https://doi.org/10.1038/s41598-022-16825-9 SN - 2045-2322 VL - 12 IS - 1 SP - 1 EP - 15 PB - Macmillan Publishers Limited CY - London AN - OPUS4-55528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Gawlitza, Kornelia A1 - Wan, Wei A1 - Wagner, Sabine A1 - Rurack, Knut ED - Tiwari, Ashutosh ED - Uzun, Lokman T1 - Fluorescent Molecularly Imprinted Polymers N2 - An ideal sensor system is a combination of a selective receptor, an effective transducer, and a sensitive detector. To utilize molecularly imprinted polymers (MIPs) as responsive recognition phases in sensors, the employment of fluorescent molecules or nanoparticles (NPs) that show prominent changes in their spectroscopic properties after binding of the target molecule in the MIP’s cavity is particularly attractive. Such fluorescent MIPs (fMIPs) act through target-induced quenching, enhancement, or spectral shifts of the fluorescence. This contribution introduces different strategies of incorporation of fluorescent dyes, probes, and NPs into fMIPs. In addition, various sensing mechanisms are reviewed, and depending on the application of the sensor, the different deployable formats, their advantages, drawbacks, and impact will be presented and discussed. KW - Dyes KW - Fluorescence KW - Molecular imprinted polymers KW - Quantum dots KW - Sensors PY - 2017 SN - 978-1-119-33629-7 SP - 89 EP - 128 PB - Scrivener Publishing, WILEY CY - Beverly, MA ET - 1 AN - OPUS4-38798 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Niederleithinger, Ernst ED - Meyendorf, N. ED - Ida, N. ED - Singh, R. ED - Vrana, J. T1 - NDE 4.0 in Civil Engineering N2 - Civil engineering industry is one of the most important industry sectors in the worldwide economy. It contributes significantly to the gross economic product and general employment. Even more important, it provides many of the basic needs of the society (e.g., housing, infrastructure, and protection from natural hazards). The concept of “Industry 4.0” or “Smart Production” has not yet made significant progress in the civil engineering industry. The designing, building, and operating processes are still widely dominated by the exchange of printed documents and drawings. Most objects (buildings and other constructions) are unique, and a large part of the production still requires a large amount of manual labor. As-built documentation and quality assurance are often neglected. Civil engineering is among the industry sectors with the lowest level of digitalization and the lowest gain in productivity. However, this is going to change. In the past decade, several drivers have challenged the ways clients, contractors, and authorities currently operate. These drivers include but are not limited to an increasing demand for serialization and automatization or the mandatory introduction of “Building Information Modeling” (BIM) in public procurement as well as the upcoming use of digital twins. NDE plays an increasing role in quality assurance, condition assessment, and monitoring of structures. However, with very few exceptions, applications are mostly nonstandardized and performed only at selected sites. To change this, the NDT-CE community including manufacturers, service providers, clients, and the scientific community must work consistently on open data formats, interfaces to BIM, standardization, and validated ways for a quantitative use of the results in the assessment of constructions. KW - NDE 4.0 KW - Civil engineering KW - BIM KW - IFC PY - 2021 SN - 978-3-030-48200-8 DO - https://doi.org/10.1007/978-3-030-48200-8 SP - 1 EP - 14 PB - Springer Nature CY - Cham, Switzerland AN - OPUS4-54161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - NDT CE from simple detectors to deep insight and quantitative structural assessment N2 - Non-destructive testing methods are available in civil engineering for decades to estimate concrete properties or to detect flaws and features. But recently we have seen the dawn of next-generation tools, methods, and applications. Some of them will be discussed in the web talk: – Better tools: deeper and more detailed insight into concrete constructions – Better methods: Quantitative use in probabilistic structural assessment – Better rules: Towards standardization, qualification, and certification – Better application: Digitalization and Elimination of the boundaries between NDT, SHM, and BIM: NDT-CE 4.0 Not enough? I might show, how cosmic rays might become a game-changer in NDT-CE. This live webinar record was provided by https://eurostruct.org T2 - Eurostruct Live Talk CY - Online meeting DA - 12.05.2021 KW - NDT-CE KW - Concrete KW - Ultrasound KW - Muons PY - 2021 AN - OPUS4-54158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Miropoltsev, M. A1 - Wegner, Karl David A1 - Häusler, I. A1 - Hodoroaba, Vasile-Dan A1 - Resch-Genger, Ute T1 - Influence of Hydrophilic Thiol Ligands of Varying Denticity on the Luminescence Properties and Colloidal Stability of Quaternary Semiconductor Nanocrystals N2 - Binary photoluminescent semiconductor nanocrystals (quantum dots, QDs) are one of the best studied fluorescent nanomaterials, and their unique optoelectronic properties paved the road to many applications in (bio)nanophotonics, optoelectronics, and photovoltaics. However, concerns related to their toxic constituents like cadmium or lead and the emerging interest in greener chemistry synthesis approaches hamper their future applicability. Interesting alternatives for some applications like biosensing or bioimaging are heavy-metal-free ternary QDs like AgInS2 (AIS), CuInS2 (CIS), and quaternary QDs such as AIS-ZnS (ZAIS). In this context, we explored the effect of ligand denticity on the organic-to-aqueous phase transfer of oleylamine-stabilized ZAIS QDs with the hydrophilic ligands mercaptopropionic acid (MPA), dihydrolipoic acid (DHLA), and 3-mercapto-2,2-bis(mercaptomethyl)propanoic acid (3MPA), bearing mono-, bi-, and trialkyl thiol groups. Spectroscopic studies of the resulting water-dispersible ZAIS QDs revealed a considerable influence of ligand denticity and ligand-to-QD ratio on the spectral position and width (FWHM; full width at half-maximum) of the photoluminescence (PL) bands, the PL quantum yields (PL QY), and the PL decay kinetics. Thiol capping and phase transfer resulted in a loss in PL by at least a factor of 2. The ligand-induced PL quenching observed particularly for ligands bearing two or three thiol groups was attributed to the facilitated formation of surface-bound disulfides. The best colloidal stability under high dilution conditions was observed for 3MPA. KW - Quantum dots KW - Ligand exchange KW - Lifetime analysis KW - Thiols PY - 2022 DO - https://doi.org/10.1021/acs.jpcc.2c05342 SN - 1932-7447 VL - 126 IS - 47 SP - 20101 EP - 20113 PB - ACS Publications AN - OPUS4-56707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Introduction to BAM and ultrasonics (and GPR) in civil engineering N2 - This presentation gives anoverview about BAM, its department 8 and in particular its division 8.2 "NDT methods for civil engineering". The focus is on methods and applications with a geoscientific context, such as methods adopted from geophysics or NDT method applied in a geological environment. T2 - GTK (Geological Survey of Finland) Semninar CY - Espoo, Finland DA - 20.01.2023 KW - NDT KW - Ultrasound KW - Radar KW - Geophysics KW - Concrete PY - 2023 AN - OPUS4-56911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kossatz, Philipp T1 - Lanthanide Nanocrystals as Authentication and Security Tags and Reporters for Optical Sensors N2 - Counterfeiting of goods has serious economic implications worldwide and can present a considerable threat to human health and national security, rendering product authentication more and more important. This led to an increasing interest in simple tags for anticounterfeiting and authentication applications for the integration into different materials and matrices that are robust enough to survive the respective production processes and can be read out in-situ with simple instrumentation. Here we present a platform of chemically inert, multi-color luminescent lanthanide nanocrystals (LnNC) consisting of a NaYF4 matrix doped with Yb, Er, Tm, or Ho as promising candidates for such applications. LnNC with characteristic multi-color emission patterns, composed of narrow bands of varying intensity in the ultraviolet, visible, near-infrared, and short-wave were synthesized via a thermal decomposition approach under inert conditions[1]. The tailor-made design of different emission pattern was achieved by tuning particle size, material composition, and particle surface chemistry in upscaleable syntheses.[2] Particle size and morphology were determined by dynamic light scattering and transmission electron microscopy and the optical properties were characterized by absorption and fluorescence spectroscopy as well as fluorescence lifetime measurements. The particles were then incorporated into security inks and consumer products. In addition, microenvironment-specific changes in the emission properties of the LnNC tag were utilized to study and sense changes of physico-chemical parameters in different matrices. T2 - JCF Frühjahrssymposium 2023 CY - Gießen, Germany DA - 21.03.2023 KW - Lanthanide Nanocrystals KW - Anti-Counterfeiting KW - Fluorescence Spectroscopy PY - 2023 AN - OPUS4-59037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kossatz, Philipp T1 - Upconversion Nanoparticles for Luminescent Barcodes and as Reporters for Optical Sensors N2 - Counterfeiting of goods has serious economic implications worldwide and can be a threat to human health and safety. Upconversion nanoparticles (UCNPs)are ideal candidates for optical encoding of various materials. Particles with tailor-made emission patterns can be used as anti-counterfeiting markers and luminophores in security inks and to track material flows. Microenvironment-specific changes in the emission properties of the UCNP tags can be used to study, signal, and sense changes of physico-chemical parameters in different environments, e.g., building materials. T2 - ANAKON 2023 CY - Vienna, Austria DA - 11.04.2023 KW - Nanomaterials KW - Anti-Counterfeiting KW - Fluorescence Spectroscopy PY - 2023 AN - OPUS4-59035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mazurenka, Mikhail T1 - NIR fluorescence imaging system for (pre)clinical applications: design, construction, and validation N2 - We developed, built, and validated a new versatile fluorescence imaging system. The system is intended to reliably test new tracers and contrast agents at different stages of (pre)clinical research. The system, in its current version, is optimized for the detection of ICG emission. The modular design enables to adapt the scanner to emerging spectral windows with traceable and standardized measurements conditions. T2 - Projektmeeting CY - Berlin, Germany DA - 28.10.2023 KW - Fluorescence imaging KW - Imaging system KW - Standardization PY - 2023 AN - OPUS4-58909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Tscheuschner, Georg A1 - Kaiser, Melanie N. A1 - Lisec, Jan A1 - Beslic, D. A1 - Muth, Thilo A1 - Krüger, M. A1 - Mages, H.-W. A1 - Dorner, B. G. A1 - Knospe, J. A1 - Schenk, J. A. A1 - Sellrie, F. A1 - Weller, Michael G. T1 - MALDI-TOF-MS-based identification of monoclonal murine anti-SARS-CoV-2 antibodies within one hour N2 - During the SARS-CoV-2 pandemic, many virus-binding monoclonal antibodies have been developed for clinical and diagnostic purposes. This underlines the importance of antibodies as universal bioanalytical reagents. However, little attention is given to the reproducibility crisis that scientific studies are still facing to date. In a recent study, not even half of all research antibodies mentioned in publications could be identified at all. This should spark more efforts in the search for practical solutions for the traceability of antibodies. For this purpose, we used thirty-five monoclonal antibodies against SARS-CoV-2 to demonstrate how sequence-independent antibody identification can be achieved by simple means applied onto the protein. First, we examined the intact and light chain masses of the antibodies relative to the reference material NIST-mAb 8671. Already half of the antibodies could be identified based solely on these two parameters. In addition, we developed two complementary peptide mass fingerprinting methods with MALDI-TOF-MS that can be performed in 45 minutes and had a combined sequence coverage of over 80%. One method is based on the partial acidic hydrolysis of the protein by 5 mM of sulfuric acid at 99 °C. Furthermore, we established a fast way for a tryptic digest without an alkylation step. We were able to show that the distinction of clones is possible simply by a brief visual comparison of the mass spectra. In this work, two clones originating from the same immunization gave the same fingerprints. Later, a hybridoma sequencing confirmed the sequence identity of these sister clones. In order to automate the spectral comparison for larger libraries of antibodies, we developed the online software ABID 2.0 (https://gets.shinyapps.io/ABID/). This open-source software determines the number of matching peptides in the fingerprint spectra. We propose that publications and other documents critically relying on monoclonal antibodies with unknown amino acid sequences should include at least one antibody fingerprint. By fingerprinting an antibody in question, its identity can be confirmed by comparison with a library spectrum at any time and context. KW - SARS-CoV-2 antibody KW - Reproducibility crisis KW - Peptide mass fingerprinting KW - Monoclonal antibody KW - Traceability KW - Antibody identification KW - Identity KW - Antibody light chain KW - MALDI-TOF-MS KW - Trypsin KW - Acidic cleavage KW - Antibody subclass KW - Database KW - Peak overlap KW - ABID KW - Sulfuric acid KW - Online software KW - Sequencing KW - Peptide coverage PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545182 DO - https://doi.org/10.20944/preprints202203.0229.v1 SN - 2310-287X SP - 1 EP - 24 PB - MDPI CY - Basel AN - OPUS4-54518 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Duewer, D. L. A1 - Murray, J. A. A1 - Wood, L. J. A1 - Wise, S. A. A1 - Hein, Sebastian A1 - Koch, Matthias A1 - Philipp, Rosemarie A1 - Werneburg, Martina A1 - Hackenberg, R. A1 - Polzer, J. A1 - Avila, M. A. A1 - Serrano, V. A1 - Kakoulides, E. A1 - Alexopoulos, C. A1 - Giannikopoulou, P. A1 - Gui, E. M. A1 - Lu, T. A1 - Teo, T. L. A1 - Hua, T. A1 - Dazhou, C. A1 - Chunxin, L. A1 - Changjun, Y. A1 - Hongmei, L. A1 - Nammoonnoy, J. A1 - Sander, L. C. A1 - Lippa, K. A1 - Quinn, L. A1 - Swiegelaar, C. A1 - Fernandes-Whaley, M. A1 - Gören, A. C. A1 - Gökcen, T. T1 - CCQM-K95.1 Low-polarity analytes in a botanical matrix: Polycyclic aromatic hydrocarbons (PAHs) in tea N2 - Extraction, chromatographic separation, and quantification of low-concentration organic compounds in complex matrices are core challenges for reference material producers and providers of calibration services. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims made by national metrology institutes (NMIs) and designated institutes (DIs). To enable NMIs and DIs to update or establish their claims, in 2014 the Organic Analysis Working Group (OAWG) initiated CCQM-K95.1 "Low-Polarity Analytes in a Botanical Matrix: Polycyclic Aromatic Hydrocarbons (PAHs) in Tea". This was a follow-on comparison from CCQM-K95 which was completed in 2014. The polycyclic aromatic hydrocarbons (PAHs) benz[a]anthracene (BaA) and benzo[a]pyrene (BaP) are considered priority pollutants by U.S. Environmental Protection Agency and are regulated contaminants in food, pose chromatographic separation challenges, and for which exist well-characterized measurement procedures and standard materials. BaA and BaP in a smoked tea were therefore selected as representative target measurands for CCQM-K95.1. Ten NMIs participated in CCQM-K95.1. The consensus summary mass fractions for the two PAHs are in the range of (50 to 70) ng/g with relative standard deviations of (6 to 10) %. Successful participation in CCQM K95.1 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molar mass of 100 g/mol to 500 g/mol and having polarity pKow −2, in a botanical matrix ranging in mass fraction from 10 ng/g to 1000 ng/g: (1) value assignment of primary reference standards (if in-house purity assessment carried out), (2) value assignment of single and/or multi-component organic solutions, (3) extraction of analytes of interest from the matrix, (4) cleanup and separation of analytes of interest from interfering matrix or extract components, and (5) separation and quantification using gas chromatography or liquid chromatography. KW - Benz[a]anthracene (BaA) KW - Benzo[a]pyrene (BaP) KW - Gas chromatography (GC) KW - Isotope dilution (ID) KW - Liquid chromatography (LC) KW - Mass spectrometry (MS) KW - Polycyclic aromatic hydrocarbon (PAH) KW - Yerba mate tea PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471430 DO - https://doi.org/10.1088/0026-1394/56/1A/08002 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1 A SP - 08002, 1 EP - 89 PB - IOP Science AN - OPUS4-47143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotthoff, Lisa A1 - Keller, Julia A1 - Lörchner, Dominique A1 - Mekonnen, Tessema F. A1 - Koch, Matthias T1 - Transformation products of organic contaminants and residues - Overview of current simulation methods N2 - The formation of transformation products (TPs) from contaminants and residues is becoming an increasing focus of scientific community. All organic compounds can form different TPs, thus demonstrating the complexity and interdisciplinarity of this topic. The properties of TPs could stand in relation to the unchanged substance or be more harmful and persistent. To get important information about the generated TPs, methods are needed to simulate natural and manmade transformation processes. Current tools are based on metabolism studies, photochemical methods, electrochemical methods, and Fenton's reagent. Finally, most transformation processes are based on redox reactions. This review aims to compare these methods for structurally different compounds. The groups of pesticides, pharmaceuticals, brominated flame retardants, and mycotoxins were selected as important residues/contaminants relating to their worldwide occurrence and impact to health, food, and environmental safety issues. Thus, there is an increasing need for investigation of transformation processes and identification of TPs by fast and reliable methods. KW - Transformation product KW - Electrochemistry KW - Photochemistry KW - Fenton’s reagent PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474108 DO - https://doi.org/10.3390/molecules24040753 SN - 1420-3049 VL - 24 IS - 4 SP - 753, 1 EP - 23 PB - MDPI CY - Basel AN - OPUS4-47410 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zaimenko, I. A1 - Jaeger, C. A1 - Brenner, H. A1 - Chang-Claude, J. A1 - Hoffmeister, M. A1 - Grötzinger, C. A1 - Detjen, K. A1 - Burock, S. A1 - Schmitt, C.A. A1 - Stein, U. A1 - Lisec, Jan T1 - Non-invasive metastasis prognosis from plasma metabolites in stage II colorectal cancer patients: The DACHS study N2 - Metastasis is the main cause of death from colorectal cancer (CRC). About 20% of stage II CRC patients develop metastasis during the course of disease. We performed metabolic profiling of plasma samples from non-metastasized and metachronously metastasized stage II CRC patients to assess the potential of plasma metabolites to serve as biomarkers for stratification of stage II CRC patients according to metastasis risk. We compared the metabolic profiles of plasma samples prospectively obtained prior to metastasis formation from non-metastasized vs. metachronously metastasized stage II CRC patients of the German population-based case–control multicenter DACHS study retrospectively. Plasma samples were analyzed from stage II CRC patients for whom follow-up data including the information on metachronous metastasis were available. To identify metabolites distinguishing non-metastasized from metachronously metastasized stage II CRC patients robust supervised classifications using decision trees and support vector machines were performed and verified by 10-fold cross-validation, by nested cross-validation and by traditional validation using training and test sets. We found that metabolic profiles distinguish non-metastasized from metachronously metastasized stage II CRC patients. Classification models from decision trees and support vector machines with 10-fold cross-validation gave average accuracy of 0.75 (sensitivity 0.79, specificity 0.7) and 0.82 (sensitivity 0.85, specificity 0.77), respectively, correctly predicting metachronous metastasis in stage II CRC patients. Taken together, plasma metabolic profiles distinguished non-metastasized and metachronously metastasized stage II CRC patients. The classification models consisting of few metabolites stratify non-invasively stage II CRC patients according to their risk for metachronous metastasis. KW - Mass-Spectrometry KW - Cancer PY - 2019 DO - https://doi.org/10.1002/ijc.32076 SN - 1097-0215 VL - 145 IS - 1 SP - 221 EP - 231 PB - Wiley AN - OPUS4-47465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knoche, Lisa A1 - Lisec, Jan A1 - Schwerdtle, T. A1 - Koch, Matthias T1 - LC-HRMS-Based Identification of Transformation Products of the Drug Salinomycin Generated by Electrochemistry and Liver Microsome N2 - The drug salinomycin (SAL) is a polyether antibiotic and used in veterinary Medicine as coccidiostat and growth promoter. Recently, SAL was suggested as a potential anticancer drug. However, transformation products (TPs) resulting from metabolic and environmental degradation of SAL are incompletely known and structural information is missing. In this study, we therefore systematically investigated the formation and identification of SAL derived TPs using electrochemistry (EC) in an electrochemical reactor and rat and human liver microsome incubation (RLM and HLM) as TP generating methods. Liquid chromatography (LC) coupled to high-resolution mass spectrometry (HRMS) was applied to determine accurate masses in a suspected target analysis to identify TPs and to deduce occurring modification reactions of derived TPs. A total of 14 new, structurally different TPs were found (two EC-TPs, five RLM-TPs, and 11 HLM-TPs). The main modification reactions are decarbonylation for EC-TPs and oxidation (hydroxylation) for RLM/HLM-TPs. Of particular interest are potassium-based TPs identified after liver microsome incubation because these might have been overlooked or declared as oxidated sodium adducts in previous, non-HRMS-based studies due to the small mass difference between K and O + Na of 21 mDa. The MS fragmentation pattern of TPs was used to predict the position of identified modifications in the SAL molecule. The obtained knowledge regarding transformation reactions and novel TPs of SAL will contribute to elucidate SAL-metabolites with regards to structural prediction. KW - Salinomycin KW - Ionophore antibiotics KW - Transformation product KW - Electrochemistry KW - Rat/human liver microsomes KW - HRMS PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542543 DO - https://doi.org/10.3390/antibiotics11020155 SN - 2079-6382 VL - 11 IS - 2 SP - 155 PB - MDPI CY - Basel AN - OPUS4-54254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mekonnen, Tessema Fenta A1 - Panne, Ulrich A1 - Koch, Matthias T1 - Glucosylation and Glutathione Conjugation of Chlorpyrifos and Fluopyram Metabolites Using Electrochemistry/Mass Spectrometry N2 - Xenobiotics and their reactive metabolites are conjugated with native biomolecules such as glutathione and glucoside during phase II metabolism. Toxic metabolites are usually detoxified during this step. On the other hand, these reactive species have a potential health impact by disrupting many enzymatic functions. Thus, it is crucial to understand phase II conjugation reactions of xenobiotics in order to address their fate and possible toxicity mechanisms. Additionally, conventional methods (in vivo and in vitro) have limitation due to matrix complexity and time-consuming. Hence, developing fast and matrix-free alternative method is highly demandable. In this work, oxidative phase I metabolites and reactive species of chlorpyrifos (insecticide) and fluopyram (fungicide) were electrochemically produced by using a boron-doped diamond electrode coupled online to electrospray mass spectrometry (ESI-MS). Reactive species of the substrates were trapped by biomolecules (glutathione and glucoside) and phase II conjugative metabolites were identified using liquid chromatography (LC)-MS/MS, and/or Triple time of flight (TripleTOF)-MS. Glutathione conjugates and glucosylation of chlorpyrifos, trichloropyridinol, oxon, and monohydroxyl fluopyram were identified successfully. Glutathione and glucoside were conjugated with chlorpyrifos, trichloropyridinol, and oxon by losing a neutral HCl. In the case of fluopyram, its monohydroxyl metabolite was actively conjugated with both glutathione and glucoside. In summary, seven bioconjugates of CPF and its metabolites and two bioconjugates of fluopyram metabolites were identified using electrochemistry (EC)/MS for the first time in this work. The work could be used as an alternative approach to identify glutathione and glucosylation conjugation reactions of other organic compounds too. It is important, especially to predict phase II conjugation within a short time and matrix-free environment. KW - Pesticide KW - Bioconjugation KW - Oxidative metabolism KW - EC/MS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-475932 DO - https://doi.org/10.3390/molecules24050898 VL - 24 IS - 5 SP - 898 EP - 910 PB - MDPI AN - OPUS4-47593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lisec, Jan T1 - Mass-Spectrometry to conduct metabolomics experiments N2 - The presentation gives an overview in MS-Technology, the process of metabolomics experiments and the use in Fluxomics studies as a particular example. T2 - Seminar CY - Max Delbrück Center for Molecular Medicine, Germany DA - 21.03.2019 KW - Mass-Spectrometry KW - Fluxomics PY - 2019 AN - OPUS4-47663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Iwert, C. A1 - Stein, J. A1 - Appelt, C. A1 - Vogt, K. A1 - Rainer, R. J. A1 - Tummler, K. A1 - Mühle, K. A1 - Stanko, K. A1 - Schumann, J. A1 - Uebe, D. A1 - Jürchott, K. A1 - Lisec, Jan A1 - Janek, K. A1 - Gille, C. A1 - Textoris-Taube, K. A1 - Sai, S. A1 - Petersen, A. A1 - Kühl, A. A. A1 - Klipp, E. A1 - Meisel, C. A1 - Sawitzki, B. T1 - TCAIM controls effector T cell generation by preventing Mitochondria-Endoplasmic Reticulum Contact Site-initiated Cholesterol Biosynthesis N2 - T cells need to adapt their cellular metabolism for effector cell differentiation. This relies on alterations in mitochondrial physiology. Which signals and molecules regulate those alterations remains unclear. We recently reported, that the mitochondrial protein TCAIM inhibits activation-induced changes in mitochondrial morphology and function and thus, CD effector T cell formation. Using conditional TCAIM knock-in (KI) and knockout (KO) mice, w now show that it also applies to CD8+ T cells and more importantly, delineate the molecular processes in mitochondria by which TCAIM controls effector cell differentiation. TCAIM KI resulted in reduced activation-induced HIF1α protein expression. Metabolomics and transcriptional data in combination with mathematical flux modeling revealed an impaired induction of anabolic pathways, especially of the mevalonate pathway and cholesterol biosynthesis in TCAIM KI CD8+ T cells. Addition of cholesterol completely rescued HIF1α protein expression, activation and proliferation of TCAIM KI CD8+ T cells. At the molecular level, TCAIM delayed activation-induced mitochondria-ER contact (MERC) formation by binding to MERC promoting proteins such as RMD3 and VDAC2. In summary, we demonstrate that TCAIM suppresses effector cell differentiation by inhibiting MERC formation, which induce HIF1α-mediated increase in cellular metabolism and cholesterol biosynthesis. KW - Mass Spectroscopy KW - Metabolomics KW - Cancer PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533543 UR - https://www.biorxiv.org/content/10.1101/2021.04.20.440500v1 DO - https://doi.org/10.1101/2021.04.20.440500 VL - April SP - 1 EP - 45 PB - Cold Spring Harbor Laboratory AN - OPUS4-53354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Blumrich, A. A1 - Vogler, G. A1 - Dresen, S. A1 - Diop, S. B. A1 - Jaeger, Carsten A1 - Leberer, S. A1 - Grune, J. A1 - Wirth, E. K. A1 - Hoeft, B. A1 - Renko, K. A1 - Foryst-Ludwig, A. A1 - Spranger, J. A1 - Sigrist, S. A1 - Bodmer, R. A1 - Kintscher, U. T1 - Fat-body brummer lipase determines survival and cardiac function during starvation in Drosophila melanogaster N2 - The cross talk between adipose tissue and the heart has an increasing importance for cardiac function under physiological and pathological conditions. This study characterizes the role of fat body lipolysis for cardiac function in Drosophila melanogaster. Perturbation of the function of the key lipolytic enzyme, brummer (bmm), an ortholog of themammalian ATGL (adipose triglyceride lipase) exclusively in the fly’s fat body, protected the heart against starvation-induced dysfunction. We further provide evidence that this protection is caused by the preservation of glycerolipid stores, resulting in a starvation-resistant maintenance of energy supply and adequate cardiac ATP synthesis. Finally, we suggest that alterations of lipolysis are tightly coupled to lipogenic processes, participating in the preservation of Lipid energy substrates during starvation. Thus, we identified the inhibition of adipose tissue lipolysis and subsequent energy preservation as a protective mechanism against cardiac dysfunction during catabolic stress. KW - High-resolution mass spectrometry KW - Nontarget analysis PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-528756 DO - https://doi.org/10.1016/j.isci.2021.102288 VL - 24 IS - 4 SP - 102288 AN - OPUS4-52875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaeger, Carsten A1 - Ritter, D. A1 - Goeritzer, M. A1 - Thiele, A. A1 - Blumrich, A. A1 - Beyhoff, N. A1 - Luettges, K. A1 - Smeir, E. A1 - Kasch, J. A1 - Grune, J. A1 - Müller, O. A1 - Klopfleisch, R. A1 - Foryst-Ludwig, A. A1 - Kintscher, U. T1 - Liver X Receptor Agonist AZ876 Induces Beneficial Endogenous Cardiac Lipid Reprogramming and Protects Against Isoproterenol-Induced Cardiac Damage N2 - Background - It is known that dietary intake of polyunsaturated fatty acids may improve cardiac function. However, relatively high daily doses are required to achieve sufficient cardiac concentrations of beneficial omega‐3 fatty acids. The liver X receptor (LXR) is a nuclear hormone receptor and a crucial regulator of lipid homeostasis in mammals. LXR activation has been shown to endogenously reprogram cellular lipid profiles toward increased polyunsaturated fatty acids levels. Here we studied whether LXR lipid reprogramming occurs in cardiac tissue and exerts cardioprotective actions. Methods and Results - Male 129SV mice were treated with the LXR agonist AZ876 (20 µmol/kg per day) for 11 days. From day 6, the mice were injected with the nonselective β‐agonist isoproterenol for 4 consecutive days to induce diastolic dysfunction and subendocardial fibrosis while maintaining systolic function. Treatment with isoproterenol led to a marked impairment of global longitudinal strain and the E/e' ratio of transmitral flow to mitral annular velocity, which were both significantly improved by the LXR agonist. Histological examination showed a significant reduction in isoproterenol‐induced subendocardial fibrosis by AZ876. Analysis of the cardiac lipid composition by liquid chromatography‐high resolution mass spectrometry revealed a significant increase in cardiac polyunsaturated fatty acids levels and a significant reduction in saturated fatty acids by AZ876. Conclusions - The present study provides evidence that the LXR agonist AZ876 prevents subendocardial damage, improves global longitudinal strain and E/e' in a mouse model of isoproterenol‐induced cardiac damage, accompanied by an upregulation of cardiac polyunsaturated fatty acids levels. Cardiac LXR activation and beneficial endogenous cardiac lipid reprogramming may provide a new therapeutic strategy in cardiac disease with diastolic dysfunction. KW - Heart failure KW - Lipids KW - Liver X receptor KW - Diastolic dysfunction KW - Nuclear receptor PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-529352 DO - https://doi.org/10.1161/JAHA.120.019473 VL - 10 IS - 14 SP - e019473 AN - OPUS4-52935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuner, Maximilian A1 - Kühn, S. A1 - Haase, H. A1 - Meyer, Klas A1 - Koch, Matthias T1 - Cleaving Ergot Alkaloids by Hydrazinolysis - A Promising Approach for a Sum Parameter Screening Method N2 - Ergot alkaloids are mycotoxins formed by fungi of the Claviceps genus, which are some of the most common contaminants of food and feed worldwide. These toxins are a structurally heterogeneous group of compounds, sharing an ergoline backbone. Six structures and their corresponding stereoisomers are typically quantified by either HPLC-FLD or HPLC-MS/MS and the values subsequently summed up to determine the total ergot alkaloid content. For the development of a screening method targeting all ergot alkaloids simultaneously, the alkaloids need to be transferred to one homogeneous structure: a lysergic acid derivative. In this study, two promising cleaving methods—acidic esterification and hydrazinolysis—are compared, using dihydroergocristine as a model compound. While the acidic esterification proved to be unsuitable, due to long reaction times and oxidation sensitivity, hydrazinolysis reached a quantitative yield in 40-60 min. Parallel workup of several samples is possible. An increasing effect on the reaction rate by the addition of ammonium iodide was demonstrated. Application of hydrazinolysis to a major ergot alkaloid mix solution showed that all ergopeptines were cleaved, but ergometrine/-inine was barely affected. Still, hydrazinolysis is a suitable tool for the development of a sum parameter screening method for ergot alkaloids in food and feed. KW - Ergot alkaloids KW - Sum parameter method KW - Hydrazinolysis KW - Esterification PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527508 DO - https://doi.org/10.3390/toxins13050342 VL - 13 IS - 5 SP - 342 PB - MDPI CY - Basel, Switzerland AN - OPUS4-52750 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Riedel, Juliane A1 - Recknagel, Sebastian A1 - Sassenroth, Diana A1 - Mauch, Tatjana A1 - Buttler, Sabine A1 - Sommerfeld, Thomas A1 - Penk, Sibylle A1 - Koch, Matthias T1 - Development and certification of a reference material for zearalenone in maize germ oil N2 - Zearalenone (ZEN), an estrogenic mycotoxin produced by several species of Fusarium fungi, is a common contaminant of cereal-based food worldwide. Due to frequent occurrences associated with high levels of ZEN, maize oil is a particular source of exposure. Although a European maximumlevel for ZEN in maize oil exists according to Commission Regulation (EC) No. 1126/2007 along with a newly developed international standard method for analysis, certified reference materials (CRM) are still not available. To overcome this lack, the first CRM for the determination of ZEN in contaminated maize germ oil (ERM®-BC715) was developed in the frame of a European Reference Materials (ERM®) project according to the requirements of ISO Guide 35. The whole process of CRM development including preparation, homogeneity and stability studies, and value assignment is presented. The assignment of the certified mass fraction was based upon an in-house study using high-performance liquid chromatography isotope dilution tandem mass spectrometry. Simultaneously, to support the in-house certification study, an interlaboratory comparison study was conducted with 13 expert laboratories using different analytical methods. The certified mass fraction and expanded uncertainty (k=2) of ERM®-BC715 (362± 22) μg kg−1 ZEN are traceable to the SI. This reference material is intended for analytical quality control and contributes to the improvement of consumer protection and food safety. KW - Fusarium mycotoxin KW - Vegetable edible oil KW - Food analysis KW - European Reference Material KW - Quality assurance PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-531831 DO - https://doi.org/10.1007/s00216-021-03532-z SN - 1618-2642 SN - 1618-2650 VL - 413 IS - 21 SP - 5483 EP - 5491 PB - Springer CY - Berlin AN - OPUS4-53183 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Morcillo, Dalia T1 - High-resolution absorption isotopic spectrometry as a tool for aging studies of Li-ion batteries N2 - Lithium (Li) is the key element in the manufacturing of batteries. Isotopic study of Li may help to identify the causes of battery aging due to isotopic fractionation during charge/discharge cycles. Isotopic ratio determination is based on monitoring the isotopic components of lithium by their spin-orbit coupling and its isotopic shift of about 15 pm for the 22P←22S electronic transition around 670.788 nm. In this work, we propose improvements to our previous work [1] by using a higher-resolution double echelle modular spectrometer (HR-DEMON II) coupled to a continuum source graphite furnace atomic absorption spectrometer (HR-CS-GF-AAS) for the isotopic analysis of Li. The data analysis was carried out by using a decision-tree-based ensemble machine learning (ML) algorithm (XGBoost). A set of samples with 6Li isotope amount fractions ranging from 0.0004 to 0.99 mol mol-1 was used for the algorithm's training. Subsequently, the procedure was validated by a set of stock chemicals (Li2CO3, LiNO3, LiCl, and LiOH) and a BAM candidate reference material, a cathode material (NMC111). Finally, the ML model was applied to determine the isotope ratio of geological samples, including anorthosite, granite, soil, rhyolite, nepheline syenite, and basalt and battery samples. These samples were measured as digested without any further purification step. Improvements in the optical resolution resolve the lithium isotopic components of the atomic spectra. In the studied geological samples, were found δ7Li values between -0.5 and 4.5 ‰ with a precision range of 1 to 2 ‰. In addition, the proposed method was validated with multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS), and these results are comparable and compatible. T2 - Caltech-BAM Meeting CY - Online meeting DA - 10.08.2022 KW - Lithium isotope KW - Machine learning KW - Battery KW - High-resolution absorption isotopic spectrometry PY - 2022 AN - OPUS4-56380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Recknagel, Sebastian A1 - Koch, Matthias A1 - Köppen, Robert A1 - Buttler, Sabine A1 - Penk, Sibylle A1 - Mauch, Tatjana A1 - Sommerfeld, Thomas A1 - Witt, Angelika T1 - Correction to: "Development of certified reference materials for the determination of cadmium and acrylamide in cocoa" N2 - The article "Development of certified reference materials for the determination of cadmium and acrylamide in cocoa" was originally published in the journal "Analytical and bioanalytical chemistry" Online First without Open Access. After publication in volume 412, issue 19, page 4659–4668, the authors decided to opt for Open Choice and to make the article an Open Access publication. Therefore, the copyright of the article has been changed to ©The Author(s) 2021 and the article is forthwith distributed under the terms of the Creative Commons Attribution 4.0 International License. PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527908 DO - https://doi.org/10.1007/s00216-021-03428-y SN - 1618-2642 SN - 1618-2650 SP - 1 PB - Springer CY - Berlin AN - OPUS4-52790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Langenhan, Jennifer A1 - Jaeger, Carsten A1 - Baum, K. A1 - Simon, M. A1 - Lisec, Jan T1 - A Flexible Tool to Correct Superimposed Mass Isotopologue Distributions in GC‐APCI‐MS Flux Experiments N2 - The investigation of metabolic fluxes and metabolite distributions within cells by means of tracer molecules is a valuable tool to unravel the complexity of biological systems. Technological advances in mass spectrometry (MS) technology such as atmospheric pressure chemical ionization (APCI) coupled with high resolution (HR), not only allows for highly sensitive analyses but also broadens the usefulness of tracer‐based experiments, as interesting signals can be annotated de novo when not yet present in a compound library. However, several effects in the APCI ion source, i.e., fragmentation and rearrangement, lead to superimposed mass isotopologue distributions (MID) within the mass spectra, which need to be corrected during data evaluation as they will impair enrichment calculation otherwise. Here, we present and evaluate a novel software tool to automatically perform such corrections. We discuss the different effects, explain the implemented algorithm, and show its application on several experimental datasets. This adjustable tool is available as an R package from CRAN. KW - Mass Spectrometry KW - Isotopologue Distribution KW - Metabolic Flux KW - R package PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547318 DO - https://doi.org/10.3390/metabo12050408 VL - 12 IS - 5 SP - 1 EP - 10 PB - MDPI AN - OPUS4-54731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kimani, Martha Wamaitha A1 - Pérez-Padilla, Victor A1 - Valderrey, Virginia A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Red-Emitting Polymerizable Guanidinium Dyes as Fluorescent Probes in Molecularly Imprinted Polymers for Glyphosate Detection N2 - The development of methodologies to sense glyphosate has gained momentum due to its toxicological and ecotoxicological effects. In this work, a red-emitting and polymerizable guanidinium benzoxadiazole probe was developed for the fluorescence detection of glyphosate. The interaction of the fluorescent probe and the tetrabutylammonium salt of glyphosate was studied via UV/vis absorption and fluorescence spectroscopy in chloroform and acetonitrile. The selective recognition of glyphosate was achieved by preparing molecularly imprinted polymers, able to discriminate against other common herbicides such as 2,4-dichlorophenoxyacetic acid (2,4-D) and 3,6-dichloro-2-methoxybenzoic acid (dicamba), as thin layers on submicron silica particles. The limits of detection of 4.8 µM and 0.6 µM were obtained for the sensing of glyphosate in chloroform and acetonitrile, respectively. The reported system shows promise for future application in the sensing of glyphosate through further optimization of the dye and the implementation of a biphasic assay with water/organic solvent mixtures for sensing in aqueous environmental samples. KW - Glyphosate KW - Guanidinium receptors KW - Fluorescent probes KW - Molecularly imprinted polymers KW - Core-shell particles PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-544441 DO - https://doi.org/10.3390/chemosensors10030099 SN - 2227-9040 VL - 10 IS - 3 SP - 1 EP - 20 PB - MDPI CY - Basel AN - OPUS4-54444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tscheuschner, Georg A1 - Kaiser, Melanie N. A1 - Lisec, Jan A1 - Beslic, D. A1 - Muth, Thilo A1 - Krüger, M. A1 - Mages, H. W. A1 - Dorner, B. G. A1 - Knospe, J. A1 - Schenk, J. A. A1 - Sellrie, F. A1 - Weller, Michael G. T1 - MALDI-TOF-MS-Based Identification of Monoclonal Murine Anti-SARS-CoV-2 Antibodies within One Hour N2 - During the SARS-CoV-2 pandemic, many virus-binding monoclonal antibodies have been developed for clinical and diagnostic purposes. This underlines the importance of antibodies as universal bioanalytical reagents. However, little attention is given to the reproducibility crisis that scientific studies are still facing to date. In a recent study, not even half of all research antibodies mentioned in publications could be identified at all. This should spark more efforts in the search for practical solutions for the traceability of antibodies. For this purpose, we used 35 monoclonal antibodies against SARS-CoV-2 to demonstrate how sequence-independent antibody identification can be achieved by simple means applied to the protein. First, we examined the intact and light chain masses of the antibodies relative to the reference material NIST-mAb 8671. Already half of the antibodies could be identified based solely on these two parameters. In addition, we developed two complementary peptide mass fingerprinting methods with MALDI-TOF-MS that can be performed in 60 min and had a combined sequence coverage of over 80%. One method is based on the partial acidic hydrolysis of the protein by 5 mM of sulfuric acid at 99 degrees C. Furthermore, we established a fast way for a tryptic digest without an alkylation step. We were able to show that the distinction of clones is possible simply by a brief visual comparison of the mass spectra. In this work, two clones originating from the same immunization gave the same fingerprints. Later, a hybridoma sequencing confirmed the sequence identity of these sister clones. In order to automate the spectral comparison for larger libraries of antibodies, we developed the online software ABID 2.0. This open-source software determines the number of matching peptides in the fingerprint spectra. We propose that publications and other documents critically relying on monoclonal antibodies with unknown amino acid sequences should include at least one antibody fingerprint. By fingerprinting an antibody in question, its identity can be confirmed by comparison with a library spectrum at any time and context. KW - Reproducibility KW - Quality control KW - Traceability KW - Peptides KW - Peptide mass fingerprinting KW - Monoclonal antibody KW - Recombinant antibody KW - Identity KW - Antibody identification KW - Sequencing KW - Light chain KW - Mass spectrometry KW - Software KW - Open science KW - Library KW - COVID-19 KW - Corona virus KW - Sequence coverage KW - NIST-mAb 8671 KW - Reference material KW - RBD KW - Spike protein KW - Nucleocapsid KW - Cleavage KW - Tryptic digest KW - MALDI KW - DHAP KW - 2,5-dihydroxyacetophenone KW - Github KW - Zenodo KW - ABID PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-547347 DO - https://doi.org/10.3390/antib11020027 VL - 11 IS - 2 SP - 1 EP - 22 PB - MDPI CY - Basel AN - OPUS4-54734 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jaeger, Carsten A1 - Lisec, Jan T1 - Towards Unbiased Evaluation of Ionization Performance in LC-HRMS Metabolomics Method Development N2 - As metabolomics increasingly finds its way from basic science into applied and regulatory environments, analytical demands on nontargeted mass spectrometric detection methods continue to rise. In addition to improved chemical comprehensiveness, current developments aim at enhanced robustness and repeatability to allow long-term, inter-study, and meta-analyses. Comprehensive metabolomics relies on electrospray ionization (ESI) as the most versatile ionization technique, and recent liquid chromatography-high resolution mass spectrometry (LC-HRMS) instrumentation continues to overcome technical limitations that have hindered the adoption of ESI for applications in the past. Still, developing and standardizing nontargeted ESI methods and instrumental setups remains costly in terms of time and required chemicals, as large panels of metabolite standards are needed to reflect biochemical diversity. In this paper, we investigated in how far a nontargeted pilot experiment, consisting only of a few measurements of a test sample dilution series and comprehensive statistical analysis, can replace conventional targeted evaluation procedures. To examine this potential, two instrumental ESI ion source setups were compared, reflecting a common scenario in practical method development. Two types of feature evaluations were performed, (a) summary statistics solely involving feature intensity values, and (b) analyses additionally including chemical interpretation. Results were compared in detail to a targeted evaluation of a large metabolite standard panel. We reflect on the advantages and shortcomings of both strategies in the context of current harmonization initiatives in the metabolomics field. KW - Mass Spectrometry KW - Non-targeted analysis KW - Method development PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548065 DO - https://doi.org/10.3390/metabo12050426 VL - 12 IS - 5 SP - 1 EP - 13 PB - MDPI AN - OPUS4-54806 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Valderrey, Virginia A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Thiourea- and Amino-Substituted Benzoxadiazole Dyes with Large Stokes Shifts as Red-Emitting Probe Monomers for Imprinted Polymer Layers Targeting Carboxylate-Containing Antibiotics N2 - Bifunctional fluorescent molecular oxoanion probes based on the benzoxadiazole (BD) chromophore are described which integrate a thiourea binding motif and a polymerizable 2-aminoethyl methacrylate unit in the 4,7-positions of the BD core. Concerted charge transfer in this electron donor-acceptor-donor architecture endows the dyes with strongly Stokes shifted (up to >250 nm) absorption and fluorescence. Binding of electron-rich carboxylate guests at the thiourea receptor leads to further analyte-induced red-shifts of the emission, shifting the fluorescence maximum of the complexes to ≥700 nm. Association constants for acetate are ranging from 1–5×105 M−1 in acetonitrile. Integration of one of the fluorescent probes through its polymerizable moiety into molecularly imprinted polymers (MIPs) grafted from the surface of submicron silica cores yielded fluorescent MIP-coated particle probes for the selective detection of antibiotics containing aliphatic carboxylate groups such as enoxacin (ENOX) at micromolar concentrations in highly polar solvents like acetonitrile. KW - Molecular imprinting KW - Anion recognition KW - Antibiotics KW - Benzoxadiazole dyes KW - Charge transfer KW - Fluorescence PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545027 DO - https://doi.org/10.1002/chem.202104525 SN - 1521-3765 SP - 1 EP - 9 PB - Wiley-VCH AN - OPUS4-54502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beyer, S. A1 - Kimani, Martha Wamaitha A1 - Zhang, Y. A1 - Verhassel, A. A1 - Sternbæk, L. A1 - Wang, T. A1 - Persson, J. L. A1 - Härkönen, P. A1 - Johansson, E. A1 - Caraballo, R. A1 - Elofsson, M. A1 - Gawlitza, Kornelia A1 - Rurack, Knut A1 - Ohlsson, L. A1 - El-Schich, Z. A1 - Gjörloff Wingren, A. A1 - Stollenwerk, M. M. T1 - Fluorescent Molecularly Imprinted Polymer Layers against Sialic Acid on Silica-coated Polystyrene Cores - Assessment of the Binding Behavior to Cancer Cells N2 - Sialic acid (SA) is a monosaccharide usually linked to the terminus of glycan chains on the cell surface. It plays a crucial role in many biological processes, and hypersialylation is a common feature in cancer. Lectins are widely used to analyze the cell surface expression of SA. However, these protein molecules are usually expensive and easily denatured, which calls for the development of alternative glycan-specific receptors and cell imaging technologies. In this study, SA-imprinted fluorescent core-shell molecularly imprinted polymer particles (SA-MIPs) were employed to recognize SA on the cell surface of cancer cell lines. The SA-MIPs improved suspensibility and scattering properties compared with previously used core-shell SA-MIPs. Although SA-imprinting was performed using SA without preference for the alpha-2,3- and alpha-2,6-SA forms, we screened the cancer cell lines analyzed using the lectins Maackia Amurensis Lectin I (MAL I, alpha-2,3-SA) and Sambucus Nigra Lectin (SNA, alpha-2,6-SA). Our results show that the selected cancer cell lines in this study presented a varied binding behavior with the SA-MIPs. The binding pattern of the lectins was also demonstrated. Moreover, two different pentavalent SA conjugates were used to inhibit the binding of the SA-MIPs to breast, skin, and lung cancer cell lines, demonstrating the specificity of the SA-MIPs in both flow cytometry and confocal fluorescence microscopy. We concluded that the synthesized SA-MIPs might be a powerful future tool in the diagnostic analysis of various cancer cells. KW - Cancer KW - Imprinting KW - Molecularly imprinted polymers KW - SA conjugates KW - Sialic acid PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546625 DO - https://doi.org/110.3390/cancers14081875 SN - 2072-6694 VL - 14 IS - 8 PB - MDPI CY - Basel AN - OPUS4-54662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kianinejad, kaveh A1 - Fedelich, Bernard A1 - Darvishi Kamachali, Reza A1 - Schriever, Sina A1 - Manzoni, Anna Maria A1 - Agudo Jácome, Leonardo A1 - Megahed, Sandra A1 - Kamrani, Sepideh A1 - Saliwan-Neumann, Romeo T1 - Experimentally informed multiscale creep modelling of additive manufactured Ni-based superalloys N2 - Excellent creep resistance at elevated temperatures, i.e. T / T_m> 0.5, due to γ-γ’ microstructure is one of the main properties of nickel-based superalloys. Due to its great importance for industrial applications, a remarkable amount of research has been devoted to understanding the underlying deformation mechanism in a wide spectrum of temperature and loading conditions. Additive manufactured (AM) nickel-based superalloys while being governed by similar γ-γ’ microstructure, exhibit AM-process specific microstructural characteristics, such as columnar grains, strong crystallographic texture (typically <001> fiber texture parallel to build direction) and compositional inhomogeneity, which in turn leads to anisotropic creep response in both stationary and tertiary phases. Despite the deep insights achieved recently on the correlation between process parameters and the resulting microstructure, the anisotropic creep behavior and corresponding deformation mechanism of these materials are insufficiently understood so far. One reason for this is the lack of capable material models that can link the microstructure to the mechanical behavior. To overcome this challenge, a multiscale microstructure-based approach has been applied by coupling crystal plasticity (CP) and polycrystal model which enables the inclusion of different deformation mechanisms and microstructural characteristics such as crystallographic texture and grain morphology. The method has been applied to experimental data for AM-manufactured INCONEL-738LC (IN738). The effect of different slip systems, texture, and morphology on creep anisotropy at 850°C has been investigated. Results suggest a strong correlation between superlattice extrinsic stacking fault (SESF) and microtwinning and observed creep anisotropy. T2 - EUROMAT 23 CY - Frankfurt a. M., Germany DA - 04.09.2023 KW - IN738LC KW - Creep anisotropy KW - Crystal plasticity PY - 2023 AN - OPUS4-58263 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sternbaek, L. A1 - Kimani, Martha Wamaitha A1 - Gawlitza, Kornelia A1 - Rurack, Knut A1 - Janicke, B. A1 - Alm, K. A1 - Gjörloff-Wingren, A. A1 - Eriksson, H. T1 - Molecularly Imprinted Polymers Exhibit Low Cytotoxic and Inflammatory Properties in Macrophages In Vitro N2 - Molecularly imprinted polymers (MIPs) against sialic acid (SA) have been developed as a detection tool to target cancer cells. Before proceeding to in vivo studies, a better knowledge of the overall effects of MIPs on the innate immune system is needed. The aim of this study thus was to exemplarily assess whether SA-MIPs lead to inflammatory and/or cytotoxic responses when administered to phagocytosing cells in the innate immune system. The response of monocytic/macrophage cell lines to two different reference particles, Alhydrogel and PLGA, was compared to their response to SA-MIPs. In vitro culture showed a cellular association of SA-MIPs and Alhydrogel, as analyzed by flow cytometry. The reference particle Alhydrogel induced secretion of IL-1b from the monocytic cell line THP-1, whereas almost no secretion was provoked for SA-MIPs. A reduced number of both THP-1 and RAW 264.7 cells were observed after incubation with SA-MIPs and this was not caused by cytotoxicity. Digital holographic cytometry showed that SA-MIP treatment affected cell division, with much fewer cells dividing. Thus, the reduced number of cells after SA-MIP treatment was not linked to SA-MIPs cytotoxicity. In conclusion, SA-MIPs have a low degree of inflammatory properties, are not cytotoxic, and can be applicable for future in vivo studies. KW - Molecularly imprinted polymers KW - Digital holographic cytometry KW - Cytotoxicity KW - Proinflammatory cytokines PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-552250 DO - https://doi.org/10.3390/app12126091 SN - 2076-3417 VL - 12 IS - 12 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-55225 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Wan, Wei A1 - Rurack, Knut T1 - Toward Label-Free Optical Multiplexing of Analytes in Indicator Release Lateral Flow Assays via Detection Zones Containing Tailored Capture Materials N2 - The use of macromolecules and materials immobilized in the detection zone of test strips for indicator capture and focusing in label-free lateral flow assays (LFAs) is described, with emphasis on its future use in low number multiplexing. Several materials such as polyelectrolytes, functionalized mesoporous silica micro- and nanoparticles, chemically modified cellulose or glass fibre (GF) membranes and molecularly imprinted polymer gels coated onto membranes were studied in model assays, before the most promising materials were combined with antibody-gated indicator delivering (gAID) sensor materials. Cellulose, nitrocellulose and GF membranes were used as supports and highly fluorescent dyes of different charge states as model indicators. Combination of the best performing capture materials with gAID systems made it possible to distinctly increase the sensitivity and reduce the measurement uncertainty in the LFA testing of pentaerythritol tetranitrate (PETN) in aqueous samples. In addition, dual-plexing of PETN and 2,4,6-trinitrotoluene (TNT) was realized on a single test strip containing two dedicated capture zones. KW - Rapid tests KW - Vor-Ort-Analytik KW - Multiplexing KW - Teststreifen KW - Molecularly imprinted polymers PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-557873 DO - https://doi.org/10.1002/anse.202100062 VL - 2 IS - 4 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-55787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Bresch, Harald A1 - Kipphardt, Heinrich A1 - Resch-Genger, Ute A1 - Koch, Matthias A1 - Rosner, M. T1 - Trends in selected fields of reference material production N2 - For more than 110 years, BAM has been producing reference materials for a wide range of application fields. With the development of new analytical methods and new applications as well as continuously emerging more stringent requirements of laboratory accreditation with regard to quality control and metrological traceability, the demand and requirements for reference materials are increasing. This trend article gives an overview of general developments in the field of reference materials as well as developments in selected fields of application in which BAM is active. This includes inorganic and metal analysis, gas analysis, food and consumer products, and geological samples. In addition to these more traditional fields of application, developments in the areas of optical spectroscopy, particulary fluorescence methods, and nanomaterials are considered. T2 - 150 years BAM: Science with impact CY - Berlin, Germany DA - 01.01.2021 KW - Reference material KW - ISO REMCO KW - Gas analysis KW - Food KW - Nanomaterials KW - Fluorescence PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548407 DO - https://doi.org/10.1007/s00216-022-03996-7 SN - 1618-2642 SN - 1618-2650 VL - 414 IS - Topical collection: Analytical methods and applications in the materials and life sciences SP - 4281 EP - 4289 PB - Springer CY - Berlin AN - OPUS4-54840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knoche, Lisa A1 - Lisec, Jan A1 - Koch, Matthias T1 - Analysis of electrochemical and liver microsomal transformation products of lasalocid by LC/HRMS N2 - Rationale: Lasalocid (LAS), an ionophore, is used in cattle and poultry farming as feed additive for its antibiotic and growth-promoting properties. Literature on transformation products (TP) resulting from LAS degradation is limited. So far, only hydroxylation is found to occur as the metabolic reaction during the LAS degradation. To investigate potential TPs of LAS, we used electrochemistry (EC) and liver microsome (LM) assays to synthesize TPs, which were identified using liquid chromatography high-resolution mass spectrometry (LC/HRMS). Methods: Electrochemically produced TPs were analyzed online by direct coupling of the electrochemical cell to the electrospray ionization (ESI) source of a Sciex Triple-TOF high resolution mass spectrometer. Then, EC-treated LAS solution was collected and analyzed offline using LC/HRMS to confirm stable TPs and improve their annotation with a chemical structure due to informative MS/MS spectra. In a complementary approach, TPs formed by rat and human microsomal incubation were investigated using LC/HRMS. The resulting data were used to investigate LAS modification reactions and elucidate the chemical structure of obtained TPs. Results: The online measurements identified a broad variety of TPs, resulting from modification reactions like (de-)hydrogenation, hydration, methylation, oxidation as well as adduct formation with methanol. We consistently observed different ion complexations of LAS and LAS-TPs (Na+; 2Na+ K+; NaNH4 +; KNH4 +). Two stable methylated EC-TPs were found, structurally annotated, and assigned to a likely modification reaction. Using LM incubation, seven TPs were formed, mostly by oxidation/hydroxylation. After the identification of LM-TPs as Na+-complexes, we identified LM-TPs as K+-complexes. Conclusion: We identified and characterized TPs of LAS using EC- and LM-based methods. Moreover, we found different ion complexes of LAS-based TPs. This knowledge, especially the different ion complexes, may help elucidate the metabolic and environmental degradation pathways of LAS. KW - Mass Spectrometry KW - Electrochemistry KW - ECR KW - Lasalocid KW - Ionophore KW - Transformation products PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553919 DO - https://doi.org/10.1002/rcm.9349 VL - 36 IS - 18 SP - 1 EP - 10 PB - Wiley online library AN - OPUS4-55391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Koch, Matthias A1 - Mauch, Tatjana A1 - Riedel, Juliane T1 - Development of a Hydrazine-Based Solid-Phase Extraction and Clean-Up Method for Highly Selective Quantification of Zearalenone in Edible Vegetable Oils by HPLC-FLD N2 - Rapid, cost-efficient, and eco-friendly methods are desired today for routine analysis of the Fusarium mycotoxin zearalenone (ZEN) in edible vegetable oils. Liquid chromatography with fluorescence detection (HPLC-FLD) is commonly used to reliably control the specified ZEN maximum levels, which requires efficient sample clean-up to avoid matrix interferences. Therefore, a highly selective extraction and clean-up method based on reversible covalent hydrazine chemistry (RCHC) using hydrazine-functionalized silica was developed. This efficient solid-phase extraction (SPE) involves reversible hydrazone formation of ZEN with the hydrazine moiety covalently bound to a solid phase. Optimal conditions were achieved with 1 mL SPE cartridges filled with 400 mg of hydrazine-functionalized silica. The developed RCHC-SPE method was validated in an interlaboratory comparison study (ILC) with twelve participants analyzing six edible vegetable oils with a focus on maize oils. The derived method parameters (ZEN recovery 83%, repeatability 7.0%, and reproducibility 18%) meet the performance criteria of Commission Regulation (EC) No 401/2006. The developed RCHC-SPE-based HPLC-FLD method allows the reliable quantification of ZEN in the range of 47–494 μg/kg for different types of edible vegetable oils, also for matrix-reach native oils. Due to the high efficiency, the significantly reduced matrix load helps to extend the lifetime of analytical equipment. Furthermore, the re-useability of the RCHC-SPE cartridges contributes to an eco-friendly approach and reduced analysis costs. To our knowledge, this is the first report on ZEN quantification in edible vegetable oils based on manual RCHC-SPE cartridges. Due to its high performance, the developed RCHC-SPE method is a promising alternative to the current European standard method EN 16924:2017 (HPLC-FLD part). KW - Mycotoxin KW - Food KW - Reversible covalent hydrazine chemistry (RCHC) KW - Quantitative determination PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-554812 DO - https://doi.org/10.3390/toxins14080549 VL - 14 IS - 8 PB - MDPI CY - Basel AN - OPUS4-55481 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munir, R. A1 - Noureen, N. A1 - Bashir, M. A1 - Shoaib, N. A1 - Ashraf, A. A1 - Lisec, Jan A1 - Zaidi, N. T1 - Cancer Awareness Measure (CAM) and Cancer Awareness Measure MYthical Causes Scale (CAM‑MY) scores in Pakistani population N2 - Lifestyle modifications could prevent almost one‑third to one‑half of all cancer cases. The awareness of cancer risk factors could motivate people to make such changes in their behaviors and lifestyles. This work aims to investigate the cancer awareness level in the Pakistani population. Telephone interviews of 657 individuals in Pakistan were carried out using the Cancer Awareness Measure (CAM) and Cancer Awareness Measure–MYthical Causes Scale (CAM‑MY). We observed that participants scored significantly better on the CAM scale than the CAM‑MY scale, and CAM scores were negatively associated with CAM‑MY scores. Years of formal education or a biology major at undergraduate or graduate level did not affect our population’s cancer awareness levels. Age displayed a weak but statistically significant negative association with CAM scores. Most participants failed to identify modifiable cancer risk factors, e.g., low physical activity. Efforts should be made to improve awareness of modifiable risk factors. We observed that brief training sessions could markedly improve people’s understanding of cancer risk factors and myths. KW - Cancer KW - Cancer awareness measure KW - Cancer risk PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548960 DO - https://doi.org/10.1038/s41598-022-13012-8 SN - 2045-2322 VL - 12 IS - 1 SP - 1 EP - 10 PB - Nature Publishing Group CY - London AN - OPUS4-54896 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tukhmetova, Dariya A1 - Lisec, Jan A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Data processing made easy: standalone tool for automated calculation of isotope ratio from transient signals – IsoCor N2 - Despite numerous advantages offered by hyphenation of chromatography and electrokinetic separation methods with multicollector (MC) ICP-MS for isotope analysis, the main limitation of such systems is the decrease in precision and increase in uncertainty due to generation of short transient signals. To minimize this limitation, most authors compare several isotope ratio calculation methods and establish a multi-step data processing routine based on the precision and accuracy of the methods. However, to the best of our knowledge, there is no universal data processing tool available that incorporates all important steps of the treatment of the transient signals. Thus, we introduce a data processing application (App) IsoCor that facilitates automatic calculation of isotope ratios from transient signals and eases selection of the most suitable method. The IsoCor App performs baseline subtraction, peak detection, mass bias correction, isotope ratio calculation and delta calculation. The feasibility and reliability of the App was proven by reproducing the results from isotope analysis of three elements (neodymium, mercury and sulfur) measured on-line via hyphenated systems. The IsoCor App provides trackability of the results to ensure quality control of the analysis. KW - Isotope ratio KW - Transient signal KW - MC-ICP-MS KW - Data processing KW - App PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559068 DO - https://doi.org/10.1039/D2JA00208F VL - 37 IS - 11 SP - 2401 EP - 2409 PB - Royal Society of Chemistry AN - OPUS4-55906 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Meermann, Björn A1 - Koch, Matthias A1 - Weller, Michael G. T1 - Editorial: Analytical methods and applications in materials and life sciences N2 - Current trends in materials and life sciences are flanked by the need to push detection limits to single molecules or single cells, enable the characterization of increasingly complex matrices or sophisticated nanostructures, speed up the time of analysis, reduce instrument complexity and costs, and improve the reliability of data. This requires suitable analytical tools such as spectroscopic, separation and imaging techniques, mass spectrometry, and hyphenated techniques as well as sensors and their adaptation to application-specific challenges in the environmental, food, consumer product, health sector, nanotechnology, and bioanalysis. Increasing concerns about health threatening known or emerging pollutants in drinking water, consumer products, and food and about the safety of nanomaterials led to a new awareness of the importance of analytical sciences. Another important driver in this direction is the increasing demand by legislation, particularly in view of the 17 sustainable development goals by the United Nations addressing clean energy, industry, and innovation, sustainable cities, clean water, and responsible consumption and production. In this respect, also the development of analytical methods that enable the characterization of material flows in production processes and support recycling concepts of precious raw materials becomes more and more relevant. In the future, this will provide the basis for greener production in the chemical industry utilizing recycled or sustainable starting materials. This makes analytical chemistry an essential player in terms of the circular economy helping to increase the sustainability of production processes. In the life sciences sector, products based on proteins, such as therapeutic and diagnostic antibodies, increase in importance. These increasingly biotechnologically produced functional biomolecules pose a high level of complexity of matrix and structural features that can be met only by highly advanced methods for separation, characterization, and detection. In addition, metrological traceability and target definition are still significant challenges for the future, particularly in the life sciences. However, innovative reference materials as required for the health and food sector and the characterization of advanced materials can only be developed when suitable analytical protocols are available. The so-called reproducibility crisis in sciences underlines the importance of improved measures of quality control for all kinds of measurements and material characterization. This calls for thorough method validation concepts, suitable reference materials, and regular interlaboratory comparisons of measurements as well as better training of scientists in analytical sciences. The important contribution of analytical sciences to these developments is highlighted by a broad collection of research papers, trend articles, and critical reviews from these different application fields. Special emphasis is dedicated to often-overlooked quality assurance and reference materials. T2 - 150 years BAM: Science with impact CY - Berlin, Germany DA - 01.01.2021 KW - Analysis KW - Life sciences KW - Analytical sciences KW - Quality assurance KW - Reference material KW - Fluorescence KW - Nanoparticle KW - Sensor KW - Material sciences KW - Pollutant KW - Environment KW - Method KW - Limit of detection KW - 150th anniversary KW - ABC KW - BAM KW - Collection KW - Editorial KW - Special issue KW - Bundesanstalt für Materialforschung und -prüfung KW - Jahrestag PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-550720 DO - https://doi.org/10.1007/s00216-022-04082-8 SN - 1618-2642 SN - 1618-2650 VL - 414 IS - Topical collection: Analytical methods and applications in the materials and life sciences SP - 4267 EP - 4268 PB - Springer CY - Berlin AN - OPUS4-55072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Koch, Matthias T1 - On-Site Detection of Volatile Organic Compounds (VOCs) N2 - Volatile organic compounds (VOCs) are of interest in many different fields. Among them are food and fragrance analysis, environmental and atmospheric research, industrial applications, security or medical and life science. In the past, the characterization of these compounds was mostly performed via sample collection and off-site analysis with gas chromatography coupled to mass spectrometry (GC-MS) as the gold standard. While powerful, this method also has several drawbacks such as being slow, expensive, and demanding on the user. For decades, intense research has been dedicated to find methods for fast VOC analysis on-site with time and spatial resolution. We present the working principles of the most important, utilized, and researched technologies for this purpose and highlight important publications from the last five years. In this overview, non-selective gas sensors, electronic noses, spectroscopic methods, miniaturized gas chromatography, ion mobility spectrometry and direct injection mass spectrometry are covered. The advantages and limitations of the different methods are compared. Finally, we give our outlook into the future progression of this field of research. KW - Volatile organic compounds KW - On-site detection KW - Mobile analytics KW - Sensors PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570885 DO - https://doi.org/10.3390/molecules28041598 VL - 28 IS - 4 SP - 1 EP - 19 PB - MDPI CY - Basel, Switzerland AN - OPUS4-57088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jiang, Shan A1 - Wang, T. A1 - Behren, S. A1 - Westerlind, U. A1 - Gawlitza, Kornelia A1 - Persson, J. L. A1 - Rurack, Knut T1 - Sialyl-Tn Antigen-Imprinted Dual Fluorescent Core–Shell Nanoparticles for Ratiometric Sialyl-Tn Antigen Detection and Dual-Color Labeling of Cancer Cells N2 - Sialyl-Tn (STn or sialyl-Thomsen-nouveau) is a carbohydrate antigen expressed by more than 80% of human carcinomas. We here report a strategy for ratiometric STn detection and dual-color cancer cell labeling, particularly, by molecularly imprinted polymers (MIPs). Imprinting was based on spectroscopic studies of a urea-containing green-fluorescent monomer 1 and STn-Thr-Na (sodium salt of Neu5Acα2-6GalNAcα-O-Thr). A few-nanometer-thin green-fluorescent polymer shell, in which STn-Thr-Na was imprinted with 1, other comonomers, and a cross-linker, was synthesized from the surface of red-emissive carbon nanodot (R-CND)-doped silica nanoparticles, resulting in dual fluorescent STn-MIPs. Dual-color labeling of cancer cells was achieved since both red and green emissions were detected in two separate channels of the microscope and an improved accuracy was obtained in comparison with single-signal MIPs. The flow cytometric cell analysis showed that the binding of STn-MIPs was significantly higher (p < 0.001) than that of non-imprinted polymer (NIP) control particles within the same cell line, allowing to distinguish populations. Based on the modularity of the luminescent core–fluorescent MIP shell architecture, the concept can be transferred in a straightforward manner to other target analytes. KW - Cancer KW - Core−shell particles KW - Dual-color labeling glycan KW - Molecular imprinting PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-563106 DO - https://doi.org/10.1021/acsanm.2c03252 SP - 1 EP - 14 PB - ACS Publications AN - OPUS4-56310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kubheka, G. A1 - Climent, Estela A1 - Tobias, Charlie A1 - Rurack, Knut A1 - Mack, J. A1 - Nyokong, T. T1 - Multiplexed Detection of Human Papillomavirus Based on AzaBODIPY-Doped Silica-Coated Polystyrene Microparticles N2 - Human papillomavirus (HPV) DNA detection can enable the early diagnosis of high-risk HPV types responsible for cervical cancer. HPV detection is also essential for investigating the clinical behavior and epidemiology of particular HPV types, characterization of study populations in HPV vaccination trials and monitoring the efficacy of HPV vaccines. In this study, two azaBODIPY dyes (1 and 2) were used as references and were doped into polystyrene particles (PS40), while a short HPV DNA single strand was used as a target molecule and was covalently bound to the silica shell. These particles were employed as optical probes in 1:1 hybridization assays, and their potential applicability as a tool for multiplex assays for the detection of different strands of HPV was evaluated using flow cytometry. A good separation in the fluorescence of the four different voncentrations prepared for each dye was observed. To perform the hybridization assays, HPV18, HPV16, HPV11 and HPV6 single strands were attached to the particles through EDC-mediated coupling. The c-DNA-1-PS40 and c-DNA-2-PS40 particles exhibited low limit of detection (LOD) and quantification (LOQ) values for HPV11, and a narrow detection range was obtained. Multiplexed assay experiments were successfully performed for both particles, and the results proved that c-DNA-1-PS40 could potentially be used as a tool for multiplexing assays and merits further in-depth study in this context. KW - Flow cytometry KW - BODIPY dyes KW - Core-shell particles KW - Multiplexed assay KW - Human papillomavirus PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-567358 DO - https://doi.org/10.3390/chemosensors11010001 SN - 2227-9040 VL - 11 IS - 1 SP - 1 EP - 21 PB - MDPI CY - Basel AN - OPUS4-56735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Burnage, Samual A1 - Bell, Jérémy A1 - Wan, Wei A1 - Kislenko, Evgeniia A1 - Rurack, Knut T1 - Combining a hybrid chip and tube microfluidic system with fluorescent molecularly imprinted polymer (MIP) core–shell particles for the derivatisation, extraction, and detection of peptides with N-terminating phosphorylated tyrosine N2 - The reliable identification and quantitation of phosphorylated amino acids, peptides and proteins is one of the key challenges in contemporary bioanalytical research, an area of particular interest when attempting to diagnose and treat diseases at an early stage. We have developed a synthetic probe for targeting phosphorylated amino acids, based on core–shell submicron-sized particles consisting of a silica core, coated with a molecularly imprinted polymer (MIP) shell. The MIP layer contains a fluorescent probe crosslinker which binds selectively to phosphorylated tyrosine (pY) moieties with a significant imprinting factor (IF) and responds with a "light-up” fluorescence signal. The bead-based ratiometric detection scheme has been successfully transferred to a microfluidic chip format and its applicability to rapid assays has been exemplarily shown by discriminating a pY-terminating oligopeptide against its nonphosphorylated counterpart. Such miniaturised devices could lead to an automated pY or pY N-terminated peptide measurement system in the future. The setup combines a modular microfluidic system for amino acid derivatisation, extraction (by micropillar co-flow) and selective adsorption and detection with the fluorescent MIP core–shell particle probes. A miniaturised optical assembly for low-light fluorescence measurements was also developed, based on miniaturised opto-electronic parts and optical fibres. The emission from the MIP particles upon binding of pY or pY N-terminated peptides could be monitored in real-time. KW - Microfluidics KW - Molecularly imprinted polymers KW - Phosphorylated peptides KW - Fluorescence KW - Core-shell particles PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569204 DO - https://doi.org/10.1039/d2lc00955b SN - 1473-0197 VL - 23 IS - 3 SP - 466 EP - 474 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-56920 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Garrido, E. A1 - Hernández-Sigüenza, G. A1 - Climent, Estela A1 - Marcos, M. D. A1 - Rurack, Knut A1 - Gaviña, P. A1 - Parra, M. A1 - Sancenón, F. A1 - Martí-Centelles, V. A1 - Martínez-Máñez, R. T1 - Strip-based lateral flow-type indicator displacement assay for γ-hydroxybutyric acid (GHB) detection in beverages N2 - The use of gamma-hydroxybutyric acid (GHB) in drug-facilitated sexual assault has increased due to its availability and high solubility in aqueous solutions and alcoholic beverages, necessitating the development of rapid methods for GHB detection. In this respect, portable testing methods for use in the field, based on lateral flow assays (LFAs) and capable of detecting trace concentrations of target analytes, are particularly attractive and hold enormous potential for the detection of illicit drugs. Using this strategy, here we report a rapid, low cost, easy-to-handle strip-based LFA for GHB analysis employing a smartphone for fluorescence readout. At molecular signalling level, the ensemble is based on a Cu2+ complex with a tetradentate ligand and the fluorescent dye coumarin 343, which indicate GHB through an indicator displacement assay (IDA) in aqueous solution. When incorporated in a LFA-based strip test this system shows a detection limit as low as 0.03 μM for GHB in MES buffer solution and is able to detect GHB at concentrations of 0.1 μM in soft drinks and alcoholic beverages in only 1 min. KW - Indicator displacement assay KW - Gamma-hydroxybutyric acid KW - Lateral flow assay KW - Test strip KW - Fluorescent dyes KW - Smartphone readout PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564631 DO - https://doi.org/10.1016/j.snb.2022.133043 SN - 0925-4005 VL - 377 SP - 1 EP - 7 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-56463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Costa, Elena A1 - Climent Terol, Estela A1 - Ast, S. A1 - Weller, Michael G. A1 - Canning, J. A1 - Rurack, Knut T1 - Development of a lateral flow test for rapid pyrethroid detection using antibody-gated indicator-releasing hybrid materials N2 - The employment of type-I pyrethroids for airplane disinfection in recent years underlines the necessity to develop sensing schemes for the rapid detection of these pesticides directly at the point-of-use. Antibody-gated indicator-releasing materials were thus developed and implemented with test strips for lateral-flow assay-based analysis employing a smartphone for readout. Besides a proper matching of pore sizes and gating macromolecules, the functionalization of both the material's outer surface as well as the strips with PEG chains enhanced system performance. This simple assay allowed for the detection of permethrin as a target molecule at concentrations down to the lower ppb level in less than 5 minutes. KW - Lateral flow test KW - Gated hybrid material KW - Fluorescence KW - Smartphone readout device KW - Pyrethroid KW - Pesticide KW - Insecticide KW - SBA-15 KW - Permethrin PY - 2020 DO - https://doi.org/10.1039/d0an00319k SN - 0003-2654 SN - 1364-5528 VL - 145 IS - 10 SP - 3490 EP - 3494 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-50756 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munir, R. A1 - Lisec, Jan A1 - Jaeger, Carsten A1 - Zaidi, N. T1 - Abundance, fatty acid composition and saturation index of neutral lipids in colorectal cancer cell lines N2 - Lipid droplets, the dynamic organelles that store Triglycerides (TG) and cholesterol esters (CE), are highly accumulated in colon cancer cells. This work studies the TG and CE subspecies profile in colon carcinoma cell lines, SW480 derived from primary tumor, and SW620 derived from a metastasis of the same tumor. It was previously reported that the total TG and CE content is dramatically higher in SW620 cells; however, TG and CE subspecies profile has not been investigated in detail. The work presented here confirms that the total TG and CE Content is significantly higher in the SW620 cells. Moreover, the fatty acid (FA) composition of TG is significantly altered in the SW620 cells, with significant decrease in the abundance of saturated triglycerides. This resulted in a significantly decreased TG saturation index in the SW620 cells. The saturation index of CE was also significantly decreased in the SW620 cells. KW - Mass Spectroscopy KW - Metabolomics KW - Cancer PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533504 DO - https://doi.org/10.18388/abp.2020_5465 VL - 68 IS - 1 SP - 1 EP - 4 PB - ABP Acta Biochimica Polonica AN - OPUS4-53350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaeger, Carsten T1 - Rapid characterization of ionization products for chemistry-aware compound annotation in nontargeted small molecule mass spectrometry N2 - Nontargeted high-resolution mass spectrometry (HRMS) is widely used for small molecule screening in biotic or abiotic samples. However, HRMS approaches like metabolomics or environmental nontarget screening currently still lack confidence in chemical annotation, i.e. computational structure assignment to all measured mass signals. As a crucial step within the annotation pipeline, molecular weight inference (MWI) deduces a compound’s intact mass from diagnostic mass differences between MS1 peaks, allowing precise database queries in subsequent steps. As the common practice of considering all possible ionization products such as adducts, multimers, multiple charges etc. in MWI suffers from high false positive rates, we aimed at selecting candidate ionization products in a chemically sensitive way. Generally, electrospray ionization produces different types of adducts depending on chromatographic system and sample matrix, necessitating application-specific optimization for optimum MWI performance. To avoid, however, the tedious and potentially biased manual data curation connected to optimization, we established an R-based workflow for automating this task. The workflow consists of two parts. Part 1 creates an MS1 spectral library by performing peak detection, spectral deconvolution and target peak assignment based on density estimation. Part 2 analyzes ion relationships within the library and returns a list of detected ionization products ranked by their frequency. We applied the workflow to a commercial 634-compound library that was acquired for two chromatographic methods (reverse phase, RP; hydrophilic liquid interaction chromatographic, HILIC) and the two ESI modes (positive, negative). As expected, different frequency distributions of ionization products were found for the two chromatographies. Interestingly, however, some of the differences were expected in terms of solvent chemistries (e.g. [M+NH4]+ in ammonium formate-buffered HILIC) while others indicated more complex ion competition (e.g. abundant [M+K]+, [M+2K-H]+ in HILIC). This demonstrated the relevance of this empirical approach. We further show that MWI accuracy clearly benefitted from derived optimized adduct lists – by adding filters or weighting terms – and present FDR calculations supporting this observation. We conclude that chemistry-aware compound annotation based on the combination of high-throughput library acquisition and statistical analysis holds significant potential for further improvements in nontargeted small molecule HRMS. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Compound annotation KW - Mass spectrometry KW - Electrospray ionization KW - Nontarget analysis KW - Accurate mass PY - 2019 AN - OPUS4-48332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sternbaek, L. T1 - Macrophage-uptake of sialic acid-targeted molecularly imprinted polymers (SA-MIPs) N2 - Sialic acid (SA) is a cell surface glycan, which has a strong role in many cell activities including differentiation, proliferation, and the immune response. The amount of SA has been found to be correlated with cancer, with an upregulation on more aggressive cancers. Therefore, there is great interest in developing methods for detection of SA on cancer cells. We are screening SA on cancer cell lines by using fluorescent molecularly imprinted polymers, SA-MIPs.Macrophages, which evolve from mono-cytes, are well known for their extraordinary ability to phagocytose foreign objects. This could lead to the hypothesis that the SA-MIPs can be recognized by macrophages as foreign object; thus leading to internalization and potential degradation. We have discovered that SA-MIPs can be detected after incubation with the RAW macrophage cells, with increasing fluorescence over time. The microscopy analysis shows that the RAW cells ingest the SA-MIP particles. This information is important when planning to use SA-MIPs in future in vivo applications. T2 - The 69th Annual Conference of the Nordic Microscopy Society, 2018 CY - Lyngby, Denmark DA - 25.06.2018 KW - Sialic acid KW - MIPs KW - Macrophages PY - 2018 AN - OPUS4-45422 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Gojani, Ardian B. A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - Towards automated scanning electron microscopy image analysis of core-shell microparticles for quasi-3D determination of the surface roughness N2 - Core-shell (CS) particles have been increasingly used for a wide range of applications due to their unique properties by merging individual characteristics of the core and the shell materials. The functionality of the designed particles is strongly influenced by their surface roughness. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task for Scanning Electron Microscopy (SEM). The SEM images contain two-dimensional (2D) information providing contour roughness data only from the projection of the particle in the horizontal plane. This study presents a practical procedure to achieve more information by tilting the sample holder, hence allowing images of different areas of a single particle to be recorded at different orientations under the same view angle. From the analysis of these images, quasi three-dimensional (3D) information is obtained. Three types of home-made particles were investigated: i) bare polystyrene (PS) particles, ii) PS particles decorated with a first magnetic iron oxide (Fe3O4) nanoparticle shell forming CS microbeads, iii) PS/Fe3O4 particles closed with a second silica (SiO2) shell forming core-shell-shell (CSS) microbeads. A series images of a single particle were taken with stepwise tilted sample holder up to 10° by an SEM with high-resolution and surface sensitive SE-InLens® mode. A reliable analysis tool has been developed by a script in Python to analyze SEM images automatically and to evaluate profile roughness quantitatively, for individual core-shell microparticles. Image analysis consists of segmentation of the images, identifying contour and the centre of the particle, and extracting the root mean squared roughness value (RMS-RQ) of the contour profile from the particle projection within a few seconds. The variation in roughness from batch-to-batch was determined with the purpose to set the method as a routine quality check procedure. Flow cytometry measurements provided complementary data. Measurement uncertainties associated to various particle orientations were also estimated. T2 - ICASS 5th International Conference on Applied Surface Science CY - Palma, Mallorca, Spain DA - 25.04.2022 KW - Core-shell particles KW - Image analysis KW - Roughness KW - Scanning electron microscopy PY - 2022 AN - OPUS4-54774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, A. A1 - Lischeid, G. A1 - Koch, Matthias A1 - Lentzsch, P. A1 - Sommerfeld, Thomas A1 - Müller, M.H. T1 - Co-Cultivation of Fusarium, Alternaria, and Pseudomonas on Wheat-Ears Affects Microbial Growth and Mycotoxin Production N2 - Mycotoxigenic fungal pathogens Fusarium and Alternaria are a leading cause of loss in cereal production. On wheat-ears, they are confronted by bacterial antagonists such as pseudomonads. Studies on these groups’ interactions often neglect the infection process’s temporal aspects and the associated priority effects. In the present study, the focus was on how the first colonizer affects the subsequent ones. In a climate chamber experiment, wheat-ears were successively inoculated with two different strains (Alternaria enuissima At625, Fusarium graminearum Fg23, or Pseudomonas simiae Ps9). Over three weeks, microbial abundances and mycotoxin concentrations were analyzed and visualized via Self Organizing Maps with Sammon Mapping (SOM-SM). All three strains revealed different characteristics and strategies to deal with co-inoculation: Fg23, as the first colonizer, suppressed the establishment of At625 and Ps9. Nevertheless, primary inoculation of At625 reduced all of the Fusarium toxins and stopped Ps9 from establishing. Ps9 showed priority effects in delaying and blocking the production of the fungal mycotoxins. The SOM-SM analysis visualized the competitive strengths: Fg23 ranked first, At625 second, Ps9 third. Our findings of species-specific priority effects in a natural environment and the role of the mycotoxins involved are relevant for developing biocontrol strategies. KW - Antagonists KW - Microbe interactions KW - Mycotoxins KW - Priority effect KW - SOM-SM PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-521554 DO - https://doi.org/10.3390/microorganisms9020443 VL - 9 IS - 2 SP - 443 PB - MDPI AN - OPUS4-52155 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liu, H. A1 - Song, W. A1 - Gröninger, Delia A1 - Zhang, L. A1 - Lu, Y. A1 - Chan, K. S. A1 - Zhou, Z. A1 - Rurack, Knut A1 - Shen, Z. T1 - Real-time monitoring of newly acidified organelles during autophagy enabled by reaction-based BODIPY dyes N2 - Real-time monitoring of newly acidified organelles during autophagy in living cells is highly desirable for a better understanding of intracellular degradative processes. Herein, we describe a reaction-based boron dipyrromethene (BODIPY) dye containing strongly electron-withdrawing diethyl 2-cyanoacrylate groups at the α-positions. The probe exhibits intense red fluorescence in acidic organelles or the acidified cytosol while negligible fluorescence in other regions of the cell. The underlying mechanism is a nucleophilic reaction at the central meso-carbon of the indacene core, resulting in the loss of π-conjugation entailed by dramatic spectroscopic changes of more than 200 nm between its colorless, non-fluorescent leuco-BODIPY form and its red and brightly emitting form. The reversible transformation between red fluorescent BODIPY and leuco-BODIPY along with negligible cytotoxicity qualifies such dyes for rapid and direct intracellular lysosome imaging and cytosolic acidosis detection simultaneously without any washing step, enabling the real-time monitoring of newly acidified organelles during autophagy. KW - Autophagy KW - BODIPY KW - Fluorescence KW - Lysosome KW - Real-time imaging PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498358 UR - https://www.nature.com/articles/s42003-019-0682-1 DO - https://doi.org/10.1038/s42003-019-0682-1 SN - 23993642 VL - 2 SP - 442 PB - Nature Research CY - London AN - OPUS4-49835 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mekonnen, Tessema F. A1 - Byrne, Liam A1 - Panne, Ulrich A1 - Koch, Matthias T1 - Investigation of chlorpyrifos and its transformation products in fruits and spices by combining electrochemistry and liquid chromatography coupled to tandem mass spectrometry N2 - The identification of transformation products (TPs) of pesticides in food is a crucial task difficult to tackle, due to the lack of standards. In this work, we present a novel methodology to synthesize five main TP standards of the insecticide chlorpyrifos (CPF) and to investigate their occurrence in selected fruits and spices. TPs were electrochemically (EC) synthesized using a boron-doped diamond electrode (BDD) and identified by EC coupled online to mass spectrometry, LC-MS/MS, and high-resolution mass spectrometry. CPF and its TPs were analyzed in the food samples by LC-MS/MS on multiple reaction monitoring (MRM) after dispersive solid-phase extraction. A good recovery of 83–103% for CPF and 65–85% for TPs was obtained. Matrix effects, which cause signal suppression, ranged between 81 to 95% for all targeted analytes. The limit of detection and quantification for CPF were 1.6–1.9 and 4.9–5.7 μg/kg, respectively. Among investigated samples, CPF was determined in fresh lemon (104 μg/kg), fenugreek seed (40 μg/kg), and black pepper (31 μg/kg). CPF content in all samples was lower than the EU maximum residue level (MRL). The most frequently detected TPs were diethylthiophosphate and diethylphosphate. Other TPs, CPF oxon and trichloropyridinol, were also detected. Hence, EC is a versatile tool to synthesize TP standards which enables the determination of contaminants and residues in foodstuffs even if no commercial standards are available. KW - Transformation product KW - Electrochemistry KW - QuEChERS KW - LC-MS/MS KW - Photodegradation KW - Foodstuffs PY - 2018 UR - https://link.springer.com/article/10.1007/s12161-018-1245-7#citeas DO - https://doi.org/10.1007/s12161-018-1245-7 SN - 1936-9751 SN - 1936-976X VL - 11 IS - 10 SP - 2657 EP - 2665 PB - Springer AN - OPUS4-45834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Koch, Matthias A1 - Köppen, Robert A1 - Buttler, Sabine A1 - Penk, Sibylle A1 - Mauch, Tatjana A1 - Sommerfeld, Thomas A1 - Witt, Angelika T1 - Development of certified reference materials for the determination of cadmium and acrylamide in cocoa N2 - Since 1 January 2019 a maximum content of 0.6 mg kg−1 cadmium (Cd) in cocoa powder sold to the final consumer or as an ingredient in sweetened cocoa powder sold to the final consumer (drinking chocolate) is set by the Commission Regulation (EU) No. 488/2014. Monitoring compliance with the specified limit value requires analytical measuring methods and reference materials for quality control. However, suitable certified reference materials intended for quality assurance and quality control purposes are still lacking. Therefore, three cocoa reference materials (ERM®-BD513, ERM®-514 and ERM®-515) were developed according to the requirements of ISO 17034 and the recommendations of ISO Guide 35. The whole process of reference material development, including material preparation, assessment of homogeneity and stability, characterisation and value assignment is presented. The assignment of the certified mass fractions was based upon an interlaboratory comparison study involving 19 expert laboratories for Cd and 12 laboratories for acrylamide. The certified mass fractions and expanded uncertainties (k = 2) of the reference materials were (0.181 ± 0.009) mg kg−1 Cd (ERM®-BD513), (0.541 ± 0.024) mg kg−1 Cd (ERM®-BD514) and (0.690 ± 0.029) mg kg−1 Cd (ERM®-BD515). Acrylamide contents are given for information. KW - Certified reference material KW - Quality assurance KW - Cocoa KW - Cadmium KW - Acrylamide KW - Food analysis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508656 DO - https://doi.org/10.1007/s00216-020-02719-0 SN - 1618-2642 SN - 1618-2650 VL - 412 IS - 19 SP - 4659 EP - 4668 PB - Springer CY - Berlin AN - OPUS4-50865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sjöberg, T. A1 - El-Schich, Z. A1 - Rurack, Knut A1 - Gjörloff Wingren, A. T1 - Colorectal Cancer Cell Spheroids Co-Cultured with Molecularly Imprinted Fluorescent Particles Targeting Sialic Acid Show Preserved Cell Viability N2 - In vitro cultured 3D models of CRC have been demonstrated to hold considerable worth in drug discovery, drug resistance analysis, and in studying cell-cell and cell-matrix interactions that occur in the tumor microenvironment. The 3D models resemble the in vivo physiological microenvironment by replicating the cell type composition and tissue architecture. Molecularly imprinted polymers (MIPs) have been investigated for use instead of antibodies against small nonimmunogenic structures, such as sialic acid (SA). Glyco-conjugates including SA are present on all cells, and often deregulated on cancer cells. Here, we present a novel approach for targeting and detecting colorectal cancer cells (CRC) by using in vitro cultured HT29 3D spheroids co-cultured in vitro with either fluorescent MIPs targeting SA, SA-MIPs, or the two lectins targeting SA, MAL I, and SNA. Both formaldehyde-fixed and viable HT29 3D spheroids with or without SA-MIPs were imaged in 3D by confocal microscopy. The results revealed a preserved cell morphology and viability of the HT29 3D spheroids co-cultured in vitro with SA-MIPs. However, the lectins MAL I and SNA targeting the alpha-2,3 or alpha-2,6 SA glycosidic linkages, respectively, affected the cell viability when co-cultured with the viable HT29 3D spheroids, and no living cells could be detected. Here, we have shown that the SA-MIPs could be used as a safe and low-cost diagnostic tool for targeting and detecting cancer cells in a physiologically relevant 3D cancer model in vitro. KW - Molecularly Imprinted Polymers KW - Durchflusszytometrie KW - Zellanalytik KW - Fluoreszenz KW - Mikroskopie PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573840 DO - https://doi.org/10.3390/app13095330 VL - 13 IS - 9 SP - 1 EP - 6 PB - MDPI CY - Basel AN - OPUS4-57384 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Sternbaek, L. A1 - Kimani, Martha Wamaitha A1 - Gawlitza, Kornelia A1 - Janicke, B. A1 - Alm, K. A1 - Gjörloff-Wingren, A. T1 - Digital Holographic Cytometry: Macrophage Uptake of Nanoprobes N2 - Digital holographic cytometry (DHC) is a state-of-the-art quantitative Phase imaging (QPI) method that permits time-lapse imaging of cells without induced cellular toxicity. DHC platforms equipped with semi-automated image segmentation and analysis software packages for assessing cell behavior are commercially available. In this study we investigate the possible uptake of nanoprobes in macrophages in vitro over time. KW - Macrophages KW - MIPs KW - Holographic microscopy KW - Sialic acid PY - 2019 VL - 21 SP - 21 EP - 23 PB - Wiley CY - Imaging and Microscopy AN - OPUS4-47793 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Temgoua, Ranil C. T. T1 - Electrochemistry Coupled to Mass Spectrometry and in silico Methods As an Alternative Strategy for Pesticides Ecotoxicity Assessment N2 - The widespread occurrence of neonicotinoid insecticides and their transformation / degradation products (TPs) in the aquatic environment raises health and environmental concerns. As a consequence pesticides, and to a lesser degree their degradation products, are monitored by authorities both in surface waters and drinking waters. In vitro and in vivo experimental models, mainly based on cell cultures, animals, healthy humans and clinical trials, are useful approaches for identifying the main metabolic pathways. However, time, cost, and matrix complexity often hinder the success of these methods. In this study, we propose an alternative non-enzymatic approach that combines electrochemistry (EC) with liquid chromatography (LC), gas chromatography (GC), mass spectrometry (MS), and in silico methods to evaluate the ecotoxicity of pesticides. In this study the formation of degradation products from electrochemical reactors (EC) of neonicotinoid insecticides and phenylurea herbicides were investigated. Firstly, electrochemical experiments were conducted using three primary methodological approaches: cyclic voltammetry (CV) and linear sweep voltammetry (LSV) for investigating electrochemical behavior and controlled-potential coulometry (CPC) for electrosynthesis. Three distinct electrochemical cell configurations were employed: the µ-PrepCell and ReactorCell for direct coupling with mass spectrometry (MS), and the SynthesisCell for batch electrosynthesis. These experiments utilized glassy carbon (GC) and boron-doped diamond (BDD) electrodes. Secondly the chemical structures of the main EC-degradation products were identified using gas chromatography coupled with mass spectrometry and liquid chromatography–mass spectrometry (GC-MS and LCMSMS). The structural elucidation of ppesticides oxidation/reduction products was based on retention time, m/z ratio in positive mode and fragmentation pattern. The ecotoxicity of neonicotinoid insecticides and the proposed TPs were estimated with the ecological structure–activity relationships (ECOSAR) model. Electrochemistry mass spectrometry hyphenated techniques represent an accessible, rapid and reliable tool to elucidate the oxidative/reductive degradation of neonicotinoids and phenylurea, including reactive degradation products and conjugates. T2 - 247th ECS (The Electrochemical Society) Meeting CY - Montreal, Canada DA - 18.05.2025 KW - Material safety KW - Quality ensurance KW - Chemical safety PY - 2025 AN - OPUS4-63531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Drzymala, Sarah T1 - Instrumental analysis, metabolism and toxicity of cis- and trans-zearalenone and their biotransformation products N2 - Trans-Zearalenone(ZEN)is a non-steroidal estrogenic mycotoxin which frequently contaminates cereal grains worldwide. Ingestion of food and feed containing ZEN causes numerous mycotoxicoses in animals and possibly humans with pronounced estrogenic effects. Due to the trans-configurated double bond, ZEN isomerizes to the cis-configuration upon the influence of light. This work investigates the instrumental analysis, metabolism and toxicity of ZEN and cis- ZEN. The first part focused on the determination of ZEN in edible oils. Due to a maximum level of 400 µg/kg ZEN in the European Union (EU), reliable analytical methods are needed. A comprehensive method comparison proved dynamic covalent hydrazine chemistry (DCHC) to be the most suitable approach. Thus, an automated solid phase extraction (SPE) coupled online to high performance liquid chromatography (HPLC) was developed with the novelty of a covalent SPE step comprising the DCHC principle. The automated online system allows an accurate, selective and reliable quantification of ZEN in edible oils in compliance with EU performance criteria while significantly reducing workload and thereby personnel costs. In contrast to ZEN, reference standards and analytical methods are missing for cis- ZEN which causes a lack of data on the occurrence, fate and risks of cis-ZEN. Therefore, a native and an isotopically labeled cis-ZEN standard were synthesized and implemented in an existing stable isotope dilution analysis HPLC tandem mass spectrometry (HPLC-MS/MS) method. Using this method, a large extent of cis-ZEN formation was observed for ZEN contaminated maize germ oils when exposed to daylight which confirms that cis-ZEN can be a relevant food contaminant and should be considered in the analysis of food and feed. Furthermore, this work investigated the in vitro phase I metabolism of ZEN and cis-ZEN in rat and human liver microsomes by using HPLC-MS and -MS/MS analyses. The metabolic pathways of cis-ZEN were found to be essentially similar to ZEN including reduction and oxidation reactions generating α- and β-cis- zearalenol as well as 13- and 15-OH-cis-ZEN. A previously unidentified oxidative metabolic pathway for both isomers of ZEN results in the formation of cis-ZEN-11,12-oxide and ZEN-11,12-oxide in human liver microsomes. The estrogenicity of cis-ZEN and its reductive metabolites was assessed using the E-Screen assay. cis-ZEN proved to be slightly more estrogenic than ZEN. Biotransformation of cis-ZEN to β-cis-ZEL corresponds to a detoxification, whereas metabolism to α-cis-ZEL resembles a metabolic activation as its estrogenicity considerably exceeds that of cis-ZEN. The catecholic metabolites can be expected to show a decreased estrogenicity as demonstrated for 15-OH- ZEN. Independent of the estrogenic effects, the catecholic and epoxidic metabolites identified in this work can be expected to act genotoxic and carcinogenic. The epoxides in particular could fundamentally change the widely accepted view of ZEN causing adverse effects exclusively through endocrine disrupting actions. T3 - BAM Dissertationsreihe - 152 KW - Hydrazinchemie KW - Isotopenstandard KW - SPE-HPLC Automatisierung KW - Zearalenon KW - Isomerisierung PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-386016 SN - 978-3-9817853-9-5 SN - 1613-4249 VL - 152 SP - 1 EP - 160 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maul, Ronald A1 - Greer, B. A1 - Campbell, K. A1 - Elliott, C.T. T1 - Detection of freshwater cyanotoxins and measurement of masked microcystins in tilapia from Southeast Asian aquaculture farms N2 - Recently, there has been a rise in freshwater harmful algal blooms (HABs) globally, as well as increasing aquaculture practices. HABs can produce cyanotoxins, many of which are hepatotoxins. An ultra-performance liquid chromatography tandem mass spectrometry method was developed and validated for nine cyanotoxins across three classes including six microcystins, nodularin, cylindrospermopsin and anatoxin-a. The method was used to analyse free cyanotoxin(s) in muscle (n = 34), liver (n = 17) and egg (n = 9) tissue samples of 34 fish sourced from aquaculture farms in Southeast Asia. Conjugated microcystin was analysed by Lemieux oxidation to ascertain the total amount of microcystin present in muscle. Some tilapia accumulated free microcystin-LR in the muscle tissue at a mean of 15.45 μg/kg dry weight (dw), with total microcystin levels detected at a mean level of 110.1 μg/kg dw, indicating that the amount of conjugated or masked microcystin present in the fish muscle accounted for 85% of the total. Higher levels of cyanotoxin were detected in the livers, with approximately 60% of those tested being positive for microcystin-LR and microcystin-LF, along with cylindrospermopsin. Two fish from one of the aquaculture farms contained cylindrospermopsin in the eggs; the first time this has been reported. The estimated daily intake for free and total microcystins in fish muscle tissue was 2 and 14 times higher, respectively, than the tolerable daily intake value. This survey presents the requirement for further monitoring of cyanotoxins, including masked microcystins, in aquaculture farming in these regions and beyond, along with the implementation of guidelines to safeguard human health. KW - Harmful algal bloom KW - UPLC-MS/MS KW - Bioaccumulation KW - Human health PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-404669 DO - https://doi.org/10.1007/s00216-017-0352-4 SN - 1618-2642 SN - 1618-2650 VL - 409 IS - 16 SP - 4057 EP - 4069 PB - Springer CY - Heidelberg AN - OPUS4-40466 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ritter, B. A1 - Krahl, T. A1 - Rurack, Knut A1 - Kemnitz, E. T1 - Nanoscale CaF2 doped with Eu3+ and Tb3+ through fluorolytic sol-gel synthesis N2 - In this article, the high potential of the fluorolytic sol–gel process to synthesize nanoscopic rare earth-doped calcium fluoride sols is shown. Through a fluorolytic sol–gel process we manage to achieve spherical monodisperse ~5 nm sized nanoparticles using a simple and reproducible one-pot-wet chemical route at room temperature. The as-synthesized clear sols exhibit an intense red and green luminescence under UV excitation at room temperature. A spectroscopic study of the sols revealed the characteristic transitions 5D0 → 7FJ of Eu3+ and 5D4 → 7FJ of Tb3+, with 5D0 → 7F2 (611 nm) of Eu3+ and 5D4 → 7F4 (581 nm) of Tb3+ as the most prominent transitions. This facile synthetic strategy is also valuable for developing other luminescent nanoparticles. KW - Calciumfluorid KW - Europium KW - Lumineszenz KW - Nanopartikel KW - Sol-Gel-Synthese KW - Terbium PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-320120 DO - https://doi.org/10.1039/c4tc01073f SN - 2050-7526 SN - 2050-7534 VL - 2 IS - 40 SP - 8607 EP - 8613 PB - Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-32012 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bolz, Axel A1 - Panne, Ulrich A1 - Rurack, Knut A1 - Buurman, Merwe T1 - Glass fibre paper-based test strips for sensitive SERS sensing N2 - We present paper-based test strips for chemical sensing with surface enhanced Raman scattering as detection method. The test strips are prepared on glass fibre paper with silver nanoparticles and a spray method with an airbrush spray setup as a low cost fabrication approach. The properties of the test strips are investigated with three classical Raman analytes rhodamine 6G, 4-aminothiophenol and adenine and optimized for a good reproducibility of the intensity measurements. All test analytes can be identified at low concentrations. For adenine, a concentration series from 10⁻⁴ M to 10⁻⁸ M is measured and the calibration data can be fitted and evaluated with a Langmuir isotherm model. The optimized test strips are applied for the identification of two antibiotics enoxacin and enrofloxacin. KW - surface enhanced Raman scattering KW - glass fibre paper KW - sensing KW - spray KW - Langmuir isotherm PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-354878 DO - https://doi.org/10.1039/C5AY03096J SN - 1759-9660 VL - 8 IS - 6 SP - 1313 EP - 1318 PB - The Royal Society of Chemistry AN - OPUS4-35487 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kramer, Claus A1 - Ried, Peter A1 - Mahn, Stefan A1 - Richter, Silke A1 - Langhammer, Nicole A1 - Kipphardt, Heinrich T1 - Design and application of a versatile gas calibration for non-metal determination by carrier gas hot extraction N2 - In carrier gas hot extraction the calibration of low amounts of non-metals with masses of a few micrograms with small uncertainty remains a challenge. To achieve high flexibility a high precision gas mixture pump was combined with an automated syringe drive. The gas mixing pump allows filling the syringe with different gas compositions; the automated syringe drive allows matching to modulate the signal profiles to those of real samples. The system was designed and its experimental potential explored. The resulting calibration curves were comparable to those obtained by calibration using solid materials of sufficient purity and stoichiometry. However smaller uncertainties and lower limits of quantification (i.e. 0.5 µg and 0.6 µg for O and N, respectively) were found using the gas calibration device. KW - Non-metal determination KW - CGHE KW - Gas calibration PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-336130 DO - https://doi.org/10.1039/c5ay00845j SN - 1759-9660 SN - 1759-9679 VL - 7 IS - 13 SP - 5468 EP - 5475 PB - RSC Publ. CY - Cambridge AN - OPUS4-33613 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lempke, L. A1 - Fischer, Tobias A1 - Bell, Jérémy A1 - Kraus, Werner A1 - Rurack, Knut A1 - Krause, N. T1 - Gold-catalyzed allene cycloisomerization for pyrrole synthesis: towards highly fluorinated BODIPY dyes N2 - A novel synthetic strategy toward highly fluorinated BODIPY dyes with exceptional photostabilities relying on sustainable gold catalysis has been developed. A key to the tailored pyrrole precursors is the gold catalysis performed in ionic liquids as the reaction medium, allowing a facile recycling of the catalysts. The dyes prepared are well-matching with the spectral windows of popular rhodamine dyes and possess high brightness while showing a distinctly higher photostability than the rhodamines especially in aprotic solvents. KW - Gold-Katalyse KW - BODIPY-Farbstoffe KW - Photostabilität KW - Fluor-Substitution KW - Fluoreszenz PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-344692 DO - https://doi.org/10.1039/c4ob02671c SN - 1477-0520 SN - 1477-0539 VL - 13 IS - 12 SP - 3787 EP - 3791 PB - RSC CY - Cambridge AN - OPUS4-34469 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pascual, L. A1 - Baroja, I. A1 - Aznar, E. A1 - Sancenón, F. A1 - Marcos, M. Dolores A1 - Murguía, J.R. A1 - Amorós, P. A1 - Rurack, Knut A1 - Martínez-Mánez, Ramon T1 - Oligonucleotide-capped mesoporous silica nanoparticles as DNA-responsive dye delivery systems for genomic DNA detection N2 - New hybrid oligonucleotide-capped mesoporous silica nanoparticles able to detect genomic DNA were designed. KW - Gesteuerte Materialien KW - Mycoplasma KW - Mesoporöse Träger KW - Sonden KW - DNA PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-321357 UR - http://pubs.rsc.org/en/content/articlepdf/2015/cc/c4cc08306g DO - https://doi.org/10.1039/C4CC08306G SN - 0022-4936 SN - 0009-241x SN - 1359-7345 SN - 1364-548x VL - 51 IS - 8 SP - 1414 EP - 1416 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-32135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chapartegui-Arias, Ander A1 - Raysyan, A. A1 - Belenguer, A. M. A1 - Jaeger, Carsten A1 - Tchipilov, Teodor A1 - Prinz, Carsten A1 - Abad Andrade, Carlos Enrique A1 - Beyer, S. A1 - Schneider, Rudolf A1 - Emmerling, Franziska T1 - Tailored mobility in a zeolite imidazolate framework (ZIF) antibody conjugate N2 - Zeolitic imidazolate framework (ZIF) hybrid fluorescent nanoparticles and ZIF antibody conjugates have been synthesized, characterized, and employed in lateral-flow immunoassay (LFIA). The bright fluorescence of the conjugates and the possibility to tailor their mobility gives a huge potential for diagnostic assays. An enzyme-linked immunosorbent assay (ELISA) with horseradish peroxidase (HRP) as label, proved the integrity, stability, and dispersibility of the antibody conjugates, LC-MS/MS provided evidence that a covalent link was established between these metal-organic frameworks and lysine residues in IgG antibodies. KW - ZIF KW - ELISA PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532096 DO - https://doi.org/10.1002/chem.202100803 SN - 0947-6539 SN - 1521-3765 VL - 27 IS - 36 SP - 9414 EP - 9421 PB - Wiley-VCH CY - Weinheim AN - OPUS4-53209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Costa, Elena A1 - Climent Terol, Estela A1 - Gawlitza, Kornelia A1 - Wan, Wei A1 - Weller, Michael G. A1 - Rurack, Knut T1 - Optimization of analytical assay performance of antibody-gated indicator-releasing mesoporous silica particles N2 - Antibody-gated indicator delivery (gAID) systems based on mesoporous silica nano- and microparticle scaffolds are a promising class of materials for the sensitive chemical detection of small-molecule analytes in simple test formats such as lateral flow assays (LFAs) or microfluidic chips. Their architecture is reminiscent of drug delivery systems, only that reporter molecules instead of drugs are stored in the voids of a porous host particle. In addition, the pores are closed with macromolecular “caps” through a tailored “gatekeeping” recognition chemistry so that the caps are opened when an analyte has reacted with a “gatekeeper”. The subsequent uncapping leads to a release of a large number of indicator molecules, endowing the system with signal amplification features. Particular benefits of such systems are their modularity and adaptability. With the example of the immunochemical detection of type-I pyrethroids by fluorescent dye-releasing gAID systems, the influence of several tuning modes on the optimisation of such hybrid sensory materials is introduced here. In particular, different mesoporous silica supports (from nano- and microparticles to platelets and short fibres), different functionalisation routes and different loading sequences were assessed. The materials’ performances were evaluated by studying their temporal response behaviour and detection sensitivity, including the tightness of pore closure (through the amount of blank release in the absence of analyte) and the release kinetics. Our results indicate that the better the paratope-accommodating Fab region of the antibody “cap” fits into the host material's pore opening, the better the closing/opening mechanism can be controlled. Because such materials are well-suited for LFAs, performance assessment included a test-strip format besides conventional assays in suspension. In combination with dyes as indicators and smartphones for read-out, simple analytical tests for use by untrained personnel directly at a point-of-need such as an aeroplane cabin can be devised, allowing for sensitivities down to the μg kg−1 range in <5 min with case-required selectivities. KW - Antibody-gated indicator delivery KW - Lateral flow assay KW - SBA-15 KW - SBA-16 KW - Type-I pyrethroids KW - Phenothrin KW - Permethrin KW - Etofenprox KW - Amplification KW - Biosensors KW - Immunoassays KW - Mesoporous particles KW - Optical detection PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-517053 DO - https://doi.org/10.1039/d0tb00371a VL - 8 IS - 22 SP - 4950 EP - 4961 PB - Royal Society of Chemistry AN - OPUS4-51705 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Rurack, Knut A1 - Hecht, Mandy T1 - Loading and Release of Charged and Neutral Fluorescent Dyes into and from Mesoporous Materials: A Key Role for Sensing Applications N2 - The aim of this study is to determine the efficiency of loading and release of several zwitterionic, neutral, anionic and cationic dyes into/from mesoporous nanoparticles to find the optimum loading and release conditions for their application in detection protocols. The loading is carried out for MCM-41 type silica supports suspended in phosphate-buffered saline (PBS) buffer (pH 7.4) or in acetonitrile, involving the dyes (rhodamine B chloride, rhodamine 101 chloride, rhodamine 101 perchlorate, rhodamine 101 inner salt, meso-(4-hydroxyphenyl)-boron–dipyrromethene (BODIPY), sulforhodamine B sodium salt and fluorescein 27). As a general trend, rhodamine-based dyes are loaded with higher efficiency, when compared with BODIPY and fluorescein dyes. Between the rhodamine-based dyes, their charge and the solvent in which the loading process is carried out play important roles for the amount of cargo that can be loaded into the materials. The delivery experiments carried out in PBS buffer at pH 7.4 reveal for all the materials that anionic dyes are more efficiently released compared to their neutral or cationic counterparts. The overall best performance is achieved with the negatively charged sulforhodamine B dye in acetonitrile. This material also shows a high delivery degree in PBS buffer. KW - Mesoporous materials KW - Charged dyes KW - Neutral dyes KW - Dye loading optimisation KW - Dye release PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522596 UR - https://www.mdpi.com/2072-666X/12/3/249 DO - https://doi.org/10.3390/mi12030249 VL - 12 IS - 3 SP - 249 PB - MDPI AN - OPUS4-52259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kimani, Martha Wamaitha A1 - Beyer, S. A1 - El-Schich, Z. A1 - Gawlitza, Kornelia A1 - Rurack, Knut A1 - Gjörloff-Wingren, A. T1 - Imprinted Particles for Direct Fluorescence Detection of Sialic Acid in Polar Media and on Cancer Cells with Enhanced Control of Nonspecific Binding N2 - Glycoproteins are abundant on the cell surface of mammals, providing structural support, modulating cell Membrane properties, and acting as signaling agents. Variation of glycosylation patterns has been found to indicate various disease states, including cell malignancy. Sialic acid (SA) is present as a terminating group on cell-surface glycans, and its overexpression has been linked to several types of cancer. Detection of SA on the cell surface is therefore critical for detection of cancer in its early stages. In this work, a fluorescent molecularly imprinted polymer layer targeting SA was synthesized on the surface of silica-coated polystyrene (PS) particles. Compared to previous works, a PS core supplies a lighter, lower-density support for improved suspension stability and scattering properties. Moreover, their smaller size provides a higher surface-area-to-volume ratio for binding. The incorporation of a fluorescent monomer in the MIP shell allowed for simple and rapid determination of binding specificity in polar media due to a deprotonation−reprotonation interaction mechanism between the fluorescent monomer and SA, which led to spectral changes. Upon titration of the MIP particles with SA in suspension, an increase in fluorescence emission of the particles was observed, with the MIP particles binding SA more selectively compared to the nonimprinted polymer (NIP) control particles. In cell staining experiments performed by flow cytometry, the binding behavior of the MIP particles compared favorably with that of SA-binding lectins. NIPs prepared with a “dummy” template served as a better negative control in cell binding assays due to the favorable inward orientation of template-binding functional groups in the polymer shell, which reduced nonspecific binding. The results show that fluorescent MIPs targeting SA are a promising tool for in vitro fluorescence staining of cancerous cells and for future diagnosis of cancer at early stages. KW - Flow cytometry KW - Sialic acid KW - Fluorescence KW - Molecularly imprinted polymers KW - Cancer cells PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-525216 DO - https://doi.org/10.1021/acsapm.0c01353 VL - 3 IS - 5 SP - 2363 EP - 2373 PB - American Chemical Society AN - OPUS4-52521 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Biyikal, Mustafa A1 - Gröninger, Delia A1 - Weller, Michael G. A1 - Martínez Mánez, R. A1 - Rurack, Knut T1 - Multiplex‐Nachweis von Analyten auf einem einzelnen Teststreifen mit Antikörper‐gesteuerten und Indikator freisetzenden mesoporösen Nanopartikeln N2 - Vor dem Hintergrund der einzigartigen Modularität, hohen Empfindlichkeit und Selektivität von Antikörper‐gesteuerten Indikatorfreisetzungssystemen (gAID‐Systemen) wurde hier ein Multiplex‐Assay für drei organische Explosivstoffmoleküle (TATP, TNT, PETN) entwickelt, der es erlaubt, die Analyten gleichzeitig in flüssiger Phase mit einem einzelnen Teststreifen und einem Fluoreszenzlesegerät bzw. Smartphone als Detektor in Konzentrationen bis in den unteren ppb‐Bereich in <5 min nachzuweisen. Alle drei Systeme, darunter die hier neu entwickelten Systeme für TNT und PETN, tolerieren zudem nicht nur gepufferte wässrige Modelllösungen, sondern auch komplexere Matrices. Neben einem konventionellen Teststreifen mit einem Kanal erlaubte uns die Anwendung von Wachsdrucktechnologie das Herstellen von mehrkanaligen Streifen mit vergleichbarer analytischer Leistungsfähigkeit, was das enorme Potenzial der modular aufgebauten, hybriden Biosensormaterialien im Hinblick auf eine für den Endanwender maßgeschneiderte Vor‐Ort‐Analytik unterstreicht. KW - Multiplex KW - Gesteuerten Nanopartikeln KW - Explosiven PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518431 DO - https://doi.org/10.1002/ange.202009000 SN - 1521-3757 SN - 0044-8249 VL - 132 IS - 52 SP - 24071 EP - 24078 PB - Wiley-VCH CY - Weinheim AN - OPUS4-51843 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Q. A1 - Shinde, S. A1 - Grasso, G. A1 - Caroli, A. A1 - Abouhany, R. A1 - Lanzillotta, M. A1 - Pan, G. A1 - Wan, Wei A1 - Rurack, Knut A1 - Sellergren, B. T1 - Selective detection of phospholipids using molecularly imprinted fluorescent sensory core-shell particles N2 - Sphingosine-1-phosphate (S1P) is a bioactive sphingo-lipid with a broad range of activities coupled to its role in G-protein coupled receptor signalling. Monitoring of both intra and extra cellular levels of this lipid is challenging due to its low abundance and lack of robust affinity assays or sensors. We here report on fluorescent sensory core-shell molecularly imprinted polymer (MIP) particles responsive to near physiologically relevant levels of S1P and the S1P receptor modulator fingolimod phosphate (FP) in spiked human serum samples. Imprinting was achieved using the tetrabutylammonium (TBA) salt of FP or phosphatidic acid (DPPA·Na) as templates in combination with a polymerizable nitrobenzoxadiazole (NBD)-urea monomer with the dual role of capturing the phospho-anion and signalling its presence. The monomers were grafted from ca 300 nm RAFT-modified silica core particles using ethyleneglycol dimethacrylate (EGDMA) as crosslinker resulting in 10–20 nm thick shells displaying selective fluorescence response to the targeted lipids S1P and DPPA in aqueous buffered media. Potential use of the sensory particles for monitoring S1P in serum was demonstrated on spiked serum samples, proving a linear range of 18–60 μM and a detection limit of 5.6 μM, a value in the same range as the plasma concentration of the biomarker. KW - Molecularly imprinted polymers KW - Phospholipids KW - Fluorescence KW - Dye monomers PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509485 DO - https://doi.org/10.1038/s41598-020-66802-3 SN - 2045-2322 VL - 10 IS - 1 SP - 9924 PB - Nature Research CY - London AN - OPUS4-50948 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kuner, Maximilian A1 - Lisec, Jan A1 - Picher, Marie-Idrissa A1 - Rigo, Massimo A1 - Konetzki, Jörg A1 - Haase, Hajo A1 - Koch, Matthias T1 - Development and Application of Isotope Labelled Internal Standards in a Sum Parameter Method for Ergot Alkaloid Screening of Food N2 - Ergot alkaloids are a group of toxic compounds, formed by fungi on infested grasses. In 2022, the European Commission set into effect maximum levels for the sum of the twelve major ergot alkaloids in multiple foods. To facilitate the laborious and costly individual quantification of the twelve major ergot alkaloids by HPLC–MS/MS or -FLD, we recently reported a sum parameter method (SPM) for ergot alkaloid quantification. Here, derivatization to lysergic acid hydrazide—a derivative of the mutual ergoline backbone in all ergot alkaloids—allowed simplified determination of all ergot alkaloids in flour via HPLC-FLD. For the measurement of more complex matrices like processed foods, we now developed a MS/MS-based SPM. Two internal standards (IS), isotopically labelled at different positions of the molecule, were synthesized and employed in the MS/MS-measurements. Method performance using either the 13CD3-labelled or the 15N2-labelled IS was evaluated on naturally contaminated rye and wheat flour samples as well as on processed food matrices. Employing the 13CD3-labelled IS leads to lower variances and better consistency with the reference data (obtained by the FLD-based SPM) in flour samples compared to the 15N2-labelled IS. The novel method significantly improves the measurement of ergot alkaloids in complex food matrices, due to their increased selectivity and thus lower interferences. Furthermore, the application of isotope labelled IS obviates the need for time-consuming steps like the determination of recovery rate based, matrix specific correction factors as described in the MS/MS-based European standard method for ergot alkaloid quantification (EN 17425). KW - Mycotoxins KW - Sum Parameter Method KW - Isotope Labelling KW - HPLC-MS/MS KW - Analytical Chemistry KW - Lysergic acid hydrazide PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588582 DO - https://doi.org/10.1007/s12161-023-02553-x SN - 1936-976X VL - 17 IS - 1 SP - 119 EP - 128 PB - Springer CY - New York, NY AN - OPUS4-58858 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Richter, Silke A1 - Vogl, Jochen A1 - Kipphardt, Heinrich T1 - On the way to SI traceable primary transfer standards for amount of substance measurements in inorganic chemical analysis N2 - During its 25 years of existence, the Inorganic Analysis Working Group of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM IAWG) has achieved much in establishing comparability of measurement results. Impressive work has been done on comparison exercises related to real-world problems in fields such as ecology, food, or health. In more recent attempts, measurements and comparisons were focused on calibration solutions which are the basis of most inorganic chemical measurements. This contribution deals with the question of how to achieve full and transparent SI traceability for the values carried by such solutions. Within this framework, the use of classical primary methods (CPMs) is compared to the use of a primary difference method (PDM). PDM is a method with a dual character, namely a metrological method with a primary character, based on the bundling of many measurement methods for individual impurities, which lead to materials with certified content of the main component. As in classical methods, where small corrections for interferences are accepted, in PDM, many small corrections are bundled. In contrast to classical methods, the PDM is universally applicable to all elements in principle. Both approaches can be used to certify the purity (expressed as mass fraction of the main element) of a high-purity material. This is where the metrological need of National Metrology Institutes (NMIs) for analytical methods meet the challenges of analytical methods. In terms of methods, glow discharge mass spectrometry (GMDS) with sufficient uncertainties for sufficiently small impurity contents is particularly noteworthy for the certification of primary transfer standards (PTS), and isotope dilution mass spectrometry (IDMS), which particularly benefits from PTS (back-spikes) with small uncertainties, is particularly noteworthy for the application. The corresponding relative uncertainty which can be achieved using the PDM is very low (< 10−4). Acting as PTS, they represent the link between the material aspect of the primary calibration solutions and the immaterial world of the International System of Units (SI). The underlying concepts are discussed, the current status of implementation is summarised, and a roadmap of the necessary future activities in inorganic analytical chemistry is sketched. It has to be noted that smaller measurement uncertainties of the purity of high-purity materials not only have a positive effect on chemical measurements, but also trigger new developments and findings in other disciplines such as thermometry or materials science. KW - Inorganic chemical analysis KW - Primary transfer standards (PTSs) KW - Traceability KW - Classical primary measurement method (CPM) KW - Primary difference measurement method (PDM) KW - Metrology in chemistry PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572743 DO - https://doi.org/10.1007/s00216-023-04660-4 SN - 1618-2642 SN - 1618-2650 VL - 415 SP - 3057 EP - 3071 PB - Springer CY - Berlin AN - OPUS4-57274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Roesch, Philipp A1 - Wittwer, Philipp A1 - Piechotta, Christian A1 - Lisec, Jan A1 - Sommerfeld, Thomas A1 - Kluge, Stephanie A1 - Herzel, Hannes A1 - Huthwelker, T. A1 - Borca, C. A1 - Simon, Franz-Georg T1 - Levels of per- and polyfluoroalkyl substances (PFAS) in various wastewater-derived fertilizers - Analytical investigations from different perspectives N2 - Solid wastewater-based fertilizers were screened for per- and polyfluoroalkyl substances (PFAS) by the extractable organic fluorine (EOF) sum parameter method. The EOF values for ten sewage sludges from Germany and Switzerland range from 154 to 7209 mg kg−1. For thermal treated sewage sludge and struvite the EOF were lower with values up to 121 mg kg−1. Moreover, the application of PFAS targeted and suspect screening analysis of selected sewage sludge samples showed that only a small part of the EOF sum parameter values can be explained by the usually screened legacy PFAS. The hitherto unknown part of EOF sum parameter contains also fluorinated pesticides, pharmaceutical and aromatic compounds. Because these partly fluorinated compounds can degrade to (ultra-)short PFAS in wastewater treatment plants they should be considered as significant sources of organic fluorine in the environment. The combined results of sum parameter analysis and suspect screening reveal the need to update current regulations, such as the German fertilizer ordinance, to focus not solely on a few selected PFAS such as perfluorooctane sulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) but consider an additional sum parameter approach as a more holistic alternative. Moreover, diffusion gradient in thin-films (DGT) passive samplers were utilized as an alternative simplified extraction method for PFAS in solid wastewater-based fertilizers and subsequently quantified via combustion ion chromatography. However, the DGT method was less sensitive and only comparable to the EOF values of the fertilizers in samples with >150 mg kg−1, because of different diffusion properties for various PFAS, but also kinetic exchange limitations. KW - Combustion ion chromatography KW - Per- and polyfluoroalkyl substances (PFAS) KW - Sewage sludge KW - Fertilizer PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583429 DO - https://doi.org/10.1039/d3va00178d SN - 2754-7000 VL - 2 IS - 10 SP - 1436 EP - 1445 PB - Royal Society of Chemistry (RSC) CY - London AN - OPUS4-58342 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agudo Jácome, Leonardo A1 - Pöthkow, K. A1 - Paetsch, O. A1 - Hege, H.-C. T1 - Three-dimensional reconstruction and quantification of dislocation substructures from transmission electron microscopy stereo pairs N2 - A great amount of material properties is strongly influenced by dislocations, the carriers of plastic deformation. It is therefore paramount to have appropriate tools to quantify dislocation substructures with regard to their features, e.g., dislocation density, Burgers vectors or line direction. While the transmission electron microscope (TEM) has been the most widely-used equipment implemented to investigate dislocations, it usually is limited to the two-dimensional (2D) observation of three-dimensional (3D) structures. We reconstruct, visualize and quantify 3D dislocation substructure models from only two TEM images (stereo pairs) and assess the results. The reconstruction is based on the manual interactive tracing of filiform objects on both images of the stereo pair. The reconstruction and quantification method are demonstrated on dark field (DF) scanning (S)TEM micrographs of dislocation substructures imaged under diffraction contrast conditions. For this purpose, thick regions (> 300 nm) of TEM foils are analyzed, which are extracted from a Ni-base superalloy single crystal after high temperature creep deformation. It is shown how the method allows 3D quantification from stereo pairs in a wide range of tilt conditions, achieving line length and orientation uncertainties of 3% and 7°, respectively. Parameters that affect the quality of such reconstructions are discussed. KW - Dislocation KW - Diffraction contrast KW - Scanning transmission electron microscopy (STEM) KW - Stereoscopy KW - Visualization PY - 2018 DO - https://doi.org/10.1016/j.ultramic.2018.08.015 SN - 0304-3991 VL - 195 SP - 157 EP - 170 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-46355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kimani, Martha Wamaitha T1 - Fluorescent core/shell molecularly-imprinted nanoparticles for staining sialic acid (SA) residues on tumor cells N2 - Cancer is a leading cause of death worldwide, and its early detection and resultant treatment contributes significantly to patient recovery and survival. Detection is currently based on magnetic resonance imaging and computed tomography, methods that are expensive, while processing of the results is time consuming. There is a need for low-cost cancer-detection techniques that give conclusive results in the shortest time possible. Molecularly imprinted polymers (MIPs) targeting tumor markers on cancerous cells may provide a cheaper solution for cancer detection. Thin MIP layers immobilized on particle platforms are known to give faster response times and increased selectivity in comparison to bulk MIPs. It has been reported that a fluorescent monomer can be incorporated into the MIP layer, allowing for faster detection of the target group, thus significantly shortening the turn-around time for biopsies. Changes in sialylation patterns of cell surface glycoproteins indicate malignancy. Here, we present the development of MIPs that target sialic acid-terminated glycoproteins (SA MIPs), prepared as a thin layer on a silica nanoparticle platform. A fluorescent monomer is incorporated into the MIP layer, and upon binding of the target group to the specific binding pockets in the MIP, the fluorescence signal is enhanced. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) are used for structural characterization. To validate the specificity, fluorescence changes of MIPs in the presence and absence of template are compared to their corresponding non-imprinted polymer particles (NIP). Initial binding experiments with tumor cells using fluorescence microscopy demonstrate that the presented technique shows promise as a cheaper alternative to current detection methods, while allowing for relatively shorter analysis of biopsy results. T2 - MIP 2018 CY - Hebrew University Jerusalem, Belgium House, Israel DA - 24.07.2018 KW - Sialic acid KW - MIPs KW - Fluorescence PY - 2018 AN - OPUS4-45419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sebald, M. A1 - Gebauer, J. A1 - Koch, Matthias T1 - Concise Synthesis of Alternariol and Alternariol-9-monomethyl ether as well as their D3-Isotopologues N2 - Abstract Alternariol (AOH) and alternariol-9-monomethyl ether (AME) are two secondary metabolites of Alternaria fungi which can be found in various foodstuff like tomatoes, nuts, and grains. Due to their toxicity and potential mutagenic activity the need for the development of high-throughput methods for the supervision of AOH- and AME-levels is of increasing interest. As the availability of both native and labeled AOH and AME analytical standards is very limited we herein wish to present a novel concise approach towards their synthesis employing a ruthenium-catalyzed ortho-arylation as the key step. Finally, we demonstrate their suitability as internal standards in stable-isotope dilution assay (SIDA)-HPLC-MS/MS analysis commonly used for the quantification of the natural products in food and feed. KW - Mycotoxins KW - Food Analysis KW - Emerging contaminants PY - 2021 DO - https://doi.org/10.1055/a-1698-8328 SN - 0039-7881 VL - 54 IS - 19 SP - 4285 EP - 4293 PB - Thieme AN - OPUS4-53994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mi, W. A1 - Josephs, R. D. A1 - Melanson, J. E. A1 - Dai, X. A1 - Wang, Y. A1 - Zhai, R. A1 - Chu, Z. A1 - Fang, X. A1 - Thibeault, M.-P. A1 - Stocks, B. B. A1 - Meija, J. A1 - Bedu, M. A1 - Martos, G. A1 - Westwood, S. A1 - Wielgosz, R. I. A1 - Liu, Q. A1 - Teo, T. L. A1 - Liu, H. A1 - Tan, Y. J. A1 - Öztuğ, M. A1 - Saban, E. A1 - Kinumi, T. A1 - Saikusa, K. A1 - Schneider, Rudolf A1 - Weller, Michael G. A1 - Konthur, Zoltán A1 - Jaeger, Carsten A1 - Quaglia, M. A1 - Mussell, C. A1 - Drinkwater, G. A1 - Giangrande, C. A1 - Vaneeckhoutte, H. A1 - Boeuf, A. A1 - Delatour, V. A1 - Lee, J. E. A1 - O'Connor, G. A1 - Ohlendorf, R. A1 - Henrion, A. A1 - Beltrão, P. J. A1 - Naressi Scapin, S. M. A1 - Sade, Y. B. T1 - PAWG Pilot Study on Quantification of SARS-CoV-2 Monoclonal Antibody - Part 1 N2 - Under the auspices of the Protein Analysis Working Group (PAWG) of the Comité Consultatif pour la Quantité de Matière (CCQM) a pilot study, CCQM-P216, was coordinated by the Chinese National Institute of Metrology (NIM), National Research Council of Canada (NRC) and the Bureau International des Poids et Mesures (BIPM). Eleven Metrology Institutes or Designated Institutes and the BIPM participated in the first phase of the pilot study (Part 1). The purpose of this pilot study was to develop measurement capabilities for larger proteins using a recombinant humanized IgG monoclonal antibody against Spike glycoprotein of SARS-CoV-2 (Anti-S IgG mAb) in solution. The first phase of the study was designed to employ established methods that had been previously studies by the CCQM Protein Analysis Working Group, involving the digestion of protein down to the peptide or amino acid level. The global coronavirus pandemic has also led to increased focus on antibody quantitation methods. IgG are among the immunoglobulins produced by the immune system to provide protection against SARS-CoV-2. Anti-SARS-CoV-2 IgG can therefore be detected in samples from affected patients. Antibody tests can show whether a person has been exposed to the SARS-CoV-2, and whether or not they potentially show lasting immunity to the disease. With the constant spread of the virus and the high pressure of re-opening economies, antibody testing plays a critical role in the fight against COVID-19 by helping healthcare professionals to identify individuals who have developed an immune response, either via vaccination or exposure to the virus. Many countries have launched large-scale antibody testing for COVID-19. The development of measurement standards for the antibody detection of SARS-CoV-2 is critically important to deal with the challenges of the COVID-19 pandemic. In this study, the SARS-CoV-2 monoclonal antibody is being used as a model system to build capacity in methods that can be used in antibody quantification. Amino acid reference values with corresponding expanded uncertainty of 36.10 ± 1.55 mg/kg, 38.75 ± 1.45 mg/kg, 18.46 ± 0.78 mg/kg, 16.20 ± 0.67 mg/kg and 30.61 ± 1.30 mg/kg have been established for leucine, valine, phenylalanine, isoleucine and proline, respectively. Agreement between nearly all laboratories was achieved for the amino acid analysis within 2 to 2.5 %, with one participant achieving markedly higher results due to a technical issue found in their procedure; this result was thus excluded from the reference value calculations. The relatively good agreement within a laboratory between different amino acids was not dissimilar to previous results for peptides or small proteins, indicating that factors such as hydrolysis conditions and calibration procedures could be the largest sources of variability. Peptide reference values with corresponding expanded uncertainty of 4.99 ± 0.28 mg/kg and 6.83 ± 0.65 mg/kg have been established for ALPAPIEK and GPSVFPLAPSSK, respectively. Not surprisingly due to prior knowledge from previous studies on peptide quantitation, agreement between laboratories for the peptide-based analysis was slightly poorer at 3 to 5 %, with one laboratory's result excluded for the peptide GPSVFPLAPSSK. Again, this level of agreement was not significantly poorer than that achieved in previous studies with smaller or less complex proteins. To reach the main text of this paper, click on Final Report. KW - Antibody quantification KW - Amino acid analysis KW - Peptide analysis KW - Round robin test PY - 2021 DO - https://doi.org/10.1088/0026-1394/59/1a/08001 VL - 59 IS - 1A SP - 08001 AN - OPUS4-54972 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bilsel, M. A1 - Goren, A.C. A1 - Gokcen, T. A1 - Gunduz, S. A1 - Koch, Matthias A1 - Kaloulides, E. A1 - Giannikopoulou, P. A1 - Wai-Tong, G.T. A1 - Chan, A. T1 - Report on key comparison CCQM-K138: determination of aflatoxins (AFB(1), AFB(2), AFG(1), AFG(2) and total AFs) in dried fig N2 - The presence of any aflatoxin contamination in exported figs needs to be monitored and measured through reliable and traceable methods, which require pure and matrix certified reference materials. On the other hand, certified reference materials (CRM) for determination of aflatoxins in dried fig are not yet available. Moreover, there is a lack of CRMs to be used in routine testing laboratories for method validation and quality control. The routine testing laboratories, participating in commercial proficiency testing (PT) programs, use the results available from consensus values to evaluate the performance of the participating laboratories, rather than metrologically traceable assigned values. This study initially proposed as a key comparison and presented at the EURAMET TC-MC SCOA meeting in Malta in 2015 and subsequently at the CCQM OAWG meeting in April 2015, proposes a CRM candidate for determination of levels of aflatoxins B1, B2, G1, G2 and their total in dried. Evidence of successful participation in formal, relevant international comparisons are needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (DIs). In total nine NMI/DI participated in the Track C Key Comparison CCQM-K138 Determination of aflatoxins (AFB1, AFB2, AFG1, AFG2 and Total AFs) in Dried Fig. Participants were requested to evaluate the mass fractions expressed in ng/g units, of aflatoxins B1, B2, G1, G2 and total aflatoxin in a dried food matrix, dried fig. The CCQM-K138 results for the determination of aflatoxins (AFB1, AFB2, AFG1, AFG2 and total AFs) are ranging from 5.17 to 7.27 ng/g with an %RSD of 10.47 for AFB1, ranging from 0.60 to 0.871 ng/g with an %RSD of 11.69 for AFB2, ranging from 1.98 to 2.6 ng/g with an %RSD of 10.36 for AFG1, ranging from 0.06 to 0.32 ng/g with an %RSD of 35.6 for AFG2, and ranging from 8.29 to 10.31 ng/g with an %RSD of 7.69 for Total AFs. All participants based their analyses on LC-MS/MS, HPLC-FLD, HR-LC/MS, and IDMS. Brief descriptions of the analytical methods used by the participants, including sample preparation, analytical technique, calibrants, and quantification approach are summarized in Appendix F. Linear Pool was used to assign the Key Comparison Reference Values (KCRVs) for B1, B2, G1, G2 and total aflatoxins. Due to the traceability requirements for the calibrants not being met, results of KEBS, INTI, VNIIM and BAM were excluded from KCRV determination. Successful participation in CCQM-K138 demonstrates the following measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having high polarity (pKow > -2), in mass fraction range from 0.05 ng/g to 500 ng/g in dried food matrices. KW - Aflatoxins KW - Mycotoxins KW - Dried fig KW - Food contaminants PY - 2019 DO - https://doi.org/10.1088/0026-1394/56/1A/08008 SN - 0026-1394 SN - 1681-7575 VL - 56 IS - 1A SP - 08008-1 EP - 08008-106 PB - IOP CY - Bristol AN - OPUS4-50326 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sebald, M. A1 - Gebauer, J. A1 - Koch, Matthias T1 - Diastereoselective synthesis of (±)-trichodiene and (±)-trichodiene-D3 as analytical standards for the on-site quantification of trichothecenes N2 - The ubiquitous Fusarium genus is responsible for the spoilage of vast amounts of cereals and fruits. Besides the economic damage, the danger to human and animal health by the concomitant exposure to mycotoxins represents a serious problem. A large number of Fusarium species produce a variety of different mycotoxins of which the class of trichothecenes are of particular importance due to their toxicity. Being identified as the common volatile precursor during the biosynthesis of trichothecenes, (−)-trichodiene (TD) is considered to be a biomarker for the respective mycotoxin content in food samples. We postulated that the development of a non-invasive, on-site GC-IMS method for the quantification of (−)-trichodiene supplemented with a stationary SIDA headspace GC-MS reference method would allow circumventing the laborious and expensive analyses of individual trichothecenes in large cereal samples. In this work we present the syntheses of the required native calibration standard and an isotope labeled (TD-D3) internal standard. KW - Mycotoxins KW - Volatile marker KW - Food analysis KW - Screening method KW - Mobile analysis PY - 2021 DO - https://doi.org/10.1039/d1ob01778k VL - 19 IS - 45 SP - 9872 EP - 9879 PB - RSC AN - OPUS4-53993 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - The SMURFnano project - standardized measurements of surface functionalities on nanoparticles N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, optoelectronics, and information storage. NP function, interaction with biological species, and environmental fate are largely determined by surface functionalities. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, and mandatory to meet increasing concerns regarding their safety. Also, industry, international standardization organizations, regulatory agencies, and policymakers need validated and standardized measurement methods and reference materials. However, methodologies for determining NP surface properties, including the amount, chemical composition, and homogeneity of surface functionalities and coatings are largely non-standardized. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR) as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. The latter less costly methods are often used by SMEs, e.g., for quality control. To validate methods, establish measurement uncertainties, test reference materials, and produce reference data, international interlaboratory comparisons (ILC) on NP surface functionalization measurements are required and well characterized test and reference nanomaterials providing benchmark values.[1] These needs are addressed by the recently started European metrology project SMURFnano involving 12 partners from different National Metrology Institutes, designated institutes, and research institutes, two university groups as well as one large company and one SME producing NPs. This project as well as first results derived from the development of test and reference materials with a well characterized surface chemistry and ongoing interlaboratory comparisons will be presented. T2 - eMRS CY - Strasbourg, France DA - 27.05.2025 KW - Quality assurance KW - Reference analysis KW - Standardization KW - Metrology KW - Reference products KW - Reference materials KW - Mission KW - Surface chemistry KW - Nano KW - Particle KW - qNMR KW - XPS KW - Fluorescence KW - Optical assays KW - Interlaboratory comparison KW - Uncertainty PY - 2025 AN - OPUS4-63243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Asadujjaman, Asad T1 - Switching of nanoparticles' fluorescence between "ON" and "OFF" states by a thermoresponsive polymeric layer N2 - Fluorescent nanoparticles that “light up”/”dim down” by applying external stimuli are of particular interest in the fields of sensing, diagnostics, photonics, protective coatings and microfluidics. The current challenge for these materials is to combine for instance fluorescence and its response to a stimulus such as temperature in a precise manner. Here we present such a system based on a core/shell/shell architecture consisting of a silica core with a fluorescent layer and a thermoresponsive shell. The silica core nanoparticles were first coated with a fluorescent shell using surface initiated reversible addition-fragmentation chain transfer (RAFT) polymerization. The fluorescent nanoparticles were then completely engulfed by a switchable protective coating made of thermoresponsive poly(N-isopropylacrylamide). The fluorescence of the nanoparticles could be “switched on” at room temperature and “switched off” with increasing environmental temperature because of the presence of the thermoresponsive layer. Insights into this phenomenon will be given based on temperature dependent fluorescence measurements and dynamic light scattering. T2 - Hybrid materials Konferenz CY - Lisbon, Portugal DA - 06.03.2017 KW - Core/shell/shell KW - Thermoresponsive polymers KW - Fluorescence materials PY - 2017 AN - OPUS4-39581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Lisec, Jan A1 - Koch, Matthias T1 - Changes in Black Truffle (Tuber melanosporum) Aroma during Storage under Different Conditions N2 - The enticing aroma of truffles is a key factor for their culinary value. Although all truffle species tend to be pricy, the most intensely aromatic species are the most sought after. Research into the aroma of truffles encompasses various disciplines including chemistry, biology, and sensory science. This study focusses on the chemical composition of the aroma of black truffles (Tuber melanosporum) and the changes occurring under different storage conditions. For this, truffle samples were stored under different treatments, at different temperatures, and measured over a total storage time of 12 days. Measurements of the truffle aroma profiles were taken with SPME/GC–MS at regular intervals. To handle the ample data collected, a systematic approach utilizing multivariate data analysis techniques was taken. This approach led to a vast amount of data which we made publicly available for future exploration. Results reveal the complexity of aroma changes, with 695 compounds identified, highlighting the need for a comprehensive understanding. Principal component analyses offer initial insights into truffle composition, while individual compounds may serve as markers for age (formic acid, 1-methylpropyl ester), freshness (2-Methyl-1-propanal; 1-(methylthio)-propane), freezing (tetrahydrofuran), salt treatment (1-chloropentane), or heat exposure (4-hydroxy-3-methyl-2-butanone). This research suggests that heat treatment or salt contact significantly affects truffle aroma, while freezing and cutting have less pronounced effects in comparison. The enrichment of compounds showing significant changes during storage was investigated with a metabolomic pathway analysis. The involvement of some of the enriched compounds on the pyruvate/glycolysis and sulfur pathways was shown. KW - Mass Spectrometry KW - Metabolomics KW - Tuber melanosporum KW - Truffle Aroma PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601731 DO - https://doi.org/10.3390/jof10050354 VL - 10 IS - 5 SP - 1 EP - 22 PB - MDPI AN - OPUS4-60173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Russo, Francesco F. A1 - Nowatzky, Yannek A1 - Jaeger, Carsten A1 - Parr, Maria K. A1 - Benner, Philipp A1 - Muth, Thilo A1 - Lisec, Jan T1 - Machine learning methods for compound annotation in non‐targeted mass spectrometry—A brief overview of fingerprinting, in silico fragmentation and de novo methods N2 - Non‐targeted screenings (NTS) are essential tools in different fields, such as forensics, health and environmental sciences. NTSs often employ mass spectrometry (MS) methods due to their high throughput and sensitivity in comparison to, for example, nuclear magnetic resonance–based methods. As the identification of mass spectral signals, called annotation, is labour intensive, it has been used for developing supporting tools based on machine learning (ML). However, both the diversity of mass spectral signals and the sheer quantity of different ML tools developed for compound annotation present a challenge for researchers in maintaining a comprehensive overview of the field.In this work, we illustrate which ML‐based methods are available for compound annotation in non‐targeted MS experiments and provide a nuanced comparison of the ML models used in MS data analysis, unravelling their unique features and performance metrics. Through this overview we support researchers to judiciously apply these tools in their daily research. This review also offers a detailed exploration of methods and datasets to show gaps in current methods, and promising target areas, offering a starting point for developers intending to improve existing methodologies. KW - Mass Spectrometry KW - Spectra annotation KW - Machine learning PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-608732 DO - https://doi.org/10.1002/rcm.9876 VL - 38 IS - 20 SP - 1 EP - 15 PB - Wiley AN - OPUS4-60873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Kun A1 - Carrod, Andrew J. A1 - Del Giorgio, Elena A1 - Hughes, Joseph A1 - Rurack, Knut A1 - Bennet, Francesca A1 - Hodoroaba, Vasile-Dan A1 - Harrad, Stuart A1 - Pikramenou, Zoe T1 - Luminescence Lifetime-Based Sensing Platform Based on Cyclometalated Iridium(III) Complexes for the Detection of Perfluorooctanoic Acid in Aqueous Samples N2 - Luminescence lifetimes are an attractive analytical method for detection due to its high sensitivity and stability. Iridium probes exhibit luminescence with long excited-state lifetimes, which are sensitive to the local environment. Perfluorooctanoic acid (PFOA) is listed as a chemical of high concern regarding its toxicity and is classified as a “forever chemical”. In addition to strict limits on the presence of PFOA in drinking water, environmental contamination from industrial effluent or chemical spills requires rapid, simple, accurate, and cost-effective analysis in order to aid containment. Herein, we report the fabrication and function of a novel and facile luminescence sensor for PFOA based on iridium modified on gold surfaces. These surfaces were modified with lipophilic iridium complexes bearing alkyl chains, namely, IrC6 and IrC12, and Zonyl-FSA surfactant. Upon addition of PFOA, the modified surfaces IrC6-FSA@Au and IrC12-FSA @Au show the largest change in the red luminescence signal with changes in the luminescence lifetime that allow monitoring of PFOA concentrations in aqueous solutions. The platform was tested for the measurement of PFOA in aqueous samples spiked with known concentrations of PFOA and demonstrated the capacity to determine PFOA at concentrations >100 μg/L (240 nM). KW - Perfluorooctanoic Acid (PFOA) KW - Cyclometalated iridium (III) complexes KW - Luminescent lifetime KW - Optically active surfaces KW - ToF-SIMS PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594535 UR - https://pubs.acs.org/doi/10.1021/acs.analchem.3c04289 DO - https://doi.org/10.1021/acs.analchem.3c04289 VL - 96 IS - 4 SP - 1565 EP - 1575 PB - American Chemical Society (ACS) AN - OPUS4-59453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tobias, Charlie A1 - López-Puertollano, Daniel A1 - Abad-Somovilla, Antonio A1 - Mercader, J. V. A1 - Abad-Fuentes, A. A1 - Rurack, Knut T1 - Development of Simple and Rapid Bead-Based Cytometric Immunoassays Using Superparamagnetic Hybrid Core−Shell Microparticles N2 - Flow cytometry-based immunoassays are valuable in biomedical research and clinical applications due to their high throughput and multianalyte capability, but their adoption in areas such as food safety and environmental monitoring is limited by long assay times and complex workflows. Rapid, simplified bead-based cytometric immunoassays are needed to make these methods viable for point-of-need applications, especially with the increasing accessibility of miniaturized cytometers. This work introduces superparamagnetic hybrid polystyrene-silica core−shell microparticles as promising alternatives to conventional polymer beads in competitive cytometric immunoassays. These beads, featuring high specificity, sensitivity, and excellent handling capabilities via magnetic separation, were evaluated with three different antibodies and binding methods, showing variations in signal intensity based on the antibody and its attachment method. The optimal performance was achieved through a secondary antibody binding approach, providing strong and consistent signals with minimal uncertainty. The optimized protocol made it possible to achieve a detection limit of 0.025 nM in a total assay time of only 15 min and was successfully used to detect ochratoxin A (OTA) in raw flour samples. This work highlights the potential of these beads as versatile tools for flow cytometry-based immunoassays, with significant implications for food safety, animal health, environmental monitoring, and clinical diagnostics. KW - Immunoassays KW - Bead-based KW - Core-shell particles KW - Cytometry KW - Mycotoxins PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-610593 DO - https://doi.org/10.1021/acsmeasuresciau.4c00038 SP - 1 EP - 11 PB - American Chemical Society CY - Washington, D.C. AN - OPUS4-61059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias A1 - Sebald, M. T1 - Novel Approach towards the Synthesis of Deuterium-labelled Alternariol- and Alternariol monomethylether-Standards for the HPLC-MS/MS-Analysis in Food & Feed N2 - Alternariol (AOH) and Alternariol monomethylether (AME) are two secondary metabolites of Alternaria fungi which can be found in various foodstuffs like tomatoes, nuts and grains. Due to their toxicity and potential mutagenic activity, the need for the development of high-throughput methods for the supervision of AOH- and AME-levels is of increasing interest. As the availability of both native and labelled AOH and AME analytical standards is very limited we herein wish to present a novel concise approach towards their synthesis employing a ruthenium-catalyzed ortho-arylation4 as the key step. T2 - 15th International Symposium on Biological and Environmental Reference Materials (BERM) CY - Berlin, Germany DA - 23.09.2018 KW - Mycotoxins KW - Stable-Isotope-Dilution-Analysis PY - 2018 AN - OPUS4-46489 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Gawlitza, Kornelia T1 - Gas standards for the calibration of novel fluorescence sensors for ammonia N2 - Ammonia and its conversion product ammonium have a strong negative impact on human health and ecosystems. Most ammonia measurements in ambient air are performed in the molar fraction range (0.5 to 500) nmol/mol. There is a need for reliable traceable ammonia gas standards as well as in situ analytical procedures for the monitoring of ammonia in ambient air. The permeation method is an effective tool for dynamically generating precise gas standards with a low uncertainty in the concentration range of a few nmol/mol to several µmol/mol in an inert carrier gas, e. g. pure nitrogen or purified ambient air. Here, we present our ammonia gas standard generator as well as results of the characterisation of its individual components supporting the uncertainty assessment according to GUM for stable gas concentrations in this range. In order to detect ammonia in the nmol/mol-range, a suitable sensor has to be developed. In this contribution, we therefore additionally present first approaches on the development of such a sensor using optical fluorescence as transduction mechanism due to its intrinsically high sensitivity and high spatial resolution. Incorporation of a fluorescent dye, which shows fluorescence enhancement in the presence of ammonia, into a polymer matrix allows to reversibly recognize low amounts of ammonia. It can be concluded that fluorescence sensor is a robust tool for measurements of ammonia; however it needs calibration for the planed use. T2 - MetNH3-workshop on the progress in ammonia metrology CY - Braunschweig, Germany DA - 24.02.2016 KW - Ammonia KW - Fluorescence sensor KW - Permeation KW - Test gas generation PY - 2016 AN - OPUS4-35810 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mansurova, Maria A1 - Johann, Sergej A1 - Kohlhoff, Harald A1 - Rurack, Knut A1 - Bartholmai, Matthias A1 - Bell, Jérémy T1 - On-Site Analytical Tool Based on Crude Oil Fluorescence and Chemometrics for the Rapid Determination of the Nature and Essential Properties of Oil Spills N2 - With the reduction of large oil spills because of stricter regulations and safety measures, the question of how to manage smaller oil spills arises. Few on-site analytical tools are available for first responders or other law enforcement personnel to rapidly test for crude oil in the early management of localized polluted areas. The approach reported here relies on well-described computer-assisted multivariate data analysis of the intrinsic fluorescence fingerprints of crude oils to build a multivariate model for the rapid classification of crude oils and the prediction of their properties. Thanks to a dedicated robust portable reader, the method allowed classification and accurate prediction of various properties of crude oil samples like density (according to API, the American Petroleum Institute and viscosity as well as composition parameters such as volume fractions of paraffins or aromatics. In this way, autonomous operation in on-site or in-the-field applications becomes possible based on the direct (undiluted and untreated) measurement of samples and a rapid, tablet-operated readout system to yield a robust and simple analytical test with superior performance. Testing in real-life scenarios allowed the successful classification and prediction of a number of oil spill samples as well as weathered samples that closely resemble samples collected by first responders. KW - Oil spills KW - Fluorescence KW - PCA KW - Petroleum KW - Rapid test KW - Portable PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-595442 DO - https://doi.org/10.1021/acsestwater.3c00648 VL - 4 IS - 2 SP - 621 EP - 627 PB - American Chemical Society (ACS) AN - OPUS4-59544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tukhmetova, Dariya A1 - Lisec, Jan A1 - Vogl, Jochen A1 - Meermann, Björn T1 - Development of an Online Isotope Dilution CE/ICP–MS Method for the Quantification of Sulfur in Biological Compounds N2 - We report an analytical methodology for the quantification of sulfur in biological molecules via a speciesunspecific postcolumn isotope dilution (online ID) approach using capillary electrophoresis (CE) coupled online with inductively coupled plasma−mass spectrometry (online ID CE/ICP−MS). The method was optimized using a mixture of standard compounds including sulfate, methionine, cysteine, cystine, and albumin, yielding compound recoveries between 98 and 105%. The quantity of sulfur is further converted to the quantity of the compounds owing to the prior knowledge of the sulfur content in the molecules. The limit of detection and limit of quantification of sulfur in the compounds were 1.3−2.6 and 4.1−8.4 mg L−1, respectively, with a correlation coefficient of 0.99 within the concentration range of sulfur of 5−100 mg L−1. The capability of the method was extended to quantify albumin in its native matrix (i.e., in serum) using experimentally prepared serum spiked with a pure albumin standard for validation. The relative expanded uncertainty of the method for the quantification of albumin was 6.7% (k = 2). Finally, we tested the applicability of the method on real samples by the analysis of albumin in bovine and human sera. For automated data assessment, a software application (IsoCor) which was developed by us in a previous work was developed further for handling of online ID data. The method has several improvements compared to previously published setups: (i) reduced adsorption of proteins onto the capillary wall owing to a special capillary-coating procedure, (ii) baseline separation of the compounds in less than 30 min via CE, (iii) quantification of several sulfur species within one run by means of the online setup, (iv) SI traceability of the quantification results through online ID, and (v) facilitated data processing of the transient signals using the IsoCor application. Our method can be used as an accurate approach for quantification of proteins and other biological molecules via sulfur analysis in complex matrices for various fields, such as environmental, biological, and pharmaceutical studies as well as clinical diagnosis. Sulfur is an essential element in living organisms, where it plays important roles in various biological processes, such as protein synthesis, enzyme activity, and antioxidant defense. However, the biological effects of different sulfur species can vary widely, and imbalances in sulfur speciation have been observed in a range of diseases, including cancer, Alzheimer’s disease, and diabetes.1−3 The accurate quantification of sulfur and its species in biological samples requires sensitive and selective analytical techniques. In recent years, separation techniques coupled online with inductively coupled plasma−mass spectrometry (ICP−MS) have emerged as powerful online analytical tools complementary to molecular spectrometric methods for speciation analysis of biological compounds. External calibration4−9 and isotope dilution (ID)10−15 are common calibration approaches applied for online quantification of sulfur species in complex samples. The ID analysis is advantageous over. KW - Analytical Chemistry KW - CE/MC-ICP-MS KW - species-specific isotope information PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594736 DO - https://doi.org/10.1021/acs.analchem.3c03553 SN - 0003-2700 SP - 1 EP - 8 PB - American Chemical Society (ACS) AN - OPUS4-59473 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Recknagel, Sebastian A1 - Prinz, Carsten A1 - Vogel, Kristin A1 - Koch, Matthias A1 - Becker, Roland T1 - eCerto—versatile software for interlaboratory data evaluation and documentation during reference material production N2 - The statistical tool eCerto was developed for the evaluation of measurement data to assign property values and associated uncertainties of reference materials. The analysis is based on collaborative studies of expert laboratories and was implemented using the R software environment. Emphasis was put on comparability of eCerto with SoftCRM, a statistical tool based on the certification strategy of the former Community Bureau of Reference. Additionally, special attention was directed towards easy usability from data collection through processing, archiving, and reporting. While the effects of outlier removal can be flexibly explored, eCerto always retains the original data set and any manipulation such as outlier removal is (graphically and tabularly) documented adequately in the report. As a major reference materials producer, the Bundesanstalt für Materialforschung und -prüfung (BAM) developed and will maintain a tool to meet the needs of modern data processing, documentation requirements, and emerging fields of RM activity. The main features of eCerto are discussed using previously certified reference materials. KW - Reference material KW - Statistics KW - Software KW - Collaborative trial PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-591851 DO - https://doi.org/10.1007/s00216-023-05099-3 SP - 1 EP - 9 PB - Springer Science and Business Media LLC AN - OPUS4-59185 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herter, Sven-Oliver A1 - Koch, Matthias A1 - Haase, Hajo T1 - First Synthesis of Ergotamine-13CD3 and Ergotaminine-13CD3 from Unlabeled Ergotamine N2 - Ergot alkaloids (EAs) formed by Claviceps fungi are one of the most common food contaminants worldwide, affecting cereals such as rye, wheat, and barley. To accurately determine the level of contamination and to monitor EAs maximum levels set by the European Union, the six most common EAs (so-called priority EAs) and their corresponding epimers are quantified using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). The quantification of EAs in complex food matrices without appropriate internal tandards is challenging but currently carried out in the standard method EN 7425:2021 due to their commercial unavailability. To address the need for isotopically labeled EAs, we focus on two semi-synthetic approaches for the synthesis of these reference standards. Therefore, we investigate the feasibility of the N6-demethylation of native ergotamine to yield norergotamine, which can subsequently be remethylated with an isotopically labeled methylating reagent, such as iodomethane (13CD3-I), to yield isotopically labeled ergotamine and its C8-epimer ergotaminine. Testing the isotopically labeled ergotamine/-inine against native ergotamine/-inine with HPLC coupled to high-resolution HR-MS/MS proved the structure of ergotamine-13CD3 and ergotaminine-13CD3. Thus, for the first time, we can describe their synthesis from unlabeled, native ergotamine. Furthermore, this approach is promising as a universal way to synthesize other isotopically labeled EAs. KW - Reference Material KW - HPLC-MS/MS KW - Mycotoxins KW - Standards KW - Organic Synthesis KW - Isotope PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-600167 DO - https://doi.org/10.3390/toxins16040199 VL - 16 IS - 4 SP - 1 EP - 12 PB - MDPI AN - OPUS4-60016 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kislenko, Evgeniia A1 - Incel, A. A1 - Gawlitza, Kornelia A1 - Sellergren, B. A1 - Rurack, Knut T1 - Towards molecularly imprinted polymers that respond to and capture phosphorylated tyrosine epitopes using fluorescent bis-urea and bis-imidazolium receptors N2 - Early detection of cancer is essential for successful treatment and improvement in patient prognosis. Deregulation of post-translational modifications (PTMs) of proteins, especially phosphorylation, is present in many types of cancer. Therefore, the development of materials for the rapid sensing of low abundant phosphorylated peptides in biological samples can be of great therapeutic value. In this work, we have synthesised fluorescent molecularly imprinted polymers (fMIPs) for the detection of the phosphorylated tyrosine epitope of ZAP70, a cancer biomarker. The polymers were grafted as nanometer-thin shells from functionalised submicron-sized silica particles using a reversible addition-fragmentation chain-transfer (RAFT) polymerisation. Employing the combination of fluorescent urea and intrinsically cationic bis-imidazolium receptor cross-linkers, we have developed fluorescent sensory particles, showing an imprinting factor (IF) of 5.0. The imprinted polymer can successfully distinguish between phosphorylated and non-phosphorylated tripeptides, reaching lower micromolar sensitivity in organic solvents and specifically capture unprotected peptide complements in a neutral buffer. Additionally, we have shown the importance of assessing the influence of counterions present in the MIP system on the imprinting process and final material performance. The potential drawbacks of using epitopes with protective groups, which can co-imprint with targeted functionality, are also discussed. KW - Functional monomers KW - Molecularly imprinted polymers KW - Phosphorylated peptides KW - Fluorescence KW - Core-shell particles PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588089 DO - https://doi.org/10.1039/d3tb01474f SN - 2050-750X SP - 1 EP - 10 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-58808 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Kristin T1 - Die Berechnung von Unsicherheiten zertifizierter Werte von Referenzmaterialien und deren Nutzung zur Berechnung von Verfahrensmessunsicherheiten N2 - Die Angabe von Unsicherheiten bei zertifizierten Werten von Referenzmaterialien ist von entscheidender Bedeutung. Die korrekte Einbindung der Unsicherheiten zur Berechnung von Verfahrensmessunsicherheiten ist wesentlich für die Gewährleistung der Genauigkeit und Zuverlässigkeit von Messungen. In diesem Vortrag werden die verschiedenen Einflussfaktoren auf die Unsicherheit zertifizierter Werte gemäß ISO Guide 35 dargestellt. Dabei werden insbesondere die Charakterisierung, Homogenität und Stabilität als entscheidende Faktoren für die Bestimmung der Unsicherheit eines Referenzmaterials betrachtet. Abschließend wird das Konzept anhand eines konkreten Beispiels veranschaulicht, um die praktische Anwendung und die Auswirkungen auf die Berechnung von Verfahrensmessunsicherheiten zu verdeutlichen. T2 - 324. PTB-Seminar Berechnung der Messunsicherheit – Empfehlungen für die Praxis CY - Berlin, Germany DA - 22.05.2023 KW - Referenzmaterialien KW - Unsicherheit PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598418 UR - https://www.ptb.de/cms/fileadmin/internet/fachabteilungen/abteilung_8/8.4_mathematische_modellierung/324_PTB_Seminar/Vortraege/324-PTB-Seminar_Unsicherheiten_zertifizierter_Werte.pdf UR - https://www.ptb.de/cms/ptb/fachabteilungen/abt8/fb-84/ag-842/seminare/324-ptb-seminar-berechnung-der-messunsicherheit-empfehlungen-fuer-die-praxis.html AN - OPUS4-59841 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, V. A1 - Uhlemann, M. A1 - Richter, Silke A1 - Pfeifer, jens T1 - Calibration capacity of hot-pressed hydrogen standards for glow discharge optical emission and mass spectrometry N2 - Mixed copper and titanium hydride powder was hot-pressed and characterized by Carrier Gas Hot Extraction, XRay Diffraction, Thermal Gravimetric Analysis coupled with Mass Spectrometry, and Scanning Electron Microscopy. The hot-pressed and five conventional samples were applied for calibration of hydrogen in Glow Discharge Optical Emission and Mass Spectrometry. Up to the introduction of 15 ng/s hydrogen the Emission yield model is useful in Glow Discharge Optical Emission Spectrometry. A correlation between saturation and even reversal of the emission yield of the spectral lines H121, H486 and H656 and low sputtering rates was found. Hydrogen effects exist for the spectral lines of Cu(II) 219 and Ti(I) 399. In Glow Discharge Mass Spectrometry, a linear dependency of the 1H ion current on the sputtered mass per time exists over the total range of hydrogen content investigated. Hydrogen effects also exist for the sensitivity of 48Ti and 63Cu. The sputtering rate of two-phase materials depends linearly on the sputtered mass per time of one phase, which allows the sputtering rate of two-phase materials with known composition to be predicted. KW - Hot-pressing KW - GD-OES KW - GD-MS KW - Calibration KW - Hydrogen KW - Titanium hydride KW - Sputtering KW - Two-phase system PY - 2021 DO - https://doi.org/10.1016/j.sab.2020.106039 VL - 176 SP - 106039 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-52074 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej A1 - Kohlhoff, Harald A1 - Gawlitza, Kornelia A1 - Bell, Jérémy A1 - Mansurova, Maria A1 - Tiebe, Carlo A1 - Bartholmai, Matthias T1 - Semi-automatic Gas Measurement Device Based on Fluorescent Multi-gas Sensors N2 - This paper describes the development of a semi-automatic gas measurement device presenting potentially a broad range of applications, noteworthy in the agricultural sector. Non-reversible fluorescent molecular sensors were designed and syn-thesized. Upon, integration into a hydrogel matrix with an optimal ratio of co-solvents, the sensors reacting selectively to ammonia were illuminated by excitation light to produce a concentration-correlated fluorescence emission. An automated mechanical-elec-trical device initiates a given gas mixture and thus simulates con-centrations similar to a threshold value. The aim of this project is to develop a sensor or a low-cost method which can monitor low concentrations of harmful gases and aid in their elimination or regulation in livestock housing, barns or stables. T2 - IEEE Sensors 2019 CY - Montreal, Canada DA - 27.10.2019 KW - gas analysis KW - fluorescence KW - embedded sensor KW - spectroscopy KW - environment KW - agricultural economy PY - 2019 SN - 978-1-7281-1634-1 SP - 88 EP - 92 PB - IEEE AN - OPUS4-49506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Sommerfeld, Thomas A1 - Koch, Matthias A1 - Mauch, Tatjana A1 - Jung, Christian A1 - Riedel, Juliane A1 - Lisec, Jan T1 - CRM BAM-A001 eCerto data file N2 - Data file (RData) containing measurement data recorded during the production process of the Certified Reference Material BAM-A001 containing Polycyclic Aromatic Hydrocarbons (PAH) in olive oil. The data can be most conveniently openend using the Shiny-App eCerto which is accessible at https://www.bam.de/eCerto. KW - Certified reference material KW - Mass spectrometry KW - Olive oil KW - Aromatic hydrocarbons KW - Reference data PY - 2023 UR - https://doi.org/10.5281/zenodo.8380870 DO - https://doi.org/10.5281/zenodo.8380869 PB - Zenodo CY - Geneva AN - OPUS4-58488 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Carl, Peter A1 - Sarma, Dominik A1 - Gregório, Bruno J. R. A1 - Hoffmann, Kristin A1 - Lehmann, Andreas A1 - Rurack, Knut A1 - Schneider, Rudolf T1 - Wash-Free Multiplexed Mix-and-Read Suspension Array Fluorescence Immunoassay for Anthropogenic Markers in Wastewater N2 - Pharmaceuticals, certain food ingredients, and mammalian endogenous metabolic products in wastewater are mostly of human origin. They are anthropogenic markers. Proper knowledge of their levels in wastewater helps to track sources of pollutants in natural waters and allows for calculation of removal efficiencies in wastewater Treatment plants. Here, we describe the development and application of an indirect competitive, multiplexing suspension Array fluorescence immunoassay (SAFIA) for the detection of carbamazepine (CBZ), diclofenac (DCF), caffeine (CAF), and isolithocholic acid (ILA) in wastewater, covering those classes of anthropogenic markers. The assay consists of haptens covalently conjugated to fluorescence-encoded polystyrene core/silica shell microparticles to create a site for competitive binding of the antibodies (Abs). Bound Abs are then stained with fluorophore-labeled Abs. Encoding and signaling fluorescence of the particles are determined by an automated flow cytometer. For compatibility of the immunoassay with the 96-well microtiter plate format, a stop reagent, containing formaldehyde, is used. This enables a wash-free procedure while decreasing time-to-result. Detection limits of 140 ± 40 ng/L for CBZ, 180 ± 110 ng/L for CAF, 4 ± 3 ng/L for DCF, and 310 ± 70 ng/L for ILA are achieved, which meet the sensitivity criteria of wastewater analysis. We demonstrate the applicability of SAFIA to real wastewater samples from three different wastewater Treatment plants, finding the results in good agreement with LC-MS/MS. Moreover, the accuracy in general exceeded that from classical ELISAs. We therefore propose SAFIA as a quick and reliable approach for wastewater analysis meeting the requirements for process analytical technology. KW - Suspension Array KW - Immunoassay KW - Carbamazepine KW - Caffeine KW - Diclofenac KW - SAFIA PY - 2019 DO - https://doi.org/10.1021/acs.analchem.9b03040 SN - 0003-2700 VL - 91 IS - 20 SP - 12988 EP - 12966 PB - ACS Publications AN - OPUS4-49305 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gotor, Raúl A1 - Rurack, Knut A1 - Bell, Jérémy T1 - Fluorescent Paper Strips for the Detection of Diesel Adulteration with Smartphone Read-out N2 - Three fluorescent molecular rotors of 4-dimethylamino-4-nitrostilbene (4-DNS) were investigated for their potential use as viscosity probes to indicate the content of kerosene in diesel/kerosene blends, a wide-spread activity to adulterate fuel. In solvents with low viscosity, the dyes rapidly deactivate via a so-called twisted intramolecular charge transfer state, efficiently quenching the fluorescence. Measurements of diesel/kerosene blends revealed a good linear correlation between the decrease in fluorescence and the increase of the fraction of the less viscous kerosene in diesel/kerosene blends. Immobilization of the hydroxy derivative 4-DNS-OH in cellulose paper yielded test strips that preserve the fluorescent indicator's behavior. Combination of the strips with a reader based on a smartphone and a controlling app allowed to create a simple field test. The method can reliably detect the presence of kerosene in diesel from 7 to 100%, outperforming present standard methods for diesel adulteration. KW - Diesel KW - Kerosene KW - Adulteration KW - Fluorescent sensor KW - Smartphone KW - Test strips PY - 2018 UR - https://www.jove.com/video/58019 DO - https://doi.org/10.3791/58019 VL - 141 SP - e58019-1 EP - e58019-6 PB - MyJoVE Corporation CY - Cambridge, MA, USA AN - OPUS4-46567 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - From molecular and nanoscale chromophores with UV/VIS/NIR/SWIR luminescence to multi method characterization of surface coatings N2 - An overview of the research activities of division Biophotonics is presented covering examples for photophysical studies of different types of molecular and nanocrystalline luminophores, luminescent particles, and sensor systems in solution, in dispersion, and in the solid state and multi-method charactreization workflow for the characterization of surface-functionalized engineered nanomaterials. In addition, the importance of reliable optical measurements, particularly standardized workflows for the determination of the key performance parameter luminescence quantum yield of transparent and scattering luminescent samples with fluorescence and integrating sphere spectroscopy, and validated methods for quantifying surface functional groups and ligands on nanomaterials is highlighted. Thereby, also ongoing standardization activities are presented as well as certified reference materials and reference materials from division Biophotonics. T2 - Chinese-German Chemical Association - Annual Meeting CY - Berlin, Germany DA - 22.08.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Quantum yield KW - Characterization KW - Advanced material KW - Surface KW - Lifetime KW - Sensor KW - Oxygen KW - Ph KW - Standardization KW - Fluorescent probe KW - Reference material PY - 2025 AN - OPUS4-64181 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogl, Jochen A1 - Kipphardt, Heinrich A1 - Richter, Silke A1 - Bremser, Wolfram A1 - Arvizu Torres, M. A1 - Lara Manzano, J. A1 - Buzoianu, M. A1 - Hill, S. A1 - Petrov, P. A1 - Goenaga-Infante, H. A1 - Sargent, M. A1 - Fisicaro, P. A1 - Labarraque, G. A1 - Zhou, T. A1 - Turk, G. C. A1 - Winchester, M. A1 - Miura, T. A1 - Methven, B. A1 - Sturgeon, R. A1 - Jährling, R. A1 - Rienitz, O. A1 - Mariassy, M. A1 - Hankova, Z. A1 - Sobina, E. A1 - Krylov, A. I. A1 - Kustikov, Y. A. A1 - Smirnov, V. V. T1 - Establishing comparability and compatibility in the purity assessment of high purity zinc as demonstrated by the CCQM-P149 intercomparison N2 - For the first time, an international comparison was conducted on the determination of the purity of a high purity element. Participants were free to choose any analytical approach appropriate for their institute’s applications and services. The material tested was a high purity zinc, which had earlier been assessed for homogeneity and previously used in CCQM-K72 for the determination of six defined metallic impurities. Either a direct metal assay of the Zn mass fraction was undertaken by EDTA titrimetry, or an indirect approach was used wherein all impurities, or at least the major ones, were determined and their sum subtracted from ideal purity of 100 %, or 1 kg/kg. Impurity assessment techniques included glow discharge mass spectrometry, inductively coupled plasma mass spectrometry and carrier gas hot extraction/combustion analysis. Up to 91 elemental impurities covering metals, non-metals and semi-metals/metalloids were quantified. Due to the lack of internal experience or experimental capabilities, some participants contracted external laboratories for specific analytical tasks, mainly for the analysis of non-metals. The reported purity, expressed as zinc mass fraction in the high purity zinc material, showed excellent agreement for all participants, with a relative standard deviation of 0.011 %. The calculated reference value, w(Zn) = 0.999 873 kg/kg, was assigned an asymmetric combined uncertainty of + 0.000025 kg/kg and – 0.000028 kg/kg. Comparability amongst participating metrology institutes is thus demonstrated for the purity determination of high purity metals which have no particular difficulties with their decomposition / dissolution process when solution-based analytical methods are used, or which do not have specific difficulties when direct analysis approaches are used. Nevertheless, further development is required in terms of uncertainty assessment, quantification of non-metals and the determination of purity of less pure elements and/or for those elements suffering difficulties with the decomposition process. KW - Purity assessment KW - Direct metal assay KW - Impurity assessment KW - Non-metal analysis KW - High-purity elements KW - SI-traceability PY - 2018 DO - https://doi.org/10.1088/1681-7575/aaa677 SN - 1681-7575 SN - 0026-1394 VL - 55 IS - 2 SP - 211 EP - 221 PB - Institute of Physics Publishing CY - Bristol AN - OPUS4-44257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maher, C. A1 - Schazmann, B. A1 - Gornushkin, Igor B. A1 - Rurack, Knut A1 - Gojani, Ardian T1 - Exploring an Application of Principal Component Analysis to LaserInduced Breakdown Spectroscopy of Stainless-Steel Standard Samples as a Research Project N2 - Laser-induced breakdown spectroscopy (LIBS) and principal component analysis (PCA) are frequently used for analytical purposes in research and industry, but they seldom are part of the chemistry Curriculum or laboratory exercises. This case study paper describes the combined application of LIBS and PCA during a research internship for an undergraduate student. The instructional method applied was based on a one-on-one mentorship, in which case the learner was engaged in a Research work. The learning activities included theoretical introductions to the LIBS and PCA methods, numerical simulation, experiments, and data analysis. The study covered three main topics: analysis of LIBS spectra, application of PCA for clustering, and use of PCA for experimental design. The realization of the study was instructive for all parties involved: from the mentorship point of view, it is concluded that the topics can be covered during an internship or developed into a one semester long research-based module of a chemistry program or a final year project. The student, on the other hand, developed profound technical skills in performing experiments and using PCA software for data analysis. KW - LIBS KW - PCA PY - 2021 DO - https://doi.org/10.1021/acs.jchemed.1c00563 VL - 98 SP - 3237 EP - 3244 PB - American Chemical Society Publications CY - USA AN - OPUS4-53515 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter T1 - Progressing Towards Rapid Multiplex Detection: A Fluorescence Immunoassay for Ergot Alkaloids, Trichothecenes, and Fusarium Toxins N2 - Ergot alkaloids, potent mycotoxins produced by Claviceps spp., particularly Claviceps purpurea, pose significant health risks when they contaminate rye and related cereals, leading to ergotism in humans and mammals [1]. In response, the European Union has established Regulation 2023/915, setting maximum residue levels for the sum of 12 principal ergot alkaloids and other mycotoxins including fumonisins (FUM), deoxynivalenol (DON), zearalenone (ZEN), and T2/HT2 toxins in food products. Given the prevalent co-occurrence of mycotoxins, their simultaneous detection is crucial for ensuring the safety of food and feed [2, 3]. Traditionally, chromatographic techniques such as liquid chromatography coupled with (tandem) mass spectrometry (LC-MS/MS) have been employed for multiplex detection of mycotoxins [4, 5]. While effective, these methods require specialized facilities, expensive equipment, and skilled personnel. Immunoassays like ELISA and lateral flow assays offer a more accessible alternative for rapid mycotoxin detection, yet they generally lack the capability for concurrent multi-toxin screening. This study introduces the SAFIA (Suspension Array Fluorescence Immunoassay), a particle-based immunoassay utilizing fluorescence-encoded microparticles for the simultaneous detection of multiple analytes [6, 7]. The assay's innovative advancement comes with the inclusion of ergot alkaloids, a novel addition to its existing detection capabilities for fusarium toxins and trichothecenes, thereby expanding its scope to a broader range of mycotoxins. The assay employs antibodies targeting the ergoline moiety common to all major ergot alkaloids, facilitated by a synthesized hapten mimicking the ergoline structure. This hapten was conjugated to amino-functionalized beads, and a panel of five monoclonal antibodies was evaluated for hapten recognition, binding specificity, and competitive binding efficiency. Our findings demonstrate that all antibodies displayed similar affinities towards the hapten and lysergol (a stable and less hazardous analogue of lysergic acid used for calibration), achieving detection limits as low as 2 ppb. Cross-reactivity studies and analysis of round-robin test material indicated a significant underestimation of ergot alkaloid levels in samples. However, accurate detection of ergot alkaloids remains feasible through the application of a correction factor to the results, which compensates for this underestimation and ensures the assay's effectiveness. Despite this adjustment, the necessity for enhancements in antibody specificity to improve assay accuracy is evident. Furthermore, the inclusion of the ergot assay in a multiplexed setup for detecting FUM, DON, ZEN, and T-2 toxins showed no interference, although an unexpected inhibition among four out of five ergot antibodies was observed. This underscores the need for an improved immunogen structure to achieve optimal detection of ergot alkaloids. In conclusion, our study presents a promising approach for the multiplexed detection of ergot alkaloids alongside other mycotoxins, highlighting the potential of SAFIA in enhancing food and feed safety through improved mycotoxin screening. Future work will focus on refining antibody specificity and assay configurations to overcome current limitations and ensure accurate, comprehensive mycotoxin detection. T2 - Mycotoxin-Workshop CY - Vienna, Austria DA - 02.06.2024 KW - Mycotoxins KW - LC-MS/MS KW - Quality assurance KW - Food safety PY - 2024 AN - OPUS4-61065 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bell, Jérémy T1 - Microfluidic platform and fluorescent sensor particles for the detection of the herbicide 2,4-D in worldwide samples N2 - Fluorescent sensory MIP (molecularly imprinted polymer) particles were combined with a droplet-based 3D microfluidic system for the sensitive and selective determination of 2,4-dichlorophenoxyacetic acid (2,4-D) in water samples. 2,4-D being an important and widely used herbicide to regulate plant growth, its extensive use leads to food or ground water contamination. Analytical assays based on MIP have emerged as a valuable tool in the field of environmental analysis thanks to low production costs, stability, format adaptability and their ability to recognize a wide variety of targets, such as the critical neutral organic molecules present in water: herbicides, pesticides, antibiotics, etc. To accomplish this, a tailor-made fluorescent indicator cross-linker was designed that translates directly the binding event into an enhanced fluorescence signal. This phenoxazinone-type cross-linker was co-polymerized into a thin MIP layer grafted from the surface of silica microparticles. The latter was achieved by integration of the fluorescent core-shell MIP sensor particles into a modular microfluidic platform that allows for an in-line phase-transfer assay, extracting the analyte from aqueous sample droplets into organic phase droplets that contain the sensor particles. This tool offering a novel simple and rapid way for the detection of herbicides, real-time fluorescence determination of 2,4-D down to 20 nM was realized with the system and applied for the analysis of worlwide surface water samples. T2 - INTERNATIONAL CONFERENCE ON CHEMISTRY AND THE ENVIRONMENT - ICCE 2017 CY - Oslo, Norway DA - 18.06.2017 KW - Microfluidics KW - MIP KW - Fluorescence KW - Pesticide PY - 2017 AN - OPUS4-42454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf A1 - Konthur, Zoltán A1 - Jaeger, Carsten T1 - Reference Material (IgG) for CCQM-PAWG Key Comparison N2 - BAM proposes a recombinant human IgG (anti-tetanus monoclonal antibody SA13) as candidate material for the 2027 CCQM-PAWG key comparison on antibody purity. The antibody is produced via hybridoma and recombinant expression systems, with detailed sequence and glycosylation profiling. Analytical methods include MALDI-TOF-MS, SEC, DLS, and UV-vis spectroscopy to assess purity, aggregation, and stability. Preliminary results show high purity, low heterogeneity, and consistent size distribution. A minimum of 40 mg IgG is required, with 100 mg preferred for deeper characterization. Production is expected to be completed by the end of 2026, with potential for a joint technical project. T2 - Spring Meeting of CCQM-PAWG CY - Sèvres, France DA - 06.04.2025 KW - Antibodies KW - Research Grade Test Material KW - Mass spectrometry KW - Affinity PY - 2025 AN - OPUS4-63503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Getting it right with photoluminescence quantum yields of molecular and nanoscale luminophores and luminescent particles N2 - Photophysical and mechanistic studies, the comparison of different emitter classes, and the rational design of the next generation of molecular and nanoscale reporters require quantitative photoluminescence measurements and the reliable determination of the key performance parameter photoluminescence quantum yield (QY), i.e., the number of emitted per absorbed photons. This is of special importance for all photoluminescence applications in the life and material sciences in the UV/vis/NIR/SWIR. To improve the reliability and comparability of photoluminescence and QY measurements across laboratories, pitfalls, achievable uncertainties, and material-specific effects related to certain emitter classes must be explored. Also, suitable protocols and reference materials are needed which have been validated in interlaboratory comparisons for different wavelength regions and transparent and scattering luminophores.[1] Based on absolute and relative photoluminescence measurements of functional dyes and nanomaterials like semiconductor quantum dots and rods, spectrally shifting lanthanide upconversion nanocrystals, perovskites, and YAG:Cer converter materials, reliable methods for determining QY of transparent and scattering luminophores, nonlinear emitters, and solid luminescent nanomaterials have been developed.[2,3] Thereby, material- and method-related uncertainties of relative and absolute QY measurements and achievable uncertainties could be quantified for linear and nonlinear UV/vis/NIR/SWIR emitters and lately for also luminescent and scattering materials and solid phoshors, here in an interlaboratory comparison of three labs utilizing integrating sphere spectroscopy.[4,5] In addition, to provide simple tools for a better comparability of QY measurements, recently, a first set of UV/vis/NIR quantum yield standards has been developed and certified with complete uncertainty budgets.[6] In the following, the outcome of these studies will be presented, thereby addressing common pitfalls and providing recommendations on the performance of reliable QY measurements of linear and non-linear emitters in transparent, scattering, and solid samples. T2 - 29th Lecture Conference on Photochemistry (LCP 2024) GDCh CY - Mainz, Germany DA - 16.09.2024 KW - Nanoparticle KW - Nano KW - Luminescence KW - Quality assurance KW - Synthesis KW - Standardization KW - Reference material KW - Quantum yield KW - Fluorescence KW - Reference data KW - Integrating sphere spectroscopy KW - ILC KW - Converter material KW - YAG:Ce KW - Optoceramic PY - 2024 AN - OPUS4-61075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Herter, Sven-Oliver T1 - Synthesis and application of stable isotopically labeled ergot alkaloids N2 - Ergot alkaloids form a toxicologically relevant group of mold toxins (mycotoxins) that are among the most common contaminants of food and animal feed worldwide. Therefore, reliable controls are indispensable for the minimization of both health risks and economic damages. As a consequence of their toxicological significance, EU limit values for 12 priority ergot alkaloids were established for the first time in 2022. These limits range from 500 µg/kg in rye milling products down to 20 µg/kg in processed cereal-based foods for infants and young children. Despite the use of high-performance liquid chromatography-mass spectrometry to quantify low concentrations of ergots in food, the current European standard procedure EN 17425:2021 cannot be fully applied due to the lack of isotopically labeled reference standards. The complex structure of the ergot alkaloids makes a total synthesis extremely challenging, expensive, and time-consuming. Consequently, we focused on a semi-synthetic approach with the aim of specifically demethylating the N6-atom of the lysergic acid moiety, a shared structural feature among all ergot alkaloids. This resulted in the formation of a norergot alkaloid, which was purified using preparative HPLC. The reaction of the norergot alkaloid with an isotopically labeled electrophilic methyl source, such as iodomethane or dimethyl sulfate, yielded the desired isotopically labeled ergot alkaloid. This methodology enabled the successful synthesis of all 12 stable isotopically labeled priority ergot alkaloids for the first time. Herein we present the problem of the current unavailability of these isotopically labeled standards and our approach to solve this urged demand. Moreover, we are able to present initial data on how these standards enhance the European standard procedure, EN 17425:2021. T2 - 11th International Symposium on RECENT ADVANCES IN FOOD ANALYSIS CY - Prague, Czech Republic DA - 05.11.2024 KW - Reference Material KW - HPLC-MS/MS KW - Mycotoxins KW - Ergot Alkaloids KW - Isotopic Labeling PY - 2024 AN - OPUS4-61690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gojani, Ardian T1 - Toward Determination of the Surface Roughness of Particles from a SEM Image N2 - Welcome to the poster Towards Determination of Surface Roughness from a SEM Image, a contribution from BAM in Berlin, Germany. This work is part of the MamaLoCA project, which aims to develop a biosensor for the detection of mycotoxins in cereals. Biosensors come in a great variety, one of which makes use of microscopic beads produced by homogenous coating of polystyrene microspheres. The beads are functionalized by decorating them with bioreceptors – in our case antibodies – which then specifically react with the analyte – in our case mycotoxins – and emit an electrical or optical signal. The functionalization of the beads depends on the surface roughness because this determines the amount and orientation of binders. In other words, the surface roughness affects the accessibility to the binding sites and influences device sensitivity, hence its quantitative determination is an important step in evaluating the quality of the biosensor in general. The presented solution to the problem of the estimation of surface roughness relies in the repetitive characteristics on the surface of the beads. A SEM image of the bead shows a raspberry like microparticle with a variation of grayscale values, which arise from the secondary electron yield. The principle of the measurement measures the variation of grayscale values along a circumference of a circle centred in the centre of the particle and with an arbitrary radius. The grayscale value variation along the given circumference gives the so-called z-modulation or the lateral profile. By performing Fast Fourier Transform on this profile we obtain the power spectrum as a function of the spatial frequencies through which the grayscales vary. The maximal value for spatial frequency then reveals the most common feature along one given circumference. Surface roughness then is the feature frequency in the spatial domain. This calculation is repeated for several concentric circles with different radii over the particle. The results for the same particle but recorded at two different accelerating voltages show that the applied method has a potential to reveal the roughness. Interpretation of results from an SE InLens SEM image obtained using 3 kV shows that surface roughness is about 21 nm, which is in a good agreement with an alternative method given in a different presentation. The results from the 10 kV are underestimated due to the loss of surface sensitivity on the SE InLens detection at high voltages. In conclusion, this method shows promise in determining quantitatively the surface roughness from a single SEM image and its validation is being sought using 3D SEM images and AFM methods. T2 - Microscopy and Microanalysis 2021 CY - Online Meeting DA - 01.08.2021 KW - MamaLoCA KW - Core-shell particles KW - Electron microscopy KW - Image processing KW - Particle characterisation KW - Roughness KW - Fast Fourier Transform PY - 2021 AN - OPUS4-53089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Herter, Sven-Oliver T1 - Semi-synthesis of isotopic labeled ergot alkaloids: New reference standards N2 - We developed a two-step semi-synthesis for the preparation of isotopically labeled EAs, starting from native EAs. This universal strategy enabled the successful synthesis of all isotopically labeled priority EAs. The structure of the isotopically labeled EAs was confirmed by HPLC-HR-MS/MS using native, unlabeled EAs as a reference standard. The next step will be the implementation of the isotopically labeled standards in the European standard procedure EN 17425 to improve the quantification of EAs in foodstuffs. T2 - 45th Mycotoxin Workshop CY - Vienna, Austria DA - 02.06.2024 KW - Reference Material KW - HPLC-MS/MS KW - Mycotoxins KW - Isotop standards KW - Organic Synthesis KW - Ergot alkaloids PY - 2024 AN - OPUS4-60239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Theiner, S. A1 - Corte Rodriguez, M. A1 - Traub, Heike ED - Golloch, A. T1 - Novel applications of lanthanoids as analytical or diagnostic tools in the life sciences by ICP-MS based techniques N2 - Inductively coupled plasma-mass spectrometry (ICP-MS) is a well-established analytical method offering high sensitivity and multi-element analysis. ICP-MS has found acceptance in various application areas ranging from material analysis to applications in the life sciences. Within the last 15 years new strategies for the sensitive detection and accurate quantification of biomolecules in complex biomedical samples have been developed. Recent instrumental improvements have contributed to this progress. As most of the biomolecules do not contain endogenous metals etectable with ICP-MS, bioconjugation with artificial metal-containing tags based on metal-loaded chelate complexes or nanoparticles is increasingly applied to determine biomolecules indirectly. Especially, the combination of immunohistochemical workflows using lanthanoid-tagged antibodies and ICP-MS detection provides new insights in the complexity and interdependency of cellular processes. Single-cell ICP-MS, also termed as mass cytometry, allows high-dimensional analysis of biomarkers in cell populations at single-cell resolution. For that purpose, lanthanoid isotope labelled antibodies are used to detect their corresponding target molecules. The visualisation of the elemental distribution is possible with laser ablation ICP-MS (LA-ICPMS) at high spatial resolution. Especially, the combination of LA with ICP time-of-flight mass spectrometry, also referred to as imaging mass cytometry (IMC), opens new possibilities for multiparametric tissue imaging at the single-cell level and even below. The lanthanoid localisation and concentration can be linked to their conjugated antibody target providing valuable information about surface markers, intracellular signalling molecules to measure biological function, and the network state of an individual cell in a tissue. This book chapter focuses on new applications, where the multi-element capabilities of ICP-MS are used for the detection of lanthanoids applied as artificial elemental stains or tags for biomolecules and in particular antibodies. KW - ICP-MS KW - Laser ablation KW - Cell KW - Antibody KW - Immunohistochemistry KW - Lanthanoid KW - Mass cytometry KW - Imaging PY - 2022 SN - 978-3-11069-645-5 SN - 978-3-11069-636-3 DO - https://doi.org/10.1515/9783110696455-013 SP - 399 EP - 444 PB - De Gruyter CY - Berlin, Boston ET - 2. rev. and exten. edition AN - OPUS4-55118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - Quantification of surface functional groups on inorganic and organic nanomaterials using cleavable reporters N2 - Engineered nanomaterials (NM) with their unique size-dependent properties are of increasing relevance for current and future developments in various fields such as medical and pharmaceutical industry, computing and electronics or food and consumer products. The performance and safety of NM are determined by the sum of their intrinsic physicochemical properties. Especially, the particle surface chemistry, which is largely controlled by the chemical nature and density of functional groups and ligands, is an important key driver for the performance, stability, and processibility of NM, as well as their interaction with the environment. Thus, methods for functional group quantification can foster the sustainable development of functional and safe(r) NM. Aiming at the development of simple, versatile and multimodal tools for the quantification of common bioanalytically relevant functional groups, we designed a catch-and-release assay based on cleavable probes that enable the quantification of the cleaved-off reporters in the supernatant after particle separation. Thus, the approach circumvents interferences resulting from particle light scattering and sample-inherent absorption or emission. To study the potential of the assay, commercially available and in-house synthesized aminated and carboxylated polymer and silica nanoparticles of different functional group densities were tested. Our cleavable probe strategy can be easily adapted to other analytical techniques requiring different reporters, or to different types of linkers that can be cleaved thermally, photochemically, or by variation of pH, utilizing well-established chemistry. In addition, it can contribute to the development of multi-method characterization strategies to provide a more detailed picture of the intrinsic physicochemical property - performance/safety relationships and thus can support the design of tailored nanomaterials with better controlled properties. T2 - E-MRS Spring Meeting 2021 / ALTECH 2021 - Analytical techniques for precise characterization of nanomaterials CY - Online meeting DA - 31.05.2021 KW - Surface modified nano- and microparticles KW - Optical assays KW - Particle surface analysis KW - Surface functional group quantification PY - 2021 AN - OPUS4-55596 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Srivastava, Priyanka T1 - Multi-color nanosensors for ratiometric measurements of acidic, neutral, and basic pH based on silica and polystyrene particles N2 - pH presents one of the most important analytes in the life and material sciences, indicating, e.g., diseases and corrosion processes. This includes the optical monitoring of pH in living cells for studying cellular internalization pathways, such as phagocytosis, endocytosis, and receptor mediated internalization with the aid of molecular and nanoscale fluorescent sensors. Nanoparticle (NP)-based sensors, that are labelled or stained with a multitude of sensor dyes, have several advantages as compared to conventional molecular probes like enhanced brightness, i.e., amplified signals, ease of designing ratiometric systems by combining analyte-sensitive and inert reference dyes, and increased photostability. Moreover, this can enable the use of hydrophobic dyes in aqueous environments. Versatile templates and carriers for the fabrication of nanosensors by staining and/or labelling with different fluorophores and sensor molecules are surface-functionalized particles like silica (SiO2) and polystyrene (PS) particles. Here we present a platform of blue-red-green fluorescent pH nanosensors for the measurement of acidic, neutral, and basic pH utilizing both types of matrices and two spectrally distinguishable sensor dyes with an integrated reference dye and demonstrate its applicability for cellular studies. T2 - E-MRS Spring Meeting 2022 CY - Online meeting DA - 30.05.2022 KW - Nanosensors KW - pH sensing KW - Silica- and polystyrene particles KW - Ratiometric sensors KW - Fluorescence PY - 2022 AN - OPUS4-55597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, M. A1 - Zhang, T. A1 - Wang, J. A1 - Cheng, Z. A1 - Liu, Y. A1 - Qiao, X. A1 - Wen, J. A1 - Resch-Genger, Ute A1 - Long, W. A1 - Ou, J. T1 - NaYF4:Yb3+/Tm3+@NaYF4:Yb3+ Upconversion Nanoparticles for Optical Temperature Monitoring and Self-Heating in Photothermal Therapy N2 - The core−shell NaYF4:Yb3+/Tm3+@NaYF4:Yb3+ upconversion nanoparticles were successfully prepared by a solvothermal method, and a layer of mesoporous silica (mSiO2) was successfully coated on the periphery of the core−shell nanoparticles to transform their surface from lipophilic to hydrophilic, further expanding their applications in biological tissues. The physical phase, morphology, structure, and fluorescence properties were characterized by X-ray diffraction (XRD), field emission transmission electron microscopy (TEM), Fourier infrared spectroscopy (FT-IR), ζ potential analysis, and fluorescence spectroscopy. It was found that the material has a hexagonal structure with good hydrophilicity and emits intense fluorescence under 980 nm pump laser excitation. The non-contact temperature sensing performance of nanoparticles was evaluated by analyzing the upconversion fluorescence of Tm3+ (1G4 → 3F4 and 3F3 → 3H6) in the temperature range of 284−344 K. The absolute and relative sensitivities were found to be 0.0067 K−1 and 1.08 % K−1, respectively, with high-temperature measurement reliability and good temperature cycling performance. More importantly, its temperature measurement in phosphate-buffered saline (PBS) solution is accurate. In addition, the temperature of the cells can be increased by adjusting the laser power density and laser irradiation time. Therefore, an optical temperature sensing platform was built to realize the application of real-time monitoring of cancer cell temperature and the dual function of photothermal therapy. KW - Sensor KW - Temperature KW - Lanthanide KW - Tag KW - Fluorescence KW - Nanoparticles KW - Synthesis KW - Environment KW - Monitoring KW - Sensing KW - Nano KW - Life sciences KW - Upconversion PY - 2023 DO - https://doi.org/10.1021/acsanm.2c05110 VL - 6 IS - 1 SP - 759 EP - 771 PB - ACS Publications AN - OPUS4-57081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Azari, H. A1 - Shams, S. A1 - Köpp, Christian A1 - Timofeev, Juri A1 - Niederleithinger, Ernst T1 - Development of reference specimens for nondestructive evaluation of concrete bridge decks N2 - Decades of non-destructive evaluation (NDE) for the quality assurance of concrete bridges revealed the necessity of developing procedures for building reference specimens for different defects. External objects have been widely used in specimen construction to represent defects. However, embedded materials can alter the actual defect characteristics, interrupting the NDE responses. This study proposes new approaches to fabricating reference specimens for reinforced concrete that feature substantial defects, including cracks, delamination, honeycombing and rebar corrosion, without external objects. As a result, realistic responses can be acquired to identify promising NDE methods for characterising actual deteriorations. The procedures were produced with the intent of being reproducible in any laboratory. Destructive and non-destructive testing methods were performed to verify the effectiveness of the processes in creating defects. This study provides research laboratories with techniques for fabricating reference specimens for characterising defects and assessing the performance of NDE technologies. KW - Concrete structures KW - Reference KW - Specimen KW - Non-destructive testing KW - Laboratory tests PY - 2023 DO - https://doi.org/10.1680/jfoen.21.00030 SN - 2043-9911 SP - 1 EP - 12 PB - ICE Publishing AN - OPUS4-56957 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Functional Luminophores – From Photophysics to Standardized Luminescence Measurements N2 - Inorganic nanocrystals with linear and nonlinear luminescence in the ultraviolet, visible, near infrared and short-wave infrared like semiconductor quantum dots and spectrally shifting lanthanide-based nanophosphors have meanwhile found applications in the life and material sciences ranging from optical reporters for bioimaging and sensing over security barcodes to solid state lighting and photovoltaics. These nanomaterials commonly have increasingly sophisticated core/shell particle architectures with shells of different chemical composition and thickness to minimize radiationless deactivation at the particle surface that is usually the main energy loss mechanism [1]. For lanthanide-based spectral shifters, particularly for very small nanoparticles, also surface coatings are needed which protect near-surface lanthanide ions from luminescence quenching by high energy vibrators like O-H groups and prevent the disintegration of these nanoparticles under high dilution conditions. [2,3,4]. The identification of optimum particle structures requires quantitative spectroscopic studies focusing on the key performance parameter photoluminescence quantum yield [5,6], ideally flanked by single particle studies to assess spectroscopic inhomogeneities on a particle-to-particle level for typical preparation methods [7,8], Moreover, in the case of upconversion nanoparticles with a multi-photonic and hence, excitation power density (P)-dependent luminescence, quantitative luminescence studies over a broad P range are required to identify particle architectures that are best suited for applications in fluorescence assays up to fluorescence microscopy. Here, we present methods to quantify the photoluminescence of these different types of emitters in the vis/NIR/SWIR and as function of P and demonstrate the importance of such measurements for a profound mechanistic understanding of the nonradiative deactivation pathways in semiconductor and upconversion nanocrystals of different size and particle architecture in different environments. T2 - Eingeladener Vortrag Uni Erlangen CY - Erlangen, Germany DA - 18.01.2023 KW - Semiconductor quantum dot KW - Upconversion nanocrystal KW - Luminescence KW - Quantitative spectroscopy KW - Photophysics KW - Quality assurance KW - Nano KW - Particle KW - Quantum yield KW - Lifetime KW - Standard KW - Reference material KW - Surface analysis KW - Quantification PY - 2023 AN - OPUS4-57011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mrkwitschka, Paul T1 - The Role of Electron Microscopy in the Development of Monodisperse Cubic Iron Oxide Nanoparticles as CRM for Size and Shape N2 - Due to their unique physico-chemical properties, nanoparticles are well established in research and industrial applications. A reliable characterization of their size, shape, and size distribution is not only mandatory to fully understand and exploit their potential and develop reproducible syntheses, but also to manage environmental and health risks related to their exposure and for regulatory requirements. To validate and standardize methods for the accurate and reliable particle size determination nanoscale reference materials (nanoRMs) are necessary. However, there is only a very small number of nanoRMs for particle size offered by key distributors such as the National Institute of Standards and Technology (NIST) and the Joint Research Centre (JRC) and, moreover, few provide certified values. In addition, these materials are currently restricted to polymers, silica, titanium dioxide, gold and silver, which have a spherical shape except for titania nanorods. To expand this list with other relevant nanomaterials of different shapes and elemental composition, that can be used for more than one sizing technique, we are currently building up a platform of novel nanoRMs relying on iron oxide nanoparticles of different shape, size and surface chemistry. Iron oxide was chosen as a core material because of its relevance for the material and life sciences. T2 - Microscopy and Microanalysis 2022 CY - Online meeting DA - 31.07.2022 KW - Certified Referencematerial KW - Cubical Iron Oxide KW - Nanoparticles KW - Electron Microscopy KW - Small-Angle X-ray Scattering PY - 2022 AN - OPUS4-57035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Design, characterization, and application of fluorescent sensor particles N2 - pH and oxygen are amongst the most important and frequently measured analytes in the life and material sciences, indicating, e.g., diseases and corrosion processes. This includes the optical monitoring of pH in living cells for studying cellular internalization pathways, such as phagocytosis, endocytosis, and receptor ligand internalization with the aid of molecular and nanoscale fluorescent sensors. Nanoparticle (NP)-based sensors, that are labeled or stained with a multitude of sensor dyes, have several advantages as compare to conventional molecular probes like enhanced brightness, i.e., amplified signals, ease of designing ratiometric systems by combining analyte sensitive and inert reference dyes, and increased photostability. Moreover, this can enable the use of hydrophobic dyes in aqueous environments. Versatile templates and carriers for the fabrication of nanosensors by the staining and/or labelling with different fluorophores and sensor molecules or surface functionalized NP like silica (SiO2-NP) and polystyrene (PS-NP) particles provide. Here we present the design of a versatile platform of color emissive nanosensors and stimuli-responsive microparticles for the measurement of pH, oxygen, and other targets utilizing both types of matrices and sets of spectrally distinguishable sensor and reference dyes and their characterization and demonstrate the applicability of representative sensor particle for cellular studies. T2 - Vortrag bei dem Projekttreffen MicraGen CY - Copenhagen, Denmark DA - 18.08.2022 KW - Dye KW - Luminescence KW - Quantitative spectroscopy KW - Photophysics KW - Quality assurance KW - Nano KW - Particle KW - Quantum yield KW - Lifetime KW - Standard KW - Integrating sphere spectroscopy KW - Sensor KW - pH KW - Oxygen KW - Microfluidics KW - Cancer KW - Cell KW - Life sciences PY - 2022 AN - OPUS4-57049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Nuclear concrete, and how to live with it more easy using NDE N2 - This keynote presentation compiles the specialities of civil engineering compared to other disciplines, of NDT in civil engineering compared to other filds of NDT and the specific challenges of applications in the nuclear energy and disposal sector. T2 - NucCon 2023 CY - Espoo, Finland DA - 25.01.2023 KW - NDT KW - Concrete KW - Nuclear PY - 2023 AN - OPUS4-56912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Silke T1 - Plasmaspectrochemistry in material sciences N2 - Plasmas as atomization and ionization/excitation sources have been used for more than 50 years. The term plasma spectrochemistry was introduced in the 1980s and is nowadays a topic of annual reviews and different conferences such as the Winter Conference on Plasma Spectrochemistry (held in USA), the European Winter Conference on Plasma Spectrochemistry, and The Nordic conference on Plasma Spectrochemistry. The development of advanced materials is inherently connected with improvements in analytical chemistry, and often is the driving force for method development in plasma-based spectrometry. Besides the determination of physical characteristics such as tensile strength, density, and conductivity, the investigation of their chemical constituents down to the trace and ultra-trace levels becomes more and more important and, therefore, the demand of sensitive and precise analytical methods is growing. In some cases, the determination of the average content is a sufficient result, for instance for the characterisation of raw material or waste management. However, lately laterally resolved analysis, depth profiling of layered materials and characterization of high purity materials are of growing importance. The aim of this article is to give an introduction into plasma spectrometry and its application in materials science. A theoretical overview of the used plasma techniques and a review on applications with a special focus on direct solid sampling will be presented. KW - Material Science KW - Plasma KW - Plasmaspectrochemistry PY - 2019 DO - https://doi.org/10.1002/9780470027318.a9341.pub2 SP - 1 PB - John Wiley & Sons CY - Hoboken, New Jersey AN - OPUS4-47840 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gonzales-Gago, C. A1 - Smid, P. A1 - Hofmann, T. A1 - Venzago, C. A1 - Hoffmann, V. A1 - Gruner, W. A1 - Pfeifer, Jens A1 - Richter, Silke A1 - Kipphardt, Heinrich T1 - Investigations of matrix independent calibration approaches in fast flow glow discharge mass spectrometry N2 - The performance of glow discharge mass spectrometry (GD-MS) is investigated for the accurate quantification of metallic impurities and oxygen in solid samples using the fast flow source GD-MS instrument ELEMENT GD. Different quantification approaches based on relative and absolute sensitivity factors are evaluated for the determination of metallic impurities using three sample matrixes (Al, Cu and Zn). The effect of the discharge conditions (voltage, current, discharge gas pressure/flow) on the sensitivity is investigated and the parameters are optimized to favour matrix independent calibrations. Improved standard relative sensitivity factors (StdRSFs) are calculated under optimal conditions based on multi-matrix calibrations. The sputtering rate corrected calibration is also presented as a multi-matrix calibration approach. The capabilities of GD-MS for oxygen determination are also investigated using a set of new conductive samples containing oxygen with mass fractions in the percent range in three different matrices (Al, Mg and Cu) produced by a sintering process. Poor limits of detection (in the order of g/kg) were obtained as consequence of the reduced sensitivity of oxygen in GD-MS and high oxygen background signal intensity as well as its variations. The absolute sensitivity procedure is shown as a matrix-independent approach, which provides quantitative values consistent with those obtained by carrier gas hot extraction (CGHE). KW - Fast flow GD KW - GDMS KW - Calibration KW - Matrix independent calibration PY - 2019 DO - https://doi.org/10.1039/c9ja00023b SN - 1364-5544 SN - 0267-9477 VL - 34 IS - 6 SP - 1109 EP - 1125 PB - Royal Society of Chemistry CY - London AN - OPUS4-47842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Köppen, Robert A1 - Kroh, L.W. A1 - Lörchner, Dominique T1 - 1,3,5-Tris-(2,3-dibromopropyl)-1,3,5-triazine-2,4,6-trione: kinetic studies and phototransformation products N2 - 1,3,5-Tris-(2,3-dibromopropyl)-1,3,5-triazine-2,4,6-trione (TDBP-TAZTO) is an emerging brominated flame retardant which is widely used in several plastic materials (electric and electronic equipment, musical instruments, automotive components). However, until today, no photochemical studies as well as the identification of possible phototransformation products (PTPs) were described in literature. Therefore, in this study, UV-(C) and simulated sunlight irradiation experiments were performed to investigate the photolytic degradation of TDBP-TAZTO and to identify relevant PTPs for the first time. The UV-(C) Irradiation experiments show that the photolysis reaction follows a first-order kinetic model. Based on this, the photolysis rate constant k as well as the half-life time t1/2 were calculated to be k = (41 ± 5 ×10−3) min−1 and t1/2=(17±2) min. In comparison, a minor degradation of TDBP-TAZTO and no formed phototransformation products were obtained under simulated sunlight. In order to clarify the photochemical behavior, different chemicals were added to investigate the influence on indirect photolysis: (i) H2O2 for generation of hydroxyl radicals and (ii) two quenchers (2-propanol, sodium azide) for scavenging oxygen species which were formed during the irradiation experiments. Herein, nine previously unknown PTPs of TDBP-TAZTO were detected under UV-(C) irradiation and identified by HPLC-(HR)MS. As a result, debromination, hydroxylation, and dehydrobromination reactions could be presumed as the main degradation pathways by high-resolution mass spectrometry. The direct as well as the OH radical-induced indirect photolysis were observed. KW - UV irradiation KW - HRMS KW - Debromination KW - Hydroxylation KW - Emerging brominated flame retardant PY - 2019 DO - https://doi.org/10.1007/s11356-019-04815-w SN - 0944-1344 VL - 26 IS - 16 SP - 15838 EP - 15846 PB - Springer AN - OPUS4-47857 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keller, Julia A1 - Borzekowski, Antje A1 - Koch, Matthias T1 - Mykotoxine in Lebensmitteln - Zearalenon und seine Transformationsprodukte N2 - Mykotoxine in Lebensmitteln stellen weltweit Probleme dar, Zearalenon in Speiseöl ist ein solches. Neue Hydrazinbasierte Analyseverfahren können jetzt helfen, den EU-Grenzwert besser zu kontrollieren. Aber auch die Strukturaufklärung von Transformationsprodukten und verlässliche Kalibrierstandards sind aktuelle Herausforderungen. KW - Analyseverfahren KW - Hydrazin KW - Speiseöle KW - Transformationsprodukte PY - 2019 IS - 03 SP - 34 EP - 36 AN - OPUS4-47858 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weber, M. T1 - Pharmacopoeial Reference Standards for Elemental Impurities N2 - Elemental impurities (EI) in medicinal products for human use are limited according to ICH guideline Q3D, which is in force since December 2017 in Europe and US. As a consequenceconsequence, the relevant texts of the European Pharmacopoeia (Ph. Eur.) and the United States Pharmacopeia (USP) have been modified to reflect and complement ICH Q3D, providing details on the analytical methods to be used. In those chapters (Ph. Eur. 2.4.20., USP <233>), it is stated that for the quantification of elemental impurities, certified reference materials (CRM) from a national metrology institute (NMI) or reference materials that are traceable to the CRM of an NMI should be used. The Ph. Eur. has so far implemented elemental impurity standards of this type for the four most important elemental impurities i.e. those corresponding to ICH Q3D Class 1: lead, cadmium, mercury and arsenic. The poster provides details on the development of those four reference standards, which was undertaken in partnership with a major institute accredited CRM producer (JRC, European Commission), and a national metrology institute (BAM and PTB, Germany), and a Designated Institute and accredited CRM producer (BAM, Germany). The reference standards were established and characterised according to rigorous metrological principles and are supplied with extended supporting information as required for the intended use. After successful completion of the project, the four reference standards have been added to the Ph.Eur. catalogue and are in distribution. It is expected that another three elemental impurity standards will be implemented and made available to users within the next three years. T2 - Joint EDQM-USP 13th International Symposium on Pharmaceutical Reference Standards CY - Strasbourg, France DA - 13.03.2019 KW - ICH guideline Q3D KW - Elemental Impurities KW - Pharmacopoeial Reference Standards PY - 2019 AN - OPUS4-47845 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roethke, A. T1 - SI-traceable monoelemental solutions on the highest level of accuracy: From the foundation of CCQM to recent advances N2 - Shortly after founding the CCQM in 1993, the first key comparison (CCQM-K2) about the determination of Cd and Pb content in river water was hosted by IRMM. It has been clear from the beginning that for the determination of an element mass fraction in a matrix, accurate reference solutions would be the key point for a metrologically sound analysis. Triggered by the not entirely satisfactory results it was decided to investigate the basis of all measurements: the reference solutions. Thus in 1999, CCQM-K8, hosted by EMPA/LNE, started the tedious but indispensable work on elemental solutions standards. Additionally, PTB, BAM and Merck KGaA initiated a project to establish a traceability system for inorganic analysis based on accurate monoelemental solutions. Within this unique approach ten high purity reference materials were fully characterized, and solutions were prepared gravimetrically thereof. These materials (forming the primary standards of elemental analysis) are available for NMIs/DIs from BAM. CCQM-P46 (Cu, Mg, Rh) demonstrated the actuality of the topic and the challenges to prepare elemental solutions for every element. The accurate preparation and use of monoelemental solutions is consequently reflected in the recurrent conduct of (key) comparisons: CCQM-P149 (purity of zinc), CCQM-K87 (Co, Cr, Pb), and the current CCQM-K143/P181 (Cu solutions), to name only a few in a long series. Is it necessary to put so much effort into the preparation of reference solutions? It clearly is! An example outside the world of academia: Recently, EDQM*, PTB, BAM and JRC have developed monoelemental reference standards traceable to the SI for toxic elements in support of the chapters of the European Pharmacopoeia, related to the analysis of elemental impurities in medicinal products. A new ICP OES method has been established allowing the comparison of two 1 g/kg mercury solutions with an outstandingly small uncertainty of Urel(w(Hg)) = 0.16 %. However, this technical progress would not have been possible without the ongoing effort of the metrological community within 25 years of research in the field of high accuracy monoelemental solutions. * EDQM: European Directorate for the Quality of Medicines and HealthCare T2 - CCQM Workshop on Advances in Metrology in Chemistry and Biology CY - Sevre DA - 10.04.2019 KW - CCQM KW - SI-traceable KW - Monoelemental solutions PY - 2019 UR - https://youtu.be/iVLk8CFnJTI AN - OPUS4-47846 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Makowski, Maike T1 - Hot-spots of non-volatile mycotoxins in cereals: How can we overcome this problem? N2 - Since cereals constitute a staple food worldwide, monitoring of growth, storage and processing represent a perseverative challenge of analytical sciences. Especially during storage infested grains breed fungal clusters (“hot spots”) in which mycotoxins accumulate and can highly exceed allowed maximum levels. Because of their unpredictable presence, analytical procedures – including representative sampling - contain invasive and time intensive steps. To avoid erroneously negative results in mycotoxin analysis in cereals, the samples´ homogeneous headspace might be investigated instead of analyzing subsamples of the grains. So-called microbial volatile organic compounds (MVOC´s) provide information for instance about the fungal status of grains. Previous investigations revealed trichodiene to be a precursor of trichothecene mycotoxins which comprises more than 180 different compounds. Due to its non-functionalised sesquiterpene structure, quantification of trichodiene using Headspace GC-MS methods is possible. Thereby, it could be used as biomarker for trichothecene contamination of cereals. Nevertheless, further investigations are necessary. To be able to draw conclusion about the trichothecene content in cereal samples, a possible correlation between trichodiene concentration in the gas phase and trichothecene concentration in the sample must be examined. Realizing this idea would widely extend the applicability of trichodiene and enormously simplify trichothecene detection. Hence, the first step of an ongoing study aims to develop a laboratory reference method using trichodiene as volatile biomarker to quantify trichothecenes in cereals. Both static headspace and SPME-enrichment coupled to gas chromatography with mass spectrometry (GC-MS) were tested and compared. In a second step, this reference method is intended to validate new approaches for fast on-site screening of trichodiene in cereals. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Trichodiene KW - Gaschromatography-Mass Spectrometry KW - Mycotoxin-Biomarker PY - 2019 AN - OPUS4-47847 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotthoff, Lisa T1 - Investigation of the veterinary drug monensin: Simulation and identification of transformation products N2 - The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for health, food and environmental matters. Monensin (MON) is an ionophore antibiotic widely used to cure and prevent coccidiosis by chicken especially in broiler farming. Residues are not only found in food products (chicken and eggs) but also in the environment (manure, soil or water). Several transformation processes can alter the parent compound MON, ranging from biotransformation in living organism to biotic/abiotic and microbial processes in environmental matters. The main objective of this work was to investigate the potential of electrochemistry (EC) to simulate oxidative transformation processes and to predict TPs of MON. An electrochemical reactor was used consisting of a flow-through cell with a glassy carbon working electrode. Derived TPs were analyzed by online coupling of EC and high-resolution mass spectrometry (HRMS) and LC-HRMS offline measurements. Among the generated TPs already known as well as unknown TPs of MON could be found. Additionally, MON was subjected also to other transformation methods such as Fenton reaction, photochemical and hydrolysis experiments as well as metabolism tests with microsomes. As a result, different targeted and suspected TPs could be identified by analysis with LC-HRMS. An overview of detected/identified TPs from this study will be presented in comparison to literature known metabolites and TPs. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Transformation Products KW - Electrochemistry KW - High-resolution MS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476813 AN - OPUS4-47681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Der Einsatz der Glimmentladungsmassenspektroskopie für die Charakterisierung von Renststoffen als primäre Kalibriersubstanzen N2 - Messergebnisse in der chemischen Analyse müssen vergleichbar sein. Dies wird durch die metrologische Rückführbarkeit (traceability) auf SI realisiert. In der Chemie dienen Reinststoffe als Primärnormale, deren Reinheit mit einer Unsicherheit von < 0.01% ermittelt werden soll. Ein eleganter Weg, die Reinheit eines realen Materials mit hoher Präzision zu bestimmen, ist, alle Verunreinigungen zu messen, diese aufzusummieren und von der idealen Reinheit von 100 Prozent abzuziehen. Die metallischen Verunreinigungen in Metallen lassen sich mittels hochauflösender Massenspektrometer ermitteln. Eine weit größere Herausforderung ist die Bestimmung von Nichtmetallen wie Sauerstoff, Wasserstoff und Stickstoff im Metall, zumal diese auch oft die Hauptverunreinigung darstellen. Für die quantitative Bestimmung von Verunreinigungen wurden mit Standards dotierte Pulverpresslinge und mit H, O und N dotierte, gesinterte Materialien auf ihre Eignung als Kalibrierstandards für die GD-OES und GD-MS untersucht. Dabei kamen unterschiedliche Plasmabedingungen (pulsed/ continuous mode; verschiedene Plasmagase) zum Einsatz. Ein Überblick über analytische Kenngrößen und Grenzen der verwendeten Kalibrierstrategien wird gegeben. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - GDMS KW - Primäre Kalibriersubstanzen KW - Reinststoffe PY - 2019 AN - OPUS4-47843 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abdelshafi, Nahla A. A1 - Bell, Jérémy A1 - Rurack, Knut A1 - Schneider, Rudolf T1 - Microfluidic electrochemical immunosensor for the trace analysis of cocaine in water and body fluids N2 - Quick but accurate testing and on‐the‐spot monitoring of cocaine in oral fluids and urine continues to be an important toxicological issue. In terms of drug testing, a number of devices have been introduced into the market in recent decades, notably for workplace inspection or roadside testing. However, these systems do not always fulfill the requirements in terms of reliability, especially when low cut‐off levels are required. With respect to surface water, the presence of anthropogenic small organic molecules such as prescription and over‐the‐counter pharmaceuticals as well as illicit drugs like cannabinoids, heroin, or cocaine, has become a challenge for scientists to develop new analytical tools for screening and on‐site analysis because many of them serve as markers for anthropogenic input and consumer behavior. Here, a modular approach for the detection of cocaine is presented, integrating an electrochemical enzyme‐linked immunosorbent assay (ELISA) performed on antibody‐grafted magnetic beads in a hybrid microfluidic sensor utilizing flexible tubing, static chip and screen‐printed electrode (SPE) elements for incubation, recognition, and cyclic voltammetry measurements. A linear response of the sensor vs. the logarithm of cocaine concentration was obtained with a limit of detection of 0.15 ng/L. Within an overall assay time of 25 minutes, concentrations down to 1 ng/L could be reliably determined in water, oral fluids, and urine, the system possessing a dynamic working range up to 1 mg/L. KW - Cocaine PY - 2018 DO - https://doi.org/10.1002/dta.2515 VL - 11 SP - 492 EP - 500 PB - Wiley CY - Weinheim AN - OPUS4-48319 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Soba, L. A1 - Tuma, Dirk T1 - Messung der Schallgeschwindigkeit in Neopentan bei Temperaturen von (263 bis 373) K und Drücken bis 20 MPa N2 - Alkan-Isomere haben signifikanten Einfluss als Spurenstoffe auf thermodynamische Eigenschaften von Erdgasgemischen. In Erdgas sind bis zu 0.35 mol-% Neopentan enthalten. Gemischmodelle basieren auf Reinstoffzustandsgleichungen der beteiligten Komponenten. Die hier untersuchte Schallgeschwindigkeit ist von besonderer Bedeutung für die Entwicklung hochgenauer Gleichungen. T2 - Thermodynamik-Kolloquium 2025 CY - Hamburg, Germany DA - 22.09.2025 KW - Neopentan KW - Schallgeschwindigkeit KW - Zustandsgleichung PY - 2025 AN - OPUS4-64226 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tavernaro, Isabella A1 - Sander, P. C. A1 - Andresen, E. A1 - Schedler, U. A1 - Resch-Genger, Ute T1 - Expanding the Toolbox of Simple, Cost-Efficient, and Automatable Methods for Quantifying Surface Functional Groups on Nanoparticles� Potentiometric Titration N2 - Measuring surface functional groups (FGs) on nanomaterials (NMs) is essential for designing dispersible and stable NMs with tailored and predictable functionality. FG screening and quantification also plays a critical role for subsequent processing steps, NM long-term stability, quality control of NM production, and risk assessment studies and enables the implementation of sustainable and safe(r)-by-design concepts. This calls for simple and cost-efficient methods for broadly utilized FGs that can be ideally automated to speed up FG screening, monitoring, and quantification. To expand our NM surface analysis toolbox, focusing on simple methods and broadly available, cost-efficient instrumentation, we explored a NM-adapted pH titration method with potentiometric and optical readout for measuring the total number of (de)protonable FGs on representatively chosen commercial and custom-made aminated silica nanoparticles (SiO2 NPs). The accuracy and robustness of our stepwise optimized workflows was assessed by several operators in two laboratories and method validation was done by cross-comparison with two analytical methods relying on different signal generation principles. This included traceable, chemo-selective quantitative nuclear magnetic resonance spectroscopy (qNMR) and thermogravimetric analysis (TGA), providing the amounts of amino silanes released by particle dissolution and the total mass of the surface coatings. A comparison of the potentiometric titration results with the reporter-specific amounts of surface amino FGs determined with the previously automated fluorescamine (Fluram) assay highlights the importance of determining both quantities for surface-functionalized NMs. In the future, combined NM surface analysis with optical assays and pH titration will simplify quality control of NM production processes and stability studies and can yield large data sets for NM grouping that facilitates further developments in regulation and standardization. KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Characterization KW - Advanced material KW - Surface KW - Standardization KW - Reference material KW - Functional group KW - Quantification KW - Coating KW - Automation KW - Potentiometry KW - Method KW - Validation KW - Optical assay KW - Fluram KW - Fluorescamine KW - qNMR KW - Comparison KW - ILC PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642371 DO - https://doi.org/10.1021/acsmeasuresciau.5c00062 SN - 2694-250X SP - 1 EP - 13 PB - American Chemical Society CY - Washington, DC AN - OPUS4-64237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - Where Do We Stand – Quantifying Amino Groups on Silica (Nano)Particles N2 - Industry and regulators are increasingly requesting validated and standardized measurement protocols to support the manufacturing, quality control, and safe use of engineered nanomaterials. Addressing a remaining gap in method development and standardization for nanomaterial characterization, we investigated in a bilateral comparison various methods commonly used for surface functional group quantification, like quantitative nuclear magnetic resonance (qNMR) spectroscopy, x-ray photoelectron spectroscopy (XPS), and optical assays. These results demonstrate not only an influence of the size and synthesis methods on the number of surface functional groups for differently sized commercial and in-house synthesized silica nanoparticles but also on their functionality. T2 - Kickoff-Meeting SMURFnano CY - Berlin, Germany DA - 09.07.2024 KW - Nano KW - Particles KW - Silica KW - Synthesis KW - Quantification KW - Functional groups KW - Quality assurance KW - Reference material KW - Interlaboratory comparison KW - Method KW - Uncertainty KW - Sensor KW - Surface analysis PY - 2024 AN - OPUS4-62164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bolz, Axel T1 - Microfluidic paper strips for SERS analysis N2 - Surface enhanced Raman scattering (SERS) is a fast and sensitive spectroscopic method for the identification of analytes. With available portable Raman spectrometers, on-site analysis is possible. However, for on-site analysis, SERS substrates, which are cheap, easy to prepare, and simple in sample handling are necessary. Relevant analytes in the addressable concentration region for SERS are e.g. antibiotics and pesticides. Here, we present paper-based test strips for SERS analysis which are coated with silver nanoparticles. The coating was realized with different deposition methods of nanoparticle solutions. The papers were also functionalised with hydrophobic barriers to create μPADs. The strips were tested with selected analytes (e.g., adenine, rhodamine-6G) over a broad concentration range. The focus of our study lay on reproducibility and optimum SERS signal intensity. For the quantification of analytes, highly reproducible signal intensities are necessary. We have realized this reproducibility in acceptable quality. Moreover, employing intensity vs concentration calibration for the analytes, data analysis revealed a behaviour that was best described by a Langmuir isotherm, stressing the strong distance dependence of the SERS effect. For a fast and reproducible analysis of the data, a Labview program was finally compiled, which was fed with the calibration data and derived the concentration of analyte unknowns accordingly. T2 - 5. Berliner Chemie Symposium & 1. Chemie in Praxis CY - Berlin, Germany DA - 12.04.2016 KW - SERS KW - Raman KW - Paper PY - 2016 AN - OPUS4-36031 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wan, Wei A1 - Descalzo, Ana B. A1 - Shinde, S. A1 - Weißhoff, Hardy A1 - Orellana, G. A1 - Sellergren, B. A1 - Rurack, Knut T1 - Ratiometric fluorescence detection of phosphorylated amino acids through excited-state proton transfer by using molecularly imprinted polymer (MIP) recognition nanolayers N2 - A 2,3-diaminophenazine bis-urea fluorescent probe monomer (1) was developed. It responds to phenylphosphate and phosphorylated amino acids in a ratiometric fashion with enhanced fluorescence accompanied by the development of a redshifted emission band arising from an excited-state proton transfer (ESPT) process in the hydrogen-bonded probe/analyte complex. The two urea groups of 1 form a cleft-like binding pocket (Kb>10^10 L^2 mol^-2 for 1:2 complex). Imprinting of 1 in presence of ethyl ester- and fluorenylmethyloxycarbonyl (Fmoc)-protected phosphorylated tyrosine (Fmoc-pTyr-OEt) as the template, methacrylamide as co-monomer, and ethyleneglycol dimethacrylate as crosslinker gave few-nanometer-thick molecularly imprinted polymer (MIP) shells on silica core microparticles with excellent selectivity for the template in a buffered biphasic assay. The supramolecular recognition Features were established by spectroscopic and NMR studies. Rational screening of comonomers and cross-linkers allowed to single out the best performing MIP components, giving significant imprinting factors (IF>3.5) while retaining ESPT emission and the ratiometric response in the thin polymer shell. Combination of the bead-based detection scheme with the phase-transfer assay dramatically improved the IF to 15.9, allowing sensitive determination of the analyte directly in aqueous media. KW - Core-shell particles KW - Excited-state proton transfer KW - Fluorescence KW - Molecular imprinting KW - Phosphorylated amino acids PY - 2017 DO - https://doi.org/10.1002/chem.201703041 SN - 1521-3765 SN - 0947-6539 VL - 23 IS - 63 SP - 15974 EP - 15983 PB - Wiley-VCH CY - Weinheim AN - OPUS4-43101 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sun, Yijuan A1 - Pérez-Padilla, Víctor A1 - Valderrey, Virginia A1 - Bell, Jérémy A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Fluorescence Detection of Perfluoroalkyl Carboxylic Acids with a Miniaturised Assay N2 - Per- and polyfluoroalkyl substances (PFAS) are a class of man-made organo-fluorine chemicals that have become environmental contaminants of emerging concern, originating from a variety of materials such as adhesive, stain- and oil-resistant coatings, firefighting foams, etc. The high strength of this C-F bond makes PFAS thermodynamically stable and resistant to (bio)degradation, thus retaining them in the environment over time. Perfluoroalkyl carboxylic acids (PFCAs), one category of the most used PFAS, consist of a fully fluorinated carbon backbone and a charged carboxylic acid headgroup, and have been classified as Substances of Very High Concern (SVHC) and added to the REACH Candidate List due to their persistence in the environment, non-biodegradability and toxicological effects.[1-2] Traditional techniques for the analysis of PFCAs include GC-MS, HRMS and HPLC-based approaches, which are laborious, not portable, costly and require trained personnel. In contrast, fluorescence assays can be designed as easy-to-operate, portable and cost-effective methods with high sensitivity and fast response. Integration of fluorescent probes with an adequately miniaturized assay enables a promising alternative for PFCAs analysis. Here, a novel guanidine fluorescent probe has been synthesized and fully characterized for the detection of PFCAs in a biphasic extract-&-detect assay. The fluorescent probe was then incorporated into polymeric matrices supported by a red dye-doped SiO2 nanoparticle to construct a dual-emission sensing platform. Such a system allows precise and selective detection of PFCAs, reducing the interference of competitors, matrix effects and other factors except for the PFCAs. The system was then employed in a droplet-based microfluidic setup which offers a portable and easy to operate detection platform. T2 - IMA 2023 CY - Chania, Greece DA - 18.09.2023 KW - PFAS KW - MIP KW - Fluorescence KW - Microfluidics KW - Fluorezsenz KW - Mikrofluidik PY - 2023 AN - OPUS4-58527 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia T1 - Electrochemistry coupled with LC/MS for production and characterization of mycotoxin oxidation products N2 - Mycotoxins cause a variety of mold-related health risks which makes it necessary to further examine their metabolic pathways in human and other mammals. Beside standard in vitro assays with liver cell microsomes an increasing interest in new and rapid simulation techniques are playing a growing role in mycotoxin research. Herein, the coupling of electrochemistry with liquid chromatography and mass spectrometry (EC/LC/MS) is presented as fast and simple method to investigate the oxidative fate of mycotoxins. For this case study, two food relevant mycotoxins (zearalenone and citrinin) were selected. Experiments were performed by using an electrochemical flow through cell integrated in the flow path of the autosampler of the chromatographic system. The reaction mixture was separated by a RP-C18 column and analyzed by a single quadrupole MS (Figure 1). Oxidation products were generated by applying potentials of 400, 800, 1200 and 1600 mV vs Pd/H2 using a glassy carbon working electrode. Different oxidation reactions like hydroxylation, dehydrogenation and dimerization lead to a diverse product pattern of the investigated mycotoxins. In a comparative study, electrochemical generated reaction products were compared with metabolites produced by human and rat liver microsomes in vitro. The obtained data show that EC/LC/MS is a versatile and promising tool in mycotoxin research to support metabolic investigations of known and unknown mycotoxins. T2 - Tag der Chemie CY - Berlin, Germany DA - 03.07.2017 KW - Electrochemistry KW - Mycotoxins PY - 2017 AN - OPUS4-42980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heilmann, Maria A1 - Kulla, Hannes A1 - Prinz, Carsten A1 - Bienert, Ralf A1 - Reinholz, Uwe A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska T1 - Advances in Nickel Nanoparticle Synthesis via Oleylamine Route N2 - Nickel nanoparticles are an active research area due to their multiple applications as catalysts in different processes. A variety of preparation techniques have been reported for the synthesis of these nanoparticles, including solvothermal, microwave-assisted, and emulsion techniques. The well-studied solvothermal oleylamine synthesis route comes with the drawback of needing standard air-free techniques and often space-consuming glassware. Here, we present a facile and straightforward synthesis method for size-controlled highly monodisperse nickel nanoparticles avoiding the use of, e.g., Schlenk techniques and space-consuming labware. The nanoparticles produced by this novel synthetic route were investigated using small-angle X-ray scattering, transmission electron microscopy, X-ray diffraction, and X-ray spectroscopy. The nanoparticles were in a size range of 4–16 nm, show high sphericity, no oxidation, and no agglomeration after synthesis. KW - Nanoparticle synthesis KW - Nickel nanoparticles KW - SAXS KW - TEM KW - XAS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507531 DO - https://doi.org/10.3390/nano10040713 VL - 10 IS - 4 SP - 713 PB - MDPI AN - OPUS4-50753 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadejde, C. A1 - Neamtu, M. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Ababei, G. A1 - Panne, Ulrich T1 - Hybrid iron-based core-shell magnetic catalysts for fast degradation of bisphenol A in aqueous systems N2 - Three types of hybrid modified magnetite (Fe₃O₄) nanoparticles, functionalized with either chitosan, chitosan/iron (II) oxalate or chitosan/iron (III) citrate, were synthesized by chemical precipitation method. The obtained nanomaterials were characterized by energy dispersive X-ray spectroscopy, X-ray diffraction, Brunauer–Emmett–Teller analysis, scanning and Transmission electron microscopy, Fourier transform infrared spectroscopy and vibrating sample magnetometry. The prepared composites were further tested as magnetic catalysts for the removal of bisphenol A (BPA) in aqueous media. The kinetic Degradation experiments were performed at laboratory scale, while the best operational parameters for all three materials were established: 1.00 g L⁻¹ of catalyst, 10 mmol L⁻¹ H₂O₂, under simulated solar light irradiation. After 15 min of UVA irradiation under the experimental conditions mentioned above, it was possible to decompose up to 99% of the micropollutant over all catalysts. Fe₃O₄/chitosan/iron oxalate catalyst showed the highest and fastest catalytic activity in BPA removal. Catalytic wet peroxide oxidation of non-biodegradable micropollutants on such iron-based hybrid nanoparticles can be a suitable pre-treatment method for wastewater decontamination, as an environment-friendly simplified Approach for water clean-up. KW - Katalysator KW - Bisphenol A KW - Nano KW - Fenton KW - Magnetische Nanopartikel PY - 2016 DO - https://doi.org/10.1016/j.cej.2016.05.090 SN - 1385-8947 VL - 302 SP - 587 EP - 594 PB - Elsevier CY - Amsterdam AN - OPUS4-37126 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kalbe, Ute A1 - Lehnik-Habrink, Petra A1 - Bandow, Nicole A1 - Sauer, Andreas T1 - Validation of European horizontal methods for the analysis of PAH, PCB and dioxins in sludge, treated biowaste and soil N2 - Draft standards for the determination of organic pollutants in the solid matter of environmental matrices such as sludge, treated biowaste and soil have been basically developed in the framework of the European standardization project HORIZONTAL. A research project financed by the German Federal Environment Agency was initiated to finalize some of these CEN standard drafts, since fully validated standard procedures are crucial for the evaluation of their reliability in the context of implementation in legislation on environmental health. Approach: Appropriate test materials (< 2mm particle size) were prepared and homogenized from contaminated soils, sludge and treated biowaste containing polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCB), dioxins, furans and dioxin-like-PCB and served, along with reference solutions, as the basis for international interlaboratory comparisons. Performance data of three analytical standard procedures were obtained by the statistical evaluation of results received from 11 to 29 participants per test material. Results: The overall variation coefficients of reproducibility (between-lab standard deviations) for the sum parameters were roughly between 10 and 35 %. The variation coefficients of repeatability (within-lab standard deviations) range between 3 % and 8 % and show no trend considering the substance groups or matrices. The highest coefficients of reproducibility were found for the analysis of PAHs, which were between 26 and 35 %, depending on the matrix, whereas 7-17 % reproducibility was observed for toxicity equivalents (TEQ) comprising dioxins, furans and dl-PCB. Conclusions: Overall, the results confirm that the procedures described in the Technical Specifications are fit for purpose for all three matrices and that the feasibility of the HORIZONTAL approach, to cover several matrices with one standard per analyte, was thereby proven. KW - Standardization KW - Analytical methods KW - Organic contaminants KW - Validation trial KW - Interlaboratory comparison PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479914 DO - https://doi.org/10.1186/s12302-019-0211-3 SN - 2190-4715 VL - 31 SP - 29, 1 EP - 10 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-47991 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kalbe, Ute T1 - Suffos - Bedingungen suffosiver Erosionsphänomene in Böden N2 - Das Projekt befasste sich mit der Suffosion in weitgestuften Erdstoffen. Dabei werden Poren- und Gefügestrukturen visualisiert und parametrisiert. Bei der Suffosion handelt es sich um eine Form der inneren Erosion bei weitgestuften Erdstoffen, die durch Umlagerung und Abtransport feiner Sedimentteilchen im Porenraum unter dem Einfluss von Wasserströmungen hervorgerufen wird. Die Suffosion kann zu Problemen mit der Stabilität des Korngerüstes von Erdstoffen führen. Relevante Anwendungsgebiete sind z.B. im Verkehrswegebau, Hochwasserschutz und allgemeinen Erdbau zu finden. Im Rahmen des Projektes wurden solche Erosionsprozesse numerisch simuliert, um auf statistischer Grundlage Grenzzustände zu formulieren. Ziel des Projekts war es, die Erosionsprozesse numerisch zu simulieren, um auf statistischer Grundlage Grenzzustände zu formulieren. KW - Suffosion KW - Erosion KW - Verkehrswegebau KW - Hochwasserschutz PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-386296 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38629 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Feiler, Torvid A1 - Bhattacharya, Biswajit A1 - Michalchuk, Adam A1 - Schröder, V. A1 - List-Kratochvil, E. A1 - Emmerling, Franziska T1 - Mechanochemical Syntheses of Isostructural Luminescent Cocrystals of 9-Anthracenecarboxylic Acid with two Dipyridines Coformers N2 - Tuning and controlling the solid-state photophysical properties of organic luminophore are very important to develop next-generation organic luminescent materials. With the aim of discovering new functional luminescent materials, new cocrystals of 9-anthracene carboxylic acid (ACA) were prepared with two different dipyridine coformers: 1,2-bis(4-pyridyl)ethylene and 1,2-bis(4-pyridyl)ethane. The cocrystals were successfully obtained by both mechanochemical approaches and conventional solvent crystallization. The newly obtained crystalline solids were characterized thoroughly using a combination of single crystal X-ray diffraction, powder X-ray diffraction, Fourier-transform infrared spectroscopy, differential thermal analysis, and thermogravimetric analysis. Structural analysis revealed that the cocrystals are isostructural, exhibiting two-fold interpenetrated hydrogen bonded networks. While the O–H···N hydrogen bonds adopts a primary role in the stabilization of the cocrystal phases, the C–H···O hydrogen bonding interactions appear to play a significant role in guiding the three-dimensional assembly. Both π···π and C–H···π interactions assist in stabilizing the interpenetrated structure. The photoluminescence properties of both the starting materials and cocrystals were examined in their solid states. All the cocrystals display tunable photophysical properties as compared to pure ACA. Density functional theory simulations suggest that the modified optical properties result from charge transfers between the ACA and coformer molecules in each case. This study demonstrates the potential of crystal engineering to design solid-state luminescence switching materials through cocrystallization. KW - Cocrystal KW - Mechanochemical synthesis KW - Luminescence KW - X-ray diffraction KW - DFT calculation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518226 DO - https://doi.org/10.3390/cryst10100889 VL - 10 IS - 10 SP - 889 PB - MDPI AN - OPUS4-51822 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kervarec, M.-C. A1 - Kemnitz, E. A1 - Scholz, G. A1 - Rudic, S. A1 - Jäger, Christian A1 - Braun, T. A1 - Michalchuk, Adam A1 - Emmerling, Franziska T1 - A HF Loaded Lewis-Acidic Aluminium Chlorofluoride for Hydrofluorination Reactions N2 - The very strong Lewis acid aluminium chlorofluo-ride (ACF) was loaded with anhydrous HF. The interactionbetween the surface of the catalyst and HF was investigatedusing a variety of characterization methods, which revealed he formation of polyfluorides. Moreover, the reactivity ofthe HF-loaded ACF towards the hydrofluorination of alkyneswas studied. KW - Aluminium KW - HF KW - Hydrofluorination KW - Metal fluorides PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508360 DO - https://doi.org/10.1002/chem.202001627 VL - 26 SP - 1 PB - Wiley Online Libary AN - OPUS4-50836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eitzen, L. A1 - Paul, S. A1 - Braun, Ulrike A1 - Altmann, Korinna A1 - Jekel, M. A1 - Ruhl, A. T1 - The challenge in preparing particle suspensions for aquatic microplastic research N2 - The occurrence of small particles consisting of organic polymers, so-called microplastic (MP), in aquatic Environments attracts increasing interest in both public and science. Recent sampling campaigns in surface Waters revealed substantial numbers of particles in the size range from a few micrometers to a few millimeters. In order to validate sample preparation, identification and quantification and to investigate the behavior of MP particles and potential toxic effects on organisms, defined MP model particles are needed. Many studies use spherical compounds that probably behave differently compared to irregularly shaped MP found in environmental samples. However, preparation and handling of MP particles are challenging tasks and have been systematically investigated in the present study. Polystyrene (PS) as a commonly found polymer with a density slightly above that of water was selected as polymer type for milling and fractionation studies. A cryogenic ball mill proved to be practical and effective to produce particles in the size range from 1 to 200 μm. The yield of small particles increased with increasing pre-cooling and milling durations. Depending on the concentration and the size, PS particles do not completely disperse in water and particles partly creep vertically up along glass walls. Stabilized MP suspensions without use of surfactants that might harm organisms are needed for toxicological studies. The stabilization of PS particle suspensions with ozone treatment reduced the wall effect and increased the number of dispersed PS particles but increased the dissolved organic carbon concentration and changed the size Distribution of the particles. KW - Reference material KW - Microplastic PY - 2018 DO - https://doi.org/10.1016/j.envres.2018.09.008 SN - 0013-9351 SN - 1096-0953 VL - 168 SP - 490 EP - 495 PB - Elsevier AN - OPUS4-46462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Per- and polyfluoroalkyl substances (PFAS) in ski waxes and snow from cross-country skiing in Germany - Comparative study of target analysis and sum parameters N2 - Per- and polyfluoroalkyl substances (PFAS) can enter the environment in different ways. Possible sources are PFAS containing consumer products. One common product that makes use of the material properties of PFAS is ski wax. Here, the PFAS ensure less frictional resistance, thus allows for increased speed. However, people who wax their ski with these waxes could absorb PFAS in their body, which can lead to health problems in the long term. Moreover, PFAS applied in ski wax abrade onto snow during use, which contaminates the environment. In our study, we analyzed various currently available ski waxes (2020s) and ski waxes from the 1980s with PFAS target analysis and with the sum parameters extractable organically bound fluorine (EOF), hydrolysable organically bound fluorine (HOF) and total fluorine (TF). Moreover, snow samples from the long-distance cross-country ski trail “Kammloipe” in the Ore mountains in Germany where sampled and analyzed with PFAS target analysis and the adsorbable organically bound fluorine (AOF) sum parameter to document the entry of PFAS from ski waxes into the environment. In opposite to the ski waxes from the 1980s much more ski waxes from the 2020s contain high (total) fluorine values. The highly fluorinated ski waxes contain up to approx. 6% of fluorine. The EOF and HOF sum parameters of the ski waxes are strongly decreased in comparison to the TF values (max. approx. 1000 mg/kg = 0.1%). But even the PFAS-free labeled ski waxes have EOF/HOF values in the low mg/kg range. In the snow samples from different spots of the ski trail, both the AOF sum parameter and the PFAS target analysis identified PFAS. Moreover, on a PFAS hotspot also soil samples were analyzed, which indicate that PFAS from the ski waxes adsorb after snow melting into the soil. Thus, our results show that the use of ski waxes is a possible contribution to the environmental contamination of PFAS, which is hopefully drastically reduced with the ban on fluorinated waxes by the International Ski and Snowboard Federation (FIS). T2 - SETAC Europe CY - Vienna, Austria DA - 11.05.2025 KW - Per- and polyfluoroalkyl substances (PFAS) KW - Contaminated Soil KW - Ski wax PY - 2025 AN - OPUS4-63096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Altmann, Korinna T1 - Reference material BAM-P206 polyethylene terephthalate (powder) N2 - This report contains detailed information on the preparation of the reference material as well as on homogeneity and stability investigations of the property of interest, the equivalent particle diameter, and on the analytical methods to determine the additional properties. The values for particle size distribution are based on the results from laser diffraction measurements of 3 different devices with at least 3 replicate measurements of 4 randomly chosen units of the reference material P206. KW - Microplastic KW - Reference material KW - PET PY - 2023 DO - https://doi.org/10.26272/opus4-59778 SP - 1 EP - 23 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-59778 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Goedecke, Caroline A1 - Bannick, C.-G. A1 - Abusafia, A. A1 - Scheid, C. A1 - Steinmetz, H. A1 - Paul, Andrea A1 - Beleites, C. A1 - Braun, U. T1 - Identification of microplastic pathways within a typical European urban wastewater system N2 - In recent years, thermoextraction/desorption-gas chromatography/mass spectrometry (TED-GC/MS) has been developed as a rapid detection method for the determination of microplastics (MP) mass contents in numerous environmentally relevant matrices and, in particular, for the measurement of polymers in water samples without time-consuming sample preparation. The TED-GC/MS method was applied to investigate a typical European municipal wastewater system for possible MP masses. Such investigations are important in view of the recent revision of the Urban Wastewater Treatment Directive. Four different representative sampling sites were selected: greywater (domestic wastewater without toilet), combined sewer, and influent and effluent of a wastewater treatment plant (WWTP). All samples were collected by fractional filtration. Filtration was carried out over mesh sizes of 500, 100, 50, and in some cases, 5 µm. Polyethylene (PE), polypropylene (PP), and polystyrene (PS) were detected in all samples, with the PE fraction dominating in all cases. Styrene-butadiene rubber which serves as an indication of tire abrasion, was only found in the influent of the WWTP. The highest MP mass contents were found in the combined sewer, so MP can become a source of pollution during heavy rain events when the capacity limits of the effluent are reached, and the polluted effluent is released uncontrolled into the environment. Based on the studies, MP retention from the WWTP could be estimated to be approximately 96%. Few trends in polymer type or mass contents were detected within the different fractions of the samples or when comparing samples to each other. KW - Microplastics KW - Microplastic analysis KW - TED-GC/MS KW - Microplastic pathways KW - Mass contents PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568289 DO - https://doi.org/doi.org/10.1002/appl.202200078 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-56828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Diffusive Gradients in Thin-films (DGT) technique as screening tool for per- and polyfluoroalkyl substances (PFAS) contamination in wastewater-based fertilizers N2 - Per- and polyfluoroalkyl substances (PFAS) are a large group of organofluorine surfactants used in the formulations of thousands of consumer goods, including aqueous film-forming foams (AFFF) used to suppress aviation fires in training scenarios, non-stick cookware, fast-food wrappers, water-repellent fabrics, medical equipment, and plastic and leather products. As a result of the perpetual use of PFAS containing products, effluents and sewage sludge from wastewater treatment plants (WWTPs) have been observed to be an important pathway for PFAS into the environment. In Germany, phosphorus and other nutrients from sewage sludge and wastewater should be recycled in WWTPs of cities with a large population. However, it is not clear if PFAS contamination from wastewater and sewage sludge end up in novel wastewater-based fertilizers. Normally, PFAS are analyzed using PFAS protocols typically with time-consuming extraction steps and LC-MS-MS quantification. However, for screening of PFAS contaminations in sewage sludge or wastewater-based fertilizers also passive sampler based on the Diffusive Gradients in Thin-films (DGT) technique can be used for the PFAS extraction. Afterwards, combustion ion chromatography (CIC) can be applied to analyse the “total” amount of PFAS on the passive sampler. Here, we show results from the DGT method in comparison to those of the extractable organic fluorine (EOF) method for a variety of wastewater-based fertilizers. Additionally, we analysed the adsorption of PFAS on the weak anion exchanger (WAX) based DGT passive sampler binding layer by infrared and fluorine K-edge X-ray adsorption near-edge structure (XANES) spectroscopy. T2 - SETAC Europe 2022 CY - Copenhagen, Denmark DA - 15.05.2022 KW - Passive sampling KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Sewage sludge KW - Wastewater PY - 2022 AN - OPUS4-54883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, U. T1 - Detection of plastics in soil N2 - Soil acts as a final sink for pollutants. Microplastics from different sources such as plastic mulching, littering, compost, sewage sludge, sedimentary deposition, and tyre abrasion are expected to be found in soil. However, representative and comprehensive information is missing on the sources, transport, and fate. Therefore, a reliable analysis method for microplastics in soils needs to be developed. The presented work describes the development of a procedure for microplastics analysis in soils. A representative sampling based on the on-site conditions and a sample preparation method was established and comprised of a drying step, the separation of microplastic particles > 1 mm, and a density separation for particles < 1 mm. The detection of the large microplastic particles (> 1 mm) was conducted with Attenuated Total Reflection - Fourier Transform infrared Spectroscopy (ATR-FTIR) , while Thermal Extraction Desorption - Gas Chromatography / Mass Spectrometry (TED-GC/MS) was applied for particles < 1 mm, gaining information on the type of polymer and mass fraction. Based on the established method, 14 environmental soil samples ? with different exposure of microplastics from agriculture, industrial sites, roads, and floods were investigated. Due to the arbitrary microplastic particle distribution among the samples for large microplastics, it was reasoned that the found particles were unrepresentative. In contrast, microplastic particles < 1 mm were discovered in a high mass in soil samples exposed to plastic mulching or fertilization with sewage sludge or compost (0 – 115 mg/kg). On average, microplastic contents detected in soil samples taken from a construction site and an inner-city lake were higher (13 – 238 mg/kg). As expected, microplastic content in soil sampled in proximity to roads was more pronounced in the upper soil layers. In contrast, very remote sampling sites, expectably uncontaminated, did not lead to the detection of microplastic regarding to thermoanalytical detection method. In a proof of concept experiment several in vivo and in vitro ecotoxicological tests were applied to evaluate the effect of microplastics (tyre abrasion, polystyrene containing hexabromocyclododecane) in natural soils. In summary, while no effects of the examined probes could be detected on higher levels of biological organization after exposures to earthworm E. andrei, significant changes in several oxidative stress related biomarkers were observed. T2 - SETAC Europe 2022 CY - Kopenhagen, Denmark DA - 15.05.2022 KW - Microplastic KW - TED-GC/MS KW - Soil PY - 2022 AN - OPUS4-55872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira Guilherme Buzanich, Ana T1 - Time resolved in situ monitoring of mechanochemical transformations by X-ray spectroscopy (XAS) N2 - Mechanochemical reactions promise a new direction for environmentally benign preparation of materials, and has been dubbed by IUPAC as one of the 10 chemical innovations that will change our world. Despite this significant promise, very little is known about the mechanisms that drive mechanochemical transformations, posing significant barriers to realizing their full potential. To this end, there is growing need to follow mechanochemical reactions in situ and in real time. We here describe advances in the development and application of XAS methods to monitor material synthesis in real time under mechanochemical conditions. We demonstrate the generality of our approaches by describing mechanochemical syntheses of materials by both vibratory ball milling and by Resonant Acoustic Mixing (RAM), where a time resolution of 1 second is for a whole XAS spectrum was achieved. Moreover, we describe how spectroscopic methods can be coupled to diffraction-based approaches, thereby providing new dimensions in understanding mechanochemical synthesis. T2 - AfLS3 CY - Online meeting DA - 14.11.2021 KW - Dipsersive XAS KW - Mechanochemistry KW - Time-resolved KW - In situ PY - 2021 AN - OPUS4-56256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kalbe, Ute A1 - Krüger, Oliver A1 - Bandow, Nicole A1 - Geburtig, Anja ED - Reichert, Thomas T1 - Laboratory Weathering Test for Simulating the Leaching from Artificial Sporting Grounds N2 - In order to estimating the amount and kind of emissions from polymeric sporting tracks a laboratory test was developed in BAM that combines artificial weathering and subsequent batch and column tests [1, 2, 3]. The goal consisted in nvestigating a possible change of emissions into soil and groundwater of a new sporting ground as a function of ageing and egradation of the system. At various stages of the weathering, the samples were removed and subjected to especially designed column extraction tests for the solid samples. Both these extracts and the accumulated rainwater run-off of the weathering device were subjected to analytical tests of their ingredients. The overall aim of the test consisted in developing ontrollable, reproducible, and standardisable conditions and methods of investigation that would allow an estimation of the emissions in the course of outdoor application of about five years. T2 - 7th European Weathering Symposium. Natural and Artificial Ageing of Polymers CY - Naples, Italy DA - 16.09.2015 KW - artificial weathering KW - emission KW - leaching KW - sporting track KW - degradation KW - ageing KW - rubber KW - extraction PY - 2015 SN - 978-3-9816286-6-1 VL - CEES 17 SP - 195 EP - 208 PB - Thomas Würtz CY - Karlsruhe, Germany AN - OPUS4-35401 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Plastik in Böden: Mikroplastik-Ergebnisse N2 - In diesem Vortrag geht um die Vorstellung der Ergebnisse des UBA Projektes Plastik in Böden. Es werden Mikroplastik-Gehalte in verschiedenen Böden präsentiert. T2 - Fachgespräch "Plastik in Böden" CY - Online meeting DA - 28.03.2022 KW - Mikroplastik KW - Mikroplastik Böden KW - Mikroplastik-Analytik PY - 2022 AN - OPUS4-54648 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wachtendorf, Volker A1 - Kalbe, Ute A1 - Krüger, O. A1 - Bandow, Nicole ED - Brown, R. ED - Gedde, U.W. ED - Hedenqvist, M.S. T1 - Influence of weathering on the leaching behaviour of zinc and PAH from synthetic sports surfaces N2 - Synthetic materials used for outdoor sports grounds consist of a mix of inorganic, organic and polymeric compounds that show ageing due to weathering and a complex leaching behaviour by percolation of rainwater, which can limit its lifetime. Additionally, weathering exposure induces degradation processes in the polymers, which leads to the formation of new surfaces allowing water to access additional reservoirs of leachable compounds. A laboratory test comprising artificial weathering, ozonisation and subsequent leaching was developed to investigate this behaviour in a reproducible and controllable way. The experiments showed a general decline of Zn, polycyclic aromatic hydrocarbons (PAH) and total organic carbon (TOC) concentrations after an initial increase. Within this general trend, the course of concentration over exposure duration is very specific for individual sample materials and the analyte under investigation. The results indicate that weathering and degradation behaviour cannot be predicted from initial material conditions. Thus, weathering experiments are recommended to fill this gap of knowledge. KW - Athletic tracks KW - Artificial turf KW - Ageing KW - Artificial weathering KW - Polymer degradation KW - Rubber granules KW - Leaching KW - Contamination PY - 2017 DO - https://doi.org/10.1016/j.polymertesting.2017.09.021 SN - 0142-9418 SN - 1873-2348 VL - 63 IS - October SP - 621 EP - 631 PB - Elsevier Ltd. CY - Amsterdam, The Netherlands AN - OPUS4-42205 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Linberg, Kevin A1 - Ali, Naveed Zafar A1 - Etter, M. A1 - Michalchuk, Adam A1 - Rademann, K. A1 - Emmerling, Franziska T1 - A Comparative Study of the Ionic Cocrystals NaX (α-d-Glucose)2 (X = Cl, Br, I) N2 - The mechanochemical formation of the ionic cocrystals of glucose (Glc) and sodium salts Glc2NaCl·H2O (1) and Glc2NaX (X = Br (2), I (3)) is presented. Products are formed by co-milling Glc with three sodium salts (NaCl, NaBr, NaI). The ionic cocrystals were obtained under both neat grinding and liquid-assisted grinding conditions, the later found to accelerate the reaction kinetics. The crystal structures of the ionic cocrystals (2) and (3) were solved from powder X-ray diffraction data. The structure solution contrasts with the structure of Glc2NaCl·H2O (1) where the electron density at three halide crystallographic sites is modeled as of being the intermediate between water molecule and a chloride ion. The reaction pathways of the three ionic cocrystals were investigated in real time using our tandem approach comprising a combination of in situ synchrotron powder X-ray diffraction and Raman spectroscopy. The results indicate the rapid formation of each cocrystal directly from their respective starting materials without any intermediate moiety formation. The products were further characterized by DTA-TG and elemental analysis. KW - In situ KW - Co-crystal KW - Mechanochemistry KW - Glucose PY - 2019 DO - https://doi.org/10.1021/acs.cgd.8b01929 VL - 19 IS - 8 SP - 4293 EP - 4299 PB - ACS Publications AN - OPUS4-48781 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tumanov, I. A1 - Tumanov, E. A1 - Michalchuk, Adam T1 - Ball size or ball mass – what matters in organic mechanochemical synthesis? N2 - Ball mass is an important parameter that is known to have an influence on the outcome of a mechanochemical reaction induced by ball-milling. A standard way of modifying the ball mass is to change the size of the ball made of the same material. In this case, however, a change in mass is accompanied by a simulatneous change in the ball size. It is therefore not possible to disentangle the effects of mass and Surface area in these cases. In the present work we report the results of experiments with specially designed and manufactured balls in which (1) milling ball mass is held constant, but their size differs, and (2) the ball mass is altered, with the diameter of the milling ball being held constant. Using the cocrystallisation of theophylline + nicotinamide as a case study it was found that both diameter and ball mass play crucial roles in determining the rate of a mechanochemical reaction. For comparison, we have also used milling balls with the same size (different mass), and others with the same mass (different size) made of different materials, as would be “traditional”. It was found that, despite having the same size, the lightest milling ball (nylon) was the most efficient in initiating the co-crystallisation, presumably due to the sorption of EtOH. Hence, the results of this manuscript also demonstrate how milling ball material can in fact be the most influential parameter, and potentially counterintuitive to classical mechanics. KW - Mechanochemistry KW - XRD PY - 2019 DO - https://doi.org/0.1039/c8ce02109k VL - 21 SP - 2174 EP - 2179 PB - RSC Royal Society of Chemistry AN - OPUS4-47851 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Elastomere und TPE – Gut für die Umwelt? – Kreislaufwirtschaft und Normung vereinen N2 - Der Vortrag fasst Projekte an der BAM mit Hinblick auf Elastomere und Umweltthemen zusammen. T2 - DIN Workshop: Elastomere und TPE – Gut für die Umwelt? – Kreislaufwirtschaft und Normung vereinen CY - Berlin, Germany DA - 08.08.2019 KW - Mikroplastik KW - Reifenabrieb KW - Sportböden PY - 2019 AN - OPUS4-49064 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Becker, C. A1 - Michalchuk, Adam A1 - Linberg, Kevin A1 - Paulus, B. A1 - Emmerling, Franziska T1 - Tuning the Apparent Stability of Polymorphic Cocrystals through Mechanochemistry N2 - Mechanochemistry has become a valuable method for the synthesis of new materials and molecules, with a particular strength for screening and preparing multicomponent crystals. In this work, two novel cocrystals of pyrazinamide (PZA) with pimelic acid (PA) were prepared mechanochemically. Their formation was monitored in real time by in situ synchrotron powder X-ray diffraction. Control over the polymorphic form was obtained through the selective choice of liquid additive via liquid assisted grinding. Slurry experiments and dispersion-corrected density functional theory calculations suggest that Form I is the thermodynamically stable form under ambient conditions. Upon aging, Form II converts to Form I. The stability of Form II upon aging was found to depend strongly on the milling duration, intensity, and material of the milling vessels. Longer or higher energy milling drastically increased the lifetime of the Form II product. For the first time, this work also demonstrates that the choice of milling jar can have a decisive effect on the aging stability of a bulk polymorphic powder. In contrast to material prepared in steel milling vessels, the preparation of Form II in Perspex (PMMA) vessels increased its lifetime 3-fold. These findings offer a new dimension to garnering control over mechanochemical cocrystallization and demonstrate the critical importance of the careful and timely ex situ screening of ball mill grinding reactions. This will be of importance for potential industrial applications of mechanochemical cocrystallization where understanding polymorph longevity is crucial for the development of a robust preparative protocol. KW - Physical and chemical processes KW - Organic compounds KW - Liquids KW - Materials KW - Stability PY - 2019 DO - https://doi.org/10.1021/acs.cgd.9b01158 VL - 19 IS - 12 SP - 7271 EP - 7279 PB - ACS Publications AN - OPUS4-50281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Mikroplastik an der BAM: TED-GC/MS und Referenzmaterialien N2 - Thema ist die Funktionsweise der TED-GC/MS als Methode für die Mikroplastik-Detektion sowie die Herstellung dazugehöriger Referenzmaterialien an der BAM T2 - 25. Kolloquium Massenspektrometrie von Polymeren CY - Online meeting DA - 17.06.2021 KW - Mikroplastik KW - TED-GC/MS KW - Referenzmaterial PY - 2021 AN - OPUS4-52835 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dittmann, Daniel T1 - Aktivkohle-Charakterisierung als weiterer Schlüssel für das Verständnis der Spurenstoffadsorption in der 4. Reinigungsstufe N2 - Aktivkohle ≠ Aktivkohle, Adäquate Materialcharakterisierung - Voraussetzung für Adsorptionsprognosen und Wasserspezifische Auswahl von Aktivkohleprodukten. Ausblick: Publikationen zu Aktivkohlecharakterisierung und Adsorptionsprognose in Vorbereitung T2 - Wasser 2021 - Jahrestagung der Wasserchemischen Gesellschaft CY - Online meeting DA - 10.05.2021 KW - Aktivkohle KW - Thermogravimetrie KW - Zersetzungsgasanalyse KW - Proximatanalyse PY - 2021 AN - OPUS4-52742 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Susset, Bernd A1 - Kalbe, Ute T1 - Spezifische Herausforderungen bei der PFAS-Elution N2 - Im Teil des Workshops, der sich mit Praxiserfahrungen zu den Elutionsverfahren DIN 19528 und DIN 19529 befasste, wurden spezifische Herausforderungen bei Elutionsuntersuchungen von Bodenproben mit einer PFAS-Kontamination vorgestellt. Aus durchgeführten Robustheitsuntersuchungen im ZAG der Universität Tübingen sowie in der BAM wurden praxisrelevante Schlussfolgerungen erläutert und für einzelne PFAS-Verbindungen und Vorläufersubstanzen konkretisiert. Dabei wurde auch auf die Vergleichbarkeit von Schüttel- und Säulenversuchen beim bewertungsrelevanten Wasser/Feststoff-Verhältnis von 2 l/kg und die Bedeutung des Fest/Flüssigtrennschrittes beim Schüttelverfahren eingegangen. Die Untersuchung von Böden auf PFAS mit Elutionsversuchen ist generell möglich, aber es besteht eine komplexe Abhängigkeit der Konzentrationen im Eluat vom Gesamtgehalt, der Löslichkeit und des Verteilungsmusters der einzelnen PFAS, der Art der Bodenmatrix und dem Einfluss der Probenaufbereitung vor der Analytik. Die geringere Sensitivität der Feststoffanalytik für PFAS im Vergleich zur Eluatanalytik erschwert die Berechnung von Massenbilanzen. T2 - Workshop / Anwendertreffen Elutionsverfahren im Regelungsbereich der Mantelverordnung (ErsatzbaustoffV / BBodSchV) und der EU-BauPVO CY - Berlin, Germany DA - 07.05.2024 KW - Elution KW - PFAS KW - Prekursoren KW - Boden KW - Säulenversuch KW - Schüttelversuch PY - 2024 AN - OPUS4-62065 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kalbe, Ute T1 - Ergebnisvergleich Teil 4 – Untersuchung von BM/BG mit und ohne CaCl2-Lösung als Elutionsmittel N2 - Im Teil des Workshops, der sich mit Praxiserfahrungen und Methodenvergleichen zu den Elutionsverfahren DIN 19528 und DIN 19529 befasste, wurden Robustheitsuntersuchungen für die Wahl des Eluenten besonders für Böden mit hohem Humusgehalt und/oder Tongehalt vorgestellt und die Einführung einer neuen Option in die Normen begründet. Der Einsatz 0,001 molarer CaCl2-Lösung als Elutionsmittel führt zu niedrigeren Trübungen im Eluat und reduziert den Aufwand zur Vorbereitung der Eluate für die Folgeanalytik, erleichtert den Fest-Flüssig-Trennschritt bei Schütteleluaten und hat Auswirkungen auf die Mobilisierung/Freisetzungspotenziale bestimmter Analyten, die häufig an Kolloide im Boden binden. T2 - Workshop / Anwendertreffen Elutionsverfahren im Regelungsbereich der Mantelverordnung (ErsatzbaustoffV / BBodSchV) und der EU-BauPVO CY - Berlin, Germany DA - 07.05.2024 KW - Elutionsverfahren KW - Eluent KW - Kolloide PY - 2024 AN - OPUS4-62063 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kalbe, Ute T1 - Robustheit und Validierung der Elutionsnormen N2 - Im Vortrag wurden die den deutschen Elutionsnormen DIN 19528 und DIN 19529 zugrunde liegenden Validierungsdaten erörtert. Dabei wurde auf die Herstellung von Referenzmaterialien durch die BAM, die Vorgehensweise bei den Robustheitsuntersuchungen und die Ableitung der Versuchsbedingungen der Normen erläutert. Die Verfahrenskenndaten aus den durch die BAM veranstalteten Ringversuchen zur Validierung der Elutionsverfahren DIN 19528 und DIN 19527/19529 wurden mit besonderem Focus auf die Vergleichbarkeit von Schüttel- und Säulenversuchen beim bewertungsrelevanten Wasser/Feststoff-Verhältnis von 2 l/kg diskutiert. Des Weiteren wurden Hintergründe für die Überarbeitung der deutschen Elutionsnormen und notwendige Angleichung an die zukünftige harmonisierte europäische Säulenversuchsnorm im Bereich Bauprodukte beleuchtet. T2 - Workshop / Anwendertreffen Elutionsverfahren im Regelungsbereich der Mantelverordnung (ErsatzbaustoffV / BBodSchV) und der EU-BauPVO CY - Berlin, Germany DA - 07.05.2024 KW - Elutionsverfahren KW - Robustheitsuntersuchungen KW - Validierung KW - Ringversuche KW - Verfahrenskenndaten PY - 2024 AN - OPUS4-62061 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Qualitätssicherung bei der Analyse von Mikroplastik per TED GC/MS N2 - Die Thermo Extraktion Desorption Gas Chromatograpie Massen Spektrometrie (TED-GC/MS) ist ein schnelles thermoanalytisches Verfahren zur Bestimmung von Gehalten an Mikroplastik (MP). Die Kombination aus teils schwerflüchtigen Analyten und Kältebrücken führt zu Memory-Effekten, denen u.a. durch häufige Blindwertmessungen begegnet werden muss. Reduzierte Probedurchsätze sind die Folge. Um Messergebnisse abzusichern und den Gerätestatus bei gleichzeitig hoher Messleistung überwachen zu können, wurde die sequentielle Standardmethode überarbeitet. T2 - Tagung der Wasserchemischen Gesellschaft 2022 CY - Online meeting DA - 23.05.2022 KW - Mikroplastik KW - Thermoanalytik KW - TED-GC/MS KW - Qualitätssicherung PY - 2022 AN - OPUS4-55087 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Harmonisation efforts of the CUSP projects N2 - The talk is about harmonisation approaches within CUSP. First the five H2020 projects for research on risk assessment regarding microplastics topic were presented. Secondly, harmonisation process were discussed. T2 - VAMAS SC 47 Meeting CY - Turin, Italy DA - 19.10.2022 KW - Microplastics KW - Harmonisation KW - Nanoplastics KW - H2020 KW - Risk assessment PY - 2022 AN - OPUS4-56077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Musyanovych, A. T1 - Polymeric Capsules with VOCs for Controlled Emission N2 - Micro-(nano-)encapsulation technology involves building a barrier between the core and the environment and offers several benefits to preserve the functional and physicochemical properties of core material. Tremendous progress has been made in synthesizing well-defined capsules to achieve desired properties such as particle size, chemical composition, and controlled release of loaded compounds. Encapsulation of volatile organic compounds (VOCs) that could evaporate with a defined rate is of immense interest for application in emission reference materials (ERM). These are urgently needed for quality assurance and quality control purposes (QA/QC) required by test standards for the determination of chemical emissions of construction and other materials for interior use. As such ERMs are hardly available on the market, the EU-funded EMPIR project MetrIAQ was started to fill this gap by developing a material with temporally constant emission of VOCs typically found in indoor air. T2 - 36th European Colloid & Interface Society Conference CY - Chania, Crete, Greece DA - 04.09.2022 KW - Capsules KW - Volatile organic compounds KW - Material emissions KW - QA/QC KW - Reference materials PY - 2022 AN - OPUS4-55917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bauer, J. A1 - Miclea, P.-T. A1 - Braun, U. A1 - Altmann, Korinna A1 - Turek, M. A1 - Hagendorf, C. T1 - Microplastic detection and analysis in water samples N2 - Microplastic detection in water samples becomes important for tracing microplastic sources. Microplastic may harm desalination facilities by blocking filters and disturbing the marine food chain. Thermo analytical methods such as pyrolysis gas chromatography mass spectroscopy, and spectroscopic methods like (micro) Raman spectroscopy or (micro) Fouriertransform infrared spectroscopy in combination with appropriate filters and sample preparation are suitable for analyzing microplastics on a scale from 1 µm to 1000 µm fast and unambiguous. While the thermo analytical methods are suitable for larger sample volumes, Raman spectroscopy and Fouriertransform infrared spectroscopy are able to detect and analyze single microplastic particles for instance in bottled water. Machine learning algorithms ensure a reliable classification of different plastic materials. T2 - International Conference on Sustainable Energy-Water-Environment Nexus in Desert Climate 2019 CY - Ar-Rayyan, Qatar DA - 02.12.2019 KW - Microplastics KW - Water samples PY - 2022 SP - 111 EP - 113 PB - Springer AN - OPUS4-56240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grimmer, Christoph T1 - Constant emitting reference material for material test procedures N2 - In industrialised countries more than 80% of the time is spent indoors. Products, such as building materials and furniture, emit volatile organic compounds (VOCs), which are therefore ubiquitous in indoor air. VOC in combination may, under certain environmental and occupational conditions, result in reported sensory irritation and health complaints. Emission concentrations can become further elevated in new or refurbished buildings where the rate of air exchange with fresh ambient air may be limited due to improved energy saving aspects. A healthy indoor environment can be achieved by controlling the sources and by eliminating or limiting the release of harmful substances into the air. One way is to use (building) materials proved to be low emitting. Meanwhile, a worldwide network of professional commercial and non-commercial laboratories performing emission tests for the evaluation of products for interior use has been established. Therefore, comparability of test results must be ensured. A laboratory’s proficiency can be proven by internal and external validation measures that both include the application of suitable emission reference materials (ERM). For the emission test chamber procedure according to EN 16516, no artificial ERM is commercially available. The EU-funded EMPIR project MetrIAQ aims to fill this gap by developing new and improved ERMs. The goal is to obtain a material with a reproducible and temporally constant compound release (less than 10% variability over 14 days). Different approaches, such as the impregnation of porous materials, are being tested. The generation as well as results of the most promising materials will be presented. T2 - Airmon 2022 CY - Bristol, UK DA - 07.11.2022 KW - Emission reference materials KW - Emission test chamber procedure KW - Quality assurance KW - Reference material PY - 2022 AN - OPUS4-56575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Detektion von Mikroplastik N2 - In dem Vortrag geht es um die Möglichkeiten der Detektion von Mikroplastik im Allgemeinen. Es werden Beispiele für die Luft gezeigt. T2 - VDI-Workshop „Mikroplastik in der Außenluft – Was wir wissen und was wir (noch) nicht wissen CY - Online meeting DA - 15.11.2022 KW - Mikroplastik KW - Mikroplastik in Luft KW - Detektion von Mikroplastik PY - 2022 AN - OPUS4-56289 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, U. T1 - Thermoanalytical methods to measure mass in microplastics N2 - The talk adresses the use of thermoanalytical methods in microplastics analysis. T2 - EUROLAB webinar: MICROPLASTICS: regulations, standards and the role of laboratories CY - Online meeting DA - 15.02.2023 KW - TED-GC/MS KW - Thermoanalytical methods KW - Microplastic mass PY - 2023 AN - OPUS4-57009 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Stakeholder Workshop – Plastictrace WP1 N2 - The talk is about WP1 in the PlasticTrace project funded by Euromat. The projects harmonizes microplastic analysis by developing SOPs and reference materials. WP1 is responsible for material selection and preparation. All particles are homogeneity and stability checked according to ISO guide 35. T2 - Stakeholder workshop of PlasticTrace project CY - Online meeting DA - 14.12.2022 KW - Microplastic KW - Microplastics standardisation KW - Reference materials PY - 2022 AN - OPUS4-56772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Altmann, Korinna A1 - Abusafia, A A1 - Bannick, C-G A1 - Braun, U A1 - Crasselt, Claudia A1 - Dittmar, S A1 - Fuchs, M A1 - Gehde, M A1 - Hagendorf, C A1 - Heller, C A1 - Herper, D A1 - Heymann, S A1 - Kerndorff, A A1 - Knefel, M A1 - Jekel, M A1 - Lelonek, M A1 - Lunkenbein, T A1 - Obermaier, N A1 - Manhart, M A1 - Meurer, Maren A1 - Miclea, P-T A1 - Paul, A A1 - Richter, S A1 - Ricking, M A1 - Rohner, C A1 - Ruhl, A A1 - Sakai, Y A1 - Saravia Arzabe, C A1 - Scheid, C A1 - Schmitt, M A1 - Schnarr, M A1 - Schwertfirm, F A1 - Steinmetz, H A1 - Wander, Lukas A1 - Wiesner, Yosri A1 - Zechmeister, L T1 - RUSEKU - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt : Abschlussbericht N2 - Im Verbundprojekt RUSEKU wurde die Probenahme von Wasserproben entscheidend weiterentwickelt. Wichtig ist hierbei zu gewährleisten, dass genügend Merkmalsträger in jeder Probe untersucht werden. Es muss daher eine für den Probenahmeort repräsentative Beprobung hinsichtlich des Wasservolumens in Abhängigkeit der Partikelanzahl gewährleistet sein. Das Hauptaugenmerk lag im vorliegenden Projekt auf einer praxisnahen Beprobungsstrategie. Es wurden verschiedene Konzepte ausprobiert. • Grundsätzlich hat sich gezeigt, dass eine Stichprobe eine Momentaufnahme des MP-Massengehaltes zeigt. Es wird eine hohe Statistik, also eine Vielzahl an Messungen am gleichen Probenahmeort, benötigt, um eine valide Aussage über den MP-Gehalt zu machen. • Es zeigt sich, dass eine integrale Probenahme über mehrere Wochen mit dem SK routinemäßig möglich ist. Die erfassten MP-Massen sind reproduzierbar und robust. • Die DFZ ist für Stichproben geeignet. Partikel < 50 µm werden eventuell unterschätzt • Die fraktionierte Filtration kann für Stich- und Mischproben direkt im Feld genutzt werden. Fraktionen von 10 und 5 µm werden später im Labor Vakuum filtriert. Es erfolgt eine Fraktionierung der Probe mit Siebmaschenweiten von 1000, 500, 100, 50, 10 und 5 µm. • Die fraktionierte Filtration kann auch anschließend an die Beprobung mit dem SK zur Anwendung kommen. Wird die mit dem SK gewonnene Wasserprobe fraktioniert filtriert, kann neben einem MP-Gesamtgehalt auch eine Einschätzung über die Partikelgrößen gewonnen werden. • Für Wässer mit geringen Partikelzahlen wurde ein Messfiltertiegel entwickelt. Dieser hat eine Maschenweite von 6 µm. Seine Anwendung kann mögliche Verluste beim Transferieren vom Probenahmetool zum Messgefäß und mögliche Kontaminationen reduzieren. Die Optimierung der Probenahmestrategie wurde durch Modellversuche und Simulationen unterstützt. Modellversuche zum Sinkverhalten und Simulationen von MP in realen Gewässern verdeutlichten das komplexe Verhalten der Partikel. Es konnte gezeigt werden, dass Partikel ab einer bestimmten Größe (und kleiner) bei genügend starker Turbulenz sich in der Wassersäule unabhängig von ihrer Dichte verhalten und so auch MP mit kleiner Dichte (z.B. PE) in der gesamten Wassersäule zu finden sind. Es konnte mit dem TEM die Existenz von NP gezeigt werden. Ein wesentlicher Aspekt des RUSEKU Projektes war die Beprobung realer Kompartimente. Beprobt wurde neben Oberflächengewässern, das urbane Abwassersystem der Stadt Kaiserslautern, Waschmaschinenabwasser und Flaschenwasser. • In Oberflächengewässern wurde hauptsächlich PE gefunden. Je nach Probe und Gewässer konnten auch PP, PS, PET, PA, SBR und Acrylate nachgewiesen werden. • Im urbanen Abwassersystem der Stadt Kaiserslautern konnte an allen Probenahmestandorten MP nachgewiesen werden. Es wurde hauptsächlich PE, neben geringeren Mengen an PP, PS und SBR gefunden. Nach einem Regenereignis war der SBR Anteil deutlich erhöht. • Die Beprobung eines realen Wäschepostens, bestehend aus T-Shirts und Hemden mit PA/CO oder PES/CO Mischgewebe, zeigte einen PA- und PES-Austrag im Waschwasser. Der überwiegende Teil der detektierten Fasern ist aber auf Baumwolle zurückzuführen. Reine gravimetrische Messungen zur Detektion von MP führen zu einer starken Überschätzung. • In Flaschenwasser (PET-Flaschen) konnte MP detektiert werden. PET wurde nur im stillen Mineralwasser, nicht in Mineralwasser mit Kohlensäure gefunden werden. Teilweise wurde auch das MP-Material des Verschlusses im Wasser detektiert. • Für Luftproben konnte ein Aufbau zur größenselektiven Beprobung getestet werden. Neben der Probenahme hat das Projekt auch gezeigt, dass die TED-GC/MS geeignet für die MP-Detektion im Routinebetrieb ist. Die TED-GC/MS konnte weiter optimiert werden. Es wurden MP-Massen bestimmt. Im Projekt wurden erste realitätsnahe Referenzmaterialien für die MP Detektion hergestellt. Die Herstellung von realitätsnahen Polymeren in ausreichender Homogenität und Menge hat sich als große Herausforderung herausgestellt. KW - Mikroplastik KW - Probennahme KW - TED-GC/MS KW - Fraktionierte Filtration KW - Mikroplastikreferenzmaterial PY - 2022 SP - 1 EP - 201 AN - OPUS4-57800 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmitt, M. A1 - Altmann, Korinna A1 - Fengler, Petra A1 - Gehde, M. T1 - Air-based polyethylene fragmentation with high yield to form microplastic particles as reference material candidates N2 - Microplastic particles with sizes between 1 to 1000 μm are widely distributed worldwide. Origin, transport pathways and fate are poorly known, as sampling, sample preparation and detection methods are major challenges. In addition, reference materials that mimic environmental particles are lacking. Most challenging is the yield of MP particle production and the need for resource-intensive grinding with liquid nitrogen. In this paper, a machine is designed to produce aged microplastic particles as reference material candidates with high yield. The machine is based on ultraviolet aging of a thin foil and mechanical fragmentation using clean air. An example of aging and fragmentation of high density polyethylene with additional physical and chemical characterization of shape, size, aging state by carbonyl index and density is presented. KW - Microplastics KW - Degradation of polyethylene KW - Air fragmentation KW - Microplastics reference material PY - 2023 DO - https://doi.org/10.1002/appl.202200121 SP - 1 EP - 18 PB - Wiley online library AN - OPUS4-57203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wiesner, Yosri T1 - Erfassung von Degradationsprodukten und Additiven sowie temperaturspezifische Pyrolyseprodukte mittels TED-GC/MS N2 - Im der Präsentation werden, neben der Möglichkeit der Mikroplastikquantifizierung, auf weitere Anwendungsfelder der Methode TED-GC/MS eigegangen. Dies beinhaltet die Erfassung von Degradationsprodukten UV/O2 geschädigter Polymere und die Detektion von Additiven. Die Optimierung der Methode betreffend Messzeit und materialspezifischer Messanforderung sind ebenfalls Gegenstand. T2 - Kolloquium Massenspektrometrie von Polymeren CY - Berlin, Germany DA - 09.05.2023 KW - TED-GC/MS KW - Polymere KW - Degradation KW - Additive PY - 2023 AN - OPUS4-57480 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Improvements in micro- & nanoplastic mass detection by TED-GC/MS N2 - Introduction to microplastics, definition, relevance, analytical approaches & challenges. TED-GC/MS working principle, features & performance. Optimisation in TED-GC/MS methodology, new validation data. Replacement of Internal Standard, outlook towards upcoming publication and application within EU´s revised drinking water directive. T2 - SETAC 2023 CY - Dublin, Ireland DA - 01.05.2023 KW - Microplastics KW - Thermoanalytics KW - Validation KW - Internal Standard PY - 2023 AN - OPUS4-57421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Miclea, P.-T. T1 - Real-life airborne micro- and nano-plastic particles and fibres on a porous membrane filter system from a textile factory suitable for both: vibrational and mass spectrometry N2 - The poster presents an application of Si wafer filter system on indoor air sampling. A textile factory producing PP fibres was sampled. T2 - SETAC Europe 2023 CY - Dublin, Ireland DA - 30.04.2023 KW - Microplastics KW - Polymer 3R KW - Textile fibres KW - Si wafer filter KW - Microplastics sampling PY - 2023 AN - OPUS4-57462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wiesner, Yosri A1 - Bednarz, Marius A1 - Braun, Ulrike A1 - Bannick, Claus Gerhard A1 - Ricking, Mathias A1 - Altmann, Korinna T1 - A promising approach to monitor microplastic masses in composts N2 - Inputs of plastic impurities into the environment via the application of fertilizers are regulated in Germany and the EU by means of ordinances. Robust and fast analytical methods are the basis of legal regulations. Currently, only macro- and large microplastic contents (>1 mm) are measured. Microplastics (1–1,000 µm), are not yet monitored. Thermal analytical methods are suitable for this purpose, which can determine the mass content and can also be operated fully automatically in routine mode. Thermal extraction desorption-gas chromatography/mass spectrometry (TED-GC/MS) allows the identification of polymers and the determination of mass contents in solid samples from natural environments. In accordance with the German or European Commission (EC) Fertiliser Ordinance, composting plants should be monitored for microplastic particles with this method in the future. In this context a compost plant was sampled. At the end of the rotting process, the compost was sieved and separated in a coarse (>1 mm) and a fine fraction (<1 mm). The fine fraction was processed using density separation comparing NaCl and NaI as possible salt alternative and screened for microplastic masses by TED-GC/MS with additional validation and quality assurance experiments. With TED-GC/MS total microplastics mass contents of 1.1–3.0 μg/mg in finished compost could be detected with polyethylene mainly. What differs much to the total mass of plastics in the coarse fraction with up to 60 μg/mg, which were visually searched, identified via ATR-FTIR and gravimetrically weighted. KW - Microplastics KW - TED-GC/MS KW - Compost KW - Monitoring KW - Soil PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586688 DO - https://doi.org/10.3389/fenvc.2023.1281558 SN - 2673-4486 VL - 4 SP - 1 EP - 12 PB - Frontiers Media CY - Lausanne AN - OPUS4-58668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Mikroplastik Detektion mit Thermoanalytischen Methoden: Analytik, Referenzmaterial, Ringversuche N2 - Ich dem Vortrag geht es um die Vorstellung von thermoanalytischen Methoden für die Mikroplastik-Detektion. Verschiedene Kopplungsmöglichkeiten werden gezeigt und die Funktionsweise der TED-GC/MS wird erklärt. Im zweiten Teil werden Referenzmaterialien für die Mikroplastik-Analytik diskutiert. PET -Tabletten des PlasticTrace Projektes werden vorgestellt. Am Ende wird der VAMAS Ringversuch zur Mikroplastik-Detektion gezeigt. T2 - Plastik, Mikroplastik, Nanopartikel, PFAS und Verunreinigungen (Agilent Workshop) CY - Hamburg, Germany DA - 28.05.2024 KW - Mikroplastik KW - TED-GC/MS KW - Polymer 3R KW - Ringversuche KW - Referenzmaterial PY - 2024 AN - OPUS4-60155 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Preliminary results of an interlaboratory comparison on microplastics organised by plasticsfate N2 - Microplastics are everywhere in the environment, but analytics is challenging. Since harmonisation is missing as well es suitable reference materials, BAM did under th umbrella of VAMAS funded by the EU Horizon 2020 project PlasticsFate a ILC for microplastic detection methods. Methods adressed were IR, Raman, Py-GC/MS and TED-GC/MS. The talk gives a first presentation and evaluation on the results. T2 - CUSP annual meeting and conference CY - Utrecht, Netherlands DA - 12.09.2023 KW - Microplastics KW - TED-GC/MS KW - Polymer 3R KW - Reference material KW - ILC on detection methods PY - 2023 AN - OPUS4-60036 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Béalu, Zoé A1 - Walther, Johanna A1 - Abusafia, Attaallah A1 - Altmann, Korinna A1 - Meurer, Maren A1 - Gretzschel, Oliver A1 - Schäfer, Michael A1 - Steinmetz, Heidrun T1 - Removal of Organic Micropollutants and Microplastics via Ozonation Followed by Granular Activated Carbon Filtration N2 - Discharge from Wastewater Treatment Plants (WWTPs) can result in the emission of organic micropollutants (OMPs) and microplastics (MPs) into the aquatic environment. To prevent this harmful release, a pilot plant consisting of an ozonation followed by a granular activated carbon (GAC) filter was operated at a WWTP in Germany, and its side-effects on the concentrations of nitrogen (N) and phosphorous (P) compounds were measured. Over 80% of OMPs and transformation products were removed during the operating time (around 6000 bed volumes) no matter the ozone dose (from around 0.1 to 0.5 mgO3/mgDOC), except for Diatrizoic acid, whose breakthrough appeared at 3500 BV. Formation of the oxidation by-product, NDMA, increased with higher ozone doses, but the concentration remained below 100 ng/L. Bromate was formed at a higher ozone dose (0.4 mgO3/mgDOC) but at a low concentration—below 10 µg/L. The MP particles detected in the inflow (PE, SBR, PP, and PS) were effectively eliminated to a high degree, with a removal rate of at least 92%. Carbon parameters (COD, DOC, and SAC254) were removed further by the pilot plant, but to different extents. As expected, nitrate was formed during ozonation, while nitrite’s concentration decreased. Further, nitrite decreased and nitrate increased within the GAC filter, while ammonium was eliminated by at least 90%. Total P concentration decreased after the pilot, but the concentration of PO4-P increased. KW - Microplastics KW - TED-GC/MS KW - Granular Activated Carbon Filtration KW - Removal of Organic Micropollutants KW - Wastewater treatment plant PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615209 DO - https://doi.org/10.3390/environments11110241 VL - 11 IS - 11 SP - 1 EP - 38 PB - MDPI AG AN - OPUS4-61520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Mikroplastik heute: Was haben wir in den letzten Jahren erreicht? N2 - In diesem Vortrag geht es um eine Übersicht über die Thematik der Mikroplastik, Was ist Mikroplastik, wie entsteht es und wo kommt es her. Es wird beschrieben wie eine repräsentative Probenahme erfolgen kann und wie welche Herausforderungen bei der Probenvorbereitung existieren. Die Detektion wird ausführlich beschrieben, sowohl mit Partikelanzahl als auch Masse. Im weiteren werden erste Referenzmaterialien und ihre Anwendung in internationalen Ringversuchen beschrieben. Der zweite Teil zeigt die Normungsaktivitäten im Bereich der Mikroplastik. T2 - Mitgliederversammlung der GdCh Lackchemie CY - Online Meeting DA - 20.09.2024 KW - Mikroplastik KW - TED-GC/MS KW - Polymer 3R KW - Reference material KW - ILC on detection methods PY - 2024 AN - OPUS4-61087 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Thermal desoprtion analysis of hydrogen trapping in micro-alloyed high strength steels N2 - Hydrogen can cause unexpected material failure under consideration of stresses (external/internal) during manufacturing, processing or service of the materials. This failure is mostly based on a certain degradation of the mechanical properties. Thus, the correlation of hydrogen trapping vs. a respective microstructure is necessary for high strength steels. Thus, the scope of this work is the improvement of existing hydrogen trap models by verification of activation energies for hydrogen traps as well as the influence of the determination method. In this scope, the thermal desorption method is appropriate to distinguish between different hydrogen traps. Nevertheless, the specimen temperature has to be accounted very carefully in case of calculating the necessary trap energy. T2 - IIW Intermediate Meeting, Meeting of commission II-A CY - Madrid, Spain DA - 29.02.2016 KW - Thermal desorption analysis (TDA) KW - Hydrogen trapping KW - High strength steels KW - Degradation KW - Heat treatment condition PY - 2016 AN - OPUS4-35544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kruschwitz, Sabine A1 - Prinz, Carsten A1 - Zimathies, Annett T1 - Study into the correlation of dominant pore throat size and SIP N2 - There is currently a debate within the SIP community about the characteristic textural length scale controlling relaxation time of consolidated porousmedia.One idea is that the relaxation time is dominated by the pore throat size distribution or more specifically the modal pore throat size as determined in mercury intrusion capillary pressure tests. Recently new studies on inverting pore size distributions from SIP data were published implying that the relaxation mechanisms and controlling length scale are well understood. In contrast new analytical model studies based on the Marshall-Madden membrane polarization theory suggested that two relaxation processes might compete: the one along the short narrow pore (the throat) with one across the wider pore in case the narrow pores become relatively long. This paper presents a first systematically focused study into the relationship of pore throat sizes and SIP relaxation times. The generality of predicted trends is investigated across a wide range of materials differing considerably in chemical composition, specific surface and pore space characteristics. Three different groups of relaxation behaviors can be clearly distinguished. The different behaviors are related to clay content and type, carbonate content, size of the grains and the wide pores in the samples. KW - Textural controls KW - Spectral induced polarization KW - Relaxation time KW - Pore throat size KW - Consolidated materials KW - Membrane polarization PY - 2016 DO - https://doi.org/10.1016/j.jappgeo.2016.07.007 VL - 135 SP - 375 EP - 386 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-40346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bungartz, M. A1 - Maenz, S. A1 - Kunisch, E. A1 - Horbert, V. A1 - Xin, L. A1 - Gunella, F. A1 - Mika, J. A1 - Borowski, J. A1 - Bischoff, S. A1 - Schubert, H. A1 - Sachse, A. A1 - Günster, Jens A1 - Illerhaus, Bernhard A1 - Bossert, J. A1 - Jandt, K. D. A1 - Kinne, R. W. A1 - Brinkmann, O. T1 - First-time systematic postoperative clinical assessment of a minimally invasive approach for lumbar ventrolateral vertebroplasty in the large animal model sheep N2 - Large animal models are highly recommended for meaningful preclinical studies, including the optimization of cement augmentation for vertebral body defects by vertebroplasty/kyphoplasty. The aim of this study was to perform a systematic characterization of a strictly minimally invasive in vivo large animal model for lumbar ventrolateral vertebroplasty. This is a prospective experimental animal study. Lumbar defects (diameter 5 mm; depth approximately 14 mm) were created by a ventrolateral percutaneous approach in aged, osteopenic, female sheep (40 Merino sheep; 6–9 years; 68–110 kg). L1 remained untouched, L2 was left with an empty defect, and L3 carried a defect injected with a brushite-forming calcium phosphate cement (CPC). Trauma/functional impairment, surgical techniques (including drill sleeve and working canula with stop), reproducibility, bone defects, cement filling, and functional cement augmentation were documented by intraoperative incision-to-suture time and X-ray, postoperative trauma/impairment scores, and ex vivo osteodensitometry, microcomputed tomography (CT), histology, static/fluorescence histomorphometry, and biomechanical testing. Minimally invasive vertebroplasty resulted in short operation times (28±2 minutes; mean±standard error of the mean) and X-ray exposure (1.59±0.12 minutes), very limited local trauma (score 0.00±0.00 at 24 hours), short postoperative recovery (2.95±0.29 hours), and rapid decrease of the postoperative impairment score to 0 (3.28±0.36 hours). Reproducible defect creation and cement filling were documented by intraoperative X-ray and ex vivo conventional/micro-CT. Vertebral cement augmentation and osteoconductivity of the CPC was verified by osteodensitometry (CPC>control), micro-CT (CPC>control and empty defect), histology/static histomorphometry (CPC>control and empty defect), fluorescence histomorphometry (CPC>control; all p<.05 for 3 and 9 months), and compressive strength measurements (CPC numerically higher than control; 102% for 3 months and 110% for 9 months). This first-time systematic clinical assessment of a minimally invasive, ventrolateral, lumbar vertebroplasty model in aged, osteopenic sheep resulted in short operation times, rapid postoperative recovery, and high experimental reproducibility. This model represents an optimal basis for standardized evaluation of future studies on vertebral augmentation with resorbable and osteoconductive CPC. KW - Computed tomography KW - Calcium phosphate cement KW - Large animal model KW - Minimal-invasive KW - Vertebroplasty KW - Void defect PY - 2016 UR - http://www.sciencedirect.com/science/article/pii/S152994301630273X DO - https://doi.org/10.1016/j.spinee.2016.06.015 VL - 16 IS - 10 SP - 1263 EP - 1275 PB - Elsevier Inc. AN - OPUS4-38429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beyer, Sebastian A1 - Prinz, Carsten A1 - Schürmann, Robin A1 - Feldmann, Ines A1 - Zimathies, Annett A1 - Blocki, Anna A1 - Bald, Ilko A1 - Schneider, Rudolf A1 - Emmerling, Franziska T1 - Ultra-sonication of ZIF-67 crystals results in ZIF-67 nano-flakes N2 - Zeolitic Imidazolate Frameworks (ZIFs) are crystalline materials that comprise of metal nodes and Imidazole derivatives as linkers. ZIF-67 is often used in polymer composite materials e. g. for gas separation membranes. Post-synthesis treatment of ZIF-67 crystals with ultrasound leads to unforeseen plasticity that resulted in sintered ZIF-67 and ZIF-67 nano-flakes. Consequently, ultrasound increases the external surface area of ZIF-67 which might improve e.g. blending with polymers in composite materials. These new morphologies of ZIF-67 were characterized by transmission electron, scanning electron, and atomic force microscopy. The ultrasound treatment of ZIF-67 did not result in the formation of an amorphous framework or a meta-stable crystal structure as indicated by powder x-ray diffraction. In addition, ultra-sonicated ZIF-67 retained the high gas adsorption capacity and pore size compared to synthesized ZIF-67. The morphological changes are hard to detect with standard analytical methods that are usually utilized for MOF characterization. These findings also suggest that sonochemical treatment of ZIFs leads to structural effects beyond increasing the amount of nucleation clusters during sono-chemical synthesis, which is currently not addressed in the field. KW - ZIF PY - 2016 DO - https://doi.org/10.1002/slct.201601513 SN - 2365-6549 VL - 1 IS - 18 SP - 5905 EP - 5908 AN - OPUS4-38496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien A1 - Hasenfelder, Uta A1 - Krebs, Holger A1 - Bruno, Giovanni T1 - Assessment of shock tube systems by synchrotron X-ray computed tomography N2 - Shock tube systems are non-electric explosive fuses employed in blasting and demolition applications to trigger the detonation of explosive charges. Their working principle is based on the explosive reaction of a fine explosive powder on the tubing's inner surface, generating a shock wave traveling at a velocity of 2,100 m/s along the length of the tube, without destroying it. One of the key aspects of the manufacturing process of these shock tubes is the size and morphology of the explosive powder grains and their distribution on the inner wall of the tube, in order to propagate the shockwave efficiently and reliably. For the first time, synchrotron X-ray computed tomography has been used to characterize non-destructively the explosive powder grains, typically Al/HMX between 10 and 20 μm in size, in terms of morphology and 3D distribution but also to characterise the presence and location of defects within the shock tube walls. KW - Explosives KW - Nonel KW - Shock wave KW - Blasting KW - Energetic systems PY - 2017 UR - http://www.ndt.net/events/iCT2017/app/content/Paper/61_Leonard.pdf SP - 1 EP - 7 CY - Leuven, Belgium AN - OPUS4-39345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - Synchrotron X-ray computed tomography for assessment of shock tube systems N2 - Shock tube systems are non-electric explosive fuses employed in blasting and demolition applications to trigger the detonation of explosive charges. Their working principle is based on the explosive reaction of a fine powder on the tubing´s inner surface, generating a percussive wave travelling at a velocity of 2,100 m/s along the length of the tube, without destroying it. One of the key aspects of the manufacturing process of these shock tubes is the size and morphology of the explosive powder grains and their distribution on the inner wall of the tube, in order to propagate the shockwave efficiently and reliably. For the first time, synchrotron X-ray computed tomography has been used to characterize non-destructively the explosive powder grains, typically Al/HMX between 10 and 20 μm in size, in terms of morphology and 3D distribution but also to characterise the presence and location of defects within the shock tube walls. T2 - 7th Conference on Industrial Computed Tomography CY - Leuven, Belgium DA - 07.02.2017 KW - Explosive KW - Nonel KW - Shock wave KW - Blasting KW - Energetic systems PY - 2017 AN - OPUS4-39168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien A1 - Bruno, Giovanni T1 - Evaluating porosity in cordierite diesel particulate filter materials: advanced X-ray and new statistical analysis methods N2 - Complex materials (e.g., porous ceramics) need high resolution techniques at multi-scale levels. Microstructure is intimately linked to properties and performance. One technique (or even a few techniques) is not enough. X-ray refraction and CT are very powerful tools. Non-destructive characterisation and quantitative image analysis techniques (2D and 3D) are necessary to understand the anisotropy. T2 - 40th International Conference and Expo on Advanced Ceramics and Composites ( ICACC) CY - Daytona Beach, USA DA - 24.01.2016 KW - X-ray computed tomography KW - X-ray refraction KW - Directional interface variance analysis (DIVA) KW - FFT periodogram PY - 2016 AN - OPUS4-41725 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine A1 - Halisch, M. A1 - Prinz, Carsten A1 - Weller, Andreas A1 - Müller-Petke, M. A1 - Dlugosch, R. T1 - Towards a better understanding of electrical relaxation N2 - Other than commonly assumed the relaxation times observed in the electrical low-frequency range (1 mHz – 40 kHz) of natural porous media like sandstones and tuff stones cannot be directly related to the dominant (modal) pore throat sizes, measured (e.g.) with mercury intrusion porosimetry (MIP). Working with a great variety of sandstones from very different origins and featuring great variations in textural and chemical compositions as well as in geometrical pore space properties, it was observed that particularly samples with narrow pore throats were characterized by long (low-frequency) relaxations. These, however, can (following the current theories) be rather explained by long “characteristic length scales” in these media or low diffusion coefficients along the electrical double layer. However, there is no straightforward way (or single approved method) of getting reliable numbers for properties such as the lengths of pore throats, the diameter and length of the wide pores and their respective distributions. Consequently we follow a multi-methodical approach and combine the benefits of MIP, micro-computed tomography (μ-CT) and nuclear magnetic resonance (NMR) to achieve much deeper insight due to the different resolutions and sensitivities to either pore constrictions (throats) or wide pores. This helps us to understand, whether the observed electrical relaxation phenomena actually depend on geometric length scales or rather on other properties such as chemical composition, clay content, clay type or cation exchange capacity. In this paper, we showcase selected results of a systematic study of a total of 16 sandstones and three tuffs. Findings and the particular advantage of the used method combination are discussed and shown in detail for a representative sample selection. T2 - Annual Symposium of the Society of Core Analysts (SCA) CY - Vienna, Austria DA - 28.08.2017 KW - Electrical relaxation KW - Complex resistivity KW - Spectral induced polarization KW - Nuclear magnetic resonance KW - Mercury intrusion porosimetry KW - Pore size distribution KW - Sandstone PY - 2017 VL - SCA2017-080 SP - 1 EP - 9 AN - OPUS4-42599 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Absorption and refraction tomography: Characterization and Non-destructive Testing of Micro-structured Materials N2 - The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces. Additionally, I will present a new technique in our portfolio, Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load. T2 - Seminare der EMPA CY - EMPA, Dubenddorf, Switzerland DA - 10.10.2017 KW - Computed Tomography KW - X-ray Refraction KW - Neutron Diffraction KW - Additive Manufacturing KW - Image Analysis PY - 2017 AN - OPUS4-42699 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bayerlein, Bernd T1 - Adopting FAIR data practices in materials science: Semantic representation of a quantitative precipitation analysis N2 - Many metallic materials gain better mechanical properties through controlled heat treatments. For example, in age-hardenable aluminium alloys, the strengthening mechanism is based on the controlled formation of nanometre-sized precipitates, which represent obstacles to dislocation movement and consequently increase the strength. Precise tuning of the material microstructure is thus crucial for optimal mechanical behaviour under service condition of a component. Therefore, analysis of the microstructure, especially the precipitates, is essential to determine the optimum parameters for the interplay of material and heat treatment. Transmission electron microscopy (TEM) is utilized to identify precipitate types and orientations in the first step. Dark-field imaging (DF-TEM) is often used to image the precipitates and thereafter quantify their relevant dimensions. Often, these evaluations are still performed by manual image analysis, which is very time-consuming and to some extent also poses reproducibility problems. Our work aims at a semantic representation of an automatable digital approach for this material specific characterization method under adaption of FAIR data practices. Based on DF-TEM images of different precipitation states of a wrought aluminium alloy, the modularizable, digital workflow of quantitative analysis of precipitate dimensions is described. The integration of this workflow into a data pipeline concept will also be discussed. Using ontologies, the raw image data, their respective contextual information, and the resulting output data of the quantitative image analysis can be linked in a triplestore. Publishing the digital workflow and the ontologies will ensure data reproducibility. In addition, the semantic structure enables data sharing and reuse for other applications and purposes, demonstrating interoperability. T2 - FEMS EUROMAT 2023 CY - Frankfurt a. M., Germany DA - 03.09.2023 KW - Semantic Representation KW - FAIR data management KW - Quantitative Precipitation Analysis KW - Knowledge graph and ontologies PY - 2023 AN - OPUS4-58199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Strategies to use neutrons as an industrial problem-solving tool N2 - For how trivial or provocative it can sound, the best neutron spectrometer in the world does not produce science and technology by itself. By definition of “Materials Science”, neutron scattering data on engineering materials must be used as a tool to understand, and even tailor, materials performance. In order for this to happen, neutron data need to be 1. Acquired under the most relevant condition possible 2. Coupled to other experimental techniques 3. Capitalized by means of proper simulations and data analysis Point 1- calls for an intense use and the development of top-notch of in-situ techniques; Point 2- means that the sole use of neutron data will not lead to any solution of a global problem; All points above hint to the fact that access to neutron sources is not routine, and therefore it is imperative to search ways to make neutron data rentable and sustainable for the material science and industrial research community. In this presentation, and based on two examples, we will show a couple of strategies to combine neutron data with other experiments, and with theoretical models to raise the validity of experiments to the level of problem-solving. As one might imagine, these are only a few among the almost infinite combinations possible to help improving material properties, performance, and safety, i.e., ripe for everyday use. T2 - MORIS Workshop CY - Garching, Germany DA - 26.04.2023 KW - Neutron Diffraction KW - Residual Stress KW - Large Scale Facilities KW - X-ray Computed Tomography PY - 2023 AN - OPUS4-57361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - A machine-learning based data fusion approach for improved corrosion damage monitoring N2 - Half-cell potential mapping (HP) is the most popular nondestructive test (NDT)-method for the localization of corrosion damage in concrete. It is generally recognized, that HP is prone to the environmental factors that arise from salt induced deterioration, such as varying moisture and chloride gradients. Additional NDT-methods are capable to determine distinctive areas, but cannot yet be used to estimate more accurate testing results. We introduce a supervised machine learning (SML) based approach for data fusion to make use of the additional sensor information. SML are methods that explore relations between different (sensor) data from predefined data labels. We use a simple linear classifier named logistic regression to distinguish defect and intact areas. The test performance improves drastically compared to the best single method, HP. In order to generate representative, labeled data we conducted a comprehensive experiment that simulates the deterioration-cycle of a chloride-exposed building part in the lab. Our data set consist of 18 measurement campaigns, each containing HP-, ground-penetrating-radar-, microwave-moisture-, and Wenner-resistivity-data. We detail the challenges that arise with a data driven approach in NDT and how we addressed them. T2 - NDE2017 CY - Chennai, India DA - 14.12.2017 KW - Data fusion KW - NDT KW - Concrete KW - Corrosion KW - Machine learning PY - 2017 AN - OPUS4-44101 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cabeza, Sandra A1 - Cawley, P. A1 - Li, Z. A1 - Dixon, S. A1 - Jarvis, R. A1 - Nagy, P. B. T1 - Experimental studies of the magneto-mechanical memory (MMM) technique using permanently installed magnetic sensor arrays N2 - The magneto-mechanical memory (MMM) method, that is often referred to as the metal magnetic memory method, has been reported to be a non-destructive testing technique capable of quantifying stress concentrations and detecting defects in ferromagnetic materials. The underlying mechanism behind MMM has been explained in the literature, but the sensitivity to stress concentration has not been satisfactorily investigated. In this paper, both the normal and tangential components of the stress-induced MMM signal were measured by permanently installed magnetic sensor arrays on specimens made from three grades of L80 alloy steel and 20 other structural steels; tests were also carried out on a pipe made from the 4140-L80 steel. As expected, the stress history affects the MMM signal, but the experimental results show that significant irreversible change of magnetization always occurs only in the first cycle of loading regardless whether the deformation is purely elastic or partially plastic. If the peak stress level is increased at a given point during cycling, the immediately following next cycle acts as a new “first” cycle at that peak stress level and causes additional significant irreversible change of magnetization, but there is no evidence that plastic deformation might build up a cumulative magnetization. The MMM effect is very small in the steel samples tested, indicating that it will not be useful in field applications. In un-notched specimens the irreversible change in magnetization caused a proportional change in the measured external magnetic field on the order of only 5–10 A/m, while in the case of notched specimens the leakage field was on the order of 30–60 A/m. KW - Magneto-mechanical memory KW - Stress concentration KW - Permanently installed sensors KW - Irreversible change KW - Cumulative magnetization PY - 2017 DO - https://doi.org/10.1016/j.ndteint.2017.07.019 SN - 0963-8695 SN - 1879-1174 VL - 92 SP - 136 EP - 148 PB - Elsevier Ltd. AN - OPUS4-42936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bungartz, M. A1 - Kunisch, E. A1 - Maenz, S. A1 - Horbert, V. A1 - Xin, L. A1 - Gunella, F. A1 - Mika, J. A1 - Borowski, J. A1 - Bischoff, S. A1 - Schubert, H. A1 - Sachse, A. A1 - Illerhaus, Bernhard A1 - Günster, Jens A1 - Bossert, J. A1 - Jandt, K. D. A1 - Plöger, F. A1 - Kinne, R. W. A1 - Brinkmann, O. T1 - GDF5 significantly augments the bone formation induced by an injectable, PLGA fiber-reinforced, brushite-forming cement in a sheep defect model of lumbar osteopenia N2 - BACKGROUND CONTEXT: Biodegradable calcium phosphate cement (CPC) represents a promising option for the surgical treatment of osteoporotic vertebral fractures. Because of augmented local bone catabolism, however, additional targeted delivery of bone morphogenetic proteins with the CPC may be needed to promote rapid and complete bone regeneration. PURPOSE: In the present study, an injectable, poly(l-lactide-co-glycolide) acid (PLGA) fiber-reinforced, brushite-forming cement (CPC) containing the bone morphogenetic Protein GDF5 was tested in a sheep lumbar osteopenia model. STUDY DESIGN/SETTING: This is a prospective experimental animal study METHODS: Defined bone defects (diameter 5 mm) were placed in aged, osteopenic female sheep. Defects were treated with fiber-reinforced CPC alone (L4; CPC+ fibers) or with CPC containing different dosages of GDF5 (L5; CPC+ fibers + GDF5; 1, 5, 100, and 500g GDF5; n = 5 or 6 each). The results were compared with those of untouched controls (L1). Three and 9 months postoperation, structural and functional effects of the CPC (±GDF5) were assessed ex vivo by measuring (1) bone mineral density (BMD); (2) bone structure, that is, bone volume/total volume (assessed by micro-computed tomography and histomorphometry), trabecular thickness, and trabecular number; (3) bone formation, that is, osteoid volume/bone volume, osteoid surface/bone surface, osteoid thickness, mineralized surface/bone surface, mineral apposition rate, and bone formation rate/bone surface; (4) bone resorption, that is, eroded surface/bone surface; and (5) compressive strength. RESULTS: Compared with untouched controls (L1), both CPC+ fibers (L4) and CPC+ fibers + GDF5 (L5) numerically or significantly improved all parameters of bone formation, bone resorption, and bone structure. These significant effects were observed both at 3 and 9 months, but for some parameters they were less pronounced at 9 months. Compared with CPC without GDF5, additional significant effects of CPC with GDF5 were demonstrated for BMD and parameters of bone formation and structure (bone volume/total volume, trabecular thickness, and trabecular number, as well as mineralized surface/bone surface). The GDF5 effects were dose-dependent (predominantly in the 5–100g range) at 3 and 9 months. CONCLUSIONS: GDF5 significantly enhanced the bone formation induced by a PLGA fiber-reinforced CPC in sheep lumbar osteopenia. The results indicated that a local dose as low as ≤100g GDF5 may be sufficient to augment middle to long-term bone formation. The novel CPC+ GDF5 combination may thus qualify as an alternative to the bioinert, supraphysiologically stiff poly-(methyl methacrylate) cement currently applied for vertebroplasty/kyphoplasty of osteoporotic vertebral fractures. KW - Bone regeneration KW - Computed tomography KW - Large animal model sheep KW - Osteoporotic vertebral fracture PY - 2017 DO - https://doi.org/10.1016/j.spinee.2017.06.007 SN - 1529-9430 SN - 1878-1632 VL - 17 IS - 11 SP - 1685 EP - 1698 PB - Elsevier Inc. AN - OPUS4-43239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine T1 - Betrachtung der SIP Relaxationseigenschaften in Zusammenhang mit einer erweiterten Porenraumanalyse durch Quecksilberporosimetrie (MIP), Gassorption (BET), μ-CT und NMR N2 - Die elektrischen Eigenschaften im Niederfrequenzbereich der Spektral Induzierten Polarisation (SIP) von silikatisch gebundenen, porösen Medien werden maßgeblich durch der Porenstruktur, der Art des Sättigungsfluids, der geochemischen Zusammensetzung und den Oberflächeneigenschaften (wie z.Bsp. der Oberflächenladung oder der Kationenaustauschkapazität) bestimmt. Einige Autoren konnten an Sandsteinen mit geringer Variation der petrophysikalischen Eigenschaften zeigen, dass die SIP-Relaxationszeit maßgeblich von der Porenhalsradienverteilung - ermittelt durch Quecksilberporosimetrie (MIP) - bestimmt wird. Diese Beobachtungen bezogen sich jedoch auf Probensätze mit dominanten Porenhalsgrößen (Ddom) im Bereich von 10 µm bis 100 µm. Betrachtet man heterogenere Datensätze von Sandsteinen mit vollkommen unterschiedlicher Herkunft und einer breiten Variation dominanter Porenhalsgrößen (z. Bsp. über vier Dekaden mit Ddom von 0.01 µm bis 100 µm), ist der Zusammenhang zwischen SIP-Relaxationszeit und MIP-Porenhalsgröße deutlich schwächer. Stattdessen beobachtet man auch für Proben mit engen Porenhälsen (Ddom < 5-10 µm) häufig relativ lange Relaxationszeiten (bzw. niederfrequente SIP-Relaxationen). Um die Porensysteme in derartigen Medien besser zu charakterisieren, führen wir zusätzlich Untersuchungen mit µ-CT, Gassorption (BET), Quecksilberporosimetrie (MIP) und Nuklear-Magnetischer Resonanz (NMR) durch und versuchen, die verfahrensspezifisch und auflösungsbedingt unterschiedlichen Ergebnisse zu einer Gesamtaussage zusammenzuführen. In unserem Beitrag zeigen wir ausgewählte Ergebnisse einer systematischen Studie an insgesamt 16 Sandsteinen und 3 Tuffsteinen. Ziel dieser Arbeit ist es, einerseits durch die Methodenkombination Porenräume allgemein ganzheitlicher abzubilden, andererseits die beobachteten SIP-Relaxationszeiten so gut wie möglich charakteristischen Längen zuordnen zu können. Dies ist ein wichtiger Beitrag zur Klärung der Frage, ob die SIP-Relaxationszeit überhaupt maßgeblich von geometrischen Porenraumeigenschaften bestimmt wird oder ggf. von anderen Eigenschaften wie der chemischen Zusammensetzung (z.B. Tongehalt, Tonart) abhängt. T2 - 77. Jahrestagung der Deutschen Geophysikalischen Gesellschaft CY - Potsdam, Germany DA - 27.03.2017 KW - Spektral Induzierte Polarisation KW - µ-CT KW - MIP KW - NMR KW - Porengrößenverteilung PY - 2017 AN - OPUS4-43242 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, G. A1 - Prinz, Carsten A1 - Zimathies, Annett A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - Hydrated and dehydrated Ca-coordination polymers based on benzene-dicarboxylates: mechanochemical synthesis, structure refinement, and spectroscopic characterization N2 - A series of Ca-based coordination polymers were prepared mechanochemically by milling Ca(OH)2 with phthalic acid (H2oBDC), isophthalic acid (H2mBDC), and terephthalic acid (H2pBDC). The hydrated compounds [Ca(oBDC)(H2O)], [Ca(mBDC)(H2O)3.4], and [Ca(pBDC)(H2O)3] were prepared for the first time via mechanochemical routes. The refined structures were validated by extended X-ray absorption data. The new dehydrated compound [Ca(oBDC)] (1-H2O), obtained after the thermal post-treatment of 1 in a reversible phase transition process, was determined ab initio based on the powder X-ray diffraction (PXRD) data. The materials were thoroughly characterized using elemental analysis, thermal analysis, and spectroscopic methods: magic-angle spinning NMR and attenuated total reflection-infrared spectroscopy. The specific surface areas and sorption properties of the hydrated and dehydrated samples were determined using the isotherms of gas sorption and dynamic vapor sorption measurements. KW - Mechanochemistry KW - XRD PY - 2018 UR - http://pubs.rsc.org/en/content/articlehtml/2017/ce/c7ce01906h DO - https://doi.org/10.1039/C7CE01906H VL - 20 SP - 946 EP - 961 PB - Royal Society of Chemistry AN - OPUS4-44440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shashev, Yury A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Evsevleev, Sergei A1 - Müller, Bernd R. A1 - Osenberg, Markus A1 - Manke, Ingo A1 - Hentschel, Manfred P. A1 - Bruno, Giovanni T1 - Optimizing the visibility of X-ray phase grating interferometry N2 - The performance of grating interferometers coming up now for Imaging interfaces within materials depends on the efficiency (visibility) of their main component, namely the phase grating. Therefore, experiments with monochromatic synchrotron radiation and corresponding simulations are carried out. The visibility of a Phase grating is optimized by different photon energies, varying detector to grating distances and continuous rotation of the phase grating about the grid lines. Such kind of rotation changes the projected grating shapes, and thereby the distribution profiles of phase shifts. This yields higher visibilities than derived from ideal rectangular shapes. By continuous grating rotation and variation of the propagation distance, we achieve 2D visibility maps. Such maps provide the visibility for a certain combination of grating orientation and detector position. Optimum visibilities occur at considerably smaller distances than in the standard setup. KW - Synchrotron, BAMline KW - Talbot-Lau interferometer KW - X-ray imaging KW - X-ray refraction KW - Grating interferometry KW - X-ray phase contrast PY - 2017 DO - https://doi.org/10.3139/120.111097 SN - 0025-5300 VL - 59 IS - 11-12 SP - 974 EP - 980 PB - Hanser Verlag AN - OPUS4-42955 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zhang, Zeyu A1 - Kruschwitz, Sabine A1 - Weller, Andreas A1 - Halisch, M. A1 - Prinz, Carsten T1 - Enhanced pore space analysis by use of μ-CT, MIP, N2 - We investigate the pore space of rock samples with respect to different petrophysical parameters using various methods, which provide data upon pore size distributions, including micro computed tomography (μ-CT), mercury intrusion porosimetry (MIP), nuclear magnetic resonance (NMR), and spectral induced polarization (SIP). The resulting cumulative distributions of pore volume as a function of pore size are compared. Considering that the methods differ with regard to their limits of resolution, a multiple length scale characterization of the pore space geometry is proposed, that is based on a combination of the results from all of these methods. The findings of this approach are compared and discussed by using Bentheimer sandstone. Additionally, we compare the potential of SIP to provide a pore size distribution with other commonly used methods (MIP, NMR). The limits of resolution of SIP depend on the usable frequency range (between 0.002 and 100 Hz). The methods with similar resolution show a similar behavior of the cumulative pore volume distribution in the overlapping pore size range. The methods μ-CT and NMR provide the pore body size while MIP and SIP characterize the pore throat size. Using this difference, the average pore body to throat ratio is determined to be about three for the Bentheimer sandstone. Our study shows that a good agreement between the pore radii distributions can only be achieved if the curves are adjusted considering the resolution and pore volume in the relevant range of pore radii. The MIP curve with the widest range in resolution should be used as reference T2 - Annual Symposium of the Society of Core Analysts 2017 CY - Vienna, Austria DA - 27.08.2017 KW - Spectral induced polarization KW - Mercury intrusion porosimetry KW - µ-CT KW - Nuclear magnetic resonance KW - Bentheimer Sandstone PY - 2017 SP - 086, 1 EP - 086, 8 AN - OPUS4-43082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Einblick auf die Computer Tomographie für die zerstörungsfreie Prüfung N2 - Ein kurzes Blick in die Computertomographie (CT) im Rahmen des RT3 Kurs der DGZfP ist gegeben. Die Radontransformation ist bildlich erklärt, und die Grundlagen der Technik mit Vergleich zu der Radiographie sind auch erwähnt. Die typische Rekonstruktionsfehler und deren Beseitigung sind behandelt. Am Ende Beispiele der Anwendungen der CT sind gegeben, aus der zerstörungsfreie Prüfung, der Materialwissenschaft und der Metrologie. T2 - RT3 Kurs DGZfP CY - BAM, Berlin, Germany DA - 08.12.2017 KW - Computertomographie KW - Radiographie KW - Laminographie KW - Zerstörungsfreie Prüfung PY - 2017 AN - OPUS4-43376 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Tiebe, Carlo A1 - Bartholmai, Matthias T1 - Airborne Remote Gas Sensing and Mapping N2 - Leaking methane (CH4) from infrastructures, such as pipelines and landfills, is critical for the environment but can also pose a safety risk. To enable a fast detection and localization of these kind of leaks, we developed a novel robotic platform for aerial remote gas sensing. Spectroscopic measurement methods for remote sensing of selected gases lend themselves for use on mini-copters, which offer a number of advantages for inspection and surveillance over traditional methods. No direct contact with the target gas is needed and thus the influence of the aerial platform on the measured gas plume can be kept to a minimum. This allows to overcome one of the major issues with gas-sensitive mini-copters. On the other hand, remote gas sensors, most prominently Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensors have been too bulky given the payload and energy restrictions of mini-copters. Here, we present the Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), which combines a novel lightweight TDLAS sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile hexacopter. The proposed system can be deployed in scenarios that cannot be addressed by currently available robots and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO). It enables tomographic reconstruction of gas plumes and a localization of gas sources. We also present first results showing its performance under realistic conditions. T2 - Networked Environmental Monitoring – from sensor principles to novel services CY - BAM, Berlin, Germany DA - 06.02.2018 KW - Localization of gas sources KW - Mobile Robot Olfaction KW - Tomographic reconstruction of gas plumes KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - UAV-REGAS PY - 2018 AN - OPUS4-44085 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gunella, F. A1 - Kunisch, E. A1 - Maenz, S. A1 - Horbert, V. A1 - Xin, L. A1 - Mika, J. A1 - Borowski, J. A1 - Bischoff, S. A1 - Schubert, H. A1 - Sachse, A. A1 - Illerhaus, Bernhard A1 - Günster, Jens A1 - Bossert, J. A1 - Jandt, K. D. A1 - Plöger, F. A1 - Kinne, R. W. A1 - Brinkmann, O. A1 - Bungartz, M. ED - Carragee, T1 - The GDF5 mutant BB-1 enhances the bone formation induced by an injectable, poly(l-lactide-co-glycolide) acid (PLGA) fiber-reinforced, brushite-forming cement in a sheep defect model of lumbar osteopenia N2 - BACKGROUND CONTEXT: Targeted delivery of osteoinductive bone morphogenetic Proteins (eg, GDF5) in bioresorbable calcium phosphate cement (CPC), potentially suitable for vertebroplasty and kyphoplasty of osteoporotic vertebral fractures, may be required to counteract augmented local bone catabolism and to support complete bone regeneration. The biologically optimized GDF5 Mutant BB-1 may represent an attractive drug candidate for this purpose. PURPOSE: The aim of the current study was to test an injectable, poly (l-lactide-co-glycolide) acid (PLGA) fiber-reinforced, brushite-forming CPC containing low-dose BB-1 in a sheep lumbar osteopenia model. STUDY DESIGN/ SETTING: This is a prospective experimental animal study. METHODS: Bone defects (diameter 5 mm) were generated in aged, osteopenic female sheep and were filled with fiber-reinforced CPC alone (L4; CPC+fibers) or with CPC containing different dosages. KW - Bone morphogenetic protein; KW - Bone regeneration; KW - Micro-Computed-Tomography; KW - Calcium phosphate cement; KW - GDF-5 mutant; KW - Large animal model sheep; KW - Osteoporotic vertebral fracture PY - 2018 DO - https://doi.org/10.1016/j.spinee.2017.10.002 SN - 1529-9430 SN - 1878-1632 VL - 18 IS - 2 SP - 357 EP - 369 PB - Elsevier CY - New York AN - OPUS4-44561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Baensch, Franziska T1 - Acoustic emission testing N2 - The phenomenon of acoustic emission (AE) and fundamentals of AE testing procedures are presented. AE based failure analysis of reinforced concrete beam under bending load, steel pipe segments under bending load and wood based materials under tension load are discussed. T2 - INFRASTAR, Training Week #03 at AAU CY - Aalborg, Denmark DA - 04.06.2018 KW - Acoustic emission PY - 2018 AN - OPUS4-45147 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine A1 - Ebell, Gino A1 - Shen, J. T1 - Towards Data Based Corrosion Analysis of Concrete with Supervised Machine Learning N2 - Half-Cell-Potential Mapping (HP) is the most popular non-destructive testing (NDT) method for the detection of active corrosion in reinforced concrete. HP is influenced by parameters such as moisture and chloride gradients in the component. The sensitivity to the spatially small, but dangerous pitting is low. In this study we show how additional measurement information can be used with multi-sensor data fusion to improve the detection performance and to automate data evaluation. The fusion is based on supervised machine learning (SML). SML are methods that recognize relationships in (sensor) data based on given labels. We use SML to distinguish "defective" and "intact" labeled areas in our dataset. It consists of 18 measurement - each contains HP, ground radar, microwave moisture and Wenner resistance data. Exact labels for changing environmental conditions were available in a laboratory study on a reinforced concrete slab, which deteriorated controlled and accelerated. The deterioration progress was monitored continuously and corrosion was generated targeted at a predefined location. The detection results are quantified and statistically evaluated. The SML results shows a significant improvement over the best single method (HP). T2 - NDE/NDT for Highway and Bridges: Structural Materials Technology (SMT 2018) and the International Symposium Non-Destructive Testing in Civil Engineering (NDT-CE 2018) CY - New Brunswick, NJ, USA DA - 27.08.2018 KW - Data fusion KW - Half-cell potential mapping KW - Data based decision making KW - Non-destuctive corrosion testing of concrete KW - Supervised machine learning PY - 2018 SP - 1 EP - 7 AN - OPUS4-45512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - Metrology for Additively Manufactured Medical Implants: The MetAMMI project N2 - Additive manufacturing (AM) offers an effective solution to the medical sector. It enables the production, on demand, of customised implants which match the patient’s anatomy, with grafts that promote bone growth, as well as surgical guides that help the surgeons. The objective of this project is to provide a comprehensive basis to enable the safe use of medical AM products with traceable and reliable dimensionalmeasurements. This will guarantee the reliability of medical AM products to notified bodies and facilitate acceptance of AM in the medical sector for a better quality of life. T2 - BPWT/BAM Workshop " Innovative Materialien und Qualitätskontrolle für additive Fertigung" CY - Berlin, Germany DA - 12.09.2018 KW - Additive manufacturing KW - X-ray computed tomography PY - 2018 AN - OPUS4-45926 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Prinz, Carsten A1 - Hase, Felix A1 - Kruschwitz, Sabine T1 - Data of embedded humidity sensors, sample weights, and measured pore volume distribution for eight screed types N2 - Four cement-based and four calcium-sulphate-based screed types are investigated. The samples have a diameter of 300 mm and a height of 35 or 70 mm. Up to ten humidity sensors are embedded directly during the concreting of the screed samples. Thus, the humidity over the sample height is monitored during hardening, hydration, evaporation, and oven drying. Furthermore, the screed samples are weighed during every measurement to determine the total mass and the corresponding moisture loss. To define the pore system precisely, mercury intrusion porosimetry as well as gas adsorption is performed. According to the data, the entire pore volume distribution is known. The measured pore diameters range from 0.8 nm to 100 µm and the total porosity of the examined screeds ranges between 11% and 22%. Based on these measurement data, moisture transport, pore saturation as well as sorption isotherms and their hysteresis may be calculated quantitatively as described in “Monitoring of the absolute water content in porous materials based on embedded humidity sensors” (Strangfeld and Kruschwitz, 1921). KW - Concrete and screed KW - Embedded humidity sensors KW - Pore volume distribution KW - Material moisture PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-462339 DO - https://doi.org/10.1016/j.dib.2018.09.020 SN - 2352-3409 VL - 21 SP - 8 EP - 12 PB - Elsevier CY - Amsterdam AN - OPUS4-46233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Strangfeld, Christoph A1 - Prinz, Carsten A1 - Hase, F. A1 - Kruschwitz, Sabine T1 - Data of embedded humidity sensors, sample weights, and measured pore volume distribution for eight screed types N2 - Four cement-based and four calcium-sulphate-based screed types are investigated. The samples have a diameter of 300 mm and a height of 35 or 70 mm. Up to ten humidity sensors are embedded directly during the concreting of the screed samples. Thus, the humidity over the sample height is monitored during hardening, hydration, evaporation, and oven drying. Furthermore, the screed samples are weighted during every measurement to determine the total mass and the corresponding moisture loss. To define the pore system precisely, mercury intrusion porosimetry as well as gas adsorption is performed. According to the data, the entire pore volume distribution is known. The measured pore diameters range from 0.8 nm to 100 μm and the total porosity of the examined screeds ranges between 11 % and 22 %. Based on these measurement data, moisture transport, pore saturation as well as sorption isotherms and their hysteresis may be calculated quantitatively as described by Strangfeld et al. KW - Concrete and screed KW - Material moisture KW - Pore volume distribution KW - Embedded humidity sensors KW - Data in brief PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-448261 UR - https://data.4tu.nl/repository/uuid:d2ba436f-78c0-4105-8a1f-5422fcb37851 DO - https://doi.org/10.4121/uuid:d2ba436f-78c0-4105-8a1f-5422fcb37851 SP - 1 EP - 4 PB - 4TU.Centre for Research Data CY - Delft AN - OPUS4-44826 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Evans, Alexander A1 - Luzin, V. A1 - Abreu Faria, G. A1 - Degener, Sebastian A1 - Polatidis, E. A1 - Čapek, J. A1 - Kromm, Arne A1 - Dovzhenko, G. A1 - Bruno, Giovanni T1 - Texture-based residual stress analysis of laser powder bed fused Inconel 718 parts N2 - Although layer-based additive manufacturing methods such as laser powder bed fusion (PBF-LB) offer an immense geometrical freedom in design, they are typically subject to a build-up of internal stress (i.e. thermal stress) during manufacturing. As a consequence, significant residual stress (RS) is retained in the final part as a footprint of these internal stresses. Furthermore, localized melting and solidification inherently induce columnar-type grain growth accompanied by crystallographic texture. Although diffraction-based methods are commonly used to determine the RS distribution in PBF-LB parts, such features pose metrological challenges in their application. In theory, preferred grain orientation invalidates the hypothesis of isotropic material behavior underlying the common methods to determine RS. In this work, more refined methods are employed to determine RS in PBF-LB/M/IN718 prisms, based on crystallographic texture data. In fact, the employment of direction-dependent elastic constants (i.e. stress factors) for the calculation of RS results in insignificant differences from conventional approaches based on the hypothesis of isotropic mechanical properties. It can be concluded that this result is directly linked to the fact that the {311} lattice planes typically used for RS analysis in nickel-based alloys have high multiplicity and less strong texture intensities compared with other lattice planes. It is also found that the length of the laser scan vectors determines the surface RS distribution in prisms prior to their removal from the baseplate. On removal from the baseplate the surface RS considerably relaxes and/or redistributes; a combination of the geometry and the scanning strategy dictates the sub-surface RS distribution. KW - Additive manufacturing KW - Electron backscattered diffraction KW - Principal stress KW - Residual stress PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578331 DO - https://doi.org/10.1107/S1600576723004855 SN - 1600-5767 VL - 56 IS - Pt 4 SP - 1076 EP - 1090 AN - OPUS4-57833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nguyen, H. G. A1 - Toman, B. A1 - van Zee, R. A1 - Prinz, Carsten A1 - Thommes, M. A1 - Ahmad, R. A1 - Kiska, D. A1 - Salinger, J. A1 - Walton, I. A1 - Walton, K. A1 - Broom, D. A1 - Benham, M. A1 - Ansari, H. A1 - Pini, R. A1 - Petit, C. A1 - Adolphs, J. A1 - Schreiber, A. A1 - Shigeoka, T. A1 - Konishi, Y. A1 - Nakai, K. A1 - Henninger, M. A1 - Petrzik, T. A1 - Kececi, C. A1 - Martis, V. A1 - Paschke, T. A1 - Mangano, E. A1 - Brandani, S. T1 - Reference isotherms for water vapor sorption on nanoporous carbon: results of an interlaboratory study N2 - This paper reports the results of an international interlaboratory study sponsored by the Versailles Project on Advanced Materials and Standards (VAMAS) and led by the National Institute of Standards and Technology (NIST) on the measurement of water vapor sorption isotherms at 25 °C on a pelletized nanoporous carbon (BAM-P109, a certified reference material). Thirteen laboratories participated in the study and contributed nine pure water vapor isotherms and four relative humidity isotherms, using nitrogen as the carrier gas. From these data, reference isotherms, along with the 95% uncertainty interval (Uk=2), were determined and are reported in a tabular format. KW - BAM-P109 KW - Interlaboratory study KW - Nanoporous carbon KW - Reference isotherm KW - VAMAS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576560 DO - https://doi.org/10.1007/s10450-023-00383-1 SN - 0929-5607 SP - 1 EP - 12 PB - Springer CY - Heidelberg AN - OPUS4-57656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Feigl, Michael T1 - Nd: YAG laser induced thermal shock testing of oxidation preotecting sol-gel alumina coatings on Ni-base alloys T2 - Eurocorr 2011 CY - Stockholm, Sweden DA - 05.09.2011 PY - 2011 AN - OPUS4-23203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias T1 - Airborne Remote Gas Sensing and Mapping N2 - Leaking methane (CH4) from infrastructures, such as pipelines and landfills, is critical for the environment but can also pose a safety risk. To enable a fast detection and localization of These kind of leaks, we developed a novel robotic platform for aerial remote gas sensing - the so-called Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS). T2 - Tag der offenen Tür auf dem Testgelände der BAM (BAM TTS) CY - Baruth/Mark - OT Horstwalde, Germany DA - 29.09.2018 KW - Localization of gas sources KW - Mobile Robot Olfaction KW - Tomographic reconstruction of gas plumes KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - UAV-REGAS PY - 2018 AN - OPUS4-46152 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Capitalizing experiments at neutron sources: a couple of possible strategies N2 - For how trivial or provocative it can sound, the best neutron spectrometer in the world does not produce science by itself. By definition of Materials Science, neutron scattering data on engineering materials must be used as a tool to understand, and even tailor, materials performance. In order for this to happen, it is clear that neutron data need to be acquired under the most relevant condition possible, coupled to other experimental techniques, and capitalized by means of proper simulations and data analysis. In fact, access to neutron sources is not routine. Consequently, it is imperative to search ways to make neutron data rentable for the material science and industrial research community. In this presentation, and based on the example of Ceramic Diesel Particulate Filters and Aluminum Matrix Composites, we will show a couple of strategies to combine neutron data with other experiments, and with theoretical models. Their combination allows raising the value of experiments from data production to problem-solving. Obviously, these are only a few among the many combinations possible to help improving materials properties, performance, and safety. T2 - Kolloquia der TUM CY - TU München, Germany DA - 16.01.2017 KW - Neutronenbeugung KW - Eigenspannungen KW - Mechanische Eigenschaften KW - Kompositen KW - Modellierung KW - Poröse Keramiken KW - TF Material PY - 2017 AN - OPUS4-38999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard T1 - Sampling of undisturbed soil samples as part of the KEYSOM field experiment N2 - Results of medicale- and Micro-CT for COST KEYSOM project T2 - Cost KEYSOM meeting Matera, Italy CY - Matera, Italy DA - 24.9.2018 KW - µCT KW - Soil science PY - 2018 AN - OPUS4-46117 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - Selective laser melting process optimisation: X-ray and neutron sources for information from powder grains to printed structures N2 - Selective laser melting process optimisation: X-ray and neutron sources for information from powder grains to printed structures T2 - BPWT/BAM Workshop " Innovative Materialien und Qualitätskontrolle für additive Fertigung" CY - Berlin, Germany DA - 12.09.2018 KW - SLS KW - X-ray computed tomography KW - Refraction KW - Neutron diffraction KW - Additive manufacturing KW - Industry 4.0 PY - 2018 AN - OPUS4-45924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Explaining deviatoric residual stresses and load transfer in aluminum alloys and composites with complex microstructure N2 - The residual stresses and load transfer in multiphase metal alloys and their composites (with both random planar-oriented short fibers and particles) will be shown, as studied by neutron diffraction, by X-ray computed tomography, and by a model based on the reformulation of classic Maxwell’s homogenization method. Contrary to common understanding and state-of-the-art models, we experimentally observe that randomly oriented phases possess non-hydrostatic residual stress. Moreover, we disclose that the unreinforced matrix alloy stays under hydrostatic compression even under external uniaxial compression. The recently developed modeling approach allows calculating the residual stress in all phases of the composites. It rationalizes the presence of deviatoric stresses accounting for the interaction of random oriented phases with fibers having preferential orientation. It also allows the explanation of the unconventional in-situ behavior of the unreinforced alloy and the prediction of the micromechanical behavior of other similar alloys. T2 - MLZ Conference 2022: Neutrons for Mobility CY - Lenggries, Germany DA - 31.05.2022 KW - Load transfer KW - Neutron Diffraction KW - micromechanical modeling KW - Computed tomography PY - 2022 AN - OPUS4-55405 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lehmann, Jens T1 - Potentialfeldmessung - Korrosionsprüfung von Stahlbetonbauwerken N2 - Durch das alkalische Porenwassermilieu ist Stahl im Beton vor Korrosion geschützt. Unter ungünstigen Umgebungsbedingungen (Karbonatisierung, Chlorideintrag) kann die passive Deckschicht auf der Stahloberfläche zerstört werden. Im weiteren Verlauf können sich korrosionsbedingte Folgeschäden, wie Risse und Abplatzungen am Bauwerk ergeben. Um notwendige Sanierungsmaßnahmen sind frühzeitige und weitgehend zerstörungsfrei ermittelte Informationen über das aktuelle Korrosionsverhalten der Stahlbewehrung von großer Bedeutung. Die Potentialfeldmessung ist ein etabliertes und weit verbreitetes Verfahren zur Beurteilung des Korrosionszustandes der Bewehrung in Stahlbetonbauwerken. Mit Hilfe dieses Verfahrens können Bereiche aktiv korrodierender Bewehrung zerstörungsfrei lokalisiert werden. In der Regel kommt diese Messmethode bei der Detektion chloridinduzierter Korrosion zum Einsatz. T2 - Fachtagung Prüfen von Beton CY - Hamburg, Germany DA - 11.10.2016 KW - Stahlbeton KW - Spannbeton KW - Korrosion KW - Zertörungsfreie Prüfung PY - 2016 AN - OPUS4-37807 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruno, Giovanni A1 - Shyam, A. A1 - Watkins, T. R. A1 - Pandey, A. A1 - Lara-Curzio, E. A1 - Parish, C. M. A1 - Stafford, R. J. T1 - The effect of porosity and microcracking on the thermomechanical properties of cordierite N2 - The effect of porosity and microcracking on the mechanical properties (strength, fracture toughness,Young’s modulus, and fracture energy) and thermal expansion of diesel particulate filter (DPF) gradecordierite materials has been investigated. A method to deconvolute the effect of porosity and microc-racking on Young’s modulus is proposed. In addition, the microcrack density and the pore morphologyfactor are calculated by applying a micromechanical differential scheme. The values of the investigatedmechanical properties are shown to decrease with an increase in porosity, but the thermal expansionvalues are insensitive to porosity. The variation in mechanical properties as a function of porosity leadsto distinct porosity dependence of thermal shock resistance for crack initiation and crack propagationfor DPF grade synthetic cordierite. KW - Diesel particulate filter KW - Cordierite KW - Porosity KW - Microcracking KW - Micromechanical differential scheme PY - 2015 DO - https://doi.org/10.1016/j.jeurceramsoc.2015.08.014 VL - 2015/35 IS - 16 SP - 4557 EP - 4566 PB - Elsevier Ltd. AN - OPUS4-37973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruno, Giovanni A1 - González-Doncel, G. A1 - Fernández, R. T1 - Primary and secondary creep in aluminum alloys as a solid state transformation N2 - Despite the massive literature and the efforts devoted to understand the creep behavior of aluminum alloys, a full description of this phenomenon on the basis of microstructural parameters and experimental conditions is, at present, still missing. The analysis of creep is typically carried out in terms of the so-called steady or secondary creep regime. The present work offers an alternative view of the creep behavior based on the Orowan dislocation dynamics. Our approach considers primary and secondary creep together as solid state isothermal transformations, similar to recrystallization or precipitation phenomena. In this frame, it is shown that the Johnson-Mehl-Avrami-Kolmogorov equation, typically used to analyze these transformations, can also be employed to explain creep deformation. The description is fully compatible with present (empirical) models of steady state creep. We used creep curves of commercially pure Al and ingot AA6061 alloy at different temperatures and stresses to validate the proposed model. KW - Creep KW - Aluminium KW - Grain boundaries KW - Precipitation KW - Computer modeling PY - 2016 DO - https://doi.org/10.1063/1.4961524 VL - 2016 IS - 120 SP - 085101-1 EP - 085101-9 PB - AIP Publishing AN - OPUS4-37965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruno, Giovanni A1 - Cabeza, Sandra A1 - Mishurova, Tatiana A1 - Garcés, G. A1 - Requena, G. T1 - The role of reinforcement orientation on the damage evolution of AlSi12CuMgNi +15% Al2O3 under compression N2 - Internal damage of an AlSi12CuMgNi alloy reinforced with planar randomshort fibres has been investigated after compression. This damage strongly influences the load partition between matrix and reinforcement. For fibres perpendicular to the applied load, breakage and interconnected cracks appear in significantly higher volume fraction than with fibres parallel to load. KW - Metal Matrix Composites KW - Damage KW - Load partition KW - Synchrotron CT KW - Neutron diffraction PY - 2016 VL - 122 SP - 115 EP - 118 PB - Elsevier Ltd. AN - OPUS4-37975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Magkos, Sotirios T1 - Suppression of cone-beam artefacts with DIRECTT N2 - A model image of the artefacts is computed just once, but it is used during each iteration of DIRECTT to “correct” the back-projected volume. The final reconstruction is a clear improvement over the one computed by the conventional FDK algorithm. T2 - MUMMERING outreach conference CY - Online meeting DA - 10.06.2021 KW - Iteration method KW - Signal processing KW - X-ray imaging KW - Computed tomography PY - 2021 AN - OPUS4-53467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Maenz, S. A1 - Brinkmann, O. A1 - Kunisch, E. A1 - Horbert, V. A1 - Gunella, F. A1 - Bischoff, S. A1 - Schubert, H. A1 - Sachse, A. A1 - Xin, L. A1 - Günster, Jens A1 - Illerhaus, Bernhard A1 - Jandt, K. D. A1 - Bossert, J. A1 - Kinne, R. W. A1 - Bungartz, M. T1 - Enhanced bone formation in sheep vertebral bodies after minimally invasive treatment with a novel, PLGA fiber-reinforced brushite cement. N2 - Injectable, brushite-forming calcium phosphate cements (CPC) show potential for bone replacement, but they exhibit low mechanical strength. This study tested a CPC reinforced with poly(l-lactide-co-glycolide) acid (PLGA) fibers in a minimally invasive, sheep lumbar vertebroplasty model. The study aimed to test the in vivo biocompatibility and osteogenic potential of a PLGA fiber-reinforced, brushite-forming CPC in a sheep large animal model. KW - µCT KW - Vertebral KW - PLGA cement PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S152994301631066X DO - https://doi.org/10.1016/j.spinee.2016.11.006 SN - 1529-9430 SN - 1878-1632 VL - 17 IS - 5 SP - 709 EP - 719 PB - Elsevier Science direct AN - OPUS4-40462 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. A1 - Kohlhoff, Harald A1 - Hüllmann, Dino A1 - Lilienthal, A.J. A1 - Kluge, Martin T1 - Bringing Mobile Robot Olfaction to the Next Dimension – UAV-based Remote Sensing of Gas Clouds and Source Localization N2 - This paper introduces a novel robotic platform for aerial remote gas sensing. Spectroscopic measurement methods for remote sensing of selected gases lend themselves for use on mini-copters, which offer a number of advantages for inspection and surveillance. No direct contact with the target gas is needed and thus the influence of the aerial platform on the measured gas plume can be kept to a minimum. This allows to overcome one of the major issues with gas-sensitive mini-copters. On the other hand, remote gas sensors, most prominently Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensors have been too bulky given the payload and energy restrictions of mini-copters. Here, we introduce and present the Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), which combines a novel lightweight TDLAS sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile hexacopter. The proposed system can be deployed in scenarios that cannot be addressed by currently available robots and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO). It enables tomographic reconstruction of gas plumes and a localization of gas sources. We also present first results showing the gas sensing and aiming capabilities under realistic conditions. T2 - IEEE International Conference on Robotics and Automation (ICRA) CY - Singapore DA - 29.05.2017 KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - 3-axis gimbal KW - Mobile Robot Olfaction KW - Tomographic reconstruction of gas plumes KW - Localization of gas sources KW - Aerial platform PY - 2017 SN - 978-1-5090-4632-4 SP - 3910 EP - 3916 PB - IEEE AN - OPUS4-40545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Bringing Mobile Robot Olfaction to the Next Dimension – UAV-based Remote Sensing of Gas Clouds and Source Localization N2 - This presentation introduces a novel robotic platform for aerial remote gas sensing. Spectroscopic measurement methods for remote sensing of selected gases lend themselves for use on mini-copters, which offer a number of advantages for inspection and surveillance. No direct contact with the target gas is needed and thus the influence of the aerial platform on the measured gas plume can be kept to a minimum. This allows to overcome one of the major issues with gas-sensitive mini-copters. On the other hand, remote gas sensors, most prominently Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensors have been too bulky given the payload and energy restrictions of mini-copters. Here, we introduce and present the Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), which combines a novel lightweight TDLAS sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile hexacopter. The proposed system can be deployed in scenarios that cannot be addressed by currently available robots and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO). It enables tomographic reconstruction of gas plumes and a localization of gas sources. We also present first results showing the gas sensing and aiming capabilities under realistic conditions. T2 - IEEE International Conference on Robotics and Automation (ICRA) CY - Singapore DA - 29.05.2017 KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - 3-axis gimbal KW - Mobile Robot Olfaction KW - Tomographic reconstruction of gas plumes KW - Localization of gas sources KW - Aerial platform PY - 2017 AN - OPUS4-40546 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - X-ray refraction 2D and 3D techniques N2 - X-ray refraction techniques represent a very promising, yet not so wide-spread, set of X-ray techniques based on refraction effects. They allow determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with nanometric detectability. While they are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of microstructural features could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. T2 - ICTMS 2017 CY - Lund, Sweden DA - 26.06.2017 KW - X-ray refraction KW - Composites KW - Damage KW - Cracks KW - Cearmics PY - 2017 AN - OPUS4-41042 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Absorption and refraction tomography: Characterization and non-destructive testing of micro-structured materials N2 - The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread equally holds for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated. I will show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. Examples of micro-structured inhomogeneous materials will be given, such as Composites, Ceramics, Concrete, and Additively manufactured parts. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces. Additionally, I will present a new technique in our portfolio, Neutron Diffraction, which is extremely well suited to the study of internal stresses, both residual and under external load. T2 - Kolloquium ICMCB Bordeaux CY - Bordeaux, France DA - 13.07.2017 KW - Computed tomography KW - X-ray refraction KW - Neutron diffraction KW - Additive manufacturing KW - Ceramics KW - Composites KW - BAM PY - 2017 AN - OPUS4-41041 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tang, Lei A1 - Magdysyuk, Oxana V. A1 - Jiang, Fuqing A1 - Wang, Yiqiang A1 - Evans, Alexander A1 - Kabra, Saurabh A1 - Cai, Biao T1 - Mechanical performance and deformation mechanisms at cryogenic temperatures of 316L stainless steel processed by laser powder bed fusion: In situ neutron diffraction N2 - Manufacturing austenitic stainless steels (ASSs) using additive manufacturing is of great interest for cryogenic applications. Here, the mechanical and microstructural responses of a 316L ASS built by laser powder bed fusion were revealed by performing in situ neutron diffraction tensile tests at the low-temperature range (from 373 to 10 K). The stacking fault energy almost linearly decreased from 29.2 ± 3.1 mJm⁻² at 373 K to 7.5 ± 1.7 mJm⁻² at 10 K, with a slope of 0.06 mJm⁻²K⁻¹, leading to the transition of the dominant deformation mechanism from strain-induced twinning to martensite formation. As a result, excellent combinations of strength and ductility were achieved at the low-temperature range. KW - Condensed Matter Physics KW - General Materials Science KW - Mechanics of Materials KW - Metals and Alloys KW - Mechanical Engineering PY - 2022 DO - https://doi.org/10.1016/j.scriptamat.2022.114806 SN - 1359-6462 VL - 218 SP - 1 EP - 7 PB - Elsevier BV CY - Amsterdam AN - OPUS4-59317 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Monitoring trace substances in wastewater and surface water by immunoanalytical assays and sensors N2 - Monitoring the elimination of trace substances in wastewater treatment plants, as required in the recast of the EU Urban Wastewater Treatment Directive and the new Kommunalabwasserrichtlinie (KARL), creates a need for on-site analyses in wastewater treatment plants. Immunoanalytical methods can be carried out on site, e.g. in the form of rapid tests, but continuously operating (immuno-bio)sensors would be ideal. And antibody-based methods have the inherent disadvantage that one antibody must be used per analyte and therefore only a small number of substances can be analysed. A set of indicators has been integrated in the directives in accordance with the list of the Kompetenzzentrum Spurenstoffe BW (KomS) and offer points of reference here. Yet, in order to be able to use immunoanalytical methods for their monitoring, (DIN/ISO) standards are required that define the necessary quality requirements and quality management measures for the sensors. In addition, for the larger part of the indicators, the required antibodies have yet to be developed and made commercially available in the long term. The talk will highlight our previous work on high-throughput methods, such as ELISA, regarding the presence of anthropogenic markers and some indicators as well as research approaches for sensor technology that could be used on-site, and will provide an overview of deficits and future efforts. T2 - Kolloquium der Abteilung Technische Umweltchemie und Sensortechnik CY - Stuttgart, Germany DA - 21.05.2025 KW - Antibodies KW - Immunoassay KW - Microfluidics KW - Biosensor KW - Trace substances PY - 2025 AN - OPUS4-63501 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Bestimmung von Spurenstoffen im (Roh-)Abwasser mittels ELISA N2 - Der Vortrag behandelt die Bestimmung von Spurenstoffen im Rohabwasser mithilfe von ELISA (Enzyme-Linked Immunosorbent Assay), einer immunanalytischen Methode, die sich durch hohe Sensitivität und Eignung für Hochdurchsatzanalysen auszeichnet. Im Rahmen der Projekte MARKERIA I & II wurden verschiedene anthropogene Marker wie Koffein, Carbamazepin, Diclofenac, Bisphenol A und Hormone wie Östron untersucht, um deren Eignung für die Abwassersurveillance zu bewerten. Die Ergebnisse zeigen, dass einige Substanzen wie Carbamazepin stabile Konzentrationen aufweisen und sich gut als Marker eignen, während andere wie Koffein starke Schwankungen zeigen. Einige Marker wie Isolithocholsäure werden zwar in hohen Konzentrationen gefunden, zeigen aber methodische Herausforderungen wie instabile Assays. Die Studie hebt hervor, dass es Hotspots mit erhöhten Konzentrationen gibt, aber insgesamt eine relativ geringe Variabilität zwischen verschiedenen Rohabwässern besteht. Zukünftige Entwicklungen sollen sich auf die Verbesserung von Antikörpern, die Entwicklung tragbarer Vor-Ort-Analysemethoden und die Standardisierung immunanalytischer Verfahren konzentrieren. T2 - AMELAG-Colloquium "Spurenstoffe im (Ab-)Wasser" CY - Online meeting DA - 20.06.2025 KW - Antikörper KW - Schnelltests KW - Abwasser KW - ELISA PY - 2025 AN - OPUS4-63500 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, Jakob A1 - Heldmann, A. A1 - Hofmann, M. A1 - Evans, Alexander A1 - Petry, W. A1 - Bruno, Giovanni T1 - Determination of diffraction and single-crystal elastic constants of laser powder bed fused Inconel 718 N2 - High energy X-ray synchrotron diffraction is used to investigate the elastic anisotropy of the nickel-based superalloy IN718 produced by laser powder bed fusion (PBF-LB). This material is characterized by a columnar grain morphology with some crystallographic texture. The material is subjected to elastic loading to determine the diffraction elastic constants (DECs). Furthermore, the single-crystal elastic constants (SCEC) are refined from these experiments using different micromechanical models. The results show that each micromechanical model predicts a specific set of SCEC that well describes the elastic anisotropy of PBF-LB/IN718. KW - Mechanical Engineering KW - Mechanics of Materials KW - Condensed Matter Physics KW - General Materials Science PY - 2023 DO - https://doi.org/10.1016/j.matlet.2023.135305 SN - 0167-577X VL - 353 SP - 1 EP - 5 PB - Elsevier B.V. AN - OPUS4-58477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Seifert, Lando T1 - Junge GfKORR - Ideen für ein Netzwerk aus Young Professionals N2 - Der Berufsverband GfKORR - Gesellschaft für Korrosionsschutz e.V. will mit der "Jungen GfKORR" ein attraktives Angebot für junge Leute schaffen, sich fachübergreifend zu vernetzen und somit einen Einstieg in die fachliche Arbeit des Verbands zu bieten. Das Netzwerk befindet sich zurzeit im Aufbau. Auf der Jahrestagung 2023 in Berlin wurde die Idee für das Netzwerk erstmals vorgestellt. T2 - Jahrestagung der GfKORR - Gesellschaft für Korrosionsschutz e.V. CY - Berlin, Germany DA - 07.11.2023 KW - Junge GfKORR KW - Netzwerkbildung PY - 2023 AN - OPUS4-58799 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chen, Xinyue A1 - Dong, Ximan A1 - Zhang, Chuyan A1 - Zhu, Meng A1 - Ahmed, Essraa A1 - Krishnamurthy, Giridharan A1 - Rouzbahani, Rozita A1 - Pobedinskas, Paulius A1 - Gauquelin, Nicolas A1 - Jannis, Daen A1 - Kaur, Kawaljit A1 - Hafez, Aly Mohamed Elsayed A1 - Thiel, Felix A1 - Bornemann, Rainer A1 - Engelhard, Carsten A1 - Schönherr, Holger A1 - Verbeeck, Johan A1 - Haenen, Ken A1 - Jiang, Xin A1 - Yang, Nianjun T1 - Interlayer Affected Diamond Electrochemistry N2 - Diamond electrochemistry is primarily influenced by quantities of sp3‐carbon, surface terminations, and crystalline structure. In this work, a new dimension is introduced by investigating the effect of using substrate‐interlayers for diamond growth. Boron and nitrogen co‐doped nanocrystalline diamond (BNDD) films are grown on Si substrate without and with Ti and Ta as interlayers, named BNDD/Si, BNDD/Ti/Si, and BNDD/Ta/Ti/Si, respectively. After detailed characterization using microscopies, spectroscopies, electrochemical techniques, and density functional theory simulations, the relationship of composition, interfacial structure, charge transport, and electrochemical properties of the interface between diamond and metal is investigated. The BNDD/Ta/Ti/Si electrodes exhibit faster electron transfer processes than the other two diamond electrodes. The interlayer thus determines the intrinsic activity and reaction kinetics. The reduction in their barrier widths can be attributed to the formation of TaC, which facilitates carrier tunneling, and simultaneously increases the concentration of electrically active defects. As a case study, the BNDD/Ta/Ti/Si electrode is further employed to assemble a redox‐electrolyte‐based supercapacitor device with enhanced performance. In summary, the study not only sheds light on the intricate relationship between interlayer composition, charge transfer, and electrochemical performance but also demonstrates the potential of tailored interlayer design to unlock new capabilities in diamond‐based electrochemical devices. KW - Nanocrystalline diamond KW - Interfaces KW - Electrochemistry KW - TOF-SIMS KW - SEM PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621576 DO - https://doi.org/10.1002/smtd.202301774 SN - 2366-9608 VL - 9 IS - 2 SP - 1 EP - 10 PB - Wiley VHC-Verlag CY - Weinheim AN - OPUS4-62157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kreft, S. A1 - Radnik, Jörg A1 - Agostini, G. A1 - Pohl, M.-M. A1 - Gericke, E. A1 - Hoell, Armin A1 - Beller, M. A1 - Junge, H. A1 - Wohlrab, S. T1 - Dye activation of heterogeneous Copper(II)-Species for visible light driven hydrogen generation N2 - Heterogeneous Cu catalysts are widely used in photocatalytic hydrogen generation. The typical working mode includes the transfer of photo-induced charges from a semiconductor to CuO which itself is reduced to Cu2O to initiate the catalytic cycle. In this contribution a photosensitizer (dye), excited by visible light absorption, was used to transfer an electron to the CuO which after reduction catalyzes the water reduction to hydrogen. Several copper(II)-catalysts on high surface silica were prepared by impregnation or precipitation and applied in photocatalytic water reduction. The best catalyst CuO(Cl0.1)/SiO2, synthesized via incipient wetness impregnation of CuCl2 in MCM-41 and a following precipitation with NaOH, achieved a 6 times higher activity (1702 mmol h-1 g-1) compared to a previously investigated copper system (280 mmol h-1 g-1 for CuI) under the same reaction conditions. All materials were fully characterized by XRD, TEM and N2 sorption and further by magnetic resonance and X-ray methods EPR, ASAXS and XAS. In situ measurements evidenced a reduction of the initial Cu(II)-species, which confirms the (proposed) photocatalytic mechanism. KW - Hydrogen generation KW - CuO nanoparticles KW - Molecular sieves PY - 2019 DO - https://doi.org/10.1016/j.ijhydene.2019.04.006 VL - 44 IS - 53 SP - 28409 EP - 28420 PB - Elsevier Ltd. AN - OPUS4-49350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Influence of welding parameters on diffusible hydrogen content in high-strength steel welds using modified spray arc N2 - In order to satisfy the growing requirements towards lightweight design and resource efficiency in modern steel constructions, e.g. mobile cranes and bridges, high-strength steels with typical yield strength ≥ 690 MPa are coming into use to an increasing extent. However, these steels require special treatment in welding. The susceptibility for degradation of the mechanical properties in presence of hydrogen increases significantly with increasing yield strength. In case of missing knowledge about how and which amount of hydrogen is uptaken during welding, hydrogen assisted cracking (HAC) can be a negative consequence. Moreover, modern weld technology like the modified spray arc process enables welding of narrower weld seams. In this context, a reduced number of weld beads, volume and total heat input are technical and economic benefits. This work presents the influence of welding parameters on the diffusible hydrogen content in both singlepass and multi-layer welds. Different hydrogen concentrations were detected by varied contact tube distance, wire feed speed, arc length as well as varied arc type (transitional arc and modified spray arc). The results show, that all welding parameters have significant influence on the diffusible hydrogen concentration in the single-pass welds. By increasing the number of weld beads in case of multi-layer welding, the hydrogen concentration have been substantially reduced. Whereby, differences in hydrogen concentrations between both arc types are present. T2 - 70th IIW Annual Assembly, Commission II-A CY - Shanghai, People's Republic of China DA - 25.06.2017 KW - Hydrogen KW - MAG Welding KW - High-strength steels KW - Process parameters PY - 2017 AN - OPUS4-40953 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - The change of dna and protein radiation damage upon hydration: in-situ observations by near-ambient-pressure xps N2 - X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. Our results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further. Furthermore, first data about the degradation of single-stranded DNA binding-proteins (G5P / GV5 and hmtSSB) under vacuum and NAP-XPS conditions are presented. T2 - AVS69 CY - Portland, USA DA - 05.11.2023 KW - Base damage KW - Base loss KW - Cancer treatment KW - DNA KW - Protein KW - Proteins KW - Geant4 KW - Dosimetry KW - Microdosimetry KW - NAP-XPS KW - Xray photo electron spectrocopy KW - Radiation damage KW - Geant4-DNA KW - G5P KW - GVP KW - Hydroxyl radical KW - LEE KW - DEA KW - DET KW - ROS KW - Prehydrated electron KW - TOPAS KW - Near ambient pressure xray photo electron spectroscopy KW - SSB KW - DSB KW - Single-strand break (SSB) KW - ESCA KW - Single-stranded DNA-binding proteins KW - Reactive oxygen species PY - 2023 AN - OPUS4-58761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Radnik, Jörg A1 - Chemello, Giovanni A1 - Knigge, Xenia A1 - Al-Sabbgh, Dominik A1 - Hodoroaba, Vasile-Dan T1 - XPS, HAXPES, XRD and SEM datasets of functionalized graphene nanoplateletes N2 - The datasets from (Hard Energy) X-ray photoelectron spectroscopy, X-ray diffraction and Scanning Electron Microsopy are related to the publication G. Chemello, X. Knigge, D. Ciornii, B.P. Reed, A.J. Pollard, C.A. Clifford, T. Howe, N. Vyas, V.-D. Hodoroaba, J. Radnik "Influence of the morphology on the functionalization of graphene nanoplatelets analyzed by comparative photoelectron spectroscopy with soft and hard X-rays" Advanced Materials Interfaces (2023), DOI: 10.1002/admi.202300116. KW - Graphene related 2D materials KW - X-ray photoelectron spectroscopy KW - Hard-energy X-ray photoelectron spectroscopy KW - Scanning electron microscopy KW - Powder X-ray diffraction PY - 2023 DO - https://doi.org/10.5281/zenodo.7956497 PB - Zenodo CY - Geneva AN - OPUS4-57898 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schneider, Rudolf T1 - Antikörperbasierte vor-Ort-Analytik für das Monitoring der Eliminierung von Spurenstoffen in Kläranlagen N2 - Die Überwachung der Eliminierung von Spurenstoffen in Kläranlagen, wie sie die Neufassung der Kommunalabwasserrichtlinie vorschreibt, ruft einen Bedarf an vor-Ort-Analytik in den Kläranlagen hervor. Immunanalytische Methoden können vor Ort, z.B. in Form von Schnelltests, durchgeführt werden, ideal aber wären kontinuierlich arbeitende (Immuno-Bio)Sensoren. Antikörperbasierte Verfahren weisen als Flaschenhals immanent die Einschränkung auf, dass pro Analyt ein Antikörper zum Einsatz kommen muss und dass daher nur eine kleinere Anzahl von Substanzen analysiert werden kann. Die Indikatorenliste der Abwasserrichtlinie liefert hier einen Anhaltspunkt. Der Artikel weist schon bisher existierende Schnell- und Hochdurchsatzverfahren aus, ebenso wie Forschungsansätze für eine Sensorik, die online einsetzbar wäre und gibt einen Überblick über Defizite und Entwicklungen. KW - Antikörper KW - Immunoassay KW - Schnelltests KW - Biosensor PY - 2025 SN - 1618-3258 VL - 31 IS - 1 SP - 12 EP - 14 AN - OPUS4-63510 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumann, Christoph T1 - Design and optimization of integrated multimode interferometers (MMIs) for dual-polarization photonic biosensors for biomedical applications in a silicon-on-insulator platform N2 - Faster, more sensitive, and cost-efficient diagnostic tests are crucial, as conventional lab tests are slow and expensive, while rapid tests often lack specificity. Advancements in medical diagnostics are crucial for early disease detection, reducing costs and testing time. Optical biosensors, particularly multimode interferometers (MMIs), offer high sensitivity and integration potential for Point-of-Care applications [1-2]. This work introduces a novel MMI biosensor utilizing orthogonal TE and TM modes, significantly minimizing the footprint. T2 - SPIE Optics + Optoelectronics 2025 CY - Prague, Czech Republic DA - 23.05.2025 KW - Interferometry KW - Semiconductor KW - Chip KW - Point-of-Care applications KW - Biomarker PY - 2025 UR - https://www.spiedigitallibrary.org/conference-proceedings-of-spie/PC13527/PC135270R/Design-and-optimization-of-integrated-multimode-interferometers-MMIs-for-dual/10.1117/12.3056490.short DO - https://doi.org/10.1117/12.3056490 AN - OPUS4-63568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fünning, Tabea T1 - Optimization of local backside released micro-ring resonators for sensing applications using silicon photonic integrated circuits in a SOI technology N2 - The integration of photonic sensors into compact systems requires space-efficient solutions, such as the backside release of waveguides on silicon-on-insulator (SOI) platforms. This study presents the design, fabrication, and characterization of fully backside-released micro-ring resonators (MRRs) using the IHP SG25H5EPIC technology. The performance of rib and strip waveguides released by either dry or wet etching of the buried oxide (BOX) layer is evaluated. While wet etching provides low-loss release of rib waveguides, dry etching is required for the release of strip waveguides but results in increased waveguide losses and reduced quality factors. The effects of these release methods on critical coupling conditions, extinction ratio (ER), full width at half maximum (FWHM), and sensor performance are analyzed. The findings confirm that both etching strategies yield structures suitable for photonic sensing, with backside release enabling co-integration with microfluidic and optoelectronic components. These results contribute to the advancement of high-performance, integrated silicon photonic sensors. T2 - SPIE Optics + Optoelectronics 2025 CY - Prague, Czech Republic DA - 23.05.2025 KW - Rib and strip waveguides KW - Wet and dry etching KW - Microfluidics KW - Biosensor KW - Germanium photodiode KW - Q-Factor PY - 2025 UR - https://www.spiedigitallibrary.org/conference-proceedings-of-spie/13527/135270U/Optimization-of-local-backside-released-micro-ring-resonators-for-sensing/10.1117/12.3056481.short DO - https://doi.org/10.1117/12.3056481 AN - OPUS4-63571 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steglich, Patrick T1 - Towards monolithic integration of polymer-based electro-optical devices in silicon photonic integrated circuits using a 250 nm SOI technology N2 - Silicon-based photonic integrated circuits (PICs) in complementary metal oxide semiconductor (CMOS) technology are essential for next-generation communication systems and neuromorphic computing. However, silicon does not have efficient electro-optical (EO) effects. Since silicon limits the performance of current photonic devices, more advanced materials such as nonlinear optical polymers are needed to exploit the full potential of PICs. As a preliminary proof of concept, we demonstrate the quadratic EO effect and the electric field-induced EO effect using a Mach-Zehnder interferometer in conjunction with a co-integrated Ge photodiode. Our concept of monolithic integration could pave the way for next-generation PICs. T2 - SPIE Optics + Optoelectronics 2025 CY - Prague, Czech Republic DA - 05.06.2025 KW - CMOS KW - Silicon-based photonic integrated circuits KW - Mach-Zehnder interferometer KW - Ge-photodiode PY - 2025 UR - https://www.spiedigitallibrary.org/conference-proceedings-of-spie/13530/135300R/Towards-monolithic-integration-of-polymer-based-electro-optical-devices-in/10.1117/12.3056280.short DO - https://doi.org/10.1117/12.3056280 AN - OPUS4-63569 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steglich, Patrick A1 - Paul, Martin A1 - Fünning, Tabea A1 - Schumann, Christoph A1 - Mai, Christian A1 - Tannenberg, Robert A1 - Mai, Andreas ED - Cheben, Pavel ED - Čtyroký, Jiří ED - Molina-Fernández, Iñigo T1 - Towards monolithic integration of polymer-based electro-optical devices in silicon photonic integrated circuits using a 250nm SOI technology N2 - Photonic micro-ring resonators (MRR) are widely studied for their high sensitivity across applications like environmental monitoring, healthcare, and chemical analysis. Their evanescent field sensing requires partially unembedded waveguides compatible with CMOS processing. Our approach uses local backside etching with an additional buried oxide (BOX) etch to release waveguides while preserving the back-end of line (BEOL) structure, enabling spatial separation of the sensing area and electronics. The BOX etch critically affects sensor performance, as waveguide surface roughness can alter MRR properties and coupling. We analyzed MRR design variations, comparing wet and dry etching techniques for their effects on optical performance across rib and strip waveguides in quasi-TE and quasi-TM modes. Wafer-level measurements show that backside-released MRR achieve high extinction ratios with slightly reduced quality factors, advancing high-sensitivity photonic sensors. T2 - SPIE Optics + Optoelectronics 2025 CY - Prague, Czech Republic DA - 05.06.2025 KW - Photonic sensors KW - Micro-ring resonator (MRR) KW - Silicon on insulator (SOI) KW - CMOS KW - Local backside etching (LBE) PY - 2025 DO - https://doi.org/10.1117/12.3056280 VL - 13530 SP - 1 EP - 8 PB - SPIE CY - Bellingham, WA , USA AN - OPUS4-63587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Engelhard, Carsten T1 - On ICP-MS with Nanosecond Time Resolution: From Nanoparticles to Microplastics N2 - In this presentation, recent developments in inductively coupled plasma mass spectrometry (ICP-MS) instrumentation for particle characterization in complex mixtures will be reviewed. The current state-of-the-art in single-particle (sp) ICP-MS instrumentation for the detection and characterization of nanoparticles (NP) and microplastics (MPs) as well as remaining challenges will be discussed. While millisecond dwell times were used in the advent of spICP-MS, the use of microsecond dwell times helped to improve nanoparticle data quality and particle size detection limits. We could show that a custom-built high-speed data acquisition unit with microsecond time resolution (μsDAQ) can be used to successfully address issues of split-particle events and particle coincidence, to study the temporal profile of individual ion clouds, and to extend the linear dynamic range by compensating for dead time related count losses. Our latest development is an in-house built data acquisition system with nanosecond time resolution (nanoDAQ). Recording of the SEM signal by the nanoDAQ is performed on the nanosecond time scale with a dwell time of approximately 2 ns and enables detection of gold nanoparticles (AuNP) as small as 7.5 nm with a commercial single quadrupole ICP-MS instrument. [1] Analysis of acquired transient data is based on the temporal distance between detector events and a derived ion event density. It was shown that the inverse logarithm of the distance between detector events is proportional to particle size. Also, the number of detector events per particle can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. In addition to inorganic nanoparticles, first results on the detection of microplastics with spICP-MS will be discussed. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Nano KW - Microplastics KW - Nanoparticle Characterization KW - ICP-MS KW - Instrumentation PY - 2025 AN - OPUS4-63580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Engelhard, Carsten T1 - From Particles to PFAS: Recent Advances in Plasma-based Instrumentation Development N2 - In this presentation, recent advances in plasma spectrochemistry with hot and cold plasma sources for the direct detection of nanoparticles as well as per- and polyfluoroalkyl substances (PFAS) will be discussed. In the first part, single-particle inductively coupled plasma mass spectrometry (spICP-MS) with an in-house built data acquisition system with nanosecond time resolution (nanoDAQ) will be presented. In the second part, we turn to a cooler plasma source. Specifically, a flowing atmospheric-pressure afterglow source (FAPA) and its application for the direct mass spectrometric analysis of PFAS will be discussed. T2 - 20th European Winter Conference on Plasma Spectrochemistry CY - Berlin, Germany DA - 02.03.2025 KW - ICP-MS KW - Instrumentation KW - Nano KW - Nanoparticle Characterization KW - PFAS PY - 2025 AN - OPUS4-63581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - "On how to influence your results" - A review on carrier gas hot extraction parameters for hydrogen determination in welded specimens N2 - Carrier gas hot extraction (CGHE) is a commonly applied technique for determination of hydrogen in welded joints using a thermal conductivity device (TCD) for quantitative measurement. The CGHE is based on the accelerated hydrogen effusion due to thermal activation at elevated temperatures. The ISO 3690 standard suggests different specimen geometries as well as necessary minimum extraction time vs. temperature. They have the biggest influence on precise hydrogen determination. The present study summarizes the results and experience of numerous test runs with different specimen temperatures, geometries and factors that additionally influence hydrogen determination. They are namely: specimen surface (polished/as-welded), limited TCD sensitivity vs. specimen volume, temperature measurement vs. effects of PID-furnace controller as well as errors due to insufficient data assessment. Summarized, the temperature is the driving force of the CGHE. Two different methods are suggested to increase the heating rate up the reach the desired extraction temperature without changing the experimental equipment. Suggestions are made to improve the reliability of hydrogen determination depended on the hydrogen signal stability during extraction accompanied by evaluation of the recorded data. Generally, independent temperature measurement with calibration specimens is useful for further data analysis, especially if this data is used for calculation of trapping kinetics by thermal desorption analysis (TDA). T2 - IIW Annual Assembly and International Conference 2018, Meeting of Commission II-E CY - Nusa Dua, Bali Island, Indonesia DA - 15.07.2018 KW - Carrier gas hot extraction (CGHE) KW - Welding KW - ISO 3690 KW - Hydrogen KW - Experimental design PY - 2018 AN - OPUS4-45520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Escobar-Carranza, Cristian C. T1 - On the Detection of Microplastics by Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (FAPA-MS) N2 - Microplastics (MPs) are widespread pollutant particles that can be analyzed using Raman and FTIR spectroscopy combined with optical microscopy. Additionally, pyrolysis (Py) or thermal extraction and desorption (TED) coupled with gas chromatography-mass spectrometry (GC-MS) are used for the characterization of MPs.[1] However, sample throughput is limited due to GC separation. This work presents a feasibility study for the direct, rapid analysis of MPs using high-resolution mass spectrometry and a plasma-based ambient desorption/ionization source (FAPA, flowing atmospheric-pressure afterglow).[2] In earlier work, an in-house built ambient ionization source (modelled after the pin-to-capillary (p2c) FAPA design by Shelley et al. [3]) was coupled to HR-Orbitrap MS and used to characterize different MPs produced in-house from plastic materials including polystyrene (PS), polypropylene (PP), low-density polyethylene (LDPE), and polycarbonate (PC). Simultaneous detection of characteristic ions and particle imaging on a sampling mesh was feasible, with detection limits (LOD) for PS MPs at 311 µm in size and 1.3 mg in mass. Principal component analysis (PCA) was used for particle differentiation. This work presents an improved desorption/ionization approach using higher temperatures for desorption enhancement (approximately 500 °C, achieved with economical and commercially available parts) and a tailored source housing combined with a halo-shaped (h-FAPA) source configuration.[4] The scope was expanded to include MPs from poly(ethylene terephthalate) (PET), poly(methyl methacrylate) (PMMA), and poly(vinyl chloride) (PVC), sized 125–250 µm. Data visualization and interpretation were performed using Kendrick mass defect plots and other multivariate analysis tools. Compared to earlier results, h-FAPA-MS yielded at least 65% higher ion signals for selected ions in all MPs. These ions were detected mainly as protonated species [M+H]+. Higher thermal desorption temperatures aided in detecting all MPs, as the presence of higher molecular weight fragments added specificity to the analysis. Notably, experiments with the h-FAPA source demonstrated lower mass-based LODs for MPs than the p2c-FAPA source (e.g., 14 µg vs 1.3 mg for PS, respectively). T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Mass Spectrometry KW - Plasma KW - FAPA-MS KW - Microplastics PY - 2025 AN - OPUS4-63604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schütz, Désirée A.-M. T1 - Feasibility Study on the Adsorption of Environmental Contaminants onto Fresh and Aged Microplastics N2 - Microplastics (MPs) refer to plastic particles, fibers, or beads with sizes ranging from 100 nm to 5 mm in size. Their pervasive distribution as environmental contaminants have escalated into a significant global concern. Primary MPs are intentionally produced particles for industrial and commercial applications, such as exfoliants in personal care and cosmetic formulations. In contrast, secondary MPs are generated through the fragmentation and degradation of larger plastic materials, due to environmental weathering processes. [1] Due to their high surface area-to-volume ratio and hydrophobic nature, MPs have the potential to serve as vectors for the accumulation and transport of diverse organic contaminants, including polycyclic aromatic hydrocarbons (PAHs), perfluoroalkyl substances (PFAS), pharmaceuticals and personal care products (PPCPs), as well as trace metals such as silver, cadmium, chromium, and copper. In the environmental, MPs are subject to aging processes driven by factors such as temperature, ultraviolet radiation, oxygen, and chemical interactions with environmental toxins. This aging can induce significant alterations in their physicochemical properties, which, in turn, can affect the adsorption behavior. [2] Classical and alternative analytical methods such as high-performance liquid chromatography (HPLC) and ambient desorption/ionization high-resolution mass spectrometry (ADI-HR-MS) can help to study the adsorption potential. ADI-HR-MS allows rapid sample analysis with minimal preparation, providing results in under a minute, much faster than traditional chromatographic techniques. [3] This study aims to investigate the influence of aging and particle size on the ability of microplastics to act as vectors for environmental contaminants. Microplastics were prepared in-house and subjected to controlled aging conditions for 12, 24, 36, and 48 hours. Subsequently, the aged MPs were exposed in plastic-free containers to model solutions to simulate co-contaminants in the environment. Adsorption onto synthesized secondary microplastics, varying in size and aging status, was investigated at different time intervals with ambient MS and time-of-flight secondary ion mass spectrometry. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Mass Spectrometry KW - FAPA-MS KW - Microplastics KW - TOF-SIMS KW - Surface Analysis PY - 2025 AN - OPUS4-63606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmitt, Johannes T1 - Data acquisition system for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution N2 - This study presents our data acquisition system prototype for single particle inductively coupled plasma mass spectrometry (spICP-MS) with nanosecond time resolution (nanoDAQ) and a matching data processing approach for time-resolved data in the nanosecond range. The system continuously samples the secondary electron multiplier (SEM) detector signal with a dwell time of approximately 2 ns and enables detection of gold nanoparticles (AuNP) as small as 7.5 nm with a commercial single quadrupole ICP-MS instrument. [1] Analysis of acquired transient data is based on the temporal distance between detector events and a derived ion event density. It was shown that the inverse logarithm of the distance between detector events is proportional to particle size. Also, the number of detector events per particle can be used to calibrate and determine the particle number concentration (PNC) of a nanoparticle dispersion. [1] Particle-by-particle-based analysis of ion event density and other parameters derived from nanosecond time resolution show promising results. High data acquisition frequency of the systems allows recording of a statistically significant number of data points in 60 s or less, which leaves only the sample uptake and rinsing steps as remaining factors for limiting the total measurement time. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - ICP-MS KW - Instrumentation KW - Nano KW - Nanoparticle Characterization PY - 2025 AN - OPUS4-63603 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sachse, René A1 - Pfüger, Mika A1 - Velasco-Vélez, Juan-Jesús A1 - Sahre, Mario A1 - Radnik, Jörg A1 - Bernicke, Michael A1 - Bernsmeier, Denis A1 - Hodoroaba, Vasile-Dan A1 - Krumrey, Michael A1 - Strasser, Peter A1 - Kraehnert, Ralph A1 - Hertwig, Andreas T1 - Assessing optical and electrical properties of highly active IrOx catalysts for the electrochemical oxygen evolution reaction via spectroscopic ellipsometry N2 - Efficient water electrolysis requires highly active electrodes. The activity of corresponding catalytic coatings strongly depends on material properties such as film thickness, crystallinity, electrical conductivity, and chemical surface speciation. Measuring these properties with high accuracy in vacuum-free and nondestructive methods facilitates the elucidation of structure−activity relationships in realistic environments. Here, we report a novel approach to analyze the optical and electrical properties of highly active oxygen evolution reaction (OER) catalysts via spectroscopic ellipsometry (SE). Using a series of differently calcined, mesoporous, templated iridium oxide films as an example, we assess the film thickness, porosity, electrical resistivity, electron concentration, electron mobility, and interband and intraband transition energies by modeling of the optical spectra. Independently performed analyses using scanning electron microscopy, energy-dispersive X-ray spectroscopy, ellipsometric porosimetry, X-ray reflectometry, and absorption spectroscopy indicate a high accuracy of the deduced material properties. A comparison of the derived analytical data from SE, resonant photoemission spectroscopy, X-ray absorption spectroscopy, and X-ray photoelectron spectroscopy with activity measurements of the OER suggests that the intrinsic activity of iridium oxides scales with a shift of the Ir 5d t2g sub-level and an increase of p−d interband transition energies caused by a transition of μ1-OH to μ3-O species. KW - Spectroscopic ellipsometry KW - Electrocatalysis KW - Oxygen evolution reaction KW - Mesoporous iridium oxide films KW - Non-destructive ambient analysis KW - Intrinsic OER activity KW - Complementary methodology and metrology PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-516288 DO - https://doi.org/10.1021/acscatal.0c03800 SN - 2155-5435 VL - 10 IS - 23 SP - 14210 EP - 14223 PB - American Chemical Society AN - OPUS4-51628 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulka, M.W. A1 - Nie, C. A1 - Nickl, P. A1 - Kerkhoff, Y. A1 - Garg, A. A1 - Salz, D. A1 - Radnik, Jörg A1 - Grunwald, I. A1 - Haag, R. T1 - Surface-Initiated Grafting of Dendritic Polyglycerol from Mussel-Inspired Adhesion-Layers for the Creation of Cell-Repelling Coatings N2 - Biofouling is a major challenge in the application of textiles, biosensors, and biomedical implants. In the current work, a straightforward method for the solvent-free polymerization of antifouling dendritic polyglycerol (dPG) from mussel-inspired dendritic polyglycerol (MI-dPG) coatings on hydrophilic titanium dioxide (TiO2) and hydrophobic polydimethylsiloxane (PDMS) is reported. Surface characterization is performed by static water contact angle (CA) measurements, X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). Significant lower CA values are obtained after dPG grafting from MI-dPG-coated TiO2 and MI-dPG coated PDMS. Furthermore, XPS shows a time-dependent increase of the CO bond content upon dPG grafting from MI-dPG-coated TiO2 and MI-dPG-coated PDMS. Analysis of the surface morphology by SEM shows a clear time-dependent increase in the surface roughness upon dPG grafting from MI-dPG-coated TiO2 and MIdPG-coated PDMS. When the viability of two adhesive cell types is studied via LIVE/DEAD staining, a strong reduction in the cell density is observed after the dPG grafting from MI-dPG-coated TiO2 and MI-dPG-coated PDMS (a decrease of >95% in all cases). The combined results show that biocompatible but highly cell-repelling surfaces are efficiently constructed via the grafting of dPG from MI-dPG-coated TiO2 and MI-dPG-coated PDMS. KW - Repelling surface coatings KW - Dendritic polyglycerol KW - Mussel-inspired adhesives KW - Surface-initated grafting PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-516590 DO - https://doi.org/10.1002/admi.202000931 SN - 2196-7350 VL - 7 IS - 24 SP - 931 PB - Wiley VCH AN - OPUS4-51659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bennet, Francesca A1 - Müller, Anja A1 - Radnik, Jörg A1 - Hachenberger, Y. A1 - Jungnickel, H. A1 - Laue, P. A1 - Luch, A. A1 - Tentschert, J. T1 - Preparation of Nanoparticles for ToF-SIMS and XPS Analysis N2 - Nanoparticles have gained increasing attention in recent years due to their potential and application in different fields including medicine, cosmetics, chemistry, and their potential to enable advanced materials. To effectively understand and regulate the physico-chemical properties and potential adverse effects of nanoparticles, validated measurement procedures for the various properties of nanoparticles need to be developed. While procedures for measuring nanoparticle size and size Distribution are already established, standardized methods for analysis of their surface chemistry are not yet in place, although the influence of the surface chemistry on nanoparticle properties is undisputed. In particular, storage and preparation of nanoparticles for surface analysis strongly influences the analytical results from various methods, and in order to obtain consistent results, sample preparation must be both optimized and standardized. In this contribution, we present, in detail, some standard procedures for preparing nanoparticles for surface analytics. In principle, nanoparticles can be deposited on a suitable substrate from suspension or as a powder. Silicon (Si) Wafers are commonly used as substrate, however, their cleaning is critical to the process. For sample preparation from suspension, we will discuss drop-casting and spin-coating, where not only the cleanliness of the substrate and purity of the suspension but also its concentration play important roles for the success of the preparation methodology. For nanoparticles with sensitive ligand shells or coatings, deposition as powders is more suitable, although this method requires particular care in fixing the sample. KW - Titania nanoparticles KW - X-ray photoelectron spectroscopy KW - Secondary ion mass spectrometry KW - Surface chemisttry PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520103 UR - https://www.jove.com/video/61758 DO - https://doi.org/10.3791/61758 VL - 163 SP - e61758 AN - OPUS4-52010 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donskyi, Ievgen A1 - Nie, C. A1 - Ludwig, K. A1 - Trimpert, J. A1 - Ahmed, R. A1 - Quaas, E. A1 - Achazi, K. A1 - Radnik, Jörg A1 - Adeli, M. A1 - Haag, R. A1 - Osterrieder, K. T1 - Graphene Sheets with Defined Dual Functionalities for the Strong SARS-CoV-2 Interactions N2 - Search of new strategies for the inhibition of respiratory viruses is one of the urgent health challenges worldwide, as most of the current therapeutic agents and treatments are inefficient. Severe acute respiratory syndrome coronavirus 2 (SARSCoV-2) has caused a pandemic and has taken lives of approximately two Million people to date. Even though various vaccines are currently under development, virus, and especially its spike glycoprotein can mutate, which highlights a Need for a broad-spectrum inhibitor. In this work, inhibition of SARS-CoV-2 by graphene platforms with precise dual sulfate/alkyl functionalities is investigated. A series of graphene derivatives with different lengths of aliphatic chains is synthesized and is investigated for their ability to inhibit SARS-CoV-2 and feline coronavirus. Graphene derivatives with long alkyl chains (>C9) inhibit coronavirus replication by virtue of disrupting viral envelope. The ability of these graphene platforms to rupture viruses is visualized by atomic force microscopy and cryogenic electron microscopy. A large concentration window (10 to 100-fold) where graphene platforms display strongly antiviral activity against native SARS-CoV-2 without significant toxicity against human cells is found. In this concentration range, the synthesized graphene platforms inhibit the infection of enveloped viruses efficiently, opening new therapeutic and metaphylactic avenues against SARS-CoV-2. KW - Graphene KW - Graphene-based polyglycerol sulfates KW - SARS-CoV2 inhibitor KW - Virucidality PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520858 DO - https://doi.org/10.1002/smll.202007091 VL - 17 IS - 11 SP - 7091 PB - Wiley VCH AN - OPUS4-52085 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hünger, K.-J. A1 - Kositz, M. A1 - Danneberg, M. A1 - Radnik, Jörg T1 - Enrichment of aluminium in the near‐surface region of natural quartzite rock after aluminium exposure N2 - Alkali–silica reaction (ASR) is an ongoing problem that causes damage to concrete constructions and reduces their durability. Therefore, minimizing this undesired reaction is of great interest for both safety and economic reasons. Additives containing high aluminium content are very effective in reducing the release of silica and enhancing the durability of concrete; however, the mechanism for this effect is still under discussion. In this study, an enrichment of aluminium in the near‐surface region was observed for natural quartzite rock after storage in Al (OH)3 and metakaolin as aluminium sources, from which we conclude that the formation of aluminosilicate sheets of a few nanometres inhibits the silica release; this hypothesis is supported by high‐resolution spectra of Al 2p, Si 2p and O 1s. KW - Alkali-silica reaction KW - Quartzite rock KW - X-ray photoelectron spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-519394 DO - https://doi.org/10.1002/sia.6918 SN - 0142-2421 SP - 1 EP - 7 PB - Wiley VCH AN - OPUS4-51939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Krahl, T. A1 - Radnik, Jörg A1 - Wagner, Andreas A1 - Werner, W. S. M. A1 - Ritter, B. A1 - Kemnitz, E. A1 - Unger, Wolfgang T1 - Chemical in-depth analysis of (Ca/Sr)F2 core–shell like nanoparticles by X-ray photoelectron spectroscopy with tunable excitation energy N2 - The fluorolytic sol–gel synthesis is applied with the intention to obtain two different types of core–shell nanoparticles, namely, SrF2–CaF2 and CaF2–SrF2. In two separate fluorination steps for core and shell formation, the corresponding metal lactates are reacted with anhydrous HF in ethylene glycol. Scanning transmission electron microscopy (STEM) and dynamic light scattering (DLS) confirm the formation of particles with mean dimensions between 6.4 and 11.5 nm. The overall chemical composition of the particles during the different reaction steps is monitored by quantitative Al Kα excitation X-ray photoelectron spectroscopy (XPS). Here, the formation of stoichiometric metal fluorides (MF2) is confirmed, both for the core and the final core–shell particles. Furthermore, an in-depth analysis by synchrotron radiation XPS (SR-XPS) with tunable excitation energy is performed to confirm the core–Shell character of the nanoparticles. Additionally, Ca2p/Sr3d XPS intensity ratio in-Depth profiles are simulated using the software Simulation of Electron Spectra for Surface Analysis (SESSA). In principle, core–shell like particle morphologies are formed but without a sharp interface between calcium and strontium containing phases. Surprisingly, the in-depth chemical distribution of the two types of nanoparticles is equal within the error of the experiment. Both comprise a SrF2-rich core domain and CaF2-rich shell domain with an intermixing zone between them. Consequently, the internal morphology of the final nanoparticles seems to be independent from the synthesis chronology. KW - Metal fluorides KW - Sol-gel synthesis KW - Synchrotron radiation KW - X-ray photoelectron spectroscopy PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-522284 DO - https://doi.org/10.1002/sia.6937 SN - 0142-2421 VL - 53 IS - 5 SP - 494 EP - 508 PB - Wiley VCH AN - OPUS4-52228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Comprehensive characterization of Al-coated titania nanoparticles with electron microscopy and surface chemical analytics N2 - The wide use of nanoforms with at least one dimension below 100 nm in our daily life requires a detailed knowledge of their physicochemical properties which are needed for risk assessment or quality control. Therefore, a comprehensive characterization of these properties was considered as relevant including: chemical composition, crystallinity, particle size, particle shape, surface chemistry, and specific surface area (SSA). We want to discuss, how Scanning Electron Microscopy (SEM), Electron Probe Microanalysis (EPMA) in the version with energy dispersive X-ray spectroscopy (EDS), Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and X-ray Photoelectron Spectroscopy (XPS) can contribute to gain comprehensive insights into the nature of the nanoparticles. SEM results provide the particle size and shape (distribution). A quick identification of the main chemical elements present in the sample can be obtained with EDS, whereas XPS allows a more detailed chemical identification of the small nanoparticles below 20 nm or of the near-surface region of larger particles. ToF-SIMS is even much more surface-sensitive and leads to a deeper understanding of the surface chemistry of the nanoparticles. As exemplary samples, two Al-coated TiO2 samples in nanopowder form were chosen from the JRC repository, capped either with a hydrophilic or a hydrophobic organic shell. A focus of our case study was to show, how reliable, reproducible and traceable data can be obtained. Therefore, each step in the workflow of sample investigation must be described in detail. For the most of these steps, well-established standards are available. Usually, the conditions of the particular measurements with each analysis method are saved as meta-data in the common file formats. But other factors like sample preparation and data reduction approaches may influence the result of the investigations in a significant manner and must be described often in a separate file (as a protocol) together with the data file. For sensitive materials like nanoobjects, the preparation of the sample influences the results crucially, e.g. measured as suspension or as powders. Furthermore, data reduction like selection of relevant peaks in spectra or particles in images, background subtraction, peak deconvolution, models for the quantification of the spectra must be considered in the interpretation of the results ideally with associated individual measurement uncertainties. Only a detailed description of all these factors allows to obtain a comprehensive characterization with reliable, reproduceable and traceable data. Examples of standardized procedures of measurement or on data reduction will be highlighted. We thank for the funding from the European Unions’s Horizon 2020 for the project NanoSolveIt (grant agreement No. 814572) and for the project NANORIGO (grant agreement No. 814530). T2 - E-MRS Spring Meeting CY - Online meeting DA - 31.05.2021 KW - Scanning Electron Microscopy KW - Energy dispersive X-ray spectroscopy KW - Time-of-Flight Secondary Ion Mass Spectrometry KW - X-ray Photoelectron Spectroscopy KW - Titania nanoparticles PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527486 AN - OPUS4-52748 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rautenberg, Max A1 - Gernhard, M. A1 - Radnik, Jörg A1 - Witt, Julia A1 - Roth, C. A1 - Emmerling, Franziska T1 - Mechanochemical synthesis of fluorine-containing Co-doped zeolitic imidazolate frameworks for producing electrocatalysts N2 - Catalysts derived from pyrolysis of metal organic frameworks (MOFs) are promising candidates to replace expensive and scarce platinum-based electrocatalysts commonly used in polymer electrolyte membrane fuel cells. MOFs contain ordered connections between metal centers and organic ligands. They can be pyrolyzed into metal- and nitrogen-doped carbons, which show electrocatalytic activity toward the oxygen reduction reaction (ORR). Furthermore, metal-free heteroatom-doped carbons, such as N-F-Cs, are known for being active as well. Thus, a carbon material with Co-N-F doping could possibly be even more promising as ORR electrocatalyst. Herein, we report the mechanochemical synthesis of two polymorphs of a zeolitic imidazole framework, Co-doped zinc 2-trifluoromethyl-1H-imidazolate (Zn0.9Co0.1(CF3-Im)2). Time-resolved in situ X-ray diffraction studies of the mechanochemical formation revealed a direct conversion of starting materials to the products. Both polymorphs of Zn0.9Co0.1(CF3-Im)2 were pyrolyzed, yielding Co-N-F containing carbons, which are active toward electrochemical ORR. KW - Mechanochemistry KW - Metal-organic-frameworks KW - Nobel-metal free electrocatalysis PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-546833 DO - https://doi.org/10.3389/fchem.2022.840758 SN - 2296-2646 VL - 10 IS - 840758 SP - 1 EP - 13 PB - Frontiers Media CY - Lausanne AN - OPUS4-54683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heilmann, Maria A1 - Prinz, Carsten A1 - Bienert, Ralf A1 - Wendt, R. A1 - Kunkel, B. A1 - Radnik, Jörg A1 - Hoell, A. A1 - Wohlrab, S. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska T1 - Size-Tunable Ni–Cu Core–Shell Nanoparticles—Structure, Composition, and Catalytic Activity for the Reverse Water–Gas Shift Reaction N2 - A facile and efficient methodology is described for the solvothermal synthesis of size-tunable, stable, and uniform NiCu core–shell nanoparticles (NPs) for application in catalysis. The diameter of the NPs is tuned in a range from 6 nm to 30 nm and to adjust the Ni:Cu ratio from 30:1 to 1:1. Furthermore, the influence of different reaction parameters on the final NPs is studied. The NPs are structurally characterized by a method combination of transmission electron microscopy, anomalous small-angle X-ray scattering, X-ray absorption fine structure, and X-ray photoelectron spectroscopy. Using these analytical methods, it is possible to elucidate a core–shell–shell structure of all particles and their chemical composition. In all cases, a depletion from the core to the shell is observed, with the core consisting of NiCu alloy, surrounded by an inner Ni-rich shell and an outer NiO shell. The SiO2-supported NiCu core–shell NPs show pronounced selectivity of >99% for CO in the catalytic reduction of CO2 to CO using hydrogen as reactant (reverse water–gas shift reaction) independent of size and Ni:Cu ratio. KW - Nanoparticles KW - Core-shell KW - Catalysis PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543606 DO - https://doi.org/10.1002/adem.202101308 SN - 1438-1656 SP - 1 EP - 13 PB - Wiley VCH AN - OPUS4-54360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bernegger, Raphael T1 - Pulsed thermography on semitransparent materials - what has to be considered? N2 - Pulsed thermography is a well-known non-destructive testing technique and has proven to be a valuable tool for examination of material defects, to determine thermal material parameters, and the thickness of test specimens through calibration or mathematical models. However, the application to semitransparent materials is quite new and demanding, especially for semitransparent materials like epoxy, polyamide 12, or glass fiber reinforced polymers with epoxy or polyamide matrix. In order to describe the temporal temperature evolution in such materials, which are recorded with an infrared camera during pulse thermography experiments, much more influences have to be considered, compared to opaque materials: - The wavelength of the excitation source and the spectral range of the infrared camera - The angles between the specimen, the excitation source and the infrared camera - The area behind the specimen - The roughness of the material surface - The scattering mechanism within the material Here, we will consider all these influences and describe how they can be treated mathematically in analytical or numerical models (using COMSOL Multiphysics software). These models describe the temperature development during the pulse thermography experiment in reflection and transmission configuration. By fitting the results of the mathematical models to experimental data it is possible to determine the thickness or the optical and thermal properties of the specimen. T2 - 20-th International Conference on Photoacoustic and Photothermal Phenomena CY - Moscow, Russia DA - 07.07.2019 KW - Numerical simulation KW - Pulsed thermography KW - Semitransparent KW - Analytical model KW - Delamination KW - GFRP PY - 2019 AN - OPUS4-49215 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Morpho-Chemical Characterisation of Me-TiO2 Nanoparticles for Enhanced Photocatalytical Activity N2 - The conversion of solar energy into electricity and solar fuels is of crucial importance for a green and sustainable future. Water splitting using semiconductor photo-catalysts is considered a sustainable method to produce clean hydrogen (H2) fuel. Nevertheless, H2 photo-production efficiency remains still low, although extensive research works to understand better the mechanisms of the Hydrogen Evolution Reaction (HER) and the Oxygen Evolution Reaction (OER) are being carried out. In this respect, TiO2 is a key photoactive material, usually employed with a co-catalyst deposited onto the surface to enhance charge carriers’ separation and catalyze surface charge transfer reactions. The deposition of a co-catalyst on the TiO2 nanoparticle surface represents one successful way to enhance the activity of the photocatalyst through a modification of its surface and redox properties. In this context, high-resolution scanning electron microscopy coupled with elemental analysis by energy-dispersive X-ray spectroscopy (EDS) is fundamental for studying and understanding the effect of the nanoparticle morphology on the functional properties of shape-controlled TiO2 crystals (bipyramides, platelets, and elongated particles). Different types of metal-semiconductor combinations, TiO2 shapes and dopant metals (Ag, Pt, etc) and metal concentrations will be discussed. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Titania nanoparticles KW - Photocatalysis KW - Scanning electron microscopy KW - Energy dispersive X-ray spectroscopy PY - 2022 AN - OPUS4-54977 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Monavari, Mehran A1 - Prellwitz, Matthias A1 - Muth, Thilo A1 - Eichstädt, Sascha A1 - Koch, Claudia T1 - Quality-X: A Federated Digital Ecosystem for the Future Quality Infrastructure N2 - Harmonized and interoperable national Quality Infrastructure (QI) systems are essential for fostering cooperation, promoting mutual trust, and facilitating trade. The true potential of the QI is realized when its elements and actors are seamlessly integrated into a cohesive digital QI ecosystem. Recent developments towards industrial international data spaces enable such an ecosystem but require the integration of QI principles. Recognizing the lack of such a platform, Quality-X aims at setting the stage for the implementation of a QI ecosystem in international data spaces (IDS), GAIA-X and related German and European projects dedicated to secure data sharing. Quality-X is not about the construction of a platform; it is the creation of an inclusive QI ecosystem with harmonized interfaces. Instead of imposing rigid data structures, it prioritizes interoperability. Through the utilization of Decentralized Identifiers (DIDs), Verifiable Credentials, and Identity Hubs, Quality-X seeks seamless interactions across diverse service provider systems. This white paper introduces the concept and vision of Quality-X and discusses the general prerequisites for integrating QI processes within data spaces. Further on, we introduce existing testbeds, which will serve as an experimental proving ground for exploring various use cases related to the implementation of the vision of a QI-Digital. +++ Harmonisierte und interoperable nationale Qualitätsinfrastrukturen (QI) sind für die Förderung der Zusammenarbeit, des gegenseitigen Vertrauens und der Erleichterung des Handels unerlässlich. Das wahre Potenzial der QI kommt zum Tragen, wenn ihre Elemente und Akteure nahtlos in ein kohärentes digitales QI-Ökosystem integriert werden. Die jüngsten Entwicklungen hin zu industriellen internationalen Datenräumen ermöglichen ein solches Ökosystem, erfordern jedoch die Integration von QI-Prinzipien. Angesichts des Fehlens einer solchen Plattform zielt Quality-X darauf ab, die Voraussetzungen für die Umsetzung eines QI-Ökosystems in internationalen Datenräumen (IDS), GAIA-X und verwandten deutschen und europäischen Projekten zum sicheren Datenaustausch zu schaffen. Bei Quality-X geht es nicht um den Aufbau einer Plattform, sondern um die Schaffung eines umfassenden QI-Ökosystems mit harmonisierten Schnittstellen. Anstatt starre Datenstrukturen aufzuerlegen, steht die Interoperabilität im Vordergrund. Durch die Verwendung von dezentralen Identifikatoren (DIDs), überprüfbaren Berechtigungsnachweisen und Identitäts-Hubs strebt Quality-X eine nahtlose Interaktion zwischen verschiedenen Systemen von Dienstleistern an. Dieses Whitepaper stellt das Konzept und die Vision von Quality-X vor und erörtert die allgemeinen Voraussetzungen für die Integration von QI-Prozessen in Datenräumen. Darüber hinaus stellen wir bestehende Testbeds vor, die als experimentelles Versuchsfeld für die Erforschung verschiedener Anwendungsfälle im Zusammenhang mit der Umsetzung der Vision einer QI-Digital dienen sollen. KW - Quality Assurance KW - Quality Infrastructure KW - Data Spaces KW - Digitalization KW - Quality Management KW - Interoperability KW - Verification KW - Identification KW - Certificate KW - Datenräume KW - Qualitätsinfrastruktur KW - Gaia-X KW - Manufacturing-X KW - Catena-X KW - Datenökosystem KW - Qualitätssicherung KW - Qualitätsmanagement PY - 2023 UR - https://www.qi-digital.de/fileadmin/user_upload/website/publikationen/1022_Brosch%C3%BCre_Quality-X_v4.pdf SP - 1 CY - Berlin AN - OPUS4-59354 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Favres, Georges T1 - European Metrology Network (EMN) for Advanced Manufacturing N2 - The European Commission has identified Advanced Manufacturing and Advanced Materials as two of six Key Enabling Technologies (KETs). By fully utilizing these KETs, advanced and sustainable economies will be created. It is considered that Metrology is a key enabler for the advancement of these KETs. EURAMET, the association of metrology institutes in Europe, has strengthened the role of Metrology for these KETs by enabling the creation of a European Metrology Network for Advanced Manufacturing. The EMN is made up of National Metrology Institutes (NMIs) and Designated Institutes (DIs) from across Europe and was formally established in October 2021. The EMN aims to provide a high-level coordination of European metrology activities for the Advanced Materials and Advanced Manufacturing community. The EMN itself is organized in three sections representing the major stages of the manufacturing chain: 1) Advanced Materials, 2) Smart Manufacturing Systems, and 3) Manufactured Components & Products. The EMN for Advanced Manufacturing is engaging with stakeholders in the field of Advanced Manufacturing and Advanced Materials (Large companies & SMEs, industry organisations, existing networks, and academia), as well as the wider metrology community (including TCs) to provide input for the preparation of a Strategic Research Agenda (SRA) for Metrology for Advanced Manufacturing. This presentation will describe the progress in the development of the SRA by the EMN for Advanced Manufacturing. The metrology challenges identified across the various key industrial sectors, which utilise Advanced Materials and Advanced Manufacturing will be presented. The EMN for Advanced Manufacturing is supported by the project JNP 19NET01 AdvManuNet. T2 - 21st International Metrology Congress, CIM 2023 CY - Lyon (Chassieu), France DA - 07.03.2023 KW - Advanced Materials KW - EMN KW - European Metrology Network for Advanced Manufacturing, Strategic Research Agenda KW - SRA PY - 2023 AN - OPUS4-59208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - O'Connor, Daniel A1 - Evans, Alexander A1 - Balsamo, Alessandro A1 - Favres, Georges A1 - Przyklenk, Anita A1 - Bosse, Harald A1 - Phillips, Dishi T1 - European Metrology Network (EMN) for Advanced Manufacturing ─ Development of the Strategic Research Agenda (SRA) N2 - The European Commission has identified Advanced Manufacturing and Advanced Materials as two of six Key Enabling Technologies (KETs). It is considered that Metrology is a key enabler for the advancement of these KETs. Consequently, EURAMET, the association of metrology institutes in Europe, has strengthened the role of Metrology for these KETs by enabling the creation of a European Metrology Network (EMN) for Advanced Manufacturing. The EMN is comprised of National Metrology Institutes (NMIs) and Designated Institutes (DIs) from across Europe and was formally established in October 2021. The aim of the EMN is to provide a high-level coordination of European metrology activities for the Advanced Manufacturing community. The EMN itself is organized in three sections representing the major stages of the manufacturing chain: 1) Advanced Materials, 2) Smart Manufacturing Systems, and 3) Manufactured Components & Products. The EMN for Advanced Manufacturing is engaging with stakeholders in the field of Advanced Manufacturing (large companies & SMEs, industry organisations, existing networks, and academia), as well as the wider Metrology community, including Technical Committees, to provide input for the Strategic Research Agenda (SRA) on Metrology for Advanced Manufacturing. This contribution will give an overview about the first version of the SRA prepared by the EMN for Advanced Manufacturing T2 - Euspen, 23rd International Conference & Exhibitio CY - Copenhagen, Danmark DA - 12.06.2023 KW - European Metrology Network (EMN) KW - Advanced Manufacturing KW - Metrology KW - Strategic Research Agenda (SRA) PY - 2023 SP - 363 EP - 364 AN - OPUS4-59196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oster, Simon A1 - Scheuschner, Nils A1 - Chand, Keerthana A1 - Altenburg, Simon A1 - Gerlach, G. T1 - Potentials and challenges of deep-learning-assisted porosity prediction based on thermographic in-situ monitoring in laser powder bed fusion N2 - Laser powder bed fusion is one of the most promising additive manufacturing techniques for printing complex-shaped metal components. However, the formation of subsurface porosity poses a significant risk to the service lifetime of the printed parts. In-situ monitoring offers the possibility to detect porosity already during manufacturing. Thereby, process feedback control or a manual process interruption to cut financial losses is enabled. Short-wave infrared thermography can monitor the thermal history of manufactured parts which is closely connected to the probability of porosity formation. Artificial intelligence methods are increasingly used for porosity prediction from the obtained large amounts of complex monitoring data. In this study, we aim to identify the potential and the challenges of deep-learning-assisted porosity prediction based on thermographic in-situ monitoring. Therefore, the porosity prediction task is studied in detail using an exemplary dataset from the manufacturing of two Haynes282 cuboid components. Our trained 1D convolutional neural network model shows high performance (R² score of 0.90) for the prediction of local porosity in discrete sub-volumes with dimensions of (700 x 700 x 40) μm³. It could be demonstrated that the regressor correctly predicts layer-wise porosity changes but presumably has limited capability to predict differences in local porosity. Furthermore, there is a need to study the significance of the used thermogram feature inputs to streamline the model and to adjust the monitoring hardware. Moreover, we identified multiple sources of data uncertainty resulting from the in-situ monitoring setup, the registration with the ground truth X-ray-computed tomography data and the used pre-processing workflow that might influence the model’s performance detrimentally. T2 - XXXVII. Messtechnisches Symposium 2023 CY - Freiburg, Germany DA - 27.09.2023 KW - Porosity prediction KW - Defect detection KW - Laser powder bed fusion (PBF-LB/M, L-PBF) KW - Selective laser melting KW - Thermography KW - Machine learning PY - 2023 DO - https://doi.org/10.1515/teme-2023-0062 SN - 0171-8096 SN - 2196-7113 VL - 90 SP - 85 EP - 96 PB - De Gruyter CY - Berlin AN - OPUS4-58366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oster, Simon T1 - Potentials and challenges of deep-learning-assisted porosity prediction based on thermographic in-situ monitoring in PBF-LB/M N2 - Laser powder bed fusion is one of the most promising additive manufacturing techniques for printing complex-shaped metal components. However, the formation of subsurface porosity poses a significant risk to the service lifetime of the printed parts. In-situ monitoring offers the possibility to detect porosity already during manufacturing. Thereby, process feedback control or a manual process interruption to cut financial losses is enabled. Short-wave infrared thermography can monitor the thermal history of manufactured parts which is closely connected to the probability of porosity formation. Artificial intelligence methods are increasingly used for porosity prediction from the obtained large amounts of complex monitoring data. In this study, we aim to identify the potential and the challenges of deep-learning-assisted porosity prediction based on thermographic in-situ monitoring. Therefore, the porosity prediction task is studied in detail using an exemplary dataset from the manufacturing of two Haynes282 cuboid components. Our trained 1D convolutional neural network model shows high performance (R2 score of 0.90) for the prediction of local porosity in discrete sub-volumes with dimensions of (700 x 700 x 40) μm³. It could be demonstrated that the regressor correctly predicts layer-wise porosity changes but presumably has limited capability to predict differences in local porosity. Furthermore, there is a need to study the significance of the used thermogram feature inputs to streamline the model and to adjust the monitoring hardware. Moreover, we identified multiple sources of data uncertainty resulting from the in-situ monitoring setup, the registration with the ground truth X-ray-computed tomography data and the used pre-processing workflow that might influence the model’s performance detrimentally. T2 - XXXVII. Messtechnisches Symposium 2023 CY - Freiburg im Breisgau, Germany DA - 27.09.2023 KW - Porosity prediction KW - Defect detection KW - Laser Powder Bed Fusion (PBF-LB/M, L-PBF) KW - Selective Laser Melting KW - Thermography KW - Machine Learning PY - 2023 AN - OPUS4-59192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias T1 - Neue Möglichkeiten der Fehlersuche auf und unter der Oberfläche durch strukturierte Laserthermografie N2 - Das thermografische Nachweisprinzip beruht auf der Analyse von instationären Temperaturverteilungen, welche durch die Wechselwirkung eines von außen zugeführten Wärmestroms mit der inneren Geometrie des Prüfobjekts oder mit darin eingeschlossenen Inhomogenitäten verursacht werden. Eine äquivalente Beschreibung dieses wechselwirkenden Wärmestroms ist die Ausbreitung von Wärmewellen im Inneren des Prüfobjekts. Obwohl die Thermografie für die Erkennung einer Vielzahl von Inhomogenitäten und für die Prüfung verschiedenster Materialien geeignet ist, besteht die grundlegende Einschränkung in der diffusen Natur der Wärmewellen und der Notwendigkeit, ihre Wirkung nur an der Prüfobjektoberfläche radiometrisch messen zu können. Der fundamentale Nachteil von diffusen Wärmewellen gegenüber propagierenden Wellen, wie sie z. B. im Ultraschall vorkommen, ist die dadurch verursachte schnelle Verschlechterung der räumlichen Auflösung mit zunehmender Defekttiefe. Diese Verschlechterung schränkt in der Regel die Anwendbarkeit der Thermografie bei der Suche nach kleinen tiefliegenden Defekten ein. Ein vielversprechender Ansatz zur Verbesserung der räumlichen Auflösung und damit der Erkennungsempfindlichkeit und der Rekonstruktionsqualität in der thermografischen Prüfung liegt in der speziellen Formung dieser diffusen Wärmewellenfelder mittels strukturierter Laserthermografie bzw. photothermischer Anregung. Einige Beispiele sind: - Schmale rissartige Defekte unterhalb der Oberfläche können durch Überlagerung mehrerer interferierender Wärmewellenfelder mit hoher Empfindlichkeit detektiert werden, - Nahe beieinander liegende Defekte können durch mehrere Messungen mit unterschiedlichen Heizstrukturen getrennt werden, - Defekte in unterschiedlichen Tiefen können durch eine optimierte zeitliche Gestaltung der thermischen Anregungsfunktion unterschieden werden, - Schmale Risse auf der Oberfläche können durch robotergestütztes Scannen mit fokussierten Laserspots gefunden werden, - Defekte, die während der additiven Fertigung auftreten, können bereits im Bauraum und mit dem Fertigungslaser detektiert werden. Wir präsentieren die neuesten Ergebnisse dieser Technologie, die mit Hochleistungslasersystemen und modernen numerischen Methoden erzielt wurden. T2 - Thermographie-Kolloquium 2022 CY - Saarbrücken, Germany DA - 27.09.2022 KW - Thermografie KW - Laser KW - Laser-Thermografie KW - Super Resolution KW - Zerstörungsfreie Prüfung PY - 2022 AN - OPUS4-55973 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Breese, Philipp Peter T1 - In-situ defect detection for laser powder bed fusion with active laser thermography N2 - Defects are still common in metal components built with Additive Manufacturing (AM). Process monitoring methods for laser powder bed fusion (PBF-LB/M) are used in industry, but relationships between monitoring data and defect formation are not fully understood yet. Additionally, defects and deformations may develop with a time delay to the laser energy input. Thus, currently, the component quality is only determinable after the finished process. Here, active laser thermography, a non-destructive testing method, is adapted to PBF-LB/M, using the defocused process laser as heat source. The testing can be performed layer by layer throughout the manufacturing process. The results of the defect detection using infrared cameras are presented for a custom research PBF-LB/M machine. Our work enables a shift from post-process testing of components towards in-situ testing during the AM process. The actual component quality is evaluated in the process chamber and defects can be detected between layers. T2 - 2023 Annual International Solid Freeform Fabrication Symposium CY - Austin, TX, USA DA - 14.08.2023 KW - Additive Manufacturing KW - Additive Fertigung KW - Laser Powder Bed Fusion KW - Nondestructive Testing KW - Flying Spot Laser Thermography PY - 2023 AN - OPUS4-58137 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oster, Simon T1 - Machine Learning based defect detection in Laser Powder Bed Fusion utilizing thermographic feature data N2 - The formation of irregularities such as keyhole porosity pose a major challenge to the manufacturing of metal parts by laser powder bed fusion (PBF-LB/M). In-situ thermography as a process monitoring technique shows promising potential in this manner since it is able to extract the thermal history of the part which is closely related to the formation of irregularities. In this study, we investigate the utilization of machine learning algorithms to detect keyhole porosity on the base of thermographic features. Here, as a referential technique, x-ray micro computed tomography is utilized to determine the part's porosity. An enhanced preprocessing workflow inspired by the physics of the keyhole irregularity formation is presented in combination with a customized model architecture. Furthermore, experiments were performed to clarify the role of important parameters of the preprocessing workflow for the task of defect detection . Based on the results, future demands on irregularity prediction in PBF-LB/M are derived. T2 - International Conference on NDE 4.0 CY - Berlin, Germany DA - 24.10.2022 KW - Laser Powder Bed Fusion KW - Thermography KW - In-situ Monitoring KW - Convolutional Neural Networks PY - 2022 AN - OPUS4-56332 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernegger, Raphael A1 - Altenburg, Simon A1 - Maierhofer, Christiane T1 - Iterative numerical 2D-modelling for quantification of material defects by pulsed thermography N2 - This paper presents a method to quantify the geometry of defects such as flat bottom holes (FBH) and notches in opaque materials by a pulse thermography (PT) experiment and a numerical model. The aim was to precisely describe PT experiments in reflection configuration with a simple and fast numerical model in order to use this model and a fit algorithm to quantify defects within the material. The algorithm minimizes the difference between the time sequence of a line shaped region of interest (ROI) on the surface (above the defect) from the PT experiment and the numerical data. Therefore, the experimental data can be reconstructed with the numerical model. In this way, the defect depth of a notch or FBH and its width or diameter was determined simultaneously. A laser was used for heating which was widened to a top hat spatial profile to ensure homogeneous illumination (rectangular impulse profile in time). The numerical simulation considers heating conditions and takes thermal losses due to convection and radiation into account. We quantified the geometry of FBH and notches in steel and polyvinyl chloride plasticized (PVC-U) materials with an accuracy of < 5 %. KW - Pulsed thermography KW - Numerical modelling KW - Data reconstruction KW - Opaque materials KW - 2D model KW - Flat bottom holes KW - Notches PY - 2019 DO - https://doi.org/10.1063/1.5099719 SN - 0094-243X SP - 020015-1 EP - 11 PB - AIP AN - OPUS4-47974 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Oster, Simon A1 - Breese, Philipp Peter A1 - Ulbricht, Alexander A1 - Mohr, Gunther A1 - Altenburg, Simon T1 - A deep learning framework for defect prediction based on thermographic in-situmonitoring in laser powder bed fusion N2 - The prediction of porosity is a crucial task for metal based additive manufacturing techniques such as laser powder bed fusion. Short wave infrared thermography as an in-situ monitoring tool enables the measurement of the surface radiosity during the laser exposure. Based on the thermogram data, the thermal history of the component can be reconstructed which is closely related to the resulting mechanical properties and to the formation of porosity in the part. In this study, we present a novel framework for the local prediction of porosity based on extracted features from thermogram data. The framework consists of a data pre-processing workflow and a supervised deep learning classifier architecture. The data pre-processing workflow generates samples from thermogram feature data by including feature information from multiple subsequent layers. Thereby, the prediction of the occurrence of complex process phenomena such as keyhole pores is enabled. A custom convolutional neural network model is used for classification. Themodel is trained and tested on a dataset from thermographic in-situ monitoring of the manufacturing of an AISI 316L stainless steel test component. The impact of the pre-processing parameters and the local void distribution on the classification performance is studied in detail. The presented model achieves an accuracy of 0.96 and an f1-Score of 0.86 for predicting keyhole porosity in small sub-volumes with a dimension of (700 × 700 × 50) μm3. Furthermore, we show that pre-processing parameters such as the porosity threshold for sample labeling and the number of included subsequent layers are influential for the model performance. Moreover, the model prediction is shown to be sensitive to local porosity changes although it is trained on binary labeled data that disregards the actual sample porosity. KW - Laser Powder Bed Fusion (PBF-LB/M, L-PBF) KW - Selective Laser Melting (SLM) KW - SWIR thermography KW - Online monitoring KW - Flaw detection KW - Machine learning KW - Convolutional neural networks (CNN) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575148 DO - https://doi.org/10.1007/s10845-023-02117-0 SN - 0956-5515 SP - 1 EP - 20 PB - Springer AN - OPUS4-57514 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taparli, Ugur Alp A1 - Kannengießer, Thomas A1 - Cieslik, K. A1 - Mory, D. A1 - Griesche, Axel T1 - In situ chemical composition analysis of a tungsten-inert-gas austenitic stainless steel weld measured by laser-induced breakdown spectroscopy N2 - The chemical composition of a weld metal determines the resulting solidification mode of stainless steel and the consequent weld metal quality. In this work tungsten inert gas (TIG) welding of EN grade 1.4435 austenitic stainless steel was monitored using laser-induced breakdown spectroscopy (LIBS) for the in situ measurement of chemical composition changes. This research aims to prototype a real-time chemical composition analysis system for welding applications and prove the feasibility of such quality control loop. LIBS was used to investigate in situ the monitoring of metal vaporization during TIG welding. We found Mn vapor formation above the weld pool and subsequent condensation of Mn on the weld metal surface using LIBS. Post-weld line scans were conducted by LIBS on various welds produced with different welding currents. Local changes of Ni and Mn were observed at higher welding currents. The results are in good agreement with the literature and proved that LIBS can be used in situ to inspect the TIG welding process. T2 - 10th Euro-Mediterranean Symposium on Laser-Induced Breakdown Spectroscopy CY - Brünn, Czechia DA - 08.09.2019 KW - LIBS KW - Welding KW - Austenitic stainless steel KW - Metal vapor KW - In situ measurement PY - 2020 DO - https://doi.org/10.1016/j.sab.2020.105826 SN - 0584-8547 VL - 167 SP - 105826 PB - Elsevier B.V. CY - Amsterdam, Niederlande AN - OPUS4-50582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bühling, Benjamin A1 - Maack, Stefan T1 - Improving onset picking in ultrasonic testing by using a spectral entropy criterion N2 - In ultrasonic testing, material and structural properties of a specimen can be derived from the time-of-flight (ToF). Using signal features, such as the first peak or envelope maximum, to calculate the ToF is error-prone in multipath arrangements or dispersive and attenuating materials, which is not the case for the signal onset. Borrowing from seismology, researchers used the Akaike information criterion (AIC) picker to automatically determine onset times. The most commonly used formulation, Maeda's AIC picker, is reassessed and found to be based on inappropriate assumptions for signals often used in ultrasonic testing and dependent on arbitrary parameters. Consequently, an onset picker for ultrasonic through-transmission measurements is proposed, based on a spectral entropy criterion (SEC) to model the signal using the AIC framework. This SEC picker takes into account the spectral properties of the ultrasonic signal and is virtually free of arbitrary parameters. Synthetic and experimental data are used to compare the performance of SEC and AIC pickers. It is shown that the accuracy of onset picking is improved for densely sampled data. KW - Akaike information criterion picker KW - Nondestructive testing KW - Ultrasound KW - Time of flight PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-594284 UR - https://pubs.aip.org/asa/jasa/article/155/1/544/3061576/Improving-onset-picking-in-ultrasonic-testing-by DO - https://doi.org/10.1121/10.0024337 SN - 0001-4966 VL - 155 IS - 1 SP - 544 EP - 554 PB - AIP Publishing CY - Melville, NY, USA AN - OPUS4-59428 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Capabilities of using mobile platforms for monitoring hazard scenarios by the example of the RASEM project N2 - This presentation shows the capabilities of mobile platforms for monitoring hazard scenarios. As an example the RASEM project is presented. Furthermore two ideas for future work are shown, namely, Aerial-based Gas Tomography and Passive Smart Dust. T2 - Climate Change @ Fire Science Workshop CY - Berlin, Germany DA - 10.11.2022 KW - RASEM KW - Dust sensor KW - Low-cost KW - Sensor network KW - Passive Smart Dust KW - Gas Tomography PY - 2022 AN - OPUS4-56296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Soruco Aloisio, Ricardo T1 - Eine Infrastruktur für den digitalen Zwilling – Use Case H2-Tankstelle N2 - Im Rahmen von der BAM und anderen Partnern ins Leben gerufene Initiative „Digitale Qualitätsinfrastruktur“ ist der Fokus auf die Entwicklung von neuen Regelwerken und Zertifizierungsworkflows ausgerichtet. Dabei ist eine besondere Bedeutung dem Zusammenführen von Operational Technology (OT) und Informationstechnik (IT) beizumessen, wenn aktuelle Prozess- und Parameterdaten zuverlässig zur Verfügung gestellt werden sollen. In dem Use Case Wasserstofftankstelle werden digitale Abbilder erprobt, die u.a. der Kalibrierung von Sensoren, dem Nachweis über die Wasserstoffreinheit und der vorausschauenden Wartung dienen sollen. Großenteils der verfahrenstechnischen Bestandsanlagen, die sogenannten Brownfield-Anlagen, sind nach einem konservativen und hierarchischen Automatisierungskonzept ausgelegt. Hierbei können sämtliche Prozessdaten, besonders aus der Feldebene, einer oberen informationstechnische Ebene unzugänglich bleiben. Eine Brückentechnologie nach der NAMUR Open Architecture (NOA) soll möglichst viele Informationen und Daten aus der vorgegebenen Brownfield-Automatisierung sicher und rückwirkungsfrei zur Verfügung stellen. Zusätzliche Sensorik soll ebenso zu der Datenerweiterung beitragen und letztendlich den digitalen Zwilling, bzw. das digitale Abbild des verfahrenstechnischen Prozesses, ergänzen. Die Herausforderungen einer solchen Infrastruktur gelten vor allem einer universellen Kommunikationsschnittstelle und der Sicherheit. Darüber hinaus werden vorgeschlagene Normen und Empfehlungen untersucht und erprobt. T2 - Jahrestreffen der "Prozess-, Apparate- und Anlagentechnik" CY - Frankfurt am Main, Germany DA - 21.11.2022 KW - QI-Digital KW - Use-Case Wasserstofftankstelle KW - Automatisierung KW - Operational Technology KW - Digitaler Zwilling KW - NAMUR Open Architecture PY - 2022 AN - OPUS4-56402 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chan, George C.-Y. A1 - Hieftje, Gary M. A1 - Omenetto, Nicoló A1 - Axner, Ove A1 - Bengtson, Arne A1 - Bings, Nicolas H. A1 - Blades, Michael W. A1 - Bogaerts, Annemie A1 - Bolshov, Mikhail A. A1 - Broekaert, José A.C. A1 - Chan, WingTat A1 - Costa-Fernández, José M. A1 - Crouch, Stanley R. A1 - De Giacomo, Alessandro A1 - D’Ulivo, Alessandro A1 - Engelhard, Carsten A1 - Falk, Heinz A1 - Farnsworth, Paul B. A1 - Florek, Stefan A1 - Gamez, Gerardo A1 - Gornushkin, Igor B. A1 - Günther, Detlef A1 - Hahn, David W. A1 - Hang, Wei A1 - Hoffmann, Volker A1 - Jakubowski, Norbert A1 - Karanassios, Vassili A1 - Koppenaal, David W. A1 - Kenneth Marcus, R. A1 - Noll, Reinhard A1 - Olesik, John W. A1 - Palleschi, Vincenzo A1 - Panne, Ulrich A1 - Pisonero, Jorge A1 - Ray, Steven J. A1 - Resano, Martín A1 - Russo, Richard E. A1 - Scheeline, Alexander A1 - Smith, Benjamin W. A1 - Sturgeon, Ralph E. A1 - Todolí, José-Luis A1 - Tognoni, Elisabetta A1 - Vanhaecke, Frank A1 - Webb, Michael R. A1 - Winefordner, James D. A1 - Yang, Lu A1 - Yu, Jin A1 - Zhang, Zhanxia T1 - Landmark Publications in Analytical Atomic Spectrometry: Fundamentals and Instrumentation Development N2 - The almost-two-centuries history of spectrochemical analysis has generated a body of literature so vast that it has become nearly intractable for experts, much less for those wishing to enter the field. Authoritative, focused reviews help to address this problem but become so granular that the overall directions of the field are lost. This broader perspective can be provided partially by general overviews but then the thinking, experimental details, theoretical underpinnings and instrumental innovations of the original work must be sacrificed. In the present compilation, this dilemma is overcome by assembling the most impactful publications in the area of analytical atomic spectrometry. Each entry was proposed by at least one current expert in the field and supported by a narrative that justifies its inclusion. The entries were then assembled into a coherent sequence and returned to contributors for a round-robin review. KW - Analytical atomic spectrometry KW - Spectroscopy KW - Instrumental analysis PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-621588 DO - https://doi.org/10.1177/00037028241263567 SN - 1943-3530 VL - 78 SP - 1 EP - 456 PB - Sage CY - London AN - OPUS4-62158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Broicher, Cornelia A1 - Zeng, F. A1 - Pfänder, N. A1 - Frisch, M. A1 - Bisswanger, T. A1 - Radnik, Jörg A1 - Stockmann, Jörg M. A1 - Palkovits, S. A1 - Beine, A. K. A1 - Palkovits, R. T1 - Iron and Manganese Containing Multi-Walled Carbon Nanotubes as Electrocatalysts for the Oxygen Evolution Reaction - Unravelling Influences on Activity and Stability N2 - Hydrogen economy is a central aspect of future energy supply, as hydrogen can be used as energy storage and fuel. In order tomake water electrolysis efficient, the limiting oxygen evolution reaction (OER) needs to be optimized. Therefore, C-based composite materials containing earth-abundant Fe and Mn were synthesized, characterized and tested in the OER. For pyrolysis temperatures above 700°C N-rich multi-walled carbon nanotubes (MWCNT) are obtained. Inside the tubes Fe3C particles are formed, Fe and Mn oxides are incorporated in the carbon matrix and metal spinel nanoparticles cover the outer surface. The best catalyst prepared at 800°C achieves a low overpotential of 389 mV (at 10 mA/cm2) and high stability (22.6 h). From electrochemical measurements and characterization it can be concluded that the high activity is mainly provided by MWCNT, Fe3C and the metal oxides in the conductive carbon matrix. The metal spinel nanoparticles in contrast protect the MWCNT from oxidation and thereby contribute to the high stability. KW - Oxygen Evolution Reaction KW - Carbon Nanotubes KW - Stability PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513955 DO - https://doi.org/10.1002/cctc.202000944 VL - 12 IS - 21 SP - 1 EP - 8 PB - Wiley Online Libary AN - OPUS4-51395 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reed, B.P. A1 - Marchesini, S. A1 - Chemello, Giovanni A1 - Morgan, D.J. A1 - Vyas, N. A1 - Howe, T. A1 - Radnik, Jörg A1 - Clifford, C,A. A1 - Pollard, A.J. T1 - The influence of sample preparation on XPS quantification of oxygen-functionalised graphene nanoplatelets N2 - X-ray photoelectron spectroscopy (XPS) is widely used for characterising the chemistry of graphene-related two-dimensional materials (GR2M), however the careful preparation of the sample for analysis is important in obtaining representative quantifications. We report an investigation by three laboratories showing that the preparation method for oxygen-functionalised graphene nanoplatelet (GNP) powders has a significant effect on the homogeneous-equivalent elemental composition measured in XPS. We show that pressing GNP powders onto adhesive tapes, into recesses, or into solid pellets results in inconsistencies in the XPS quantification. The measured oxygen-to-carbon atomic ratio from GNP pellets depends upon the die pressure used to form them and the morphology of the GNPs themselves. We recommend that powder samples of GR2Ms are pelletised prior to XPS analysis to improve repeatability and reproducibility of measurements. KW - X-ray photoelectron spectroscopy KW - Graphene related two-dimensional materials (GR2M) KW - Pelletization KW - Powder PY - 2023 DO - https://doi.org/10.1016/j.carbon.2023.118054 SN - 0008-6223 VL - 211 SP - 1 EP - 6 PB - Elsevier Ltd. AN - OPUS4-57694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nickl, Philip A1 - Radnik, Jörg A1 - Azab, W. A1 - Donskyi, Ievgen T1 - Surface characterization of covalently functionalized carbon-based nanomaterials using comprehensive XP and NEXAFS spectroscopies N2 - Reliable and straightforward characterization and analysis of carbon-based nanomaterials on the atomic level is essential to exploring their potential for application. Here we use a combination of highly surface sensitive x-ray photoelectron (XP) spectroscopy and near edge x-ray absorption fine structure spectroscopy (NEXAFS) to study and quantify the covalent functionalization of nanographene and single-walled carbon nanotubes with nitrene [2 + 1]-cycloaddition. With this comprehensive analytical approach, we demonstrate that the π-conjugated system of functionalized carbon-based nanomaterials is preserved according to NEXAFS analysis, which is challenging to prove with XP spectroscopy investigation alone. Using this combination of analytical approaches, we show significant similarities after functionalization for various carbon-based nanomaterials. Both analytical methods are strongly suited to study possible post-modification reactions of functionalized carbon-based nanomaterials. KW - Graphene KW - Carbon nanotubes KW - Covalend functionalization PY - 2023 DO - https://doi.org/10.1016/j.apsusc.2022.155953 VL - 613 SP - 1 EP - 7 PB - Elsevier B.V. AN - OPUS4-56865 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane A1 - Thiel, Erik A1 - Altenburg, Simon A1 - Mohr, Gunther A1 - Thiede, Tobias A1 - Mishurova, Tatiana A1 - Paul, Andrea A1 - Kranzmann, Axel A1 - Hilgenberg, Kai A1 - Pittner, Andreas A1 - Bruno, Giovanni A1 - Sommer, Konstantin A1 - Gumenyuk, Andrey T1 - Quality control in additive manufacturing via in-situ monitoring and non-destructive testing N2 - More than 80 representatives of SMEs, industrial companies and research institutes met on September 12 at the workshop "Challenges in Additive Manufacturing: Innovative Materials and Quality Control" at BAM in Adlershof to discuss the latest developments in materials and quality control in additive manufacturing. In special lectures, researchers, users and equipment manufacturers reported on the latest and future developments in additive manufacturing. Furthermore, funding opportunities for projects between SMEs and research institutions on a national and European level were presented. T2 - Challenges in Additive Manufacturing: Innovative Materials and Quality Control CY - Berlin, Germany DA - 12.09.2018 KW - Additive manufacturing KW - Quality control KW - Non-destructive testing KW - In-situ monitoring PY - 2018 AN - OPUS4-46072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria T1 - Size-Tunable Ni-Cu Core-Shell Nanoparticles: Structure, Composition, and Catalytic Activity N2 - Nanoparticles (NPs) have become important materials for a variety of chemical technologies, including catalysis. One of the main challenges is the reduction of green house gases, such as CO2. One opportunity besides the capturing is the conversion to synthesis gas via the reverse water-gas shift reaction. A facile and efficient method is described for the solvothermal synthesis of size-tunable, stable, and uniform NiCu core-shell NPs. The diameter of the NPs can be tuned in a range from 6 nm to 30 nm and the Ni:Cu ratio from 30:1 to 1:1. The NPs are structurally characterized with combination of transmission electron microscopy, anomalous small-angle X-ray scattering, X-ray photoelectron spectroscopy, and X-ray absorption fine structure. Using these analytical methods, a core-shell-shell structure their chemical composition is elucidated. A depletion from the core to the shell is observed, with the core consisting of NiCu alloy, surrounded by an inner Ni-rich shell and an outer NiO shell. The SiO2-supported NiCu core-shell NPs show pronounced selectivity of >99% for CO in the catalytic reduction of CO2 to CO using hydrogen as reactant (reverse water–gas shift reaction). T2 - Nanoalloys: recent developments and future perspectives Faraday Discussion CY - London, UK DA - 21.09.2022 KW - Nanoparticles KW - Core-shell KW - Catalysis PY - 2022 AN - OPUS4-56831 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - How to measure the chemical composition of industrial graphene - New insights from an interlaboratory comparison N2 - International standards describing reliable protocols will facilitate the commercialization of graphene and related 2D materials. One physico-chemical key property next to flake size and thickness is the chemical composition of the material. Therefore, an ISO standard is under development with X-ray photoelectron spectroscopy having a prominent role. With its information depth of around 10 nm which is the similar length scale as the thickness as of particles of 2D materials consisting of a few monolayer XPS seems to be highly suitable for this purpose. Different sample preparation methods like pressing the powders onto adhesive tapes, into recesses, or into solid pellets result in inconsistencies in the quantification. For the validation of the quantification with XPS an interlaboratory comparison was initiated under the auspice of the “Versailles Project on Advanced Materials and Standards” (VAMAS). First results confirm that the sample preparation method (pellet vs. powder) influences the quantification results clearly. T2 - Characterization of Nanomaterials Colloquium CY - Berlin, Germany DA - 04.07.2023 KW - X-ray photoelectron spectroscopy KW - Functionalized graphene KW - Interlaboratory comparison PY - 2023 AN - OPUS4-57897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mohammadifar, E. A1 - Ahmadi, V. A1 - Gholami, M.F. A1 - Oehrl, A. A1 - Kolyvushko, O. A1 - Nie, C. A1 - Donskyi, Ievgen A1 - Herziger, S. A1 - Radnik, Jörg A1 - Ludwig, K. A1 - Böttcher, C. A1 - Rabe, J.P. A1 - Osterrieder, K. A1 - Azab, W. A1 - Haag, R. A1 - Adeli, M. T1 - Graphene-Assisted Synthesis of 2D Polyglycerols as Innovative Platforms for Multivalent Virus Interactions N2 - 2D nanomaterials have garnered widespread attention in biomedicine and bioengineering due to their unique physicochemical properties. However, poor functionality, low solubility, intrinsic toxicity, and nonspecific interactions at biointerfaces have hampered their application in vivo. Here, biocompatible polyglycerol units are crosslinked in two dimensions using a graphene-assisted strategy leading to highly functional and water-soluble polyglycerols nanosheets with 263 ± 53 nm and 2.7 ± 0.2 nm average lateral size and thickness, respectively. A single-layer hyperbranched polyglycerol containing azide functional groups is covalently conjugated to the surface of a functional graphene template through pH-sensitive linkers. Then, lateral crosslinking of polyglycerol units is carried out by loading tripropargylamine on the surface of graphene followed by lifting off this reagent for an on-face click reaction. Subsequently, the polyglycerol nanosheets are detached from the surface of graphene by slight acidification and centrifugation and is sulfated to mimic heparin sulfate proteoglycans. To highlight the impact of the two-dimensionality of the synthesized polyglycerol sulfate nanosheets at nanobiointerfaces, their efficiency with respect to herpes Simplex virus type 1 and severe acute respiratory syndrome corona virus 2 inhibition is compared to their 3D nanogel analogs. Four times stronger in virus Inhibition suggests that 2D polyglycerols are superior to their current 3D counterparts.2D nanomaterials have garnered widespread attention in biomedicine and bioengineering due to their unique physicochemical properties. However, poor functionality, low solubility, intrinsic toxicity, and nonspecific interactions at biointerfaces have hampered their application in vivo. Here, biocompatible polyglycerol units are crosslinked in two dimensions using a graphene-assisted strategy leading to highly functional and water-soluble polyglycerols nanosheets with 263 ± 53 nm and 2.7 ± 0.2 nm average lateral size and thickness, respectively. A single-layer hyperbranched polyglycerol containing azide functional groups is covalently conjugated to the surface of a functional graphene template through pH-sensitive linkers. Then, lateral crosslinking of polyglycerol units is carried out by loading tripropargylamine on the surface of graphene followed by lifting off this reagent for an on-face click reaction. Subsequently, the polyglycerol nanosheets are detached from the surface of graphene by slight acidification and centrifugation and is sulfated to mimic heparin sulfate proteoglycans. To highlight the impact of the two-dimensionality of the synthesized polyglycerol sulfate nanosheets at nanobiointerfaces, their efficiency with respect to herpes Simplex virus type 1 and severe acute respiratory syndrome corona virus 2 inhibition is compared to their 3D nanogel analogs. Four times stronger in virus Inhibition suggests that 2D polyglycerols are superior to their current 3D counterparts. KW - 2D Materials KW - Graphene template KW - Multivalency KW - Polyglycerol KW - Virus inhibition PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527726 DO - https://doi.org/10.1002/adfm.202009003 VL - 31 IS - 32 SP - 2009003 PB - Wiley VCH AN - OPUS4-52772 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Ziegler, Mathias A1 - Altenburg, Simon A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane A1 - Scheuschner, Nils A1 - Marquardt, E A1 - Mühlberger, W. A1 - Nagel, F. A1 - Neumann, E. A1 - Rohwetter, P. A1 - Rutz, F. A1 - Schwake, C. A1 - Schramm, S. A1 - Schwaneberg, F. A1 - Taubert, R. D. T1 - Thermografie und Strahlungsthermometrie - Stand und Trends N2 - In vielen Umgebungen, besonders bei hohen Temperaturen, korrosiven Umgebungen oder auf bewegten oder schlecht zugänglichen Flächen, kann die Temperatur nicht oder nur mit nicht akzeptablem Aufwand mit Berührungsthermometern gemessen werden. Diese Umgebungsbedingungen sind unter anderem in der chemischen Industrie, der Lebensmittel-, Metall-, Glas-, Kunststoff- und Papierherstellung sowie bei der Lacktrocknung anzutreffen. In diesen Bereichen kommen Strahlungsthermometer zum Einsatz. Der VDI-Statusreport zeigt typische Anwendungsfelder von nicht radiometrisch kalibrierten Wärmebildkameras und von radiometrisch kalibrierten Thermografiekameras. Um verlässlich mit spezifizierten Messunsicherheiten berührungslos Temperaturen zu messen, müssen die Strahlungsthermometer und Thermografiekameras nicht nur kalibriert, sondern radiometrisch und strahlungsthermometrisch umfassend charakterisiert werden. Auch die optische Materialeigenschaft, der spektrale Emissionsgrad und die Gesamtstrahlungsbilanz (Strahlung des Messobjekts und der Umgebung) sind bei der industriellen Temperaturmessung von großer Bedeutung. In den letzten Jahrzehnten ist dazu ein umfassendes technisches Regelwerk entstanden, das wir Ihnen mit diesem VDI-Statusreport vorstellen. Manche in den Richtlinien beschriebenen Kennwerte mögen abstrakt wirken. In diesem Statusreport zeigen wir an konkreten Beispielen, was diese Kenngrößen für die berührungslose Temperaturmessung bedeuten. Beispiele von Anwendungen zeigen, wo temperaturmessende Thermografiekameras und ausschließlich bildgebende Wärmebildkameras in der Praxis eingesetzt werden. Mit einer Analyse, welche Themen und Anwendungen derzeit besonders intensiv diskutiert werden, versuchen wir Trends für zukünftige Entwicklungen herauszuarbeiten. KW - Thermografie KW - Temperaturmessung PY - 2021 UR - https://www.vdi.de/ueber-uns/presse/publikationen/details/thermografie-und-strahlungsthermometrie-stand-und-trends SP - 1 EP - 40 PB - VDI Verein Deutscher Ingenieure e.V. CY - Düsseldorf AN - OPUS4-52904 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blume, Simon T1 - Exploiting Lithium Self-Absorption in a Laser-Induced Breakdown Plasma for Isotopic Analysis via Spatial Heterodyne Spectroscopy N2 - Lithium-ion batteries are ubiquitous in modern life. From powering consumer electronics to enabling electric mobility and energy storage, they are a key building block of a sustainable future. Determination of the ratio of the two naturally abundant stable isotopes, 7Li and 6Li, provides access to a wide variety of information, such as studying the aging processes of lithium-ion batteries or elucidating the isotopic fingerprinting of natural or recycled sources of lithium. However, accurately measuring the lithium isotope ratio in complex samples remains challenging, often requiring either extensive sample pretreatment or specialized equipment, thus impeding in-situ and high-throughput demands of global industries. Recognition and determination of the individual lithium isotopes with conventional laser-induced breakdown spectroscopy (LIBS) setups is nearly impossible. While LIBS offers several advantages, such as obviating time- and resource-intensive sample preparation and enabling rapid measurements, the high temperature (~20,000 K) of the plasma, as well as the Stark-broadening caused by the nascent free electrons spectrally broaden the atomic emission lines to such an extent that the isotopic shift of the lithium doublet at 670 nm cannot be resolved. Since, the excited state energy for this transition amounts to only 14,900 cm-1, lithium exhibits a pronounced self-absorption dip in the emission signal. This self-absorption dip is significantly less affected by the broadening effects, therefore, allowing for the resolution of the isotopic shift from its line shape. Spatial heterodyne spectroscopy (SHS) offers the superior resolution capabilities necessary to differentiate the individual isotopic contributions. To address the generally limited sensitivity of SHS, a high-repetition-rate (>10 kHz) laser allows the accumulation of more than 10,000 lasing events per spectral recording for a sufficient signal-to-noise ratio and gain statistical validity. Optical lithium fluoride serves as a model sample to showcase the analytical performance. Additionally, the impact of the laser parameters on the self-absorption will also be discussed. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Isotopic Analysis KW - Spatial Heterodyne Spectroscopy PY - 2025 AN - OPUS4-63559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Palásti, Dávid jenö T1 - Interferometric sensing in the UV range – Investigation and comparison of the all-reflective spatial heterodyne spectrometer designs N2 - Spatial heterodyne spectrometers (SHS) are optical interferometric devices, working in the UV and visible spectral ranges [1]. The most common SHS setup is similar to the Michelson interferometer, both utilizes a beam splitter in the incoming beam path. In case of the SHS the split beams are not aimed towards orthogonal mirrors, but reflective optical gratings, set under a selected angle. These optical gratings diffract the beams, the direction of every wavelength will depend on the grating constant and the angle of the gratings. The wavefronts belonging to different wavelengths are going to cross each other under a unique angle, resulting in a spatial interference, which is recorded by a digital camera. This relatively compact setup provides high resolution and light throughput, which properties were harnessed for tasks requiring good line separation and/or high sensitivity [2]. However, SHS are only applicable on wavelengths for which an adequate transmissive beam splitter is available like the visible range, but not the far UV. To overcome this limitation, different all-reflective designs were introduced [3]. These instruments utilize symmetric optical gratings for the splitting and recombination of the beams. Although these SHS devices solve the main limitations of the traditional ones, they come with their fair share of drawbacks as well, such as more complex arrangement and the requirement for more delicate tuning. The behaviour of the traditional SHS is well documented [4,5], but in regards of the all-reflective ones we have much less available information. In this current study we utilized computational modelling to predict the behaviour of the all-reflective SH spectrometers, with special attention to the effects of the different alignment errors. Later we utilize this knowledge to fine tune an SHS for sensing (LIBS, Raman) in the UV region. Furthermore, we are introducing two new all-reflective SHS setups and compering them to their older counterparts. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - SHS KW - Spectroscopy PY - 2025 AN - OPUS4-63556 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Jungnickel, H. A1 - Tentschert, J. A1 - Luch, A. A1 - Sogne, V. A1 - Maier, F. A1 - Burr, L. A1 - Schmid, D. A1 - Yoon, T.-H. A1 - Petters, R. A1 - Briffa, S.M. A1 - Valsami-Jones, E. T1 - Automation and Standardization—A Coupled Approach Towards Reproducible Sample Preparation Protocols for Nanomaterial Analysis N2 - Whereas the characterization of nanomaterials using different analytical techniques is often highly automated and standardized, the sample preparation that precedes it causes a bottleneck in nanomaterial analysis as it is performed manually. Usually, this pretreatment depends on the skills and experience of the analysts. Furthermore, adequate reporting of the sample preparation is often missing. In this overview, some solutions for techniques widely used in nano-analytics to overcome this problem are discussed. Two examples of sample preparation optimization by au-tomation are presented, which demonstrate that this approach is leading to increased analytical confidence. Our first example is motivated by the need to exclude human bias and focuses on the development of automation in sample introduction. To this end, a robotic system has been de-veloped, which can prepare stable and homogeneous nanomaterial suspensions amenable to a variety of well-established analytical methods, such as dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), field-flow fractionation (FFF) or single-particle inductively coupled mass spectrometry (sp-ICP-MS). Our second example addresses biological samples, such as cells exposed to nanomaterials, which are still challenging for reliable analysis. An air–liquid interface has been developed for the exposure of biological samples to nanomaterial-containing aerosols. The system exposes transmission electron microscopy (TEM) grids under reproducible conditions, whilst also allowing characterization of aerosol composition with mass spectrometry. Such an approach enables correlative measurements combining biological with physicochemical analysis. These case studies demonstrate that standardization and automation of sample preparation setups, combined with appropriate measurement processes and data reduction are crucial steps towards more reliable and reproducible data. KW - Sample preparation KW - Automation KW - Nanomaterial analysis KW - Standardization PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543988 DO - https://doi.org/10.3390/molecules27030985 VL - 27 IS - 3 SP - 1 EP - 22 PB - MDPI AN - OPUS4-54398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bennet, Francesca A1 - Opitz, R. A1 - Ghoreishi, N. A1 - Plate, K. A1 - Barnes, J.-P. A1 - Bellew, A. A1 - Bellu, A. A1 - Ceccone, G. A1 - de Vito, E. A1 - Delcorte, A. A1 - Franquet, A. A1 - Fumageli, F. A1 - Gilliland, D. A1 - Jungnickel, H. A1 - Lee, T.G. A1 - Poleunis, C. A1 - Rading, D. A1 - Shon, H.K. A1 - Spampinato, V. A1 - Son, J.G. A1 - Wang, F. A1 - Wang, Y.-C. A. A1 - Zhao, Y. A1 - Roloff, A. A1 - Tentschert, J. A1 - Radnik, Jörg T1 - VAMAS TWA2 interlaboratory comparison: Surface analysis of TiO2 nanoparticles using ToF-SIMS N2 - Due to the extremely high specific surface area of nanoparticles and corresponding potential for adsorption, the results of surface analysis can be highly dependent on the history of the particles, particularly regarding sample preparation and storage. The sample preparation method has, therefore, the potential to have a significant influence on the results. This report describes an interlaboratory comparison (ILC) with the aim of assessing which sample preparation methods for ToF-SIMS analysis of nanoparticles provided the most intra- and interlaboratory consistency and the least amount of sample contamination. The BAM reference material BAM-P110 (TiO2 nanoparticles with a mean Feret diameter of 19 nm) was used as a sample representing typical nanoparticles. A total of 11 participants returned ToF-SIMS data,in positive and (optionally) negative polarity, using sample preparation methods of “stick-and-go” as well as optionally “drop-dry” and “spin-coat.” The results showed that the largest sources of variation within the entire data set were caused by adventitious hydrocarbon contamination or insufficient sample coverage, with the spin-coating protocol applied in this ILC showing a tendency toward insufficient sample coverage; the sample preparation method or the participant had a lesser influence on results. KW - Secondary Ion Mass Spectrometry KW - VMAAS KW - Titania KW - Interlaboratory comparison KW - Reproducibility PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582290 DO - https://doi.org/10.1116/6.0002814 SN - 0734-2101 VL - 41 IS - 5 SP - 053210-1 EP - 053210-13 PB - AIP (American Institute of Physics) AN - OPUS4-58229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Broichert, C. A1 - Klingenhof, M. A1 - Frisch, M. A1 - Dresp, S. A1 - Kubo, N.M. A1 - Artz, J. A1 - Radnik, Jörg A1 - Palkovits, S. A1 - Beine, A.K. A1 - Strasser, P. A1 - Palkovits, R. T1 - Particle size-controlled synthesis of highperformance MnCo-based materials for alkaline OER at fluctuating potentials N2 - For the large-scale generation of hydrogen via water electrolysis the design of long term stable and active catalysts for the oxygen evolution reaction (OER) remains a key challenge. Most catalysts suffer from severe structural corrosion that becomes even more pronounced at fluctuating potentials. Herein, MnCo based cubic particles were prepared via a hydrothermal approach, in which the edge length of the micron-sized particles can be controlled by changing the pH value of the precursor solution. The cubes are composed of varying amounts of MnCo2O4, CoCO3 and a mixed (Mn/Co)CO3 phase. Structure–activity relationships were deduced revealing a volcano-type behavior for the intrinsic OER activity and fraction of spinel oxide phase. A low overpotential of 0.37 V at 10 mA cm−2 and a stability of more than 25 h was achieved in 1.0 M KOH using a rotating disc electrode (RDE) setup. The best performing catalyst material was successfully tested under dynamic process conditions for 9.5 h and shows a superior catalytic activity as anode for the Overall water splitting in an electrolyser setup in 1.0 M KOH at 333 K compared to a reference NiCo-spinel catalyst. KW - Water electrolysis KW - Oxygen evolution reaction KW - Structure activity relationships PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536050 DO - https://doi.org/10.1039/d1cy00905b SN - 2044-4753 VL - 11 IS - 12 SP - 7278 EP - 7286 PB - Royal Society of Chemistry AN - OPUS4-53605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pignatelli, Giuseppe T1 - Simultaneous temperature measurement during LMD by OES and thermography N2 - While sensors for monitoring the energy source, the melt pool size or temperatures during the process of metal-based Additive Manufacturing (AM) systems are commercially available, the impact of their results on the part quality are often unclear. In the BAM project ProMoAM, results of different process monitoring techniques are combined to achieve quality assurance for the produced parts during the build. Here, first results of simultaneous measurements of optical emission spectroscopy and thermography during the laser metal deposition process using 316L are presented. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Additive Manufacturing KW - Spectroscopy KW - Thermographie KW - LMD PY - 2019 AN - OPUS4-48525 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Afantitis, A. A1 - Melagraki, G. A1 - Isigonis, P. A1 - Tsoumanis, A. A1 - Varsou, D. D. A1 - Valsami-Jones, E. A1 - Papadiamantis, A. A1 - Ellis, L.-J. A. A1 - Sarimveis, H. A1 - Doganis, P. A1 - Karatzas, P. A1 - Tsiros, P. A1 - Liampa, I. A1 - Lobaskin, V. A1 - Greco, D. A1 - Serra, A. A1 - Kinaret, P. A. S. A1 - Saarimäki, L. A. A1 - Grafström, R. A1 - Kohonen, P. A1 - Nymark, P. A1 - Willighagen, E. A1 - Puzyn, T. A1 - Rybinska-Fryca, A. A1 - Lyubartsev, A. A1 - Jensen, K. A. A1 - Brandenburg, J. G. A1 - Lofts, S. A1 - Svendsen, C. A1 - Harrison, S. A1 - Maier, D. A1 - Tamm, K. A1 - Jänes, J. A1 - Sikk, L. A1 - Dusinska, M. A1 - Longhin, E. A1 - Rundén-Pran, E. A1 - Mariussen, E. A1 - El Yamani, N. A1 - Unger, Wolfgang A1 - Radnik, Jörg A1 - Tropsha, A. A1 - Cohen, Y. A1 - Lesczynski, J. A1 - Hendren, C. O. A1 - Wiesner, M. A1 - Winkler, D. A1 - Suzuki, N. A1 - Yoon, T. H. A1 - Choi, J.-S. A1 - Sanabria, N. A1 - Gulumian, M. A1 - Lynch, I. T1 - NanoSolveIT Project: Driving nanoinformatics research to develop innovative and integrated tools for in silico nanosafety assessment N2 - Nanotechnology has enabled the discovery of a multitude of novel materials exhibiting unique physicochemical (PChem) properties compared to their bulk analogues. These properties have led to a rapidly increasing range of commercial applications; this, however, may come at a cost, if an association to long-term health and environmental risks is discovered or even just perceived. Many nanomaterials (NMs) have not yet had their potential adverse biological effects fully assessed, due to costs and time constraints associated with the experimental assessment, frequently involving animals. Here, the available NM libraries are analyzed for their suitability for integration with novel nanoinformatics approaches and for the development of NM specific Integrated Approaches to Testing and Assessment (IATA) for human and environmental risk assessment, all within the NanoSolveIT cloud-platform. These established and well-characterized NM libraries (e.g. NanoMILE, NanoSolutions, NANoREG, NanoFASE, caLIBRAte, NanoTEST and the Nanomaterial Registry (>2000 NMs)) contain physicochemical characterization data as well as data for several relevant biological endpoints, assessed in part using harmonized Organisation for Economic Co-operation and Development (OECD) methods and test guidelines. Integration of such extensive NM information sources with the latest nanoinformatics methods will allow NanoSolveIT to model the relationships between NM structure (morphology), properties and their adverse effects and to predict the effects of other NMs for which less data is available. The project specifically addresses the needs of regulatory agencies and industry to effectively and rapidly evaluate the exposure, NM hazard and risk from nanomaterials and nano-enabled products, enabling implementation of computational ‘safe-by-design’ approaches to facilitate NM commercialization. KW - Nanoinformatics KW - Hazard assessment KW - (Quantitative) Structure-Active Relationships KW - Safe-by-design KW - Predictive modelling PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505952 DO - https://doi.org/10.1016/j.csbj.2020.02.023 VL - 18 SP - 583 EP - 602 PB - Elsevier B.V. AN - OPUS4-50595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nickl, Philip A1 - Hilal, T. A1 - Olal, D. A1 - Donskyi, Ievgen A1 - Radnik, Jörg A1 - Ludwig, K. A1 - Haag, R. T1 - A New Support Film for Cryo Electron Microscopy Protein Structure Analysis Based on Covalently Functionalized Graphene N2 - Protein adsorption at the air–water interface is a serious problem in cryogenic electron microscopy (cryoEM) as it restricts particle orientations in the vitrified ice-film and promotes protein denaturation. To address this issue, the preparation of a graphene-based modified support film for coverage of conventional holey carbon transmission electron microscopy (TEM) grids is presented. The chemical modification of graphene sheets enables the universal covalent anchoring of unmodified proteins via inherent surface-exposed lysine or cysteine residues in a one-step reaction. Langmuir–Blodgett (LB) trough approach is applied for deposition of functionalized graphene sheets onto commercially available holey carbon TEM grids. The application of the modified TEM grids in single particle analysis (SPA) shows high protein binding to the surface of the graphene-based support film. Suitability for high resolution structure determination is confirmed by SPA of apoferritin. Prevention of protein denaturation at the air–water interface and improvement of particle orientations is shown using human 20S proteasome, demonstrating the potential of the support film for structural biology. KW - Functionalized graphene KW - Transmission electron microsocpy KW - Protein structure PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-566443 DO - https://doi.org/10.1002/smll.202205932 SN - 1613-6810 SP - 2205932 PB - Wiley VCH AN - OPUS4-56644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ascher, Lena T1 - Imaging of Eu doped very small iron oxide nanoparticle in atherosclerotic plaques via LA-ICP-MS N2 - Atherosclerotic lesions can be visualized by magnetic resonance imaging (MRI) using very small iron oxide nanoparticles (VSOP). VSOP accumulate in atherosclerotic plaques and thus serve as an atherosclerosis probe. The aim of this project was to image the distribution of europium doped VSOP (Eu-VSOP) by laser ablation ICP-MS in histological thin cuts of the aortic root region of ApoE knockout mouse model that is rich in atherosclerotic plaques. In addition, it was investigated whether VSOP accumulation in the plaques correlates with other biomarkers of inflammation for example macrophages and altered endothelium to assess whether it correlates with instability or vulnerability of the plaque regions. For this purpose, antibodies were labeled with various lanthanide elements and correlated with the Eu-VSOP distribution using LA-ICP-MS in a multiplex measurement mode. T2 - ESAS/CANAS 2018 CY - Berlin, Germany DA - 20.03.2018 KW - Bioimaging KW - LA-ICP-MS KW - Immunoassay KW - Nanoparticle KW - Labeling PY - 2018 AN - OPUS4-45131 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kluge, Martin A1 - Habib, Abdel Karim A1 - van Wingerden, Kees T1 - Unterfeuerung von Flüssigwassersttofftanks - Topologie eines kritischen Behälterversagens N2 - In einer Versuchsreihe im Realmaßstab wurden drei Flüssigwasserstofftanks (LH2) unterfeuert. Hierbei sollte unter anderem geklärt werden, ob es, analog zu druckverflüssigten Gasen, zu einem BLEVE (Boiling Liquid Expanding Vapor Cloud Explosion) kommen kann. Die Experimente wurden auf dem Testareal Wasserstoffsicherheit des Testgeländes Technische Sicherheit der Bundesanstalt für Materialforschung und -prüfung (BAM-TTS) im Rahmen einer Forschungskooperation zwischen der BAM und Gexcon, als Teil des SH2IFT-Programms durchgeführt. Es handelte sich um doppelwandige, vakuumisolierte Tanks von 1 m³ Volumen. Die zylindrischen Tanks unterschieden sich durch ihre Ausrichtung (horizontal oder vertikal) und das verwendete Isoliermaterial (Perlit oder Mehrschichtisolierung (MLI). Der Füllgrad der Tanks betrug bei jedem der durchgeführten Tests etwa 35-40 %. Die Brandlast wurde homogen durch ein propangasbetriebenes Brennersystem erzeugt. Gemessen wurden die Bedingungen im Behälter (Temperaturen und Druck) sowie äußere Randbedingungen und Auswirkungen beim Versagen (Wärmestrahlung, Druckwellen, Flammenballentwicklung und Fragmentierung). Mit Bolometern wurde die Wärmestrahlung gemessen, die sowohl durch das Propanfeuer als auch durch einen möglichen Feuerball/BLEVE erzeugt wurde. Zur Messung der durch das Bersten von Behältern/BLEVEs erzeugten Druckwellen wurden sog. Pencil-Probes verwendet. Des Weiteren wurden mehrere Kameras zur Überwachung der Experimente eingesetzt: Normalbildkameras, Infrarot (IR)-Kameras und Hochgeschwindigkeitskameras, sowohl bodengestützt als auch mittels einer Drohne. Zwei der untersuchten Tanks, ein horizontaler und der vertikale, die beide mit Perlit isoliert waren, hielten der Brandbelastung stand, ohne dass es zu einem Behälterversagen kam. Der mit MLI isolierte horizontale Behälter barst nach 1 Stunde und 6 Minuten und erzeugte dabei einen Feuerball, Trümmerflug und eine Druckwelle. Neben der Beschreibung der Auswirkungen eines kritischen Versagens eines LH2-Tanks sind weitere Ziele der Arbeit die Identifizierung kritischer Behälterzustände sowie die Erstellung eines umfassendes Datensatzes der Trümmer des geborstenen Tanks. Die größten Abstände für kritische Abstände ergaben sich durch Fragmentwurf. Hier sollen 3D-Scans für die Verwendung in CAD und FEM Anwendungen bereitgestellt werden. Umfassende Daten zu den Fragmentwurfweiten, -massen und -positionen wurden bereits publiziert. Damit soll die Voraussetzung geschaffen werden, um vorhandene Wurfweitenmodelle, die bisher nur für einschalige Behälter konzipiert wurden auf ihre Eignung für mehrschalige Behälter zu überprüfen oder mögliche Anpassungen anhand der realen Daten vornehmen zu können. Zudem wurde damit begonnen die nicht geborstenen Tanks zu vermessen und zu zerlegen, um u.a. die Perlit-Schüttung auf Beeinträchtigungen durch den Transport und die Unterfeuerung zu untersuchen. T2 - Magdeburg-Köthener Brandschutz- und Sicherheitstagung 2024 CY - Magdeburg, Germany DA - 14.03.2024 KW - LH2 KW - Flüssigwasserstoff KW - Bleve KW - Tank KW - Bersten KW - Unterfeuerung PY - 2024 SN - 978-3-948749-42-2 SP - 117 EP - 126 CY - Magdeburg AN - OPUS4-59711 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Shedding light on global warming: high-resolution optical spectroscopy for magnesium isotope analysis N2 - Magnesium is a major element in the hydrosphere and biosphere, and it is direct correlated with the carbon cycle. Therefore, the study of its isotopic fractionation in sediments and sea water helps to understand the earth’s climate and global warming. Mg has three stable isotopes, 24Mg, 25Mg and 26Mg, and traditionally isotope amount ratios are measured by mass spectrometric methods. Their drawbacks include the high costs for instruments and their operation, experienced operators and elaborate time-consuming chromatographic sample preparation. Recently, an optical spectrometric method has been proposed as faster and low-cost alternative for the analysis of isotope ratios: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). For the determination of Mg isotope ratios in selected rock reference materials, the high-resolution molecular absorption spectrum of in-situ generated MgF molecule was studied applying multivariate analysis and the results compared with MC-ICP-MS. Samples were dissolved by acid digestion and Mg isotopes analyzed with and without matrix extraction. The absorption spectra were recorded for MgF for the electronic transition X 2Σ → B 2Σ+. The MgF spectrum is described as the linear combination of their isotopic components or isotopologues: 24MgF, 25MgF, and 26MgF. The isotope analysis was done by deconvolution of the MgF spectrum by partial least square regression (PLS). A PLS model was built and calibrated with enriched isotope spikes and certified reference materials. Spectra data was preprocessed by a derivate of second order and venetian blinds cross-validation was employed for finding the optimum latent variables. Finally, the model was refined by a genetic algorithm which identified the best subset of variables for a precise and accurate regression. Results are compatible with those obtained by MC-ICP-MS with an accuracy of ± 0.3‰ with uncertainties ranging between 0.02 to 0.6‰. This accuracy and precision discriminate the isotope fractionation in geological samples, and it is suitable for earth’s climate studies. T2 - Adlershofer Forschungsforum 2019 CY - Berlin, Germany DA - 11.11.2019 KW - Isotope analysis KW - Geological thermometer KW - Magnesium KW - Optical spectroscopy PY - 2019 AN - OPUS4-49890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Akhmetova, Irina A1 - Beyer, Sebastian A1 - Schutjajew, K. A1 - Tichter, T. A1 - Wilke, Manuel A1 - Prinz, Carsten A1 - B. Martins, Inês C. A1 - Al-Sabbagh, Dominik A1 - Roth, C. A1 - Emmerling, Franziska T1 - Cadmium benzylphosphonates - the close relationship between structure and properties N2 - Cadmium benzylphosphonate Cd(O3PBn)·H2O and its fluorinated derivates Cd(O3PBn-3F)·H2O, Cd(O3PBn-4F)·H2O, and Cd(O3PBn-F5)·H2O were synthesized mechanochemically. The Crystal structures of the compounds were determined based on powder X-ray diffraction (PXRD) data. The influence of the ligand substitution on the crystal structure of the metal phosphonate was determined. The hydrophobicity as a function of degree of fluorination was investigated using dynamic vapor sorption. KW - Mechanochemistry KW - Metal phosphonates KW - PXRD KW - DVS PY - 2019 DO - https://doi.org/10.1039/c9ce00776h VL - 21 SP - 5958 EP - 5964 PB - RSC Royal Society of Chemistry AN - OPUS4-49930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Michalik-Onichimowska, Aleksandra A1 - Beitz, T. A1 - Panne, Ulrich A1 - Löhmannsröben, H.-G. A1 - Riedel, Jens T1 - Laser ionization ion mobility spectrometric interrogation of acoustically levitated droplets N2 - Acoustically levitated droplets have been suggested as compartmentalized, yet wall-less microreactors for high-throughput reaction optimization purposes. The absence of walls is envisioned to simplify up-scaling of the optimized reaction conditions found in the microliter volumes. A consequent pursuance of high-throughput chemistry calls for a fast, robust and sensitive analysis suited for online interrogation. For reaction optimization, targeted Analysis with relatively low sensitivity suffices, while a fast, robust and automated sampling is paramount. To follow this approach, in this contribution, a direct coupling of levitated droplets to a homebuilt ion mobility spectrometer (IMS) is presented. The sampling, Transfer to the gas phase, as well as the ionization are all performed by a single exposure of the sampling volume to the resonant output of a mid-IR laser. Once formed, the nascent spatially and temporally evolving analyte ion cloud needs to be guided out of the acoustically confined trap into the inlet of the ion mobility spectrometer. Since the IMS is operated at ambient pressure, no fluid dynamic along a pressure Gradient can be employed. Instead, the transfer is achieved by the electrostatic potential gradient inside a dual ring electrode ion optics, guiding the analyte ion cloud into the first stage of the IMS linear drift tube accelerator. The design of the appropriate atmospheric pressure ion optics is based on the original vacuum ion optics design of Wiley and McLaren. The obtained experimental results nicely coincide with ion trajectory calculations based on a collisional model. KW - Ambient pressure laser ionization KW - Ionmobility spectrometry KW - Acoustic levitation KW - ion optics PY - 2019 DO - https://doi.org/10.1007/s00216-019-02167-5 VL - 411 IS - 30 SP - 8053 EP - 8061 PB - Springer CY - Heidelberg AN - OPUS4-50132 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria T1 - Synthesis of bimetallic nickel nanoparticles as catalysts for the Sabatier reaction N2 - Nanoparticles (NPs) have become important materials for a variety of chemical technologies. The enhanced surface-area-to-volume ratio of NPs, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles. Monodisperse monometallic Ni NPs were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the NPs are stable while the surface is not entirely covered. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni. Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage. T2 - Adlershofer Forschungsforum 2019 CY - Berlin, Germany DA - 11.11.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria T1 - Synthesis of bimetallic nickel nanoparticles for catalysis N2 - We present the synthesis of monodisperse monometallic Ni nanoparticles (NPs) and bimetallic NiCu respectively NiCo NPs. The NPs were investigated using SAXS, STEM, EDX, and XANES, showing that the NPs are size tunable and stable while the surface is not entirely covered. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4. T2 - 11th Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 04.12.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria T1 - Synthesis of bimetallic nickel nanoparticles as catalysts for the Sabatier reaction N2 - Nanoparticles (NP) have become important materials for a variety of chemical technologies. The enhanced surface-area-to-volume ratio of NPs, making them excellent for use as catalyst, in analytical assays, and for antimicrobial applications. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4, and could replace the rare earth elements such as Ru, PT, or Rh. In this work we describe the solvothermal synthesis of monometallic and bimetallic nickel nanoparticles. Monodisperse monometallic Ni NPs were synthesized using Oleylamin as solvent and reducing agent. The nanoparticles were investigated using small angle scattering (SAXS), scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX), showing that the NPs are stable while the surface is not entirely covered. However, Ni has a high propensity to undergo oxidation, and becoming deactivated by coke formation. Hence, we further explore the preparation of bimetallic NPs, where a second metal is added to stabilize the Ni. Bimetallic Cu-Ni NPs were synthesized by simultaneous solvothermal reduction. These bimetallic NPs exhibit excellent catalytic properties are promising candidates to be used as catalysts for efficient energy storage. T2 - 31. Tag der Chemie 2019 CY - Berlin, Germany DA - 11.07.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50171 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobina, E. A1 - Zimathies, Annett A1 - Prinz, Carsten A1 - Emmerling, Franziska A1 - de Santis Neves, R. A1 - Wang, H. A1 - Mizuno, K. A1 - Devoille, L. A1 - Steel, E. A1 - Ceyhan, A. A1 - Sadak, E. ED - Sobina, E. T1 - Final report of CCQM-K153 Measurement of Specific Adsorption A [mol/kg] of N-2 and Kr on nonporous SiO2 at LN temperature (to enable a traceable determination of the Specific Surface Area (BET) following ISO 9277) N2 - CCQM key comparison K-153 Measurement of Specific Adsorption A [mol/kg] of N-2 and Kr on nonporous SiO2 at LN temperature (to enable a traceable determination of the Specific Surface Area (BET) following ISO 9277) has been performed by the Surface Analysis Working Group (SAWG) of the Consultative Committee for Amount of Substance (CCQM). The objective of this key comparison is to compare the equivalency of the National Metrology Institutes (NMIs) and Designated Institutes (DIs) for the measurement of specific adsorption, BET specific surface area) of nonporous substances (sorbents, ceramics, catalytic agents, etc) used in advanced technology. In this key comparison, a commercial nonporous silicon dioxide was supplied as a sample. Eight NMIs participated in this key comparison, but only five NMI's have reported in time. All participants used a gas adsorption method, here nitrogen and (or) krypton adsorption at 77.3 K, for analysis according to the international standards ISO 15901-2 and 9277. In this key comparison, the degrees of equivalence uncertainties for specific adsorption nitrogen and krypton, BET specific surface area were established. KW - Nonporous SiO2 KW - Specific Adsorption of N-2 and Kr KW - BET specific surface area PY - 2019 DO - https://doi.org/10.1088/0026-1394/56/1A/08013 VL - 56 IS - 1A SP - 08013 PB - IOP publishing Ltd CY - Bristol, UK AN - OPUS4-50358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Separation of polysterene nanoparticles with different coatings using 2D off-line coupling of asymmetrical flow field flow fractionation and capillary electrophoresis N2 - The successful off-line coupling of asymmetrical flow field flow fractionation (AF4) and capillary electrophoresis (CE) for Separation of nanoparticles (NPs) with different surface coatings was shown. Two mixtures of polystyrene nanoparticles (PS-NPs) with comparable core sizes (20 nm and 50 nm) but different coatings (no coating/carboxyl-coated) were studied. Separation in either method resulted in non-baseline resolved or non-separated peaks. In contrast, two-dimensional off-line coupling of AF4 and CE resulted in clearly separated regions in their 2 D plots and can obviouly improve separation resolution. T2 - FFF 2020 CY - Wien, Austria DA - 23.02.2020 KW - Capillary electrophoresis KW - Nanoparticle PY - 2020 AN - OPUS4-50487 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - da Silva, D.A. A1 - Greiser, Sebastian A1 - Contro, J. A1 - Medeiros, V.L. A1 - Nery, J.G. A1 - Jäger, Christian T1 - 1H, 29Si and 119Sn double and triple resonance NMR spectroscopy of the small-pore framework sodium stannosilicate Na2SnSi3O9⋅2H2O N2 - The small-pore framework sodium stannosilicate AV-10, chemical composition Na2SnSi3O9⋅2H2O and known crystallographic structure, was synthesized by hydrothermal crystallization. This stannosilicate is built up of a three-dimensional network of corner-shared SiO4 tetrahedra and SnO6 octahedra. The SnO6 sites are linked to six SiO4 tetrahedra (Sn(6Si)) while each of the two crystallographically different SiO4 units are connected to two SnO6 and SiO4 units (Si(2Si,2Sn)). This material was used as model compound for developing a solid-state MAS NMR strategy aimed on the challenges and possibilities for structural studies, particularly considering the short and medium range order to verify the connectivity of SiO4 and SnO6 of such compounds despite the low natural abundances of 4.68% for 29Si and 8.59% for 119Sn nuclei as a real challenge. 29Si{119Sn} and 119Sn{29Si} REDOR (Rotational-Echo Double-Resonance) NMR measurements after 1H cross-polarization (CP) were carried out. The REDOR curves show a significant change after the “normal” quadratic short time evolution from which both (i) the shortest internuclear 29Si – 119Sn distances (and vice versa) and (ii) the number of corner-sharing SiO4 tetrahedra around the SnO6 octahedra (and vice versa) can be obtained. Based on these data, optimized 29Si {119Sn} and 119Sn{29Si} REPT-HMQC (Recoupled Polarization Transfer-Heteronuclear Multiple-Quantum Correlation, again after 1H CP) experiments were implemented, which directly show those heterogroup connectivity as correlation peaks in a 2D spectrum. This information was also obtained using 2D29Si{119Sn}-J-Coupling NMR experiments. Furthermore, 2D29Si INADEQUATE NMR experiments are also feasible, showing the connectivity of SiO4 tetrahedra. The combination of REDOR, REPT-HMQC, J-Coupling and INADEQUATE experiments yielded a complete analysis of the short and medium range structure of this microporous stannosilicate, in agreement with the previously published structure obtained Ab Initio from powder X-Ray diffraction data (XRD). KW - Stannosilicates KW - REDOR KW - REPT-HMQC KW - INADEQUATE PY - 2020 DO - https://doi.org/10.1016/j.ssnmr.2020.101661 SN - 0926-2040 VL - 107 SP - 101661 PB - Elsevier Inc. AN - OPUS4-50710 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oster, Simon T1 - Defect prediction on the Base of Thermographic features in Laser Powder Bed Fusion Utilizing Machine Learning Algorithms N2 - Avoiding the formation of defects such as keyhole pores is a major challenge for the production of metal parts by Laser Powder Bed Fusion (LPBF). The use of in-situ monitoring by thermographic cameras is a promising approach to detect defects, however the data is hard to analyze by conventional algorithms. Therefore, we investigate the use of Machine Learning (ML) in this study, as it is a suitable tool to model complex processes with many influencing factors. A ML model for defect prediction is created based on features extracted from process thermograms. The porosity information calculated from an x-ray Micro Computed Tomography (µCT) scan is used as reference. Physical characteristics of the keyhole pore formation are incorporated into the model to increase the prediction accuracy. Based on the prediction result, the quality of the input data is inferred and future demands on in-situ monitoring of LPBF processes are derived. T2 - Additive Manufacturing Benchmarks 2022 CY - Bethesda, MA, USA DA - 14.08.2022 KW - Laser Powder Bed Fusion KW - Thermography KW - In-situ Monitoring KW - Machine Learning KW - Defect prediction PY - 2022 AN - OPUS4-55591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ha, Q. L. M. A1 - Armbruster, U. A1 - Atia, Hanan A1 - Lund, H. A1 - Agostini, G. A1 - Radnik, Jörg A1 - Vuong, H. T. A1 - Martin, A. T1 - Development of active and stable low nickel content catalysts for dry reforming of methane N2 - Methane dry reforming (DRM) was investigated over highly active Ni catalysts with low metal content (2.5wt%) supported on Mg-Al mixed oxide. The aim was to minimize carbon Deposition and metal sites agglomeration on the working catalyst which are known to cause catalyst deactivation. The solids were characterized using N2 adsorption, X-ray diffraction, temperature-programmed reduction, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectroscopy. The results showed that MgO-Al2O3 solid solution phases are obtained when calcining Mg-Al hydrotalcite precursor in the temperature range of 550–800 °C. Such phases contribute to the high activity of catalysts with low Ni content even at low temperature (500 °C). Modifying the catalyst preparation with citric acid significantly slows the coking rate and reduces the size of large octahedrally coordinated NiO-like domains, which may easily agglomerate on the surface during DRM. The most effective Ni catalyst shows a stable DRM course over 60 h at high weight hourly space velocity with very low coke deposition. This is a promising result for considering such catalyst systems for further development of an industrial DRM technology. KW - Dry reforming of methane KW - Carbon dioxide KW - Ni PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-402904 DO - https://doi.org/10.3390/catal7050157 SN - 2073-4344 VL - 7 IS - 5 SP - 157, 1 EP - 157, 17 PB - MDPI AN - OPUS4-40290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Radnik, Jörg A1 - Dang, T. T. H. A1 - Gatla, S. A1 - Raghuwanshi, V. S. A1 - Tatchev, D. A1 - Hoell, A. T1 - Identifying the location of Cu ions in nanostructured SAPO-5 molecular sieves and its impact on the redox properties N2 - Combining X-ray Absorption Fine Spectroscopy (XAFS) with Anomalous Small-Angle X-ray Scattering (ASAXS) determines the location of Cu2+ ions in silicoaluminophosphate (SAPO-5) frameworks prepared by hydrothermal crystallization or impregnation. As expected, for the hydrothermally prepared sample, incorporation in the SAPO-5 framework was observed. For the first time preferential location of Cu2+ ions at the inner and outer surfaces of the framework is determined. Temperature-Programmed Reduction (TPR) and X-ray Photoelectron Spectroscopy (XPS) investigations demonstrated that such Cu2+ is stable in an argon (Ar) atmosphere up to 550 °C and can only be reduced under a hydrogen atmosphere. In contrast, Cu2+ deposited by impregnation on the pure SAPO-5 framework can be easily reduced to Cu+ in an Ar atmosphere. At lower Cu amounts, mononuclear tetrahedrally coordinated Cu species were formed which are relatively stable in the monovalent form. In contrast, at higher Cu amounts, CuO particles were found which change easily between the mono- and bivalent species. KW - Nanostructured material KW - Molecular sieves KW - X-ray absorption Fine Spectroscopy KW - Anomalous Small Angle X-ray Scattering KW - X-ray Photoelectron Spectroscopy PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-474793 DO - https://doi.org/10.1039/c8ra10417d SN - 2046-2069 VL - 9 IS - 12 SP - 6429 EP - 6437 PB - RSC AN - OPUS4-47479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Heinrich, Thomas A1 - Tougaard, S. A1 - Werner, W. S. M. A1 - Hronek, M. A1 - Kunz, Valentin A1 - Radnik, Jörg A1 - Stockmann, Jörg M. A1 - Hodoroaba, Vasile-Dan A1 - Benemann, Sigrid A1 - Nirmalananthan-Budau, Nithiya A1 - Geißler, Daniel A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy N2 - Core–shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core–shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a nonideal morphology. In this work, we investigated poly(tetrafluoroethylene)–poly(methyl methacrylate) (PTFE–PMMA) and poly(tetrafluoroethylene)–polystyrene (PTFE–PS) polymer CSNPs with a constant core diameter (45 nm) but varying shell thicknesses (4–50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE–PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE–PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA v2.0 was used to analyze the intensities of the elastic peaks, and the QUASES software package was employed to evaluate the shape of the inelastic background in the XPS survey spectra. For the first time, nanoparticle shell thicknesses are presented, which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS) of the PTFE–PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. As opposed to that, no variation is observed in the PCA score plots of the PTFE–PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM. KW - XPS KW - T-SEM KW - ToF-SIMS KW - Core-shell nanoparticles PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499165 DO - https://doi.org/10.1021/acs.jpcc.9b09258 VL - 123 IS - 49 SP - 29765 EP - 29775 PB - American Chemical Society CY - Washington, DC AN - OPUS4-49916 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Seeburg, Dominik A1 - Liu, Dongjing A1 - Radnik, Jörg A1 - Atia, Hanan A1 - Pohl, Marga-Martina A1 - Schneider, Matthias A1 - Martin, Andreas A1 - Wohlrab, Sebastian T1 - Structural changes of highly active Pd/MeOx (Me = Fe, Co, Ni) during catalytic methane combustion N2 - Fe2O3, Co3O4 and NiO nanoparticles were prepared via a citrate method and further functionalized with Pd by impregnation. The pure oxides as well as Pd/Fe2O3, Pd/Co3O4, and Pd/NiO (1, 5 and 10 wt % Pd) were employed for catalytic methane combustion under methane lean (1 vol %)/oxygen rich (18 vol %, balanced with nitrogen) conditions. Already, the pure metal oxides showed a high catalytic activity leading to complete conversion temperature of T100 ≤ 500 °C. H2-TPR (Temperature-programmed reduction) experiments revealed that Pd-functionalized metal oxides exhibited enhanced redox activity compared to the pure oxides leading to improved catalytic combustion activity at lower temperatures. At a loading of 1 wt % Pd, 1Pd/Co3O4 (T100 = 360 °C) outperforms 1Pd/Fe2O3 (T100 = 410 °C) as well as 1Pd/NiO (T100 = 380 °C). At a loading of 10 wt % Pd, T100 could only be slightly reduced in all cases. 1Pd/Co3O4 and 1Pd/NiO show reasonable stability over 70 h on stream at T100. XPS (X-ray photoelectron spectroscopy) and STEM (Scanning transmission electron microscopy) investigations revealed strong interactions between Pd and NiO as well as Co3O4, respectively, leading to dynamic transformations and reoxidation of Pd due to solid state reactions, which leads to the high long-term stability. KW - Methane total oxidation KW - Methane removal KW - Carbon dioxide KW - X-ray photoelectron spectroscopy PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-439412 DO - https://doi.org/10.3390/catal8020042 SN - 2073-4344 VL - 8 IS - 2 SP - Article 42, 1 EP - 13 PB - MDPI AN - OPUS4-43941 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tu, Z. A1 - Donskyi, Ievgen A1 - Qiao, H. A1 - Zhu, Z. A1 - Unger, Wolfgang A1 - Hackenberger, C. P. R. A1 - Chen, W. A1 - Adeli, M. A1 - Haag, R. T1 - Graphene Oxide-Cyclic R10 Peptide Nuclear Translocation Nanoplatforms for the Surmounting of Multiple-Drug Resistance N2 - Multidrug resistance resulting from a variety of defensive pathways in Cancer has become a global concern with a considerable impact on the mortality associated with the failure of traditional chemotherapy. Therefore, further research and new therapies are required to overcome this challenge. In this work, a cyclic R10 peptide (cR10) is conjugated to polyglycerol-covered nanographene oxide to engineer a nanoplatform for the surmounting of multidrug resistance. The nuclear translocation of the nanoplatform, facilitated by cR10 peptide, and subsequently, a laser-triggered release of the loaded doxorubicin result in efficient anticancer activity confirmed by both in vitro and in vivo experiments. The synthesized nanoplatform with a combination of different features, including active nucleus-targeting, highloading capacity, controlled release of cargo, and photothermal property, provides a new strategy for circumventing multidrug resistant cancers. KW - Graphen Oxide KW - Nanoplatform KW - Cancer PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510061 DO - https://doi.org/10.1002/adfm.202000933 VL - 30 IS - 35 SP - 2000933 PB - Wiley VCH AN - OPUS4-51006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stockmann, Jörg M. A1 - Radnik, Jörg A1 - Bütefisch, S. A1 - Busch, I. A1 - Weimann, T. A1 - Passiu, C. A1 - Rossi, A. A1 - Unger, Wolfgang T1 - A new test specimen for the determination of the field of view of small-area X-ray photoelectron spectrometers N2 - Small-area/spot photoelectron spectroscopy (SAXPS) is a powerful tool for the investigation of small surface features like microstructures of electronic devices, sensors or other functional surfaces, and so forth. For evaluating the quality of such microstructures, it is often crucial to know whether a small signal in a spectrum is an unwanted contamination of the field of view (FoV), defined by the instrument settings, or it originated from outside. To address this issue, the d80/20 parameter of a line scan across a chemical edge is often used. However, the typical d80/20 parameter does not give information on contributions from the long tails of the X-ray beam intensity distribution or the electron-optical system as defined by apertures. In the VAMAS TWA2 A22 project “Applying planar, patterned, multi-metallic samples to assess the impact of analysis area in surface-chemical analysis,” new test specimen was developed and tested. The here presented testing material consists of a silicon wafer substrate with an Au-film and embedded Cr circular and square spots with decreasing dimensions from 200 μm down to 5 μm. The spot sizes are traceable to the length unit due to size measurements with a metrological SEM. For the evaluation of the FoV, we determined the Au4f intensities measured with the center of the FoV aligned with the center of the spot and normalized to the Au4f intensity determined on the Au-film. With this test specimen, it was possible to characterize, as an example, the FoV of a Kratos AXIS Ultra DLD XPS instrument. T2 - ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Field of view KW - Reference material KW - Selected area XPS KW - Small-area XPS KW - Small-spot XPS PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509902 DO - https://doi.org/10.1002/sia.6831 SN - 1096-9918 VL - 52 IS - 12 SP - 890 EP - 894 PB - John Wiley & Sons Ltd AN - OPUS4-50990 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agostini, G. A1 - Radnik, Jörg T1 - Spectroscopy in Catalysis N2 - Knowledge-based catalyst development is always an interaction between preparation, analysis and catalytic testing. Only if these three factors fit together can success be expected. For the analytic side of this triangle, spectroscopic methods play a crucial role. Whereas with diffraction, scattering and microscopy, decisive insights into the structure and morphology of the catalysts can be obtained, spectroscopy produces new knowledge about the chemical nature of the catalyst, e.g., its bonding and valence states. KW - Spectroscopy KW - Catalysis KW - Operando KW - In situ PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506507 DO - https://doi.org/10.3390/catal10040408 VL - 10 IS - 4 SP - 408 PB - MDPI CY - Basel AN - OPUS4-50650 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Müller, Anja A1 - Heinrich, Thomas A1 - Tougaard, S. A1 - Werner, W. S. M. A1 - Hronek, M. A1 - Kunz, Valentin A1 - Radnik, Jörg A1 - Stockmann, Jörg M. A1 - Hodoroaba, Vasile-Dan A1 - Benemann, Sigrid A1 - Nirmalananthan-Budau, Nithiya A1 - Geißler, Daniel A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Correction to "Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy" N2 - This is a corrigendum to the original article "Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy" that was published in "The journal of physical chemistry C", vol. 123 (2019), no. 49 pp. 29765-29775. PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-505451 DO - https://doi.org/10.1021/acs.jpcc.0c00027 SN - 1932-7447 SN - 1932-7455 VL - 124 IS - 6 SP - 3923 PB - American Chemical Society CY - Washington, DC AN - OPUS4-50545 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kazlagić, Anera A1 - Vogl, Jochen A1 - Gluth, Gregor A1 - Stephan, D. T1 - Provenancing of cement using elemental analyses and isotope techniques – The state-of-the-art and future perspectives N2 - With the aim of identifying the origin and the manufacturer of a cement, a reliable procedure that provides unambiguous results is needed. Such procedure could resolve practical issues in damage research, liability issues and forensic investigations. A substantial number of attempts for fingerprinting of building materials, including cement, has already been carried out during the last decades. Most of them were based on concentration analysis of the main elements/components. This review provides an overview of provenance studies of cement and the main approaches commonly used. Provenance studies of cement via isotope techniques are also presented and discussed as representatives of the state-of-the-art in the field. Due to the characteristic properties and the occurrence of carefully selected isotope ratios, unique fingerprints of different kinds of materials can be provided by these methods. This property has largely been explored in various scientific fields such as geo- and cosmochemistry, food forensics, archaeology, geochronology, biomedical studies, and climate change processes. However, the potential of isotope techniques in cement and concrete research for provenance studies has barely been investigated. Therefore, the review outlines a suitable approach using isotope ratios, which could lead to reliable provenancing of cementitious materials in the future. KW - Cement KW - Sr isotopes KW - Provenance PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533762 DO - https://doi.org/10.1039/d1ja00144b VL - 36 IS - 10 SP - 2030 EP - 2042 PB - The Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-53376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pietsch, Franziska T1 - Selection of resistance in bacterial biofilms grown on antimicrobial surfaces in a multidrug environment N2 - Background Bacterial biofilms are regarded as the most common cause of chronic infections and are often associated with medical devices, such as implants and catheters. Bacteria growing in biofilms produce a protective, extracellular matrix, which enables them to tolerate much higher antimicrobial concentrations than free-living bacteria and survive long enough to acquire antimicrobial resistance. Preventive and therapeutic strategies against biofilm infections in clinical settings commonly involve the application of multiple antimicrobials: biocidal coatings on the biomaterials and systemically administered antibiotics. This frequent practice harbors the risk of the development of cross-resistance via shared resistance mechanisms between antimicrobials used in material coatings and administered antibiotics. Aim Our goal is to determine how bacteria adapt to antimicrobials during biofilm formation on surfaces coated with antimicrobials and how population dynamics within biofilms affect the transmission of resistance mutations. Specifically, we want to identify antimicrobial-antibiotic-combinations that select for and against antibiotic resistance in biofilms by following the population dynamics of resistant and susceptible strains in competition assays on a single cell level. Methodology To study the effect of antimicrobial-antibiotic exposure on resistance development and population dynamics on bacterial biofilms in a multidrug environment, we will grow Pseudomonas aeruginosa on glass surfaces with and without antimicrobial coatings and expose them to antibiotics. First, we will screen in vitro for combinations of antibiotics and antimicrobials that select for and against antibiotic resistance. Second, effective combinations will be chosen for in-depth investigations during bacterial adhesion and of mature biofilms of resistant and susceptible genotypes. Third, based on the outcome of the screen and the obtained mechanistic understanding we will choose a clinical example in which we study the relevance of our findings in biofilms grown in vivo. Relevance Studying the biointerfacial interactions between bacterial biofilms and medical devices in terms of population dynamics as well as on single cell level during multidrug selection will help us understand how drug resistance develops and spreads in persistent biofilm infections. Based on our findings we aim to provide clinical recommendations for improved administration of antibiotics/antimicrobials in combination with medical device materials in order to mitigate against biofilm associated antimicrobial resistance. T2 - Biofilms 8 Conference CY - Aarhus, Denmark DA - 27.05.2018 KW - Resistance KW - Antimicrobials PY - 2018 AN - OPUS4-46524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, Holger A1 - Knizia, Christian A1 - Kuhne, Maren A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - LC–ELISA as a contribution to the assessment of matrix effects with environmental water samples in an immunoassay for estrone (E1) N2 - Estrone (E1), a metabolite of the estrogenic hormones 17β-estradiol (β-E2) and 17α-estradiol (α-E2), is itself a potent estrogen which can have a significant impact on the hormonal balance. Due to ist high potential for adverse effects on human health and aquatic life even at pg/L to ng/L levels, its appearance in water should be monitored. E1 has also been considered a marker substance for the presence of other estrogens. This study presents a newly developed direct competitive enzymelinked immunosorbent assay (ELISA) for quantification of E1 in environmental water samples using new monoclonal antibodies. The quantification range of the ELISA is 0.15 μg/L to 8.7 μg/L E1, and the limit of detection is around 60 ng/L for not pre-concentrated water samples. A pre-concentration step after careful selection of suitable phases for SPE was developed, too. The influence of organic solvents and natural organic matter on the ELISA was assessed. The high selectivity of the monoclonal antibody was demonstrated by determining the cross-reactivity against 20 structurally related compounds. For the assessment of matrix effects, a concept (“LC–ELISA”) is thoroughly exploited, i.e., separating complex samples by HPLC into 0.3 min fractions and determination of the apparent E1 concentration. Furthermore, fractions with interferences for nontarget/suspected-target analysis can be assigned. A dilution approach was applied to distinguish between specific interferences (cross-reactants) and non-specific interferences (matrix effects). In the determination of 18 environmental samples, a good agreement of the E1 concentration in the respective fractions was obtained with mean recoveries of 103 % to 132 % comparing ELISA to LC–MS/MS. KW - Validierung KW - Immunoassay KW - Matrixeffekte KW - Abwasser KW - Oberflächenwasser KW - ELISA KW - LC-MS/MS KW - Hormone KW - Endokrine Disruptoren PY - 2018 DO - https://doi.org/10.1007/s00769-018-1351-7 SN - 1432-0517 SN - 0949-1775 VL - 23 IS - 6 SP - 349 EP - 364 PB - Springer CY - Heidelberg AN - OPUS4-46891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abad Andrade, Carlos Enrique A1 - Florek, S. A1 - Becker-Ross, H. A1 - Huang, M.-D. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Radtke, Martin A1 - Lippitz, Andreas A1 - Hodoroaba, Vasile-Dan A1 - Schmid, Thomas A1 - Heinrich, Hans-Joachim A1 - Recknagel, Sebastian A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Zirconium permanent modifiers for graphite furnaces used in absorption spectrometry: understanding their structure and mechanism of action N2 - The mechanism of action of zirconium permanent modifiers on graphite surfaces was investigated in order to understand its influence on the analytical signal in atomic and molecular absorption spectrometry (AAS/MAS). For this, the molecule formation of CaF was studied, which is used for the indirect analytical determination of fluorine in high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). The kinetics of this reaction was established by monitoring its molecular spectrum at different atomisation temperatures. An Arrhenius plot showed a pseudo-first order reaction with respect to fluorine (n = 1). An intermediate state was isolated, and its structure was elucidated by spectroscopic methods: scanning electron microscopy with energy dispersive X-ray spectroscopy (SEMEDX), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XANES and EXAFS), and Raman microspectroscopy. We propose here a mechanism, where ZrO2 acts as a heterogeneous catalyst: after a pyrolytic step, an intermediate state of ZrO(OCaF) is activated, and at higher temperatures, CaF(g) is released from the zirconium-coated graphite surface. No evidence of the formation of zirconium carbide was found. Consequently, as the CaF formation is catalysed by a heterogeneous catalyst, surface modifications with ZrO2 nanoparticles and ZrO xerogels were investigated in order to increase the surface area. Their influence was evaluated in the molecule formation of CaF, CaCl, CaBr, and CaI. Graphite furnace modification with zirconium oxide nanoparticles proves to be the best choice for fluorine analysis with a signal enhancement of more than eleven times with respect a non-coated graphite furnace. However, the influence of zirconium modifications in the analytical signals of Cl, and I is lower than the F signals or even negative in case of the Br. Understanding zirconium modifiers as heterogeneous catalysts offers a new perspective to AAS and MAS, and reveals the potential of surface analytical methods for development of improved permanent modifiers and graphite furnace coatings. KW - Zirconium KW - HR-CS-MAS KW - Graphite furnace KW - Nanoparticles KW - Xerogel KW - Calcium monofluoride KW - Absorption spectrometry PY - 2018 UR - https://pubs.rsc.org/en/content/articlelanding/2018/ja/c8ja00190a DO - https://doi.org/10.1039/C8JA00190A SN - 0267-9477 VL - 33 IS - 12 SP - 2034 EP - 2042 PB - Royal Society of Chemistry AN - OPUS4-46775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - "Keine Dienstmagd" - Analytical Sciences in Action N2 - Analytical Sciences has developed from Ostwald’s “unentbehrlichen Dienstmagd” to a chemical discipline at the core of many of today’s fundamental and applied scientific problems and innovations. An atomic or molecular understanding of basic processes in chemistry, soft matter physics, materials and life science is enabled only through new analytical methods and instrumentation. Similar observations can be found for pressing sociopolitical conflicts of the future: A rational discussion of global climate change or new energy sources is only possible with reliable analytical results. Progress in Analytical Sciences is only possible if the underlying interdisciplinary character is acknowledged and valued. The talk will illustrate the scope of modern Analytical Science through examples from process analysis relevant to modern process intensification and industry 4.0 to bioanalysis and the use of synchrotron radiation to elucidate fundamental reactions materials. T2 - MChG Talk CY - Technische Universität München, Germany DA - 27.11.2018 KW - Analytical Sciences PY - 2018 AN - OPUS4-46940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - BAM’s role in materials science and hydrogen in metals: TOF-SIMS imaging N2 - Due to its low mass and high diffusivity in presence of compositional, thermal and mechanical gradients, hydrogen within a metallic microstructure can result in severe loss in ductility even at low concentrations and might lead eventually to a catastrophic and unpredictable failure of structural components during service. In this context, hydrogen mapping at the microscale is still considered among the most important challenges on the pathway towards a better understanding of the hydrogen transport and assisted cracking phenomena in metals, specifically in structural components, e.g. steels. Among the very few available techniques to localize hydrogen at the microscale, Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a reliable tool. Based on the assumption that deuterium influence the microstructure similarly to hydrogen, in the following contribution ToF-SIMS was applied as the main technique to detect and locally map the deuterium distribution in several alloys: lean 2101 and standard 2205 duplex stainless steel (DSS), AISI 304L austenitic stainless steel and titanium 6Al-4V alloy. These alloys were selected as case studies in this work due to the wide use of them in many applications and environments which frequently provide critical conditions for hydrogen absorption and assisted degradation. The innovative design of in-situ and ex-situ experiments enabled us to elucidate the permeation, transport and trapping of deuterium in the microstructure in sub-micron resolution for the first time. In addition to the novel experimental setups, further progress was gained by applying computational multivariate data analysis (MVA) on the raw data and data fusion with high resolution structural characterization methods (scanning electron microscopy and electron back-scattered diffraction – SEM/EBSD). This combination allowed us to correlate the deuterium distribution and the influence on the microstructure. T2 - 4th Symposium on Innovative Measurement and Analysis for Structural Materials CY - Tokyo, Japan DA - 13.11.2018 KW - ToF-SIMS KW - Duplex stainless steel KW - Austenitic stainless steel KW - Principal Component Analysis KW - Data-fusion PY - 2018 UR - https://unit.aist.go.jp/tia-co/project/SIP-IMASM/sympo/2018/index.html AN - OPUS4-46867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Nanoparticles separation using capillary electrophoresis (CE) and asymmerical flow-field flow fractionation (AF4) N2 - Nowadays, different nanoparticles have been developed for commercial applications. However, since data on toxicity are barely available, their increasing application in cosmetic products, food and their release in the environment might cause severe problems. An accurate separation, identification and characterization of nanoparticles becomes increasingly important. A common method for nanoparticle separation, which was introduced in 1976 by Giddings, represents asymmetrical field-flow fractionation (AF4). It is a flow based separation method, which can be theoretically used to separate particles range from 1 nm to 50 µm. However, when the particles are smaller than 10 nm, separation with AF4 will become difficult to perform. Because in this case strong separation force, which induces aggregation of particles, should be applied. This will decrease recoveries of analytes and limit its application in accurate quantitative analysis. Capillary electrophoresis (CE) is another well-developed separation technique, in which samples will be separated in relation to their electrophoretic mobility. In recent years, CE has been used to separate different kinds of nanoparticles like, gold colloids or CdSe Quantum dots. However, till now only separation of particles smaller than 50 nm was reported. Because large size distribution of bigger particles will result in strong peak broadening and long separation time. A two-dimensional coupling of AF4 and CE might provide us a new separation method, which can extend the separation ranges of both methods and be a way to characterise particles with large size distributions. T2 - BAM PhD seminar CY - PhD seminar, Berlin, Germany DA - 22.06.2018 KW - Nanoparticles separation capillary electrophoresis asymmetrcial flow field flow fractionation PY - 2018 AN - OPUS4-47187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Separation of polystyrene nanoparticles with different coatings using 2D off-line coupling of asymmetrical flow field flow fractionation (AF4) and capillary electrophoresis (CE) N2 - Nowadays, different nanoparticles have been developed for commercial applications. However, since data on toxicity are barely available, their increasing application in cosmetic products, food and their release in the environment might cause severe problems. An accurate separation, identification and characterization of nanoparticles becomes increasingly important1,2. In this presentation, a two-dimensional separation approach based on AF4 and CE was showed and used to separate NPs with similar sizes but different coatings. Standard reference polystyrene NPs having comparable core sizes but different coatings were investigated. Different migration time and profiles were compared. Separation in either method resulted in non-baseline resolved or non-separated peaks. In contrast, two-dimensional coupling of AF4 and CE resulted in clearly separated regions in their 2 D plots in case of 20 and 50 nm particle mixtures, whereas the 100 nm NP mixture could not be separated. Various factors affecting the separation like hydrodynamic diameter or SDS concentration were discussed. Future investigations will be focussed on inorganic NPs with differently charged coatings. There, AF4-CE coupling can be coupled with inductively coupled plasma mass spectrometry (ICP-MS) to enhance the sensitivity of this method. T2 - 6th FFF-MS Tagung CY - Berlin, Germany DA - 22.11.2018 KW - Nanoparticles separation capillary electrophoresis asymmetrcial flow field flow fractionation PY - 2018 AN - OPUS4-47191 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Nanoparticles separation using capillary electrophoresis N2 - A common method for nanoparticle separation, which was introduced in 1976 by Giddings, represents asymmetrical field-flow fractionation (AF4). It is a flow based separation method, which can be theoretically used to separate particles range from 1 nm to 50 µm. However, when the particles are smaller than 10 nm, separation with AF4 will become difficult to perform. Because in this case strong separation force, which induces aggregation of particles, should be applied. This will decrease recoveries of analytes and limit its application in accurate quantitative analysis. Capillary electrophoresis (CE) is another well-developed separation technique, in which samples will be separated in relation to their electrophoretic mobility. In recent years, CE has been used to separate different kinds of nanoparticles like, gold colloids or CdSe Quantum dots. However, till now only separation of particles smaller than 50 nm was reported. Because large size distribution of bigger particles will result in strong peak broadening and long separation time. A two-dimensional coupling of AF4 and CE might provide us a new separation method, which can extend the separation ranges of both methods and be a way to characterise particles with large size distributions. T2 - BAM PhD seminar CY - PhD seminar, Berlin, Germany DA - 23.06.2017 KW - Nanoparticles separation capillary electrophoresis asymmetrcial flow field flow fractionation PY - 2017 AN - OPUS4-47186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Nanoparticles separation using capillary electrophoresis N2 - Nowadays, different nanoparticles have been developed for commercial applications. However, since data on toxicity are barely available, their increasing application in cosmetic products, food and their release in the environment might cause severe problems. An accurate separation, identification and characterization of nanoparticles becomes increasingly important. A common method for nanoparticle separation, which was introduced in 1976 by Giddings, represents asymmetrical field-flow fractionation (AF4). It is a flow based separation method, which can be theoretically used to separate particles range from 1 nm to 50 µm. However, when the particles are smaller than 10 nm, separation with AF4 will become difficult to perform. Because in this case strong separation force, which induces aggregation of particles, should be applied. This will decrease recoveries of analytes and limit its application in accurate quantitative analysis. Capillary electrophoresis (CE) is another well-developed separation technique, in which samples will be separated in relation to their electrophoretic mobility. In recent years, CE has been used to separate different kinds of nanoparticles like, gold colloids or CdSe Quantum dots. However, till now only separation of particles smaller than 50 nm was reported. Because large size distribution of bigger particles will result in strong peak broadening and long separation time. A two-dimensional coupling of AF4 and CE might provide us a new separation method, which can extend the separation ranges of both methods and be a way to characterise particles with large size distributions. T2 - ESAS-CANAS Konferenz CY - Berlin, Germany DA - 21.03.2018 KW - Nanoparticles separation capillary electrophoresis asymmetrcial flow field flow fractionation PY - 2018 AN - OPUS4-47188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stephan-Scherb, Christiane T1 - Elucidation of competitive oxidation/sulfidation reactions on binary ferritic alloys N2 - Ferritic-austenitic chromia-forming alloys are frequently used as boiler tubes and heat exchanger materials for fossil-,biomass, and co-fired power plants. In all applied environments several strongly corrosive gaseous species such as CO2, SO2, SO3, H2O, O2 exist, causing materials degradation by high-temperature corrosion. The elucidation of degradation mechanisms introduced by multiple gases is challenging due to the presence of different oxidizing agents contributing to the competing reactions for oxidation, sulfurization or carburization. The degradation processes can be divided into initial stages, a transitional stage and the further proceeding steady-state oxidation reaction. Especially the long-term steady-state oxidation and further materials’ life-time are strongly dependent on the initial stages. The adsorption and absorption of the reactive species at the alloy surface and the growing oxide in the initial reaction is further influenced by dissociation and re-reactions of the gas phase molecules. To understand these mechanisms from a fundamental point of view in more detail, dedicated experiments and advanced characterization techniques on various length scale need to be applied. Real-time approaches using highly energetic synchrotron X-ray diffraction showed a high potential to enlighten competitively mechanisms by following the corrosion reactions in-situ in the environment they occur. Despite various other thin film characterization techniques, time of flight secondary ion mass spectroscopy (ToF-SIMS) is a powerful tool to visualize light atoms or labeled isotopes enabling the Differentiation between different oxidizing species. It was especially shown to be applicable in challenging atmospheres containing KCl deposits or in CO/CO2/O2 environments. The present study analyses the competing oxidation/sulfidation process in a humid atmosphere on two ferritic alloys with 2 and 9 % in weight chromium by in situ energy dispersive X-ray diffraction (EDXRD) and comparative tube furnace exposure using S16O2 and H2 18O atmosphere. T2 - Conference on High Temperature Corrosion and Protection of Materials HTCPM 2021 CY - Online Meeting DA - 29.03.2021 KW - Oxidation KW - High Temperature Corrosion KW - Ferritic Alloys KW - SIMS KW - EDXRD PY - 2021 AN - OPUS4-52363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tsamos, Athanasios T1 - Computed tomography data conditioning with AI: A Multi-Level Framework to enhance qualitatively and visually what we already have! N2 - Irrespective of the experimental care used to acquire Computed Tomography Data, certain artifacts might still exist such as: Noise, Blurring, Ring Artifacts etc. To tackle this problem, a complete multi-level framework employing AI (Deep Artificial Neural Nets), targeting specific artifacts individually, is presented. The goal is to render the data suitable for subsequent unproblematic segmentation without any loss of information, compared to manual conditioning with traditional filters. The strategy can therefore be used to acquire faster CT data (e.g. in-situ investigations) and ensure legacy with existing data obtained, perhaps, on older instruments. T2 - Machine Learning Workshop CY - Online Meeting DA - 18.03.2021 KW - Computed Tomography KW - CT KW - Data Conditioning KW - AI KW - Machine Learning KW - Neural Nets KW - Noise Reduction PY - 2021 AN - OPUS4-52321 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, Gudrun A1 - Krahl, Thoralf A1 - Prinz, Carsten A1 - Emmerling, Franziska A1 - Kemnitz, E. T1 - Luminescent properties of Eu3+/Tb3+ doped fluorine containing coordination polymers N2 - Lanthanides doped coordination polymers (CPs) with different binding motifs were synthesized to investigate the influence of the different fluorine positions in the structure on the decay time τ of the excited states. Fluorine can be integrated into the network mechanochemically via a fluorinated organic linker, here barium tetrafluoroterephthalate Ba(p-BDC-F4)2 or directly via a metal-fluorine bond (barium terephthalate fluoride BaF(p-BDC)0.5). The CP with a metal-fluorine bond shows the highest lifetime of the excited states of lanthanides (Eu3+, Tb3+ or Eu3+& Tb3+). The excitation of the lanthanides can be performed directly via the excitation wavelength typical for lanthanides and via the excitation wavelength of the linker. This enabled the simultaneous excitation of Eu3+ and Tb3+ in one CP. In the emission spectra (λem = 393 nm) of the mixed doped CPs (Eu3+ and Tb3+) the bands of both lanthanides can be observed. The integration into the crystal lattice and the homogeneous distribution of the lanthanides in the CPs is shown by X-ray diffraction, TEM, STEM-EDS measurements and the long decay times. KW - Alkaline earth metal coordination polymers KW - Fluorine coordination polymers KW - Lanthanides doped coordination polymers KW - Luminescence PY - 2021 DO - https://doi.org/10.1016/j.solidstatesciences.2021.106614 VL - 117 SP - 106614 PB - Elsevier Masson SAS AN - OPUS4-52559 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, Holger A1 - Baldofski, Stefanie A1 - Hoffmann, Kristin A1 - Flemig, Sabine A1 - Silva, C. P. A1 - Esteves, V. I. A1 - Emmerling, Franziska A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - Structural considerations on the selectivity of an immunoassay for sulfamethoxazole N2 - Sulfamethoxazol (SMX),a sulfonamide, is a widely used bacteriostatic antibiotic and therefore a promising marker for the entry of anthropogenic Pollution in the environment. SMX is frequently found in wastewater and surface water. This study presents the production of high affinity and selective polyclonal antibodies for SMX and the development and Evaluation of a direct competitive enzyme-linked immunosorbent assay(ELISA)for the quantification of SMX in environmental watersamples. The crystal structures of the cross-reacting compounds sulfamethizole, N4-acetyl-SMX andsuccinimidyl-SMX were determined by x-ray diffraction aiming to explain their high cross-reactivity. These crystal structures are described for the first time. The quantification range of the ELISA is 0.82–63 µg/L. To verify our results, the SMX concentration in 20 environmental samples,including wastewater and surfacewater,was determined by ELISA and tandem mass spectrometry(MS/MS).A good Agreement of the measured SMX concentrations was found with average recoveries of 97–113%for the results of ELISA compared to LC-MS/MS. KW - X-Ray diffraction KW - Sulfamethoxazole KW - ELISA KW - LC-MS/MS PY - 2016 DO - https://doi.org/10.1016/j.talanta.2016.05.049 SN - 0039-9140 SN - 1873-3573 IS - 158 SP - 198 EP - 207 PB - Elsevier B.V. CY - Amsterdam, Netherlands AN - OPUS4-36676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lingott, Jana A1 - Lindner, Uwe A1 - Telgmann, Lena A1 - Esteban-Fernández, Diego A1 - Jakubowski, Norbert A1 - Panne, Ulrich T1 - Gadolinium-uptake by aquatic and terrestrial organisms-distribution determined by laser ablation inductively coupled plasma mass spectrometry N2 - The uptake of gadolinium containing chelates by plants and animals grown in exposed water or on soil irrigated with exposed water was investigated. Gd contrast agents was studied by monitoring the elemental distribution with laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). KW - Gadolinium-uptake KW - Speciation KW - HILIC KW - ICP-MS PY - 2016 DO - https://doi.org/10.1039/c5em00533g SN - 2050-7887 VL - 18 IS - 2 SP - 200 EP - 207 PB - Royal Society of Chemistry CY - Cambridge, UK AN - OPUS4-36281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sötebier, Carina T1 - Characterization of Ag nanoparticles: limitation and advantages of field-flow fractionation N2 - Silver nanoparticles (Ag NPs) are widely used in consumer products due to their excellent antibacterial properties. Their broad application has led to a variety of recent regulation on their use and labelling. Thus, a highly specific analytical method for their characterization and quantification is needed. Due to their large separation range, field-flow fractionation (FFF) techniques are repeatedly applied for the analysis of NP. Limitations of FFF include quantification, sample loss and insufficient recovery rates. Another challenge can be non-ideal elution behavior of particles in complex and unknown matrices. The possible sources for sample losses of Ag NP have been studied using an asymmetric flow FFF (AF4) in combination with inductively coupled plasma mass spectrometry (ICP-MS). The influence of different parameters, for example the sample concentration, on the recovery rates and sample loss has been investigated. Using laser ablation ICP-MS, the Ag deposition on the membrane was located and quantified. Our results identified ionic silver as the main sources of sample loss. These results can be useful for further method improvement. However, when a Ag NP sample containing an unknown complex matrix is analyzed, FFF method optimization is challenging as the sample might show a shift in the retention times and lower recovery rates. In this case, ICP-MS experiment in the single particle mode (sp-ICP-MS) can be a useful addition to the FFF measurement. Here, upon assumption of spherical particles, the geometric diameters can be calculated. This fast and easy approach can be helpful in order to interpret the FFF fractograms and advice the FFF method optimization process. T2 - 18th International Symposium on Field- and Flow-Based Separations CY - Dresden, Germany DA - 22.05.2016 KW - Silver KW - Nanoparticles KW - Field-flow fractionation KW - ICP-MS PY - 2016 AN - OPUS4-36352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Franziska T1 - Polymorphism of mechanochemically synthesized Cocrystals: an in situ study N2 - In situ investigations using PXRD coupled with Raman spectroscopy permit the evaluation of the formation pathways of milling reactions. The liquid-assisted grinding cocrystallisation of theophylline with benzamide leading to polymorphic compounds was investigated. The dipole moment of the solvent used in the synthesis determines the structure of the polymorphic product. A detailed investigation allows determining the kinetically and thermodynamically favored product. In situ observations of the formation pathway during the grinding process of both polymorphs show that the thermodynamically favored cocrystal is formed in a two-step mechanism with the kinetic cocrystal as intermediate. The evaluation of the mechanochemical formation pathways reveals the importance of in situ investigations for an in depth understanding of mechanochemical synthesis mechanisms. Our study demonstrates that the choice of the solvent in the LAG synthesis is decisive for the controlled formation of a desired polymorphic final product. T2 - CGOM/ BACG 47th Annual British Association of Crystal Growth Conference CY - Leeds, UK DA - 28.06.2016 KW - Cocrystal KW - Mechanochemistry KW - Milling PY - 2016 AN - OPUS4-36764 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abdelshafi, Nahla A. A1 - Panne, Ulrich A1 - Schneider, Rudolf T1 - Screening for cocaine on Euro banknotes by a highly sensitive enzyme immunoassay N2 - This study focused on quantitative detection of cocaine on Euro banknotes in Germany. A sensitive direct competitive immunoassay was developed and optimized with a limit of detection (LOD) of 5.6 ng/L. Exhaustive cocaine extraction by solvent was tested using different methanol concentrations and buffered solutions. Crossreactivity studies were performed to determine the degree of interference of cocaine metabolites with the immunoassay. Sixty-five Euro banknotes obtained from different districts in Berlin were evaluated. A 100% contamination frequency with cocaine was detected. A comparison between the amount of cocaine extracted by cotton swabbing of one square centimeter of the banknote showed a good correlation for lower contamination levels. This assay showed high sensitivity of detecting pg of cocaine per 1 cm2 of one banknote by swabbing 1 cm2: 0, 14, and 21 pg/cm2. Moreover, three notes of different denominations revealed high cocaine concentration; 1.1 mg/note, and twice 55 μg/note. KW - Cocaine KW - Euro banknotes KW - Drugs on bills KW - Enzyme-Linked Immunosorbent Assay KW - ELISA PY - 2017 DO - https://doi.org/10.1016/j.talanta.2017.01.004 SN - 0039-9140 SN - 1873-3573 VL - 165 SP - 619 EP - 624 PB - Elsevier AN - OPUS4-39150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Michalik-Onichimowska, Aleksandra A1 - Beitz, T. A1 - Panne, Ulrich A1 - Löhmannsröben, H.-G. A1 - Riedel, Jens T1 - Microsecond mid-infrared laser pulses for atmospheric pressure laser ablation/ionization of liquid samples N2 - In many laser based ionization techniques with a subsequent drift time separation, the laser pulse generating the ions is considered as the start time t0. Therefore, an accurate temporal definition of this event is crucial for the resolution of the experiments. In this contribution, the laser induced plume dynamics of liquids evaporating into atmospheric pressure are visualized for two distinctively different laser pulse widths, Δt = 6 nanoseconds and Δτ = 280 microseconds. For ns-pulses the expansion of the generated vapour against atmospheric pressure is found to lead to turbulences inside the gas phase. This results in spatial and temporal broadening of the nascent clouds. A more equilibrated expansion, without artificial smearing of the temporal resolution can, in contrast, be observed to follow μs-pulse excitation. This leads to the counterintuitive finding that longer laser pulses results in an increased temporal vapour formation definition. To examine if this fume expansion also eventually results in a better definition of ion formation, the nascent vapour plumes were expanded into a linear drift tube ion mobility spectrometer (IMS). This time resolved detection of ion formation corroborates the temporal broadening caused by collisional impeding of the supersonic expansion at atmospheric pressure and the overall better defined ion formation by evaporation with long laser pulses. A direct comparison of the observed results strongly suggests the coexistence of two individual ion formation mechanisms that can be specifically addressed by the use of appropriate laser sources. KW - Plume KW - Laser ablation KW - Ion mobility spectrometry KW - Pulse duration KW - Ionization PY - 2017 DO - https://doi.org/10.1016/j.snb.2016.06.155 VL - 238 SP - 298 EP - 305 PB - Elsevier CY - Amsterdam, NL AN - OPUS4-37158 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Herrmann, Antje T1 - Simple and fast metal staining procedures for identification of single cells via Laser Ablation ICP-MS N2 - Biological systems exhibit a very high complexity, because they consist of various cell populations showing heterogenic characteristics. Therefore the individual analysis of single cells is important to understand cellular processes as well as their function in a cell system. Especially investigation in the question about what is biological variability and what is a substantial difference between two cells of the same type (which might lead to dysfunction or disease) is of high interest. Today improved spatial and temporal resolution enable the use of laser ablation inductively coupled mass spectrometry (LA-ICP-MS) for element microscopy of single cells. Next to the characterization of natural trace elements the introduction of artificial metal labels into cells is of high interest. Element labeling of cell compartments and/or proteins allows its simultaneous analysis and localization within a cell via element microscopy. Two fast and simple metal staining procedures of adherent cells for identification of single cells via LA-ICP-MS at sub micrometer resolution are presented. An Iridium-intercalator is utilized to stain the cell nuclei whereas the whole cell is stained by maleimido-mono-amide-DOTA-complexes (mDOTA) loaded with lanthanide(III) isotope ions. The metal staining procedures allow the visualization of single cells by element microscopy independent of a superposition of analyte’s 2D element intensity profile with a prior taken bright field image of the sample. T2 - EWLA 2016 CY - Ljubljana, Slovenia DA - 12.07.2016 KW - bioimaging KW - single cell analysis PY - 2016 AN - OPUS4-37077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Michalik-Onichimowska, Aleksandra T1 - On-line monitoring of photoreactions within levitated droplets by LA-DBD-MS N2 - Real time monitoring of chemical reactions has become a key step in industrial processes due to constantly increasing demands on product performance and environmental compatibility. In contrast to spectroscopic methods that usually require sample pretreatment, mass spectrometry (MS) has been proven as a robust method for multicomponent analysis. As an especially demanding reaction process, we here report successfully on the entirely contactless conduction and interrogation of a chemical reaction inside an acoustically levitated microliter droplet of reaction mixture. The approach represents a proof of concept study for fast reaction optimization approaches with minimal resource consumption. The sampling is done by repeated laser desorption of small fractions of the droplets volume spread over the timescale of the reaction process. T2 - 49. Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie CY - Hamburg, Germany DA - 28.02.2016 KW - Monitoring of chemical reactions KW - Acoustic levitation KW - Mass spectrometry PY - 2016 AN - OPUS4-37157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Michalik-Onichimowska, Aleksandra T1 - Real time monitoring of photoreactions performed within levitated droplets by LA-DBD-MS N2 - The upscaling from small scale academic reactors to large industrial processes typically suffers from a large change in surface-to-volume ratio. A promising approach is the general avoidance of surfaces as in levitated droplet techniques. However, up to now, no mass spectrometric interface for online reaction monitoring in levitated droplets has been provided. As model reaction the photoinitiated thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was studied. A droplet of 5 µL reactand solution was provisioned into an acoustic trap aligned lateral to the MS inlet. Contactless sampling by laser ablation (LA) is followed by dielectric barrier discharge (DBD) postionization. The latter is needed to address non polar reaction partners. T2 - 21st International Mass Spectrometry Conference CY - Toronto, Canada DA - 20.08.2016 KW - Monitoring of chemical reactions KW - Acoustic levitation KW - Laser ablation KW - Mass spectrometry PY - 2016 AN - OPUS4-37159 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Rhode, Michael A1 - Münster, C. A1 - Mente, Tobias A1 - Böllinghaus, Thomas ED - Somerday, B.P. ED - Sofronis, P. T1 - Influence of experimental conditions and calculation method on hydrogen diffusion coefficient evaluation at elevated temperatures N2 - Literature provides a wide range of hydrogen diffusion coefficients for low alloyed steels used in power plants. In fact, experimental boundary conditions and calculation methods have influence on the determination of these coefficients. The diffusion and trapping behavior in creep-resistant steel 7CrMoVTiB10-10 has been studied. Based on experimental carrier gas hot extraction (CGHE) data, a numerical model has been developed to describe the hydrogen transport and respective hydrogen distribution at elevated temperatures. The numerical results suggest that common calculation methods for diffusion coefficients are limited for experimental data analysis. The sample preparation time before CGHE experiment influences the determined diffusion coefficients with the consequence that non-homogeneous hydrogen concentration profiles have to be considered in the simulations. KW - Temperature effect KW - Hydrogen diffusion KW - Creep-resistant steel KW - Hydrogen assisted cracking KW - Carrier gas hot extraction PY - 2017 SN - 978-0-7918-6138-7 DO - https://doi.org/10.1115/1.861387_ch56 SP - 495 EP - 503 PB - ASME CY - New York, USA ET - 1 AN - OPUS4-42502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - The characterization of oxygen diffusion in (Na1/2Bi1/2)TiO3 piezo-ceramics by Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) N2 - The ferroelectric ceramic NBT and its solid solutions with barium titanate (BT) are examples for the most promising lead free materials to substitute the dominant Pb(Zr,Ti)O3 (PZT). Lead based material should generally be disregarded due to environmental and health reasons. However, there is no class of lead-free piezoelectric materials that can replace PZT entirely. Not only the often inferior ferroelectric properties but also the lack of understanding of the defect chemistry of NBT is still a challenge for the replacement of lead containing piezo-ceramics. Just recently it could be shown by Li et al.[1] that NBT obtains extraordinarily high oxygen ionic conductivity when doped with Mg as acceptor. It was actually expected that doping just leads to a hardening of the ferroelectric properties. However, it became clear that the known defect chemical behavior of PZT cannot be extrapolated to NBT materials. Hence, to gain information on general doping effects a better defect chemical investigation is needed. This is particularly important for the applications with high reliability demands to investigate possible degradation and fatigue mechanisms. In the present work Time-of-flight-secondary ion mass spectrometry (ToF-SIMS) was used in order to observe the influence of different acceptor dopants (Fe, Ni, Al) on the oxygen diffusion in NBT. ToF-SIMS holds the ability to gain a full elemental distribution in a sub-micron resolution and was therefore chosen to provide the essential information on the favorable diffusion paths of oxygen in NBT in dependence of the chosen doping element. 18O was used as a tracer for oxygen as its natural abundance is only 0.2%. The doped NBT samples have been annealed for 5 h at 500°C in a 0.2 bar 18O-tracer atmosphere to be able to detect oxygen ion diffusion. ToF-SIMS investigations were conducted on a ToF-SIMS IV (ION TOF GmbH, Münster, Germany) using a Bi+ primary ion beam (25KeV in collimated burst alignment mode with a beam diameter of ~150 nm) and a Cs+ sputter beam (3KeV). The results illustrate the different impact of dopants on the diffusion properties which is evidence for a highly non-linear dependence on dopant type and concentration. 1) Li, M., et al., Nature Materials, 2014. 13(1): p. 31-35. T2 - 21st International Conference on Secondary Ion Mass Spectrometry - SIMS21 CY - Krakow, Poland DA - 10.09.2017 KW - NBT-Piezoceramics KW - ToF-SIMS PY - 2017 UR - http://sims.confer.uj.edu.pl/boa_poster.php?id=93 AN - OPUS4-42863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - The characterization of oxygen diffusion in (Na1/2Bi1/2)TiO3 piezo-ceramics by Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) N2 - The ferroelectric ceramic NBT and its solid solutions with barium titanate (BT) are examples for the most promising lead free materials to substitute the dominant Pb(Zr,Ti)O3 (PZT). Lead based material should generally be disregarded due to environmental and health reasons. However, there is no class of lead-free piezoelectric materials that can replace PZT entirely. Not only the often inferior ferroelectric properties but also the lack of understanding of the defect chemistry of NBT is still a challenge for the replacement of lead containing piezo-ceramics. Just recently it could be shown by Li et al. that NBT obtains extraordinarily high oxygen ionic conductivity when doped with Mg as acceptor. It was actually expected that doping just leads to a hardening of the ferroelectric properties. However, it became clear that the known defect chemical behavior of PZT cannot be extrapolated to NBT materials. Hence, to gain information on general doping effects a better defect chemical investigation is needed. This is particularly important for the applications with high reliability demands to investigate possible degradation and fatigue mechanisms. In the present work Time-of-flight-secondary ion mass spectrometry (ToF-SIMS) was used in order to observe the influence of different acceptor dopants (Fe, Ni, Al) on the oxygen diffusion in NBT. ToF-SIMS holds the ability to gain a full elemental distribution in a sub-micron resolution and was therefore chosen to provide the essential information on the favorable diffusion paths of oxygen in NBT in dependence of the chosen doping element. 18O was used as a tracer for oxygen as its natural abundance is only 0.2%. The doped NBT samples have been annealed for 5 h at 500°C in a 0.2 bar 18O-tracer atmosphere to be able to detect oxygen ion diffusion. ToF-SIMS investigations were conducted on a ToF-SIMS IV (ION TOF GmbH, Münster, Germany) using a Bi+ primary ion beam (25KeV in collimated burst alignment mode with a beam diameter of ~150 nm) and a Cs+ sputter beam (3KeV). The results illustrate the different impact of dopants on the diffusion properties which is evidence for a highly non-linear dependence on dopant type and concentration. T2 - 21st International Conference on Secondary Ion Mass Spectrometry - SIMS21 CY - Krakow, Poland DA - 10.09.2017 KW - ToF-SIMS KW - NBT KW - Piezoceramics PY - 2017 UR - http://sims.confer.uj.edu.pl/boa_poster.php?id=93 AN - OPUS4-42911 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Observations of the deuterium distribution and the structural changes in standard and lean duplex stainless steels by ToF-SIMS and EBSD N2 - The use of duplex stainless steels (DSS) in energy related applications is well known. Nowadays, DSSs become more favorable than austenitic steels due to the outstanding mechanical properties, the good corrosion resistance and the lower nickel content.However, the use of the duplex grade in acidic environments such as seawater can lead to a severe degradation in the structural integrity of the steel by hydrogen-induced/assisted cracking mechanisms, which can eventually result in premature failure. Hydrogen assisted degradation and cracking of steels remains unclear even though this topic is intensively studied for more than a century. The main gap lies in the validation of the proposed theoretical models at the sub-micron scale. Industrial and the research communities define a need for an accurate method by which it is possible to image the distribution of hydrogen in the microstructure. Among the very few available methods nowadays, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) provides precise mapping of hydrogen in the microstructure. Moreover, the powerful combination of ToF-SIMS with multivariate data analysis (MVA), electron backscattered diffraction (EBSD) for providing a the structural information and the use of data fusion techniques can contribute to a better understanding of the hydrogen induced degradation processes in the material. In the present work two types of duplex grades were chosen as a case study (standard and lean DSS). The duplex class, consist of equivalent amounts of ferrite and austenite, was investigated by ToF-SIMS and EBSD during and after electrochemical deuterium charging in order to simulate the service of a component in acidic environments. Deuterium is known to act on the steel similarly to hydrogen and therefore was used as a tracer for hydrogen. The results show that the ferrite was affected almost identical in both steels whereas in the austenitic phase significant differences were observed in the lean duplex in comparison to the standard duplex. The advantage of the combined techniques is reflected by the ability to correlate the hydrogen distribution in the microstructure to the resulted structural changes. T2 - 21st International Conference on Secondary Ion Mass Spectrometry - SIMS21 CY - Krakow, Poland DA - 10.09.2017 KW - ToF-SIMS KW - Duplex-steel KW - EBSD KW - Data-fusion PY - 2017 UR - http://sims.confer.uj.edu.pl/boa_oral.php?id=23 AN - OPUS4-42864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tuma, Dirk T1 - Preparation and Analysis of Trace Compounds in Hydrogen in the ppm and Sub-ppm Region Relevant for Applications N2 - ISO 14687 defines threshold limits for expectable impurities in hydrogen that is assigned for use in polymer electrolyte membrane (PEM) fuel cells. This work describes the establishment of the traceability of some selected impurities by preparation and analysis of reference gases with the lowest possible uncertainty in composition. Primary reference gases were produced by the gravimetric method according to ISO 6142-1 and the analysis was carried out by operating measurement protocols according to ISO 12963 on two customized trace GC analysers. T2 - ANAKON 2023 CY - Vienna, Austria DA - 11.04.2023 KW - Hydrogen analysis KW - Gravimetric preparation KW - Gas chromatography PY - 2023 AN - OPUS4-57329 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Analytical Sciences: From Ostwald's maid to enabling science N2 - The talk will address the paradigm shift in Analytical Sciences in regard to chemistry as a discipline. To illustrate this metamorphose examples from spectroschemical analysis, ufluidics, bioanalysis, and the didgital transformation of analytical sciences are discussed. T2 - GDCh-Wissenschaftsforum 2019 CY - Aachen, Germany DA - 15.09.2019 KW - Spectrochemical analysis KW - Analytical Sciences PY - 2019 AN - OPUS4-51471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Olivera, Paulo A1 - Michalchuk, Adam A1 - Marquardt, Julien A1 - Feiler, Torvid A1 - Prinz, Carsten A1 - Torresi, R. A1 - Camargo, P. A1 - Emmerling, Franziska T1 - Investigating the role of reducing agents on mechanosynthesis of Au nanoparticles N2 - Control over the bottom up synthesis of metal nanoparticles (NP) depends on many experimental factors, including the choice of stabilising and reducing agents. By selectively manipulating these species, it is possible to control NP characteristics through solution-phase synthesis strategies. It is not known, however, whether NPs produced from mechanochemical syntheses are governed by the same rules. Using the Au NPs mechanosynthesis as a model system, we investigate how a series of common reducing agents affect both the reduction kinetics and size of Au NPs. It is shown that the relative effects of reducing agents on mechanochemical NP synthesis differ significantly from their role in analogous solution-phase reactions. Hence, strategies developed for control over NP growth in solution are not directly transferrable to environmentally benign mechanochemical approaches. This work demonstrates a clear need for dedicated, systematic studies on NP mechanosynthesis. KW - Mechanochemistry KW - Metal nanoparicels PY - 2020 DO - https://doi.org/10.1039/d0ce00826e VL - 22 IS - 38 SP - 6261 EP - 6267 PB - Royal Society of Chemistry AN - OPUS4-51757 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Schneider, Rudolf T1 - Wasserdiagnose durch die Verwendung von Markern N2 - Die Überwachung des gesamten Wasserkreislaufs auf Mikroverunreinigungen ist aus gesundheitlicher und ökologischer Hinsicht wünschenswert und gewinnt durch den Klimawandel und das zunehmende Erfordernis der Wiederverwendung des Brauchwassers weiter an Bedeutung. Die schnellen und kostengünstigen antikörperbasierten Methoden („Immunoassays“) können helfen, Informationslücken zu schließen und kürzere Reaktionszeiten zu ermöglichen. Von Labormethoden über tragbare Analysengeräte bis hin zu Online-Sensoren sind viele Formate möglich (u. a. ELISA, Abb. 1). Es muss zudem die Bereitstellung der notwendigen, hochqualitativen Antikörper gewährleistet werden. Da aber gilt „1 Analyt – 1 Antikörper“, ist die Herstellung eines Konsenses bezüglich der vordringlich zu bestimmenden Indikatoren/Marker notwendig. Auch die Normung der Verfahren ist parallel in Angriff zu nehmen. KW - Antikörper KW - Immunoassay KW - Abwasser KW - ELISA PY - 2025 UR - https://analyticalscience.wiley.com/content/article-do/wasserdiagnose-durch-die-verwendung-von-markern VL - 2025 IS - 1 SP - 1 EP - 4 PB - WILEY CY - Hoboken, NJ, USA AN - OPUS4-63508 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Yi T1 - Differential Mobility Analysis with Acoustic Ion Manipulation (AIM) N2 - Ion mobility analyses provide complementarity to mass spectrometry in analyte ion identification through the introduction of a higher-pressure separation modality. The recently discovered acoustic ion manipulation (AIM) phenomenon, which exploits unique behaviors of ions in acoustic fields, presents a novel, electric-field-free means to distinguish ions by mobility. In one form of AIM, a static pressure field in an ultrasonic resonator causes a displacement of the ion stream toward the node region, when initially directed toward the antinode. When the static field strength falls below the threshold for all ion deflection, the partitioning reflects ion-specific acoustic mobilities or acoustic radiation impedance. This study demonstrates ion-oriented mobility separation with the AIM approach for mass-spectrometric analysis. An Orbitrap mass spectrometer was used to record ion signal variations as a function of acoustic field strength. An acoustic pressure source with a transducer–reflector configuration was used to generate a standing acoustic wave for partial ion deflection. The drive frequency was swept near resonance to modulate the static pressure field. An alternating-current (AC) plasma discharge source was used to produce an ion beam directed toward an antinode of the resonant structure and later deflected into the mass spectrometer inlet with the acoustic field. Several small molecule analytes, including methanol, ethanol, acetone, and toluene, were doped in the discharge gas to distinguish ions formed in the source from those produced in transit to the MS inlet. An ion beam, offset relative to the inlet capillary of the mass spectrometer, yielded minimal ion detection in the absence of the resonant acoustic field. A sweep of the frequency near resonance induced a low–high–low transition in the static pressure within the resonator. Consequently, the total ion signal as a function of drive frequency resembled a horn gain curve, which is commonly recognized as a key characteristic in ultrasonic transducer design. Maximum ion signal was attained at the resonance frequency, while a pronounced minimum occurred at the anti-resonance frequency. Analysis of drive frequency response curves for distinct ion peaks revealed that source-generated ions displayed a congruent pattern to the overall ion count, thereby suggesting the formation of clusters prior to the vacuum region of the mass spectrometer. A finer frequency scan near the resonance region differentiated these clusters. For instance, response curves for toluene-related ions are slightly deviated from those associated with alcohols. Notably, a series of ions, presumably originating from an identical chemical precursor, manifested an entirely distinctive drive frequency response; their maximal signal occurred at a frequency not associated with any characteristic of the acoustic system or its electronics. The frequency response curves of the ions allowed implementation of a modified cross-correlation (mXcorr) algorithm to categorize ions according to chemical origin or clustering. The use of frequency, rather than the transducer voltage/power, offers the advantage of electronically measuring the horn gain curve in tandem with ion-specific analysis. This gain curve subsequently serves as a reference to decode latent chemical information for enhanced analytical accuracy. T2 - ASMS 2025 Conference CY - Baltimore, MA, USA DA - 01.06.2025 KW - Acoustic Ion Manipulation KW - Mass Spectrometry PY - 2025 AN - OPUS4-63512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Plouffe, A. A1 - Lee, R. G. A1 - Byrne, K. A1 - Kjarsgaard, I. M. A1 - Petts, D. C. A1 - Wilton, D.H.C. A1 - Ferbey, T. A1 - Oelze, Marcus T1 - Tracing Detrital Epidote Derived from Alteration Halos to Porphyry Cu Deposits in Glaciated Terrains: The Search for Covered Mineralization N2 - Distal alteration related to porphyry Cu mineralization is typically characterized by an abundance of green minerals, such as epidote, tremolite, and chlorite, within the propylitic and sodic-calcic alteration zones and extends far outside (>1 km) the mineralized zone(s). Glacial erosion and dispersal derived from rocks affected by propylitic and sodic-calcic alteration have resulted in the development of extensive dispersal trains of epidote in till (glacial sediment) that can reach 8 to 330 km2 as observed at four porphyry Cu study sites in the Quesnel terrane of south-central British Columbia: Highland Valley Copper, Gibraltar, Mount Polley, and Woodjam deposits. At each of these sites, epidote is more abundant in heavy mineral concentrates of till collected directly over and down-ice from mineralization and associated alteration. Epidote grains in till with >0.6 ppm Sb and >8 ppm As (as determined by laser ablation-inductively coupled plasma-mass spectrometry) are attributed to a porphyry alteration provenance. There is a greater abundance of epidote grains with high concentrations of trace elements (>12 ppm Cu, >2,700 ppm Mn, >7 ppm Zn, and >37 ppm Pb) in each porphyry district com� pared to background regions. This trace element signature recorded in till epidote grains is heterogeneously distributed in these districts and is interpreted to reflect varying degrees of metal enrichment from a porphyry fluid source. Tracing the source of the epidote in the till (i.e., geochemically tying it to porphyry-related propy� litic and/or sodic-calcic alteration), coupled with porphyry vectoring tools in bedrock, will aid in the detection of concealed porphyry Cu mineralization in glaciated terrains. KW - Indicator minerals KW - Porphyry Cu deposits KW - Epidote KW - Glaciated terrains KW - Propylitic alteration PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635209 DO - https://doi.org/10.5382/econgeo.5049 SN - 1554-0774 VL - 119 IS - 2 SP - 305 EP - 329 PB - Society of Economic Geologists, Inc. AN - OPUS4-63520 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sötebier, Carina T1 - Application of ICP-MS in the single particle mode and isotope dilution analysis on the example of silver nanoparticles N2 - Due to its simplicity, speed and ability to obtain a particle number size distribution, single particle ICP-MS (spICP-MS) has emerged as an important tool for the analysis of nanoparticles (NPs). However, when NPs are suspended in a complex, unknown solution, matrix effects can occur affecting the instrument’s sensitivity. As a result, an over- or underestimation of the particle size is possible. In this work, a proof-of-concept study of the combination of isotopic dilution analysis (IDA) and spICP-MS compensating for possible matrix effects is presented. As an example, an isotopically enriched 109Ag standard solution was added to silver NPs (Ag NP) suspensions. Different NP suspensions with mean particle diameters between 30 and 80 nm were chosen. The mixtures were analyzed using a quadrupole ICP-MS instrument. Both Ag isotopes (107Ag and 109Ag) were monitored during one experiment. The result show a good agreement with the diameters obtained using conventional spICP-MS. In a second step, the Ag NPs were suspended in a simulated seawater matrix. Using conventional spICP-MS, a great reduction in the signal intensities and consequently in the particle sizes, was monitored. The application of the IDA-spICP-MS approach on these samples was able to obtain similar diameters compared to the samples without matrix. T2 - Anwendertreffen Plasmaspektrometrie CY - Berlin, Germany DA - 22.02.2016 KW - Single particle ICP-MS KW - Silver nanoparticles KW - Isotope dilution analysis PY - 2016 AN - OPUS4-35627 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Greiser, Sebastian T1 - 29Si-27Al NMR to verify and distinguish Qn(mAl) sites in zeolites and geopolymers N2 - One-part-geopolymers, produced by addition of water to a mixture of solid silica and sodium alumi-nate, are a less exhaustively studied approach to form geopolymeric binders. Depending on the silica source, the reaction products show significant amounts of zeolite Na-A besides amorphous compounds. Previously, 29Si MAS NMR has been used to analyze the chemical structure of such one-part geopolymers, having crystalline structures and amorphous phases (Q2, Q3, Q4). In this work, pure zeolites and three different one-part-geopolymers cured for 1 day were investigated by 29Si-27Al TRAPDOR NMR. It was used to identify aluminum phases in overlapping silicon sites. Zeolites Na-X (Si/Al=1.4) and Na-Y (Si/Al=2.7) served as model systems to measure the TRAPDOR effect of the structural units Q4(mAl). Both materials show several Q4(mAl) signals, which are all separated by their chemical shifts. The more aluminum surrounds the silicon tetrahedron the higher are the normalized TRAPDOR difference signals (S0/∆S). The intensity ratios between Q4(mAl) to Q4({m-1}Al) of these signals is fixed but vary slightly between both zeolites. These results are transferred to the complex geopolymer structure. T2 - 57th Experimental nuclear magnetic resonance conference CY - Pittsburgh, PA, USA DA - 10.04.2016 KW - NMR KW - 29Si-27Al TRAPDOR MAS KW - Geopolymer KW - One-part formulation KW - Rice husk ash PY - 2016 AN - OPUS4-35864 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Phukphatthanachai, Pranee T1 - Determination of total sulfur in a metal matrix by ICP-IDMS: Example Cu matrix N2 - Previously on sulfur determination in metal revealed a lack of traceability and inconsistent results. Solving the problems a reference procedure for sulfur measurement in metal are required to build up a reliable reference value. In this study a procedure was developed for quantification of total sulfur at low concentration (in sub ppm level) in metal using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS). The ion exchange method and complexing agent were applied in this procedure to avoid loading large amount of metal into the instrument. Adding ammonia as a complexing agent into sample solution to reduce sulfur-metal co-elute. The procedure shows high performance and it is expressed in % recovery of sulfur (> 90%) and % metal elimination (>99 %). Additionally, relative measurement uncertainties were calculated less than 1.5 % and the results are traceable directly to SI units. This study would establish as reference procedure for sulfur measurement in metal sample which fit for these purpose as follows; for certified reference material and assigned value for inter-laboratory comparison. T2 - Anwendertreffen Plasmaspektrometrie CY - Berlin, Germany DA - 22.02.2016 KW - Isotope dilution KW - Separation KW - Traceability PY - 2016 AN - OPUS4-36075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bremser, Wolfgang A1 - Tuma, Dirk T1 - International reference values for calibration of process gas chromatographs (PGCs) and related uncertainties N2 - In a mutual framework agreement, the two German national institutes BAM (Federal Institute of Materials Research and Testing) and PTB (Physikalisch-Technische Bundesanstalt) agreed upon the development, provision, and dissemination of national measurement standards for chemical analysis via primary reference measuring systems. Traceability to national standards and international comparability is of key importance for the acceptance of measurement results in metrology. T2 - 6th International Gas Analysis Symposium & Exhibition -- GAS 2011 CY - Rotterdam, The Netherlands DA - 09.02.2011 KW - Metrology KW - Gas standards KW - Certification PY - 2011 AN - OPUS4-35943 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadejde, C. A1 - Neamtu, M. A1 - Schneider, Rudolf A1 - Hodoroaba, Vasile-Dan A1 - Ababei, G. A1 - Panne, Ulrich T1 - Catalytical degradation of relevant pollutants from waters using magnetic nanocatalysts N2 - The catalytic efficiency of two magnetically responsive nanocatalysts was evaluated for the Degradation of Reactive Black 5 (RB5) and Reactive Yellow 84 (RY84) azo dyes using hydrogen peroxide as oxidant undervery mild conditions (atmospheric pressure, room temperature). In order to obtain the nanocatalysts, thesurface of magnetite (Fe3O4) nanoparticles, prepared by a co-precipitation method, was further modified with ferrous oxalate, a highly sensitive non-hazardous reducing agent. The sensitized nanomaterials were characterized by X-ray diffraction, scanning and transmission electron microscopy, energy-dispersive X-ray spectroscopy and vibrating sample magnetometry, and used in the catalytic wet hydrogen peroxideoxidation (CWHPO) of RB5 and RY84, in laboratory-scale experiments. The effect of important variables such as catalyst dosage, H2O2 concentration, and contact time was studied in the dye Degradation kinetics. The results showed that it was possible to remove up to 99.7% dye in the presence of 20 mM H2O2 after 240 min of oxidation for a catalyst concentration of 10 g L−1at 25◦C and initial pH value of 9.0.CWHPO of reactive dyes using sensitized magnetic nanocatalysts can be a suitable pre-treatment methodfor complete decolorization of effluents from textile dyeing and finishing processes, once the Optimum operating conditions are established. T2 - 10th International Conference On Physics Of Advanced Materials (ICPAM-10) CY - Iasi, Romania DA - 22.09.2014 KW - Sensitized magnetic nanocatalysts KW - Catalytic wet peroxide oxidation KW - Reactive azo dye degradation PY - 2015 UR - http://www.sciencedirect.com/science/article/pii/S0169433215000483 DO - https://doi.org/10.1016/j.apsusc.2015.01.036 SN - 0169-4332 VL - 352 SP - 42 EP - 48 PB - Elsevier B.V. AN - OPUS4-38760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nadejde, C. A1 - Neamtu, M. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Paul, Andrea A1 - Ababei, G. A1 - Panne, Ulrich T1 - Tannic acid- and natural organic matter-coated magnetite as green Fenton-like catalysts for the removal of water pollutants N2 - The use of magnetic materials as heterogeneous catalysts has attracted increasing attention in the last years since they proved to be promising candidates for water treatment. In the present study, two types of surface-modified magnetite (Fe3O4) nanoparticles, coated with non-hazardous naturally occurring agents—either tannic acid (TA) or dissolved natural organic matter—were evaluated as magnetic heterogeneous catalysts. Chemical synthesis (co-precipitation) was chosen to yield the nanocatalysts due to its well-established simplicity and efficiency. Subsequently, the properties of the final products were fully assessed by various characterization techniques. The catalytic activity in heterogeneous oxidation of aqueous solutions containing a model pollutant, Bisphenol A (BPA), was comparatively studied. The effect of operational parameters (catalyst loading, H2O2 dosage, and UV light irradiation) on the Degradation performance of the oxidation process was investigated. The optimum experimental parameters were found to be 1.0 g/L of catalysts and 10 mM H2O2, under UV irradiation. The highest mineralization rates were observed for Fe3O4-TA catalyst. More than 80 % of BPA was removed after 30 min of reaction time under the specified experimental conditions. The obtained results showed that the two catalysts studied here are suitable candidates for the removal of pollutants in wastewaters by means of heterogeneous reaction using a green sustainable treatment method. KW - Nanocatalysts KW - Photo-Fenton oxidation KW - Wastewater KW - Bisphenol A degradation KW - Environment KW - Mitigation PY - 2015 UR - http://link.springer.com/article/10.1007/s11051-015-3290-0 DO - https://doi.org/10.1007/s11051-015-3290-0 VL - 17 IS - 12 SP - 476 (1) EP - 476 (10) PB - Springer AN - OPUS4-38758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silverstein, R. A1 - Sobol, Oded A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang A1 - Eliezer, D. T1 - Hydrogen behavior in SAF 2205 duplex stainless steel N2 - This paper describes austenitic-ferritic duplex stainless steels, SAF 2205, in the presence of hydrogen. The duplex stainless steels (DSS) properties include excellent resistance to stress corrosion cracking, high strength and good weldability. Those steels are preferably used in industries combining hydrogen and loads. Hydrogen location in addition to hydrogen binding energy with the steel's defects are of great importance for the analysis of hydrogen embrittlement model in that steel. It is known from previously published works that the susceptibility to hydrogen embrittlement will depend on the competition between reversible and irreversible traps; meaning a direct relation to the hydrogen's state and position in the steel. In this work, we examine the local hydrogen concentration, trapping and distribution by two modern and advanced techniques: thermal desorption spectrometry (TDS) and we support it by time of flight-secondary ion mass spectrometer (ToF-SIMS). In this paper, we support and give for the first time new insights and better understanding to the hydrogen embrittlement mechanism in SAF 2205. The trapping energies levels were calculated using TDS and Lee and Lee's model. This model revealed reversible in addition to irreversible trapping sites. Also the trapping controlling mechanism was found to be a combination of detrapping controlled mechanism and diffusion controlled mechanism. The use of ToF-SIMS for local imaging the distribution of hydrogen species supports the discussion of the different hydrogen traps in this type of steel. The hydrogen embrittlemet phenomenon in SAF 2205 will be discussed in details in that paper. KW - Hydrogen trapping KW - Duplex stainless steel KW - Thermal desorption spectrometry (TDS) KW - ToF-SIMS PY - 2017 DO - https://doi.org/10.1016/j.jallcom.2016.11.184 SN - 0925-8388 SN - 1873-4669 VL - 695 SP - 2689 EP - 2695 PB - Elsevier B.V. AN - OPUS4-38856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling and diagnostics of laser induced plasma for needs of spectrochemical analysis N2 - Two topics will be addressed: (1) calibration-free LIBS based on Monte Carlo spectral optimization and (2) insight into the possibility of simultaneous elemental and molecular analysis by LIBS. Both topics heavily rely on modeling of laser induced plasma and are closely connected to experiment. In Monte Carlo LIBS (MC LIBS), concentrations are found by fitting model-generated synthetic spectra to experimental spectra. The model of a static uniform isothermal plasma in local thermodynamic equilibrium is employed. Many configurations of plasma parameters and their corresponding spectra are simultaneously generated using a graphic processing unit (GPU). Using the GPU allows for the reduction of computational time down to several minutes for one experimental spectrum that presents the significant progress in comparison with earlier versions of MC LIBS. The method is tested by analyzing industrial oxides containing various concentrations of CaO, Fe2O3, MgO, and TiO2. The agreement within several percent between found and certified concentrations is achieved. Next, a newly developed collisional-dominated model of a laser induced plasma is introduced. The model includes the coupled Navier-Stokes, state, radiative transfer, and material transport equations and incorporates plasma chemistry through the equilibrium approach based on the use of atomic and molecular partition functions. Simple chemical systems are modeled including ablation of Si and C in N2 and Ar atmospheres.The model is used to study evolution of number densities of atomic and molecular species in the expanding plasma plume. The distribution is compared to experimental observations obtained by optical imaging and tomography. To further verify the model, dynamic plasma T2 - FLAMN 2016 CY - St. Petersburg, Russia DA - 27.06.2016 KW - Plasma diagnostics KW - Laser induced plasma KW - LIBS KW - Plasma modeling PY - 2016 AN - OPUS4-38775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling and diagnostics of molecules in laser induced plasmasmodeling and diagnostics of molecules in laser induced plasmas N2 - A collisional-dominated model of a laser induced plasma will be presented which includes the coupled Navier-Stokes, state, radiative transfer, and material transport equations and incorporates plasma chemistry through the equilibrium approach based on the use of atomic and molecular partition functions. Simple chemical systems are modeled including ablation of Si, C, SiC, CaCl2 in N2 or Ar atmospheres with the formation of molecules N2, C2, Si2, CN, Cl2, SiN, SiC, CaCl, CaCl2 and their corresponding positive and negative ions1,2. The initial conditions are specially chosen to emulate the plasma state on the onset of expansion just after the laser pulse had ended. The model is used to study evolution of number densities of atomic and molecular species in the expanding plasma plume. The distribution is compared to experimental observations obtained by optical imaging and tomography. The model and experiment serve to elucidate mechanisms of molecular formation in LIPs, the topic which has recently received much attention in the LIBS community. T2 - LIBS 2016 CY - Chamonix, France DA - 12.09.2016 KW - Plasma diagnostics KW - Plasma physics PY - 2016 AN - OPUS4-38776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Modeling and diagnostics of molecules in laser induced plasmasmodeling and diagnostics of molecules in laser induced plasmas N2 - A collisional-dominated model of a laser induced plasma will be presented which includes the coupled Navier-Stokes, state, radiative transfer, and material transport equations and incorporates plasma chemistry through the equilibrium approach based on the use of atomic and molecular partition functions. Simple chemical systems are modeled including ablation of Si, C, SiC, CaCl2 in N2 or Ar atmospheres with the formation of molecules N2, C2, Si2, CN, Cl2, SiN, SiC, CaCl, CaCl2 and their corresponding positive and negative ions. The model is used to study evolution of number densities of atomic and molecular species in the expanding plasma plume. The distribution is compared to experimental observations obtained by optical imaging and tomography. The model and experiment serve to elucidate mechanisms of molecular formation in LIPs, the topic which has recently received much attention in the LIBS community. T2 - SCIX 2016 CY - Minneapolis, USA DA - 18.09.2016 KW - Plasma diagnostics KW - Plasma physics PY - 2016 AN - OPUS4-38777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - Fitting of physically motivated spectral models – a simple calibration-free method for evaluation of online NMR spectra N2 - Currently, research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algorithm to interpret the obtained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16-inch polymer tubing working as a flow cell. Single scan 1H NMR spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in non-deuterated solvents while its time-resolved behaviour was characterised with step tracer experiments. Through the application of spectral modeling the signal area for each reactant can be deconvoluted in the online spectra and thus converted to the respective concentrations or molar ratios. The signals which were suitable for direct integration were used herein for comparison purposes of both methods. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) CY - Kaiserslautern, Germany DA - 19.01.2017 KW - Online NMR spectroscopy KW - Thiol-ene coupling KW - Data processig PY - 2017 AN - OPUS4-39009 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eschlböck-Fuchs, S. A1 - Huber, N. A1 - Ahamer, C. M. A1 - Hechenberger, J. G. A1 - Kolmhofer, P. J. A1 - Heitz, J. A1 - Rössler, R. A1 - Demidov, Alexander A1 - Schmid, Thomas A1 - Gornushkin, Igor B. A1 - Panne, Ulrich A1 - Pedarnig, J. D. T1 - Application of laser-induced breakdown spectroscopy for the analysis of slags in industrial steel production N2 - Laser-induced breakdown spectroscopy (LIBS) is a fast and versatile technique for (semi) quantitative element analysis of solids, liquids, gases, and particulate matter. The LIBS method is used for optical sensing in various branches of industrial production. In the contribution we review some of our recent results on LIBS analysis of slags from secondary metallurgy in industrial steel making. Major oxides in steel slags are measured at-line and after homogenization using a calibration-free (CF) method. Two approaches for CF analysis based on the Boltzmann plot method and on the calculation of synthetic spectra are compared for the analysis of quaternary oxides. We also present the research in cooperation with our industrial partners in the process-analytical chemistry network PAC. T2 - 11. Kolloquium Arbeitskreis Prozessanalytik CY - Vienna, Austria DA - 30.11.2015 KW - Laser-induced breakdown spectroscopy (LIBS) KW - Process analytical technology KW - Steel slag PY - 2015 PB - Plandruck+ Gesellschaft m.b.H. CY - Wien AN - OPUS4-39005 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Sebastian A1 - Gluth, Gregor A1 - Peys, A. A1 - Onisei, S. A1 - Banerjee, D. A1 - Pontikes, Y. T1 - The fate of iron during the alkali-activation of synthetic (CaO-)FeOx-SiO2 slags: An Fe K-edge XANES study N2 - Slags from the nonferrous metals industry have great potential to be used as feedstocks for the production of alkali-activated materials. Until now, however, only very limited information has been available about the structural characteristics of these materials. In the work presented herein, synthetic slags in the CaO–FeOx–SiO2 system, representing typical compositions of Fe-rich slags, and inorganic polymers (IPs) produced from the synthetic slags by activation with alkali Silicate solutions have been studied by means of X-ray absorption near-edge structure (XANES) spectroscopy at the Fe K-edge. The iron in the slags was largely Fe2+, with an average coordination number of approximately 5 for the iron in the amorphous fraction. The increase in average oxidation number after alkali-activation was conceptualized as the consequence of slag dissolution and IP precipitation, and employed to calculate the degrees of reaction of the slags. The degree of reaction of the slags increased with increasing amorphous fraction. The iron in the IPs had an average coordination number of approximately 5; thus, IPs produced from the Fe-rich slags studied here are not Fe-analogs of aluminosilicate geopolymers, but differ significantly in terms of structure from the latter. KW - Alkali-activated slag KW - Inorganic polymers KW - Iron speciation KW - Nonferrous slag KW - X-ray absorption near-edge structure KW - X-ray absorption spectroscopy PY - 2018 DO - https://doi.org/10.1111/jace.15354 SN - 1551-2916 SN - 0002-7820 VL - 101 IS - 5 SP - 2107 EP - 2118 PB - John Wiley & Sons, Inc. AN - OPUS4-43880 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Prinz, Carsten A1 - Scholz, Gudrun A1 - Kemnitz, Erhard A1 - Emmerling, Franziska T1 - Ca-, Sr-, and Ba-Coordination polymers based on anthranilic acid via mechanochemistry N2 - Ca-, Sr-, and Ba-Based coordination polymers (CPs) were prepared mechanochemically by milling metal-hydroxide samples with anthranilic acid (oABAH). {[Ca(oABA)2(H2O)3]}n consists of one-dimensional polymeric chains that are further connected by a hydrogen-bonding network. {[Sr(oABA)2(H2O)2]·H2O}n is a one-dimensional CP in which water molecules bridge Sr2+ ions and increase the dimensionality by building an extended network. {[Ba(oABA)2(H2O)]}n crystallizes as a two-dimensional CP comprising one bridging water molecule. The cation radii influence the inorganic connectivity and dimensionality of the resulting crystal structures. The crystal structures were refined from powder X-ray diffraction data using the Rietveld method. The local coordination environments were studied via extended X-ray absorption fine structure (EXAFS) measurements. The compounds were further characterized using comprehensive analytical methods such as elemental analysis, thermal analysis, MAS NMR, imaging, and dynamic vapor sorption (DVS) measurements. Compounds 1, 2, and 3 exhibit small surface areas which decrease further after thermal annealing experiments. All compounds exhibit a phase transformation upon heating, which is only reversible in 3. KW - Mechanochemistry KW - XRD PY - 2019 DO - https://doi.org/10.1039/c9dt00991d SN - 1477-9226 SN - 1477-9234 VL - 48 IS - 19 SP - 6513 EP - 6521 PB - Royal Society of Chemistry AN - OPUS4-48014 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Separation of polystyrene nanoparticles with different coatings using 2D off-line coupling of asymmetrical flow field flow fractionation (AF4) and capillary electrophoresis (CE) N2 - The successful off-line coupling of asymmetrical flow field flow fractionation (AF4) and capillary electrophoresis (CE) for Separation of nanoparticles (NPs) with different surface coatings was shown. Two mixtures of polystyrene nanoparticles (PS-NPs) with comparable core sizes (20 nm and 50 nm) but different coatings (no coating/carboxyl-coated) were studied. Separation in either method resulted in non-baseline resolved or non-separated peaks. In contrast, two-dimensional off-line coupling of AF4 and CE resulted in clearly separated regions in their 2 D plots and can obviouly improve separation resolution. T2 - Anakon 2019 CY - Münster, Germany DA - 25.03.2019 KW - Capillary electrophoresis (CE) KW - Nanoparticles with same nominal diameter; surface coating; two-dimensional off-line coupling KW - Asymmetrical flow field flow fractionation (AF4) PY - 2019 AN - OPUS4-47746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neamtu, Mariana A1 - Nadejde, C. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Ababei, G. A1 - Panne, Ulrich T1 - Photocatalysis of γ-cyclodextrin-functionalised Fe3O4 nanoparticles for degrading Bisphenol A in polluted waters N2 - The efficiency, relatively low cost and eco-friendly nature of hydrogen peroxide-assisted photocatalysis treatment procedures are significant advantages over conventional techniques for wastewater remediation. Herein, we evaluate the behaviour of g-cyclodextrin (g-CD) immobilised on either bare or chitosan (CS)–functionalised Fe3O4 nanoparticles, for photodegrading Bisphenol A (BPA) in ultrapure water and in real wastewater samples. The BPA removal efficiencies with Fe3O4/g-CD and Fe3O4/CS/g-CD were compared with those of Fe3O4/b-CD, and were monitored under UVA irradiation at near-neutral pH. The addition of H2O2 at low concentrations (15 mmol L-1) significantly increased BPA photodegradation in the presence of each nanocomposite. The highest catalytic activity was shown by both Fe3O4/g-CD and Fe3O4/CS/g-CD nanocomposites (,60 and 27%BPA removal in ultrapure water and real wastewater effluent, respectively). Our findings reveal the superior performance of g-CD-functionalised Fe3O4 relative to that of Fe3O4/b-CD. The use of CD-based nanocomposites as photocatalytic materials could be an attractive option in the pre- or post-treatment stage of wastewaters by advanced oxidation processes before or after biological treatment. KW - Photooxidation KW - Sonochemical synthesis KW - Wastewater PY - 2019 DO - https://doi.org/10.1071/EN18181 SN - 1448-2517 VL - 16 IS - 2 SP - 125 EP - 136 PB - CSIRO Publishing CY - Clayton South AN - OPUS4-48316 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - LC-ELISA as a contribution to the validation of immunoassays N2 - Coupling ELISA and liquid chromatography yields a powerful too to detect cross-reacting substances, interfering matrix compounds and thus to validation of binding assays. T2 - CCQM Workshop: "Advances in Metrology in Chemistry and Biology" CY - Paris, France DA - 08.04.2019 KW - ELISA KW - Immunoassay KW - Validierung PY - 2019 AN - OPUS4-48322 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sötebier, Carina A. A1 - Weidner, Steffen A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Bettmer, J. T1 - Separation and quantification of silver nanoparticles and silver ions using reversed phase high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry in combination with isotope dilution analysis N2 - A reversed phase high performance liquid chromatography coupled to an inductively coupled Plasma mass spectrometer (HPLC–ICP-MS) approach in combination with isotope dilution analysis (IDA) for the separation and parallel quantification of nanostructured and ionic silver (Ag) is presented. The main Focus of this work was the determination of the ionic Ag concentration. For a sufficient stabilization of the Ions without dissolving the nanoparticles (NPs), the eluent had to be initially optimized. The determined Ag ion concentration was in a good agreement with results obtained using ultrafiltration. Further, the mechanism of the NP separation in the HPLC column was investigated. Typical size exclusion effects were found by comparing results from columns with different pore sizes. Since the recovery rates decreased with increasing Ag NP size and large Ag NPs did not elute from the column, additional interactions of the particles with the stationary phase were assumed. Our results reveal that the presented method is not only applicable to Ag NPs, but also to gold and polystyrene NPs. Finally, IDA-HPLC-ICP-MS experiments in single particle mode were performed to determine the particle cut-off size. The comparison with conventional spICP-MS experiments resulted in a similar diameter and particle size distribution. KW - ICP-MS KW - Silver nanoparticles KW - Speciation KW - High performance liquid chromatography KW - Isotope dilution analysis PY - 2016 DO - https://doi.org/10.1016/j.chroma.2016.09.028 SN - 0021-9673 VL - 1468 SP - 102 EP - 108 AN - OPUS4-37652 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Forschen - Prüfen - Beraten - Ziele und Aufgaben der Ressortforschung N2 - Der Vortrag gibt einen Überblick die deutsche Ressortforschung. Neben einer Einordnung in das deutsche Wissenschaftssystem werden in einem historischen Überblick die Besonderheiten der Ressortforschung diskutiert. Besonderes Augenmerk wird der Frage gewidmet „Was ist gute Ressortforschung“. Kritisch erscheint besonders die Vereinbarkeit von exzellenter Wissenschaft und seriöser und unabhängiger Politikberatung. T2 - Auftaktveranstaltung des BMVI-Expertennetzwerks Wissen - Können - Handeln CY - BMVI, Berlin, Germany DA - 19.04.2016 KW - Ressortforschung KW - Ressortforschungseinrichtung KW - Wissenschaftliche Politikberatung PY - 2016 AN - OPUS4-37530 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzweber, Markus T1 - Surface chemical characterization and shelf life studies of reference glycan microarrays using ToF-SIMS, XPS and fluorescence spectroscopy N2 - Covalent modification of surfaces with carbohydrates (glycans) is a prerequisite for a variety of glycomics-based biomedical applications, including functional biomaterials, glycan-arrays, and glycan-based biosensors. The chemistry of glycan immobilization plays an essential role in the bioavailability and function of surface bound carbohydrate moieties. For biomedical applications the stability over time (shelf life) of a glycan-array is a crucial factor. Basic requirements for the production of microarrays are first of all stable signals without any loss of quality. Therefore, the investigation of the shelf life for carbohydrate microarrays is an important part in the development of glycan-arrays. Motivated by the need of reliable quality control for glycan microarrays, we developed reference arrays using fluorescent model glycans. Since the long term stability of glycan microarrays is a crucial factor for their clinical application the shelf life at different storage conditions of glycan microarrays was studied in detail using the two model glycan compounds. Herein, we present a shelf life study of model glycan microarrays on epoxy modified glass surfaces over a period of 320 days. This was carried out using different analyzing techniques such as Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS), X-ray Photoelectron Spectroscopy (XPS) and Fluorescence Spectroscopy. To analyze and interpret the ToF-SIMS dataset the multivariate technique principal component analysis (PCA) was used. The dependence of the array´s shelf life upon storage conditions was specifically studied. T2 - SIMS Europe 2016 CY - Münster, Germany DA - 18.9.2016 KW - Glycan microarray KW - XPS KW - SIMS KW - Fluorescence spectroscopy PY - 2016 AN - OPUS4-37638 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Michalik-Onichimowska, Aleksandra A1 - Riedel, Jens A1 - Panne, Ulrich A1 - King, R. A1 - Maiwald, Michael T1 - “Click” analytics for “click” chemistry – a simple method for calibration-free evaluation of online NMR spectra N2 - Currently research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales ondemand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algorithm to interpret the obtained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16 inch polymer tubing working as a flow cell. Single scan 1H spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in non-deuterated solvents while its time-resolved behaviour was characterised with step tracer experiments Through the application of spectral modeling the signal area for each reactant can be deconvoluted in the online spectra and thus converted to the respective concentrations or molar ratios. The signals which were suitable for direct integration were used herein for comparison purposes of both methods. T2 - 4th European Conference on Process Analytics and Control Technology (EuroPACT 2017) CY - Potsdam, Germany DA - 10.05.2017 KW - Online NMR Spectroscopy KW - Process Analytical Technology KW - Click Chemistry KW - Reaction Monitoring KW - Process control KW - Indirect Hard Modeling KW - Spectral Modeling PY - 2017 SP - 156 EP - 157 CY - Frankfurt a. M. AN - OPUS4-40232 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nadejde, C. A1 - Neamtu, Mariana A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Ababei, G. A1 - Panne, Ulrich T1 - Characterization and application of Green Fenton-like catalysts for the removal of water pollutants N2 - Three types of magnetite-chitosan/iron oxalate/iron citrate nanoparticles (NP) were evaluated as magnetic heterogeneous catalysts for water treatment. T2 - PTIM 2015, 1st International Caparica Conference on Pollutant Toxic Ions and Molecules CY - Caparica, Portugal DA - 02.112015 KW - Bisphenol A degradation KW - Nanocatalysts KW - Characterization KW - Fenton oxidation KW - Wastewater PY - 2015 SN - 978-989-99361-6-4 SP - 186 EP - 187 PB - Proteomass AN - OPUS4-40082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bierstedt, Andreas A1 - Kersten, H. A1 - Glaus, Reto A1 - Gornushkin, Igor B. A1 - Panne, Ulrich A1 - Riedel, Jens T1 - Characterization of an airborne laser-spark ion source for ambient mass spectrometry N2 - An airborne laser plasma is suggested as an ambient ion source for mass spectrometry. Its fundamental physical properties, such as an excellent spatial and temporal definition, high electron and ion densities and a high effective cross section in maintaining the plasma, make it a promising candidate for future applications. For deeper insights into the plasma properties, the optical plasma emission is examined and compared to mass spectra. The results show a seemingly contradictory behavior, since the emitted light reports the plasma to almost entirely consist of hot elemental ions, while the corresponding mass spectra exhibit the formation of intact molecular species. Further experiments, including time- resolved shadowgraphy, spatially resolved mass spectrometry, as well as flow-dependent emission spectroscopy and mass spectrometry, suggest the analyte molecules to be formed in the cold plasma vicinity upon interaction with reactive species formed inside the hot plasma center. Spatial separation is maintained by concentrically expanding pressure waves, inducing a strong unidirectional diffusion. The accompanying rarefaction inside the plasma center can be compensated by a gas stream application. This replenishing results in a strong increase in emission brightness, in local reactive species concentration, and eventually in direct mass spectrometric sensitivity. To determine the analytical performance of the new technique, a comparison with an atmospheric pressure chemical ionization (APCI) source was conducted. Two kitchen herbs, namely, spearmint and basil, were analyzed without any sample pretreatment. The presented results demonstrate a considerably higher sensitivity of the presented laser-spark ionization technique. KW - Laser-spark KW - Laser induced plasma KW - Ambient mass spectrometry KW - Optical emission spectroscopy KW - Ionization PY - 2017 DO - https://doi.org/10.1021/acs.analchem.6b04178 SN - 0003-2700 SN - 1520-6882 VL - 89 IS - 6 SP - 3437 EP - 3444 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-39474 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Meyer, Klas T1 - Fitting of physically motivated spectral models – a simple calibration-free method for evaluation of online NMR spectra N2 - Currently, research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algorithm to interpret the obtained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16-inch polymer tubing working as a flow cell. Single scan 1H NMR spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in non-deuterated solvents while its time-resolved behaviour was characterised with step tracer experiments. Through the application of spectral modeling the signal area for each reactant can be deconvoluted in the online spectra and thus converted to the respective concentrations or molar ratios. The signals which were suitable for direct integration were used herein for comparison purposes of both methods. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Photoreaction KW - Online NMR spectroscopy KW - Spectral modeling KW - Reaction monitoring PY - 2017 AN - OPUS4-39694 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Phukphatthanachai, Pranee T1 - Determination of total sulfur in a metal matrix by ICP-IDMS: Example Cu matrix N2 - Previously on sulfur determination in metal revealed a lack of traceability and inconsistent results. Solving the problems a reference procedure for sulfur measurement in metal are required to build up a reliable reference value. In this study a procedure was developed for quantification of total sulfur at low concentration (in sub ppm level) in metal using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS). The ion exchange method and complexing agent were applied in this procedure to avoid loading large amount of metal into the instrument. Adding ammonia as a complexing agent into sample solution to reduce sulfur-metal co-elute. The procedure shows high performance and it is expressed in % recovery of sulfur (> 90%) and % metal elimination (>99 %). Additionally, relative measurement uncertainties were calculated less than 1.5 % and the results are traceable directly to SI units. This study would establish as reference procedure for sulfur measurement in metal sample which fit for these purpose as follows; for certified reference material and assigned value for inter-laboratory comparison. T2 - Anwendertreffen Plasmaspektrometrie 2016 CY - Berlin, Germany DA - 22.02.2016 KW - IDMS KW - Sulfur-matrix separatio KW - Purity assessment PY - 2016 AN - OPUS4-40027 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Neamtu, M. A1 - Nadejde, C. A1 - Hodoroaba, Vasile-Dan A1 - Schneider, Rudolf A1 - Panne, Ulrich T1 - Singlet oxygen generation potential of porphyrin-sensitized magnetite nanoparticles: Synthesis, characterization and photocatalytic application N2 - Singlet oxygen generation potential of two novel free-base-porphyrin photocatalysts was investigated. The freebase-porphyrin-sensitized Fe3O4 magnetic nanoparticles (MNPs) were tested for the degradation of the model pollutant Bisphenol A (BPA) in aqueous solution, for the first time. MNPs with either cubic or spherical shape were synthesized using the sonochemical approach, followed by sensitizing with photoactive 4,4′,4′′,4′′′- (Porphine-5,10,15,20-tetrayl)tetrakis(benzoic acid) (TCPP). The resulted photocatalysts were characterized in detail by scanning and transmission electron microscopy, Brunauer–Emmett–Teller analysis, spectral techniques and vibrating sample magnetometry. The electron spin resonance experiments have confirmed the high activity of the photocatalysts through the efficient formation of singlet oxygen in solution. The optimum operational parameters for BPA degradation were established as follows: 1.0 μmol L−1 BPA, 1.0 g L−1 of photocatalyst, 100 μmol L−1 H2O2, under UVA irradiation. In these conditions, the results for both photocatalysts revealed that after only 10 min of reaction, over 64% and ca. 90% of BPA have been removed from solution in the absence and presence of H2O2, respectively. Whereas after 60 minutes of treatment, only 24% of BPA in real wastewater effluent samples were removed under UVA irradiation in the absence of H2O2, showing the high complexity of real wastewater. Moreover, both photocatalysts were successfully used for BPA removal in three consecutive runs, without significant loss of catalytic features. KW - Bisphenol A KW - Magnetpartikel KW - Photooxidation KW - Singulettsauerstoff KW - TEM KW - SEM KW - Brunauer-Emmett-Teller KW - Katalysator KW - Abwasser KW - ESR PY - 2018 DO - https://doi.org/10.1016/j.apcatb.2018.03.079 SN - 0926-3373 VL - 232 SP - 553 EP - 561 PB - Elsevier B.V. CY - Amsterdam, NL AN - OPUS4-45267 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sobol, Oded T1 - Observations of the deuterium distribution and the structural changes in standard and lean duplex stainless steels by ToF-SIMS and EBSD N2 - Duplex (DSS) and austenitic stainless steels (ASS) are frequently used in many energy related applications. The duplex grade is considered to have outstanding mechanical properties as well as good corrosion resistance. The austenitic phase combines high ductility, even at low temperatures, with sufficient strength, and therefore such materials are applied in storage and transport of high-pressure hydrogen. During service in acidic environments large amounts of hydrogen can ingress into the microstructure and induce many changes in the mechanical properties of the steel. Embrittlement of steels by hydrogen remains unclear even though this topic has been intensively studied for several decades. The reason for that lies in the inability to validate the proposed theoretical models in the sub-micron scale. Among the very few available methods nowadays, Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) enables a highly accurate mapping of hydrogen in the microstructure in a spatial resolution below 100 nm. In the present work ToF-SIMS was used as a main tool in order to investigate the effect of deuterium on a duplex microstructure of lean and standard DSSs during and after the electrochemical charging process. Electrochemical charging simulates the service of a component in acidic environments under conditions of cathodic protection that are commonly applied to prevent corrosion reactions. ToF-SIMS after multivariate data analysis (MVA) was combined with high resolution topographic images and electron back-scattered diffraction (EBSD) data to characterize the structural changes. It was observed that the ferritic phase was affected almost identical in all steels whereas in the austenitic phase significant differences were obtained in the lean duplex in comparison to the standard DSS. The obtained results have been compared to similar investigations on a AISI 304L austenitic stainless steel. The advantage of the combined techniques is reflected by the ability to correlate the hydrogen distribution in the microstructure and the resulted phase transformation. T2 - Third International Conference on Metals & Hydrogen CY - Ghent, Belgien DA - 29.05.2018 KW - Data-fusion KW - ToF-SIMS KW - PCA KW - DSS KW - LDX KW - EBSD PY - 2018 AN - OPUS4-45094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholz, Philipp A1 - Ulbricht, Alexander A1 - Joshi, Y. A1 - Gollwitzer, Christian A1 - Weidner, Steffen T1 - Microstructure of polymer-imprinted metal–organic frameworks determined by absorption edge tomography N2 - Mechanochemically synthesized metal–organic Framework material HKUST-1 in combination with acrylonitrile butadiene styrene polymer was used to form a polymer metal–organic framework composite material by a simple extruder. This composite filament was used for 3D printing. Xray diffraction measurements were used to prove the homogeneous distribution of the metal–organic framework in the polymer on a centimeter scale, whereas X-ray Absorption Edge Tomography using a synchrotron radiation source was able to evaluate the 3D distribution of the metal–organic framework material both in the filament and the resultant printed sample with a resolution of a few lm. Our very first data indicate that, apart from a few clusters having significantly higher Cu concentration, HKUST-1 is distributed homogeneously down to the 100 lm length scale in both polymer bulk materials in the form of clusters with a size of a few lm. Absorption Edge Tomography in combination with data fusion also allows for the calculation of the metal–organic framework amount located on the external polymer surface. KW - MOF KW - Polymer KW - AET PY - 2019 DO - https://doi.org/10.3139/146.111817 SN - 1862-5282 SP - 1 EP - 10 PB - Carl Hanser Verlag AN - OPUS4-49483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nietzold, Carolin A1 - Dietrich, Paul A1 - Lippitz, Andreas A1 - Panne, Ulrich A1 - Unger, Wolfgang T1 - Cyclodextrin – ferrocene host – guest complexes on silicon oxide surfaces N2 - Research on carbohydrate based interactions with proteins, nucleic acids or antibodies has gained increased interest in the last years especially in clinical diagnosis or drug development. The efficiency of diagnostic interfaces depends upon the number of probe molecules, e.g. carbohydrates. The control of surface parameters as density and distribution of immobilized carbohydrates is essential for a reliable interaction with protein analytes. A controlled production of biomolecular interfaces can be reached by a stepwise quality control during buildup of these biointerfaces. Here, ß-amino-cyclodextrin molecules were attached to amine-reactive silicon oxide surfaces via click chemistry to construct a model biosensor surface. The amount of surface bound carbohydrates was determined indirectly after chemical derivatization with 4-(trifluoromethyl)-benzylamine (TFMBA). Moreover, these surfaces were used to form host-guest complexes of ferrocene (guest) and β-cyclodextrin (host) moieties to mimic the target binding (sensing) of the model biosensor. Surface chemical analysis of all steps during biosensor construction was performed using X-ray photoelectron spectroscopy (XPS) and near-edge X-ray absorption fine structure spectroscopy (NEXAFS). Our approach widens the possibilities to generate switchable surfaces based on ß-Cyclodextrin surfaces for biosensor applications. KW - ß-amino-cyclodextrin KW - Ferrocene KW - Guest complexe KW - XPS KW - NEXAFS PY - 2016 DO - https://doi.org/10.1002/sia.5958 SN - 0142-2421 SN - 1096-9918 VL - 48 IS - 7 SP - 606 EP - 610 PB - Wiley AN - OPUS4-36856 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Stable isotope amount ratio analysis by using high-resolution continuum source graphite furnace molecular absorption spectrometry N2 - Analysis of stable isotopes has been used as proof of provenance of mineral and biological samples, to estimate a contamination source and to determine geological processes. This kind of analysis needs high accuracy and precision for reliable conclusions. Currently, stable isotope analysis is dominated by mass spectrometric techniques that are time consuming and expensive. Here we present a fast and low cost alternative for isotope analysis of boron and magnesium: high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS-GFMAS). Two stable isotope systems were evaluated separately: boron (10B:11B) and magnesium (24Mg:25Mg:26Mg). Their isotope amount ratios were estimated by monitoring their absorption spectra in-situ generated monohydrides. The molecular absorption spectrum of a XH molecule (X= B or Mg) with n isotopes would be a linear combination of n isotopologue spectra and the amount of each component (isotope) could be calculated by a multivariate regression (n= 2 and 3 for B and Mg respectively). For the analysis of boron certified reference materials (CRM), the band 1→1 for the electronic transition X1Σ+ → A1Π was measured around wavelength 437.1 nm. Since boron has a memory effect in graphite furnaces, a combination of 2 % (v/v) hydrogen gas in argon, 1 % trifluoromethane in argon, an acid solution of calcium chloride and mannitol as chemical modifiers were used during the BH vaporization at 2600 °C. Partial least square regression (PLS) for analysis of samples was applied. For this, a spectral library with different isotope ratios for PLS regression was created. Magnesium does not have memory effect. Therefore, only 2 % of hydrogen in argon as gas modifier during vaporization at 2500 °C was employed for analysis of magnesium CRM. Absorption spectra of MgH for the X2Σ→A2Π electronic transition (band 0→0) were recorded around wavelength 513.45 nm. A similar PLS procedure to the BH was applied. Results for B and Mg CRM are metrologically compatible with those reported by mass spectrometric methods. An accuracy of 0.08 ‰ for B and 0.1 ‰ Mg was obtained as the average deviation from the isotope CRM. Expanded uncertainties with a coverage factor of k = 2 range between 0.10 - 0.40 ‰. T2 - FACSS / SciX Conference 2017 CY - Reno, NV, USA DA - 08.10.2017 KW - Boron isotopes KW - High-Resolution Continuum Source Molecular Absorption Spectrometry KW - Graphite furnace KW - Isotopic shift KW - Hydride KW - Isotope ratio PY - 2017 AN - OPUS4-43350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Janine A1 - Fettig, I. A1 - Philipp, Rosemarie A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Fisicaro, P. A1 - Alasonati, E. T1 - Determination of tributyltin in whole water matrices under the European water framework directive N2 - Monitoring of water quality is important to control water pollution. Contamination of the aquatic systemhas a large effect on human health and the environment. Under the European Water Framework Directive(WFD) 2000/60/EC and the related directive on environmental quality standards (EQS) in the field of waterpolicy 2008/105/EC, the need for sensitive reference methods was highlighted. Since tributyltin (TBT) isone of the WFD listed priority substances a method was developed which is capable to qualify and quantifythe pollutant at the required low WFD EQS of 0.2 ng L⁻¹ in whole water bodies, i.e. in non-filtered watersamples with dissolved organic carbon and suspended particulate matter. Therefore special attention waspaid on the interaction of TBT with the suspended particulate matter and humic substances to obtain acomplete representation of the pollution in surface waters. Different water samples were investigatedvarying the content of organic dissolved and suspended matter. Quantification was performed usingspecies-specific isotope dilution (SSID) and gas chromatography with inductively coupled plasma massspectrometry (GC-ICP-MS). Different sample treatment strategies were evaluated and compared. Theprocess of internal standard addition was investigated and optimized, hence the equilibrium betweeninternal standards and matrix is of primary importance to perform accurate SSID. Samples spiked at EQSlevel were analyzed with a recovery between 95 and 105 %. Additionally real surface water samples wereinvestigated and the TBT concentration for the whole water body was determined and compared withconventional routine analysis method. KW - Tributyltin (TBT) KW - Environmental quality standard (EQS) KW - Isotope dilution KW - Humic acid KW - Surface water KW - Suspended particulate matter PY - 2016 DO - https://doi.org/10.1016/j.chroma.2016.06.068 SN - 0021-9673 VL - 1459 SP - 112 EP - 119 AN - OPUS4-36930 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Franziska A1 - Fendel, Nicole A1 - Greiser, Sebastian A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - Impact is important - Systematic investigation of the influence of milling balls in mechanochemical reactions N2 - A newly established in situ technique using Raman spectroscopy was employed for the detailed kinetic investigation of mechanochemical reaction pathways. This approach was applied for the systematic investigation of the direct influence of colliding balls on the reaction rate constants of a mechanochemical cocrystallization reaction. As a model reaction, the mechanochemical cocrystallization of felodipine and the coformer imidazole was investigated. Keeping the total ball mass constant by varying the number of milling balls, our study reveals that the impact of each single collision has a more significant influence on the reaction kinetics than expected. KW - Mechanochemistry KW - In situ KW - Cocrystal PY - 2017 UR - http://pubs.acs.org/doi/abs/10.1021/acs.oprd.6b00435 DO - https://doi.org/10.1021/acs.oprd.6b00435 SN - 1083-6160 SN - 1520-586X VL - 21 IS - 4 SP - 655 EP - 659 AN - OPUS4-40355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Unger, Wolfgang T1 - Tof-SIMS imaging of Deuterium in DSS steel microstructures and data fusion with SEM topography data: Towards a better understanding of hydrogen assisted cracking in steel N2 - The use of duplex stainless steels (DSS) in energy related applications is well known. Nowadays, DSS steels become more favorable than austenitic steels due to the outstanding mechanical properties, the good corrosion resistance and the lower nickel content. However, the use of the duplex grade in acidic environments such as seawater often leads to severe degradation of the structural integrity of the steel by hydrogen-induced/assisted cracking (HAC) phenomena, which can eventually result in premature failure. Hydrogen assisted degradation and cracking of steels are active fields of research even though this topic is intensively studied for more than a century. A bottleneck is the analytical validation of the theoretical models proposed ion the literature at the sub-micron scale. Industrial and the research communities see a need for an accurate analytical method by which it is possible to image the distribution of hydrogen in the microstructure of a steels or and other alloys. Among the very few available methods hydrogen imaging methods, Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) has the principal capability for mapping of hydrogen in a steel’s microstructure. The combination of ToF-SIMS with multivariate data analysis (MVA), electron microscopy (SEM) and electron-backscattered diffraction (EBSD) is a powerful approach for providing chemical and structural information. The use of data fusion techniques has been shown recently to enhance the better understanding of the hydrogen induced degradation processes in in a DSS steel. T2 - The Scientific International Symposium on SIMS and Related Techniques Based on Ion-Solid Interactions (SISS19) CY - Kyoto, Japan DA - 11.5.17 KW - Hydrogen KW - DSS steel KW - ToF SIMS KW - SEM KW - EDX KW - EBSD KW - Data fusion PY - 2017 AN - OPUS4-40276 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riaz, Muhammad T1 - Influence of the of dealumination and porosity on the acid sites of natural zeolite clinoptilolite N2 - Heavy feedstock from crude and bio oil is a widely available and renewable resource for production of fuel and starting materials for other organic valuables by cracking or hydrocracking. Catalytic processing of heavy feedstock can meet the increased demand of energy up to a great extent. It requires the application of acidic catalysts like zeolites. However, the used synthetic catalysts are difficult to recover and reuse and are mostly spent. The use of natural zeolite as spent catalysts may open new perspectives in the chemical use of heavy feed feedstock by chemical conversion. Natural zeolites are not expensive, widely available and environment friendly. Clinoptilolite is the most abundant natural zeolite. Clinoptilolite has a crystalline structure with a defined micropore system of medium size showing unique ion exchange and sorption properties. However, it is catalytically active only in the H-form. Also certain porosity is required for improvement of the accessibility of active sites. This paper deals with the tuning of acid properties and of the mesoporosity of the clinoptilolite by variation of the Si/Al framework ratio, extra-framework aluminum and modification of the porosity by specific acid and water vapor treatment. The preparation of hierarchical pore structures containing interconnected micro-meso-macropores is an important factor influencing the catalytic performance. The obtained materials have been characterized by XRD, TEM, FTIR, Raman, TG/DSC. The chemical composition has been determined by ICP-AES. The porosity have been investigated by nitrogen adsorption desorption measurements. The acidity has been measured by Ammonia-TPD. The extent of dealumination, stability of the clinoptilolite against acid treatment and the change in the nature of acid sites and their local structure has been studied by solid state 29Si and 27Al MAS NMR spectroscopy in detail. The catalytic activity has been investigated in the acetalization of benzaldehyde with 1,3-butanediol. The impact of the porosity, change of the Si/Al ratio as well as present Al species on catalytic properties will be discussed. T2 - Deutsche Zeolith Tagung 2016 CY - Gießen, Germany DA - 02.03.2016 KW - Natural zeolite Clinoptilolite PY - 2016 AN - OPUS4-40681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - “Click” analytics for “click” chemistry – a simple method for calibration-free evaluation of online NMR spectra N2 - Currently research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algorithm to interpret the obtained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16 inch polymer tubing working as a flow cell. Single scan 1H spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in non-deuterated solvents while its time-resolved behaviour was characterised with step tracer experiments Through the application of spectral modeling the signal area for each reactant can be deconvoluted in the online spectra and thus converted to the respective concentrations or molar ratios. The signals which were suitable for direct integration were used herein for comparison purposes of both methods. T2 - EuroPACT 2017 CY - Potsdam, Germany DA - 10.05.2017 KW - Online NMR Spectroscopy PY - 2017 AN - OPUS4-40283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eschlböck-Fuchs, S. A1 - Demidov, Alexander A1 - Gornushkin, Igor B. A1 - Schmid, Thomas A1 - Rössler, R. A1 - Huber, N. A1 - Panne, Ulrich A1 - Pedarnig, J. D. T1 - Tomography of homogenized laser-induced plasma by Radon transform technique N2 - Tomography of a laser-induced plasma in air is performed by inverse Radon transform of angle-resolved plasma images. Plasmas were induced by single laser pulses (SP), double pulses (DP) in collinear geometry, and by a combination of single laser pulses with pulsed arc discharges (SP-AD). Images of plasmas on metallurgical steel slags were taken at delay times suitable for calibration-free laser-induced breakdown spectroscopy (CFLIBS). Delays ranged from few microseconds for SP and DP up to tens of microseconds for SP-AD excitation. The white-light and the spectrally resolved emissivity ε(x,y,z) was reconstructed for the three plasma excitation schemes. The electron number density Ne(x,y,z) and plasma temperature Te(x,y,z) were determined from Mg and Mn emission lines in reconstructed spectra employing the Saha-Boltzmann plot method. The SP plasma revealed strongly inhomogeneous emissivity and plasma temperature. Re-excitation of plasma by a second laser pulse (DP) and by an arc discharge (SP-AD) homogenized the plasma and reduced the spatial variation of ε and Te. The homogenization of a plasma is a promising approach to increase the accuracy of calibration-free LIBS analysis of complex materials. KW - Plasma tomography KW - Laser induced plasma KW - Radon transform technique KW - Laser induced breakdown spectroscopy (LIBS) KW - Steel slag KW - Calibration-free analysis PY - 2016 DO - https://doi.org/10.1016/j.sab.2016.07.007 VL - 123 SP - 59 EP - 67 PB - Elsevier B.V. AN - OPUS4-37452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sobol, Oded A1 - Holzlechner, Gerald A1 - Nolze, Gert A1 - Wirth, Thomas A1 - Eliezer, D. A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) imaging of deuterium assisted cracking in a 2205 duplex stainless steel microstructure N2 - In the present work, the influence of deuterium on the microstructure of a duplex stainless steel type EN 1.4462 has been characterized by Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) supported by scanning electron microscopy (SEM), focused ion beam (FIB), electron back scattered diffraction(EBSD) and energy dispersive x-ray (EDX) investigations. Characterization has been carried out before and after electrochemical charging with deuterium which has been used as a tracer, due to its similar behavior to hydrogen in the steel microstructure. In a first approach, the distribution of the deuterium occurring at temperatures above 58 °C has been visualized. Further it turned out that sub-surface micro blisters are formed in the ferrite-austenite interface, followed by the formation of needle shaped plates and subsequent cracking at the ferrite surface. In the austenite phase, parallel cracking alongside twins and hexagonal close packed (martensitic) regions has been observed. In both phases and even in the apparent interface, cracking has been associated with high deuterium concentrations, as compared to the surrounding undamaged microstructure. Sub-surface blistering in the ferrite has to be attributed to the accumulation and recombination of deuterium at the ferrite-austenite interface underneath the respective ferrite grains and after fast diffusing through this phase. Generally, the present application of chemometric imaging and structural analyses allows characterization of hydrogen assisted degradation at a sub-micron lateral resolution. KW - ToF-SIMS KW - Hydrogen assisted cracking KW - Hydrogen embrittlement KW - SEM KW - FIB KW - EBSD PY - 2016 UR - http://www.sciencedirect.com/science/article/pii/S0921509316310334 DO - https://doi.org/10.1016/j.msea.2016.08.107 SN - 0921-5093 VL - 676 SP - 271 EP - 277 PB - Elsevier B.V. AN - OPUS4-37298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Holzweber, Markus A1 - Sobol, Oded A1 - Wirth, Thomas A1 - Böllinghaus, Thomas A1 - Unger, Wolfgang T1 - Deuterium permeation and cracking in duplex steels as viewed by ToF-SIMS and HR-SEM with data fusion N2 - Better understanding of hydrogen assisted degradation and trapping mecha-nisms requires sufficient imaging techniques for respective hydrogen-microstructure interaction studies, in particular with multi-phase metallic micro-structures [1]. The present work is focusing on the elucidation of deuterium be-havior in two austenitic-ferritic duplex stainless steels (DSS) under the assumption that deuterium behaves in many ways similarly to hydrogen [2]. For case studies standard 2205 and lean 2101 DSSs were chosen due to the extensive use of these steels in industry [3]. The analyses were conducted by using a novel in-situ permeation and Time-of-Flight secondary ion mass spectrometry (ToF-SIMS) imaging technique or by ex-situ ToF-SIMS imaging following electrochemical charging experiments. Another pioneering procedure was data fusion (including chemometry) of results of powerful laterally resolved chemical analysis and high resolution structural characterization techniques . Results for the ex-situ observations showed a different influence of deuterium loading on the two steel grades as well as different damage mechanisms in each phase. Formation of sub-surface blisters between the ferrite and austenite were obtained in both the standard and the lean DSS. In both steels, an increased deuterium concentration was observed around deformed regions such as cracks, confirming that they originate from the presence of deuterium [4]. The formation of parallel cracks was obtained only in the austenite within the standard duplex whereas in the lean duplex the highest intensity of deuterium was obtained in the austenite along the ferrite-austenite interphase. In comparison, application of the novel in-situ permeation technique enabled to register and record the deuterium permeation through the material and the respective saturation sequence of the two phases as well as the interfaces. Faster diffusion of the deuterium was observed in the ferrite and a direct proof for deuterium enrichment at the austenite-ferrite interface has been given [1]. The integration of the specified techniques gives a better insight into the processes leading to hydrogen induced failure. These two experimental techniques provide very valuable tools for elucidation of respective metallurgical failure mechanisms that can be used for the validation of respective numerical models for hydrogen assisted cracking (HAC). T2 - 19. Arbeitstagung Angewandte Oberflächenanalytik CY - Soest, Germany DA - 05.09.2016 KW - ToF-SIMS KW - Hydrogen assisted cracking KW - Data fusion KW - SEM PY - 2016 AN - OPUS4-37484 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Influence of experimental conditions and calculation method on hydrogen diffusion coefficient evaluation at elevated temperatures N2 - Hydrogen-assisted cracking (HAC) represents a significant failure risk for (high strength) creep resistant low-alloyed steel components in fossil-fired power plant applications at temperatures of up to and above 200 °C. This particularly applies to respective start-up and shut-down processes associated with alternating service-conditions in terms of load flexible power plants. For quantitative determination of localized crack critical hydrogen concentrations, the temperature dependent hydrogen diffusion coefficients have to be determined as exactly as possible. However, available literature provides a wide range of hydrogen diffusion coefficients for low alloyed steels with similar microstructures. Additionally, the available diffusion data seem not to be very reliable and their scatter increases with decreasing temperature. One reason is that the experimental boundary conditions can have a major impact on the determination of respective effective diffusion coefficients. Hence, the scope of this study is to evaluate the influence of the experimental boundary conditions on the derived diffusion coefficients. In addition, different methods for calculating diffusion coefficients are discussed. To elucidate such influences and to draw a line to practical application, the diffusion and trapping behavior in the creep resistant steel 7CrMoVTiB10 10 has been studied. For such purpose, hydrogen charged specimens were isothermally degassed at different temperatures using carrier gas hot extraction (CGHE). Based on experimental data, a numerical model has been developed by which the hydrogen transport behavior and the respective hydrogen distribution during CGHE can be assessed. It is demonstrated that the specimen heating rate has a large influence on the calculated diffusion coefficients under assumption of isothermal degassing which elsewhere has been underestimated in the assessment of diffusion data in creep-resistant steels. The numerical results suggest that calculation methods for diffusion coefficients are limited if compared to experimental results. It also turned out that the sample preparation time before CGHE can enormously influence determined diffusion coefficients. Consequently, non-homogeneous hydrogen concentration profiles have to be anticipated in the simulations to arrive at characteristic effusion curves consistent to respective CGHE experiments. In turn, validated diffusion coefficients are now available for the low-alloyed Cr-Mo-V steel which might be helpful to calculate appropriate hydrogen removal heat treatment procedures, for instance. T2 - International Hydrogen Conference - Material Performance in Hydrogen Environments CY - Jackson Lake Lodge, Moran, Wyoming, USA DA - 11.09.2016 KW - Hydrogen diffusion KW - Elevated temperatures KW - Welding KW - Creep-resistant steel KW - Numerical modeling KW - Calculation PY - 2016 AN - OPUS4-37403 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jakubowski, Norbert T1 - Metal detection at cellular levels by use of laser ablation ICP-MS N2 - We are using laser ablation (LA)-ICP-MS to image the local distribution of elements (metals and hetero-elements) directly or (metallo-)proteins by metal-tagged antibodies in cells and tissue indirectly. Different applications will be discussed to demonstrate the state of the art and to visualize the elemental distribution pattern in soft bio-materials (tissue, single cells). In the first application Pt-containing drugs for cancer treatment are investigated and elemental distribution pattern are shown for tissue samples from animal experiments. Different standardization and quantification schemes including isotope dilution analysis will be discussed. In the second application, which is dedicated to toxicological research, the up-take of nano-particles by single cells are discussed and metal containing stains are used to visualize the distribution of nano-particles, proteins and DNA in a single cell simultaneously. This information is correlated with the distribution of the nanoparticles to identify the cell compartments where nano-particles are enriched. Quantification schemes have been developed to transform the measured intensities into number of particles up taken by the cells. In the third and last application LA-ICP-MS is applied to visualize the local distribution of proteins, which are used as bio-markers for prostate cancer. For this purpose, biopsy samples from patients have been simultaneously stained by eight differently metal-tagged antibodies in a multiplex approach. Detection of house-keeping proteins serves as internal standards to overcome differences in protein expression. Additionally ink-jet printing of metal doped inks onto the surface of these tissue samples has been applied for internal standardization and drift corrections. Finally future trends to develop an “elemental microscope” will be discussed. T2 - PITTCON 2017 CY - Chicago, IL, USA DA - 05.03.2017 KW - Element-microscopy KW - LA-ICP-MS KW - Nanoparticles KW - Immuno-assays PY - 2017 AN - OPUS4-39364 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon T1 - “Click” analytics for “click” chemistry – a simple method for calibration-free evaluation of online NMR spectra N2 - Currently research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual campaigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market [1]. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algo-rithm to interpret the obtained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16 inch polymer tubing working as a flow cell. Single scan 1H spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s. T2 - 11. Doktorandenseminar 2017 des Arbeitskreis Prozessanalytik der GDCh und DECHEMA CY - Berlin, Germany DA - 12.03.2017 KW - Online NMR Spectroscopy KW - Click chemistry KW - Data analysis PY - 2017 AN - OPUS4-39397 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Panne, Ulrich A1 - Falkenhagen, Jana T1 - Power of ultra performance liquid chromatography/electrospray ionization-MS reconstructed ion chromatograms in the characterization of small differences in polymer microstructure N2 - From simple homopolymers to functionalized, 3-dimensional structured copolymers, the complexity of polymeric materials has become more and more sophisticated. With new applications for instance in the semiconductor or pharmaceutical industry, the requirements for the characterization have risen with the complexity of the used polymers. For each additional distribution, an additional dimension in analysis is needed. Small, often isomeric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector, but affect the properties of materials significantly. For a drug delivery system for example, the degree of branching and branching distribution is crucial for the formation of micelles. Instead of a complicated, time consuming and/or expensive 2d-chromatography or ion mobility spectrometry (IMS) method, that also has its limitations, in this work a simple approach using size exclusion chromatography (SEC) coupled with electrospray ionization mass spectrometry (ESI) is proposed. The online coupling allows the analysis of reconstructed ion chromatograms (RIC) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities. Although some microstructural heterogeneities like short chain branching can for large polymers be characterized with methods such as light scattering, for oligomers where the heterogeneities just start to form and their influence is at the maximum, they are inaccessible with these methods. It is also shown, that with a proper calibration even quantitative information can be obtained. This method is suitable to detect small differences in e. g. branching, 3d-structure, monomer sequence or tacticity and could potentially be used in routine analysis to quickly determine deviations. KW - Polymer KW - Microstructure KW - UPLC KW - ESI-TOF-MS KW - Reconstructed ion chromatograms PY - 2018 DO - https://doi.org/10.1021/acs.analchem.7b05214 SN - 0003-2700 SN - 1520-6882 VL - 90 IS - 5 SP - 3467 EP - 3474 PB - ACS Publ. CY - Washington, DC AN - OPUS4-44423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Phukphatthanachai, Pranee T1 - Quantification of sulfur in copper metals and its alloys by ICP-IDMS N2 - Sulfur is one of the major impurity elements in copper. Previously applied methods for the quantification of sulfur in copper and other pure metals revealed a lack of traceability and showed inconsistent result. Therefore, in this study a procedure was developed for the quantification of total sulfur in copper at low concentration levels using inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS). A major challenge for the quantification of sulfur in copper (alloyed/unalloyed) by ICPMS is the copper matrix itself, causing matrix effects and making an extensive cleaning (cones, extraction lens) necessary after measurements. Matschat et al investigated the analysis of high-purity metals (including copper) by high resolution ICP-MS and found that the copper matrix shows strong matrix effects on the sensitivity resulting from Cu deposition on the cones. Therefore, the major part of the copper matrix has to be separated, which was accomplished by adding ammonia which forms a complex with the copper while releasing the sulfur. This was followed by a chromatographic separation using a weak cation resin. After that the sulfur fraction was further purified by chromatographic means using an anion exchange method followed by a chelating resin. The anion exchange resin (AG1X8), however, is selective to sulfate and sulfite but less-selective to sulfide. Therefore, when quantifying total sulfur in copper, the different species of sulfur need to be oxidized to sulfate prior to the sulfur-matrix separation on the AG1X8 resin in order to avoid any measurement bias. When applying the HPA oxidation with concentrated HNO3 and H2O2 a complete conversion from sulfide and sulfite to sulfate could be achieved. The recovery of all investigated sulfur species is quantitative within measurement uncertainties. The copper samples investigated in this study contain copper in the range of 0.85-0.99 kg·kg-1 and zinc from <10 to 300 g·kg-1. Approximately 0.10-0.25 g of these samples were used to perform the sulfur-copper separation. After applying the complete three stage separation procedure the mass fractions of both elements were significantly reduced to below 400 ng·g-1 for copper and below 50 ng·g-1 for zinc, respectively. The developed procedure shows high performance, especially concerning high efficiency in matrix removal (> 99.999%) while keeping the recovery of sulfur above 80%. The procedure blank was determined by IDMS as well and yielded values for the individual IDMS measurement sequences ranging from 3 ng to 53 ng. The average of these individual procedure blanks (n=22) was calculated and yielded a total procedure blank of 14 ng sulphur with standard deviation of 12 ng. The limit of detection (LOD, blank+3SD) calculated on this basis was 0.20 µg·g-1 while the limit of quantification (LOQ, blank+10SD) was 0.54 µg·g-1, when considering a sample weight of 0.25 g. The quantification of low sulfur contents (< 15 µg/g) by conventional IDMS is hindered by the very high Cu/S ratio, which clearly affects the separation in a negative way: The recovery of sulfur dropped to about 30 % for four replicates, while two further replicates even showed recoveries below 10%. To enable measurement without completely changing the separation procedure, an exact amount of sulfur was added prior to spiking, such that the sulfur mass fraction was shifted to the optimum working range of the separation procedure. Thus exact amounts of sulfur were added to enhance the mass fraction of sulfur from 15 µg·g-1 to 40 µg·g-1, then the IDMS analysis was performed as usual and finally the added sulfur amount was subtracted. The so obtained measurement result agreed well with the certified value within the uncertainties. The relative expanded measurement uncertainties for conventional IDMS are below 1%. When applying the modified IDMS procedure, where back-spike is added to the sample before spiking, the relative expanded measurement uncertainties are larger and up to 5%. With the presented sulfur-matrix procedure a working range from approximately 15 µg·g-1 to 1500 µg·g-1 can be achieved. The developed procedure for the quantification of low sulfur amounts in copper has been validated here via three different routes: first an inter-laboratory comparison at highest metrological level, second a step-by-step validation by checking each single step of the procedure and third the setup of a complete uncertainty budget. The procedure is sufficient to facilitate value assignment of total sulfur mass fraction in reference materials. Additionally, relative measurement uncertainties were calculated below 1 % and the measurement results are traceable to the SI, which is clearly demonstrated in this work. The procedure reported in this study is a new reference procedure for sulfur measurement in copper, well meeting the requirements of the two major purposes: the certification of reference materials and the assignment of reference values for inter-laboratory comparison. T2 - Winter Conference on Plasma Spectrochemistry CY - Amelia Island, FL, USA DA - 08.01.2018 KW - Isotope dilution mass spectrometry KW - Sulfur-copper-sepration KW - SI traceability KW - Measurement uncertainty KW - ICP-MS KW - Sulfur species conversion PY - 2018 AN - OPUS4-44640 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Stable isotope analysis via hydrides using molecular absorption spectrometry N2 - Small variations in the isotopic composition of some elements have been used as proof of provenance of mineral and biological samples, to describe geological processes, and to estimate a contamination source. Routinely, isotope compositions are measured by mass spectrometry; the working horse of the isotope analysis. However, mass spectrometric methods are expensive, time-consuming and they require a high qualified analyst. Here, an alternative faster and low-cost optical method for isotope ratio determination is investigated: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Stable isotope amount composition of X = Li, B, Mg, Ca and Sr have been determined by monitoring the absorption spectra of their in situ generated hydrides (XH) in graphite furnace HR-CS-MAS. For example, the system of two stable isotopes of boron (10B and 11B) was studied via its hydride for the electronic transition X1Σ+ → A1Π (Fig. 1a). The spectrum of a given sample is a linear combination of the 10BH molecule and its isotopologue 11BH. Therefore, isotopic composition of samples and reference materials are calculated by a partial least square regression (PLS). For this, a spectral library is built by using samples with known isotope composition. Results are metrologically compatible with those reported by mass spectrometric methods. [1] Similar results are obtained for n isotope systems like Mg (24Mg, 25Mg, and 26Mg), where isotope shift of their isotopologues can be resolved as shown in Fig.1 b. The extension of this methodology to other elements like Li, Ca and Sr is discussed [2]. References: [1] C. Abad, S. Florek, H. Becker-Ross, M.-D. Huang, H.-J. Heinrich, S. Recknagel, J. Vogl, N. Jakubowski, U. Panne, Determination of boron isotope ratios by high-resolution continuum source molecular absorption spectrometry using graphite furnace vaporizers, Spectrochim. Acta, Part B, 136 (2017) 116-122. [2] C. Abad et al., unpublished results, 2018. T2 - ESAS & CANAS 2018 CY - Berlin, Germany DA - 20.03.2018 KW - Isotope KW - HR-CS-MAS KW - Mono-hydride KW - Spectrometry PY - 2018 AN - OPUS4-45826 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Optical spectrometry versus mass spectrometry for stable isotope analysis of B and Mg N2 - Mass spectrometric methods (MC-ICP-MS and TIMS) are without doubt the working horse of stable isotope analysis. However, drawbacks of these methods include the high costs for instruments and their operation, experienced operators and elaborate chromatographic sample preparation which are time consuming. We propose a lower-cost and faster optical alternative for the analysis of isotope ratios of selected elements: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Stable isotope amount compositions of boron (B) and magnesium (Mg) were determined based on the absorption spectra of in-situ generated mono-hydrides and halide (MH and MX) using graphite furnace HR-CS-MAS. The use of a modular simultaneous echelle spectrograph (MOSES) helps to find the maximal isotope shift in the diatomic molecular spectra produced in a graphite furnace by using isotopic spike solutions. Isotopes of boron (10B and 11B) were studied via their hydrides for the electronic transition X 1Σ+ → A 1Π. The spectrum of a given sample is a linear combination of the 10BH molecule and its isotopologue 11BH. Therefore, the isotopic composition of samples can be calculated by a partial least square regression (PLS). For this, a spectral library was built by using samples and spikes with known isotope composition. Boron isotope ratios measured by HR-CS-MAS are identical with those measured by mass spectrometric methods at the 0.15 ‰ level. Similar results were obtained for a multiple isotope system like Mg (24Mg, 25Mg, and 26Mg), where isotope shifts of their isotopologues can be resolved in the MgF molecule for the electronic transition X 2Σ → A 2 Πi. The extension of this methodology to other elements like Li, Ca, Cu, and Sr is discussed. T2 - 13. Symposium „Massenspektrometrische Verfahren der Elementspurenanalyse“ zusammen mit dem 26. ICPMS-Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - Isotope KW - HR-CS-MAS KW - Isotopic shift KW - Spectrometry KW - Boron monohydride KW - Magnesium monofluoride KW - Molecular absorption spectrometry PY - 2018 AN - OPUS4-45868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Stable Isotope Analysis Using Molecular Absorption Spectrometry N2 - We propose an alternative faster and low-cost optical method for isotope analysis: high-resolution continuum source molecular absorption spectrometry (HR-CS-MAS). Stable isotope amount composition of X = Li, B, Mg, Ca and Sr were determined by monitoring the absorption spectra of their in situ generated mono-hydrides (XH) in graphite furnace HR-CS-MAS. Isotopes of boron (10B and 11B) were studied via their hydrides for the electronic transition X1Σ+ → A1Π (Fig. 1a). The spectrum of a given sample is a linear combination of the 10BH molecule and its isotopologue 11BH. Therefore, the isotopic composition of samples can be calculated by a partial least square regression (PLS). For this, a spectral library is built by using samples with known isotope composition. Results with an accuracy of 0.15 ‰ are metrologically compatible with those reported by mass spectrometric methods. Similar results are obtained for n isotope systems like Mg (24Mg, 25Mg, and 26Mg), where isotope shifts of their isotopologues can be resolved as shown in Fig.1b. The extension of this methodology to other elements like Li, Ca and Sr is discussed. T2 - Goldschmidt Conference 2018 CY - Boston, MA, USA DA - 12.08.2018 KW - Isotope KW - HR-CS-MAS KW - Mono-hydride KW - Spectrometry PY - 2018 AN - OPUS4-45825 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Monavari, M. A1 - Homaeigohar, S. A1 - Fuentes-Chandía, M. A1 - Nawaz, Q. A1 - Monavari, Mehran A1 - Venkatraman, A. A1 - Boccaccini, A. T1 - 3D printing of alginate dialdehyde-gelatin (ADA-GEL) hydrogels incorporating phytotherapeutic icariin loaded mesoporous SiO2-CaO nanoparticles for bone tissue engineering N2 - 3D printing enables a better control over the microstructure of bone restoring constructs, addresses the challenges seen in the preparation of patient-specific bone scaffolds, and overcomes the bottlenecks that can appear in delivering drugs/growth factors promoting bone regeneration. Here, 3D printing is employed for the fabrication of an osteogenic construct made of hydrogel nanocomposites. Alginate dialdehyde-gelatin (ADA-GEL) hydrogel is reinforced by the incorporation of bioactive glass nanoparticles, i.e. mesoporous silica-calcia nanoparticles (MSNs), in two types of drug (icariin) loading. The composites hydrogel is printed as superhydrated composite constructs in a grid structure. The MSNs not only improve the mechanical stiffness of the constructs but also induce formation of an apatite layer when the construct is immersed in simulated body fluid (SBF), thereby promoting cell adhesion and proliferation. The nanocomposite constructs can hold and deliver icariin efficiently, regardless of its incorporation mode, either as loaded into the MSNs or freely distributed within the hydrogel. Biocompatibility tests showed that the hydrogel nanocomposites assure enhanced osteoblast proliferation, adhesion, and differentiation. Such optimum biological properties stem from the superior biocompatibility of ADA-GEL, the bioactivity of the MSNs, and the supportive effect of icariin in relation to cell Proliferation and differentiation. Taken together, given the achieved structural and biological properties and effective drug delivery capability, the hydrogel nanocomposites show promising potential for bone tissue engineering. KW - 3D printed hydrogel KW - ADA-GEL KW - Drug delivery KW - Mesoporous SiO2-CaO nanoparticles KW - Bone tissue engineering PY - 2021 DO - https://doi.org/10.1016/j.msec.2021.112470 VL - 131 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-53848 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wooley, A. T. A1 - Cárdenas, S. A1 - Cavazzini, A. A1 - Panne, Ulrich T1 - Meet the three newest ABC Editors N2 - Editorial - Introduction of the new editors. KW - ABC PY - 2023 DO - https://doi.org/10.1007/s00216-023-04615-9 SP - 1 EP - 3 PB - Springer Verlag GmbH CY - Germany AN - OPUS4-57188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Przyklenk, A. T1 - Progress of the European Metrology Network for Advanced Manufacturing N2 - The European Metrology Network (EMN) for Advanced Manufacturing has been established in June 2021. Currently nine EMNs focussing on different important topics of strategic importance for Europe exist and form an integral part of EURAMET, the European Association of National Metrology Institutes (NMI). EMNs are tasked to ▪ develop a high-level coordination of the metrology community in Europe in a close dialogue with the respective stakeholders (SH) ▪ develop a strategic research agenda (SRA) within their thematic areas ▪ provide contributions to the European Partnership on Metrology research programme Based on the analysis of existing metrology infrastructures and capabilities of NMIs, the metrology research needs for advanced manufacturing are identified in close cooperation with academic, governmental and industrial stakeholders. Here, we report on the progress of the EMN for Advanced Manufacturing. T2 - Euspen 22nd International Conference & Exhibition (Euspen 2022) CY - Genf, Switzerland DA - 30.05.2022 KW - JNP AdvManuNet KW - Metrology KW - Advanced manufacturing KW - European Metrology Network KW - EMN PY - 2022 AN - OPUS4-55805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Mehta, B. A1 - Nyborg, L. A1 - Virtanen, E. A1 - Markötter, Henning A1 - Hryha, E. A1 - Bruno, Giovanni T1 - Failure Mechanisms Investigation by Means of in-situ Synchrotron Computed Tomography in Aluminum MMC-based Alloy Tailored for Additive Manufacturing (AM) N2 - The availability of high-performance Al alloys in AM is limited due to difficulties in printability, requiring both the development of synergetic material and AM process to mitigate problems such as solidification cracking during laser powder bed fusion (LPBF). The goal of this work was to investigate the failure mechanism in a LPBF 7017 Aluminium alloy + 3 wt% Zr + 0.5 wt% TiC. The processing leads to different categories of Zr-rich inclusions, precipitates and defects. T2 - Alloys for Additive Manufacturing Symposium 2022 (AAMS22) CY - Munich, Germany DA - 11.09.2022 KW - Additive manufacturing KW - Laser powder bed fusion KW - Synchrotron X-ray computed tomography KW - MMC PY - 2022 AN - OPUS4-56110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Magkos, Sotirios T1 - Iterative reconstruction from under-sampled Computed Tomography data N2 - In X-ray computed tomography (XCT), an X-ray beam of intensity I0 is transmitted through an object and its attenuated intensity I is measured when it exits the object. The attenuation of the beam depends on the attenuation coefficients along its path. The attenuation coefficients provide information about the structure and composition of the object and can be determined through mathematical operations that are referred to as reconstruction. The standard reconstruction algorithms are based on the filtered backprojection (FBP) of the measured data. While these algorithms are fast and relatively simple, they do not always succeed in computing a precise reconstruction, especially from under-sampled data. Alternatively, an image or volume can be reconstructed by solving a system of linear equations. Typically, the system of equations is too large to be solved but its solution can be approximated by iterative methods, such as the Simultaneous Iterative Reconstruction Technique (SIRT) and the Conjugate Gradient Least Squares (CGLS). This dissertation focuses on the development of a novel iterative algorithm, the Direct Iterative Reconstruction of Computed Tomography Trajectories (DIRECTT). After its reconstruction principle is explained, its performance is assessed for real parallel- and cone-beam CT (including under-sampled) data and compared to that of other established algorithms. Finally, it is demonstrated how the shape of the measured object can be modelled into DIRECTT to achieve even better reconstruction results. KW - Computed tomography KW - DIRECTT KW - Iterative algorithm KW - X-ray imaging KW - Metrics PY - 2022 SP - 1 EP - 94 PB - Universitätsbibliothek Potsdam CY - Potsdam AN - OPUS4-56465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning T1 - Synchrotron X-Ray Tomography Techniques at BAMline N2 - A recent upgrade of key equipment of the BAMline widens its imaging capabilities: shorter scan acquisition times are now possible, in situ and operando studies can now be routinely performed, and different energy spectra can easily be set up. In fact, the upgraded double-multilayer monochromator brings full flexibility by yielding different energy spectra to optimize flux and energy resolution as desired. T2 - HZB User Meeting CY - Online meeting DA - 08.12.2022 KW - BAMline KW - X-ray imaging KW - Tomography PY - 2022 AN - OPUS4-56568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Comparison of the separation performance of a conventional and a miniaturized AF4 channels N2 - Currently available separation channels for asymmetric flow field-flow fractionation (AF4), which results in long analysis time and solvent consumption, limits the application of AF4 in [1} the field of nanoparticle analysis . A miniaturized AF4 channel was introduced for the rapid analysis of different nanoparticle samples. UV-Vis-MALS provides the possibility to measure the particle size and molar mass and offers a powerful tool for the investigation of [2] separation performances of different AF4 channels . Our objective was to develop fast and reliable separation methods for both channels and enable a direct comparison by the corresponding chromatographic parameters. T2 - 2016 BfR PhD Retreat DA - 31.08.2016 KW - Nanoparticles separation asymetrical flow field flow fractionation PY - 2016 AN - OPUS4-47192 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Nanoparticles separation using capillary electrophoresis N2 - Capillary electrophoresis (CE) is an analytical technique that separates analytes based on their electrophoretic mobility with the use of an applied voltage. Nanoparticles separation using CE exhibits good separation and analysis efficiency, especially for nanoparticles smaller than 30 nm. The coupling of CE with inductively coupled plasma mass spectrometry (ICP-MS) provides the possibility to detect nanoparticles in the concentration range of nanograms per litre and enables the simultaneous detection of nanoparticles and its [1][2] ionic counter parts. Our objective is to develop a fast and reliable separation method for differently modified nanoparticles using capillary electrophoresis. T2 - 2017 BAM PhD Day DA - 18.09.2017 KW - Nanoparticles separation capillary electrophoresis asymmetrcial flow field flow fractionation PY - 2017 AN - OPUS4-47195 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - You, Zengchao A1 - Jakubowski, Norbert A1 - Panne, Ulrich A1 - Weidner, Steffen T1 - Separation of polystyrene nanoparticles with different coatings using two-dimensional off-line coupling of asymmetrical flow field flow fractionation and capillary electrophoresis N2 - The successful off-line coupling of asymmetrical flow field flow fractionation (AF4) and capillary electrophoresis (CE) for separation of nanoparticles (NPs) with different surface coatings was shown. We could successfully demonstrate that, in a certain NP size range, hyphenation of both techniques significantly improved the separation of differently coated NPs. Three mixtures of polystyrene nanoparticles (PS-NPs) with comparable core sizes but different coatings (no coating/carboxyl-coated) were studied. Separation in either method resulted in non-baseline resolved or non-separated peaks. In contrast, two-dimensional off-line coupling of AF4 and CE resulted in clearly separated regions in their 2 D plots in case of 20 and 50 nm particle mixtures, whereas the 100 nm NP mixture could not be separated at all. Various factors affecting the separation like hydrodynamic diameter or SDS concentration were discussed. KW - Capillary electrophoresis (CE) KW - Nanoparticles with same nominal diameter KW - Surface coating KW - Two-dimensional off-line coupling KW - Asymmetrical flow field flow fractionation (AF4) PY - 2019 DO - https://doi.org/10.1016/j.chroma.2019.01.056 VL - 1593 SP - 119 EP - 126 PB - Elsevier AN - OPUS4-47363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian T1 - Synchrotron based absorption edge tomography for the analysis of 3D printed polymer MOF N2 - Absorption edge tomography is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. The beamline BAM line at BESSY II, which is operated by the Federal Institute for Materials Research and Testing, can provide a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%. Together with the microtomography setup, this enables differential tomography sensitive to any element with N >= 24 (Cr) by using an appropriate K- or L-edge in this range. Here, a polymer filament embedding metal organic framework (MOF) was prepared and used for 3D printing. Absorption edge tomography at the copper K edge was employed to perform a non-destructive 3D characterization of the microstructure of the embedded MOF. Data fusion was then used to determine the size distribution of the embedded MOF. T2 - iCT 2019 CY - Padua, Italy DA - 12.02.2019 KW - Synchrotron tomography KW - BAMline KW - MOF KW - Absorption edge tomography PY - 2019 AN - OPUS4-47392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian T1 - Synchrotron based absorption edge tomography for the analysis of 3D printed polymer MOF N2 - Absorption edge tomography is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. The beamline BAM line at BESSY II, which is operated by the Federal Institute for Materials Research and Testing, can provide a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%. Together with the microtomography setup, this enables differential tomography sensitive to any element with N >= 24 (Cr) by using an appropriate K- or L-edge in this range. Here, a polymer filament embedding metal organic framework (MOF) was prepared and used for 3D printing. Absorption edge tomography at the copper K edge was employed to perform a non-destructive 3D characterization of the microstructure of the embedded MOF. Data fusion was then used to determine the size distribution of the embedded MOF. T2 - iCT 2019 CY - Padua, Italy DA - 12.02.2019 KW - Synchrotron tomography KW - BAMline KW - MOF KW - Absorption edge tomography PY - 2019 AN - OPUS4-47391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Digital Analytical Sciences N2 - Based on inductive reasoning scientific inquiry in Analytical Sciences has a long tradition. The talk addresses in which way the digital transformation will change the scientific paradigm in Analytical Sciences to a data-driven discipline. Three main areas, integration, instruments, and methods, are discussed in their transformation through machine learning and other digital tools. Finally, some shortcomings and pitfalls in the deployments of algorithmic shortcuts are illustrated. T2 - ANAKON Münster CY - Westfälischen Wilhelms-Universität (WWU), Münster, Germany DA - 25.03.2019 KW - Digital transformation KW - Analytical Sciences KW - Digital PY - 2019 AN - OPUS4-47735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Léonard, Fabien T1 - On nominal-actual comparisons for additive manufacturing applications N2 - Nominal-actual comparisons are routinely performed to compare a manufactured specimen to a reference specimen. X-ray Computed Tomography (CT) has brought a profound change in the way that tolerance verifications are performed in industry, by allowing the inner and outer geometries of an object to be measured, without the need for external access or destructive testing. As a results, CT is increasingly used in additive manufacturing applications, where a nominal-actual comparison performed between the digital model (CAD file), used as an input for the 3D printer, and the CT volume from the printed part, can provide invaluable information as to the accuracy of the printing process. However, the nominal-actual comparison process is somewhat different when applied to additively manufactured specimens by comparison to conventionally manufactured specimens. T2 - 9th Conference on Industrial Computed Tomography CY - Padova, Italy DA - 14.02.2019 KW - Computed tomography KW - X-ray computed tomography KW - Implants PY - 2019 AN - OPUS4-47832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Olaf T1 - Analysis of very volatile organic compounds (VVOC) with thermal desorption GC-MS N2 - Most VVOC were rarely considered in the evaluation of construction products. (Salthammer, 2014) In Germany this will change because the latest version of the German AgBB scheme for health evaluation (2015) now include VVOC, e.g. ethyl acetate and ethanol. In this study selected compounds were tested with the procedure described in ISO 16017 and a method for measuring VVOC with thermal desorption was developed. Three different adsorbents Tenax TA, Carbograph 5TD and Carbopack X were tested to analyse VVOC according to ISO 16017. For the tested VVOC, Carbograph 5TD showed the best results under the chosen analytical conditions. T2 - Indoor Air 2016, The 14th international conference of Indoor Air Quality and Climate CY - Gent, Belgium DA - 03.07.2016 KW - Thermal desorption KW - VVOC KW - Carbograph 5TD KW - Carbopack X PY - 2016 AN - OPUS4-37037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wilke, Olaf T1 - Reproducibly emitting reference material for quality assurance/quality control of emission test chamber measurements N2 - Volatile Organic Compounds (VOC) are ubiquitous in the indoor air, since they emit from materials used indoors. Investigations of these materials are mostly carried out in test chambers under controlled climatic conditions. Quality control of these test chamber measurements is important but there is a lack of commercially available homogenous reference materials as required for round robin tests or quality assurance of laboratories. The approach of the present study is the impregnation of a supporting material with VOC, which are reproducibly released in measurable chamber air concentrations under standardised test conditions. A polymer made of Thermoplastic Polyurethane (TPU) was chosen as carrier material. It was impregnated with the VOC trimethyl pentanediol isobutyrat (texanol). T2 - Healthy Buildings 2017 Europe CY - Lublin, Poland DA - 02.07.2017 KW - Emissions testing KW - Volatile organic compounds KW - Polymeric material KW - CO2 assisted impregnation PY - 2017 AN - OPUS4-42351 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Matthias T1 - Two new promising approaches for quality assurance measures for materials emissions testing N2 - Two new approaches towards an emission reference material for use in quality assurance measures for materials emissions testing were developed and intensively tested. The overall goal was to obtain solid materials with homogenous and reproducible (S)VOC release. Since the application in inter-laboratory comparisons is aimed at, it should furthermore be long-term stable to ensure safe shipment to the customer without sustaining compound losses. In the first approach, thermoplastic polyurethane (TPU) was impregnated with the VOC texanol under high-pressure with liquid CO2 as solvent. In the second, styrene (VOC) and the SVOC 2,6-diisopropylnaphthalene (DIPN) were spiked into vacuum grease (VG) and a mixture of paraf-fin/squalane (P/S). For the prediction of the emission rates a finite element model (FEM) was developed for the VG and P/S type materials. All requirements for reference materials were fulfilled, whereas the TPU samples need to be aged for about 10 days until repeatable and reproducible emission rates were obtained. T2 - Indoor Air 2018 CY - Philadelphia, PA, USA DA - 22.07.2018 KW - Emission reference material KW - Volatile organic compounds KW - CO2 assisted impregnation KW - FEM model PY - 2018 AN - OPUS4-45611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Matthias A1 - Horn, Wolfgang A1 - Mölders, N. A1 - Sauerwald, T. A1 - Schultealbert, C. A1 - Mull, B. T1 - Two new promising approaches for quality assurance measures for materials emissions testing N2 - Two new approaches towards an emission reference material for use in quality assurance measures for materials emissions testing were developed and intensively tested. The overall goal was to obtain solid materials with homogenous and reproducible (S)VOC release. Since the application in inter-laboratory comparisons is aimed at, it should furthermore be long-term stable to ensure safe shipment to the customer without sustaining compound losses. In the first approach, thermoplastic polyurethane (TPU) was impregnated with the VOC texanol under high-pressure with liquid CO2 as solvent. In the second, styrene (VOC) and the SVOC 2,6-diisopropylnaphthalene (DIPN) were spiked into vacuum grease (VG) and a mixture of paraf-fin/squalane (P/S). For the prediction of the emission rates a finite element model (FEM) was developed for the VG and P/S type materials. All requirements for reference materials were fulfilled, whereas the TPU samples need to be aged for about 10 days until repeatable and re-producible emission rates were obtained. T2 - Indoor Air 2018 CY - Philadelphia, PA, USA DA - 22.07.2018 KW - Emission reference material KW - Volatile organic compounds KW - CO2 assisted impregnation KW - FEM model PY - 2018 SP - 1 EP - 8 AN - OPUS4-45610 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Bannick, C.G. A1 - Szewzyk, R. A1 - Ricking, M. A1 - Schniegler, S. A1 - Obermaier, N. A1 - Barthel, A. K. A1 - Altmann, Korinna A1 - Eisentraut, Paul T1 - Development and testing of a fractionated filtration for sampling of microplastics in water N2 - A harmonization of sampling, sample preparation and detection is pivotal in order to obtain comparable data on microplastics (MP) in the environment. This paper develops and proposes a suitable sampling concept for waterbodies that considers different plastic specific properties and influencing factors in the environment. Both artificial water including defined MP fractions and the discharge of a wastewater treatment plant were used to verify the derived sampling procedure, sample preparation and the subsequent analysis of MP using thermal extraction-desorption gas chromatography - mass spectrometry (TED-GC-MS). A major finding of this paper is that an application of various particle size classes greatly improves the practical handling of the sampling equipment. Size classes also enable the TED-GC-MS to provide any data on the MP size distribution, a substantial sampling property affecting both the necessary sampling volume and the optimal sampling depth. In the artificial water with defined MP fractions, the recovery rates ranged from 80 to 110%, depending on the different MP types and MP size classes. In the treated wastewater, we found both Polyethylene and polystyrene in different size classes and quantities. KW - Microplastics KW - Sampling KW - Sampling techniques KW - Water PY - 2019 DO - https://doi.org/10.1016/j.watres.2018.10.045 SN - 0043-1354 VL - 149 SP - 650 EP - 658 PB - Elsevier AN - OPUS4-47200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Detektion von Kunststoffen mittels TED-GC-MS N2 - Vortrag zur Funktionsweise der TED-GC-MS für die Analyse von Mikroplastik in Umweltproben T2 - Arbeitsgespräch der Ressortforschungseinrichtungen CY - Berlin, Germany DA - 26.11.2018 KW - Mikroplastik KW - TED-GC-MS PY - 2018 AN - OPUS4-47184 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sturm, Heinz T1 - Notwendigkeit von (Realistischen) Referenzmaterialien N2 - Die Herstellung von Mikroplastik Referenzmaterialien wird vorgestellt. T2 - Statusfonferenz der BMBF Fördermassnahme "Plastik in der Umwelt" CY - Berlin, Germany DA - 09.04.2019 KW - Ringversuch KW - Mikroplastik KW - Referenzmaterialien PY - 2019 AN - OPUS4-47798 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - New sampling strategies for optimised microplastic analysis in surface waters N2 - The occurrence of microplastic particles (MP) in nearly each environmental compartment but especially in water is well documented in an increasing amount of publication within the last few years. However, a comprehensive understanding of MP occurrence, sources and pathways in the environment as well as effects of MP on the environment is still unclear. Many of the studies are not compatible, because they used different sampling, sample preparation and detection techniques, resulting in a very broad variation and very different dimension of archived results. Hence a useful avoiding strategy for reduction the MP entry in the environment is not possible. Furthermore, the existing methods are often very time consuming, need user knowledge and labour force, which is often not acceptable for the routine monitoring of an action or sanction. The call for harmonised methods become loud and louder and promising efforts are done in this area. However, the scientific discussion is often focus on advantages and disadvantages of detection tools and sample preparation, less initiative is given to the sampling strategy. That is a pity, because every environmental scientist knows, a good analytical result depend on a good sampling strategy. The sampling of water seems on the first view easy because the sampling process include already an up concentration of the MP by means of sieves and filters. However, this filtering of water is often limited by filter cake on the sieves, consisting of high amount of natural particular matter. Hence often a small water volume is filtered, which will not own a representative amount of trait carriers or complex sieves cascades are used, which need a high technical equipment. Recently we presented a fast thermoanalytical method for the detection of polymers fractions in water samples. This method, thermo-extraction desorption gas chromatography mass spectrometry (TED-GC-MS) can analyse MP in water filtrates without sample preparations within 2-3 hours. Advantageous is the additional analysis of rubber particles from tires beside the MP. In order to come even faster we now start to develop new sampling strategies, which should be use for different water systems. It is intended to reduce the effort in the field and to elongate times for sampling to obtain a representatives result without random effects. In the present presentation we will show first result using a sedimentation box for sampling of MP from surface water. Advantages and disadvantages will be discussed and comparison to data from conventional fractionated filtration will be given. T2 - SETAC CY - Helsinki, Finland DA - 26.05.2019 KW - Microplastics KW - Sampling KW - Sampling techniques KW - Water PY - 2019 AN - OPUS4-48118 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Krom, I. T1 - CRMs for (semi-)VOCs in sorbent tubes N2 - EN 16516 sets the test method and requirements for the determination of emissions of Volatile Organic Compounds (VOCs) from building materials into indoor air. To address the quality control requirements for the class of semi-VOCs (SVOCs), VSL developed gaseous reference materials. A novel home-made dynamic gas mixture preparation system, operating according to ISO 6145-4 (continuous injection method), has recently been developed and validated. Thanks to the stable temperature control up to 100 oC, the system can prevent condensation of the SVOCs in air at indoor air concentration levels. The in-situ obtained SVOC gas standards can be sampled in sorbent tubes to obtain SVOC transfer standards. A study was performed to determine the optimal sorbent material and storage conditions. This study will be presented together with the results of the 2018 Round Robin test for emission test chamber measurements organised by BAM. Using the novel system, VSL prepared transfer standards with known amounts of VOCs and SVOCs for participants to evaluate their analytical performance. T2 - Emissions and Odours from Materials CY - Brussels, Belgium DA - 07.10.2019 KW - CRM KW - VOC transfer standards KW - Round robin test KW - Material emissions testing PY - 2019 AN - OPUS4-49423 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ricking, M. T1 - Probennahmestrategie für die kontinuierliche Mikrokunststoff-Analyse in Oberflächengewässern N2 - Das Poster stellt erste Ergebnisse zur Mikroplastik-Probennahme mit einem Sedimentationskasten dar. T2 - Wasser 2019 CY - Erfurt, Germany DA - 24.05.2019 KW - Mikroplastik KW - Sedimentationskasten KW - Probennahme PY - 2019 AN - OPUS4-49069 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Becker, Roland A1 - Altmann, Korinna A1 - Sommerfeld, Thomas A1 - Braun, Ulrike T1 - Quantification of microplastics in a freshwater suspended organic matter using different thermoanalytical methods – outcome of an interlaboratory comparison N2 - A sedimented freshwater suspended organic matter fortified with particles of polyethylene (PE), polypropylene (PP), polystyrene (PS), and polyethylene terephthalate (PET) was employed in an interlaboratory comparison of thermoanalytical methods for microplastics identification and quantification. Three laboratories performed pyrolysis gas chromatography-mass spectrometry (Py-GC-MS), three others provided results using thermal extraction desorption followed by gas chromatography coupled to mass spectrometry (TED-GC-MS). One participant performed thermogravimetry-infrared spectroscopy (TGA-FTIR) and two participants used thermogravimetry coupled to mass spectrometry (TGA-MS). Further participants used differential scanning microscopy (DSC), a procedure based on micro combustion calorimetry (MCC) and a procedure based on elemental analysis. Each participant employed a different combination of sample treatment, calibration and instrumental Settings for polymer identification and quantification. Though there is obviously room for improvements regarding the between-laboratory reproducibility and the harmonization of procedures it was seen that the participants Performing Py-GC-MS, TED-GC-MS, and TGA-FTIR were able to correctly identify all polymers and to report reasonable quantification results in the investigated concentration range (PE: 20.0 μg/mg, PP: 5.70 μg/mg; PS: 2.20 μg/mg, PET: 18.0 μg/mg). Although for the other methods limitations exists regarding the detection of specific polymers, they showed potential as alternative approaches for polymer quantification in solid environmental matrices. KW - Interlaboratory comparison KW - Microplastics KW - Suspended organic matter KW - Pyrolysis PY - 2020 DO - https://doi.org/10.1016/j.jaap.2020.104829 VL - 148 SP - 1 EP - 6 PB - Elsevier B.V. AN - OPUS4-50977 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dittmann, Daniel A1 - Saal, L. A1 - Zietzschmann, F. A1 - Mai, M. A1 - Altmann, Korinna A1 - Al-Sabbagh, Dominik A1 - Ruhl, A. S. A1 - Jekel, M. A1 - Braun, U. T1 - Aktivkohlecharakterisierung als weiterer Schlüssel für Adsorptionsprognosen organischer Spurenstoffe in der vierten Reinigungsstufe N2 - In diesem Beitrag wird der Einfluss des Aktivkohleprodukts auf die Adsorption von Spurenstoffen aus Kläranlagenablauf gezeigt und diskutiert. Im zweiten Teil wird das Material Aktivkohle analytisch charakterisiert und die Eigenschaften systematisiert. Die gewonnenen Erkenntnisse werden mit Bezug zu Praxislösungen zusammengefasst. T2 - Wasser 2021 CY - Online meeting DA - 10.05.2021 KW - Aktivkohle KW - Thermogravimetrie KW - Zersetzungsgasanalyse KW - Proximatanalyse PY - 2021 SP - 373 EP - 378 AN - OPUS4-52740 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Braun, U. A1 - Herper, D. A1 - Knefel, M. A1 - Bednarz, M. A1 - Bannick, C.-G. T1 - Smart filters for the analysis of microplastic in beverages filled in plastic bottles N2 - The occurrence of microplastic (MP) in food products, such as beverages in plastic bottles, is of high public concern. Existing analytical methods focus on the determination of particle numbers, requiring elaborate sampling tools, laboratory infrastructure and generally time-consuming imaging detection methods. A comprehensive routine analysis of MP in food products is still not possible. In the present work, we present the development of a smart filter crucible as sampling and detection tool. After filtration and drying of the filtered-off solids, a direct determination of the MP mass content from the crucible sample can be done by thermal extraction desorption gas chromatography mass spectroscopy (TED-GC/MS). The new filter crucible allows a filtration of MP down to particle sizes of 5 µm. We determined MP contents below 0.01 µg/L up to 2 µg/L, depending on beverages bottle type. This may be directly related to the bottle type, especially the quality of the plastic material of the screw cap. Dependent on the plastic material, particle formation increases due to opening and closing operations during the use phase. However, we have also found that some individual determinations of samples were subjected to high errors due to random events. A conclusive quantitative evaluation of the products is therefore not possible at present. KW - Microplastic KW - TED-GC/MS KW - Plastic bottles KW - Bbeverages KW - Filter crucible PY - 2021 DO - https://doi.org/10.1080/19440049.2021.1889042 SN - 1944-0057 VL - 38 IS - 4 SP - 691 EP - 700 PB - Taylor & Francis AN - OPUS4-52323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt (RUSEKU) N2 - Der Vortrag wurde im Rahmen der Abschlusskonferenz des Forschungsschwerpunktes "Plastik in der Umwelt" des BMBF gehalten. Er fasst die Ergebnisse des Verbundprojektes RUSEKU zusammen. Es wurde die Herstellung verschiedener Testmaterialien für die Mikroplastik (MP) Analytik beschrieben. Im weiteren geht es um verschiedene Ansätze MP kostengünstig und schnell zu detektieren, z.B. mit Nahinfrarotspektroskopie. Nanoplastik konnte mit der Transmissionselektronenmikroskopie sichtbar gemacht werden. Für die praxisnahe Beprobung von Gewässern wurde die Fraktionierte Filtration entwickelt. Integrale Beprobungen können mit dem Sedimentationskasten erfolgen. Als Beispiele für die Beprobung realer Gewässer wurde das urbane Abwassersystem Kaiserslautern, Getränkewasser und Waschmaschinenwasser gezeigt. T2 - Abschlusskonferenz des Forschungsschwerpunktes "Plastik in der Umwelt" des BMBF CY - Online meeting DA - 20.04.2021 KW - Mikroplastik KW - TED-GC/MS KW - Probennahme KW - RUSEKU PY - 2021 AN - OPUS4-52546 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna A1 - Hodoroaba, Vasile-Dan T1 - CUSP inter-laboratory comparisons N2 - In this breakout session first, an introduction is given on the planning and organisation of an inter-laboratory comparison (ILC) under the pre-standardisation plattform VAMAS within the newly formed technical working area TWA 45 Micro and Nano Plastics in the Environment. An update with the ILCs on micro- and nanoplastic performed so far is also given. In the third part, the requirements for a reference materials are presented. The needs from the different H2020 micro- and nanoplastic projects are collected and compiled in an ILC matrix for joint activities as the next steps. T2 - The European Research Cluster to Understand the Health Impact of Micro- and Nanoplastics (CUSP) Launching Event CY - Online meeting DA - 10.06.2021 KW - Microplastic KW - Nanoplastic KW - Inter-laboratory comparison KW - VAMAS KW - Reference material PY - 2021 AN - OPUS4-52808 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Olaf A1 - Horn, Wolfgang A1 - Richter, Matthias A1 - Jann, Oliver T1 - Volatile organic compounds from building products - Results from six round robin tests with emission test chambers conducted between 2008 and 2018 N2 - Emission testing of volatile organic compounds (VOC) from materials and products is commonly based on emission test chamber measurements. To ensure the comparability of results from different testing laboratories, their measurement performance must be verified. For this purpose, Bundesanstalt für Materialforschung und -prüfung (BAM) organizes an international proficiency test (round robin test, RRT) every two years using well-characterized test materials (one sealant, one furniture board, and four times a lacquer) with defined VOC emissions. The materials fulfilled the requirements of homogeneity, reproducibility, and stability. Altogether, 36 VOCs were included of which 33 gave test chamber air concentrations between 13 and 83 µg/m3. This is the typical concentration range to be expected and to be quantified when performing chamber tests. Three compounds had higher concentrations between 326 and 1105 µg/m3. In this paper, the relative standard deviations (RSD) of BAM round robin tests since 2008 are compared and the improvement of the comparability of the emission chamber testing is shown by the decrease of the mean RSD down to 28 % in 2018. In contrast, the first large European interlaboratory comparison in 1999 showed a mean RSD of 51 %. KW - Construction product KW - Emission test chamber KW - Interlaboratory comparison KW - Proficiency testing KW - Rround robin test KW - VOC emission PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526139 DO - https://doi.org/10.1111/ina.12848 VL - 31 IS - 6 SP - 2049 EP - 2057 PB - Wiley AN - OPUS4-52613 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - BAM activities on microplastics N2 - The presentation is about BAM's activities on the topic of microplastics. It describes what BAM has done in this field in recent years. On the one hand, TED-GC/MS is presented as an analytical method, on the other hand, currently available microplastic reference materials are presented. T2 - JRC/BAM Workshop on ILC CY - Online meeting DA - 11.02.2021 KW - Microplastic KW - TED-GC/MS KW - Microplastic particles KW - Reference materials PY - 2021 AN - OPUS4-52120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dudziak, Mateusz A1 - Topolniak, Ievgeniia A1 - Silbernagl, Dorothee A1 - Altmann, Korinna A1 - Sturm, Heinz T1 - Long-time behavior of surface properties of microstructures fabricated by multiphoton lithography N2 - The multiphoton lithography (MPL) technique represents the future of 3D microprinting, enabling the production of complex microscale objects with high precision. Although the MPL fabrication parameters are widely evaluated and discussed, not much attention has been given to the microscopic properties of 3D objects with respect to their surface properties and time-dependent stability. These properties are of crucial importance when it comes to the safe and durable use of these structures in biomedical applications. In this work, we investigate the surface properties of the MPL-produced SZ2080 polymeric microstructures with regard to the physical aging processes during the post-production stage. The influence of aging on the polymeric microstructures was investigated by means of Atomic Force Microscopy (AFM) and X-ray Photoelectron Spectroscopy (XPS). As a result, a time-dependent change in Young’s Modulus, plastic deformation, and adhesion and their correlation to the development in chemical composition of the surface of MPL-microstructures are evaluated. The results presented here are valuable for the application of MPL-fabricated 3D objects in general, but especially in medical technology as they give detailed information of the physical and chemical time-dependent dynamic behavior of MPL-printed surfaces and thus their suitability and performance in biological systems. KW - Multiphoton lithography KW - Additive manufacturing KW - Microfabrication KW - SZ2080 negative photo-resist KW - Young´s modulus KW - Aging KW - Surface properties KW - X-ray photoelectron spectroscopy KW - Atomic force microscopy KW - Force-distance-curve PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542166 DO - https://doi.org/10.3390/nano11123285 SN - 2079-4991 VL - 11 IS - 12 SP - 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-54216 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Eisentraut, Paul T1 - Fast quantitative detection of microplastics using TED-GC/MS, an innovative thermoanalytical method N2 - Im Vortrag wird die BAM vorgestellt und die Motivation für Engagement im Feld der Mikroplastikanalysen dargelegt. Die Herausforderungen bei der Analyse werden aufgezeigt und der Umgang mit ihnen. Das Arbeitsprinzip der TED-GC/MS sowie Leistungsparameter werden erläutert sowie das Vorgehen zur Identifikation und Quantifizierung von Polymeren in er Umwelt. An ausgewählten Beispielen werden interessante Ergebnisse präsentiert und die Mikroplastikreferenzmaterialien der BAM vorgestellt. N2 - In the talk, the BAM is introduced and the motivation for our engagement in the field of microplastic analysis is explained. The challenges in the analysis of microplastics are shown and how we deal with them. The working principle of TED-GC/MS and its performance parameters are presented, as well as the procedure for identifying and quantifying polymers in environmental samples. Interesting results are shown using selected examples. Finally, BAM's microplastic reference materials are highlighted. T2 - National Environmental Monitoring Conference CY - Online meeting DA - 02.08.2021 KW - Microplastic KW - TED-GC/MS KW - Environmental analysis PY - 2021 AN - OPUS4-53081 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna A1 - Braun, U. T1 - Monitoring von Mikroplastik N2 - Der Vortrag gibt einen Überblick was bei der Analyse von Mikroplastik zu beachten ist und beschreibt die Vor- und Nachteile der TED-GC/MS. T2 - Abschlusstreffen MikroPlaTas CY - Online meeting DA - 23.06.2021 KW - Mikroplastik KW - TED-GC/MS KW - Mikroplastik-Analytik PY - 2021 AN - OPUS4-52916 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gollwitzer, Christian T1 - 3D printing material filled with metal organic frameworks analyzed by synchrotron based absorption edge tomography N2 - Absorption edge tomography, also known as differential tomography at absorption edges, is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. Synchrotron radiation is the best source for absorption edge tomography, because of its small bandwidth, high intensity and easily adjustable photon energy. The synchrotron beamline BAMline at the synchrotron radiation facility BESSY II in Berlin, which is operated by the Bundesanstalt für Materialforschung und -prüfung (BAM), provides a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%, when the double multilayer monochromator is used. Together with the microtomography setup, this enables differential tomography with submicron resolution at the K edge of the elements from chromium up to the lanthanides, and up to uranium, when the L edges are used as well. In this work, metal organic frameworks (MOFs) embedded in polymer are characterized using differential tomography. MOFs are microporous structures of metal ions, coordinated by organic linker molecules, that can be used in a broad field of applications, especially in gas storage and catalysis. In this work, polymer embedded MOFs were extruded into filaments, which could be used for 3d-printing to profit from the specific properties of the MOFs in polymeric materials combined with the arbitrary shapes provided by 3d-printing. For the extrusion, different polymer classes like ABS, polyester- and polyetherurethanes, as well as different MOFs (ZIF-8, ZIF-67, HKUST-1) were used to create MOF containing filaments with a nominal diameter of 3.0 mm. Differential tomography at the edges of the Zn, Co, and Cu was then used to find the distribution of the corresponding MOF in the filament and to analyze the shape of the inclusions. T2 - MSE 2018 CY - Darmstadt, Germany DA - 26.09.2018 KW - Absorption edge KW - Tomography KW - Metal organic framework KW - Synchrotron PY - 2018 AN - OPUS4-46429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Procedures to Quantitatively Characterize Morphological Features of Triply Periodic Minimal Surface Structures N2 - Additively manufactured (AM) metallic sheet-based Triply Periodic Minimal Surface Structures (TPMSS) meet several requirements in both bio-medical and engineering fields: Tunable mechanical properties, low sensitivity to manufacturing defects, mechanical stability, and high energy absorption. However, they also present some challenges related to quality control. In fact, the optimization of both the AM process and the properties of TPMSS is impossible without considering structural characteristics as manufacturing accuracy, internal defects, and as well as surface topography and roughness. In this study, the quantitative non-destructive analysis of TPMSS manufactured from Ti-6Al-4V alloy by electron beam melting was performed by means of laboratory X-ray computed tomography (XCT). T2 - International conference on tomography of material and structures 2022 CY - Grenoble, France DA - 27.06.2022 KW - Additive manufacturing KW - Scaffold KW - Lightweight structures KW - Computed tomography PY - 2022 AN - OPUS4-55229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Gojani, Ardian A1 - Völker, Tobias A1 - Günther, Tobias A1 - Gornushkin, Igor B. A1 - Wilsch, Gerd A1 - Günster, Jens T1 - Investigation of grain sizes in cement-based materials and their influence on laser-induced plasmas by shadowgraphy and plasma imaging N2 - The effect of particle grain sizes in different cement-based mixtures on the laser-induced plasma evolution is studied using two experimental methods: (i) temporal and spatial evolution of the laser-induced shock wave is investigated using shadowgraphy and two-dimensional plasma imaging, and (ii) temporal and spatial distribution of elements in the plasma is investigated using two-dimensional spectral imaging. This study is motivated by the interest in applying laser-induced breakdown spectroscopy (LIBS) for chemical analysis of concrete, and subsequently obtain information related to damage assessment of structures like bridges and parking decks. The distribution of grain sizes is of major interest in civil engineering as for making concrete different aggregate grain sizes defined by a sieving curve (64mm to 0.125 mm) are needed. Aggregates up to a size of 180 μm can be excluded from the data set, therefore only the amount of small aggregates with a grain size below 180 μm must be considered with LIBS. All components of the concrete with a grain size smaller than 0.125mm are related to the flour grain content. Tested samples consisted of dry and hardened cement paste (water-cement ratio w/z=0.5), which served as a reference. Aggregate mixtures were made by adding flour grains (size 40 μm) and silica fume (size 0.1 μm) in different ratios to cement: 10%, 30%, 50% and 60%, all combined to the remaining percentage of dry or hydrated cement. The visualization results show that a dependance in the evolution of the plasma as a function of sample grain size can be detected only in the initial stages of the plasma formation, that is, at the initial 3 μs of the plasma life. Spectral information reveals the elemental distribution of the silicon and calcium in plasma, in both neutral and ionized form. Here also, a significant effect is observed in the first 1 μs of the plasma lifetime. KW - LIBS KW - Cement-based materials KW - Particle size KW - Shadowgraphy KW - Plasma imaging PY - 2020 DO - https://doi.org/10.1016/j.sab.2020.105772 VL - 165 SP - 105772 PB - Elsevier B.V. AN - OPUS4-50319 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Fioresi, R. A1 - Faglioni, F. A1 - Bruno, Giovanni T1 - A novel iterative algorithm to improve segmentations with deep convolutional neural networks trained with synthetic X-ray computed tomography data (i.S.Sy.Da.T.A) N2 - We propose a novel iterative segmentation algorithm (i.S.Sy.Da.T.A: Iterative Segmentation Synthetic Data Training Algorithm) employing Deep Convolutional Neural Networks and synthetic training data for X-ray tomographic reconstructions of complex microstructures. In our method, we reinforce the synthetic training data with experimental XCT datasets that were automatically segmented in the previous iteration. This strategy produces better segmentations in successive iterations. We test our algorithm with experimental XCT re constructions of a 6-phase Al-Si Matrix Composite reinforced with ceramic fibers and particles. We perform the analysis in 3D with a special network architecture that demonstrates good generalization with synthetic training data. We show that our iterative algorithm returns better segmentations compared to the standard single training approach. More specifically, phases possessing similar attenuation coefficients can be better segmented: for Al2O3 fibers, SiC particles, and Intermetallics, we see an increase of the Dice score with respect to the classic approach: from 0.49 to 0.54, from 0.66 to 0.72, and from 0.55 to 0.66 respectively. Furthermore, the overall Dice score increases from 0.77 to 0.79. The methods presented in this work are also applicable to other materials and imaging techniques. KW - Metal matrix composites (MMC) KW - Multi-phase materials KW - 3D imaging KW - Dice score KW - Automatic segmentation KW - Deep convolutional neural network (DCNN) KW - Modified U-net architectures PY - 2023 DO - https://doi.org/10.1016/j.commatsci.2023.112112 SN - 0927-0256 VL - 223 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-57482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Greco, A. A1 - Starostin, V. A1 - Karapanagiotis, Christos A1 - Hinderhofer, A. A1 - Gerlach, A. A1 - Pithan, L. A1 - Liehr, Sascha A1 - Schreiber, Frank A1 - Kowarik, Stefan T1 - Fast fitting of reflectivity data of growing thin films using neural networks N2 - X-ray reflectivity (XRR) is a powerful and popular scattering technique that can give valuable insight into the growth behavior of thin films. This study Shows how a simple artificial neural network model can be used to determine the thickness, roughness and density of thin films of different organic semiconductors [diindenoperylene, copper(II) phthalocyanine and alpha-sexithiophene] on silica from their XRR data with millisecond computation time and with minimal user input or a priori knowledge. For a large experimental data set of 372 XRR curves, it is shown that a simple fully connected model can provide good results with a mean absolute percentage error of 8–18% when compared with the results obtained by a genetic least mean squares fit using the classical Parratt formalism. Furthermore, current drawbacks and prospects for improvement are discussed. KW - Artificial neural networks KW - X-ray reflectivity PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498997 DO - https://doi.org/10.1107/S1600576719013311 SN - 1600-5767 VL - 52 SP - 1342 EP - 1347 PB - Wiley AN - OPUS4-49899 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keshmiri, Hamid A1 - Armin, F. A1 - Elsayad, K. A1 - Schreiber, Frank A1 - Moreno, M. T1 - Leaky and waveguide modes in biperiodic holograms N2 - This study details a theoretical analysis of leaky and waveguide modes in biperiodic all-dielectric holograms. By tuning diffraction orders and subsequently confining local density of optical states at two distinct resonance wavelengths, we present a new class of highly sensitive refractive index biosensing platforms that are capable of resolving 35.5 to 41.3 nm/RIU of spectral shift for two separate biological analytes. KW - Antimicrobial resistance KW - Bacteria KW - Photonics KW - Diffractive gratings PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527632 DO - https://doi.org/10.1038/s41598-021-89971-1 SN - 2045-2322 (online) VL - 11 IS - 1 SP - 10991 PB - Springer Nature AN - OPUS4-52763 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Valentin, Jules D. P. A1 - Altenried, Stefanie A1 - Varadarajan, Adithi R. A1 - Ahrens, Christian H. A1 - Schreiber, Frank A1 - Webb, Jeremy S. A1 - van der Mei, Henny C. A1 - Ren, Qun T1 - Identification of Potential Antimicrobial Targets of Pseudomonas aeruginosa Biofilms through a Novel Screening Approach N2 - Pseudomonas aeruginosa is an opportunistic pathogen of considerable medical importance, owing to its pronounced antibiotic tolerance and association with cystic fibrosis and other life-threatening diseases. The aim of this study was to highlight the genes responsible for P. aeruginosa biofilm tolerance to antibiotics and thereby identify potential new targets for the development of drugs against biofilm-related infections. By developing a novel screening approach and utilizing a public P. aeruginosa transposon insertion library, several biofilm-relevant genes were identified. The Pf phage gene (PA0720) and flagellin gene (fliC) conferred biofilm-specific tolerance to gentamicin. Compared with the reference biofilms, the biofilms formed by PA0720 and fliC mutants were completely eliminated with a 4-fold-lower gentamicin concentration. Furthermore, the mreC, pprB, coxC, and PA3785 genes were demonstrated to play major roles in enhancing biofilm tolerance to gentamicin. The analysis of biofilm-relevant genes performed in this study provides important novel insights into the understanding of P. aeruginosa antibiotic tolerance, which will facilitate the detection of antibiotic resistance and the development of antibiofilm strategies against P. aeruginosa. KW - Antimicrobial resistance KW - Bacteria KW - Biofilms KW - Pseudomonas aeruginosa PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570205 DO - https://doi.org/10.1128/spectrum.03099-22 SP - 1 EP - 5 PB - ASM Journals AN - OPUS4-57020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Völker, Christoph A1 - Kruschwitz, Sabine A1 - Ebell, Gino T1 - Datengesteuerte Multisensor-Fusion zur Korrosionsprüfung von Stahlbetonbauteilen N2 - Potentialfeldmessung (PM) ist die beliebteste Methode der Zerstörungsfreien Prüfung (ZfP) zur Lokalisierung von aktiver Betonstahlkorrosion. PM wird durch Parameter wie z. B. Feuchtigkeits- und Chloridgradienten im Bauteil beeinflusst, so dass die Sensitivität gegenüber der räumlich sehr begrenzten, aber gefährlichen Lochkorrosion gering ist. Wir zeigen in dieser Studie, wie zusätzliche Messinformationen mit Multisensor-Datenfusion genutzt werden können, um die Detektionsleistung zu verbessern und die Auswertung zu automatisieren. Die Fusion basiert auf überwachtem maschinellen Lernen (ÜML). ÜML sind Methoden, die Zusammenhänge in (Sensor-) Daten anhand vorgegebener Kennzeichnungen (Label) erkennen. Wir verwenden ÜML um „defekt“ und „intakt“ gelabelte Bereiche in einem Multisensordatensatz zu unterscheiden. Unser Datensatz besteht aus 18 Messkampagnen und enthält jeweils PM-, Bodenradar-, Mikrowellen-Feuchte- und Wenner-Widerstandsdaten. Exakte Label für veränderliche Umweltbedingungen wurden in einer Versuchsanordnung bestimmt, bei der eine Stahlbetonplatte im Labor kontrolliert und beschleunigt verwittert. Der Verwitterungsfortschritt wurde kontinuierlich überwacht und die Korrosion gezielt erzeugt. Die Detektionsergebnisse werden quantifiziert und statistisch ausgewertet. Die Datenfusion zeigt gegenüber dem besten Einzelverfahren (PM) eine deutliche Verbesserung. Wir beschreiben die Herausforderungen datengesteuerter Ansätze in der zerstörungsfreien Prüfung und zeigen mögliche Lösungsansätze. T2 - DGZfP Jahrestagung 2018 CY - Leipzig, Germany DA - 07.05.2018 KW - Maschinelles Lernen KW - Datenfusion KW - ZfP KW - Beton KW - Korrosion PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444852 UR - http://www.ndt.net/?id=23106 SN - 1435-4934 VL - 23 IS - 9 SP - 1 EP - 9 PB - NDT.net CY - Kirchwald AN - OPUS4-44485 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Anker, A. S. A1 - Annadurai, V. A1 - Balazs, D. M. A1 - Bienert, Ralf A1 - Bouwman, W. G. A1 - Breßler, Ingo A1 - Breternitz, J. A1 - Brok, E. S. A1 - Bryant, G. A1 - Clulow, A. J. A1 - Crater, E. R. A1 - De Geuser, F. A1 - Del Giudice, A. A1 - Deumer, J. A1 - Disch, S. A1 - Dutt, S. A1 - Frank, K. A1 - Fratini, E. A1 - Garcia, P. R. A. F. A1 - Gilbert, E. P. A1 - Hahn, Marc Benjamin A1 - Hallett, J. A1 - Hohenschutz, M. A1 - Hollamby, M. A1 - Huband, S. A1 - Ilavsky, J. A1 - Jochum, J. K. A1 - Juelsholt, M. A1 - Mansel, B. W. A1 - Penttilä, P. A1 - Pittkowski, R. K. A1 - Portale, G. A1 - Pozzo, L. D. A1 - Rochels, L. A1 - Rosalie, Julian A1 - Saloga, Patrick E. J. A1 - Seibt, S. A1 - Smith, A. J. A1 - Smith, G. N. A1 - Spiering, G. A. A1 - Stawski, Tomasz M. A1 - Taché, O. A1 - Thünemann, Andreas A1 - Toth, K. A1 - Whitten, A. E. A1 - Wuttke, J. T1 - The human factor - Results of a small-angle scattering data analysis round robin N2 - A round-robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions and two from powders. Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5% and half of the population width entries within 40%. Due to the added complexity of the structure factor, far fewer people submitted answers on the powder datasets. For those that did, half of the entries for the means and widths were within 44 and 86%, respectively. This round-robin experiment highlights several causes for the discrepancies, for which solutions are proposed. KW - Round Robin KW - Data analysis KW - Small-angle scattering KW - Nanomaterials KW - Interlaboratory comparability KW - Nanostructure quantification KW - Methodology KW - MOUSE PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587091 DO - https://doi.org/10.1107/S1600576723008324 SN - 1600-5767 VL - 56 IS - 6 SP - 1618 EP - 1629 PB - Wiley-Blackwell CY - Oxford AN - OPUS4-58709 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Moeez, A. A1 - Hörmann, Anja A1 - Breßler, Ingo T1 - Example configurations and test cases for the Python HDF5Translator framework. N2 - This is a set of use examples for the HDF5Translator framework. This framework lets you translate measurement files into a different (e.g. NeXus-compatible) structure, with some optional checks and conversions on the way. For an in-depth look at what it does, there is a blog post here. The use examples provided herein are each accompanied by the measurement data necessary to test and replicate the conversion. The README.md files in each example show the steps necessary to do the conversion for each. We encourage those who have used or adapted one or more of these exampes to create their own conversion, to get in touch with us so we may add your example to the set. KW - Measurement data conversion KW - Data conversion KW - HDF5 KW - NeXus KW - NXsas KW - Framework KW - Python PY - 2024 DO - https://doi.org/10.5281/zenodo.10925971 PB - Zenodo CY - Geneva AN - OPUS4-59796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, L. M. A1 - Müller, J. T. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Schmidt, J. A1 - Bekheet, M. F. A1 - Gurlo, A. A1 - Simon, U. T1 - Hierarchically porous and mechanically stable monoliths from ordered mesoporous silica and their water filtration potential N2 - Mechanically stable structures with interconnected hierarchical porosity combine the benefits of both small and large pores, such as high surface area, pore volume, and good mass transport capabilities. Hence, lightweight micro-/meso-/macroporous monoliths are prepared from ordered mesoporous silica COK-12 by means of spark plasma sintering (SPS, S-sintering) and compared to conventionally (C-) sintered monoliths. A multi-scale model is developed to fit the small angle X-ray scattering data and obtain information on the hexagonal lattice parameters, pore sizes from the macro to the micro range, as well as the dimensions of the silica population. For both sintering techniques, the overall mesoporosity, hexagonal pore ordering, and amorphous character are preserved. The monoliths' porosity (77–49%), mesopore size (6.2–5.2 nm), pore volume (0.50–0.22 g cm-3 ), and specific surface area (451–180 m2 g-1) decrease with increasing processing temperature and pressure. While the difference in porosity is enhanced, the structural parameters between the C-and S-sintered monoliths are largely converging at 900 C, except for the mesopore size and lattice parameter, whose dimensions are more extensively preserved in the S-sintered monoliths, however, coming along with larger deviations from the theoretical lattice. Their higher mechanical properties (biaxial strength up to 49 MPa, 724 MPa HV 9.807 N) at comparable porosities and ability to withstand ultrasonic treatment and dead-end filtration up to 7 bar allow S-sintered monoliths to reach a high permeance (2634 L m-2 h-1 bar-1), permeability (1.25 x 10^-14 m2), and ability to reduce the chemical oxygen demand by 90% during filtration of a surfactant-stabilized oil in water emulsion, while indicating reasonable resistance towards fouling. KW - SAXS KW - Hierarchically porous KW - Silica KW - Water filtration PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-555928 DO - https://doi.org/10.1039/D2NA00368F SN - 2516-0230 SP - 1 EP - 17 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-55592 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Falqueto, J. B. A1 - Clark, A. H. A1 - Štefančič, A. A1 - Smales, Glen Jacob A1 - Vaz, C. A. F. A1 - Schuler, A. J. A1 - Bocchi, N. A1 - Kazzi, M. E. T1 - High performance doped Li-rich Li1+xMn2–xO4 cathodes nanoparticles synthesized by facile, fast, and efficient microwave-assisted hydrothermal route N2 - Li-rich nanoparticles of Li1+xMn2–xO4 doped with Al, Co, or Ni are successfully synthesized using a facile, fast, and efficient microwave-assisted hydrothermal route. Synchrotron X-ray diffraction confirms the formation of the crystalline cubic spinel phase type. X-ray absorption spectroscopy analysis at the Co and Ni K- and L-edges verifies that the dopants are within the Li1+xMn2–xO4 spinel structure and are inactive during cycling in the bulk and at the surface. Moreover, we demonstrate that nanocrystallinity and cationic doping play an important role in improving the electrochemical performance with respect to LiMn2O4 microparticles. They significantly reduce the charge-transfer resistance, lower the first cycle irreversible capacity loss to 6%, and achieve a capacity retention between 85 and 90% after 380 cycles, with excellent Coulombic efficiency close to 99% without compromising the specific charge at a 5C cycling rate. Furthermore, the Mn K- and L-edges attest that after long cycling, the Mn oxidation state in the bulk differs from that at the surface caused by the Mn disproportion reaction; however, the cationic doping helps mitigate the Mn dissolution with respect to the undoped Li1+xMn2–xO4 nanoparticles, as indicated by inductively coupled plasma atomic emission spectrometry. KW - XAS KW - SAXS KW - Li-ion battery KW - Cathode material KW - Spinel KW - The MOUSE PY - 2022 DO - https://doi.org/10.1021/acsaem.2c00902 SN - 2574-0962 VL - 5 IS - 7 SP - 8357 EP - 8370 PB - ACS Publ. CY - Washington, DC AN - OPUS4-55359 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sprachmann, J. A1 - Grabicki, N. A1 - Möckel, Anna A1 - Maltitz, J. A1 - del Refugio Monroy Gómez, J. A1 - Smales, Glen Jacob A1 - Dumele, O. T1 - Substituted Benzophenone Imines for COF Synthesis via Formal Transimination N2 - Covalent organic frameworks (COFs) are a prominent class of organic materials constructed from versatile building blocks via reversible reactions. The quality of imine-linked COFs can be improved by using amine monomers protected with benzophenone forming benzophenone imines. Here, we present a study on substituted benzophenones in COF synthesis via formal transimination. 12 para-substituted N-aryl benzophenone imines, with a range of electron-rich to electron-poor substituents, were prepared and their hydrolysis kinetics were studied spectroscopically. All substituted benzophenone imines can be employed in COF synthesis and lead to COFs with high crystallinity and high porosity. The substituents act innocent to COF formation as the substituted benzophenones are cleaved off. Imines can be tailored to their synthetic demands and utilized in COF formation. This concept can make access to previously unattainable, synthetically complex COF monomers feasible. KW - Materials Chemistry KW - Metals and Alloys KW - Surfaces, Coatings and Films KW - General Chemistry KW - Ceramics and Composites KW - Electronic, Optical and Magnetic Materials KW - Catalysis PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586449 DO - https://doi.org/10.1039/D3CC03735E SN - 1359-7345 SP - 1 EP - 4 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Digital Everything: X-ray Scattering and Synthesis Laboratories N2 - In our (dramatically understaffed) X-ray scattering laboratory, developing a systematic, holistic methodology let us provide scattering and diffraction information for more than 2100 samples for 200+ projects led by 120+ collaborators. Combined with automated data correction pipelines, and our analysis and simulation software, this led to more than 40 papers in the last 5 years with just over 2 full-time staff members. This year, our new, modular synthesis platform has made more than 1000 additional samples for us to analyse and catalogue. By virtue of the automation, the synthesis of these samples is automatically documented in excruciating detail, preparing them for upload and exploitation in large-scale materials databases. This talk is intended to spark ideas and invite collaborations by providing an overview of: 1) the current improvements in our wide-range X-ray scattering laboratory methodology, and 2) introducing our open, modular robotic platform for systematic sample preparation. T2 - Seminar at KIT CY - Karlsruhe, Germany DA - 17.08.2023 KW - Lab automation KW - Data stewardship KW - Scattering KW - X-ray scattering KW - Automated synthesis KW - Data pipelines PY - 2023 AN - OPUS4-58234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Glimpses of the future: a “full stack”, highly automated materials research laboratory N2 - In our (dramatically understaffed) X-ray scattering laboratory, developing a systematic, holistic methodology let us provide scattering and diffraction information for more than 2100 samples for 200+ projects led by 120+ collaborators. Combined with automated data correction pipelines, and our analysis and simulation software, this led to more than 40 papers in the last 5 years with just over 2 full-time staff members. This year, our new, modular synthesis platform has made more than 1000 additional samples for us to analyse and catalogue. By virtue of the automation, the synthesis of these samples is automatically documented in excruciating detail, preparing them for upload and exploitation in large-scale materials databases. Having developed these proof-of-concepts, we find that materials research itself is changed dramatically by automating dull tasks in a laboratory. This talk is intended to spark ideas and collaborations by providing an overview of: 1) the current improvements in our scattering laboratory methodology, 2) introducing our open, modular robotic platform that is used for systematic sample preparation, and 3) demonstrating the data structure of the synthesis logs and measurements. Finally, the remaining bottlenecks and points of attention across all three are highlighted. T2 - FAIRmat seminar CY - Berlin, Germany DA - 28.09.2023 KW - Data stewartship KW - Metadata collection KW - Laboratory methodology KW - MOUSE KW - Robotics KW - Lab automation KW - Holistic science PY - 2023 UR - https://www.fairmat-nfdi.eu/events/brian-pauw AN - OPUS4-58464 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Glimpses of the Future : Advancing X-ray Scattering in an Automated Materials Research Laboratory N2 - In our (dramatically understaffed) X-ray scattering laboratory, developing a systematic, holistic methodology1 let us provide scattering and diffraction information for more than 2100 samples for 200+ projects led by 120+ collaborators. Combined with automated data correction pipelines, and our analysis and simulation software, this led to more than 40 papers2 in the last 5 years with just over 2 full-time staff members. This year, our new, modular synthesis platform has made more than 1000 additional samples for us to analyse and catalogue. By virtue of the automation, the synthesis of these samples is automatically documented in excruciating detail, preparing them for upload and exploitation in large-scale materials databases. Having developed these proof-of-concepts, we find that materials research itself is changed dramatically by automating dull tasks in a laboratory. This talk is intended to spark ideas and invite collaborations by providing an overview of: 1) the current improvements in our wide-range X-ray scattering laboratory methodology, 2) Introduce some of our open-source analysis and simulation software, touching on scattering, diffraction and PDF, and 3) introducing our open, modular robotic platform for systematic sample preparation. Finally, the remaining bottlenecks and points of attention across all three are highlighted. T2 - Swiss Society for Crystallography (SSCr) annual meeting CY - Zurich, Switzerland DA - 08.09.2023 KW - Lab automation KW - Fourier transforms KW - X-ray scattering KW - Robotic synthesis KW - Data stewardship KW - Holistic experimental procedures KW - MOUSE KW - Metal-organic frameworks KW - High-throughput measurements PY - 2023 AN - OPUS4-58237 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Glimpses of the Future : Oh my god it’s full of metadata! N2 - In this talk, the importance of metadata is underscored by real-world examples. Metadata is essential to alleviating the reproducibility crises in science. This imples that a wide range of metadata must be collected, with a heavy emphasis on the automated collection of such metadata. This must subsequently be organized in an intelligible, archival structure, when possible with units and uncertainties. Such metadata can aid in improving the usage efficiency of instrumentation, as is demonstrated on the MOUSE instrument. This metadata can now be used to connect the various aspects of the holistic experimental procedure to gain better insights on the materials structure. A second example shows the extraction and organization of such metadata from an automated materials development platform, collected during the synthesis of 1200 samples. These metadata from the synthesis can then be linked to the results from the analysis of these samples, to find direct correlations between the synthesis parameters and the final structure of the materials. T2 - Helmholtz Incubator Summer Academy - Next Level Data Science CY - Online meeting DA - 18.09.2023 KW - Metadata KW - Lab automation KW - Data provenance KW - High-throughput KW - Correlative analysis KW - MOUSE KW - X-ray scattering KW - Robotics PY - 2023 AN - OPUS4-58463 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - A holistic experiment chain for scattering-powered materials science investigations N2 - In our (dramatically understaffed) X-ray scattering laboratory, developing a systematic, holistic methodology1 let us provide scattering and diffraction information for more than 2100 samples for 200+ projects led by 120+ collaborators over the last five years. Combined with universal, automat-ed data correction pipelines, as well as our analysis and simulation software, this led to more than 40 papers2 in the last 5 years with just over 2 full-time staff members. While this approach greatly improved the consistency of the results, the consistency of the samples and sample series provided by the users was less reliable nor necessarily reproducible. To address this issue, we built an EPICS-controlled, modular synthesis platform to add to our laboratory. To date, this has prepared over 1200 additional (Metal-Organic Framework) samples for us to meas-ure, analyse and catalogue. By virtue of the automation, the synthesis of these samples is automat-ically documented in excruciating detail, preparing them for upload and exploitation in large-scale materials databases alongside the morphological results obtained from the automated X-ray scat-tering analysis. Having developed these proof-of-concepts, we find that the consistency of results are greatly im-proved by virtue of their reproducibility, hopefully adding to the reliability of the scientific findings as well. Additionally, the nature of the experiments has changed greatly, with much more emphasis on preparation and careful planning. This talk will discuss the advantages and disadvantages of this highly integrated approach and will touch upon upcoming developments. T2 - canSAS-XIII CY - Grenoble, France DA - 16.10.2023 KW - Methodology KW - Lab automation KW - X-ray scattering KW - Automated synthesis KW - Data stewardship KW - Holistic experimental procedures KW - Scicat PY - 2023 AN - OPUS4-58643 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - Holistic Experimentation in the HExX-Lab N2 - Through bottom-up, comprehensive digitalisation of all aspects of an experiment, the HEX-lab improves the trustworthiness (traceability, reproducibility, quality) of scientific findings. The five main parts that make up a materials science experiment, i.e. Sample preparation, Measurements, Processing, Analysis, and Interpretation, each have been addressed in thorough and unique ways in this lab, building up a foundation for a wide range of materials science collaborations. Improvements span the spectrum. Hardware developments include new sample environments and stages, such as grazing incidence motion towers, electrochemistry cells and flow-through holders, electronic components such as safety interlocks and multipurpose I/O controllers, and liquid handling systems such as coolant flow cross-over systems. Software developments include: 1) a new comprehensive control system operating on both the RoWaN as well as the MOUSE allowing for full Python control and sequencing of all experimentation, 2) Automated scripts for instrument optimization, sample alignments and measurements, 3) revamped data pipelines and analysis software, standalone or launched as part of operations sequencing dashboards on servers, and 4) meticulously structured archival datafiles, fully documenting sample preparation, measurements, processing and analyses. These allow for holistic databases and dashboards to be constructed to investigate the links between synthesis parameters and resulting morphology. This poster will highlight some of the tools and techniques developed and available in the HEX-lab over the years, from sample environments to overarching experiment and data organisation structures. T2 - Materials Science Core Facility Synergy Forum 2025 CY - Bremen, Germany DA - 26.02.2025 KW - Digitalization KW - Holistic experiments KW - Traceability KW - Data provenance PY - 2025 AN - OPUS4-62675 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hallier, Dorothea C. A1 - Smales, Glen Jacob A1 - Seitz, H. A1 - Hahn, Marc Benjamin T1 - Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine N2 - Small-angle X-ray scattering (SAXS) can be used for structural determination of biological macromolecules and polymers in their native states (e.g. liquid phase). This means that the structural changes of (bio-)polymers, such as proteins and DNA, can be monitored in situ to understand their sensitivity to changes in chemical environments. In an attempt to improve the reliability of such experiments, the reduction of radiation damage occurring from exposure to X-rays is required. One such method, is to use scavenger molecules to protect macromolecules against radicals produced during radiation exposure, such as reactive oxygen species (ROS). In this study we investigate the feasibility of applying the compatible solute, osmolyte and radiation protector Ectoine (THP(B)), as a scavenger molecule during SAXS measurements of the single-stranded DNA-binding protein Gene-V Protein (G5P/GVP). In this case, we monitor the radiation induced changes of G5P during bio-SAXS measurments and the resulting microscopic energy-damage relation was determined from microdosimetric calculations by Monte-Carlo based particle scattering simulations with TOPAS/Geant4 and a custom target-model. This resulted in a median-lethal energy deposit of pure G5P at 4 mg mL−1 of E1/2 = 7 ± 5 eV, whereas a threefold increase of energy-deposit was needed under the presence of Ectoine to reach the same level of damage. This indicates that Ectoine increases the possible exposure time before radiation-damage to G5P is observed. Furthermore, the dominant type of damage shifted from aggregation in pure solutions towards a fragmentation for solutions containing Ectoine as a cosolute. These results are interpreted in terms of indirect radiation damage by reactive secondary species, as well as post-irradiation effects, related to preferential-exclusion of the cosolute from the protein surface. Hence, Ectoine is shown to provide a non-disturbing way to improve structure-determination of proteins via bio-SAXS in future studies. KW - BioSAXS KW - Bio-SAXS KW - Cosolute KW - Ectoine KW - G5P KW - GVP KW - Radiation damage KW - Radical Scavenger KW - Single-stranded DNA-binding proteins KW - X-ray scattering KW - DNA KW - ssDNA KW - Protein KW - SAXS KW - Small-angle xray scattering KW - McSAS3 KW - Dosimetry KW - Microdosimetry KW - Geant4 KW - Geant4-DNA KW - Topas KW - Topas-MC KW - Monte-Carlo simulations KW - Particle scattering simulations KW - Topas-nBio KW - OH Radical KW - OH radical scavenger KW - LEE KW - Ionizing radiation damage KW - Protein unfolding KW - Ectoin PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568909 DO - https://doi.org/10.1039/d2cp05053f SN - 1463-9076 SN - 1463-9084 VL - 25 IS - 7 SP - 5372 EP - 5382 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-56890 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hallier, Dorothea C. A1 - Smales, Glen Jacob A1 - Seitz, H. A1 - Hahn, Marc Benjamin T1 - Inside back cover for the article "Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine" N2 - Showcasing research from the Federal Institute for Material Research and Testing Berlin and Fraunhofer Institute for Celltherapy and Immunology Branch Bioanalytics and Bioprocesses Potsdam. Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine. We aimed to increase the possible undisturbed exposure time during bio-SAXS measurements of single-stranded DNA-binding proteins. Therefore small angle X-ray scattering was performed on Gene-V Protein (G5P/GVP), which is involved in DNA repair processes. To achieve this, irradiations were performed in presence and absence of the hydroxyl-radical scavenger and osmolyte Ectoine, which showed efficient radiation protection and prevented protein aggregation, thus allows for a non-disturbing way to improve structure-determination of biomolecules. KW - Bio-SAXS KW - BioSAXS KW - Cosolute KW - DNA KW - Dosimetry KW - Ectoin KW - Ectoine KW - G5P KW - GVP KW - Geant4 KW - Geant4-DNA KW - Ionizing radiation damage KW - LEE KW - McSAS3 KW - Microdosimetry KW - Monte-Carlo simulations KW - OH Radical KW - OH radical scavenger KW - Protein KW - Protein unfolding KW - Radiation damage KW - Radical Scavenger KW - SAXS KW - Single-stranded DNA-binding proteins KW - Small-angle xray scattering KW - Topas-MC KW - Topas-nBio KW - TopasMC KW - X-ray scattering KW - Particle scatterin simulations KW - ssDNA PY - 2023 DO - https://doi.org/10.1039/D3CP90056H SN - 1463-9076 SN - 1463-9084 VL - 25 IS - 7 SP - 5889 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-57006 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hunter, R. D. A1 - Hayward, E. C. A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Kulak, A. A1 - Guan, S. A1 - Schnepp, Z. T1 - The effect of nitrogen on the synthesis of porous carbons by iron-catalyzed graphitization N2 - This paper reports a systematic study into the effect of nitrogen on iron-catalyzed graphitization of biomass. Chitin, chitosan, N-acetylglucosamine, gelatin and glycine were selected to represent nitrogen-rich saccharides and amino-acid/polypeptide biomass precursors. The materials were pyrolyzed with an iron catalyst to produce carbons with a wide range of chemical and structural features such as mesoporosity and nitrogen-doping. Many authors have reported the synthesis of nitrogen-doped carbons by pyrolysis and these have diverse applications. However, this is the first systematic study of how nitrogen affects pyrolysis of biomass and importantly the catalytic graphitization step. Our data demonstrates that nitrogen inhibits graphitization but that some nitrogen survives the catalytic graphitization process to become incorporated into various chemical environments in the carbon product. KW - Graphitization KW - Nanoparticles KW - Nanocomposite KW - Porous carbon KW - Nitrogen KW - Scattering PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575351 DO - https://doi.org/10.1039/d3ma00039g VL - 4 SP - 2070 EP - 2077 PB - Royal Society of Chemistry AN - OPUS4-57535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Extending Bio-SAXS measurements of Single-Stranded DNA-Binding Proteins: Radiation Protection of G5P by Cosolutes N2 - Small-angle X-ray scattering (SAXS) can be used for structural de- termination of biological macromolecules and polymers in their na- tive states. To improve the reliability of such experiments, the re- duction of radiation damage occurring from exposure to X-rays is needed.One method, is the use of scavenger molecules that protect macromolecules against radicals produced by radiation exposure.In this study we investigate the feasibility to apply the compatible solute, osmolyte and radiation protector Ectoine (THP(B)) as a scavenger throughout SAXS measurements of single-stranded DNA-binding protein Gene-V Protein (G5P/GVP). Therefore we monitor the radiation induced changes of G5P during bio-SAXS. The resulting microscopic energy-damage relation was determined by particle scattering simu- lations with TOPAS/Geant4. The results are interpreted in terms of radical scavenging as well as post-irradiation effects, related to preferential-exclusion from the protein surface. Thus, Ectoine provides an non-disturbing way to improve structure-determination of proteins via bio-SAXS in future studies. T2 - MultiChem Conference 2023 CY - Prague, Czech Republic DA - 26.04.2023 KW - Bio-SAXS KW - BioSAXS KW - Compatible solute KW - Cosolute KW - DNA KW - Dosimetry KW - Ectoin KW - Ectoine KW - Ectoin KW - G5P KW - GVP KW - Geant4 KW - Geant4-DNA KW - Gene five protein KW - Hydroxyectoine KW - Ionizing radiation damage KW - LEE KW - McSAS3 KW - Microdosimetry KW - Monte-Carlo simulations KW - OH Radical KW - OH radical scavenger KW - Osmolyte KW - Particle scattering simulations KW - Protein KW - Protein unfolding KW - Proteins KW - ROS KW - Radiation damage KW - Radical Scavenger KW - Radical scavenger KW - SAXS KW - Single-stranded DNA-binding proteins KW - Small-angle xray scattering KW - Topas KW - Topas-MC KW - Topas-nBio KW - X-ray scattering KW - ssDNA KW - Median lethal energy deposit PY - 2023 AN - OPUS4-57407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - BP150: Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine N2 - Small-angle X-ray scattering (SAXS) can be used for structural determination of biological macromolecules and polymers in their native states (e.g. liquid phase). This means that the structural changes of (bio-)polymers, such as proteins and DNA, can be monitored in situ to understand their sensitivity to changes in chemical environments. In an attempt to improve the reliability of such experiments, the reduction of radiation damage occurring from exposure to X-rays is required. One such method, is to use scavenger molecules to protect macromolecules against radicals produced during radiation exposure, such as reactive oxygen species (ROS). In this study we investigate the feasibility of applying the compatible solute, osmolyte and radiation protector Ectoine (THP(B)), as a scavenger molecule during SAXS measurements of the single-stranded DNA-binding protein Gene-V Protein (G5P/GVP). In this case, we monitor the radiation induced changes of G5P during bio-SAXS measurments and the resulting microscopic energy-damage relation was determined from microdosimetric calculations by Monte-Carlo based particle scattering simulations with TOPAS/Geant4 and a custom target-model. This resulted in a median-lethal energy deposit of pure G5P at 4 mg mL−1 of E1/2 = 7 ± 5 eV, whereas a threefold increase of energy-deposit was needed under the presence of Ectoine to reach the same level of damage. This indicates that Ectoine increases the possible exposure time before radiation-damage to G5P is observed. Furthermore, the dominant type of damage shifted from aggregation in pure solutions towards a fragmentation for solutions containing Ectoine as a cosolute. These results are interpreted in terms of indirect radiation damage by reactive secondary species, as well as post-irradiation effects, related to preferential-exclusion of the cosolute from the protein surface. Hence, Ectoine is shown to provide a non-disturbing way to improve structure-determination of proteins via bio-SAXS in future studies. T2 - DPG Frühjahrstagung CY - Dresden, Germany DA - 26.03.2023 KW - Bio-SAXS KW - BioSAXS KW - Compatible solute KW - Cosolute KW - DNA KW - Dosimetry KW - Ectoin KW - Ectoine KW - G5P KW - GVP KW - Gene five protein KW - Geant4 KW - Geant4-DNA KW - Hydroxyectoine KW - Ionizing radiation damage KW - LEE KW - McSAS3 KW - Microdosimetry KW - Monte-Carlo simulations KW - OH Radical KW - OH radical scavenger KW - Osmolyte KW - Particle scattering simulations KW - Protein KW - Proteins KW - Protein unfolding KW - ROS KW - Radiation damage KW - Radical Scavenger KW - SAXS KW - Single-stranded DNA-binding proteins KW - Small-angle xray scattering KW - Topas KW - Topas-MC KW - Topas-nBio KW - X-ray scattering KW - Radical scavenger KW - ssDNA PY - 2023 AN - OPUS4-57254 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Anker, A. S. A1 - Balazs, D. M. A1 - Beyer, F. L. A1 - Bienert, Ralf A1 - Bouwman, W. G. A1 - Breßler, Ingo A1 - Breternitz, J. A1 - Brok, E. S. A1 - Bryant, G. A1 - Clulow, A. J. A1 - Crater, E. R. A1 - De Geuser, F. A1 - Giudice, A. D. A1 - Deumer, J. A1 - Disch, S. A1 - Dutt, S. A1 - Frank, K. A1 - Fratini, E. A1 - Gilbert, E. P. A1 - Hahn, Marc Benjamin A1 - Hallett, J. A1 - Hohenschutz, Max A1 - Hollamby, M. J. A1 - Huband, S. A1 - Ilavsky, J. A1 - Jochum, J. K. A1 - Juelsholt, M. A1 - Mansel, B. W. A1 - Penttilä, P. A1 - Pittkowski, R. K. A1 - Portale, G. A1 - Pozzo, L. D. A1 - Ricardo de Abreu Furtado Garcia, P. A1 - Rochels, L. A1 - Rosalie, Julian A1 - Saloga, P. E. J. A1 - Seibt, S. A1 - Smith, A. J. A1 - Smith, G. N. A1 - Annadurai, V. A1 - Spiering, G. A. A1 - Stawski, Tomasz A1 - Taché, O. A1 - Thünemann, Andreas A1 - Toth, K. A1 - Whitten, A. E. A1 - Wuttke, J. T1 - The human factor - Results of a small-angle scattering data analysis round robin N2 - A Round Robin study has been carried out to estimate the impact of the human element in small-angle scattering data analysis. Four corrected datasets were provided to participants ready for analysis. All datasets were measured on samples containing spherical scatterers, with two datasets in dilute dispersions, and two from powders. Most of the 46 participants correctly identified the number of populations in the dilute dispersions, with half of the population mean entries within 1.5 % and half of the population width entries within 40 %, respectively. Due to the added complexity of the structure factor, much fewer people submitted answers on the powder datasets. For those that did, half of the entries for the means and widths were within 44 % and 86 % respectively. This Round Robin experiment highlights several causes for the discrepancies, for which solutions are proposed. KW - Round robin KW - Sall-angle scattering KW - Nanostructure quantification KW - Nanostructure KW - SAXS KW - MOUSE KW - X-ray scattering KW - Size distribution KW - Nanoparticles PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571342 DO - https://doi.org/10.48550/arXiv.2303.03772 SP - 1 EP - 23 PB - Cornell University CY - Ithaca, NY AN - OPUS4-57134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pütz, E. A1 - Smales, Glen Jacob A1 - Jegel, O. A1 - Emmerling, Franziska A1 - Tremel, W. T1 - Tuning ceria catalysts in aqueous media at the nanoscale: how do surface charge and surface defects determine peroxidase- and haloperoxidase-like reactivity N2 - Designing the shape and size of catalyst particles, and their interfacial charge, at the nanometer scale can radically change their performance. We demonstrate this with ceria nanoparticles. In aqueous media, nanoceria is a functional mimic of haloperoxidases, a group of enzymes that oxidize organic substrates, or of peroxidases that can degrade reactive oxygen species (ROS) such as H2O2 by oxidizing an organic substrate. We show that the chemical activity of CeO2−x nanoparticles in haloperoxidase- and peroxidaselike reactions scales with their active surface area, their surface charge, given by the ζ-potential, and their surface defects (via the Ce3+/Ce4+ ratio). Haloperoxidase-like reactions are controlled through the ζ-potential as they involve the adsorption of charged halide anions to the CeO2 surface, whereas peroxidase-like reactions without charged substrates are controlled through the specific surface area SBET. Mesoporous CeO2−x particles, with large surface areas, were prepared via template-free hydrothermal reactions and characterized by small-angle X-ray scattering. Surface area, ζ-potential and the Ce3+/Ce4+ ratio are controlled in a simple and predictable manner by the synthesis time of the hydrothermal reaction as demonstrated by X-ray photoelectron spectroscopy, sorption and ζ-potential measurements. The surface area increased with synthesis time, whilst the Ce3+/Ce4+ ratio scales inversely with decreasing ζ-potential. In this way the catalytic activity of mesoporous CeO2−x particles could be tailored selectively for haloperoxidase- and peroxidase-like reactions. The ease of tuning the surface properties of mesoporous CeO2x particles by varying the synthesis time makes the synthesis a powerful general tool for the preparation of nanocatalysts according to individual needs. KW - SAXS KW - Ceria KW - Zeta potential PY - 2022 DO - https://doi.org/10.1039/D2NR03172H SP - 1 EP - 12 PB - Royal Society of Chemistry AN - OPUS4-55649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Henning, L. M. A1 - Smales, Glen Jacob A1 - Colmenares, M. G. A1 - Bekheet, M. F. A1 - Simon, U. A1 - Gurlo, A. T1 - Synthesis and properties of COK-12 large-pore mesocellularsilica foam N2 - Large, ink-bottle-shaped pores in mesocellular foams (MCFs) are desired for various applications requiring enhanced mass transfer or the immobilization of larger compounds. Hence, the cylindrical pores of COK-12, an ordered mesoporous silica structurally comparable to SBA-15 but synthesized at room-temperature at quasi-neutral pH, are chemically swollen into ink-bottle pores. Therefore, p-xylene is used as a more sustainable swelling agent compared to popular alternatives. Its high boiling point allows for an additional thermal aging step to amplify the mesostructure enlargement without needing additional chemicals. For COK-12, the MCFs obtained at room temperature reach an unprecedented plateau for the modal mesopore cell and window diameter of 19.9 and 5.5 nm, respectively, with an underlying broad pore size distribution and distorted hexagonal lattice up to 14.5 nm, involving hexagonal and spherical structures. The combined chemical and thermal swelling resulted in the selective enlargement of the window diameter to more than 200% and a slightly increased cell diameter, pore size distribution, and hexagonal lattice distortion in comparison to the room temperature synthesis. Such materials are thought to be promising alternatives to SBA-15-based MCFs, often utilizing toxic catalysts during synthesis. The presented results pave the way for enhanced adsorptive, catalytic, and drug delivery performances for COK-12-based materials. KW - SAXS KW - MOUSE KW - Mesocellular foam KW - Mesoporous silica PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569590 DO - https://doi.org/10.1002/nano.202200223 SP - 1 EP - 11 AN - OPUS4-56959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine N2 - Small-angle X-ray scattering (SAXS) can be used for structural determination of biological macromolecules and polymers in their native states (e.g. liquid phase). This means that the structural changes of (bio-)polymers, such as proteins and DNA, can be monitored in situ to understand their sensitivity to changes in chemical environments. In an attempt to improve the reliability of such experiments, the reduction of radiation damage occurring from exposure to X-rays is required. One such method, is to use scavenger molecules to protect macromolecules against radicals produced during radiation exposure, such as reactive oxygen species (ROS). In this study we investigate the feasibility of applying the compatible solute, osmolyte and radiation protector Ectoine (THP(B)), as a scavenger molecule during SAXS measurements of the single-stranded DNA-binding protein Gene-V Protein (G5P/GVP). In this case, we monitor the radiation induced changes of G5P during bio-SAXS measurments and the resulting microscopic energy-damage relation was determined from microdosimetric calculations by Monte-Carlo based particle scattering simulations with TOPAS/Geant4 and a custom target-model. This resulted in a median-lethal energy deposit of pure G5P at 4 mg mL−1 of E1/2 = 7 ± 5 eV, whereas a threefold increase of energy-deposit was needed under the presence of Ectoine to reach the same level of damage. This indicates that Ectoine increases the possible exposure time before radiation-damage to G5P is observed. Furthermore, the dominant type of damage shifted from aggregation in pure solutions towards a fragmentation for solutions containing Ectoine as a cosolute. These results are interpreted in terms of indirect radiation damage by reactive secondary species, as well as post-irradiation effects, related to preferential-exclusion of the cosolute from the protein surface. Hence, Ectoine is shown to provide a non-disturbing way to improve structure-determination of proteins via bio-SAXS in future studies. T2 - #RSCposter 2023 CY - Online meeting DA - 28.02.2023 KW - Bio-SAXS KW - BioSAXS KW - Cosolute KW - DNA KW - Dosimetry KW - Ectoin KW - Ectoine KW - G5P KW - GVP KW - Geant4 KW - Geant4-DNA KW - Ionizing radiation damage KW - LEE KW - McSAS3 KW - Microdosimetry KW - Monte-Carlo simulations KW - OH Radical KW - OH radical scavenger KW - Particle scattering simulations KW - Protein KW - Protein unfolding KW - Radiation damage KW - Radical Scavenger KW - SAXS KW - Single-stranded DNA-binding proteins KW - Small-angle xray scattering KW - Topas KW - Topas-MC KW - Topas-nBio KW - X-ray scattering KW - ssDNA KW - Osmolyte KW - Hydroxyectoine KW - Compatible solute KW - ROS KW - radical scavenger PY - 2023 UR - https://pubs.rsc.org/en/content/articlehtml/2023/cp/d2cp05053f AN - OPUS4-57064 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - Electric Safety Interlock N2 - This interlock is designed to prevent electrical shock from high voltage (>60V) equipment. While the general safety interlock can be generically applied, this particular example employs an external vacuum-activated switch. It is for safeguarding human operations inside a vacuum sample chamber while the chamber doors are open. The circuit is closed (output is active) when a sufficient level of vacuum is reached, i.e. when all accessible openings are necessarily closed. The initial application is to interrupt power to a 220V, 250W heating cartridge (itself mounted inside a small sample holder with potentially exposed contacts) when the sample chamber is open. The external circuit can be modified to use different interlock mechanisms as needed. Note that the external interlock circuit is only a single circuit (with two signal lines) and thus is not protected against external shorts. To accomodate a range of safety interlocks, the 4-pin M12 connector is wired as follows: Pin 1 (Brown): +24V for power supply, max current 0.6A Pin 2 (White): Safety interlock system signal 1 (0 or 24V) Pin 3 (Blue) : Safety interlock system signal 2 (0 or 24V) Pin 4 (Black): 0V for power supply The safety is interlocked (output active) when both signal pins are set high (24V), with sufficient current to activate the two relays. Pin 1 and 4 can be used to power safety hardware (such as light curtains or proximity detectors) with 24VDC up to a current of 0.6A. A larger power supply can be installed when higher currents are needed, while staying within the current limits imposed by the wiring cross-section. KW - Electric Safety Interlock KW - MOUSE KW - 60-230V PY - 2023 DO - https://doi.org/10.6084/m9.figshare.22265920.v1 PB - Digital Science CY - Cambridge, MA, USA AN - OPUS4-57138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - X-ray Scattering USAXS/SAXS/WAXS (/XRD/PDF) N2 - A ten minute introduction to the technique of X-ray scattering. This talk discusses the foundation and the resulting morphological parameters that can be obtained from the technique. The talk is prepared for discussion within the framework of the OECD REACH guideline for nanomaterials. T2 - Digitaler Info-Tag "Nano or not Nano" CY - Berlin, Germany DA - 16.02.2023 KW - X-ray scattering KW - BAM Academy KW - SAXS KW - XRD KW - WAXS KW - Nanomaterial KW - REACH KW - OECD KW - Guideline PY - 2023 AN - OPUS4-57013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Kolmangadi, Mohamed Aejaz T1 - X-ray scattering datasets associated with the publication "Molecular Mobility of Polynorbornenes with Trimethylsiloxysilyl side groups: Influence of the Polymerization Mechanism" N2 - X-ray scattering datasets for samples described in the 2022 publication "Molecular Mobility of Polynorbornenes with Trimethylsiloxysilyl side groups: Influence of the Polymerization Mechanism". This dataset includes both raw and processed X-ray scattering data for samples APTCN and MPTCN, alongside background measurements files (BKG). KW - X-ray scattering KW - SAXS KW - MOUSE KW - Membrane polymers KW - Microporous polymers PY - 2023 DO - https://doi.org/10.5281/zenodo.7621204 PB - Zenodo CY - Geneva AN - OPUS4-56972 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Kolmangadi, Mohamed Aejaz T1 - X-ray scattering datasets associated with the publication "Side chain length dependent dynamics and conductivity in self assembled ion channels" N2 - X-ray scattering datasets for samples described in the 2022 publication "Side chain length dependent dynamics and conductivity in self assembled ion channels". This dataset includes both raw and processed X-ray scattering data for samples ILC8, ILC10, ILC12, ILC14 and ILC16 alongside background measurement files (BKG). KW - X-ray scattering KW - SAXS KW - MOUSE KW - Columnar ionic liquid crystals KW - Liquid crystals PY - 2023 DO - https://doi.org/10.5281/zenodo.7621358 PB - Zenodo CY - Geneva AN - OPUS4-56973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Wetzel, Annica A1 - Oczan, Ozlem A1 - Nietzke, Jonathan A1 - Richter, Tim A1 - Schröpfer, Dirk T1 - Hydrogen diffusion and local Volta potential in high- and medium-entropy alloys N2 - High-entropy alloys (HEAs) are characterized by a solid solution of minimum five and medium-entropy alloys (MEAs) of minimum three principal alloying elements in equiatomic proportions. They show exceptional application properties, such as high-strength and ductility or corrosion resistance. Future HEA/MEA-components could be exposed to hydrogen containing environments like vessels for cryogenic or high-pressure storage where the hydrogen absorption and diffusion in these materials is of interest. In our study, we investigated the HEA Co20Cr20Fe20Mn20Ni20 and the MEA Co33.3Cr33.3Ni33.3. For hydrogen ingress, cathodic charging was applied and diffusion kinetic was measured by high-resolution thermal desorption spectros-copy using different heating rates up to 0.250 K/s. Peak deconvolution resulted in high-temperature desorption peaks and hydrogen trapping above 280 °C. A total hydrogen concentration > 40 ppm was identified for the MEA and > 100 ppm for HEA. This indicates two important effects: (1) delayed hydrogen diffusion and (2) considerable amount of trapped hydrogen that must be anticipated for hydrogen assisted cracking phenomenon. Local electrochemical Volta potential maps had been measured for the hydrogen free condition by means of high-resolution Scanning Kelvin Probe Force Microscopy (SKPFM). T2 - Symposium on Materials and Joining Technology CY - Online meeting DA - 07.09.2020 KW - Hydrogen KW - High-entropy alloy KW - Diffusion KW - Scanning kelvin probe force microscopy KW - Corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511684 DO - https://doi.org/10.1088/1757-899X/882/1/012015 VL - 882 SP - 1 EP - 15 PB - IOP Publishing CY - Bristol AN - OPUS4-51168 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buzolin, R. H. A1 - Richter, Tim A1 - Pixner, F. A1 - Rhode, Michael A1 - Schröpfer, Dirk A1 - Enzinger, N. T1 - Microstructure characterisation of multi-principal element alloys welds produced by electron beam welding N2 - This work explores the feasibility of producing bead-on-plate welds of a CrCoNi medium entropy alloy and a CrMnFeCoNi high entropy alloy using electron beam welding. The alloys were welded in two states: one in an as-cold-rolled condition and the other in an annealed condition. In addition, the materials are welded with two different parameters. The FCC microstructure of the welds is investigated using scanning electron microscopy assisted by energy-dispersive X-ray spectroscopy and electron-backscattered diffraction. The impact of the weld on the microstructure is discussed. The heat-affected zone is negligible for the annealed condition of both medium and high entropy alloys since there is no driving force for recrystallisation and the exposure time to high temperature is insufficient for grain coarsening. The texture formed in the fusion zone is also discussed and compared to the texture in the base metal and the heat-affected zone. Although the grain growth along the (100) crystallographic direction is preferential in all cases, the crystallographic texture type differs from each weld. Higher hardness values are measured in the medium entropy alloy’s base metal and fusion zone than in the high entropy alloy. KW - Multi-principal element alloy KW - Electron backscattered diffraction KW - Electron beam welding KW - High-entropy alloy KW - Microstructure characterization PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568129 DO - https://doi.org/10.1016/j.matdes.2023.111609 SN - 1873-4197 VL - 225 SP - 1 EP - 14 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-56812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hufgard, Josefin T1 - Traveling Wave Acoustic Ion Manipulation (AIM) for Ion Trajectory Alteration N2 - Acoustic ion manipulation (AIM) is a recent discovery reliant on the sound-ion interactions under ambient conditions. Instead of relying upon conventional electric or magnetic fields, this technique initially exploits standing acoustic waves to focus, gate, deflect, and separate ions. Compared to AIM in a standing wave scenario, the transportation of ions and their response to traveling acoustic waves remain less understood. In contrast to standing waves, which establish stationary pressure domains, traveling waves engender continuously propagating pressure variations. Here, we report on AIM effects induced by traveling acoustic waves that occur from a single-transducer setup. The changes in ion trajectory induced by acoustic traveling waves, ion-specific responses to the traveling wave and its analytical applications will be investigated. A home-built alternating-current (AC) plasma source was used to produce a laminar ion stream, positioned ~10 cm from the inlet capillary of an Orbitrap mass spectrometer. A Langevin-type ultrasonic transducer operated at 40 kHz and ~50 W was used to introduce a diverging sound gradient arranged perpendicular to the ion beam direction. Small model analytes, such as methanol, isopropanol, and acetone, were doped in the discharge gas flow as traces produced in the source, to differentiate from ions produced between the source and MS inlet capillary. Aerodynamic information on both the sound field and the gas stream is provided by defocusing shadowgraphy images. T2 - ASMS 73rd Conference on Mass spectrometry and Allied topics CY - Baltimore, Maryland, USA DA - 01.06.2025 KW - Mass spectrometry KW - Acoustic Ion Manipulation (AIM) KW - Traveling acoustic wave PY - 2025 AN - OPUS4-63380 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aliyah, K. A1 - Prehal, C. A1 - Diercks, J. S. A1 - Diklić, N. A1 - Xu, L. A1 - Ünsal, S. A1 - Appel, C. A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Guizar-Sicairos, M. A1 - Herranz, J. A1 - Gubler, L. A1 - Büchi, F. N. A1 - Eller, J. T1 - Quantification of PEFC Catalyst Layer Saturation via In Silico, Ex Situ, and In Situ Small-Angle X-ray Scattering N2 - The complex nature of liquid water saturation of polymer electrolyte fuel cell (PEFC) catalyst layers (CLs) greatly affects the device performance. To investigate this problem, we present a method to quantify the presence of liquid water in a PEFC CL using small-angle X-ray scattering (SAXS). This method leverages the differences in electron densities between the solid catalyst matrix and the liquid water filled pores of the CL under both dry and wet conditions. This approach is validated using ex situ wetting experiments, which aid the study of the transient saturation of a CL in a flow cell configuration in situ. The azimuthally integrated scattering data are fitted using 3D morphology models of the CL under dry conditions. Different wetting scenarios are realized in silico, and the corresponding SAXS data are numerically simulated by a direct 3D Fourier transformation. The simulated SAXS profiles of the different wetting scenarios are used to interpret the measured SAXS data which allows the derivation of the most probable wetting mechanism within a flow cell electrode. KW - Polymer electrolyte fuel cell KW - Water management KW - Catalyst layer KW - Representative morphology modeling KW - Small-angle X-ray scattering KW - MOUSE KW - SAXS PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575973 DO - https://doi.org/10.1021/acsami.3c00420 SN - 1944-8244 VL - 15 IS - 22 SP - 26538 EP - 26553 PB - ACS Publications AN - OPUS4-57597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - Small-angle scattering data analysis round robin dataset - Original for participants N2 - These are four datasets that were made available to the participants of the Small-angle Scattering data analysis round robin. The intent was to find out how comparable results from different researchers are, who analyse exactly the same processed, corrected dataset. In this repository, there are: 1) a PDF document with more details for the study, 2) the datasets for people to try and fit, 3) an Excel spreadsheet to document the results. Datasets 1 and 2 were modified from: Deumer, Jerome, & Gollwitzer, Christian. (2022). npSize_SAXS_data_PTB (Version 5) [Data set]. Zenodo. https://doi.org/10.5281/zenodo.5886834 Datasets 3 and 4 were collected in-house on the MOUSE instrument. KW - Round robin KW - SAXS KW - Small angle scattering KW - SANS KW - X-ray KW - Neutron KW - Human factor KW - Data analysis KW - Data fitting KW - Human influence PY - 2023 DO - https://doi.org/10.5281/zenodo.7506365 PB - Zenodo CY - Geneva AN - OPUS4-56799 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - A quick intro to our NeXus format… N2 - A brief introduction is given into our data collection and organization procedure, and why we have settled on the HDF5-based NeXus format for describing experimental data. The links between NeXus and the SciCat data catalog is also provided, showing how the NeXus metadata is automatically added as searchable metadata in the catalog. T2 - NFDI NeXus Workshop CY - Online meeting DA - 17.03.2022 KW - Data management KW - Measurement organization KW - Measurement data KW - NFDI KW - FAIR KW - Open access KW - Data mining KW - Data tagging KW - Automated data tagging PY - 2022 AN - OPUS4-54823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard T1 - McSAS3 N2 - McSAS3 is a refactored version of the original McSAS (see DOI 10.1107/S1600576715007347). This software fits scattering patterns to obtain size distributions without assumptions on the size distribution form. The refactored version has some neat features: - Multiprocessing is included, spread out over as many cores as number of repetitions! - Full state of the optimization is stored in an organized HDF5 state file. - Histogramming is separate from optimization and a result can be re-histogrammed as many times as desired. - SasModels allow a wide range of models to be used - If SasModels does not work (e.g. because of gcc compiler issues on Windows or Mac), an internal sphere model is supplied - Simulated data of the scattering of a special shape can also be used as a McSAS fitting model. Your models are infinite! - 2D fitting also works. KW - X-ray scattering KW - Polydispersity KW - Monte carlo KW - Scattering pattern analysis KW - Analysis approach KW - Neutron scattering KW - Automation KW - Command line PY - 2023 DO - https://doi.org/10.6084/m9.figshare.21814128.v1 PB - Digital Science CY - Cambridge, MA, USA AN - OPUS4-56787 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob T1 - X-ray scattering Datasets of gold and silver nanoparticle composites, relating to the publication "Gold and silver dichroic nanocomposite in the quest for 3D printing the Lycurgus cup" N2 - Wide-range X-ray scattering datasets and analyses for all samples described in the 2020 publication "Gold and silver dichroic nanocomposite in the quest for 3D printing the Lycurgus cup". These datasets are composed by combining multiple small-angle x-ray scattering and wide-angle x-ray scattering curves into a single dataset. They have been analyzed using McSAS to extract polydispersities and volume fractions. They have been collected using the MOUSE project (instrument and methodology). KW - X-ray scattering KW - MOUSE KW - Saxs KW - Waxs KW - Analyses KW - Datasets PY - 2022 DO - https://doi.org/10.5281/zenodo.7193859 PB - Zenodo CY - Geneva AN - OPUS4-55979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard T1 - Technical Drawings for The MOUSE Modular Sample Holder: Capillary Flow-through Cell N2 - OpenSCAD, STL and technical drawings for the capillary flow-through cell designed primarily for use with The MOUSE instruments. This flow-through cell can be used in conjunction with: - Modular sample holder (10.5281/zenodo.7499416) - Solid sample rack/plate (10.5281/zenodo.7499424) - Laser-cut sample holder (10.5281/zenodo.7499437) KW - X-ray scattering KW - SAXS KW - Sample holder KW - MOUSE PY - 2023 DO - https://doi.org/10.5281/zenodo.7499421 PB - Zenodo CY - Geneva AN - OPUS4-56776 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard T1 - Technical Drawings for The MOUSE Modular Sample Holder: Solid Sample Rack/Plate N2 - OpenSCAD, STL and technical drawings for the solid sample rack designed primarily for use with The MOUSE instruments. This solid sample rack can be used in conjunction with: - Laser-cut sample holder (10.5281/zenodo.7499437) - Modular sample holder (10.5281/zenodo.7499416) - Capillary flow-cell for liquid samples (10.5281/zenodo.7499421) KW - X-ray scattering KW - SAXS KW - Sample holder KW - MOUSE PY - 2023 DO - https://doi.org/10.5281/zenodo.7499424 PB - Zenodo CY - Geneva AN - OPUS4-56778 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard T1 - Technical Drawings for The MOUSE Modular Sample Holder N2 - OpenSCAD, STL and technical drawings for the Modular sample holder designed primarily for use with The MOUSE instruments. This modular sample holder can be used in conjunction with the following: - Capillary flow-cell for liquid samples (10.5281/zenodo.7499421) - Solid sample rack/plate (10.5281/zenodo.7499424) - Laser-cut sample holder (10.5281/zenodo.7499437) KW - X-ray scattering KW - SAXS KW - Sample holder KW - MOUSE PY - 2023 DO - https://doi.org/10.5281/zenodo.7499416 PB - Zenodo CY - Geneva AN - OPUS4-56775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard T1 - Technical Drawings for The MOUSE Modular Sample Holder: Laser-cut Sample Holder N2 - PDF file for the laser-cut sample holder designed primarily for use with The MOUSE instruments. This sample holder can be used in conjunction with: - Solid sample rack/plate (10.5281/zenodo.7499424) - Modular sample holder (10.5281/zenodo.7499416) - Capillary flow-cell for liquid samples (10.5281/zenodo.7499421) KW - X-ray scattering KW - SAXS KW - Sample holder KW - MOUSE PY - 2023 DO - https://doi.org/10.5281/zenodo.7499437 PB - Zenodo CY - Geneva AN - OPUS4-56779 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - The human factor: A round robin study on the variation in data analyses N2 - How much do we, the small-angle scatterers, influence the results of an investigation? What uncertainty do we add by our human diversity in thoughts and approaches, and is this significant compared to the uncertainty from the instrumental measurement factors? After our previous Round Robin on data collection, we know that many laboratories can collect reasonably consistent small-angle scattering data on easy samples. To investigate the next, human component, we compiled four existing datasets from globular (roughly spherical) scatterers, each exhibiting a common complication, and asked the participants to apply their usual methods and toolset to the quantification of the results (https://lookingatnothing.com/index.php/archives/3274). Accompanying the datasets was a modicum of accompanying information to help with the interpretation of the data, similar to what we normally receive from our collaborators. More than 30 participants reported back with volume fractions, mean sizes and size distribution widths of the particle populations in the samples, as well as information on their self-assessed level of experience and years in the field. While the Round Robin is still underway (until the 25th of April, 2022), the initial results already show significant spread in the results. Some of these are due to the variety in interpretation of the meaning of the requested parameters, as well as simple human errors, both of which are easy to correct for. Nevertheless, even after correcting for these differences in understanding, a significant spread remains. This highlights an urgent challenge to our community: how can we better help ourselves and our colleagues obtain more reliable results, how could we take the human factor out of the equation, so to speak? In this talk, we will introduce the four datasets, their origins and challenges. Hot off the press, we will summarize the anonymized, quantified results of the Data Analysis Round Robin. (Incidentally, we will also see if a correlation exists between experience and proximity of the result to the median). Lastly, potential avenues for improving our field will be offered based on the findings, ranging from low-effort yet somehow controversial improvements, to high-effort foundational considerations. T2 - International Small-Angle Scattering Conference (SAS2022) CY - Campinas, Brazil DA - 11.09.2022 KW - Round robin KW - Data analysis KW - Small angle scattering KW - Nanomaterials KW - MOUSE KW - Interlaboratory comparison KW - Intercomparability KW - Reliability KW - Data analysis round robin KW - Large number of participants PY - 2022 AN - OPUS4-55762 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Brian Richard T1 - X-ray scattering for nanostructure quantification, and the quest for the perfect experiment N2 - Measuring an X-ray scattering pattern is relatively easy, but measuring a steady stream of high-quality, useful patterns requires significant effort and good laboratory organization. Such laboratory organization can help address the reproducibility crisis in science, and easily multiply the scientific output of a laboratory, while greatly elevating the quality of the measurements. We have demonstrated this for small- and wide-angle X-ray scattering in the MOUSE project (Methodology Optimization for Ultrafine Structure Exploration). With the MOUSE, we have combined a comprehensive and highly automated laboratory workflow with a heavily modified X-ray scattering instrument. This combination allows us to collect fully traceable scattering data, within a well-documented, FAIR-compliant data flow (akin to what is found at the more automated synchrotron beamlines). With two full-time researchers, our lab collects and interprets thousands of datasets, on hundreds of samples, for dozens of projects per year, supporting many users along the entire process from sample selection and preparation, to the analysis of the resulting data. This talk will briefly introduce the foundations of X-ray scattering, present the MOUSE project, and will highlight the proven utility of the methodology for materials science. Upgrades to the methodology will also be discussed, as well as possible avenues for transferring this holistic methodology to other instruments T2 - SNI 2022 CY - Berlin, Germany DA - 05.09.2022 KW - Methodology KW - X-ray scattering KW - Laboratory management KW - Instrumentation utilization KW - MOUSE KW - SAXS KW - WAXS KW - Automation PY - 2022 AN - OPUS4-55760 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - VIDEO A1 - Pauw, Brian Richard T1 - The human factor: A round robin study on the variation in data analyses N2 - This is a remote presentation I gave at the 2022 Small-angle Scattering conference in Campinas, Brazil. The video has been obtained from the conference organisers with their explicit permission for use on YouTube. I've tried to spruce up the audio from the remote recording the best I could. The conference abstract for this talk was: "How much do we, the small-angle scatterers, influence the results of an investigation? What uncertainty do we add by our human diversity in thoughts and approaches, and is this significant compared to the uncertainty from the instrumental measurement factors? After our previous Round Robin on data collection, we know that many laboratories can collect reasonably consistent small-angle scattering data on easy samples. To investigate the next, human component, we compiled four existing datasets from globular (roughly spherical) scatterers, each exhibiting a common complication, and asked the participants to apply their usual methods and toolset to the quantification of the results (https://lookingatnothing.com/index.php/archives/3274). Accompanying the datasets was a modicum of accompanying information to help with the interpretation of the data, similar to what we normally receive from our collaborators. More than 30 participants reported back with volume fractions, mean sizes and size distribution widths of the particle populations in the samples, as well as information on their self-assessed level of experience and years in the field. While the Round Robin is still underway (until the 25th of April, 2022), the initial results already show significant spread in the results. Some of these are due to the variety in interpretation of the meaning of the requested parameters, as well as simple human errors, both of which are easy to correct for. Nevertheless, even after correcting for these differences in understanding, a significant spread remains. This highlights an urgent challenge to our community: how can we better help ourselves and our colleagues obtain more reliable results, how could we take the human factor out of the equation, so to speak? In this talk, we will introduce the four datasets, their origins and challenges. Hot off the press, we will summarize the anonymized, quantified results of the Data Analysis Round Robin. (Incidentally, we will also see if a correlation exists between experience and proximity of the result to the median). Lastly, potential avenues for improving our field will be offered based on the findings, ranging from low-effort yet somehow controversial improvements, to high-effort foundational considerations." T2 - International Small-Angle Scattering Conference (SAS2022) CY - Campinas, Brazil DA - 11.09.2022 KW - Round robin KW - Data analysis KW - X-ray scattering KW - Neutron scattering KW - Nanomaterials KW - Metrology KW - Interlaboratory comparison PY - 2023 UR - https://www.youtube.com/watch?v=t1Rowo--Osg DO - https://doi.org/10.26272/opus4-56897 PB - YouTube, LLC CY - San Bruno, CA, USA AN - OPUS4-56897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Smales, Glen Jacob A1 - Hahn, Marc Benjamin A1 - Hallier, Dorothea C. A1 - Seitz, H. T1 - X-ray scattering datasets and simulations associated with the publication "Bio-SAXS of single-stranded DNA-binding proteins: Radiation protection by the compatible solute ectoine" N2 - This dataset contains the processed and analysed small-angle X-ray scattering data associated with all samples from the publications "Bio-SAXS of Single-Stranded DNA-Binding Proteins: Radiation Protection by the Compatible Solute Ectoine" (https://doi.org/10.1039/D2CP05053F). Files associated with McSAS3 analyses are included, alongside the relevant SAXS data, with datasets labelled in accordance to the protein (G5P), its concentration (1, 2 or 4 mg/mL), and if Ectoine is present (Ect) or absent (Pure). PEPSIsaxs simulations of the GVP monomer (PDB structure: 1GV5 ) and dimer are also included. TOPAS-bioSAXS-dosimetry extension for TOPAS-nBio based particle scattering simulations can be obtained from https://github.com/MarcBHahn/TOPAS-bioSAXS-dosimetry which is further described in https://doi.org/10.26272/opus4-55751. This work was funded by the Deutsche Forschungsgemeinschaft (DFG, German Research Foundation) under grant number 442240902 (HA 8528/2-1 and SE 2999/2-1). We acknowledge Diamond Light Source for time on Beamline B21 under Proposal SM29806. This work has been supported by iNEXT-Discovery, grant number 871037, funded by the Horizon 2020 program of the European Commission. KW - SAXS KW - Radiation protection KW - Microdosimetry KW - G5P KW - Ectoine KW - DNA-Binding protein PY - 2023 DO - https://doi.org/10.5281/zenodo.7515394 PB - Zenodo CY - Geneva AN - OPUS4-56811 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Röder, Bettina A1 - Smales, Glen Jacob T1 - High temperature in-vacuum flow-through sample holder (sandwich design version 1.1) N2 - Technical drawings and documents for building a compact, heated, vacuum compatible flow-through sample holder. This holder is in use at the BAM MOUSE instrument as well as at the I22 beamline at the Diamond Light Source (see references for instrument details). This holder has several features: - The holder can be used in vacuum environments as well as in atmosphere - It has two G 1/4" UNF fittings to attach HPLC tubing for (optionally) flowing a medium through the sample cell - There are two additional (unflowed) sample positions for backgrounds and calibrants, held at the same temperature - The low-mass design coupled with a 250W heating element can achieve heating rates of 1 degree C per second, when coupled (for example) with an Omron E5CC PID controller. - The sample holder insert can be made from various materials depending on the application. Sealing the sample from the vacuum can be achieved using kapton, teflon or Magic tape, depending on the temperature requirements. The inlet and outlet holes will need to be punctured with a needle to enable flow. - Large exit cones ensure a clear exit angle of at least 45 degrees two theta. - It has been tested with temperatures up to 400 degrees C. - Compression area has been raised and polished to ensure a good vacuum seal. KW - SAXS KW - X-ray scattering KW - Sample cell KW - Sample holder KW - Heated KW - Flow-through KW - Vacuum compatible KW - XRD KW - WAXS PY - 2023 DO - https://doi.org/10.5281/zenodo.7501030 PB - Zenodo CY - Geneva AN - OPUS4-56777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Smales, Glen Jacob A1 - Pauw, Brian Richard A1 - Kolmangadi, Mohamed Aejaz T1 - X-ray scattering datasets associated with the publication "Molecular Dynamics of Janus Polynorbornenes: Glass Transitions and Nanophase Separation" N2 - X-ray scattering datasets for samples described in the 2020 publication "Molecular Dynamics of Janus Polynorbornenes: Glass Transitions and Nanophase Separation". This dataset includes both raw and processed X-ray scattering data for samples PTCHSiO-Pr, Bu, Hx, Oc and De, alongside background measurements files (BKG). This data was collected using the MOUSE project (instrument and methodology). KW - X-ray scattering KW - SAXS KW - MOUSE KW - Alkyls KW - Polymers PY - 2023 DO - https://doi.org/10.5281/zenodo.7614835 PB - Zenodo CY - Geneva AN - OPUS4-56971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Smales, Glen Jacob A1 - Sprachmann, J. T1 - Datasets of Antiaromatic COFs associated with the publication "Antiaromatic Covalent Organic Frameworks Based on Dibenzopentalenes" N2 - X-ray scattering and sorption data associated with the publication "Antiaromatic Covalent Organic Frameworks Based on Dibenzopentalenes". X-ray scattering data is provided for COF and POP materials, including data from stability tests, as three-column ascii files with columns q (nm-1), I (m-1) and uncertainty on I, as well as being provided in 2θ. KW - X-ray scattering KW - SAXS KW - Covalent Organic Frameworks KW - Antiaromaticity KW - MOUSE PY - 2023 DO - https://doi.org/10.5281/zenodo.7509377 PB - Zenodo CY - Geneva AN - OPUS4-56868 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Smales, Glen Jacob A1 - Rosalie, Julian T1 - Small-angle scattering data analysis round robin - Anonymized results, figures and Jupyter notebook N2 - The intent of this round robin was to find out how comparable results from different researchers are, who analyse exactly the same processed, corrected dataset. This zip file contains the anonymized results and the jupyter notebook used to do the data processing, analysis and visualisation. Additionally, TEM images of the samples are included. KW - Round robin KW - Small-angle scattering KW - Data analysis PY - 2023 DO - https://doi.org/10.5281/zenodo.7509710 PB - Zenodo CY - Geneva AN - OPUS4-56803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sprachmann, J. A1 - Wachsmuth, T. A1 - Bhosale, M. A1 - Burmeister, D. A1 - Smales, Glen Jacob A1 - Schmidt, M. A1 - Kochovski, Z. A1 - Grabicki, N. A1 - Wessling, R. A1 - List-Kratochvil, E. J. W. A1 - Esser, B. A1 - Dumele, O. T1 - Antiaromatic Covalent Organic Frameworks Based on Dibenzopentalenes N2 - Despite their inherent instability, 4n π systems have recently received significant attention due to their unique optical and electronic properties. In dibenzopentalene (DBP), benzanellation stabilizes the highly antiaromatic pentalene core, without compromising its amphoteric redox behavior or small HOMO−LUMO energy gap. However, incorporating such molecules in organic devices as discrete small molecules or amorphous polymers can limit the performance (e.g., due to solubility in the battery electrolyte solution or low internal surface area). Covalent organic frameworks (COFs), on the contrary, are highly ordered, porous, and crystalline materials that can provide a platform to align molecules with specific properties in a well-defined, ordered environment. We synthesized the first antiaromatic framework materials and obtained a series of three highly crystalline and porous COFs based on DBP. Potential applications of such antiaromatic bulk materials were explored: COF films show a conductivity of 4 × 10−8 S cm−1 upon doping and exhibit photoconductivity upon irradiation with visible light. Application as positive electrode materials in Li-organic batteries demonstrates a significant enhancement of performance when the antiaromaticity of the DBP unit in the COF is exploited in its redox activity with a discharge capacity of 26 mA h g−1 at a potential of 3.9 V vs. Li/Li+ . This work showcases antiaromaticity as a new design principle for functional framework materials. KW - SAXS KW - MOUSE KW - Covalent Organic Frameworks KW - Batteries PY - 2023 DO - https://doi.org/10.1021/jacs.2c10501 SP - 1 EP - 12 PB - ACS Publications AN - OPUS4-56958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael A1 - Nietzke, Jonathan A1 - Richter, Tim T1 - Hydrogen diffusion and desorption characteristics of a CoCrFeMnNi high entropy and a CoCrNi medium entropy alloy N2 - High-entropy alloys (HEAs) are innovative high-performance materials that have attracted more and more research attention. HEAs are characterized by a solid solution of typically five equiatomic metallic elements. In addition, medium-entropy alloys (MEA, with three elements) are of interest and become more and more important. Depending on the alloy concept, HEAs and MEAs show exceptional mechanical properties, especially high-strength and ductility combinations at both cryogenic and elevated temperatures combined with excellent corrosion resistance. Future structural HEA/MEA components can be exposed to potential applications with hydrogen containing environments like high-temperature water in pressurized nuclear reactors or aerospace structures. Other potential applications could be in materials for vessel walls in the field of cryogenic and high-pressure hydrogen storage. So far, the susceptibility of HEAs/MEAs to hydrogen assisted cracking (if any) and the hydrogen diffusion is not investigated in detail yet and can limit or extend possible applications of HEA/MEA as structural materials. In our work, we focused on the hydrogen absorption, diffusion, and distribution in a HEA (CoCrFeMnNi the original Cantor-alloy) and a MEA (CoCrNi). Cathodic hydrogen charging was carried out for the hydrogen ingress, and thermal desorption analysis (TDA) revealed complex hydrogen trapping in both alloy types up to 300 °C. The absorbed total hydrogen concentrations were > 100 ppm for the HEA and > 40 ppm for MEA. In addition, the assessment of the peak deconvolution is not trivial and must consider both experimental and microstructure influences. T2 - 4th International Conference on Metals and Hydrogen - Steely & Hydrogen 2022 CY - Ghent, Belgium DA - 11.10.2022 KW - Hydrogen KW - High-entropy alloy KW - Multiple principal element alloy KW - Thermal desorption analysis KW - Diffusion PY - 2022 SP - 1 EP - 11 CY - Ghent, Belgium AN - OPUS4-56076 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana A1 - Bruno, Giovanni T1 - BAM activities in material characterization by advanced X-ray imaging N2 - The overview of the activity of Federal Institute for Material Research and Testing (BAM, Belin, Germany) in the field of additively manufacturing material characterization will be presented. The research of our group is focused on the 3D imaging of AM materials by means of X-ray Computed Tomography at the lab and at synchrotron, and the residual stress characterization by diffraction (nondestructive technique). Also, two successful research project in collaboration with CAM2, Sweden are presented. T2 - CAM2 Annual Meeting CY - Gothenburg, Sweden DA - 25.10.2023 KW - Additive manufacturing KW - Residual stress KW - X-ray computed tomography PY - 2023 AN - OPUS4-58828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lorenzoni, R. A1 - Curosu, I. A1 - Léonard, Fabien A1 - Paciornik, S. A1 - Mechtcherine, V. A1 - Silva, F. A. A1 - Bruno, Giovanni T1 - Combined mechanical and 3D-microstructural analysis of strain-hardening cement-based composites (SHCC) by in-situ X-ray microtomography N2 - The paper presents the results of a series of combined mechanical and in-situ morphological investigations on highstrength strain-hardening cement-based Composites (SHCC). Tension and compression experiments were performed in a CT scanner employing a dedicated mechanical testing rig. The in-situ microtomographic scans enabled correlating the measured specimen response with relevant microstructural features and fracture processes. The microstructural segmentation of SHCC was performed in the framework of Deep Learning and it targeted an accurate segmentation of pores, fibers and aggregates. Besides their accurate volumetric representation, these phases were quantified in terms of content, size and orientation. The fracture processes were monitored at different loading stages and Digital Volume Correlation (DVC) was employed to spatially map the strains and cracks in the specimens loaded in compression. The DVC analysis highlighted the effect of loading conditions, specimen geometry and material heterogeneity at the mesolevel on the strain distribution and fracture localization. KW - Digital Volume Correlation KW - High Strength Concrete KW - In-situ Computed Tomography KW - composites PY - 2020 DO - https://doi.org/10.1016/j.cemconres.2020.106139 VL - 136 SP - 106139 PB - Elsevier Ltd. AN - OPUS4-51054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Gas Tomography Up In The Air! N2 - In this paper, we present an autonomous aerial robot to reconstruct tomographic 2D slices of gas plumes in outdoor environments. Our platform, the so-called Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS) combines a lightweight Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile octocopter. The TDLAS sensor provides integral gas concentration measurements but no information regarding the distance traveled by the laser diode's beam or the distribution of the gas along the optical path. We complemented the set-up with a laser rangefinder and apply principles of Computed Tomography (CT) to create a model of the spatial gas distribution from these integral concentration measurements. To allow for a rudimentary ground truth evaluation of the applied gas tomography algorithm, we set up a unique outdoor test environment based on two 3D ultrasonic anemometers and a distributed array of 10 infrared gas transmitters. We present first results showing the 2D plume reconstruction capabilities of the system under realistic conditions. T2 - IEEE Sensors 2018 CY - New Delhi, India DA - 28.10.2018 KW - Aerial robot KW - TDLAS KW - Gas tomography KW - Plume PY - 2018 AN - OPUS4-46478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Neumann, Patrick P. T1 - Bringing Mobile Robot Olfaction to the Next Dimension – UAV-based Remote Sensing of Gas Clouds and Source Localization N2 - This presentation introduces a novel robotic platform for aerial remote gas sensing. Spectroscopic measurement methods for remote sensing of selected gases lend themselves for use on mini-copters, which offer a number of advantages for inspection and surveillance. No direct contact with the target gas is needed and thus the influence of the aerial platform on the measured gas plume can be kept to a minimum. This allows to overcome one of the major issues with gas-sensitive mini-copters. On the other hand, remote gas sensors, most prominently Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensors have been too bulky given the payload and energy restrictions of mini-copters. Here, we introduce and present the Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), which combines a novel lightweight TDLAS sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile hexacopter. The proposed system can be deployed in scenarios that cannot be addressed by currently available robots and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO). It enables tomographic reconstruction of gas plumes and a localization of gas sources. We also present first results showing the gas sensing and aiming capabilities under realistic conditions. T2 - IEEE International Conference on Robotics and Automation (ICRA) CY - Singapore DA - 29.05.2017 KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - 3-axis gimbal KW - Mobile Robot Olfaction KW - Tomographic reconstruction of gas plumes KW - Localization of gas sources KW - Aerial platform PY - 2017 AN - OPUS4-40547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bernard, D. T1 - On the use of autocorrelation functions, permeability tensors, and computed tomography to characterize the anisotropy of Diesel particulate filter materials N2 - 3D images such as those produces by X-ray tomography can provide a wealth of information on the internal structure of materials, but quantification of specific geometrical or topological characteristics linked to some bulk physical property is far from being straightforward. This study focuses on methods to quantify the differences in physical properties as a function of direction, i.e. their anisotropy, and how it can be linked to measures of anisotropy of the internal structure of the material. The auto-correlation function gives a similarity measure in the volume as a function of distance and direction. This is a cross-correlation of the image with itself fast to compute and relatively insensitive to noise. It is why we focus on this method to compare with the physical property of our DPF material. Diesel Particulate Filter (DPF) materials are porous ceramics that; a) can be used at very high temperatures; b) have very good thermal shock resistance; c) are inert; d) can be manufactured with tailored porosity. Their usual way of production consists of the extrusion of a slurry into the desired filter shape, with successive ceramming at high temperature. This process causes anisotropy at both microscopic and macroscopic levels. T2 - ICTMS 2019 CY - Cairns, Australia DA - 22.07.2019 KW - Structure-property relationship KW - Anisotropy estimate KW - Porous ceramics KW - Autocorrelation PY - 2019 AN - OPUS4-49226 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lehmann, Jens A1 - Ebell, Gino A1 - Burkert, Andreas T1 - Potentialfeldmessung - Korrosionsprüfung von Stahlbetonbauwerken N2 - Durch das alkalische Porenwassermilieu ist Stahl im Beton vor Korrosion geschützt. Unter un-günstigen Umgebungsbedingungen (Karbonatisierung, Chlorideintrag) kann die passive Deck-schicht auf der Stahloberfläche zerstört werden. Im weiteren Verlauf können sich korrosionsbe-dingte Folgeschäden, wie Risse und Abplatzungen am Bauwerk ergeben. Um notwendige Sanie-rungsmaßnahmen sind frühzeitige und weitgehend zerstörungsfrei ermittelte Informationen über das aktuelle Korrosionsverhalten der Stahlbewehrung von großer Bedeutung. Die Potentialfeld-messung ist ein etabliertes und weit verbreitetes Verfahren zur Beurteilung des Korrosionszu-standes der Bewehrung in Stahlbetonbauwerken. Mit Hilfe dieses Verfahrens können Bereiche aktiv korrodierender Bewehrung zerstörungsfrei lokalisiert werden. In der Regel kommt diese Messmethode bei der Detektion chloridinduzierter Korrosion zum Einsatz. T2 - Fachtagung Prüfen von Beton CY - Berlin und Hamburg, Germany DA - 06.10.2016 und 11.10.2016 KW - Stahlbeton KW - Spannbeton KW - Korrosion KW - Zerstörungsfreie Prüfung PY - 2016 SP - 51 EP - 57 AN - OPUS4-37710 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - 3D imaging and residual stress analysis of AM Materials N2 - In this seminar, the capabilities for materials characterization at Division 8.5, BAM will be shon. Particular focus will be given to residual stress analysis and defect imaging in additively manufactured materials and components T2 - Skoltech - The 3rd International Workshop of Advanced Manufacturing Technologies CY - Online meeting DA - 18.04.2023 KW - Neutron Diffraction KW - X-ray diffraction KW - X-ray Computed Tomography KW - X-ray refraction radiography KW - Residual stress KW - Additive manufacturing PY - 2023 AN - OPUS4-57360 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mishurova, Tatiana A1 - Thiede, Tobias A1 - Cabeza, Sandra A1 - Bruno, Giovanni A1 - Kromm, Arne A1 - Nadammal, Naresh T1 - The influence of the support structure on residual stress and distortion in SLM Inconel 718 parts N2 - The effect of support structure and of removal from the base plate on the residual stress state in Selective Laser Melted IN718 parts was studied by means of synchrotron X-ray diffraction. The residual stresses in subsurface region of two elongated prisms in as-built condition and after the cutting from the base plate were determined. One sample was directly built on a base plate and another one on a support structure. Also, the distortion on the top surface due to stress release was measured by contact profilometry. High tensile residual stress values were found, with pronounced stress gradient along the hatching direction. In the sample on support stress redistribution took place after removal of the base plate, as opposed to simple stress relaxation for the sample without support. The sample on support structure showed larger distortion compared to sample without support. We conclude that the use of a support decreases stress values but stress relieving heat treatments are still needed. T2 - User Meeting HZB 2018 CY - Berlin, Germany DA - 14.12.2017 KW - Additive manufacturing KW - Selective laser melting KW - Residual stress KW - Synchrotron X-ray diffraction PY - 2017 AN - OPUS4-43460 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Völker, Christoph T1 - Toward Data based corrosion analysis of concrete with supervised machine learning N2 - Half-Cell-Potential Mapping (HP) is the most popular non-destructive testing (NDT) method for the detection of active corrosion in reinforced concrete. HP is influenced by parameters such as moisture and chloride gradients in the component. The sensitivity to the spatially small, but dangerous pitting is low. In this study we show how additional measurement information can be used with multi-sensor data fusion to improve the detection performance and to automate data evaluation. The fusion is based on supervised machine learning (SML). SML are methods that recognize relationships in (sensor) data based on given labels. We use SML to distinguish "defective" and "intact" labeled areas in our dataset. It consists of 18 measurement - each contains HP, ground radar, microwave moisture and Wenner resistivity data. Exact labels for changing environmental conditions were determined in a laboratory study on a reinforced concrete slab, which deteriorated controlled and accelerated. The deterioration progress was monitored continuously and corrosion was generated targeted at a predefined location. The detection results are quantified and statistically evaluated. The data fusion shows a significant improvement over the best single method (HP). We describe the challenges of data-driven approaches in nondestructive testing and show possible solutions. T2 - SMT/NDT-CE 2018 CY - New Brunswick, NJ, USA DA - 26.08.2018 KW - SMT KW - NDT-CE PY - 2018 AN - OPUS4-46261 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rifai, Haifa A1 - Staude, Andreas A1 - Meinel, Dietmar A1 - Illerhaus, Bernhard A1 - Bruno, Giovanni T1 - In-situ pore size investigations of loaded porous concrete with non-destructive methods N2 - Subject of this investigation is the in-situ evolution of pore volume and pore size distribution in Ytong (a porous concrete material) under increasing pressure with two different non-destructive analytical methods: Nuclear Magnetic Resonance (NMR) and X-ray Computed Tomography (CT). For both methods special strain devices to apply external pressure were constructed. The results from the two techniques yield complementary information on the pore size distribution and allows covering different pore size regions. KW - Pore size KW - Porous concrete KW - Computed tomography KW - Nuclear magnetic resonance PY - 2018 DO - https://doi.org/10.1016/j.cemconres.2018.06.008 SN - 0008-8846 SN - 1873-3948 VL - 111 SP - 72 EP - 80 PB - Elsevier Ltd. AN - OPUS4-45617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartholmai, Matthias A1 - Johann, Sergej A1 - Wu, Cheng-Chieh T1 - Airborne remote gas sensing and mapping N2 - Leaking methane (CH4) from infrastructures, such as pipelines and landfills, is critical for the environment but can also pose a safety risk. To enable a fast detection and localization of these kind of leaks, we developed a novel robotic platform for aerial remote gas sensing. Spectroscopic measurement methods for remote sensing of selected gases lend themselves for use on mini-copters, which offer a number of advantages for inspection and surveillance over traditional methods. No direct contact with the target gas is needed and thus the influence of the aerial platform on the measured gas plume can be kept to a minimum. This allows to overcome one of the major issues with gas-sensitive mini-copters. On the other hand, remote gas sensors, most prominently Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensors have been too bulky given the payload and energy restrictions of mini-copters. Here, we present the Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), which combines a novel lightweight TDLAS sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile hexacopter. The proposed system can be deployed in scenarios that cannot be addressed by currently available robots and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO). It enables tomographic reconstruction of gas plumes and a localization of gas sources. We also present first results showing its performance under realistic conditions. T2 - 5th International Conference on Smart Monitoring, Assessment and Rehabilitation of Civil Structures (SMAR 2019) CY - Potsdam, Germany DA - 27.08.2019 KW - Localization of gas sources KW - Mobile Robot Olfaction KW - Tomographic reconstruction of gas plumes KW - Tunable Diode Laser Absorption Spectroscopy (TDLAS) KW - UAV-REGAS PY - 2017 AN - OPUS4-48789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lucka, R. A1 - Elshani, B. A1 - Kilic, M. S. A1 - Klimke, S. A1 - Krüger, C. A1 - Menzel, Michael A1 - Stößer, R. A1 - Titiš, J. A1 - Boča, R. A1 - Renz, F. T1 - ESR and Mössbauer spectroscopy of iron(III) spin crossover complexes based on pentadentate Schiff base ligands with pseudohalide coligands N2 - Two iron(III) spin crossover complexes [Fe(5Cl-L)(NCS)] (1) and [Fe(5Cl-L)(NCSe)] (2) were synthesized with the pentadentate Schiff base ligand 5Cl-L and thiocyanato and selenocyanato as coligands. 5Cl-L, as an asymmetric {N3O2} donor Schiff base, was synthesized by a condensation reaction of 5-chlorosalicyladehyde using the asymmetric N-(2-aminoethyl)-1,3-propanediamine. The complexes exhibited a spin crossover at 280 (1) and 293 K (2), respectively, and were subjected to electron spin resonance (ESR) and Mössbauer spectroscopy at 77, 295 and 325 K. Ab initio CASSCF calculations followed by the NEVPT2 method were applied for predicting the g-tensor components as well as Mössbauer parameters. KW - Spin crossover KW - Iron(III) complexes KW - Mössbauer spectroscopy KW - ESR spectroscopy KW - Ab initio calculations PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-634061 DO - https://doi.org/10.3390/magnetochemistry11050043 SN - 2312-7481 VL - 11 IS - 5 SP - 1 EP - 9 PB - MDPI CY - Basel AN - OPUS4-63406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Was kann die Neutronenbeugung für die ZfP tun? N2 - Neutronenbeugung hat verschiedenste Anwendungen, die auf die eigenartigen physikalischen Eigenschaften der Neutronen berühen. Während die Beugungstechniken wie z.B. die klassische Pulverbeugung, die Kleinwinkelstreuung und die Texturanalyse besonders für die Materialcharakterisierung nutzbar sind, setzt sich die Neutronenbeugung als zerstörungsfreies Verfahren für Eigenspannungsanalyse extrem relevant ein. Allerdings sind nur wenig die Leute, die die Neutronenbeugung in der ZfP Community benutzen. Dieser Vortrag hat das Ziel die Interesse an der Nutzung von einem solchen Grossgerätwerkzeug aufzuwecken und ein Paar impactvolle Anwendungsbeispiele einiger Techniken zu zeigen. Die Bestimmung mikroskopischer mechanischen Eigenschaften von Kompositen (MMC oder CMC), sowie der Mapping von Eigenspannungsfelder in Komponenten werden bearbeitet. Es wird gezeigt, dass Neutronenbeugung grundsätzlich eine zerstörungsfreie Methode für beide die Materialcharakterisierung und die Komponentenintegrität ist, die hohes Potentiell hat, zum Verfahrensportfolio der zerstörungsfreier Prüfung zu gehören. T2 - 381. Sitzung des Arbeitskreises Berlin der DGZfP CY - BAM, Berlin, Deutschland DA - 01.11.2016 KW - Neutronenbeugung KW - Eigenspannungen KW - Kompositen KW - Legierungen KW - Schweißnähte KW - TF Material PY - 2016 AN - OPUS4-38313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kruschwitz, Sabine A1 - Halisch, M. A1 - Dlugosch, R. A1 - Prinz, Carsten T1 - Toward a better understanding of low-frequency electrical relaxation - An enhanced pore space characterization N2 - Relaxation phenomena observed in the electrical low-frequency range (approximately 1 mHz-10 kHz) of natural porous media like sandstones is often assumed to be directly related to the dominant (modal) pore throat sizes measured, for instance, with mercury intrusion porosimetry. Attempts to establish a universally valid relationship between pore size and peak Spectral Induced Polarization (SIP) relaxation time have failed, considering sandstones from very different origins and featuring great variations in textural and chemical compositions as well as in geometrical pore space properties. In addition working with characteristic relaxation times determined in Cole-Cole or Debye decomposition fits to build the relationship have not been successful. In particular, samples with narrow pore throats are often characterized by long SIP relaxation times corresponding to long “characteristic length scales” in these media, assuming that the diffusion coefficients along the electrical double layer were constant. Based on these observations, three different types of SIP relaxation can be distinguished. We present a new way of assessing complex pore spaces of very different sandstones in a multi-methodical approach to combine the benefits of mercury intrusion porosimetry, micro-computed tomography, and nuclear magnetic resonance. In this way, we achieve much deeper insight into the pore space due to the different resolutions and sensitivities of the applied methods to both pore constrictions (throats) and wide pores (pore bodies). We experimentally quantify pore aspect ratios and volume distributions within the two pore regions. We clearly observe systematic differences between three SIP relaxation types identified previously and can attribute the SIP peak relaxation times to measured characteristic length scales within our materials. We highlight selected results for a total of nine sandstones. It seems that SIP relaxation behavior depends on the size difference of the narrow pore throats to the wide pore bodies, which increases from SIP Type 1 to Type 3. KW - µ-CT KW - Spectral induced polarization KW - Nuclear magnetic resonance KW - Pore space PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509763 DO - https://doi.org/10.1190/GEO2019-0074.1 SN - 0016-8033 VL - 85 IS - 4 SP - MR257 EP - MR270 PB - Society of Exploration Geophysicists AN - OPUS4-50976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kruschwitz, Sabine A1 - Munsch, Sarah Mandy A1 - Telong, Melissa A1 - Schmidt, Wolfram A1 - Bintz, Thilo A1 - Fladt, Matthias A1 - Stelzner, Ludwig T1 - The NMR core analyzing TOMograph: A multi-functional tool for non-destructive testing of building materials N2 - NMR is becoming increasingly popular for the investigation of building materials as it is a non-invasive technology that does not require any sample preparation nor causes damage to the material. Depending on the specific application it can offer insights into properties like porosity and spatial saturation degree as well as pore structure. Moreover it enables the determination of moisture transport properties and the (re-)distribution of internal moisture into different reservoirs or chemical phases upon damage and curing. However, as yet most investigations were carried out using devices originally either designed for geophysical applications or the analysis of rather homogeneous small scale (< 10 mL) samples. This paper describes the capabilities of an NMR tomograph, which has been specifically optimized for the investigation of larger, heterogeneous building material samples (diameters of up to 72 mm, length of up to 700 mm) with a high flexibility due to interchangeable coils allowing for a high SNR and short echo times (50 - 80 m s). KW - Fire spalling KW - Moisture transport KW - Concrete KW - Cement hydration KW - Sensitivity KW - Supplementary cementitous materials KW - Frost salt attack PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-573755 DO - https://doi.org/10.1016/j.mrl.2023.03.004 SN - 2097-0048 VL - 3 IS - 3 SP - 207 EP - 219 PB - Elsevier B.V. AN - OPUS4-57375 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Radnik, Jörg T1 - Minimale Anforderungen an Referenzdaten anhand von Beispielen aus der Elektronenmikroskopie und Oberflächenanalytik N2 - In dem Vortrag werden, anhand ausgewählten Beispielen aus der Elektronenmikroskopie und Oberflächenanalytik (EDX und XPS), die minimalen Anforderungen an Referenzdaten für zuverlässige und reproduzierbare Ergebnisse (z.B. Partikelgrößenverteilung, Elementzusammensetzung) vorgestellt und diskutiert. T2 - Workshop "Referenzdaten" CY - Berlin, Germany DA - 13.03.2020 KW - Referenzdaten KW - Nanopartikel KW - Elektronenmikroskopie KW - Oberflächenanalytik KW - Standardarbeitsanweisung KW - SOP KW - Standardisierung PY - 2020 AN - OPUS4-50571 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Analytical and Characterisation Excellence in nanomaterial risk assessment: A tiered approach Task2.5 N2 - The final results of Task 2.5 "Optimization of sample preparation for characterization of ENPs using TOF-SIMS under real-life conditions (a.) UfZ: polymer template; b.) BAM: pressing of pellets)" were presented. T2 - ACEnano General Meeting CY - Amsterdam, The Netherlands DA - 05.03.2020 KW - Nanoparticles KW - ToF-SIMS KW - Preparation PY - 2020 AN - OPUS4-50572 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arinchtein, A. A1 - Schnack, R. A1 - Kraffert, K. A1 - Radnik, Jörg A1 - Dietrich, P. A1 - Sachse, René A1 - Krähnert, R. T1 - Role of Water in Phase Transformations and Crystallization of Ferrihydrite and Hematite N2 - The oxides, hydroxides, and oxo-hydroxides of iron belong to the most abundant materials on earth. They also feature a wide range of practical applications. In many environments, they can undergo facile phase transformations and crystallization processes. Water appears to play a critical role in many of these processes. Despite numerous attempts, the role of water has not been fully revealed yet. We present a new approach to study the influence of water in the crystallization and phase transformations of iron oxides. The approach employs model-type iron oxide films that comprise a defined homogeneous nanostructure. The films are exposed to air containing different amounts of water reaching up to pressures of 10 bar. Ex situ analysis via scanning electron microscopy, Transmission electron microscopy, selected area electron diffraction, and X-ray diffraction is combined with operando near-ambient pressure X-ray photoelectron spectroscopy to follow water-induced changes in hematite nd ferrihydrite. Water proves to be critical for the nucleation of ematite domains in ferrihydrite, the resulting crystallite orientation, and the underlying crystallization mechanism. KW - Iron oxide KW - Ferrihydrite KW - Hematite KW - Water KW - NAP-XPS KW - High pressure PY - 2020 DO - https://doi.org/10.1021/acsami.0c05253 VL - 12 SP - 38714 EP - 38722 PB - ACS Publication AN - OPUS4-51201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stockmann, Jörg M. T1 - Reference material for the determination of the field of view of small-area X-ray photoelectron spectrometers N2 - Small-area/spot photoelectron spectroscopy (SAXPS) is a powerful tool for the investigation of small surface features like microstructures of electronic devices, sensors or other functional surfaces. For evaluating the quality of such microstructures, it is crucial to know whether a small signal in a spectrum is an unwanted contamination of the field of view (FoV), defined by the instrument settings, or it originated from outside. The aperture has a major influence on the signal-contribution from the outside. For the evaluation of the FoV, we determined the Au4f intensities measured with the center of the FoV aligned with the center of the spot and normalized to the Au4f intensity determined on the Au-film. With this test specimen, it was possible to characterize the FoV: The signal-contribution from the outside is reduceable down to lower than 50 %, when the aperture is 30 % of the structure dimension for our Kratos AXIS Ultra DLD system. T2 - Kratos User's Meeting 2020 CY - Online meeting DA - 21.09.2020 KW - Small-area XPS KW - Field of View KW - Imaging XPS KW - Reference Material PY - 2020 AN - OPUS4-51412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Surface chemical analysis surface chemical analysis of cells and biofilms N2 - The status of the planned technical report "Surface characterization of biomaterials" will be presented. T2 - ISO TC201 Meeting CY - Online meeting DA - 05.09.2020 KW - X-ray photoelectron spectroscopy KW - X-ray spectroscopy KW - Biomaterials KW - Standardization PY - 2020 AN - OPUS4-51197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Füllenbach, L.C. A1 - Perez, J. P. H. A1 - Freeman, H.M. A1 - Thomas, A.N. A1 - Mayanna, S. A1 - Parker, J. E. A1 - Göttlicher, J. A1 - Steininger, R. A1 - Radnik, Jörg A1 - Benning, L.G. A1 - Oelkers, E.H. T1 - Nanoanalytical Identification of Siderite Dissolution-Coupled Pb Removal Mechanisms from Oxic and Anoxic Aqueous Solutions N2 - Lead(II) is a toxic pollutant often found in metalcontaminated soils and wastewaters. In acidic aqueous environments, Pb(II) is highly mobile. Chemical treatment strategies of such systems therefore often include neutralization agents and metal sorbents. Since metal solubility and the retention potential of sorbents depend on the redox state of the aqueous system, we tested the efficiency of the naturally occurring redox-sensitive ferrous iron carbonate mineral siderite to remove Pb(II) from acidic aqueous solutions in batch experiments under oxic and anoxic conditions over a total of 1008 h. Siderite dissolution led to an increase in reactive solution pH from 3 to 5.3 and 6.9, while 90 and 100% of the initial aqueous Pb(II) (0.48 × 10−3 mol kg−1) were removed from the oxic and anoxic systems, respectively. Scanning and transmission electron microscopy, combined with X-ray absorption and photoelectron spectroscopy, indicated that under oxic conditions, Pb(II) was consumed by cerussite precipitation and inner-sphere surface complexation to secondary goethite. Under anoxic conditions, Pb(II) was removed by the rapid precipitation of cerussite. This efficient siderite dissolution-coupled sequestration of Pb(II) into more stable solid phases demonstrates this potential method for contaminated water Treatment regardless of the redox environment. KW - Siderite KW - X-ray absorption spectroscopy KW - X-ray photoelectron spectroscopy KW - Wastewater treatment PY - 2020 DO - https://doi.org/10.1021/acsearthspacechem.0c00180 VL - 4 IS - 11 SP - 1966 EP - 1977 PB - ACS Publication AN - OPUS4-51961 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Analytical & Characterisation Excellence in nanomaterial risk assessment: A tiered approach N2 - The work packages of the EU H2020 project ACEnano are presented and their activities in standardization and guidance for regulators and SMEs. T2 - ISO/TC 229 Strategy meeting CY - Online meeting DA - 10.11.2020 KW - Nanomaterials KW - Standardization KW - Risk assessment PY - 2020 AN - OPUS4-51611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Crasselt, Claudia A1 - Schmidt, Wolfram A1 - Sturm, Heinz T1 - Influence of Rheology Modifying Admixtures on Hydration of Cementitious Suspensions N2 - The presence of polycarboxylate ether (PCE) based superplasticizers (SPs) has an enormous influence on the early hydration of cement. The hydration is retarded and the timing of formation and the morphology of hydrates is affected. This short paper presents experimental results about the influence of delayed addition time of PCE SPs on hydration of cement and alite pastes, investigated by isothermal heat flow calorimetry. For cement as well as for alite pastes the hydration is retarded with SP, whereby the high charge PCE has a stronger retarding effect than the low charge PCE. The retardation caused by PCE is much more pronounced for alite than for cement mixes. If PCE is added later to the mix, the induction period is shortened and the hydration is accelerated compared to simultaneous addition. This applies for cement and alite pastes. With delayed PCE addition the alite shows a clearly less retarded setting and main hydration than after simultaneous addition. It is obvious that for alite pastes there is less retardation the later the addition of SP. T2 - 6th International Symposium on Nanotechnology in Construction CY - Hong Kong, China DA - 02.12.2018 KW - Polycarboxylate ether (PCE) KW - Early hydration KW - Cement PY - 2018 SP - 1 EP - 8 AN - OPUS4-47204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Oster, Simon A1 - Scheuschner, Nils A1 - Chand, Keerthana A1 - Altenburg, Simon A1 - Gerlach, G. T1 - Erratum to: Potentials and challenges of deep-learning-assisted porosity prediction based on thermographic in-situ monitoring in laser powder bed fusion N2 - In this erratum to our previously published study section, we correct an error related to the first paragragh of section 5 "Prediction framework". PY - 2024 DO - https://doi.org/10.1515/teme-2023-0166 SN - 0171-8096 SN - 2196-7113 VL - 91 IS - 2 SP - 139 EP - 141 PB - De Gruyter CY - Berlin AN - OPUS4-59471 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Near-ambient-pressure Xray photoelectron spectroscopy (XPS) to monitor DNA radiation damage directly in water N2 - Ionizing radiation damage to DNA plays a fundamental role in cancer therapy. X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. The results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further. T2 - RADeleven CY - Herceg Novi, Montenegro DA - 19.06.2023 KW - Base damage KW - Base loss KW - Cancer treatment KW - DNA KW - DNA radiation damage KW - Direct damage KW - Dissociative electron attachment (DEA) KW - Dissociative electron transfer (DET) KW - Dosimetry KW - Double-strand break (DSB) KW - ESCA KW - Energy deposit KW - Geant4 KW - Geant4-DNA KW - Hydrated DNA KW - Hydrated electron KW - Hydrated electrons KW - Hydration shell KW - Hydroxyl radical KW - Indirect damage KW - Ionisation KW - Ionization KW - LEE KW - DEA KW - DET KW - Low energy electrons KW - MCS KW - Microdosimetry KW - NAP-XPS KW - Near ambient pressure xray photo electron spectroscopy KW - Net-ionization reaction KW - OH radical KW - PES KW - Particle scattering KW - Prehydrated electron KW - Presolvated electron KW - Protein KW - Quasi-direct damage KW - ROS KW - Radiation damage KW - Radiation therapy KW - Radical KW - Radiolysis KW - Radiotherapy KW - Reactive oxygen species KW - Simulation KW - Single-strand break (SSB) KW - Single-stranded DNA-binding proteins KW - TOPAS KW - TOPAS-nbio KW - XPS KW - Xray photo electron spectrocopy PY - 2023 AN - OPUS4-57782 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - BP153: The change of DNA radiation damage upon hydration: In-situ observation by near-ambient pressure XPS N2 - Ionizing radiation damage to DNA plays a fundamental role in cancer therapy. X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. The results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further. T2 - DPG Frühjahrstagung CY - Dresden, Germany DA - 26.03.2023 KW - Base damage KW - Base loss KW - Cancer treatment KW - DNA KW - DNA radiation damage KW - Direct damage KW - Dissociative electron attachment (DEA) KW - Dissociative electron transfer (DET) KW - Dosimetry KW - Double-strand break (DSB) KW - Energy deposit KW - Geant4 KW - Geant4-DNA KW - Hydrated DNA KW - Hydrated electron KW - Hydration shell KW - Hydroxyl radical KW - Indirect damage KW - Ionization KW - LEE KW - Low energy electrons KW - MCS KW - Microdosimetry KW - NAP-XPS KW - Near ambient pressure xray photo electron spectroscopy KW - Net-ionization reaction KW - OH radical KW - PES KW - Prehydrated electron KW - Quasi-direct damage KW - ROS KW - Radiation damage KW - Radiation therapy KW - Radical KW - Radiolysis KW - Radiotherapy KW - Reactive oxygen species KW - Simulation KW - Single-strand break (SSB) KW - TOPAS KW - TOPAS-nbio KW - XPS KW - Xray KW - Xray photo electron spectrocopy KW - Particle scattering KW - Presolvated electron KW - ESCA PY - 2023 AN - OPUS4-57255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Near-ambient-pressure XPS as as tool to monitor DNA radiation damage directly in water N2 - Ionizing radiation damage to DNA plays a fundamental role in cancer therapy. X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. The results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further. T2 - Miller Conference CY - Furiani, France DA - 03.06.2023 KW - Base damage KW - Base loss KW - Cancer treatment KW - DNA KW - DNA radiation damage KW - Direct damage KW - Dissociative electron attachment (DEA) KW - Dissociative electron transfer (DET) KW - Dosimetry KW - Double-strand break (DSB) KW - ESCA KW - Energy deposit KW - G5P KW - Geant4 KW - Geant4-DNA KW - Hydrated DNA KW - Hydrated electron KW - Hydroxyl radical KW - Indirect damage KW - Ionisation KW - Ionization KW - LEE KW - Low energy electrons KW - MCS KW - Microdosimetry KW - NAP-XPS KW - Near ambient pressure xray photo electron spectroscopy KW - Net-ionization reaction KW - OH radical KW - PES KW - Particle scattering KW - Prehydrated electron KW - Presolvated electron KW - Protein KW - Quasi-direct damage KW - ROS KW - Radiation damage KW - Radiation therapy KW - Radical KW - Radiolysis KW - Radiotherapy KW - Reactive oxygen species KW - Simulation KW - Single-strand break (SSB) KW - Single-stranded DNA-binding proteins KW - TOPAS KW - TOPAS-nbio KW - XPS KW - Xray KW - Xray photo electron spectrocopy KW - Hydration shell PY - 2023 AN - OPUS4-57646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - The change of DNA AND PROTEIN radiation damage upon hydration: In-situ observations by near-ambient-pressure XPS N2 - X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. Our results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further. T2 - Dyson Conference 2023 CY - Prague, Czech Republic DA - 24.04.2023 KW - Base damage KW - Base loss KW - Cancer treatment KW - DNA KW - DNA radiation damage KW - Direct damage KW - Dissociative electron attachment (DEA) KW - Dissociative electron transfer (DET) KW - Dosimetry KW - Double-strand break (DSB) KW - ESCA KW - Energy deposit KW - Geant4 KW - Geant4-DNA KW - Hydrated DNA KW - Hydrated electron KW - Hydration shell KW - Hydroxyl radical KW - Indirect damage KW - Ionization KW - Ionisation KW - LEE KW - Low energy electrons KW - MCS KW - Microdosimetry KW - NAP-XPS KW - Near ambient pressure xray photo electron spectroscopy KW - Net-ionization reaction KW - OH radical KW - PES KW - Particle scattering KW - Prehydrated electron KW - Presolvated electron KW - Quasi-direct damage KW - ROS KW - Radiation damage KW - Radiation therapy KW - Radical KW - Radiolysis KW - Radiotherapy KW - Reactive oxygen species KW - Simulation KW - Single-strand break (SSB) KW - TOPAS KW - TOPAS-nbio KW - XPS KW - Xray KW - Xray photo electron spectrocopy KW - G5P KW - Protein KW - Single-stranded DNA-binding proteins PY - 2023 AN - OPUS4-57406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hallier, Dorothea C. T1 - An XPS study on X-ray radiation damage: Chemical changes to Gene-V Protein of Bacteriophage M13 N2 - X-ray photoelectron spectroscopy (XPS) is used to analyze the direct damage of ionizing radiation to a single-stranded DNA binding protein: Gene-V Protein (G5P). T2 - Science Day Uni Potsdam Institut für Biochemie und Biologie CY - Potsdam, Germany DA - 11.10.2022 KW - XPS KW - Radiaton damage KW - G5P GVP KW - Single-stranded DNA-binding protein KW - X-ray KW - DNA PY - 2022 AN - OPUS4-56541 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - The change of DNA radiation damage upon hydration: In-situ observations by near-ambient-pressure XPS N2 - Ionizing radiation damage to DNA plays a fundamental role in cancer therapy. X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. The results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further. T2 - #RSCposter 2023 CY - Online meeting DA - 28.02.2023 KW - Cancer treatment KW - DNA KW - Dosimetry KW - Energy deposit KW - Geant4 KW - Geant4-DNA KW - TOPAS KW - TOPAS-nbio KW - particle scattering KW - Simulation KW - Radiolysis KW - Radiation therapy KW - Radiotherapy KW - LEE KW - Low energy electrons KW - MCS KW - Base damage KW - Base loss KW - DNA radiation damage KW - Direct damage KW - Dissociative electron transfer (DET) KW - Dissociative electron attachment (DEA) KW - Double-strand break (DSB) KW - Hydrated DNA KW - Hydrated electron KW - Ionization KW - Hydration shell KW - Hydroxyl radical KW - Indirect damage KW - Microdosimetry KW - NAP-XPS KW - Near ambient pressure xray photo electron spectroscopy KW - Net-ionization reaction KW - OH radical KW - PES KW - Prehydrated electron KW - Quasi-direct damage KW - Radiation damage KW - Radical KW - Reactive oxygen species KW - ROS KW - Single-strand break (SSB) KW - XPS KW - Xray KW - Xray photo electron spectrocopy KW - presolvated electron PY - 2023 UR - https://www.nature.com/articles/s42004-021-00487-1 AN - OPUS4-57063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Hahn, Oliver A1 - Denker, A. A1 - Merchel, S. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Wolff, T. ED - Armbruster, B. ED - Eilbracht, H. ED - Hahn, Oliver ED - Heinrich-Tamaska, O. T1 - Zerstörungsfreie Analyse von Metallartefakten - Eine Fallstudie N2 - Die naturwissenschaftliche Analyse historischer Materialen ermöglicht die Beantwortung kulturhistorischer Fragestellungen, die mit kunsthistorischen oder archäologischen Ansätzen allein nicht zu leisten sind. In dieser Studie wurden sechs römische Münzen mit unterschiedlich stark ausgeprägten Korrosionsschichten an unbehandelten und polierten Stellen mit vier zerstörungsfreien analytischen Methoden untersucht: Hoch- und Niederenergie Protonen Induzierter Röntgenemission (HE-/PIXE), Synchrotronstrahlungsinduzierte-Röntgenfluoreszenzanalyse (SY-RFA) und Mikro-Röntgenfluoreszenzanalyse (Mikro-RFA) mit einem mobilen Gerät. Aufgrund von Unterschieden in den Messbedingungen und dem Einfluss der Patina-Schichten auf diese ergaben sich nur für wenige Elemente Übereinstimmungen in den quantitativen Daten. Zur Validierung zukünftiger Messkampagnen mit verschiedenen Methoden sind daher Vergleichstudien unerlässlich. N2 - Investigations of physical properties and chemical composition of ancient materials generate important data for answering culture-historical questions that cannot be solved by art historical and archaeological methods alone. This contribution reports on the analysis of six Roman coins, with different degrees of corrosion layers in parts that were not handled or polished, using four non-destructive methods: low-energy particle-induced X-ray emission (PIXE, 2 MeV), high-energy PIXE (68 MeV), μ-X-ray fluorescence (XRF) spectrometry with a portable device and synchrotron-radiation induced XRF. Because of differences in the conditions needed for measurement and the influence of the layers of patina on these measurements, there were few elements where the quantitative data were in agreement. Thus comparative analyses are essential to validate future measurement projects using different methods. KW - Zerstörungsfreie Prüfung KW - Protoneninduzierte Röntgenemission KW - Röntgenfluoreszenzanalyse KW - Non-destructive testing KW - Particle-induced X-ray emission KW - X-ray fluorescence analysis PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-385702 SN - 978-3-9816751-5-3 VL - Berlin studies of the ancient world, Band 35 SP - 117 EP - 137 PB - Edition Topoi CY - Berlin AN - OPUS4-38570 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nöller, R. A1 - Hahn, Oliver T1 - Illuminated manuscripts from Turfan - Tracing Silk Road glamour by analyzing pigments N2 - Investigation of manuscripts found in sites along the Silk Road shows the history of communication and exchange between Asia and the Mediterranean over the centuries. Different scripts and languages preserved on paper in certain styles provide information about traditions and provenance. To get an idea of the cultural background of the highly developed painting techniques obvious in some illuminated manuscripts, the material used for writing and painting is analyzed. Singular Sogdian and Tocharian manuscripts from Turfan show text on one side with a colorful painting on the other side of the document. In comparison with other productions of different periods or usages from the site, special features are worked out to characterize cultural roots or influence in the network of relationships. Details analyzed in the most elaborated documents Show various influences led to the colorful masterpieces. KW - Pigments KW - X-ray fluorescence analysis KW - Archaeometry PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-391654 DO - https://doi.org/10.1080/20548923.2015.1133120 SN - 2054-8923 VL - 1 IS - 2 SP - 50 EP - 59 PB - Routledge, Taylor & Francis Group AN - OPUS4-39165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF ED - Hahn, Oliver ED - Doil, Thorsten T1 - Workshop Kulturguterhaltung - Vom Dampfkessel zu Nanomaterialien N2 - Sehr geehrte Damen und Herren, liebe Leserinnen und Leser, bereits im ersten Band der N.i.Ke. Schriftenreihe des Netzwerks zur interdisziplinären Kulturerhaltung hatte ich angeführt, dass bei der Untersuchung von kulturellen Artefakten naturwissenschaftliche Untersuchungsmethoden zunehmend an Bedeutung gewinnen, sie eigentlich unverzichtbar geworden sind. Ein besonders einprägsames Beispiel dieser fächerübergreifenden Zusammenarbeit zwischen Geisteswissenschaften, Naturwissenschaften und Restaurierungswissenschaften war die Ausstellung Johannes Vermeer. Vom Innehalten, die in diesem Jahr in der Gemäldegalerie Alter Meister in den staatlichen Kunstsammlungen Dresden gezeigt wurde. Eigens für diese Ausstellung wurde das Gemälde Brieflesendes Mädchen am offenen Fenster einer grundlegenden Restaurierung unterzogen. Diese Restaurierung diente jedoch nicht nur der Reparatur des Bildes. Um sich dem ursprünglichen Zustand des Gemäldes zwischen 1657 und 1659 anzunähern, wurden später hinzugefügte Malschichten großflächig abgenommen. Möglich wurde dies durch unterschiedliche, bildgebende materialwissenschaftliche Untersuchungen im Vorfeld, welche die wissenschaftlichen Grundlagen für die Diskussion über den weiteren Umgang mit der Lesenden schufen. Materialanalytische Verfahren wurden und werden ständig weiterentwickelt und optimiert. Sei es, um aus einer Vielzahl von Einzelmessungen ein Gesamtbild zu erstellen, oder die Größe einer Probenentnahme so zu reduzieren, dass von einer „minimal-invasiven“ oder „quasi nicht-invasiven“ Untersuchung ausgegangen werden kann. Nun feiert die Bundesanstalt für Materialforschung und -prüfung, zusammen mit ihren Vorgängerinstitutionen, den königlichen Versuchsanstalten, in diesem Jahr ihren einhundertfünfzigsten Geburtstag. Sie blickt damit auf eine lange Tradition materialwissenschaftlicher Analysen zurück, an deren Beginn beispielsweise die metallographischen Untersuchungen von Adolf Martens stehen. Derartige Untersuchungen bilden auch heute noch einen wesentlichen Bestandteil archäometallurgischer Forschung. Die Historie bzw. die Weiterentwicklung der Methodik lässt sich hier besonders gut nachzeichnen. Jedoch blicken auch Verfahren zur Charakterisierung weiterer Werkstoffe, wie Glas, Keramik, oder organischer Materialien auf eine lange Geschichte zurück. Die in diesem Band der N.i.Ke.-Schriftenreihe präsentierten Beiträge dokumentieren einerseits aktuelle Forschungsarbeiten, die erst in diesem Jahr in entsprechenden Fachjournalen publiziert wurden, andererseits liegen einige der Arbeiten bereits 50 Jahre zurück. Sie bekunden damit nicht nur die materialtechnologische und historische Bandbreite der Projekte, sondern offenbaren die Vielfältigkeit kulturhistorischer oder restauratorischer Fragestellungen, zu deren Beantwortung natur- und materialwissenschaftliche Forschung wesentliche Beiträge liefern können. Ich bedanke mich bei allen Kolleginnen und Kollegen, die zur Erstellung dieser dritten Ausgabe der N.i.Ke. Schriftenreihe des Netzwerks zur interdisziplinären Kulturerhaltung beigetragen haben. Ihre Aufsätze ermöglichen den Blick in die Vielfältigkeit materialwissenschaftlicher Untersuchungen im Bereich Kunst- und Kulturgut. Ich wünsche Ihnen viel Spaß auf dieser kleinen Zeitreise. T2 - Workshop Kulturguterhaltung - Vom Dampfkessel zu Nanomaterialien CY - Berlin, Germany DA - 17.11.2021 KW - Pergamonmuseums KW - Schriftrollen vom Toten Meer KW - Gold mit Synchrotronstrahlung KW - Kandelaber des Ensembles am Charlottenburger Tor KW - Berliner Tuffsteinfassaden KW - Betondickglasfenster des Glockenturms am Eiermannbau KW - Kaiser-Wilhelm-Gedächtniskirche KW - Radiografische Untersuchung PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543239 UR - https://netzwerke.bam.de/Netzwerke/Navigation/DE/Netzwerke/NIKE/nike.html VL - 3 SP - 1 EP - 155 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-54323 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Steger, Simon A1 - Oesterle, D. A1 - Bretz, S. A1 - Frenzel, L. A1 - Stege, H. A1 - Winkelmeyer, I. A1 - Hahn, Oliver A1 - Geiger, G. T1 - Kandinsky’s fragile art: a multidisciplinary investigation of four early reverse glass paintings (1911–1914) by Wassily Kandinsky N2 - This work highlights the rediscovery of the technique of reverse glass painting by the artists of the “Blaue Reiter” collective in the early 20th-century and focusses particularly on the role of Wassily Kandinsky (1866–1944). Kandinsky created more than 70 reverse paintings on glass and showed several of them in exhibitions together with paintings on canvas and cardboard, implying a coequal importance of these techniques. Four of his early (1911–1914) reverse glass paintings (Auferstehung, Allerheiligen II, Rudern, Apokalyptischer Reiter II) were selected for investigation and their iconography, painting techniques and painting materials were examined. Two paintings were executed on so-called cathedral glass, revealing a “hammered surface”, whereas Kandinsky used a corrugated glass panel for Rudern. A multi-analytical, non-invasive approach [X-ray fluorescence (XRF), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), VIS spectroscopy (VIS), Raman spectroscopy] was taken to identify the pigments and classify the binding media. The results reveal a broad palette of materials. Several pigments like lead white, zinc white, Strontium yellow, Prussian blue, viridian, cadmium yellow, ultramarine blue, cinnabar and carbon black were found in most of the four paintings. The use of the rare synthetic organic pigments PR60 and PB52 is discussed. In two works of art, cadmium carbonate is associated with cadmium yellow. The identification of aluminium foil along with tin foils in Rudern indicates an early use of this material for reverse glass paintings. KW - Reverse glass painting KW - Non-invasive analysis KW - Raman spectroscopy KW - DRIFTS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480075 DO - https://doi.org/10.1186/s40494-019-0268-8 VL - 7 IS - 27 SP - 1 EP - 17 PB - Springer AN - OPUS4-48007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nöller, Renate A1 - Danielewski, A. A1 - Giel, R. A1 - Overgaauw, E. A1 - Hahn, Oliver T1 - Material analysis of Aztec codices in Berlin. Assignment of small fragments compiled as cutouts on one plate in Humboldt’s “Atlas pittoresque du voyage” N2 - The collection Manuscripta Americana in Berlin consists of fragmented codices acquired by Alexander von Humboldt in Mexico. Some of these Humboldt Codices are published as hieroglyphic writings of the Aztecs in “Vues des Cordilleres et Monuments des Peuples indigènes de l’Amerique”. Starting from a special compilation of seven fragments on plate 36 in the “Atlas”, we investigated the corresponding original fragments using material analysis in order to clarify their historical relations. The analyses were carried out with X-ray fluorescence analysis, VIS spectroscopy, and infrared spectroscopy in diffuse reflection and revealed typical indigenous colors like cochineal, indigo, and organic yellows (e.g. mangrove and zacatlaxcalli). Four fragments under investigation show exactly the same material and thus must once have belonged together in one compendium. An additional manuscript from Mizquiahuala also shown on plate 36 can be matched to another one that is not published in the “Atlas”. KW - Manuscripts KW - Alexander von Humboldt KW - Non-destructiv testing KW - Colourants KW - Writing materials PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-498971 DO - https://doi.org/10.1080/20548923.2019.1682816 SN - 2054-8923 SP - 1 EP - 14 PB - Routledge, Taylor & Francis Group CY - London AN - OPUS4-49897 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Hahn, Oliver A1 - Golle, U. A1 - Wintermann, Carsten A1 - Laurenza, D. ED - Quenzer, J. B. T1 - Scientific Analysis of Leonardo’s Manuscript with Anatomic Drawings and Notes N2 - In this paper, we discuss the importance of scientifically investigating cultural artefacts in a non-invasive way. Taking as test case Leonardo da Vinci’s Manuscript with anatomic drawings and notes, which is stored in Weimar, we clarify fundamental steps in the chronology of this folio. By means of microscopy, infrared reflectography, UV photography, and X-ray fluorescence analysis, we were able to identify various types of sketching material and several varieties of iron gall ink. For his sketches, Leonardo used two different sketching tools, a lead pencil and a graphite pencil, as well as several types of ink for developing these sketches into drawings. With regard to ink, it is important to observe that there is no difference between the ink Leonardo used for drawing and the ink he used for writing text. Based on the materials analysed, we suggest a chronology for the creation of this unique folio. KW - Archaeometry KW - Non-invasive analysis KW - Drawings KW - Leonardo da Vinci PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543460 SN - 978-3-11-074545-0 DO - https://doi.org/10.1515/9783110753301-011 VL - 25 SP - 213 EP - 228 PB - Walter de Gruyter GmbH CY - Berlin/Boston AN - OPUS4-54346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nöller, Renate A1 - Hahn, Oliver A1 - Overgaauw, E. A1 - Danielewski, A. A1 - Giel, R. T1 - Analyse von Humboldt Codices aus Mizquiahuala im Vergleich zu Fragmenten in Mexiko und Paris N2 - Unter den von Humboldt in Amerika erworbenen Schriftstücken der Kolonialzeit findet sich eine Tributliste aus dem Jahr 1569, die der Otomí Bevölkerung aus dem Ort Mizquahuala im Staat Hidalgo/ Mexiko zugeordnet wird. Sie ist in Form eines Kalenders ausgeführt, Wochentage und verschiedene Produkte lassen sich unterscheiden. Eduard Seler beschreibt dieses Manuskript zusammen mit einer weiteren Tributliste, die in Inhalt und Zeichnung anders gestaltet ist, jedoch ebenfalls aus dieser Region stammt. Mit den für die Analyse von Manuskripten bewährten Untersuchungsmethoden werden Papier und Farbmittel identifiziert. Hierzu zählen Raman-, FTIR-, Röntgenfluoreszenz- und VIS- Spektroskopie. Charakteristisch für die Herstellung von schriftlichen Dokumenten in der Kolonialzeit von Amerika ist die Verwendung von indigenem Material wie Papier aus Baumrinde und Pflanzenfarben zusammen mit den aus Europa bekannten Materialien. Geklärt wird, welche Auswahl von Farbstoffen zur Herstellung der Dokumente genutzt wurde, die diese als Gruppe klassifizieren könnte. Die den beiden Fragmenten zugeordneten Farbmaterialien sowie formale und inhaltliche Aspekte lassen vermuten, dass zwei weitere Schriftstücke der Berliner Sammlung `Manuscripta Americana´, deren Herkunft nicht bekannt ist, mit ihnen in Beziehung gebracht werden können. Stilistisch gleiche Fragmente befinden sich zudem in Mexiko, Paris und den USA. Im Vergleich dieser Fragmente untereinander wird diskutiert, inwieweit die über die Materialanalyse identifizierten spezifischen Farbstoffe einen Hinweis auf eine gemeinsame lokale Herkunft zulassen. T2 - Jahrestagung Archäometrie und Denkmalpflege CY - Wien, Austria DA - 11.09.2019 KW - VIS- Spektroskopie KW - Humboldt Codices KW - RFA PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-499192 SN - 0947-6229 VL - Sonderheft 9 SP - 186 EP - 189 CY - Bochum AN - OPUS4-49919 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Dietz, G. A1 - Eggert, Claudia A1 - Golle, U. A1 - Hahn, Oliver A1 - Ketelsen, T. A1 - Ludwig, A. A1 - Melzer, C. A1 - Rabin, Ira A1 - Wintermann, C. ED - Hahn, Oliver ED - Doil, Thorsten ED - Wintermann, C. T1 - Die Materialität der Zeichnung - Eine naturwissenschaftliche Annäherung N2 - Der Band 5 der N.i.Ke.-Schriftenreihe präsentiert den aktuellen Stand materialwissenschaftlicher und bildgebender Verfahren, die bei der Untersuchung von Zeichnungen Anwendung finden. Im ersten Teil der Publikation werden die klassischen Zeichnungsträger und Zeichnungsmaterialien vorgestellt. Der mittlere Teil der Publikation beschreibt die relevanten materialwissenschaftlichen und bildgebenden Verfahren. Der letzte Teil diskutiert anhand einiger Fallbeispiele die Möglichkeiten und Grenzen der Methoden. KW - Archäometrie KW - Zeichnungen KW - Zerstörungsfreie Prüfung KW - Papier KW - Pergament KW - Zeichenmaterialien PY - 2024 SN - 2567-1251 N1 - Es gibt eine parallele Sprachausgabe (englisch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (English), a link is in the field related identifier VL - 5 SP - VII EP - 111 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-60751 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Hahn, Oliver ED - Doil, Thorsten T1 - Der Bestand der Rembrandt-Zeichnungen in der Klassik Stiftung Weimar - Kritischer Katalog und materialtechnischer Befund N2 - Mit dem aktuellen Band 6 der N.i.Ke.-Schriftenreihe erscheint der kritische Katalog aller Rembrandt-Zeichnungen in der Klassik Stiftung Weimar. Im Unterschied zu vielen anderen Graphischen Kabinetten, die ihre Rembrandt-Bestände bereits erfolgreich publiziert haben, existierte eine solche Gesamtschau in Weimar bisher nicht. Die nun vorliegende Publikation mit 51 Katalognummern umfasst alle, aktuell Rembrandt zugeschriebenen Blätter, alle rembrandtesken Zeichnungen, die ehemals als Werk Rembrandts angesehen wurden, aber auch alle Zeichnungen, die einmal mit Rembrandt und seiner Schule in Verbindung gebracht wurden. Der Titel "Der Bestand der Rembrandt-Zeichnungen in der Klassik Stiftung Weimar - Kritischer Katalog und materialtechnischer Befund" macht deutlich, dass hier neue Wege beschritten wurden. Auch diese Publikation basiert auf Quellen der klassischen Kunstgeschichte, wie etwa bestehende Werkverzeichnisse. Die Befunde werden jedoch mit materialwissenschaftlichen Erkenntnissen erheblich erweitert. Jedes der hier besprochenen Blätter wurde verschiedenen naturwissenschaftlichen Untersuchungen unterzogen, um die Materialität jeder Zeichnung in ihrer Gesamtheit zu bestimmen. Es wird der Versuch unternommen, die Materialität mit der klassischen Stilkritik zu verzahnen, um neue Hinweise auf die Genese, den Gebrauch oder die Funktion der Zeichnung zu erhalten. Nicht jedes naturwissenschaftliche Ergebnis findet sich im Katalogteil, aber alle Hinweise, die zum Verständnis der Materialität der Zeichnung unmittelbar notwendig sind, werden zitiert. T2 - Rembrandt in Weimar - Ein Beitrag zur Neujustierung der Kennerschaft CY - Weimar, Germany DA - 20.03.2025 KW - Rembrandt KW - Zeichnung KW - Katalog KW - Materialität PY - 2025 SN - 2567-1251 VL - 6 SP - 1 EP - 242 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-63538 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Dietz, G. A1 - Eggert, Claudia A1 - Golle, U. A1 - Hahn, Oliver A1 - Ketelsen, T. A1 - Ludwig, A. A1 - Melzer, C. A1 - Rabin, Ira A1 - Wintermann, C. ED - Hahn, Oliver ED - Doil, Thorsten ED - Wintermann, C. T1 - The materiality of drawings - A scientific approach N2 - Volume 5 of the N.i.Ke. series presents the current state of materials science and imaging techniques used in the examination of drawings. The first part of the publication introduces the classic drawing substrates and materials. The middle part of the publication describes the relevant materials science and imaging techniques. The final part discusses the possibilities and limitations of these methods using several case studies. KW - Archaeometry KW - Paper KW - Parchment KW - Drawing materials KW - Drawings KW - Nondestructive testing PY - 2024 SN - 2567-1251 N1 - Es gibt eine parallele Sprachausgabe (deutsch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (German), a link is in the field related identifier VL - 5 SP - VII EP - 110 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-63672 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Determining thickness and completeness of the shell for polymer core shell nanoparticles by XPS, ToF SIMS and T SEM N2 - Core-shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core-shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a non-ideal morphology. In this work, we investigated PTFE-PMMA (four samples) and PTFE-PS (six samples) polymer CSNPs with constant core diameter (45 nm) but varying shell thickness (4-50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE-PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE-PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA V2.0 was used to analyze the intensities of the elastic peaks and the QUASES software package to evaluate the shape of the inelastic background in the XPS Survey spectra. For the first time, nanoparticle shell thicknesses are presented which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA) assisted time-of-flight secondary ion mass spectrometry (ToF-SIMS) of the PTFE-PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. Opposed to that, no variation is observed in the PCA scores plots of the PTFE-PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM. T2 - 18th European Conference on Applications of Surface and Interface Analysis (ECASIA) CY - Dresden, Germany DA - 15.09.2019 KW - Core-shell nanoparticles KW - Polymers KW - ToF-SIMS KW - XPS KW - XPS background analysis PY - 2019 AN - OPUS4-49187 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Improved estimation of the transmission function with UNIFIT 2022 N2 - The recent development of x-ray photoelectron spectroscopy using excitation sources different from the usual lab-source Mg Kα and Al Kα and spectrometers with more sophisticated lens systems requires flexible approaches for determining the transmission function. Therefore, the approach using quantified peak areas (QPA) was refined.1 A new algorithm allows a more precise estimation of the transmission function which could be shown by comparing the results obtained with the new version with former calculations. Furthermore, next to the established reference materials Cu, Ag and Au, ionic liquids can be used for estimating the transmission function at beamlines with variable excitation energies. Comparison between the measured and stoichiometric composition shows that a transmission function was determined which allows a reasonable quantification. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - X-ray photoelectron spectroscopy KW - Transmission function KW - Synchrotron radiation KW - Iionic liquid PY - 2022 AN - OPUS4-54962 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinelt, Manuel T1 - Feasibility Study on the Direct Detection of Per- and Polyfluoroalkyl Substances (PFAS) with Surface-Assisted Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (SA-FAPA-MS) N2 - Per- and polyfluoroalkyl substances (PFAS) are a large class of thousands of synthetic chemicals that are used worldwide. However, growing environmental and human health concerns in the last two decades have led to more stringent regulatory requirements and the development of quantitative analytical methods for PFAS detection. Today, standardized and powerful methods exist, e.g., for the determination of PFAS in water, sludge, compost, soil, and drinking water (DIN 38407-42, DIN 38414-14, ISO 21675, and DIN EN 17892). While liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) is often used, blank levels, sample preparation, and total analysis times can be challenging. [1] Here, ambient desorption/ionization mass spectrometry (ADI-MS) is considered interesting because it requires only minimal sample preparation and was able to reduce total analysis time in other types of applications. [2] Previously, we used a plasma-based pin-to-capillary flowing atmospheric-pressure afterglow source (FAPA) [3] to probe samples directly from thin-layer chromatography (TLC) plates and to perform quantitative analysis and mass spectral imaging [4]. In this work, a feasibility study for the direct detection of PFAS with FAPA-MS is reported. Selected PFAS samples were directly probed on functionalized TLC surfaces (normal-phase silica, reversed-phase-modified silica, cyano [CN]-modified silica, and dimethyl [RP2]-modified silica, diol modified silica, and amino [NH2]-modified silica). The suitability of the surfaces was evaluated and the compatibility of different solvents with the surfaces was studied. CN-HPTLC and RP2-TLC surfaces showed the best performance for direct PFAS detection with FAPA-MS. In addition, direct analysis of PFAS mixtures and selected matrices was performed with little sample preparation and short analysis time. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Mass Spectrometry KW - FAPA-MS KW - Instrumentation KW - PFAS KW - Surface Analysis PY - 2025 AN - OPUS4-63605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Reliable chemical characterization of industrial graphene related materials N2 - International standards describing reliable protocols will facilitate the commercialization of graphene and related 2D materials. One physico-chemical key property next to flake size and thickness is the chemical composition of the material. Therefore, an ISO standard is under development with X-ray photoelectron spectroscopy having a prominent role. With its information depth of around 10 nm which is the similar length scale as the thickness as of particles of 2D materials consisting of a few monolayer XPS seems to be highly suitable for this purpose. Different sample preparation methods like pressing the powders onto adhesive tapes, into recesses, or into solid pellets result in inconsistencies in the quantification. For the validation of the quantification with XPS an interlaboratory comparison was initiated under the auspice of the “Versailles Project on Advanced Materials and Standards” (VAMAS). First results confirm that the sample preparation method (pellet vs. powder) influences the quantification results clearly. Considering this effect, a good agreement of the results from the different participants were observed. Similar results were observed for raw, N- and F-functionalized graphene. T2 - Graphene CY - Manchester, England, UK DA - 27.06.2023 KW - X-ray photoelectron spectroscopy KW - Functionalized graphene KW - Interlaboratory comparison KW - VAMAS PY - 2023 AN - OPUS4-57895 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pelkner, Matthias A1 - Casperson, Ralf A1 - Pohl, Rainer A1 - Munzke, Dorit A1 - Becker, Ben T1 - Eddy current testing of composite pressure vessels N2 - The application of composite pressure vessels is of great interest due to tremendous weight saving. Nevertheless, ageing of CFRP (carbon fiber reinforced plastic) composites pressure vessels underlies complex interactions between metallic liner and composite and is not fully understood yet. One main challenge is the application of appropriate testing methods for detecting the influences of pressure cycles and creep behavior on the material. This contribution presents results achieved by using conventional eddy current testing (ET) and high frequency ET. Here, we could show that also conventional ET with low frequencies are useable to investigate pressure vessels of different material combinations like aluminum-CFRP and synthetics-CFRP. KW - CFRP KW - Eddy current KW - Ageing KW - Composite PY - 2019 DO - https://doi.org/10.3233/JAE-171044 VL - 59 IS - 4 SP - 1221 EP - 1226 PB - IOP Publ. Ltd. AN - OPUS4-47803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nymark, P. T1 - Grouping of representative nanomaterials is efficiently executed by combining high-throughput-generated biological data with physicochemical data N2 - Grouping of nanomaterials (NM) promises to serve effectively to reduce the extensive safety testing needs associated with regulatory risk assessment. Key challenges in this task are how to rapidly and cost-efficiently generate the needed data, and how to best combine structural material characteristics with biological effects data. Herein, we performed NM grouping from combining existing physiochemical data with high-throughput screening (HTS)-derived hazard assessment data generated in the human lung epithelial cell line BEAS-2B. Twenty-one NMs from the European Joint Research Centre´s Representative Nanomaterials Repository (diverse nanoforms of substances ZnO, SiO2 and TiO2) and five reference chemicals were analyzed by HTS assays for cytotoxicity/cell viability (CellTiterGlo, Dapi-staining), oxidative stress (8-OHdG), apoptosis (Caspase-3), and DNA damage repair (γH2AX). Additionally, physicochemical data relevant for grouping of NMs under REACH (ECHA, 2017 Appendix R.6-1) were collated for 15 of the NMs, including from EU-funded projects (NanoReg2, caLIBRAte) and the OECD Testing Programme of Nanomaterials. The diverse data types were scaled, normalized and integrated using a newly developed scoring pipeline inspired by the US-EPA Toxicological Prioritization Index (ToxPi). Results demonstrated that the in vitro-derived hazard data permitted substance-based grouping of the selected NMs, whereas integration of physicochemical data deepened the grouping of specific nanoforms within each substance group. Furthermore, a case study on 10 TiO2 NMs showed that hazard-based grouping allowed for read across of physicochemical data between 6 NMs acting as source nanoforms and 4 NMs acting as target nanoforms. The ToxPi tool and scoring pipeline permitted transparent visualization of the final grouping, while giving equal weight to different types of data/results related to structure and biology. Overall, this study aligns fully with the ECHA recommendations for grouping of NM (Appendix R.6-1), i.e. i) to aim at identification of criteria for grouping nanoforms (and non-nanoforms) within one substance, and ii) to provide additional information beyond physicochemical data to support read across between nanoforms. T2 - Eurotox 2019 CY - Helsinki, Finland DA - 08.09.2019 KW - Grouping KW - Nanomaterials KW - Regulatory risk assesment KW - High-throughput screening PY - 2019 AN - OPUS4-49439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer T1 - Direct comparison of two pyrometers and a low-cost thermographic camera for time resolved LWIR temperature measurements N2 - The contactless measurement of temperatures with pyrometers is state of the art and a number of different commercial devices are available. Alternatively, these temperature measurements can be performed by means of infrared cameras. In light of permanently falling costs, the application of IR cameras simply as contactless thermometers appears to be an alternative to the use of pyrometers. For a current study, the surface temperature development of a sample has to be measured and recorded with at least 20 Hz sampling rate in a temperature range between 0°C and 70°C and with a temperature resolution of 0.1 K. The absolute value of the temperature is not as important as relative changes. Due to disturbing irradiation in the SWIR and MWIR regions, the sensor should work in the LWIR. We compared two pyrometers and a low-cost infrared camera with regard to the requirements defined above. In this paper we describe the setup, the results and the data evaluation. Both, raw data and post processed data, were considered. Surprisingly, the infrared camera had by far the best performance of the considered devices. Particularly, due to the large number of pixel (160 x 120), the S/N could be reduced considerably compared to the pyrometers. We also studied the stability of the frame rate and the related time steps of the IR camera. Although the frame rate is unstable (running under Windows operating system), the output data for the time steps were found to be correct and the required time resolution was achieved. The application of IR cameras simply as contactless thermometers appears to be an alternative to the use of pyrometers. For a current study, the surface temperature development of a sample has to be measured and recorded with at least 20 Hz sampling rate in a temperature range between 0°C and 70°C and with a temperature resolution of 0.1 K. We compared two pyrometers and a low-cost infrared camera both sensitive in the LWIR only. Surprisingly, the infrared camera had by far the best performance of the considered devices. T2 - Thermosense XXXIX: Thermal Infrared Applications CY - Anaheim, CA, USA DA - 10.04.2017 KW - Contactless temperature measurement KW - Layer thickness KW - Pyrometer KW - Infrared camera PY - 2017 AN - OPUS4-43391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Mente, Tobias A1 - Steppan, E. A1 - Kannengießer, Thomas A1 - Steger, J. T1 - Hydrogen trapping in T24 Cr-Mo-V steel weld joints - microstructure effect vs. experimental influence on activation energy for diffusion N2 - Hydrogen-assisted cracking is a critical combination of local microstructure, mechanical load and hydrogen concentration. Welded microstructures of low-alloyed creep-resistant Cr-Mo-V steels show different hydrogen trapping kinetics. This influences the adsorbed hydrogen concentration as well as the diffusion by moderate or strong trapping. A common approach to describe hydrogen traps is by their activation energy that is necessary to release hydrogen from the trap. In the present study, Cr-Mo-V steel T24 (7CrMoVTiB10-10) base material and TIG weld metal were investigated. Electrochemically hydrogen charged specimens were analyzed by thermal desorption analysis (TDA) with different linear heating rates. The results show two different effects. At first, the microstructure effect on trapping is evident in terms of higher hydrogen concentrations in the weld metal and increased activation energy for hydrogen release. Secondly, it is necessary to monitor the real specimen temperature. A comparison between the adjusted heating rate and the real specimen temperature shows that the calculated activation energy varies by factor two. Thus, the trap character in case of the base material changes to irreversible at decreased temperature. Hence, the effect of the experimental procedure must be considered as well if evaluating TDA results. Finally, realistic temperature assessment is mandatory for calculation of activation energy via TDA. KW - Creep-resistant steel KW - Hydrogen assisted cracking KW - Thermal desorption analysis KW - Welding KW - Microstructure KW - Diffusion PY - 2018 DO - https://doi.org/10.1007/s40194-017-0546-6 SN - 0043-2288 SN - 1878-6669 VL - 62 IS - 2 SP - 277 EP - 287 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-44505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Radnik, Jörg ED - Wandelt, K. T1 - X-ray photoelectron spectroscopy for investigation of heterogeneous catalytic process N2 - Heterogeneous catalysis is a key technology in modern industrial societies. The main steps of a catalytic process take place at the surfaces of complex materials. For the investigations of these surfaces X-ray photoelectron spectroscopy is widely used and fits ideally. At some suitable examples, it will be explained how XPS can help to understand such catalysts better. The focus is on selective oxidation catalysts, one of the main challenges of present research. Here it will illustrate, how changes in the near surface region influence the catalyst performance and, herewith the different stages (activation, maximum performance and deactivation) in the life of catalysts. Additionally, it will be stressed out how important information at different depth regions (surface, near-surface region, bulk) can be useful for comprehensive understanding of the material. Another important subject is nanostructured catalysts with molecular sieves as supports or defined complexes as precursors. Finally, the combination of XPS with other methods used in the analysis of catalysts, e.g. electron microscopy, X-ray absorption spectroscopy and low energy ion scattering will be discussed. KW - X-ray photoelectron spectroscopy KW - Depth information KW - Heterogeneous catalysis KW - Structure-properties relationships PY - 2018 SN - 978-0-12-809739-7 VL - 1 SP - 607 EP - 614 PB - Elsevier AN - OPUS4-44876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Material analysis of manuscripts: methodological introduction N2 - Natural sciences play auxiliary role in the studies of manuscripts. The success of their contribution depends strongly on the formulation of the question and the choice of the methods to obtain the requested answer. Therefore, one should try to go beyond the understanding of the basic principles of the scientific analysis. We will start with a glance at the basic principles of the techniques used in the material science for determination of the elemental composition (X-ray emission) and molecular composition (FTIR & Raman). We will move then to the bench and mobile equipment commonly used in the field of cultural heritage. At the end we will choose a question to be answered and design an ideal experiment that will be modified according to the limitations dictated by on-site conditions. T2 - ManuSciences 17 CY - Fréjus, France DA - 10.09.2017 KW - Mobile instrumentation KW - Manuscripts PY - 2017 AN - OPUS4-43451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Specimen temperature during CGHE and influence on hydrogen determination N2 - Hydrogen determination in weld seams is standardized in ISO 3690. In accordance to this standard, a defined time for hydrogen collection has to be anticipated for different extraction temperatures. In other words, the temperature is the most important value that has to be monitored in addition to the aimed hydrogen determination. The specimen geometry has influence on the real sample temperature during CGHE vs. the adjusted furnace temperature. This presentation gives a short summary on possible influences on the "correct" hydrogen determination temperature during carrier gas hot extraction (CGHE) using infrared radiation driven furnace. The main findings are: (1) specimen surface is important in terms of polished or oxidized condition, (2) specimen geometry is important for fast heating, (3) PID-values of control software are a considerable influence to accelerate the heating process depite thick specimens and (4) independent sample temperature determination before CGHE is strongly recommended. T2 - Intermediate Meeting of IIW Subcommission II-E CY - Genoa, Italy DA - 05.03.2018 KW - Hydrogen KW - Welding KW - Carrier gas hot extraction KW - Temperature KW - Measurement PY - 2018 AN - OPUS4-44427 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Photoelectron spectroscopy N2 - A short introduction into the basics of Photoelectron Spectroscopy with the focus on surface sensitivity and applications is presented. T2 - Industrietreffen im Forschungs- und Innovationszentrum (FIZ) der BMW Group CY - Munich, Germany DA - 09.01.2018 KW - XPS KW - ESCA KW - Surface analytics PY - 2018 AN - OPUS4-43737 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maierhofer, Christiane T1 - Passive and active thermography applied to buildings and cultural heritage - Cracks and protection layers N2 - Artificial and natural cracks have been investigated with active and passive thermography. For the determination of the thickness of protection layers on concrete, an active thermography method has been developed. T2 - Short Courses of the QIRT 2018 Conference CY - Berlin, Germany DA - 25.6.2018 KW - Active themrography KW - Passive thermography KW - Cracks KW - Concrete PY - 2018 AN - OPUS4-45456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cohen, Zina T1 - Cairo Genizah documents of the 11th century: analysis of writing materials N2 - The Cairo Genizah is a well-known “archive” discovered in the 19th century in Ben Ezra Synagogue in Fustat, a district in Old Cairo (Egypt), located south of the center of modern Cairo. The giant collection of mostly Jewish documents that vary in genres, languages and writing supports contains a large number of early medieval Hebrew manuscripts, mostly in fragmentary form. The larger part of the Cairo Genizah is stored today in the Cambridge University Library, containing about 200,000 fragments. The Genizah provides sources for the literary, linguistic, historical studies of the various aspects Jewish and non-Jewish life. As the documents attest, at least two Jewish communities co-existed in Fustat up to 11th century: a so-called Babylonian and Palestinian. These communities had different leaders, different traditions and lived independently. The differences manifest themselves also in the paleographical properties of the manuscripts produced by each community. Although Genizah manuscripts have attracted a great deal of scholarly attention, the material aspects of these documents seem to have been largely neglected. The current study aims to obtain information on the composition of the writing supports and the inks used, in order to obtain insights on trade, local production techniques and social structures. Can we extend the differences detected by the paleographical analysis to differences in composition of the writing materials ? Can we relate the differences in the composition to a community, to the manuscript type (legal, private...), or to another criterion? T2 - Konferenz EAJS CY - Crakow, Poland DA - 14.07.2018 KW - Ink KW - Manuscript KW - XRF analysis PY - 2018 AN - OPUS4-46038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Anja T1 - Progress Talk 3 / Non-destructive depth profiling of core-shell nanoparticles by ER-XPS N2 - This presentation deals with the progress between month twenty and twenty-nine of my PhD thesis. I prepared it, in order to update my supervisor Prof. Kemnitz and my colleagues from the department of chemistry at the Humboldt-Universität zu Berlin (HU). T2 - Working Group Meeting of Prof. Erhard Kemnitz CY - Humboldt-Universität zu Berlin (HU), Germany DA - 20.11.2018 KW - ER-XPS KW - Synchrotron KW - Core-shell nanoparticles KW - Depth-profiling PY - 2018 AN - OPUS4-46676 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mino, L. A1 - Pellegrino, F. A1 - Rades, Steffi A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - Spotto, G. A1 - Maurino, V. A1 - Martra, G. T1 - Beyond shape engineering of TiO2 nanoparticles: Post-synthesis treatment dependence of surface hydration, hydroxylation, Lewis acidity and photocatalytic activity of TiO2 anatase nanoparticles with dominant {001} or {101} facets N2 - TiO2 anatase nanoparticles are among the relevant players in the field of light-responsive semiconductor nanomaterials used to face environmental and energy issues. In particular, shape-engineered TiO2 anatase nanosheets with dominant {001} basal facets gained momentum because of the possibility to exploit different and/or improved functional behaviors with respect to usual bipyramidal TiO2 anatase nanoparticles, mainly exposing {101} facets. Nevertheless, such behavior depends in a significant extent on the physicochemical features of surfaces exposed by nanosheets. They can vary in dependence on the presence or removal degree of capping agents, namely, fluorides, used for shape-engineering, and experimental investigations in this respect are still a few. Here we report on the evolution of interfacial/ surface features of TiO2 anatase nanosheets with dominant {001} facets from pristine nanoparticles fluorinated both in the bulk and at their surface to nanoparticles with F− free surfaces by treatment in a basic solution and to totally F− free nanoparticles by calcination at 873 K. The nanoparticles fluorine content and its subsequent evolution is determined by complementary techniques (ion chromatography, TOF-SIMS, XPS, AES, SEM-EDX), probing different depths. In parallel, the evolution of the electronic properties and the Ti valence state is monitored by UV−vis spectroscopy and XPS. The calcination treatment results in {001} facets poorly hydroxylated, hydrated, and hydrophilic, which appear as surface features consequent to the expected (1 × 4) reconstruction. Moreover, IR spectroscopy of CO adsorbed as probe molecule indicates that the Lewis acidity of Ti4+ sites exposed on (1 × 4) reconstructed {001} facets of calcined TiO2 nanosheets is weaker than that of cationic centers on {101} facets of bipyramidal TiO2 anatase nanoparticles. The samples have also been tested in phenol photodegradation highlighting that differences in surface hydration, hydroxylation, and Lewis acidity between TiO2 nanoparticles with nanosheet (freed by F− by calcination at 873 K) and bipyramidal shape have a strong impact on the photocatalytic activity that is found to be quite limited for the nanoparticles mainly exposing (1 × 4) reconstructed {001} facets. KW - Nanoparticles KW - TiO2 KW - F- doping KW - Shape-controlled nanoparticles KW - Nanosheets PY - 2018 DO - https://doi.org/10.1021/acsanm.8b01477 SN - 2574-0970 VL - 1 IS - 9 SP - 5355 EP - 5365 PB - ACS Publications CY - Washington, DC, U.S.A. AN - OPUS4-46157 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rades, Steffi A1 - Oswald, F. A1 - Narbey, S. A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Analytical approach for characterization of morphology and chemistry of a CH3NH3PbI3/TiO2 solar cell layered system N2 - Manufacturing of new perovskite layered solar cells with constant high light conversion Efficiency over time may be hampered by the loss of efficiency caused by structural and/or chemical alterations of the complex layered system. SEM/EDX combined with XPS were chosen as an appropriate methodical approach to characterize perovskite laboratory cells in depth and at surface, before and after light exposure. The layered perovskite system investigated here is based on glass covered with fluorine doped tin oxide, followed by thin films of TiO2, ZrO2, and a thick monolithic carbon. TiO2 film is subdivided into a dense layer covered by porous one constituted of nanoparticles of truncated bipyramidal shape. This layered system serves as the matrix for the perovskite. EDX spectral maps on cross sections of specimen have shown that Pb and I are distributed homogeneously throughout the porous layers C, ZrO2, and TiO2. SEM/EDX data show that 20 weeks of ambient daylight did not change significantly the in‐depth distribution of the elemental composition of Pb and I throughout the entire solar cell system. It was confirmed with EDX that nanoparticles identified in high‐resolution SEM micrographs contain mainly Pb and I, indicating these to be the perovskite crystals. However, a compositional and chemical altering began in the near‐surface region of the outermost ~10 nm after 2 months of illumination which was observed with XPS. T2 - ECASIA 2017 CY - Montpellier, France DA - 24.09.2017 KW - Solar Cell KW - SEM KW - EDX KW - XPS KW - layered system PY - 2018 DO - https://doi.org/10.1002/sia.6410 SN - 0142-2421 SN - 1096-9918 VL - 50 IS - 11 SP - 1234 EP - 1238 PB - John Wiley & Sons, Ltd. AN - OPUS4-46394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Already producing or still assembling? – Perspectives towards modular production and quality control in a digitized process industry N2 - The CLEAN ENERGY Flagship is an initiative designed to utilize recent game changing developments in digital, materials and manufacturing technologies to catalyze a radical paradigm shift towards clean, reliable, efficient and cost-optimal energy. Unifying and drastically accelerating radically new energy material design, processing and integration across the entire value chain addressing energy production, conversion, storage and systems. CLEAN ENERGY participants are all distinguished research organisations that each benefit from their own industry networks and contacts with regions and state-level activities and have a long history of collaborating with each other (for 10 years now under the umbrella of EERA) within a European collaborative framework. Through EERA, CLEAN ENERGY aims to become a crucial partner in the SET-Plan, supporting long-lasting approaches through its established networks and internal collaborations. T2 - Clean Energy Workshop on Autonomous Materials Development Platforms CY - Brussels, Belgium DA - 02.10.2018 KW - Digitization KW - Energy production KW - Energy storage KW - Energy systems KW - Clean energy technology PY - 2018 AN - OPUS4-46135 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bernegger, Raphael T1 - Numerical 2D model to quantify defects in semitransparent materials by pulsed thermography N2 - Pulsed thermography is a well-known non-destructive testing technique and has proven to be a valuable tool for evaluation of material defects. Material defects are often simulated by flat-bottom holes (FBH) or grooves. Typically, analytical 1D models are used to determine the defect depth of FBHs, grooves or delaminations. However, these models cannot take into account lateral heat flows, or only to a limited extent (semi-empirical model). Their applicability is therefore limited by the FBHs aspect ratio (diameter to remaining wall thickness), to ensure that the heat flow above the defect can still be described one-dimensionally. Additionally, the surfaces of semi-transparent materials have to be blackened to absorb the radiation energy on the surface of the material. Without surface coatings, these models cannot be used for semi-transparent materials. Available 1D analytical models for determination of sample or layer thicknesses also do not take into account lateral heat flows. Here, we present an approach for quantitative determination of the geometry of FBHs or grooves in semi-transparent materials by considering lateral heat flow. For this purpose, the results of a numerical 2D model are fitted to experimental data, e.g., to determine simultaneously the defect depth of a FBH or groove and its diameter or width, respectively. The model considers semi-transparency of the sample within the wavelength range of the excitation source as well as of the IR camera and thermal losses at its surfaces. Heat transport by radiation within the sample is neglected. It supports the use of an arbitrary temporal shape of the heating pulse to properly describe the measurement conditions for different heat sources. T2 - Progress in Photoacoustic & Photothermal Phenomena CY - Erice, Italy DA - 06.09.2018 KW - Pulse thermography KW - Numerical modelling KW - 2D model KW - Data reconstruction KW - Flat bottom holes KW - Notches KW - Semitrasnparent materials PY - 2018 AN - OPUS4-46105 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bernegger, Raphael T1 - Iterative numerical 2D-modeling for quantification of material defects by pulsed thermography N2 - Pulsed thermography is a well-known non-destructive testing technique and has proven to be a valuable tool for examination of material defects. Typically, analytical 1D models are used to determine the defect depth of flat-bottom holes (FBH), grooves or delamination. However, these models cannot take into account lateral heat flows, or only to a limited extent. They are therefore limited by the FBHs aspect ratio (diameter to remaining wall thickness), to ensure that the heat flow above the defect can still be described one-dimensionally. Here, we present an approach for quantitative determination of the geometry for FBH or grooves. For this purpose, the results of a numerical 2D model are fitted to experimental data, e.g., to determine simultaneously the defect depth of a groove or FBH and its diameter of width. The model takes lateral heat flows into account as well as thermal losses. Figure 1 shows the temperature increase of a pulsed thermography measurement at three different locations on the sample. The numerical model is fitted to the experimental data (red lines) to quantify the groove. The numerical simulation matches the experimental data well. T2 - 45th Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Burlington, VT, USA DA - 15.07.2018 KW - Opaque materials KW - Pulse thermography KW - Numerical modelling KW - 2D model KW - Data reconstruction KW - Flat bottom holes KW - Notches PY - 2018 AN - OPUS4-46353 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altenburg, Simon A1 - Bernegger, Raphael A1 - Krankenhagen, Rainer T1 - Absorption coefficient dispersion in flash thermography of semitransparent solids N2 - Pulse and flash thermography are experimental techniques which are widely used in the field of non-destructive testing for materials characterization and defect detection. We recently showed that it is possible to determine quantitatively the thickness of semitransparent polymeric solids by fitting of results of an analytical model to experimental flash thermography data, for both transmission and reflection configuration. However, depending on the chosen experimental configuration, different effective optical absorption coefficients had to be used in the model to properly fit the respective experimental data, although the material was always the same. Here, we show that this effect can be explained by the wavelength dependency of the absorption coefficient of the sample material if a polychromatic light source, such as a flash lamp, is used. We present an extension of the analytical model to describe the decay of the heating irradiance by two instead of only one effective absorption coefficient, greatly extending its applicability. We show that using this extended model, the experimental results from both measurement configurations and for different sample thicknesses can be fitted by a single set of parameters. Additionally, the deviations between experimental and modeled surface temperatures are reduced compared to a single optimized effective absorption coefficient. T2 - 19th International Conference on Photoacoustic and Photothermal Phenomena CY - Bilbao, Spain KW - Absorptance KW - Dispersion KW - Flash thermography KW - Infrared thermography KW - NDT KW - Semitransparency PY - 2018 DO - https://doi.org/10.1007/s10765-018-2474-0 SN - 0195-928X SN - 1572-9567 VL - 40 IS - 1 SP - 13, 1 EP - 13 PB - Springer Nature AN - OPUS4-47105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Introduction to photoelectronspectroscopy N2 - A short introduction to XPS/ESCA with the focus on nanoparticles and the preparation of such particles for the measurements T2 - Meeting of ACE Nano CY - Berlin, Germany DA - 18.02.2019 KW - ESCA/XPS KW - Nanoparticles KW - Preparation PY - 2019 AN - OPUS4-47437 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brozowski, E. A1 - Colini, C. A1 - Hahn, Oliver A1 - Rabin, Ira ED - Ayo, Charles K. T1 - Scientific investigations on paper and writing materials of Mali: A pilot study N2 - The investigation of physical properties and chemical composition generates data important for answering cultural-historical questions that cannot be solved by historical and philological methods alone. Due to technological developments, technical diagnostics in art and culture are in ever-greater demand in such fields of transdisciplinary research. Natural sciences play auxiliary role in the studies of manuscripts. The success of their contribution depends strongly on the formulation of the question, the choice of the methods to obtain the requested answer, and appropriate reference databases. First, report was given on the measurements performed on local raw materials, such as, plants, minerals and animals, which constitute the reference session. Then, the first results of the scientific analysis of several fragments from the Malian manuscript collections were present. KW - Manuscripts KW - Inks KW - Colorants KW - Non-destructive testing PY - 2019 DO - https://doi.org/10.5897/JASD2017.0453 SN - 2141-2189 VL - 11 IS - 3 SP - 28 EP - 50 PB - Academic Journals CY - Nairobi, Kenya AN - OPUS4-48100 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Hydrogen in weld joints - An underestimated risk? - Utilization potential of gas analytics versus safety of welded components N2 - Hydrogen was once called “the versatile embrittler” [1], which summarizes very well the effect on reduction of ductility and/or toughness in technical alloys like steel. In that connection, welding is one of the most important component fabrication technologies. During welding, hydrogen can be transferred to the weld pool from manifold sources (like contaminations, residuals at the surface, etc.). As hydrogen embrittles a material, the safety of welded components with hydrogen is always a critical issue. Weld heat input causes additional changes in the microstructure like grain growth or partial dissolution of precipitates and many more. All these things influence the mechanical properties and also represent hydrogen traps. These traps decrease the hydrogen diffusion compared to the ideal lattice. The result can be so-called delayed hydrogen assisted cracking (HAC) of the weld joint due to the significantly decreased diffusivity by trapped hydrogen. This is often an underestimated risk as those cracks can appear in the weld joint even after some days! It is essential to know about hydrogen ingress during welding and the microstructure specific hydrogen diffusion. Both are depended on weld parameter influence and the chemical composition of the base material and weld metal. For that purpose, gas analytic methods like solid-state carrier gas hot extraction (CGHE) are useful tools to: (1) identify detrimental hydrogen concentrations from weld joints, (2) binding energies from hydrogen traps by thermal desorption analysis or (3) high-temperature diffusion coefficients. Those values are extremely important for welding practice in terms of recommendations on realistic hydrogen removal heat treatment (HRHT) after welding. Considering the increasing use of “digital” experiments, the data is also needed for reliable numerical simulations of HAC process or HRHT-effectiveness. The present contribution gives an overview on the influence of hydrogen on weld joints, the necessity, methods and standards for hydrogen determination (CGHE) with the aim of fabrication of safe welded and crack-free components. [1] R. A. Oriani (1987), Corrosion 43(7):390-397. doi: 10.5006/1.3583875 T2 - 20. Tagung Festkörperanalyse - FKA20 CY - Vienna, Austria DA - 01.07.2019 KW - Hydrogen KW - Welding KW - Gas analytic PY - 2019 AN - OPUS4-48402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Perez, Jeffey Paulo H. A1 - Tobler, Dominique J. A1 - Thomas, Andrew N. A1 - Freeman, Helen M. A1 - Dideriksen, Knud A1 - Radnik, Jörg A1 - Benning, Liane G. T1 - Adsorption and reduction of arsenate during the Fe2+-induced transformation of ferrihydrite N2 - Iron (oxyhydr)oxides play an important role in controlling the mobility and toxicity of arsenic (As) in contaminated soils and groundwaters. However, dynamic subsurface geochemical conditions can potentially impact As sequestration since this is highly dependent on the dominant iron mineral phases present and the pathways through which they form. In this study, we investigated the Fe2+-induced transformation of As(V)-bearing ferrihydrite (As-FH) to more crystalline phases under relevant anoxic subsurface conditions. Specifically, we examined the influence of varying Fe2+(aq)/Fe(III)solid¬ ratios on the behavior and speciation of the mineral-bound As species during the mineralogical transformation of As-FH at pH 6.5 for 24 h. At lower Fe2+(aq)/Fe(III)solid¬ ratios (0.5 to 1), goethite, green rust sulfate (GR¬SO4) and lepidocrocite formed within the first 2 hours of the reaction, but only goethite and some unreacted FH remained after 24 h. At Fe2+(aq)/Fe(III)solid¬ ratio = 2, GRSO4 remained stable throughout the 24 h reaction, alongside goethite and unreacted FH. Despite >82% of the As-FH being transformed to goethite  GRSO4 in these reactions, no significant As release (>99.9% removal) was observed. However, while As remained mineral-bound, partial oxidation of the initially added As(V) was reduced to As(III), most likely, by the goethite-Fe2+(aq) redox couple. The extent of As(V) reduction increased from ~40% to ~50%, as the Fe2+(aq)/Fe(III)solid¬ ratio increased from 0.5 to 2. Overall, these results provide important insights into transformation pathways of iron (oxyhydr)oxide minerals in As contaminated, anoxic soils and sediments, and also demonstrate the great impact these can have on As oxidation state and, hence, toxicity and mobility in these environments. KW - Ferrihydrite KW - Mineral tranformation KW - XPS KW - Green rust KW - Goethite KW - XAS PY - 2019 DO - https://doi.org/10.1021/acsearthspacechem.9b00031 SN - 2472-3452 VL - 3 IS - 6 SP - 884 EP - 894 PB - ACS AN - OPUS4-48436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Combining surface analytic and toxicity data for safer nanomaterials N2 - Nanomaterials are present in our everyday life. Paint coats, sunscreens, catalysts and additives for tyres are good examples for the use of such materials in mass-market products. The problem of the safety of nanomaterials is recognized as a problem for health and environment, which lead to the special registration of nanomaterials according to an annex of REACH as of 2020. But a great problem for the risk assessment of nanomaterials that several factors could influence the hazardous nature of them. Additional to composition, crystal structure, size and shape the surface properties of such particles belong to these parameters for risk assesment. The reason for the relevance of the surface is obvious: the smaller the particle, the higher is the share of the surface. Additionally, the surface is the region of the particle which interacts with the surrounding which is another crucial factor for the understanding the effect of a nanomaterial on health and environment. In the OECD Testing Programme on Manufactured Nanomaterials exists consequently an Endpoint 4.30 Surface Chemistry in Chapter 4. PHYSICAL AND CHEMICAL PROPERTIES. In summary, there is obviously a need for a correlation between surface chemical analytic data and toxicity. To fill in this gap, we present surface analytic results obtained with X-ray photoelectron spectroscopy and Time-of-Flight Secondary Ion Mass Spectrometry and correlate them with cytotoxic data gain by high-throughput screening experiments. It must be noted, that these experiments were done at the same set of titania materials taken from the JRC (Joint Research Centre of the European Union) Nanomaterials Repository. As material TiO2 was chosen due to its widespread use in consumer products, e.g. paint coats and sunscreens. With this new approach a better understanding of the influence of surface properties on the toxicity can be expected leading to a better risk assessment of these materials. T2 - ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Risk assessment KW - Nanomaterials KW - Surface analytic KW - Toxicology PY - 2019 AN - OPUS4-49090 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Stockmann, Jörg M. T1 - A new reference material for the determination of the Field of View of Small Area XPS N2 - Small Area Photoelectron Spectroscopy (XPS) is a powerful tool for investigating small surface features. It is often unclear, if the signal in the spectrum is an unwanted contamination of the Field of View (FoV) or is it originated from outside. The reason is, that XPS-spectra are affected by beam shapes. Scheithauer proposed to measure Pt apertures of different diameters and normalize the Pt4f count rate by a second measurement on the Pt metal. New reference materials were developed and tested in the VAMAS TWA2 A22 Project. T2 - ECASIA 2019 CY - Dresden, Germany DA - 15.09.2019 KW - Reference material KW - Small Area XPS KW - Selected Area XPS KW - Small Spot XPS KW - Field of Analysis PY - 2019 AN - OPUS4-49236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinelt, Manuel T1 - Feasibility Study on the Direct Detection of Per- and Polyfluoroalkyl Substances (PFAS) with Surface-Assisted Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (SA-FAPA-MS) N2 - Per- and polyfluoroalkyl substances (PFAS) are a large class of thousands of synthetic chemicals that are used worldwide. However, growing environmental and human health concerns in the last two decades have led to more stringent regulatory requirements and the development of quantitative analytical methods for PFAS detection. Today, standardized and powerful methods exist, e.g., for the determination of PFAS in water, sludge, compost, soil, and drinking water (DIN 38407-42, DIN 38414-14, ISO 21675, and DIN EN 17892). While liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) is often used, blank levels, sample preparation, and total analysis times can be challenging. [1] Here, ambient desorption/ionization mass spectrometry (ADI-MS) is considered interesting because it requires only minimal sample preparation and was able to reduce total analysis time in other types of applications. [2] Previously, we used a plasma-based pin-to-capillary flowing atmospheric-pressure afterglow source (FAPA) [3] to probe samples directly from thin-layer chromatography (TLC) plates and to perform quantitative analysis and mass spectral imaging [4]. In this work, a feasibility study for the direct detection of PFAS with FAPA-MS is reported. Selected PFAS samples were directly probed on functionalized TLC surfaces (normal-phase silica, reversed-phase-modified silica, cyano [CN]-modified silica, and dimethyl [RP2]-modified silica, diol modified silica, and amino [NH2]-modified silica). The suitability of the surfaces was evaluated and the compatibility of different solvents with the surfaces was studied. CN-HPTLC and RP2-TLC surfaces showed the best performance for direct PFAS detection with FAPA-MS. In addition, direct analysis of PFAS mixtures and selected matrices was performed with little sample preparation and short analysis time. T2 - 56th Annual Conference of the DGMS CY - Göttingen, Germany DA - 04.03.2025 KW - FAPA-MS KW - Instrumentation KW - Mass Spectrometry KW - PFAS KW - Surface Analysis PY - 2025 AN - OPUS4-63643 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schütz, Désirée A.-M. T1 - Feasibility Study on the Adsorption of Environmental Contaminants onto Fresh and Aged Microplastics N2 - Microplastics (MPs) refer to plastic particles, fibers, or beads with sizes ranging from 100 nm to 5 mm in size. Their pervasive distribution as environmental contaminants have escalated into a significant global concern. Primary MPs are intentionally produced particles for industrial and commercial applications, such as exfoliants in personal care and cosmetic formulations. In contrast, secondary MPs are generated through the fragmentation and degradation of larger plastic materials, due to environmental weathering processes. [1] Due to their high surface area-to-volume ratio and hydrophobic nature, MPs have the potential to serve as vectors for the accumulation and transport of diverse organic contaminants, including polycyclic aromatic hydrocarbons (PAHs), perfluoroalkyl substances (PFAS), pharmaceuticals and personal care products (PPCPs), as well as trace metals such as silver, cadmium, chromium, and copper. In the environmental, MPs are subject to aging processes driven by factors such as temperature, ultraviolet radiation, oxygen, and chemical interactions with environmental toxins. This aging can induce significant alterations in their physicochemical properties, which, in turn, can affect the adsorption behavior. [2] Classical and alternative analytical methods such as high-performance liquid chromatography (HPLC) and ambient desorption/ionization high-resolution mass spectrometry (ADI-HR-MS) can help to study the adsorption potential. ADI-HR-MS allows rapid sample analysis with minimal preparation, providing results in under a minute, much faster than traditional chromatographic techniques. [3] This study aims to investigate the influence of aging and particle size on the ability of microplastics to act as vectors for environmental contaminants. Microplastics were prepared in-house and subjected to controlled aging conditions for 12, 24, 36, and 48 hours. Subsequently, the aged MPs were exposed in plastic-free containers to model solutions to simulate co-contaminants in the environment. Adsorption onto synthesized secondary microplastics, varying in size and aging status, was investigated at different time intervals with ambient MS and time-of-flight secondary ion mass spectrometry. T2 - 56th Annual Conference of the DGMS CY - Göttingen, Germany DA - 04.03.2025 KW - FAPA-MS KW - Mass Spectrometry KW - Microplastics KW - Surface Analysis KW - TOF-SIMS PY - 2025 AN - OPUS4-63644 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Keeping the Y N2 - The talk traces my career path and presents BAM as an attractive employer. It also offers advice on shaping one's own career after PhD. T2 - IWC Alumni Day 2025 CY - Garching bei München, Germany DA - 04.07.2025 KW - Antibodies KW - ELISA KW - Career PY - 2025 AN - OPUS4-63640 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Elemental Composition and Thickness Determination of Thin Films by Electron Probe Microanalysis (EPMA) N2 - microscopy (AFM), or X-ray reflectometry. For the additional determination of thin film composition, techniques like X-ray photoelectron spectroscopy (XPS) or mass spectrometry-based techniques can be used. An alternative non-destructive technique is electron probe microanalysis (EPMA). This method assumes a sample of homogenous (bulk) chemical composition, so that it cannot be usually applied to thin film samples. However, in combination with the thin film software StrataGEM, the thickness as well as the composition of such films on a substrate can be determined. This has been demonstrated for FeNi on Si and SiGe on Al2O3 film systems. For both systems five samples with different elemental composition and a reference were produced and characterised by Korean research institute KRISS using inductively coupled plasma mass spectrometry (ICP-MS), Rutherford backscattering (RBS), and transmission electron microscopy (TEM). These samples were used for an international round robin test. In 2021, a new and open-source thin film evaluation programme called BadgerFilm has been released. It can also be used to determine thin film composition and thickness from intensity ratios of the unknown sample and standards (k-ratios). In this contribution, we re-evaluated the data acquired for the FeNi and SiGe systems using the BadgerFilm software package and compared the resulting composition and thickness with the results of the established StrataGEM software and other reference methods. With the current evaluation, the BadgerFilm software shows good agreement with the composition and thickness calculated by StrataGEM and as the reference values provided by the KRISS. T2 - ECASIA 2022 CY - Limerick, Ireland DA - 29.05.2022 KW - Thin films KW - Electron Probe Microanalysis KW - Interlaboratory Comparisons PY - 2022 AN - OPUS4-54963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Wolfram A1 - Tchetgnia Ngassam, Ines Leana A1 - Olonade, K. A. A1 - Mbugua, R. A1 - Kühne, Hans-Carsten T1 - Plant based chemical admixtures – potentials and effects on the performance of cementitious materials N2 - While today, engineers can choose from a wide range of rheology modifying admixtures, in some parts of the world, these are difficult to access, due to their complex processing. However, alternatives can be bio‐based polymers such as polysaccharides from various sources. These are easily accessible all over the world, do not demand for complicated processing, and typically they are more sustainable than many established materials, which are crude oil‐based. The paper presents the effects of acacia gum, cassava starch and the gum of triumfetta pendrata A. Rich on the rheological performance of cementitious systems. It is shown that acacia gum can be as efficient as polycarboxylate based superplasticisers, cassava starch can reduce the yield stress slightly with little effect on the plastic viscosity, and the gum of triumfet ta pendrata A. Rich increases the thixotropy of cement pastes with plasticizing polymers significantly. KW - Polysaccharides KW - Rheology KW - Cement KW - Chemical admixtures KW - Bio-based concrete PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-476748 DO - https://doi.org/10.21809/rilemtechlett.2018.83 VL - 3 SP - 124 EP - 128 PB - RILEM S.A.R.L. CY - Paris AN - OPUS4-47674 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Tchetgnia Ngassam, Ines A1 - Breitschaft, G. A1 - Virchow, S. ED - Diouri, A. ED - Boukhari, A. ED - Ait Brahim, L. ED - Bahi, L. ED - Khachani, N. ED - Saadi, M. ED - Aride, J. ED - Nounah, A. T1 - Challenges of the growing African cement market – environmental issues, regulative framework, and quality infrastructure requirements N2 - The African cement, concrete and construction business is growing at rapid pace. The cement sales are expected to grow rapidly until 2050. The number of newly built cement plants increases dramatically and in addition more cements are being imported from outside the continent, e.g. from Turkey, Pakistan, Indonesia, and China, driven by overcapacities in the countries of origin. This causes a high number of potentials and challenges at the same time. Newly built cement plants can operate directly at best technological state of the art and thus incorporate more sustainable technologies as well as produce new and more sustainable products such as cements blended with sustainable supplementary cementitious materials such as calcined clays, and industrial or agricultural by products. At the same time the new variety of binding agent as well as the international imports, which are driven by price considerations, make the cement market prone to quality scatter. This puts pressure on the quality control regulations and institutions to ensure safety of construction, healthy application, and environmental safety for the population. The paper presents possible solutions to build up the rapidly increasing African cement production more sustainably than in the rest of the world as well as the related challenges and obstacles that need to be overcome. Based on experiences with a series of pan-African cement testing laboratory proficiency schemes conclusions are made on technical, regulative and political level. T2 - 2nd International Congress on Materials & Structural Stability (CMSS-2017) CY - Rabat, Morocco DA - 22.11.2017 KW - Quality Infrastructure KW - Africa KW - Proficiency Testing KW - Cement KW - Admixtures PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444330 DO - https://doi.org/10.1051/matecconf/201814901014 SN - 2261-236X VL - 149 SP - 01014-1 EP - 01014-8 PB - EDP Sciences CY - Les Ulis AN - OPUS4-44433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Wolfram A1 - Kühne, Hans-Carsten A1 - Leinitz, Sarah ED - Diouri, A. ED - Boukhari, A. ED - Ait Brahim, L. ED - Bahi, L. ED - N., Khachani ED - Saadi, M ED - Aride, J. ED - Nounah, A. T1 - Concrete casting robustness improvement due to active rheology N2 - With ongoing innovation in process technology, the challenges of concrete technology are more and more focused on the rheological optimisation for these processes, since improper mixture stability or poor compaction ability negatively affect the concrete homogeneity and quality. However, along with the increasing complexity of today’s concrete mixture compositions, concrete becomes more prone to failure regarding the casting process. Variable properties of the raw materials typically cause changing workability. The reasons can be found among others in scattering water contents, physical or chemical properties of the cement or varying environmental temperatures. Robustness in the delicately adjusted rheology, however, is of utmost importance for modern and future process technology, from sprayed concrete over pumpable concrete towards 3D-printing, with regard to the long-term strength, the function and the durability. Typically, material induced changes cannot be identified easily due to the complex interactions of concrete constituents. Therefore, a precise and prompt counteraction is impossible. However, it is known that the yield stress can be controlled by addition of supplementary superplasticizer or stabilising agent. In combination with computerized process observation tools that can rapidly interpret and react on changes in the rheology, it is therefore thinkable, that only these two admixture types can adjust the rheology steadily and permanently, regardless of the actual root cause for observed macroscopic rheology change. The presentation will firstly give a comprehensive overview of effects at the interface between pore solution, particles and hydrates, which affect the rheology of fresh concrete. Secondly, ways are recommended how the rheology can be actively manipulated before eventually computerized methods are demonstrated that help to actively and rapidly assess and counteract performance scatter during steady casting processes. T2 - 2nd International Congress on Materials & Structural Stability (CMSS-2017) CY - Rabat, Morocco DA - 22.11.2017 KW - Cusum KW - Rheology KW - Control Chart KW - Concrete KW - Robustness PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444317 DO - https://doi.org/10.1051/matecconf/201814901001 SN - 2261-236X VL - 149 SP - 01001-1 EP - 01001-7 PB - EDP Sciences CY - Les Ulis AN - OPUS4-44431 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kühne, Hans-Carsten A1 - Schmidt, Wolfram A1 - Priebe, Nsesheye Susan T1 - SPIN - Spearhead Network for Innovative, Clean and Safe Cement and Concrete Technologies N2 - Globally, cement and concrete experts are at the cutting-edge to sustainable, green, healthy but nonetheless high-performance concrete. Today concrete is not yet well established in Africa, which offers the unique opportunity to build up a cement and concrete market based on the highest available state of technology. As this industry needs high level expertise, a central issue in implementation of skilled technology is crosslinking research institutions and laboratories. It should not be neglected that concrete is a product with low transport ranges. This means that an improved concrete market mainly supports the local economy without exceeding financial drains to the international market. Thus it fosters the fight against poverty, which is an urgent need in most African countries. The project aims to cross-link experts with industry and policy making bodies, aiming to establish sustainable cement and concrete construction in Africa. KW - High-performance concrete KW - Cement technologies KW - Concrete technologies KW - Sustainable development PY - 2012 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-387428 N1 - Geburtsname von Priebe, Nsesheye Susan: Msinjili, N. S. - Birth name of Priebe, Nsesheye Susan: Msinjili, N. S. SP - 1 EP - 3 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-38742 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gordon, Nehemia A1 - Patrick, Andrist A1 - Hahn, Oliver A1 - Vasileiadis, Pavlos D. A1 - Calvillo, Nelson A1 - Rabin, Ira T1 - Did the Original Scribes Write the Distigmai in Codex Vaticanus B of the Bible (Vat. gr. 1209)? N2 - The fourth-century Greek Bible manuscript Codex Vaticanus B (Vat. gr. 1209) contains pairs of horizontally aligned marginal dots known as distigmai, which correspond to textual variants in other manuscripts. The production of the distigmai has been variously dated to the 4th or 16th centuries. A fourth-century date would prove the early existence of hundreds of textual variants, many of which are otherwise only witnessed by later manuscripts. Near infrared microscope reflectography combined with micro-X-ray fluorescence spectroscopy proved that the distigmai, both those categorized as “apricot” (which are visually similar to the ink of the original main text) and “chocolate” (which are visually similar to the reinking of the main text) were written with ink(s) made from chemically purified vitriol, a process that only became standard in the 16th century. As a result, there is no reasonable chance that the distigmai were written in the fourth century. Horizontal lines that have been hypothesized to function as text-critical obeloi were written in the same ink as the original main text, which differs completely from that of the distigmai. In other words, the distigmai and horizontal lines tested were not produced during the same writing session and are separated by more than 1,000 years, making it impossible for them to have functioned as conjoining text-critical symbols in the 4th century. KW - Bible manuscripts KW - New Testament KW - Paratextual features KW - Textual criticism KW - Obelos KW - Septuagint KW - XRF KW - Greek palaeography PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-622902 DO - https://doi.org/10.1163/27728641-00302005 SN - 2772-8633 VL - 3 IS - 2 SP - 125 EP - 156 PB - Brill CY - Leiden AN - OPUS4-62290 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Rabin, Ira A1 - Caldararo, N. A1 - Rimon, H. ED - Russel, R.E. ED - Lange, A. T1 - The Role of DNA Analysis in the Study of the Biblical Manuscripts N2 - Interest in the type of skin used in scriptural materials and preparation methods increased from the nineteenth into the twentieth century. This was due partly to the number of newly discovered fragments and to the invention of new instruments and scientific procedures to identify animal skins and produce qualitative means to demonstrate specific preparation reagents and techniques. The invention of various means of analyzing the DNA of organic materials brought about a revolution in archaeology and in conservation. Difficulties in overcoming contamination of archaeological samples resulted in a number of controversies but also produced advances and improvement in the techniques of ancient DNA analysis and interpretation of results. KW - DNA KW - Dead Sea Scrolls KW - Parchment PY - 2023 SN - 2468-3027 VL - 3D SP - 120 EP - 123 PB - Brill CY - Leiden / Boston AN - OPUS4-58914 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Ketelsen, T. A1 - Golle, U. A1 - Hahn, Oliver A1 - Wintermann, C. ED - Hahn, Oliver ED - Doil, Thorsten T1 - Katalog der Rembrandt-Zeichnungen in Weimar N2 - Hiermit liegt der kritische Katalog aller Rembrandt-Zeichnungen in der Klassik Stiftung Weimar vor. Im Unterschied zu vielen anderen Graphischen Kabinetten, die ihre Rembrandt-Bestände bereits erfolgreich publiziert haben, existierte eine solche Gesamtschau in Weimar bisher nicht. Die umfassten 51 Katalognummern umfassen alle aktuell Rembrandt zugeschriebenen Blätter, alle rembrandtesken Zeichnungen, die ehemals als Werk Rembrandts angesehen wurden, aber auch alle Zeichnungen, die einmal mit Rembrandt und seiner Schule in Verbindung gebracht wurden. T2 - Rembrandt in Weimar - Ein Beitrag zur Neujustierung der Kennerschaft CY - Weimar, Germany DA - 20.03.2025 KW - Katalog KW - Materialität KW - Rembrandt KW - Zeichnung PY - 2025 SN - 2567-1251 N1 - Serientitel: N.i.Ke. Schriftenreihe des Netzwerks zur interdisziplinären Kulturguterhaltung – Series title: N.i.Ke. Schriftenreihe des Netzwerks zur interdisziplinären Kulturguterhaltung VL - 6 SP - 57 EP - 217 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-63618 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Ketelsen, T. A1 - Hahn, Oliver ED - Hahn, Oliver ED - Doil, Thorsten T1 - Von 25 auf 6: Der Bestand der Rembrandt-Zeichnungen in Weimar N2 - Das Rembrandt-Projekt ist ein Teilresultat, das aus der dreijährigen Katalogisierung der niederländischen und flämischen Zeichnungen in den Graphischen Sammlungen erwachsen ist. Es umfasst alle heute Rembrandt zugeschriebenen Blätter, alle rembrandtesken Zeichnungen, die ehemals als Rembrandts angesehen wurden, aber auch alle Zeichnungen, die einmal mit Rembrandt und seiner Schule in Verbindung gebracht wurden. T2 - Rembrandt in Weimar - Ein Beitrag zur Neujustierung der Kennerschaft CY - Weimar, Germany DA - 20.03.2025 KW - Katalog KW - Materialität KW - Rembrandt KW - Zeichnung PY - 2025 SN - 2567-1251 N1 - Serientitel: N.i.Ke. Schriftenreihe des Netzwerks zur interdisziplinären Kulturguterhaltung – Series title: N.i.Ke. Schriftenreihe des Netzwerks zur interdisziplinären Kulturguterhaltung VL - 6 SP - 10 EP - 12 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-63576 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Ludwig, A. A1 - Eggert, Claudia ED - Hahn, Oliver ED - Doil, Thorsten T1 - Einführung N2 - Der vorliegende, sechste Band der N.i.Ke.-Schriftenreihe zum Workshop "Rembrandt in Weimar - Ein Beitrag zur Neujustierung der Kennerschaft", den die Museen der Klassik Stiftung Weimar am 20./21.3.2025 gemeinsam mit der Bundesanstalt für Materialforschung und -prüfung (BAM) im Goethe-Nationalmuseum ausrichtet, ist jenen 51 Blättern aus der Sammlung der Museen der Klassik Stiftung Weimar gewidmet, die einst als Konvolut authentischer Rembrandt-Zeichnungen galten, inzwischen aber als eigenhändige Arbeiten erkannt oder Werken von Adepten oder Schülern des Niederländischen Meister zugeschrieben werden konnten. T2 - Rembrandt in Weimar - Ein Beitrag zur Neujustierung der Kennerschaft CY - Weimar, Germany DA - 20.03.2025 KW - Katalog KW - Materialität KW - Rembrandt KW - Zeichnung PY - 2025 SN - 2567-1251 N1 - Serientitel: N.i.Ke. Schriftenreihe des Netzwerks zur interdisziplinären Kulturguterhaltung – Series title: N.i.Ke. Schriftenreihe des Netzwerks zur interdisziplinären Kulturguterhaltung VL - 6 SP - 9 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-63539 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schardt, Annika T1 - Fast screening method for nanoparticles in surface waters via nanosecond spICP-MS and a tailored automated ion cloud recognition algorithm N2 - Single particle inductively coupled plasma mass spectrometry (spICP-MS) is a powerful technique for nanoparticle (NP) analysis in aqueous samples, which provides essential information on size distribution and particle number concentration (PNC) of nanometer-sized particles in various water samples for risk assessment and toxicity tests. In contrast to spectroscopic particle analysis methods, this mass spectrometry-based tool can provide chemical information on the elemental composition of NPs after minimal sample preparation. We recently presented a novel spICP-MS instrumentation and tailored software that acquires data with nanosecond time resolution, lowering the particle size detection limit to 7 nm for gold NP (1). The system directly samples the output signal of the electron multiplier and records the detection of individual ions with a time resolution of only a few nanoseconds. With nanosecond time resolution, we were able to visualize profiles of ion clouds that were produced from ionization of nanoparticles in the ICP on a single-ion basis and to use the temporal gap between those ions for particle sizing. Our latest improvement of the data acquisition system (nanoDAQ) features ca. 2 ns integration time and a matching processing software prototype, which automatically recognizes and counts ion clouds in the transient data. With this combination we achieved an experimentally determined size detection limit of ca. 5 nm for gold nanoparticles. A feasibility study shows that the nanoDAQ in combination with the ion cloud recognition algorithm succeeds in fast detection and counting of NP containing Ag, Ce, or Zr in waste water and surface water samples from the area of Siegen. PNCs ranged from ca. 7 x 106–2 x 108 particles/L, which is in good agreement with concentrations reported for similar water samples in the literature. T2 - 56th Annual Conference of the German Society for Mass Spectrometry (DGMS) CY - Göttingen, Germany DA - 04.03.2025 KW - Instrumentation KW - Mass Spectrometry KW - Nanoparticles KW - spICP-MS PY - 2025 AN - OPUS4-63662 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schmidt, Wolfram A1 - Alexander, Mark A1 - John, Vanderley T1 - Education for sustainable use of cement based materials N2 - Structural design and application have always been linked to the compressive strength of concrete as the main relevant criterion. This was justifiable in the past, where concrete consisted of water, ordinary Portland cement and aggregates, but this concept is no longer relevant for modern and more sustainable cement and concrete. Despite these new developments, existing standards, guidelines and academic curricula have not been much updated and are still used worldwide. There is a need to change this situation by proper education of the users. This overview describes the challenges that arise at a user Level from the higher complexity of modern concrete, and defines needs and requirements for enhanced applicability of sustainable concrete concepts. Furthermore, recommendations are given on how better concrete practice can be communicated to all the involved parties, from civil and design engineers to constructors and site-appliers on the construction site. KW - Cement KW - Concrete KW - Sustainability KW - Environment KW - Carbon footprint KW - Education KW - Climate PY - 2018 UR - https://www.sciencedirect.com/science/article/pii/S0008884616307189?via%3Dihub DO - https://doi.org/10.1016/j.cemconres.2017.08.009 SN - 0008-8846 SN - 1873-3948 VL - 114 SP - 103 EP - 114 PB - Elsevier AN - OPUS4-47673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Escobar-Carranza, Cristian C. T1 - On the Detection of Microplastics by Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (FAPA-MS) N2 - Microplastics (MPs) are widespread pollutant particles analyzed using Raman and FTIR spectroscopy combined with optical microscopy. Pyrolysis (Py) or thermal extraction and desorption (TED) coupled with gas chromatography-mass spectrometry (GC-MS) are used for the characterization of MPs, though GC limits sample throughput. This work explores direct, rapid MP analysis using high-resolution (HR) MS and a plasma-based ambient desorption/ionization source (FAPA, flowing atmospheric-pressure afterglow). Previously, an in-house pin-to-capillary (p2c) FAPA source coupled to HRMS characterized MPs made in-house from polystyrene (PS), polypropylene (PP), low-density polyethylene (LDPE), and polycarbonate (PC). Simultaneous detection of characteristic ions and particle imaging on a sampling mesh was feasible, with detection limits (LOD) for PS MPs at 311 µm in size and 1.3 mg in mass. Principal component analysis (PCA) was used for particle differentiation. This work introduces a high-temperature desorption method (~500 °C) with economical and commercially available parts and a tailored housing combined with a halo-shaped (h-FAPA) source configuration. The study expands to include poly(ethylene terephthalate) (PET), poly(methyl methacrylate) (PMMA), and poly(vinyl chloride) (PVC) MPs (125–250 µm). Data visualization and interpretation were performed using Kendrick mass defect plots and other multivariate analysis tools. Compared to earlier results, h-FAPA-MS yielded at least 65% higher ion signals for selected ions in all MPs. These ions were detected mainly as protonated species [M+H]+. Higher thermal desorption temperatures aided in detecting all MPs, as the presence of higher molecular weight fragments added specificity to the analysis. Notably, experiments with the h-FAPA source demonstrated lower mass-based LODs for MPs than the p2c-FAPA source (e.g., 14 µg vs 1.3 mg for PS, respectively). T2 - 56th Annual Conference of the German Society for Mass Spectrometry (DGMS) CY - Göttingen, Germany DA - 04.03.2025 KW - Instrumentation KW - Mass Spectrometry KW - FAPA-MS KW - Microplastics PY - 2025 AN - OPUS4-63663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Colini, Claudia A1 - Shevchuk, I. A1 - Huskin, K. A. A1 - Rabin, Ira A1 - Hahn, Oliver ED - Quenzer, J. B. T1 - A New Standard Protocol for Identification of Writing Media N2 - Our standard protocol for the characterisation of writing materials within advanced manuscript studies has been successfully used to investigate manuscripts written with a pure ink on a homogeneous writing surface. However, this protocol is inadequate for analysing documents penned in mixed inks. We present here the advantages and limitations of the improved version of the protocol, which now includes imaging further into the infrared region (1100−1700 nm). KW - Archaeometry KW - Manuscripts KW - Non-destructive testing PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-543454 SN - 978-3-11-074545-0 DO - https://doi.org/10.1515/9783110753301-009 VL - 25 SP - 161 EP - 182 PB - Walter de Gruyter GmbH CY - Berlin/Boston AN - OPUS4-54345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Investigating the Thermal Decomposition of PFAS in a Full-Scale Commercial Hazardous Waste Incinerator N2 - Incineration is currently the only commercial full-scale technology available to destroy per- and polyfluoroalkyl substances (PFAS) in large solid and liquid waste streams. Given previous experience of dioxin formation during halogenated waste incineration, concerns about the emission of products of incomplete destruction (PIDs) from PFAS incineration exist. The overarching objective of this project is to track the fate of fluorine during full-scale hazardous waste incineration in order to demonstrate the readiness, viability, and level of safety for thermal PFAS destruction in various waste streams. The specific objectives of this project are (1) to enhance our understanding of key variables and conditions on PFAS incineration performance, (2) to identify major PIDs under insufficient treatment conditions, (3) to explore the catalytic role of fly ash and other process-relevant surfaces in thermal PFAS decomposition, and (4) to determine the potential formation of polyfluorinated dibenzodioxins and dibenzofurans. T2 - CEN/TC 264/WG48 Symposium - Emissions and ambient air - Determination of PFAS CY - Düsseldorf, Germany DA - 16.07.2025 KW - Per- and polyfluoroalkyl substances (PFAS) KW - Incineration PY - 2025 AN - OPUS4-63714 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Peplinski, Burkhard T1 - Nanocrystalline and stacking-disordered beta-cristobalite AlPO4 stabilized at room temperature: synthesis and X-ray powder diffraction data N2 - X-ray powder diffraction (XRD) patterns of the high-temperature (HT) cristobalite form of SiO2 and its isoelectronic AlPO4 analogue are essentially influenced by the dynamic disorder of these crystal structures. The nature of this disorder and of the phase transition between the α- and β-form has been the subject of intensive research during the last four decades [1]. By 1989 it became possible to stabilize the HT-form of cristobalite SiO2 at room temperature in laboratory and engineering ceramic industries by applying solid solution forming techniques [2]. However, for the HT-form of cristobalite AlPO4 nothing similar has been known until 2014 when it was discovered that nanocrystalline and stacking-disordered β-cristobalite AlPO4 is the major component of the fly ash of a large incineration facility operated by the waste water treatment authorities of Frankfurt/M. [3]. Previous comprehensive investigations of this fly ash failed to interpret its complex XRD pattern – presumably mainly due to the lack of a matching experimental digital pattern in the Powder Diffraction Database. The present paper reports on a synthesis route that facilitates the crystallization of nanocrystalline and stacking-disordered β-cristobalite AlPO4 that is free of crystalline impurity phases and long-term stable at ambient. Its room temperature XRD pattern is presented with parameters traced back to certified reference materials. [1] Yuan F. and Huang L., Phys. Rev, B, 2012, 85, 134114. [2] Perrotta J.A., Grubbs D.K., Martin E.S., Dando N.R., McKinstry H.A. and Huang C.-Y., J. Am. Ceram. Soc., 1989, 72, 441. [3] Peplinski B., Adam C., Adamczyk B., Müller R., Michaelis M., Krahl Th. and Emmerling F., Powder Diffraction Journal, 2015, 30, 2, Supp. 1, S31. T2 - 15. European Powder Diffraction Conference (EPDIC15) CY - Bari, Italy DA - 12. June 2016 KW - Stabilization of HT-structures at room temperature KW - β-cristobalite structure type KW - Databases PY - 2016 AN - OPUS4-36727 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meyer, Andreas A1 - Weidner, Steffen M. A1 - Kricheldorf, Hans R. T1 - Star-shaped poly(l-lactide)s based on pentaerythritol: About crystallization and polycondensation plus disproportionation and ring formation in the solid state N2 - Star-shaped poly( L-lactide)s (s-PLAs), were prepared by ring-opening polymerization of with pentaerythritol and catalyzed by tin(II) 2-ethylhyexanoate (SnOct out in bulk at either 120 ◦ C or 160 ◦ L-lactide (LA) initiated 2 ). Two small series of ROPs were carried C with variation of the LA/initiator ratio. Matrix-assisted laser desorption/ ionization time-of-flight (MALDI-TOF) mass spectra revealed traces of cycles in 120 ◦ C samples only at low initiator/catalyst ratios. In contrast, higher fractions of cycles were detected in samples prepared at 160 C, suggesting a "back-biting" origin. The influence of arm length and thermal history on crystallinity was investigated by differential scanning calorimetry (DSC) and wide-angle x-ray scattering (WAXS). It was shown that annealing increased the melting temperature (T ◦ ◦ m ) and crystallinity. However, annealing at 140 ◦ C for 14 d also caused significant solid-state transesterification. In addition, crystallites composed of s-PLAs with extended arms and, simultaneously, crystallites composed exclusively of extended rings were formed, identified by their typical "sawtooth" pattern in the MALDI mass spectra. Small angle x-ray scattering (SAXS) indicated that the crystal thickness was lower than that of linear PLAs annealed under identical conditions, but increased upon annealing at 140 C. KW - MALDI-TOF MS KW - Polylactide KW - Crystallisation KW - AStar-shaped polymers PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636832 DO - https://doi.org/10.1016/j.polymer.2025.128709 SN - 0032-3861 VL - 334 SP - 1 EP - 11 PB - Elsevier Ltd. AN - OPUS4-63683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, Hans R. A1 - Weidner, Steffen M. T1 - H2O-Initiated Polymerization of L-Lactide N2 - Water-initiated ring-opening polymerizations (ROPs) of L-lactide (LA) were performed in bulk at 140 °C, whereupon 11 different salts or complexes of low-toxic metal ions such as tin (II), Zn(II), Zr(IV), and Bi(III) were used as catalysts. Only four catalysts gave satisfactory results despite a long reaction time (24 h). The influence of the temperature was studied with tin (II) 2-ethylhexanoate (SnOct2), dibutyltin oxide (Bu2SnO), and zinc bis-acetylacetonate (Zn(acac)2) and zirconium acetylacetonate (Zr(acac)4). With SnOct2, Bu2SnO and Zr(acac)4 the time was varied at 140 °C to compare their reactivity. Furthermore, two series of ROPs were carried out with variation of the LA/H2O ratio to verify the control of the molecular weight by the monomer-initiator ratio. Bi- or tri-modal molecular weight distributions (MWD) were found for most of the ROPs and bimodal melting endotherms in the differential scanning calorimetry (DSC) heating traces. The thickness and dependence of the 3D packing of the crystallites were monitored by small-angle X-ray scattering (SAXS) measurements. KW - MALDI-TOF MS KW - Polylactide KW - Crystallization KW - Ring-opening polymerization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636852 DO - https://doi.org/10.1007/s10924-025-03565-w SN - 1566-2543 VL - 33 IS - 6 SP - 2843 EP - 2857 PB - Springer Science and Business Media LLC AN - OPUS4-63685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rösler, Alexander A1 - Weidner, Steffen M A1 - Klamroth, Tillmann A1 - Müller, Axel HE A1 - Schlaad, Helmut T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents N2 - AbstractThe kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations. © 2025 The Author(s). Polymer International published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry. KW - Myrcene KW - Anionic polymerization KW - Reaction order KW - Activation energy KW - Microstructure KW - Quantum chemical calculation PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-636840 DO - https://doi.org/10.1002/pi.6772 SN - 0959-8103 SP - 1 EP - 8 PB - Wiley AN - OPUS4-63684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Ralf T1 - Vacuum hot extraction: Detection of volatiles N2 - Der Vortrag gibt einen Überblick über die Möglichkete und Grenzen der Methode der Vakuum-Heiß-Extraktion an der BAM T2 - Seminar Instrumentelle Analytik, Fakultät III Prozesswissenschaften, Lehrstuhl Keramik TU Berlin CY - Berlin, Germany DA - 25.01.2019 KW - Heißgasextraktion KW - Glas PY - 2019 AN - OPUS4-50434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stajanca, Pavol A1 - Cetinkaya, O. A1 - Schukar, Marcus A1 - Mergo, P. A1 - Webb, D. J. A1 - Krebber, Katerina T1 - Molecular alignment relaxation in polymer optical fibers for sensing applications N2 - A systematic study of annealing behavior of drawn PMMA fibers was performed. Annealing Dynamics were investigated under different environmental conditions by fiber longitudinal shrinkage monitoring. The shrinkage process was found to follow a stretched exponential decay function revealing the heterogeneous nature of the underlying molecular dynamics. The complex dependence of the fiber shrinkage on initial degree of molecular alignment in the fiber, annealing time and temperature was investigated and interpreted. Moreover, humidity was shown to have a profound effect on the annealing process, which was not recognized previously. Annealing was also shown to have considerable effect on the fiber mechanical properties associated with the relaxation of molecular alignment in the fiber. The consequences of fiber annealing for the climatic stability of certain polymer optical fiber-based sensors are discussed, emphasizing the importance of fiber controlled pre-annealing with respect to the foreseeable operating conditions. KW - Polymer optical fibers KW - Optical fiber sensor climatic stability KW - Thermal annealing KW - Molecular alignment relaxation KW - Humidity induced annealing PY - 2016 DO - https://doi.org/10.1016/j.yofte.2015.12.006 SN - 1068-5200 VL - 28 SP - 11 EP - 17 PB - Academic Press CY - Orlando AN - OPUS4-35288 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Applications of X-ray refraction to non-destructive characterization of ceramics and composites N2 - X-ray refraction is analogous to visible light deflection by matter, with two main differences: 1- convex objects cause divergence (i.e., the refraction index n is smaller than 1), and 2- deflection angles are very small, from a few seconds to a few minutes of arc (i.e., n is near to 1). Trivially but importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks, and quantify their densities in bulk (light) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, their detectability is simply limited by the wavelength of the radiation. We will thereby show the application of X-ray refraction 2D mapping (topography) and tomography to different sorts of problems in ceramic science and technology: 1) Sintering of SiC green bodies; 2) Porosity analysis in diesel particulate filter silicates; 3) fiber de-bonding in metal and polymer matrix composites; 4) micro-cracking of glass-precursor -eucryptite. We will see that the use of X-ray refraction analysis yields quantitative results, also directly usable in available models. T2 - Herbsttreffen des Verbandes der Keramik Industrien CY - Fraunhofer IWM, Freiburg im Breisgau, Germany DA - 27.10.2016 KW - Röntgenrefraktion KW - Kompositen KW - Keramiken KW - Computertomographie KW - TF Material PY - 2013 AN - OPUS4-38301 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Reinsch, Stefan T1 - Glass transition and viscosity of hydrous soda-lime-borate glasses N2 - Boron oxide glasses usually show low glass transition temperature Tg due to the three-fold oxygen coordination of boron. Adding of alkali and alkaline earth oxides to the glass composition will not decrease but increase Tg due to a change in boron coordination from trigonal to tetrahedral, known as the boron anomaly. Only for higher fractions of alkali oxides, non-bridging oxygens (NBO) are progressively formed in competition with tetrahedrally coordinated boron, which leads to a decrease in viscosity. ln contrast to this well-known behavior of alkali oxides (R2O), there is little known about adding H2O to borate glasses. The present work therefore aims in shedding light on the rheological properties of hydrous soda lime borate glasses with particular focus on the role of water. For doing so, we determined Tg as a function of Na2O and H2O content using differential thermal analysis (DTA) backed up by micropenetration viscosity measurements. Results show that water decreases Tg for all glasses and water concentrations under study (< 8 wt.% total water). Obviously, water mostly causes the formation of NBO having no significant influence on boron coordination as seen for alkaline. T2 - Crystallization 2015 CY - Shanghai, China DA - 07.04.2016 KW - Borate glasses KW - Thermal analyses KW - Viscosity KW - Water-bearing glasses PY - 2016 AN - OPUS4-38318 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Per- and Polyfluoroalkyl Substances (PFAS): from analytical methods to thermal and mechanochemical treatment N2 - Per- and polyfluoroalkyl substances (PFAS) are a large group of more than 12,000 organofluorine surfactants. As a result of continuous and prolific use, mainly in aviation firefighting foams, thousands of industrial and military installations have been found to contain contaminated soil, groundwater and surface water. . Current decontamination strategies of PFAS-burdened soils mainly consist of adsorption methods using adsorbents for fixation of PFAS in the ground. A second option is the utilization of a “pump and treat” process, cycling polluted soils through a washing plant leading to the concentration of the pollutants in the fine fraction. Both approaches are cost-intensive and not intended for the direct decomposition of all PFAS contaminants. Furthermore, the contaminated adsorbants have to be safely thermal treated for recovery. Hence, there is a great demand for innovative developments, dealing with new strategies of tackling the PFAS problem. Previously, mechanochemical treatment of polychlorinated organic compounds in soils showed an efficient dechlorination. Thus, we investigated mechanochemical treatment of PFAS contaminated soils with various additives in a ball mill. T2 - Al-Balqa Applied University seminar CY - Al-Salt, Jordan DA - 23.02.2025 KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) KW - XANES spectroscopy KW - Thermal treatment KW - Remediation PY - 2025 AN - OPUS4-62617 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Hentschel, Manfred P. A1 - Onel, Yener A1 - Lange, Axel A1 - Kupsch, Andreas A1 - Wolk, Thomas A1 - Staude, Andreas A1 - Ehrig, Karsten A1 - Müller, Bernd R. T1 - Bewertung von Porositätsparametern in Cordierit-Diesel-Partikelfilter-Materialien mit fortgeschrittenen Röntgenverfahren und statistischer Analyse N2 - Bikontinuierliche poröse Keramiken für Filteranwendungen weisen eine komplizierte Mikrostruktur auf, in der Poren und Festkörperphase 'vermischt' sind. Mechanische, thermische sowie Filtereigenschaften können nur präzise bestimmt werden, wenn die Morphologie beider Phasen quantitativ angegeben werden kann. Hier werden unter Anwendung von 3D Computertomographie (CT) und verschiedenen Techniken, die auf der Röntgenrefraktion basieren, die Porosität und die Porenorientierung in keramischen Cordierit-Dieselpartikelfiltern bewertet. Dabei werden zur Auswertung der Tomogramme die Fouriertransformierten sowie eine neu entwickelte richtungssensitive Bildanalyse (DIVA, directional interface variance analysis) angewandt. Sowohl die genannten Messtechniken als auch der statistische Ansatz gestatten die Extraktion optional ortsaufgelöster oder gemittelter Werte. Es ergeben sich sehr gute Übereinstimmungen der experimentell ermittelten Porositätswerte mit Ergebnissen aus Quecksilberintrusionsversuchen als auch der ermittelten Porenorientierung im Vergleich zu publizierten Angaben zur kristallographischen Textur. Dies legt den Schluss nahe, dass die Kenntnis der Grenzflächen (zwischen Poren und Materie) genügt, die morphologischen Eigenschaften solcher Materialien hinreichend zu beschreiben. T2 - DGZfP-Jahrestagung 2014 CY - Potsdam, Germany DA - 26.05.2014 KW - Cordierit KW - Poröse Keramik KW - Porenorientierung KW - Röntgenrefraktion KW - Computer-Tomographie KW - 3D-Mikrostruktur PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-312946 SN - 978-3-940283-61-0 VL - 148 SP - 1 EP - 8 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-31294 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Hentschel, Manfred P. A1 - Lange, Axel A1 - Bruno, Giovanni A1 - Müller, Bernd R. T1 - Direkte Röntgenrefraktion an Mikrostrukturen N2 - Die durch Brechung an Mikrostrukturen abgelenkte Röntgenstrahlung wird direkt zweidimensional abgebildet. Dazu werden Modellproben einfacher Geometrie (Fasern, Kapillaren, monodisperse Nano- und Mikropartikel) mit einem auf 50 µm kollimierten Synchrotronstrahl (20 keV) gescannt. Die nach den Regeln der geometrischen Optik an prismatischen und linsenartigen Grenzflächen abgelenkte Strahlung wird in etwa 3 Metern Entfernung von einem Flächendetektor mit 7 µm Ortsauflösung zusätzlich zu der ungestörten Resttransmission des Primärstrahls registriert. In der Abfolge der Radiogramme werden die lokalen Orientierungsänderungen der Probekörper-Grenzflächen bei deren Abtastung mit wenigen Mikrometern Schrittweite bildhaft verfolgt. Mit der hier erreichten Winkelauflösung von etwa 3 Bogensekunden (Streuvektor-Inkremente Δk = 10-3nm-1) kann bei 50 µm Ortsauflösung das Materialvolumen bezüglich innerer Grenzflächen mit Nanometer-Separation auch bei hohen Abtastraten unterhalb einer Sekunde pro Bild charakterisiert werden. T2 - DGZfP-Jahrestagung 2014 CY - Potsdam, Germany DA - 26.05.2014 KW - Computertomographie (CT) KW - Rekonstruktionsalgorithmus KW - DIRECTT KW - Missing wedge KW - Statistische Bewertung PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-312931 UR - http://www.ndt.net/article/dgzfp2014/papers/di1b2.pdf SN - 978-3-940283-61-0 IS - DGZfP-BB 148 SP - Di.1.B.2, 1 EP - 9 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-31293 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Adamczyk, Burkart A1 - Simon, Franz-Georg A1 - Adam, Christian T1 - RecArc - Verwertung von Rückständen aus der Metallurgie mit der Lichtbogentechnologie N2 - In dem Projekt soll die vollständige Wiederverwertbarkeit der Schlacke und ihrer Bestandteile demonstriert werden. Dazu gehören die vollständige Rückgewinnung der metallischen Phase, die in die Edelstahlherstellung zurückgeführt werden kann, sowie die Aufwertung der mineralischen Fraktion, die ihre uneingeschränkte Verwendung als Zementzumahlstoff oder mineralischer Baustoff erlaubt. Bei geeigneter Prozessführung des elektrischen Lichtbogenofens können durch „reduzierendes Schmelzen“ die chromhaltigen Wertstoffe zusammen mit anderen Schwermetallen zu 97% in einer Metalllegierung angereichert und separiert werden. Diese kann als Rohstoff in der Metallurgie eingesetzt werden. Der Chromgehalt der mineralischen Komponte der Schlacke konnte von ca. 3% auf unter 0,1% verringert werden. Die mineralische Fraktion lässt sich durch entsprechende Zuschläge während des Schmelzbetriebes und eine anschließende Granulation der schmelzflüssigen Phase zu einem Material aufwerten, das in seiner Zusammensetzung und seinen Eigenschaften typischen Zementkomponenten entspricht und als Rohstoff in der Zementproduktion eingesetzt werden kann. Dafür müssen allerdings noch die rechtlichen Voraussetzungen geschaffen werden, da der Rohstoffeinsatz gerade im Zement strengen Auflagen unterliegt und die Zemente bestimmte Normen erfüllen müssen. Durch die in RECARC aufgezeigte Möglichkeit der Wiederverwertung können somit Stoffkreisläufe geschlossen werden, die ansonsten zu einem Verlust wertvoller Rohstoffe führen. Vor allem die steigenden Rohstoffkosten, aber auch die immer stärker limitierten CO2-Emissionen zeigen die hohe Relevanz im Umgang mit metallurgischen Reststoffen. Eine Überführung des in RECARC demonstrierten Verfahrens in die Industrie könnte einen wichtigen Beitrag zur nachhaltigen Schonung der natürlichen Ressourcen und der Umwelt leisten. KW - Chrom KW - Lichtbogenofen KW - Recycling KW - Rückgewinnung KW - Schlacke PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-390197 SP - 1 EP - 4 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-39019 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Paciornik, S. A1 - Bruno, Giovanni T1 - Advanced Deep Learning-Based 3D Microstructural Characterization of Multiphase Metal Matrix Composites N2 - The quantitative analysis of microstructural features is a key to understanding the micromechanical behavior of metal matrix composites (MMCs), which is a premise for their use in practice. Herein, a 3D microstructural characterization of a five-phase MMC is performed by synchrotron X-ray computed tomography (SXCT). A workflow for advanced deep learning-based segmentation of all individual phases in SXCT data is shown using a fully convolutional neural network with U-net architecture. High segmentation accuracy is achieved with a small amount of training data. This enables extracting unprecedently precise microstructural parameters (e.g., volume fractions and particle shapes) to be input, e.g., in micromechanical models. KW - Computed tomography KW - Convolutional neural networks KW - Deep learning KW - Metal matrix composites KW - Segmentations PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504261 DO - https://doi.org/10.1002/adem.201901197 SN - 1438-1656 VL - 22 IS - 4 SP - 1901197 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-50426 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mani, Deepak A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Diffraction Enhanced Imaging Analysis with Pseudo-Voigt Fit Function N2 - Diffraction enhanced imaging (DEI) is an advanced digital radiographic imaging technique employing the refraction of X-rays to contrast internal interfaces. This study aims at qualitatively and quantitatively evaluating images acquired using this technique and to assess how different fitting functions to the typical rocking curves (RCs) influence the quality of images. RCs are obtained for every image pixel. This allows the separate determination of the absorption and the refraction properties of the material in a position-sensitive manner. Comparison of various types of fitting functions reveals that the Pseudo-Voigt (PsdV) function is best suited to fit typical RCs. A robust algorithm was developed in the Python programming language, which reliably extracts the physically meaningful information from each pixel of the image. We demonstrate the potential of the algorithm with two specimens: a silicone gel specimen that has well-defined interfaces, and an additively manufactured polycarbonate specimen. KW - Diffraction Enhanced Imaging KW - Analyzer-Based Imaging KW - X-ray refraction KW - Non-Destructive Evaluation KW - Pseudo-Voigt fit function KW - Python PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553791 DO - https://doi.org/10.3390/jimaging8080206 SN - 2313-433X VL - 8 IS - 8 SP - 1 EP - 13 PB - MDPI CY - Basel, Switzerland AN - OPUS4-55379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laquai, René A1 - Schaupp, Thomas A1 - Griesche, Axel A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Hannemann, Andreas A1 - Kannengießer, Thomas A1 - Bruno, Giovanni T1 - Quantitative analysis of hydrogen-assisted microcracking in duplex stainless steel through X-ray refraction 3D imaging N2 - While the problem of the identification of mechanisms of hydrogen assisted damage has and is being thoroughly studied, the quantitative analysis of such damage still lacks suitable tools. In fact, while, for instance, electron microscopy yields excellent characterization, the quantitative analysis of damage requires at the same time large field-of-views and high spatial resolution. Synchrotron X-ray refraction techniques do possess both features. In this work, we show how synchrotron X-ray refraction computed tomography (SXRCT) can quantify damage induced by hydrogen embrittlement in a lean duplex steel, yielding results that overperform even those achievable by synchrotron X-ray absorption computed tomography. As already reported in literature, but this time using a non-destructive technique, we show that the hydrogen charge does not penetrate to the center of tensile specimens. By the comparison between virgin and hydrogen-charged specimens, we deduce that cracks in the specimen bulk are due to the rolling process rather than hydrogen-assisted. We show that (micro)cracks propagate from the surface of tensile specimens to the interior with increasing applied strain, and we deduce that a significant crack propagation can only be observed short before rupture. KW - 2101 duplex stainless steel KW - Hydrogen embrittlement KW - Synchrotron radiation KW - X-ray refraction KW - Computed tomography KW - Microcracking PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542811 DO - https://doi.org/10.1002/adem.202101287 SN - 1438-1656 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. A1 - Soares, A.P. A1 - Kupsch, Andreas A1 - Baum, D. A1 - Hesse, B. A1 - Zaslansky, P. T1 - Untersuchung der Integrität von glasfaserverstärkten Zahnstiften mittels Synchrotron-Röntgenrefraktion N2 - Die Integrität der Verstärkungsfasern in Komposit-Zahnstiften ist entscheidend für die Biegefestigkeit und die langfristige Haftung am Zement in den Wurzelkanälen. Es wurde vermutet, dass die Integrität von glasfaserverstärkten Zahnstiften durch das Beschleifen während der zahnmedizinischen Behandlung beeinträchtigt wird. Eine Beschädigung der Fasern führt zu einer erheblichen strukturellen Schwächung über den gesamten Stiftdurchmesser. Glasfragmente, die durch den Kontakt mit dem Zahnbohrer entstehen, können sich vom Stift lösen und die Haftfähigkeit erheblich verringern. Mit Hilfe hochauflösender Synchrotron-Röntgen-Refraktions-Radiographie (SXRR) konnte das Ausmaß der Schäden zuverlässig identifiziert und charakterisiert werden. Dazu wurden die Glasfaserstifte sowohl im Herstellungszustand als auch nach der Bearbeitung mit einem Diamantbohrer untersucht. Die Datensätze wurden zur Visualisierung und Quantifizierung der morphologischen Charakteristika intakter und durch das Beschleifen beschädigter Regionen analysiert. Sie zeigen Schäden im bearbeiteten Bereich (z. B. Brüche, Splitter und Risse) sowie herstellungsbedingte Inhomogenitäten der Fasern mit einer signifikanten Zunahme der inneren Oberflächen in Probenregionen, die durch das Beschleifen beschädigt wurden. T2 - DGZfP Jahrestagung 2022 CY - Kassel, Germany DA - 23.05.2022 KW - Röntgen-Refraktion KW - Verbundwerkstoffe KW - Zahnstifte PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-549231 SP - 1 EP - 7 AN - OPUS4-54923 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Léonard, F. A1 - Lange, A. A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - On the Morphological and Crystallographic Anisotropy of Diesel Particulate Filter Materials N2 - The determination of the anisotropy of materials’ microstructure and morphology (pore space) in diesel particulate filter (DPF) materials is an important problem to solve, since such anisotropy determines the mechanical, thermal, and filtration properties of such materials. Through the use of a dedicated (and simple) segmentation algorithm, it is shown how to exploit the information yielded by 3D X-ray computed tomography data to quantify the morphological anisotropy. It is also correlated that such anisotropy of the pore space Such anisotropy of the pore space is also correlated with the microstructure and crystallographic anisotropy of the material in several showcases: a microstructurally isotropic material, such as SiC, and some morphologically and microstructurally anisotropic cordierite materials. In the later case, the finer the grain size, the more isotropic the microstructure. KW - Diesel Particulate Filter Materials PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-540705 DO - https://doi.org/10.1002/adem.202101380 VL - 24 IS - 2101380 SP - 1 EP - 12 PB - Wiley VCH GmbH CY - Weinheim AN - OPUS4-54070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wipfler, B. A1 - Bradler, S. A1 - Büsse, S. A1 - Hammel, J. A1 - Müller, Bernd R. A1 - Pass, G. T1 - Evolutionary morphology of the antennal heart in stick and leaf insects (Phasmatodea) and webspinners (Embioptera) (Insecta: Eukinolabia) N2 - The morphology of the antennal hearts in the head of Phasmatodea and Embioptera was investigated with particular reference to phylogenetically relevant key taxa. The antennal circulatory organs of all examined species have the same basic construction: they consist of antennal vessels that are connected to ampullae located in the head near the antenna base. The ampullae are pulsatile due to associated muscles, but the points of attachment differ between the species studied. All examined Phasmatodea species have a Musculus (M.) interampullaris which extends between the two ampullae plus a M. ampulloaorticus that runs from the ampullae to the anterior end of the aorta; upon contraction, all these muscles dilate the lumina of both ampullae at the same time. In Embioptera, only the australembiid Metoligotoma has an M. interampullaris. All other studied webspinners instead have a M. ampullofrontalis which extends between the ampullae and the frontal region of the head capsule; these species do not have M. ampulloaorticus. Outgroup comparison indicates that an antennal heart with a M. interampullaris is the plesiomorphic character state among Embioptera and the likely ground pattern of the taxon Eukinolabia. Antennal hearts with a M. ampullofrontalis represent a derived condition that occurs among insects only in some embiopterans. These findings help to further clarify the controversially discussed internal phylogeny of webspinners by supporting the view that Australembiidae are the sister group of the remaining Embioptera. KW - Phylogeny KW - Polyneoptera KW - Metoligotoma PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-527795 DO - https://doi.org/10.1007/s00435-021-00526-4 SN - 1432-234X VL - 140 IS - 3 SP - 331 EP - 340 PB - Springer AN - OPUS4-52779 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, Henning A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Evsevleev, Sergei A1 - Arlt, T. A1 - Ulbricht, Alexander A1 - Dayani, Shahabeddin A1 - Bruno, Giovanni T1 - A Review of X-Ray Imaging at the BAMline (BESSY II) N2 - The hard X-ray beamline BAMline at BESSY II (Berlin, Germany) has now been in service for 20 years. Several improvements have been implemented in this time, and this review provides an overview of the imaging methods available at the BAMline. Besides classic full-field synchrotron X-ray computed tomography (SXCT), also absorption edge CT, synchrotron X-ray refraction radiography (SXRR), and synchrotron X-ray refraction tomography (SXRCT) are used for imaging. Moreover, virtually any of those techniques are currently coupled in situ or operando with ancillary equipment such as load rigs, furnaces, or potentiostats. Each of the available techniques is explained and both the current and the potential usage are described with corresponding examples. The potential use is manifold, the examples cover organic materials, composite materials, energy-related materials, biological samples, and materials related to additive manufacturing. The article includes published examples as well as some unpublished applications. KW - Material science KW - Radiography KW - Refraction KW - Tomography KW - X-ray imaging PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572417 DO - https://doi.org/10.1002/adem.202201034 SN - 1438-1656 SP - 1 EP - 22 PB - Wiley VHC-Verlag AN - OPUS4-57241 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Machado Ferreira de Araujo, F. A1 - Duarte-Ruiz, D. A1 - Saßnick, H.-D. A1 - Gentzmann, Marie C. A1 - Huthwelker, T. A1 - Cocchi, C. T1 - Electronic Structure and Core Spectroscopy of Scandium Fluoride Polymorphs N2 - Microscopic knowledge of the structural, energetic, and electronic properties of scandium fluoride is still incomplete despite the relevance of this material as an intermediate for the manufacturing of Al−Sc alloys. In a work based on first-principles calculations and X-ray spectroscopy, we assess the stability and electronic structure of six computationally predicted ScF3 polymorphs, two of which correspond to experimentally resolved single-crystal phases. In the theoretical analysis based on density functional theory (DFT), we identify similarities among the polymorphs based on their formation energies, chargedensity distribution, and electronic properties (band gaps and density of states). We find striking analogies between the results obtained for the ow- and high-temperature phases of the material, indirectly confirming that the transition occurring between them mainly consists of a rigid rotation of the lattice. With this knowledge, we examine the X-ray absorption spectra from the Sc and F K-edge contrasting firstprinciples results obtained from the solution of the Bethe−Salpeter equation on top of all-electron DFT with high-energy-resolution fluorescence detection measurements. Analysis of the computational results sheds light on the electronic origin of the absorption maxima and provides information on the prominent excitonic effects that characterize all spectra. A comparison with measurements confirms that the sample is mainly composed of the high- and low-temperature polymorphs of ScF3. However, some fine details in the experimental results suggest that the probed powder sample may contain defects and/or residual traces of metastable polymorphs. KW - Scandium KW - X-ray spectroscopy PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-570727 DO - https://doi.org/10.1021/acs.inorgchem.2c04357 SN - 0020-1669 VL - 62 IS - 10 SP - 4238 EP - 4247 PB - ACS Publications CY - Washington DC AN - OPUS4-57072 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Trappe, Volker A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Rissentwicklung in CFK-Laminaten nachgewiesen durch in situ Röntgen-Refraktion N2 - In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Röntgen-Refraktion KW - Synchrotronstrahlung KW - CFK KW - Rissentwicklung PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576230 SN - 978-3-947971-29-9 VL - BB 180 SP - 1 EP - 8 AN - OPUS4-57623 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Hoffmann, Marie A1 - Taube, Mareike A1 - Krüger, O. A1 - Baran, R. A1 - Adam, Christian T1 - Uranium and thorium species in phosphate rock and sewage sludge ash based phosphorus fertilizers N2 - Phosphorus (P) is an essential element for all forms of life and is thus often applied as phosphate rock-based P-fertilizers in agriculture to enable continuous farming. However, these P-fertilizers contain also hazardous uranium (U) and thorium (Th), up to 660 and 220 mg/kg, respectively. On the contrary, novel P-fertilizers made from sewage sludge (ash) contain only low mass fractions of U and Th. In addition to the total amount of U and Th in P-fertilizers, their mobility and bioavailability is important, which depends to a large extent on their chemical state, especially oxidation state and chemical bonding. Thus, we analyzed their chemical state in various P-fertilizers by U and Th L3-edge HERFD-XANES spectroscopy. Phosphate rocks and sewage sludge-based P-fertilizers contain mainly U(IV) compounds which have only a low bioavailability. In contrast, acidic treatment of phosphate rock to produce super phosphates lead to an oxidation to U(VI) compounds (including formation of uranium phosphates) with a strongly increased bioavailability. On the contrary, all analyzed P-fertilizers contain Th in form of strongly insoluble phosphates and oxides with a low bioavailability. Additionally performed water extractions and Diffusive Gradients in Thin-films (DGT) experiments support these findings. KW - Phosphorus fertilizer KW - Sewage sludge KW - X-ray absorption near-edge structure (XANES) spectroscopy KW - Diffusive Gradients in Thin-films (DGT) KW - Extraction PY - 2020 DO - https://doi.org/10.1016/j.jhazmat.2019.121100 SN - 0304-3894 VL - 382 SP - 121100, 1 EP - 6 AN - OPUS4-48872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Marc Benjamin A1 - Dietrich, P. M. A1 - Radnik, Jörg T1 - In situ monitoring of the influence of water on DNA radiation damage by near-ambient pressure X-ray photoelectron spectroscopy N2 - Ionizing radiation damage to DNA plays a fundamental role in cancer therapy. X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS xperiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. The results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further. KW - DNA KW - XPS KW - NAP-XPS KW - Radiation damage KW - Single-strand break (SSB) KW - Double-strand break (DSB) KW - Xray KW - OH radical KW - Hydroxyl radical KW - LEE KW - Low energy electrons KW - Dosimetry KW - Geant4 KW - Geant4-DNA KW - TOPAS KW - TOPAS-nbio KW - Microdosimetry KW - DNA radiation damage KW - Direct damage KW - Indirect damage KW - Quasi-direct damage KW - Hydration shell KW - Dry DNA KW - Hydrated DNA KW - ROS KW - Radical KW - Reactive oxygen species KW - Net-ionization reaction KW - Radiation therapy KW - Cancer therapy KW - Xray photo electron spectrocopy KW - Near ambient pressure xray photo electron spectroscopy KW - Base damage KW - Base loss KW - Dissociative electron transfer (DET) KW - Dissociative electron attachment (DEA) KW - Hydrated electron KW - Prehydrated electron KW - Ionization KW - PES PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-524060 DO - https://doi.org/10.1038/s42004-021-00487-1 SN - 2399-3669 VL - 4 IS - 1 SP - 50 PB - Springer Nature CY - London AN - OPUS4-52406 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hahn, Marc Benjamin A1 - Meyer, Susann A1 - Schröter, Maria-Astrid A1 - Seitz, H. A1 - Kunte, Hans-Jörg A1 - Solomun, Tihomir A1 - Sturm, Heinz T1 - Direct electron irradiation of DNA in fully aqueous environment. Damage determination in combination with Monte Carlo simulations N2 - We report on a study in which plasmid DNA in water was irradiated with 30 keV electrons generated by a scanning electron microscope and passed through a 100 nm thick Si3N4 membrane. The corresponding Monte Carlo simulations suggest that the kinetic energy spectrum of the electrons throughout the water is dominated by low energy electrons (<100 eV). The DNA radiation damage, single-strand breaks (SSB) and double-strand breaks (DSB), was determined by electrophoresis. The median lethal dose of D1/2 = 1.7 ± 0.3 Gy was found to be much smaller compared to partially or fully hydrated DNA irradiated under vacuum conditions. The ratio of DSB to SSB was found to be (1:12) as compared to 1:88) found for hydrated DNA. Our method enables quantitative measurements of radiation damage to biomolecules (DNA, proteins) in solutions under varying conditions (pH, salinity, cosolutes) for an electron energy range which is difficult to probe by standard methods. KW - Plasmid DNA in water KW - Monte Carlo simulation KW - Low energy electrons KW - DNA radiation damage KW - Single-strand break (SSB) KW - Double-strand break (DSB) KW - Lethal dose KW - Radiation damage to biomolecules KW - Solutions (pH, salinity, cosolutes) PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-386981 DO - https://doi.org/10.1039/C6CP07707B SN - 1463-9076 SN - 1463-9084 VL - 19 IS - 3 SP - 1798 EP - 1805 PB - Royal Society of Chemistry AN - OPUS4-38698 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröter, Maria-Astrid A1 - Meyer, Susann A1 - Hahn, Marc Benjamin A1 - Solomun, Tihomir A1 - Sturm, Heinz A1 - Kunte, Hans-Jörg T1 - Ectoine protects DNA from damage by ionizing radiation N2 - Ectoine plays an important role in protecting biomolecules and entire cells against environmental stressors such as salinity, freezing, drying and high temperatures. Recent studies revealed that ectoine also provides effective protection for human skin cells from damage caused by UV-A radiation. These protective properties make ectoine a valuable compound and it is applied as an active ingredient in numerous pharmaceutical devices and cosmetics. Interestingly, the underlying mechanism resulting in protecting cells from radiation is not yet fully understood. Here we present a study on ectoine and its protective influence on DNA during electron irradiation. Applying gel electrophoresis and atomic force microscopy, we demonstrate for the first time that ectoine prevents DNA strand breaks caused by ionizing electron radiation. The results presented here point to future applications of ectoine for instance in cancer radiation therapy. KW - Plasmid DNA pUC19 KW - Electron irradiation 30 [kV] KW - Effective irradiation dose 0.2-16 [Gy] KW - Gel electrophoresis KW - AFM intermittent contact KW - Radioprotector ectoine KW - Compatible solute PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-428287 DO - https://doi.org/10.1038/s41598-017-15512-4 SN - 2045-2322 VL - 7 IS - 1 SP - 15272, 1 EP - 15272, 7 PB - Nature AN - OPUS4-42828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Panorama of Black writing inks: From Antiquity to the Middle Ages N2 - Black writing inks in the period under consideration can be divided into three different classes: soot, tannin and iron-gall ink. The first one is a fine dispersion of carbon pigments in a water-soluble binding agent, the second one is a solution of plant extract from tree barks or gallnuts, while the third one contains both soluble and insoluble phases. This last ink is based on metal (iron) and is produced by a chemical reaction of soluble iron (II) with tannin in aqueous solution. Tracing the transition from writing inks based on carbon pigments (soot or charcoal), common in Antiquity to the iron-gall inks commonly used in the Middle Ages builds a focus of our investigative work at the BAM (Federal Institute of Material Analysis and Testing) [1-5]. With the aim of creating a detailed history of writing black inks, we worked out a non-invasive protocol to collect statistically relevant ink data from dated and localized manuscripts covering a large time span and different geographic areas. The first step of our protocol consists of the screening carried out by means of imaging in the near infrared region. The optical differences between carbon, tannin, and iron-gall inks are best recognized by comparing their response to the infrared light: carbon ink has a deep black colour, iron-gall ink becomes transparent above 1400 nm, and tannin ink disappears at about 750 nm, we have simplified the analysis using a small USB microscope with built-in NIR (940 nm) and UV (395 nm) LED in addition to an external white light source [1]. Comparing the images under white and near infrared illumination, we determine the ink typology by observing the changes in the opacity of the ink. Here, carbon-based inks show no change in their opacity when illuminated with near infrared light, while the opacity of iron-gall inks changes considerably, and tannin inks become transparent. Our own recent finding that mixed carbon / iron-gall inks were quite popular in the late Antiquity and early Middle Ages suggested to return to the conventional method using infrared light in the spectral region 1000 – 1400 nm. The presentation will show the panorama of historic inks and our attempt to follow up the transition of the inks from those based on soot to the iron-gall inks commonly used in the Middle Ages. T2 - Public lecture CY - Manchester, UK DA - 01.02.2024 KW - Ink KW - Historic ink PY - 2024 AN - OPUS4-61201 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Methoden und Erkenntnismöglichkeiten von Tintenanalysen N2 - Der Vortrag stellt die Palette der zerstörungsfreien analytischen Methoden, die zur Identifizierung und Vergleich der Tinten, Tuschen und Pigmente verwendet werden. T2 - Experten-Workshop CY - Hamburg, Germany DA - 06.10.2022 KW - Tinte KW - Tusche KW - Pigmente PY - 2022 AN - OPUS4-61195 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Unveiling the use of writing materials in Carolingian manuscripts N2 - After having been neglected for a long time, materiality is nowadays of great interest in the study of manuscripts. This allows us to explore the variety (and potential coexistence) of different inks and pigments in type and composition in their use over time and geographical area. In this presentation, we aim to contribute to their study through archaeometric analyses of black and red inks used in Carolingian manuscripts copied between the 8th and the 10th centuries. These analyses are based on an interdisciplinary strategy, bringing together knowledge from the humanities and natural sciences to understand the global use of black and red inks in the Carolingian Empire. In this regard, we adopted a non-invasive protocol that included near-infrared imaging and X-ray fluorescence spectroscopy for on-site measurements supported by historical and palaeographic analysis. The results have been collected in the framework of two projects at the University of Hamburg in close collaboration with the Bundesanstalt für Materialforschung und -prüfung, Berlin (BAM) and will be compared with several other archaeometric studies of contemporary manuscripts. T2 - Novel approaches to Digital Codicology CY - Tours, France DA - 10.05.2023 KW - Carolingian manuscripts KW - Historick inks KW - Pigments PY - 2023 AN - OPUS4-61199 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Imaging micro-XRF in studies of manuscripts N2 - Availability of mobile XRF-equipment with an interaction spot of ca. 100 µm produced a revolution in the studies of manuscripts. A protocol for the use of line-scans introduced in the beginning of 2000 permitted large scale and extremely successful investigations of the medieval iron-gall inks. Here, we usually focus on a comparison of the characteristic metallic components in the inks. In our work, we encountered cases that could be adequately addressed only using large area imaging XRF. However, conducting an M6 scan on a bound manuscript or on a scroll of huge dimensions is not a simple and easy matter. In our presentation, we want to share our experience by presenting a series of the case studies, in which many an original solution was found. T2 - M6 JETSTREAM European User Meeting CY - London, GB DA - 03.04.2023 KW - Micro-XRF KW - Manuscripts KW - Imaging PY - 2023 AN - OPUS4-61198 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Authentic vs. inauthentic Dead Sea Scrolls from the point of view of material analysis N2 - The paper seeks to illuminate the problem of identifying forgeries among the Dead Sea Scrolls from the point of view of material analysis. It will present the sum of our technical knowledge of the skin-based material of the Dead Sea Scrolls, which includes the original treatment of the skins and the resulting typology as well as degradation effects due to their sojourn in caves and post-discovery interventions. We will try then to list the characteristic properties that must be found in the authentic material. We will supplement the presentation with a short description of the relevant methods of material analysis and their contribution to the secure identification of inauthentic Dead Sea Scrolls. T2 - Annual Meeting of the Siciety of Biblical Literature CY - Denver, CO, USA DA - 19.11.2022 KW - Dear Sea Scrolls KW - Forgery PY - 2022 AN - OPUS4-61196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Material analysis - results N2 - The presentations describes the results obtained by material analysis of the writing materials. Their relevance in the field of digital editing and publishing is discussed. T2 - Communicating Revealed Texts: Best Practices for Born-Digital Editions Using Enhanced Imaging CY - Iowa City, IA, USA DA - 29.06.2024 KW - Writing materials KW - Manuscripts KW - Material analysis PY - 2024 AN - OPUS4-61202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cohen, Zina A1 - Hahn, Oliver A1 - Rabin, Ira A1 - Ward, Aengus T1 - Centenary Paper: Of Inks and Scribes: The Composition of a Thirteenth-Century Castilian Manuscript – British Library Res 20787 N2 - This article presents the results of the first scientific analysis of the inks of a thirteenth-century Castilian manuscript – British Library Res 20787, a copy of the Fuero de las leyes. The analysis reveals the fingerprint of the inks used in the codex and points the way to future cross-disciplinary research based on a wider corpus of evidence. KW - Archaeometry KW - Manuscript KW - Colorant KW - Cinnabar PY - 2024 DO - https://doi.org/10.3828/bhs.2024.56 SN - 1475-3839 VL - 101 SP - 703 EP - 720 PB - Liverpool University Press AN - OPUS4-61435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cohen, Z. A1 - Hennings, T. A1 - Hahn, Oliver A1 - Depreux, P. A1 - Rabin, Ira T1 - Black inks under examination. Part 2: a case study of Carolingian manuscripts N2 - With this paper, we would like to contribute to the study of black writing materials by investigating the black inks used in the manuscripts from monastic production in the eastern part of the Frankish kingdom, especially in the region of Lake Constance and in Bavaria and dated to the period between the 8th and the 10th centuries. The corpus under study contains manuscripts with formulae, i.e. model letters and charters, besides numerous other types of texts with no clear separation between them (for example by titles). Sixty-three manuscripts have been studied with the aim of reconstructing the history of both their copying and their use. To this aim, we adopted a non-invasive approach that included near-infrared imaging and X-ray fluorescence spectroscopy for on-site measurements, supported by historical and palaeographic analysis. The results obtained in this project are compared with several other archaeometric studies of contemporary manuscripts with the general aim of understanding the use of black ink in medieval manuscripts. KW - Manuscript KW - Ink analysis KW - Carolingian PY - 2023 DO - https://doi.org/10.4000/techne.18919 SN - 2239-0243 VL - 56 SP - 105 EP - 113 AN - OPUS4-61582 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rabin, Ira T1 - Advances in Characterization of Written Heritage N2 - The session discusses three brances of teh work on the manuscripts: ink analysis, parchment analysis by proteomics (Matthew Collins) and lipids (Mélanie Roffet-Salque); revealing of hidden text using AI. The example of Vesuvium Challenge is presented and discussed by Bren Seales. T2 - Scientific Methods in Cultural Heritage Research Gordon Research Conference CY - Vaud, Switzerland DA - 07.07.2024 KW - Written Heritage KW - Vesuvius challenge KW - Proteomics KW - Lipids PY - 2024 AN - OPUS4-61203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Operando electrochemical spectroscopic ellipsometry: Material properties of highly active mesoporous IrO IrOxfilms revealed under realistic OER conditions N2 - Rising energy demand and the impending climate change require the development of a sustainable, fossil-free fuel and chemical production on a global scale. Hydrogen production via water electrolysis will be a fundamental cornerstone in this endeavor. The activity and stability of respective electrode coatings strongly depends on the coating's properties, i.e. phase composition, crystallinity, electrical conductivity, accessible surface, wettability and many other factors. The key to the development of improved catalysts is a better understanding of the relations between their performance, stability and physicochemical properties. However, those relations can be complex, and are strongly influenced also by the reaction environment. Hence, operando analysis of the catalyst material during catalysis at realistic potentials and current densities is highly desirable. Yet, many analytical techniques cannot be applied in liquid environments at realistic potentials and current densities. We propose environmental ellipsometric analysis in a dedicated electrochemical flow cell as a new method to evaluate gas evolution reactions operando under realistic working conditions. Figure 1 illustrates schematically the developed technique. Key factors to success are highly active model-type catalysts with template-controlled porosity, a suitable sample environment, a deep understanding of the spectroscopic method and respective model development, as well as concise cross validation with numerous other analytical techniques. The method was developed and validated by analyzing a calcination series (300 - 600°C) of mesoporous templated IrOx films ex-situ and operando under oxygen evolution reaction (OER) conditions. The employed environmental electrochemical spectroscopic ellipsometric analysis (ECSE) revealed during OER the change of optical and electronic properties, i.e. the dielectric functions (real ε1 and imaginary part ε2), electrical and electronic properties such as resistivity (ρ) and band-to-band transitions (p-d band transitions). Film thickness and porosity were validated by means of scanning electron microscopy (SEM), X-ray reflectometry (XRR) or ellipsometric porosimetry (EP), electrical and electronic properties by means of conductivity measurements, X-ray photoelectron spectroscopy (XPS) or UV-Vis-NIR absorption spectroscopy. The electronic structures of the catalysts from valence electron energy loss spectra (VEELS) derived from the real (ε1) and imaginary part (ε2) of the dielectric function from SE measurements reveal a direct correlation with electrochemical activities in OER. In the presentation reversible and irreversible potential-dependent changes of the catalyst properties during operation will be discussed along with the dynamics of gas formation, transport and dissolution at different potentials. T2 - 54. Jahrestreffen deutscher Katalytiker CY - Online meeting DA - 16.03.2021 KW - Spectroscopic ellipsometry KW - Electrocatalysis KW - Oxygen evolution reaction KW - Mesoporous iridium oxide films KW - Non-destructive operando analysis PY - 2021 AN - OPUS4-52928 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Marc Benjamin T1 - Near-Ambient-Pressure XPS to investigate radiation damage to DNA N2 - X-ray photoelectron-spectroscopy (XPS) allows simultaneous irradiation and damage monitoring. Although water radiolysis is essential for radiation damage, all previous XPS studies were performed in vacuum. Here we present near-ambient-pressure XPS experiments to directly measure DNA damage under water atmosphere. They permit in-situ monitoring of the effects of radicals on fully hydrated double-stranded DNA. Our results allow us to distinguish direct damage, by photons and secondary low-energy electrons (LEE), from damage by hydroxyl radicals or hydration induced modifications of damage pathways. The exposure of dry DNA to x-rays leads to strand-breaks at the sugar-phosphate backbone, while deoxyribose and nucleobases are less affected. In contrast, a strong increase of DNA damage is observed in water, where OH-radicals are produced. In consequence, base damage and base release become predominant, even though the number of strand-breaks increases further. T2 - Physical and Chemical Analysis of Polymers seminar CY - Online meeting DA - 12.10.2021 KW - Base damage KW - Base loss KW - Cancer therapy KW - DNA KW - DNA radiation damage KW - Direct damage KW - Dissociative electron attachment (DEA) KW - Dissociative electron transfer (DET) KW - Dosimetry KW - Double-strand break KW - DSB KW - Dry DNA KW - Geant4 KW - Geant4-DNA KW - Hydrated DNA KW - Hydrated electron KW - Hydration shell KW - Hydroxyl radical KW - Indirect damage KW - Ionization KW - LEE KW - Low energy electrons KW - Microdosimetry KW - NAP-XPS KW - Near ambient pressure xray photo electron spectroscopy KW - Net-ionization reaction KW - OH radical KW - PES KW - Prehydrated electron KW - Quasi-direct damage KW - ROS KW - Radiation damage KW - Radiation therapy KW - Radical KW - Reactive oxygen species KW - Single-strand break KW - SSB KW - TOPAS KW - TOPAS-nbio KW - XPS KW - Xray KW - Xray photo electron spectrocopy PY - 2021 AN - OPUS4-53611 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - XPS of GR2M N2 - The activities of ISO-G-Scope are presented. The influence of the sample preparation and the results of XPS/HAXPES measurements are discussed. T2 - Graphene Workshop @ ISO TC 229 Meeting CY - Teddington, UK DA - 16.11.2022 KW - Graphene related materials KW - X-ray photoelectron spectroscopy KW - Sample preparation KW - Hard X-ray photoelectron spectroscopy PY - 2022 AN - OPUS4-56434 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Operando electrochemical spectroscopic ellipsometry: Material properties of highly active mesoporous IrO IrOxfilms revealed under realistic OER conditions N2 - Rising energy demand and the impending climate change require the development of a sustainable, fossil-free fuel and chemical production on a global scale. Hydrogen production via water electrolysis will be a fundamental cornerstone in this endeavor. The activity and stability of respective electrode coatings strongly depends on the coating's properties, i.e. phase composition, crystallinity, electrical conductivity, accessible surface, wettability and many other factors. The key to the development of improved catalysts is a better understanding of the relations between their performance, stability and physicochemical properties. However, those relations can be complex, and are strongly influenced also by the reaction environment. Hence, operando analysis of the catalyst material during catalysis at realistic potentials and current densities is highly desirable. Yet, many analytical techniques cannot be applied in liquid environments at realistic potentials and current densities. We propose environmental ellipsometric analysis in a dedicated electrochemical flow cell as a new method to evaluate gas evolution reactions operando under realistic working conditions. Figure 1 illustrates schematically the developed technique. Key factors to success are highly active model-type catalysts with template-controlled porosity, a suitable sample environment, a deep understanding of the spectroscopic method and respective model development, as well as concise cross validation with numerous other analytical techniques. The method was developed and validated by analyzing a calcination series (300 - 600°C) of mesoporous templated IrOx films ex-situ and operando under oxygen evolution reaction (OER) conditions. The employed environmental electrochemical spectroscopic ellipsometric analysis (ECSE) revealed during OER the change of optical and electronic properties, i.e. the dielectric functions (real ε1 and imaginary part ε2), electrical and electronic properties such as resistivity (ρ) and band-to-band transitions (p-d band transitions). Film thickness and porosity were validated by means of scanning electron microscopy (SEM), X-ray reflectometry (XRR) or ellipsometric porosimetry (EP), electrical and electronic properties by means of conductivity measurements, X-ray photoelectron spectroscopy (XPS) or UV-Vis-NIR absorption spectroscopy. The electronic structures of the catalysts from valence electron energy loss spectra (VEELS) derived from the real (ε1) and imaginary part (ε2) of the dielectric function from SE measurements reveal a direct correlation with electrochemical activities in OER. In the presentation reversible and irreversible potential-dependent changes of the catalyst properties during operation will be discussed along with the dynamics of gas formation, transport and dissolution T2 - E MRS 2021 SPRING MEETING CY - Online meeting DA - 31.05.2021 KW - Spectroscopic ellipsometry KW - Ectrocatalysis KW - Oxygen evolution reaction KW - Mesoporous iridium oxide films KW - Non-destructive operando analysis PY - 2021 AN - OPUS4-52929 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias T1 - Process monitoring in metal AM@BAM, the project ProMoAM N2 - In this presentation we give an overview of activities regarding non-destructive testing of AM components during the manufacturing process. For this purpose, we installed different NDT methods inside the AM systems. The results obtained during the manufacturing process are presented and discussed. T2 - 74th IIW Annual Assembly and International Conference CY - Online meeting DA - 07.07.2021 KW - Non-destructive testing KW - Additive manufacturing KW - Online monitoring PY - 2021 AN - OPUS4-53186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Hahn, Oliver ED - Ackermann, U. ED - Golle, U. ED - Hahn, Oliver ED - Wintermann, Carsten T1 - Die Farben des frühen Bauhauses N2 - Der Beitrag beschäftigt sich mit zerstörungsfreien Untersuchungen an den Farbmitteln früher Bauhauszeichnungen. Mit welchen Farbmitteln wurden diese Zeichnungen gestaltet? Wurden hier neueste Zubereitungen genutzt, von denen viele im ersten Drittel des 20. Jahrhunderts gerade auf den Markt kamen, oder fanden – der ebenfalls am Bauhaus propagierten Materialökonomie folgend – althergebrachte Materialien Verwendung, die günstiger zu beschaffen waren? Weitere Fragen widmen sich dem Themenkomplex Original, Kopie und Nachahmung sowie der Auffindung von Fälschungen. Restauratorische, konservatorische und kuratorische Fragestellungen und Entscheidungen sind grundsätzlich damit verknüpft. Zwölf exemplarisch vorgestellte Zeichnungen ermöglichen einen guten Über blick über die verwendeten Farbmittel des frühen Bauhauses von 1919 bis 1925. Trotz der Vielfalt der betrachteten Studien, Entwürfen und Arbeitsblättern, ergibt sich ein homogenes Gesamtbild. Bis auf wenige Ausnahmen dominieren anorganische Pigmente die Farbmittelpalette. Dieser Befund wird durch eine weitaus größere Stichprobe materialtechnologisch untersuchter Zeichnungen aus dem Bestand des Bauhaus-Museums Weimar bestätigt KW - Archäometrie KW - Bauhaus Weimar KW - Zerstörungsfreie Prüfung KW - Zeichenmaterialien PY - 2022 SN - 978-3-7443-0424-5 SP - 18 EP - 31 AN - OPUS4-56730 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hahn, Oliver T1 - Original, Kopie, Fälschung? Multispektralanalyse von Bauhauszeichnungen N2 - Der Vortrag widmet sich der materialwissenschaftlichen Analyse von Zeichnungen einiger Bauhausschülerinnen und Bauhausschüler und legt besonderen Fokus auf die verwendeten Farbmittel. Die Objekte werden mit nicht-invasiven bildgebenden Verfahren untersucht, in dem die Wechselwirkung zwischen Röntgen-, sichtbarem und infraroten Licht und den Zeichnungen studiert wird. Dier Analysen liefern nicht nur generell Erkenntnisse über die Art und Zusammensetzung und damit das Alter der verwendeten Farbmittel. Durch die Auffindung von Vorzeichnungen, die Bestimmung von Überarbeitungen und Korrekturen werden Erkenntnisse über die Genese von Zeichnungen gewonnen. Auf der Basis dieser materialwissenschaftlichen Erkenntnisse werden die Begriffe Original, Kopie, Fälschung diskutiert. Da die nicht-invasiven Untersuchungen einen umfassenden Einblick in die Materialität der – überwiegend aus Papier bestehenden – Objekte erlauben, bilden sie die Grundlage für die Erstellung nachhaltiger Konservierungs- und Restaurierungskampagnen und deren dauerhaften Erhalt. T2 - Rahmenprogramm zur Ausstellung "Das Leben der Objekte. Farbe und Papier am Weimarer Bauhaus" CY - Weimar, Germany DA - 12.01.2023 KW - Bauhaus KW - Zerstörungsfreie Prüfung KW - Farbmittel PY - 2023 AN - OPUS4-56847 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Knigge, Xenia A1 - Radnik, Jörg T1 - 1-Propyl-3-methyl-imidazolium bis(trifluoromethylsulfonyl)imide (Solarpur®) analyzed by hard x-ray photoelectron spectroscopy N2 - 1-Propyl-3-methyl-imidazolium bis(trifluoromethylsulfonyl)imide (Solarpur®), an ionic liquid was purchased from Merck (formerly Sigma Aldrich), was analyzed using hard x-ray photoelectron spectroscopy (HAXPES). The liquid is UHV stable, vertically and laterally homogeneous, and is easy to clean; thus, it can be used as a reference material. The HAXPES spectra of Solarpur® obtained using monochromatic Cr Kα radiation at 5414.8 eV include a survey scan, high-resolution spectra of C 1s, O 1s, N 1s, S 2p, S 1s, S 2s, F 1s, and S KLL. KW - HAXPES KW - Hard x-ray photoelectron spectroscopy KW - Ionic liquid KW - Solarpur PY - 2021 DO - https://doi.org/10.1116/6.0001414 VL - 28 IS - 2 SP - 1 EP - 8 PB - AVS: Science & Technology of Materials, Interfaces, and Processing AN - OPUS4-54113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Xps/Haxpes at (core shell) nanoparticles N2 - The principles of (Hard) X-ray photoelectron spectroscopy and some application in the field of (core-shell) nanoparticles will be presented. The presentation should answer hoe to get reliable results. Furthermore, examples of the correlation between physical-chemical measurments and toxicological results are given which are crucial for the risk assessment of nanoparticles. T2 - Training Course Metrological Determination of Micro and Nano Contaminants in Food CY - Berne, Switzerland DA - 05.09.2023 KW - X-ray photoelectron spectroscopy KW - Core-shell nanoparticles KW - Reliabiilty KW - Risk assessment PY - 2023 AN - OPUS4-59496 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Dietz, Georg A1 - Dumas, C. A1 - Golle, U. A1 - Melzer, C. A1 - Mildenberger, H. A1 - Orth, C. A1 - Seifert, C. T. A1 - Wintermann, Carsten A1 - Ketelsen, T. A1 - Hahn, Oliver ED - Ketelsen, T. ED - Hahn, Oliver T1 - Die Sammlung der Niederländischen Zeichnungen in Weimar. Ein Handbuch N2 - Die Klassik-Stiftung Weimar besitzt eine umfangreiche Sammlung niederländischer und flämischer Zeichnungen vom 15. bis 19. Jahrhundert. Im Rahmen des Forschungsprojektes »Kennerschaft heute« wurde der Bestand der über 1.500 Zeichnungen erstmals wissenschaftlich erschlossen. Das Handbuch führt anhand bedeutender Werkgruppen, darunter Zeichnungen von Lucas van Leyden, Dirck Vellert, Roelant Savery und Rembrandt, den Reichtum der Weimarer Sammlung vor Augen, die zum großen Teil auf die Sammelleidenschaft von Johann Wolfgang Goethe zurückgeht. Im Zentrum des Buches steht aber die Zusammenarbeit von traditioneller Stilkritik und naturwissenschaftlicher Materialanalyse. In zwölf Fallbeispielen wird die Notwendigkeit einer methodischen Neuausrichtung der Kennerschaft darlegt. Einen Schwerpunkt der Untersuchungen bildet hierbei das große Konvolut an Zeichnungen von Rembrandt und seinen Schülern, das erstmals systematisch auf die verwendeten Zeichenmaterialien und Papiere untersucht wird. KW - Archäometrie KW - Zeichnungen KW - Papier KW - Zeichenmaterialien KW - Rembrandt PY - 2022 SN - 978-3-95498-715-3 SP - 1 EP - 312 PB - Sandstein Verlag CY - Dresden AN - OPUS4-56720 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier A1 - Del Mastro, G. A1 - Hammerstaedt, J. A1 - Mocella, V. A1 - Rabin, Ira ED - Capasso, M. ED - Davoli, P. ED - Pellé, N. T1 - XRF Ink Analysis of Selected Fragments from the Herculaneum Collection of the Biblioteca Nazionale di Napoli N2 - Hundreds of papyrus rolls, carbonized during the 79CE eruption of Mount Vesuvius, were discovered in 1754 at Herculaneum. Sophisticated mechanical methods for unrolling the best-preserved scrolls have been applied, with varying success. However, such processes have been abandoned, to prevent risk from irremediable damage or loss and to preserve the integrity of the extremely fragile rolls. Following the development of X-ray based non-invasive techniques, attempts to virtually unroll the scrolls were made. The most common ink in Antiquity was carbon-based, and the main element of carbonized papyrus is carbon, making these investigations difficult. However, some attempts with synchrotron X-ray phase-contrast tomography (XPCT) were successful. Recently, the identification of antique inks containing metals raised hope that if some of the inks contain metal the rolls can be virtually unrolled using conventional CT- technique. We investigated the inks of a selection of partially unrolled fragments stored at the Biblioteca Nazionale di Napoli with X-ray fluorescence in order to select the best candidates for tomography. Despite the many difficulties (analysis of several layers sticking together, letters barely visible, difficulty to separate contribution from the ink and from the papyrus, inhomogeneity of the support, fragility of the fragments…), encouraging results were found, with a number of inks from Greek fragments found to contain additions to the soot (Fe, Pb, Cu P). KW - XRF KW - ink KW - Herculaneum KW - papyrus PY - 2022 UR - http://siba-ese.unisalento.it/index.php/29th_ICP/issue/view/1881 SN - 978-88-8305-177-7 DO - https://doi.org/10.1285/i99788883051760 SP - 200 EP - 213 PB - Centro di Studi Papirologici dell’Università del Salento CY - Lecce AN - OPUS4-54756 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rhode, Michael T1 - Bericht zum Fortschritt des laufenden Projekts: "Entwicklung von Wärmenachbehandlungskonzepten zur Vermeidung von Spannungsrelaxationsrissen" N2 - Dieses Dokument fasst den Projekfortschritt des BAM-Projektes "Entwicklung von Wärmenachbehandlungsstrategien zur Vermeidung von Spannungsrelaxationsrissen" im Rahmen des Fachausschusses 1 "Schweißmetallurgie" des DVS e.V. für das Projektjahr 2021 zusammen und stellt die wichtigsten Ergebnisse in Kurzform vor. T2 - Sitzung des FA1 "Schweißmetallurgie" der Forschungsvereinigung Schweißen und verwandte Verfahren des DVS e.V. CY - Online meeting DA - 22.03.2022 KW - UP-Schweißen KW - Spannungsrelaxationsriss KW - Wärmenachbehandlung KW - Eigenspannungen KW - Schallemissionsanalyse PY - 2022 AN - OPUS4-54525 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - VAMAS-Enabling international standardisation for increasing the take up of Emerging Materials N2 - VAMAS (Versailles Project on Advanced Materials and Standards) supports world trade in products dependent on advanced materials technologies by providing technical basis for harmonized measurements, testing, specification, reference materials and standards. The major tools for fulfilling this task are interlaboratory comparisons (ILC). The organisation structure of VAMAS is presented. It is discussed, how a new technical activity can initiate. T2 - DIN NA062-08-16 Oberflächenanalytik Frühjahrstreffen CY - Berlin, Germany DA - 11.05.2022 KW - Advanced Materials KW - Standards KW - Interlaboratory Comparisons PY - 2022 AN - OPUS4-54831 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabin, Ira A1 - Gordon, Nehemia A1 - Cohen, Zina T1 - Inks of the Bologna Scroll: A Preliminary Study N2 - Rotolo 2 at the Biblioteca Universitaria di Bologna, also known simply as the “Bologna Scroll,” is currently the oldest known complete Torah scroll without later replacement sheets or significant lacunae. The Bologna Scroll has some unusual scribal features. According to one opinion in the Babylonian Talmud, a Torah scroll must be written with carbon ink to be valid for liturgical use.12 The main inks of the Bologna Scroll are very black, and the inks of the marginal corrections in tiny letters are even blacker. In this study, eh inks were tested by means of XRF-spectroscopy and NIR imaging. Conreary to the expectations, the current tests have definitively determined that the Bologna Scroll was both written and corrected using multiple iron-gall inks. KW - Torah KW - Ink KW - Historic ink PY - 2024 DO - https://doi.org/10.1353/mns.2024.a945374 VL - 9 IS - 2 SP - 222 EP - 242 AN - OPUS4-62264 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN ED - Hahn, Oliver ED - Danielewski, A. ED - Nöller, Renate ED - Doil, Thorsten T1 - Manuscripta americana - Den Azteken auf der Spur - Eine Ausstellung im Kulturwerk der Staatsbibliothek zu Berlin - 07. Dezember 2022 bis 26. Februar 2023 N2 - Die Publikation befasst sich mit einer einzigartigen Sammlung mexikanischer und südamerikanischer Handschriften, die zu Beginn des 19. Jahrhunderts ins Leben gerufen wurde, als Alexander von Humboldt der Königlichen Bibliothek zu Berlin Fragmente indigener mexikanischer Bilderhandschriften aus dem 16. Jahrhundert schenkte. Sie sind heute auch unter der Bezeichnung Humboldt-Fragmente bekannt und stellen den bedeutendsten Teil der Sammlung dar, die im Laufe der Zeit durch den Ankauf verschiedener Arten von Handschriften aus Mittelamerika, vorwiegend in indigenen Sprachen und lateinischer Schrift, erweitert wurde. In den zwei Jahren von April 2017 bis März 2019 verfolgten die Staatsbibliothek zu Berlin – Preußischer Kulturbesitz (SBB-PK) und die Bundesanstalt für Materialforschung und -prüfung (BAM) ein gemeinsames, von der Deutschen Forschungsgemeinschaft (DFG) großzügig gefördertes wissenschaftliches Projekt: Materialanalysen und kulturgeschichtliche Untersuchungen mexikanischer Handschriften aus der Kolonialzeit in Berlin und Krakau. Die Hauptziele des Projekts bestanden darin, die Provenienz der Manuscripta americana zu ermitteln und, da sie einen hohen Grad an Fragmentierung aufweisen, festzustellen, wie sie untereinander und mit Objekten außerhalb der Sammlung in Beziehung stehen. Zu diesem Zweck wurden ethno-kulturhistorische und naturwissenschaftliche Methoden kombiniert. Dank einer guten Zusammenarbeit mit der Jagiellonen-Bibliothek konnten wir die Manuscripta americana sowohl in Berlin als auch in Krakau sehen und studieren und sie wissenschaftlich vermessen. T2 - Manuscripta americana - Den Azteken auf der Spur - Eine Ausstellung im Kulturwerk der Staatsbibliothek zu Berlin CY - Berlin, Germany DA - 07.12.2022 KW - Archäometrie KW - Zerstörungsfreie Prüfung KW - Manuskripte KW - Amate PY - 2022 SN - 2567-1251 N1 - Es gibt parallele Sprachausgaben (englisch und spanisch), Links befinden sich im Feld zugehöriger Identifikator - There are parallel language editions (English and Spanish), links are in the field related identifier VL - 4 SP - 1 EP - 120 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-56729 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schukar, Marcus T1 - Faser-Bragg-Gitter-Sensoren überwachen Strahlung am Elektronenspeicherring BESSY II. N2 - Untersuchung der Eignung von FBG-Strahlungssensoren zur verteilten Überwachung auftretender ionisierender Strahlung an Elektronenspeicherringen. Test des Messverfahrens am Undulator U 49/1 des Elektronenspeicherrings BESSY II T2 - 8. Dresdner Sensorsymposium CY - Dresden, Germany DA - 10.02.2007 PY - 2007 AN - OPUS4-16291 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Witt, Jens T1 - Smart medical textiles with embedded optical fibre sensors for continuous monitoring of respiratory movements during MRI N2 - We report on three respiration sensors based on pure optical technologies developed during the FP6 EU project OFSETH. The developed smart medical textiles can sense elongation up to 3%, while maintaining the stretching properties of the textile substrates for a good comfort of the patient. The sensors, based on silica and polymer fibre, are developed for monitoring of patients during MRI examination. The OFSETH harness allows a continuous measurement of respiration movements while all vitals organs are free for medical staff actions. The sensors were tested in MRI environment and on healthy adults. T2 - 4th European Workshop on Optical Fibre Sensors (EWOFS) CY - Oporto, Portugal DA - 08.09.2010 PY - 2010 AN - OPUS4-22061 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - de Oliveira, Rui T1 - Advanced composite materials with embedded POF sensors for structural health monitoring N2 - A long period grating (LPG) mechanically imprinted in a microstructured polymer optical fibre (mPOF) is embedded in a carbon fibre reinforced polymer (CFRP) unidirectional laminate. Processing steps were established in order to ensure that mPOF does not suffer significant degradation. The strain and temperature responses of the embedded mPOF-LPG were then investigated. T2 - The 19th International Conference on Plastic Optical Fibers CY - Yokohama, Japan DA - 19.10.2010 PY - 2010 AN - OPUS4-22416 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Analysis of fluorine/PFAS in battery black mass at HESEB N2 - Lithium iron phosphate (LiFePO4) batteries are a safe, cost-effective alternative to traditional lithium-ion batteries, but industrial-scale recycling is not yet available. The recycling process faces challenges, especially in purifying materials like lithium, phosphate, and iron, and managing fluorine contamination from fluoropolymers and salts (including PFAS). Fluorine K-edge XANES spectroscopy was used to analyze the chemical states of fluorine in the recycled materials for a safe reuse of elements and defluorination. T2 - SESAME – Germany Support and Networking Meeting CY - Hamburg, Germany DA - 30.06.2025 KW - Per- and polyfluoroalkyl substances (PFAS) KW - Battery PY - 2025 AN - OPUS4-63560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bintz, Thilo T1 - An NMR tomograph for building materials - applications , experimental studies and limitations N2 - Introduction of the NMR Tomograph of Department 8.0 at BAM, the applications, technical limitations, and uses in laboratory studies. T2 - International Conference on Electromagnetic Wave Interaction with Water and Moist Substances (ISEMA) 2021 CY - Kiel, Germany DA - 26.07.2021 KW - NMR relaxometry KW - NMR imaging KW - Sensitivity KW - Building materials PY - 2021 N1 - Geburtsname von Munsch, Sarah Mandy: Nagel, S. M. - Birth name of Munsch, Sarah Mandy: Nagel, S. M. AN - OPUS4-53043 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Elucidating core shell nanostructures with surface analytics N2 - XPS is a versatile tool for elucidating core shell structures. XPS can obtain information for organic compounds (polymer particle, organic coating ) which are hardly or not detectable with other Methods. XPS is an important tool for the risk assessement of nanoparticles T2 - Kratos German User Meeting CY - Online meeting DA - 26.05.2021 KW - Core-shell nanoparticles KW - X-ray photoelectron spectroscopy KW - Complementary methods PY - 2021 AN - OPUS4-52717 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Elemental composition of an ionic liquid surface N2 - (1) First results show the suitability of IL as reference for quantification of XPS (at least for organic materials). (2) Different quantification methods lead to similar results (with a slight advantage for “background method”). (3)Promising reference material for a better understanding and traceable protocols for the quantification of organic materials with XPS. T2 - BIPM / SAWG Spring Meeting CY - Online meeting DA - 12.05.2021 KW - Ionic liquid KW - X-ray photoelectron spectroscopy KW - Quantification PY - 2021 AN - OPUS4-52688 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Radnik, Jörg T1 - BAM reference data - XPS raw data of Al-coated titania nanoparticles (JRCNM62001a and JRCNM62002a) N2 - XPS raw data of Al-coated titania nanoparticles (JRCNM62001 and JRCNM62002a) provided by the JRC repository are provided. KW - XPS KW - Titania nanoparticles KW - BAM reference data PY - 2021 DO - https://doi.org/10.5281/zenodo.4986068 PB - Zenodo CY - Geneva AN - OPUS4-52880 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sachse, René T1 - Operando electrochemical spectroscopic ellipsometry: Material properties of highly active mesoporous IrO IrOxfilms revealed under realistic OER conditions N2 - In the face of rising energy demand and the impending climate change the development of a sustainable, fossil-free fuel and chemical production is of global importance. One possible goal is the development of electrochemical conversion processes using catalysts. Porous materials play an important role in such energy applications. The activity and stability of each catalyst is highly dependent on the properties of the coating, i.e., phase composition, crystallinity, accessible surface area, and many other factors. The key to the development of improved catalysts is a better understanding of the relations between their performance, stability and physico-chemical properties. However, the complex morphology of such catalysts constitutes a challenge even for modern analytical techniques. Spectroscopic ellipsometry (SE) is a versatile method for studying material properties by using appropriate models (e.g., film thickness, optical and electronic properties). Ellipsometric models need to be validated in order to produce accurate results. In a first step, the model for the ellipsometric fit studies of a calcination series of mesoporous iridium oxide films (300 – 600 °C) was investigated and validated with respect to their material properties.[4] The information on electronic structure of the catalysts shows a direct correlation with electrochemical activities. The development of an environmental electrochemical cell offers the possibility of investigations under operando conditions. Thus, changes in optical and electronic properties can be induced and monitored during the electrocatalytic oxygen evolution reaction. T2 - 9th International Conference on Spectroscopic Ellipsometry CY - Beijing, China DA - 22.05.2022 KW - Mesoporous iridium oxide films KW - Non-destructive operando analysis KW - Oxygen evolution reaction KW - Spectroscopic ellipsometry PY - 2022 AN - OPUS4-54915 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier T1 - XRF Ink analysis of selected fragments from the Herculaneum collection N2 - Hundreds of papyrus rolls, carbonized during the 79CE eruption of Mount Vesuvius, were discovered in 1754 at Herculaneum. Sophisticated mechanical methods for unrolling the best-preserved scrolls have been applied, with varying success. However, such processes have been abandoned, to prevent risk from irremediable damage or loss and to preserve the integrity of the extremely fragile rolls. Following the development of X-ray based non-invasive techniques, attempts to virtually unroll the scrolls were made. The most common ink in Antiquity was carbon-based, and the main element of carbonized papyrus is carbon, making these investigations difficult. However, some attempts with synchrotron X-ray phase-contrast tomography (XPCT) were successful. Recently, the identification of antique inks containing metals raised hope that if some of the inks contain metal the rolls can be virtually unrolled using conventional CT- technique. We investigated the inks of a selection of partially unrolled fragments stored at the Biblioteca Nazionale di Napoli with X-ray fluorescence in order to select the best candidates for tomography. Despite the many difficulties (analysis of several layers sticking together, letters barely visible, difficulty to separate contribution from the ink and from the papyrus, inhomogeneity of the support, fragility of the fragments…), encouraging results were found, with a number of inks from Greek fragments found to contain additions to the soot (Fe, Pb, Cu P). T2 - International Symposium on Archaeometry CY - Online meeting DA - 16.05.2022 KW - XRF KW - Ink KW - Herculaneum KW - Papyrus PY - 2022 AN - OPUS4-54892 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - ISO-G-Scope Standardisation of structural and chemical properties of graphene N2 - The objectives and tasks of the EMPIR project ISO-G-Scope are presented. The last results was shown. Esspecially, the interlaboratory comparison about XPS of functionalized graphene is presented. T2 - DIN NA062-08-16 Oberflächenanalytik Frühjahrstreffen CY - Berlin, Germany DA - 11.05.2022 KW - Graphene KW - Standardization KW - Structural characterisation KW - Chemical composition PY - 2022 AN - OPUS4-54834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - VAMAS Project A33: Chemical composition of functionalized graphene with X ray photoelectron spectroscopy (XPS) N2 - The results of the interlaboratory comparison about the chemical composition of functionalized graphene are presented. T2 - DIN Meeting NA 062-08-16 AA CY - Berlin, Germany DA - 25.05.2023 KW - X-ray photoelectron spectroscopy KW - Functionalized graphene KW - Interlaboratory comparison KW - VAMAS PY - 2023 AN - OPUS4-57650 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Rabin, Ira ED - Russel, R.E. ED - Lange, A. T1 - Non-invasive Analytic Tools in Studies of Manuscripts N2 - Physico-chemical analyses of writing materials offer insight into various questions associated with historical, cultural, and conservational aspects of manuscript studies. The catalogue of questions that can be addressed with these methods includes authenticity, dating, the attribution of various parts of the text to different scribes and the relation between the primary and secondary texts. Similarly, preservation of the manuscripts requires knowledge of the composition of the original materials versus old repairs, identification of damage, as well as recognition of natural aging and degradation processes. The material sciences can contribute data about the chemical compositions of the writing materials, elucidation of the techniques of their production and the absolute age of organic components, as well as characterization of corrosion effects, evaluation of conservation treatment, and monitoring of the preservation state. KW - Material Analysis KW - Manuscripts PY - 2023 SN - 2468-3027 VL - 3D SP - 114 EP - 116 PB - Brill CY - Leiden / Boston AN - OPUS4-58912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine A1 - Lorenzoni, Renata A1 - Telong, Melissa A1 - Lauinger, Robert A1 - Munsch, Sarah Mandy A1 - Schmidt, Wolfram T1 - Investigation of the hydration of clinker-reduced cementitious binders by 1H NMR N2 - In this paper, we demonstrate the value of 1H NMR relaxometry for studying the hydration of clinker-reduced, more climate-friendly cementitious binders. The results were obtained on typical CEM I cements and sister samples containing two different reactive agricultural ashes as well as non-reactive biochars as supplementary cementitious materials. The findings prove that time-resolved NMR measurements provide valuable additional information when combined with classical heat flow calorimetry. T2 - International Conference on Electromagnetic Wave Interaction with Water and Moist Substances of the International Society for Electromagnetic Aquametry (ISEMA) 2023 CY - Brisbane, Ausralia DA - 25.09.2023 KW - Carbon emission KW - 1H NMR relaxometry KW - Heat flow calorimetry KW - Cement, hydration KW - Clinker reduction PY - 2023 SP - 1 EP - 3 AN - OPUS4-58936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bretz, S. A1 - Hagnau, C. A1 - Hahn, Oliver A1 - Ranz, H.-J. ED - Bretz, S. ED - Hagnau, C. ED - Hahn, Oliver ED - Ranz, H.-J. T1 - Kunsthistorische, kunsttechnologische und materialanalytische Untersuchungen an deutscher und niederländischer Hinterglasmalerei von 1300 bis 1600 N2 - Die wissenschaftliche Auseinandersetzung mit Kunst- und Kulturgut schließt neben kunsthistorischen Untersuchungen zunehmend kunsttechnologische und materialwissenschaftliche Analysen mit ein. Der folgende Beitrag fasst die Erkenntnisse der fächerübergreifenden Forschung an deutschen und niederländischen Hinterglasmalereien des 14. bis 16. Jahrhunderts zusammen und soll einen Beitrag zur Neubewertung der Kunstgattung leisten. Nach einer Positionsbestimmung der Hinterglasmalerei gegenüber der Glas- und Tafelmalerei wird auf den Herstellungsprozess ein gegangen, wobei eine detaillierte Beschreibung der Ausgestaltung von Hinterglasbildern mit Schwarzlot, Lüsterfarben und Blattmetallen (Eglomisé) sowie deckenden Malfarben vorgenommen wird. KW - Archäometrie KW - Kunst- und Kulturgut KW - ZfP PY - 2016 SN - 978-3-422-07262-6 SP - 46 EP - 67 PB - Deutscher Kunstverlag CY - Berlin AN - OPUS4-63590 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bretz, S. A1 - Hagnau, C. A1 - Hahn, Oliver A1 - Ranz, H.-J. ED - Bretz, S. ED - Hagnau, C. ED - Hahn, Oliver ED - Ranz, H.-J. T1 - Glas als Bildträger und Rahmungen in der spätmittelalterlichen Hinterglasmalerei N2 - Da in der Hinterglasmalerei der durchsichtige Malgrund und Bildträger stets sichtbar bleibt, kam der Auswahl des Glases eine große Bedeutung zu. Glasmaler wie auch Hinterglasmaler strebten danach, qualitätvolles Glas zu bearbeiten, welches optische Verzerrungen und Spitzlichter ausschloss. Untersuchungen an Hinterglasbildern aus dem 14. bis 16. Jahrhundert zeigen, dass dies bei spätmittelalterlichen Gläsern nicht immer der Fall war. An den gläsernen Bildträgern lassen sich aufgrund typischer Beschaffenheitsmerkmale wie oberflächlicher Unebenheiten und Schlieren, Abdruckspuren des eingesetzten Arbeitswerkzeuges, eingeschlossener Gasbläschen und bearbeiteter Kanten Rückschlüsse auf die Methode ihrer Herstellung ziehen. Die fragilen Glastafeln verlangen nach schützenden Rahmungen, die in verschiedenen Konstruktionsformen als hölzerne Rahmen und/oder Bleiruten ausgeführt wurden. Der untersuchte Bestand an Hinterglasgemälden umfasst zumeist Einzelbilder, doch sind auch Triptychen und ein Deckelkästchen mit Hinterglaseinlagen vertreten. KW - Archäometrie KW - Kunst- und Kulturgut KW - ZfP PY - 2016 SN - 978-3-422-07262-6 SP - 102 EP - 109 PB - Deutscher Kunstverlag CY - Berlin AN - OPUS4-63592 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bretz, S. A1 - Hagnau, C. A1 - Hahn, Oliver A1 - Ranz, H.-J. ED - Bretz, S. ED - Hagnau, C. ED - Hahn, Oliver ED - Ranz, H.-J. T1 - Nachahmung oder Fälschung? Hinterglasbilder aus dem Spätmittelalter oder dem 19. Jahrhundert N2 - Die kunsthistorische Forschung befasst sich immer wieder mit der Frage, ob es sich bei Kunstwerken um Originale, Kopien oder Fälschungen handelt. Die Kunstfälschung hat eine lange Tradition und wurde in allen Gattungen ausgeübt. Handelt es sich bei einer Fälschung um die getreue Wiedergabe eines Originals oder die Neuschöpfung eines Kunstwerks als Imitation einer gewissen Zeitspanne mit betrügerischer Intention, so stehen dem die Kopie und die eigene künstlerische Schöpfung entgegen. Insbesondere im 19. Jahrhundert war bedingt durch die intensive Sammelleidenschaft die Nachfrage nach erlesenen Kunstwerken sehr hoch, ebenso wie die Konkurrenz der Sammler untereinander. Und so verführte die Spezialisierung auf ein Sammelgebiet Händler dazu, immer mehr Ware herbeizuschaffen. Unter diesen Gesichtspunkten sind auch einige Werke der Hinterglasmalerei, die bislang dem 14. bis 16. Jahrhundert zugeordnet werden, hinsichtlich ihrer Datierung zu überprüfen. KW - Archäometrie KW - Kunst- und Kulturgut KW - ZfP PY - 2016 SN - 978-3-422-07262-6 SP - 128 EP - 135 PB - Deutscher Kunstverlag CY - Berlin AN - OPUS4-63594 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bretz, S. A1 - Hagnau, C. A1 - Hahn, Oliver A1 - Ranz, H.-J. ED - Bretz, S. ED - Hagnau, C. ED - Hahn, Oliver ED - Ranz, H.-J. T1 - Hinterglasmalerei des 14. bis 16. Jahrhunderts in weiteren Regionen Europas N2 - Die Produktion qualitätvoller Hinterglasbilder aus dem 14. bis 16. Jahrhundert beschränkte sich nicht auf die niederländischen und deutschen bzw. ober- bis niederrheinischen Kunstlandschaften. Es haben sich ebenso prachtvolle Werke aus Frankreich (Burgund), Süddeutschland und Italien erhalten. Da zusätzlich zu den diskutierten Katalognummern weitere Hinterglasbilder kunstwissenschaftlich und materialtechnologisch untersucht wurden, werden diese im Folgenden beispielhaft vorgestellt. KW - Archäometrie KW - Kunst- und Kulturgut KW - ZfP PY - 2016 SN - 978-3-422-07262-6 SP - 120 EP - 125 PB - Deutscher Kunstverlag CY - Berlin AN - OPUS4-63593 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Bretz, S. A1 - Hagnau, C. A1 - Hahn, Oliver A1 - Ranz, H.-J. ED - Bretz, S. ED - Hagnau, C. ED - Hahn, Oliver ED - Ranz, H.-J. T1 - Einführung in die Hinterglasmalerei N2 - Die Hinterglasmalerei fand als Zwischengattung der Glas- und Tafelmalerei eher wenig Beachtung, war sie doch lange mit dem Begriff der Glasmalerei belegt. Dieses geschah jedoch zu Unrecht, wie die Auswahl an Hinterglasbildern, die in dieser Publikation vorgestellt wird, eindrucksvoll belegt. Auch wenn Glas in beiden Fällen das Trägermaterial darstellt, wird in der Hinterglasmalerei die Rückseite der Glastafel mit organisch gebundenen Malfarben verziert, während aufzubrennende Schmelzfarben das Glas in der Glasmalerei schmücken. Der wesentliche Unterschied offenbart sich in der Lichtführung: Hinterglasbilder werden ausschließlich bei auffallendem Licht betrachtet. Der Malvorgang bei hintermalten Gläsern verläuft grundsätzlich von vorne nach hinten, da der Malgrund zugleich die Schauseite darstellt. KW - Archäometrie KW - Kunst- und Kulturgut KW - ZfP PY - 2016 SN - 978-3-422-07262-6 SP - 12 EP - 13 PB - Deutscher Kunstverlag CY - Berlin AN - OPUS4-63562 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Helfenstein, J. A1 - Massey, M. A1 - Sekine, R. A1 - Kretzschmar, R. A1 - Beiping, L. A1 - Peter, T. A1 - Chadwick, O. A1 - Tamburini, F. A1 - Rivard, C. A1 - Herzel, Hannes A1 - Adam, Christian A1 - Pradas del Real, A. A1 - Castillo-Michel, H. A1 - Zuin, L. A1 - Wang, D. A1 - Félix, R. A1 - Lassalle-Kaiser, B. A1 - Frossard, E. T1 - Microspectroscopy reveals dust-derived apatite grains in acidic, highly-weathered Hawaiian soils N2 - Dust deposition is an important source of phosphorus (P) to many ecosystems. However, there is little evidence of dust-derived P-containing minerals in soils. Here we studied P forms along a well-described climatic Gradient on Hawaii, which is also a dust deposition gradient. Soil mineralogy and soil P forms from six sites along the climatic gradient were analyzed with bulk (X-ray diffraction and P K-edge X-ray absorption near edge structure) and microscale (X-ray fluorescence, P K-edge X-ray absorption near edge structure, and Raman) analysis methods. In the wettest soils, apatite grains ranging from 5 to 30 μm in size were co-located at the micro-scale with quartz, a known continental dust indicator suggesting recent atmospheric deposition. In addition to co-location with quartz, further evidence of dust-derived P included backward trajectory modeling indicating that dust particles could be brought to Hawaii from the major global dust-loading areas in central Asia and northern Africa. Although it is not certain whether the individual observed apatite grains were derived from long-distance transport of dust, or from local dust sources such as volcanic ash or windblown fertilizer, these observations offer direct evidence that P-containing minerals have reached surface layers of highly-weathered grassland soils through atmospheric deposition. KW - Phosphorus KW - soil KW - microspectroscopy KW - Raman spectroscopy KW - XANES spectroscopy KW - x-ray diffraction PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-511522 DO - https://doi.org/10.1016/j.geoderma.2020.114681 SN - 0166-0918 SN - 1872-6259 VL - 381 SP - 114681-1 EP - 114681-11 PB - Elsevier CY - Amsterdam AN - OPUS4-51152 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Hoffmann, Marie A1 - Krüger, O. A1 - Murzin, V. A1 - Caliebe, W. A1 - Adam, Christian T1 - Chromium (VI) in phosphorus fertilizers determined with the diffusive gradients in thin-films (DGT) technique N2 - Phosphorus (P) fertilizers from secondary resources became increasingly important in the last years. However, these novel P-fertilizers can also contain toxic pollutants such as chromium in its hexavalent state (Cr(VI)). This hazardous form of chromium is therefore regulated with low limit values for agricultural products even though the correct determination of Cr(VI) in these fertilizers may be hampered by redox processes, leading to false results. Thus, we applied the novel diffusive gradients in thin-films (DGT) technique for Cr(VI) in fertilizers and compared the results with the standard wet chemical extraction method (German norm DIN EN 15192) and Cr K-edge X-ray Absorption near-edge structure (XANES) spectroscopy. We determined an overall good correlation between the wet chemical extraction and the DGT method. DGT was very sensitive and for most tested materials selective for the analysis of Cr(VI) in P-fertilizers. However, hardly soluble Cr(VI) compounds cannot be detected with the DGT method since only mobile Cr(VI) is analyzed. Furthermore, Cr K-edge XANES spectroscopy showed that the DGT binding layer also adsorbs small amounts of mobile Cr(III) so that Cr(VI) values are overestimated. Since certain types of the P fertilizers contain mobile Cr(III) or partly immobile Cr(VI), it is necessary to optimize the DGT binding layers to avoid aforementioned over- or underestimation. Furthermore, our investigations showed that the Cr K-edge XANES spectroscopy technique is unsuitable to determine small amounts of Cr(VI) in fertilizers (below approx. 1% of Cr(VI) in relation to total Cr). KW - Phosphorus fertilizer KW - Sewage sludge ash KW - Diffusive Gradients in thin films (DGT) KW - Chemical extraction KW - XANES spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509578 DO - https://doi.org/10.1007/s11356-020-08761-w SN - 0944-1344 VL - 27 SP - 24320 EP - 24328 PB - Springer AN - OPUS4-50957 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, Xunyu A1 - Riedel, Jens A1 - You, Yi T1 - Spectrally resolved lithium isotope quantification through high-resolution spatial heterodyne spectrometry N2 - Isotope ratio determination of lithium is increasingly important in fields ranging from geochemistry to battery diagnostics. While mass spectrometry remains the gold standard, it is costly, cumbersome, and incompatible with portable or inline implementations. Optical emission spectroscopy presents an appealing alternative. However, it is traditionally limited by insufficient spectral resolution or resolving power to separate lithium isotope emissions due to their generalized designs for a wide spectral range; this often requires overly complicated algorithms to overcome the instrumental drawbacks. (79) Results Here, we report a high-resolution optical method for lithium isotope quantification using a custom-built spatial heterodyne spectrometer (SHS) combined with a reduced-pressure glow discharge source. This configuration yielded a resolving power of 189,000 and enabled baseline resolution of lithium d-line emission features even without the need for preliminary data processing. Despite the inherent low sensitivity of SHS, a detection limit of 30 pmol was achieved using a standard industrial camera. To improve quantitative accuracy, we introduced a deconvolution-based spectral lineshape recovery technique alongside a bootstrapping-based error propagation strategy. These methods facilitated robust isotope ratio calibration using both peak-height and peak-area metrics. The SHS platform additionally enabled the determination of relative transition probabilities, suggesting the feasibility of calibration-free operation. This work demonstrates the practical viability of SHS for high-specificity, high-resolution lithium isotope analysis. The approach is compact, potentially field-deployable, and adaptable to other elements with optically resolvable isotope shifts, offering a route toward accessible and calibration-free optical isotopic analyses. KW - SHS KW - Isotope KW - High-resolution spectroscopy PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-635139 DO - https://doi.org/10.1016/j.aca.2025.344329 SN - 1873-4324 VL - 1368 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-63513 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laquai, René A1 - Müller, Bernd R. A1 - Kasperovich, G. A1 - Haubrich, J. A1 - Requena, G. A1 - Bruno, Giovanni T1 - X-ray refraction distinguishes unprocessed powder from empty pores in selective laser melting Ti-6Al-4V N2 - For the first time, X-ray refraction techniques are proven for the identification of void formation in Ti-6Al-4V parts produced by selective laser melting. The topology and volume fraction of pores are measured in samples produced with different laser energy density. Unique X-ray refraction methods identify different kinds of defects, characteristic to the regions below and above the Optimum laser energy density, namely unprocessed powder (unmolten powder particles, balling effect, and Fusion defects) from empty keyhole pores. Furthermore, it is possible to detect small inhomogeneities (voids or cracks) with sizes below the spatial resolution of optical microscopy and X-ray computed tomography. KW - Additive manufacturing KW - X-ray refraction KW - Microscopy KW - X-ray computed tomography KW - Porosity PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-434041 DO - https://doi.org/10.1080/21663831.2017.1409288 SN - 2166-3831 VL - 6 IS - 2 SP - 130 EP - 135 PB - Taylor & Francis Group CY - London, UK AN - OPUS4-43404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Radnik, Jörg T1 - Correlating HR-TEM and XPS to elucidate the core-shell structure of ultrabright CdSE/CdS semiconductor quantum dots N2 - Controlling the thickness and tightness of surface passivation shells is crucial for many applications of core-shell nanoparticles (NP). Usually, to determine shell thickness, core and core/shell particle are measured individually requiring the availability of both nanoobjects. This is often not fulfilled for functional nanomaterials such as many photoluminescent semiconductor quantum dots (QD) used for bioimaging, solid state lighting, and display technologies as the core does not show the application-relevant functionality like a high photoluminescence (PL) quantum yield. This calls for a whole nanoobject approach. Moreover, the thickness of the organic coating remains often unclear. By combining high-resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS), a novel whole nanoobject approach is developed representatively for an ultrabright oleic acid-stabilized, thick shell CdSe/CdS QD with a PL quantum yield close to unity. The size of this spectroscopically assessed QD, is in the range of the information depth of usual laboratory XPS. Information on particle size and monodispersity were validated with dynamic light scattering (DLS) and small angle X-ray scattering (SAXS) and compared to data derived from optical measurements. The results of the different methods match very well within the different measurement uncertainties. Additionally, results obtained with energy-resolved XPS using excitation energies between 200 eV and 800 eV are discussed with respect to a potential core/shell intermixing. Moreover, the future application potential of this approach correlating different sizing and structural methods is discussed considering the method-inherent uncertainties and other core/multi-shell nanostructures. T2 - E-MRS Fall Meeting CY - Online meeting DA - 20.09.2021 KW - Core-shell nanoparticles KW - Quantum dots KW - High-resolution transmission electron microscopy KW - X-ray Photoelectron Spectroscopy PY - 2021 AN - OPUS4-53365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauli, Jutta A1 - Würth, Christian A1 - Güttler, Arne A1 - Resch-Genger, Ute T1 - Reliable Determination of the Signal-Relevant Spectroscopic Key Characteristics of Luminescent Reporters and Optical Probes for Imaging in the vis/NIR/SWIR N2 - Introduction. Comparing different emitter classes and rationally designing the next generation of molecular and nanoscale probes for bioimaging applications require accurate and quantitative methods for the measurement of the key parameter photoluminescence quantum yield f.1 f equals the number of emitted per number of absorbed photons. This is particularly relevant for increasingly used fluorescence imaging in the short wave-infrared region (SWIR) ≥ 900 nm providing deeper penetration depths, a better image resolution, and an improved signal-to-noise or tumor-to-background ratio.2, 3 However, spectroscopic measurements in the SWIR are more challenging and require specific calibrations and standards. T2 - EMIM 2021 CY - Göttingen, Germany DA - 24.08.2021 KW - Fluorescence KW - Optical probe KW - Dye KW - Photophysics KW - Quantum yield KW - Mechanism KW - NIR KW - SWIR KW - Imaging KW - Reference material KW - Reliability KW - Nano KW - Particle KW - Method KW - Quality assurance PY - 2021 AN - OPUS4-53233 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Relling, Alexander T1 - Copper doped AgInS2-ZnS QDs from a single-source-precursor N2 - Quaternary semiconductor nanocrystals like AgInS2-ZnS solid solution quantum dots (QDs) are a highly promising material for material science and biomedical applications due to their tunable photoluminescence (PL), their high quantum yields (QY), and their low cytotoxicity1. A red shift of the PL into the NIR and SWIR region could further increase their application potential. Copper doping has been proven to be a suitable approach for bathochromically shifting the PL of QDs2. The synthesis of copper doped AgInS2-ZnS QDs from a single-source-precursor should enable an easily scalable synthesis with high reproducibility. T2 - Summer School "Exciting nanostructures: characterizing advanced confined systems" CY - Bad Honnef, Germany DA - 18.07.2021 KW - Nanocrystals KW - Quantum dots KW - Doping KW - AgInS2 KW - Single-source-precursor PY - 2021 AN - OPUS4-53129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bandi, V.G. A1 - Luciano, M.P. A1 - Saccomano, M. A1 - Patel, N.L. A1 - Bischof, Th. S. A1 - Lingg, J.G.P. A1 - Tsrunchev, P.T. A1 - Nix, M.N. A1 - Ruehle, Bastian A1 - Sanders, C. A1 - Riffle, L. A1 - Robinson, C.M. A1 - Difilippantonio, S. A1 - Kalen, J.D. A1 - Resch-Genger, Ute A1 - Ivanic, J. A1 - Bruns, O.T. A1 - Schnermann, M. T1 - Targeted multicolor in vivo imaging over 1,000 nm enabled by nonamethine cyanines N2 - Recent progress has shown that using wavelengths between 1,000 and 2,000 nm, referred to as the shortwave-infrared or near-infrared (NIR)-II range, can enable high-resolution in vivo imaging at depths not possible with conventional optical wavelengths. However, few bioconjugatable probes of the type that have proven invaluable for multiplexed imaging in the visible and NIR range are available for imaging these wavelengths. Using rational design, we have generated persulfonated indocyanine dyes with absorbance maxima at 872 and 1,072 nm through catechol-ring and aryl-ring fusion, respectively, onto the nonamethine scaffold. Multiplexed two-color and three-color in vivo imaging using monoclonal antibody and dextran conjugates in several tumor models illustrate the benefits of concurrent labeling of the tumor and healthy surrounding tissue and lymphatics. These efforts are enabled by complementary advances in a custom-built NIR/shortwave-infrared imaging setup and software package for multicolor real-time imaging. KW - Photoluminescence KW - Fluorescence KW - Dye KW - Cyanine KW - Antibody KW - Bioconjugate KW - Conjugate KW - Quantum yield KW - Photophysics KW - Lifetime KW - Sensor KW - NIR KW - SWIR KW - Mechanism KW - Imaging KW - Application KW - Contrast agent KW - Bioimaging PY - 2021 DO - https://doi.org/10.1038/s41592-022-01394-6 VL - 19 IS - 3 SP - 353 EP - 358 PB - Nature Research AN - OPUS4-54465 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Daly, H.C A1 - Matikonda, S.S A1 - Steffens, H.C A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Ivanic, J. A1 - Schermann, M.J T1 - Daly_Photochem Photobiol 2021_Ketone Incorporation Extends the Emission Properties of the Xanthene Scaffold N2 - Imaging in the shortwave-infrared region (SWIR, λ = 1000–2500 nm) has the potential to enable deep tissue imaging with high resolution. Critical to the development of these Methods is the identification of low molecular weight, biologically compatible fluorescent probes that emit beyond 1000 nm. Exchanging the bridging oxygen atom on the xanthene scaffold (C10’ position) with electron withdrawing groups has been shown to lead to significant redshifts in absorbance and emission. Guided by quantum chemistry computational modeling studies, we investigated the installation of a Ketone bridge at the C10’ position. This simple modification extends the absorbance maxima to 860 nm and the emission beyond 1000 nm, albeit with reduced photon output. Overall, These studies demonstrate that broadly applied xanthene dyes can be extended into the SWIR range. KW - Flourescence KW - Optical probe KW - Dye KW - Photophysics KW - Quantum yield KW - Mechanism KW - NIR KW - SWIR KW - Imaging KW - Reliability KW - Method KW - Quality assurance PY - 2021 DO - https://doi.org/10.1111/php.13544 SN - 1751-1097 VL - 98 IS - 2 SP - 325 EP - 333 PB - Wiley Online Library AN - OPUS4-54080 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bertorelle, F. A1 - Wegner, Karl David A1 - Berkulic, M. P. A1 - Fakhouri, H. A1 - Comby-Zerbino, C. A1 - Sagar, A. A1 - Bernadó, P. A1 - Resch-Genger, Ute A1 - Bonacic-Koutecký, V. A1 - Le Guével, X. A1 - Antoine, R. T1 - Tailoring the NIR-II Photoluminescence of Single Thiolated Au25 Nanoclusters by Selective Binding to Proteins N2 - Atomically precise gold nanoclusters are a fascinating class of nanomaterials that exhibit molecule-like properties and have outstanding photoluminescence (PL). Their ultrasmall size, molecular chemistry, and biocompatibility make them extremely appealing for selective biomolecule labeling in investigations of biological mechanisms at the cellular and anatomical levels. In this work, we report a simple route to incorporate a preformed Au25 nanocluster into a model bovine serum albumin (BSA) protein. A new approach combining small-angle X-ray scattering and molecular modeling provides a clear localization of a single Au25 within the protein to a cysteine residue on the gold nanocluster surface. Attaching Au25 to BSA strikingly modifies the PL properties with enhancement and a redshift in the second near-infrared (NIR-II) window. This study paves the way to conrol the design of selective sensitive probes in biomolecules through a ligand-based strategy to enable the optical detection of biomolecules in a cellular environment by live imaging. KW - Fluorescence KW - Aggregation KW - Signal enhancement KW - Cluster KW - Nano KW - Metal KW - NIRII KW - SWIR KW - Sensor KW - Quantum yield KW - Lifetime KW - Photophysics KW - Synthesis KW - Protein KW - Imaging KW - Bioimaging KW - Ligand KW - Gold PY - 2022 DO - https://doi.org/10.1002/chem.202200570 SN - 1521-3765 VL - 28 IS - 39 SP - 1 EP - 8 PB - Wiley-VCH CY - Weinheim AN - OPUS4-55077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wang, Cui A1 - Reichenauer, F. A1 - Kitzmann, W.R. A1 - Kerzig, Ch. A1 - Heintze, K. A1 - Resch-Genger, Ute T1 - Efficient Triplet-Triplet Annihilation Upconversion Sensitized by a Chromium(III) Complex via an Underexplored Energy Transfer Mechanism N2 - Sensitized triplet-triplet annihilation upconversion (sTTA-UC) mainly relies on precious metal complexes thanks to their high intersystem crossing (ISC) efficiencies, excited state energies, and lifetimes, while complexes of abundant first-row transition metals were only rarely utilized and with often moderate UC quantum yields. [Cr(bpmp)2]3+ (bpmp = 2,6-bis(2-pyridylmethyl)pyridine) containing earth-abundant chromium possesses an absorption band suitable for green light excitation, a doublet excited state energy matching the triplet energy of 9,10-diphenyl anthracene (DPA), a close to millisecond excited state lifetime, and high photostability. Combined ISC and doublet-triplet energy transfer from excited [Cr(bpmp)2]3+ to DPA gives 3DPA with close-to-unity quantum yield. TTA of 3DPA furnishes greento-blue UC with a quantum yield of 12.0 % (close to the theoretical maximum). Sterically less-hindered anthracenes undergo a [4+4] cycloaddition with [Cr(bpmp)2]3+ and green light. KW - Fluorescence KW - Optical probe KW - Sensor KW - ph KW - Quantum yield KW - Quality assurance KW - Cr(III) KW - Lifetime KW - Ligand KW - Theory KW - TTA-UC KW - Energy transfer KW - Upconversion KW - Mechanism KW - Anthracene KW - Photochemistry KW - DFT KW - Cycloaddition KW - Transient absorbtion spectroscopy PY - 2022 DO - https://doi.org/10.1002/anie.202202238 VL - 61 IS - 24 SP - 1 EP - 8 PB - Wiley online library AN - OPUS4-54604 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pasquato, Leone T1 - Embedded Sensors System to Monitor Cemented Waste Drums N2 - BAM (Federal Institute for Materials Research and Testing) is developing an electronic measurement system to be placed inside a waste drum, which will be filled with concrete. The goal of this measurement system is to monitor the process of hardening and the evolution of the concrete itself over time to indirectly identify potential defects such as corrosion or cracking. The measured parameters are humidity, temperature, and pressure. In this regard, particular attention was given to the design of the electronic board’s enclosure, to allow the sensors to measure the state of the concrete without being in direct contact with it. In the scope of the European Commission’s project of PREDIS, the supply of power to the battery-less sensors and the data acquired by such sensors are transmitted through the metallic waste drum by an innovative wireless technology developed by VTT (Technical Research Centre of Finland) in order to ensure long-term operation while keeping the integrity of the sealed container. T2 - SafeND Conference CY - Berlin, Germany DA - 13.09.2023 KW - RFID KW - Moisture KW - Embedded Sensors KW - Nuclear Waste PY - 2023 AN - OPUS4-58774 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pasquato, Leone T1 - Embedded Sensors System to Monitor Cemented Waste Drums N2 - BAM is developing an electronic measurement system to be placed inside a waste drum, which will be filled with concrete. The goal of this measurement system is to monitor the process of hardening and the evolution of the concrete itself over time to indirectly identify potential defects such as corrosion or cracking. The measured parameters are humidity, temperature, and pressure. In this regard, particular attention was given to the design of the electronic board’s enclosure, to allow the sensors to measure the state of the concrete without being in direct contact with it. In the scope of the EU project PREDIS, the data acquired by such sensors are transmitted from inside to outside the metallic waste drum through wireless technology. The sensing system is made of a chain of small sensing units, called SensorNodes. Each SensorNode includes two off-the-shelf sensors, one for relative humidity and temperature and one for pressure and temperature. A SensorNode is designed to have a unique identifier, in order to be connected to other units while being uniquely discoverable by a standard communication protocol. In this way, a distributed matrix of measurement points is created. One of the most challenging tasks in designing a measurement system to run in a harsh environment (such as hardening concrete) is to let the sensors sense the external environment without damaging the sensor itself. To keep the external environment away from the electronic board while still letting the sensors measure the concrete behavior, holes have been drilled through the lid and covered from the inside with a layer of a porous membrane. The membrane's pores allow water and gas particles to pass through and let the enclosed air equilibrate with the external environment. With the help of the developed sensors, monitoring concrete in cemented waste drums will be possible. The derived data will also serve as the basis for ongoing modeling approaches for digital twins within the Predis project. Overall, the sensors provide a means of enabling safe nuclear waste management through advanced monitoring T2 - ASME 2023 International Conference on Environmental Remediation and Radioactive Waste Management CY - Stuttgart, Germany DA - 03.10.2023 KW - RFID KW - Moisture KW - Embedded Sensors KW - Nuclear Waste PY - 2023 AN - OPUS4-58775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Herter, Sven-Oliver A1 - Haase, Hajo A1 - Koch, Matthias T1 - Semisynthesis of Stable Isotope-Labeled Ergot Alkaloids for HPLC-MS/MS Analysis N2 - Ergot alkaloids (EAs) are prevalent food contaminants affecting cereals, such as rye, wheat, and barley worldwide. To ensure EU safety standards, the six most common EAs: ergometrine, ergotamine, ergosine, ergocornine, ergocristine, and ergocryptine, and their epimers, are quantified using HPLC-MS/MS, as described in the European Standard Method EN 17425:2021. However, this can be challenging and time-consuming in food matrices without appropriate internal standards and highlights the need for more robust and precise analytical tools to support their monitoring. The development of isotope-labeled EAs directly addresses this gap, offering improved accuracy and leading to more consistency across laboratories and consequently to more consumer safety. Therefore, we developed a semisynthetic approach, building upon our previous work where native ergotamine was N6-demethylated to norergotamine and subsequently remethylated using iodomethane (13CD3-I). Herein, we are now able to present the successful synthesis of all of the isotopically labeled priority EAs. These isotope-labeled standards were tested against their native counterparts using HPLC coupled with HR-MS/MS. The chromatographic and mass spectrometric properties of the unlabeled and isotopically labeled EAs match exactly, confirming their successful synthesis and structure. These standards can now be utilized to enhance the accuracy and reliability of EA quantification in food and feed. KW - Reference Material KW - HPLC-MS/MS KW - Mycotoxins KW - Ergot Alkaloids KW - Stable Isotope Dilution Analysis KW - Semisynthesis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639692 DO - https://doi.org/10.1021/acs.jafc.5c03345 SN - 0021-8561 VL - 73 IS - 29 SP - 18412 EP - 18419 PB - American Chemical Society (ACS) AN - OPUS4-63969 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keller, Julia A1 - Borzekowski, Antje A1 - Haase, H. A1 - Menzel, R. A1 - Rueß, L. A1 - Koch, Matthias T1 - Toxicity assay for citrinin, zearalenone and zearalenone-14-sulfate using the nematode Caenorhabditis elegans as model organism N2 - To keep pace with the rising number of detected mycotoxins, there is a growing need for fast and reliable toxicity tests to assess the potential threat to food safety. Toxicity tests with the bacterial-feeding nematode Caenorhabditis elegans as model organism are well established. In this study the C. elegans wildtype strain N2 (var. Bristol) was used to investigate the toxic effects of the food-relevant mycotoxins citrinin (CIT) and zearalenone-14-sulfate (ZEA-14-S) and zearalenone (ZEA) on different life cycle parameters including reproduction, thermal and oxidative stress resistance and lifespan. The metabolization of the mycotoxins by the nematodes in vivo was investigated using HPLC-MS/MS. ZEA was metabolized in vivo to the reduced isomers α-zearalenol (α-ZEL) and β-ZEL. ZEA 14-S was reduced to α-/β-ZEL 14-sulfate and CIT was metabolized to mono-hydroxylated CIT. All mycotoxins tested led to a significant decrease in the number of nematode offspring produced. ZEA and CIT displayed negative effects on stress tolerance levels and for CIT an additional shortening of the mean lifespan was observed. In the case of ZEA-14-S, however, the mean lifespan was prolonged. The presented study shows the applicability of C. elegans for toxicity testing of emerging food mycotoxins for the purpose of assigning potential health threats. KW - Mycotoxins KW - Metabolization KW - Toxicity testing KW - Biotests PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-455772 DO - https://doi.org/10.3390/toxins10070284 VL - 10 IS - 7 SP - 284, 1 EP - 12 PB - MDPI AN - OPUS4-45577 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winckelmann, Alexander A1 - Morcillo Garcia-Morato, Dalia A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Riedel, Jens A1 - Vogl, Jochen A1 - Panne, Ulrich A1 - Abad Andrade, Carlos Enrique T1 - Determination of lithium in human serum by isotope dilution atomic absorption spectrometry N2 - The therapeutic dose of lithium (Li) compounds, which are widely used for the treatment of psychiatric and hematologic disorders, is close to its toxic level; therefore, drug monitoring protocols are mandatory. Herein, we propose a fast, simple, and low-cost analytical procedure for the traceable determination of Li concentration in human serum, based on the monitoring of the Li isotope dilution through the partially resolved isotope shift in its electronic transition around 670.80 nm using a commercially available high-resolution continuum source graphite furnace atomic absorption spectrometer. With this technique, serum samples only require acidic digestion before analysis. The procedure requires three measurements—an enriched 6Li spike, a mixture of a certified standard solution and spike, and a mixture of the sample and spike with a nominal 7Li/6Li ratio of 0.82. Lanthanum has been used as an internal spectral standard for wavelength correction. The spectra are described as the linear superposition of the contributions of the respective isotopes, each consisting of a spin-orbit doublet, which can be expressed as Gaussian components with constant spectral position and width and different relative intensity, reflecting the isotope ratio in the sample. Both the spectral constants and the correlation between isotope ratio and relative band intensity have been experimentally obtained using commercially available materials enriched with Li isotopes. The Li characteristic mass (mc) obtained corresponds to 0.6 pg. The procedure has been validated using five human serum certified reference materials. The results are metrologically comparable and compatible to the certified values. The measurement uncertainties are comparable to those obtained by the more complex and expensive technique, isotope dilution mass spectrometry. KW - Lithium KW - Human serum KW - Isotope dilution KW - Atomic absorption spectrometry KW - High-resolution continuum source graphite furnace atomic absorption spectrometry PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-532446 DO - https://doi.org/10.1007/s00216-021-03636-6 VL - 414 IS - 1 SP - 251 EP - 256 PB - Springer CY - Berlin AN - OPUS4-53244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Lisec, Jan A1 - Jaeger, C. ED - Antonio, C. T1 - Statistical and Multivariate Analysis of MS-Based Plant Metabolomics Data N2 - Raw data from metabolomics experiments are initially subjected to peak identification and signal deconvolution to generate raw data matrices m × n, where m are samples and n are metabolites. We describe here simple statistical procedures on such multivariate data matrices, all provided as functions in the programming environment R, useful to normalize data, detect biomarkers, and perform sample classification. KW - Mass-Spectrometry KW - Multivariate Statistics PY - 2018 SN - 978-1-4939-7819-9 SN - 978-1-4939-7818-2 DO - https://doi.org/10.1007/978-1-4939-7819-9_20 SN - 1064-3745 SN - 1940-6029 VL - 1778 SP - Chapter 20, 285 EP - 296 PB - Springer-Verlag AN - OPUS4-45492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Standardized Measurements of Surface - Functionalities on Nanoparticles N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, optoelectronics, and information storage. NP function, interaction with biological species, and environmental fate are largely determined by surface functionalities. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, and mandatory to meet increasing concerns regarding their safety. Also, industry, international standardization organizations, regulatory agencies, and policymakers need validated and standardized measurement methods and reference materials. However, methodologies for determining NP surface properties, including the amount, chemical composition, and homogeneity of surface functionalities and coatings are largely non-standardized. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR) as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. The latter less costly methods are often used by SMEs, e.g., for quality control. To validate methods, establish measurement uncertainties, test reference materials, and produce reference data, international interlaboratory comparisons (ILC) on NP surface functionalization measurements are required and well characterized test and reference nanomaterials providing benchmark values.[1] These needs are addressed by the recently started European metrology project SMURFnano involving 12 partners from different National Metrology Institutes, designated institutes, and research institutes, two university groups as well as one large company and one SME producing NPs. This project as well as first results derived from the development of test and reference materials with a well characterized surface chemistry and ongoing interlaboratory comparisons will be presented. T2 - eMRS CY - Strasbourg, France DA - 27.05.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Silica KW - Upconversion nanoparticles KW - Optical assay KW - qNMR KW - Surface analysis KW - Ligand KW - Quantification KW - Functional group KW - XPS KW - ToF-SIMS KW - Polymer particle KW - Surface modification KW - Potentiometry KW - Metrology KW - Method KW - Validation KW - ILC PY - 2025 AN - OPUS4-63339 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Muon tomography applied to assessment of concrete structures: First experiments and simulations. N2 - Non-destructive techniques for reinforced or prestressed concrete inspection such as ultrasound or radar have found regular, successful practical application but sometimes suffer from limited resolution and accuracy, imaging artefacts or restrictions in detecting certain features. Until the 1980s X-ray transmission was used in case of special demands and showed a much better resolution than other NDT techniques. However, due to safety concerns and cost issues, this method is almost never used anymore. Muon tomography has received much attention recently. Novel detectors for cosmic muons and tomographic imaging algorithms have opened new fields of application. As a first step towards practical application in civil engineering and as a proof of concept we used an existing system to image the interior of a reference reinforced 600 kg concrete block. Even with a yet not optimized setup for this kind of investigation, the muon imaging results are at least of similar quality compared to ultrasonic and radar imaging, potentially even better. In a second step, we have performed simulations to assess the potential for a set of important testing problems such as grouting defects in tendon ducts. The next steps include the development of mobile detectors and optimizing acquisition and imaging parameters. T2 - NDT-CE 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Muon tomography KW - Concrete KW - Inspection KW - Simulation PY - 2022 AN - OPUS4-56323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholtz, Lena T1 - Luminescent Polymer Microbeads – Synthesis & Applications N2 - Differently sized, luminescent polymer beads encoded with QDs were prepared with a simple, optimized polymerization procedure. The optical properties of the resulting particles were studied to ensure sufficient fluorescence. In addition, possible future applications were identified. T2 - Future WiNS: New Energies for a Sustainable World CY - Berlin, Germany DA - 07.12.2022 KW - Polymerization KW - Quantum dots KW - Fluorescence KW - Luminescence PY - 2022 AN - OPUS4-56560 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Güttler, Arne A1 - Richter, Maria A1 - Würth, Christian A1 - Resch-Genger, Ute T1 - New Reference Materials for Quantification and Standardization of Fluorescence-based Measurements N2 - Luminescence techniques are amongst the most commonly used analytical methods in the life and material sciences due to their high sensitivity and non-destructive and multiparametric character. Photoluminescence signals are, however, affected by wavelength-, polarization-, and time-dependent instrument specific effects and the compound-specific photoluminescence quantum yield. The former hamper the comparability of fluorescence measurements, while the relative determination of the latter requires suitable quantum yield standards with well-known photoluminescence quantum yields. For the simple correction of instrument specific effects in the wavelength region of 300 nm to 950 nm, the set of the five certified spectral fluorescence standards (CRM) BAM-F001 – BAM-F005, has been extended to the NIR range by including two new fluorescence standards currently under certification. T2 - 17th conference on Methods and Applications in Fluorescence CY - Gothenburg, Sweden DA - 11.09.2022 KW - Luminescence KW - Photoluminescence KW - Fluorescence KW - Quantum yield KW - Certified reference material KW - Standard PY - 2022 AN - OPUS4-56441 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abram, Sarah-Luise A1 - Mrkwitschka, Paul A1 - Thünemann, Andreas A1 - Radnik, Jörg A1 - Häusler, I. A1 - Bresch, Harald A1 - Hodoroaba, Vasile-Dan A1 - Resch-Genger, Ute T1 - Iron Oxide Nanocubes as a New Certified Reference Material for Nanoparticle Size Measurements N2 - The rational design and increasing industrial use of nanomaterials require a reliable characterization of their physicochemical key properties like size, size distribution, shape, and surface chemistry. This calls for nanoscale reference materials (nanoRMs) for the validation and standardization of commonly used characterization methods closely matching real-world nonspherical nano-objects. This encouraged us to develop a nonspherical nanoRM of very small size consisting of 8 nm iron oxide nanocubes (BAM-N012) to complement spherical gold, silica, and polymer nanoRMs. In the following, the development and production of this nanoRM are highlighted including the characterization by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS) as complementary methods for size and shape parameters, homogeneity and stability studies, and calculation of a complete uncertainty budget of the size features. The determination of the nanocubes’ edge length by TEM and SAXS allows a method comparison. In addition, SAXS measurements can also provide the mean particle number density and the mass concentration. The certified size parameters, area equivalent circular diameter and square edge length, determined by TEM with a relative expanded uncertainty below 9%, are metrologically traceable to a natural constant for length, the very precisely known (111) lattice spacing of silicon. Cubic BAM-N012 qualifies as a certified nanoRM for estimating the precision and trueness, validation, and quality assurance of particle size and shape measurements with electron microscopy and SAXS as well as other sizing methods suitable for nanomaterials. The production of this new iron oxide nanocube RM presents an important achievement for the nanomaterial community, nanomaterial manufacturers, and regulators. KW - Certification KW - SAXS KW - Homogeneity KW - Nano KW - Particle KW - Iron oxide KW - Quality assurance KW - Reference material KW - Size KW - Electron microscopy KW - Stability KW - Shape PY - 2023 DO - https://doi.org/10.1021/acs.analchem.3c00749 SN - 0003-2700 VL - 95 IS - 33 SP - 12223 EP - 12231 PB - American Chemical Society CY - Columbus, Ohio AN - OPUS4-58176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan A1 - Niederleithinger, Ernst T1 - Imaging of Ultrasonic Echo Measurements for Reconstruction of Technical Data of Bridges – Possibilities, Limitations and Outlook N2 - When reassessing existing concrete bridges, the challenge is often to obtain missing or incomplete information on the internal structure. In particular, the number and position of the existing reinforcement as well as the geometric dimensions of the components are of interest. Non-destructive testing methods, like radar or ultrasound, which work on the basis of the pulse-echo method, have been established for this purpose, as they only require access to the component from one side. The measurement data recorded on the structure require pre-processing to be able to reproduce the internal structure geometrically accurately. Besides different steps of data processing, the geometrical reconstruction of the measured data based on the Synthetic Aperture Focusing Technique (SAFT) is state of the art today. In this paper, the technical possibilities of the ultrasonic echo method are presented based on measurements in the laboratory and on a real bridge structure. The precision of the reconstruction and its limitations are shown. In addition to the state of the art SAFT technique, open questions and the latest research approaches, such as imaging by reverse time migration (RTM) including initial results are discussed. T2 - 13th German-Japanese Bridge Symposium CY - Osaka, Japan DA - 29.08.2023 KW - Bridge KW - Non destructive testing and evaluation KW - Concrete KW - Validation PY - 2023 SP - 1 EP - 8 AN - OPUS4-58327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kossatz, Philipp T1 - Upconversion Nanoparticles as Luminescent Probes for Cement N2 - Safety is a key parameter for the design and construction of buildings. The most widely used construction material to date is concrete that consists of about 15-20 wt.-% cement, which is responsible for the main concrete properties, i.e., strength and durability. Despite many standards regulating the quality of cement, at present, there exists no viable method to track the cement life cycle “from cradle to grave”. This led to an increasing interest in simple and robust methods for studying the processes and changes occurring during the life cycle of cement. In this context, we explored the applicability of fluorescence measurements which can be performed with relatively inexpensive and miniaturized instrumentation yet require robust optical probes which survive the harsh cement environment. Therefore, we developed a platform of lanthanide-based upconversion nanoparticles (UCNPs), consisting of a NaYF4 matrix doped with Yb3+ and Er3+ with sizes between 20 nm and 55 nm, which show characteristic multi-color emission patterns, composed of narrow bands of varying intensity in the ultraviolet, visible, near-infrared, and short-wave spectral region and examined their potential for cement probing and the non-invasive monitoring of the hydration processes occurring during cement formation. UCNPs of different size and chemical composition were synthesized via a thermal decomposition approach under inert conditions. The tailor-made design of different emission patterns was achieved by tuning particle size and morphology, material composition, and particle surface chemistry in upscaleable syntheses. For cement probing, different types of UCNPs were added to cement and the evolution of the UCNP emission pattern was used to probe in-situ changes of physico-chemical parameters in the cementitious environment during hydration, utilizing a simple and portable custom-designed optical setup. The observed changes in the UCNP emission patterns are characteristic for a given particle size, surface chemistry, and cement composition. In addition to fluorescence measurements, conventional isothermal heat flow calorimetry was used to study the influence of UCNP addition on cement hydration kinetics. Subsequently, both sets of measurements were correlated. Our results underline the potential of our optical approach ad UCNPs for the non-invasive probing of cementitious systems and cement hydration. This can be also exploited for cutting-edge applications of construction materials such as 3D concrete printing. T2 - Summer School Exciting Nanostructures CY - Bad Honnef, Germany DA - 31.07.2023 KW - Cement Hydration KW - Upconversion KW - Fluorescence Spectroscopy PY - 2023 AN - OPUS4-58203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - El Abbassi, Abdelouahad T1 - Multifaceted Nanoparticles: Labeling, Heterostructures, and Aggregation-induced Dual-emission Systems for Advanced Applications N2 - Nanoparticles with novel physico-chemical properties have an impact on various scientific disciplines, including medical diagnostics, energy conversion, catalysis, and solid-state lighting. Here, I present examples from my previous work on organic and inorganic nanoscale systems, such as superparamagnetic iron oxide nanoparticles (SPIONs) for blood platelet labeling and magnetic copper-doped bioactive glasses for bone cancer therapy. Additionally, I provide a first insight into my recently started Ph.D. project focusing on bichromophoric organic fluorophores exhibiting Aggregation-Induced Dual-Emission (AIDE) and their integration into nanostructures for water-dispersible nanoscale reporters and nanosensors. T2 - Bad-Honnef Summer School Exciting Nanostructures 2023 CY - Bad Honnef, Germany DA - 30.07.2023 KW - Nanoparticles KW - AIE KW - SPIONS PY - 2023 AN - OPUS4-58204 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Osipova, Viktoriia T1 - Incorporation of near-infrared light emitting chromium (III) complexes into the core and shell of silica nanoparticles and optimisation of their optical properties N2 - In recent years, chromium (III) complexes have received a lot of attention as novel near-infrared (NIR) emitters. This interest was triggered by the report on the first molecular ruby Cr(ddpd)2(BF4)3 with a high photoluminescence quantum yield of 13.7% of its near infrared (NIR) emission band and a long luminescence lifetime of 1.122 ms at room temperature. Meanwhile, the influence of triplet oxygen, temperature, and pressure on the optical properties of different molecular rubies have been assessed. These features make these molecular rubies promising candidates for multi-analyte optical sensing applications and the generation of singlet oxygen for photocatalysis and photodynamic therapy. However, in an oxygen-containing environment, the photoluminescence quantum yields and luminescence lifetimes of these chromium(III) complexes show only very small values. This hampers their application as NIR luminescence labels. This application, that cannot be tackled by conventional deoxygenating approaches, requires suitable strategies to protect the luminescence of the chromium(III) complexes from oxygen quenching. Typical approaches to reduce the oxygen sensitivity of long-lived luminophores include the encapsulation into an oxygen-shielding matrix or less commonly employed, by tuning the bulkiness of the ligands for oxygen-sensitive coordination compounds. An elegant approach to reduce the undesired luminescence quenching by triplet oxygen explored by us presents the incorporation of these chromium(III) complexes into amorphous, non-porous silica nanoparticles, that can be simply surface functionalized, e.g., with targeting ligands and/or other sensor molecules. This can enable the use of such chromium(III) complexes as reporters for bioanalytical assays and bioimaging without the need to introduce reactive groups into the ligands and can pave the road to lifetime tuning. In this work, as first proof-of-concept experiments, a set of chromium (III) complexes constituting of different ligands and counter anions, were embedded into the core of silica nanoparticles. As an alternative synthesis strategy, selected complexes were incorporated into a silica shell formed around the core of self-made silica nanoparticles. Subsequently, the optical properties of the resulting luminescent silica nanoparticles were spectroscopically assessed by steady state and time-resolved luminescence spectroscopy. First results of time-resolved luminescence measurements of the Cr(ddpd)2(PF6)3 complex incorporated into 25nm large silica nanoparticles dispersed in aerated water in comparison to the decay kinetics obtained for this complex in acetonitrile in air showed an increase in lifetime from 46 µs to 1147 µs. This confirming our design concept of nanoscale NIR emissive Cr(III) reporters. T2 - Bad Honnef summer school CY - Bad Honnef, Germany DA - 30.07.2023 KW - Chromium (III) complexes KW - Silica Nanoparticles KW - Luminescence lifetime measurments PY - 2023 AN - OPUS4-58076 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wegner, Karl David T1 - Exploring the photoluminescence of gold NCs and Ag2S NPs to boost their SWIR emission N2 - Current challenges and objectives for non-invasive optical bioimaging are deep tissue penetration, high detection sensitivity, high spatial and temporal resolution, and fast data acquisition. A promising spectral window to tackle these challenges is the short-wave infrared (SWIR) ranging from 900 nm to 1700 nm where scattering, absorption, and autofluorescence of biological components are strongly reduced compared to the visible/NIR. At present, the best performing SWIR contrast agents are based on nanomaterials containing toxic heavy-metal ions like cadmium or lead, which raises great concerns for biological applications. Promising heavy-metal free nanoscale candidates are gold nanoclusters (AuNCs) and Ag2S nanoparticles (NPs). The photoluminescence (PL) of both types of nanomaterials is very sensitive to their size, composition of their surface ligand shell, and element composition, which provides an elegant handle to fine-tune their absorption and emission features and boost thereby the size of the signals recorded in bioimaging studies. Aiming for the development of SWIR contrast agents with optimum performance, we dived deeper into the photophysical processes occurring in these nanomaterials, thereby exploring in depth how the environment, surface ligand composition, and the incorporation of transition metals influence the optical properties of AuNCs and Ag2S NPs. We observed a strong enhancement of the SWIR emission of AuNCs upon exposure to different local environments (in solution, polymer, and in the solid state). Addition of metal ions such as Zn2+ to Ag2S based NPs led to a strong PL enhancement, yielding PL quantum yields of about 10% and thus making them highly suitable for non-invasive deep imaging of vascular networks and 3D fluid flow mapping. T2 - NaNaX 10 - Nanoscience with Nanocrystals CY - Klosterneuburg, Austria DA - 03.07.2023 KW - Quantum dots KW - Ag2S KW - Fluorescence KW - SWIR KW - Gold nanocluster KW - Nanomaterial KW - bioimaging PY - 2023 AN - OPUS4-58104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Pauli, J. A1 - Güttler, Arne A1 - Richter, Maria A1 - Fiedler, Saskia A1 - Frenzel, Florian A1 - Wegner, Karl David A1 - Würth, Christian T1 - Photoluminescence Quantum Yields of Luminescent Nanocrystals and Particles in the UV/vis/NIR/SWIR N2 - The rational design of functional luminescent materials such as semiconductor quantum dots and lanthanide-based upconversion nanoparticles, all photophysical and mechanistic studies, and the comparison of different emitters require accurate and quantitative photoluminescence measurements. Particularly the reliable determination of the key performance parameter photoluminescence quantum yield (f), the number of emitted per absorbed photons, and the brightness are of special importance for luminescence applications in the life and material sciences and nano(bio)photonics.[1] In this context, examples for absolute measurements of the photoluminescence quantum yields of UV/vis/NIR/SWIR emissive semiconductor quantum dots and rods, made from different materials, and spectrally shifting lanthanide upconversion nanocrystals with different surface chemistries in transparent matrices are presented including excitation wavelength and power density dependent studies utilizing integration sphere spectroscopy.[2,3] In addition, procedures for the absolute determination of the photoluminescence quantum yields of scattering dispersions of larger size quantum rods and differently sized inorganic particles have been developed as well as procedures for the characterization of solid luminescent nanomaterials such as different perovskites and YAG:Cer converter materials.[4] Thereby, challenges and pitfalls of f measurements in different wavelength regions including the SWIR and material-specific effects related to certain emitter classes are addressed, achievable uncertainties are quantified, and relative and absolute measurements of photoluminescence quantum yield measurements are compared to underline limitations of the former approach. Finally, a set of novel UV/vis/NIR quantum yield standards is presented including their certification with a complete uncertainty budget.[5] T2 - NANAX 10 CY - Klosterneuburg, Austria DA - 03.07.2023 KW - Fluorescence KW - Optical spectroscopy KW - Reference data KW - Traceability KW - NIR KW - Scattering KW - Reference material KW - Certification KW - Quality assurance KW - Dye KW - Reference product KW - SWIR KW - Nano KW - Particle KW - Perovskite KW - Integrating sphere spectroscopy KW - Quantum yield PY - 2023 AN - OPUS4-58238 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - pH- and O2-Responsive Nanoparticles – The MiGraGen Project N2 - In recent years, the demand for reliable, versatile, fluorescent pH and oxygen sensors has increased rapidly in many biomedical applications since these analytes are important indicators of cell function or certain diseases. Therefore, sensor particles are needed that are small enough to penetrate cells, non-toxic, and allow for close-up optical monitoring. When developing such sensor systems, one must consider the pH and oxygen range detectable by the sensor dye and the matrix material of the used carrier particles. Here, we present the development of pH- and oxygen-responsive polymeric beads functionalized with fluorescent dyad molecules that consist of an analyte-responsive fluorophore and an analyte-inert dye. T2 - MiGraGen Project Meeting 09.08.2023 CY - Online Meeting DA - 09.08.2023 KW - Nano- and microsensors KW - Functionalized silica and polymeric particles KW - pH sensing KW - Oxygen sensing KW - Fluorescence PY - 2023 AN - OPUS4-58071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholtz, Lena T1 - Luminescent, nanoparticle-loaded polymer microparticles - comparing synthesis routes N2 - Our comparison showed that the route used for the synthesis of luminescent, NP-loaded PSMPs can play a significant role for the luminescence properties, as well as the number of accessible SFGs, and hence subsequent functionalization. This should be considered for future applications. T2 - Bunsen-Tagung 2023 CY - Berlin, Germany DA - 05.06.2023 KW - Fluorescence KW - Polymerization KW - Microbeads KW - Quantum dots KW - Comparison PY - 2023 AN - OPUS4-57628 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - pH-Responsive Dyad Molecules: MiGraGen Project N2 - Optical pH sensors utilizing colorimetric or fluorescent indicator dyes are highly promising in many biomedical and life science applications where electrochemical sensors fail. For instance, optical sensors are not prone to electrical interferences, they are noninvasive and enable remote measurements. Moreover, fluorescence detection is very fast, highly sensitive, and provides several readout parameters ideal for multiplexing with nanometer resolution using simple, inexpensive, and miniaturizable instrumentation. Here, we present the design of a dyad sensor molecule, consisting of an analyte-responsive and an analyte inert reference fluorophore. T2 - MiGraGen Project Meeting 16.06.2023 CY - Online Meeting DA - 16.06.2023 KW - Dyad molecules KW - pH sensing KW - Fluorescent indicator KW - Ratiometric sensors PY - 2023 AN - OPUS4-58070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Forschung in einer Bundesoberbehörde wie der BAM N2 - Die Bundesanstalt für Materialforschung und -prüfung (BAM) ist eine forschende Bundesoberbehörde und Einrichtung der Ressortforschung der Bundesrepublik Deutschland. Unter ihrer Leitlinie „Sicherheit in Technik und Chemie“ ist sie zuständig für die öffentliche technische Sicherheit und für metrologische Aufgaben in der Chemie. Das Aufgabenspektrum der BAM, das sich an aktuellen Fragestellungen aus Wissenschaft, Wirtschaft, Politik und Normung orientiert, bietet sehr viele interessante Tätigkeitsfelder für Naturwissenschaftler*Innen und Ingenieur*Innen. T2 - WIFO Leipzig 2023 CY - Leipzig, Germany DA - 05.09.2023 KW - Quality assurance KW - Optical spectroscopy KW - Certification KW - Reference product KW - Integrating sphere spectroscopy KW - Fluorescence KW - Quantum yield KW - Reference material KW - Reference data KW - Traceability KW - Nano KW - Particle KW - Analytical chemistry KW - Sensor KW - Safety PY - 2023 AN - OPUS4-58397 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan A1 - Niederleithinger, Ernst T1 - Imaging of Ultrasonic Echo Measurements for Reconstruction of Technical Data of Bridges – Possibilities, Limitations and Outlook N2 - When reassessing existing concrete bridges, the challenge is often to obtain missing or incomplete information on the internal structure. In particular, the number and position of the existing reinforcement as well as the geometric dimensions of the components are of interest. Non-destructive testing methods, like radar or ultrasound, which work on the basis of the pulse-echo method, have been established for this purpose, as they only require access to the component from one side. The measurement data recorded on the structure require pre-processing to be able to reproduce the internal structure geometrically accurately. Besides different steps of data processing, the geometrical reconstruction of the measured data based on the Synthetic Aperture Focusing Technique (SAFT) is state of the art today. In this paper, the technical possibilities of the ultrasonic echo method are presented based on measurements in the laboratory and on a real bridge structure. The precision of the reconstruction and its limitations are shown. In addition to the state of the art SAFT technique, open questions and the latest research approaches, such as imaging by reverse time migration (RTM) including initial results are discussed. T2 - 13th German-Japanese Bridge Symposium CY - Osaka, Japan DA - 29.08.2023 KW - Bridge KW - Non destructive testing and evaluation KW - Concrete KW - Validation PY - 2023 AN - OPUS4-58328 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan A1 - Niederleithinger, Ernst T1 - Low frequency ultrasonic dataset for comparison and validation of signal processing and imaging techniques in civil engineering N2 - The evaluation of technical components and materials in terms of condition and quality with the aid of non-destructive testing methods plays an outstanding role both in industrial serial production and in the individual assessment of components. The ultrasonic echo method is used for a wide variety of testing tasks, such as measuring the thickness of a component. At the Bundesanstalt für Materialforschung und -prüfung (BAM) in Berlin, test methods are developed and their performance is demonstrated. For this purpose, references such as materials, test procedures or data sets are generated, which are used to evaluate these developed test methods. An important component of these references are data sets that are created according to the BAM Data Policy and made available to the scientific community and users of test methods in practice on the basis of the FAIR principles (Findability, Accessibility, Interoperability, and Reuse). T2 - The International Symposium on Nondestructive Testing in Civil Engineering (NDT-CE) 2022 CY - Zurich, Switzerland DA - 16.08.2022 KW - Reference data KW - Non destructive testing and evaluation KW - Ultrasonic KW - Civil engineering PY - 2022 AN - OPUS4-58440 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Design and Quantitative Characterization of Functional Molecular Chromophores and Nanomaterials with UV/vis/NIR/IR Emission – An Overview of Research Activities in Division Biophotonics N2 - In the focus of division Biophotonics are the design, preparation, analytical and spectroscopic characterization, and application of molecular and nanoscale functional materials, particularly materials with a photoluminescence in the visible, near infrared (NIR) and short-wave infrared (SWIR). This includes optical reporters for bioimaging and sensing, security and authentication barcodes, and materials for solid state lighting, energy conversion, and photovoltaics. For the identification of optimum particle structures quantitative spectroscopic studies are performed under application-relevant conditions, focusing on the key performance parameter photoluminescence quantum yield. In addition, simple, cost-efficient, and standardizable strategies for quantifying functional groups on the surface of nano- and microparticles are developed, here with a focus on optical assays and electrochemical titration methods, cross-validated by more advanced methods such as quantitative NMR. In addition, reference materials and reference products are developed for optical methods, particularly luminescence techniques, and for analytical methods utilized for the characterization of nanomaterials. T2 - Projekttreffen Nile-Chrome 2.0 CY - Mainz, Germany DA - 11.12.2023 KW - Fluorescence KW - Quantum yield KW - Optical spectroscopy KW - Reference material KW - Reference data KW - Quality assurance KW - Dye KW - Reference product KW - NIR KW - SWIR KW - Nano KW - Particle KW - Silica KW - Polymer KW - Surface group analysis KW - Sensor molecules PY - 2023 AN - OPUS4-59123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - A Multimodal Approach to Quantify Surface Functional Groups on Nanomaterials for Safe and Sustainable by Design N2 - Engineered nanomaterials (NM) with their large surface-to-volume ratios and their for some materials observed size-dependent functional properties are of increasing relevance for current and future developments in various fields such as medical and pharmaceutical industry, computing and electronics or food and consumer products. The performance and safety of NM are determined by the sum of their intrinsic physicochemical properties. Especially, the particle surface chemistry, which is largely controlled by the chemical nature and density of functional groups (FG) and ligands, is an important key driver for NM performance, stability, and processibility as well as the interaction of NM with the environment. Thus, methods for FG quantification can foster the sustainable development of functional and safe(r) NM. Aiming at the development of simple, versatile, and multimodal tools for the quantification of many bioanalytically relevant FG and ligands, we investigated and compared various analytical methods commonly used for FG quantification. This includes electrochemical titration methods, dye-based optical assays, and other instrumental analytical techniques such as nuclear magnetic resonance and thermal analysis methods. The potential of our multimodal approach for FG quantification was demonstrated for commercial and custom-made polymeric and silica particles of varying FG, used as optical pH sensors. In the future, our strategy can contribute to establish multi-method characterization strategies to provide a more detailed picture of the structure-properties relationship. T2 - NanoSAFE & NanoSafety Cluster 2023 CY - Grenoble, France DA - 05.06.2023 KW - Engineered Nanomaterials KW - Safe-by-Design KW - Sustainable-by-Design KW - Surface Group Analysis KW - Silica and Polystyrene Particles KW - Surface Modification KW - Dye KW - Optical Spectroscopy KW - Quantitative NMR KW - Electrochemical Titration KW - Functionalized Nanomaterials KW - Nanosafety PY - 2023 AN - OPUS4-59126 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Osipova, Viktoriia T1 - Incorporation of near-infrared light emitting chromium (III) complexes into silica nanoparticles and spectroscopic characterization N2 - In recent years, chromium (III) complexes have received a lot of attention as novel near-infrared (NIR) emitters triggered by the report on the first molecular ruby Cr(ddpd)2(BF4)3 with a high photoluminescence quantum yield of 13.7% of its near infrared (NIR) emission band and a long luminescence lifetime of 1.122 ms at room temperature.[1] However, in an oxygen-containing environment, the photoluminescence quantum yields and luminescence lifetimes of these chromium(III) complexes show only very small values. This hampers their application as NIR luminescence labels. This application, that cannot be tackled by conventional deoxygenating approaches, requires suitable strategies to protect the luminescence of the chromium(III) complexes from oxygen quenching. An elegant approach to reduce the undesired luminescence quenching by triplet oxygen explored by us presents the incorporation of these chromium(III) complexes into different types of amorphous, non-porous silica nanoparticles, that can be simply surface functionalized, e.g., with targeting ligands and/or other sensor molecules. In this work, as first proof-of-concept experiments, a set of chromium (III) complexes constituting of different ligands and counter anions, were embedded into the core of silica nanoparticles. Subsequently, the optical properties of the resulting luminescent silica nanoparticles were spectroscopically assessed by steady state and time-resolved luminescence spectroscopy. First results of time-resolved luminescence measurements confirm our design concept of nanoscale NIR emissive Cr(III) complex-based reporters T2 - Projekttreffen Nile-Chrome 2.0 CY - Mainz, Germany DA - 11.12.2023 KW - Cr(III) complex KW - NIR KW - Luminescence KW - Nano KW - Silica KW - Lifetime KW - Quantum Yields KW - Particle Synthesis KW - Sensors KW - Probe KW - Surface Group Analysis PY - 2023 AN - OPUS4-59149 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - A Multimodal Approach to Quantify Surface Functional Groups and Ligands on Amorphous Silica Nanoparticles N2 - Nowadays amorphous silica nanoparticles (SiO2-NP) are one of the most abundant engineered nanomaterials, that are highly stable and can be easily produced on a large scale at low cost. Surface functionalized SiO2-NP are of great interest in the life and material sciences, as they can be used e.g. as drug carriers, fluorescent sensors, and multimodal labels in bioanalytical assays and imaging applications. Their performance in such applications depends not only on particle size, size distribution, and morphology, but also on surface chemistry, i.e. the total number of surface functional groups (FG) and the number of FG accessible for subsequent functionalization with ligands or biomolecules, which in turn determines surface charge, colloidal stability, biocompatibility, and toxicity. Aiming at the development of simple, versatile, and multimodal tools for the quantification of many bioanalytically relevant FG and ligands, we investigated and compared various analytical methods commonly used for FG quantification. This includes electrochemical titration methods, dye-based optical assays, and other instrumental analytical techniques such as nuclear magnetic resonance and thermal analysis methods. The potential of our multimodal approach for FG quantification was demonstrated for commercial and custom-made silica particles of varying FG, showing not only an influence of the synthesis methods on the number of FG but also on the performance. In the future, our strategy can contribute to establish multi-method characterization strategies to provide a more detailed picture of the structure-properties relationship. T2 - Advanced Materials Safety 2023 CY - Saarbrücken, Germany DA - 08.11.2023 KW - Amorphous silica particles KW - Surface group analysis KW - Ligands KW - Reference material KW - Optical spectroscopy KW - Quantitative NMR KW - Optical assays KW - Titration KW - Engineered nanomaterials KW - Advanced Materials PY - 2023 AN - OPUS4-59124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Standardised Measurements of Surface Functionalities on Nanoparticles N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, opto-electronics, and information storage which improve the quality of life and European prosperity. NP function, performance, interaction with biological species, and environmental fate are largely determined by their surface functionalities. Standardized repeatable surface characterization methods are therefore vital for quality control of NPs, and to meet increasing concerns regarding their safety. Therefore, industry, regulatory agencies, and policymakers need validated traceable measurement methods and reference materials. This calls for fit-for-purpose, validated, and standardized methods, and reference data and materials on the surface chemistry of engineered NPs. Here, we present a concept for the development of such standardized measurement protocols utilizing method cross-validation and interlaboratory comparisons (ILCs) with emphasis on both advanced measurement methods such as quantitative Nuclear Magnetic Resonance (qNMR), X-ray photoelectron spectroscopy (XPS) and secondary ion mass spectrometry (SIMS) and cost-efficient, non-surface specific methods like optical assays and electrochemical titration methods. T2 - European Partnership on Metrology 2023 Review Conference CY - Amsterdam, Netherlands DA - 07.11.2023 KW - Surface chemistry KW - Quality assurance KW - Traceability PY - 2023 AN - OPUS4-59142 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Püschel, S. A1 - Liestmann, Z. A1 - Kalusniak, S. A1 - Kränkel, C. A1 - Schulz, Andreas A1 - Traub, Heike A1 - Tanaka, H. T1 - Impact of Ho3+, Er3+, and Tm3+ on laser cooling of Yb:YLF N2 - Ytterbium-doped LiYF4 (Yb:YLF) is a promising material for all-solid-state optical cryocoolers, but the impact of foreign rare-earth impurities on the laser-cooling performance is not completely understood. In particular, Tm3+ has been reported to reduce the background absorption. This study quantitatively assesses the impact of Ho3+, Tm3+, and Er3+ impurities on laser-cooling of Yb:YLF by anti-Stokes fluorescence. We grew five Yb(5%):YLF crystals intentionally doped with tens of ppm levels of these impurities. Laser-induced thermal modulation spectroscopy tests confirmed that these rare-earth impurities reduce the external quantum efficiency of Yb:YLF without affecting the background absorption coefficient. Although Er3+ is a well-known quencher for Yb3+, Er3+ co-doping only slightly decreases the laser-cooling efficiency at low pump intensities but becomes detrimental at high pump intensities (>5 kW cm−2). However, this detrimental effect diminishes at lower temperatures, as evidenced by cooling an Er3+ co-doped crystal to the same minimum temperature of 144K as a solely Yb3+-doped crystal. Contrary to previous reports, Tm3+ proved to be the most detrimental among the three impurities. KW - ICP KW - Laser cooling KW - Impurity KW - LiYF4 KW - Crystal PY - 2024 DO - https://doi.org/10.1364/OME.538215 VL - 14 IS - 10 SP - 2334 EP - 2348 PB - Optica Publishing Group CY - Washington DC, USA AN - OPUS4-61046 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sommerfeld, Thomas A1 - Riedel, Juliane A1 - Lisec, Jan A1 - Mauch, Tatjana A1 - Richter, Silke A1 - Koch, Matthias T1 - Development of a certified reference material for per- and polyfluoroalkyl substances (PFAS) in textiles N2 - Per- and polyfluoroalkyl substances (PFASs) are a large group of emerging organic pollutants that contaminate the environment, food, and consumer products. Textiles and other outdoor products are a major source of PFAS exposure due to their water-repellent impregnations. Determination of PFASs in textiles is increasingly important for enhancing their contribution to the circular economy. While maximum levels and restrictions exist for certain key compounds under the Stockholm Convention on Persistent Organic Pollutants and the REACH regulation, certified reference materials (CRMs) are not currently available. To address this issue, the first CRM for determining PFASs in outdoor textiles (BAM-B003) was developed. It fully complies with the requirements of ISO 17034 and ISO 33405. This work presents the entire process of CRM development process, including preparation, a homogeneity study, a stability study, and value assignment. Certification was based on an in-house study at BAM using liquid chromatography tandem mass spectrometry (LC–MS/MS) with stable isotope dilution analysis (SIDA). The certified mass fractions of 18 PFASs range widely from 0.46 to 69 µg/kg, with a prevalence of PFOA (69 µg/kg), PFOS (41 µg/kg) and PFHxA (35 µg/kg) exceeding legal limits. BAM-B003 is intended for analytical quality control and contributes to improving the chemical safety of textiles and strengthening the circular economy. KW - Reference Material KW - PFAS KW - Textiles PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641040 DO - https://doi.org/10.1007/s00216-025-06098-2 SN - 1618-2642 SP - 1 EP - 9 PB - Springer Science and Business Media LLC AN - OPUS4-64104 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - Is LIBS ready for the future? N2 - Recent years have brought up many challenges for an analytical tracing of material flows. While planetary boundaries force end of life material into circular recycling pathways, geopolitical tension creates demands regarding the origin of raw materials. The analytical demands on any instrumentation to tackle the arising challenges of this scenario are straight forward: No sample preparation, precision in the percentage region, and high throughput at comparably low cost. All these demands make LIBS a perfect candidate, why it is time for a re-evaluation of how it exploits the potential possibilities arising from todays’ technology. While being a relatively young technique, the vast majority of conducted LIBS experiments still relies on well established instrumentation, sometimes ignoring the innovations and breakthroughs in the development of its empowering technology sectors such as battery powered compact high repetition rate lasers with tuneable pulse rate and length, low priced cameras with millions of small sized pixels and extremely fast shutter and readout times, optical modulators, galvonometer scanners, and simple robotics. In this talk we will showcase some examples on how the implantation of all these new tools can lead to extremely affordable and compact instrumentation with unprecedented acquisition speed and a spectral resolution sufficient to resolve atomic isotope lines. T2 - FACCS SCiX CY - Raleigh, NC, USA DA - 20.10.2024 KW - LIBS KW - Isotopes KW - Instrumentation PY - 2024 AN - OPUS4-61970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Lisec, Jan T1 - CorMID - Correct Mass Isotopologue Distribution Vectors N2 - The investigation of metabolic fluxes and metabolite distributions within cells by means of tracer molecules is a valuable tool to unravel the complexity of biological systems. Technological advances in mass spectrometry (MS) technology such as atmospheric pressure chemical ionization (APCI) coupled with high resolution (HR), not only allows for highly sensitive analyses but also broadens the usefulness of tracer-based experiments, as interesting signals can be annotated de novo when not yet present in a compound library. However, several effects in the APCI ion source, i.e., fragmentation and rearrangement, lead to superimposed mass isotopologue distributions (MID) within the mass spectra, which need to be corrected during data evaluation as they will impair enrichment calculation otherwise. Here, we present and evaluate a novel software tool to automatically perform such corrections. We discuss the different effects, explain the implemented algorithm, and show its application on several experimental datasets. This adjustable tool is available as an R package from CRAN. KW - Mass Spectrometry KW - Software KW - R package KW - Mass Isotopomer Distribution KW - Flux Analysis PY - 2022 UR - https://github.com/cran/CorMID/ PB - GitHub CY - San Francisco, CA, USA AN - OPUS4-56442 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Adamus, A. A1 - Ali, I. A1 - Vasileiadis, V. A1 - Al-Hileh, L. A1 - Lisec, Jan A1 - Frank, M. A1 - Seitz, G. A1 - Engel, N. T1 - Vincetoxicum arnottianum modulates motility features and metastatic marker expression in pediatric rhabdomyosarcoma by stabilizing the actin cytoskeleton N2 - Background: Prevention of metastatic invasion is one of the main challenges in the treatment of alveolar rhabdomyosarcoma. Still the therapeutic options are limited. Therefore, an anti-tumor screening was initiated focusing on the anti-metastatic and anti-invasion properties of selected medicinal plant extracts and phytoestrogens, already known to be effective in the prevention and treatment of different cancer entities. Methods: Treatment effects were first evaluated by cell viability, migration, invasion, and colony forming assays on the alveolar rhabdomyosarcoma cell line RH-30 in comparison with healthy primary cells. Results: Initial anti-tumor screenings of all substances analyzed in this study, identified the plant extract of Vincetoxicum arnottianum (VSM) as the most promising candidate, harboring the highest anti-metastatic potential. Those significant anti-motility properties were proven by a reduced ability for migration (60%), invasion (99%) and colony formation (61%) under 48 h exposure to 25 μg/ml VSM. The restricted motility features were due to an induction of the stabilization of the cytoskeleton – actin fibers were 2.5-fold longer and were spanning the entire cell. Decreased proliferation (PCNA, AMT, GCSH) and altered metastasis (e. g. SGPL1, CXCR4, stathmin) marker expression on transcript and protein level confirmed the significant lowered tumorigenicity under VSM treatment. Finally, significant alterations in the cell metabolism were detected for 25 metabolites, with levels of uracil, N-acetyl serine and propanoyl phosphate harboring the greatest alterations. Compared to the conventional therapy with cisplatin, VSM treated cells demonstrated a similar metabolic shutdown of the primary cell metabolism. Primary control cells were not affected by the VSM treatment. Conclusions: This study revealed the VSM root extract as a potential, new migrastatic drug candidate for the putative treatment of pediatric alveolar rhabdomyosarcoma with actin filament stabilizing properties and accompanied by a marginal effect on the vitality of primary cells. KW - Mass Spectroscopy KW - Metabolomics KW - Cancer PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533530 DO - https://doi.org/10.1186/s12906-021-03299-x VL - 21 IS - 1 PB - Springer Nature AN - OPUS4-53353 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, X.M. A1 - Li, H.M. A1 - Zhang, Q.H. A1 - Lu, X.H. A1 - Li, S.Q. A1 - Koch, Matthias A1 - Polzer, J. A1 - Hackenber, R. A1 - Moniruzzaman, M. A1 - Khan, M. A1 - Kakoulides, E. A1 - Pak-Wing, K. A1 - Richy, A1 - Chi-Shing, N. A1 - Lu, T. A1 - Gui, E.M. A1 - Cheow, P.S. A1 - Teo, T.L. A1 - Rego, E. A1 - Garrido, B. A1 - Carvalho, L. A1 - Leal, R. A1 - Violante, F. A1 - Baek, S.Y. A1 - Lee, S. A1 - Choi, K. A1 - Kim, B. A1 - Bucar-Miklavcic, M. A1 - Hopley, C. A1 - Nammoonnoy, J. A1 - Murray, J. A1 - Wilson, W. A1 - Toman, B. A1 - Itoh, N. A1 - Gokcen, T. A1 - Krylov, A. A1 - Mikheeva, A. T1 - CCQM-K146 low-polarity analyte in high fat food: benzo a pyrene in olive oil N2 - The demonstration of competency and equivalence for the assessment of levels of contaminants and nutrients in primary foodstuffs is a priority within the 10-year strategy for the OAWG Track A core comparisons. The measurements are core challenges for reference material producers and providers of calibration Services. This key comparison related to low polarity analytes in a high fat, low protein, low carbohydrate food matrix and Benzo[a]pyrene in edible oil was the model System selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (Dis). 16 National Metrology Institutions participated in the Track A Key Comparison CCQM-K146 Low-Polarity Analyte in high fat food: Benzo[a]pyrene in Olive Oil. Participants were requested to evaluate the mass fractions, expressed in µg/kg, of Benzo[a]pyrene in the olive oil material. The KCRV was determined from the results of all NMIs/DIs participating in the key comparison that used appropriately validated methods with demonstrated metrological traceability. Different methods such as liquid-liquid extraction, GPC and SPE were applied in the sample pretreatment and HPLC-FLD, HPLC-MS/MS, and GC-MS or GC-MS/MS were applied for detection by the participants. The mass fractions for BaP were in the range of (1.78 to 3.09) µg/kg with Standard uncertainties of (0.026 to 0.54) µg/kg, with corresponding relative Standard uncertainties from 0.9% to 21%. Five labs withdrew their result from the Statistical evaluation of the KCRV for technical reasons. One lab was excluded from the KCRV evaluation, as they did not meet the CIPM metrological traceability requirements. A Hierarchical Bayes option was selected for the KCRV value, which was determined as 2.74 µg/kg with a Standard uncertainty of 0.03 µg/kg. The 10 institutes those were included in the calculation of the consensus KCRV all agreed within their Standard uncertainties. Successful participation in CCQM-K146 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 0.1 µg/kg to 1000 µg/kg in a high fat, low protein, low carbohydrate food matrix. KW - Metrology KW - CCQM KW - Food KW - PAH PY - 2020 DO - https://doi.org/10.1088/0026-1394/57/1a/08017 VL - 57 IS - 1a SP - 08017 AN - OPUS4-52435 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Josephs, R. A1 - Choteau, T. A1 - Daireaux, A. A1 - Stoppacher, N. A1 - Wielgosz, R. A1 - Davies, S. A1 - do Rego, E. A1 - Wollinger, W. A1 - Garrido, B. A1 - Fernandes, J. A1 - Lima, J. A1 - Oliveira, R. A1 - de Sena, R. A1 - Windust, A. A1 - Huang, T. A1 - Dai, X. A1 - Quan, C. A1 - He, H. A1 - Zhang, W. A1 - Wei, C. A1 - Li, N. A1 - Gao, D. A1 - Liu, Z. A1 - Lo, M. A1 - Wong, W. A1 - Pfeifer, Dietmar A1 - Koch, Matthias A1 - Dorgerloh, Ute A1 - Rothe, Robert A1 - Philipp, Rosemarie A1 - Hanari, N. A1 - Rezali, M. A1 - Arzate, C. A1 - Berenice, M. A1 - Caballero, V. A1 - Osuna, M. A1 - Krylov, A. A1 - Kharitonov, S. A1 - Lopushanskaya, E. A1 - Liu, Q. A1 - Lin, T. A1 - Fernandes-Whaley, M. A1 - Quinn, L. A1 - Nhlapo, N. A1 - Prevoo-Franzsen, D. A1 - Archer, M. A1 - Kim, B. A1 - Baek, S. A1 - Lee, S. A1 - Lee, J. A1 - Marbumrung, S. A1 - Kankaew, P. A1 - Chaorenpornpukdee, K. A1 - Chaipet, T. A1 - Shearman, K. A1 - Gören, A. A1 - Gündüz, S. A1 - Yilmaz, H. A1 - Un, I. A1 - Bilsel, G. A1 - Clarkson, C. A1 - Bedner, M. A1 - Camara, J. A1 - Lang, B. A1 - Lippa, K. A1 - Nelson, M. A1 - Toman, B. A1 - Yu, L. T1 - Mass fraction assignment of folic acid in a high purity material - CCQM-K55.d (Folic acid) Final Report N2 - The comparison required the assignment of the mass fraction of folic acid present as the main component in the comparison sample. Performance in the comparison is representative of a laboratory's measurement capability for the purity assignment of organic compounds of medium structural complexity [molecular weight range 300–500] and high polarity (pKOW < −2). Methods used by the eighteen participating NMIs or DIs were based on a mass balance (summation of impurities) or qNMR approach, or the combination of data obtained using both methods. The qNMR results tended to give slightly lower values for the content of folic acid, albeit with larger associated uncertainties, compared with the results obtained by mass balance procedures. Possible reasons for this divergence are discussed in the report, without reaching a definitive conclusion as to their origin. The comparison demonstrates that for a structurally complex polar organic compound containing a high water content and presenting a number of additional analytical challenges, the assignment of the mass fraction content property value of the main component can reasonably be achieved with an associated relative standard uncertainty in the assigned value of 0.5% KW - CCQM key comparison KW - Purity assessment KW - Folic acid PY - 2018 UR - https://www.bipm.org/utils/common/pdf/final_reports/QM/K55/CCQM-K55.d.pdf DO - https://doi.org/10.1088/0026-1394/55/1A/08013 VL - 55 IS - Technical Supplement, 2018 SP - 08013, 1 EP - 38 PB - Institute of Physics Publishing (IOP) ; Bureau International des Poids et Mesures AN - OPUS4-44999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ocker, L. A1 - Lisec, Jan A1 - Seitz, G. A1 - Adamus, A. A1 - Hempfling, L. A1 - Wagner, B. A1 - Vahdad, R. A1 - Verburg, F. A. A1 - Luster, M. A1 - Schurrat, T. A1 - Bier, D. A1 - Frank, M. A1 - Engel, N. T1 - Hypericin and its radio iodinated derivatives – A novel combined approach for the treatment of pediatric alveolar rhabdomyosarcoma cells in vitro N2 - In this in vitro study, we got a first insight of a possible potential of Hypericin for the treatment of pediatric soft tissue sarcoma. By coupling with radioiodine, we developed a novel approach for a combined anti-tumor treatment. The in vitro experiments lay the foundation for further in vivo experiments, which are needed to study the effects of a sequential administration of 131I-HYP and HYP. KW - Mass-Spectrometry KW - Cancer PY - 2020 VL - 29 SP - 101588 PB - Elsevier B.V. AN - OPUS4-49601 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Kobelt, D. A1 - Walther, W. A1 - Mokrizkij, M. A1 - Grötzinger, C. A1 - Jaeger, Carsten A1 - Baum, K. A1 - Simon, M. A1 - Wolf, J. A1 - Beindorf, N. A1 - Brenner, W. A1 - Stein, U. T1 - Systematic Identification of MACC1-Driven Metabolic Networks in Colorectal Cancer N2 - MACC1 is a prognostic and predictive metastasis biomarker for more than 20 solid Cancer entities. However, its role in cancer metabolism is not sufficiently explored. Here, we report on how MACC1 impacts the use of glucose, glutamine, lactate, pyruvate and fatty acids and show the comprehensive analysis of MACC1-driven metabolic networks. We analyzed concentrationdependent changes in nutrient use, nutrient depletion, metabolic tracing employing 13C-labeled substrates, and in vivo studies. We found that MACC1 permits numerous effects on cancer metabolism. Most of those effects increased nutrient uptake. Furthermore, MACC1 alters metabolic pathways by affecting metabolite production or turnover from metabolic substrates. MACC1 supports use of glucose, glutamine and pyruvate via their increased depletion or altered distribution within metabolic pathways. In summary, we demonstrate that MACC1 is an important regulator of metabolism in cancer cells. KW - Mass Spectroscopy KW - Metabolomics KW - Cancer PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-533526 DO - https://doi.org/10.3390/cancers13050978 VL - 13 IS - 5 SP - 1 EP - 22 PB - MDPI Journal Cancers AN - OPUS4-53352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Richter, Silke A1 - Roethke, A. A1 - Rienitz, O. A1 - Matschat, Ralf A1 - Schiel, D. A1 - Jaehrling, R. A1 - Goerlitz, V. A1 - Kipphardt, Heinrich T1 - SI-traceable monoelemental solutions on the highest level of accuracy: 25 years from the foundation of CCQM to recent advances in the development of measurement methods N2 - Within the Working Group on Inorganic Analysis (IAWG) of the Consultative Committee for Amount of Substance: Metrology in Chemistry and Biology (CCQM) international key comparisons and pilot studies related to inorganic analysis are carried to ensure consistency in this field at the highest level. Some of these comparisons deal directly with the preparation and characterization of monoelemental solutions or with topics, closely related. The importance of monoelemental solutions lies in the fact that almost every measurement in inorganic analysis relies on the comparison with either a reference material, or references in form of solutions, usually (mono)elemental solutions. All quantitative measurement approaches, e.g. isotope dilution or standard addition, need an accurate reference solution made from a well characterized reference material, prepared under full gravimetric control. These primary (monoelemental) solutions do not only serve as arbitrary references/calibration solutions, but they also link up measurement results to the International System of units (SI), this way establishing the so-called metrological traceability to a measurement unit of the SI. Without such solutions on the highest possible level of accuracy and with the smallest possible associated uncertainties (for e.g. element content and/or impurities), an analysis itself can never be as good as it could be with appropriate reference solutions. This article highlights select key comparisons and pilot studies dealing with monoelemental solution related topics within the IAWG from the foundation of CCQM – 25 years ago – up to latest achievements in the field of inorganic analysis. KW - Metrology KW - SI Traceability KW - CCQM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-496080 DO - https://doi.org/10.1088/1681-7575/ab5636 SN - 0026-1394 SN - 1681-7575 SP - 1 EP - 23 PB - IOP CY - Bristol AN - OPUS4-49608 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter T1 - Environmental screenings of bioactive compounds in wastewater using a novel multiplex suspension array fluorescence immunoassay N2 - Monitoring water quality regarding emerging pollutants, such as drug residues, demands for selective, high-throughput and multi-target analytical methods. On the one hand, the influence of sewage on natural surface waters must be routinely monitored. On the other hand, estimation of removal efficiencies of pollutants, such as drug residues, is in the focus of industrial and public wastewater treatment. Immunoassays, such as ELISA, offer the possibility to be highly sensitive and selective due to the high target affinity and specificity of target recognition by antibodies. Batch-wise processing in microtiter plates allows for the necessary high-throughput, but only a single analyte can be determined within one measurement. To overcome these disadvantages, we developed a four-plex Suspension Array Fluorescence Immunoassay (SAFIA), which is adaptable for the microtiter plate format. The modular and self-prepared bead support consists of polystyrene-core silica-shell microparticles. While the polystyrene core is used for encoding, by introducing different amounts of fluorescent dyes, the silica shell creates a solid-support for the immunoassay: the target analytes, three drugs, carbamazepine, diclofenac and caffeine, and the fecal marker isolithocholic acid are covalently coupled to amino groups on the surface via NHS chemistry. Specific recognition of these haptens is accomplished by further introduction of PEG moieties, suppressing non-specific binding. A competitive immunoassay is subsequently conducted in a simple mix-and-read procedure, eliminating the demand for laborious washing steps and decreasing time-to-result. An automated flow cytometer is used for simultaneous decoding and quantification. After optimization, the SAFIA showed limits of detection for all analytes in the low µg L 1 range, meeting the sensitivity criteria for wastewater analysis. Then, applicability of the SAFIA was studied on real wastewater samples from three different wastewater treatment plants in Berlin. The results were in good comparability to LC-MS/MS indicating high matrix stability. Moreover, the accuracy of the assay exceeded that of the respective ELISA. Finally, we used SAFIA to assess the influent of treated and untreated wastewater on the Douro river estuary in Portugal. The obtained results of the analysis were comparable to ELISA. However, the measurements by SAFIA could be carried out in one quarter the time of analysis required for ELISA. Acknowledgements: The authors acknowledge financial support from Deutscher Akademischer Austauschdienst and from Fundação das Universidades Portuguesas under the protocol CRUP-DAAD (Ações Integradas Luso-Alemãs nºE-20/16, DAAD Zuwendungsvertrag 57212899). T2 - ANALÍTICA – 2018 CY - Porto, Portugal DA - 26.03.2018 KW - Bead-based assay KW - Suspension array KW - Fluoresence KW - Anthropogenic markers KW - Emerging pollutants PY - 2018 AN - OPUS4-44591 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Döring, Sarah T1 - Novel Trypsin-functionalized Corundum Particles for Improved Antibody Digestion N2 - Therapeutic monoclonal antibodies are the fastest-growing class of biological agents and the development of reliable analytical methods for their quantification is becoming increasingly important. Liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) represents one of the leading technologies for antibody quantification. The serin protease trypsin has emerged as the gold standard enzyme for digesting intact protein into peptides for this approach. However, many protocols exist that often lead to different results. However, many protocols exist that often lead to different results depending on the digestion procedure. In particular, the type and amounts of detergents added during sample preparation for protein unfolding before digestion is known to create undesirable structure modifications of proteins (e.g. carbamylation) and significant bias in measurement results by inhibiting enzyme activity. The source and nature of the enzyme itself can also have an influence, whereby immobilized variants are increasingly being used to improve their stability, minimize self-digestion and enable a higher substrate-enzyme ratio. Here, we explored the potential of a novel thermostable trypsin and surface-functionalized corundum particles for enhanced antibody digestion. For this purpose, the inactive proenzym was recombinantly produced in inclusion bodies of E. coli and successfully folded back into functional conformation via multi-stage dialysis using a cysteine-cystine redox system. After cleavage of the propeptide and purification of active variants, enzyme activity was comparable to commercially available trypsin product. In addition, produced trypsin showed increased thermal stability under typical digestion conditions compared to reference product. In solution digestion experiments of antibody have revealed that the thermostable variant demonstrates enhanced digestive efficacy compared to the wild type. Furthermore, APTES-silanization followed by polymerization of corundum surface prevent nonspecific protein adsorption during the protein digestion procedure and the immobilized enzyme still showed substrate activity after covalent binding. Compared to wild-type and a non-immobilized enzyme, the surface-functionalized thermostable variant showed increased activity at temperatures above 80°C. Thus, this novel type of trypsin particles promises to not only improve antibody digestion at high temperatures, but also to prevent self-digestion and enable the separation of trypsin from target peptides in LC–MS analysis. T2 - Adlershofer Forschungsforum CY - Berlin, Germany DA - 11.11.2024 KW - Antibody Quantification KW - Corundum KW - Enzyme Immobilization KW - LC-MS/MS PY - 2024 AN - OPUS4-61680 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Weller, Michael G. A1 - Martínez-Mánez, R. A1 - Rurack, Knut T1 - Immunochemical design of antibody-gated indicator delivery (gAID) systems based on mesoporous silica nanoparticles N2 - In this work, the optimization of the immunochemical response of antibody-gated indicator delivery (gAID) systems prepared with mesoporous silica nanoparticles has been studied along various lines of system tailoring, targeting the peroxide-type explosive TATP as an exemplary analyte. The mechanism of detection of these gAID systems relies on a displacement of an antibody “cap” bound to hapten derivatives anchored to the surface of a porous hybrid material, allowing the indicator cargo stored in the mesopores to escape and massively amplify the analyte-related signal. Since our aim was to obtain gAID systems with the best possible response in terms of sensitivity, selectivity, and assay time, sera obtained from different immunization boosts were screened, the influence of auxiliary reagents was assessed, structural hapten modification (hapten heterology) was investigated, and various indicator dyes and host materials were tested. Considering that highly selective and sensitive immunological responses are best obtained with high-affinity antibodies which, however, could possess rather slow dissociation constants, leading to slow responses, the main challenge was to optimize the immunochemical recognition system for a rapid response while maintaining a high sensitivity and selectivity. The best performance was observed by grafting a slightly mismatching (heterologous) hapten to the surface of the nanoparticles in combination with high-affinity antibodies as “caps”, yielding for the first time gAID nanomaterials for which the response time could be improved from hours to <5 min. The materials showed favorable detection limits in the lower ppb range and discriminated TATP well against H2O2 and other explosives. Further optimization led to straightforward integration of the materials into a lateral flow assay without further treatment or conditioning of the test strips while still guaranteeing remarkably fast overall assay times. KW - Antibody-gated indicator delivery systems KW - Signal amplification KW - Immunochemical response optimization KW - Test strip analysis KW - TATP KW - Explosives detection KW - Heterologous hapten PY - 2022 DO - https://doi.org/10.1021/acsanm.1c03417 SN - 2574-0970 VL - 5 IS - 1 SP - 626 EP - 641 PB - American Chemical Society CY - Washington, DC AN - OPUS4-54176 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bell, Jérémy A1 - Climent Terol, Estela A1 - Hecht, Mandy A1 - Buurman, Merwe A1 - Rurack, Knut T1 - Combining a droplet-based microfluidic tubing system with gated indicator releasing nanoparticles for mercury trace detection N2 - A droplet-based microfluidic sensor was developed for the detection of Hg2+ traces in water. The approach uses gated mesoporous nanoparticles loaded with a fluorescent BODIPY dye. The squaraine-based gating mechanism is highly selective for Hg2+ and the indicator release mechanism ensures sensitive detection. The microfluidic system is modular and was assembled from simple PTFE/PFA tubes, while detection was realized with standard optomechanic, optic, and electronic parts. The sensor shows a stable response without memory effects and allows the detection of Hg2+ in water down to 20 ppt. KW - Microfluidic sensor KW - Gated delivery system KW - Fluorescence KW - Mercury KW - Hybrid nanoparticles PY - 2016 DO - https://doi.org/10.1021/acssensors.5b00303 SN - 2379-3694 VL - 1 IS - 4 SP - 334 EP - 338 PB - American Chemical Society CY - Washington, DC AN - OPUS4-35831 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jankevics Jones, H. T1 - Determination of core-shell particle mass and size distribution, density and distinguishing shell thickness by resonant mass measurements N2 - In micro or nano particles development it is important to understand and control the particle structure, as it affects among other things the potential further surface functionalisation/modification possible. This work shows the capability of resonant mass measurements (RMM) to measure the mass and density of micron sized particles. The technology utilizes a suspended MEMS microchannel resonator, through which individual particles transit across the resonator altering the resonant frequency, which is then detected using an optical-based method. Changes in frequency observed when a particle enters the microchannel resonator are proportional to the buoyant mass of the particle, and can be translated into mass, size or surface area. RMM therefore allows particle concentration to be determined as well as particle mass in a single measurement. Furthermore, a method for estimating the density distribution of particles from RMM measurements has been developed. This uses the convolution of the buoyant mass distribution of the particles obtained when suspended in different fluids. By combining the data from the density and mass determinations, small mass shifts arising from applying a coating to a particle can be estimated, and the resulting shell thicknesses calculated. These methods have been applied to silica coated and uncoated polystyrene latex particles. RMM shows that it can be used to measure, and distinguish between, silica shell thicknesses that are in the order of 10 to 55 nanometres on hybrid micron-sized particles. RMM can also determine the shell density. T2 - UK Colloids 2017 CY - Manchester, UK DA - 10.07.2017 KW - Core-shell particles KW - Resonant mass measurement PY - 2017 AN - OPUS4-42262 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Assessing different types of silica networks for the complete protection of nir luminescent molecular rubies from oxygen quenching in air N2 - The application of emerging luminophores such as near-infrared (NIR) emissive earth-abundant chromium(III) (CrIII) complexes and triplet-triplet annihilation upconversion (TTA-UC) systems in air as optical reporters for bioimaging or photonic materials for energy conversion requires simple and efficient strategies for their complete protection from luminescence quenching by oxygen. Therefore, we explored the influence of sol-gel synthesis routes on the oxygen protection efficiency of the resulting core and core/shell silica nanoparticles (SiO2 NPs), utilizing the molecular ruby-type luminophores CrPF6 ([Cr(ddpd)2](PF6)3; ddpd = N,N’-dimethyl- N,N’-dipyridin-2-ylpyridin-2,6-diamine) and CrBF4 ([Cr(ddpd)2](BF4)3) with their oxygen-dependent, but polarity-, proticity-, viscosity-, and concentration-independent luminescence as optical probes for oxygen permeability. The sol-gel chemistry routes we assessed include the classical Stöber method and the underexplored larginine approach, which relies on the controlled hydrolysis of tetraethoxysilane (TEOS) in a biphasic cyclohexane/water system with the catalyst l-arginine. As demonstrated by luminescence measurements of air- and argon-saturated dispersions of CrPF6- and CrBF4-stained SiO2 NPs of different size and particle architecture, utilizing the luminescence decay kinetics of argon-saturated solutions of CrPF6 and CrBF4 in acetonitrile (ACN) as benchmarks, only SiO2 NPs or shells synthesized by the l-arginine approach provided complete oxygen protection of the CrIII complexes under ambient conditions. We ascribe the different oxygen shielding efficiencies of the silica networks explored to differences in density and surface chemistry of the resulting nanomaterials and coatings, leading to different oxygen permeabilities. Our l-arginine based silica encapsulation strategy can open the door for the efficient usage of oxygen-sensitive luminophores and TTA-UC systems as optical reporters and spectral shifters in air in the future. T2 - eMRS Strasbourg CY - Strasbourg, France DA - 26.05.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Quantum yield KW - NIR KW - Mechanism KW - Characterization KW - Electron microscopy KW - Silica KW - Oxygen sensing KW - Surface KW - Doping KW - Lifetime KW - Cr(III) complex PY - 2025 AN - OPUS4-63300 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Investigation of degradation of the aluminum current collector in lithium-ion batteries by glow-discharge optical emission spectroscopy N2 - Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs.[1] Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs. T2 - European Winter Conference on Plasma Spectrochemistry (EWCPS 2023) CY - Ljubljana, Slovenia DA - 29.01.2023 KW - Lithium-ion batteries KW - Aging mechanisms KW - Depth-profiling PY - 2023 AN - OPUS4-56992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lozano-Torres, B. A1 - Marcos, M. Dolores A1 - Pardo, T. A1 - Sancenón, F. A1 - Martínez-Mánez, Ramon A1 - Rurack, Knut T1 - Anilinopyridine–metal complexes for the selective chromogenic sensing of cyanide anion N2 - Probe 1, which contains an anilinopyridine chromophore and an azaoxa macrocyclic subunit, presented an absorption band centered at 340 nm in acetonitrile. Addition of Fe(III), Cr(III) and Hg(II) induced the growth of a new absorption band at 430 nm (with color change from colorless to yellow), whereas in the presence of Cu(II), Zn(II) and Pb(II), less marked changes were observed. The color changes observed upon addition of Fe(III), Cr(III) and Hg(II) were ascribed to the formation of 1:1 stoichiometry complexes with probe 1. Coordination of Fe(III), Cr(III) and Hg(II) with the pyridine fragment of 1 induced an enhancement of the charge transfer character accompanied with a marked bathochromic shift that was reflected in a color change from colorless to yellow. The strength of the interaction between probe 1 and Fe(III) cation was modulated upon interaction with anions. Of all the anions tested, only cyanide was able to induce the bleaching of the yellow 1·Fe(III) complex solution. This bleaching was ascribed to the formation of 1·Fe(III)-CN complex that restored, to some extent, the optical features of the free probe allowing the chromogenic sensing of cyanide. Besides, 1·Fe(III) complex was used to detect cyanide in acetonitrile-water 90:10 v/v mixtures with good recoveries. KW - Anilinopyridine KW - Charge Transfer KW - Iron Complex KW - Colorimetric Test KW - Cyanide PY - 2018 DO - https://doi.org/10.1080/00958972.2018.1434719 SN - 0095-8972 VL - 71 IS - 6 SP - 786 EP - 796 PB - Taylor & Francis Group CY - London AN - OPUS4-45398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Buchholz, Michelle T1 - Dual Fluorescent Molecularly Imprinted Polymers (MIPs) for Detection of the Prevalent Anti-Inflammatory Drug Diclofenac N2 - Ensuring the purity of air and water is essential for the overall well-being of life on earth and the sustainability of the planet's diverse ecosystems. To achieve the goal of zero pollution, as outlined in the 2020 European Green Deal by the European Commission,[1] significant efforts are in progress. A key aspect of this commitment involves advancing more efficient and economically viable methods for treating wastewater. This includes the systematic monitoring of harmful pollutants such as heavy metals, microplastics, pesticides, and pharmaceuticals. One example is the presence of the anti-inflammatory drug diclofenac in water systems, primarily originating from its use as a gel or lotion for joint pain treatment. Diclofenac contamination in surface waters has been detected at approximately 10 μg L-1 (0.03 μM)[2] which is not solely due to widespread usage but also because of the drug's resistance to microbial degradation. Conventional wastewater treatment plants (WWTPs), which rely on biodegradation, sludge sorption, ozone oxidation, and powdered activated carbon treatment, struggle to efficiently remove diclofenac from wastewater.[3],[4] For instance, to enable WWTPs to efficiently monitor and optimize their processes, it would be advantageous to develop on-site detection and extraction methods for persistent pharmaceutical residues in aqueous samples. In this work, a sol-gel process was used to prepare Nile blue-doped silica nanoparticles (dSiO2-NPs) with a diameter of ca. 30 nm that were further functionalized to enable reversible-addition-fragmentation chain-transfer (RAFT) polymerization. To achieve fluorescence detection, a fluorescent monomer was used as a probe for diclofenac in ethyl acetate, generating stable complexes through hydrogen bond formation. The diclofenac/fluorescent monomer complexes were imprinted into thin molecularly imprinted polymer (MIP) shells on the surface of the dSiO2-NPs. Thus, the MIP binding behaviour could be easily evaluated by fluorescence titrations to monitor the spectral changes upon addition of the analyte. Doping the core substrate with Nile blue generates effective dual fluorescent signal transduction. This approach does not solely depend on a single fluorescence emission band in response to analyte recognition. Instead, it enables the fluorescent core to function as an internal reference, minimizing analyte-independent factors such as background fluorescence, instrumental fluctuation, and operational parameters.[5] Rebinding studies showed that the MIP particles have excellent selectivity towards the imprinted template and good discrimination against the competitor ibuprofen, with a discrimination factor of 2.5. Additionally, the limit of detection was determined to be 0.6 μM. Thus, with further optimization of the MIP, there is potential for the development of a MIP-based biphasic extract-&-detect fluorescence assay for simple, sensitive and specific sensing of diclofenac in aqueous samples down to the required concentrations of 0.03 μM. T2 - MIP2024: The 12th International Conference on Molecular Imprinting CY - Verona, Italy DA - 18.06.2024 KW - Sensor KW - Diclofenac KW - Molecularly Imprinted Polymers KW - Fluorescence KW - Pollutant PY - 2024 AN - OPUS4-60439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tobias, Charlie T1 - Design, Synthesis and Application of Polymer Core/Mesoporous Silica Shell Particles as Promising Tools for Multiplexed Assays N2 - The simultaneous detection of different analytes has gained increasing importance in recent years, especially in the fields of environmental and health monitoring. Particularly suitable formats for multiplexing are bead-based assays. The beads employed need to fulfil size and density requirements important for instance for flow cytometry and shall exhibit an as high as possible surface area for anchoring capture probes to allow for low limits of detection. Core/shell particles are ideally suited in this sense because of their modularity in design and adaptability for various (bio)analytical assays. Here, polystyrene particles coated with different kinds of mesoporous silica shells are presented, possessing distinctly higher surface areas in comparison to non-porous core/shell particles. Different factors such as pH and amount and type of mediator salt used during shell preparation were evaluated with shell inspection by scanning/transmission scanning electron microscopy (SEM/tSEM) being key to architecture control of the monodisperse particles. For a cytometric model assay, the optimized core/shell particles were functionalized with capture oligonucleotides for DNA detection. After covalent attachment of single-stranded DNA to the silane-modified silica surface, a hybridisation assay using labelled t-DNA complementary strands was carried out to demonstrate particle performance, showing how tailoring of the shell’s surface area controls sensitivity and dynamic range of the assay. Finally, a multiplex assay for the determination of DNA from different human papilloma virus (HPV) lines was developed. Using our optimized particles, we were able to detect down to 10 amolμl‒1, which is an improvement of one order of magnitude compared to assays using non-porous particles reported in the literature. In addition, multiplexed detection could successfully be demonstrated. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Core−shell particles KW - Bead-based assay KW - Flow cytometry KW - Multiplex PY - 2019 AN - OPUS4-48082 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - PT project „PAH in toys rubber“ N2 - Es werden die Arbeiten und aktuellen Ergebnisse zum Proficiency Test (PT)-Projekt "PAH in toys rubber" vorgestellt. Der PT wurde von der BAM organisiert und erfolgte im Rahmen der deutsch-chinesischen Arbeitsgruppe "Produktsicherheit" (BMWi/AQSIQ). Ziel des PT war es, die Messfähigkeiten deutscher und chinesischer Laboratorien hinsichtlich PAK in Spielzeugprodukten zu bewerten. Hintergrund sind neue PAK-Grenzwerte für Verbraucherprodukte und Spielzeug seit 27.12.2015 (EU-Verordnung 1272/2013). Neben der Herstellung und Charakterisierung des "PAK in Gummi" Referenzmaterials werden im Vortrag die Labor-Ergebnisse vorgestellt, die statistische Auswertung präsentiert und eine Bewertung der verwendeten Analysenverfahren vorgenommen. T2 - Fachworkshop zu den Themen Ringversuch und Referenzmaterialien CY - Xiamen, China DA - 19.10.2017 KW - Polyzyklische aromatische Kohlenwasserstoffe (PAK) KW - Ringversuch KW - Spielzeug PY - 2017 AN - OPUS4-43249 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bell, Jérémy A1 - Climent, Estela A1 - Gotor, Raúl A1 - Tobias, Charlie A1 - Martin-Sanchez, Pedro M. A1 - Rurack, Knut T1 - Dipstick coated with polystyrene-silica core-shell particles for the detection of microbiological fuel contamination N2 - Microbial contamination of fuels by fungi or bacteria poses risks such as corrosion and fuel system fouling, which can lead to critical problems in refineries and distribution systems and has a significant economic impact at every stage of the process. Many factors have been cited as being responsible for microbial growth, like the presence of water in the storage tanks. In fact, only 1 % water in a storage system is sufficient for the growth of microorganisms like bacteria or yeasts, as well as for the development of fungal biomass at the oil/water interface. This work presents a rapid test for the accurate determination of genomic DNA from aqueous fuel extracts. The detection is based on the use of polystyrene-mesoporous silica core-shell particles onto which modified fluorescent molecular beacons are covalently grafted. These beacons contain in the hairpin loop a target sequence highly conserved in all bacteria, corresponding to a fragment of the 16S ribosomal RNA subunit. The designed single-stranded molecular beacon contained fluorescein as an internal indicator and a quencher in its proximity when not hybridized. Upon hybridization in presence of the target sequence, the indicator and the quencher are spatially separated, resulting in fluorescence enhancement. To perform the assay the developed particles were deposited on different glass fibre strips to obtain a portable and sensitive rapid test. The assays showed that the presence of genomic DNA extracts from bacteria down to 50–70 μg L–1 induced a fluorescence response. The optical read-out was adapted for on-site monitoring by fitting a 3D-printed case to a conventional smartphone, taking advantages of the sensitivity of the CMOS detector. Such embedded assembly enabled the detection of genomic DNA in aqueous extracts down to the mg L–1 range and represents an interesting step toward on-site monitoring of fuel contamination. T2 - IMA 2023 CY - Chania, Greece DA - 18.09.2023 KW - Teststreifen KW - Test strip KW - Microbial KW - Mikrobiell KW - Smartphone KW - Particles KW - Partikeln PY - 2023 AN - OPUS4-58526 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hülagü, Deniz T1 - From 2D and Single Particle to 3D and Batch Analysis as a Routine Quality Check Procedure for the Morphological Characterization of Core-Shell Microparticles N2 - This study presents a practical procedure to give access to more information by tilting the sample holder and hence allowing images of a single particle to be recorded at different orientations under the same view angle. From the analysis of these images, extended information on surface roughness of the particle can be extracted. Thus, instead of obtaining 2D information from a single SEM image, three-dimensional (3D) information is obtained from 2D projections recorded at different particle orientations. T2 - Microscopy & Microanalysis 2022 CY - Online meeting DA - 31.07.2022 KW - Core-shell particles KW - 3D image analysis KW - Roughness KW - SEM tilting KW - Batch analysis PY - 2022 AN - OPUS4-55452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia T1 - Kopplung von Elektrochemie und Massenspektrometrie in der Mykotoxinforschung N2 - Mykotoxine werden als sekundäre Metabolite von Schimmelpilzen gebildet und haben diverse schädliche Effekte auf Menschen, Tiere und Pflanzen. Laut FAO sind weltweit bis zu 25 % aller Lebens- und Futtermittel mit Mykotoxinen kontaminiert, wodurch jährlich immense ökonomische Verluste entstehen. Neben den eigentlichen Mykotoxinen rücken zunehmend deren Transformationsprodukte (TPs) in den Fokus. Diese können als natürliche Stoffwechselprodukte toxischer sein als das eigentliche Mykotoxin und stellen eine potenzielle zusätzliche Gefahr für den Verbraucher dar. TPs werden überwiegend mit in vitro und in vivo Techniken untersucht, welche sowohl zeit- als auch kostenintensiv sind. Ziel war es nun, schnelle und zudem verlässliche Techniken zur Simulation von TPs diverser Mykotoxine zu testen. Die Kopplung von Elektrochemie und Massenspektrometrie, kurz EC/MS, als rein instrumenteller Ansatz ist seit vielen Jahren in der pharmazeutischen Forschung etabliert. Hierbei wird mithilfe einer elektrochemischen Durchflusszelle der oxidative Metabolismus einer Substanz simuliert und zugleich analysiert. Unter Verwendung von EC/MS, EC/LC/MS und HPLC-MS Techniken (MS/MS und FT-ICR) wurden nun die Mykotoxine Zearalenon, Citrinin und Dihydroergocristin (als Modellsubstanz für die Ergotalkaloide) elektrochemisch bei Potentialen bis zu 2500 mV vs. Pd/H2 oxidiert und deren TPs mit mikrosomalen in vitro Ansätzen verglichen. Hierbei konnten mehrere Übereinstimmungen hydroxylierter Spezies, sowohl elektrochemisch als auch biochemisch generiert, festgestellt werden. Die EC/MS ist somit auch in der Lebensmittelanalytik als nützliches und vielseitiges Werkzeug verwendbar. T2 - 24. Arbeitstagung des Regionalverband Nordost der LChG CY - Berlin, Germany DA - 06.03.2018 KW - Elektrochemie KW - Mykotoxine KW - Metabolismus PY - 2018 AN - OPUS4-44425 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Measurements of Photoluminescence Quantum Yields of Scattering LED Converter Materials N2 - How to Get it Right with the Absolute Measurement of Photoluminescence Quantum Yields of Scattering LED Converter Materials Saskia Fiedler+,a, Florian Frenzel+,a, Christian Würth a, Isabella Tavernaro a, Michelle Grüne c, Stefan Schweizer c,d, Axel Engel e, and Ute Resch-Genger a* a Division Biophotonics, Federal Institute for Materials Research and Testing (BAM), Richard-Willstaetter-Strasse 11, D-12489 Berlin, Germany; email: ute.resch@bam.de b Present address: Photonic Materials, NWO-Institute AMOLF, Science Park 104, 1098 XG Amsterdam, The Netherlands c Faculty of Electrical Engineering, South Westphalia University of Applied Sciences, Lübecker Ring 2, 59494, Soest, Germany d Fraunhofer Application Center for Inorganic Phosphors, Branch Lab of Fraunhofer Institute for Microstructure of Materials and Systems IMWS, Lübecker Ring 2, 59494, Soest, Germany e Schott AG Technical Services, Hattenbergstrasse 10, D-55122 Mainz, Germany Optical measurements of scattering materials such as luminescent nano- and microparticles and phosphors dispersed in liquid and solid matrices play an important role in energy conversion, solid-state lighting, medical diagnostics, and security barcoding. A key performance parameter is the photoluminescence quantum yield QY, i.e., the number of emitted per number of absorbed photons. QY of transparent luminophore solutions can be obtained relative to a fluorescence QY standard of known QY, meanwhile available as certified reference materials.[1] The determination of QY of scattering liquid and solid samples like nanoparticle dispersions, phosphors, and optoceramics requires, however, absolute measurements with an integrating sphere setup. Despite the need for reliable absolute QY measurements, no interlaboratory comparison (ILCs) on measurement uncertainties has been performed and scattering standards with known QY are not available. We present the results of an ILC of 3 labs from academia and industry on measurements of transparent and scattering dye solutions and solid phosphors and converter materials like YAG:Ce optoceramics with commercial stand-alone integrating sphere setups of different illumination and detection geometries. Special emphasis was dedicated to the influence of measurement geometry, optical properties of the blank for determining the number of incident photons absorbed by the sample, and sample-specific surface roughness. Matching QY values could be obtained for transparent dye solutions and scattering dispersions with a blank with scattering properties closely matching those of the sample, QY measurements of optoceramic samples with different blanks revealed substantial differences of more than 20 %. Based on our data, we recommend non-absorbing blank materials with a high reflectivity (>95 %) such as a 2 mm-thick PTFE target placed on the sample holder as blanks. T2 - eMRS CY - Strasbourg, France DA - 26.05.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Quantum yield KW - NIR KW - Characterization KW - Electron microscopy KW - Film KW - Integrating sphere spectroscopy KW - Calibration KW - Lifetime KW - Advanced materials KW - LED converter KW - YAG:Ce KW - ILC KW - Measurement uncertainty KW - Absolute quantum yield PY - 2025 AN - OPUS4-63327 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Gotor, Raul A1 - Tobias, Charlie A1 - Bell, Jérémy A1 - Martin-Sanchez, Pedro A1 - Rurack, Knut T1 - Dip Sticks Embedding Molecular Beacon-Functionalized Core−Mesoporous Shell Particles for the Rapid On-Site Detection of Microbiological Fuel Contamination N2 - Microbial contamination of fuels by fungi and bacteria presents risks of corrosion and fuel system fouling. In this work, a rapid test for the determination of microbial genomic DNA from aqueous fuel extracts is presented. It combines test strips coated with polystyrene core/mesoporous silica shell particles, to the surface of which modified fluorescent molecular beacons are covalently grafted, with a smartphone detection system. In the hairpin loop, the beacons incorporate a target sequence highly conserved in all bacteria, corresponding to a fragment of the 16S ribosomal RNA gene, which is also present to a significant extent in the 18S rRNA gene of fungi, allowing for broadband microbial detection. In the developed assay, the presence of genomic DNA extracts from bacteria and fungi down to ca. 20−50 μg L−1 induced a distinct fluorescence response. The optical read-out was adapted for on-site monitoring by combining a 3D-printed case with a conventional smartphone, taking advantage of the sensitivity of contemporary complementary metal oxide semiconductor (CMOS) detectors. Such an embedded assembly allowed to detect microbial genomic DNA in aqueous extracts down to ca. 0.2−0.7 mg L−1 and presents an important step toward the on-site uncovering of fuel contamination in a rapid and simple fashion. KW - Bacteria KW - Fungi KW - Rapid test KW - Fluorescence KW - Smartphone KW - Biofouling PY - 2020 DO - https://doi.org/10.1021/acssensors.0c01178 SN - 2379-3694 VL - 6 IS - 1 SP - 27 EP - 34 PB - American Chemical Society CY - Washington, DC AN - OPUS4-51956 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Streeck, C. T1 - Characterization of bio-molecular surfaces and liquids by means of reference-free X-ray spectrometry N2 - An increasing field of application for X-ray spectrometry and related analysis techniques is the investigation of tailor made functional surfaces modified by organic molecules. For a detailed understanding and further development of such functionalized surfaces, a quantitative determination of the surface density of molecular species or even specific functional groups is required. By means of reference-free X-Ray Fluorescence (XRF) spectrometry such customized surfaces can be analyzed quantitatively, when using specific marker elements. A chemical analysis of molecular bonds can be accomplished by X-Ray Absorption Spectroscopy in the Near-Edge region (NEXAFS). Especially in the soft X-ray range an access to relevant light elements like carbon C, nitrogen N and oxygen O is possible. Especially, the characterization of liquids and solid-liquid interfaces aiming at the determination of bio-molecular moieties (functional groups) is of great interest. The characterization of such systems requires the analysis of bio-molecules in their liquid environment. For the understanding of (biomolecular) reactions and binding processes the verification and quantification of biomolecule immobilization is essential. However, the analysis in the soft-X-ray range involves a higher experimental effort. In this contribution various successful applications of the characterizations of organofunctionalized surfaces, solid-liquid interfaces and liquids containing bio-molecular species by means of reference-free X-ray spectrometry will be presented. The experiments were performed at the plane-grating monochromator beamline (PGM-U49) in the soft X-ray range at the synchrotron radiation facility BESSY II. Using calibrated instrumentation and a quantification approach based on atomic fundamental parameters a quantitative access without any calibration sample or reference material is possible. In a complementary analysis by X-Ray Photoelectron Spectroscopy (XPS) and fluorescence measurements based on laserexcitation in the optical light spectrum the functional-group density of silane monolayers were determined. Here, the nitrogen atoms of the head-group of the label molecule employed could be used as specific marker for the reference-free quantitative XRF analysis and is used for traceable calibration of XPS and fluorescence spectroscopy. Furthermore, a novel UHV-compatible liquid-cell developed to investigate liquids and solidliquid interfaces will be presented. Protein attachment at the solid-liquid interface was investigated by detection of the characteristic N1s→π*(O=C-N) amide bond resonance in the N K-edge NEXAFS by using ultra-thin epoxy-functionalized SiC-windows. T2 - European Conference on X-Ray Spectrometry (EXRS) CY - Gothenburg, Sweden DA - 19.06.2016 KW - Bio-molecular surfaces KW - NEXAFS KW - XPS KW - XRS PY - 2016 AN - OPUS4-36965 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Russo, Francesco Friedrich T1 - Upscaling of spectral libraries for HREI- MS based non target analytics N2 - Gas Chromatography coupled with Electron Ionisation Mass Spectrometry (GC-EI-MS) is a well-established technique which, in combination with spectral libraries, has the potential to identify compounds in a sample. Nevertheless, most libraries are dominated by spectra with nominal mass resolution which does not allow to make full use of the data generated by modern high-resolution instruments. The production of high-resolution spectral library is time consuming and expensive, while in silico fragmentation tools that are capable of generating HR mass spectra are still too computationally intensive. We explored the alternative of using ML models to upscale existing spectral libraries. The models were trained with spectra from the RECETOX metabolome (DOI: 10.5281/zenodo.5483564), RECETOX Exposome (DOI: 10.5281/zenodo.4471216), and MassBank (10.5281/zenodo.7436394) HR-GC-MS libraries. The model was used to generate a synthetic library which was compared with a synthetic library simulated with CFM-ID (DOI: 10.1021/acs.analchem.6b01622). T2 - ANAKON 2023 CY - Vienna, Austria DA - 11.04.2023 KW - ML KW - GC-MS KW - EI-MS PY - 2023 AN - OPUS4-57358 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matschat, Ralf A1 - Hassler, J. A1 - Richter, Silke A1 - Kleve, M. A1 - Dette, A. T1 - Multielement trace analysis of pure graphite powders using optical emission spectrometry coupled to a magnetically stabilized DC arc supplied with halogenating gases as chemical modifiers – a rapid and robust methodology N2 - A magnetically stabilized DC arc device, designed for operation with OES spectrometers was used to determine the elements Ag, Al, B, Ba, Be, Ca, Co, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Nb, Ni, Si, Sn, Sr, Ti, V, Zr at trace levels of some μg kg−1 up to some 10 mg kg−1 in graphite powders. The coil for the generation of the homogeneous magnetic field was placed outside the closed arc chamber. The time programs of variable current strengths of the magnetic coil (up to 6 A) and of the arc (up to 17 A) which was burning in air were computer controlled. Halogenating gases (mainly CCl2F2, alternatively SF6 and NF3) were used as chemical modifiers to allow an effective release of the carbide forming trace elements. The mass flow controlled modifier gas was led through a special carrier electrode near the arc plasma. The emission radiation was guided by an optical fiber alternatively into two different ICP spectrometers in which the ICP torches were removed. The synergistic interaction of the magnetic field with the halogenating modifier gases resulted in a significant improvement in the analytical performance of the optimized analytical method. All our results for 22 trace elements were in good agreement with the means of an inter-laboratory comparison by BAM for certification of a pure graphite powder material; this holds also for our results for two other graphite materials. The optimized method showed an analytical performance suitable for comprehensive trace analysis of pure graphite. The instrumentation could be integrated into modern DC arc emission spectrometers to improve their analytical capabilities substantially. KW - Graphit KW - DC-Arc KW - High purity KW - Optical emission spectroscopy KW - Magnetically stabilized PY - 2018 DO - https://doi.org/10.1039/C7JA00387K SN - 1364-5544 SN - 0267-9477 VL - 33 IS - 3 SP - 468 EP - 480 PB - Royal Society of Chemistry AN - OPUS4-44398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gawlitza, Kornelia A1 - Johann, Sergej A1 - Mansurova, Maria A1 - Kohlhoff, Harald A1 - Tiebe, Carlo A1 - Bell, Jérémy A1 - Bartholmai, Matthias A1 - Rurack, Knut T1 - Semi-automatic Measurement Device for Long-Term Monitoring of Ammonia in Gas Phase N2 - In the present paper the development of a semi-automated device for long-term monitoring of gaseous ammonia is described. A sensor material was produced that changes its optical properties in the pres-ence of low concentrations of ammonia in air. The implementation into an electronic device enables precise, simple, economic and fast monitoring of low concentrations of harmful gases, like ammonia, and hence can help to improve the climate monitoring in livestock housing, barns or stables. T2 - SMSI 2021 CY - Online meeting DA - 03.05.2021 KW - Spectroscopy KW - Embedded sensor KW - Environment KW - Air quality PY - 2021 SP - 133 EP - 134 AN - OPUS4-52576 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Makowski, Maike T1 - Etablierung einer nicht-invasiven GC-MS Methode zur Messung von Trichodien als volatilen Mykotoxin-Marker in Getreide N2 - Aufgrund des weltweit steigenden Getreidekonsums ist die Überwachung des Getreidewachstums, der Lagerung und der Verarbeitung von immer größerer Bedeutung. Besonders während der Lagerung bilden Schimmelpilze sogenannte „Hot Spots“, in denen die Gehalte der Schimmelpilzgifte (Mykotoxine) weit über den vorgegebenen Grenzwerten liegen können. Wegen der ungleichen Verteilung der Toxine stellen Probenahme und die invasive, zeitaufwändige Analyse der Mykotoxine eine Herausforderung dar. Daher werden schnellere und einfachere Methoden benötigt, die sowohl die Probenahme als auch die Analyse beinhalten. Ein möglicher Ansatz ist die nicht-invasive Untersuchung der homogenen Gasphase über der Getreideprobe. Allerdings setzt diese Vorgehensweise die Anwesenheit von MVOC´s (microbial volatile organic compounds) voraus. Vorangegangene Studien zeigten, dass Trichodien ein Vorläufermolekül der Trichothecene – einer Mykotoxingruppe mit über 180 Substanzen – ist. Aufgrund seiner simplen sesquiterpenoiden Struktur war es bereits möglich, Trichodien mit Hilfe einer Headspace GC-MS Methode zu quantifizieren. Daher könnte es als Trichothecen-Markermolekül Anwendung finden. Allerdings bedarf dieser Sachverhalt weiterführender Untersuchungen. Der Zusammenhang zwischen der Trichodienkonzentration in der Gasphase und dem Mykotoxingehalt in der Probe muss beleuchtet werden, um Aussagen über den Trichothecengehalt in der Probe treffen zu können. Durch die Umsetzung dieser Überlegungen könnte der Nutzen von Trichodien erweitert und die Quantifizierung der Trichothecene stark vereinfacht werden. Daher beinhaltet der erste Schritt dieser laufenden Studie die Etablierung einer Referenzmethode unter Nutzung von Gaschromatographie gekoppelt mit Massenspektrometrie zur Messung von Trichodien als volatilen Mykotoxin-Marker in Getreide. Statische Headspace und SPME (solid phase micorextraction) wurden hierfür genutzt. In einem nächsten Schritt soll diese Referenzmethode zur Validierung einer schnellen vor-Ort Methode zur Bestimmung von Trichodien in Getreide dienen. T2 - 47. Lebensmittelchemikertag CY - Berlin, Germany DA - 17.09.2018 KW - Trichodien KW - Mykotoxin-Biomarker KW - Gaschromatographie-Massenspektrometrie PY - 2018 AN - OPUS4-46018 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - Entwicklung von Analysenverfahren, Standards und Referenzmaterialien für die Lebensmittelanalytik N2 - Mykotoxine gehören weltweit zu den am meisten untersuchten Kontaminanten in Lebensmitteln. Ihre zuverlässige Bestimmung ist zur Kontrolle geltender Grenzwerte notwendig und erfordert die Verfügbarkeit reiner Kalibrierstandards, valider Analysenverfahren sowie (zertifizierter) Referenzmaterialien. Im Vortrag werden die aktuellen Aktivitäten der BAM hinsichtlich der Entwicklung von Standards, Analysenverfahren und Referenzmaterialien für die Mykotoxin-Analytik vorgestellt. T2 - Netzwerk Diagnostik Berlin-Brandenburg e.V. CY - Berlin, Germany DA - 29.06.2016 KW - Mykotoxine KW - Lebensmittel KW - Qualitätssicherung PY - 2016 AN - OPUS4-38862 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Prakash, Swayam T1 - Silane Functionalized Paper Test Strips for Rapid and Sensitive Faecal Pigments Detection towards On-site Water Quality Testing N2 - Introduction. W.H.O estimated that globally at least 2 billion people use drinking water sources contaminated with faeces and according to UNICEF, most of these faecal detection methods are expensive, time-consuming (18–24 h time to result), and, with few exceptions, not suited for on-site analysis. Hence, there is an urgent need for the development of analytical methods that allow to unequivocally test for drinking water quality directly on-site. Aims. Development of rapid and sensitive fluorescence based analytical methods for faecal pigments (FPs) detection towards on-site water quality testing. Methods. Silane functionalized glass fiber paper test strips were developed for the sensitive drop-&-detect analysis of FPs. Drop casting of water samples containing faecal pigment on specifically functionalized test strips allowed the sensitive detection of FPs with a smartphone coupled to a 3D printed optical setup. Results. A series of silanes were used to functionalize glass fiber paper and tune its hydrophobicity, exploiting the influence of matrix tailoring to enhance binding of the Zn salt used as co-reagent to urobilin for optimal fluorescence response. Combination of bis(2-hydroxyethyl)-3-aminopropyltriethoxysilane with zinc chloride-impregnated test strips demonstrated optimum fluorescence response for sensitive (nano- and sub-nanomolar concentration) smartphone-based faecal pigments detection. The obtained fluorescence sensing results were validated with a benchtop fluorometer. Furthermore, the developed analytical method was successfully applied to the analysis of real water samples. Conclusions. The possibilities of matrix tailoring and co-reagent nature on the development of a rapid, sensitive, and embedded fluorescence-based on-site strip test are presented and discussed. This technique has potential application for faecal biomarker detection/primary screening for water quality in developing countries, where sophisticated instruments may not be available. T2 - 18th Conference of Methods and Applications in Fluorescence CY - Valencia, Spain DA - 08.09.2024 KW - Faecal contamination KW - Fluorescence KW - Metal complexes KW - Water analysis PY - 2024 AN - OPUS4-61479 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Climent Terol, Estela T1 - Novel specific bio-gated hybrid materials and their integration into versatile platforms for advanced sensing applications N2 - Methods for the rapid and sensitive detection of target analytes are gaining importance in medical diagnostics and environmental monitoring, in the security, occupational health and safety as well as food sectors. Among all of the methods employed for rapid tests, lateral flow assays (LFAs) are the most commonly used, and hundreds of test kits based on this technique are available on the market. A major drawback is that most of these capture agents either indicate the analyte only indirectly, and in most cases a second binding agent able to bind directly or indirectly to the analytes is necessary (e.g., a secondary labeled antibody). Furthermore, in certain cases in which the (ultra)trace detection of an analyte is required, the traditional approach of a certain number of probe molecules being conjugated to a particular support is not sufficient. Therefore, novel concepts implementing steps of effective signal amplification are urgently required. Keeping in mind these limitations, we thought that the sensitivity of these systems should be improvable through employment of gated reporter molecule-releasing hybrid nanoparticle materials on novel lateral flow devices. On one hand, the gated sensor material can produce a massive signal amplification, by releasing many reporter molecules only after chemical recognition of a few analyte molecules has taken place in an independent and separate step at the pore openings. On the other hand, the employment of tailored capture materials for the selective interaction with the released reporter molecules in a second arbitrary zone on the strip allows to concentrate or focus the latter for more efficient detection or to create selective multi-spot detection zones, which renders the simultaneous detection of several reporter molecules at the same time in multiplexed detection of various analytes possible. For that purpose, we have prepared several stimuli-responsive materials for small-molecule sensing based on specific interactions between biomolecules such as antibodies with the corresponding analytes for the detection of certain explosives. In order to prepare these bio-capped materials, we have selected silica mesoporous nanoparticles (MSNs) as inorganic support due to their unique properties such as defined void structure, high inner surface area and flexible functionalization chemistry. These MSNs are loaded with a brightly fluorescent indicator dye, and the external surface is subsequently functionalized with suitable molecules able to interact with antibodies, efficiently inhibiting dye release. The opening protocol and delivery of the entrapped dye is reminiscent of a displacement reaction involving the presence of the target analyte, producing a displacement of the biomolecule and allowing the detection of the target analyte. The presentation discusses general aspects of system design as well as analytical performance and highlights the integration into a lateral-flow assay, showing as an example the determination of the explosives TATP, TNT and PETN with fluorescence readout, in single-substance and multiplexing modes. T2 - EBS 2019 CY - Florence, Italy DA - 18.02.2019 KW - Bio-gated hybrid materials KW - Signal amplification KW - Explosives determination KW - Fluorescence KW - Rapid test KW - Dip-stick assay PY - 2019 AN - OPUS4-47920 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Herter, Sven-Oliver T1 - Quantifying Ergot Alkaloids in Food Using Newly Developed Stable Isotope-Labeled Standards N2 - Ergot alkaloids are a class of mycotoxins produced by fungi of the Claviceps genus, which are commonly found in contaminated cereals. Due to their toxic effects, the European Union introduced the first regulatory limit values for ergot alkaloids in food in 2022. Accurate quantification is crucial for food safety monitoring; however, the lack of stable isotopically labeled (SIL) standards has been a major limitation in the development of analytical methods via HPLC-MS/MS. In order to overcome this challenge, all 12 priority ergot alkaloids were synthesized as 13CD3-labeled analogues for the first time and used as internal standards for mass spectrometry-based analysis. Using HPLC-MS/MS, we quantified ergot alkaloids in various food matrices, including bread, rye – and wheat flour, and bran. The performance of the SIL standards was evaluated by comparing results obtained using external calibration and standard addition approaches. Our study demonstrates that the use of SIL standards significantly improves the accuracy and precision of ergot alkaloid quantification by correcting for matrix effects and signal variations in mass spectrometric analysis. The newly synthesized 13CD3-labeled ergot alkaloids provide a valuable tool for food safety assessments, ensuring more reliable and reproducible data. Furthermore, these findings support the advancement of analytical methods for ergot alkaloid monitoring, contributing to improved food quality control and regulatory compliance. T2 - 16th International Symposium on Biological and Environmental Reference Materials CY - Halifax, Nova Scotia, Canada DA - 01.06.2025 KW - Reference Material KW - HPLC-MS/MS KW - Metrology KW - Stable isotope dilution analysis KW - Quality assurance KW - Ergot alkaloids KW - Food Safety PY - 2025 AN - OPUS4-63409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Röthke, A. T1 - As good as or even better than ID-ICP-MS? High accuracy ICP OES determination of 1 g/kg mercury solutions N2 - To establish the SI traceability of the element content w(Hg) of a gravimetrically prepared 1 g/kg mercury solution, the latter was compared to a primary reference solution by means of high accuracy inductively coupled plasma optical emission spectrometry (ICP OES) measurements. For this purpose, the ICP OES bracketing method previously described [1] was improved to yield a relative expanded uncertainty of the mercury element content of Urel(w(Hg)) = 0.5 % (with k = 2) associated with the comparison of two monoelemental solutions. In case of mercury, such a small uncertainty was achieved for the first time. Before, in general, such small uncertainties were only reported applying isotope dilution methods performed with MC-ICP-MS. However, for mercury solutions at this concentration range, several dilution steps are necessary to prepare the samples for ID-MC-ICP-MS. The sum of the uncertainty contributions stemming from the dilution steps, as well as the intrinsic difficulties of measuring mercury at low concentrations, result in an overall uncertainty of the ICP-MS measurements, which is comparable to or even larger than those, achieved with the ICP OES method applied. We will present details of the sample preparation as well as of the dedicated ICP OES measurement approach, which were crucial to achieve such a small measurement uncertainty. The newly developed method was successfully applied in the context of the development and production of elemental solution chemical reference standards (CRS), which are distributed by the EDQM. The CRS are intended to support measurements required by the European Pharmacopoeia, which has recently incorporated a new international guideline for the control of elemental impurities in medicinal products. T2 - ICP-MS Anwendertreffen CY - Berlin, Germany DA - 03.09.2018 KW - Traceability KW - Mercury solution PY - 2018 AN - OPUS4-46218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - Applications of atomic absorption spectrometry for lithium isotope analysis N2 - An alternative method for lithium isotope analysis by using high-resolution atomic absorption spectrometry (HR-CS-AAS) is proposed herein. This method is based on monitoring the isotope shift of approximately 15 pm for the electronic transition 22P←22S at around the wavelength of 670.8 nm, which can be measured by state-of-the-art HR-CS-AAS. Isotope analysis can be used for (i) the traceable determination of Li concentration and (ii) isotope amount ratio analysis based on a combination of HR-CS-AAS and spectral data analysis by machine learning (ML). In the first case, the Li spectra are described as the linear superposition of the contributions of the respective isotopes, each consisting of a spin-orbit doublet, which can be expressed as Gaussian components with constant spectral position and width and different relative intensity, reflecting the isotope ratio in the sample. Precision was further improved by using lanthanum as internal spectral standard. The procedure has been validated using human serum-certified reference materials. The results are metrologically comparable and compatible with the certified values. In the second case, for isotope amount ratio analysis, a scalable tree boosting ML algorithm (XGBoost) was employed and calibrated using a set of samples with 6Li isotope amount fractions ranging from 0.06 to 0.99 mol mol−1. The training ML model was validated with certified reference materials. The procedure was applied to the isotope amount ratio determination of a set of stock chemicals and a BAM candidate reference material NMC111 (LiNi1/3Mn1/3Co1/3O2), a Li-battery cathode material. These determinations were compared with those obtained by MC-ICP-MS and found to be metrologically comparable and compatible. The residual bias was −1.8‰, and the precision obtained ranged from 1.9‰ to 6.2‰. This precision was sufficient to resolve naturally occurring variations. The NMC111 cathode candidate reference material was analyzed using high-resolution continuum source atomic absorption spectrometry with and without matrix purification to assess its suitability for technical applications. The results obtained were metrologically compatible with each other. T2 - Colloquium Spectroscopicum Internationale XLII (CSI XLII) CY - Gijón, Spain DA - 30.05.2022 KW - Lithium KW - HR-CS-AAS KW - Chemometrics KW - Atomic spectrometry PY - 2022 AN - OPUS4-56498 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella A1 - Abram, Sarah-Luise A1 - Homann, Christian A1 - Scholtz, Lena A1 - Radnik, Jörg A1 - Resch-Genger, Ute T1 - Validated and standardized measurements and quantification of surface functionalities on nanoparticles N2 - Surface-functionalized organic and inorganic engineered nanomaterials (NMs) are widely applied in the life and materials sciences. NM performance depends on key factors such as particle size and shape, crystal phase, morphology, chemical composition, and surface chemistry, i.e., surface coatings, functional groups (FGs), and ligands.1 The latter controls their processability and interaction with the environment and largely their possible toxicity. Thus, methods for FG quantification are important tools for quality control of NM production processes and can foster the sustainable development of functional and safe(r) NMs. This underlines the importance of validated and standardized analytical methods for surface analysis and reference materials.2 This encouraged us to explore simple and versatile tools for quantifying common bioanalytically relevant FGs such as optical assays, electrochemical titration methods, quantitative nuclear magnetic resonance spectroscopy (qNMR), and X-Ray photoelectron spectroscopy (XPS) and to perform a first interlaboratory comparison (ILC) on surface FG quantification.3,4 In a follow-up ILC, BAM and NRC explored qNMR sample preparation, measurement, and data evaluation protocols for commercial and custom-made aminated SiO2 NPs with sizes of 20-100 nm, different amounts of surface amino FGs, and different porosity.5,6 First, the number of amino FGs accessible for a dye reporter was determined with a cost-efficient, automated optical fluorescamine assay. Then, qNMR workflows and protocols were stepwise fine-tuned. The qNMR ILC was complemented by joint XPS measurements. BAM also examined the applicability of fast and automatable potentiometric titrations to screen the total amount of (de)protonable FGs on aminated SiO2 NPs. Our results underline the need to evaluate protocols for FG quantification in ILCs and the advantages of multi-method characterization strategies for efficient method cross validation. T2 - Surface and Micro/Nano Analysis Working Group CY - Paris, France DA - 08.04.2025 KW - Quality assurance KW - Reference material KW - Fluorescence KW - Nano KW - Particle KW - Surface analysis KW - XPS KW - Traceability KW - Metrology KW - Calibration KW - Reference data KW - Reference product KW - Digital certificate KW - QNMR KW - Potentiometry PY - 2025 AN - OPUS4-62969 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Climent Terol, Estela T1 - Antibody-gated indicator releasing mesoporous materials: a potential biosensor platform to be used in the development of rapid tests N2 - The urgent necessity to carry out reliable and relevant analytical measurements directly at a point-of-need is one of the current drivers for the development of miniaturised analytical systems, quick tests and wearables. Despite their simplicity, this type of tests must guarantee analytical relevance and reliability like laboratory-based analysis, e.g., in terms of sensitivity, selectivity, immunity against false positives and false negatives as well as robustness and repeatability. Keeping in mind the high sensitivity offered by gated indicator-releasing micro- and nanoparticles due to their inherent features of signal amplification, we performed several optimisations to develop a potential biosensor platform for use in rapid tests. Conceptually, these gated materials are closely related to drug delivery systems, consisting of high porous materials usually closed with macromolecular “caps” and loaded with indicator molecules that are released in presence of a target analyte. However, the key difference between the two types of functional materials is that many drug delivery systems should deliver their cargo over a longer period, often many hours, whereas the gated materials prepared for sensing should show fast release kinetics, on the order of <5 min. With the aim to optimise and adapt gated materials for sensing purposes, we prepared in this work several antibody-gated materials for small-molecule sensing. The materials consisted of porous silica particles containing indicator molecules in the pores and certain hapten molecules grafted to the particle surface close to the pore openings. The pores were then capped with antibodies binding to these haptens, thus inhibiting the escape of the indicators from inside of the pores. In presence of the corresponding analyte, the antibody is displaced from the surface of the material, allowing the escape of the indicators. This allows the detection of the analyte indirectly through an inherent signal amplification. In this work, the insecticide permethrin, a type-I pyrethroid, was selected as target model, because type-I pyrethroids play an important role in airplane disinfection. A first in-depth study of the various chemical tuning options of such antibody gated systems was performed. Different mesoporous silica supports, different functionalisation routes and different loading sequences were assessed. The materials’ performances were evaluated by studying their temporal response behaviour and detection sensitivity, including the tightness of pore closure (through the amount of blank release in absence of analyte) and the release kinetics. Our results indicate that the better the paratope-accommodating Fab region of the antibody “cap” fits into the host material’s pore openings, the better the closing/opening mechanism can be controlled. Because such materials can be used in various different formats from suspension assays[1] via microfluidic chips[2] to test strip-based lateral flow assays,[3] such materials present a powerful analytical particle platform for the sensitive analytics and diagnostics outside of a laboratory, realising sensitivities down to the µg kg–1 range in less analysis times of less than 5 min as we have recently demonstrated.[4] T2 - Biosensors for Pandemics CY - Online conference DA - 06.05.2020 KW - Hybrid materials KW - Pyrethroids KW - Signal amplification PY - 2020 UR - http://www.confstreaming.com/Biosensors2020/ AN - OPUS4-50746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Novel mobile multi-gas sensor for ammonia detection in the environment N2 - Pollution through emission of toxic gases becomes an increasing problem for the environment in agricultural, industrial and urban areas. In future, environmental emissions as well as ambient air must be monitored at even lower concentrations as nowadays. Consequently, demands arouse for measuring concentrations as low as the lower ppm or even ppb range. Current state-of-the-art technologies, as for instance electrochemical sensors, have reached their limits in this regard. The developed ammonia gas standard generator produces standard gas mixtures which comply with the metrological traceability for ammonia gas standards in the desired environmentally relevant measurement range of e. g. 0.5 to 500 nmol/mol. This gas standard preparation method is based on the permeation of ammonia through a membrane at a constant temperature as well as the mixing of this permeated gas with a carrier gas to adjust a gas standard of known concentration. The ammonia gas standard is suitable for the calibration of standard optical methods, e. g cavity ring-down spectroscopy (CRDS) and multi-gas sensors. The detection of gaseous ammonia in the lower ppm or even ppb range is obtained by incorporation of a fluorescent dye, which shows fluorescence enhancement in the presence of the analyte, into a polymer support being responsible for the accumulation of the analyte. The use of optical fluorescence as transduction mechanism enables high sensitivity as well as high temporal resolution. Here, we present first results on such a sensor system including the use of the developed gas standard generator for calibration issues. Additional benefits, particularly of fluorescence-based sensors, are their capability for miniaturization and potential multiplex mode. Beside the development of a highly sensitive and selective sensor, the integration of such systems into mobile sensor devices is addressed. These sensors and sensor systems are developed and will be validated and operated in form of functional models for the application areas, structure-integrated sensors and mobile multi-gas sensors. T2 - 2nd MetNH3 workshop on ammonia measurement methodology CY - Bern, Switzerland DA - 09.05.2017 KW - Ammonia KW - Permeation KW - Gas standard preparation KW - Fluorescence-based sensors PY - 2017 AN - OPUS4-40206 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartelmeß, Jürgen T1 - Developments Towards a BODIPY-based fluorometric sensing device for multiple hazardous gases N2 - Fluorometric sensing is a versatile approach for trace analysis outside of the laboratory, requiring suitable sensor materials and their integration into sensing devices. The versatility of fluorophores as probes, especially in terms of the possibility to tailor their optical as well as their recognition properties by synthetic modifications in a wide range, renders them as superior active component for the preparation of optical sensing devices. Recent works at BAM in this field include, for example, the detection of nerve gas agents, illustrating impressively the aforementioned benefits of fluorophores in optical sensing applications. In the interdisciplinary project presented here, we target hazardous gases such as ammonia, benzene, and hydrogen sulfide, next to others, which pose a major threat to human health and environmental safety and for which the availability of a sensitive and reliable detection method is highly desirable. The dyes presented follow a “turn-on” fluorescence schematic, which allows for the selective and sensitive detection of the respective gaseous analyte. The immobilization of the probe in polymeric matrices is then the next step toward the fabrication of a prototype device for molecular sensing. Further steps in the project include the assembly of instruments for test-atmosphere generation, the referencing of the sensor system, development and implementation of an optical setup, and the testing of the prototype device under laboratory conditions and in the field. In this presentation, we give an overview over the recent developments on this topic in our groups. Highlights are hydrogen sulfide sensitive, BODIPY based transition metal complexes, which allow for a sensitive as well as selective detection of the toxic gas. In addition, we present a novel class of highly substituted BODIPY derivatives – pocket-BODIPYs – which are of a synthetically high versatility and can readily be modified to create pockets in the periphery of the molecule of defined geometries. This is illustrated on the successful encapsulation of benzene by a pocket-BODIPY derivative, confirmed by X-ray crystallographic analysis as well as by further spectroscopic and analytical methods. T2 - International Conference on Porphyrins and Phthalocyanins (ICPP-10) CY - Munich, Germany DA - 01.07.2018 KW - BODIPY dye KW - Fluorometric sensing KW - Gas sensing PY - 2018 AN - OPUS4-45646 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Hoffmann, F. A1 - Jaeger, C. A1 - Bhattacharya, A. A1 - Schmitt, C. A. T1 - Nontargeted Identification of Tracer Incorporation in High- Resolution Mass Spectrometry N2 - “Fluxomics” refers to the systematic analysis of metabolic fluxes in a biological system and may uncover novel dynamic properties of metabolism that remain undetected in conventional metabolomic approaches. In labeling experiments, tracer molecules are used to track changes in the isotopologue distribution of metabolites, which allows one to estimate fluxes in the metabolic network. Because unidentified compounds cannot be mapped on pathways, they are often neglected in labeling experiments. However, using recent developments in de novo annotation may allow to harvest the information present in these compounds if they can be identified. Here, we present a novel tool (HiResTEC) to detect tracer incorporation in high-resolution mass spectrometry data sets. The software automatically extracts a comprehensive, nonredundant list of all compounds showing more than 1% tracer incorporation in a nontargeted fashion. We explain and show in an example data set how mass precision and other filter heuristics, calculated on the raw data, can efficiently be used to reduce redundancy and noninformative signals by 95%. Ultimately, this allows to quickly investigate any labeling experiment for a complete set of labeled compounds (here 149) with acceptable false positive rates. We further re-evaluate a published data set from liquid chromatography-electrospray ionization (LC-ESI) to demonstrate broad applicability of our tool and emphasize importance of quality control (QC) tests. HiResTEC is provided as a package in the open source software framework R and is freely available on CRAN. KW - Fluxomics KW - R package KW - Mass-Spectrometry PY - 2018 DO - https://doi.org/10.1021/acs.analchem.8b00356 VL - 90 IS - 12 SP - 7253 EP - 7260 PB - ACS Publications AN - OPUS4-45493 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - On the Integration of Fluorescent Probes with Molecularly Imprinted Polymers for Powerful Sensor Materials N2 - Molecularly imprinted polymers (MIPs) are an established and powerful matrix for the selective enrichment and separation of chemical species, especially of small organic molecules. Because MIPs contain cavities in their matrix that are complementary in size, shape and electronic/electrostatic or hydrogen bonding demand to the imprinted target molecule or template, they are frequently termed “artificial antibodies”. Compared to natural antibodies, they are chemically and physically much more robust. MIP formation proceeds through the polymerization of a mixture of functional monomers and cross-linkers in the presence of the template with subsequent extraction of the latter. While this strategy has been successfully employed for separation MIPs since decades, the development of sensory MIPs has long been limited to the combination of a MIP as enrichment phase with a separate signalling element in a discontinuous fashion, being unsuitable for many sensing applications. Only very recently, the implementation of specifically designed fluorescent probes into MIPs has been successfully accomplished, fluorescence being one of the most versatile, sensitive and easily miniaturizable techniques. This presentation will introduce basic design considerations, challenges, limitations and the potential that lies with such sensor materials on the background of the work carried out in our group. T2 - Bioinspired Materials 2017 CY - Manchester, UK DA - 31.08.2017 KW - Molecular imprinting KW - Dyes KW - Fluorescence KW - Sensing PY - 2017 AN - OPUS4-42260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hülagü, Deniz T1 - Analysis of the profile roughness of core-shell microparticles by electron microscopy N2 - A particle roughness analysis tool, based on electron microscopy (EM) images. The influence of various parameters on the calculated roughness was also investigated: the setting of the proper threshold, accelerating voltage, etc. The samples were gradually tilted to extend imaging information of more than only one projection. Furthermore, the measurement uncertainty of the profile roughness of particles associated to various orientations was estimated. T2 - Microscopy and Microanalysis 2021 CY - Online Meeting DA - 01.08.2021 KW - MamaLoCA KW - Particle characterization KW - Electron microscopy KW - Roughness KW - Core-shell particles KW - Image processing PY - 2021 AN - OPUS4-53069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Jaeger, C. A1 - Zaidi, Nousheen T1 - Cancer cell lipid class homeostasis is altered under nutrient-deprivation but stable under hypoxia N2 - Under oxygen/nutrient deprivation cancer cells modify the Balance between fatty acid (FA) synthesis and uptake, which alters the levels of individual triglyceride or phospholipid sub-species. These modifications may affect survival and drug-uptake in cancer cells. Here, we aimed to attain a more holistic overview of the lipidomic profiles of cancer cells under stress and assess the changes in Major lipid-classes. First, expressions of markers of FA synthesis/uptake in cancer cells were assessed and found to be differentially regulated under metabolic stress. Next, we performed a broad lipidomics assay, comprising 244 lipids from six major classes, which allowed us to investigate robust stress induced changes in median levels of different lipid classes -additionally stratified by fatty acid side chain saturation status. The lipidomic profiles of cancer cells were predominantly affected by nutrient-deprivation. Neutral lipid compositions were markedly modified under serum-deprivation and, strikingly, the cellular level of triglyceride subspecies decreased with increasing number of double bonds in their fatty acyl chains. In contrast, cancer cells maintained lipid class homeostasis under hypoxic stress. We conclude that although the levels of individual lipid moieties alter under hypoxia, the robust averages of broader lipid class remain unchanged. KW - Mass-Spectrometry KW - Tumor metabolism KW - Fatty acid metabolism KW - Lipidomic profile KW - Metabolic stress PY - 2018 DO - https://doi.org/10.1101/382457 SP - 1 EP - 25 PB - Cold Spring Harbor Laboratory CY - Cold Spring Harbor, NY AN - OPUS4-46814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tjaden, B. A1 - Baum, K. A1 - Marquardt, V. A1 - Simon, M. A1 - Trajkovic-Arsic, M. A1 - Kouril, T. A1 - Siebers, B. A1 - Lisec, Jan A1 - Siveke, J. T. A1 - Schulte, J. H. A1 - Benary, U. A1 - Remke, M. A1 - Wolf, J. A1 - Schramm, A. T1 - MYCN-induced metabolic rewiring creates novel therapeutic vulnerabilities in neuroblastoma N2 - MYCN is a transcription factor that is aberrantly expressed in many tumor types and is often correlated with poor patient prognosis. Recently, several lines of evidence pointed to the fact that oncogenic activation of MYC family proteins is concomitant with reprogramming of tumor cells to cope with an enhanced need for metabolites during cell growth. These adaptions are driven by the ability of MYC proteins to act as transcriptional amplifiers in a tissue-of-origin specific manner. Here, we describe the effects of MYCN overexpression on metabolic reprogramming in neuroblastoma cells. Ectopic expression of MYCN induced a glycolytic switch that was concomitant with enhanced sensitivity towards 2-deoxyglucose, an inhibitor of glycolysis. Moreover, global metabolic profiling revealed extensive alterations in the cellular metabolome resulting from overexpression of MYCN. Limited supply with either of the two main carbon sources, glucose or glutamine, resulted in distinct shifts in steady-state metabolite levels and significant changes in glutathione metabolism. Interestingly, interference with glutamine-glutamate conversion preferentially blocked proliferation of MYCN overexpressing cells, when glutamine levels were reduced. Thus, our study uncovered MYCN induction and nutrient levels as important metabolic master switches in neuroblastoma cells and identified critical nodes that restrict tumor cell proliferation. KW - Mass-spectrometry KW - Tumor metabolism KW - MYCN PY - 2018 DO - https://doi.org/10.1101/423756 SP - 1 EP - 21 PB - Cold Spring Harbor Laboratory CY - Cold Spring Harbor, NY AN - OPUS4-46815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gawlitza, Kornelia A1 - Johann, Sergej A1 - Mansurova, M. A1 - Kohlhoff, Harald A1 - Tiebe, Carlo A1 - Bell, Jérémy A1 - Bartholmai, Matthias A1 - Rurack, Knut T1 - Semi-automatic Measurement Device for Long-Term Monitoring of Ammonia in Gas Phase N2 - The present paper describes the development of a sensor material that changes its fluorescence in the presence of gaseous ammonia in a relevant concentration range. The implementation into a semi-automatic gas measurement device enables low-cost, precise, simple and fast monitoring of low con-centrations of harmful gases, like ammonia, and hence can help to improve the climate monitoring in livestock housing, barns or stables. T2 - SMSI 2020 CY - Meeting was canceled KW - Spectroscopy KW - Emmbedded sensor KW - Environment KW - Air quality PY - 2020 DO - https://doi.org/10.5162/SMSI2020/B5.4 SP - 133 EP - 134 AN - OPUS4-50867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ritter, B. A1 - Haida, P. A1 - Fink, F. A1 - Krahl, T. A1 - Gawlitza, Kornelia A1 - Rurack, Knut A1 - Scholz, G. A1 - Kemnitz, E. T1 - Novel and easy access to highly luminescent Eu and Tb doped ultra-small CaF2, SrF2 and BaF2 nanoparticles – structure and luminescence N2 - A universal fast and easy access at room temperature to transparent sols of nanoscopic Eu3+ and Tb3+ doped CaF2, SrF2 and BaF2 particles via the fluorolytic sol–gel synthesis route is presented. Monodisperse quasi-spherical nanoparticles with sizes of 3–20 nm are obtained with up to 40% rare earth doping showing red or green luminescence. In the beginning luminescence quenching effects are only observed for the highest content, which demonstrates the unique and outstanding properties of these materials. From CaF2:Eu10 via SrF2:Eu10 to BaF2:Eu10 a steady increase of the luminescence intensity and lifetime occurs by a factor of ≈2; the photoluminescence quantum yield increases by 29 to 35% due to the lower phonon energy of the matrix. The fast formation process of the particles within fractions of seconds is clearly visualized by exploiting appropriate luminescence processes during the synthesis. Multiply doped particles are also available by this method. Fine tuning of the luminescence properties is achieved by variation of the Ca-to-Sr ratio. Co-doping with Ce3+ and Tb3+ results in a huge increase (>50 times) of the green luminescence intensity due to energy transfer Ce3+ → Tb3+. In this case, the luminescence intensity is higher for CaF2 than for SrF2, due to a lower spatial distance of the rare earth ions. KW - Luminescence materials KW - Alkaline earth metal fluorides KW - Fluorolytic sol–gel synthesis PY - 2017 DO - https://doi.org/10.1039/C6DT04711D VL - 46 IS - 9 SP - 2925 EP - 2936 PB - Royal Society of Chemistry AN - OPUS4-39286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Costa, Elena T1 - Development of a rapid test for on-site measurement of pyrethroid surface residues N2 - Type-I pyrethroids are frequently used for disinfection purposes against insects such as adult mosquitoes, or diseases carried by insects, like Malaria or Zika in cabins of airplanes on long-distance flights especially from tropical destinations. This treatment is mandatory at various airports but compliance with the rules is difficult to test for. Moreover, if improperly used, these compounds can entail negative health effects for crews and passengers. The detection of the pyrethroids will be achieved thanks to an antibody-gated indicator delivery system (gAID) utilizing monoclonal antibodies and hybrid sensory nanoparticles. After the interaction of the pyrethroid with the gAID, the liberated indicator (dye) will be detected. Since only few analyte molecules are necessary for pore opening yet release a large number of dyes, the system shows intrinsic signal amplification. The device system to be developed has to be so simple that chemically untrained personnel, such as ground or cabin crew, can use it and obtain a result in a reasonably short period of time, e.g., ≤5 min. The need for high accuracy and sufficient sensitivity, established at 0.001 g m–2, is a critical requirement and imposes another significant challenge since this value is beyond current LFTs reported in the literature for pesticide detection to date. In order to achieve the selectivity and sensitivity required by the test itself, and to avoid cross reactivity with other type I pyrethroids, the production of a monoclonal antibody for both Permethrin and Phenontrin is necessary. The synthesis of the two hapten molecules and the subsequent immunization with different immunogens represent the first goal of the work. T2 - Rapid Methods Europe 2018 CY - Amsterdam, The Netherlands DA - 05.11.2018 KW - Pyrethroids KW - Raid test KW - Test strip KW - Delivery system KW - Air traffic PY - 2018 AN - OPUS4-47128 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Temgoua, Ranil C. T. T1 - Hyphenated Electrochemistry-Liquid Chromatography-Mass Spectrometry (EC-LC-MS) N2 - The coupling of electrochemistry with mass spectrometry (EC-MS) represents a revolutionary approach for studying redox-active compounds, which constitute over 90% of known chemical entities. This poster demonstrates the versatility of EC-MS as a rapid and environmentally friendly alternative to traditional in-vivo and in-vitro methods. Our focus encompasses three key applications: Simulation of drug metabolism pathways, investigation of environmental xenobiotic degradation/fate (eFate), and green synthesis of analytical standards. T2 - 56th annual conference of the DGMS (Deutschen Gesellschaft für Massenspektrometrie) CY - Göttingen, Germany DA - 04.03.2025 KW - Electrochemistry KW - Mass Spectrometry KW - Emerging pollutants KW - Transformation products PY - 2025 AN - OPUS4-63517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pisonero, J. A1 - Bouzas-Ramos, D. A1 - Traub, Heike A1 - Cappella, Brunero A1 - Álvarez-Llamas, C. A1 - Richter, Silke A1 - Mayo, J. C. A1 - Costa-Fernandez, J. M. A1 - Bordel, N. A1 - Jakubowski, Norbert T1 - Critical evaluation of fast and highly resolved elemental distribution in single cells using LA-ICP-SFMS N2 - The analytical potential of a nanosecond laser ablation coupled plasma mass spectrometer (ns-LA-ICP-SFMS)system is investigated for fast and highly spatially resolved (~µm) elemental distribution within single cells. The size, morphology and overlapping of laser-induced craters has been investigated with Atomic Force Microscopy (AFM). KW - Atomic Force Microscopy KW - Laser Ablation KW - Elemental Distribution PY - 2019 DO - https://doi.org/10.1039/c8ja00096d SN - 0267-9477 VL - 34 IS - 4 SP - 655 EP - 663 PB - RSC AN - OPUS4-48549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Gojani, Ardian B. A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - From 2D and Single Particle to 3D and Batch Analysis as a Routine Quality Check Procedure for the Morphological Characterization of Core-Shell Microparticles N2 - CS particles show unique properties by merging individual characteristics of the core and the shell materials. An alteration particularly in their surface roughness affects the final performance of the particles in the targeted application. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task employing microscopic techniques being scarce and showing large differences in terms of methodology and results. In our previous work, we have reported a systematic study with a reliable analysis tool, which evaluates profile roughness quantitatively, for individual core-shell microparticles using electron microscopy (EM) images of both types, Scanning Electron Microscopy (SEM) and transmission mode SEM (or TSEM). The SEM images contain two-dimensional (2D) information, therefore, provide profile roughness data only from the projection in the horizontal plane (in other words, from the “belly”) of a spherical particle. The present study offers a practical procedure to give access to more information by tilting the sample holder and hence allowing images of a single particle to be recorded at different orientations under the same view angle. From the analysis of these images, extended information on surface roughness of the particle can be extracted. Thus, instead of obtaining 2D information from a single SEM image, three-dimensional (3D) information is obtained from 2D projections recorded at different particle orientations. T2 - Microscopy and Microanalysis 2022 CY - Oregon, Portland, USA DA - 31.07.2022 KW - Core-shell particles KW - Image processing KW - Roughness KW - Scanning electron microscopy KW - Tilting PY - 2022 DO - https://doi.org/10.1017/S1431927622002094 SN - 1431-9276 VL - 28 IS - S1 SP - 332 EP - 334 PB - Cambridge University Press AN - OPUS4-55373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pfeifer, Jens T1 - RSFs for nickel matrix using doped pressed powder samples as needed for fast flow glow discharge mass spectrometry (GD-MS) N2 - Direct current (DC) fast flow glow discharge mass spectrometry is an important and versatile tool for multielemental trace analysis of conductive solid materials down to the µg/kg level. Special benefits are minimum demands on sample preparation, avoiding losses and contamination, and only short analysis time. For fast flow GD sources, the quantification strategy based on relative standard sensitivity factors (Standard RSFs) which are independent of matrix is not sufficiently satisfying regarding accuracy for each matrix and element [1]. Therefore matrix-matched calibration samples (MMCS) are required to achieve reliable quantification. In fact, the list of existing certified reference materials (CRM) appropri-ate for calibration in trace analysis is rather short. Convenient synthesis of homogeneous MMCS, as e.g. easily obtained in liquid sampling spectrometry, can facilitate the application of fast flow GD-MS for quantification of impurities in a variety of matrices. Pressing of metal powders for the preparation of MMCS for GD-MS was suggested earlier [2], the method was further modified by use of analyte solutions for doping of rather pure metal powders such as Cu and Zn [3], but has not yet been applied Ni matrix. In the present work we describe the determination of matrix-dependent relative sensitivity factors (RSFs) for Mg, Al, Cr, Mn, Fe, Co, Cu, Zn, Ag, Cd, Tl, Pb and Bi in pure Ni by using the liquid doping approach for the preparation of synthetic pressed Ni-powder samples. A four point-calibration was used applying the fast flow glow discharge mass spectrometer, Element GD (Thermo Fisher). The determined RSF were verified against suitable CRM and compared with the standard RSF given by the supplier of the instrument. The obtained results demonstrate a satisfying Agreement with the certified values of the CRM and a significant improvement for the quantification of most of the determined elements in comparison with standard RSF. T2 - International glow discharge spectroscopy symposium CY - Liverpool, UK DA - 18.04.2016 KW - GD-MS KW - Glow discharge KW - Nickel RSF KW - Calibration KW - Quantification PY - 2016 AN - OPUS4-35818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Makowski, Maike T1 - Non-invasive Cereal Analysis by GC-MS detection of Trichodiene as a Volatile Mycotoxin Biomarker N2 - Due to the increasing consumption of cereals worldwide, the monitoring of growth, storage and processing is becoming more and more crucial. Particularly when stored, infested grains breed fungal clusters (“hot spots”) in which mycotoxins greatly exceed allowed maximum levels. Because of their unpredictable presence, current sample drawing and procedures for mycotoxin analysis represent a complex challenge for operators, involving invasive and cost intensive steps. Therefore, new time- and labour-saving mycotoxin control methods including sampling and analysis steps are needed. A possible approach is the non-invasive analysis of the homogeneous gas phase above the crops, instead of analyzing random samples. However, this procedure requires microbial volatile organic compounds (MVOC´s) being released by the samples and representing the present mycotoxins. Previous investigations revealed trichodiene to be a precursor in trichothecenes biosynthesis – one of the largest mycotoxin groups with over 180 compounds. Due to its non-functionalized sesquiterpene structure, trichodiene has already been quantified using Headspace GC-MS methods (for instance). Thereby, it can possibly be used as a biomarker for trichothecene contamination in foodstuff. However, further investigations are necessary. The correlation between trichodiene concentration in the gas phase and trichothecenes mass fraction in the sample must be examined closely to draw conclusions about the exact trichothecene content within samples. Realizing this idea, would widely extend the applicability of trichodiene and enormously simplify trichothecene quantification. Hence, this first step of an ongoing study aims to develop a laboratory reference method using trichodiene as volatile biomarker to quantify trichothecenes in cereals. Static headspace and SPME-enrichment coupled to gas chromatography with mass spectrometry (GC-MS) were employed. In a second step, this reference method is intended to validate new approaches for fast on-site screening of trichodiene in cereals. T2 - 10th World Mycotoxin Forum Conference CY - Amsterdam, The Netherlands DA - 11.03.2018 KW - Trichodiene KW - GC-MS KW - Mycotoxin Biomarker PY - 2018 AN - OPUS4-44509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholl, Juliane T1 - Fluorinated Additives used in LiBs: Forever Chemicals of Tomorrow? N2 - Fluorinated organic compounds (FOCs) are a type of man-made chemicals characterized by their robust carbon-fluorine bonds, which contribute to their chemical stability and resistance to degradation. This durability makes them valuable in various applications, such as lithium-ion batteries (LiBs) [1-3], could have a significant impact on the environment, but this potential has not yet been fully considered. This study examines the environmental impact of two fluorinated aromatics, tris(pentafluorophenyl)borane (TPFPB) and tris(pentafluorophenyl)phosphine (TPFPP), given their role in enhancing the performance of LiBs[4, 5]. In order to achieve this, a number of laboratory simulation methods were employed, including total oxidizable precursor assay, electrochemistry (EC), Fenton reaction, UV-C irradiation, and hydrolysis. Liquid chromatography and gas chromatography coupled with high-resolution mass spectrometry were employed for the identification of transformation products (TPs) and the prediction of their molecular formulae. Notwithstanding their structural similarities, TPFPB and TPFPP exhibited distinct differences in their electrochemical behavior and degradation pathways. TPFPB was readily transformed via hydroxylation and hydrolysis, resulting in a diverse range of 49 TPs. In total, 28 TPs were newly identified, including oligomers and highly toxic dioxins. In contrast, TPFPP degraded only under extreme conditions, highlighting the need to develop new conditioning protocols for EC. Overall, the simulation experiments produced 9 structurally unique compounds, including 7 previously unidentified partially defluorinated byproducts. This study emphasizes the potential hazards linked to the use of FOCs in lithium-ion batteries and enhances our understanding of the complex environmental interactions of these compounds. T2 - Adlershofer Forschungsforum 2024 CY - Berlin, Germany DA - 11.11.2024 KW - PFAS KW - Lithium-ion batteries KW - Fluorinated Compounds KW - Simulation methods KW - Liquid chromatography/ QTOF-MS KW - Gas chromatography/ QTOF-MS KW - Electrochemistry KW - Photochemistry KW - Top-Assay PY - 2024 AN - OPUS4-61681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schrezenmeier, E. A1 - Hoffmann, F. A1 - Jaeger, C. A1 - Schrezenmeier, J. A1 - Lisec, Jan A1 - Glander, P. A1 - Algharably, E. A1 - Kreutz, R. A1 - Budde, K. A1 - Duerr, M. A1 - Halleck, F. T1 - Pharmacokinetics of Daclatasvir, Sofosbuvir and GS-331007 in a Prospective Cohort of HCV positive Kidney Transplant Recipients N2 - Limited data exist on the pharmacokinetic profile of novel direct acting antivirals in kidney transplant recipients. Daclatasvir is primarily eliminated via the biliary route and sofosbuvir via the renal route; here we report the pharmacokinetic profile of combined treatment with these compounds in a prospective study of hepatitis C virus positive kidney transplant recipients (EudraCT: 2014-004551-32). In this study plasma samples of 16 HCV positive kidney transplant recipients receiving daclatasvir and sofosbuvir were collected at 4 time points at day 1, 7, 14, 21, 56, and 84 after start of treatment. Inclusion criteria were stable graft function and an estimated GFR (eGFR) > 30mL/min/1.73m. Daclatasvir, sofosbuvir and GS-331007 (inactive metabolite of sofosbuvir) plasma concentrations were determined using ultra-performance liquid chromatography quadrupole time of flight mass spectrometry. All patients showed a rapid virological response with HCV RNA below the detection limit 21 days after the start of therapy (medium time to viral clearance). No difference of the areas under the concentration-time curve (AUC) of daclatsavir, sofosbuvir and GS-331007 was observed between patients with an eGFR below or ≥ 60mL/min. For GS-331007, no relevant changes of trough levels were observed over time. Mean GS-331007 trough levels were 339.5±174.9 ng/mL in patients with an eGFR ≥ 60mL/min and 404.3±226 ng/mL in patients with an eGFR < 60mL/min at day 7 (p=0.52). At day 84, GS-331007 trough levels were 357.8±200.8 ng/mL and 404.2±70.2 ng/mL in patients with an eGFR ≥ 60 mL/min and in patients with an eGFR < 60 mL/min, respectively (p=0.51). The accumulation ratios of renally eliminated GS-331007 for AUC and Cmax did not significantly differ between the two eGFR groups at day 7. An impaired eGFR (30-60 mL/min) does not lead to a dose accumulation of daclatasvir, sofosbuvir and GS-331007. This study provides the rationale for future studies investigating the pharmacokinetic profile of sofosbuvir based HCV treatment in kidney transplant recipients with an eGFR < 30 mL/min. KW - Mass-Spectrometry PY - 2018 DO - https://doi.org/10.1097/FTD.0000000000000567 SN - 0163-4356 VL - 41 IS - 1 SP - 53 EP - 58 PB - Wolters Kluwer AN - OPUS4-46647 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - X-rays without X-rays: Can muon tomography provide pictures from within concrete and other objects? N2 - Until the 1980s radiography was used to inspect civil structures in case of special demands and showed a much better resolution than other NDT techniques. However, due to safety concerns and cost issues, this method is almost never used anymore. Meanwhile, non-destructive techniques such as ultrasound or radar have found regular, successful practical application but sometimes suffer from limited resolution and accuracy, imaging artefacts or restrictions in detecting certain features when applied to reinforced or prestressed concrete inspection. Muon tomography has received much attention recently. Muons are particles generated naturally by cosmic rays in the upper atmosphere and pose no risk to humans. Novel detectors and tomographic imaging algorithms have opened new fields of application, mainly in the nuclear sector, but also in spectacular cases such as the Egyptian pyramids. As a first step towards practical application in civil engineering and as a proof of concept we used an existing system to image the interior of a reference reinforced 600 kg concrete block. Even with a yet not optimized setup for this kind of investigation, the muon imaging results have been at least of similar quality compared to ultrasonic and radar imaging, potentially even better. Recently, the research was expanded to more realistic testing problems such as the detection of voids in certain structural elements. However, before practical implementation, more robust, mobile, and affordable detectors would be required as well as user-Friendly imaging and simulation software. The talk also discusses other applications , such as volcanology, mining and geothermal exploration. T2 - RWTH Aachen, Geophysikalisches Seminar CY - Aachen, Germany DA - 11.01.2024 KW - Muon tomography KW - Civil engineering KW - Mining KW - Geothermal engineering PY - 2024 AN - OPUS4-59349 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - X-rays without X-rays: Can muon tomography provide pictures from within concrete objects? N2 - Until the 1980s radiography was used to inspect civil structures in case of special demands and showed a much better resolution than other NDT techniques. However, due to safety concerns and cost issues, this method is almost never used anymore. Meanwhile, non-destructive techniques such as ultrasound or radar have found regular, successful practical application but sometimes suffer from limited resolution and accuracy, imaging artefacts or restrictions in detecting certain features when applied to reinforced or prestressed concrete inspection. Muon tomography has received much attention recently. Muons are particles generated naturally by cosmic rays in the upper atmosphere and pose no risk to humans. Novel detectors and tomographic imaging algorithms have opened new fields of application, mainly in the nuclear sector, but also in spectacular cases such as the Egyptian pyramids. As a first step towards practical application in civil engineering and as a proof of concept we used an existing system to image the interior of a reference reinforced 600 kg concrete block. Even with a yet not optimized setup for this kind of investigation, the muon imaging results have been at least of similar quality compared to ultrasonic and radar imaging, potentially even better. Recently, the research was expanded to more realistic testing problems such as the detection of voids in certain structural elements. However, before practical implementation, more robust, mobile, and affordable detectors would be required as well as user-Friendly imaging and simulation software. T2 - ISNT NDE 2023 CY - Pune, India DA - 07.12.2023 KW - Muon tomography KW - Concrete KW - Civil engineering PY - 2023 AN - OPUS4-59347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Scholtz, Lena A1 - Resch-Genger, Ute T1 - Behind the Paper - Dual color pH probes made from silica and polystyrene nanoparticles and their performance in cell studies N2 - In this contribution we highlight the importance of comparison for scientific research while developing a new, functional pH sensor system, and the valuable insights this can provide. KW - Dye KW - Optical Spectroscopy KW - pH probe KW - Silica and Polystyrene Particles KW - Nano KW - Surface groups KW - Safe-by-Design KW - Cell studies KW - Sensors KW - Particle Synthesis KW - Fluorescence PY - 2023 UR - https://communities.springernature.com/posts/dual-color-ph-probes-made-from-silica-and-polystyrene-nanoparticles-and-their-performance-in-cell-studies SP - 1 EP - 2 PB - Springer Nature CY - London AN - OPUS4-59150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - ridge Monitoring by Ultrasonic Coda Wave Interferometry N2 - The built infrastructure ages and requires regular inspection and, when in doubt, monitoring. To ensure that older concrete bridges showing signs of deterioration can be used safely, several innovative monitoring tools have been introduced, including but not limited to optical, fiber-optic, or acoustic emission techniques. However, there are gaps in the portfolio. A sensing technique that covers a wide range of damage scenarios and larger volumes, while still being sensitive and specific, would be beneficial. For about 15 years, research has been conducted on ultrasonic monitoring of concrete structures that goes beyond the traditional ultrasonic pulse velocity test (PV test), mostly using a very sensitive data evaluation technique called coda wave interferometry. At BAM we have developed sensors and instrumentation specifically for this method. We have instrumented a 70-year-old, severely damaged prestressed concrete bridge in Germany in addition to a commercial monitoring system. We have now collected data for almost 3 years. We can show that we can provide information about the stress distribution in the bridge. We have also been able to confirm that there has been no significant additional damage to the bridge since the installation. T2 - ISNT NDE 2023 CY - Pune, India DA - 07.12.2023 KW - Coda wave interferometry KW - Structural health monitoring KW - Ultrasound KW - Concrete KW - Bridges PY - 2023 AN - OPUS4-59346 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Petrov, Eugene A1 - Würth, Christian A1 - Richter, Maria A1 - Resch-Genger, Ute T1 - Fluorescence Standards from BAM - Dye Solutions and Polymer systems N2 - For fluorescence microscopy, there is an increasing need for suitable calibration tools and reference materials for microscope calibration, the determination of performance parameters, and the regular control and validation of instrument performance. This is addressed in the BmWk-financed project FluMikal (WIPANO program) by two research groups from academia and two companies, that is coordinated by BAM. Here we present different approaches to liquid and solid fluorescence standards for the determination of the wavelength-dependent spectral sensitivity of fluorescence microscopes and ideas concerning the choice of suitable fluorescence lifetime standard for increasingly utilized fluorescence lifetime imaging (FLIM). T2 - FluMiKal Projectmeeting CY - Munich, Germany DA - 27.11.2023 KW - Reference material KW - Reference product KW - Fluorescence microscopy KW - Quality assurance KW - Instrument performance validation KW - Lifetime standard PY - 2023 AN - OPUS4-59120 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - Design of Fluorescent, Amorphous Silica-NPs and their Versatile Use in Sensing Applications N2 - Surface functionalized silica nanoparticles (SiO2-NP) gained great interest in the life and material sciences, as they can be used e.g. as drug carriers, fluorescent sensors, and multimodal labels in bioanalytical assays and imaging applications. They are highly stable, are easily produced and modified on a large scale at low cost and can be labeled or stained with a multitude of sensor dyes. These dye modified particle conjugates have several advantages as compared to conventional molecular probes like enhanced brightness, ease of designing ratiometric systems by combining analyte-sensitive and inert reference dyes, and increased photostability. Moreover, stained nanoparticles can enable the use of hydrophobic dyes in aqueous environments. Here we present our work on multicolored sensors for the measurement of pH, oxygen and saccharides utilizing amorphous SiO2 NPs. T2 - Focus Area Day Analytical Sciences 2023 CY - Berlin, Germany DA - 20.04.2023 KW - Amorphous silica particles KW - Particle Synthesis KW - Nano KW - Ratiometric Sensors KW - Fluorescence KW - pH probe KW - Dye PY - 2023 AN - OPUS4-59151 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wegner, Karl David T1 - SWIR luminescent nanomaterials – key chemical parameters for bright probes for in vivo bioimaging N2 - A current challenge for studying physio-pathological phenomena and diseaserelated processes in living organisms with non-invasive optical bioimaging is the development of bright optical reporters that enable deep tissue penetration, a high detection sensitivity, and a high spatial and temporal resolution. The focus of this project are nanomaterials, which absorb and emit in the shortwave infrared (SWIR) between ~900–2500 nm where scattering, absorption, and autofluorescence of the tissue are strongly reduced compared to the visible and NIR. T2 - QD2024 - 12th International Conference on Quantum Dots CY - Munich, Germany DA - 18.03.2024 KW - Quantum dots KW - Advanced nanomaterials KW - Fluorescence KW - Quality assurance KW - Gold nanocluster KW - Shortwave infrared KW - Spectroscopy KW - Bioimaging PY - 2024 AN - OPUS4-59783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute T1 - Tumore abbilden, Biomarker nachweisen, Messungen standardisieren N2 - Zu den am häufigsten eingesetzten Analysemethoden in den Lebens- und Materialwissenschaften gehören Lumineszenzmethoden. Sie nutzen die Emission von Licht nach Absorption von Energie, um Signale zu erzeugen, und umfassen spektroskopische und mikroskopische Messungen. KW - Quality assurance KW - Sensor KW - Imaging KW - Reference material KW - Nano KW - Particle KW - Nanomaterial KW - Upconversion KW - Nanoparticle KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Excitation KW - Power density KW - Single particle KW - Brightness KW - NIR PY - 2021 SP - 75 EP - 77 PB - GDCH AN - OPUS4-53526 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Würth, Christian A1 - Pauli, Jutta A1 - Weigert, Florian T1 - Quantitative optical-spectroscopic characterization of luminescent nanomaterials - Photoluminescence Quantum Yields N2 - Accurate and quantitative photoluminescence measurements are mandatory for the comparison of different emitter classes and the rational design of the next generation of molecular and nanoscale reporters as well as for most applications relying on their luminescence features in the life and material sciences and nanobiophotonics. In the following, procedures for the determination of the spectroscopic key parameter photoluminescence quantum yield, i.e., the number of emitted per absorbed photons, in the UV/vis/NIR/SWIR are presented including pitfalls and achievable uncertainties and material-specific effects related to certain emitter classes are addressed. Special emphasis is dedicated to luminescent nanocrystals. T2 - International Workshop on "Emerging Nanomaterials for Displays and SSL" CY - Dresden, Germany DA - 11.11.2021 KW - Nano KW - Nanomaterial KW - Nanocrystal KW - Semiconductor quantum dot KW - Lanthanide KW - Photoluminescence KW - Quantum yield KW - Photophysics KW - Lifetime KW - Surface chemistry KW - Brightness KW - NIR KW - SWIR KW - Method KW - Uncertainty KW - Rreference material PY - 2021 AN - OPUS4-53783 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Orell, S. T1 - Differential toxicities of particulate matter components linked to air pollution and adverse health effects N2 - There are significant differences in toxicity of PM components and cellular responses that can be linked to adverse health effects. Soot and copper oxide induced toxicity, reduced metabolic activity, increased ROS and altered immune response. Increased ROS generation and mitochondrial dysfunctions are well known features in COPD pathology. Toxicity of individual airborne particles can be used to better understand adverse health effects and improve air quality guidelines. T2 - ERS International Congress 2021 CY - Online meeting DA - 05.09.2021 KW - Particulate matter KW - Toxicity KW - Airborne particles KW - Air pollution KW - Inflammation KW - Epithelial cell PY - 2021 DO - https://doi.org/10.1183/13993003.congress-2021.PA3195 N1 - The abstract of the poster presentation was published in: European Respiratory Journal 2021; 58: Suppl. 65, PA3195. AN - OPUS4-53134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maack, Stefan T1 - Zerstörungsfreie Prüfung an Bestandsbrücken aus Beton - Fallbeispiele aus Nachrechnung und Ertüchtigung N2 - Präsentation der Ergebnisse von zerstörungsfreien Bauwerksprüfungen an Bestandsbrücken. Stand der Technik - Stand der Wissenschaft T2 - Koordinierungsausschuss Erhaltung (KoA-Erh 21/038) CY - Online meeting DA - 02.11.2021 KW - Zerstörungsfreie Prüfung KW - Messdaten KW - Brücken KW - Bildgebende Darstellung KW - Bauwesen KW - Qualitätssicherung PY - 2021 AN - OPUS4-53685 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Boyraz, B. A1 - Saatz, Jessica A1 - Pompös, I.-M. A1 - Gad, Michel A1 - Dernedde, J. A1 - Maier, A.-M. B. A1 - Moscovitz, O. A1 - Seeberger, P. H. A1 - Traub, Heike A1 - Tauber, R. T1 - Imaging Keratan Sulfate in Ocular Tissue Sections by Immunofluorescence Microscopy and LA-ICP-MS N2 - Carbohydrate-specific antibodies can serve as valuable tools to monitor alterations in the extracellular matrix resulting from pathologies. Here, the keratan sulfate-specific monoclonal antibody MZ15 was characterized in more detail by immunofluorescence microscopy as well as laser ablation ICP-MS using tissue cryosections and paraffin-embedded samples. Pretreatment with keratanase II prevented staining of samples and therefore demonstrated efficient enzymatic keratan sulfate degradation. Random fluorescent labeling and site-directed introduction of a metal cage into MZ15 were successful and allowed for a highly sensitive detection of the keratan sulfate landscape in the corneal stroma from rats and human tissue. KW - Laser ablation KW - Imaging KW - Glycosaminoglycan KW - ICP-MS KW - Immunohistochemistry KW - Immunofluorescence KW - Tissue PY - 2022 DO - https://doi.org/10.1021/acsabm.1c01240 VL - 5 IS - 2 SP - 853 EP - 861 PB - American Chemical Society CY - Washington AN - OPUS4-54341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meng, M. A1 - Zhang, T. A1 - Wang, J. A1 - Cheng, Z. A1 - Yang, J. A1 - Qiao, X. A1 - Wen, J. A1 - Resch-Genger, Ute A1 - Ou, J. T1 - Fluorescence temperature sensing of NaYF4:Yb3+/Tm3+@NaGdF4:Nd3+/Yb3+ nanoparticles at low and high temperatures N2 - NaYF4:Yb3+/Tm3+@NaGdF4:Nd3+/Yb3+ upconversion nanoparticles (UCNPs) were prepared using a solvothermal method, and the effects of key factors such as the content of sensitiser Nd 3+ and Yb3+ on their luminescence properties were investigated. The nanoparticles are homogeneous in size and well dispersed. Under 808 nm excitation, it can produce strong upconversion fluorescence. At the same time, the nanoparticles have good temperature-sensing properties at the thermally coupled energy levels of 700 nm and 646 nm for Tm3+. Using its fluorescence intensity ratio (FIR), accurate temperature measurements can be performed, and it has been found that it exhibits different temperature sensing properties in low and high-temperature regions. The maximum relative sensitivity was found to be 0.88% K-1 and 1.89% K-1 for the lowtemperature region of 285 K-345 K and the high-temperature region of 345 K-495 K. The nanoparticles were applied to the internal temperature measurement of lithium batteries and the actual high-temperature environment, respectively, and were found to have good temperature measurementt performance. KW - Fluorescence KW - Sensor KW - Temperature KW - Ratiometric KW - Lanthanide KW - Quantum yield KW - Integrating sphere spectroscopy KW - Absolute fluorescence KW - Quality assurance KW - Nano KW - Particle KW - Application KW - Upconversion nanoparticle PY - 2022 DO - https://doi.org/10.1088/1361-6528/ac84e4 SN - 1361-6528 VL - 33 IS - 34 SP - 1 EP - 15 PB - IOP Publishing CY - Bristol AN - OPUS4-55454 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - Quantification of the Total and Accessible Number of Functional Groups and Ligands on Nanomaterials N2 - Surface-functionalized organic and inorganic nanoparticles (NP) are of great interest in the life and material sciences, as they can be used e.g. as drug carriers, fluorescent sensors, and multimodal labels in bioanalytical assays and imaging applications. NP performance in such applications depends not only on particle size, size distribution, and morphology, but also on surface chemistry, i.e. the total number of surface functional groups (FG) and the number of FG accessible for subsequent functionalization with ligands or biomolecules, which in turn determines surface charge, colloidal stability, biocompatibility, and toxicity. Methods for FG quantification should be simple, robust, reliable, fast, and inexpensive, and allow for the characteriza-tion of a broad variety of nanomaterials differing in size, chemical composition, and optical properties. Aiming at the development of simple, versatile, and multimodal tools for the quantification of many bioanalytically relevant FG such as amine, carboxy, thiol and aldehyde functionalities, we investigated and compared various analytical methods commonly used for functional group quantification. This includes electrochemical titration methods, dye-based optical assays, and other instrumental analytical techniques such as nuclear magnetic resonance, mass spectrometry, and thermal analysis methods. T2 - Nanotech France CY - Paris, France DA - 15.06.2022 KW - Optical assays KW - Functionalized nano- and microparticles KW - Particle surface analysis KW - Surface group quantification KW - Terminal functional groups PY - 2022 AN - OPUS4-55208 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Traub, Heike T1 - Unraveling the interaction of MRI contrast agents with tissue using LA ICP MS N2 - Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is increasingly used to study the distribution of metal-containing drugs, imaging probes and nanomaterials in connection with disease related changes and therapy progress. Additionally, biomolecules can be detected indirectly by using metal-tagged antibodies. The extracellular matrix (ECM) is, besides the cells, an important component of all body tissues. The macromolecular network of the ECM consists of structural proteins (e.g., collagen, elastin) and proteoglycans composed of highly negatively charged carbohydrates, the glycosaminoglycans (GAGs), which are covalently linked to a protein core. Many diseases, including inflammatory processes and tumors, are associated with characteristic ECM changes at an early stage. Recent studies have shown that contrast agents for magnetic resonance imaging (MRI), which are based on gadolinium containing chelate complexes or iron oxide nanoparticles, can bind themselves to ECM components. To elucidate the role of GAGs like keratan sulfate (KS) and its modification state in disease, highly specific tools are necessary. As a complement to conventional immunohistochemistry LA-ICP-MS was applied to investigate the distribution of KS in tissue thin sections using a well characterized anti-KS antibody labelled with metal ions. Furthermore, LA-ICP-MS was used for the detection of MRI contrast agents and the identification of their target cells and molecules in tissue samples from animal models, e.g. for cardiovascular diseases. The results show the possibilities of LA-ICP-MS for the elucidation of pathological tissue changes. T2 - European Workshop on Laser Ablation (EWLA 2022) CY - Berne, Switzerland DA - 12.07.2022 KW - Laser ablation KW - Imaging KW - ICP-MS KW - Antibody PY - 2022 AN - OPUS4-55315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Tavernaro, Isabella A1 - Abram, Sarah-Luise A1 - Andresen, Elina A1 - Matiushkina, Anna T1 - Quantifying the number of total and accessible functional groups on nanomaterials N2 - Inorganic and organic functional nanomaterials (NM) of different size, shape, chemical composition, and surface chemistry are relevant for many key technologies of the 21st century. Decisive for most applications of NM are their specific surface properties, which are largely controlled by the chemical nature and number of ligands and functional groups (FG on the NM surface. The surface chemistry can strongly affect the physicochemical properties of NM, their charge, hydrophilicity/hydrophobicity, reactivity, stability, and processability and thereby their impact on the environment and biological species as well as their possible risk for human health. Thus, reliable, validated, and eventually standardized analytical methods for the characterization of NM surface chemistry, i.e., the chemical identification, quantification, and accessibility of FG and surface ligands 1,2] flanked by interlaboratory comparisons, control samples, and reference materials, 2 ,3 are of considerable importance for process and quality control of NM production and function. This is also important for the safe use of NM the design of novel NM, and sustainable concepts for NM fabrication. Here, we provide an overview of analytical methods for FG analysis and quantification and highlight method and material related challenges for selected NM. Analytical techniques address ed include electrochemical titration methods, optical assays, nuclear magnetic resonance (NMR) and vibrational (IR) spectroscopy, and X ray based and thermal analysis methods. Criteria for method classification and evaluation include the need for a signal generating label, provision of either the total or derivatizable number of FG, and suitability for process and production control. T2 - AUC - Analytical Ultracentrifugation CY - Nuremberg, Germany DA - 22.07.2024 KW - Nanoparticle KW - Particle KW - Microparticle KW - Silica KW - Quantum dot KW - Polymer KW - Surface group KW - Luminescence KW - Quality assurance KW - Synthesis KW - Surface modification KW - ILC KW - Optical assay KW - Functional group KW - Ligand KW - qNMR KW - Conductometry KW - Potentiometry KW - Standardization KW - Reference product KW - Reference material PY - 2024 AN - OPUS4-60749 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - A journey in science from a graduate student in physical chemistry to head of division biophotonics N2 - I will provide a personal overview of the most important steps of my career in science, a journey from a graduate student in physical chemistry in an environment dominated by male-scientists over a postdoc with a female professor in the US to the leader of a research group, head of division Biophotonics at BAM. This will include my choices of research topics, how I learnt to write well cited publications, even on topics such as reference materials and quality assurance,1-4 and eventually started to give lectures at Free University Berlin granting me the right to act as first supervisor of undergraduate and graduate students. T2 - Women in Science CY - Erlangen, Germany DA - 22.07.2024 KW - Lanthanide KW - Nanoparticle KW - Silica KW - Quantum dot KW - Polymer KW - Surface group KW - Luminescence KW - Quantitative spectroscopy KW - Quantum yield KW - Lifetime KW - Quality assurance KW - Synthesis KW - Surface modification KW - Photophysics PY - 2024 AN - OPUS4-60724 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wegner, Karl David A1 - Walter, J. T1 - Size-resolved emission properties of core/shell CdSe/CdS quantum dots via multiwavelength emission analytical ultracentrifugation N2 - Colloids provide manifold opportunities for targeted product design due to their tunable properties with respect to size, shape, composition, surface, and spectral characteristics. However, the determination of structure-property relationships is quite challenging as most particulate samples exhibit polydispersity of their disperse properties. Analytical ultracentrifugation (AUC) is a fractionating technique and highly accurate method for the multidimensional analysis of nanoparticles as it permits the differentiation of spectral information linked to hydro- and thermodynamic properties of the particles. So far, characterization capabilities for fluorescent nanoparticles by AUC were limited, as the formerly commercially available fluorescence detector could not provide any spectral information. Using a multiwavelength emission detector developed in our group, it is possible to extract spectra of fluorescent particles and biomolecules alongside their sedimentation and diffusion coefficients within a single centrifugation experiment. In our contribution, we will highlight that even narrowly distributed core/shell CdSe/CdS quantum dots still show size- and structure-dependent shifts of their fluorescence spectra, which can be resolved with our AUC system in an ensemble measurement. Thereby, we can link spectral changes of only a few nanometers to particle sizes retrieved with Angstrom size resolution. Single-particle measurements not only supported the results obtained with the AUC system but also provided deeper insights into the photophysical processes of individual QDs, clearly demonstrating the complementary nature of the techniques used. With our novel multiwavelength emission detector and the established extinction-based detector for AUC, a comprehensive platform for the holistic characterization of fluorescent colloids is now available. T2 - 26th International Analytical Ultracentrifugation Symposium CY - Bad Staffelstein, Germany DA - 24.07.2024 KW - Quantum dots KW - Analytical ultracentrifugation KW - Reference materials KW - Calibrated fluorescence measurements KW - Size-resolved emission PY - 2024 AN - OPUS4-60814 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Descalzo, Ana B. A1 - Ashokkumar, Pichandi A1 - Shen, Z. A1 - Rurack, Knut T1 - On the Aggregation Behaviour and Spectroscopic Properties of Alkylated and Annelated BoronDipyrromethene (BODIPY) Dyes in Aqueous Solution N2 - The tendency of boron-dipyrromethene (BODIPY) dyes to associate in water is well known, and usually a cause for inferior fluorescence properties. Synthetic efforts to chemically improve BODIPYs’ water solubility and minimize this problem have been numerous in the past. However, a deeper understanding of the phenomena responsible for fluorescence quenching is still required. Commonly, the spectroscopic behaviour in aqueous media has been attributed to aggregate or excimer formation, with such works often centring on a single BODIPY family. Herein, we provide an integrating discussion including very diverse types of BODIPY dyes. Our studies revealed that even subtle structural changes can distinctly affect the association behaviour of the fluorophores in water, involving different photophysical processes. The palette of behaviour found ranges from unperturbed emission, to the formation of H or J aggregates and excimers, to the involvement of tightly bound, preformed excimers. These results are a first step to a more generalized understanding of spectroscopic properties vs. structure, facilitating future molecular design of BODIPYs, especially as probes for biological applications. KW - Aggregates KW - BODIPY KW - Excimers KW - Fluorescence KW - Photophysics PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-497771 DO - https://doi.org/10.1002/cptc.201900235 SN - 2367-0932 VL - 4 IS - 2 SP - 120 EP - 131 PB - WILEY-VCH CY - Weinheim AN - OPUS4-49777 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krahl, T. A1 - Beer, F. A1 - Relling, A. A1 - Gawlitza, Kornelia A1 - Rurack, Knut A1 - Kemnitz, E. T1 - Toward Luminescent Composites by Phase Transfer of SrF2 :Eu3+ Nanoparticles Capped with Hydrophobic Antenna Ligands N2 - Transparent dispersions of hydrophobic SrF2 :Eu3+ nanoparticles in cyclohexane with up to 20% europium were obtained by fluorolytic sol-gel synthesis followed by Phase transfer into cyclohexane through capping with sodium dodecylbenzenesulfonate (SDBS). The particles were characterized by TEM, XRD and DLS as spherical objects with a diameter between 6 and 11 nm in dry state. 1H-13CP MAS NMR experiments revealed the binding of the anionic sulfonate head group to the particle surface. The particles show bright red luminescence upon excitation of the aromatic capping agents, acting as antennas for an Energy transfer from the benzenesulfonate unit to the Eu3+ centers in the particles. This synthesis method overcomes the current obstacle of the fluorolytic sol-gel synthesis that transparent dispersions can be obtained directly only in hydrophilic solvents. To demonstrate the potential of such hydrophobized alkaline-earth fluoride particles, transparent luminescent organic-inorganic composites with 10% SrF2 :Eu3+ embedded into polyTEGDMA, polyBMA, poly-BDDMA and polyD3MA, respectively, were prepared, endowing the polymers with the luminescence features of the nanoparticles. KW - Nanoparticles KW - Fluorides KW - Sol-gel process KW - Organic-inorganic hybrid composites PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508668 DO - https://doi.org/10.1002/cnma.202000058 SP - 1 EP - 11 PB - Wiley AN - OPUS4-50866 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sebald, M.A. A1 - Gebauer, J. A1 - Sommerfeld, Thomas A1 - Koch, Matthias T1 - First Synthesis of (−)-Altenuene-D3 Suitable as Internal Standard for Isotope Dilution Mass Spectrometry N2 - Metabolites from Alternaria fungi exhibit a variety of biological properties such as phytotoxic, cytotoxic, or antimicrobial activity. Optimization of a literature procedure culminated in an efficient total synthesis of (−)-altenuene as well as a stable isotope-labeled derivative suitable for implementation in a LC-MS/MS method for mycotoxin analysis. KW - Altenuene KW - Alternaria mycotoxins KW - Food safety KW - Isotope-labeled KW - SIDA-LC-MS/MS KW - Suzuki coupling PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-500696 DO - https://doi.org/10.3390/molecules24244563 SN - 1420-3049 VL - 24 SP - 4563 PB - MDPI CY - Basel AN - OPUS4-50069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Borzekowski, Antje A1 - Anggriawan, R. A1 - Auliyati, M. A1 - Kunte, Hans-Jörg A1 - Koch, Matthias A1 - Rohn, S. A1 - Karlovsky, P. A1 - Maul, Ronald T1 - Formation of Zearalenone Metabolites in Tempeh Fermentation N2 - Tempeh is a common food in Indonesia, produced by fungal fermentation of soybeans using Rhizopus sp., as well as Aspergillus oryzae, for inoculation. Analogously, for economic reasons, mixtures of maize and soybeans are used for the production of so-called tempeh-like products. For maize, a contamination with the mycoestrogen zearalenone (ZEN) has been frequently reported. ZEN is a mycotoxin which is known to be metabolized by Rhizopus and Aspergillus species. Consequently, this study focused on the ZEN transformation during tempeh fermentation. Five fungal strains of the genera Rhizopus and Aspergillus, isolated from fresh Indonesian tempeh and authentic Indonesian inocula, were utilized for tempeh manufacturing from a maize/soybean mixture (30:70) at laboratory-scale. Furthermore, comparable tempeh-like products obtained from Indonesian markets were analyzed. Results from the HPLC-MS/MS analyses show that ZEN is intensely transformed into its metabolites alpha-zearalenol (alpha-ZEL), ZEN-14-sulfate, alpha-ZEL-sulfate, ZEN-14-glucoside, and ZEN-16-glucoside in tempeh production. alpha-ZEL, being significantly more toxic than ZEN, was the main metabolite in most of the Rhizopus incubations, while in Aspergillus oryzae fermentations ZEN-14-sulfate was predominantly formed. Additionally, two of the 14 authentic samples were contaminated with ZEN, alpha-ZEL and ZEN-14-sulfate, and in two further samples, ZEN and alpha-ZEL, were determined. Consequently, tempeh fermentation of ZEN-contaminated maize/soybean mixture may lead to toxification of the food item by formation of the reductive ZEN metabolite, alpha-ZEL, under model as well as authentic conditions. KW - Modified mycotoxins KW - Zearalenone sulfate KW - a-zearalenol KW - Food fermentation KW - Rhizopus and Aspergillus oryzae PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-491126 DO - https://doi.org/10.3390/molecules24152697 VL - 24 IS - 15 SP - 2697 PB - MDPI AN - OPUS4-49112 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kotthoff, Lisa A1 - Lisec, Jan A1 - Schwerdtle, T. A1 - Koch, Matthias T1 - Prediction of transformation products of monensin by electrochemistry compared to microsomal assay and hydrolysis N2 - The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for animal health, food, and environmental matters. The active agent Monensin (MON) belongs to the ionophore antibiotics and is widely used as a veterinary drug against coccidiosis in broiler farming. However, no electrochemically (EC) generated TPs of MON have been described so far. In this study, the online coupling of EC and mass spectrometry (MS) was used for the generation of oxidative TPs. EC-conditions were optimized with respect to working electrode material, solvent, modifier, and potential polarity. Subsequent LC/HRMS (liquid chromatography/high resolution mass spectrometry) and MS/MS experiments were performed to identify the structures of derived TPs by a suspected target analysis. The obtained EC-results were compared to TPs observed in metabolism tests with microsomes and hydrolysis experiments of MON. Five previously undescribed TPs of MON were identified in our EC/MS based study and one TP, which was already known from literature and found by a microsomal assay, could be confirmed. Two and three further TPs were found as products in microsomal tests and following hydrolysis, respectively. We found decarboxylation, O-demethylation and acid-catalyzed ring-opening reactions to be the major mechanisms of MON transformation. KW - Transformation products KW - Monensin KW - Veterinary drugs KW - Electrochemistry KW - Hydrolysis KW - LC/HRMS PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-485689 DO - https://doi.org/10.3390/molecules24152732 SN - 1420-3049 VL - 24 IS - 15 SP - 2732, 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-48568 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tjaden, B. A1 - Lisec, Jan A1 - Schramm, A. T1 - N-Myc-induced metabolic rewiring creates novel therapeutic vulnerabilities in neuroblastoma N2 - N-Myc is a transcription factor that is aberrantly expressed in many tumor types and is often correlated with poor patient prognosis. Recently, several lines of evidence pointed to the fact that oncogenic activation of Myc family proteins is concomitant with reprogramming of tumor cells to cope with an enhanced need for metabolites during cell growth. These adaptions are driven by the ability of Myc proteins to act as transcriptional amplifiers in a tissue-of-origin specific manner. Here, we describe the effects of N-Myc overexpression on metabolic reprogramming in neuroblastoma cells. Ectopic expression of N-Myc induced a glycolytic switch that was concomitant with enhanced sensitivity towards 2-deoxyglucose, an inhibitor of glycolysis. Moreover, global metabolic profiling revealed extensive alterations in the cellular metabolome resulting from overexpression of N-Myc. Limited supply with either of the two main carbon sources, glucose or glutamine, resulted in distinct shifts in steady-state metabolite levels and significant changes in glutathione metabolism. Interestingly, interference with glutamine-glutamate conversion preferentially blocked proliferation of N-Myc overexpressing cells, when glutamine levels were reduced. Thus, our study uncovered N-Myc induction and nutrient levels as important metabolic master switches in neuroblastoma cells and identified critical nodes that restrict tumor cell proliferation. KW - Mass-Spectrometry KW - Cancer KW - MYCN PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507193 DO - https://doi.org/10.1038/s41598-020-64040-1 VL - 10 IS - 1 SP - 7157 AN - OPUS4-50719 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bartelmeß, Jürgen A1 - Valderrey, Virginia A1 - Rurack, Knut T1 - Development of a “Turn-on” Fluorescent Probe-Based Sensing System for Hydrogen Sulfide in Liquid and Gas Phase N2 - A “turn-on” fluorescence sensing system based on a BODIPY-cobaloxime complex for the detection of H2S in liquid and gas phase was developed. To that aim, two cobaloxime complexes bearing an axial pyridyl-BODIPY ligand were initially evaluated as sensitive fluorescent HS− indicators in aqueous solution. The sensing mechanism involves the selective substitution of the BODIPY ligand by the HS− anion at the cobalt center, which is accompanied by a strong fluorescence enhancement. The selection of a complex with an ideal stability and reactivity profile toward HS− relied on the optimal interaction between the cobalt metal-center and two different pyridyl BODIPY ligands. Loading the best performing BODIPY-cobaloxime complex onto a polymeric hydrogel membrane allowed us to study the selectivity of the probe for HS− against different anions and cysteine. Successful detection of H2S by the fluorescent “light-up” membrane was not only accomplished for surface water but could also be demonstrated for relevant H2S concentrations in gas phase. KW - Sulfide sensing KW - Fluorescence KW - BODIPYs KW - Cobaloxime complex KW - Gas sensing PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-492186 DO - https://doi.org/10.3389/fchem.2019.00641 SN - 2296-2646 VL - 7 SP - Art. Nr. 641 PB - Frontiers Media CY - Lausanne AN - OPUS4-49218 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Scholl, Juliane A1 - Bagheri, Abbas A1 - Meiers, Emelie A1 - Lisec, Jan A1 - Russo, Francesco A1 - Haase, Hajo A1 - Koch, Matthias T1 - Unveiling Aging Mechanisms of Electrolytes in Commercial End-of-Life Lithium-Ion Batteries N2 - In this study, 77 end-of-life (EOL) commercial lithium-ion batteries (LIBs) of different formats were systematically analyzed to investigate electrolyte degradation mechanisms and the influence of pristine electrolyte composition on aging. Comprehensive chemical characterization employed targeted and non-targeted mass spectrometry (MS), combining liquid and gas chromatography (LC-MS/MS, GC-MS) with high-resolution MS (HRMS). This approach identified confirmed pristine components and complex degradation products. Commercial rechargeable pouch and cylindrical cells often deviated from conventional research model systems, using mixed lithium salt anions, ionic liquids (ILs), and high concentrations of triflates, triflimides, and bis(fluorosulfonyl)imide (FSI), functioning as solvents, salts, or additives. Specific IL degradation products and previously unreported pathways were proposed. A novel series of oligomerization products from propylene carbonate (PC) was also identified. In contrast, non-rechargeable coin cells showed prevalent use of per- and polyfluoroalkyl substances (PFAS) in their original electrolytes. Distinct PFAS degradation mechanisms were proposed for the first time. The absence of carbonate oligomers and lithium salt-derived products in coin cells, alongside standard carbonates, suggests lithium counterion coordination critically influences Lewis acid-catalyzed degradation. These findings provide new insight into real-world LIB aging, highlighting differences between commercial devices and model systems. KW - Mass Spectrometry KW - PFAS KW - Electrolyte degradation KW - Transformation products KW - Battery aging PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-641059 DO - https://doi.org/10.2139/ssrn.5395937 SP - 1 EP - 15 PB - Elsevier BV AN - OPUS4-64105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Junge, Florian A1 - Wittwer, Philipp A1 - Sommerfeld, Thomas A1 - Gehrenkemper, Lennart A1 - Zoister, Christian A1 - Nickl, Philip A1 - Koch, Matthias A1 - Meermann, Björn A1 - Haag, Rainer T1 - Adsorber Charge Dominates over Hydrophobic or Fluorophilic Functionalization in Influencing Adsorption of PFCA onto Polystyrene Resins N2 - A systematic series of industrial-relevant polystyrene-based anion exchange resins that are functionalized with hydro- or fluorocarbon chains are compared regarding their adsorption behavior toward perfluorocarboxylic acids (PFCA) in respect to their charge, chain length, and type of chain. The results clearly show the dominance of electrostatic interactions in the adsorption process as uncharged adsorber materials showed no adsorption at all. In contrast, the charged adsorber materials showed in general a PFCA removal of 80% to 30% over the experiment depending on effluent fraction. Unexpectedly, for perfluorobutanoic acid (PFBA) the highest removal rate is found with consistently >90%. Despite observing significant benefits in the adsorption of PFCA for fluoroalkylated adsorbers in comparison to their non-fluorinated counterparts, this effect of fluoroalkylation is comparatively small and can not be clearly attributed to fluorophilic interactions between the fluoroalkyl chains. These findings help clarifying that the introduction of fluorocarbon moieties in adsorber materials is not necessary in order to remove fluorocarbon molecules from the environment. KW - PFAS KW - Remediation KW - Adsorption KW - Fluorophilic interactions PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-601883 DO - https://doi.org/10.1002/admi.202400199 SN - 2196-7350 SP - 1 EP - 10 PB - John Wiley & Sons CY - Hoboken, New Jersey, USA AN - OPUS4-60188 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Biyikal, Mustafa A1 - Gröninger, Delia A1 - Weller, Michael G. A1 - Martínez Mánez, R. A1 - Rurack, Knut ED - Climent Terol, Estela T1 - Multiplexed Detection of Analytes on Single Test Strips with Antibody-Gated Indicator-Releasing Mesoporous Nanoparticles N2 - Rapid testing methods for the use directly at apointof need are expected to unfold their true potential especiallywhen offering adequate capabilities for the simultaneousmeasurement of multiple analytes of interest. Considering theunique modularity,high sensitivity,and selectivity of antibody-gated indicator delivery (gAID) systems,amultiplexed assayfor three small-molecule explosives (TATP, TNT,PETN) wasthus developed, allowing to detect the analytes simultaneouslywith asingle test strip at lower ppb concentrations in the liquidphase in < 5min using afluorescence reader or asmartphonefor readout. While the TNT and PETN systems were newlydeveloped here,all the three systems also tolerated harshermatrices than buffered aqueous model solutions.Besidesasingle-track strip,the outstanding modularity of the hybridbiosensor materials in combination with strip-patterningtechnologies allowed us to obtain amultichannel strip inastraightforwardmanner,offering comparable analyticalperformance while allowing to be tailored even more to theusersneed. KW - Multiplexing KW - Explosives detection KW - Gated materials KW - Fluorescence PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-518424 DO - https://doi.org/10.1002/anie.202009000 SN - 1433-7851 SN - 1521-3773 VL - 59 IS - 52 SP - 23862 EP - 23869 PB - Wiley-VCH CY - Weinheim AN - OPUS4-51842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pisonero, J. A1 - Bouzas-Ramos, D. A1 - Traub, Heike A1 - Cappella, Brunero A1 - Alvarez-Llamas, C. A1 - Richter, Silke A1 - Mayo, J. C. A1 - Costa-Fernandez, J. M. A1 - Bordel, N. A1 - Jakubowski, Norbert T1 - Critical evaluation of fast and highly resolved elemental distribution in single cells using LA-ICP-SFMS N2 - The analytical potential of a nanosecond laser ablation inductively coupled plasma mass spectrometer (ns-LA-ICP-SFMS) system, equipped with an ultra-fast wash-out ablation chamber, is critically investigated for fast and highly spatially resolved (∼μm) qualitative elemental distribution within single cells. Initially, a low surface roughness (< 10 nm) thin In–SnO2 layer (total coating thickness ∼200 nm) deposited on glass is employed to investigate the size, morphology and overlapping of laser-induced craters obtained at different laser repetition rates, making use of Atomic Force Microscopy (AFM). Conical craters with a surface diameter of about 2 µm and depths of about 100 nm were measured after a single laser shot. Furthermore, the influence of the sampling distance (i.e. distance between the sample surface and the inner sniffer of the ablation chamber) on the LA-ICP-MS ion signal wash-out time is evaluated. A significant decrease of the transient 120Sn+ ion signal is noticed after slight variations (±200 μm) around the optimum sampling position. Ultra-fast wash-outs (< 10 ms) are achieved reducing the aerosol mixing from consecutive laser shots even when operating the laser at high repetition rates (25 – 100 Hz). Fast and highly spatially resolved images of elemental distribution within mouse embryonic fibroblast cells (NIH/3T3 fibroblast cells) and human cervical carcinoma cells (HeLa cells), incubated with gold nanoparticles (Au NPs) and Cd-based quantum dots (QDs), respectively, are determined at the optimized operating conditions. Elemental distribution of Au and Cd in single cells is achieved using a high scanning speed (50 µm/s) and high repetition rate (100 Hz). The results obtained for the distribution of fluorescent Cd-based QDs within the HeLa cells are in good agreement with those obtained by confocal microscopy. The size, morphology and overlapping of laser-induced craters in the fixed cells are also investigated using AFM, observing conical craters with a surface diameter of about 2.5 µm and depths of about 800 nm after a single laser shot. KW - Laser ablation KW - ICP-MS KW - Nanoparticle KW - Atomic Force Microscopy KW - Cell PY - 2018 DO - https://doi.org/10.1039/c8ja00096d SP - 1 EP - 9 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-45564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Hecht, Mandy A1 - Witthuhn, Heike A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Mix‐&‐read determination of Mercury(II) at trace levels with hybrid mesoporous silica materials incorporating fluorescent probes by a simple mix‐&‐load technique N2 - The synthesis, characterization, and application of mesoporous materials containing boron–dipyrromethene (BODIPY) moieties that allow the sensitive and selective detection of HgII in aqueous environments by fluorescence enhancement is reported. For this purpose, BODIPY dye I containing a thia‐aza crown ether receptor as the fluorescent probe for the detection of HgII in aqueous environments is encapsulated into mesoporous materials to avoid self‐quenching or aggregation in water. Determination of HgII is accomplished within a few seconds with high selectivity and sensitivity, reaching a limit of detection of 12 ppt. The determination of trace amounts of HgII in natural waters and in fish extracts is demonstrated by using our sensing material. The incorporation of the material into several μ‐PAD strips yields a portable, cheap, quick, and easy‐to‐handle tool for trace HgII analysis in water. KW - Dyes/pigments KW - Test strips KW - Mesoporous materials KW - Mercury KW - Fluorescence PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-460138 DO - https://doi.org/10.1002/open.201800277 SN - 2191-1363 VL - 7 IS - 12 SP - 957 EP - 968 PB - Wiley-VCH CY - Weinheim AN - OPUS4-46013 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Borzekowski, Antje A1 - Drewitz, T. A1 - Keller, Julia A1 - Pfeifer, Dietmar A1 - Kunte, Hans-Jörg A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, R. T1 - Biosynthesis and characterization of zearalenone-14-sulfate, zearalenone-14-glucoside and zearalenone-16-glucoside using common fungal strains N2 - Zearalenone (ZEN) and its phase II sulfate and glucoside metabolites have been detected in food and feed commodities. After consumption, the conjugates can be hydrolyzed by the human intestinal microbiota leading to liberation of ZEN that implies an underestimation of the true ZEN exposure. To include ZEN conjugates in routine analysis, reliable standards are needed, which are currently not available. Thus, the aim of the present study was to develop a facilitated biosynthesis of ZEN-14-sulfate, ZEN-14-glucoside and ZEN-16-glucoside. A metabolite screening was conducted by adding ZEN to liquid fungi cultures of known ZEN conjugating Aspergillus and Rhizopus strains. Cultivation conditions and ZEN incubation time were varied. All media samples were analyzed for metabolite formation by HPLC-MS/MS. In addition, a consecutive biosynthesis was developed by using Fusarium graminearum for ZEN biosynthesis with subsequent conjugation of the toxin by utilizing Aspergillus and Rhizopus species. ZEN-14-sulfate (yield: 49%) is exclusively formed by Aspergillus oryzae. ZEN-14-glucoside (yield: 67%) and ZEN-16-glucoside (yield: 39%) are formed by Rhizopus oryzae and Rhizopus oligosporus, respectively. Purities of ≥73% ZEN-14-sulfate, ≥82% ZEN-14-glucoside and ≥50% ZEN-16-glucoside were obtained by 1H-NMR. In total, under optimized cultivation conditions, fungi can be easily utilized for a targeted and regioselective synthesis of ZEN conjugates. KW - Mycotoxin KW - Zearalenone KW - Conjugate KW - Biosynthesis KW - Fusarium KW - Aspergillus KW - Rhizopus PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444246 DO - https://doi.org/10.3390/toxins10030104 SN - 2072-6651 VL - 10 IS - 3 SP - Article 104, 1 EP - 15 PB - MDPI CY - Basel AN - OPUS4-44424 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Alnajjar, M. A. A1 - Bartelmeß, Jürgen A1 - Hein, R. A1 - Ashokkumar, Pichandi A1 - Nilam, M. A1 - Nau, W. M. A1 - Rurack, Knut A1 - Hennig, A. T1 - Rational design of boron-dipyrromethene (BODIPY) reporter dyes for cucurbit[7]uril N2 - We introduce herein boron-dipyrromethene (BODIPY) dyes as a new class of fluorophores for the design of reporter dyes for supramolecular host–guest complex formation with cucurbit[7]uril (CB7). The BODIPYs contain a protonatable aniline nitrogen in the meso-position of the BODIPY chromophore, which was functionalized with known binding motifs for CB7. The unprotonated dyes show low fluorescence due to photoinduced electron transfer (PET), whereas the protonated dyes are highly fluorescent. Encapsulation of the binding motif inside CB7 positions the aniline nitrogen at the carbonyl rim of CB7, which affects the pKa value, and leads to a host-induced protonation and thus to a fluorescence increase. The possibility to tune binding affinities and pKa values is demonstrated and it is shown that, in combination with the beneficial photophysical properties of BODIPYs, several new applications of host–dye reporter pairs can be implemented. This includes indicator displacement assays with favourable absorption and emission wavelengths in the visible spectral region, fluorescence correlation spectroscopy, and noncovalent surface functionalization with fluorophores. KW - BODIPY KW - Cucurbituril KW - Fluorescence KW - PH KW - Photoinduced Electron Transfer KW - Supramolecular Chemistry PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-456361 UR - https://www.beilstein-journals.org/bjoc/content/pdf/1860-5397-14-171.pdf DO - https://doi.org/10.3762/bjoc.14.171 SN - 1860-5397 VL - 14 SP - 1961 EP - 1971 PB - Beilstein-Institut CY - Frankfurt a. M. AN - OPUS4-45636 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gotor, Raul A1 - Ashokkumar, Pichandi A1 - Hecht, Mandy A1 - Keil, Karin A1 - Rurack, Knut T1 - Optical pH Sensor Covering the Range from pH 0−14 Compatible with Mobile-Device Readout and Based on a Set of Rationally Designed Indicator Dyes N2 - In this work, a family of pH-responsive fluorescent probes has been designed in a rational manner with the aid of quantum chemistry tools, covering the entire pH range from 0−14. Relying on the boron−dipyrromethene (BODIPY) core, all the probes as well as selected reference dyes display very similar spectroscopic properties with ON−OFF fluorescence switching responses, facilitating optical readout in simple devices used for detection and analysis. Embedding of the probes and reference dyes into hydrogel spots on a plastic strip yielded a test strip that reversibly indicates pH with a considerably small uncertainty of ~0.1 pH units. These strips are not only reusable but, combined with a 3D-printed case that can be attached to a smartphone, the USB port of which drives the integrated LED used for excitation, allows for autonomous operation in on-site or in-the-field applications; the developed Android application software (“app”) further simplifies operation for unskilled users. KW - Fluorescence KW - pH measurement KW - BODIPY KW - Smartphone KW - Test strip PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-422571 DO - https://doi.org/10.1021/acs.analchem.7b01903 SN - 0003-2700 SN - 1520-6882 VL - 89 IS - 16 SP - 8437 EP - 8444 PB - American Chemical Society CY - Washington, D.C., USA AN - OPUS4-42257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schloß, S. A1 - Hackl, T. A1 - Herz, C. A1 - Lamy, E. A1 - Koch, Matthias A1 - Rohn, S. A1 - Maul, R. T1 - Detection of a Toxic Methylated Derivative of Phomopsin A Produced by the Legume-Infesting Fungus Dioporthe toxica N2 - Phomopsin A (PHO-A), produced by the fungus Diaporthe toxica, is a mycotoxin known to be responsible for fatal liver disease of lupin-fed sheep. The füll spectrum of the toxic secondary metabolites produced by D. toxica is still unknown. PHO-A and the naturally occurring derivatives B—E have been subject to several studies to reveal their structures as well as chemical and toxicological properties. In this work, a methylated derivative of PHO-Aisolated firom lupin seeds inoculated %vith D. toxica is described. It was characterized by high-resolution mass and NMR data and shown to be the N-methylated derivative of PHO-A 1 is cytotoxic againstHepG2 cells. KW - Mycotoxins KW - Identification KW - Food PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-411167 DO - https://doi.org/10.1021/acs.jnatprod.6b00662 VL - 80 IS - 6 SP - 1930 EP - 1934 PB - ACS Publications AN - OPUS4-41116 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bell, Jérémy A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Die 3D-Mikrofluidik mit molekular geprägten Polymerpartikeln eröffnet neue Möglichkeiten der selektiven Pestizid-Bestimmung in Wasser N2 - 2,4-D ist ein in der Landwirtschaft weitverbreitetes Pflanzenschutzmittel, das Grundwasser kontaminiert, sich innerhalb der Nahrungskette anreichert und Umwelt- und Gesundheitsprobleme verursachen kann. Hier stellen die Autoren ein mikrofluidisches Nachweissystem für die Echtzeitdetektion von 2,4-D in Grund- oder Oberflächenwasser vor. Es basiert auf der Kombination 2,4-D-selektiver, fluoreszierender, molekular geprägter Polymer-(MIP-)Mikropartikel mit einem 3D-mikrofluidischen Extraktions- und Detektionssystem. Messungen vor Ort sollen damit künftig möglich sein. KW - 3D-Mikrofluidik KW - Sensorpartikel KW - MIP KW - Pestizid PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-444781 UR - https://www.labo.de/epaper/LA0318/index.html SN - 0344-5208 IS - 3 SP - 10 EP - 13 PB - WEKA Business Medien GmbH AN - OPUS4-44478 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bell, Jérémy A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Mit Tröpfchen Spielen N2 - Mikrofluidische Systeme sind leistungsstarke analytische Tools mit attraktiven Eigenschaften wie miniaturisierter Größe, geringem Reagenzien und Probenverbrauch, schneller Ansprech- und kurzer Messzeit. Der Bedarf solcher leistungsstarken, miniaturisierten und direkt vor Ort anwendbaren Sensorsysteme steigt kontinuierlich, hauptsächlich durch das Bedürfnis der Gesellschaft, schneller, besser und umfassender über kritische Faktoren im Lebens- und Arbeitsumfeld sowie der Umwelt informiert zu sein. KW - Mikrofluidik KW - Sensorpartikel PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-459120 UR - https://www.git-labor.de/forschung/umwelt/mit-troepfchen-spielen VL - 8 IS - 8 SP - 2 EP - 4 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim, Deutschland AN - OPUS4-45912 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bell, Jérémy A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Playing with Droplets N2 - Microfluidic devices are powerful analytical tools with appealing features such as miniaturized size, low reagent and sample consumption, rapid response and short measurement times. As society wants to be ever better, earlier and more comprehensively informed about critical factors in life, work, and the environment, the demand for powerful measurement devices for use outside of the laboratory constantly increases. KW - Microfluidics KW - Sensory particles PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-459131 UR - https://www.laboratory-journal.com/ VL - 4 SP - 2 EP - 4 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim, Deutschland AN - OPUS4-45913 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sarma, Dominik A1 - Carl, Peter A1 - Climent Terol, Estela A1 - Schneider, Rudolf A1 - Rurack, Knut T1 - Multifunctional polystyrene core/silica shell microparticles with antifouling properties for bead-based multiplexed and quantitative analysis N2 - Commercial bead-based assays are commonly built upon polystyrene particles. The polymeric carrier can be encoded with organic dyes and has ideal material properties for cytometric applications such as low density and high refractive index. However, functional groups are conventionally integrated during polymerization and subsequent modification is limited to the reactivity of those groups. Additionally, polystyrene as the core material leads to many hydrophobic areas still being present on the beads’ surfaces even after functionalization, Rendering the particles prone to nonspecific adsorption during an application. The latter calls for several washing steps and the use of additives in (bio)analytical assays. In this contribution, we show how these limitations can be overcome by using monodisperse polystyrene (PS) core/silica (SiO2) shell particles (SiO2@PS). Two different hydrophobic BODIPY (boron−dipyrromethene) dyes were encapsulated inside a poly(vinylpyrrolidone) (PVP) -stabilized polystyrene core in different concentrations to create 5-plex arrays in two separate detection channels of a cytometer. A subsequent modification of the silica shell with an equimolar APTES/PEGS (aminopropyltriethoxysilane/polyethylene glycol silane) blend added multifunctional properties to the hybrid core/Shell microparticles in a single step: APTES provides amino groups for the attachment of a caffeine derivative (as a hapten) to create antigen-coupled microspheres; the PEG moiety effectively suppresses nonspecific binding of antibodies, endowing the surface with antifouling properties. The particles were applied in a competitive fluorescence immunoassay in suspension, and a highly selective wash-free assay for the detection of caffeine in beverages was developed as a proof of concept. KW - Core−shell particles KW - Bead-based assay KW - Multiplex KW - Antifouling surface KW - Mixed surface PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-472931 UR - https://pubs.acs.org/doi/10.1021/acsami.8b10306 DO - https://doi.org/10.1021/acsami.8b10306 SN - 1944-8244 VL - 11 IS - 1 SP - 1321 EP - 1334 PB - American Chemical Society CY - Online Library AN - OPUS4-47293 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ghasem Zadeh Khorasani, Media A1 - Elert, Anna Maria A1 - Hodoroaba, Vasile-Dan A1 - Agudo Jácome, Leonardo A1 - Altmann, Korinna A1 - Silbernagl, Dorothee A1 - Sturm, Heinz T1 - Short- and long-range mechanical and chemical interphases caused by interaction of Boehmite (γ-AlOOH) with anhydride-cured epoxy resins N2 - Understanding the interaction between boehmite and epoxy and the formation of their interphases with different mechanical and chemical structures is crucial to predict and optimize the properties of epoxy-boehmite nanocomposites. Probing the interfacial properties with atomic force microscopy (AFM)-based methods, especially particle-matrix long-range interactions, is challenging. This is due to size limitations of various analytical methods in resolving nanoparticles and their interphases, the overlap of interphases, and the effect of buried particles that prevent the accurate interphase property measurement. Here, we develop a layered model system in which the epoxy is cured in contact with a thin layer of hydrothermally synthesized boehmite. Different microscopy methods are employed to evaluate the interfacial properties. With intermodulation atomic force microscopy (ImAFM) and amplitude dependence force spectroscopy (ADFS), which contain information about stiffness, electrostatic, and van der Waals forces, a soft interphase was detected between the epoxy and boehmite. Surface potential maps obtained by scanning Kelvin probe microscopy (SKPM) revealed another interphase about one order of magnitude larger than the mechanical interphase. The AFM-infrared spectroscopy (AFM-IR) technique reveals that the soft interphase consists of unreacted curing agent. The long-range electrical interphase is attributed to the chemical alteration of the bulk epoxy and the formation of new absorption bands. KW - Nanocomposites KW - Interphase KW - Intermodulation AFM KW - Electron microscopy KW - Infrared nano AFM PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483672 UR - https://www.mdpi.com/2079-4991/9/6/853/htm DO - https://doi.org/10.3390/nano9060853 SN - 2079-4991 VL - 9 IS - 6 SP - 853, 1 EP - 20 PB - MDPI AN - OPUS4-48367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Jaeger, Carsten A1 - Rashid, R. A1 - Munir, R. A1 - Zaidi, N. T1 - Cancer cell lipid class homeostasis is altered under nutrient-deprivation but stable under hypoxia N2 - Background: Cancer cells modify the balance between fatty acid (FA) synthesis and uptake under metabolic stress, induced by oxygen/nutrient deprivation. These modifications were shown to alter the levels of individual triglyceride (TG) or phospholipid sub-species. To attain a holistic overview of the lipidomic profiles of cancer cells under stress we performed a broad lipidomic assay, comprising 244 lipids from six major classes. This assay allowed us to perform robust analyses and assess the changes in averages of broader lipid-classes, stratified on the basis of saturation index of their fatty-acyl side chains. Methods: Global lipidomic profiling using Liquid Chromatography-Mass Spectrometry was performed to assess lipidomic profiles of biologically diverse cancer cell lines cultivated under metabolically stressed conditions. Results: Neutral lipid compositions were markedly modified under serum-deprived conditions and, strikingly, the cellular level of triglyceride subspecies decreased with increasing number of double bonds in their fatty acyl chains. In contrast and unexpectedly, no robust changes were observed in lipidomic profiles of hypoxic (2% O2) cancer cells despite concurrent changes in proliferation rates and metabolic gene expression. Conclusions: Serum-deprivation significantly affects lipidomic profiles of cancer cells. Although, the levels of individual lipid moieties alter under hypoxia (2% O2), the robust averages of broader lipid classes remain unchanged. KW - Tumor metabolism KW - Fatty acid metabolism KW - Lipidomic profile KW - Metabolic stress PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-483186 DO - https://doi.org/10.1186/s12885-019-5733-y SN - 1471-2407 VL - 19 SP - 501 PB - Springer Nature CY - Berlin AN - OPUS4-48318 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mekonnen, Tessema Fenta A1 - Panne, Ulrich A1 - Koch, Matthias T1 - New photodegradation products of the fungicide fluopyram: Structural elucidation and mechanism identification N2 - Identifying the fate of agrochemicals is important to understand their potential risk for living organisms. We report here new photodegradation products (PPs) of the fungicide fluopyram. The PPs were produced by irradiating a fluopyram standard in 0.1% acetonitrile aqueous media by a 150-W medium pressure Hg-lamp that emits wavelengths between 200–280 nm. The structural elucidation of PPs was achieved by combining the retention time, isotopic pattern, targeted fragmentation, and accurate mass measurements using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and high resolution-MS (HRMS). In addition to previously known PPs, seven new PPs of fluopyram were identified in this work: mainly dihydroxyl and hydroxylimide fluopyram as well as mono, di, and trihydroxyl lactam. Additionally, two PPs were found to be formed by rearrangement after the loss of H2C=CH2. Hence, the results of the work contribute to extending the current knowledge regarding the photoinduced fate of agrochemicals, and fluopyram in particular. KW - Photodegradation KW - Transformation products KW - LC-MS/MS KW - HRMS KW - Fungicide PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-466347 DO - https://doi.org/10.3390/molecules23112940 SN - 1420-3049 VL - 23 IS - 11 SP - 2940, 1 EP - 13 PB - MDPI CY - Basel AN - OPUS4-46634 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gotor, Raúl A1 - Bell, Jérémy A1 - Rurack, Knut T1 - Tailored fluorescent solvatochromic test strips for quantitative on-site detection of gasoline fuel adulteration N2 - Gasoline adulteration is a frequent problem world-wide, because of the chance of quick, maximized profits. However, addition of cheaper ethanol or hydrocarbons like kerosene does not only result in economic damage but also poses problems for vehicles and the environment. To enable law enforcement forces, customers or enterprises to uncover such a fraudulent activity directly upon suspicion and without the need to organize for sampling and laboratory analysis, we developed a simple strip-based chemical test. Key to the favorable performance was the dedicated materials tailoring, which led to test strips that consisted of a cellulose support coated with silica, passivated with hexamethyldisilazane and functionalized covalently with a molecular probe. The probe fluoresces brightly across a broad solvent polarity range, enabling reliable quantitative measurements and data analysis with a conventional smartphone. The assays showed high reproducibility and accuracy, allowing not only for the detection of gasoline adulteration but also for the on-site monitoring of the quality of commercial E10 gasoline. KW - Gasoline KW - Adulteration KW - Test strips KW - Benzin KW - Teststreifen KW - Fluorescence KW - Cellulose KW - Zellulose KW - Fluoreszenz PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-479231 UR - https://pubs.rsc.org/en/content/articlelanding/2019/tc/c8tc04818e DO - https://doi.org/10.1039/C8TC04818E SN - 2050-7526 VL - 7 IS - 8 SP - 2250 EP - 2256 PB - Royal Society of Chemistry CY - London, UK AN - OPUS4-47923 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keller, Julia A1 - Moldenhauer, Daniel A1 - Byrne, L. A1 - Haase, H. A1 - Resch-Genger, Ute A1 - Koch, Matthias T1 - Complexes of the mycotoxins citrinin and ochratoxin A with aluminum ions and their spectroscopic properties N2 - The sensitive detection of the mycotoxin citrinin (CIT) utilizing ist fluorescence requires approaches to enhance the emission. In this respect, we studied the complexation of CIT and ochratoxin A (OTA) with Al3+ in methanol using absorption and fluorescence spectroscopy. In this context, an isocratic high performance liquid chromatography (HPLC) method using a polymer column and a fluorescence detector was also developed that enables the separation of the metal ion complexes from the free ligands and non-complexed Al3+. CIT and OTA showed distinct changes in their absorption and fluorescence properties upon Al3+-coordination, and the fluorescence of CIT was considerably enhanced. Analysis of the photometrically assessed titration of CIT and OTA with Al3+ using the Job plot method revealed 1:2 and 1:1 stoichiometries for the Al3+ complexes of CIT (Al:CIT) and OTA (Al:OTA), respectively. In the case of CIT, only one -diketone moiety participates in Al3+ coordination. These findings can be elegantly exploited for signal amplification and provide the base to reduce the limit of detection for CIT quantification by about an order of magnitude, as revealed by HPLC measurements using a fluorescence detector. KW - Complexation KW - Aluminum KW - Fluorescence KW - Job plot KW - HPLC-DAD/FLD PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-470502 DO - https://doi.org/10.3390/toxins10120538 SN - 2072-6651 VL - 10 IS - 12 SP - 538, 1 EP - 8 PB - MDPI CY - Basel AN - OPUS4-47050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keller, Julia A1 - Hantschke, Luisa A1 - Haase, H. A1 - Koch, Matthias T1 - Synthesis and Structural Identification of a Biaryl Ether-Linked Zearalenone Dimer N2 - A new dimer of the food-relevant mycotoxin zearalenone was isolated after electrochemical and chemical oxidation. The structure was determined as a 16-O-15'-biaryl ether-linked dimer based on spectroscopic analyses (1H- and 13C-NMR, COSY, HMBC, and HSQCAD) and high-Resolution mass spectrometry analysis (Q-TOF). KW - Mycotoxin KW - Dimerization KW - HRMS KW - NMR PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-464940 DO - https://doi.org/10.3390/molecules23102624 SN - 1420-3049 VL - 23 IS - 10 SP - 2624 EP - 2628 PB - MDPI CY - Basel AN - OPUS4-46494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Hecht, Mandy A1 - Witthuhn, Heike A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Cover profile for the article "Mix‐&‐read determination of Mercury(II) at trace levels with hybrid mesoporous silica materials incorporating fluorescent probes by a simple mix‐&‐load technique" N2 - Invited for this month’s cover picture is the group of Dr. Knut Rurack at the Department of Analytical Chemistry; Reference Materials at the Bundesanstalt fuer Materialforschung und -pruefung (BAM) in Berlin (Germany). The cover picture shows how differences in color and fluorescence on a test strip can be easily read out with a mobile device. Two reference spots Frame the sensitive spot that indicates the presence of trace amounts of HgII below the threshold in a natural water sample. This dipstick contains a hybrid material that combines boron-dipyrromethene (BODIPY) probes sterically loaded into specifically tailored mesoporous silica particles, allowing for ultrasensitive HgII detection through enhanced fluorescence in a few seconds. The applicability in real water samples and fish extracts are also studied. KW - Mercury KW - Fluorescence KW - Dip-stick assay KW - Group profile PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-471267 DO - https://doi.org/10.1002/open.201800231 SN - 2191-1363 VL - 7 IS - 12 SP - 932 EP - 933 PB - Wiley-VCH CY - Weinheim AN - OPUS4-47126 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Rurack, Knut T1 - Streifenschnelltest mit ppt-Empfindlichkeit durch Kombination von Elektrochemilumineszenz-Detektion mit Aptamer-gesteuerter Indikatorfreisetzung aus mesoporösen Nanopartikeln N2 - Die Kombination aus elektrogenerierter Chemilumineszenz (ECL) und Aptamer-gesteuerter Indikatorfreisetzung (gAID) aus magnetischen mesoporösen Silica-Nanopartikeln, die in mit Poly(ethylenglycol) und N-(3-Triethoxysilylpropyl) diethanolamin funktionalisiertes Glasfaserpapier eingebettet sind, ermöglichte die Entwicklung eines Schnelltests, mit dem sich Penicillin direkt in verdünnter Milch bis auf 50 +/- 9 ppt in <5 min nachweisen lässt. Die kovalente Bindung der Aptamer-Kappe an das Siliciumdioxid-Gerüst ermöglichte den Verschluss der Poren durch nicht-kovalente elektrostatische Wechselwirkungen mit Oberflächen-Aminogruppen. Die Bindung von Penicillin führte zu einer Faltung des Aptamers, wodurch der zuvor in das Material geladene ECL-Reporter Ru(bpy)32+ freigesetzt wurde und nach lateralem Fluss von einer Smartphone-Kamera nach elektrochemischer Anregung mit einer in einen 3D-gedruckten Halter eingesetzten Siebdruckelektrode detektiert wird. Der Ansatz ist einfach, generisch und bietet Vorteile hinsichtlich Empfindlichkeit, Messunsicherheit und Robustheit gegenüber konventioneller Fluoreszenz- oder elektrochemischer Detektion, insbesondere für Point-of-Need-Analysen anspruchsvoller Matrices und Analyten im Ultraspurenbereich. KW - Schnelltests KW - Elektrochemilumineszenz KW - Aptamere KW - Teststreifen KW - Gesteuerte Freisetzung PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-540205 DO - https://doi.org/10.1002/ange.202110744 VL - 133 IS - 50 SP - 26491 EP - 26501 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54020 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Smeir, E. A1 - Leberer, S. A1 - Blumrich, A. A1 - Vogler, G. A1 - Vasiliades, A. A1 - Dresen, S. A1 - Jaeger, Carsten A1 - Gloaguen, Y. A1 - Klose, C. A1 - Beule, D. A1 - Schulze, P. A1 - Bodmer, R. A1 - Foryst-Ludwig, A. A1 - Kintscher, U. T1 - Depletion of Cardiac Cardiolipin Synthase Alters Systolic and Diastolic Function N2 - Cardiolipin (CL) is a major cardiac mitochondrial phospholipid maintaining regular mitochondrial morphology and function in cardiomyocytes. Cardiac CL production includes ist biosynthesis and a CL-remodeling process. Here we studied the impact of CL-biosynthesis and the enzyme Cardiolipin Synthase (CLS) on cardiac function. CLS and cardiac CL-species were significantly downregulated in cardiomyocytes following catecholamine-induced cardiac damage in mice, accompanied by increased oxygen consumption rates, signs of oxidative stress and mitochondrial uncoupling. RNAi-mediated cardiomyocyte-specific knockdown of CLS in Drosophila melanogaster resulted in marked cardiac dilatation, severe impairment of systolic performance and slower diastolic filling velocity assessed by fluorescence-based heart imaging. Finally, we showed that CL72:8 is significantly decreased in cardiac samples from patients with heart failure with reduced ejection fraction (HFrEF). In summary, we identified CLS as a regulator of cardiac function. Considering the cardiac depletion of CL-species in HFrEF, pharmacological targeting of CLS may be a promising therapeutic approach.zeige mehrzeige weniger KW - High-resolution mass spectrometry KW - Nontarget analysis KW - Heart failure KW - Cardiolipins KW - Lipidomics PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-536833 DO - https://doi.org/10.1016/j.isci.2021.103314 VL - 24 IS - 11 SP - 103314 PB - Cell Press AN - OPUS4-53683 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hudson, A.D. A1 - Jamieson, O. A1 - Crapnell, R.D. A1 - Rurack, Knut A1 - Soares, T.C.C. A1 - Mecozzi, F. A1 - Laude, A. A1 - Gruber, J. A1 - Novakovic, K. A1 - Peeters, M. T1 - Dual detection of nafcillin using a molecularly imprinted polymer-based platform coupled to thermal and fluorescence read-out N2 - Reported here is the production of molecularly imprinted polymer (MIP) films, integrating a fluorescent moiety that serves as both an element for template interaction and signalling, for the thermal and optical detection of the beta-lactam antibiotic nafcillin. Fluorescein methacrylate (FluMa) was synthesized and introduced during the molecular imprinting process as the sole monomer and in a 1 : 1 mixture with methacrylic acid (MAA), allowing to draw first conclusions on the MIP formation potential of such a rather large and rigid monomer. At first, MIP microparticles containing FluMa were prepared by free radical polymerisation. Optical batch rebinding experiments revealed that FluMa can act as a functional monomer for selective detection of nafcillin; however, the addition of MAA as co-monomer significantly improved performance. Subsequently, thin MIP films containing FluMa were deposited onto functionalised glass slides and the influence of porogen, drying time, and monomer composition was studied. These MIP-functionalised glass electrodes were mounted into a customised 3D-printed flow cell, where changes in the liquid were either evaluated with a thermal device or using fluorescence bright field microscopy. Thermal analysis demonstrated that multiple MIP layers enhanced sensor specificity, with detection in the environmentally relevant range. The fluorescence bright field microscope investigations validated these results, showing an increase in the fluorescence intensity upon exposure of the MIP-functionalised glass slides to nafcillin solutions. These are promising results for developing a portable sensor device that can be deployed for antibiotics outside of a dedicated laboratory environment, especially if sensor design and fluorophore architecture are optimised. KW - Molecularly Imprinted Polymers KW - Fluorescence KW - Antibiotics KW - Heat-transfer Measurements KW - Thin films PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-540044 DO - https://doi.org/10.1039/D1MA00192B VL - 2 IS - 15 SP - 5105 EP - 5115 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-54004 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kazlagić, Anera A1 - Russo, Francesco A1 - Vogl, Jochen A1 - Sturm, Patrick A1 - Stephan, D. A1 - Gluth, Gregor ED - Resch-Genger, Ute ED - Koch, Matthias ED - Meermann, Björn ED - Weller, Michael G. T1 - Development of a sample preparation procedure for Sr isotope analysis of Portland cements N2 - The 87Sr/86Sr isotope ratio can, in principle, be used for provenancing of cement. However, while commercial cements consist of multiple components, no detailed investigation into their individual 87Sr/86Sr isotope ratios or their influence on the integral 87Sr/86Sr isotope ratio of the resulting cement was conducted previously. Therefore, the present study aimed at determining and comparing the conventional 87Sr/86Sr isotope ratios of a diverse set of Portland cements and their corresponding Portland clinkers, the major component of these cements. Two approaches to remove the additives from the cements, i.e. to measure the conventional 87Sr/86Sr isotopic fingerprint of the clinker only, were tested, namely, treatment with a potassium hydroxide/sucrose solution and sieving on a 11-µm sieve. Dissolution in concentrated hydrochloric acid/nitric acid and in diluted nitric acid was employed to determine the 87Sr/86Sr isotope ratios of the cements and the individual clinkers. The aim was to find the most appropriate sample preparation procedure for cement provenancing, and the selection was realised by comparing the 87Sr/86Sr isotope ratios of differently treated cements with those of the corresponding clinkers. None of the methods to separate the clinkers from the cements proved to be satisfactory. However, it was found that the 87Sr/86Sr isotope ratios of clinker and cement generally corresponded, meaning that the latter can be used as a proxy for the clinker 87Sr/86Sr isotope ratio. Finally, the concentrated hydrochloric acid/nitric acid dissolution method was found to be the most suitable sample preparation method for the cements; it is thus recommended for 87Sr/86Sr isotope analyses for cement provenancing. KW - Cement KW - Provenancing KW - Sr isotopes KW - Portland clinker KW - Dissolution PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542239 DO - https://doi.org/10.1007/s00216-021-03821-7 SN - 1618-2642 SN - 1618-2650 VL - 414 IS - 15 (Topical collection: Analytical methods and applications in the materials and life sciences) SP - 4379 EP - 4389 PB - Springer CY - Berlin AN - OPUS4-54223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Climent Terol, Estela A1 - Gojani, Ardian A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - Generalized Analysis Approach of the Profile Roughness by Electron Microscopy with the Example of Hierarchically Grown Polystyrene–Iron Oxide–Silica Core–Shell–Shell Particles N2 - The roughness as a property of core–shell (CS) microparticles plays a key role in their functionality. Quantitative evaluation of the roughness of CS microparticles is, however, a challenging task with approaches using electron microscopy images being scarce and showing pronounced differences in terms of methodology and results. This work presents a generalized method for the reliable roughness determination of nonplanar specimens such as CS particles from electron microscopic images, the method being robust and reproducible with a high accuracy. It involves a self-written software package (Python) that analyzes the recorded images, extracts corresponding data, and calculates the roughness based on the deviation of the identified contour. Images of single particles are taken by a dual mode scanning electron microscopy (SEM) setup which permits imaging of the same field-of-view of the sample with high resolution and surface sensitive in SE InLens mode as well as in transmission mode (TSEM). Herein, a new type of polystyrene core–iron oxide shell–silica shell particles is developed to serve as a set of lower micrometer-sized study objects with different surface roughness; the analysis of their images by the semiautomatic workflow is demonstrating that the particles’ profile roughness can be quantitatively obtained. KW - Core–shell particles KW - Image analysis KW - Nanoparticles KW - Roughness KW - SEM KW - transmission mode PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542576 DO - https://doi.org/10.1002/adem.202101344 SP - 1 EP - 9 PB - Wiley-VCH AN - OPUS4-54257 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sommerfeld, Thomas A1 - Jung, Christian A1 - Riedel, Juliane A1 - Mauch, Tatjana A1 - Sauer, Andreas A1 - Koch, Matthias T1 - Development of a certified reference material for the determination of polycyclic aromatic hydrocarbons (PAHs) in rubber toy N2 - Polycyclic aromatic hydrocarbons (PAHs) are a large group of priority organic pollutants, which contaminate environmental compartments, food, and consumer products as well. Due to their frequent occurrence associated with elevated Levels of PAHs, plastic and rubber parts of consumer products and toys are particular sources of exposure. Although European maximum levels exist for eight carcinogenic PAHs in consumer products and toys according to REACH Regulation (EC) No. 1907/2006, certified reference materials (CRM) are still not available. To overcome this lack, the first CRM for the determination of PAHs in rubber toys (BAM-B001) was developed according to the requirements of ISO Guide 35. The whole process of CRM development including preparation, homogeneity and stability studies, and value assignment is presented. The assignment of the certified mass fractions was based upon in-house study at BAM using stable isotope Dilution analysis (SIDA) gas chromatography mass spectrometry (GC–MS). The obtained values were confirmed by the results of two interlaboratory comparison (ILC) studies with more than 50 expert laboratories from Germany and China. The mass fractions of 14 PAHs including all REACH and GS mark regulated compounds were certified ranging between 0.2 and 15.4 mg/ kg accompanied by expanded uncertainties (coverage factor k = 2). In addition, informative values were determined for 4 PAHs, mainly due to higher uncertainties and/or lack of ILC data for confirmation. BAM-B001 is intended for analytical quality control particularly based on the AfPS GS 2019:01 PAK method and contributes to improve the chemical safety of consumer products including toys. KW - PAHs KW - Consumer Products KW - Toys KW - Chemical Safety KW - Certified reference material KW - Quality assurance PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-539920 DO - https://doi.org/10.1007/s00216-021-03796-5 VL - 414 IS - 15 SP - 4369 EP - 4378 PB - Springer AN - OPUS4-53992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nowatzky, Yannek A1 - Russo, Francesco Friedrich A1 - Lisec, Jan A1 - Kister, Alexander A1 - Reinert, Knut A1 - Muth, Thilo A1 - Benner, Philipp T1 - FIORA: Local neighborhood-based prediction of compound mass spectra from single fragmentation events N2 - Non-targeted metabolomics holds great promise for advancing precision medicine and biomarker discovery. However, identifying compounds from tandem mass spectra remains a challenging task due to the incomplete nature of spectral reference libraries. Augmenting these libraries with simulated mass spectra can provide the necessary references to resolve unmatched spectra, but generating high-quality data is difficult. In this study, we present FIORA, an open-source graph neural network designed to simulate tandem mass spectra. Our main contribution lies in utilizing the molecular neighborhood of bonds to learn breaking patterns and derive fragment ion probabilities. FIORA not only surpasses state-of-the-art fragmentation algorithms, ICEBERG and CFM-ID, in prediction quality, but also facilitates the prediction of additional features, such as retention time and collision cross section. Utilizing GPU acceleration, FIORA enables rapid validation of putative compound annotations and large-scale expansion of spectral reference libraries with high-quality predictions. KW - Metabolomics KW - Machine Learning KW - Mass spectrometry KW - Bioinformatics PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627585 DO - https://doi.org/10.1038/s41467-025-57422-4 SN - 2041-1723 VL - 16 IS - 1 SP - 1 EP - 17 PB - Springer Science and Business Media LLC AN - OPUS4-62758 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - López-Puertollano, Daniel A1 - Duncan, Hadyn A1 - Abad-Somovilla, Antonio A1 - Abad-Fuentes, Antonio A1 - Rurack, Knut T1 - Competitive cytometry-based immunoassay for patulin determination in apple juice N2 - Patulin is a mycotoxin that is frequently found in apples and apple-derived products. Given the potential harm it can cause to humans, maximum levels for patulin in food have been set worldwide. Conventional methods for the detection of patulin are often time-consuming or lack sensitivity. In this study, a novel cytometry approach based on specific monoclonal antibodies is presented. These high-affinity binders do not target patulin itself, but a stable derivative (adduct) that is rapidly obtained in an aqueous medium at room temperature. To develop the assay, a specific fluorescent competitor was designed and synthesized. After optimizing the assay conditions, including the concentration of the fluorescent competitor and of the antibody bound to polystyrene-silica core–shell microparticles, a detection limit of 0.03 μg L-1 in buffer was achieved. Finally, validation according to Commission Regulation (EU) 2023/2782 demonstrated that apple juice samples spiked with patulin at 25 or 50 μg L-1 (permissible limits set by the EU) were properly scored as non-compliant without any additional treatment other than a simple dilution step in buffer. The developed assay offers several key advantages, including rapid analysis, high sensitivity and specificity, and the potential for multiplexing, making it a promising analytical tool for routine monitoring of patulin contamination in food. KW - Bead-based assay KW - Cytometry KW - Derivatization KW - Mycotoxin KW - Patulin PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-627659 DO - https://doi.org/10.1016/j.microc.2025.113287 SN - 1095-9149 VL - 212 SP - 1 EP - 8 PB - Elsevier B.V. AN - OPUS4-62765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - López-Puertollano, Daniel A1 - Tobias, Charlie A1 - Bell, Jérémy A1 - Abad-Somovilla, A. A1 - Abad-Fuentes, A. A1 - Rurack, Knut T1 - Superparamagnetic Bead-Based Microfluidic Fluoroimmunoassay Platform for Rapid Ochratoxin A Detection in Flour N2 - Simplification and reduction of time and costs are the primary goals in the development and use of onsite methods in diagnostics and food safety. To facilitate the transition from laboratory techniques to simple, miniaturized devices, we have developed a modular microfluidic platform. This platform integrates a competitive fluorescence immunoassay on the surface of superparamagnetic beads, serving as a complementary technique to traditional cytometry assays. In the first chip module, a fast competitive reaction (5 min) occurs, after which the particles are retained in the second module. This module consists of a PDMS chip and a permanent magnet, allowing only the fluorescent competitor to reach the detection module. Ochratoxin A (OTA) was chosen as the model analyte for device development, using fluorescein-labeled OTA as a competitor. The system efficiently separates particles, with OTA concentration directly correlated to the amount of fluorescent competitor remaining in solution after the competitive reaction. This innovative setup allows to perform rapid measurements with small sample volumes in a short time (10 min), achieving a limit of detection for OTA of 1.2 μg L–1. The system was successfully applied to the accurate determination of OTA in wheat flour spiked at regulatorily relevant concentrations. Using this device, conventional cytometry immunoassays can be seamlessly transformed into user-friendly, miniaturized analytical methods at reduced cost for applications outside of a laboratory directly at the point of need. KW - Bead-based assay KW - Fluorescence KW - Immunoassay KW - Microfluidics KW - mycotoxins PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-638472 DO - https://doi.org/10.1021/acssensors.5c01119 SN - 2379-3694 SP - 1 EP - 10 PB - American Chemical Society CY - Washington, D.C. AN - OPUS4-63847 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Winckelmann, Alexander A1 - Nowak, S. A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Riedel, Jens A1 - Vogl, Jochen A1 - Panne, Ulrich A1 - Abad Andrade, Carlos Enrique T1 - High-Resolution Atomic Absorption Spectrometry Combined With Machine Learning Data Processing for Isotope Amount Ratio Analysis of Lithium N2 - An alternative method for lithium isotope amount ratio analysis based on a combination of high-resolution atomic absorption spectrometry and spectral data analysis by machine learning (ML) is proposed herein. It is based on the well-known isotope shift of approximately 15 pm for the electronic transition 22P←22S at around the wavelength of 670.8 nm, which can be measured by the state-of-the-art high-resolution continuum source graphite furnace atomic absorption spectrometry. For isotope amount ratio analysis, a scalable tree boosting ML algorithm (XGBoost) was employed and calibrated using a set of samples with 6Li isotope amount fractions, ranging from 0.06 to 0.99 mol mol–1, previously determined by a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS). The calibration ML model was validated with two certified reference materials (LSVEC and IRMM-016). The procedure was applied toward the isotope amount ratio determination of a set of stock chemicals (Li2CO3, LiNO3, LiCl, and LiOH) and a BAM candidate reference material NMC111 (LiNi1/3Mn1/3Co1/3O2), a Li-battery cathode material. The results of these determinations were compared with those obtained by MC-ICP-MS and found to be metrologically comparable and compatible. The residual bias was −1.8‰, and the precision obtained ranged from 1.9 to 6.2‰. This precision was sufficient to resolve naturally occurring variations, as demonstrated for samples ranging from approximately −3 to +15‰. To assess its suitability to technical applications, the NMC111 cathode candidate reference material was analyzed using high-resolution continuum source atomic absorption spectrometry with and without matrix purification. The results obtained were metrologically compatible with each other. KW - Lithium KW - Isotope KW - Machine learning KW - Algorithms KW - Reference material KW - AAS KW - Atomic Absorption Spectrometry PY - 2021 DO - https://doi.org/10.1021/acs.analchem.1c00206 SN - 1520-6882 VL - 93 IS - 29 SP - 10022 EP - 10030 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-53028 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pisonero, J. A1 - Fandino, J. A1 - Nordlien, J. H A1 - Richter, Silke A1 - Pfeifer, Jens A1 - Quarles, C. D. A1 - Gonzalez, J. A1 - Jakubowski, Norbert A1 - Bordel, N. T1 - Improving the analytical performance of pulsed-GD-SFMS for multi-elemental depth profile analysis of heat-treated Zn coatings on extruded aluminium N2 - The formation of diffusion layers on Zn layers deposited on Al substrates is mainly used to prevent corrosion effects. Evaluation of the influence exerted by different coating methodologies and heat treatments on the formation of these diffusion layers is of great interest for the aluminium industry. Particularly, multi-elemental in-depth distributions of major, minor and trace elements in Zn-coatings is highly demanded before and after heat treatments. A fast characterization of these materials require a direct solid analytical technique able to provide high sensitivity and high depth resolution. For this purpose, an improved analytical method based on the use of pulsed glow discharge sector field mass spectrometry (pulsed-GD-SFMS) is investigated. Glow discharge operating parameters (e.g. pulse duration, pulse frequency), glow discharge source design (e.g. flow tube lengths), and SFMS mass spectra acquisition conditions (e.g. integration time) are evaluated to achieve low sputtering rates, high mass spectra acquisition rates and improved depth resolution. At the optimize conditions Zn coatings deposited by arc-spray and electrodeposition are analysed before and after heat treatments to evaluate the diffusion of different key elements. Moreover, results are validated using femtosecond laser ablation (fs-LA)-ICP-MS, which provides additional information about the heterogeneous distribution of some elements in the Zn coatings. KW - GDMS KW - Pulsed-GD-SFMS KW - Depht profiling KW - Zn KW - Aluminium PY - 2019 DO - https://doi.org/10.1039/c9ja00189a VL - 34 IS - 11 SP - 2252 EP - 2260 PB - Royal Society of Chemistry CY - London AN - OPUS4-49451 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Döring, Sarah A1 - Konthur, Zoltán A1 - Weller, Michael G. A1 - Jaeger, Carsten A1 - Reinders, Yvonne T1 - Challenges and Insights in Absolute Quantification of Recombinant Therapeutic Antibodies by Mass Spectrometry: An Introductory Review N2 - This review describes mass spectrometry (MS)-based approaches for the absolute quantification of therapeutic monoclonal antibodies (mAbs), focusing on technical challenges in sample treatment and calibration. Therapeutic mAbs are crucial for treating cancer and inflammatory, infectious, and autoimmune diseases. We trace their development from hybridoma technology and the first murine mAbs in 1975 to today’s chimeric and fully human mAbs. With increasing commercial relevance, the absolute quantification of mAbs, traceable to an international standard system of units (SI units), has attracted attention from science, industry, and national metrology institutes (NMIs). Quantification of proteotypic peptides after enzymatic digestion using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has emerged as the most viable strategy, though methods targeting intact mAbs are still being explored. We review peptide-based quantification, focusing on critical experimental steps like denaturation, reduction, alkylation, choice of digestion enzyme, and selection of signature peptides. Challenges in amino acid analysis (AAA) for quantifying pure mAbs and peptide calibrators, along with software tools for targeted MS data analysis, are also discussed. Short explanations within each chapter provide newcomers with an overview of the field’s challenges. We conclude that, despite recent progress, further efforts are needed to overcome the many technical hurdles along the quantification workflow and discuss the prospects of developing standardized protocols and certified reference materials (CRMs) for this goal. We also suggest future applications of newer technologies for absolute mAb quantification. KW - Monoclonal antibody KW - Therapeutic antibodies KW - Mass spectrometry KW - Liquid chromatography KW - Absolute quantification KW - Metrology KW - Traceability KW - Certified reference material PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-623707 DO - https://doi.org/10.3390/antib14010003 SN - 2073-4468 VL - 14 IS - 1 SP - 1 EP - 26 PB - MDPI CY - Basel, Schweiz AN - OPUS4-62370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholl, Juliane A1 - Lisec, Jan A1 - Haase, Hajo A1 - Koch, Matthias T1 - Identification of transformation products from fluorinated lithium-ion battery additives TPFPB and TPFPP: forever chemicals of tomorrow? N2 - AbstractFluorinated organic compounds (FOCs) represent a class of synthetic chemicals distinguished by their resilient carbon–fluorine bonds, which demonstrate an ability to withstand environmental degradation over an extended period. The integration of FOCs into cutting-edge applications, including lithium-ion batteries (LiBs), presents considerable potential for environmental harm that has not yet been sufficiently addressed. This study focuses on the environmental fate of two fluorinated aromatics, tris(pentafluorophenyl)borane (TPFPB) and tris(pentafluorophenyl)phosphine (TPFPP), given their important role in improving the performance of LiBs. To achieve this, laboratory simulation methods including total oxidizable precursor assay, electrochemistry (EC), Fenton reaction, UV-C irradiation, and hydrolysis were employed. Liquid chromatography and gas chromatography coupled with high-resolution mass spectrometry were used for identification of transformation products (TPs) and prediction of their molecular formulae. Despite the structural similarity between TPFPB and TPFPP, distinct differences in electrochemical behavior and degradation pathways were observed. TPFPB readily underwent hydroxylation and hydrolysis, resulting in a wide range of 49 TPs. A total of 28 TPs were newly identified, including oligomers and highly toxic dioxins. In contrast, TPFPP degraded exclusively under harsh conditions, requiring the development of innovative conditioning protocols for EC. In total, the simulation experiments yielded nine structurally different compounds, including seven previously undescribed, partially defluorinated TPs. This study highlights the potential risks associated with the use of FOCs in LiBs and provides insight into the complex environmental behavior of FOCs. KW - Mass Spectrometry KW - LiBs KW - POPs KW - Transformation products KW - Electrochemistry PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611339 DO - https://doi.org/10.1007/s00216-024-05526-z SP - 1 EP - 15 PB - Springer Science and Business Media LLC AN - OPUS4-61133 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Verhassel, Alejandra A1 - Kimani, Martha Wamaitha A1 - Gidwani, Kamlesh A1 - Sandholm, Jouko A1 - Gawlitza, Kornelia A1 - Rurack, Knut A1 - Härkönen, Pirkko T1 - Detection of Tn-antigen in breast and prostate cancer models by VVL-labeled red dye-doped nanoparticles N2 - Aim: Fluorescence detection of breast and prostate cancer cells expressing Tn-antigen, a tumor marker, with Vicia villosa lectin (VVL)-labeled nanoparticles. Materials & methods: Breast and prostate cancer cells engineered to express high levels of Tn-antigen and non-engineered controls were incubated with VVL-labeled or unlabeled red dye-doped silica-coated polystyrene nanoparticles. The binding to cells was studied with flow cytometry, confocal microscopy, and electron microscopy. Results: Flow cytometry showed that the binding of VVL-labeled nanoparticles was significantly higher to Tn-antigen-expressing cancer cells than controls. Confocal microscopy demonstrated that particles bound to the cell surface. According to the correlative light and electron microscopy the particles bound mostly as aggregates. Conclusion: VVL-labeled nanoparticles could provide a new tool for the detection of Tn-antigen-expressing breast and prostate cancer cells. KW - Breast cancer cells KW - Fluorescence detection KW - Lectin labeling KW - Prostate cancer cells KW - Silica-coated polystyrene nanoparticles KW - Tn-antigen KW - VVL PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613451 DO - https://doi.org/10.1080/17435889.2024.2405454 SN - 1743-5889 VL - 19 SP - 2463 EP - 2478 PB - Taylor & Francis CY - London AN - OPUS4-61345 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jamieson, O. D. A1 - Bell, Jérémy A1 - Hudson, A. A1 - Saczek, J. A1 - Perez-Padilla, Victor A1 - Kaiya, G. A1 - Novakovic, K. A1 - Davies, M. A1 - Foster, E. A1 - Gruber, J. A1 - Rurack, Knut A1 - Peeters, M. T1 - Design and Application of an Imprinted Polymer Sensor for the Dual Detection of Antibiotic Contaminants in Aqueous Samples and Food Matrices N2 - An innovative polymer-based dual detection microfluidic platform has been developed for the accurate and reliable sensing of trace amounts of antibiotic tetracycline in environmental and food samples. This was achieved through the production of a bespoke polymeric material formed via an imprinting technique using a fluorescent dye. Thus, this enables dual detection of tetracycline, both thermally, via analyzing the heat-transfer resistance at the solid−liquid interface, and optically, through the inner filter effect. The combination of these two methods achieved a nanomolar limit of detection for tetracycline while also providing rapid, selective, and cost-effective sensing. Additionally, this method successfully detected tetracycline levels of 0.56 μM in blank egg samples which was significantly lower than the maximum residual level of 400 μg L−1 (0.9 μM). Our work shows that this approach can be used for the efficient detection of trace antibiotics in complex environmental and food samples, offering enhanced reliability through the integration of two complementary analysis techniques. This sensor has the potential to identify sources of antimicrobial resistance, which is crucial for targeted efforts to combat this pressing global health challenge. KW - Molecularly imprinted polymers KW - Antibiotics monitoring KW - Orthogonal detection KW - Sensors PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-626497 DO - https://doi.org/10.1021/acsapm.4c03218 SN - 2637-6105 VL - 7 IS - 4 SP - 1 EP - 9 PB - American Chemical Society CY - Washington, D.C. AN - OPUS4-62649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Morcillo, Dalia A1 - Winckelmann, Alexander A1 - Frick, Daniel A. A1 - Jacobsen, Lars A1 - Seger, Tino A1 - Florek, Stefan A1 - Richter, Silke A1 - Vogl, Jochen A1 - Recknagel, Sebastian A1 - Panne, Ulrich A1 - Abad Andrade, Carlos Enrique T1 - Lithium isotope ratio analysis of geological samples using atomic absorption spectrometry with improved spectral resolution N2 - This study introduces an improved spectrometric method with enhanced precision to determine isotope ratios in geological samples without chromatographic separation. Firstly, the improvement is achieved by increasing the spectral resolution of the spectrometer applied in well-known high-resolution continuum source atomic absorption spectrometry (HR-CS-AAS). The resulting resolving power and linear dispersion of the upgraded setup, which is denoted in the following as HR+CS-AAS, is well adapted to the line widths of the Li isotope components we investigated. Secondly, our proposed method combines optical absorption spectrometry with machine learning data analysis using an extreme gradient boosting algorithm (XGBoost). This method was applied to analyze certified geological reference materials with δLSVEC(7Li/6Li) (hereafter δ7Li) values ranging from −0.5 ‰ to 4.5 ‰. With a pixel related optical resolving power of λ/∆λ ≈ 780 000, we obtain precisions in δ7Li measurements from 1.0 ‰ to 2.5 ‰. The method is validated by comparing the results with multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS), confirming its metrological compatibility. This work presents a fast, robust, and reliable method for δ7Li measurement in geological samples. KW - Isotope KW - High-resolution continuum source atomic absorption spectroscopy KW - Lithium KW - Machine learning KW - Echelle spectrometer PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611807 DO - https://doi.org/10.1016/j.sab.2024.107013 VL - 220 SP - 1 EP - 5 PB - Elsevier BV AN - OPUS4-61180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuner, Maximilian T1 - Cleaving ergot alkaloids - development of a novel food screening method N2 - Mycotoxins (toxic compounds formed by fungi) in food and feed have caused problems for mankind since the beginning of time. The group of ergot alkaloids plays a special role in human history. Several tens of thousands of deaths during the middle ages caused by to ergotism (the disease caused by continuous intake of ergot alkaloid contaminated food) underscore the importance of reliable analytical methods to ensure food safety. More than 50 compounds belong to the group of ergot alkaloids. The 12 most found structures – the major ergot alkaloids – are typically measured, when it comes to ergot alkaloid quantification. High performance liquid chromatography (HPLC) with a fluorescence detector (FLD) is typically used to quantify the ergot alkaloid content. The main disadvantage of this method are the high costs for calibration standards (12 different calibration substances are required). But also, the time and effort required for the analysis of 12 peaks and overlapping signals that occur in complex food samples such as bread. As all ergot alkaloids share the ergoline structure and just differ in the substituents attached to this backbone, measurement of all ergot alkaloids in one sum parameter presents a time and cost saving alternative. The most important step for the development of such a sum parameter method is the reaction used to transfer all ergot alkaloids to one uniform structure. Two promising reactions, the acidic esterification to lysergic acid methyl ester and hydrazinolysis to lysergic acid hydrazide, were examined for possible use in a routine analysis method. In addition to yield and reaction rate, factors such as handling of the reaction and the possibility of parallel sample workup play a role. T2 - Adlershofer Forschungsforum 2022 CY - Berlin, Germany DA - 11.11.2022 KW - Ergot alkaloids KW - Screening PY - 2022 AN - OPUS4-56585 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hülagü, Deniz A1 - Tobias, Charlie A1 - Gojani, Ardian A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - Analysis of the profile roughness of core-shell microparticles by electron microscopy N2 - A particle roughness analysis tool, based on electron microscopy images (SEM and TEM). The influence of various parameters on the calculated roughness was also investigated: the setting of the proper threshold, accelerating voltage, etc. The samples were gradually tilted to extend imaging information of more than only one projection. Furthermore, the measurement uncertainty of the profile roughness of particles associated to various orientations was estimated. KW - Core-shell particles KW - Electron microscopy KW - Image processing KW - MamaLoCa KW - Particle Characterization KW - Roughness PY - 2021 DO - https://doi.org/10.1017/S1431927621007285 VL - 27 IS - Suppl. 1 SP - 2002 EP - 2004 PB - Cambridge University Press AN - OPUS4-53123 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - PFAS Sensors N2 - This contribution provides an introduction to the development of sensors for PFAS analysis, presents the most common approaches, and describes the opto-microfluidic strategy in combination with polymerizable indicators and detection matrices currently being pursued by the Chemical and Optical Sensing Division at BAM. T2 - Advancements of Analytical Techniques for Per- and Polyfluoroalkyl Substances (PFAS) – Second Workshop 2023 CY - Berlin, Germany DA - 19.09.2023 KW - PFAS KW - Sensors KW - Molecularly imprinted polymers KW - Microfluidics KW - Fluorescence PY - 2023 AN - OPUS4-58533 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Morcillo, Dalia T1 - Atomic absorption spectrometry with machine learning as a tool for lithium isotope analysis N2 - The general interest in the implementation of renewable energies, particularly in the development of lithium-ion batteries, makes lithium a key element to be analyzed. We are working to develop this tool to determine if the isotopic effect of lithium has an impact on battery aging. T2 - SALSA Konferenz CY - Berlin, Germany DA - 16.09.2021 KW - Atomic absorption spectrometry KW - Battery KW - Machine learning KW - Lithium KW - Isotope PY - 2021 AN - OPUS4-53693 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kimani, Martha Wamaitha A1 - Kislenko, Evgeniia A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Author correction: Fluorescent molecularly imprinted polymer particles for glyphosate detection using phase transfer agents N2 - This is a corrigendum to the original article "Fluorescent molecularly imprinted polymer particles for glyphosate detection using phase transfer agents" that was published in the journal "Scientific reports", vol. 12 (2022), article no. 14151. PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642416 DO - https://doi.org/10.1038/s41598-023-28025-0 SN - 2045-2322 VL - 13 IS - 1 SP - 1 EP - 2 PB - Macmillan Publishers Limited CY - London AN - OPUS4-64241 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matiushkina, Anna T1 - Quantification of Hydrophilic Surface Ligands on Nanoparticles N2 - The rapid development of nanotechnology is driven by a wide range of possible applications of nanoparticles (NPs) depending on their functions and composition, for example, in biomedicine, energy harvesting, and optoelectronics. Due to the large surface-to-volume ratio of nanoparticles, their properties and function are often highly dependent on surface chemistry, which also determines their stability and interaction with the environment. To ensure the successful advancement of nanomaterials in biomedical applications as well as in material sciences, it is hence crucial to develop reliable methods to control and quantify ligand molecules and functional groups on the NP surface for different NP processing steps including ligand exchange and the subsequent functionalization with, e.g., antifouling agents and recognition moieties. These methods must then be validated and eventually standardized. This also calls for suitable reference materials with known surface chemistries or functionalities. Methods for determining and quantifying surface functional groups and NP capping ligands include quantitative nuclear magnetic resonance (qNMR) techniques, thermogravimetric analysis (TGA), mass spectrometric (MS) methods, high-performance liquid chromatography (HPLC), and optical assays with photometric and/or fluorometric readout.[1] In the focus of this study on ligand exchange and quantification are differently sized iron oxide nanoparticles (IONPs), already used in biomedicine with applications as magnetic resonance imaging (MRI) contrast agents or for magnetic hyperthermia. IONPs can be prepared by a high temperature synthesis in nonpolar solvents, resulting in a superior monodispersity and crystallinity compared to particles prepared by aqueous synthesis methods. Such IONPs bear, however, hydrophobic surface ligands, that need to be exchanged for hydrophilic molecules to ensure water dispersibility required for biomedical applications. For these applications, a complete removal of potentially toxic surface ligands remaining from IONP synthesis is crucial. Here, we will present the synthesis of differently sized spherical IONPs capped with hydrophobic oleic acid molecules and an in-depth study of the ligand exchange to hydrophilic molecules such as citrate. We assessed the size, size distribution, and colloidal stability of the IONPs utilizing transmission electron microscopy (TEM), dynamic light scattering (DLS), and Zeta potential measurements before and after ligand exchange. In addition, several approaches to ligand quantification have been explored involving a variety of analytical tools. Our ultimate goal is here to identify the optimal methods for ligand analysis and to develop schemes for method validation, via the comparison of analytical techniques relying on different principles of signal generation (method cross-validation). T2 - E-MRS 2024 SPRING MEETING CY - Strasbourg, France DA - 27.05.2024 KW - Nano KW - Particle KW - Iron oxide KW - Ligand KW - Quantification KW - Advanced material KW - Surface analysis KW - Functional group PY - 2024 AN - OPUS4-62296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ashokkumar, Pichandi A1 - Bell, Jérémy A1 - Buurman, Merwe A1 - Rurack, Knut T1 - Analytical platform for sugar sensing in commercial beverages using a fluorescent BODIPY "light-up" probe N2 - Because of the globally increasing prevalence of diabetes, the need for accurate, efficient and at best miniaturized automated analytical systems for sugar detection in medical diagnostics and the food industry is still urgent. The development of molecular probes for sugars based on boronic acid receptors offers an excellent alternative to the kinetically slow enzyme-based sugar sensors. Moreover, by coupling such chelating units with dye scaffolds like BODIPYs (boron–dipyrromethenes), highly fluorescent sugar sensing schemes can be realized. In this work, a boronic acid-functionalized BODIPY probe was developed, which binds selectively to fructose’s adjacent diols to form cyclic boronate esters. Placement of an amino group in direct neighborhood of the boronic acid moiety allowed us to obtain a broad working range at neutral pH, which distinguishes the probe from the majority of systems working only at pH > 8, while still meeting the desired sensitivity in the micro-molar range due to a pronounced analyte-induced fluorescence increase. To enhance the applicability of the test in the sense described above, integration with a microfluidic chip was achieved. Here, fructose was selectively detected by fluorescence with similar sensitivity in real time on chip, and an assay for the straightforward detection of sugar in (colored) sodas without sample clean-up was established. KW - BODIPY dyes KW - Boronic acid KW - Fluorescence KW - Microfluidics KW - Sugars PY - 2018 DO - https://doi.org/10.1016/j.snb.2017.09.201 SN - 0925-4005 VL - 256 SP - 609 EP - 615 PB - Elsevier CY - Amsterdam AN - OPUS4-43102 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Descalzo, Ana B. A1 - Xu, H.-J. A1 - Shen, Z. A1 - Rurack, Knut T1 - Influence of the meso-substituent on strongly red emitting phenanthrene-fused boron–dipyrromethene (BODIPY) fluorophores with a propeller-like conformation N2 - Highly emissive phenanthrene-fused boron–dipyrromethene (PBDP) dyes have been spectroscopically characterized in a series of solvents. The influence of different substituents (-H, -I, -CN, -DMA or a 15C5-crown ether) in the para-position of a phenyl ring attached to the meso-position of the BODIPY core is discussed. This family of dyes has an intense emission at lambda > 630 nm, with fluorescence quantum yields between 0.7 and 1.0 in all solvents studied, except in the case of the dimethylamino-substituted derivative, PBDP-DMA, which undergoes excited-state intramolecular charge transfer (CT), leading to broadband dual fluorescence in highly polar solvents. Introduction of a weaker electron donor such as a benzocrown to the meso-position is not able to trigger a second (charge or electron transfer) process and, interestingly, heavy atom (iodine, PBDP-I derivative) substitution at that moiety does also not have a relevant influence on the photophysics, i.e., enhanced intersystem crossing was not observed. Electrochemical studies of PBDP-DMA complement the data reported and stress the fact that the decrease in fluorescence of PBDP-DMA in highly polar solvents is due to an excited-state CT process rather than to a photoinduced electron transfer (PET). KW - BODIPY dyes KW - Charge transfer KW - Fluorescence KW - Ring fusion PY - 2018 DO - https://doi.org/10.1016/j.jphotochem.2017.10.034 SN - 1010-6030 VL - 352 SP - 98 EP - 105 PB - Elsevier CY - Amsterdam AN - OPUS4-43100 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Empowering test strips for rapid, highly sensitive and multiplexed analysis of small molecule analytes at a point-of-need N2 - In particular, the rapid development of lateral flow assays as indispensable tools for everyone to contain the SARS-CoV-2 pandemic has fuelled the global demand for analytical tests that can be used outside dedicated laboratories. In addition to their use in medical diagnostics, rapid tests and assays have become increasingly important in various fields such as food safety, security, forensics, and environmental management. The advantage is obvious: taking the assay directly to the sample minimizes the time between suspicion and decision-making, allowing faster action. Especially today, when mobile communication devices with powerful computing capabilities and built-in cameras are ubiquitous, more people than ever before around the world have the basic skills to operate a powerful detector at their fingertips. This sets the stage for a much wider use of analytical measurements in terms of prognosis and prevention, enabling professional laypersons in particular. However, current strip-based systems are primarily focused on single parameter analysis, whether it is SARS-CoV-2 biomarkers, blood glucose levels, or lead concentrations in water samples. Industrial applications of such methods also often still rely on single-parameter assays, requiring multiple runs even for a limited number of key parameters. Overcoming these limitations depends on developing low-number multiplexing strategies that ensure robustness, reliability, speed, ease of use, and sensitivity. This lecture will give an overview of several generic approaches developed in recent years to address these challenges. It will highlight how the synergy of supramolecular (bio)chemistry, luminescence detection, hybrid (nano)materials and device miniaturization can result in powerful (bio)analytical assays that can be used at a point-of-need.1-5 Selected examples will introduce key aspects of such systems that include tailored signaling mechanisms and recognition elements, materials functionalization and device integration, including hybrid nanomaterials, gated indicator release systems, strip modification, and smartphone-based analysis. T2 - 15th Rapid Methods Europe Conference CY - Amsterdam, Netherlands DA - 06.11.2023 KW - Test strips KW - Lateral flow assays KW - Explosives KW - Pesticides KW - Rapid testing KW - Multiplexing PY - 2023 AN - OPUS4-58816 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - Rational Design of Analyte-responsive Fluorescent Particle Sensors for Life Sciences Applications N2 - Engineered and tailor-made nanomaterials (NM) are of increasing relevance for current and future developments in the life and material sciences for applications, e.g., as drug carriers, fluorescent sensors, and multimodal labels in bioanalytical assays, and reporters for imaging applications. For instance, NM-based reporters and sensors, that are labelled or stained with a multitude of conventional or sensor dyes, have several advantages as compared to molecular probes like enhanced brightness, i.e., amplified signals, ease of designing ratiometric systems by combining analyte-sensitive and inert reference dyes, and increased photostability. Moreover, this can enable the use of hydrophobic dyes in aqueous environments. For rational NM design, choosing and tailoring the intrinsic physicochemical properties, such as particle size, size distribution, morphology, and surface chemistry of the NM application-specific considerations like biocompatibility, ease and low cost of preparation, and colloidal stability and performance in the targeted environment must be considered. In this lecture, different design concepts of inorganic, organic, and hybrid NM and microparticles with hydrophilic surface chemistries and different functionalities are presented that can be used for the targeting of lysosomes; and to monitor functional parameters of endo-lysosomal compartments, like pH or enable oxygen sensing. T2 - Chemical Probes for Lysosomal Biology CY - York, United Kingdom DA - 09.09.2024 KW - Luminescence KW - Quantification KW - Nano KW - Particle KW - Quality assurance KW - Fluorescence KW - Method KW - Uncertainty KW - Reference material KW - Sensor KW - Synthesis KW - Dye KW - pH KW - Silica KW - Polystyrene KW - Surface analysis PY - 2024 AN - OPUS4-62173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heller, Benedikt T1 - Reaction-based detection of cyanide anions using a non-fluorescent polymer via “turn-on” fluorescence N2 - Cyanide is known to be a very hazardous and toxic substance. Through the binding to cytochrome oxidase it inhibits the oxygen utilization in cells. The LD50 of cyanide is as low as 1.0 mg/kg. Therefore it is inalienable to develop sensing methods to detect cyanide with a very high selectivity and sensitivity. In our group we developed a non-fluorescent monomer which is able to detect cyanide-anions with very high selectivity and sensitivity based on a “turn-on” fluorescence method. As cyanide-source we used tetrabutylammoniumcyanide (TBAC). Using an excitation wavelength of 600 nm the increase in fluorescence at 642 nm is strictly selective with cyanide-anions. Different anions like fluoride, hydroxide or acetate show no increase at all. With this new detection system, concentrations as low as 1.6 nM can be detected. T2 - Europ(t)rode 2018 CY - Naples, FL, USA DA - 25.03.2018 KW - Cyanide detection KW - Fluorescence KW - Optical sensing PY - 2018 AN - OPUS4-45663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mekonnen, Tessema Fenta A1 - Panne, Ulrich A1 - Koch, Matthias T1 - Electrochemistry coupled online to liquid chromatography-mass spectrometry for fast simulation of biotransformation reactions of the insecticide chlorpyrifos N2 - An automated method is presented for fast simulation of (bio)transformation products (TPs) of the organophosphate insecticide chlorpyrifos CPF)based on electrochemistry coupled online to liquid chromatography-mass spectrometry (EC-LC-MS). Oxidative TPs were produced by a boron doped diamond (BDD) electrode, separated by reversed phase HPLC and online detected by electrospray ionization-mass spectrometry (ESI-MS). Furthermore, EC oxidative TPs were investigated by HPLC-tandem mass spectrometry (LC-MS/MS) and FT-ICR high resolution mass spectrometry (HRMS) and compared to in-vitro assay metabolites (rat and human liver microsomes). Main phase I metabolites of CPF: chlorpyrifos oxon (CPF oxon), trichloropyridinol (TCP), diethylthiophosphate (DETP), diethylphosphate (DEP), desethyl chlorpyrifos (De-CPF), and desethyl chlorpyrifos oxon (De-CPF oxon), were successfully identified by the developed EC-LC-MS method. The EC-LC-MS method showed similar metabolites compared to the in-vitro assay with possibilities of determining reactive species. Our results reveal that online EC-(LC)-MS brings an advantage on time of analysis by eliminating sample preparation steps and Matrix complexity compared to conventional in-vivo or in-vitro methods. KW - Organophosphate agrochemicals KW - Electrochemical oxidation KW - Metabolism KW - In vitro KW - EC-LC-MS KW - LC-MS/MS PY - 2017 DO - https://doi.org/10.1007/s00216-017-0277-y SN - 1618-2642 SN - 1618-2650 VL - 409 IS - 13 SP - 3359 EP - 3368 PB - Springer CY - Berlin Heidelberg AN - OPUS4-40179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Chips or strips – the importance of embedding and integration in (bio)chemical assay development N2 - The most important aspect of developing a miniaturized or compact (bio)chemical assay for use outside a dedicated laboratory environment is, of course, the design of the recognition and signaling element that best achieves the required selectivity and sensitivity in relation to the target analyte and analytical scenario. For luminescence assays, this essentially means that the appropriate combination of small-molecule binding units, ligands or biomacromolecular binders such as antibodies or aptamers and organic, metal-organic or rare earth metal ion luminophores or luminescent nanoparticles such as semiconductor nanocrystals, carbon nanodots, polymer dots or fluorescently doped silica or polymer nanoparticles as well as the best strategy for combining binding and signaling unit must be selected. Having accomplished this task and obtained first promising results in a conventional laboratory setting with the use of pipettes, cuvettes and benchtop spectrometers, the challenge is to bridge the gap between such a model assay and an assay that uses a mobile and robust device in the hands of a layperson and does not require complicated operation and extensive manual steps, especially when handling liquids, at best in line with the ASSURED principle, being affordable, sensitive, specific, user-friendly, rapid and robust, equipment free and deliverable to end-users, or, as recently proposed, the REASSURED principle, which furthermore includes real-time connectivity and ease of specimen collection (translating into ease of sampling in the non-diagnostic world). In order to close this gap, it is of utmost importance to know the further requirements of the assay, i.e., whether only one or more than one analyte needs to be detected, what the main potential interferents are and how tolerant the assay is to the sample matrix, as well as how many assays are typically performed per hour/day/week, how long a run should take and how expensive a single analysis should be. These parameters usually determine the most appropriate format, i.e., whether it is a dip stick, a test strip, a lateral flow assay, a microfluidic chip, a 3D-microfluidic approach or a combination thereof, in conjunction with a dedicated readout system or a mobile communication device. This choice in turn determines the most appropriate strategy for integration, i.e., whether the recognition and signaling element are used directly in liquid solution,8 embedded in polymer layers or gels, attached to surfaces of planar substrates, micro- or nanoparticles or immobilized or loaded in micro- or nanoparticles, which could then enable direct or controlled/gated access. This contribution discusses various aspects of this multi-stage process using examples from the group. T2 - How to develop a sensor? Academic Approaches vs. Industrial Interests (EU Training School) CY - Kaiserslautern, Germany DA - 18.09.2024 KW - Sensing KW - Rapid testing KW - Microfluidics KW - Test strips KW - Device integration PY - 2024 AN - OPUS4-61429 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Biyikal, Mustafa A1 - Rurack, Knut T1 - Development of a Lab-on-a-Chip for the Detection of Nerve Agents with a Handheld Device N2 - The development of a Lab-on-a-Chip (LoC) is presented, which can detect reactive phosphorous compounds in the gas phase in combination with an optochemical hand-held sensor. The LoC prototype contains three pairs of sensing materials containing fluorescent indicator dyes in various carrier materials. By measuring the fluorescence response to phosphoryl chloride, a surrogate compound, the detection of chemical warfare agents (CWAs) in gas phase becomes possible within seconds, introducing a novel approach to CWA detection. T2 - 2023 IEEE SENSORS Conference CY - Vienna, Austria DA - 29.10.2023 KW - Lab-on-a-Chip KW - Nerve agents KW - Hand-held KW - Fluorescence KW - Toxic industrial chemicals PY - 2023 UR - https://ieeexplore.ieee.org/document/10325263 SN - 979-8-3503-0387-2 DO - https://doi.org/10.1109/SENSORS56945.2023.10325263 SP - 1 EP - 4 PB - IEEE CY - New York AN - OPUS4-59367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Integrating BODIPY Probes with Devices for On-site Sensing Applications N2 - The detection of potential contaminants as early as possible and as close to their point of emission as well as immission is becoming increasingly important in contemporary environmental analytical chemistry. In addition, real-time monitoring of important chemical parameters for process control is strongly gaining relevance within the context of Industry 4.0. Not only is the development of powerful optical probes thus necessary but also their integration into a matrix and/or device that allows for the application of such systems in realistic measurement scenarios. Integrating fluorescent probes with sensing matrices, however, presents a major challenge because usually, when confined in a rather rigid matrix, fluorophores tend to behave completely different than for instance in the molecular state in solution. The present contribution will highlight recent examples of successful integration of BODIPY (boron–dipyrromethene) based probes with devices that have been developed in our group. A simple system utilizing a test strip for direct readout with a conventional miniaturized camera as for instance routinely used in smartphones was recently devised by us for the determination of organophosphate nerve or chemical warfare agents (CWAs) Sarin (GB), Soman (GD), and Tabun (GA) in aqueous environments. Here, we coupled a reactive BODIPY to the inner and outer surface of mesoporous silica nanoparticles. In the presence of CWAs, the reactive BODIPY dye with an optimally positioned hydroxyl group undergoes an acylation reaction, yielding a bicyclic product that is non-emissive. The strong fluorescence quenching response allows reaching LODs in the pM range in natural waters. Steric embedding, again relying on test strip analysis in combination with a smartphone-based readout and data processing, was sufficient to create a reusable optical pH stick. The family of pH-responsive fluorescent BODIPY probes used for this purpose has been designed in a rational manner with the aid of quantum chemistry tools. All the probes display very similar spectroscopic properties with ON−OFF fluorescence switching responses, being retained after embedding of the probes into hydrogel sensor spots on a plastic strip. Dispensing with a matrix yet invoking microfluidic chips finally permits to use a highly sensitive boronic acid-functionalized BODIPY probe for in-line sugar analysis for instance in the beverage industry. Placement of an amino group in direct neighbourhood of the boronic acid moiety yielded a broad working range at neutral pH while meeting the desired sensitivity in the micro-molar range due to a pronounced analyte-induced fluorescence increase, guaranteeing the straightforward detection of sugar in (coloured) sodas without sample clean-up. T2 - 10th International Conference on Porphyrins & Phthalocyanines CY - Munich, Germany DA - 01.06.2018 KW - BODIPY dyes KW - Nerve agents KW - PH KW - Sugars KW - Devices KW - Fluorescence sensing PY - 2018 AN - OPUS4-45642 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter A1 - Schneider, Rudolf T1 - A wash-free, multiplex microbead assay for determination of emerging bioactive compounds in wastewater N2 - Pollutants of low molecular weight, such as drug residues, are in the focus of water quality assessment: some of them, like carbamazepine are only partially degraded in wastewater treatment plants. Thus, these pollutants can serve as marker substances for elimination efficiencies. Monitoring water quality demands for selective, high-throughput and multi-target analytical methods. Immunoassays, such as ELISA, offer the possibility to be highly sensitive and selective due to the specific recognition by high affinity of target molecules to antibodies (Abs). Batch-wise processing in microtiter plates allows for the necessary high-throughput, however only a single analyte can be determined within one measurement. To overcome these disadvantages, we developed a four-plex microbead-based flow cytometric assay, which is adaptable for the microtiter plate format. The modular and self-prepared bead support consists of polystyrene-core/silica-shell particles. While, the polystyrene core is used for encoding, by introducing different amounts of fluorescent dyes, the silica shell creates a solid support for the immunoassay: The target analytes, three drugs, carbamazepine, diclofenac and caffeine and the fecal marker isolithocholic acid are coupled covalently to the surface via NHS chemistry to amino groups on the surface. For determination of the pollutants, a mixture of specific Abs is incubated with the samples, to bind competitively on the “anchor” molecules on the surface of the beads or the analyte in solution. Bound antibodies are then visualized via fluorescent dye-labelled secondary Abs. Flow-cytometry allows for decoding of the beads and signal read-out, without washing the system. In order to decrease non-specific binding, we investigated different types of surface modifications, finding, that a PEG-based surface is suitable to support our immunoassay format. For maximum sensitivity, a design-of-experiment approach was chosen for optimization of the assay parameters. The resulting immunoassay is appropriate to quantify the pollutants in the low μg/L-range. T2 - EBS 2017 CY - Potsdam, Germany DA - 20.03.2017 KW - Immunoassay KW - Bead-based assay KW - Flow-cytometry PY - 2017 AN - OPUS4-39522 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - PE-Rezyklat Einsatz in Gefahrgutbehältern? N2 - In diesem Vortrag geht es darum zu beschreiben, ob Rezyklat für PE Behälter gefüllt mit Gefahrgut Anwendung finden darf. Kanister aus Neuware und Rezyklat wurden verschiedenen Untersuchungen unterzogen. Es wurde der Feststoff und Leachable getestet. Methoden sind TED-GC/MS und GC-HRMS. Proben der Leachable wurden nach 1 und 4 Wochen genommen und die Peakanzahl vergleichen dargestellt. Als Lösemittel wurden Wasser, Ethanol, EtOAc, Ammoniak und HNO3 verwendet. T2 - Fachaustausch Projekt GeSKAR CY - Dessau, Germany DA - 10.01.2025 KW - Gefahrgutbehälter KW - Rezyklat PY - 2025 AN - OPUS4-62396 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bell, Jérémy T1 - Phosphorylated amino acids detection and extraction combining fluorogenic MIP core-shell particles and microfluidics N2 - The identification and quantification of phosphorylated amino acids, peptides and proteins is one of the key challenges in contemporary bioanalytical research, noteworthy to diagnose and treat diseases at an early stage. Small sensing devices like microfluidic chips combined with “smart” detection chemistry and simple data assessment, processing and presentation are attractive in this regard. We developed novel synthetic probes, targeting phosphorylated amino acids, based on core-shell microparticles consisting of a silica core coated with a molecularly imprinted polymer shell (MIP). These “plastic antibodies” which are extremely robust, resist denaturing solvents and high temperatures, can be reproducibly produced at low cost, can potentially overcome many of the problems in the current detection strategies. The MIP layer, containing a fluorescent probe monomer, responds to phosphorylated amino acids such as phosphorylated tyrosine (pTyr) with a significant imprinting factor, i.e. selectivity, higher than 3.5, and a “lighting-up” of its fluorescence accompanied by the development of a strongly red-shifted emission band. The bead-based ratiometric detection scheme has also been successfully transferred to a microfluidic chip format to demonstrate its applicability to rapid assays. Such a device could yield an automated pTyr measurement system in the future. The setup was built by coupling a PDMS/Teflon/glass microfluidic chip with an optical setup for fluorescence measurements able to extract and monitor pTyr concentration from 0.5–200 μM. T2 - International Conference on "Instrumental Methods of Analysis: Modern Trends and Applications", IMA 2017 CY - Heraklion, Greece DA - 17.09.2017 KW - Microfluidics KW - MIP KW - Fluorescence KW - Amino acids PY - 2017 AN - OPUS4-42456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Herausforderungen und Möglichkeiten bei der Beantragung von Drittmitteln N2 - Die Einwerbung von Drittmitteln wird immer mehr zur zwingenden Notwendigkeit, wenn man Forschung betreiben möchte. Drittmittel sorgen nicht dafür, dass man zusätzliches Geld für die Forschung ausgeben kann, wie das früher einmal der Fall war, sie werden mehr und mehr zur Grundbedingung für Forschung überhaupt. Zu den Drittmitteln zählen insbesondere Projektmittel der Forschungsförderung des Bundes, der Länder, der EU und anderer öffentlicher Stellen, der Wirtschaft zur Durchführung von Forschungsaufträgen sowie der Deutschen Forschungsgemeinschaft. Sie machen bereits einen entscheidenden Teil des Budgets von Universitäten (25-30%, Tendenz steigend) und Forschungseinrichtungen aus. In den Präsidien und Rektoraten werden Stabsstellen eingerichtet, um mögliche Fördertöpfe zu finden und erfolgreiches Formulieren von Anträgen zu unterstützen und die Formalien der Antragstellung zu optimieren. Je mehr Drittmittel eine Einheit einwirbt, mit umso mehr Grundmitteln darf sie rechnen. Dem hohen Zeitaufwand der Wissenschaftler für das Schreiben von Anträgen stehen jedoch immer niedrigere Bewilligungsquoten gegenüber. Sehr umfangreiche Projekte mit sehr vielen Partnern scheinen immer schwieriger zu begründen zu sein. Lange Bearbeitungszeiten bis zur Bewilligung von Projekten und Laufzeiten von 4 Jahren stehen im Widerspruch zu den Planungszeiträumen für Forschungsprojekte im Industrielabor. Im Zeichen immer stärker geforderter Interdisziplinarität müssen andere Wege gefunden werden, um die Stärken einer Messtechnik überzeugend einzubringen. Was ist zu tun? In diesem Diskussionsbeitrag werden Informationen zusammengetragen, um Fördermöglichkeiten der Grundlagenforschung und Applikationen von GD-techniken auszuloten und die Kooperation von Forschungseinrichtungen und Industriepartnern praktikabel zu realisieren. T2 - Anwendertreffen "Analytische Glimmentladungsspektroskopie" CY - Bremen, Germany DA - 16.05.2017 KW - Drittmittel PY - 2017 AN - OPUS4-46219 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Chemometrical analysis of spectral data obtained from glow discharge optical emission spectroscopy for elemental analysis of metals N2 - The poster shows the combination of GD-OES and machine learning. The gola of this project is to establish a new and robust calibration model, which can be used to identify elemental composition and concentration of metals from a single spectra. T2 - Salsa make and measure Konferenz CY - Online meeting DA - 16.09.2021 KW - Glow discharge optical emission spectroscopy KW - Machine learning PY - 2021 AN - OPUS4-53323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bell, Jérémy A1 - Biyikal, Mustafa A1 - Rurack, Knut T1 - Embedded sensor based on tandem smartphone-microfluidic device for the detection of TNT in surface and sea waters N2 - The globe's seas were used as dumping ground after the world wars and those millions of ammunition, most of all containing 2,4,6-trinitrotoluene (TNT), represent a pressing danger for fishermen, dredging operations, submarine cable installations and tourism. We developed an extremely selective indication method for TNT based on a specific reaction that produces a highly fluorescent compound. The indication system was integrated into a microfluidic PDMS chip for the solid-liquid extraction of TNT from water samples, offering environmental monitoring possibilities. Combining the advantages of a light-up indicator, microfluidics and a smartphone as detector, the embedded sensor allows for the remote and rapid detection of TNT down to ng in surface and sea waters. T2 - µTAS 2020 CY - Online meeting DA - 05.10.2020 KW - Smartphone KW - Rapid test KW - TNT KW - Ammunition KW - Schnelltest KW - Munition PY - 2020 AN - OPUS4-51444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Li, X.Q. A1 - Li, H.M. A1 - Jiao, H. A1 - Guo, Z.H. A1 - Zhang, Q.H. A1 - Kneeteman, L.E. A1 - Lewin, M. A1 - Pires do Rego, E.C. A1 - Leal, R.V. A1 - Violante, F.G.M. A1 - Riedel, Juliane A1 - Koch, Matthias T1 - CCQM Key Comparison track A CCQM-K168: Non-polar analytes in high carbohydrate food matrix: trans-zearalenone in maize powder N2 - Demonstrating competency and equivalence for the measurement capacity of contaminants and nutrients in primary foodstuffs is a priority of the OAWG 10-year strategy for Track A core comparisons. Such measurements have posed significant challenges for reference material producers and calibration service providers. This key comparison (KC), under the topic of “non- polar analyte in high carbohydrate food matrix: trans-Zearalenone (trans-ZEN) in maize powder” , was a sector of the model system selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to demonstrate the Calibration and Measurement Capabilities (CMCs) of national metrology institutes (NMIs) and designated institutes (DIs). 17 NMIs and DIs participated in the Track A KC CCQM- 168 “non-polar analyte in high carbohydrate food matrix: trans-ZEN in maize powder” . Participants were requested to evaluate the mass fraction (μg/kg) of trans-ZEN in maize powder material. Methods like liquid-liquid extraction and SPE were applied in the pre-treatment, and HPLC-MS/MS and HPLC-FLD were used for detection by the participants. The mass fractions for trans-ZEN were in the range of (91.8 to 169) μg/kg with standard uncertainties of (1.5 to 24.7) μg/kg, and corresponding relative standard uncertainties from 1.5% to 14.6%. Two labs, INTI and BAM were excluded from the KCRV evaluation. INTI result was identified as an outlier and confirmed their method had insufficient specificity. For BAM the calibration approach they used does not meet the CIPM traceability requirements. The other 15 labs included in the calculation of the consensus KCRV all agreed within their standard uncertainties. Hierarchical Bayes was used as estimators in calculating KCRV and standard uncertainty. Successful participation in CCQM-K168 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 1 μg/kg to 1000 μg/kg in a high carbohydrate food matrix. KW - Metrology KW - Quality Assurance KW - Mycotoxin Analysis KW - Sustainable Food Safety PY - 2023 DO - https://doi.org/10.1088/0026-1394/60/1A/08021 VL - 60 IS - 1a SP - 08021 AN - OPUS4-59059 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wagner, Sabine A1 - Bell, Jérémy A1 - Biyikal, Mustafa A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Integrating fluorescent molecularly imprinted polymer (MIP) sensor particles with a modular microfluidic platform for nanomolar smallmolecule detection directly in aqueous samples N2 - Fluorescent sensory MIP (molecularly imprinted polymer) particles were combined with a droplet-based 3D microfluidic system for the selective determination of a prototype small-molecule analyte of environmental concern, 2,4-dichlorophenoxyacetic acid or 2,4-D, at nanomolar concentration directly in water samples. A tailor-made fluorescent indicator cross-linker was thus designed that translates the binding event directly into an enhanced fluorescence signal. The phenoxazinone-type cross-linker was co-polymerized into a thin MIP layer grafted from the surface of silica microparticles following a RAFT (reversible addition-fragmentation chain transfer) polymerization protocol. While the indicator cross-linker outperformed its corresponding monomer twin, establishment of a phase-transfer protocol was essential to guarantee that the hydrogen bond-mediated signalling mechanism between the urea binding site on the indicator cross-linker and the carboxylate group of the analyte was still operative upon real sample analysis. The latter was achieved by integration of the fluorescent core-shell MIP sensor particles into a modular microfluidic platform that allows for an in-line phasetransfer assay, extracting the analyte from aqueous sample droplets into the organic phase that contains the sensor particles. Real-time fluorescence determination of 2,4-D down to 20 nM was realized with the system and applied for the analysis of various surface water samples collected from different parts of the world. KW - Molecular imprinting KW - Microfluidics KW - Fluorescence KW - Core-shell particles KW - Droplets PY - 2018 DO - https://doi.org/10.1016/j.bios.2017.07.053 SN - 0956-5663 VL - 99 IS - 1 SP - 244 EP - 250 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-42258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mansurova, Maria A1 - Gotor, Raúl A1 - Johann, Sergej A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias A1 - Rurack, Knut A1 - Bell, Jérémy T1 - Fluorescent Hydrophobic Test Strips with Sterically Integrated Molecular Rotors for the Detection of Hydrocarbons in Water and Soil with an Embedded Optical Read-Out N2 - Contamination of natural bodies of water or soil with oils and lubricants (or generally, hydrocarbon derivatives such as petrol, fuels, and others) is a commonly found phenomenon around the world due to the extensive production, transfer, and use of fossil fuels. In this work, we develop a simple system for the on-field detection of total petroleum hydrocarbons (TPHs) in water and soil. The test is based on the measurement of the fluorescence signal emitted by the molecular rotor 2-[ethyl[4-[2-(4-nitrophenyl)ethenyl]phenyl]amino]ethanol (4-DNS-OH). This dye is embedded in a hydrophobic polymeric matrix (polyvinylidene fluoride), avoiding interactions with water and providing a robust support for use in a test strip fashion. Together with the strips, an embedded optical system was designed for fluorescence signal read-out, featuring a Bluetooth low-energy connection to a commercial tablet device for data processing and analysis. This system works for the detection and quantification of TPHs in water and soil through a simple extraction protocol using a cycloalkane solvent with a limit of detection of 6 ppm. Assays in surface and sea waters were conclusive, proving the feasibility of the method for in-the-field operation. KW - Test strip KW - Sensor KW - Smartphone KW - Fluorescence KW - Test Streifen KW - Sensoren KW - Fluoreszenz KW - Petrol KW - Öl PY - 2023 DO - https://doi.org/10.1021/acs.energyfuels.3c01175 SN - 0887-0624 SP - 1 EP - 6 PB - American Chemical Society CY - Washington, United States AN - OPUS4-57892 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Sensitive and multiplexed assays for point-of-need applications: innovations for robust, reliable, and user-friendly diagnostics N2 - The development of portable analytical assays, particularly during the SARS-CoV-2 pandemic, has revolutionized diagnostics and expanded their use to areas such as food safety, environmental monitoring and forensics. These assays offer the advantage of rapid on-site decision making without the need for laboratory facilities. The omnipresence of mobile devices with advanced cameras and processing power further increases their usability. However, most current assays are limited to detecting single parameters. The challenge now is to develop robust multiplexed assays that can simultaneously detect multiple parameters with high sensitivity. This lecture will present generic approaches developed at BAM with a focus on supramolecular chemistry, luminescence detection, nanomaterials and miniaturization of devices. Examples include mesoporous nanomaterials, gated indicator systems, imprinted polymers, microfluidic devices, test strips and smartphone-based analysis. T2 - Kolloquium Optische Technologien der FH Münster CY - Steinfurt, Germany DA - 18.12.2024 KW - Rapid testing KW - Fluorescence KW - Explosives KW - Environmental contaminants KW - Multiplexing PY - 2024 AN - OPUS4-62322 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zhang, Y. T1 - Fluorescent molecularly imprinted polymers (MIPs) as novel tools for detection of sialic acid on tumor cells N2 - Cancer is the second leading cause of death globally according to the WHO 2018. Lung, prostate, colorectal, stomach and liver cancer are the most common types of cancer in men, while breast, colorectal, lung, cervix and thyroid cancer are the most common among women. Sialic acid (SA) plays an important role in a variety of biological processes in cells. Tumor cells express high levels of SA, which is often associated with poor prognosis due to increased invasive potential. In this study, we have performed a screening of SA-MIPs binding to different cancer cell lines. The overall aim is to use the SA-MIPs for detection of tumor cells, analyzed by flow cytometry and fluorescence microscopy. To confirm the levels of SA expression on the investigated cell lines, we started out by analyzing the binding of the lectins MAL I and SNA. The staining pattern of the two lectins binding to either α-2,3 or α-2,6 linkage SA, respectively, was compared with the staining pattern of the SA-MIPs. We show that the different cell types analyzed have a varying pattern of SA-MIP binding. The comparison with lectin binding will be further evaluated. T2 - Biomarkers – methods and technologies CY - Malmö, Sweden DA - 25.10.2018 KW - Cancer KW - Sialic acid KW - MIPs PY - 2018 AN - OPUS4-46492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Russo, Francesco Friedrich T1 - Upscaling of spectral libraries for HR- EI-MS based non target analytics N2 - Non-target (NT) mass spectrometry techniques play a crucial role in metabolomics applications, particularly in areas such as environmental safety. Soft ionization methods, such as electrospray ionization (ESI), are commonly employed due to their ability to generate spectra containing molecular ions, aiding in the identification of unknown peaks. However, ESI may fail to ionize certain compounds effectively, resulting in their absence in NT approaches. In contrast, hard ionization methods like electron impact (EI) can ionize a wide range of compounds but often lack information about the molecular ion. Although extensive databases of EI spectra exist, their nominal mass resolution (NR) limits their utility for modern high-resolution (HR) EI mass spectrometers. Here, the often-applied conversion of HR spectra to nominal mass leads to the loss of unique characteristics, i.e. by grouping distinct masses into more ambiguous nominal masses. Our study aims to (i) quantify the negative impact of such a binning approach and (ii) develop a machine learning (ML) tool capable of enhancing existing nominal mass spectral libraries. In the initial phase, we employed the RECETOX Exposome HR-[EI+]-MS library to assess the influence of HR spectra on identification. We compared the dot product of each spectrum against all others, utilizing bin sizes of 0.001 and 1 Da. The difference in dot product between the second-best candidate and the query spectrum (the best candidate, with a score of 1) was calculated for both HR and nominal mass spectra. Subsequently, we explored the application of ML techniques to predict HR spectra from nominal mass spectra using the before mentioned dataset. Preliminary findings demonstrate the potential of high-resolution spectral libraries. As anticipated, HR spectra consistently exhibited lower similarity scores for the second candidate. This observation likely stems from the high redundancy and resulting ambiguity associated with nominal masses. Even after eliminating spectra containing multiple HR masses mapped to the same nominal mass, the aforementioned trend persisted. Furthermore, initial investigations into ML have revealed its ability to predict up to 40% of HR masses within a 10 mDa precision window. T2 - Tag der Chemie 2023 CY - Berlin, Deutschland DA - 05.07.2023 KW - HR-EI-MS KW - ML PY - 2023 AN - OPUS4-58172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - You, Zengchao T1 - Detection of aluminum deposition on the cathodes of aged lithium ion batteries by GD-OES N2 - The use of renewable energy sources, electromobility, and portable electronics relies on lithium-ion batteries (LIBs). However, one detrimental effect, which can result in significant performance loss, is the corrosion of the current collectors caused by the aging mechanisms, especially in high-energy-density batteries Glow discharge optical emission spectroscopy (GD-OES) provides depth profile analysis through sputtering using argon plasma, which enables the analysis of the corrosion behavior at different depths of the cathodes. T2 - GD-OES Anwendertreff CY - Dresden, Germany DA - 26.27.2022 KW - glow KW - discharge KW - optical KW - emission KW - spectroscopy PY - 2022 AN - OPUS4-56105 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Biyikal, Mustafa A1 - Gawlitza, Kornelia A1 - Dropa, T. A1 - Urban, M. A1 - Costero, A. M. A1 - Martínez-Mánez, Ramon A1 - Rurack, Knut T1 - Determination of the chemical warfare agents Sarin, Soman and Tabun in natural waters employing fluorescent hybrid silica materials N2 - A novel mesoporous silica material containing boron–dipyrromethene (BODIPY) moieties (I) is employed for the detection of nerve agent simulants (NASs) and the organophosphate nerve or chemical warfare agents (CWAs) Sarin (GB), Soman (GD), and Tabun (GA) in aqueous environments. The reactive BODIPY dye with an optimum positioned hydroxyl group undergoes acylation reactions with phosph(on)ate substrates, yielding a bicyclic ring. Due to aggregation of the dyes in water, the sensitivity of the free dye in solution is very low. Only after immobilization of the BODIPY moieties into the silica substrates is aggregation inhibited and a sensitive determination of the NASs diethyl cyanophosphonate (DCNP), diethyl chlorophosphate (DCP) and diisopropyl fluorophosphate (DFP) possible. The signaling mode is a strong quenching of the fluorescence, reaching LODs in the pM range. The best performing hybrid material was singled out from a library of hybrid silicas varying in morphology and surface functionalization. The response to actual CWAs such as GB, GD, and GA has also been tested, offering similar behavior as for the simulants. The proposed reaction mechanism has been verified by investigation of other model materials, containing for instance BODIPY moieties without an optimum hydroxyl group (III) or a BODIPY dye with an all-aliphatic counterpart (IV). The latter can only form a monocyclic reaction product, showing much less reactivity as I. Assays with other possible competitors have been additionally carried out, showing favorably low cross-reactivities. Finally, the determination of NASs in several natural waters has been demonstrated. KW - Nerve agent simulants KW - Mesoporous silica materials KW - Fluorescence detection PY - 2017 UR - http://www.sciencedirect.com/science/article/pii/S0925400517303428 DO - https://doi.org/10.1016/j.snb.2017.02.115 SN - 0925-4005 VL - 246 SP - 1056 EP - 1065 PB - Elsevier B.V. AN - OPUS4-39739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jiang, Shan T1 - Carbon Nanodots (CNDs) Doped Molecularly Imprinted Polymers (MIPs) for Tumor- Associated Glycan Imaging N2 - Glycosylation is heavily altered in tumor cells compared with healthy cells, because of the different levels of expression of glycosyltransferases, glycosidases and monosaccharide transporters within a cancerous microenvironment. 1 Tumor-associated glycans, especially sialic acid (SA) conjugates, which are good candidates of tumor markers, can be used for Cancer early diagnosis. 2 However, studies on SA-binding lectins demonstrate that the type of SAlinkage and the glycosylation position of carbohydrate can greatly influence the affinity. 3 Therefore, there is a need for diagnostic tools owning high specificity and strong affinity to analyze and determine SA glycosylation motifs. 4 Herein, we report the development of fluorescent core/shell/shell nanoparticles where the outermost layer is a thin molecularly imprinted polymer (MIP) film binding to tumor cells in vitro by targeting cell surface SA. The core is made of N-doped red carbon nanodots (R-CNDs) which were prepared by hydrothermal synthesis, emitting intense red fluorescence under fluorescence microscopy imaging conditions. Silica coating of R-CNDs was achieved by a microemulsion method, resulting in ca. 40 nm large silica-coated CNDs (named R-CSNs). Finally, a thin MIP-shell was accomplished by using a combination of non-fluorescent monomer (3), functional monomers (1, 2) and cross-linker (EGDMA) for polymerization (Figure 1). Transmission electron microscopy (TEM) is used for structural characterization of the formation of MIP layer, and the results of cell-based binding tests show a promising binding affinity of MIPs to tumor cells, allowing a relatively robust, specific and rapid analytical method for cancer biopsies. T2 - GSSMIP2019 CY - Berlin, Germany DA - 28.08.2019 KW - MIP KW - Carbon Nanodots KW - Glycan PY - 2019 UR - https://sites.google.com/view/gssmip2019/gss-mip-2019 AN - OPUS4-49252 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Epping, Ruben T1 - Aroma Sensing of Truffles N2 - The aim of this project is to develop a mobile technical device to search for truffles. This way, truffles can be harvested faster, cheaper and more efficiently compared to the current method using dogs. For this purpose, suitable marker substances in the aroma of ripe truffles were identified using analytical-chemical methods. The collected data was used to create aroma profiles of different truffle species. The specificity of possible marker substances was confirmed with a truffle dog study. The hypothesis “If trained truffle dogs recognize the substances as supposed truffles in the context of an experiment, they can be regarded as specific” was made. The results show that the truffle aroma is mainly characterized and perceived by dogs by dimethyl sulfide and dimethyl disulfide. For the concentration measurement of these markers in the ambient air, we are currently building our own detector. The Challenge is to get a fast measurement with a very low limit of detection at the same time. The device will resemble a metal detector in terms of shape and handling and be particularly suitable for mobile use. The R&D cooperation project between the Federal Institute for Materials Research and Testing (BAM) and sglux GmbH thus enables truffles to be harvested professionally and systematically. This brings the technical advances that have revolutionized agriculture over the last hundred years to truffle cultivation for the first time. T2 - Adlershofer Forschungsforum CY - Berlin, Germany DA - 11.11.2022 KW - Truffle KW - Volatile organic compounds KW - Gas chromatography KW - Canine olfactometry PY - 2022 AN - OPUS4-56301 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Agudo Jácome, Leonardo A1 - Manzoni, Anna Maria T1 - Elementverteilung in Hochentropiewürfelchen N2 - Seit Beginn der Luftfahrt Anfang des letzten Jahrhunderts ist die Menschheit auf der Suche nach neuen Materialien, die das Abenteuer Fliegen sicherer, angenehmer, schneller und rentabler gestalten. Hochentropielegierungen sind solche vielversprechenden Materialien. Die richtige Analytik hilft dabei, besser zu verstehen, wie deren Zusammensetzung und atomare Anordnung die makroskopischen Eigenschaften beeinflusst. KW - Chemically complex alloy KW - Transmissionselektronenmikroskopie KW - Energiedisersive Röntgenspektroskopie PY - 2022 UR - https://www.gdch.de/fileadmin/downloads/Netzwerk_und_Strukturen/Fachgruppen/Analytische_Chemie/Mitteilungsblatt/Internet_AC04-2022.pdf SN - 0939-0065 IS - 4 SP - 12 EP - 14 PB - Gesellschaft Deutscher Chemiker CY - Frankfurt, Main AN - OPUS4-56699 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sarma, Dominik A1 - Mielke, Johannes A1 - Sahre, Mario A1 - Beck, Uwe A1 - Hodoroaba, Vasile-Dan A1 - Rurack, Knut T1 - TSEM-based contour analysis as a tool for the quantification of the profile roughness of silica shells on polystyrene core particles N2 - Core-shell (CS) particles with a polymeric core and a silica shell play an important role in the materials and (bio)analytical sciences. Besides the establishment of reliable synthesis procedures, comprehensive particle characterization is essential for batch-to-batch reproducibility and objective performance assessment across architectures, protocols, and laboratories. Particle characterization with respect to size, size distribution, shell thickness and texture, surface area and roughness or materials composition is commonly conducted with different analytical methods, often on different samples. Our approach uses a dual-mode TSEM/SEM set-up with an EDX detector to obtain a complementary data set with sufficient statistical confidence of one and the same sample on a single instrument. Our protocol reveals information about size, size distribution and shell thickness of the various particles employed from overview images, while an increased field of view (FOV) and high-resolution EDX analysis yields detailed information on shell texture and elemental composition. An image analysis tool was developed to derive and quantify the profile roughness of CS particles from individual beads. Comparison with surface roughness data from AFM showed a similar trend in roughness across the series of particles. Reliable classification into smooth and rough is proposed and roughness changes within different particle batches were tracked systematically. KW - Core-shell particles KW - Electron microscopy KW - Transmission mode KW - Roughness KW - Image analysis PY - 2017 DO - https://doi.org/10.1016/j.apsusc.2017.07.099 SN - 0169-4332 SN - 1873-5584 VL - 426 IS - 1 SP - 446 EP - 455 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-42256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Koch, Matthias A1 - Wise, S. A. A1 - Panne, Ulrich T1 - Fifteenth international symposium on biological and environmental reference materials (BERM-15) N2 - The 15th International Symposium on Biological and Environmental Reference Materials (BERM-15), organized by BAM, took place at in Berlin in September 2018. An overview on main topics of the conference is given. KW - BERM KW - Reference materials PY - 2019 DO - https://doi.org/10.1007/s00769-019-01377-9 SN - 1432-0517 SN - 0949-1775 VL - 24 IS - 3 SP - 249 EP - 250 PB - Springer Verlag AN - OPUS4-48203 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matiushkina, Anna T1 - Quantification of Citrate Ligands on the Surface of Nanoparticles N2 - In this study, different methods for determining nanoparticle surface ligands including thermogravimetric analysis (TGA) are explored to quantify citrate as one of the most popular hydrophilic ligands on the surface of nanoparticles such as iron oxide nanoparticles (IONPs). The purpose of work is to understand which analytical methods are best suited for surface chemistry analysis of citrate stabilized IONPs and to validate these methods. T2 - SALSA Make and Measure 2024: Interfaces CY - Berlin, Germany DA - 11.09.2024 KW - Nano KW - Particle KW - Iron oxide KW - Ligand KW - Quantification KW - Advanced material KW - Surface analysis KW - Functional group PY - 2024 AN - OPUS4-62298 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Matiushkina, Anna T1 - Quantification of Citrate Ligands on the Surface of Nanoparticles N2 - In this study, different methods for determining nanoparticle surface ligands including thermogravimetric analysis (TGA) are explored to quantify citrate as one of the most popular hydrophilic ligands on the surface of nanoparticles such as iron oxide nanoparticles (IONPs). The purpose of work is to understand which analytical methods are best suited for surface chemistry analysis of citrate stabilized IONPs and to validate these methods. T2 - SALSA Make and Measure 2024: Interfaces CY - Berlin, Germany DA - 11.09.2024 KW - Nano KW - Particle KW - Iron oxide KW - Ligand KW - Quantification KW - Advanced material KW - Surface analysis KW - Functional group PY - 2024 AN - OPUS4-62310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maul, Ronald T1 - Biosynthesis of zearalenone conjugates by fungi N2 - Zearalenone (ZEN) and its sulfate and glucoside conjugates have been detected in (a broad variety of) food and feed commodities1. Both conjugated derivatives are formed as part of fungal or plant secondary metabolism and thus, belong to the group of modified mycotoxins2. After consumption of contaminated foodstuff, the conjugates can be hydrolyzed by human intestinal microbiota leading to liberation of ZEN that implies an underestimation of the true ZEN exposure. In order to include ZEN conjugates in routine analysis, as well as for toxicological investigation reliable standards are needed. The objective of the present study was to develop a simple and economic method for biosynthesis of ZEN conjugates. Preceding experiments on the biotransformation of ZEN by Rhizopus and Aspergillus species showed a mixed metabolite formation3. Therefore, these known ZEN conjugating fungal strains were screened for their potential to selectively synthesize the ZEN derivatives ZEN-14-sulfate (Z14S), ZEN-14-glucoside (Z14G) and ZEN-16-glucoside (Z16G). The screening was conducted by adding ZEN to liquid fungal cultures. Cultivation conditions and ZEN incubation time were varied. All media samples were analyzed for metabolite formation by HPLC-MS/MS. Z14S was exclusively formed by A. oryzae. Under optimized conditions a specific biosynthesis of Z14G by R. oryzae and Z16G by R. oligosporus was achieved. After liquid-liquid-extraction and preparative chromatographic cleanup 1H-NMR purities of ≥ 73% for Z14S, ≥ 82% for Z14G and ≥ 50% for Z16G were obtained. In addition, a consecutive biosynthesis was developed by first using Fusarium graminearum for ZEN biosynthesis on rice based liquid medium. After inactivation of Fusarium the subsequent conjugation reaction was conducted utilizing Aspergillus and Rhizopus species under the various optimized conditions. In this study an easy and cost-efficient biosynthesis for Z14S, Z14G and Z16G was developed. The developed biosynthesis could be also used for other metabolites like ZEL conjugates. Our results of the in vitro screening indicate also the formation of a ZEL-glucoside and α ZEL-sulfate as major metabolites by R. oryzae. In sum, under optimized cultivation conditions fungi can be easily utilized for a targeted and stereospecific synthesis of ZEN conjugates. T2 - 10th World Mycotoxin Forum Conference CY - Amsterdam, The Netherlands DA - 12.03.2018 KW - Mycotoxins KW - Food safety KW - Analytical standards PY - 2018 AN - OPUS4-44547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Herter, Sven-Oliver T1 - New PFAS Reference Materials for Environment and Circular Economy N2 - Per- and polyfluorinated alkyl substances (PFAS) are a group of synthetic compounds that have been used in various industrial and consumer products for decades. Their wide range of applications is due to water- and oil-repellent properties, as well as their chemical and thermal stability. However, the use of PFAS has raised concerns due to their persistence in environment and their adverse health effects, leading to regulations aimed at controlling their use and minimizing exposure. Substances such as PFOS, PFHxS, and PFOA are listed in the Stockholm Convention on Persistent Organic Pollutants (POP Regulation, EU 2019/1021). Maximum values have been set for PFAS in environmental matrices such as soil and water, but also for textiles as a relevant area of circular economy and part of the current German standardization roadmap “Circular Economy”. Reliable PFAS analysis requires an increasing global demand for certified reference materials (CRM). However, CRMs for PFAS in soils and textiles are rare or currently not available. To improve the metrological infrastructure and support PFAS measurements, two CRMs for PFAS in soil (BAM-U027) and PFAS in textiles (BAM-B003) based on ISO 17034 and ISO 33405 were developed. This poster provides an overview of the different steps for preparation and characterization of the two candidate materials. The assignment of the certified mass fractions for relevant PFAS targets (18 PFAS targets for BAM-B003) is based isotope dilution HPLC-MS/MS at three independent workplaces. The results of the BAM in-house study on BAM-U027 were supported by an interlaboratory comparison study. T2 - 16th International Symposium on Biological and Environmental Reference Materials CY - Halifax, Nova Scotia, Canada DA - 01.06.2025 KW - Certified Reference Material KW - PFAS KW - Circular Economy KW - Textiles KW - Quality assurance PY - 2025 AN - OPUS4-63404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tobias, Charlie A1 - Climent Terol, Estela A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Polystyrene Microparticles with Convergently Grown Mesoporous Silica Shells as a Promising Tool for Multiplexed Bioanalytical Assays N2 - Functional core/shell particles are highly sought after in analytical chemistry, especially in methods suitable for single-particle analysis such as flow cytometry because they allow for facile multiplexed detection of several analytes in a single run. Aiming to develop a powerful bead platform of which the core particle can be doped in a straightforward manner while the shell offers the highest possible sensitivity when functionalized with (bio)chemical binders, polystyrene particles were coated with different kinds of mesoporous silica shells in a convergent growth approach. Mesoporous shells allow us to obtain distinctly higher surface areas in comparison with conventional nonporous shells. While assessing the potential of narrow- as well as wide-pore silicas such as Mobil composition of matter no. 41 (MCM-41) and Santa Barbara amorphous material no. 15 (SBA-15), especially the synthesis of the latter shells that are much more suitable for biomolecule anchoring was optimized by altering the pH and both, the amount and type of the mediator salt. Our studies showed that the best performing material resulted from a synthesis using neutral conditions and MgSO4 as an ionic mediator. The analytical potential of the particles was investigated in flow cytometric DNA assays after their respective functionalization for individual and multiplexed detection of short oligonucleotide strands. These experiments revealed that a two-step modification of the silica surface with amino silane and succinic anhydride prior to coupling of an amino-terminated capture DNA (c-DNA) strand is superior to coupling carboxylic acid-terminated c-DNA to aminated core/shell particles, yielding limits of detection (LOD) down to 5 pM for a hybridization assay, using labeled complementary single-stranded target DNA (t-DNA) 15mers. The potential of the use of the particles in multiplexed analysis was shown with the aid of dye-doped core particles carrying a respective SBA-15 shell. Characteristic genomic sequences of human papillomaviruses (HPV) were chosen as the t-DNA analytes here, since their high relevance as carcinogens and the high number of different pathogens is a relevant model case. The title particles showed a promising performance and allowed us to unequivocally detect the different high- and low-risk HPV types in a single experimental run. KW - Bead-based assay KW - Core-shell particles KW - Human papillomavirus KW - Mesoporous silica KW - Multiplexing PY - 2020 DO - https://doi.org/10.1021/acsami.0c17940 SN - 1944-8244 VL - 13 IS - 1 SP - 207 EP - 218 PB - American Chemical Society CY - Washington, DC AN - OPUS4-51955 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Herter, Sven-Oliver T1 - Synthesis and application of isotopic labelled ergot alkaloids N2 - Ergot alkaloids form a toxicologically relevant group of mould toxins (mycotoxins) that are among the most common contaminants of foodstuff and animal feed worldwide. Reliable controls are essential to minimise health risks and economic damage. Due to their toxicological relevance, EU limit values for 12 priority ergot alkaloids have been introduced for the first time in 2022 and range from 500 μg/kg in rye milling products down to 20 ug/kg Processed cereal-based foods for infants and young children[1]. High-performance liquid chromatography - mass spectrometry is used to quantify low concentrations of ergots in food, however the European standard analytical procedure cannot be applied due to the lack of isotopically labelled reference standards. The complex structure of the ergot alkaloids makes a total synthesis extremely challenging, expensive and time-consuming. Therefore, we are focusing on different semi-preparative methods (electrochemistry, organic synthesis, heterogeneous catalysis) to specifically N-demethylate the C8 carbon atom of the lysergic acid moiety. The norergot alkaloid formed is then isotopically labelled using an electrophilic methyl source, i.e. iodomethane or dimethyl sulphate to obtain the specific isotopic labelled ergot alkaloid. Initial experiments have shown that N-demethylation of the ergot alkaloid ergotamine is possible by both electrochemical and wet-chemical organic synthesis. The next step is to improve the previously determined reaction conditions to enable the synthesis of norergotamine on a mg scale for further reactions. T2 - ISEAC-41 CY - Amsterdam, Netherlands DA - 20.11.2023 KW - Reference Material KW - Isotope KW - Standards KW - Mykotoxine KW - HPLC-MS PY - 2023 AN - OPUS4-59315 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia T1 - Electrochemistry coupled to mass spectrometry (EC/MS) – A valuable tool to simulate metabolic processes of mycotoxins? N2 - Mycotoxins are secondary metabolites produced by fungi contaminating food and feed worldwide. Intake of these foodborne toxins can cause several diseases in humans and animals highlighting the need to understand metabolic pathways of mycotoxins. Methods of choice have been in vitro and in vivo approaches, so far. Beside hundreds of documented mycotoxins numerous new ones need to be elucidated and enhance the demand for fast and reliable methods. Here, we present electrochemistry coupled to mass spectrometry (EC/MS set up Fig. 1) as novel and promising tool in mycotoxin research. Electrochemical oxidation of mycotoxins like zearalenone, citrinin or dihydroergocristine lead to several oxidation products known from phase I biotransformation as well as new interesting reaction products analyzed by EC/MS, LC MS/MS and ESI-HRMS. To ensure a comparative overview results obtained from electrochemical oxidation experiments were compared to Fenton reaction, UV irradiation and microsomal experiments. The presentation will point out the benefits and drawbacks of EC/MS in mycotoxin research on the basis of selected food relevant mycotoxins. T2 - ANAKON CY - Tübingen, Deutschland DA - 03.04.2017 KW - Electrochemistry KW - Mycotoxin KW - Metabolism PY - 2017 AN - OPUS4-39766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Development of a Lab-on-a-Chip for the Detection of Nerve Agents with a Handheld Device N2 - The development of a Lab-on-a-Chip (LoC) is presented, which can detect reactive phosphorous compounds in the gas phase in combination with an optochemical hand-held sensor. The LoC prototype contains three pairs of sensing materials containing fluorescent indicator dyes in various carrier materials. By measuring the fluorescence response to phosphoryl chloride, a surrogate compound, the detection of chemical warfare agents (CWAs) in gas phase becomes possible within seconds, introducing a novel approach to CWA detection. T2 - IEEE Sensors Conference CY - Vienna, Austria DA - 29.10.2023 KW - Chemical warfare agents KW - Lab-on-a-chip KW - Handheld sensors KW - Toxic industrial chemicals KW - Fluorescence PY - 2023 AN - OPUS4-58815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Temgoua Tonleu, Ranil C. A1 - Koch, Matthias T1 - Simulation of the Environmental Degradation of TBBPA by EC-LC-MS N2 - Oxidative degradation processes of tetrabromobisphenol A (TBBPA), a brominated flame retardant (BFR) in wood, plastics and electronics, were investigated by electrochemistry (EC) coupled online to electrospray ionization mass spectrometry (ESI/MS). Oxidative phase I and II metabolites production was achieved using an electrochemical flow-through cell equipped with a boron doped diamond electrode. Structural elucidation and prediction of oxidative metabolism pathways of TBBPA according to type II ipso-substitution were based on retention time, m/z ratio in negative mode and fragmentation pattern. Using the data obtained through high resolution MS analysis and the identification of single electron transfer (SET) as the initial step of a two-electron oxidation provided the necessary information to propose a mechanism for the electrochemical oxidation of TBBPA. Oxidation reactions involving aromatic hydroxylation and β-scission were the main degradation observed when studying the electrochemical behavior of TBBPA. Computational chemistry experiments using density functional theory (DFT) allowed to identify mono-hydroxylated reaction intermediate and dismissed the mechanism involving two concurrent hydroxylation. TBBPA oxidation products were compared to known metabolites of its biological and environmental degradation confirming the ability of electrochemistry to simulate β-scission reactions. T2 - Mass Spectrometry Forum 2024 CY - Vienna, Austria DA - 21.02.2024 KW - Emerging pollutants KW - Chemical characterization KW - Electrochemistry KW - Chemical and material safety KW - Mass spectrometry KW - Environment-material interactions PY - 2024 AN - OPUS4-59571 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hartmann, Yannic A1 - El Abbassi, Abdelouahad A1 - Mayer, Bernhard A1 - Resch‐Genger, Ute A1 - Müller, Thomas J. J. T1 - Ester‐Aroyl‐S,N‐Ketene Acetals with Solid‐State Luminescence: AIEgens from Sequential Three‐Component Desymmetrization N2 - AbstractDi(hetero)aroyl dichlorides are desymmetrized upon sequential reaction with alcohols and 2‐methyl N‐benzyl thiazolium salts within the course of a one‐pot three‐component reaction yielding ester‐substituted aroyl‐S,N‐ketene acetals under mild conditions in good yields. A prerequisite for the concise one‐pot process is the different nucleophilicity of the alcohols and in situ generated S,N‐ketene acetals. The resulting compounds are merocyanines with dominant charge‐transfer absorption bands which are fluorescent in the solid state, but not in solution. In water/ethanol solvent mixtures of increasing water content, the water‐insoluble dyes display typical aggregation‐induced emission (AIE) characteristics. The water fraction inducing AIE as well as the emission color, and fluorescence quantum yield (Φf) of the aggregated dyes can be controlled by the alcohol part of the ester moiety. Encapsulation into polystyrene nanoparticles can lead to a considerable increase of the fluorescence quantum yield Φf to 30% as shown for a representatively chosen dye revealing the highest Φf of 11% within the dye series in the water/ethanol mixtures and enabling the usage of these dyes as fluorescent reporters in aqueous environments. KW - Dye KW - Fluorescence KW - Aggregation KW - Mechanism KW - Signal enhancement KW - Nano KW - Particle KW - Characterization KW - Quantum yield KW - Photophysics KW - Probe KW - Sensor KW - Lifetime KW - Polarity PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642400 DO - https://doi.org/10.1002/chem.202502071 SN - 0947-6539 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-64240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholtz, Lena T1 - Luminescent, Semiconductor Nanoparticle-Loadedpolymer Microbeads–Comparingparticlearchitectures N2 - Luminescent polymer microparticles (PMPs) are applied in various (bio)analytical and diagnostic processes.[1] The staining of these beads is important for the realization of optically distinguishable barcodes that can be read out, e.g., by a flow cytometer or fluorescence microscope. Typically, luminescent semiconductor nanoparticles (NPs) absorb in a broad wavelength range and show narrow emission bands, which enables simultaneous excitation of differently colored luminophores and facilitates a spectral discrimination.[1] This makes them ideal candidates for this purpose and encouraged us to explore and develop a simple, effective approach to luminescent semiconductor NP encoding of polystyrene PMPs and identify suitable synthesis conditions.[2] Until now, mainly semiconductor quantum dots (QDs) have been used for the synthesis of luminescent PMPs, although NPs with different shapes could introduce beneficial new features. Aiming for the application of our developed procedure to non-spherical NPs, we systematically investigated the luminescence properties of the resulting NP-stained beads using fluorescence and integrating sphere spectroscopy as well as fluorescence and electron microscopy. These studies showed that the suitability of semiconductor NPs for the synthesis of luminescent PMPs depends not only on their shape, but also heavily on their surface chemistry.[3] The successful incorporation of nonspherical NPs opens the path to include even more NPs, and the results can help to deduce future applications for the beads which best suit their specific properties. T2 - E-MRS Fall Meeting 2025 CY - Warsaw, Poland DA - 15.09.2025 KW - Quality assurance KW - Fluorescence KW - Nano KW - Particle KW - Synthesis KW - Quantum dot KW - Quantum rod KW - Platelet KW - Quantum yield KW - Polymer particle KW - Encoding KW - Surface chemistry KW - Mechanism KW - Characterization KW - Lifetime KW - Barcode KW - Polymerization KW - Method PY - 2025 AN - OPUS4-64242 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholtz, Lena T1 - Standardized Measurements of Surface Functionalities on Nanoparticles N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely and commonly fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, opto-electronics, and information storage. NP function, their interaction with biological species, and also their environmental fate are largely determined by the surface functionalities of the particles. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, determination of their applicability, and mandatory to meet increasing concerns regarding their safety. In addition, industry as well as international standardization organizations, regulatory agencies, and policymakers need validated and standardized measurement methods and reference materials. However, methodologies for determining NP surface properties, including the amount, chemical composition, and homogeneity of surface functionalities and coatings are largely non-standardized up until now. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR), as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. The latter, typically less costly methods are often used by SMEs, e.g., for quality control. To validate methods, establish measurement uncertainties, test reference materials, and produce reference data, international interlaboratory comparisons (ILC) on NP surface functionalization measurements are required to provide well characterized test and reference nanomaterials including benchmark values.[1] These needs are addressed by the current European metrology project SMURFnano, involving 12 partners from different National Metrology Institutes, designated and research institutes, two university groups as well as one large company and one SME producing NPs. This project, as well as first results derived from the development of test and reference materials with a well characterized surface chemistry, and ongoing interlaboratory comparisons, will be presented. T2 - eMRS - Fall Meeting 2025 CY - Warsaw, Poland DA - 15.09.2025 KW - Nano KW - Particle KW - Silica KW - Polymer KW - Metrology KW - Quality assurance KW - Reference material KW - Surface chemistry KW - Size KW - Shape KW - Particle number concentration KW - Method KW - Optical assay KW - qNMR KW - Validation KW - Potentiometry KW - XPS PY - 2025 AN - OPUS4-64243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej A1 - Bartholmai, Matthias A1 - Neumann, Patrick P. A1 - Tiebe, Carlo A1 - Gawlitza, Kornelia A1 - Bartelmeß, Jürgen T1 - Adaptable multi-sensor device for gas detection N2 - Innovation is the catalyst for the technology of the future. It is important to develop new and better technologies that can continuously monitor the environmental impact, e.g., for air quality control or emission detection. In the recently at BAM developed Universal Pump Sensor Control (UPSC3) module, different components and sensors are fused. The combination of the individual components makes the UPSC3 module an excellent monitoring and reference system for the development and characterization of gas specific sensors. Measurements over long periods are possible, for mixed gas loads or for certain gas measurements. The system is part of a mobile sensor network of several sensor units, which can also be used as standalone systems. The motivation and objective of this research is to develop gas sensors based on fluorescence detection with range of ppm / ppb. For this task a reference system is required, which contains volatile organic compound (VOC) sensors for reference data from different scenarios. The integrated multi-sensor unit can measure different gases through the integrated 3-fold VOC sensor, which can be adapted to the addressed scenario. . The system-integrated flow control, with pump and flow sensor, allows the gas molecules to be transported directly to the VOC sensor. The entire measurement is permanently stored on an integrated memory card. If the previously determined limit range is exceeded, an alarm is generated. The system is an important tool towards further developments in the field of gas sensors and is primarily used for the validation of chemically based gas sensors. T2 - Colloquium of Optical Spectrometry (COSP) 2017 CY - Berlin, Germany DA - 27.11.2017 KW - Gas detection KW - Multi sensor device KW - Pump control KW - VOC PY - 2017 AN - OPUS4-43193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Multifunctional hybrid microparticles for rapid cytometric and microfluidic mix-&-detect bioassays N2 - Besides the application-oriented parameters selectivity and sensitivity, simplicity and speed as well as robustness and reliability are the key features that determine success, dissemination and acceptance of analytical assays and methods for use in the field. For bioassays based on antibodies or nucleic acid binders, bead-based assays have become one of the main working horses of lab-based methods. However, these approaches are often limited by complicated and time-consuming workflows, which are mainly compensated by massive parallelisation, keeping the average cost and time-to-result within acceptable limits due to the sheer number and constant flow of samples processed. In on-site applications, where analyses need to be performed on suspicion or on demand because results are needed as quickly as possible for proactive decision making, the number, frequency and type of samples are much more diverse, so analytical assays need to be adapted to remain cost-effective and operable by non-expert users in environments where no lab infrastructure is available. With this in mind, we have developed a multifunctional hybrid microparticle platform that enables fast and simple mix-&-detect bioassays in combination with fluidic cytometry- and chip-based analytical methods. The present contribution will give an overview of the beads, their functions and how they can be combined with immunoanalytical and nucleic acid-based detection technologies. Starting from simple polymeric core/silica shell particles [1], we have progressively introduced coding [2,3], anti-fouling [2], high-surface area [4] and magnetic schemes [5] and in recent years have shown how these beads can be used in simple mix-&-detect assays for a range of different environmental, health and food analytes [1-5]. In addition to cytometry, we have also successfully implemented such assays using miniaturised microfluidic and strip-based approaches [6]. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Bead-based assay KW - Core-shell particles KW - Lab-on-a-chip KW - Mycotoxin PY - 2025 AN - OPUS4-62766 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mekonnen, Tessema Fenta T1 - Metabolic transformation products of pesticides by electrochemical cell coupled to LC-MS (EC-LC-MS) N2 - Metabolic transformation products (TPs) of the insecticide chlorpyrifos (CPF), the new fungicide fluopyram (FLP) and the broad-spectrum herbicide, glyphosate (GLP), were studied by electrochemistry coupled to mass spectrometry (EC-MS) for the first time. Phase I metabolites of the three pesticides from rat liver in-vitro assay experiments were studied by LC-MS/MS and compared to electrochemically oxidized products from EC-MS. Known metabolites from S-oxidation, O-dealkylation and hydroxylation of the insecticide chlorpyrifos have been identified by EC-MS and simulated to in-vitro assays. Chlorpyrifos-oxon (CPF-oxon), diethylthiophosphate (DETP), 3,5,6-trichloropiridinol (TCP), diethylphosphate (DEP) and 2,3,5-trichloropyridine (TCPy) were the main EC oxidative TPs and in-vitro assay metabolites of CPF which was also reported by Choe et al.. Fluopyram was extensively converted to a number of electrochemical products including mono- and dihydroxylated derivatives and yet unidentified TPs. Rat liver microsomal assay experiments showed mainly hydroxylated metabolites of FLP which was also reported by the European Food Safety Agency (EFSA). Aminomethyl phosphonic acid (AMPA) was the main TP of glyphosate detected from both EC-MS analysis and in-vitro assay tests. A number of TPs of CPF, FLP and GLP have been identified by electrochemistry online mass spectrometry and compared to in-vitro assays. Using electrochemistry upfront MS enables fast and matrix free prediction of metabolic pathways, transformation products and/or fate of pesticides. Further studies will focus on structural characterization of detected compounds, phase II metabolites and investigation of real samples. T2 - 9th European Conference on Pesticides and Related Organic Micropollutants in the Environment: 15th Symposium on Chemistry and Fate of Modern Pesticides CY - Santiago de Compostela, Spain DA - 04.10.2016 KW - EC-MS KW - Pesticides KW - Transformation products (TPs) KW - Metabolites PY - 2016 AN - OPUS4-37707 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertin, Annabelle T1 - Endowing nanoparticles with orthogonal functionalities via core / shell / shell architecture N2 - Dual orthogonal functionality in a single material is highly desirable in many fields such as bio-imaging, sensing, coating or diagnostic and therapy. However, combining two different functionalities in a precise and controlled way is still a challenging task. Here we present how simply dual functional hybrid nanoparticles consisting of a silica core with a fluorescent and a thermoresponsive polymeric layers can be prepared. As a first step of this work, silica core particles were coated by a fluorescent layer using surface-initiated reversible addition-fragmentation chain transfer polymerization. Afterwards, the fluorescent silica nanoparticles were completely enclosed in a switchable protective coating made of thermoresponsive poly(N-isopropylacrylamide). The thermoresponsive poly(N-isopropylacrylamide) changes its properties with varying the surroundings temperature and this behavior is reversible and controllable. To the best of our knowledge these types of hybrid dual functional core-shell-shell nanoparticles have not yet been prepared, despite the prospect of many potential applications. T2 - World Congress on Living Polymerizations and Polymers - LPP16 CY - Budapest, Hungary DA - 29.05.2016 KW - Fluorescent and thermoresponsive nanoparticles KW - Core KW - Shell KW - Shell nanoparticles PY - 2016 AN - OPUS4-37367 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bertin, Annabelle T1 - Endowing nanoparticles with orthogonal functionalities via core / shell / shell architecture N2 - Dual orthogonal functionality in a single material is highly desirable in many fields such as bio-imaging, sensing, coating or diagnostic and therapy. However, combining two different functionalities in a precise and controlled way is still a challenging task. Here we present how simply dual functional hybrid nanoparticles consisting of a silica core with a fluorescent and a thermoresponsive polymeric layers can be prepared. As a first step of this work, silica core particles were coated by a fluorescent layer using surface-initiated reversible addition-fragmentation chain transfer polymerization. Afterwards, the fluorescent silica nanoparticles were completely enclosed in a switchable protective coating made of thermoresponsive poly(N-isopropylacrylamide). The thermoresponsive poly(N-isopropylacrylamide) changes its properties with varying the surroundings temperature and this behavior is reversible and controllable. To the best of our knowledge these types of hybrid dual functional core-shell-shell nanoparticles have not yet been prepared, despite the prospect of many potential applications. T2 - 251st American Chemical Society National Meeting CY - San Diego, USA DA - 13.03.2016 KW - Fluorescent and thermoresponsive nanoparticles KW - Core / shell / shell / nanoparticles PY - 2016 AN - OPUS4-37370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Payton, E. J. A1 - Agudo Jácome, Leonardo A1 - Nolze, Gert T1 - Phase Identification by Image Processing of EBSD Patterns N2 - Automated electron backscatter diffraction (EBSD) is generally unable to distinguish between multiple cubic phases in a specimen without additional information, such as that obtained by simultaneous energy dispersive X-ray spectroscopy (EDS). Small particles of phases with relatively similar compositions push the limits of phase identification using simultaneous EBSD and EDS, and a mismatch exists between the spatial resolutions of these two techniques due to them having different electron interaction volumes. In a recent paper, the present authors explored using backscatter detectors mounted on top of the EBSD detector to obtain atomic number (Z) contrast images that could be used for phase segmentation in cases where the results from the EBSD and EDS signals remain ambiguous. In the present work, we show that similar information can be obtained from the raw EBSD patterns themselves at higher spatial resolution than was obtained from the backscatter detectors, with the additional advantage of having no spatial mismatch between the data collection grids. KW - Phase identification KW - Backscattered electrons KW - EBSD KW - SEM PY - 2013 DO - https://doi.org/10.1017/S143192761300620X VL - 19 IS - Suppl. 2 SP - 842 EP - 843 AN - OPUS4-37985 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Noordmann, J. T1 - Gravimetric preparation and characterization of a primary reference solution of molybdenum N2 - Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes to the purity of the solid materials they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Unit. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project called SIB09 Primary standards for challenging elements, a reference solution of molybdenum was prepared directly from the respective metal with a relative expanded uncertainty associated with the mass fraction of Urel(w) < 0.05 %. A highly accurate and precise ICP OES and MC-ICP-MS method was developed to assist with the preparation and as a dissemination tool. T2 - ANACON CY - Graz, Austria DA - 23.03.2015 KW - Metrology KW - Primary standards KW - Mo PY - 2015 AN - OPUS4-38038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartelmeß, Jürgen T1 - Highly substituted boron dipyrromethene (BODIPY) fluorophores for hosting benzene and its derivatives – A Sensing Approach N2 - BODIPY fluorophores are popular functional dyes in a multitude of fields in chemistry, physics, and materials sciences due to their excellent properties such as a good photostability, high fluorescence quantum yields, and almost unlimited possibilities for tailoring their properties by chemical functionalization. In sensing applications, BODIPY dyes are widely employed. In this work, we present an approach for creating a BODIPY-based pocket-like structure for the recognition of volatile organic compounds (VOC) such as benzene and its derivatives. This may lead to the development of sensing devices for this class of compounds, which receive special attention by environmental chemists and regulatory authorities due to severe adverse effects on humans in particular and the environment in general. The low reactivity of benzene-derived hazardous compounds is thereby a major fact that has to be taken into consideration. While for other reactive gaseous compounds, fluorophore-based detection performance is achieved by the chemical modification of the fluorophore itself, e.g. by bond cleavage, addition, oxidation or reduction reactions; this is not possible for many VOCs. Several metal complexes were described for the sensing of benzene and its derivatives, but no organic dyes such as BODIPYs are known with these capabilities. Our unique concept towards BODIPY-based molecules acting as scavengers for VOCs is supposed to overcome the problem of benzene’s low reactivity by enforcing π-π-interactions between the fluorophore and the volatile aromatic analyte in pocket-like molecular structures. T2 - 25. Lecture Conference on Photochemistry CY - Jena, Germany DA - 26.09.2016 KW - KonSens KW - Benzene sensor KW - Fluorescence spectroscopy PY - 2016 AN - OPUS4-37826 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wagner, Sabine A1 - Zapata, Carlos A1 - Wan, Wei A1 - Gawlitza, Kornelia A1 - Weber, M. A1 - Rurack, Knut T1 - Role of Counterions in Molecularly Imprinted Polymers for Anionic Species N2 - Small-molecule oxoanions are often imprinted noncovalently as carboxylates into molecularly imprinted polymers (MIPs), requiring the use of an organic counterion. Popular species are either pentamethylpiperidine (PMP) as a protonatable cation or tetraalkylammonium (TXA) ions as permanent cations. The present work explores the influence of the TXA as a function of their alkyl chain length, from methyl to octyl, using UV/vis absorption, fluorescence titrations, and HPLC as well as MD simulations. Protected phenylalanines (Z-L/D-Phe) served as templates/analytes. While the influence of the counterion on the complex stability constants and anion-induced spectral changes shows a monotonous trend with increasing alkyl chain length at the prepolymerization stage, the cross-imprinting/rebinding studies showed a unique pattern that suggested the presence of adaptive cavities in the MIP matrix, related to the concept of induced fit of enzyme−substrate interaction. Larger cavities formed in the presence of larger counterions can take up pairs of Z-X-Phe and smaller TXA, eventually escaping spectroscopic detection. Correlation of the experimental data with the MD simulations revealed that counterion mobility, the relative distances between the three partners, and the hydrogen bond lifetimes are more decisive for the response features observed than actual distances between interacting atoms in a complex or the orientation of binding moieties. TBA has been found to yield the highest imprinting factor, also showing a unique dual behavior regarding the interaction with template and fluorescent monomer. Finally, interesting differences between both enantiomers have been observed in both theory and experiment, suggesting true control of enantioselectivity. The contribution concludes with suggestions for translating the findings into actual MIP development. KW - Anion receptors KW - Fluorescence sensing KW - Molecular dynamics simulations KW - Molecularly imprinted polymers KW - Rational design PY - 2018 DO - https://doi.org/10.1021/acs.langmuir.8b00500 SN - 0743-7463 VL - 34 IS - 23 SP - 6963 EP - 6975 PB - American Chemical Society CY - Washington, D.C. AN - OPUS4-45399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Panne, Ulrich T1 - Polymerwissenschaften@BAM - Sicherheit macht Märkte N2 - Die Bundesanstalt für Materialforschung und -prüfung (BAM) ist eine Ressortforschungseinrichtung, die zum Schutz von Mensch, Umwelt und Sachgüter, forscht, prüft und berät. Im Fokus aller Tätigkeiten in der Materialwissenschaft, der Werkstofftechnik und der Chemie steht dabei die technische Sicherheit von Produkten und Prozessen. Dazu werden Substanzen, Werkstoffe, Bauteile, Komponenten und Anlagen sowie natürliche und technische Systeme erforscht und auf sicheren Umgang oder Betrieb geprüft und bewertet. Schwerpunkt des Vortrages sind multimodale Polymeranalytik, nanoskalige Sensormaterialien und die Charakterisierung von technischen Eigenschaften von Polymeren sowie ihre Alterung und Umweltrelevanz. T2 - Institutsvortrag CY - Fraunhofer IAP, Potsdam, Germany DA - 18.05.2018 KW - Polymerwissenschaften PY - 2018 AN - OPUS4-45243 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Hans-Joachim T1 - Certification of the mass fractions of trace elements in a medium purity graphite reference material N2 - The increasing application of graphite materials in various fields of technology and science enhances the demand for strictly controlled properties which are often directly correlated to the contents of trace element impurities. Therefore, the availability of powerful, rapid and reliable analytical methods for the determination of trace impurities is essential for process and quality control. Certified reference materials, indispensable for the development and validation of appropriate trace analytical methods for the characterization of special purity graphite materials are still lacking. Therefore, BAM in co-operation with the working group “Special Materials” of the committee of chemists of GDMB (Gesellschaft der Metallurgen und Bergleute e.V.) certified an industrially sourced graphite material with genuine elemental impurities. The candidate material was a commercial product (NBG 18) taken from the customary production line of the producer SGL CARBON, Chedde (France). The homogeneity of the powdered material was assessed by means of ETV-ICP OES and DC Arc-OES. Certification of the candidate reference material was based on an inter-laboratory comparison involving 17 expert laboratories from Germany, France, Slovenia, USA, South Africa. A variety of different mineralization, digestion, leaching, fusion and combustion techniques prior to ICP OES and photometry, methods without sample preparation (INAA, k0-INAA) as well as typical solid sampling methods (ETV-ICP OES, ETV-ICP-MS, SS-ET AAS, DC Arc-OES, MF-DC Arc-OES) were used to characterise the material. Certified mass fractions and their expanded uncertainties (k = 2) were assigned for 27 elements (Al, B, Ba, Be, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Si, Sr, Ti, V, W, Y, Zn, Zr), ranging from (0.00050 ± 0.00027) mg/kg for Be to (41 ± 6) mg/kg for Si. Additionally, informative values are given for the: trace element contents of Ag, As, Au, Bi, Cd, Cs, Dy, Eu, Ga, Gd, Hg, In, La, Nb, Rb, Re, Rh, Sb, Sc, Se, Sm, Sn, Ta, Tb, Te, Th, U; method specific values obtained by ETV-ICP OES (BETV and SiETV) and the ash content of the material. The certified material “BAM-S009 Medium Purity Graphite Powder” is available for purchase from BAM. T2 - ESAS & CANAS 2018 CY - Berlin, Germany DA - 20.03.2018 KW - Graphite KW - Certification KW - Trace elements KW - Reference material PY - 2018 AN - OPUS4-44775 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mekonnen, Tessema Fenta T1 - Electrochemistry coupled to mass spectrometry for biotransformation and metabolite elucidation of pesticides N2 - Online coupling of electrochemistry with mass spectrometry (EC/MS) is highly promising for prediction and simulation of metabolic processes of xenobiotics in living organisms. Less time and cost of analysis, matrix free detection, and automation make EC/MS-based metabolomics superior over traditional in-vivo and in-vitro methods. Furthermore, EC/MS has a special feature to identify reactive intermediates and reaction mechanisms. The main objective of this work was to simulate biotransformation processes of pesticides by EC/MS and to elucidate the Transformation products (TPs). We have studied the oxidative phase I metabolism processes of selected pesticides by EC/MS or with liquid chromatography (EC/LC/MS) and compared the derived TPs with cytochrome based metabolites. The electrochemical TPs were produced by boron-doped diamond electrode, separated by LC, and detected by single quadrupole ESI-MS online. Structural identification of both electrochemical oxidation and liver microsome metabolites were based on accurate mass measurements by FT-ICR high-resolution mass spectrometry, isotopic pattern, MS/MS fragmentation, and Retention time alignments. Main phase I oxidative metabolites by P-oxidation, N- & O- dealkylation, dechlorination, hydroxylation, and -OH- oxidation have been identified. Many targeted and untargeted metabolites have been identified by EC/(LC)/MS. Additionally, reactive species have been trapped online by biomolecules to study phase II conjugative reactions. Furthermore, we synthesized TP standards by EC/MS and applied them for pesticide's TPs occurrence investigation in foodstuf matrices. T2 - European Mass Spectrometry Conference (EMSC) 2018 CY - Saarbrücken, Germany DA - 11.03.2018 KW - Transformation product KW - EC/LC/MS KW - Pesticide KW - Biotransformation KW - Electrochemical oxidation PY - 2018 AN - OPUS4-44495 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Makowski, Maike T1 - Non-invasive Cereal Analysis by GC-MS detection of Trichodiene as a Volatile Mycotoxin Biomarker N2 - Due to the increasing consumption of cereals worldwide, the monitoring of growth, storage and processing is becoming more and more crucial. Particularly when stored, infested grains breed fungal clusters (“hot spots”) in which mycotoxins greatly exceed allowed maximum levels. Because of their unpredictable presence, current sample drawing and procedures for mycotoxin analysis represent a complex challenge for operators, involving invasive and cost intensive steps. Therefore, new time- and labour-saving mycotoxin control methods including sampling and analysis steps are needed. A possible approach is the non-invasive analysis of the homogeneous gas phase above the crops, instead of analyzing random samples. However, this procedure requires microbial volatile organic compounds (MVOC´s) being released by the samples and representing the present mycotoxins. Previous investigations revealed trichodiene to be a precursor in trichothecenes biosynthesis – one of the largest mycotoxin groups with over 180 compounds. Due to its non-functionalized sesquiterpene structure, trichodiene has already been quantified using Headspace GC-MS methods (for instance]). Thereby, it can possibly be used as a biomarker for trichothecene contamination in foodstuff. However, further investigations are necessary. The correlation between trichodiene concentration in the gas phase and trichothecenes mass fraction in the sample must be examined closely to draw conclusions about the exact trichothecene content within samples. Realizing this idea, would widely extend the applicability of trichodiene and enormously simplify trichothecene quantification. Hence, this first step of an ongoing study aims to develop a laboratory reference method using trichodiene as volatile biomarker to quantify trichothecenes in cereals. Static headspace and SPME-enrichment coupled to gas chromatography with mass spectrometry (GC-MS) were employed. In a second step, this reference method is intended to validate new approaches for fast on-site screening of trichodiene in cereals. T2 - 10th World Mycotoxin Forum Conference CY - Amsterdam, The Netherlands DA - 11.03.2018 KW - Trichodiene KW - GC-MS KW - Mycotoxin Biomarker PY - 2018 AN - OPUS4-44508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia T1 - Using the model organism Caenorhabditis elegans for the toxicity testing of citrinin, zearalenone and zearalenone-14-sulfate N2 - To keep up with emerging mycotoxins and their transformation products fast and reliable toxicity tests are needed. Toxicity testing of mycotoxins is carried out usually by performing in vitro assays or is evaluated by using laboratory animals like mice, rats or chicken in in vivo studies. Settled between classical in vitro approaches and in vivo studies with higher animals are tests with the nematode Caenorhabditis elegans. Since Sydney Brenner described 1974 the cultivation and handling of C. elegans, this worm is widely used as model organism in developmental biology and neurology. Due to many benefits like easy and cheap cultivation, a completely sequenced genome and short generation time, it also plays an important role in toxicological research. Finally, the high number of conserved genes between human and C. elegans make the worm an ideal candidate for toxicological investigations. In this study we used C. elegans to assess the toxic effects of the relevant food mycotoxin citrinin (CIT), the mycoestrogen zearalenone (ZEN) and the modified mycotoxin ZEN-14-sulfate (ZEN-14-S) on different lifetable parameters including reproduction, thermal and oxidative stress tolerance and lifespan. All tested mycotoxins significantly decreased the amount of offspring. In case of ZEN and CIT also significant negative effects on stress tolerance and lifespan were observed compared to the control group. Moreover, metabolization of mycotoxins in the worms was investigated by using LC MS/MS. Extraction of the worms treated 5 days with mycotoxin-containing and UVC-killed bacteria showed metabolization of ZEN to α-ZEL and β-ZEL (ZEL = zearalenol, ratio about 3:2). ZEN 14-S was reduced to ZEL 14-S and CIT was metabolized to mono hydroxylated CIT. T2 - 40th Mycotoxin Workshop CY - Munich, Germany DA - 11.06.2018 KW - Mycotoxins KW - Caenorhabditis elegans KW - Toxicity testing PY - 2018 AN - OPUS4-45170 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Makowski, Maike T1 - Non-invasive GC-MS Analysis of Trichodiene as Volatile Mycotoxin Biomarker in Cereals N2 - Due to the increasing consumption of cereals worldwide, monitoring of growth, storage and processing is becoming more crucial. Particularly when stored, infested grains breed fungal clusters (“hot spots”) in which mycotoxins greatly exceed allowed maximum levels. Because of their unpredictable presence, current sampling and procedures for mycotoxin analysis are complex and contain invasive and cost intensive steps. A possible approach to avoid sampling inaccuracies is the non-invasive analysis of the homogeneous gas phase above the crops, instead of analyzing random samples. However, this procedure requires microbial volatile organic compounds (MVOC´s) being released by the samples. Previous investigations revealed trichodiene to be a precursor in trichothecenes biosynthesis – one of the largest mycotoxin groups with more than 180 compounds. Due to its non-functionalized sesquiterpene structure, quantification of trichodiene using Headspace GC-MS methods is possible (e.g. [1]). Thereby, it could be used as biomarker for trichothecene contamination in foodstuff. However, further studies are necessary. The correlation between trichodiene concentration in the gas phase and trichothecenes mass fraction in the sample must be examined closely to draw conclusions about the trichothecene content in samples. Realizing this idea, would widely extend the applicability of trichodiene and enormously simplify trichothecene quantification. Hence, this first step of an ongoing study aims to develop a laboratory reference method using trichodiene as volatile biomarker to quantify trichothecenes in cereals. Static headspace and SPME-enrichment coupled to gas chromatography with mass spectrometry (GC-MS) were employed. In a second step, this reference method is intended to validate new approaches for fast on-site screening of trichodiene in cereals. T2 - 40th Mycotoxin Workshop CY - Munich, Germany DA - 11.06.2018 KW - Trichodiene KW - Gaschromatography-Mass Spectrometry KW - Mycotoxin Biomarker PY - 2018 AN - OPUS4-45314 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sternbaek, L. T1 - Macrophage-uptake of sialic acid-targeted molecularly imprinted polymers (SA-MIPs) N2 - Sialic acid (SA) is a cell surface glycan, which has a decisive role in many cell activities including differentiation, proliferation, and the immune response. The amount of SA has been found to correlate with cancer, with an upregulation on more aggressive cancers. Therefore, there is a great interest in developing methods for detection of SA on cancer cells. We are screening SA on cancer cell lines by using fluorescent molecularly imprinted polymers, SA-MIPs. Macrophages, which evolve from mono-cytes, are well known for their extraordinary ability to phagocytose foreign objects. This could lead to the hypothesis that the SA-MIPs can be recognized by macrophages as foreign object; thus leading to internalization and potentially degradation. We have demonstrated that SA-MIPs can be detected after incubation with the RAW macrophage cells, with increasing fluorescence over time. The microscopy analysis shows that the RAW cells ingest the SA-MIP particles. This information is important when planning to use SA-MIPs in future in vivo applications. T2 - 1st National Meeting of the Swedish Chemical Society CY - Lund University, Sweden DA - 17.06.2018 KW - Sialic acid KW - MIPs KW - Macrophages PY - 2018 AN - OPUS4-45421 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sebald, M. T1 - Under Investigation: Novel Approach towards the Synthesis of Deuterium-labelled Alternariol- and Alternariol monomethylether-Standards for the HPLC-MS/MS-Analysis in Food & Feed N2 - Alternariol (AOH) and Alternariol monomethylether (AME) are two secondary metabolites of Alternaria fungi which can be found in various foodstuffs like tomatoes, nuts and grains. Due to their toxicity and potential mutagenic activity the need for the development of high-throughput methods for the supervision of AOH- and AME-levels is of increasing interest. As the availability of both native and labelled AOH and AME analytical standards is very limited we herein wish to present a novel concise approach towards their synthesis employing a ruthenium-catalyzed ortho-arylation4 as the key step. T2 - 13th International Symposium on the Synthesis and Applications of Isotopes and Isotopically Labelled Compounds CY - Prague, Czech Republic DA - 03.06.2018 KW - Mycotoxins KW - Mass Spectrometry PY - 2018 AN - OPUS4-45268 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Tobias A1 - Dietrich, Paul A1 - Unger, Wolfgang A1 - Rurack, Knut T1 - Multimode surface functional group determination: combining steady-state and time-resolved fluorescence with X‑ray photoelectron spectroscopy and absorption measurements for absolute quantification N2 - The quantitative determination of surface functional groups is approached in a straightforward laboratory-based method with high reliability. The application of a multimode BODIPY-type fluorescence, photometry, and X-ray photoelectron spectroscopy (XPS) label allows estimation of the labeling ratio, i.e., the ratio of functional groups carrying a label after reaction, from the elemental ratios of nitrogen and fluorine. The amount of label on the surface is quantified with UV/vis spectrophotometry based on the molar absorption coefficient as molecular property. The investigated surfaces with varying density are prepared by codeposition of 3-(aminopropyl) triethoxysilane (APTES) and cyanoethyltriethoxysilane (CETES) from vapor. These surfaces show high functional group densities that result in significant fluorescence quenching of surface-bound labels. Since alternative quantification of the label on the surface is available through XPS and photometry, a novel method to quantitatively account for fluorescence quenching based on fluorescence lifetime (τ) measurements is shown. Due to the complex distribution of τ on high-density surfaces, the stretched exponential (or Kohlrausch) function is required to determine representative mean lifetimes. The approach is extended to a commercial Rhodamine B isothiocyanate (RITC) label, clearly revealing the problems that arise from such charged labels used in conjunction with silane surfaces. KW - surface group quantification KW - fluorescence spectroscopy KW - absorption spectroscopy KW - X-ray photoelectron spectroscopy KW - dyes PY - 2016 DO - https://doi.org/DOI: 10.1021/acs.analchem.5b03468 SN - 0003-2700 VL - 88 IS - 2 SP - 1210 EP - 1217 PB - American Chemical Society CY - Washington, DC AN - OPUS4-35832 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo T1 - 3D reconstruction, visualization and quantification of dislocations from TEM stereo-pairs N2 - A wide range of properties in crystalline materials is affected by the presence of dislocations, the carriers of plastic deformation. Dislocations can be thought of as filiform structures, characterized by geometrical factors such as their Burgers vector, slip plane, length per unit volume (dislocation density) and line direction. In technical materials such as functional and structural alloys, as well as in minerals, the understanding of bulk deformation driven by dislocation activity is of paramount importance, and thus also the techniques that allow its characterization. Since decades, diffraction contrast in the transmission electron microscope (TEM) is widely implemented to image and describe two-dimensional (2D) projections of dislocation substructures in thin foils [1]. Recently, the use of electron tomography was applied for the first time to fully reconstruct a 3D dislocation network in a GaN epilayer [2]. Although this latter technique has gained popularity, it usually requires an elaborate experimental setup, as well as sophisticated image post-processing methods for a successful reconstruction. Stereoscopic methods in the TEM also have traditionally allowed the three-dimensional (3D) observation of dislocations [e. g. 3]. For this purpose, the same region of a TEM foil is imaged using the same diffraction vector with two beam directions slightly tilted from each other. Subsequently, the pair of images is observed with help of stereo-viewers or 3D glasses. Based on this principle, a system based on a special hardware and software combination was developed for segmentation and analysis of stereomicroscopy data in biological research, and it was also used to analyze simple dislocation structures [4]. In the present contribution a simple software tool is introduced, which has been developed to reconstruct, visualize and quantify dislocation substructures in the thicker regions of electron-transparent foils. A special focus is set on the use of scanning (S)TEM for its implementation. As depicted in Figure 1, the tool is based on the separate tracing of dislocation line segments on both images of a stereo-pair. The points 1, 2 and 3 are marked on the images viewed by the left and right eyes (Figures 1a and b, respectively), showing an relative displacement Δx on the superimposed images in the anaglyph of Figure 1c. This Δx is given by the point’s depth Δh and by the stereo-angle ϑ, as shown in Figure 1d. By knowing the beam direction for the left and right images (BL and BR, respectively), ϑ can be determined, and hence also Δh. Once the depth information from all traced nodes is gained, a reconstruction is made (Figure 1e) where the line length can directly be read from the tool’s interface. The setup is merely geometrical and only needs the relative tilt between both images, the direction of the tilt axis and the image calibration, thus allowing asymmetrical tilts with respect to the foil normal. The foil thickness is measured directly from the endings of the dislocations on the bottom and top surfaces of the TEM foil, and is determined as t ~ 370 nm for the region in Figure 1. With t, the volume is in Figure 1e is also known, and the total dislocation density of the region is calculated as ρt = 44.4 x 1012 m∙m-3. It is clear from Figure 1 that in the Ni-base superalloy presented here, the dislocation substructures are highly localized towards the interface between the two phases of which the microstructure is composed, γ and γ’ (labeled in Figure 1a). The reconstructed model allows a separation of the dislocation densities within the γ and the γ’ phases and at their interface, which would be rather difficult by using common methods such as the one proposed by Ham [5]. Thus the partial dislocation densities are measured as ργ = 1.7 x 1012 m∙m-3, ργ’ = 2.7 x 1012 m∙m-3 and ργ/γ’ = 40.0 x 1012 m∙m-3. The tool also incorporates the knowledge of the crystallographic positions at the two tilts to enable plotting the line segment orientations. One can chose to display the resulting line directions as an interactive table; as an additional spherical spatial graph, where all lines extend from the center of a sphere; as a 2D plot of the spherical coordinates θ and φ; or as points plotted on a stereographic projection. Thus, a simple software tool has been developed that allows the reconstruction, visualization and quantification of foil thickness, localized dislocation densities (or other filiform substructures) and orientations based on only one stereo-pair T2 - Microscopy and Microanalysis 2016 CY - Columbus, OH, USA DA - 24.06.2016 KW - Dislocation KW - Diffraction contrast KW - 3D reconstruction KW - Stereoscopy KW - Scanning transmission electron microscopy PY - 2016 AN - OPUS4-39278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter A1 - Schneider, Rudolf T1 - Determination of pharmacologically active compounds in wastewater by a bead-based flow-cytometric immunoarray N2 - The assessment of water quality demands for multi-target compatible analytical methods. On the one hand, the influence of sewage on natural surface waters must be routinely monitored. On the other hand, estimation of removal efficiencies of pollutants, such as drug residues, is in the focus of industrial and public wastewater treatment. Immunoassays, such as ELISA, are often applied in this area, however, it is only possible to measure a single analyte in one measurement. In contrast, array technology is capable for measuring multiple substances in parallel. Here we present a four-plex bead-based flow cytometric assay for measuring three drugs (carbamazepine, an antiepileptic drug, diclofenac, an antiphlogistic and caffeine, a psychoactive substance) and the bile acid isolithocholic acid, which is proposed to be used as a fecal marker. In this suspension array core-shell particles, consisting of a polystyrene core and a silica shell, are used. They can be easily encoded with a fluorophore which is introduced to the core while the shell is functionalized with amino groups to which the analytes or their derivates are bound via NHS chemistry. They are the competitor binding sites for the antibodies. For the determination of the pollutants, the beads are incubated with a mixture of the analyte-specific antibodies. The molecules on the surface of the beads and the free analyte in solution compete for the binding sites of the antibodies. Bead-bound antibodies can then be visualized via dye-labelled secondary antibodies. For read-out a flow cytometer is used to virtually separate the differently encoded beads. In order to obtain highly selective binding of the antibodies, we investigated different types of surface modifications to overcome unspecific binding, finding that a PEG-based surface is suitable to support our immunoassay format. The resulting multiplexing assay is appropriate to detect the marker substances in the low µg/L range. T2 - Pittcon 2017 CY - Chicago, IL, USA DA - 05.03.2017 KW - Immunoassay KW - Bead-based assay KW - Flow-cytometry KW - Anthropogenic markers PY - 2017 AN - OPUS4-39524 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia A1 - Lörchner, Dominique T1 - Development of analytical method and certified reference material for zearalenone in edible oils N2 - Quality and safety of food products require their reliable analysis. Contaminants, in particular mycotoxins, are key-components for food safety. About 25 % of the world's food crops are contaminated with mycotoxins posing a severe health risk to humans. In order to strengthen food safety and consumer protection the European Commission (EC) set maximum levels for priority mycotoxins in certain foods for human consumption. In 2013, the EC and CEN (European Committee for Standardization) started an initiative to standardize analytical methods for mycotoxins in food which gained increasing relevance, e.g. zearalenone (ZEN).[1] ZEN, an estrogenic mycotoxin produced by several Fusarium species, contaminates cereal crops worldwide. Due to its lipophilic nature ZEN is often found in edible oils (particularly in maize germ oils) derived from contaminated plants. Therefore, an European maximum level of 400 µg/kg is currently in force.[2] To perform reliable food analysis a sustainable metrological infrastructure is of major importance enabling the quantification of priority mycotoxins (here: ZEN). To achieve this goal an integrated approach is needed targeted at the development of validated analytical methods and certified reference materials (CRM). A highly selective method for ZEN in edible oils will be presented, based on solid phase extraction (SPE) using hydrazine-functionalized particles. This method was developed for manual application using commercial SPE cartridges as well as for automated SPE-HPLC online coupling. While ZEN is covalently coupled to the solid phase by means of a hydrazone bond, undesired matrix components can be removed very efficiently. Finally, ZEN is decoupled from the solid phase, leading to highly purified extracts which are measured by HPLC-FLD. The development of the first European Reference Material (ERM®) for ZEN in maize germ oil (ERM®-BC715) will be presented and discussed. This ERM®-project underpins the urgent need for mycotoxin-CRMs to support food safety and public health. [1] European Commission (EC) Mandate M/520 (2013) for standardisation addressed to CEN for methods of analysis for mycotoxins in food. [2] Commission Regulation (EC) No 1126/2007 amending Regulation (EC) No 1881/2006 setting maximum levels for certain contaminants in foodstuffs as regards Fusarium toxins in maize and maize products. T2 - Anakon CY - Tübingen, Germany DA - 03.04.2017 KW - Mycotoxins KW - Food safety KW - Analytical method KW - Reference material PY - 2017 AN - OPUS4-39860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia T1 - Simulating biotransformation reactions of citrinin by electrochemistry/mass spectrometry N2 - Mycotoxins can be found worldwide in food and feed and cause a variety of mold-related health risks which makes it necessary to further examine their metabolic fate in human and other mammals. Beside standard in vitro assays with liver cell preparations an increasing interest in new simulation methods are playing a growing role. The online coupling of electrochemistry with mass spectrometry (EC/MS) is one of these novel techniques, successfully applied in pharmacological and drug research for several years now. The primary objective of this study was to investigate the capability of EC/MS to elucidate metabolic pathways of the mycotoxin citrinin as relevant food contaminant. For this purpose, a coulometric flow through cell equipped with a glassy carbon working electrode was used by applying a ramped potential between 0 and 2 V vs Pd/H2. The electrochemically generated oxidation products analyzed by EC/MS were compared to those obtained from in vitro assays. To receive a comprehensive assessment of EC/MS other non-microsomal oxidation techniques such as Fenton-like reaction and UV irradiation were applied. Several hydroxylated derivatives of citrinin were generated by EC/MS and Fenton-like reaction which are similar to microsomal biotransformation products. These data show that EC/MS is a versatile tool that can be easily applied in mycotoxin research to support metabolic investigations of known and unknown mycotoxins. T2 - ANAKON CY - Tübingen, Deutschland DA - 03.04.2017 KW - Electrochemistry KW - Citrinin KW - Mass spectrometry PY - 2017 AN - OPUS4-39765 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Asadujjaman, Asad T1 - Temperature switches “on” and “off” nanoparticle fluorescence in a core/shell/shell architecture N2 - Fluorescent nanoparticles that light “on/off” by applying external stimuli are of particular interest in the fields of sensing, diagnostics, photonics, protective coatings and microfluidics. The current challenge for these materials is for instance to combine fluorescence and its response to a stimulus such as temperature in a precise manner. Here we present such a system based on a core/shell/shell architecture consisting of a silica core with a fluorescent layer and a thermoresponsive shell. In this work the silica core nanoparticles were first coated with a fluorescent shell using surface initiated reversible addition-fragmentation chain transfer (RAFT) polymerization. The fluorescent nanoparticles were then completely engulfed by a switchable protective coating made of thermoresponsive poly(N-isopropylacrylamide). The fluorescence of the nanoparticles could be “switched on” at room temperature and “switched off” with increasing environmental temperature because of the presence of the thermoresponsive layer. Insights into this phenomenon will be given based on temperature dependent fluorescence measurements and dynamic light scattering. T2 - Makromolecular Konferenz CY - Freiburg, Germany DA - 15.02.2017 KW - Thermoresponsive polymers KW - Sensors KW - Core/Shell/Shell PY - 2017 AN - OPUS4-39230 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - Lebensmittel-relevante Mykotoxine aus Sicht der Europäischen Normung und Regulierung N2 - Etwa 25% aller weltweit produzierten Nahrungsmittel sind mit Schimmelpilzgiften (Mykotoxinen) kontaminiert. Dies birgt nicht nur gesundheitliche Risiken sondern verursacht auch hohe wirtschaftliche Verluste. Daher werden in der EU seit Jahren Anstrengungen unternommen, die Mykotoxin-Analytik voranzutreiben und Grenzwerte zu etablieren. Im Vortrag werden aktuelle Trends der Mykotoxin-Analytik und entsprechende Bedarfe präsentiert. Neben einer verbesserten Verfügbarkeit rückführbarer nativer und isotopenmarkierter Standards treten verstärkt maskierte Mykotoxine in den Fokus. T2 - ASCA/Sigma Mykotoxin-Workshop CY - Berlin, Germany DA - 18.11.2016 KW - Mykotoxine KW - Lebensmittel KW - Standards KW - Qualitätssicherung PY - 2016 AN - OPUS4-38863 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholl, Juliane A1 - Meiers, Emelie T1 - Bestimmung von Trifluoressigsäure (TFA) in Acker- und Grünlandböden N2 - Aufgrund ihrer Persistenz, Mobilität und Toxizität haben per- und polyfluorierte Alkylverbindungen (PFAS) zunehmend an Aufmerksamkeit und Relevanz gewonnen. Mit der PFAS-Belastung von Umweltmatrices ist auch der Bedarf an analytischen Methoden gestiegen. Trifluoressigsäure (TFA) gehört als kürzeste perfluorierte Carbonsäure zur Gruppe der PFAS und gilt als emerging pollutant, dessen Gehalte in der Umwelt zukünftig eine stärkere Überwachung erfordern. Im Vortrag wird zunächst auf die Entwicklung einer sensitiven Analysenmethode zur Bestimmung von TFA in Böden mittels HPLC-MS/MS eingegangen. Anschließend werden die TFA-Ergebnisse von 100 ausgewählten Acker- und Grünlandproben aus Deutschland vorgestellt und diskutiert. T2 - PFAS-Länderaustausch – Erfassung und Erstbewertung PFAS-relevanter Flächen CY - Online meeting DA - 18.11.2024 KW - PFAS KW - LC-MS/MS KW - HILIC KW - TFA KW - Boden PY - 2024 AN - OPUS4-61684 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Costa, Elena T1 - Type-I Pyrethroids Detection with an Antbody-gated Dye Delivery System N2 - The goal of the project is the immunological detection of residual pesticides directly on site using rapidly responding lateral flow test (LFT) strips in combination with indicator dyes and smartphone-based readout and analysis. Specifically, the system consists on a class-selective LFT strip system, which will test for relevant pyrethroid pesticides (Permethrin, d-Phenothrin and others type-I pyrethroids) in parallel. Type-I pyrethroids are frequently used for disinfection purposes against insects such as adult mosquitoes, or diseases carried by insects, like Malaria or Zika in cabins of airplanes on long-distance flights especially from tropical destinations. This treatment is mandatory at various airports but compliance with the rules is difficult to test for. Moreover, if improperly used, these compounds can entail negative health effects for crews and passengers. The detection of the pyrethroids will be achieved thanks to an antibody-gated indicator delivery system (gAID) utilizing monoclonal antibodies and hybrid sensory nanoparticles. After the interaction of the pyrethroid with the gAID, the liberated indicator (dye) will be detected. Since only few analyte molecules are necessary for pore opening yet release a large number of dyes, the system shows intrinsic signal amplification. The device system to be developed has to be so simple that chemically untrained personnel, such as ground or cabin crew, can use it and obtain a result in a reasonably short period of time, e.g., ≤5 min. The need for high accuracy and sufficient sensitivity, established at 0.001 g m–2, is a critical requirement and imposes another significant challenge since this value is beyond current LFTs reported in the literature for pesticide detection to date. In order to achieve the selectivity and sensitivity required by the test itself, and to avoid cross reactivity with other type I pyrethroids, the production of a monoclonal antibody for both Permethrin and Phenontrin is necessary. The synthesis of the two hapten molecules and the subsequent immunization with different immunogens represent the first goal of the work. T2 - Rapid Methods Europe 2018 CY - Amsterdam, The Netherlands DA - 05.11.2018 KW - Pyrethroids KW - Raid test KW - Test strip KW - Delivery system KW - Air traffic PY - 2018 AN - OPUS4-47127 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo T1 - 3D reconstruction and quantification of dislocation substructures from TEM stereo pairs N2 - Dislocations are the carriers of plastic deformation. As such, their characterization offers important information on the properties they affect. In this contribution, a new tool is presented, which is incorporated in Amira ZIB Edition and allows for three-dimensional (3D) imaging and quantification of dislocations substructures from thick regions an electron-transparent specimen. In the tool, the dislocation segments are traced on diffraction contrast images that are obtained in the transmission electron microscope (TEM). The uncertainties related to the experimental setup and to the proposed method are discussed on the base of a tilt series. T2 - AVIZO / AMIRA User Meeting CY - Berlin, Germany DA - 14.11.2018 KW - Dislocation KW - Diffraction contrast KW - Scanning transmission electron microscopy (STEM) PY - 2018 AN - OPUS4-47394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Munir, R. A1 - Lisec, Jan A1 - Swinnen, J. V. A1 - Zaidi, N. T1 - Lipid metabolism in cancer cells under metabolic stress N2 - Cancer cells are often exposed to a metabolically challenging environment with scarce availability of oxygen and nutrients. This metabolic stress leads to changes in the balance between the endogenous synthesis and exogenous uptake of fatty acids, which are needed by cells for membrane biogenesis, energy production and protein modification. Alterations in lipid metabolism and, consequently, lipid composition have important therapeutic implications, as they affect the survival, membrane dynamics and therapy response of cancer cells. In this article, we provide an overview of recent insights into the regulation of lipid metabolism in cancer cells under metabolic stress and discuss how this metabolic adaptation helps cancer cells thrive in a harsh tumour microenvironment. KW - Mass-Spectrometry KW - Lipidomics KW - Lipid metabolism KW - Cancer cells PY - 2019 DO - https://doi.org/10.1038/s41416-019-0451-4 VL - 120 IS - 12 SP - 1090 EP - 1098 PB - Nature AN - OPUS4-48005 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR ED - Resch-Genger, Ute ED - Koch, Matthias ED - Meermann, Björn ED - Weller, Michael G. T1 - Topical collection: Analytical methods and applications in the materials and life sciences N2 - Current trends in materials and life sciences are flanked by the need to push detection limits to single molecules or single cells, enable the characterization of increasingly complex matrices or sophisticated nanostructures, speed up the time of analysis, reduce instrument complexity and costs, and improve the reliability of data. This requires suitable analytical tools such as spectroscopic, separation and imaging techniques, mass spectrometry, and hyphenated techniques as well as sensors and their adaptation to application-specific challenges in the environmental, food, consumer product, health sector, nanotechnology, and bioanalysis. Increasing concerns about health threatening known or emerging pollutants in drinking water, consumer products, and food and about the safety of nanomaterials led to a new awareness of the importance of analytical sciences. Another important driver in this direction is the increasing demand by legislation, particularly in view of the 17 sustainable development goals by the United Nations addressing clean energy, industry, and innovation, sustainable cities, clean water, and responsible consumption and production. In this respect, also the development of analytical methods that enable the characterization of material flows in production processes and support recycling concepts of precious raw materials becomes more and more relevant. In the future, this will provide the basis for greener production in the chemical industry utilizing recycled or sustainable starting materials. This makes analytical chemistry an essential player in terms of the circular economy helping to increase the sustainability of production processes. In the life sciences sector, products based on proteins, such as therapeutic and diagnostic antibodies, increase in importance. These increasingly biotechnologically produced functional biomolecules pose a high level of complexity of matrix and structural features that can be met only by highly advanced methods for separation, characterization, and detection. In addition, metrological traceability and target definition are still significant challenges for the future, particularly in the life sciences. However, innovative reference materials as required for the health and food sector and the characterization of advanced materials can only be developed when suitable analytical protocols are available. The so-called reproducibility crisis in sciences underlines the importance of improved measures of quality control for all kinds of measurements and material characterization. This calls for thorough method validation concepts, suitable reference materials, and regular interlaboratory comparisons of measurements as well as better training of scientists in analytical sciences. The important contribution of analytical sciences to these developments is highlighted by a broad collection of research papers, trend articles, and critical reviews from these different application fields. Special emphasis is dedicated to often-overlooked quality assurance and reference materials. T2 - 150 years BAM: Science with impact CY - Berlin, Germany DA - 01.01.2021 KW - 150th anniversary KW - ABC KW - Analysis KW - Analytical sciences KW - BAM KW - Collection KW - Environment KW - Fluorescence KW - Life sciences KW - Limit of detection KW - Material sciences KW - Method KW - Nanoparticle KW - Pollutant KW - Quality assurance KW - Reference material KW - Sensor KW - Special issue KW - Bundesanstalt für Materialforschung und -prüfung KW - Jahrestag PY - 2022 UR - https://link.springer.com/journal/216/topicalCollection/AC_16a2ef9b81853377e321ef84d9c4a431 SN - 1618-2642 SN - 1618-2650 VL - 414 SP - 4267 EP - 4529 PB - Springer CY - Berlin AN - OPUS4-55670 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Burnage, Samual Charles T1 - Microfluidic Platform for Functionalisation, Extraction and Detection of Phosphorylated Amino Acids Using Fluorescent Sensory Particles N2 - The reliable identification and quantification of phosphorylated amino acids, peptides and proteins is one of the key challenges in contemporary bioanalytical research, noteworthy, to diagnose and treat diseases at an early developmental stage1. Miniaturised sensing devices like microfluidic chips combined with “smart” detection chemistry, simple data assessment, processing and presentation are very attractive for benchtop use in clinical environments. We developed novel synthetic probes targeting phosphorylated amino acids, based on core-shell microparticles consisting of a silica core coated with a molecularly imprinted polymer (MIP) shell. These “plastic antibodies” are extremely robust, resist denaturing solvents and elevated temperatures, can be reproducibly produced at low cost, and potentially overcome many of the practical problems in current bioanalytical detection strategies. The MIP layer contains a fluorescent probe monomer, binds selectively to phosphorylated tyrosine (pY) with a significant imprinting factor higher than 3.5 and responds with a “lighting-up” of its fluorescence accompanied by the development of a strongly red-shifted emission band toward the analyte. In analogy to our previous work4, the bead-based ratiometric detection scheme has also been successfully transferred to a microfluidic chip format to demonstrate its applicability to rapid assays. Such a miniaturised device could yield an automated pY measurement system in the future. The setup was built by coupling a modular microfluidic system5 for amino acid functionalisation (Fmoc protection) and, as shown in Figure 1, a multi-layer PDMS/Teflon/glass microfluidic chip6 for buffering, extraction (micropillars co-flow extraction) and selective adsorption on the MIP core-shell particles. A miniaturised optical assembly for low-light fluorescence measurements was also developed. Based on small opto-electronic parts and optical fibres, the emission from the MIP particles upon addition of pY concentrations from 0.5-200 μM could be monitored in real-time. T2 - GSS2019 CY - BAM Adlershof, Berlin, Germany DA - 29.08.2019 KW - MIPs KW - Microfluidics KW - Sensing KW - Fluorescence PY - 2019 AN - OPUS4-49202 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotthoff, Lisa T1 - Kopplung von Elektrochemie mit LC/MS zur Simulation von Transformationsprodukten - Untersuchung von Monensin N2 - Die Identifizierung von Transformationsprodukten (TPs) von Tierarzneimittelwirkstoffen ist wichtig für Gesundheit, Lebensmittel und Umwelt. Monensin (MON) gehört zu den Ionophoren Antibiotika und wird genutzt zum Schutz und zur Behandlung von Kokzidiose bei Geflügel, vorwiegend prophylaktisch in der Geflügelmast. Rückstände können in tierischen Produkten (Geflügel und Eier) aber auch in der Umwelt (Tiermist, Gewässer, Böden) gefunden werden. Verschiedene Transformationsprozesse können auftreten, beginnend bei der Biotransformation in lebenden Organismen bis hin zu biotischen und abiotischen Prozessen in der Umwelt. Die Kopplung von Elektrochemie und Massenspektrometrie, kurz EC/HRMS, als rein instrumenteller Ansatz zur Simulation von Transformationsprodukten ist seit vielen Jahren in der pharmazeutischen Forschung etabliert. Hierbei wird mithilfe einer elektrochemischen Durchflusszelle der oxidative Metabolismus einer Substanz simuliert und zugleich analysiert. Unter Verwendung von EC/HRMS und LC-HRMS wurde MON elektrochemisch bei Potentialen bis zu 2.5 V vs Pd/H2 oxidiert und die entstehenden TPs mit Metabolismustests mit Rattenlebermikrosomen verglichen. Als Ergebnis wurden verschiedene TPs von MON gefunden und Strukturvorschläge wurden erstellt. Ein Überblick über die detektierten und identifizierten TPs wird dargestellt. T2 - Lebensmittelsicherheit in Deutschland - was bleibt? CY - Potsdam-Rehbrücke, Germany DA - 04.06.2019 KW - Transformationsprodukte KW - Elektrochemie KW - Ionophore Antibiotika KW - Hochauflösende Massenspektrometrie PY - 2019 AN - OPUS4-48155 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Valderrey, Virginia T1 - Fluorescent Molecularly Imprinted Polymers N2 - The development of new strategies for the sensing of phosphorylated and carboxylate-containing biomolecules such as phosphorylated tyrosine and histidine or sialic acid is currently of strong interest because those molecules are often involved in cancerous processes. Molecularly Imprinted Polymers (MIPs) are formed through the polymerization of a set of functional monomers and cross-linkers in the presence of a target molecule or an analogue of it. The target molecule is incorporated into the polymer network due to non-covalent interactions established with one or more functional monomers. Because those interactions are weak, the target molecule can be desorbed a posteriori from the polymer matrix, leaving imprinted cavities of complementary size, shape and electronic nature. Resembling the antigen-binding site of an antibody, MIPs can then be highly selective towards the target molecule. Besides these features, our approach involves also the use of functional fluorescent monomers which undergo fluorescence changes upon binding of the target molecule. This allows us to investigate the sensing process using fluorescence as a highly sensitive read-out. To that aim we present here the use of silica particles which contain a MIP shell formed by thiourea or guanidinium functionalized dyes for the recognition of phosphorylated and carboxylate-containing molecules of biological relevance in polar, protic solvents. T2 - ANAKON 2019 CY - Münster, Germany DA - 25.03.2019 KW - Molecularly Imprinted Polymers KW - Fluorophores KW - Fluorescence PY - 2019 AN - OPUS4-47919 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotthoff, Lisa T1 - Electrochemistry coupled to LC/HRMS to investigate transformation products of the veterinary drug monensin N2 - The knowledge of transformation pathways and identification of transformation products (TPs) of veterinary drugs is important for health, food and environmental matters. Monensin (MON) is an ionophore antibiotic widely used to cure and prevent coccidiosis by chicken especially in broiler farming. Residues can be found in food products (chicken and eggs) and in the environment (manure, soil, water). Several transformation processes can alter the parent compound MON, ranging from biotransformation in living organism to biotic/abiotic and microbial processes in environmental matters. The main objective of this work was to investigate the potential of electrochemistry (EC) to simulate oxidative transformation processes of MON and to predict TPs. An electrochemical reactor was used consisting of a flow-through cell with a glassy carbon working electrode. Derived TPs were analyzed by online coupling of EC and high-resolution mass spectrometry (HRMS) and LC/HRMS offline measurements. Among the generated TPs already known as well as unknown TPs of MON could be found. Additionally, MON was subjected also to other transformation experiments like metabolism tests with rat microsomes or the pH-dependent hydrolysis. As a result, different targeted and suspected TPs could be identified by analysis with LC/HRMS. An overview of detected/identified TPs from this study will be presented in comparison to literature known metabolites and TPs. T2 - ElCheMS 2019 – 5th Workshop on Electrochemistry/Mass Spectrometry 2019 CY - Münster, Germany DA - 11.06.2019 KW - Transformation product KW - Electrochemistry KW - High-resolution MS KW - Ionophore antibiotic PY - 2019 AN - OPUS4-48209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kimani, Martha Wamaitha T1 - Dual-fluorescent sialic acid-imprinted polymer nanoparticles for staining of glycans on cancerous cells N2 - Cancer is a leading cause of death worldwide, and its early detection and resultant treatment contributes significantly to patient recovery and survival. Detection is currently based on magnetic resonance imaging and computed tomography, methods that are expensive, while processing of the results is time-consuming1. There is a need for low-cost cancer detection techniques that give conclusive results in the shortest time possible. When equipped with a reporter function, molecularly imprinted polymers (MIPs) targeting tumor markers on cancerous cells may provide a cheaper solution for imaging-based cancer detection. Thin MIP layers immobilized on particle platforms are ideal in this regard, because a fluorescence reporter can be integrated into the particle core and/or MIP shell and such core/shell nanoparticles show faster response times and increased selectivity in comparison to bulk MIPs. Changes in sialylation patterns of cell surface glycans indicate malignancy2. Here, we present the development of MIPs that target sialic acid-terminated glycans (SA MIPs), prepared as a thin layer on a polystyrene core/silica shell nanoparticle platform. The MIP particles contain fluorescent emitters and can be applied in fluorescence imaging of malignant tumors. Dynamic light scattering (DLS) and transmission electron microscopy (TEM) are used for structural characterization. Binding capacity of the MIPs to target glycans and competing sugars is also evaluated and compared to that of the corresponding non-imprinted polymer particles (NIP). T2 - Graduate Student Symposium on Molecularly Imprinted Polymers CY - Berlin, Germany DA - 29.08.2019 KW - Cancer KW - Sialic acid KW - MIPs PY - 2019 AN - OPUS4-48826 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuner, Maximilian T1 - Measuring the sum – A novel screening method for ergot alkaloids in food N2 - Ergot alkaloids play a significant role in human history for more than 1000 years and are part of the most common contaminants of food and feed worldwide. Their high toxicity against humans and livestock even at low concentrations causes a high demand for quick and reliable analytics even though no European limits for ergot alkaloids have been determined yet. Currently the most common methods for the quantitation of the six major ergot alkaloids and their corresponding stereoisomers are HPLC based, using either fluorescence or mass spectrometric detection. Whereas these conventional detection methods measure each compound individually, a novel approach is to transfer all ergot alkaloids to one basic structure, which could be measured as a sum parameter. Since all ergots contain a lysergic acid amide moiety and a differing peptide component, cleaving the molecule into a simple lysergic acid derivative, which could be quantified via either HPLC-FLD or MS/MS, is intended. To clean up the cleavage reaction mixture molecularly imprinted polymers (MIPs) are a simple and effective way to separate the desired structure. Due to the selectivity of MIPs, an improved matrix separation is expected, which results in fewer interferences in the FLD and the possibility to measure samples with more complex matrices. When fully developed, the novel method could overcome some major drawbacks of the conventional detection methods. Higher throughput and the need for less well-trained personnel are just two advantages, that should lead to a quick and cheap quantitation of ergot alkaloids. First results of this project will be presented, funded by the German ZIM program (Zentrales Innovationsprogramm Mittelstand) of the Federal Ministry for Economic Affairs and Energy. T2 - WMFmeetsIUPAC 2019 CY - Belfast, UK DA - 14.10.2019 KW - Ergot KW - Mycotoxins KW - Molecularly imprinted polymers PY - 2019 AN - OPUS4-49436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - LIBs–trends and developments for recycling applications N2 - Recent years have brought up many challenges for an analytical tracing of material flows. While planetary boundaries force end of life material into circular recycling pathways, geopolitical tension creates demands regarding the origin of raw materials. The analytical demands on any instrumentation to tackle the arising challenges of this scenario are straight forward: No sample preparation, precision in the percentage region, and high throughput at comparably low cost. All these demands make LIBS a perfect candidate, why it is time for a re-evaluation of how it exploits the potential possibilities arising from todays’ technology. While being a relatively young technique, the vast majority of conducted LIBS experiments still relies on well established instrumentation, sometimes ignoring the innovations and breakthroughs in the development of its empowering technology sectors such as battery powered compact high repetition rate lasers with tuneable pulse rate and length, low priced cameras with millions of small sized pixels and extremely fast shutter and readout times, optical modulators, galvonometer scanners, and simple robotics. In this talk we will showcase some examples on how the implantation of all these new tools can lead to extremely affordable and compact instrumentation with unprecedented acquisition speed and a spectral resolution sufficient to resolve atomic isotope lines. T2 - Institute Seminar CY - Rostock, Germany DA - 09.01.2024 KW - LIBS KW - Sorting KW - Automatisation PY - 2024 AN - OPUS4-62136 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sarma, Dominik A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Polystyrene Core−Silica Shell Particles with Defined Nanoarchitectures as a Versatile Platform for Suspension Array Technology N2 - The need for rapid and high-throughput screening in analytical laboratories has led to significant growth in interest in suspension array technologies (SATs), especially with regard to cytometric assays targeting a low to medium number of analytes. Such SAT or bead-based assays rely on spherical objects that constitute the analytical platform. Usually, functionalized polymer or silica (SiO2) microbeads are used which each have distinct advantages and drawbacks. In this paper, we present a straightforward synthetic route to highly monodisperse SiO2-coated polystyrene core−shell (CS) beads for SAT with controllable architectures from smooth to raspberry- and multilayer-like shells by varying the molecular weight of poly(vinylpyrrolidone) (PVP), which was used as the stabilizer of the cores. The combination of both organic polymer core and a structurally controlled inorganic SiO2 shell in one hybrid particle holds great promises for flexible next-generation design of the spherical platform. The particles were characterized by electron microscopy (SEM, T-SEM, and TEM), thermogravimetry, flow cytometry, and nitrogen adsorption/desorption, offering comprehensive information on the composition, size, structure, and surface area. All particles show ideal cytometric detection patterns and facile handling due to the hybrid structure. The beads are endowed with straightforward modification possibilities through the defined SiO2 shells. We successfully implemented the particles in fluorometric SAT model assays, illustrating the benefits of tailored surface area which is readily available for small-molecule anchoring. Very promising assay performance was shown for DNA hybridization assays with quantification limits down to 8 fmol. KW - core-shell particles KW - shell morphology KW - flow cytometry KW - scanning electron microscopy KW - stabilizer PY - 2016 DO - https://doi.org/DOI: 10.1021/acs.langmuir.6b00373 SN - 0743-7463 VL - 32 IS - 15 SP - 3717 EP - 3727 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-35833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Auditoren und Bewerterschulung - Bestimmung von Messunsicherheiten N2 - Analytische Kenngrößen von Messverfahren und Messergebnissen (wie Genauigkeit, Präzision und Richtigkeit) werden erläutert und Wege zur Abschätzung von Messunsicherheiten gegeben. T2 - Auditoren und Bewerterschulung CY - BAM, Berlin, Germany DA - 05.04.2017 KW - Messunsicherheit KW - Statistik KW - Richtigkeit KW - Präzision KW - Genauigkeit PY - 2017 AN - OPUS4-41106 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - QM Schulung - Bestimmung von Messunsicherheiten N2 - Unterschiedliche Verfahren zur Abschätzung von Messunsicherheiten als Kenngrößen analytischer Messergebnisse wird anhand von Beispielen erläutert. T2 - QM Weiterbildung CY - BAM, Berlin, Germany DA - 11.07.2017 KW - Messunsicherheit KW - GUM PY - 2017 AN - OPUS4-41107 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Borzekowski, Antje T1 - Fungi Isolated from Indonesian Tempeh Production Capable of Zearalenone Conjugation N2 - Zearalenone (ZEN) and its metabolites such as the phase II sulfate and glucoside conjugates have been detected in food and feed commodities1. In addition to these naturally occurring ZEN conjugates, food fermentation by fungi may also lead to conjugate formation. Fungal strains of the genera Rhizopus and Aspergillus are used in tempeh fermentation, and it is known that some strains can conjugate ZEN2. Moreover, during this process the reductive phase I metabolites α- and β-zearalenol (α-/β-ZEL) and their conjugates are formed by the same microorganisms in vitro. As the conjugates can be hydrolysed by human intestinal microbiota, also sulfates and glucosides represent a relevant source for the human exposure to ZEN. If the unprocessed grains for tempeh fermentation like soybeans and/or maize are contaminated with ZEN, upon analysis ZEN content of the final tempeh product may be underestimated, because ZEN has been conjugated during food processing. Very recently, the EU-CONTAM Panel found it appropriate to set a group tolerable daily intake (TDI) expressed as ZEN equivalents for ZEN and its modified forms (phase I and phase II metabolites)3. In this study a total of 70 strains of fungal species commonly found in tempeh fermentation were screened for ZEN metabolite formation in vitro. The fungal strains were isolated from inocula or fresh tempeh from different tempeh producers and market areas in Indonesia. ZEN (c = 0.3 µM) was added to liquid cultures of the fungi. After two days of incubation the media were analyzed for metabolite formation by HPLC-MS/MS. The conjugate formation varied with the fungal strain. In most cultures ZEN-14-sulfate was the major metabolite accompanied by rapid disappearance of ZEN; also, formation of α- and β-ZEL, ZEN-16-glucoside and two ZEL-sulfates has been observed. The in vitro-screening showed that fungal strains used in tempeh fermentation have the potential for ZEN conversion leading to ZEN and ZEL conjugate formation. Therefore, reference substances of ZEN conjugates are urgently needed for monitoring food safety of tempeh and other fermented products manufactured from grains that can be contaminated with ZEN. T2 - 39th Mycotoxin Workshop CY - Bydgoszcz, Poland DA - 19.06.2017 KW - Mycotoxin KW - Tempeh PY - 2017 AN - OPUS4-40964 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Koch, Matthias T1 - Development of certified reference material and analytical method for zearalenone in edible oil N2 - Quality and safety of food products require their reliable analysis. Contaminants, in particular mycotoxins, are key-components for food safety. About 25 % of the world's food crops are contaminated with mycotoxins posing a severe health risk to humans. In order to strengthen food safety and consumer protection the European Commission (EC) set maximum levels for priority mycotoxins in certain foods for human consumption. In 2013, the EC and CEN (European Committee for Standardization) started an initiative to standardize analytical methods for mycotoxins in food which gained increasing relevance, e.g. zearalenone (ZEN). ZEN, an estrogenic mycotoxin produced by several Fusarium species, contaminates cereal crops worldwide. Due to its lipophilic nature ZEN is often found in edible oils (particularly in maize germ oils) derived from contaminated plants. Therefore, an European maximum level of 400 µg/kg is currently in force. To perform reliable food analysis a sustainable metrological infrastructure is of major importance enabling the quantification of priority mycotoxins (here: ZEN). To achieve this goal, an integrated approach is needed targeted at the development of validated analytical methods and certified reference materials (CRM). A highly selective method for ZEN in edible oils will be presented, based on solid phase extraction (SPE) using hydrazine-functionalized particles. This method was developed for manual application using commercial SPE cartridges as well as for automated SPE-HPLC online coupling. While ZEN is covalently coupled to the solid phase by means of a hydrazone bond, undesired matrix components can be removed very efficiently. Finally, ZEN is decoupled from the solid phase, leading to highly purified extracts which are measured by HPLC-FLD. The development of the first European Reference Material (ERM®) for ZEN in maize germ oil (ERM®-BC715) will be presented and discussed. This ERM®-project underpins the urgent need for mycotoxin-CRMs to support food safety and public health. T2 - 40. Generalversammlung ISO/REMCO CY - Berlin, Germany DA - 27.06.2017 KW - Certified reference materials KW - Mycotoxin KW - Food PY - 2017 AN - OPUS4-40902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Temgoua, Ranil C. T. T1 - Hyphenated Electrochemistry Mass Spectrometry (EC MS): A Powerful Tool for Investigating the Environmental Fate of Emerging Contaminants N2 - Electrochemistry coupled to mass spectrometry (EC-MS) is emerging as a powerful and versatile technique for studying chemical transformations in various fields. This communication provides an overview of recent advances in EC-MS, focusing on its applications in drug metabolism studies, environmental degradation of xenobiotics, and green synthesis of analytical standards. EC-MS offers significant advantages over conventional methods, including in situ simulation of metabolic and environmental processes, rapid generation of transformation products, and the possibility of performing milligram-scale syntheses with a reduced environmental footprint. The major contributions of leading equipment manufacturers, such as Antec Scientific for electrochemistry and Agilent, Shimadzu, Thermo Fisher Scientific, Bruker, Waters, and Sciex for mass spectrometry, will be highlighted. Finally, a portion of our work on the ecotoxicity study of neonicotinoid pesticides, using EC-MS, will be presented to illustrate the potential of this technique. Our study investigates the formation of degradation products from electrochemical reactors (EC) for neonicotinoid insecticides and phenylurea herbicides. T2 - 29th meeting of the RCJSM (Youth Club of the French Society of Mass Spectrometry CY - Toulouse, France DA - 31.03.2025 KW - Material safety KW - Quality ensurance KW - Chemical safety PY - 2025 AN - OPUS4-63530 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Döring, Sarah T1 - Surface Immobilization of Recombinant Trypsin onto Corundum Particles for Optimized Antibody Digestion N2 - Therapeutic monoclonal antibodies are the fastest-growing class of biological agents and the development of reliable analytical methods for their quantification is becoming increasingly important. Liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) represents one of the leading technologies for antibody quantification. The serin protease trypsin has emerged as the gold standard enzyme for digesting intact protein into peptides for this approach. However, many protocols exist that often lead to different results depending on the digestion procedure. In particular, the type and amounts of detergents added during sample preparation for protein unfolding before digestion is known to create undesirable structure modifications of proteins (e.g. carbamylation) and significant bias in measurement results by inhibiting enzyme activity. The source and nature of the enzyme itself can also have an influence, whereby immobilized variants are increasingly being used to improve their stability, minimize self-digestion and enable a higher substrate-enzyme ratio. Here, we explored the potential of a novel thermostable trypsin and surface-functionalised corundum particles for enhanced antibody digestion. For this purpose, the inactive zymogen was recombinantly produced in E. coli, activated with enterokinase digestion and finally affinity purified by benzamidine purification. The enzyme activity was analogous to commercially available MS-grade trypsin product. In addition, produced trypsin showed increased thermal stability under typical digestion conditions compared to reference product. Furthermore, APTES-silanization followed by glutaraldehyde modification of corundum surface with an additional blocking step prevents nonspecific protein adsorption during the protein digestion procedure and the immobilized enzyme still showed substrate activity after covalent binding. Compared to wild-type and a non-immobilized enzyme, the surface-functionalized thermostable variant showed increased activity at elevated temperatures. Thus, this novel type of trypsin particles promises to not only improve antibody digestion at high temperatures, but also to prevent self-digestion and enable the separation of trypsin from target peptides in LC–MS analysis. T2 - ANAKON 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Antibody Quantification KW - Corundum KW - Enzyme Immobilization KW - LC-MS/MS PY - 2025 AN - OPUS4-63480 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Bestimmung von Halogen in Metallen mittels spektrometrischer Verfahren N2 - Die metallischen Verunreinigungen in Metallen lassen sich mittels hochauflösender Massenspektrometer relativ einfach ermitteln. Die Glimmentladungs-Massenspektrometrie (GD-MS) stellt hierfür eine schnelle Multielementmethode dar. Aufgrund ihrer höheren Anregungs- und Ionisationsenergien ist die Bestimmung von Nichtmetallen eine weit größere Herausforderung. Außerdem fehlt es an für die direkte Feststofftechnik notwendigen Kalibrierstandards z.B. in Form zertifizierter Referenzmaterialien. Für die quantitative Bestimmung von Verunreinigungen wurden mit Standards dotierte Pulverpresslinge und dotierte, gesinterte Materialien auf ihre Eignung als Kalibrierstandards für die GD-MS untersucht. Dabei kamen unterschiedliche Plasmabedingungen (gepulster/ kontinuierlicher Betrieb; verschiedene Plasmagase) zum Einsatz. Ein Überblick über analytische Kenngrößen und Grenzen der verwendeten Kalibrierstrategien wird gegeben. Zur Validierung des Verfahrens wurde die hochauflösende Continuum Source Absorptionsspektrometrie (HR-CS-MAAS) verwendet. Die analytische Nutzung der Molekül-absorptionsspektrometrie zur Bestimmung von Halogenen basiert auf der Bildung insitu-generierter zweiatomiger Moleküle (AlCl, GaF). Die entstehenden Molekülspektren werden im Echelle-Spektrometer aufgespalten und mittels CCD-Array detektiert, was eine sehr empfindliche Messung und präzise Quantifizierung ermöglicht. T2 - CANAS CY - Freiberg, Germany DA - 23.09.2019 KW - Spectroscopy KW - Halogene KW - Reinstmetalle PY - 2019 AN - OPUS4-49450 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Bestimmung von halogen in Metallen mittels spektrometrischer Verfahren N2 - Die metallischen Verunreinigungen in Metallen lassen sich mittels hochauflösender Massenspektrometer relativ einfach ermitteln. Die Glimmentladungs-Massenspektrometrie (GD-MS) stellt hierfür eine schnelle Multielementmethode dar. Aufgrund ihrer höheren Anregungs- und Ionisationsenergien ist die Bestimmung von Nichtmetallen eine weit größere Herausforderung. Außerdem fehlt es an für die direkte Feststofftechnik notwendigen Kalibrierstandards z.B. in Form zertifizierter Referenzmaterialien. Für die quantitative Bestimmung von Verunreinigungen wurden mit Standards dotierte Pulverpresslinge und dotierte, gesinterte Materialien auf ihre Eignung als Kalibrierstandards für die GD-MS untersucht. Dabei kamen unterschiedliche Plasmabedingungen (gepulster/ kontinuierlicher Betrieb; verschiedene Plasmagase) zum Einsatz. Ein Überblick über analytische Kenngrößen und Grenzen der verwendeten Kalibrierstrategien wird gegeben. Zur Validierung des Verfahrens wurde die hochauflösende Continuum Source Absorptionsspektrometrie (HR-CS-MAAS) verwendet. Die analytische Nutzung der Molekül-absorptionsspektrometrie zur Bestimmung von Halogenen basiert auf der Bildung insitu-generierter zweiatomiger Moleküle (AlCl, GaF). Die entstehenden Molekülspektren werden im Echelle-Spektrometer aufgespalten und mittels CCD-Array detektiert, was eine sehr empfindliche Messung und präzise Quantifizierung ermöglicht. T2 - CANAS 2019 CY - Freiberg, Germany DA - 23.09.2019 KW - Halogene PY - 2019 AN - OPUS4-49610 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Bestimmung von Nichtmetallen in Carbiden N2 - Vortrag zur Bestimmung von Nichtmetallen in Carbiden halten. Hierbei geht es um die Bestimmung von C, O und N in Vanadiumcarbid, Wolframcarbid und Niobcarbidmaterialien, einen hierzu durchgeführten Ringversuch mit Beteiligung der Kollegen des AK Sonderwerkstoffe und den Vergleich von Verfahrenskenngrößen. T2 - Vollversammlung Chemikerausschuss der GDMB CY - Kassel, Germany DA - 05.11.2019 KW - Niobcarbid KW - Wolframcarbid KW - Vanadiumcarbid KW - Nichtmetalle PY - 2019 AN - OPUS4-50261 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kislenko, Evgeniia T1 - Fluorescent molecularly imprinted polymers (MIPs) for sensing of phosphorylated protein epitopes N2 - Early detection of cancer is instrumental for successful therapeutic outcomes, but it is presently a considerable challenge. Biopsy of potentially cancerous tissues is the gold standard in medicine for the diagnosis and prognosis of this disease; however, it may not be possible in many cases due to tumour position or other complications. Liquid biopsy-based detection of specific cancer markers in biological fluids can be easily performed via immunoanalytical techniques. However, antibody-based methods suffer from high cost of tumour specific antibodies due to difficult and lengthy production. Furthermore, antibodies may have limited specificity to the target molecule, and limited lifetimes. The so-called “plastic antibodies” as MIPs can be a more affordable, reliable and stable alternative to antibodies, especially for cancer diagnostics. Our goal is to create MIP particles to selectively bind cancer biomarkers and rapidly display a fluorescence change upon interaction with molecules of interest. Epitopes containing the phosphorylated tyrosine (pY) motif such as tripeptide YpYG and tetrapeptide pYEEI were selected as target analytes. Cancers may disrupt tyrosine phosphorylation processes regulated by human tyrosine kinases such as ZAP-70 and subsequently lead to a pronounced increase in pY residues on proteins. To ensure fast diffusion of analyte and rapid response core/shell silica micro- and nanoparticles with a thin polymer shell was chosen as the format for MIP synthesis. Fluorescent probe monomers consisting of fluorophore and recognition units are directly integrated in the polymer shell to obtain fluorescence response upon analyte binding. We have synthesized the fluorescent MIP particles based on the previously published report [W. Wan et al., Chem. Eur. J., 2017, 23, 15974-1598] for the novel phosphorylated targets with a high imprinting factor and high degree of discrimination between target analyte and non-phosphorylated and smaller competitors. The synthesized particles may be used in microfluidic devices for the rapid diagnostics of cancer. T2 - GSSMIP2019 CY - Berlin, Germany DA - 28.08.2019 KW - Analytical Sciences KW - Sensorik PY - 2019 AN - OPUS4-50227 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kislenko, Evgeniia T1 - Fluorescent molecularly imprinted polymers (MIPs) for sensing of phosphorylated protein epitopes N2 - Early detection of cancer is instrumental for successful therapeutic outcomes, but it is presently a considerable challenge. Biopsy of potentially cancerous tissues is the gold standard in medicine for the diagnosis and prognosis of this disease; however, it may not be possible in many cases due to tumour position or other complications. Liquid biopsy-based detection of specific cancer markers in biological fluids can be easily performed via immunoanalytical techniques. However, antibody-based methods suffer from high cost of tumour specific antibodies due to difficult and lengthy production. Furthermore, antibodies may have limited specificity to the target molecule, and limited lifetimes. The so-called “plastic antibodies” as MIPs can be a more affordable, reliable and stable alternative to antibodies, especially for cancer diagnostics. Our goal is to create MIP particles to selectively bind cancer biomarkers and rapidly display a fluorescence change upon interaction with molecules of interest. Epitopes containing the phosphorylated tyrosine (pY) motif such as tripeptide YpYG and tetrapeptide pYEEI were selected as target analytes. Cancers may disrupt tyrosine phosphorylation processes regulated by human tyrosine kinases such as ZAP-70 and subsequently lead to a pronounced increase in pY residues on proteins. To ensure fast diffusion of analyte and rapid response core/shell silica micro- and nanoparticles with a thin polymer shell was chosen as the format for MIP synthesis. Fluorescent probe monomers consisting of fluorophore and recognition units are directly integrated in the polymer shell to obtain fluorescence response upon analyte binding. We have synthesized the fluorescent MIP particles based on the previously published report for the novel phosphorylated targets with a high imprinting factor and high degree of discrimination between target analyte and non-phosphorylated and smaller competitors. The synthesized particles may be used in microfluidic devices for the rapid diagnostics of cancer. T2 - GSSMIP2019 CY - Berlin, Deutschland DA - 28.08.2019 KW - Analytical Sciences KW - Sensorik PY - 2019 AN - OPUS4-50228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kuner, Maximilian T1 - Measuring the sum – A novel screening method for ergot alkaloids in food N2 - Ergot alkaloids play a significant role in human history for more than 1000 years and are part of the most common contaminants of food and feed worldwide. Their high toxicity against humans and livestock even at low concentrations causes a high demand for quick and reliable analytics even though no European limits for ergot alkaloids have been determined yet. Currently the most common methods for the quantitation of the six major ergot alkaloids and their corresponding stereoisomers are HPLC based, using either fluorescence or mass spectrometric detection. Whereas these conventional detection methods measure each compound individually, a novel approach is to transfer all ergot alkaloids to one basic structure, which could be measured as a sum parameter. Since all ergots contain a lysergic acid amide moiety and a differing peptide component, cleaving the molecule into a simple lysergic acid derivative, which could be quantified via either HPLC-FLD or MS/MS, is intended. To clean up the cleavage reaction mixture molecularly imprinted polymers (MIPs) are a simple and effective way to separate the desired structure. Due to the selectivity of MIPs, an improved matrix separation is expected, which results in fewer interferences in the FLD and the possibility to measure samples with more complex matrices. When fully developed, the novel method could overcome some major drawbacks of the conventional detection methods. Higher throughput and the need for less well-trained personnel are just two advantages, that should lead to a quick and cheap quantitation of ergot alkaloids. First results of this project will be presented, funded by the German ZIM program (Zentrales Innovationsprogramm Mittelstand) of the Federal Ministry for Economic Affairs and Energy. T2 - WMFmeetsIUPAC 2019 CY - Belfast, UK DA - 14.10.2019 KW - Ergot KW - Mycotoxins KW - Molecularly imprinted polymers PY - 2019 AN - OPUS4-49437 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hesse, Almut A1 - Biyikal, Mustafa A1 - Rurack, Knut A1 - Weller, Michael G. T1 - Development of highly sensitive and selective antibodies for the detection of the explosive pentaerythritol tetranitrate (PETN) by bioisosteric replacement N2 - An improved antibody against the explosive pentaerythritol tetranitrate (PETN) was developed. The immunogen was designed by the concept of bioisosteric replacement, which led to an excellent polyclonal antibody with extreme selectivity and immunoassays of very good sensitivity. Compounds such as nitroglycerine, 2,4,6-trinitrotoluene, 1,3,5-trinitrobenzene, hexogen (RDX), 2,4,6-trinitroaniline, 1,3-dinitrobenzene, octogen (HMX), triacetone triperoxide (TATP), ammonium nitrate, 2,4,6-trinitrophenol and nitrobenzene were tested for potential cross-reactivity. The detection limit of a competitive enzyme-linked immunosorbent assay (ELISA) was determined to be around 0.5 µg/L. The dynamic range of the assay was found to be between 1 µg/L and 1000 µg/L, covering a concentration range of three decades. This work shows the successful application of the bioisosteric concept in immunochemistry by exchange of a nitroester to a carbonate diester. The antiserum might be used for the development of quick tests, biosensors, microtitration plate immunoassays, microarrays and other analytical methods for the highly sensitive detection of PETN, an explosive frequently used by terrorists, exploiting the extreme difficulty of its detection. KW - bioisosteric replacement KW - immunoassay KW - antibody KW - explosives KW - hapten KW - Semtex KW - ELISA KW - security KW - terrorism PY - 2016 UR - http://onlinelibrary.wiley.com/doi/10.1002/jmr.2511/abstract DO - https://doi.org/10.1002/jmr.2511 SN - 1099-1352 VL - 29 SP - 88 EP - 94 PB - John Wiley & Sons, Ltd. CY - New York, USA AN - OPUS4-35827 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - The Integration of Fluorescent Probes with Sensing Matrices N2 - Integrating fluorescent probes with sensing matrices presents a major challenge because usually, when confined in a rather rigid matrix, fluorophores tend to behave completely different than for instance in the molecular state in solution. The lecture reviews the major strategies that have been devised recently to circumvent such issues with special focus on the works carried out in this field by BAM’s Chemical and Optical Sensing Division. Moreover, it will be shown that by using certain strategies not only can the response behavior be retained but synergistic effects can even endow the hybrid with a much better performance than the probe molecule alone. T2 - GDCh-Kolloquium CY - Braunschweig, Germany DA - 14.11.2016 KW - Fluorescence KW - Probes KW - Sensor KW - Molecularly imprinted polymers KW - Gated release systems PY - 2016 AN - OPUS4-38794 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Improving the Sensing Performance of Macrocycle-containing Fluorescent Probes by Integration into Mesoporous Silica N2 - Macrocycle-containing fluorescent probes continue to be one of the most popular classes of indicator molecules for the sensitive optical detection of ionic inorganic analytes, in particular metal ions, since the first integration of crown ether building blocks into chromophoric π systems more than 30 years ago. However, whereas a large multitude of such probes have been described for operation in organic or mixed aqueous environments, the step to realistic analytical media such as water samples, aqueous food extracts or body fluids is still scarce. On one hand, this is due to considerably low complex stability constants for instance for alkali and alkaline-earth metal ions. On the other hand, many classes of organic dyes that show favourable spectroscopic properties and ion-induced responses in organic solvents are not soluble in neat aqueous media and/or exhibit only significantly quenched fluorescence, even if transition metal ions are binding strongly to the receptor unit. A way to circumvent such problems in a rather simple manner is the steric incorporation of fluorescent probes into mesoporous silica nanomaterials. The local polarity in such pores, whether nascent or modified appropriately with functional silanes, resembles much more a quasi-organic environment while at the same time allowing for free diffusion of water and its cargo. Two examples of powerful hybrid signalling systems will be presented, utilizing charge transfer-type indicator molecules that show inferior sensing properties in their molecular state. One example discusses mercury(II) determination over an extended concentration range and the other discusses silver(I) and mercury(II) discrimination simply on the basis of photophysical effects retained in the hybrid materials. T2 - The 1st Nanjing/Dijon Symposium on Functional Macrocyclic Molecules CY - Nanjing, People's Republic of China DA - 09.07.2016 KW - Fluorescence KW - Probes KW - Macrocycles KW - Mesoporous Silica KW - Sensor PY - 2016 AN - OPUS4-38795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Purity Statements of High purity N2 - Purity statements of high purity materials serving as primary standards by GDMS. Primary standards are materials known for their total purity and therefore appropriate to realise the link with the International System of Units (SI). The realisation and dissemination of primary standards is of fundamental importance for comparability of measurement results through traceability in all fields of chemical analysis. To serve as a primary standard for element determination the total purity of a high purity material needs to be measured. In order to achieve a sufficiently small uncertainty (i.e. < 0.01%) this involves determining all possible impurity contributions and to subtract their sum from the ideal purity of 100%. GD-MS has the potential to reduce the effort for purity determination, as a fast sensitive multi-element analysis without extensive sample preparation. Similar to other solid sampling techniques, glow discharge requires calibration link the measured signal and the content of the impurities in the matrix. The use of the concept Relative Sensitivity Factors (RSFs) provides good approximations especially for high purity materials. However, it only works with a wide uncertainty of the results. The preparation of synthetic pressed powder samples by different modifications of liquid and powder doping used for the determination of both metallic and none-metallic impurities are described. Efficient determination of metallic impurities by GD-MS via differential and absolute measurements with a significantly reduced target uncertainty of 20 % for absolute measurements using liquid doped pressed powder calibration could be achieved. The determination of impurities has been evaluated by independent analytical methods such as HR-ICP-MS, ETAAS; CGHE and combustion analysis T2 - The 3 rd International Glow Discharge Spectroscopy Symposium IGDSS2016 CY - Liverpool, UK DA - 17.04.2016 KW - Metrology KW - GDMS KW - Purity KW - Standards PY - 2016 AN - OPUS4-38726 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Bright Long-Wavelength Pyrrolic Dyes - Prospects for Applications in Fluorescence Sensing N2 - Since more than 20 years, optical spectroscopic techniques, in particular fluorescence-based methods, are on the rise in many different areas of chemical and biochemical analysis, with no end being in sight.1,2 Advances in miniaturization and remote applications on one hand and ground-breaking developments in microscopy and laser-based high-throughput instrumentation on the other hand have fuelled these developments substantially.3,4 At the core of utmost of these applications however is not only the instrument, but a small entity that is able to absorb and emit photons and thus to report on the actual (bio)chemistry that is going on in a particular sample of interest.5,6 Besides intense research on various types of luminescent particles (e.g., quantum dots and carbon dots) and proteins, dye chemistry has thus seen its revival and the number of publications dealing with the design, synthesis and application of new fluorescent dyes as probes, stains, labels or indicators is still continuing to grow. Among the various classes of dyes available as bright fluorophores for a wavelength range that is compatible with many (bio)analytical applications and the respective instrumentation, in particular pyrrolic dyes that do not belong to the classical porphyrins or phthalocyanines have received strong attention recently. Starting perhaps with the revival of the traditional boron-dipyrromethene laser dye ca. 15 years ago,7 these so-called BODIPYs have developed into a colourful spectrum of different derivatives.8 However, the interest in expanding the range of pyrrole-containing π-systems beyond BODIPYs has also constantly increased and has brought about several other pyrrole-based ring systems such as diketopyrrolopyrroles9 or dipyrrolonaphthyridinediones which possess a favourable brightness and other interesting properties. The present contribution will give a critical overview of the field, pinpointing advantages and prospects as well as discussing potential aspects of improvement with an emphasis on the chemical sensing and the longer wavelength range. T2 - Ninth International Conference on Porphyrins and Phthalocyanines CY - Nanjing, People's Republic of China DA - 03.07.2016 KW - Fluorescence KW - Dyes KW - Sensor KW - NIR KW - Pyrroles PY - 2016 AN - OPUS4-38796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia T1 - Interactions of (1,3-dicarbonyl)-mycotoxins and metal ions N2 - Mycotoxins are secondary metabolites of fungi which have diverse detrimental effects on humans, animals and crops. Traceable worldwide in foods and animal feeds, these contaminants cause manifold diseases and extensive economic losses. Therefore, European legislation set maximum levels of distinct mycotoxins to minimize the risks for the buying public. But standardized food analysis techniques fail to detect masked mycotoxins, whose research increasingly moves to the fore in recent years. They are formed from detoxification metabolism of plants as well as from fungi, which conjugate for example with glucosides or dihexosides. All masked mycotoxins have one thing in common: They are not detectable with standard methods, thereby contributing to the overall exposure and pose an additional health risk for the consumer. The dissertation work will focus on the following potential new group of masked toxins. Food safety relevant mycotoxins like zearalenone and ochratoxin A possess one or more 1,3-dicarbonyl moieties. Latter are principally able to form thermodynamically stable chelate complexes with metal cations. First investigations at BAM showed interactions between zearalenone and copper ions and it is conceivable that they possibly build a complex. Our main focus is now to identify, characterize and quantify 1,3-dicarbonyl mycotoxin metal complexes as potential candidates within the group of conjugated mycotoxins. We will simulate processes of biotransformation and identify distinct metabolites by electrochemistry coupled to liquid chromatography/mass spectrometry (EC-HPLC-MS). The obtained knowledge contributes to a better understanding of masked mycotoxins and an improved monitoring of foods and feeds, to ensure food safety. T2 - BAM PhD Retreat CY - Wandlitz, Germany DA - 05.06.2015 KW - Mycotoxins KW - Metal ions PY - 2015 AN - OPUS4-38222 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sarma, Dominik T1 - Hybrid Core-Shell Particles in Diagnostic Applications - a versatile platform for multiplexed cytometric bead assays N2 - Multiplexed bead-based array formats play an increasingly important role in analytical laboratories. Due to the high surface-to-volume ratio, fast reaction kinetics and modular assay design, these sensor formats are applied in clinical diagnostic, drug development and classical biosensors with great success. As the spherical platform, researchers utilize micron sized particles made from polymeric or silica material. Such beads are commercially available from vendors such as BD or Luminex. However, we have encountered several problematic issues which accompany these platforms: first, bigger sized beads, which are required for particle handling reasons, are difficult to prepare with high monodispersity - a key requirement for cytometric application. Second, plain beads, made from either polymer or silica, have each several disadvantages such as inferior scattering properties in case of silica or limited flexibility for coupling strategies in the case of latex beads. In order to overcome this problem, we have developed a versatile core-shell (CS) platform which consists of a polymeric core with a structurally controlled silica shell. In our approach, the core building block can be easily prepared with high yields and high monodispersity in a dispersion polymerization from approximately 500 nm to 1.3 µm. Then, silica is coated in a classical sol-gel process to protect the core with a stable yet modifiable surface (see SEM image in Figure 1, platform). Here, we combine ideal scattering properties and easy preparation of the polymeric core with the chemical flexibility of a silica surface. Moreover, the additional shell domain adds density to the composite, which makes particle handling feasible also for nanometer sized beads. In this contribution we present proof-of-principle results of competitive immunoassays with fluorescence detection using our CS beads – each performed in mix-and-read fashion without washing steps. All sizes are applicable in cytometric read-out which and can be used for size encoding (see Set 1 to 3 in Figure 1, size encoding). However, further multiplexing for a set of at least 20 parameters can be achieved by swelling hydrophobic dyes into the core. To the same time, precise tuning of the surface with mixed silane layers allowed us to improve the selectivity towards small molecules in competitive immunoassays significantly (see example in Figure 1, Application). We believe that our platform allows researchers to gain access to superior assay performance in combination with a low-threshold approach for the synthesis of the spherical platform. T2 - Functional Nanomaterials in Industrial Applications CY - Preston, UK DA - 29.03.2016 KW - Core/shell particles KW - Cytometry KW - Multiplexing KW - Diagnostics KW - Hybrid materials PY - 2016 AN - OPUS4-38797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia T1 - Electrochemistry-mass spectrometry (EC-MS) as a versatile tool to simulate the biotransformation of citrinin – A comparative study N2 - Mycotoxins can be found worldwide in foods and feed and cause a variety of mold-related health risks which makes it necessary to further examine their toxic effects and metabolic fate in human and other mammals. Beside standard in vitro and in vivo assays with liver cell preparations or rodents an increasing interest in new simulation methods are playing a growing role. Electrochemistry (EC) is one of these novel techniques and has been used successfully and efficiently in pharmacological and drug research for several years now. The primary objective of this study was to determine the capability of EC as a supportive and versatile instrument to elucidate metabolic pathways of mycotoxins. On the example of the food relevant mycotoxin Citrinin a coulometric flow through cell equipped with a carbon working electrode was used to oxidize Citrinin by applying potential between 0.7 and 2.5 V vs. Pd/H2. The electrochemically generated oxidation products were then analyzed by mass-spectrometric detection coupled online to EC (EC-MS) and compared with data from a standard in vitro model with human and rat liver microsomes preparations. To receive a comprehensive assessment of oxidative techniques chemical oxidation by Fenton´s reaction was performed as well. The obtained LC-MS/MS data confirmed the production of Dihydrocitrinone by all of the three tested oxidation systems and demonstrates the potential of EC-MS for the successful prediction of the main phase I metabolic reactions of mycotoxins, since Dihydrocitrinone is the mainly formed metabolite by humans after intake of Citrinin. Beside the identified Dihydrocitrinone from electrochemical, enzymatic and chemical oxidation of Citrinin there is still a number of yet unknown compounds. As the next step structural characterization of the generated oxidation products by NMR and X-ray analysis will be enabled by their large-scale production using preparative EC cells. T2 - Rapid Methods CY - Amsterdam, The Netherlands DA - 07.11.2016 KW - Electrochemistry KW - Mycotoxin KW - Oxidation PY - 2016 AN - OPUS4-38215 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wander, Lukas A1 - Paul, Andrea A1 - Rurack, Knut A1 - Biyikal, Mustafa A1 - Juritsch, Elevtheria A1 - Bernstein, Thomas A1 - Bartholmai, Matthias A1 - Noske, Reinhard T1 - Kompaktsensor zur Online-Überwachung von Nitroaromaten N2 - Nitroaromaten und insbesondere Trinitrotoluol (TNT) sind weit verbreitete Spreng- und Umweltschadstoffe. Die größte Herausforderung bei der Detektion von TNT in der Gasphase ist der geringe Dampfdruck. Derzeit werden vielerorts günstige, schnelle, handliche und einfach zu bedienende Alternativen zur klassischen TNT-Analytik entwickelt. Aktuell existieren keine einheitlichen Richtlinien für Sprengstoffsensoren. Hier wird die Entwicklung eines Messplatzes zur Validierung von Sprengstoffsensoren sowie die Erprobung eines kompakten Mustersensors vorgestellt. T2 - 12. Kolloquium Prozessanalytik CY - Berlin, Germany DA - 28.11.2016 KW - Nitroaromaten KW - Fluoreszenzlöschung KW - Sensor PY - 2016 SP - P11, 61 EP - 62 AN - OPUS4-38402 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abdelshafi, Nahla A. A1 - Bell, Jérémy A1 - Rurack, Knut A1 - Schneider, Rudolf T1 - Microfluidic electrochemical immunosensor for the trace analysis of cocaine in water and body fluids N2 - Quick but accurate testing and on‐the‐spot monitoring of cocaine in oral fluids and urine continues to be an important toxicological issue. In terms of drug testing, a number of devices have been introduced into the market in recent decades, notably for workplace inspection or roadside testing. However, these systems do not always fulfill the requirements in terms of reliability, especially when low cut‐off levels are required. With respect to surface water, the presence of anthropogenic small organic molecules such as prescription and over‐the‐counter pharmaceuticals as well as illicit drugs like cannabinoids, heroin, or cocaine, has become a challenge for scientists to develop new analytical tools for screening and on‐site analysis because many of them serve as markers for anthropogenic input and consumer behavior. Here, a modular approach for the detection of cocaine is presented, integrating an electrochemical enzyme‐linked immunosorbent assay (ELISA) performed on antibody‐grafted magnetic beads in a hybrid microfluidic sensor utilizing flexible tubing, static chip and screen‐printed electrode (SPE) elements for incubation, recognition, and cyclic voltammetry measurements. A linear response of the sensor vs. the logarithm of cocaine concentration was obtained with a limit of detection of 0.15 ng/L. Within an overall assay time of 25 minutes, concentrations down to 1 ng/L could be reliably determined in water, oral fluids, and urine, the system possessing a dynamic working range up to 1 mg/L. KW - ELISA KW - Kokain KW - Lab-on-chip KW - Speichel KW - Urin KW - Drogenanalytik KW - Schnelltest KW - Biosensor PY - 2018 DO - https://doi.org/10.1002/dta.2515 SN - 1942-7611 VL - 11 IS - 3 SP - 492 EP - 500 PB - Wiley-VCH CY - Hoboken, New Jersey, USA AN - OPUS4-46888 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kyrey, T. A1 - Ganeva, M. A1 - Gawlitza, Kornelia A1 - Witte, J. A1 - von Klitzing, R. A1 - Soltwedel, O. A1 - Di, Z. A1 - Wellert, S. A1 - Holderer, O. T1 - Grazing incidence SANS and reflectometry combined with simulation of adsorbed microgel particles N2 - Adsorbed ethylene glycol based microgel particles on a Silicon surface were studied. Neutron reflectometry (NR) and grazing incidence small-angle neutron scattering (GISANS) were performed to investigate their internal structure. Scattering experiments on soft matter systems such as adsorbed microgels often give only partial Information about the inner structure of the polymer system. In this contribution, we discuss how the detailed inner structure of adsorbed microgel particles can be reconstructed by a combination of the specular Neutron Reflectivity (NR), Grazing Incidence Small Angle Neutron Scattering (GISANS), Atomic Force Microscopy (AFM) and a simulation in the framework of the Distorted Wave Born Approximation. KW - Grazing incidence small-angle neutron scattering KW - Neutron reflectometry KW - BornAgain simulation KW - Adsorbed microgel particles PY - 2018 DO - https://doi.org/10.1016/j.physb.2018.03.049 SN - 0921-4526 VL - 551 SP - 172 EP - 178 PB - Elsevier B.V. AN - OPUS4-47011 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Qualitätssicherung in der Analytischen Chemie - Genauigkeitskenngrößen N2 - Die Junganalytiker der Fachgruppe „Analytische Chemie“ der Gesellschaft Deutscher Chemiker (GDCh) veranstalteten in Zusammenarbeit mit der BAM eine Herbstschule zum Thema „Qualitätssicherung in der Analytischen Chemie“. Schulung v.a. für Doktoranden, um den Umgang mit qualitätssichernden Aspekte bei der Entwicklung analytischer Methoden zu erlernen. Die wichtigsten Grundbegriffe der Genauigkeitskenngrößen von Messgrößen werden in diesem Vortrag vermittelt. T2 - GDCH Herbstschule 2018 CY - Berlin, Germany DA - 29.10.2018 KW - Genauigkeit KW - Unsicherheitsabschätzung KW - RIchtigkeit KW - Präzision KW - Validierung PY - 2018 AN - OPUS4-46682 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo T1 - Ammoniakbestimmung mit einem portablen Fluoreszenzsensor N2 - Ammoniakemissionen in die Umwelt erfolgen insbesondere durch die Landwirtschaft (93,6 %), aber auch durch Verbrennungsprozesse in der die Abfallwirtschaft (2,3 %) und den Straßenverkehr (1,8 %). Dieser Stoff ist selbst in geringen Konzentrationen nicht nur eine Geruchsbelästigung, sondern auch eine Substanz mit ökologischer und klimatischer Relevanz. Die Bestimmung von Ammoniak in relevanten Konzentrationen von kleiner 25 μg m-3 erfolgt im Allgemeinen über NH4+ als Analyten, spektralfotometrisch oder mit der Ionenchromatographie nach Überführung in die flüssige Phase. Wegen der niedrigen Konzentrationen an Ammoniak in der Außenluft wird meist eine gesammelte Probe verwendet oder die Bestimmung erfolgt nach einer aktiven, anreichernden Probenahme. Die eigenen Arbeiten sollen dazu beitragen, die Ammoniak-Bestimmung in der Außenluft präziser, sowie schneller und kostengünstiger zu machen. Die BAM prüfte daher kommerzielle elektrochemische und Metalloxid-basierte Sensoren, die für diesen Konzentrationsbereich aber nur bedingt geeignet sind. Deshalb wurden alternativ eigene Entwicklungen zum Nachweis von Ammoniak im Spurenbereich aufgenommen, wobei der Analyt über die Änderung der Fluoreszenz eines BODIPY-Farbstoffs bei 550 nm mittels eines portablen Fluoreszenz-Sensors direkt aus der Gasphase gemessen wird. Zur Kalibrierung von Ammoniak-Sensoren und -Messgeräten steht ein stationäres System basierend auf der Mischung von zertifizierten Prüfgasen aus Druckflaschen mit kalibrierten Massendurchfluss-regler (MFC) zur Verfügung. Darüber hinaus erfolgt eine chemische Analyse der verwendeten Gasgemische mittels eines Massenspektrometers. Für die Kalibrierung und Prüfung von Sensoren und Messgeräten vor Ort wurde ein mobiles Prüfsystem entwickelt. Die Generierung von Ammoniak-haltigen Gasen im Spurenbereich von 0,5 nmol/mol bis 500 nmol/mol erfolgt durch das Permeationsverfahren nach ISO 6145-10. Für die Realisierung der Rückführbarkeit der Ammoniakbestimmung werden von den Nationalen Metrologischen Instituten sowie designierten Instituten Standards bereitgestellt und auch weiterentwickelt. Die primären metrologischen Standards beruhen auf SI-Einheiten und sind die Basis für eine Rückführbarkeit der Sensoren bzw. Analysengeräte. T2 - 5. Fachsymposium „Intelligente Sensorik/Analytik und sichere Sensornetze: Innovative Technologien und neue Anwendungsfelder“ CY - Karlsruhe, Germany DA - 14.11.2018 KW - Ammoniak KW - Sensor KW - Multigassensorik PY - 2018 AN - OPUS4-46926 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Hans-Joachim T1 - Certification of the mass fractions of trace elements in a medium purity graphite reference material N2 - The increasing application of graphite materials in various fields of technology and science enhances the demand for strictly controlled properties which are often directly correlated to the contents of trace element impurities. Therefore, the availability of powerful, rapid and reliable analytical methods for the determination of trace impurities is essential for process and quality control. Certified reference materials, indispensable for the development and validation of appropriate trace analytical methods for the characterization of special purity graphite materials are still lacking. Therefore, BAM in co-operation with the working group “Special Materials” of the committee of chemists of GDMB (Gesellschaft der Metallurgen und Bergleute e.V.) certified an industrially sourced graphite material with genuine elemental impurities. The candidate material was a commercial product (NBG 18) taken from the customary production line of the producer SGL CARBON, Chedde (France). The homogeneity of the powdered material was assessed by means of ETV-ICP OES and DC Arc-OES. Certification of the candidate reference material was based on an inter-laboratory comparison involving 17 expert laboratories from Germany, France, Slovenia, USA, South Africa. A variety of different mineralization, digestion, leaching, fusion and combustion techniques prior to ICP OES and photometry, methods without sample preparation (INAA, k0-INAA) as well as typical solid sampling methods (ETV-ICP OES, ETV-ICP-MS, SS-ET AAS, DC Arc-OES, MF-DC Arc-OES) were used to characterise the material. Certified mass fractions and their expanded uncertainties (k = 2) were assigned for 27 elements (Al, B, Ba, Be, Ca, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Si, Sr, Ti, V, W, Y, Zn, Zr), ranging from (0.00050 ± 0.00027) mg/kg for Be to (41 ± 6) mg/kg for Si. Informative values are given for further parameters: trace element contents of Ag, As, Au, Bi, Cd, Cs, Dy, Eu, Ga, Gd, Hg, In, La, Nb, Rb, Re, Rh, Sb, Sc, Se, Sm, Sn, Ta, Tb, Te, Th, U; method specific values obtained by ETV-ICP OES (BETV and SiETV) and ash content. The new certified material is available as BAM Reference Material BAM-S009 Medium Purity Graphite Powder. T2 - BERM-15 CY - Berlin, Germany DA - 23.09.2018 KW - Certification KW - Graphite KW - Reference material KW - Trace elements PY - 2018 AN - OPUS4-46235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Burnage, Samual Charles T1 - Combination of Fluorescent Molecularly Imprinted Polymers and Microfluidics for the Detection of Cancer Biomarker Phosphorylated Tyrosine N2 - Cancer is modern medicine’s biggest challenge. It is now thought to be responsible for one in six deaths worldwide making early diagnosis, and treatment thereon, essential for better prognoses1. Protein phosphorylation is a post-translational modification of particular interest as a biomarker in the understanding of neurodegenerative diseases and a number of cancer pathways. There is therefore a need for robust, fast and low-cost techniques for the detection of these phosphorylations. Fluorescent molecularly imprinted polymers (MIPs) are a cheap and selective material for both the extraction and detection of a multitude of analytes. Often referred to as “plastic antibodies”, MIPs provide added robustness and chemical stability compared to their natural counterparts. Application of these fluorescent MIPs to a microfluidic lab-on-a-chip platform offers a fast, versatile method for the detection of biomarkers containing phosphorylated amino-acids such as phosphorylated tyrosine. Here, we present a tuneable core-shell MIP system consisting of a polystyrene core, silica inner-shell and MIP outer-shell. The MIP outer-shell contains a urea-based fluorescent probe monomer co-polymerised into the polymer matrix that can detect phosphorylated-tyrosine based on a change in its optical properties. The phosphate group interacts with the fluorescent probe via hydrogen bonding interactions yielding a fluorescence enhancement in organic solvents. The fluorescent MIPs are to be applied to a microfluidic platform, for rapid extraction of the analyte from the aqueous sample phase and simple optical detection in the organic phase that contains the MIP microparticles. T2 - Rapid Methods Europe 2018 (RME2018) CY - Amsterdam, The Netherlands DA - 05.11.2018 KW - Molecularly Imprinted Polymers KW - Microfluidics KW - Fluorescent MIPs KW - MIPs KW - Phosphorylated Tyrosine KW - Biomarker PY - 2018 AN - OPUS4-47019 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Verhassel, A. T1 - Application of novel tumor cell glycan-specific nanoprobes for detecting and targeting breast and prostate cancer N2 - Glycosylation is a post-translational modification that is involved in the regulation of many biological processes. The glycosylation pattern in cancer cells differs from that in normal cells. One of the main alterations that has been observed in several cancers is the increase of sialic acids at the end of the glycan. The increase of sialic acids and other alterations affect development and progression of tumors and are found to play an important role in cancer invasiveness and metastasis. Molecularly imprinted polymers (MIPs) are synthetic recognition elements that show high selectivity and affinity for their targets. These polymers show promising applications in detection methods for cancer cells. In this study newly synthesized MIPs, labelled with a nitrobenzoxadiazole (NBD) fluorophore, are investigated for their specificity and utility in the detection of cancer cell-related sialic acids. T2 - Biomarkers – methods and technologies CY - Malmö, Sweden DA - 25.10.2018 KW - Nanoparticles KW - MIPs KW - Cancer PY - 2018 AN - OPUS4-46490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sternbaek, L. T1 - Holographic microscopy-Macrophage uptake of SA MIPs N2 - Sialic acid (SA) is a cell surface glycan, which has been found to be upregulated on more aggressive cancers. Therefore, there is a great interest in developing methods for detection of SA on a great interest in developing methods for detection of SA o on cancer cells. We are screening SA on cell lines by fluorescent molecularly imprinted polymers, SA fluorescent molecularly imprinted polymers, SA fluorescent molecularly imprinted polymers, SA fluorescent molecularly imprinted polymers, SA fluorescent molecularly imprinted polymers, SA fluorescent molecularly imprinted polymers, SA -MIPs. Quantitative phase imaging (QPI) is a digital holographic technique. Various cellular parameters can be visualized and calculated from the particular hologram, including individual cell area, thickness, volume and population confluence and cell counts. The aim was to investigate the possible uptake of SA in macrophage cell lines in in vitro cell cultures and check if they affected the cell. T2 - Biomarkers – methods and technologies CY - Malmö, Sweden DA - 25.10.2018 KW - Digital holographic microscopy KW - MIPs KW - Sialic acid PY - 2018 AN - OPUS4-46493 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Climent Terol, Estela T1 - Antibody-gated dye delivery systems for Type-I pyrethroids detection N2 - Type-I pyrethroids are frequently used for disinfection purposes on airplanes from and to tropical areas. The WHO (Word Health Organization) defines “disinfection” as the procedure whereby health measures are taken to control or kill the insect vectors of human diseases including dengue, yellow fever and malaria.1 Due to this, a new effective and rapid method for pyrethroids analysis directly in the plane is needed. To detect type-I pyrethroids, gated materials are constructed for the purpose of finely tuning the movement of a cargo from voids of a mesoporous inorganic support to a solution, in response to a predefined stimulus.2 Antibodies are bound to specific functional groups grafted on the support’s surface with the two-fold aim of closing the mesopores and working as biological receptors for the target compounds.2 A specific opening mechanism, activated selectively in presence of pyrethroids as analytes, is able to control the release of an indicator dye previously loaded inside the inorganic support. As only few molecules of pyrethroids are necessary to open a pore and release a large amount of dyes, the system shows an intrinsic signal amplification quantified as a fluorescence emission intensity.3 Different mesoporous silica supports (from nano- and microparticles to platelets and short fibers) were synthetized, characterized and functionalized following different capping strategies. In this contribution, we will compare the temporal response behaviour of the optimized gated materials to verify if the respective delivery systems are properly closed and how fast they can be opened in presence of the analytes. Our results indicate that the trends of the kinetics observed in solution show a better control of the closing/opening mechanism when the epitope region of the antibody (around 10 nm) properly fits the pore size of the carriers. Because the incorporation of an antibody-gated dye-delivery system with a conventional test-strip-based lateral-flow assay allows for the detection of analytes down to the ppb level in an easy-to-operate manner and an overall assay time of 2–5 min, which is fast for a biochemical test,3 we carried out first model studies for a lateral flow test assay on membranes, using a smartphone setup for read-out. T2 - XV EUROPT(R)ODE 2021 CY - Online meeting DA - 28.11.2021 KW - Antibody-gated materials KW - Lateral flow assay KW - Pyrethroids detection PY - 2021 AN - OPUS4-53862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Reaction-based BODIPY dyes as powerful tools in fluorescence sensing applications N2 - The reversible analyte-induced switching between a colourless leuco form of a dye and its coloured all-π-conjugated form is one of the oldest concepts in probe- or indicator-based optical analysis,1 constituting so-called “one-color indicators”.2 In contrast to colour changes in the visible region, for which usually a bond-forming or a non-covalent interaction between a functional group on an indicator and an analyte is responsible, the extraordinarily large shifts of 150–250 nm seen for leuco-to-all-π-conjugated transformation are only possible when the reaction takes place directly at a site that is an intrinsic part of a dye’s π-system; the classic case are triphenylmethane dyes.3 Despite its obvious potential, this approach has not been a very popular area of scientific research for decades, perhaps because it is much more difficult to implement selectivity than by modifying terminal functional groups. However, in recent years, reaction-based fluorescence probes have attracted increasing attention by virtue of their superior sensitivity.4,5 Nowadays, rhodamines and fluoresceins are by far the most prominent groups of reaction-based indicators.5 They are usually switched between a colourless and non-fluorescent and a greenish-yellowish absorbing and yellowish-reddish emitting form. Typically, the coloured and fluorescent form is ionic, while the colourless form is neutral, reactions having mainly be designed to occur at the end groups of the xanthenoid π-system. BODIPY dyes, with their favourable spectroscopic and chemical properties as well as facile wavelength tunability features have only very recently been explored into this direction.6,7 Reaction at the core dipyrrin framework of these dyes led to strong colour and fluorescence modulations with potential applications in materials sciences6 and cell imaging.7 The present contribution will highlight the mechanisms at play and the sensing performance realized so far, and will compare core-reactive approaches to reaction-based signalling that involves π-extension of BODIPYs.8,9 T2 - 11th International Conference on Porphyrins and Phthalocyanines (ICPP-11) CY - Online meeting DA - 26.06.2021 KW - Indicators KW - Fluorescence KW - Sensing KW - BODIPY Dyes PY - 2021 AN - OPUS4-54001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sun, Yijuan T1 - Molecularly Imprinted Polymer Embedded BODIPY Probes for the Fluorescence Detection of Antibiotics N2 - Antibiotics are widely used to combat bacterial infections in humans and animals and their use has greatly improved modern healthcare. However, frequent and reckless use of antibiotics can cause antibiotic resistance in bacteria and pollute ecosystems. Therefore, the rapid and reliable detection of antibiotics is crucial. Fluorescence sensing is particularly attractive because of its high sensitivity and low limits of detection. Fluorescence assays can be carried out in a variety of platforms such as strips and particles among others. Recently, core-shell molecularly imprinted polymers (MIPs) have emerged as a promising sensor platform for (bio)chemical detection due to their low-cost, high stability, reusability, high affinity and selectivity.MIPs in combination with fluorescent molecular probes are gorgeous, since the covalently embedded probe allows for direct indication of a rebound template and provides a wealth of information about the binding state of a MIP through the multitude of fluorescence parameters accessible, facilitating MIP optimization. In the present work, we have developed a novel series of fluorescent functional monomers, which consist of a fluorophore with a π-conjugated urea recognition site and one or two polymerizable units. The fluorescent monomers are covalently embedded into the MIP matrix to generate fluorescence changes upon template binding (Figure 1). Preliminary titrations of the dye monomer with the analytes show a blue shift of the absorption spectrum and a decrease in the fluorescence intensity which confirms the formation of hydrogen bonds between the urea and the carboxylate group of the antibiotic. Compared with the non-imprinted polymers, the MIP shells on core carrier particles have demonstrated an effective imprinting by showing a higher fluorescence response upon analyte binding. T2 - EUROPT(R)ODE2021 CY - Warsaw, Poland DA - 28.11.2021 KW - Antibiotics KW - Fluorescent dye KW - Molecularly Imprinted Polymer PY - 2021 AN - OPUS4-53891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Morcillo, Dalia T1 - High-resolution optical isotopic spectrometry as a tool for aging studies of Li-ion batteries N2 - Current activities on Department Analytical Chemistry, Reference Materials about optical isotopic spectrometry as a tool for aging studies of Li-ion batteries. T2 - Adlershofer Kolloquium - FB 1.6 CY - Online meeting DA - 18.05.2021 KW - High-resolution KW - Battery aging KW - Storage Technologies KW - Optical isotopic spectrometry KW - Lithium-ion batteries KW - Inorganic Reference Materials KW - Pouch cell KW - Anode KW - Cathode KW - Electrochemistry KW - Isotope PY - 2021 AN - OPUS4-53712 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pérez-Padilla, Victor T1 - Fluorescent molecularly imprinted polymer particles for detection of environmental contaminants N2 - Analysis of environmental contaminants such as pesticides is increasing in importance due to frequent detection of residues in water reserves and food stuff, as well as lowering of maximum residue levels (MRLs). Molecularly imprinted polymers (MIPs) have been developed for preconcentration of these analytes prior to analysis by chromatographic techniques. MIPs are prepared by polymerization of monomers in a matrix containing the analyte, followed by extraction of the analyte to obtain binding sites that are complementary to the analyte of interest. Recently, our group developed MIPs containing fluorescent reporter molecules that can be used for direct detection and quantification of 2,4-D in contaminated water. Core/shell MIP particles were employed, consisting of submicron silica nanoparticles coated with a MIP shell containing a fluorescent reporter whose signal was enhanced upon binding with 2,4-D in water. A limit of detection of 20 nM was attained. We present here a comparable system, composed of fluorescent core-shell MIPs for the direct analysis of pesticides in environmental samples. T2 - Europtrode 2021 CY - Warsaw, Poland DA - 29.11.2021 KW - Glyphosate KW - Guanidinium Receptors KW - Fluorescent Probes KW - Molecularly Imprinted Polymers KW - Core-Shell Particles PY - 2021 AN - OPUS4-53878 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Approaches to Sensitive and Multiplexed Assays for Robust, Reliable and User-friendly Point-of-Need Analysis N2 - Analytical assays that can be used outside of a dedicated laboratory environment have received unprecedented attention all around the globe during the last one and a half years, in which the world was struggling with and trying to contain the SARS-CoV-2 pandemic. However, besides their current prominence in the field of medical diagnostics, rapid tests and assays have also become increasingly important in other areas ranging from food and feed via security and forensics to environmental management. The advantage is obvious: taking the assay to the sample instead of bringing the sample to the laboratory minimizes the time between first suspicion and first decision taking. Especially today, where mobile communication devices with powerful computing capabilities and onboard cameras are omnipresent, the majority of the global population possesses the basic skills of operating a powerful detector, ready at their fingertips. The stage is thus set for a much broader use of analytical measurements in terms of prognostics and prevention. Today, however, tests for single parameters are still prevailing, whether it is a SARS-CoV-2 biomarker, the glucose level in blood or the concentration of lead in a water sample. Also, for industrial use, many mobile analytical systems still target a single parameter, and several separate runs or tests have to be used even if one wants to screen for only a small number of key parameters. Current challenges in the field thus lie with the development of low-number multiplexing strategies while allowing for robust, reliable, fast, and user-friendly operation and while still reaching the required sensitivities. This lecture will give an overview of various generic approaches developed in BAM’s Chemical and Optical Sensing Division over the years to address these challenges. In particular, it will highlight how the combination of supramolecular (bio)chemistry, luminescence detection, hybrid (nano)materials and device miniaturization can result in powerful (bio)analytical assays that can be used at a point-of-need. Selected examples will introduce key aspects of such systems like tailored signaling mechanisms and recognition elements, materials functionalization and device integration, including hybrid mesoporous nanomaterials, gated indicator release systems, molecularly imprinted polymers, microfluidic devices, test strips and smartphone-based analysis. T2 - Advanced Analytical Technologies Seminar CY - Online meeting DA - 08.12.2021 KW - Rapid tests KW - Multiplexing KW - Trace analysis PY - 2021 AN - OPUS4-54002 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Greer, B. A1 - McNamee, S.E. A1 - Boots, B. A1 - Cimarelli, L. A1 - Guillebault, D. A1 - Helmi, K. A1 - Marcheggiani, S. A1 - Panaiotov, S. A1 - Breitenbach, U. A1 - Akcaalan, R. A1 - Medlin, L.K. A1 - Kittler, Katrin A1 - Elliott, C.T. A1 - Campbell, K. T1 - A validated UPLC–MS/MS method for the surveillance of ten aquatic biotoxins in European brackish and freshwater systems N2 - Over the past few decades, there has been an increased frequency and duration of cyanobacterial Harmful Algal Blooms (HABs) in freshwater systems globally. These can produce secondary metabolites called cyanotoxins, many of which are hepatotoxins, raising concerns about repeated exposure through ingestion of contaminated drinking water or food or through recreational activities such as bathing/swimming. An ultra-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) multi-toxin method has been developed and validated for freshwater cyanotoxins; microcystins-LR, -YR, -RR, -LA, -LY and -LF, nodularin, cylindrospermopsin, anatoxin-a and the marine diatom toxin domoic acid. Separation was achieved in around 9 min and dual SPE was incorporated providing detection Limits of between 0.3 and 5.6 ng/L of original sample. Intra- and inter-day precision analysis showed relative standard deviations (RSD) of 1.2–9.6% and 1.3 –12.0% respectively. The method was applied to the analysis of aquatic samples (n = 206) from six European countries. The main class detected were the hepatotoxins; microcystin-YR (n = 22), cylindrospermopsin (n = 25), microcystin-RR (n = 17), micro-cystin-LR (n = 12), microcystin-LY (n = 1), microcystin-LF (n = 1) and nodularin (n = 5). For microcystins, the levels detected ranged from 0.001 to 1.51 mg/L, with two samples showing combined levels above the guideline set by the WHO of 1 mg/L for microcystin-LR. Several samples presented with multiple Toxins indicating the potential for synergistic effects and possibly enhanced toxicity. This is the first published pan European survey of freshwater bodies for multiple biotoxins, including two identified for the first time; cylindrospermopsin in Ireland and nodularin in Germany, presenting further incentives for improved monitoring and development of strategies to mitigate human exposure. KW - Biotoxins - Biotoxine KW - Harmful Algal Bloom (HAB) KW - UPLC-MS/MS PY - 2016 DO - https://doi.org/10.1016/j.hal.2016.01.006 SN - 1568-9883 VL - 55 SP - 31 EP - 40 PB - Elsevier CY - Amsterdam AN - OPUS4-35515 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Chulvi Iborra, Katherine T1 - Pd(II)-LMOF based material for the sensing of molecular hydrogen in gas phase N2 - Current interest in hydrogen gas as an energy source is growing due to its attractive properties such as high chemical energy density and the fact that its combustion produces water as by-product, qualifying this gas as an appealing clean energy source. In particular, the use of molecular hydrogen in automotive applications such as the hydrogen internal combustion engine (HICE) or hydrogen fuel cells is an excellent clean alternative. Despite these promising opportunities, hydrogen gas has a distinct disadvantage as an everyday energy medium, that is, it is highly flammable. Hydrogen processing apparatuses should therefore be constantly monitored so that leaks are immediately detected. The implementation of direct sensing systems for H2(g) is thus a decisive factor for its application and acceptance as a clean energy source. Because the automotive market alone is already a mass market, these sensors do not only have to be reliable, robust and dimensionally small, but operation has to be simple and the device itself cost-effective. In addition, very low detection limits are a must as already escape of small quantities of H2(g) is directly related to public health and safety. Besides electrochemical or semiconductor sensors, optical sensors are especially appealing because the equipment is usually simple and accessible, easily miniaturized and measurements can be performed in situ and in real time. If one cannot rely for instance on metallic palladium as interacting matrix, a major challenge for optochemical hydrogen sensors is to find a suitable material that fulfils all the requirements mentioned above and undergoes a dedicated indication reaction with H2(g). One such alternative can be Metal-Organic Frameworks (MOFs) which constitute a predefined, organized, mesoporous structure built up from metal ions and organic bridging ligands. With a myriad of building blocks being available, MOFs can be equipped with internal H2 reception sites that shall allow for selective and sensitive indication. For instance, if Pd ions are implemented in such a way that they express open metal sites (OMS), these OMS shall possess a strong affinity for hydrogen. If light absorbing and emitting organic ligands are additionally chosen, luminescent MOFs (LMOFs) can result that are perfect candidates for optical sensors, as changes at the analyte reception site can be effectively transduced into a measurable signal. In this contribution, we intended to discuss the development of a new luminescent sensor material for the detection of the highly flammable H2(g). This sensor material is based on an LMOF assembled from Pd(II) and aromatic bridging ligands, the advent of hydrogen at the OMS in the LMOF producing distinct variations in the material’s optical properties. T2 - 24th Congress and General Assembly of the International Union of Crystallography CY - Hyderabad, India DA - 21.08.2017 KW - Optical sensor KW - Hydrogen KW - LMOF PY - 2017 UR - http://www.iucr2017.org/abstract/myaccount/pdf/iucr2017-abstract-0b61b4c101d7bf652ae5b0dffd66e5fd.pdf AN - OPUS4-42362 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter T1 - Multiplex suspension array fluorescence immunoassay (SAFIA) for environmental screening of bioactive compounds in wastewater. N2 - Due to the demand of monitoring the water quality regarding emerging pollutants, such as drug residues, selective, high-throughput and multi-target analytical methods must be established. On the one hand, the influence of sewage on natural surface waters must be routinely monitored. On the other hand, estimation of removal efficiencies of pollutants, such as drug residues, is in the focus of industrial and public wastewater treatment. Immunoassays, such as ELISA, offer the possibility to be highly sensitive and selective due to the high target affine and specific recognition of antibodies to target molecules. Batch-wise processing in microtiter plates allow the necessary high-throughput, but only a single analyte can be determined within one measurement. To overcome these disadvantages, we developed a four-plex micro-bead based flow cytometric assay, which is adaptable for the microtiter plate format. The modular and self-prepared bead support consists of polystyrene-core-silica-shell particles. While the polystyrene core is used for encoding, by introducing different amounts of fluorescent dyes, the silica-shell creates a solid-support for the immunoassay: The target analytes, three drugs, carbamazepine, diclofenac and caffeine and the f ecal marker isolithocholic acid are covalently coupled to amino-groups on the surface via NHS-chemistry. A competitive immunoassay is subsequently conducted in a simple mix-and-read procedure. Finally, we could use SAFIA to assess the influent of treated and untreated waste water on the Douro river estuary in Portugal. The results of the analysis are comparable to ELISA. However, measurements could be carried out in 25% the time of analysis. T2 - Adlershofer For­schungs­forum 2017 CY - Berlin, Germany DA - 10.11.2016 KW - Immunoassay KW - Anthropogenic markers KW - Wastewater KW - Flowcytometry KW - Bead-based assay PY - 2017 AN - OPUS4-42824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo T1 - Quantitative 3D Stereo Microscopy in Diffraction Contrast (S)TEM N2 - The realistic description of plastic deformation caused by dislocations demands the representative measurement of their features, e.g., Burgers vector, slip plane, line direction and density. In the case of bulk deformation of technical alloys, reliable data must be ensured for large regions. Nonetheless, the (thin) filiform nature of dislocations and also the heterogeneity in some microstructures additionally require flexible analysis techniques that resolve the details of their interactions. Strong and clear channeling contrasts, faint extinction contours and the absence of chromatic aberration make scanning transmission electron microscopy (STEM) an ideal imaging mode in wide and thick regions of TEM foils, as opposed to conventional (C)TEM. It is the purpose of this contribution to show how STEM can be applied for quantitative measurement of dislocation features. Furthermore, a new tool will be presented, which enables the three-dimensional (3D) reconstruction, visualization and quantification of dislocation densities and directions from stereo-pairs. The application of these techniques will be shown on a monocrystalline Ni-base superalloy, an important class of structural materials that has been implemented in the first row blades of gas turbines. The examples are extracted from specimens subjected to creep deformation at high temperature and low stress under various macroscopic deformation geometries. The spacial and angular accuracy are discussed as well as possible sources of error. T2 - Symposium on Advanced Mechanical and Microstructural Characterization Methods for SX Ni- and Co-based Superalloys CY - Bochum, Germany DA - 13.09.2017 KW - Dislocation KW - Scanning Transmission Electron Microscopy KW - Microscopy KW - 3D reconstruction PY - 2017 AN - OPUS4-42175 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jankevics Jones, H. T1 - Determination of core-shell particle mass and size distribution, density, and distinguishing shell thicknesses by resonant mass measurements N2 - An important aspect of micro or nano particles development is the understanding and control of the particle structure, as it can be determining for particle’s final function, and it affects among other things potential further surface functionalisation/modification. This work shows the capability of resonant mass measurements (RMM) to measure the mass and density of micron sized particles. The technology utilizes a suspended MEMS microchannel resonator, through which individual particles transit across the resonator altering the resonant frequency, which is then detected using an optical-based method. Changes in frequency observed when a particle enters the microchannel resonator are proportional to the buoyant mass of the particle, and can be translated into mass, size or surface area. RMM therefore allows particle concentration to be determined as well as particle mass in a single measurement. Furthermore, a method for estimating the density distribution of particles from RMM measurements has been developed. This uses the convolution of the buoyant mass distribution of the particles obtained when suspended in different fluids. By combining the data from the density and mass determinations, small mass shifts arising from applying a coating to a particle can be estimated, and the resulting shell thicknesses calculated. These methods have been applied to silica coated and uncoated polystyrene latex particles. RMM shows that it can be used to measure, and distinguish between, silica shell thicknesses that are in the order of 10s of nanometres on hybrid micron-sized particles T2 - 7th International Colloids Conference CY - Sitges, Barcelona, Spain DA - 18.06.2017 KW - Core-shell particles KW - Resonant mass measurement PY - 2017 AN - OPUS4-42259 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Agudo Jácome, Leonardo T1 - 3D Reconstruction, Visualization and Quantification of Dislocations from TEM Stereo-Pairs N2 - Dislocations, as carriers of plastic deformation, affect important properties in technical materials, e. g., plasticity. The realistic description of plastic deformation caused by dislocations demands the representative measurement of their features, e.g., line direction, slip plane, Burgers vector and density. Bulk deformation of structural and functional alloys requires reliable data from large regions. The filiform nature of dislocations interacting with complex microstructures additionally demands observation and analysis techniques that allow resolving the details of their interactions in space. The use of electron tomography for this purpose is bound to difficult and time consuming experimental setups, which are not always applicable to any material. In this contribution a new tool is presented, which enables the three-dimensional reconstruction, visualization and quantification of dislocation densities and directions from manual tracing of scanning transmission electron microscopy (STEM) stereo-pairs. Examples are shown from samples of a creep-deformed monocrystalline Ni-base superalloy. T2 - 3D Materials Science 2016 CY - St. Charles, Illinois, USA DA - 10.07.2016 KW - Dislocation KW - Scanning Transmission Electron Microscopy KW - 3D KW - Quantification KW - Superalloy PY - 2016 AN - OPUS4-42173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bolz, Axel T1 - Microfluidic Paper-Based Analytical Devices with Surface Enhanced Raman Scattering Detection N2 - Microfluidic paper-based analytical devices (μPADs) in combination with surface enhanced Raman scattering (SERS) provide a way for analyses of complex mixtures. The μPADs can be used for the chromatographic separation of different compounds of mixtures in combination with the separate detection of the analytes in different zones on the paper by SERS. SERS allows to observe analytes directly without labelling in low concentrations in aqueous solutions and to identify them by their spectral fingerprint. SERS substrates on the μPADs were created by drying standard silver nanoparticle (AgNP) solution on the paper. The microfluidic structure of the μPADs was prepared by wax printing. As a model system, an aqueous solution of the non-fluorescent analyte adenine and two fluorescent dyes tris(2,2’-bipyridyl)dichlororuthenium(II) and sulforhodamine B was tested. The dependency of the SERS signal intensity on the analyte concentration can be fitted using a Langmuir isotherm curve progression. With this approach, a semi-quantitative analysis of the components is possible. The reproducibility and stability of the measurement procedure was tested with several measurements over time, different NP batches, and with different analytes in different concentrations and resulted in an average relative standard deviation of 16 %. The SERS spectra of the mixture of the model system are dominated by one compound depending on the concentration ratio. For the detection and identification of all components of the mixture, the compounds were therefore separated on the μPADs and measured at different positions. The position of adenine on the μPADs is dependent on the AgNP coverage of the paper. Due to this effect, it possible to detect adenine on a defined point on the μPADs and to get an information on the concentration in a mixture of three components. T2 - 30. Tag der Chemie Humboldt-Universität zu Berlin CY - Berlin, Germany DA - 05.07.2017 KW - SERS KW - µPAD PY - 2017 AN - OPUS4-42265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mekonnen, Tessema Fenta T1 - Transformation products of pesticides: simulation and detection N2 - Pesticides including fungicides, herbicides and insecticides are among primary residues detected in food and feed. They are transformed to a variety of products due to metabolic reactions in living organisms, microbial activities, industrial processes and photochemical reactions. To understand metabolic transformation products (TPs), in-vitro and in-vivo methods were used for a long period of time. However, these conventional methods are hampered by the long-time of analysis and by the matrix complexity. Nowadays, online coupling of electrochemistry with mass spectrometry is a technique of interest for fast prediction/ simulation of metabolic TPs and to understand the mechanism of metabolic processes. The main objective of this work was to understand the mechanism of fluopyram (fungicide) and chlorpyrifos (insecticide) metabolism and to identify TPs by electrochemistry coupled to liquid chromatography-mass spectrometry (EC-LC-MS). Additionally, TPs of fluopyram by photochemical reaction have been investigated. Furthermore, the TPs and parent compounds in real food matrices were investigated by LC-MS/MS. Phase-I metabolism via N- and O-dealkylation, P-oxidation and hydroxylation mechanisms were successfully simulated/predicted by EC-LC-MS. Additionally, metabolites produced by human and rat liver microsomes were identified by LC-MS/MS and high resolution mass spectrometry (HR-MS) and simulated with EC oxidation products. It is known that some phase-I metabolites are further conjugated with different biomolecules such as glucoside and glutathione. Phase-II metabolism was simulated by trapping the oxidized products (phase-I) online by biomolecules and allowing them to react in the loop before the electrospray ionization interface of the MS. Standard solution of fluopyram was irradiated with a medium pressure Hg-lamp (150 W) at 12.5 0C for 2 hrs and aliquots were characterized by LC-MS/MS. In conclusion, the EC-LC-MS method enables fast, cost effective and matrix free detection and prediction of metabolic pathways compared to in-vitro assays. Its versatilities to synthesis reference substances and metabolites for off-line characterization (such as NMR and HR-MS) and possibilities of determining fast reactive intermediates make EC-LC-MS more advantageous than in-vitro assays. T2 - XIX EUROANALYSIS:Europe's Analytical Chemistry Meeting CY - Stockholm, Sweden DA - 28.08.2017 KW - Metabolism KW - EC/LC/MS KW - Transformation product KW - Electrochemical oxidation KW - Photooxidation PY - 2017 AN - OPUS4-42580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tavernaro, Isabella T1 - How to Quantify the Total and Accessible Number of Functional Groups and Ligands on Nanomaterials Using a Multimodal Approach – A Bilateral Comparison N2 - Surface-functionalized organic and inorganic engineered nanomaterials (NM) have gained increasing interest in various fields of application such as nanomedicine, bioimaging and sensing, or as additives in food and consumer products. The performance and safe use of these NM in such applications depend not only on their composition, primary particle size, and morphology, but also on surface chemistry, which controls surface charge, colloidal stability, biocompatibility, and toxicity.[1] NM surface chemistry is mainly determined by the total number of surface functional groups (FG) and the number of FG accessible for subsequent functionalization with ligands or biomolecules. Thus, methods for FG quantification are not only important tools for the control of NM production processes, but can also foster the sustainable development of functional and safe(r) NM. In addition, this need underlines the importance of validated and standardized analytical methods that provide accurate information on application-relevant physicochemical properties with known uncertainties, flanked by suitable quality control samples and reference materials. Aiming at the development of simple, versatile, and multimodal tools for the quantification of common bioanalytically relevant FG, we investigated and compared various analytical methods commonly used for FG quantification.[2,3] The potential of multimodal approaches for FG quantification was recently demonstrated in a bilateral comparison of the surface analysis of commercially available aminated silica nanoparticles (SiO2-NP).[3] These results demonstrate not only an influence of the size and synthesis methods on the number of FG but also on NM performance. This concept is currently explored in a second bilateral comparison of quantitative nuclear magnetic resonance (qNMR) measurements and optical assays for differently sized commercial and in-house synthesized SiO2-NP with varying amounts of amine functionalities, utilizing further optimized protocols for sample preparation, qNMR measurements, and data evaluation. This strategy can contribute to establishing multi-method characterization strategies for NMs and can provide a more detailed picture of structure-properties relationships for different types of functional NM. T2 - E-MRS Spring Meeting 2024 & ALTECH 2024 CY - Strasbourg, France DA - 27.05.2024 KW - Quantification KW - Nano KW - Particle KW - Quality assurance KW - Interlaboratory comparison KW - Method KW - Uncertainty KW - Reference material KW - Sensors KW - Synthesis KW - Silica KW - Surface analysis PY - 2024 AN - OPUS4-62161 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaeger, Carsten T1 - Comparing Nontargeted LC-MS Methods by Co-visualizing Linear Dynamic Range and Chemical Coverage N2 - INTRODUCTION Biological and environmental samples contain thousands of small molecule species that all vary in chemical properties and concentration range. Identifying and quantifying all these chemical entities remains a long-term goal in metabolomics and related systems approaches. Due to its broad selectivity, nontargeted LC-MS is usually the method of choice for broad chemical screening. Optimizing nontargeted LC-MS methods, however, is less straightforward than for targeted methods where sensitivity, specificity, linearity etc. serve as well-established performance criteria. We therefore investigated linear dynamic range (LDR) and chemical classification as alternative performance criteria to guide nontargeted method development. EXPERIMENTAL METHODS LDR was defined as the linear portion of a feature’s response curve over multiple concentration levels. Comparing the LDR of features across methods can be expected to be significantly more robust than comparing signal intensities for a single concentration. To determine LDR for all features, a computational workflow was implemented in the R programming language. For estimating the linear portion of a curve, several mathematical approaches including linear, non-linear and piecewise linear regression were evaluated. Chemical classification was based on ClassyFire, which computes chemical classes for a given structure. To avoid false classifications for incorrectly annotated compounds, we took the following statistical approach. For each compound, multiple likely annotation hypotheses were derived using a recently described workflow[2]. All annotation hypotheses were submitted to ClassyFire and obtained classifications were ranked by frequency. The most frequently suggested class was kept for further analysis. Finally, LDR and chemical classes were visualized together on a molecular network, which was constructed using the well-established MS/MS similarity approach. RESULTS AND DISCUSSION For technical validation of the workflow, several hundred curve fits obtained from the different regression models were reviewed visually. Piecewise linear regression performed the most reliably with respect to the heterogeneous curve shapes of ‘real-life’ features. Validation of chemical classification was performed against a compound library, which showed that 90% of ~450 library compounds were correctly classified using the described approach. Two liquid chromatography methods (HILIC, RPC) as well as two electrospray ionization variants (low/high-temperature ESI) applied to urinary metabolomics were exemplarily studied to test the workflow. Molecular network visualization indicated that of all analytical setups, HILIC/high temperature ESI performed best in terms of high LDR achieved over a wide range of compound classes. Despite one order of magnitude lower sensitivity, HILIC/low temperature ESI showed similar chemical coverage, except for organic nitrogen compounds that were underrepresented compared to high-temperature ESI. Both RPC setups were inferior to the HILIC setups in terms of high-LDR features, supporting previous findings for the given matrix. The higher relative representation of benzenoids and lipids in RPC demonstrated that the workflow successfully captured expected selectivity differences between chromatographies. CONCLUSION When comparing nontargeted LC-MS methods for optimization purposes, ideally all available quantitative and qualitative information should be integrated. The present workflow follows this idea. Visualizing LDR and chemical classes of all features on a molecular network quickly indicated differences in method selectivity that were otherwise difficult to spot. As an automated approach, it is easily applied to repeated optimization steps, enabling effective optimization strategies. T2 - EURACHEM Workshop CY - Tartu, Estonia DA - 20.05.2019 KW - Linear dynamic range KW - Liquid chromatography-mass spectrometry KW - Nontargeted approach KW - Method development KW - Chemical coverage PY - 2019 AN - OPUS4-48333 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Johann, Sergej T1 - Semi-automatic Gas Measurement Device Based on Fluorescent Multi-gas Sensors N2 - This paper describes the development of a semi-automatic gas measurement device presenting potentially a broad range of applications, noteworthy in the agricultural sector. Non-reversible fluorescent molecular sensors were designed and syn-thesized. Upon, integration into a hydrogel matrix with an optimal ratio of co-solvents, the sensors reacting selectively to ammonia were illuminated by excitation light to produce a concentration-correlated fluorescence emission. An automated mechanical-elec-trical device initiates a given gas mixture and thus simulates con-centrations similar to a threshold value. The aim of this project is to develop a sensor or a low-cost method which can monitor low concentrations of harmful gases and aid in their elimination or regulation in livestock housing, barns or stables. T2 - IEEE Sensors 2019 CY - Montreal, Canada DA - 27.10.2019 KW - Gas analysis KW - Fluorescence KW - Embedded sensor KW - Spectroscopy KW - Environment KW - Agricultural economy PY - 2019 AN - OPUS4-49502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Deumer, J. A1 - Andresen, Elina T1 - SAXS data of bipyramidal LiYF4 nanoparticles N2 - SAXS data of bipyramidal LiYF4 nanoparticles synthesized by the Federal Institute for Materials Research and Testing (BAM) and measured by the Physikalisch-Technische Bundesanstalt (PTB) at the synchrotron facility Bessy II, Berlin, Germany. KW - Reference data set KW - Simulation KW - Reference material KW - Upconversion nanoparticles KW - Particle number concentration KW - SAXS PY - 2024 DO - https://doi.org/10.5281/zenodo.13691409 PB - Zenodo CY - Geneva AN - OPUS4-62134 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jiang, Shan A1 - Gawlitza, Kornelia A1 - Rurack, Knut T1 - Dual-Fluorescent Nanoparticle Probes Consisting of a Carbon Nanodot Core and a Molecularly Imprinted Polymer Shell N2 - Dual-fluorescent molecularly imprinted nanoparticles with a red-emissive carbon nanodot-doped silica core and a chlorogenic acid-imprinted fluorescent polymer layer are prepared and their use in ratiometric fluorometric analysis is described. Nanoparticle probes consisting of a shielded and stably emitting core and a shell with embedded binding sites that indicates the presence of an analyte with a change in emission allow for internally referenced measurements potentially accounting for detrimental influences from instrument drifts, light source fluctuations or sensor materials-related inhomogeneities. KW - Molecular imprinting KW - Fluorescence KW - Core-shell particles KW - Chlorogenic acid KW - Ratiometric measurement PY - 2021 DO - https://doi.org/10.1007/978-1-0716-1629-1_17 VL - 2359 SP - 195 EP - 208 PB - Springer CY - Humana, New York, NY AN - OPUS4-53336 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meermann, Björn A1 - Lisec, Jan A1 - Jaeger, Carsten A1 - Saatz, Jessica A1 - Traub, Heike A1 - von der Au, Marcus T1 - Mehr Analyten, kleinere Proben N2 - Molekülmassenspektrometrie entwickelt sich weg von klassischer Target- hin zu Nontarget-Analytik. Elementmassenspektrometrie liefert hohe Ortsauflösung beim Element-Imaging und analysiert einzelne Zellen. Aufgrund der Fortschritte bei den Geräten für Timeof-Flight-Massenspektrometrie mit induktiv gekoppeltem Plasma (ICPToF-MS) lässt sich das gesamte Periodensystem der Elemente in kurzen transienten Signalen quasi-simultan massenspektrometrisch erfassen. KW - Massenspektrometrie KW - Non-target KW - ICP-ToF-MS KW - Laser Ablation/Imaging PY - 2021 VL - 69 IS - Juni SP - 64 EP - 67 PB - Wiley-VCH AN - OPUS4-52800 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Rudolf T1 - Microfluidic electrochemical lab-on-chip immunosensor for ultrasensitive analysis of cocaine in water, saliva, and urine N2 - A sensitive microfluidic assay for the detection of cocaine in different matrices. T2 - 2nd European Biosensor Symposium CY - Florenz, Italy DA - 18.02.2019 KW - Cocaine KW - Lab-on-chip KW - Microfluidic KW - Electrochemical PY - 2019 AN - OPUS4-48320 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Döring, Sarah A1 - Tscheuschner, Georg A1 - Flemig, Sabine A1 - Weller, Michael G. A1 - Konthur, Zoltán T1 - Cost-Effective Method for Full-Length Sequencing of Monoclonal Antibodies from Hybridoma Cells N2 - Background: Monoclonal antibodies play an important role in therapeutic and analytical applications. For recombinant expression, the coding sequences of the variable regions of the heavy and light chains are required. In addition, cloning antibody sequences, including constant regions, reduces the impact of hybridoma cell loss and ensures preservation of the naturally occurring full antibody sequence. Method: We combined amplification of IgG antibody variable regions from hybridoma mRNA with an advanced method for fulllength cloning of monoclonal antibodies in a simple two-step workflow. Following Sanger sequencing and evaluation of consensus sequences, the best matching variable, diversity, and joining (V-(D-)J) gene segments were identified according to identity scores from IgBLAST reference sequences. Simultaneously, the mouse IgG subclass was determined at the DNA level based on isotype-specific sequence patterns in the CH1 domain. Knowing the DNA sequence of V-(D-)J recombination responsible for the complementary determining region 3 (CDR 3), variable region-specific primers were designed and used to amplify the corresponding antibody constant regions. Results: To verify the approach, we applied it to the hybridoma clone BAM-CCMV-29-81 and obtained identical full-length antibody sequences as with RNA Illumina sequencing. Further validation at the protein level using an established MALDI-TOF MS-fingerprinting protocol showed that five out of six genetically encoded CDR domains of the monoclonal antibody BAM-CCMV-29-81 could be efficiently correlated. Conclusion: This simple, streamlined method enables the cost-effective determination of the full-length sequence of monoclonal antibodies from hybridoma cell lines, with the added benefit of obtaining the DNA sequence of the antibody ready for recombinant expression. KW - Full-length antibody sequencing KW - Hybridoma cell loss KW - MALDI-TOF MS KW - Immunoglobulin isotyping KW - RNA Illumina sequencing PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-639599 DO - https://doi.org/10.3390/antib14030072 SN - 2073-4468 VL - 14 IS - 3 SP - 1 EP - 17 PB - MDPI CY - Basel AN - OPUS4-63959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, V. A1 - Richter, Silke T1 - Progress at the calibration of light elements N2 - Analytical glow discharges with optical (GD-OES) and mass spectrometric (GD-MS) detection are able to obtain depth resolved information about the light elements hydrogen, carbon, nitrogen and oxygen in solid samples, where most of the other analytical techniques fail. However, the interpretation or even quantification of the measured signals is still very challenging. Problems arise due to physical effects (plasma processes such as the ‘Hydrogen effect’, the Doppler effect, self absorption or diffusion of hydrogen in the sample during sputtering) chemical effects(e.g. formation of compounds with argon or the matrix, poisoning of the sample or gettering) as well as instrumental difficulties (e.g. of the sensitivity, calibration and vacuum quality).. The GD techniques are direct solid sampling methods and require reference materials for calibration. Unfortunately the list of available certified reference materials (CRM) suited for calibration of light elements in different matrix is relatively short Therefore, sintered materials doped with the analytes H2, O2 and N2 were produced at IFW Dresden and applied as calibration standards for hydrogen, oxygen and nitrogen. Due to the high analyte concentration added, it is very likely that the real concentration agree well with the added amount of light elements in the corresponding phases. The validation of the determination of the light element concentration in the sintered samples was possible in some cases only due to the lack of suitable techniques. This fact proves the need for the development of a reliable quantification of light elements by GDS. A systematic dependence of the sputtering rate on the composition was found and can be explained by basic principles. Using mixtures of TiH2 and ZrH2 with Cu the ratio of hydrogen and Cu lines has a good correlation with the corresponding concentration ratio. The hydrogen emission yield however decreases over 0.3 m% hydrogen and finally the hydrogen intensity may even decrease. This behaviour can be explained by a very similar quenching of the hydrogen and copper intensity caused by the hydrogen effect. First experiments with GD-MS show no saturation of the hydrogen ion current and thus confirm the quenching of the emission yield in GD-OES. Sintered material for the oxygen calibration (Al2O3, CuO, Cu2O and MgO mixed with Cu, Al and Mg) confirmed the blue line shift effect at O I 130.22 nm, first time reported by Köster 2009 [1]. The effect is more pronounced at Mg than in Al and Cu, which due to line interference leads to a matrix dependent EY. This effect is negligible at O I 777.19 nm and the EY is matrix independent. Using GD-MS first promising results for the calibration of oxygen with these sintered samples could be obtained, when the sputtering rate was included in the evaluation. More recently also sintered material for nitrogen calibration (AlN mixed with Al and Si3N4 mixed with Cu) was produced and points to a matrix independent emission yield of nitrogen T2 - 04 IGDSS CY - Berlin, Germany DA - 15.04.2018 KW - Glow Discharge KW - Non metals PY - 2018 AN - OPUS4-46223 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pisonero, J. T1 - Fast elemental depth profile analysis of nano and micro layers with high sensitivity using pulsed glow discharge mass spectrometry N2 - Innovative material with outstanding physical and chemical properties are produced upon the deposition of thin and ultrathin coatings on different substrates. For instance, hard disks able to store Tera-bytes of information are based on the deposition of multiple nano-layers, which include magnetic and non-magnetic layers. Many other analogous examples, including photovoltaic cells, coated Al substrates, oxidized thin film composite membranes, coated glasses, coated polymers, etc. could be cited. The physical performance of these emerging materials is directly related to their chemical properties, including the elemental distribution within the different layers and at the layer-interfaces, or the presence of critical non-desired trace elements. Therefore, quality control and R+D advances require the development of direct solid analytical techniques able to provide fast multi-elemental chemical analysis of these materials, with high depth resolution (to monitor the different layers) and high sensitivity (to detect major, minor and trace elements). Atomic spectrometry techniques have long been used for direct elemental chemical characterization. Techniques, such as Secondary Ion Mass Spectrometry or Auger Electron Spectroscopy provide very valuable information about the chemical composition of the surfaces/coatings; however, they also have some major drawbacks, such as high operating costs, complex sample pre-treatment and handling, low sample throughput and/or severe matrix effects that result in difficult quantification procedures. To overcome some of these drawbacks Glow Discharge Mass Spectroscopy is proposed as a complementary methodology that provides an ideal solution for fast and accurate bulk and layer analyses. In this work, we evaluate the advantages and limitations of this technique and we discuss about recent progresses and new applications. T2 - JAI Conference , 15th Instrumental Analysis Conference CY - Barcelona, Spain DA - 03.10.2017 KW - GDMS KW - Pulsed KW - Depth profile PY - 2017 AN - OPUS4-46226 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pisonero, J. T1 - Glow Discharge Mass Spectrometry: a superstar for fast depth profiling N2 - A plethora of innovative materials are produced by depositing thin and ultrathin coatings on different substrates. For instance, hard disks able to store terabytes of information are based on multiple magnetic and non-magnetic nano-layers. Moreover, protectives coatings might be used to enhance the mechanical properties of substrate materials; for instance Zn-based coatings are used in the Al industry. In this context, solid analytical techniques are required to provide fast multi-elemental chemical analyses with high depth resolution (to monitor the different layers) and high sensitivity (to detect major, minor and trace elements). Direct solid analytical techniques, including Secondary Ion Mass Spectrometry, Secondary Neutral Mass Spectrometry, Auger Electron Spectroscopy or X-Ray Photoelectron Spectroscopy provide very valuable information about the atomic chemical composition of the surfaces/coatings; however, they also have some major drawbacks, such as high operating costs, complex sample pre-treatment and handling, low sample throughput and/or severe matrix effects that result in difficult quantification procedures. In order to overcome some of these drawbacks Glow Discharge Mass Spectroscopy (GD-MS) is proposed as a complementary methodology that provides an ideal solution for fast and accurate bulk and layer analyses. In this work, we evaluate the advantages and limitations of this technique and we discuss about recent progresses and new applications. T2 - Scix CY - Reno, USA DA - 08.10.2017 KW - GDMS KW - Depth profiling PY - 2017 AN - OPUS4-46228 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - The USE of GDMS in the certification procedure of reference materials N2 - Reference materials are essential, when the accuracy and reliability of measurement results need to be guaranteed in order to generate confidence in the analysis. These materials are frequently used for determining measurement uncertainty, for validation of methods, suitability testing and quality assurance. Especially direct solid sampling methods require reference materials for calibration. They guarantee that measurement results can be compared to recognized reference values. This presentation gives an overview about the use of GDMS in various certification procedures. Because it represents a fast, sensitive, multielement analyses technique without extensive sample preparation it plays a special role for the purity determination of high purity standards. Various calibration strategies and the preparation of traceable matrix matched calibration standards will be discussed. For the certification of analyte content in matrix materials mainly techniques with solvent sample preparation are used. Here GD-MS is used to identify possible loss or contamination with analytes during the sample preparation step. Typically used acids to dissolve matrices lead to interferences in the ICP- mass spectrometric detection of various analytes and their quantification. Here GD-MS as direct method can also add an important contribution in the certification process. T2 - 4th IGDSS CY - Berlin, Germany DA - 15.04.2018 KW - GDMS KW - Reference materials PY - 2018 AN - OPUS4-46222 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weber, M. T1 - European Pharmacopoeia reference standards to underpin the legal requirements in Europe for the control of elemental impurities in medicinal products for human use N2 - Guideline ICH Q3D on elemental impurities (EI) was adopted by the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) and published in December 2014. The European Medicines Agency (EMA) Committee for Medicinal Products for Human use (CHMP) adopted guideline Q3D in December 2014 and defined the dates for coming into effect . ICH Q3D is the first globally harmonised guidance to control 24 elemental impurities in drug products administered by oral, parenteral and inhalation routes. The policy entails a paradigm shift, moving away from substance-based testing towards risk-based assessment and control strategy. In the context of implementing Q3D in Europe, several texts and monographs of the European Pharmacopoeia (Ph. Eur.) were revised, rendering the guideline legally binding in 38 European countries. Ph. Eur. general chapter 5.20. has been modified to reflect ICH Q3D guideline and the old fashioned heavy metals test, Ph. Eur. 2.4.8., has been deleted from individual Ph. Eur. monographs for substances for human use. Furthermore, general chapter Ph. Eur. 2.4.20. Determination of metal catalyst and metal reagent residues has been completely revised and renamed Determination of elemental impurities. Whatever the chosen analytical method, reference materials with a known content of the target element are required for the quantification of elemental impurities. This led EDQM to consider the establishment of suitable reference materials. However, due to lack of specific experience and technical equipment, external partners were sought. Three key European institutes (JRC, BAM and PTB) were identified and involved in the project. To mitigate the overall risk at first the project focussed on the elements classified by ICH Q3D as Class 1: lead, cadmium, mercury and arsenic. A key necessity was the traceability of the element content to the SI (International System of Units Measurement) to allow metrologically reliable and reproducible determination. This required new and specific approaches to be developed by the partners in charge (BAM and PTB). Since January 2018 lead solution CRS, cadmium solution CRS, mercury solution CRS and arsenic solution CRS are available to the users of the Ph. Eur. . T2 - BERM-15 CY - Berlin, Germany DA - 23.09.2018 KW - Pharmacopea KW - Reference standards KW - Elemental impurities KW - Medicinal products PY - 2018 AN - OPUS4-46217 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Bestimmung von Messunsicherheiten N2 - Praxisbezogene Ansätze zur Abschätzung der Messunsicherheit von Daten aus dem chemischen Labor werden gegeben. T2 - Jahrestagung GDMB CY - Kassel, Germany DA - 07.11.2017 KW - Messunsicherheit KW - GUM PY - 2017 AN - OPUS4-46220 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Zertifizierung von Referenzmaterialien an der BAM N2 - Wege zur Zertifizierung von Referenzmaterialien an der BAM werden anhand des Leitfadens und praktischer Beispiele gegeben. T2 - Schulung zur Zertifizierung von RM CY - Berlin, Germany DA - 11.04.2018 KW - Referenzmaterialien KW - Zertifizierung PY - 2018 AN - OPUS4-46221 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Richter, Silke T1 - Characterisation of a high purity nickel material to be used as a primary standard for element determination N2 - A candidate material for the use as primary standard for nickel determination was characterized with respect to total purity. For element determination a pure material can serve as primary standard. However, real world materials are never absolutely pure, hence the total purity of such materials need to be determined experimentally. A reasonable target uncertainty for the purity statement is 10-4 relative. Usually, the purer the material, the easier it is to achieve this target uncertainty. There are two basic ways in order to be able to establish a total purity statement. One is to determine the main component of a high purity material by a direct method such as coulometry, gravimetry or titrimetry. However, these methods are not selective enough for one element and therefore require certain efforts to analyse the material with respect to impurities with interfering analytes. Moreover, to reach the defined target uncertainty is not easy or often impossible to achieve. The second approach is to determine the sum of all possible impurities (as mass fraction) and to subtract it from the ideal purity of 100 % (1 kg/kg). In principle all impurities (all elements not being the matrix element), metals and non-metals must be considered. In this work both approaches to determine the total purity of the nickel material were followed and compared. The primary (solid) standards are usually used to prepare primary calibration solutions to which secondary and lower order calibration solutions are linked. T2 - BERM-15 CY - Berlin, Germany DA - 23.09.2018 KW - Primary standard KW - High purity material KW - Nickel PY - 2018 AN - OPUS4-46216 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tobias, Charlie T1 - Dip-stick coated with Polystyrene-Silica Core-Shell particles for the detection of microbiological fuel contamination N2 - The microbial contamination of fuels by fungi or bacteria presents risks such as corrosion and fuel system fouling, which can produce critical problems in refineries and distribution systems and has a significant economic impact at every phase of the process. Many factors have been cited as responsible for microbial growth, like the presence of water in the storage tanks. Indeed, only 1 % water in a storage system is enough for the growth of microorganisms like bacteria or yeasts, as well as for the development of fungal biomass at the oil/water interface.1 In this work, a rapid test for the accurate determination of genomic DNA from aqueous fuel extracts is presented. The detection is based on the employment of polystyrene-mesoporous silica core-shell particles, on which modified fluorescent molecular beacons are covalently grafted. Those beacons incorporate in the hairpin loop a target sequence highly conserved in all bacteria, corresponding to a fragment of the 16S ribosomal RNA subunit. The designed single-stranded molecular beacon contained fluorescein as an internal indicator and a quencher in its proximity when not hybridized. Upon hybridization in presence of the target sequence, the indicator and the quencher are spatially separated, resulting in fluorescence enhancement. To perform the assay the designed particles were disposed on different glass fiber strips to try to achieve a portable and sensitive rapid test. Assays showed that presence of genomic DNA extracts from bacteria down to 50–70 μg L-1 induces a fluorescence response. The optical read-out was adapted for on-site monitoring by adapting a 3D-printed case on a conventional smartphone, taking advantages of the CMOS detector sensitivity.2 Such embedded assembly allowed to detect genomic DNA in aqueous extracts down to the mg L-1 range and presents an interesting step toward on-site monitoring of fuel contamination. T2 - Europtrode 2021 CY - Warsaw, Poland DA - 28.11.2021 KW - Bacgteria KW - Fungi KW - Rapid test KW - Fluorescence KW - Smartphone KW - Biofouling PY - 2021 AN - OPUS4-53867 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Next level lithium isotope analysis by atomic absorption spectrometry in combination with machine learning N2 - An alternative method for lithium isotope amount ratio analysis is proposed by combining atomic absorption spectrometry with spectra data analysis by machine leaning. It is based on the well-known isotope shift of around 15 pm for the electronic transition at wavelength 670.7845 nm which can be measured by a high-resolution continuum source atomic absorption spectrometer (HR-CS-AAS). For isotope amount ratio analysis, a scalable three boosting machine learning algorithm (XGBoost) was employed and calibrated with a set of samples with a 6Li isotope amount fraction ranging from 99% to 6%. The absolute Li isotope amount fractions of these calibration samples were previously measured by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) and used as ab-initio data for the machine learning algorithm. Validation of the machine leaning model was performed with two standard reference materials (LSVEC and IRMM-016). The procedure was employed for the isotope amount ratio determination of a set of stock chemicals (Li2CO3, LiNO3, LiCl, LiOH, and LiF) as well as a BAM candidate LiMNC cathode reference material. Achieved uncertainties are one order of magnitude higher than those obtained by MC-ICP-MS. This precision and accuracy is nonetheless sufficient to resolve natural occurring variations in Lithium isotope ratios. Also, the LiMNC material was analyzed by HR-CS-AAS with and without matrix purification. The results are comparable within statistical error. T2 - Make and Measure 2020 CY - Online Meeting DA - 15.10.2020 KW - Lithium batteries KW - HR-CS-AAS KW - Machine learning KW - Isotope analysis KW - Spectrometry PY - 2020 AN - OPUS4-51541 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bell, Jérémy A1 - Tillo, Adam A1 - Chauhan, Vraj P. A1 - Bartelmeß, Jürgen A1 - Rurack, Knut T1 - Microfluidic analytical tool coupling a fluorescent molecular probe and a micro-hydrocyclone for the detection of water chlorination level N2 - Chlorination of pool water and wastewater, in food and pharmaceutical production, as well as in pesticide and paper manufacturing is a routinely used technique. However, the amount of chlorine in water must be strictly adjusted, to ensure enough concentration to kill pathogenic bacteria and viruses, while preventing too high concentrations inducing negative effects on human health. As an indicator, a molecular fluorescent probe based on a BODIPY structure was designed. This indicator exhibits a sensitive and selective fluorescence response upon increasing concentrations of hypochlorite in aqueous solvent mixtures. Real-time analyses became possible after the integration of this fluorescent indicator into newly designed 2D & 3D microfluidic chips incorporating a passive sinusoidal mixer and a micro-hydrocyclone, respectively. A comparison of the two microfluidic systems, including their ability to prevent accumulation or circulation of microbubbles, has shown excellent fluidic behaviour for the micro-hydrocyclone device. This system was distinctly more robust against gas bubbles, showed a higher signal gain and allowed to halve the limit of detection to 0.02 mg L–1. The use of the 3D system to quantify the chlorine content of pool water samples for sensitive and quantitative chlorine monitoring has been demonstrated. T2 - Konferenz CY - Ioannina, Greece DA - 22.09.2019 KW - Chlorine KW - Fluorescence KW - Microfluidics KW - Water KW - Chlor KW - Fluoreszenz KW - Mikrofluidik KW - Wasser PY - 2019 UR - https://media.conferre.gr/index.php/photos-videos/ima2019 AN - OPUS4-49130 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gojani, Ardian A1 - Tobias, Charlie A1 - Hülagü, Deniz A1 - Rurack, Knut A1 - Hodoroaba, Vasile-Dan T1 - Toward determination of the surface roughness of particles from a SEM image N2 - In this communication, we address the issue of roughness measurement by investigating if the grayscale values from SEM images can be used for surface roughness determination of spherical particles. KW - MamaLoCA KW - Core-shell particles KW - Electron microscopy KW - Image processing KW - Particle characterisation KW - Roughness PY - 2021 DO - https://doi.org/10.1017/S1431927621011375 SN - 1431-9276 SN - 1435-8115 VL - 27 IS - Suplement S1 SP - 3302 EP - 3305 PB - Cambridge University Press CY - New York, NY AN - OPUS4-53283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Andresen, Elina T1 - Lanthanide based multi element nanoparticles: a versatile platform for surface chemistry analysis and potential reference materials N2 - The use of engineered nanoparticles of different size, shape, and composition is continuously increasing in the life and materials sciences. This calls for methods and reference materials enabling the reliable and accurate determination of nanoparticle size, particle size distribution, shape, number concentration, degree of aggregation and agglomeration in different environments as well as for nanoparticle dispersibility and stability. We are currently building up and exploring a platform of lanthanide-based nanocrystals (LnNCs) with application-specifically tuned size, shape, composition, architecture, optical properties, and surface chemistry for emerging applications in life sciences. As a prerequisite for the broad applicability of these nanomaterials, we assess simple, robust, and easily upscaleable synthesis protocols for LnNCs with defined morphologies and tunable optical properties, and the short-term and long-term stability of LnNCs with selected surface coatings in aqueous environments under different application-relevant conditions. T2 - Anakon 2025 CY - Leipzig, Germany DA - 10.03.2025 KW - Nano KW - Particle KW - Method KW - Lanthanide KW - Synthesis KW - Upconversion KW - Ligand KW - Quality assurance KW - Particle number concentration KW - Reference material KW - Surface chemistry PY - 2025 AN - OPUS4-62768 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bierstedt, Andreas A1 - Warschat, Carsten A1 - You, Yi A1 - Rurack, Knut A1 - Riedel, Jens T1 - Stimulated Raman scattering by intracavity mixing of nanosecond laser excitation and fluorescence in acoustically levitated droplets N2 - Raman spectroscopy is becoming a commonly used, powerful tool for structural elucidation and species identification of small liquid samples, e.g. in droplet-based digital microfluidic devices. Due to the low scattering cross sections and the temporal restrictions dictated by the droplet flow, however, it depends on amplification strategies which often come at a cost. In the case of surface-enhanced Raman scattering (SERS), this can be an enhanced susceptibility towards memory effects and cross talk, whereas resonant and/or stimulated Raman techniques require higher instrumental sophistication, such as tunable lasers or the high electromagnetic field strengths which are typically provided by femtosecond lasers. Here, an alternative instrumental approach is discussed, in which stimulated Raman scattering (SRS) is achieved using the single fixed wavelength output of an inexpensive diode-pumped solid-state (DPSS) nanosecond laser. The required field strengths are realized by an effective light trapping in a resonator mode inside the interrogated droplets, while the resonant light required for the stimulation is provided by the fluorescence signal of an admixed laser dye. To elucidate the underlying optical processes, proof-of-concept experiments are conducted on acoustically levitated droplets, mimicking a highly reproducible and stable digital fluidic system. By using isotope-labeled compounds, the assignment of the emitted radiation as Raman scattering is firmly corroborated. A direct comparison reveals an amplification of the usually weak spontaneous Stokes emission by up to five orders of magnitude. Further investigation of the optical power dependence reveals the resulting gain to depend on the intensity of both, the input laser fluence and the concentration of the admixed fluorophore, leaving SRS as the only feasible amplification mechanism. While in this study stable large droplets have been studied, the underlying principles also hold true for smaller droplets, in which case significantly lower laser pulse energy is required. Since DPSS lasers are readily available with high repetition rates, the presented detection strategy bears a huge potential for fast online identification and characterization routines in digital microfluidic devices. KW - Ultrasonic levitation KW - Stimulated Raman Spectroscopy PY - 2020 DO - https://doi.org/10.1039/D0AY01504K VL - 12 IS - 42 SP - 5046 EP - 5054 PB - Royal Society of Chemistry AN - OPUS4-51566 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gojani, Ardian T1 - Examples of embedded & microfluidic-based sensors N2 - Sensors are the scientific and technological extension of human senses and enormously expand human capabilities. Despite the fact that scientific and technological advances are usually seen in a positive light, the name of this conference, Sensors for Good, put me in a bit of a trouble, because in general science does not operate in ethical categories, but instead it just tells how far from the truth one is. In this respect, sensors help us in recognizing states and events beyond our immediate reach. Fortunately, sensors are used for many applications, such as environmental monitoring, food control, and alike, which unequivocally benefit society. I will focus on a particular type of sensors, those that rely on microfluidics for operation and which are typically realized in lab-on-a-chip (LOC) devices. In this domain, where at least one of the dimensions through which a fluid flows is submillimetric, our natural senses fail, because the phenomena are too small to be detected either by eye, smell, touch, and even the common sense explanation that we learn for many years in school is not applicable, because the phenomena are dominated by different parameters. To give one simple example, in general the direction of flow in microfluidic channels does not depend on the up-down direction of the channel, because gravitational force or the weight of the fluid is negligible compared to the viscous forces present on the chip. This presentation consists of three parts: initially, two sensors produced in our lab are presented, followed by a simulation oriented discussion on microfluidics and biosensors, and finally a project in progress that we are involved in is presented, concluding with a list of open issues raised during the presentation. T2 - Software Freedom Kosova Conference CY - Online meeting DA - 26.09.2020 KW - Sensors KW - Cocaine detection KW - Fuel adulteration KW - MamaLoCA PY - 2020 AN - OPUS4-51396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wan, Wei A1 - Wagner, Sabine A1 - Rurack, Knut T1 - Fluorescent monomers: "bricks" that make a molecularly imprinted polymer "bright" N2 - Molecularly imprinted polymers (MIPs) are potent and established recognition phases in separation and enrichment applications. Because of their robustness, versatility and format adaptability, they also constitute very promising sensing phases, especially when the active sensing element is directly integrated into the MIP. Fluorescent MIPs incorporating fluorescent monomers are perhaps the best developed and most successful approach here. This article reviews the state of the art in this field, discussing the pros and cons of the use of fluorescent dye and probe derivatives as such monomers, the different molecular interaction forces for template complexation, signalling modes and a variety of related approaches that have been realized over the years, including Förster resonance energy transfer processes, covalent imprinting, postmodification attachment of fluorescent units and conjugated polymers as MIPs; other measurement schemes and sensing chemistries that use MIPs and fluorescence interrogation to solve analytical problems (fluorescent competitive assays, fluorescent analytes, etc.) are not covered here. Throughout the article, photophysical processes are discussed to facilitate understanding of the effects that can occur when one is planning for a fluorescence response to happen in a constrained polymer matrix. The article concludes with a concise assessment of the suitability of the different formats for sensor realization. KW - Chemical sensors KW - Fluorescence KW - Molecularly imprinted polymers KW - Dyes KW - Sol-gel PY - 2016 DO - https://doi.org/10.1007/s00216-015-9174-4 SN - 1618-2642 SN - 1618-2650 VL - 408 IS - 7 SP - 1753 EP - 1771 PB - Springer CY - Berlin AN - OPUS4-35830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gotor, Raúl A1 - Tiebe, Carlo A1 - Schlischka, Jörg A1 - Bell, Jérémy A1 - Rurack, Knut T1 - Detection of adulterated diesel using fluorescent test strips and smartphone readout N2 - The fluorescence properties of three molecular rotors, related to 4-dimethylamino-4-nitrostilbene (4-DNS), are studied versus different diesel/kerosene blends. In nonviscous solvents, these compounds can populate a twisted intramolecular charge transfer state which deactivates nonradiatively, successfully suppressing fluorescence emission. Solution experiments with diesel/kerosene blends showed a good linear correlation between the fluorescence intensity of the probe molecules and the diesel fraction of the blend. The dyes have been immobilized on paper, retaining their fluorescence behavior, i.e., negligible emission in the presence of nonviscous organic solvents and increasing fluorescence when the environment is increasingly viscous. When the impregnated paper is devised as a test strip, the latter is compatible with a newly designed smartphone reader system, which allows in-the-field measurements. The method can safely detect the presence of kerosene in diesel at ≥7%, which competes favorably with current standard methods for the detection of diesel adulteration. KW - Fuel adulteration KW - Diesel KW - Fluorescence KW - Test strip KW - Molecular rotor KW - Smartphone PY - 2017 DO - https://doi.org/10.1021/acs.energyfuels.7b01538 SN - 0887-0624 VL - 31 IS - 11 SP - 11594 EP - 11600 PB - American Chemical Society CY - Washington, D.C. AN - OPUS4-43103 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gawlitza, Kornelia A1 - Tiebe, Carlo A1 - Banach, Ulrich A1 - Noske, Reinhard A1 - Bartholmai, Matthias A1 - Rurack, Knut T1 - Novel sensor for long-term monitoring of ammonia in gas phase N2 - Because ammonia and its reaction products can cause considerable damage to human health and ecosystems, there is a need for reliably operating and reversibly interacting sensor materials to monitor traces of gaseous ammonia in ambient air, which at best can be used on-site for in-the-field measurements. Herein, the development of a sensor material for gaseous ammonia in the lower ppm to ppb range using optical fluorescence as transduction mechanism is presented. A fluorescent dye, which shows reversible fluorescence enhancement in the presence of ammonia is incorporated into a polymer matrix, the latter to ensure the accumulation of ammonia. The sensor material is integrated into a prototype of a miniaturized sensor device, facilitating long-term operation. To calibrate the optical sensor system a gas standard generator, producing standard gas mixtures, is used, leading to a sensitivity down to lower ppm concentrations of ammonia. T2 - 13. Dresdner Sensor-Symposium 2017 CY - Dresden, Germany DA - 04.12.2017 KW - Ammonia gas sensor KW - Fluorescence KW - Air quality monitoring KW - Standard gas generator KW - Miniaturized sensor device PY - 2017 DO - https://doi.org/10.5162/13dss2017/P4.02 SP - P4.02, 272 EP - 276 AN - OPUS4-43352 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mekonnen, Tessema Fenta T1 - Investigation of chlorpyrifos and its transformation products in food samples N2 - Chlorpyrifos (CPF), an anticholinesterase organophosphate insecticide, is commonly used to control pests in agricultural sectors. In recent years, it is one of the most frequently detected residues in fruits and vegetables. On the other hand, pesticides including chlorpyrifos undergo extensive abiotic (industrial processes, waste treatments and photodegradations) and/or biotic (metabolism and microbial activities) processes which lead to transformation products (TPs) with different toxicity. Furthermore, lack of representative standards and complexity of transformation mechanisms make monitoring of TPs in real samples difficult. The aim of this work was to investigate CPF and its TPs in selected food matrices. Representative standards of TPs were synthesized by electrochemistry coupled online to liquid chromatography-mass spectrometry (EC/LC/MS) that equipped with a follow-through and/or synthesis cell with boron doped diamond working electrode. The TPs were characterized by LC-MS/MS and high resolution mass spectrometry (HRMS) and used for real sample investigations. Different fruit and spice samples (fortified by TPs standards and blank) were extracted by dispersive solid phase extraction (dSPE) and analyzed by LC-MS/MS. Recoveries were obtained ranging between 94 – 101% (with matrix effect 85 – 97%). The method limit of detection (LOD) and quantification (LOQ) for CPF were 1.9 and 5.7 µg/kg, respectively. Among investigated samples CPF was detected in fresh lemon, black pepper and fenugreek seed with a content of 104, 31 and 4 µg/kg, respectively. Coriander and cinnamon samples also contained trace levels of CPF (150 µg/kg, because of different diffusion properties for various PFAS, but also kinetic exchange limitations. However, the DGT approach has the advantage that almost no sample preparation is necessary. Moreover, the PFAS adsorption on the DGT binding layer was investigated via surface sensitive spectroscopical methods, such as Fourier-transform infrared (FT-IR) and fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy. T2 - DGT Konferenz CY - Paris, France DA - 11.10.2023 KW - Combustion Ion Chromatography KW - Per- and Polyfluoroalkyl substances (PFAS) KW - Sewage sludge PY - 2023 AN - OPUS4-58575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - López-Puertollano, Daniel T1 - Superparamagnetic core-shell particles application: from cytometry assay to simplified fluidic system N2 - Superparamagnetic hybrid polystyrene-core silica-shell beads have emerged as promising alternatives to traditional in flow cytometry-based competitive antibody assays [1]. These materials consist of a polystyrene core and a silica shell, in which magnetic nanoparticles are embedded, facilitating the handling and retention in tests. The outer silica surface allows for easy modification through silane chemistry, allowing the attachment of antibodies, or other molecules of interest. Ochratoxin A (OTA), a mycotoxin that can be found in grain products, coffee, cacao, or grapes, was chosen as the main target analyte to detect [2]. In this study, previously in house produced anti-OTA antibodies [3] were attached to the surface of the particles and the whole system was used as detection entity. In a first approach, the system was used for the development of a competitive cytometry assay using an OTA-fluorescein (OTA-F) adduct as competitor and marker. In this assay the fluorescence emitted by the OTA-F competitor on the surface of the particle was detected at a wavelength of 518 nm using a 533/30.H filter and was correlated to the forward scatter (FSC) to distinguish it from the excess of competitor still in solution. Under optimised conditions, the final assay showed a limit of detection of 0.03 nM. In a second approach, a simplified ready-to-inject fluidic system was built based on a laser (488 nm) and a photomultiplier detector to measure the signal of competitor still in solution. The competition step was carried out in a vial and the whole mixture was injected into the fluidic system. To avoid signal scattering, the particles were separated in-line using a magnet and only the OTA-F competitor still in solution was detected, reaching a limit of detection of 1.2 nM. With the aim to reduce user manipulation, the final assay is still under development for in-line incubation during the competitive step. T2 - 15th Rapid Methods Europe Conference CY - Amsterdam, Netherlands DA - 06.11.2023 KW - Microfluidics KW - Flow cytometry KW - Bead-based assays KW - Magnetic beads KW - Core-shell particles KW - Immunoassays PY - 2023 AN - OPUS4-58817 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Chemical characterization of aging processes in high energy-density lithium-ion batteries N2 - Introduction Lithium-ion batteries (LIBs) are one key technology to overcome the climate crisis and energy transition challenges. Demands of electric vehicles on higher capacity and power drives research on innovative cathode and anode materials. These high energy-density LIBs are operated at higher voltages, leading to increased electrolyte decay and the current collectors' degradation. Even though this fundamental corrosion process significantly affects battery performance, insufficient research is being done on the aluminum current collector. Fast and convenient analytical methods are needed for monitoring the aging processes in LIBs. Methods In this work glow-discharge optical emission spectrometry (GD-OES) was used for depth profile analysis of aged cathode material. The measurements were performed in pulsed radio frequency mode. Under soft and controlled plasma conditions, high-resolution local determination (in depth) of the elemental composition is possible. Scanning electron microscopy (SEM) combined with a focused ion beam (FIB) cutting and energy dispersive X-ray spectroscopy (EDX) was used to confirm GD-OES results and obtain additional information on elemental distribution. Results The aging of coin cells manufactured with different cathode materials (LCO, LMO, NMC111, NMC424, NMC532, NMC622, and NMC811) was studied. GD-OES depth profiling of new and aged cathode materials was performed. Quantitative analysis was possible through calibration with synthetic standards and correction by sputter rate. Different amounts of aluminum deposit on the cathode surface were found for different materials. The deposit has its origin in the corrosion of the aluminum current collector. The results are compatible with results from FIB-EDX. However, GD-OES is a faster and less laborious analytical method. Therefore, it will accelerate research on corrosion processes in high energy-density batteries. Innovative aspects - Quantitative depth profiling of cathode material -Monitoring of corrosion processes in high energy-density lithium-ion batteries - Systematic investigation of the influence of different cathode materials T2 - ANAKON 2023 CY - Vienna, Austria DA - 11.04.2023 KW - Lithium Ion Batteries KW - GD-OES KW - Depth-profiling PY - 2023 AN - OPUS4-58586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lisec, Jan T1 - When drowning in data - start swimming N2 - A presentation on the subject of Automatic Data Processing Skills in Chemistry to Enhance Scientific Research. T2 - 7th PhD Seminar of the German Working Group for Analytical Spectroscopy (DAAS) in the GDCh Division of Analytical Chemistry CY - Berlin, Germany DA - 15.11.2023 KW - Data KW - Automation KW - Programming PY - 2023 AN - OPUS4-58902 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Lisec, Jan T1 - MetabolomicsBasics (R package to process and analyze metabolomics datasets) N2 - Raw data from metabolomics experiments are initially subjected to peak identification and signal deconvolution to generate raw data matrices m × n, where m are samples and n are metabolites. We describe here simple statistical procedures on such multivariate data matrices, all provided as functions in the programming environment R, useful to normalize data, detect biomarkers, and perform sample classification. KW - Software KW - Mass Spectrometry KW - R package KW - Data processing PY - 2018 UR - https://github.com/cran/MetabolomicsBasics/ PB - GitHub CY - San Francisco, CA, USA AN - OPUS4-57854 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lisec, Jan T1 - Metabolomics N2 - A 90 minutes overview on metabolomics as an analytical method for life sciences. T2 - IceBio Network training event CY - Grenoble, France DA - 29.02.2024 KW - Mass Spectrometry KW - Metabolomics KW - Data Analyses PY - 2024 AN - OPUS4-59596 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Abad Andrade, Carlos Enrique T1 - What does GD-OES reveal about the aging and manufacturing processes of lithium-ion batteries? N2 - Glow-Discharge Optical Emission Spectroscopy (GD-OES), a powerful analytical technique, sheds light on the two critical aspects of lithium-ion batteries (LIBs): manufacturing and aging 1, 2. We optimized cell production in manufacturing by adjusting parameters, including cathode doping, electrolyte concentration, and pressing force. GD-OES provided in-depth elemental composition and homogeneity analysis, which is crucial for identifying optimal manufacturing conditions. These findings were validated by electrochemical impedance spectroscopy, confirming the quality of the manufactured batteries. Shifting the focus to aging, we use GD-OES for fluorine depth profiling, a key element in understanding polymer and electrolyte degradation. However, fluorine presents analytical challenges. We addressed this by substituting argon with a neon:argon mixture, which significantly enhanced fluorine detection sensitivity. This advancement not only improves accuracy but also holds the potential to guide sustainable and cost-efficient manufacturing strategies. Through its versatility, GD-OES has proven to be a powerful tool for not only optimizing LIB manufacturing processes but also gaining deeper insights into their aging mechanisms. This research extends beyond academic interest, offering tangible benefits for the industry by translating into improved battery quality, extended lifespan, and overall performance. T2 - The 6th International Glow Discharge Spectroscopy Symposium CY - Liverpool, United Kingdom DA - 21.04.2024 KW - GD-OES KW - Depth profiles KW - Lithium KW - Battery KW - Fluorine KW - Aging KW - Manufacturing KW - Glow-discharge PY - 2024 AN - OPUS4-59945 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Prakash, Swayam T1 - Photophysical Understanding of Urobilin and its Zinc Complexes for Water Quality Testing N2 - Faecal contaminants in water are considered serious threats for human health, due to the presence of viruses, bacteria and other harmful microorganisms.1 Urobilin (UB) is a well-known faecal pigment and can be used as a marker for faecal matter in water.2 UB is commonly present in the urine of all mammals as the catabolic end product of bilirubin degradation.2 As the only simple chemical approach to its detection, Schlesinger’s test is usually used to enhance the weak fluorescence of UB in alcoholic media by complexation with Zinc.2, 3 The major limitation of this method is the only weak enhancement of the intrinsically weak UB fluorescence in aqueous media.3 This work presents an approach to introduce different Zn salts for improved fluorescence response, where we found a clear dependence of the fluorescence yield of UB-Zn(II) complexes on the counterion of the salt in water. By employing a combination of fluorescence parameters like transition energy, fluorescence intensity, and fluorescence lifetime, a photophysical understanding of the structure and conformation of the UB-Zn(II) complexes responsible for the fluorescence enhancement in water could be gained. The possibilities of developing a sensitive analytical method based on the acquired understanding are also discussed. T2 - Central European Conference on Photochemistry CECP 2024 CY - Bad Hofgastein, Austria DA - 18.02.2024 KW - Water analysis KW - Faecal contamination KW - Metal complexes KW - Fluorescence PY - 2024 AN - OPUS4-59874 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Herter, Sven-Oliver T1 - Synthesis and application of isotopic labelled ergot alkaloids N2 - Ergot alkaloids form a toxicologically relevant group of mould toxins (mycotoxins) that are among the most common contaminants of food and animal feed worldwide. Reliable controls are essential to minimise health risks and economic damage. Due to their toxicological relevance, EU limit values for 12 priority ergot alkaloids have been introduced for the first time in 2022 and range from 500 µg/kg in rye milling products down to 20 ug/kg Processed cereal-based foods for infants and young children[1]. High-performance liquid chromatography - mass spectrometry is used to quantify low concentrations of ergots in food, however the European standard analytical procedure cannot be applied due to the lack of isotopically labelled reference standards. The complex structure of the ergot alkaloids makes a total synthesis extremely challenging, expensive and time-consuming. Therefore, we are focusing on different semi-preparative methods (electrochemistry, organic synthesis, heterogeneous catalysis) to specifically N-demethylate the C8 carbon atom of the lysergic acid moiety. The norergot alkaloid formed is then isotopically labelled using an electrophilic methyl source, i.e. iodomethane or dimethyl sulphate to obtain the specific isotopic labelled ergot alkaloid. Initial experiments have shown that N-demethylation of the ergot alkaloid ergotamine is possible by both electrochemical and wet-chemical organic synthesis. The next step is to adapt the previously determined reaction conditions to enable the synthesis of norergotamine on a mg scale. T2 - 41. International Conference on Environmental & Food Monitoring CY - Amsterdam, Netherlands DA - 20.11.2023 KW - Reference materials KW - Metrology KW - Isotope dilution analysis KW - Calibration standards PY - 2023 AN - OPUS4-59234 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Fluorine Depth Profiling in Lithium-Ion Battery Materials by GD-OES N2 - Lithium-ion batteries are a key technology for tackling challenges in energy and climate crisis, but up to 30 % are discarded right after production. Quality is closely related to the homogeneity of the used materials and coatings. Fluorine compounds, both in the polymer and from degradation of the electrolyte, are of special interest for the formation and aging of LIBs. Glow-discharge optical emission spectroscopy (GD-OES) emerged as a fast and convenient method for depth-profiling of battery materials. However, fluorine remains a spectroscopic challenge due to a high excitation energy and only few strong emission lines in the UV/Vis spectral range. We investigated the partial substitution of argon with neon in the plasma gas. The main emission line at 685.603 nm was monitored by both photo multiplier tube (PMT) with Czerny-Turner monochromator at 20 µm slit-size, and charge-coupled device (CCD) with 1200 lines/mm grating. For calibration, we used a set of hot-pressed copper cylinders with varying calcium fluoride amount fraction, ranging from 1.6 % to 4.4 %. Plasma gas mixtures with a mole fraction of 5 %, 10 % and 20 % neon in argon were used. Sensitivity in comparison to pure argon was increased by factor 4, 7 and 14, respectively. In general, PMT detection was more sensitive than CCD. As expected, sputter rates decreased with higher neon content in the plasma gas. Depth-profiling of the cathodes was performed in pulsed mode at constant voltage and pressure, which resulted in stable plasma conditions. We achieve matrix-independent quantitative information on fluorine distribution by correction based on sputter rates. This advancement in GD-OES provides a more accurate analytical approach for evaluating the homogeneity of lithium-ion battery materials, potentially leading to more sustainable and cost-effective manufacturing processes. T2 - 6th International Glow Discharge Spectroscopy Symposium CY - Liverpool, United Kingdom DA - 21.04.2024 KW - Lithium Ion Batteries KW - GD-OES KW - depth-profiling KW - fluorine PY - 2024 AN - OPUS4-60200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Jaeger, Carsten T1 - Umfassende Analyse von Leachables aus rezyklierten HDPE-Kanistern N2 - Weitestgehendes Recycling vorhandener Materialien und Produkte ist ein wesentlicher Bestandteil der Kreislaufwirtschaft. Verpackungen auf Kunststoffbasis, darunter Behälter für Lebensmittel und Getränke, aber auch für die Lagerung und den Transport von Chemikalien und Gefahrgütern, werden derzeit größtenteils aus fossilen Rohstoffen hergestellt. Doch selbst für diese „kontaktempfindlichen“ Produkte besteht weiterhin das Ziel der Nachhaltigkeit durch den Einsatz von Recyclingmaterialien. Diese sehr aktuelle Diskussion findet derzeit im Rahmen der EU-Verpackungs- und Verpackungsabfallverordnung (PPWR) statt, die voraussichtlich noch in diesem Jahr abgeschlossen sein wird. Bei Verpackungen für den Transport gefährlicher Güter sind die Sicherheitseigenschaften der Behälter aus „neuen“ Materialien, einschließlich Polyethylen (PE), gut bekannt und werden im Rahmen ihrer Bauartzulassung getestet. Über ihre Gegenstücke aus Recyclingmaterialien ist jedoch weitaus weniger bekannt. Abgesehen von Materialschwächung kann der Eintrag von Rückständen in recycelte Kunststoffe zu einer Verunreinigung der Waren in der Verpackung führen. Um diese Lücke zu schließen, haben wir Kanister aus hochdichtem PE (HDPE) aus Post-Consumer-Abfällen auf die Freisetzung von Kunststoffzusätzen und Verunreinigungen untersucht. Mithilfe eines umfassenden, nicht zielgerichteten Ansatzes mit hochauflösender Massenspektrometrie (HRMS) konnten wir je nach Art der gelagerten Chemikalie und Lagerdauer 895 verschiedene Komponenten detektieren. Die meisten Komponenten waren alleinig oder in wesentlich höherer Konzentration in recyceltem HDPE als in herkömmlichem HDPE nachzuweisen. 154 der Komponenten konnten identifiziert und auf ihre funktionale Verwendung hin analysiert werden. Interessanterweise ergab diese Analyse „Kosmetik“, „Duftstoffe“ und „Geschmacksstoffe“ als Hauptassoziationen neben bekannten und erwarteten Verwendungen im Bereich „Kunststoffe“. Dies deutete auf einen erheblichen Eintrag von Fremdverunreinigungen in das Produkt hin. Rezyklierte Kanister zeigten damit deutliche Nachteile im Vergleich zu herkömmlichen Kanistern. Eine detaillierte Bewertung der Ergebnisse im Hinblick auf die Materialsicherheit in diesem Produktsegment steht noch aus. T2 - Erfahrungsaustausch Verpackungen 2024 CY - Berlin, Germany DA - 17.09.2024 KW - Extractables & Leachables KW - Hochauflösende Massenspektrometrie KW - Nontarget-Analyse KW - Gefahrgutbehälter PY - 2024 AN - OPUS4-61057 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Temgoua, Ranil C. T. T1 - Understanding the behavior of phenylurazoletyrosine- click electrochemical reaction N2 - The electrochemical behavior of 4-phenylurazole (Ph-Ur) was studied and the latter was used as a molecular anchor for the electrochemical bioconjugation of tyrosine (Y). Cyclic voltammetry (CV) and controlled potential coulometry (CPC) allowed to generate in situ from phenylurazole the PTAD (4-phenyl-3H-1,2,4-triazole-3,5(4H)-dione) species on demand for tyrosine electrolabeling. To evaluate the performance of tyrosine electrolabeling, coulometric analyses at controlled potentials were performed on solutions of phenylurazole and the phenylurazole-tyrosine mixture in different proportions (2:1, 1:1, and 1:2). The electrolysis of the phenylurazole-tyrosine mixture in the ratio (1:2) produced a charge of 2.07 C, very close to the theoretical value (1.93 C) with high reaction kinetics, a result obtained here for the first time. The products obtained were identified and characterized by liquid chromatography coupled to high-resolution electrospray ionization mass spectrometry (LC-HRMS and LC-HRMMS). Two products were formed from the click reactions, one of which was the majority. Another part of this work was to study the electrochemical degradation of the molecular anchor 4-phenylazole (Ph-Ur). Four stable degradation products of phenylurazole were identified (C7H9N2O, C6H8N, C6H8NO, C14H13N4O2) based on chromatographic profiles and mass spectrometry results. The charge generated during the electrolysis of phenylurazole (two-electron process) (2.85 C) is inconsistent with the theoretical or calculated charge (1.93 C), indicating that secondary/parasitic reactions occurred during the electrolysis of the latter. In conclusion, the electrochemically promoted click phenylurazole-tyrosine reactions give rise to click products with high reaction kinetics and yields in the (1:2) phenylurazole-tyrosine ratios, and the presence of side reactions is likely to affect the yield of the click phenylurazole-tyrosine reaction. T2 - Les Journées d’Électrochimie 2024 CY - Saint-Malo, France DA - 01.07.2024 KW - Electrochemistry KW - Mass Spectrometry KW - Simulation PY - 2024 AN - OPUS4-61063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Temgoua, Ranil C. T. T1 - Mimicking Environmental Degradation of Carbendazim Pesticide by EC-MS N2 - Currently, there is a growing interest in the study of environmental degradation pathways of organic contaminants such as pesticides, with the objective to better understand their potential risk for environmental systems and living organisms. In this context, DFT (conceptual density functional theory) and predictive methods may systematically be used to simplify and accelerate the elucidation of environmental degradation. We report herein the electrochemical behavior/degradation of the carbendazim (CBZ) fungicide widely used to treat cereal and fruit crops. Oxidative degradation of CBZ was studied using an electrochemical flow-through cell directly coupled to a mass spectrometer for rapid identification of CBZ degradation products. The structural elucidation of CBZ oxidation products was based on retention time, accurate mass, isotopic distribution and fragmentation pattern by using LC-HRMS an LC-HRMS2. The most important chemical reactions found to occur in the transformation of CBZ were hydrolysis and hydroxylation. EC-LC-MS and EC-MS analysis has made it possible to highlight the identification of degradation products of CBZ. In addition to previously known transformation products common to those observed during environmental degradation (monocarbomethoxyguanidine, benzimidazole-isocyanate, 2-aminobenzimidazole, hydroxy-2-aminobenzimidazole, hydroxycarbendazim, CBZ-CBZ dimer), two new degradation products were identified in this work: a quinone imine and a nitrenium ion. Electrochemistry mass spectrometry hyphenated techniques represent an accessible, rapid and reliable tool to elucidate the oxidative degradation of CBZ, including reactive degradation products and conjugates. T2 - 36th Topical Meeting of the International Society of Electrochemistry CY - Šibenik, Croatia DA - 26.05.2024 KW - Electrochemistry KW - Mass Spectrometry KW - Emerging pollutants KW - Transformation products PY - 2024 AN - OPUS4-61062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Biyikal, Mustafa T1 - Development of a handheld device for the trace detection of explosives N2 - This presentation introduces a new explosives trace detector (ETD), a handheld device developed by True Detection Systems (TDS). Addressing the limitations of current handheld detectors—such as unreliable measurements and cumbersome operation— the new ETD XT-1 integrates advanced sensor technology, including a Lab-on-a-Chip, to deliver high sensitivity and accuracy. Capable of detecting trace levels of substances like TNT, TATP, and ammonium nitrate, the device offers rapid, user-friendly detection through AI/ML-enhanced algorithms. These algorithms enable precise substance identification by analyzing absorption and desorption rates, significantly reducing false positives. The XT-1 has broad applications in security, hazardous material detection, and environmental monitoring. T2 - Photonics Days Berlin Brandenburg CY - Berlin, Germany DA - 09.10.2024 KW - Explosives KW - Trace detection KW - Handheld device KW - Lab-on-a-chip KW - Fluorescence PY - 2024 AN - OPUS4-61433 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tavernaro, Isabella A1 - Matiushkina, Anna A1 - Rother, Kai Simon A1 - Mating, Celina A1 - Resch-Genger, Ute T1 - Exploring the potential of simple automation concepts for quantifying functional groups on nanomaterials with optical assays N2 - Until now, automation in nanomaterial research has been largely focused on the automated synthesis of engineered nanoparticles (NPs) including the screening of synthesis parameters and the automation of characterization methods such as electron microscopy. Despite the rapidly increasing number of NP samples analyzed due to increasing requirements on NP quality control, increasing safety concerns, and regulatory requirements, automation has not yet been introduced into workflows of analytical methods utilized for screening, monitoring, and quantifying functional groups (FGs) on NPs. To address this gap, we studied the potential of simple automation tools for the quantification of amino surface groups on different types of aminated NPs, varying in size, chemical composition, and optical properties, with the exemplarily chosen sensitive optical fluorescamine (Fluram) assay. This broadly applied, but reportedly error-prone assay, which utilizes a chromogenic reporter, involves multiple pipetting and dilution steps and photometric or fluorometric detection. In this study, we compared the influence of automated and manual pipetting on the results of this assay, which was automatically read out with a microplate reader. Special emphasis was dedicated to parameters like accuracy, consistency, achievable uncertainties, and speed of analysis and to possible interferences from the NPs. Our results highlight the advantages of automated surface FG quantification and the huge potential of automation for nanotechnology. In the future, this will facilitate process and quality control of NP fabrication, surface modification, and stability monitoring and help to produce large data sets for nanomaterial grouping approaches for sustainable and safe-by-design, performance, and risk assessment studies. KW - Automation KW - Quantification of amino groups KW - Fluorescamine assay KW - Amorphous silica nanoparticles KW - Iron oxide nanoparticles KW - Upconversion nanoparticles PY - 2024 DO - https://doi.org/10.1007/s12274-024-6970-1 VL - 17 IS - 11 SP - 10119 EP - 10126 PB - Springer AN - OPUS4-61459 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Jens T1 - Current Transformations and Challenges through the Eyes of a Scientist at a German Federal Research Agency N2 - Innovative research, harmonized standards, certification of reference products, policy advice and regulatory action. To most researchers, federal research agencies (FRAs) are abstract chimeras as these tasks appear cryptic and unrelated or even entirely incompatible with each other. Instead of one body, they are pictured as a loose conglomerate of individual institutes, agencies, and offices. The German federal institute for materials research and testing (BAM), is currently undergoing a change process to tear down the walls between these disjunct facilities. Apart from an organizational streamlining, such an infrastructure ideally allows for a holistic approach to tackle complex problems. This presentation will shed some light onto the challenges and opportunities arising. Recent years have been dominated by pivotal changes, crises, and challenges. Many scientists see an increasing circularity in material flows and a fossil fuel phase out to be the only feasible way to proceed. By all this, the material world is faced with a plethora of the above mentioned complicate and complex problems. Parallel to these analog challenges, paradigm-changing advancements in robotics, semantic-data technology, and artificial intelligence, currently empower the digital world with unprecedented speed. Using the example of lithium-ion batteries, the talk will showcase modern FRAs as nutritious ecosystem for a holistic approach towards accelerating all future research and development processes. It will give a glimpse of the complex interplay of different stakeholders like industry, politics, researchers, and end-users but also a simultaneous work on simulation, research and development, characterization, standardization, and regularization. After a brief introduction into these different facets of our institute, a deep dive will be given into the development of novel spectroscopic techniques (e.g. laser induced breakdown spectroscopy (LIBS), glow discharge optical emission spectroscopy, and Raman scattering), directly addressing the demands identified by the above stakeholders. Since by design, a future applicability is already included into this chemical characterization methodologies, all the presented techniques all share the same characteristics to be relatively inexpensive, fast, robust and do not need laborious sample preparation. T2 - Institute Seminar CY - Troy, NY, USA DA - 29.10.2024 KW - Federal research KW - Transformation KW - Analytical Chemistry KW - Instrumentation PY - 2024 AN - OPUS4-61971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Döring, Sarah T1 - Surface Immobilization of Thermostable Trypsin for Optimized Antibody Digestion N2 - Therapeutic monoclonal antibodies are the fastest-growing class of biological agents generating yearly sales of approx. USD 220 billion in 2023 which is expected to triple over the next decade. With the growing market significance of therapeutic antibodies, analytical methods allowing reproducible and metrologically traceable quantification need to be developed. In recent years, antibody quantification at the peptide level using liquid chromatography coupled with tandem mass spectrometry (LC-MS) has emerged as the leading technology. The serin protease trypsin has become the gold standard enzyme for digesting intact protein into peptides for this approach. However, many protocols exist that often lead to different results depending on the digestion procedure. In particular, the type and amount of detergents added during sample preparation for protein unfolding before digestion is known to create undesirable structure modifications of proteins (e.g. carbamylation) and significant bias in measurement results by inhibiting enzyme activity. The enzymes themselves can also have an influence, whereby immobilized variants are increasingly being used to improve their stability, minimize self-digestion and enable a higher substrate-enzyme ratio. Here, we studied the implementation of a thermostable and surface-functionalized trypsin-variant for improved antibody digestion. T2 - 23rd Human Proteome Organization World Congress CY - Dresden, Germany DA - 20.10.2024 KW - Antibody Quantification KW - Corundum KW - Enzyme Immobilization KW - LC-MS/MS PY - 2024 AN - OPUS4-61679 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Asadujjaman, Asad T1 - Endowing nanoparticles with orthogonal functionalities via a core/shell/shell architecture N2 - Dual orthogonal functionalities in a single material is highly desirable in many fields such as bio-imaging, sensing, coating or diagnostic and therapy. However, a precise and controlled approach to prepare two different functionalities is still a challenging task. Herein, we show the simple preparation method for the synthesis of dual-functional hybrid core/shell/shell nanoparticles consisting of a silica core with a fluorescent and a thermoresponsive polymeric layer. Silica core particles were first coated by a fluorescent layer using surface- nitiated reversible addition-fragmentation chain transfer (RAFT) polymerization. The fluorescent silica nanoparticles were then completely enclosed within a switchable protective coating made of thermoresponsive poly(N-isopropylacrylamide) via RAFT polymerization. Thermoresponsive poly(N-isopropylacrylamide) is known to change its properties according to the surroundings temperature in a reversible and controllable way (LCST behavior). The successful preparation of well-defined dual-functional hybrid core/shell/shell nanoparticles was shown by scanning electron microscopy, thermogravimetric analysis and Fourier transform infrared spectroscopy, while their fluorescence and thermoresponsive properties were confirmed by fluorescence spectroscopy and dynamic light scattering measurements, respectively. T2 - Macromolecular Colloquium 2016 CY - Freiburg, Germany DA - 24.02.2016 KW - Polymer KW - thermoresponsive PY - 2016 AN - OPUS4-35473 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bolz, Axel T1 - SERS microfluidic paper-based analytical devices N2 - The fast identification and quantification of analytes in the field of food safety or environmental analysis is difficult. Surface enhanced Raman scattering (SERS) is an analytical method which can be used simultaneously for the rapid identification and concentration determination of trace analytes,[1,2] usually covering a large dynamic range from nanomolar up to molar concentrations. The identification of the molecules is accomplished through the specific fingerprint of a molecule’s Raman spectrum. For facile and straightforward SERS measurements, we present here a combination of paper-based SERS test strips with microfluidic systems on paper as a microfluidic paper-based analytical device (μPAD). The SERS μPAD is thus principally suited for cheap, fast, non-destructive, label-free and portable detection of analytes. In this system basically, the use of the microfluidic structured paper increases the sensitivity and suppresses background signals of the SERS assay. Deposition of the SERS substrate on the test strips is simple and relies on an inkjet printer. For the optimization of the reproducibility and intensity of the SERS signal, we tested different nanoparticles, different numbers of print cycles and different paper types. The nanoparticle solutions used in the μPAD preparation were gold and silver nanoparticle solutions. The paper types were cellulose and glass fiber. SERS arrays were prepared by printing and compared to arrays prepared by spraying. The optimized μPAD was used for the identification and quantification of pure analyte solutions (e.g., adenine) and mixtures of compounds, the concentration series following Langmuir isotherms. Relevant analytes in the field of food safety are antibiotics and pesticides. We apply the SERS microfluidic paper-based analytical devices for the detection of antibiotics (enoxacin, enrofloxacin) and pesticides. T2 - Europtrode XIII CY - Graz, Austria DA - 20.03.2016 KW - SERS KW - Paper PY - 2016 AN - OPUS4-35702 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Keller, Julia T1 - Electrochemistry coupled with mass spectrometry - a versatile tool to investigate metabolic processes of mycotoxins N2 - To understand the metabolic fate of food relevant mycotoxins in vitro systems were mainly used as the method of choice, so far. Yet, in recent years coupling of electrochemistry mass spectrometry (EC-MS) gained increasing importance as promising technique for fast simulation of metabolic processes and was successfully applied in particular for drug metabolism [1]. The aim of our work was to investigate the potential of EC-MS to predict phase I metabolites of priority mycotoxins and to compare the results with in vitro experiments. Hence, the EU-regulated Fusarium mycotoxins zearalenone (ZEN) and patulin as well as dihydroergocristine (DHEC) as model compound of ergot alkaloids were electrochemically oxidized and analyzed by EC MS for the first time. Electrochemical conditions were set-up individually for each of the three mycotoxins. By using a coulometric flow through cell with a diamond working electrode oxidation of the chosen mycotoxins was observed after applying potentials between 1.7 and 2.0 V vs. Pd/H2. The electrochemically generated reaction products were analyzed online by mass-spectrometric detection. All of the three chosen mycotoxins were electrochemically converted to mono- and/or dihydroxylated products confirming the results of ZEN related metabolism studies [2, 3] and in case of DHEC own results from in vitro assays. Due to a lack of metabolism studies concerning the oxidative fate of patulin, interpretation of EC-MS data and performing microsomal studies is of particular relevance. Beside the identified products from electrochemical oxidation of ZEN, patulin and DHEC there is still a number of yet unknown compounds. Additional structural characterization of detected compounds by NMR and X-ray analysis will be facilitated by their large-scale production using preparative EC cells. T2 - Mycotoxin Workshop CY - Berlin, Germany DA - 02.05.2016 KW - Mycotoxins KW - Electrochemistry KW - Biotransformation KW - Mass spectrometry PY - 2016 AN - OPUS4-35981 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Climent Terol, Estela T1 - Rapid, sensitive and selective fluorescence sensing device for the determination of the nerve agents Sarin, Soman and Tabun in the gas phase N2 - The organophosphate nerve agents Tabun (GA), Sarin (GB) and Soman (GD) are among the most toxic chemical warfare agents (CWA) known, and exert their biological effects by irreversibly inhibiting acetylcholinesterase enzymes of the human nerve system. The use of these agents in the past century has killed millions of civilians around the world during World Wars I and II, and after that, approximately 40.000 tons of chemical ammunition were dumped into the Baltic Sea, containing ca. 13.000 tons of chemical warfare agents. Since their production, almost all the nations of the world have been strictly avoiding the development and use of CWA, participating in active destruction of CWA stockpiles, especially since the Chemical Weapon Convention (CWC) of 1993. However, CWA have been used in offensive ways against civilian population by terrorists, as for instance in the fatal Tokyo subway terror incident of 1995 or, most recently, against antigovernment demonstrators in Syria in 2013. Due to their higher toxicity and continuous use, it is therefore very important to develop simple and fast detection methods relying on new nerve agent sensing modalities for use in control and inspection. A practically useful fluorescent probe must possess a rapid response and high sensitivity, and shall be implementable into easy-to-use devices for real time detection by untrained personnel. Taking into account this fact, in this work we have synthesized several mesoporous silica materials containing boron–dipyrromethene (BODIPY) moieties for the detection of nerve agents GA, GB and GD in the gas phase. Development of our system indicated that the most potent materials are able to respond to the presence of nerve agent simulants diethyl cyanophosphonate, diethyl chlorophosphate and diisopropyl fluorophosphate, which have to be used in a laboratory setting, yet also for the real nerve agents Sarin, Soman and Tabun, producing a strong quenching of the fluorescence. Furthermore, a portable device for the detection of GA, GB and GD in the gas phase has been prepared for in situ sensing and rapid screening applications, consisting of strips that are able to indicate the targets down to below 1 mgm-3 which is below the LD50 values. T2 - XIII Europtrode Conference CY - Graz, Austria DA - 20.03.2016 KW - nerve agent KW - mesoporous material KW - sensor PY - 2016 AN - OPUS4-35921 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hachenberger, Yves Uwe T1 - Reproduzierbarkeit & Grundlagen der papierbasierten Atmosphärendruck Massenspektrometrie N2 - Die papierbasierte Massenspektrometrie (PB MS) ist ein vielversprechendes Ionisationsverfahren unter atmosphärischen Bedingungen, welches seit 2010 rege Forschungsinteressen erfährt. Die großen Vorteile der PB MS sind die Einfachheit der Umsetzung des Prinzips der Methode, auch bei komplexen Matrizes, und die geringen Kosten des verwendeten Materials. Diese Arbeit enthält systematische Untersuchungen zu verschiedenen Einflussfaktoren der PB MS. Im Vordergrund standen dabei Erkenntnisse zur Reproduzierbarkeit und Standardisierung der Methode. Durch den Vergleich der Zeitverläufe des Ionenstroms und aus den daraus resultierenden Spektren, selbst unter gleichen Bedingungen, zeigte sich, dass die Reproduzierbarkeit einzelner Messverläufe und der daraus erhaltenen Ergebnissen verbessert werden muss. Dies betrifft sowohl Messungen unter gleichen Rahmenbedingungen, als auch solche mit unterschiedlichen experimentellen Aufbauten. Die Reproduzierbarkeit ist somit die aktuelle Herausforderung der PB MS Forschung, die einer universelleren Verwendung als Ionisierungsmethode der Wahl im Wege steht. Die Beschaffenheit, zufällige Anordnung und Ausrichtung der Papierfasern, genauer die Morphologie des Materials selbst spielt dabei eine erhebliche Rolle. Darüber hinaus stützen die in dieser Arbeit erhaltenen Daten die Vermutung, dass der zu Grunde liegende Mechanismus der PB MS auf den Antenneneffekten jener Faserenden beruht. Die zufällige Verteilung der Faserenden ist ein Unsicherheitsfaktor, der durch die Verwendung strukturmodifizierter Papiere ausgeglichen werden soll. Die Unterschiede zwischen den Papieren ergeben sich neben der verschiedenen chemische Modifikation auch aus den morphologischen Details des jeweiligen Papiers. Diese umfassen neben den oben genannten Einflussgrößen auch die Starrheit des Papieres selbst. Es ist durch die Vielzahl der voneinander unabhängigen Einflussgrößen schwierig, allgemeingültige und optimale Konditionen für die PB MS zu entwickeln. Jedoch konnten Einblicke in den Spray- und Ionisationsvorgang gewonnen werden. Als Konsequenz dieser Erkenntnisse konnten verschiedene Möglichkeiten der Signalverstärkung und Verbesserung der Reproduzierbarkeit getestet werden, die vielversprechende Ergebnisse lieferten, jedoch weiterer Optimierung bedürfen. T2 - 49. Jahrestagung der Deutschen Gesellschaft für Massenspektrometrie CY - Hamburg, Germany DA - 28.02.2016 KW - Ambient KW - ToF MS KW - Paper Spray Ionization KW - Atmosphärendruck KW - Flugzeitmassenspektrometrie KW - Papierbasiert KW - Chemisch modifziert KW - Chemical modified PY - 2016 AN - OPUS4-35767 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hachenberger, Yves Uwe T1 - Paper spray ionization mass spectrometry using chemical modified paper tips N2 - Since it´s first report in 2010, paper spray ionization mass spectrometry (PSI-MS), has rapidly become a promising ionization method for ambient MS. It combines the simplicity of direct analysis due to chromatographic retention of matrix elements and disposability due to the usage of low-cost materials. As a result the quantification of analytes out of complicated matrices, e.g. as of dried blood spots is possible when internal standards are used. However, on the downside the method exhibits a poor sensitivity and reproducibility. Especially the reproducibility suffers from batch to batch fluctuations in the exact morphology and composition of the used paper. Thus, so far the stability of consecutive measurements varies from tip to tip and batch to batch. This work shows the potentials of chemical modifications of cellulose chromatography paper and their possible use for PSI-MS. The systematic comparison of the obtained data exhibits a clear trend potentially paving the way of possibilities towards a future applicability as a standard routine in analytical chemistry. T2 - 5. Berliner Chemie Symposium CY - Berlin, Germany DA - 12.04.2016 KW - Ambient KW - ToF MS KW - Paper spray ionization KW - Chemical modification KW - Atmosphärendruck KW - Flugzeitmassenspektrometrie KW - Papierbasiert KW - Chemische Modifizierung PY - 2016 AN - OPUS4-35769 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lindner, Uwe T1 - Speciation of Gd contrast agents using HILIC-ICP-MS N2 - Hydrophilic interaction chromatography (HILIC)coupled with inductively coupled plasma mass spectrometry (ICP-MS) were optimised for the direct determination of gadolinium-based contrast agents in tap water. With the speciation method described, tap water samples from the area of Berlin were analysed and for the first time, three Gd species, Gd-BT-DO3A, Gd-DOTA and Gd-BOPTA, were found in tap water samples at concentrations of about 10–20 ng Gd per litre. These are the same Gd species which have been previously detected predominantly in surface waters of the Berlin area. T2 - Anwendertreffen Plasmaspektrometrie CY - Berlin, Germany DA - 22.02.2016 KW - Gadolinium-based contrast agents KW - Hydrophilic interaction chromatography (HILIC) KW - Speciation KW - Inductively coupled plasmamass spectrometry (ICP-MS) KW - Internal standard KW - Berlin tap water PY - 2016 AN - OPUS4-35875 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gawlitza, Kornelia A1 - Fischer, Tobias A1 - Rurack, Knut T1 - Chemical functionalization for quantitative spectroscopic labeling on macroscopically flat surfaces N2 - This chapter highlights the application of chemical derivatization (CD) to facilitate the quantification of surface functional groups being an important issue for a wide field of applications. The selective attachment of a chemical label to a surface functional group being afterwards exclusively detectable by a highly sensitive technique overcomes the problem of characterizing low amounts of functional groups on macroscopically flat surfaces. The most frequently employed methods include CD X-ray photoelectron spectroscopy, ultraviolet/visible absorption, and fluorescence spectroscopy, as well as time-of-flight secondary ion mass spectrometry. Herein, the basic conditions for the different techniques regarding the specific surface functional group which need to be quantified are discussed. Additionally, the substrate highly influences the compatibility of the corresponding method. Because not just the quantification but also the preparation of the desired application is important, a summary of different preparation methods for glass, polymer and gold substrates is presented. KW - Chemical derivatization KW - Fluorescence KW - Surface group quantification KW - Time-of-flight secondary ion mass spectrometry KW - UV/vis spectroscopy KW - X-ray photoelectron spectroscopy PY - 2018 SN - 978-0-12-409547-2 DO - https://doi.org/10.1016/B978-0-12-409547-2.13191-9 SP - 1 PB - Elsevier AN - OPUS4-43767 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Keller, Julia A1 - Haase, H. A1 - Koch, Matthias T1 - Hydroxylation and dimerization of zearalenone: comparison of chemical, enzymatic and electrochemical oxidation methods N2 - Investigations of the metabolic pathway of mycotoxins by microsomal techniques are often laborious, causing an increasing demand for easy and rapid simulation methods. Thus, the non-microsomal oxidation technique of electrochemistry coupled online to mass spectrometry (EC/MS) was applied to simulate phase I biotransformation of the Fusarium mycotoxin zearalenone (ZEA). The obtained transformation products were identified by high resolution mass spectrometry (FT-ICR) and HPLC-MS/MS. Transformation products (TPs) from EC/MS were compared to those of other oxidative methods such as Fenton-like and Ce(IV) reactions and metabolites derived from in vitro assays (human and rat liver microsomes). Electrochemical oxidization of ZEA was achieved by applying a potential between 0 and 2,500 mV vs. Pd/H2 using a flow-through cell with a boron-doped diamond working electrode. Several mono-hydroxylated TPs were generated by EC/MS and Fenton-like reaction, which could also be found in microsomal in vitro assays. EC and Ce(IV) led to the formation of structurally different ZEA dimers and dimeric quinones probably connected over covalent biaryl C-C and C-O-C bonds. Although the dimerization of phenolic compounds is often observed in natural processes, ZEA dimers have not yet been reported. This is the first report on the formation of stable ZEA dimers and their related quinones. The tested non-microsomal methods, in particular EC/MS, could be useful in order to predict the biotransformation products of mycotoxins, even in cases where one to one simulation is not always feasible. KW - Electrochemistry KW - Zearalenone KW - Dimer PY - 2017 DO - https://doi.org/10.3920/WMJ2017.2213 SN - 1875-0710 SN - 1875-0796 VL - 10 IS - 4 SP - 297 EP - 307 PB - Wageningen Academic Publishers AN - OPUS4-43393 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Carl, Peter T1 - Multiplex suspension array fluorescence immunoassay (SAFIA) for environmental screening of bioactive compounds in wastewater N2 - Due to the demand of monitoring the water quality regarding emerging pollutants, such as drug residues, selective, high-throughput and multi-target analytical methods must be established. On the one hand, the influence of sewage on natural surface waters must be routinely monitored. On the other hand, estimation of removal efficiencies of pollutants, such as drug residues, is in the focus of industrial and public wastewater treatment. Immunoassays, such as ELISA, offer the possibility to be highly sensitive and selective due to the high target affine and specific recognition of antibodies to target molecules. Batch-wise processing in microtiter plates allow the necessary high-throughput, but only a single analyte can be determined within one measurement. To overcome these disadvantages, we developed a four-plex micro-bead based flow cytometric assay, which is adaptable for the microtiter plate format. The modular and self-prepared bead support consists of polystyrene-core-silica-shell particles. While the polystyrene core is used for encoding, by introducing different amounts of fluorescent dyes, the silica-shell creates a solid-support for the immunoassay: The target analytes, three drugs, carbamazepine, diclofenac and caffeine and the f ecal marker isolithocholic acid are covalently coupled to amino-groups on the surface via NHS-chemistry. A competitive immunoassay is subsequently conducted in a simple mix-and-read procedure. Finally, we could use SAFIA to assess the influent of treated and untreated waste water on the Douro river estuary in Portugal. The results of the analysis are comparable to ELISA. However, measurements could be carried out in 25% the time of analysis. T2 - BAM - BfR-Seminar Scientific exchange between: BAM und Abteilung „Chemikalien und Produktsicherheit" (Abteilung 7) des BfR CY - Berlin, Germany DA - 15.02.2018 KW - Bead based assay KW - Fluorescence KW - Emerging pollutants KW - Environment KW - Flow cytometry PY - 2017 AN - OPUS4-44337 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Streeck, C. T1 - Characterization of bio-molecular nano-layers by means of reference-free X-ray Spectrometry N2 - Characterization of bio-molecular nano-layers by means of reference-free X-ray Spectrometry An increasing field of application, e.g. in biotechnology is the dedicated adjustment of surface properties by functionalization with organic molecules. For a detailed understanding and further development of such nano-layers, a quantitative determination of the surface density of molecular species is required. By means of reference-free X-Ray Fluorescence (XRF) spectrometry such surfaces can be analyzed quantitatively by detecting specific marker elements. Using calibrated instrumentation and a quantification approach based on atomic fundamental parameters a SI-traceable quantitative analysis without any calibration sample or reference material is possible. A chemical analysis of molecular bonds can be accomplished by X-Ray Absorption Spectroscopy in the Near-Edge region (NEXAFS). Especially in the soft X-ray range an access to relevant light elements like Carbon C, Nitrogen N and Oxygen is possible. Here, aminated surfaces with varying densities of amino groups prepared from binary mixtures of silanes were investigated. In a complementary analysis by X-Ray Photoelectron Spectroscopy (XPS) and Fluorescence measurements based on laser-excitation in the optical light spectrum the functional-group density of silane monolayers were determined. The nitrogen atom in the head-group of the silane-molecule could be used as specific marker for the reference-free quantitative XRF analysis and were used for traceable calibration of XPS and Fluorescence Spectroscopy. T2 - EMRS Spring Meeting 2017, ALTECH 2017, Symposium S, Analytical techniques for precise characterization of nano materials CY - Strasbourg, France DA - 22.05.2017 KW - XPS KW - XRF KW - Amino silane film KW - Traceability PY - 2017 AN - OPUS4-43374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Neumann, Patrick P. A1 - Bartholmai, Matthias T1 - Development of a gas standard generator N2 - Pollution through emission of toxic gases is an increasing problem for the environment. It affects similarly agricultural, industrial and urban areas. In future, environmental emissions in ambient air must be monitored at even lower concentrations as nowadays. One environmental relevant compound is ammonia and its conversion product ammonium that have strong negative impact on human health and ecosystems. Most ammonia measurements in ambient air are performed in the range below 1000 nmol·mol 1 and thus there is a need for reliable traceable ammonia gas standards and in addition in situ analytical procedures for monitoring (in ambient air to avoid that thresholds are exceeded). Therefore, the use of reference materials is necessary for development accompanying test or for calibration, e. g. of structure-integrated sensors and mobile multi-gas sensors. The developed gas standard generator produces gas mixtures that comply with the metrological traceability for ammonia gas standards in the desired environmentally relevant measurement range. The method is based on the permeation of ammonia through a membrane at constant temperature and pressure. The resulting ammonia penetrant gas flow is then mixed with a carrier gas flow to generate a gas standard flow of known concentration. The dynamic rage is enlarged by using a two dilution steps. Depending on the permeation rate, generable molar fractions are possible in the range nmol·mol-1 to a few µmol·mol-1. We present the design of an ammonia gas standard generator and first results of the characterisation of its individual components supporting the uncertainty assessment according to GUM for stable gas concentrations in this range. The relative uncertainty of the generated ammonia gas standard is smaller than 4 % (k = 2). T2 - Networked Environmental Monitoring – from sensor principles to novel services CY - BAM, Berlin, Germany DA - 06.02.2018 KW - Permeation KW - Gas standard generator PY - 2018 AN - OPUS4-44089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gawlitza, Kornelia T1 - Wieviel Schmutz ist rein? Über das Arbeiten im Reinraum N2 - Um verlässliche Methoden für die medizinische Diagnostik und Umweltanalytik zu entwickeln sowie Zellen zu kultivieren, ist staub- bzw. keimfreies Arbeiten in einem Reinraum erforderlich. Aber was ist ein Reinraum? Viele stellen sich hier sterile Räume, keine Fenster und Personen in weißen Anzügen und Schutzmaske vor. Hier können die Besucher einen Blick hinter die Kulissen werfen und erfahren, was die Eigenschaften und Bedingungen eines Reinraumes sind und welche Anforderungen an die dort Beschäftigten gestellt werden. KW - Reinraum PY - 2017 UR - http://www.aktuelle-wochenschau.de/main-navi/aktuelle-wochenschau-2017/kw49-wieviel-schmutz-ist-rein-ueber-das-arbeiten-im-reinraum.html SP - 1 EP - 2 AN - OPUS4-43355 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Climent Terol, Estela A1 - Rurack, Knut T1 - Combining electrochemiluminescence detection with aptamer-gated indicator releasing mesoporous nanoparticles enables ppt sensitivity for strip-based rapid tests N2 - The combination of electrogenerated chemiluminescence (ECL) and aptamer-gated indicator delivering (gAID) magnetic mesoporous silica nanoparticles embedded into glass fibre paper functionalised with poly(ethyleneglycol) and N-(3-triethoxysilylpropyl)diethanolamine allowed the development of a rapid test that detects penicillin directly in diluted milk down to 50 ± 9 ppt in <5 min. Covalent attachment of the aptamer ‘cap’ to the silica scaffold enabled pore closure through non-covalent electrostatic interactions with surface amino groups, while binding of penicillin led to a folding-up of the aptamer thus releasing the ECL reporter Ru(bpy)32+ previously loaded into the material and letting it be detected after lateral flow by a smartphone camera upon electrochemical excitation with a screen printed electrode inserted into a 3D-printed holder. The approach is simple, generic and presents advantages with respect to sensitivity, measurement uncertainty and robustness compared with conventional fluorescence or electrochemical detection, especially for point-of-need analyses of challenging matrices and analytes at ultra-trace levels. KW - Electrochemiluminiscence KW - Hybrid materials KW - Signal amplification KW - Test strip analysis KW - Penicillin PY - 2021 DO - https://doi.org/10.1002/anie.202110744 SN - 1433-7851 SN - 1521-3773 SP - 1 EP - 11 PB - Wiley-VCH CY - Weinheim AN - OPUS4-53447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Climent Terol, Estela T1 - Fluorescence-based multiplexed detection on single test strips with antibody-gated mesoporous materials N2 - Rapid testing methods for the use directly at a point-of-need are expected to unfold their true potential especially when offering adequate capabilities for the simultaneous measurement of multiple analytes of interest. However, the implementation of multiplexing features while retaining simplicity, performance and portability is one of the prominent challenges in the field. Keeping in mind these challenges, we decided to combine the use of stimuli-responsive materials for small-molecule sensing relying on chemical signal amplification and their incorporation on paper strips for lateral-flow assays in a straightforward manner. Considering the modularity, high sensitivity and selectivity of antibody-gated indicator delivery systems, a multiplexed assay for three small-molecule explosives TATP, TNT and PETN was developed, allowing to detect the analytes simultaneously with a single test strip at lower ppb concentrations in liquid phase in <5 min, using a fluorescence reader or a smartphone for readout. Because of the versatility of the hybrid material and the modularity of the assay architecture, it is obvious that this generic approach should be easily transferable to food or environmental analysis, point-of-care diagnostics and other areas of application in which the rapid screening for multiple parameters from liquid samples without clean-up in a dedicated laboratory is in demand. T2 - 2021 On-line Symposium on Bioluminiscence, Chemiluminiscence and luminescence spectrometry ISLS-ISBC CY - Online meeting DA - 24.06.2021 KW - Multiplexing KW - Hybrid materials KW - Signal amplification KW - Test Strip analysis KW - Explosives PY - 2021 AN - OPUS4-52889 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Langenhan, Jennifer T1 - PEGomics: A meta-study on factors affecting polyethylene glycol (PEG) levels in human blood N2 - Polyethylene glycols (PEGs) are widely used in everyday items such as food additives and in personal care products. In addition, they have multiple medical applications: as laxatives, excipients, and covalently coupled to drug molecules leading to improved pharmacokinetics (PEGylation). While generally regarded as biologically inert, the human body is known to produce antibodies against PEGylated molecules. In addition, PEGs have been shown to be part of a biomarker signature to predict colon cancer outcome, suggesting a more complex and yet unknown behavior of PEGs in the human body. Here, we introduce PEGomics, a retrospective screening approach of publicly available LC-MS data. Using a custom R script to process entire studies, the presence of PEGs was reveled in most human plasma, serum and whole blood samples investigated. Several PEG species and adducts were identified and their correlation with different diseases and health conditions was investigated further. Blood PEG levels significantly differed between patient groups in multiple clinical studies related to e.g. pregnancy duration, fasting and smoking. We discuss possible causes for these effects in the light of recent reports of allergies against PEGs and outline our further strategies to identify the source of PEGs in the human body as well as possible metabolic transformations. T2 - ACS Spring 2021 CY - Online meeting DA - 05.04.2021 KW - PEG KW - Polyethylene glycole KW - PEGomics KW - Retrospective analysis KW - Meta-study PY - 2021 AN - OPUS4-53392 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gawlitza, Kornelia T1 - Long-Term Monitoring of Gaseous Ammonia with a Semi-automated Measuring Device N2 - In the present paper the development of a semi-automated device for long-term monitoring of gaseous ammonia is described. A sensor material was produced that changes its optical properties in the pres-ence of low concentrations of ammonia in air. The implementation into an electronic device enables precise, simple, economic and fast monitoring of low concentrations of harmful gases, like ammonia, and hence can help to improve the climate monitoring in livestock housing, barns or stables. T2 - SMSI 2021 CY - Online meeting DA - 03.05.2021 KW - Spectroscopy KW - Embedded sensor KW - Environment KW - Air quality PY - 2021 AN - OPUS4-52575 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Langenhan, Jennifer T1 - PEGs in the human body: where they are coming from and what they are doing N2 - The general understanding has been that PEGs are biologically inert, meaning they pass the human body without any relevant reaction with anything. But recent studies have shown that migth not be correct. Here a retrospective analysis of LC-MS data was performed to determine correlations between blood PEG levels in humans and different experimental factors. T2 - Make and Measure 2021 CY - Online meeting DA - 16.09.2021 KW - PEG KW - Polyethylene glycole KW - Retrospective analysis PY - 2021 AN - OPUS4-53391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hoffmann, A. T1 - Priority effects influence the production of mycotoxins of Fusarium and Alternaria N2 - Mycotoxigenic fungal pathogens Fusarium and Alternaria are a leading cause of loss in cereal production. On wheat-ears, they are confronted by bacterial antagonists such as pseudomonads. Studies on these groups’ interactions often neglect the infection process’s temporal aspects and the associated priority effects. In the present study, the focus was on how the first colonizer affects the subsequent ones. In a climate chamber experiment, wheat-ears were successively inoculated with two different strains (Alternaria tenuissima At625, Fusarium graminearum Fg23, or Pseudomonas simiae Ps9). Over three weeks, microbial abundances and mycotoxin concentrations were analyzed and visualized via Self Organizing Maps with Sammon Mapping (SOM-SM). All three strains revealed different characteristics and strategies to deal with co-inoculation: Fg23, as the first colonizer, suppressed the establishment of At625 and Ps9. Nevertheless, primary inoculation of At625 reduced all of the Fusarium toxins and stopped Ps9 from establishing. Ps9 showed priority effects in delaying and blocking the production of the fungal mycotoxins. The SOM-SM analysis visualized the competitive strengths: Fg23 ranked first, At625 second, Ps9 third. Our findings of species-specific priority effects in a natural environment and the role of the mycotoxins involved are relevant for developing biocontrol strategies. T2 - 42. Mycotoxin Workshop CY - Online meeting DA - 30.05.2021 KW - Microbe interactions KW - Antagonists KW - Mycotoxins PY - 2021 AN - OPUS4-52815 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Epping, Ruben T1 - Development of an analytical device to search for truffles N2 - The goal of this project is to develop a mobile technical solution for tracking down truffles, with which they can be harvested easier, faster, cheaper and more efficiently than with the current method of using trained dogs. The R&D cooperation project between BAM and sglux GmbH contains the characterization of the truffle aroma and identification of marker substances therein, the development of a fast, sensitive separation and quantification method based on ozone chemiluminescence as well as the construction of a prototype device. T2 - Tag der Chemie CY - Online Meeting DA - 06.07.2021 KW - Truffles KW - Volatile organic compounds KW - Chemiluminescence KW - Mobile device KW - Trace analysis PY - 2021 AN - OPUS4-52725 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Werneburg, Martina T1 - In situ analysis of trichodiene as a volatile biomarker for the fast and non-invasive gas-phase analysis of cereal mycotoxins N2 - Typically, mycotoxigenic moulds and consequently small percentages of extremely contaminated portions (“hot spots”) are randomly distributed in a cereal lot. Therefore, an efficient sampling procedure for mycotoxin analysis represents a complex challenge for operators involving invasive and cost intensive steps. Establishing an in situ analysis of mycotoxins from the homogeneous gas-phase above cereal crops instead of analysing random samples could address this difficult issue. During studies for microbial volatile organic compounds (MVOCs) indicating an infection with Fusarium, trichodiene was identified as a unique biosynthesis intermediate of trichothecenes - one of the largest groups of the mycotoxin family. The sesquiterpene trichodiene is the only volatile biogenic precursor of the trichothecenes, thus, early and fast in situ detection of this biomarker might be of interest for a potential trichothecene infestation. However, there is no commercial trichodiene standard available needed for the quantification of trichodiene in cereal grains. The aim of the current project is to develop a fast, easy-to-handle and non-invasive gas-phase quantification of trichodiene in the field. Therefore, trichodiene was prepared by total synthesis based on a tandem orthoester Claisen rearrangement - oxidation - Robinson annulation strategy providing the racemic natural product in 9 steps and 8 % overall yield. Its structure was fully elucidated by NMR and MS. With the reference standard in hand, a protocol was established for the quantitative headspace analysis of trichodiene above crop spikes by GC/MS in the < 10 µg/kg range. Besides a sample survey and a trichodiene - trichothecene correlation study, it is aimed to transfer the validated analytical method from the laboratory into a field-portable analytical system. The fast and reliable in situ detection of trichodiene as a volatile biomarker for trichothecene mycotoxins will contribute to a reduction of food production/analysis costs and to an improvement of food safety. T2 - 38th Mycotoxin Workshop CY - Berlin, Germany DA - 02.05.2016 KW - Fungal Volatiles KW - Fusarium Mycotoxins KW - Trichodiene KW - Headspace Analysis KW - Synthesis PY - 2016 AN - OPUS4-36193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mekonnen, Tessema Fenta T1 - Simulation of metabolic transformation products of pesticides by EC-LC-MS N2 - Among major food contaminants agrochemicals (including insecticides, fungicides and herbicides) are a threat for food safety in many countries. Once they entered the food chain or the environment, the parent compound can be transformed into different products by manmade and natural processes. The transformation products (TPs) might be more toxic and stable than the parent compound. In addition to this the transformation products might undergo conjugation with different compounds and/or changed to phase II metabolites. Conventional in-vivo or in-vitro methods to study phase I and II metabolism have drawbacks of long-time sample preparation and matrix complexity. Online coupling of an electrochemical cell with liquid chromatography-mass spectrometry (EC–LC–MS) is a promising technique to study metabolites, fate and transformation products of pesticides. The new approach enables to identify metabolic transformation products by oxidizing analyte of interest on the EC, separate the metabolites on HPLC and identifying them by MS. The aim of the present study is to identify/mimic pesticides phase I metabolites using electrochemical cell coupled to liquid chromatography-mass spectrometry (EC-LC-MS). Metabolic transformed products of two model compounds, fluopyram (fungicide) and chlorpyrifos (insecticide) were studied by EC upfront with MS. The results of EC-LC-MS are compared and discussed with those derived from in-vitro assays and the metabolites identified by LC-MS/MS. T2 - ISEAC39- International Conference Series on Environmental & Food Monitoring CY - Hamburg, Germany DA - 19.07.2016 KW - Metabolic transformation KW - Pesticides KW - EC-MS PY - 2016 AN - OPUS4-36953 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schloß, Svenja T1 - Neue Trends & Alte Probleme: Das Leguminosenmykotoxin Phomopsin A in einer "worst case"-Betrachtung N2 - Leguminosen wie z.B. Bohnen, Erbsen, Soja und zunehmend auch die Samen der Süßlupine liefern aufgrund ihres hohen Proteingehaltes einen wertvollen Beitrag zu einer veganen oder vegetarischen Ernährung. Jedoch sind Lupinen anfällig für Infektionen mit dem Pilz Diaporthe toxica, der u.a. Phomopsin A als hepatotoxischen Sekundärmetaboliten bildet. Ziel der Arbeiten waren die Gewinnung und Anwendung eines 15N-isotopenmarkierten internen Standards für die HPLC-MS/MS-Analyse dieses Toxins sowie die Quantifizierung der Toxinbildung in einem „worst case“-Szenario. T2 - 50. DGQ-Vortragstagung (Deutsche Gesellschaft für Qualitätsforschung e. V.) CY - Berlin, Germany DA - 14.03.2026 KW - Phomopsin A KW - Leguminosen KW - SIDA-HPLC-MS/MS KW - Quantifizierung KW - Toxinbelastung PY - 2016 AN - OPUS4-37059 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schloß, Svenja T1 - Sensitive und selektive Untersuchung des Leguminosenmykotoxins Phomopsin A - eine "worst case"-Betrachtung N2 - Leguminosen wie z.B. Bohnen, Erbsen, Soja und zunehmend auch die Samen der Süßlupine liefern aufgrund ihres hohen Proteingehaltes einen wertvollen Beitrag zu einer veganen oder vegetarischen Ernährung. Jedoch sind Lupinen anfällig für Infektionen mit dem Pilz Diaporthe toxica, der u.a. Phomopsin A als hepatotoxischen Sekundärmetaboliten bildet. Ziel der Arbeiten waren die Gewinnung und Anwendung eines 15N-isotopenmarkierten internen Standards für die HPLC-MS/MS-Analyse dieses Toxins sowie die Quantifizierung der Toxinbildung in einem „worst case“-Szenario. T2 - 53. Wissenschaftlicher Kongress der Deutschen Gesellschaft für Ernährung e.V. CY - Fulda, Germany DA - 02.03.2016 KW - Phomopsin A KW - Leguminosen KW - Stabilisotopenverdünnungsanalyse KW - HPLC-MS/MS KW - Toxinbelastung PY - 2016 AN - OPUS4-37060 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maul, R. T1 - Phomopsins in legumes - a multidimensional approach N2 - Fungal secondary metabolites such as phomopsin A (PHO-A) produced by the fungus Diaporthe toxica are referred to as “emerging” mycotoxins. Recently, we developed a biosynthetic approach to gain access to 15N-isotopically labelled PHO-A as internal standard (IS) for PHO-A matrix independent quantification of PHO-A in various commodities. Aim of the present work was to elucidate the applicability of the new IS for accurate quantification and to investigate the phomopsin formation on various legume seeds as well as plant material. In summary, the applicability of the SIDA-HPLC-MS/MS method could be proven and the potential of D. toxica to produce high amounts of phomopsins under unfavorable conditions on lupins and other legume seeds could be shown. Moreover, a novel toxic methylated PHO-A derivative was unveiled in natural samples infested with D. toxica. T2 - 38. Mycotoxin-Workshop CY - Berlin, Germany DA - 02.05.2016 KW - Phomopsin-Derivate KW - Leguminosen KW - Stabilisotopenverdünnungsanalyse KW - HPLC-MS/MS KW - HRMS-Identifizierung KW - Toxizität PY - 2016 AN - OPUS4-37056 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bolz, Axel T1 - Paper-based SERS test strips N2 - For the non-destructive chemical analysis of organic compounds, several different methods such as NMR, UV-vis absorption, IR, Raman, or fluorescence spectroscopy are available. However, all available methods have some restrictions such as the necessity of a large sample amount, interferences in the presence of water, or overlapping signals from the analytes or matrix. Surface enhanced Raman scattering (SERS) allows to observe analytes directly without labelling in low concentrations in aqueous solutions and to identify them by their spectral fingerprint. Therefore, in this work we use SERS as a detection method for different analytes in low concentrations in combination with paper-based test strips as SERS substrates and for sample preparation. We present a spray method for the preparation of SERS test stripes.[1] With this spray method, nanoparticle solution was deposited on cellulose and glass fibre paper as SERS substrate. The prepared paper-based test strips were tested with classical SERS reporter molecules, e.g. rhodamine 6G, 4-aminothiophenol, and adenine. For the quantification of analytes, highly reproducible signal intensities are necessary, which can be realized with the test strips in acceptable quality. Moreover, employing intensity vs concentration calibration for the analytes, data analysis revealed a behaviour that was best described by a Langmuir isotherm, stressing the strong distance dependence of the SERS effect. For an easier identification of analytes in a mixture of compounds, the paper-based test strips were functionalised with hydrophobic barriers by wax printing. With these microfluidic paper-based analytical devices (µPAD) the sample mixture can be separated by the chromatographic effects of the paper and the different analytes can be separately detected and identified by SERS. [1] A. Bolz, U. Panne, K. Rurack, M. Buurman, Glass fibre paper-based test strips for sensitive SERS sensing, Anal. Methods, 2016, 8, 1313-1318. T2 - International RamanFest 2016 CY - Berlin, Germany DA - 19.05.2016 KW - SERS KW - Raman KW - Paper PY - 2016 AN - OPUS4-36726 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Combining Fluorescent Probes, Functionalized Surfaces, Tailored Particles and Device Embedding for Robust, Reliable and User-friendly Analytical Assays N2 - Supramolecular chemistry, fluorescence detection, hybrid (nano)materials and device miniaturization are in themselves highly interesting areas of research, yet especially their combination paves the way to (bio)chemical analysis systems that show outstanding performance. The lecture gives an overview of the toolbox of single components developed in BAM’s Chemical and Optical Sensing Division over the years, and how their combination can result in powerful sensors, quick tests and assays. While at the core of a development is the analytical problem, that is, the determination of a certain analyte in a sample of interest with the required sensitivity and selectivity by a specific end user in a given setting, signaling mechanisms, recognition elements, signal transduction modes, materials functionalization, device design and system integration are adequately chosen, tailored and adapted. Examples including molecularly imprinted polymers, hybrid mesoporous nanomaterials, gated indicator release systems, microfluidic devices, test strips and smartphone-based analysis will be presented. T2 - GDCh CY - Chemnitz, Germany DA - 21.06.2018 KW - Fluorescence KW - Particles KW - Rapid tests KW - Device embedding PY - 2018 AN - OPUS4-45640 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rurack, Knut T1 - Molecularly Imprinted Polymers with Integrated Fluorescence as Versatile Biomimetic Sensing Matrices N2 - Molecularly imprinted polymers (MIPs) are an established, versatile and high-performance matrix for the selective separation or enrichment of (bio)chemical species, especially small molecules of biochemical or environmental relevance. MIPs are prepared through the polymerization of a mixture of functional monomers and cross-linkers in the presence of the template with subsequent extraction of the latter. Conceptionally, this process can be seen as mimicking in a strongly accelerated, though single-step manner a biological process such as antibody formation. Because the resulting MIPs contain cavities in their matrix that are complementary in size, shape and electronic/ electrostatic or hydrogen bonding demand to the imprinted target molecule or template, these polymers are frequently termed “artificial antibodies”. Compared to natural antibodies, they are chemically and physically much more robust. Regarding sensitivity and selectivity, however, there is still a gap to bridge before MIPs can fully compete with antibodies. Another favorable aspect that distinguishes MIPs from antibodies is that they can be endowed with an explicit function, allowing the use of MIPs in applications that require more than only an efficient binder. For instance, if specifically designed and polymerizable fluorescent indicators are integrated as functional monomers into a MIP, direct fluorescence sensing can be accomplished. Because MIPs can be prepared in a variety of different formats, their combination with miniaturized or other specific analytical techniques or sensory devices is possible, especially when the transduction mode is light. This presentation will introduce basic design considerations, challenges, limitations and the potential that lies with such sensor materials with some recent examples of our group, targeting various organic oxoanions as analytes. T2 - 8th International Symposium on Bioanalysis, Biomedical Engineering and Nanotechnology CY - Changsha, Hunan, China DA - 25.05.2018 KW - Molecularly imprinted polymers KW - Fluorescence KW - Anion recognition PY - 2018 AN - OPUS4-45641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Bartholmai, Matthias T1 - Two tasks in environmental monitoring - calibration and characterization of gas sensors and remote sensing with multicopter platforms - Part 2 N2 - Emissions of ammonia into the environment are mainly caused by agriculture, but also by combustion processes in waste and by road traffic. Even at low concentrations, this substance is not only an odour nuisance, but also a substance with ecological and climatic relevance. Therefore, BAM tested commercial electrochemical, and metal oxide based sensors, which have limited suitability for measuring in the environmental molar fraction range. Alternatively, own developments for the detection of ammonia in the trace range were implemented, wherein the analyte is measured by changing the fluorescence of a BODIPY dye at 550 nm by means of a portable fluorescence sensor directly from the gas phase. For the calibration of ammonia sensors and measuring instruments, a stationary system based on the mixture of certified test gases from pressure cylinders with calibrated mass flow controllers is available. A test gas generator was developed for on-site calibration and testing of sensors and measuring devices. The generation of ammonia-containing gases in the environmental relevant range of levels below 1000 nmol/mol is carried out by the permeation method according to ISO 6145-10. For the traceability of ammonia, standards are provided and further developed by the National Metrological Institutes and designated institutes. Metrological standards are based on SI units and are a basis for traceability of sensors or gas analysers. T2 - Aarhus University, Department of Environmental Science, External seminar with Matthias Bartholmai and Carlo Tiebe CY - Roskilde, Denmark DA - 29.08.2018 KW - Environmental monitoring KW - Test gas generation KW - Fluorescence sensor KW - Ammonia PY - 2018 AN - OPUS4-45842 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kislenko, Evgeniia T1 - Molecularly Imprinted Polymers for Fluorescence Sensing of the Herbecide 2,4-D N2 - Application of pesticides is ubiquitous to better manage agricultural production. However, most of these compounds are harmful or toxic for humans and highly persistent in the environment, even in the crops themselves. Therefore, the rapid and reliable monitoring of pesticide residues is a very important area of environmental analysis. If conducted directly in the field, the use of fluorescence sensing methods is particularly attractive, because they allow for sensitive and rapid analyses while being very versatile. Recently, molecularly imprinted polymers (MIPs) have emerged as promising candidates for the primary sensing phase. Their robustness, low price and tunability render them an attractive alternative to more conventional biosensors based on antibodies. At present, a number of MIP formats are available besides the initial bulk polymer monoliths. Core/shell micro- and nanoparticles are especially suitable for sensor applications. A thin shell provides many advantages compared to a bulk polymer, such as fast diffusion of analyte, homogeneity of binding cavities and a higher number of binding sites closer to the surface. A strategy for sensory MIP synthesis is to introduce the fluorophore covalently into the polymer layer. The fluorescent probe monomer may thus consist of a fluorophore unit, a polymerizable unit and a recognition unit. One of the issues in targeting acidic pesticides such as 2,4-D is the fact that usually their deprotonated form is used for imprinting in organic solvents, commonly as the tetraalkylammonium salt. This approach harbours drawbacks when it comes to analytical rebinding, because real samples seldom contain such counterions. In our group, we have thus developed a new fluorescent probe monomer containing the 2-aminopyridine moiety, which forms strong enough intermolecular hydrogen bonds with the carboxylic acid group of neat 2,4-D. During a titration of the probe monomer with the analyte, hydrogen bond formation is indicated by spectral shifts and fluorescence enhancement. Crystallography studies verified complex formation. The higher fluorometric response of the core-shell MIP compared to a non-imprinted control polymer proved successful imprinting. Here, we will discuss the pros and cons of neutral molecule vs. salt imprinting, potentially expanding the possibilities of fluorescent sensory MIPs. T2 - MIP2018 CY - Hebrew University, Jerusalem, Israel DA - 24.06.2018 KW - Molecularly imprinted polymers KW - 2,4-D KW - Fluorescence KW - Sensing PY - 2018 AN - OPUS4-45598 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotthoff, Lisa T1 - Untersuchung von Biotransformationsprozessen von Ionophoren Antbiotika mittels online-Kopplung Elektrochemie LC-MS N2 - Ionophore Antibiotika werden zum Schutz gegen Kokzidiose eingesetzt, hauptsächlich in der Geflügelmast. Rückstände dieser Substanzen und deren Transformationsprodukte (TP) gelangen über den Metabolismus zum einen in das Geflügelfleisch, aber auch durch Ausscheidung in die Umwelt, da Tiermist als Dünger verwendet wird. Ziel dieser Forschungsarbeit ist es, die TP-Bildung von vier verschiedenen Ionophoren Antibiotika (Monensin (MON), Salinomycin (SAL), Maduramicin (MAD) und Lasalocid (LAS)) zu untersuchen. TPs werden durch den Biotransformationsprozess (Metabolismus) gebildet, dieser Prozess kann in zwei Phasen eingeteilt werden. Während in Phase I Oxidations-, Reduktions- oder Hydrolysereaktionen auftreten, ist Phase II von Konjugationsreaktionen geprägt. Durch diesen Prozess werden die Substanzen besser ausscheidbar. Natürliche Redox-Vorgänge, wie sie bei der Biotransformation (Phase I) auftreten, können mit elektrochemischen (EC) Systemen simuliert werden. In einer EC-Durchflusszelle findet die Reaktion abhängig vom angelegten Potential statt. Im positiven Potentialbereich (0.0 bis 3.0 V; vs. Pd/H2) werden die Analyten oxidiert und somit oxidative TPs generiert. Durch die online-Kopplung mit Flüssigkeitschromatografie (LC) und Massenspektrometrie (MS) wird zunächst eine säulenchromatografische Trennung der generierten TPs erhalten, gefolgt von der massenspektrometischen Detektion. Durch die online-Kopplung von EC-(LC)-MS ergibt sich eine schnelle Analysemöglichkeit von der TP-Erzeugung ausgewählter Substanzen bis hin zur Detektion, wodurch gleichzeitig eine Identifizierung möglich ist. Die ausgewählten Ionophoren Antibiotika wurden mittels EC-(LC)-MS auf auftretende TPs untersucht. Die ersten Ergebnisse zeigen ein breites Spektrum unterschiedlicher TPs abhängig von gewählten EC-Parametern wie Lösemittel, Modifier und insbesondere vom Arbeitselektrodenmaterial der EC-Durchflusszelle. Unter den erhaltenen TPs sind sowohl bekannte als auch unbekannte TPs vertreten, so dass weitere Untersuchungen zur Strukturaufklärung und vergleichende Tests zu Phase I Metaboliten (z.B. durch Metabolismus-Studien mit Mikrosomen) geplant sind. T2 - 47. Deutscher Lebensmittelchemikertag CY - Berlin, Germany DA - 17.09.2018 KW - Transformationsprodukte KW - Elektrochemie KW - Ionophore Antibiotika PY - 2018 AN - OPUS4-46007 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bartelmeß, Jürgen T1 - Developments Towards a fluorometric sensing device for multiple hazardous gases N2 - Fluorometric sensing is a versatile approach for trace analysis outside of the laboratory, requiring suitable sensor materials and their integration into sensing devices. The versatility of fluorophores as probes, especially in terms of the possibility to tailor their optical as well as their recognition properties by synthetic modifications in a wide range, renders them as superior active component for the preparation of optical sensor devices. Recent works at BAM in this field include, for example, the detection of nerve gas agents,illustrating impressively the aforementioned benefits of fluorophores in optical sensing applications. In the interdisciplinary approach presented here, we target hazardous gases such as ammonia, benzene, and hydrogen sulfide, next to others, which pose a major threat to human health and environmental safety and for which the availability of a sensitive and reliable detection method is highly desirable. The dyes presented follow a “turn-on” fluorescence schematic, which allows for the selective and sensitive detection of the respective gaseous analyte. The immobilization of the probe in polymeric matrices is then the next step toward the fabrication of a prototype device for molecular sensing. Further steps in the project include the assembly of instruments for test-atmosphere generation, the referencing of the sensor system, development and implementation of an optical setup, and the testing of the prototype device under laboratory conditions and in the field. In this presentation, we give an overview over the recent developments on this topic in our groups, including fluorophore designs investigated for the detection of benzene, ammonia, and hydrogen sulfide as well as approaches for the design of the sensing device. T2 - EUROPT(R)ODE XIV CY - Neapel, Italy DA - 25.03.2018 KW - Gas sensor KW - Fluorometric sensing KW - BODIPY dye PY - 2018 AN - OPUS4-45645 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kotthoff, Lisa T1 - Investigation of ionophore antibiotics and their transformation products by using electrochemistry coupled to LC-MS N2 - Ionophore antibiotics are used to cure and prevent coccidiosis by chicken especially in broiler farming. The residues are found not only in food products (chicken and eggs) but also in the environment (manure, soil or water). In this work the ionophores monensin (MON), salinomycin (SAL), maduramicin (MAD) and lasalocid (LAS) are investigated aiming to study their transformation products (TPs) through biotransformation processes. Biotransformation can be divided into two phases, phase I: oxidation, reduction or hydrolysis and Phase II: conjugation reactions. It is necessary to further examine the biotransformation pathways to determine TPs to be able to detect residues more specifically in different matrices. The technique of electrochemistry (EC) offers the opportunity to simulate biotransformation processes and to generate TPs for further analysis. The combination of EC with liquid chromatography and mass spectrometry (EC-LC-MS) provide a fast and simple tool to separate and determine the EC-generated TPs. The electrochemical flow through cell is coupled to the (LC)-MS system, allowing the reaction mixture to be separated by a RP-18 column and then analyzed in the MS. The oxidation products are generated at different potentials between 0.0 – 2.5 V vs. Pd/H2 using glassy carbon or boron doped diamond as working electrode materials . The results show a broad spectrum of different TPs depending on used solvents and working electrode materials. Among the generated TPs already known as well as unknown TPs of the drugs can be found. Further investigations on structure elucidation of unkown TPs are planned. T2 - World Conference on Analytical and Bioanalytical Chemistry CY - Barcelona, Spain DA - 23.07.2018 KW - Transformation Product KW - Electrochemistry KW - Ionophore Antibiotics PY - 2018 AN - OPUS4-45600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mansurova, Maria T1 - Fluorescence-based optical system for the detection of total petroleum hydrocarbons in water and soil with smartphone read-out compatibility - Spectrocube, a sensor for rapid oil test in water and soil N2 - Contamination of natural bodies of water with oil and lubricants (or generally, hydrocarbon derivatives such as petrol, fuel and others) is a commonly found phenomenon around the world due to the extensive production, transfer and use of fossil fuels. The timely identification of these contaminants is of utmost importance, since they directly affect water quality and represent a risk for wildlife and human health even in trace amounts. In this work, we develop a simple system for the on-field detection of total petroleum hydrocarbons (TPH) in water and soil, the "Spectrocube". The test is based on the measurement of the fluorescence signal emitted by the molecular rotor 4-DNS-OH dye. This dye is embedded in a hydrophobic polymeric matrix (PVDF), avoiding interactions of water with the dye and providing a robust support for use in test-strip fashion. The test-strip’s fluorescence intensity increases linearly at low concentrations of TPH, reaching a saturation value at higher concentrations. For excitation and evaluation of the test-strip fluorescence, a simple miniature optical system was designed. The system works semi-quantitatively as solvent-free TPH detection kit, as well as quantitatively when using a simple cyclopentane extraction step. To simplify the fluorescence read-out, the device is coupled to a tablet computer via Bluetooth, running a self-programmed software ("app"). T2 - Oil Spill India 2018 CY - New Delhi, India DA - 05.07.2018 KW - Oil analysis KW - Water analysis KW - Fluorescence KW - Spectrocube KW - Rapid test KW - Field test KW - Spectroscopy KW - Sensor PY - 2018 AN - OPUS4-45606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mansurova, Maria T1 - Embedded Fluorescence-Based Optical System for the Detection of Total Petroleum Hydrocarbons in Water and Soil N2 - Contamination of natural bodies of water with oil and lubricants (or generally, hydrocarbon derivatives such as petrol, fuel and others) is a commonly found phenomenon around the world due to the extensive production, transfer and use of fossil fuels. In this work, we develop a simple system for the on-field detection of total petroleum hydrocarbons (TPH) in water and soil. The test is based on fluorescence emission of a 4-dimethylamino-4′-nitrostilbene derivative (4-DNS-OH). This fluorescent molecular rotor is embedded in a hydrophobic polymeric matrix (PVDF), avoiding interactions with water and providing a robust support for use in test-strip fashion. For the fluorescence detection a portable sensor device was developed, featuring two excitation LEDs, a micro-spectrometer and Bluetooth control. A limit of detection of at least 6 ppm of TPH in water was demonstrated. T2 - Europtrode 2018 CY - Naples, Italy DA - 25.03.2018 KW - Water KW - Fluorescence KW - Spectrocube KW - Rapid test KW - Oil PY - 2018 AN - OPUS4-45605 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogel, Christian T1 - Current status of monitoring of PFAS release from industrial facilities N2 - Increasing studies report per- and polyfluoroalkyl substances (PFAS) in the ambient air and emissions from diverse industrial sources. Therefore, a comprehensive framework for characterizing PFAS emissions by identifying source-specific chemical fingerprints, evaluating emission pathways and assessing the impact of remediation technologies is needed. Depending on the type of PFAS, dedicated sampling and analytical procedures are required. Here, also the detection of possible PFAS transformation products, so-called products of incomplete combustion (PICs) are more mobile or toxic, is also of great interest to evaluate these technologies in terms of mineralisation potential and fluorine mass balance. T2 - Consortium for analysis and remediation of per- and polyfluoroalkyl substances (CAR-PFAS Japan) visit Uni Örebro CY - Online meeting DA - 09.10.2025 KW - Per- and polyfluoroalkyl substances (PFAS) KW - Incineration KW - Remediation PY - 2025 AN - OPUS4-64318 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - PlasticTrace WP1 – Stakeholder Workshop N2 - The talk summarizes the achievments of WP1 of the PlasticTrace project. Microplastic reference materials were developed by producing tablets. Different preparation methods were compared. Characterisation of the tablets was done after filtration with µFTIR, QCL, µRaman, Py-GC/MS and TED-GC/MS after ISO standards ISO 16094-2 and ISO/FDIS 16094-3. Polymer types are polypropylene and polyethylene terephthalate. T2 - Stakeholder Workshop PlasticsTrace CY - Online meeting DA - 09.09.2025 KW - Microplastics KW - Reference materials KW - TED-GC/MS KW - PET PY - 2025 AN - OPUS4-64258 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bolling, Janina A1 - Koch, Claudia T1 - Digital LabHub: Inkubator für die Digitale Transformation der Laborbranche N2 - In den Praxiswerkstätten für Prüf- und Kalibrierlabore, einem Dialogprozess mit der Laborbranche, der von BAM, DAkkS und dem Verband unabhängiger Prüflabore gestaltet wurde, wurde der Bedarf der Labore nach einem Zentralen Informations- und Netzwerkangebot zum Thema digitale Transformation im Labor als zentral identifiziert. Der Vortrag präsentiert die daraufhin gestartete Initiative des Digital Labhub. Als Zusammenschluss zentraler Akteure zu Themen der digitalen Transformation im Labor, treiben die Akteur*innen gemeinsam die Gestaltung eines vernetzten, standardisierten und interoperablen digitalen Labor-Ökosystems voran. Der Vortrag gibt Einblick in die Initiative. T2 - VUP Jahrestagung CY - Berlin, Germany DA - 24.06.2025 KW - Qualitätsinfrastruktur KW - Prüflabor KW - Kalibrierlabor KW - QI-Digital KW - Digitalisierung KW - Digitale Transformation PY - 2025 AN - OPUS4-64277 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Blaschke, Jil T1 - Laser Induced Breakdown Spectroscopy (LIBS) for the chemical investigation of concrete - Status of practical application and regulations in Germany N2 - Laser-Induced Breakdown Spectroscopy (LIBS) is an advanced, yet still underutilized, analytical technique that has gained increasing recognition for its potential in evaluating cementitious materials. Over the past several years, LIBS has demonstrated exceptional capabilities in providing detailed insights into the microstructural and chemical properties of concrete, with particular relevance to durability studies and service life assessment. One of the defining features of LIBS is its high spatial resolution, which enables precise mapping of ion transport processes within the binder matrix. This ability is critical for understanding concrete behavior under diverse environmental and operational conditions, such as chloride ingress, sulfate attack, or carbonation. By allowing the simultaneous detection of multiple elements, LIBS is uniquely suited for investigating complex interactions, including the co-migration of ions. Such comprehensive analyses yield detailed ion ingress profiles, improving the accuracy of key input parameters used in service life models. As a result, LIBS contributes to more reliable predictions of a structure's remaining lifespan and its susceptibility to environmental degradation. In addition to ion profiling, LIBS is particularly effective in identifying local anomalies that would otherwise not be detected by conventional methods. For instance, LIBS can reveal zones of elevated ion concentration in microcracks or other vulnerable regions, offering critical insights into structural integrity. LIBS supports the assessment of repair processes not only during application but also over long-term monitoring periods, thus contributing to the optimization of rehabilitation strategies. This presentation showcases a series of practical applications of LIBS in the laboratory analysis of building materials, supported by extensive comparative studies. Case studies highlight LIBS's transformative role in repair planning and decision-making, emphasizing its capacity to revolutionize infrastructure monitoring and maintenance. T2 - NDT-CE 2025 CY - Izmir, Türkiye DA - 24.09.2025 KW - LIBS KW - Concrete analysis KW - Ion transport profiling KW - Structural durability assessment PY - 2025 AN - OPUS4-64294 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dalichow, Dirk A1 - Blaschke, Jil A1 - Wilsch, Gerd A1 - Völker, Tobias T1 - Revolutionizing Concrete Analysis and Maintenance with Laser-Induced Breakdown Spectroscopy N2 - Laser-induced breakdown spectroscopy (LIBS) is a valuable complement to established methods for the chemical analysis of concrete. Compared to conventional techniques, LIBS enables spatially resolved imaging of harmful ion distributions within the cementitious matrix. It allows the simultaneous detection of all relevant ions and degradation mechanisms, facilitating a better understanding of interacting processes. The benefits of multi-element analysis are illustrated through selected examples that highlight the method’s superior information content. Ion penetration profiles are recorded at a resolution of 0.25 mm, providing high-quality input data for service life modelling. Instead of drill dust, a 50 mm core sample is used. The measurement is automated, requires no chemical reagents or elaborate sample preparation, and is completed within minutes. KW - LIBS KW - Durability KW - Ion transport profiling KW - Concrete analysis KW - Service life assessment PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642846 DO - https://doi.org/10.58286/31656 SN - 1435-4934 VL - 30 IS - 10 SP - 1 EP - 8 PB - NDT.net GmbH & Co. KG AN - OPUS4-64284 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heide, Maximilian A1 - Reifenrath, Jonas A1 - Herrmann, Alexander A1 - Engelhard, Carsten T1 - Fast and Sustainable Active Pharmaceutical Ingredient (API) Screening in Over-the-Counter and Prescription Drug Products by Surface-Assisted Plasma-Based Desorption/Ionization High-Resolution Mass Spectrometry N2 - Fast chemical analysis of pharmaceutical preparations is important for quality assurance, counterfeit drug detection, and consumer health. While quantitative methods such as high-performance liquid chromatography mass spectrometry (HPLC-MS) are powerful, there is a need for sustainable and environmentally friendly methods, which require less chemicals and produce less waste. Here, solvent-free ambient desorption/ionization (ADI) MS methods are attractive because they do not require time-consuming chromatography, produce little to no chemical waste, and, thus, contribute to green chemistry practice. In addition, sample throughput can be higher compared to HPLC-MS. In this study, a method for direct analysis of single- and multi agent drugs using a plasma-based ADI source (flowing atmospheric-pressure afterglow, FAPA) coupled to high-resolution (HR) MS was developed and optimized for best performance. The approach is rapid and only requires analytes to be in solution (only a few µL) before application onto thin-layer chromatography (TLC) surfaces, specifically dimethyl (RP2-) and cyano (CN-) modified silica, for surface-assisted (SA) FAPA-HRMS measurements. No chromatographic separation was required, and the TLC plates served only as sample carriers. A broad variety of 19 active pharmaceutical ingredients (APIs) was carefully selected to cover analgesics, anesthetics, antibiotics, antiepileptics, calcium channel blockers, diuretics, expectorants, opioids, peripheral vasodilators, stimulants, and sympathomimetics. Fast screening and identification of APIs was performed by SA-FAPA-HRMS. Typically, the protonated molecular ion ([M+H]+) was the most abundant species, while some compounds (codeine, metamizole, phenoxymethylpenicillin, and torasemide) did show some degree of fragmentation. As a proof-of-principle application, benzocaine was directly detected in saliva samples post-intake of a lozenge. Time-resolved semi-quantitative screening was performed. The limit of detection for benzocaine in saliva was 8 ng/mL (48.4 fmol) using internal standard calibration and CN-HPTLC plates. In addition, direct quantification of artificially spiked saliva was performed with minimal sample preparation. Here, SA-FAPA-HRMS with a CN-HPTLC sample substrate yielded best performance (20.02±0.52 µg/mL, RSD=2.6%, deviation of -1.9% from the theoretical value) compared to RP2-TLC (18.97±1.37 µg/mL, RSD=7.2%, -7.0%), and HPLC-UV (18.51±0.03 µg/mL, RSD=0.2%, -9.3%) results. In conclusion, SA FAPA HRMS is considered attractive for rapid and sustainable analysis of pharmaceuticals with potential in non-invasive patient monitoring. KW - Mass Spectrometry KW - Pharmaceuticals KW - Green Chemistry KW - Ambient Desorption/Ionization PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640718 DO - https://doi.org/10.1039/D5AY01050K SN - 1759-9660 VL - 17 IS - 18 SP - 7799 EP - 7809 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oskoei, Parastu T1 - Thermoresponsive UCNP@MSN Nanoparticles for Doxorubicin Delivery in Melanoma Cells N2 - Upconversion nanoparticles (UCNPs) possess unique photophysical characteristics, such as excita bility by near infrared (NIR) light, which facilitates deep tissue penetration, multi color emission , long luminescence lifetimes, and an excellent photostability. These features have made UCNPs promising tools for biomedical applications . M esoporous silica nanoparticles (MSNs) functionalized with stimuli responsive nanovalves or specific coatings enable the encapsulation and controlled release of therapeutic agen ts, thereby offering spatiotemporal precision in drug delivery 1 3 ]]. Among drug delivery strategies, photoresponsive systems have attracted growing attention due to their potential for clinical applications . This is especially relevant for melanoma, an aggressive skin cancer with increasing global incidence, for which conventional therapeutic modalities remain largely insufficient in advanced stage 4 In this work, core shell UCNP@MSN nanoparticles were synthetised by coating UCNPs with a mesoporous silica layer, which was subsequently functionalized with thermoresponsive retro Diels Alder nanovalves [ and loaded with the chemotherapeutic agent doxorubicin (DOX). Controlled drug release was effectively achieved under 980 nm NIR i llumination . Treatment with functionalized nanoparticles significantly reduced the viability of melanoma cell lines, with an enhanced cytotoxicity being observed upon combined nanoparticle exposure and NIR illumination . Mechanistic analyses revealed that neither UCNPs nor NIR i llumination alone could induce the production of reactive oxygen species (ROS); however, their combination induced a marked increase in ROS levels in two of the three tested cell lines. Furthermore, this dual treatment promoted substantial apoptotic and/or necrotic responses across all cell models. These findings underscore the potential of UCNP@MSN nanoplatforms, equipped with thermoresponsive ga tes , as efficient photoactivated drug delivery systems for melanoma therapy. T2 - Conference Jornadas CICECO CY - Aveiro, Portugal DA - 09.10.2025 KW - Nano KW - Particle KW - Lanthanide KW - Upconversion KW - Surface chemistry KW - Mesoporous silica KW - Doxorubicin KW - Nanomedicine KW - Triggered release KW - pH KW - Cellular uptake KW - Toxicity KW - Folate KW - Ligand PY - 2025 AN - OPUS4-64371 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oskoei, Párástu T1 - Cell mechanisms induced by doxorubicin-loaded UCNP@MSN nanoparticles with a thermosresponsive nanovalve in melanoma cells N2 - Upconversion nanoparticles (UCNPs) exhibit several remarkable optical properties, including excitation by near infrared (NIR) light, which enables deep tissue penetration, multiple distinct emission bands across a wide range of wavelengths, long luminescen ce lifetimes, and high photostability. These features make them particularly attractive for various biomedical applications. Mesoporous silica nanoparticles (MSNs), functionalized with nanovalves or specific coatings, have been explored for controlled and targeted drug delivery, where therapeutic agents are encapsulated within the nanopores, allowing spatiotemporal release 1 3 ]]. Among the promising approaches, photoactivated drug delivery systems have drawn considerable interest due to their versatility and potential. One relevant application is in the treatment of melanoma, an aggressive form of skin cancer with a rising global incidence. In advanced stages, conventional therapies often fail to achieve complete tumour eradication, resulting in poor prognose s 4 In this study, UCNPs were coated with a mesoporous silica shell to form core shell UCNP@MSN nanoparticles, which were further functionalized with thermoresponsive retro Diels Alder nanovalves and loaded with doxorubicin (DOX), a chemotherapeutic drug used in melanoma treatment. Upon exposure to 980 nm NIR light, DOX release was successfully triggered in the culture medium. Exposure to functionalized UCNPs decreased the viability of the tested melanoma cell lines, with further reductions observed when the ex posure to the nanoparticles was combined with irradiation. Subsequently, t he toxicity mechanisms were evaluated and showed that w hile individual treatments with either the functionalized UCNPs or NIR irradiation alone had no effect on reactive oxygen species (ROS) production, their combination significantly increased ROS levels in two of the three tested cell lines. This combined treatment also led to notable increases in apoptotic , necrotic or both type of cells’ percentages on all cell lines. Overall, these findings highlight the potential of these nanoparticles with thermoresponsive gating mechanisms as effective platforms for targeted drug delivery in melanoma therapy. T2 - EUROTOX 2025 CY - Athens, Greece DA - 14.09.2025 KW - Nano KW - Particle KW - Lanthanide KW - Upconversion KW - Surface chemistry KW - Mesoporous silica KW - Doxorubicin KW - Nanomedicine KW - Triggered release KW - pH KW - Cellular uptake KW - Toxicity KW - Folate KW - Ligand PY - 2025 AN - OPUS4-64372 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Oskoei, Párástu T1 - Effects of upconversion nanoparticles with a thermo-responsive nanovalve loaded with doxorubicin in melanoma cells N2 - Melanoma skin cancer has an increasingly higher incidence , and w hen detected in advanced stages, tumour eradication is often incomplete, contributing to poor prognosis with conventional treatments. Upconversion nanoparticles (UCNPs) have unique properties, such as excitability under near infrared (NIR) excitation light, which confers a relatively high penetration depth in tissue that allow their effective use in several biomedical applications Mesoporous silica nanoparticles (MSN) with nanovalves or derived coatings have widely been used for triggered and targeted drug delivery in the past. Anticancer drugs can be loaded into the pores of MSN, enabling controlled drug release. In this work, UCNPs were coated with a mesoporous silica shell yielding UCNP@MSN core shell nanoparticles which were equipped with thermoresponsive retro Diels Alder nanovalves and then loaded with DOX , a chemotherapeutic agent for melanoma treatmen t (UCNP@MSN DOX) Subsequent DOX release from this drug delivery system was triggered by 980 nm NIR light. Melanoma cells exposed to UCNP@MSN DOX or the NIR laser exhibited no change in ROS production , while the combination of both induced an increase in ROS production. This combination of conditions also induced changes on apoptosis and necrosis levels. These findings underscore the potential use of UCNP @MSN drug delivery systems with thermoresponsive caps as effective drug delivery platforms for melanoma therapy. T2 - VII iBiMED Symposium CY - Aveiro, Portugal DA - 23.05.2025 KW - Nano KW - Particle KW - Lanthanide KW - Upconversion KW - Surface chemistry KW - Mesoporous silica KW - Doxorubicin KW - Nanomedicine KW - Triggered release KW - pH KW - Cellular uptake KW - Toxicity KW - Folate KW - Ligand PY - 2025 AN - OPUS4-64373 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute T1 - Standardized Measurements of Surface Functionalities on Nanoparticles - F. Synthesis and characterization of functional nanocomposite materials N2 - Engineered nanoparticles (NPs) with various chemical compositions and surface functionalities are routinely and commonly fabricated for industrial applications such as medical diagnostics, drug delivery, sensing, catalysis, energy conversion and storage, opto-electronics, and information storage. NP function, their interaction with biological species, and also their environmental fate are largely determined by the surface functionalities of the particles. Reliable, reproducible, and standardized surface characterization methods are therefore vital for quality control of NPs, determination of their applicability, and mandatory to meet increasing concerns regarding their safety. In addition, industry as well as international standardization organizations, regulatory agencies, and policymakers need validated and standardized measurement methods and reference materials. However, methodologies for determining NP surface properties, including the amount, chemical composition, and homogeneity of surface functionalities and coatings are largely non-standardized up until now. Suitable methods for determining surface functionalities on ligand-stabilized core and core/shell NPs include advanced techniques such as traceable quantitative nuclear magnetic resonance (qNMR), as well as X-ray electron spectroscopy (XPS) and time of flight secondary ion mass spectrometry (ToF-SIMS), and simpler optical and electrochemical methods. The latter, typically less costly methods are often used by SMEs, e.g., for quality control. To validate methods, establish measurement uncertainties, test reference materials, and produce reference data, international interlaboratory comparisons (ILC) on NP surface functionalization measurements are required to provide well characterized test and reference nanomaterials including benchmark values.[1] These needs are addressed by the current European metrology project SMURFnano, involving 12 partners from different National Metrology Institutes, designated and research institutes, two university groups as well as one large company and one SME producing NPs. This project, as well as first results derived from the development of test and reference materials with a well characterized surface chemistry, and ongoing interlaboratory comparisons, will be presented. T2 - Shift 2025 CY - La Laguna, Tenerife DA - 13.10.2025 KW - Nano KW - Particle KW - Silica KW - Iron oxide KW - Lanthanide KW - Metrology KW - Quality assurance KW - Reference material KW - Surface chemistry KW - Size KW - Shape KW - Particle number concentration KW - Method KW - Optical assay KW - qNMR KW - Validation KW - Potentiometry KW - XPS KW - ILC KW - Standardization PY - 2025 AN - OPUS4-64370 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Riedel, Juliane T1 - New PFAS reference materials for environment and consumer products N2 - Per- and polyfluoroalkyl substances (PFAS) are a large group of emerging organic pollutants that contaminate the environment, food, and consumer products. They have a wide range of applications due to their water- and oil-repellent properties, as well as their chemical and thermal stability. However, the use of PFAS has raised concerns due to their persistence in the environment and their adverse health effects, leading to regulations aimed at controlling their use and minimizing exposure. Substances such as PFOS, PFHxS, and PFOA are listed in the Stockholm Convention on Persistent Organic Pollutants (POP Regulation, EU 2019/1021). Maximum levels have been set for PFAS in environmental matrices such as soil and water, but also for textiles as a relevant area of circular economy. Reliable PFAS analysis leads to an increasing global demand for certified reference materials (CRM). However, CRMs for PFAS in soils and textiles are rare or currently not available. To improve the metrological infrastructure and support PFAS measurements, two CRMs for PFAS in soil (BAM-U027) and PFAS in textiles (BAM-B003) based on ISO 17034 and ISO 33405 were developed. This poster provides an overview of the different steps for the preparation and characterization of these two reference materials. The assignment of the certified mass fractions for relevant PFAS targets (18 PFAS compounds for BAM-B003) is based on isotope dilution HPLC-MS/MS at three independent workplaces. The results of the BAM in-house study on BAM-U027 were supported by an interlaboratory comparison study. T2 - PFAS – Challenges and Scientific Perspectives in Human Health Risk Assessment CY - Berlin, Germany DA - 08.10.2025 KW - Quality assurance KW - Reference material KW - PFAS in textiles KW - PFAS in soil PY - 2025 AN - OPUS4-64356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Abad, Carlos A1 - Jegielka, Dennis A1 - Aloysius, Allen A1 - Recknagel, Sebastian T1 - SI-traceable total analysis of nitrate and nitrite by isotope dilution optical spectroscopy and its application to Berlin surface waters N2 - Accurate nitrate and nitrite data support water-quality regulation, yet routine methods rely on external calibration and rarely achieve SI traceability. We report a calibration-free determination of nitrate and nitrite by combining isotope dilution with high-resolution continuum-source graphite furnace molecular absorption spectrometry (ID-HR-CS-GF-MAS). A 15N-enriched nitrate spike (its concentration verified by reverse isotope dilution against the standard reference material NIST 3185) provides the SI link, and it is gravimetrically added to samples; nitrate and residual nitrite are converted in situ to nitric oxide (NO), whose 215 nm band is recorded at a pixel resolution of λ/Δλ ≈ 140 000. The 0.2127 nm shift between 14NO and 15NO electronic spectra is resolved, and a three-latent-variable partial least squares regression model yields the 15N/14N ratio with 0.3% precision. Instrumental LoD values of 4.8 ng (14N) and 3.2 ng (15N) translate to a method LoD of 4.8 ng of nitrogen (equivalent to 1.05 mg L−1 NO3− for a 20 μL aliquot). The furnace program allows for successive drying/pyrolysis loops, so additional 20 μL aliquots can be layered onto the graphite platform. Alternatively, a 10 mL anion-exchange solid-phase extraction step concentrates nitrate and nitrite fivefold, allowing for the analysis of even lower sample concentrations. Results for four certified reference materials (2.9 to 1000 mg L−1 NO3−) agreed with certified values, giving relative expanded uncertainties of 2 to 4%. Analysis of twenty Berlin surface-water samples revealed concentrations ranging from 0.10 to 7.3 mg L−1 NO3−, indicating that the Panke River and Teltow Canal are the primary sources of nitrogen. ID-HR-CS-GF-MAS thus delivers ID-MS-level accuracy in a few minutes per run with bench-top optics, and, with optional on-platform or SPE pre-concentration, extends SI-traceable nitrate/nitrite monitoring into the low-ng regime. KW - Isotope dilution KW - Nitrate and nitrite determination KW - SI-traceable quantification KW - Calibration-free analysis KW - Water quality KW - Berlin surface waters KW - NO molecular absorption bands PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643785 DO - https://doi.org/10.1039/D5JA00252D SN - 0267-9477 VL - 40 IS - 10 SP - 2692 EP - 2701 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Morcillo, Dalia A1 - Winckelmann, Alexander A1 - Oelze, Marcus A1 - Leonhardt, Robert A1 - Schmidt, Anita A1 - Richter, Silke A1 - Recknagel, Sebastian A1 - Vogl, Jochen A1 - Panne, Ulrich A1 - Abad, Carlos T1 - Exploring Age-Induced Lithium Isotope Fractionation in Lithium-Ion Batteries using Microwave-Induced Cold Nitrogen Plasma Mass Spectrometry N2 - This study explores Microwave-Inductively Coupled Atmospheric-pressure Plasma Mass Spectrometry (MICAP-MS) as a cost-effective alternative to Multi-Collector Inductively Coupled Plasma Mass Spectrometry (MC-ICP-MS) for analyzing lithium isotopic composition in lithium-ion batteries (LIBs). We investigate the performance of MICAP-MS in measuring Li isotope ratios in new and aged commercial lithium cobalt oxide (LCO) batteries. Our results show that MICAP-MS, operating under cold plasma conditions at 800 W with an 8 mm torch position, achieves results metrologically compatible with MC-ICP-MS, with a precision ranging from 0.6‰ to 3.4‰ for δ7Li values. MICAP-MS benefits from a dielectric resonator for uniform plasma, better ion velocity control, and higher energy efficiency. Optimal settings were identified with dwell times of 10 ms for 6Li and 1 ms for 7Li. The study of LIBs revealed that 6Li migrates towards the anode over multiple charge–discharge cycles, causing 7Li to accumulate in the cathode, a fractionation effect that becomes more pronounced with prolonged cycling. MICAP-MS provides a cost-effective, precise alternative to MC-ICP-MS, with lower operational costs and enhanced portability, advancing the study of isotopic fractionation and aging in lithium-ion batteries. KW - MICAP-MS KW - Lithium KW - Battery aging KW - Lithium isotopes KW - Nitrogen plasma KW - Isotope fractionation KW - lithium cobalt oxide KW - LCO PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643777 DO - https://doi.org/10.1039/d4ja00324a SN - 0267-9477 SP - 1 EP - 11 PB - Royal Society of Chemistry (RSC) AN - OPUS4-64377 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Recknagel, Sebastian A1 - Richter, Silke A1 - Hoppe, Marion A1 - Meckelburg, Angela A1 - Prinz, Carsten A1 - Roik, Janina A1 - Abad, Carlos T1 - Powering precision: development of a certified reference material for elemental composition analysis of lithium nickel manganese cobalt oxide (Li-NMC) cathode material for lithium-ion batteries N2 - This work presents the development and certification of the world’s first certified reference material (CRM), BAM-S014, for a lithium nickel manganese cobalt oxide (LiNi0.33Mn0.33Co0.33O2 or Li-NMC 111) cathode material—an integral component in high-energy-density lithium-ion batteries that power electric vehicles (EVs), portable electronics, and stationary energy storage systems. By providing certified mass fractions for 11 elements, this CRM addresses a critical need for accurate and traceable elemental analysis, supporting quality control and regulatory compliance in the global battery industry. Ensuring reliable and harmonized measurements supports the efficient use of resources, including the reuse of recycled materials, and ultimately helps maintain product performance and safety. The values were assigned through an interlaboratory comparison involving 16 participating laboratories and various analytical techniques such as inductively coupled plasma optical emission spectrometry (ICP-OES), inductively coupled plasma mass spectrometry (ICP-MS), X-ray fluorescence (XRF) spectrometry, and combustion analysis. In addition to chemical characterization, the certification process includes homogeneity and stability testing of the candidate material. Details are provided on the analytical methods used for chemical characterization and the calculation of the uncertainties of the certified mass fractions. In addition to detailing the development of the CRMs, this work provides an overview of ongoing standardization activities in Li-component analysis, thereby guiding the calibration of analytical methods and contributing to the establishment of globally accepted standards for evaluating energy storage materials and advancing sustainable mobility and clean energy solutions. KW - Certified reference material KW - Lithium nickel manganese cobalt oxide KW - LNMC KW - Lithium-ion battery KW - Cathode material PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643763 DO - https://doi.org/10.1007/s00216-025-05766-7 SN - 1618-2642 VL - 417 IS - 12 SP - 2643 EP - 2653 PB - Springer Nature AN - OPUS4-64376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Recknagel, Sebastian T1 - Production of reference materials - not only for batteries N2 - The presentation describes the basic procedure used by BAM to produce certified reference materials. In particular, BAM's reference material activities in the field of lithium batteries are discussed. Following the first NMC 111 reference material, which is already commercially available, further materials are in production, including black masses and lithium carbonate. T2 - Rigaku Battery Forum 2025 CY - Neu-Isenburg, Germany DA - 24.06.2025 KW - Reference material KW - Li-battery KW - Cathode material PY - 2025 AN - OPUS4-64374 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Obenlüneschloß, Jorit A1 - Boysen, Nils A1 - Rönnby, Karl A1 - Muriqi, Arbresha A1 - Hoffmann, Volker A1 - Abad, Carlos A1 - Rogalla, Detlef A1 - Brokmann, Ulrike A1 - Rädlein, Edda A1 - Nolan, Michael A1 - Devi, Anjana T1 - Rare Mononuclear Lithium–Carbene Complex for Atomic Layer Deposition of Lithium Containing Thin Films N2 - Lithium is the core material of modern battery technologies and fabricating the lithium‐containing materials with atomic layer deposition (ALD) confers significant benefits in control of film composition and thickness. In this work, a new mononuclear N‐heterocyclic carbene (NHC) stabilized lithium complex, [Li(tBuNHC)(hmds)], is introduced as a promising precursor for ALD of lithium‐containing thin films. Structural characterization is performed, comparing density functional theory (DFT) and single‐crystal X‐ray diffraction (SC‐XRD), confirming a rare mononuclear structure. Favorable thermal properties for ALD applications are evidenced by thermogravimetric analysis (TGA). The compound exhibits a low melting point, clean evaporation, and its volatility parameters are encouraging compared to other lithium precursors. ALD trials using [Li(tBuNHC)(hmds)] with ozone demonstrate its effectiveness in depositing LiSixOy films. The ALD process exhibits a saturated growth per cycle (GPC) of 0.95 Å. Compositional analysis using Rutherford backscattering spectrometry/nuclear reaction analysis (RBS/NRA), X‐ray photoelectron spectrometry (XPS), and glow discharge optical emission spectrometry (GD‐OES), confirms the presence of lithium and silicon in the expected ratios. This work not only presents a new ALD precursor but also contributes to the understanding of lithium chemistry, offering insights into the intriguing coordination chemistry and thermal behavior of lithium complexes stabilized by NHC ligands. KW - Atomic layer deposition (ALD) KW - N-heterocyclic carbene (NHC) ligands KW - Lithium ALD precursor chemistry KW - Mononuclear Li–carbene complex [Li(tBuNHC)(hmds)] KW - Li-silicate thin films (LiSixOy) KW - Thermal properties & TGA/volatility KW - Compositional analysis (RBS/NRA, XPS, GD-OES) PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643790 DO - https://doi.org/10.1002/anie.202513066 SN - 1433-7851 SP - 1 EP - 11 PB - Wiley VHC-Verlag AN - OPUS4-64379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rua-Ibarz, Ana A1 - Nakadi, Flávio V. A1 - Bolea-Fernandez, Eduardo A1 - Bazo, Antonio A1 - Battistella, Beatrice A1 - Matiushkina, Anna A1 - Resch-Genger, Ute A1 - Abad, Carlos A1 - Resano, Martín T1 - Discrete entity analysis via microwave-induced nitrogen plasma–mass spectrometry in single-event mode N2 - In this work, single-event microwave-induced nitrogen plasma–mass spectrometry (single-event MINP-MS) was evaluated for the first time for the analysis of discrete entities such as nanoparticles, biological cells, and microplastics. Nitrogen (N2) effectively overcomes Ar-based polyatomic interferences, enabling (ultra)trace element determination of Fe and Se using their most abundant isotopes, 56Fe (91.66%) and 80Se (49.82%). Iron oxide nanoparticles (Fe2O3 NPs) ranging from 20 to 70 nm were accurately characterized, with excellent agreement with established sizing techniques, such as transmission electron microscopy (TEM) and dynamic light scattering (DLS). A limit of detection (LoD) of 8.6 ag for Fe─equivalent to an LoDsize of 19 nm for Fe2O3─was achieved, which is significantly lower than recent values reported for high-end quadrupole-based ICP-MS. Selenium nanoparticles (SeNPs) of 150 and 250 nm were also accurately characterized, without the N2-based plasma experiencing issues handling relatively large metallic NPs (linearity, R2 = 0.9994). Se-enriched yeast cells (SELM-1 certified reference material) were successfully analyzed via single-cell MINP-MS using external calibration based on SeNPs and a transport efficiency-independent approach. In addition, 2–3 μm polystyrene (PS) and polytetrafluoroethylene (PTFE) were accurately sized by monitoring 12C+, confirming the method’s suitability for handling micrometer-sized polymeric materials (microplastics). The average duration of individual events (680 ± 160 μs) suggests that the digestion of individual entities in N2-based plasmas is comparable to that in Ar-based plasmas. These results open new avenues for this instrumentation as an alternative to ICP ionization sources, also in the context of discrete entity analysis. KW - Microwave-Induced Nitrogen Plasma KW - Discrete entity analysis KW - Particle/droplet event counting KW - Comparison to SP-ICP-MS methodologies KW - Nitrogen plasma vs. argon ICP trade-offs KW - Trace elemental quantification at the single-entity level KW - Time-resolved mass spectrometry for discrete entities PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643825 DO - https://doi.org/10.1021/acs.analchem.5c04341 SN - 0003-2700 SP - 1 EP - 8 PB - American Chemical Society (ACS) AN - OPUS4-64382 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -